Dokumen - Pub Transport Processes and Separation Technologies 1st Ed 9783030478551 9783030478568

Advanced Structured Materials
J. M. P. Q. Delgado
A. G. Barbosa de Lima Editors
Transport
Processes and
Separation
Technologies
Volume 133
Series Editors
Andreas Öchsner, Faculty of Mechanical Engineering, Esslingen University of
Applied Sciences, Esslingen, Germany
Lucas F. M. da Silva, Department of Mechanical Engineering, Faculty of
Engineering, University of Porto, Porto, Portugal
Holm Altenbach , Faculty of Mechanical Engineering,
Otto von Guericke University Magdeburg, Magdeburg, Sachsen-Anhalt, Germany
Common engineering materials reach in many applications their limits and new
developments are required to fulfil increasing demands on engineering materials.
The performance of materials can be increased by combining different materials to
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This book series addresses the fundamental relationship between materials and their
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etc.) and applications.
The topics of Advanced Structured Materials include but are not limited to
• classical fibre-reinforced composites (e.g. glass, carbon or Aramid reinforced
plastics)
• metal matrix composites (MMCs)
• micro porous composites
• micro channel materials
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• truss structures
• nanocomposite materials
• biomaterials
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• concrete
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• smart materials
Advanced Structured Materials is indexed in Google Scholar and Scopus.
More information about this series at http://www.springer.com/series/8611

J. M. P. Q. Delgado A. G. Barbosa de Lima
•
Editors
Transport Processes
and Separation Technologies
123
Editors
J. M. P. Q. Delgado A. G. Barbosa de Lima
CONSTRUCT-LFC, Department of Civil Department of Mechanical Engineering
Engineering Federal University of Campina Grande
University of Porto Campina Grande, Paraíba, Brazil
Porto, Portugal
ISSN 1869-8433 ISSN 1869-8441 (electronic)

ISBN 978-3-030-47855-1 ISBN 978-3-030-47856-8 (eBook)
https://doi.org/10.1007/978-3-030-47856-8
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Contents
1 Clay Ceramic Materials: From Fundamentals and Manufacturing

to Drying Process Predictions . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 1
A. G. Barbosa de Lima, J. M. P. Q. Delgado, L. P. C. Nascimento,
E. S. de Lima, V. A. B. de Oliveira, A. M. V. Silva, and J. V. Silva
1.1 Ceramic Materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
1.1.1 History . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
1.1.2 Fundamental Concepts . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
1.1.3 The Ceramic Industry and Clay Products . . . . . . . . . . . . . 3
1.1.4 Red Ceramic Product Manufacturing Process . . . . . . . . . . 5
1.2 The Drying Process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
1.2.1 General Principles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
1.2.2 The Mathematical Modeling of the Drying
Process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
1.3 Lumped Model Application: Drying of Clay Ceramic Brick . . . . . 13
1.3.1 The Experimental Data . . . . . . . . . . . . . . . . . . . . . . . . . . 14
1.3.2 Phenomenological Mathematical Modeling . . . . . . . . . . . . 15
1.3.3 Results Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
1.4 Concluding Remarks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
2 Vegetable Fiber Drying: Theory, Advanced Modeling
and Application . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 31
J. F. Brito Diniz, A. R. C. de Lima, I. R. de Oliveira, R. P. de Farias,
F. A. Batista, A. G. Barbosa de Lima, and R. O. de Andrade
2.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
2.2 Drying of Sisal Fibers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
2.2.1 Experimental Study . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
2.2.2 Theoretical Study . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
2.2.3 Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52
2.3 Conclusions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60
v
vi Contents
3 Foam-Mat Drying Process: Theory and

Applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 61
E. R. Mangueira, A. G. Barbosa de Lima, J. de Assis Cavalcante,
N. A. Costa, C. C. de Souza, A. K. F. de Abreu, and A. P. T. Rocha
3.1 Drying Theory of Porous Materials . . . . . . . . . . . . . . . . . . . . . . . 62
3.1.1 Fundamentals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62
3.1.2 Mathematical Modeling in Drying . . . . . . . . . . . . . . . . . . 64
3.2 Foam-Mat Drying . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 66
3.2.1 General Foundations . . . . . . . . . . . . . . . . . . . . . . . . . . . . 66
3.2.2 Different Methods for Foam Formation . . . . . . . . . . . . . . . 68
3.2.3 Foaming Agents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69
3.3 Applications: Drying of Egg White and Yolk of Duck Egg . . . . . . 70
3.3.1 Material Preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 70
3.3.2 Experimental Planning . . . . . . . . . . . . . . . . . . . . . . . . . . . 70
3.3.3 Experiment of Foam-Mat Drying . . . . . . . . . . . . . . . . . . . 72
3.3.4 Analysis of Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73
3.4 Final Considerations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 82
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 85
4 Drying Process of Jackfruit Seeds . . . . . . . . . . . . . . . . . . ......... 89
T. M. Q. de Oliveira, R. A. de Medeiros, V. S. O. Farias,
W. P. da Silva, C. M. R. Franco, and A. F. da Silva Júnior
4.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 90
4.2 Methodology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 91
4.2.1 Experiments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 91
4.2.2 Mathematical Modeling . . . . . . . . . . . . . . . . . . . . . . . . . . 92
4.3 Results Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 98
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 102
5 Spouted Bed Drying of Fruit Pulps: A Case Study on Drying
of Graviola (Annona muricata) Pulp . . . . . . . . . . . . . . . . . . . . . . . . . 105
F. G. M. de Medeiros, I. P. Machado, T. N. P. Dantas, S. C. M. Dantas,
O. L. S. de Alsina, and M. F. D. de Medeiros
5.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 106
5.2 Fundamentals of Spouted Bed Drying . . . . . . . . . . . . . . . . . . . . . 107
5.3 Spouted Bed Drying of Fruit Pulps . . . . . . . . . . . . . . . . . . . . . . . 109
5.4 Phytochemicals on Spouted Bed Dried Fruit
Powders . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 111
5.4.1 Impact of Spouted Bed Drying on the Phytochemicals
Content . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 112
5.4.2 Use of Drying Carriers . . . . . . . . . . . . . . . . . . . . . . . . . . . 115
5.5 Spouted Bed Drying of Graviola (Annona muricata) Pulp:
A Case Study . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 116
5.5.1 Fundamentals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 117
5.5.2 Materials and Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . 118
Contents vii
5.5.3 Results and Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . 122

5.5.4 Final Comments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 140
5.6 Conclusions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 141
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 142
6 Osmo-convective Dehydration of Fresh Foods: Theory
and Applications to Cassava Cubes . . . . . . . . . . . . . . . . . . . . . . . . . 151
T. R. Bezerra Pessoa, A. G. Barbosa de Lima, P. C. Martins,
V. C. Pereira, T. C. O. Alves, E. S. da Silva, and E. S. de Lima
6.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 152
6.1.1 Drying Fundamentals . . . . . . . . . . . . . . . . . . . . . . . . . . . . 152
6.1.2 The Focus of This Work . . . . . . . . . . . . . . . . . . . . . . . . . 153
6.2 Application: Hybrid Drying of Cassava Cubes . . . . . . . . . . . . . . . 153
6.2.1 The Raw Material . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 153
6.2.2 Osmotic Dehydration Tests . . . . . . . . . . . . . . . . . . . . . . . 154
6.2.3 Convective Drying Tests . . . . . . . . . . . . . . . . . . . . . . . . . 158
6.2.4 Results and Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . 160
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 178
7 Heat Transfer in a Packed-Bed Elliptic Cylindrical Reactor:
Theory, Heterogeneous Transient Modeling, and
Applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 185
A. S. Pereira, R. M. da Silva, R. S. Santos, A. G. Barbosa de Lima,
R. O. de Andrade, W. M. P. B. de Lima, and G. S. de Lima
7.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 186
7.2 Porous Media and Packed-Bed Reactors . . . . . . . . . . . . . . . . . . . 186
7.2.1 Porous Media . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 186
7.2.2 Chemical Reactors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 190
7.3 Heat Transfer in Fixed-Bed Elliptical Reactor via Two-Phase
Model . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 191
7.3.1 Physical Problem and Geometry . . . . . . . . . . . . . . . . . . . . 191
7.3.2 Governing Equations . . . . . . . . . . . . . . . . . . . . . . . . . . . . 194
7.3.3 Numerical Treatment of Heat Transport
Equations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 200
7.4 Application: Heat Transfer in an Elliptic Cylindrical Reactor
Filled with Spheroidal Particles . . . . . . . . . . . . . . . . . . . . . . . . . . 205
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 213
Chapter 1
Clay Ceramic Materials: From
Fundamentals and Manufacturing
to Drying Process Predictions
A. G. Barbosa de Lima, J. M. P. Q. Delgado, L. P. C. Nascimento,

E. S. de Lima, V. A. B. de Oliveira, A. M. V. Silva, and J. V. Silva
Abstract This chapter is devoted to study heat and mass transfer and dimension
variations of arbitrary-shaped porous materials. The focus is on the drying process
of clay ceramic materials. Here, different topics related to history, manufacturing,
drying process, phenomenological lumped modeling, and parameters estimation are
present and discussed. Emphasis is given to industrial clay bricks, with theoretical
and experimental approaches.
Keywords Drying · Brick · Experimental · Simulation · Lumped model
A. G. B. de Lima (B) · L. P. C. Nascimento · E. S. de Lima · A. M. V. Silva · J. V. Silva

Department of Mechanical Engineering, Federal University of Campina Grande, Av. Aprígio
Veloso, 882, Bodocongó, Campina Grande, PB 58429-900, Brazil
e-mail: antonio.gilson@ufcg.edu.br
L. P. C. Nascimento
e-mail: lucaspereira.cn@hotmail.com
E. S. de Lima
e-mail: limaelisianelima@hotmail.com
A. M. V. Silva
e-mail: andersonmelch@gmail.com
J. V. Silva
e-mail: jvieira7@gmail.com
J. M. P. Q. Delgado
CONSTRUCT-LFC, Civil Engineering Department, Faculty of Engineering, University of Porto,
Porto, Portugal
e-mail: jdelgado@fe.up.pt
V. A. B. de Oliveira
State University of Paraiba, Rodovia PB 075, S/N, km 1, Guarabira, PB 58200-000, Brazil
e-mail: profvitaloliveira@gmail.com
© The Editor(s) (if applicable) and The Author(s), under exclusive license 1
to Springer Nature Switzerland AG 2021
J. M. P. Q. Delgado and A. G. Barbosa de Lima (eds.), Transport Processes
and Separation Technologies, Advanced Structured Materials 133,
https://doi.org/10.1007/978-3-030-47856-8_1
2 A. G. B. de Lima et al.
1.1 Ceramic Materials
1.1.1 History
The art of pottery is one of the oldest in the world due mainly to the abundance of
clay and the ease of extraction and fabrication. There is evidence of activity of this
art in almost all peoples of antiquity and to improve their quality of life, man has
always been seeking to perfect the various uses of ceramic materials.
Pottery was invented in the Neolithic (polished stone age) in 25000 BC and during
this period prehistoric man-made wicker baskets with clay, that is, the first objects
were intended to store grain and liquids and were just simple objects. Later, the
plasticity of clays was discovered, where it was noted that by adding water the clay
could be molded, dried in the sun, and hardened when exposed to high temperatures.
Following, ceramics were widely used for various purposes, such as pieces with
nozzles and handles made with relief images, or with living paintings that were
considered decorative objects (Cavalcanti 2010).
Each civilization and each culture have developed its own forms and characteris-
tics in the use of clay, so that pottery is one of the greatest auxiliaries in historical
research. One of the greatest ancient peoples who have strong ties to ceramics is the
Greeks, who for a long time produced the finest pieces in the Mediterranean world.
It was common at that time to sell these products at fairs and there was a continuous
export of generally ovoid and handled vessels (Phoenician amphora), which could
often be used to serve water, wine, and olive oil (Silva 2009).
In addition to the Greeks and Romans, other ancient peoples such as the Byzan-
tines and Arabs were responsible for transmitting their practices throughout Europe,
which consequently have varied styles of construction in their territories. It was
precisely with the growth of civil construction that the manufacture of ceramic pieces
evolved from a more artisanal activity to an industrial one. Initially, around 1850,
the first bricks were made on animal-powered molding machines, only later that the
manufacturing would go through a major leap.
Production systems were stagnant until the nineteenth century, i.e., drying was
still done in the sun, burning in trapezoidal ovens and production was still mostly by
hand. Only with the emergence of the first steam-powered machines, it was possible
to increase production as raw material extraction, preparation, and forming opera-
tions became mechanized. Thus, in the modern era countries like Spain, France and
Germany stood out in the market as producers of red ceramics and as equipment
manufacturers. It is important to highlight that Italy was one of the great pioneers in
the production of bricks in series with good quality (Silva 2016).
Later, in the mid-twentieth century, the technological development of the ceramic
industry boosted the manufacture of high strength and low weight cast structural
blocks, a major evolution compared to previously manufactured solid bricks. At this
time, including Brazil, there was a resurgence of structural masonry with ceramic
products, competing economically with conventional reinforced concrete structures
in medium-sized buildings (up to about 8–10 floors) (Silva 2009).
1 Clay Ceramic Materials: From Fundamentals … 3
Following, the ceramic industry underwent major developments, now based on

research, technology, and studies by specialized laboratories. Along with the study
of ceramics, the study of ovens, better glazing, molding apparatus, dry molding, high
strength porcelain was developed and it was possible that the field of use of ceramics
grew a lot, enabling aerospace and technology applications, such as space shuttle
thermal shielding, nanofilm production, sensors to detect toxic gases, and among
others.
With regard to Brazil, construction ceramics currently occupies a prominent place
in the national economy. Great growth came in the industry when the Government’s
Growth Acceleration Programs (PAC) and My House My Life (MCMV) were imple-
mented. Therefore, because it represents a sector of great importance in job creation
and income distribution, it has received the attention of government sectors, research
institutes, universities, and various entities (Rodrigues Neto and Mota 2016).
1.1.2 Fundamental Concepts
Ceramic or ceramic material can be defined as any non-metallic and inorganic mate-
rial whose structure, after heat treatment at high temperatures, is wholly or partially
crystallized. They are composed of total or predominantly ionic interatomic bonds,
but having some covalent character. Ceramics are known to have different raw mate-
rials in their composition, but the main one is clay, which can be defined as an earthy,
thin, and natural material that, by adding water, acquires a certain plasticity and can
be easily molded (Callister 2007; Callister and Rethwisch 2008).
Ceramic materials have a wide range of structural arrangement types. The exis-
tence of several ceramic phases makes possible the combinations of metallic and
non-metallic atoms (which form many structural arrangements) making them widely
applicable in various sectors besides construction. It is noteworthy that the structure
of the ceramic material defines its properties (Silva 2009; Callister 2007; Callister
and Rethwisch 2008).
1.1.3 The Ceramic Industry and Clay Products
The ceramic industry sector plays a very important role in Brazil’s economy, with a
share of approximately 1% of GDP. Gaining prominence, the evolution of Brazilian
companies has been very fast, mainly due to the abundance of natural raw material,
alternative sources of energy, and the availability of practical technologies. Among
the regions of the country, the ones that stand out and have a large concentration of
industries are the Southeast and the South; this is because they have higher demo-
graphic density, greater industrial and agricultural activity, better infrastructure, and
better income distribution. It is noteworthy that the other regions of the country have
shown a certain degree of development, especially in the northeast due to the large
occurrence of mineral resources, abundance of natural gas, expanding market, and

great export potential (Silva 2009).
Despite the greatness of the Brazilian ceramics industry and its great potential,
it is quite heterogeneous. In addition to the red ceramics industries, several mining
companies, ceramic tiles, sanitary ware, thermal ceramics, enamels, and others have
already been installed or are in phase of deployment. However, within the current
scenario of globalization, it can be said that the segments that are best adapted and
structured are the covering, refractory, and sanitary ware. In the other segments, there
are some modern companies that stand out from the others, but this contingent is not
so expressive.
One of the most important areas in the industry is related to red ceramic products.
According to data from SEBRAE/Brazil (SEBRAE 2019), there is a range of 8500–
11,000 companies in the country, generating around 300,000 direct jobs and 1.5
million indirect jobs. Despite having good numbers, the production activity of the
sector has a great technological backwardness, since most of the companies are of
small or medium size and family order. It is also worth noting that this large number of
jobs that the sector generates is caused by the low level of knowledge and investment
required to start activities.
In the northeast region, and especially in the State of Paraíba (Brazil), there is
a marked industrial activity in this area. There are around 60 active red ceramic
factories throughout the state, distributed in at least 30 towns, offering about 3000
direct jobs. Research carried out in the state of Paraíba shows, as to geographic
regions and watersheds, that studies in the area are concentrated in some specific
regions of the state, especially in the coast and in the Agreste. On the other hand,
in the Sertão and Cariri regions there is a large concentration of potentially usable
deposits, but, to date, there is no systematic study regarding their exploitation and
use.
Red ceramics encompass various products such as blocks, tiles, solid bricks,
plumbing pipes, slabs, castings, and also expanded clay, which are often used in
construction. It is also present in household items such as filters, decorative vases,
and clay pots. This type of ceramics has the nomenclature “red” due to the presence
of ferrous compounds that develop reddish coloration.
The basic raw material of structural ceramics is common clay, which is used in
a single dough to shape products, unlike other segments of the ceramics industry
that mix clay with other substances such as talc, kaolin, and others (Callister 2007;
Callister and Rethwisch 2008; Cabral et al. 2008). Natural clay seeks an ideal compo-
sition of plasticity and fusibility so that it provides good workability and mechanical
resistance during firing.
Red ceramic products are classified according to the manufacturing process used
and can be pressed or extruded. In summary, red or structural ceramics can be grouped
generically according to Table 1.1, as follows.
The clay used for the production of red ceramics is composed of a large amount
of amorphous material, in other words, those that do not have long-distance spatial
ordering; however, the crystalline material predominates, which is grouped in well-
defined mineralogical species. From the physicochemical point of view, clays can be
Table 1.1 Types and characterization of red ceramics (Silva 2009)

Types Description
Porous Solid bricks, pressed solid bricks, laminated bricks, hollow bricks,
prefabricated panels, tiles, components for slabs, tiles, conductors for electrical
cables, and others (sills, cladding plates, etc.)
Glazed Tiles, glazed glazes, laminated bricks, pipes, glazed internally, glazed internally
and externally, and unglazed
Expanded clay Obtained from thermo-expansion of some types of clays (illite). In the
production process, mineral oil is added to the ceramic mass. They are launched
in an inclined rotary kiln with a burner at the bottom
considered as dispersed mineral systems in which particles below 2 µm in diameter

predominate (Silva 2016).
A great advantage of the clay used in red ceramics is that it has great plasticity
while wet, allowing the manufacture of pieces of various shapes using simple equip-
ment. Another important point is that when cooked at more than 800 °C it has a good
mechanical resistance, making the final product suitable for various applications
(Brito 2016).
To produce bricks and tiles the clay used is generally quaternary and sometimes
tertiary. One of the main characteristics is to present, in large quantities, iron, and
alkalis in their composition. They are fine-grained and have a considerable organic
matter content, factors that are responsible for their high plasticity.
It is recommended that the clays used have easy molding, flexural strength before
and after sintering, have a reddish color after sintering, with a minimum of cracks
and warping. It is noteworthy that high levels of bivalent iron and alkaline elements
may reduce the range of vitrification and cause undesirable coloration (Silva 2009).
1.1.4 Red Ceramic Product Manufacturing Process
Red ceramics can generate a wide variety of products and for this it goes through
a specific production process, which is sometimes still poorly evolved compared to
other segments of the ceramic industry. However, due to the increasing emergence
of technological innovations in some companies, we can find good quality produc-
tion processes with high production rates. Most of these technological advances are
related to equipment automation and, consequently, the reduction of labor costs.
The production process, exemplified in Fig. 1.1, is common to all red ceramic
companies in general, with slight variations depending on the particular charac-
teristics of each raw material or end product. For example, some companies use
rudimentary equipment and others have more modern equipment, or some have a
much higher degree of production, among other differences.
The production process of pieces with red ceramic comprises several steps that
can be divided into four major stages, namely, extraction and preparation of raw
Fig. 1.1 Manufacturing flowchart of red ceramic pieces
materials, mechanical forming, thermal processing, and shipping. The following

best describes these steps:
1.1.4.1 Extraction and Preparation of Raw Materials
The manufacturing process begins with the extraction of clay, which is removed from
the deposits with the aid of backhoes and then transported to storage sheds, which
may be owned by companies or third parties. At this stage, the material goes through
a “rest”, thus undergoing chemical changes and being unpacked. Shed storage also
ensures continued production in rainy seasons. After this phase, we have the dosage,
in which the clays are proportionally dosed in a feeder coffin obeying their ceramic
characteristics.
Following the manufacturing process is disintegration, which is the step respon-
sible for bringing the hardest and most compacted clays to a disintegrator that will
crush the larger clumps of clay to facilitate subsequent operations. Then, the raw
material goes to the mixer, where it will be homogenized, thus allowing the addition
of water in the mixture to obtain adequate moisture and plasticity for extrusion.
The last step of this first major stage is lamination, which is responsible for a
thickening of the mixture, eliminating air bubbles or clumps that may have remained
so far. With the end of this stage, the raw material already prepared can be directed
to the extruders, which may even have a rolling mill attached to them.
1.1.4.2 Mechanical Forming
The mechanical conformation stage is responsible for transforming the clay plastic
mass into products with different shapes and sizes. Thus, according to the type of
product to be obtained and also depending on the plasticity characteristics of the
available raw material, it will be possible to choose the appropriate forming system.
The main systems of this stage are extrusion and cutting. Firstly, the clay mass
will take the desired shape upon entering the extruder, which contains a steel plate
perforated in a vacuum chamber. Then, through the manual or automatic cutter, the
extruded block is cut to standard sizes, thus obtaining products such as bricks, tiles,
ceramic tubes, and among others (Oliveira and Bernils 2006).
1.1.4.3 Thermal Processing
This stage consists of the drying and burning steps of the already formed parts. This
is where the composition and structure transformations will occur, generating the
final properties of the product, such as color, gloss, porosity, flexural strength, high
temperatures, and among others (Silva 2009).
During drying, a large amount of thermal energy is used to slowly and evenly
evaporate the water added during the molding process. This step usually takes place
inside drying chambers and aims to reduce the moisture content of the products from
20–25% to 3–10% after the process.
An important property of any clay is that it has water in the constitution of its
crystal lattice. Thus, during the drying process, the water that has been added is
easily removed, with the temperature starting from room temperature and reaching
approximately 110 °C. However, water that is in the clay crystal lattice will only be
removed at temperatures above 400 °C and may vary to even higher values depending
on the type of clay.
During the drying process, the clay may contract as the spaces that were occupied
by water inside the material become empty after evaporation. This shrinkage is
proportional to the degree of moisture removed. Thus, it is important to control
the process well, as a possible consequence of this shrinkage is that it can cause
deformation or cracking in the material.
Following is the firing step, in which the product is taken to a kiln and, as well
as drying, will receive an even greater amount of thermal energy. Once these steps
are completed, the product will have lower porosity and greater mechanical strength
and will also be ready for commercialization and use.
1.1.4.4 Expedition
Shipment is the final stage of the production process, where finished product is
inspected to identify excessively cracked, broken, chipped, or burned products. Then,
the parts are stored in a covered area until they leave for delivery to the customer. In
Brazil, transportation of the parts is usually made by trucks on the highways of the
country.
The thermal processing stage must be performed correctly, otherwise the parts
could present a series of defects and thus, the products will not be able to perform
their respective functions. Given this, the most common defects are as follows (Silva
2009; Silva et al. 2011):
(a) Commitments—This defect is a deformation of the part usually caused by
residual shrinkage stresses, which arise when one side of the material dries faster
than the other, i.e., it is important that the drying is done evenly. Commitments
may also arise due to poor positioning of the product on the drying support.
(b) Cracks—It is important that during the drying process the air velocity and
temperature are controlled, because when we have a very fast drying, it is
common the appearance of cracks, which are nothing more than small fissures
that start at the edges and spread until the center of the piece. Cracks may also
appear in the firing step, which may be by heating or cooling. The heating ones
are characterized by being open, little winding, and with jagged edges, while the
cooling ones are characterized by being closed and very thin, usually S-shaped
edges. It is important to point out that all drying starts must be done with the
plastic-covered part, to prevent a very fast outflow of water that is closer to the
surface, causing a localized shrinkage that can cause cracks.
(c) Black heart—This type of defect is black or gray spots that can be seen along the
cross section of the part and appear after the firing process. The existence of the
“black heart” is associated with the presence of carbon-containing compounds,
which are formed due to the small amount of oxygen, preventing the complete
oxidation of carbon compounds and organic matter.
(d) Efflorescence—Efflorescence occurs on the outer surface of the product and
is a salt deposit accumulated in some regions, which may cause undesirable
stains and colors. This defect appears as the water interferes with salts. If the
piece, after burning, absorbs moisture, the salts will be dissolved; however, if
the external environment becomes dry, the opposite process occurs, the surface
water is evaporated and the crystallization of the salts occurs.
(e) Defects related to steps before or after drying—It is common for small cracks
to occur when the clay paste is improperly mixed in the mixing step. This defect
is most pronounced in areas with higher moisture content and is quite common
in manual manufacturing processes. Finally, it is worth mentioning the problem
of moisture absorption. Depending on the type of clay, if the time elapsed from
the clay leaves the dryer to when it is introduced into the kiln is large and the
ambient absolute humidity is very high, a rehydration (reabsorption) process
may occur, which may cause breakage and/or explosion when material enters
the kiln.
1.2 The Drying Process
1.2.1 General Principles
Drying can be explained as a thermodynamic process responsible for the partial

removal of a liquid, usually water, from the porous material by providing energy to it
and providing water loss by evaporation. In this process, there is a simultaneous heat
and mass transfer, and the transport of moisture from the interior to the surface of the
material may occur in the form of liquid and/or vapor, depending on the percentage
of moisture present and the type of product (Brooker et al. 1992; Strumillo and Kudra
1986).
The drying process has become, among many other uses, one of the most important
steps in the manufacture of ceramic parts. In the case of red ceramic, this step is of
relevant importance, since if the moisture is not removed properly, severe stresses
occur inside the part, causing deformations, cracks, and reducing the quality of the
product post-drying process. Thus, it is noteworthy that the in-depth study related
to drying of ceramic materials increases the overall efficiency of the ceramic sector
by reducing losses and increasing material quality and provides an environment
conducive to progress and sustainable development.
There are three ways to classify drying: natural, artificial, or mixed. Whatever the
type of drying, it has to fulfill four basic functions: the transport of the heat necessary
for water evaporation, the removal of the produced water vapor, the reduction of the
saturated vapor layer formed on the product surface and the movement of liquid,
and/or vapor inside the part.
The process time depends on the special conditions of the drying environment,
such as temperature, relative humidity, and air velocity, and may reach periods of up
to six weeks (natural drying). Artificial drying is carried out in drying chambers or
dryers, usually taking advantage of the residual heat of the kiln, which significantly
reduces the drying time. In addition, the artificial drying period also depends on the
characteristics of the raw material, the shape of the parts, and the type of dryer.
Convective drying technique differs from other separation techniques such as
osmotic dehydration, evaporation, and decantation by the way water is removed from
the solid. In convective drying, there is a difference between the partial pressure of
the water vapor at the surface of the product and the surrounding air, which allows
the migration of the liquid from the inside and consequently the removal of the water
molecules from it. In osmotic dehydration, for example, this moisture removal may
occur due to a pressure difference between the product and a hypertonic solution,
due to a density difference, or due to temperature increase (Silva 2016; Brooker et al.
1992; Strumillo and Kudra 1986).
In order, to perform a thermodynamic analysis of drying it is necessary to under-
stand the influence of velocity, relative humidity, and temperature of the drying air on
the process. Relative humidity can be defined as the ratio of the vapor partial pressure
in the air to the vapor saturation pressure, which varies with temperature. The ability
of air to absorb water vapor will be higher when the saturation pressure of water
vapor is greater than the partial pressure of water vapor. Therefore, the ability of air
to absorb water vapor increases with temperature, so that the higher the air temper-
ature, the greater its drying capacity, in fixed conditions of the air relative humidity.
In addition, if the air is warmer, the volume of air needed for drying decreases and,
as a result, the powers of the hoods and air circulators are reduced, reducing drying
costs.
The speed with which the product is dried can be affected by many factors, such
as moisture movement mechanism, product shape, external environment conditions,
and green product porosity. Thus, it is of great importance to verify the influence
of the shape and volume of the pores in the part, because it is inside them that
is the moisture, that even under favorable conditions can be retained inside these
pores. This occurs when the surface of the part is dried very quickly, as the pores,
being very narrow, reduce moisture migration for a rate less than the evaporation
rate. Another important point is that with a higher drying air temperature and lower
relative humidity there will be an increase in drying rate.
The drying process is generally divided into four distinct phases: adaptation,
colloidal water outlet, void formation, and interstitial moisture expulsion. In the first
phase occurs the adaptation of the product to environmental conditions (tempera-
ture, relative humidity, and pressure), in which drying will be performed. In the
second phase, there is evaporation of the colloidal water, and sensible variations in
the dimensions of the part occur due to the approximation of the particles of its
microstructure. Even at this stage water continually migrates to the surface of the
part, constantly forming an evaporating saturated wet film. In the third phase occurs
the disappearance of the water film on the surface of the piece, which provokes
changes in color. The last drying phase, which is not always reached in the dryers
and is often performed in the kilns, is the expulsion of the last amounts of moisture
from interstitial origin, in which the moisture removal rate decreases to near zero
(Silva 2009).
Given the importance and complexity of the drying process, a large number of
researchers have been working intensively on its analysis. Some focus on external air
conditions, such as temperature, relative humidity, and velocity, correlated with the
product’s drying rate, while others consider the internal conditions of the product,
with emphasis on the mechanisms of moisture movement and their effects on it. In
this regard, several drying theories have been proposed to describe heat and mass
transport in capillary porous media, namely,
(a) Liquid diffusion theory;
(b) Vaporization–condensation theory;
(c) Cappilary theory;
(d) Kricher’s theory;
(e) Luikov’s theory;
(f) Philip and De Vrie’s theory;
(g) Berger and Pei’s theory;
(h) Fortes and Okos theory.
A more detailed discussion of drying theories can be found in the literature

(Brooker et al. 1992; Strumillo and Kudra 1986; Lima et al. 2014). According to
the drying theories listed before, the following mechanisms of moisture transport in
porous material have been cited in the literature:
(a) Transport of liquid by diffusion due to moisture concentration gradients;
(b) Transport of vapor by diffusion due to moisture concentration gradients and
vapor partial pressure (caused by temperature gradients);
(c) Transport by effusion (Knudsen flow) that occurs when the average free path
of vapor molecules is of the same order as the pore diameter. It is important for
high vacuum conditions such as freeze drying;
(d) Transport of vapor by thermofusion due to temperature gradients;
(e) Transport of liquids by capillary forces due to capillarity phenomena;
(f) Transport of fluid by osmotic pressure due to osmotic force;
(g) Transport of liquid due to gravity;
(h) Transport of liquid and vapor due to total pressure difference caused by external
pressure, shrinkage, high temperature, and capillarity;
(i) Transport of liquid and vapor by surface diffusion due to the migration of these
phases through the pores of the product surface.
Then, based on the drying theories and moisture migration mechanisms, several
drying models have been reported in the literature. This topic will be discussed
following.
1.2.2 The Mathematical Modeling of the Drying Process
The main objective of an appropriated drying modeling is to mathematically describe

the physical phenomena, so that it is possible to choose appropriate operating condi-
tions, the most appropriate method of drying and also to control and know the process
deeply. Thus, we can optimize the steps of drying and eliminate or minimize existing
irregularities.
The development of mathematical models to describe the drying process is
increasingly recurrent and has been studied for several decades. This is because the
process has great importance in the production of different products and also involves
complex phenomena of heat and mass transfer, linear momentum, and dimension
variations of the product.
The principle of modeling is based on having a system of mathematical equations
that completely characterizes the system to be modeled. In particular, the solution
of these equations makes it possible to predict process parameters as a function of
drying time based only on initial and boundary conditions, and some simplifications.
The starting point in mathematical modeling is the definition of the process to be
modeled, in particular the description of the input data that influence the process, as
well as the variables that depend on the process behavior.
The complexity of the drying process depends on the geometric and thermophys-
ical parameters of the material and thickness of the material layer in study. They
can then be classified in thin-layer drying models (particle level models) and thick-
layer models (dryer models). The dryer mathematical models (thick-layer model)
most used by the researchers take into account the thermophysical properties, drying
kinetics, and mass and energy balance in the device. Some researchers have applied
dryer model to predict drying process of clay ceramic materials with particular refer-
ence to industrial clay bricks (Almeida et al. 2013; Tavares et al. 2014; Almeida et al.
2016; Silva 2018). From a practical point of view, thin-layer drying is very limited.
But to have a good understanding of the thick-layer drying process it is necessary to
have thin-layer equations for the drying kinetics of a particular material under certain
predetermined operating conditions (Macedo 2016).
Several thin-layer mathematical models have been proposed to describe the rate
of moisture loss during drying and can be divided into two large groups: lumped
and distributed models. Distributed models express heat and mass transfer rates as
a function of position within the part and drying time, taking into account external
and internal resistances. Lumped models, on the other hand, express the same rates
only as a function of process time and ignoring the existing internal resistance for
heat end mass transfer.
The following general balance equation (distributed model) has been applied to
predict drying process (by diffusion only) of irregularly-shaped porous body:
d(λΦ)
= ∇ · (Γ Φ ∇Φ) + Φ (1.1)
dt
where λ and Γ Φ are transport properties. Φ is the unknow, Φ is the source term,
and t is the time.
Distributed models based on the liquid diffusion theory have been applied to
predict drying of ceramic porous materials. For example, clay plates (Silva et al.
2009), clay pipes (Santos 2018), roof tiles (Farias et al. 2013; Silva et al. 2012;
Farias et al. 2012), and bricks (Araújo et al. 2019a, b, 2017; Brito et al. 2017; Araújo
et al. 2017; Silva et al. 2011; Lima et al. 2015; Santos et al. 2020).
This chapter addresses the use of the lumped model to describe the drying process.
The equations of the lumped model can be classified as empirical, semi-empirical,
and theoretical. It is noteworthy that in this analysis the effects of temperature and
moisture variation inside the material are neglected during the process.
When it comes to empirical equations, they have a direct link between mois-
ture content and drying time, while semi-empirical ones are analogous to Newton’s
law of cooling, assuming that the drying rate is proportional to the difference
between moisture content of the product and its equilibrium moisture content for
the specified drying conditions. Theoretical equations generally use heat and mass
balances between the product and air surrounding it, taking account different phys-
ical phenomena during the process. Some researchers have applied lumped models
to describe drying process of clay porous materials. For example, clay pipes (Silva
et al. 2016), bricks (Silva 2009; Almeida et al. 2013; Tavares et al. 2014; Silva 2018;
Fig. 1.2 Representative scheme of the drying process of an arbitrarily-shaped solid based on a
lumped analysis
Silva et al. 2011; Lima et al. 2015), and others geometries (Silva et al. 2016; Lima
et al. 2018; Lima 2017).
For a better understanding of the lumped analysis method (theoretical model),
consider the solid with arbitrary geometry, illustrated in Fig. 1.2.
In this scheme, the arbitrary solid will receive on its surface a flux per unit area
of the potential of interest Φ and has uniformly distributed internal generation per
unit volume. According to what has already been mentioned, when applying the
lumped analysis method, the effects of the potential variation within the material are
neglected. Thus, all flux of Φ received and generated will diffuse instantly through the
solid. In order for this condition to be physically possible and well approximated, the
flux resistance within the solid must be much lower than the flux resistance between
the solid and its vicinity.
Thus, the balance of Φ (potential of interest) can be obtained as follows:

d λΦ
V = Φ S + Φ V (1.2)
dt
in which Φ and Φ are flux of Φ per unit area and source term, respectively. Further,
λ includes transport parameters and S and V are the surface area and volume of the
porous material, respectively.
1.3 Lumped Model Application: Drying of Clay Ceramic

Brick
As an application, in this topic will be developing new research methods and tech-
niques, particularly process modeling and simulation involving heat and mass trans-
port in solid–liquid systems, with particular reference to drying of clayey ceramic
materials, via lumped models.
The focus is to develop a phenomenological mathematical modeling and its analyt-

ical solution via method of separation of variables to predict heat and mass transfer
in clayey, cast, and arbitrary-shaped ceramic materials (industrial ceramic bricks).
1.3.1 The Experimental Data
The materials used for drying in oven were parallelepiped-shaped ceramic bricks with
8 rectangular holes (industrial ceramic bricks). Figure 1.3 illustrates the test body
model used, as well as the positions where the measurements of length (R1 ), width
(R2 ), height (R3 ), and dimensions that characterize the brick holes, a1 , a2 , a3 , and
a4 , were obtained. Initially, dimensions were measured with a digital caliper, mass
with a digital scale, brick temperature (vertex) with infrared thermometer, and room
temperature and relative humidity with thermohygrometer. Then, the samples were
taken inside the forced-air oven where drying was performed. In this process, the
internal temperature of the oven was set as desired with the temperature controller. At
predefined intervals, the brick was taken from the oven and measured its temperature,
mass, and dimensions.
Table 1.2 summarizes, for each experimental condition, the product, and air data.
Table 1.3 presents, for each operating condition, the dimensions, volume, and surface
area of the sample before the drying process begins.
During the process, measurements were taken every 10 min until the mass had
minimal variation. Then, the measurements were changed every 30 min, and the next
measurements were taken every 60 min until it reached constant mass. Soon after, the
Fig. 1.3 Hollow brick with dimensions

Table 1.2 Experimental air and brick parameters for each drying test (Silva 2009)
T (°C) Air Brick Time, t (h)
UR (%) V(m/s) M o (db) M f (db) M e (db) θ o (°C) θ f (°C)
50 80 0.05 0.13969 0.0 0.00011 20.6 41.0 18.5
60 79 0.06 0.14795 0.0 0.00268 20.5 50.2 13.7
70 69 0.07 0.15414 0.0 0.00076 26.0 64.5 17.8
80 66 0.08 0.15248 0.0 0.00039 21.4 69.2 15.0
90 68 0.09 0.15921 0.0 0.00151 21.0 78.5 11.5
100 52 0.10 0.16903 0.0 0.00038 26.1 93.2 12.3
sample was dried for 24 h at the same drying temperature to obtain the equilibrium
mass and then, for another 24 h at 105 °C to obtain the mass of the dried product.
All experiment was performed by Silva (2009). This author also performed an
adjustment of experimental data related to mass transfer (moisture content) during the
process and proposed an exponential equation with two terms and four parameters.
The equation has the form:
M = A1 exp(k1 t) + A2 exp(k2 t) (1.3)
where t is given in minutes. The A1 , A2 , k 1 , and k 2 parameters were estimated using

the Statistica® Software, the Rosembrock and Quasi-Newton numerical method, and
a convergence criterion of 0.001. After fitting, Silva (2009) presented the parameters
reported in Table 1.4.
The experimental data of the brick vertex temperature was fitted to an equation
with four parameters. The equation has the form:

θ = B1 + B2 log10 t K 1 + B3 (1.4)
where t is given in minutes. Parameters B1 , B2 , K 1 , and B3 were estimated using

Statistica® Software, the Quasi-Newton numerical method, and with a convergence
criterion of 0.0001.
Table 1.5 summarizes the coefficients of Eq. 1.4 obtained after fitting to the
experimental data.
1.3.2 Phenomenological Mathematical Modeling
To predict the drying process was developed an advanced and phenomenological

mathematic model. It is based on the following hypotheses:
16
Table 1.3 Brick dimensions before the drying process begins (Silva 2009)
T R1 (mm) R2 (mm) R3 (mm) a1 (mm) a2 (mm) a3 (mm) a4 (mm) V o (mm3 ) S o (mm2 )
(°C)
50 93.36 197.00 200.00 9.04 7.10 7.88 6.30 141,5643.80 371,100.44
60 92.75 195.00 200.00 8.34 7.32 7.11 6.45 1,367,269.30 369,020.69
70 93.16 197.00 203.00 8.54 9.87 7.99 6.96 1,621,580.85 162,158.85
80 92.76 197.00 201.00 8.16 7.20 7.84 6.66 1,408,074.95 37,214.46
90 93.10 197.00 201.00 8.88 7.95 6.57 6.78 1428,426.08 37,233.87
100 92.80 198.00 202.00 1.70 9.41 8.74 8.00 1,734,026.10 36,116.49
A. G. B. de Lima et al.
Table 1.4 Parameters of Eq. 1.3 obtained after fitting to experimental data of average moisture
content
T (°C) Parameter R (–) Explained
A1 (–) k 1 (mm−1 ) A2 (–) k 2 (mm−1 ) variance (%)
50 0.576178 −0.004711 0.482232 −0.004711 0.997676745 0.995358888

60 0.547740 −0.005945 0.513349 −0.005945 0.997968284 0.995940696
70 0.000000 −0.006781 1.045050 −0.0070948 0.999112861 0.998226509
80 0.535201 −0.009190 0.527668 −0.009190 0.998502641 0.997007523
90 10.63554 −0.014298 −9.613313 −0.015018 0.998876724 0.997754709
100 4.875507 −0.008383 −3.827964 −0.007881 0.998297496 0.996597890
Table 1.5 Parameters of Eq. 1.4 obtained after fitting to experimental data of the vertex temperature
B1 (°C) B2 (°C/min) k 1 (–) B3 (min) variance (%)
50 −546.0430 283.1605 0.42554 101.18296 0.960840804 0.923215051

60 −48.7454 39.22594 0.86804 66.362934 0.981233190 0.962818573
70 −18.4408 40.19277 0.698315 11.943974 0.953411275 0.908993060
80 −21.3661 37.35810 0.871389 14.410538 0.970896765 0.942640529
90 −30.7995 33.11958 1.222654 47.338410 0.981074082 0.962506354
100 −2.86969 15.41788 2.234665 118.38213 0.984632771 0.969501694
(a) Brick is composed of liquid water and solid matter;

(b) Water migrates from the interior of the brick in liquid form and evaporates on
the surface;
(c) On the solid surface there is thermal convection, evaporation, and heating of
produced vapor;
(d) Dimensional variations were considered during drying process;
(e) Heat and mass generation were neglected;
(f) Constant mechanical and thermophysical properties.
1.3.2.1 Geometric and Dimensional Analysis
From the various measurements of the brick dimensions, made during the drying
process, mathematical equations were proposed to calculate the volume and surface
area of the brick (Fig. 1.3). The brick volume at any time t was calculated as follows:
Vf = aV aH R3 (brick holes volume) (1.5)
V = (R1 R2 R3 ) − (8Vf )(brick volume) (1.6)

The brick surface area at any time t was determined by using the following
equation:
S = (2R1 R3 ) + (2R2 R3 ) + 2[(R1 R2 ) − (8aH aV )] + 8[(2aH R3 ) + (2aV R3 )]

(1.7)
where in Eqs. 1.5, 1.6, and 1.7:
aV = (R2 − 2a1 − 3a3 )/4 (height of a hole) (1.8)
aH = (R1 − 2a2 − a4 )/2 (width of a hole) (1.9)
After determination of the volume and surface area at different moments of drying,
it was possible to adjust them to mathematical models that describe the volumetric
variation and surface area of the brick during the drying process. This procedure was
realized by using Statistica® software (Simplex numerical method and convergence
criterion of 0.00001). For this, a third-degree polynomial model was proposed for
both volume and surface area, as follows:
V (t) = C1 t 3 + C2 t 2 + C3 t + C4 (1.10)
S(t) = D1 t 3 + D2 t 2 + D3 t + D4 (1.11)
1.3.2.2 Mass Transfer Analysis
The complexity of the drying process depends, among other parameters, on the
analysis taken into account. Distributed models express heat and mass transfer rates
as a function of position within the part and drying time, taking into account external
and internal resistances. Already the lumped models express the same rates only as
a function of the process time and ignoring the existing internal resistance for this
transfer. This study makes use of the lumped model analysis to describe the drying
process of ceramic brick. Thus, from Eq. 1.2, we have the following mass balance:
dM
V = −h m S(M − Me ) + V Ṁ (1.12)
dt
where S and V represent the surface area and volume of the solid at any time t, hm
is the convective mass transfer coefficient, M is the average moisture content, M e is
the equilibrium moisture content of the brick, and t is the time.
Considering M = M − M e , it is valid dM = dM. Therefore, it is possible to
write:
dM
V = −h m S M + V Ṁ (1.13)
dt
Separating the variables and rearranging the terms, Eq. 1.13 results in:
dM hm S
=− dt (1.14)

(M ) − h m S
V Ṁ V
Since that M = M 0 at t = 0, and that there are no reactions that can generate water
inside the product, it was considered Ṁ = 0. So, Eq. 1.14 can be integrated from the
initial condition. Thus, it is possible to write:
e
M−M t

dM hm S
=− dt (1.15)
(M ) V
M0 −Me 0
Putting Eqs. 1.10 and 11.11 into Eq. 1.15 and integrating it, we obtain the following
equation, which defines the mass transfer, considering dimensional variations during
the process:
⎧ ⎡ ⎧ ⎫⎤⎫
⎨ ⎨ a 1 t + a 2 arctan a 3 a 4 + 2t + a 5 log a 6 − t ⎬ ⎬
M = (M0 − Me ) exp⎣−h m ⎦ + Me (1.16)
⎩ ⎩ + a 7 log a 8 + a 9 t + t 2 − a 10 ⎭ ⎭

where the coefficients a k are specified according to drying conditions.
1.3.2.3 Heat Transfer Analysis
Similarly, to mass transfer, for heat transfer analysis, considering constant the heat
flux per area unit, the following energy balance is given:
dθ
ρV Cp = [h c S(θ∞ − θ )] + q̇ V (1.17)
dt
where ρ and C p represent the density and specific heat of the brick, respectively,
hc is the convective heat transfer coefficient, θ and θ ∞ represent, respectively, the
average product temperature at any time t and the equilibrium temperature (which
is equal to the drying air temperature).
Considering T = θ∞ − θ , it turns out that dT = −dθ. Then, putting this result
into Eq. 1.17, separating the variables, this equation can be rewritten as follows:
dT hc S
=− dt (1.18)
T + q̇ V ρV Cp
(h c S)
Since that θ = θ 0 at t = 0, and that there are no chemical reactions that can
generate heat inside the product, it is possible to consider q̇ = 0. So, Eq. 1.18 can be
integrated from the initial condition. Thus, we have that:
θ
∞ −θ t
dT hc S
=− dt (1.19)
[T ] ρV Cp
θ∞ −θo 0
Now, putting Eqs. 1.10 and 1.11 into Eq. 1.19 and integrating it, we obtain as results
the following equation, which defines the heat transfer, considering dimensional
variations during the process:
⎧ ⎡ ⎧ ⎫⎤⎫
⎪ ⎪
⎨ b1 t + b2 arc tan b3 b4 + 2t + b5 log b6 − t ⎪
⎬ ⎪

⎨ ⎬
⎢ hc ⎥
θ = θ∞ − (θ∞ − θo ) exp⎣− ⎦
⎪ ρCp ⎪ ⎪
⎭ ⎪

⎩ ⎩ + b7 log b8 + b9 t + t 2 − b10 ⎭
(1.20)

where the coefficients bk are specified according to drying conditions.

Equations 1.16 and 1.20 were fitted to the experimental data of the average mois-
ture content (Eq. 1.3) and surface temperature (Eq. 1.4) of the ceramic brick using the
Statistica® software (Quasi-Newton numerical method and convergence criterion of
0.0001). From the non-linear regression, it was possible to estimate the convective
mass transfer (hm) and heat transfer (hc) coefficients.
1.3.3 Results Analysis
1.3.3.1 Dimensional Variations
Tables 1.6 and 1.7 summarize the parameters obtained for Eqs. 1.10 and 1.11,
respectively.
Table 1.6 Parameters of Eq. 1.10 that describe the volumetric behavior of the brick during drying
process
C1 (m3 /min3 ) C2 (m3 /min2 ) C3 (m3 /min) C4 (m3 ) variance (%)
50 −0.000862 1.76499 −1099.66 1,381,400 0.98227288 96.486

60 −0.001538 2.46177 −1213.49 1,356,500 0.98812668 97.639
70 −0.000678 1.36975 −911.113 1,546,700 0.94004504 88.368
80 −0.001273 2.02475 −977.457 1,374,700 0.94563064 89.422
90 −0.003695 4.40681 −1596.91 1,392,300 0.9535488 90.926
100 −0.003480 5.278373 −2066.011 1,551,571 0.81039933 65.675
Table 1.7 Parameters of Eq. 1.11 that describe the surface area behavior of the brick during drying
process
D1 (m2 /min3 ) D2 (m2 /min2 ) D3 (m2 /min) D4 (m2 ) variance (%)
50 −0.000126 0.259821 −163.671 371,912 0.99130038 98.268

60 −0.000315 0.45662 −202.289 368,692 0.98169467 96.372
70 −0.000200 0.366684 −192.89 366,801 0.93426766 87.286
80 −0.000267 0.41566 −190.31 370,685 0.9335808 87.157
90 −0.000628 0.761024 −271.251 373,572 0.95696019 91.577
100 −0.000226 0.322700 −134.0546 355,682 0.82398847 67.896
Statistica® software also provides graphs of the estimated functions compared to

the collected experimental points. Thus, Figs. 1.4 and 1.5 show the transient volume
and surface area variations under operating conditions from 50 to 100 °C.
After analysis of Figs. 1.4 and 1.5, it is possible to notice that the volume and
surface area have a decreasing behavior over time. This is because the water inside the
brick is being evaporated during drying (shrinkage) and it is being heated during the
process (volumetric expansion). Since that, drying at higher temperatures provokes
increases in the drying and heating rates, these phenomena are more intensive.
It is also possible to see that the experimental data found at 100 °C have a less
accurate adjustment for both volume and surface area variation. This is due to possible
measurement errors with brick drying and large temperature variations due to the
fact that the brick was removed from the oven so that measurements could be made.
It can be verified that at 50 °C, the brick volume decreased by 17.88% and at
100 °C a reduction of 20.57% occurred. At 100 °C, the amount of evaporated water
is greater. With regard to surface area at temperature 50 °C the brick was reduced
in surface area by 8.46% and at 100 °C by 5.83%. Thus, we can see that the area
reduction was much smaller than the volume, which shows that the drying was done
properly and the brick did not suffer large deformations, maintaining its original
shape, but in a smaller size.
1.3.3.2 Drying Process
Table 1.8 summarizes the coefficients of Eqs. 1.16 and 1.20. With this, it was possible
to adjust these equations to the experimental data of moisture content (Eq. 1.3) and
surface temperature (Eq. 1.4) and to estimate the convective heat transfer and mass
transfer coefficients.
Figures 1.6 and 1.7 illustrate a comparison between the predicted and experimental
brick average moisture content as a function of time for drying at 50 and 100 °C,
respectively.
Fig. 1.4 Predicted (---) and experimental (ooo) volume variations of the brick during drying. a 50 °C
and b 100 °C
Fig. 1.5 Predicted (---) and experimental (ooo) surface area variations of the brick during drying.
a 50 °C and b 100 °C
Table 1.8 Parameters of Eqs. 1.16 and 1.20 that describe mass transfer and heat transfer of the
brick during drying process
Parameter T (°C)
50 60 70 80 90 100

a 1 = b1 0.15 0.20 0.29 0.21 0.17 0.06

a 2 = b2 95.11 48.35 47.31 39.10 44.57 88.20

a 3 = b3 0.0005 0.0006 0.0005 0.0006 0.0008 0.0009

a 4 = b4 −218.45 −128.91 −85.22 −44.78 −83.38 −194.00

a 5 = b5 −51.82 −14.11 −25.59 −21.74 −27.83 −34.53

a 6 = b6 1829.10 1471.72 1935.06 1545.75 1109.26 1322.77

a 7 = b7 24.85 22.52 14.76 14.41 12.28 20.15

a 8 = b8 876141.16 599290.09 1.18 × 106 698617.29 339691.29 337060.33

a 9 = b9 −218.45 −128.91 −85.22 −44.78 −83.38 −194.00

a 10 = b10 −60.3635 192.68 401.945 33.22 −41.86 −6.50
Fig. 1.6 Predicted and experimental average moisture content of ceramic brick as a function of
drying time (T = 50 °C)
From the analyzes of the figures, we can state that the drying of brick occurred in
the falling drying rate period, for two reasons: the drying rate isn’t constant and the
brick temperature arises during the drying process.
Further, the drying rate increases with increasing drying temperature. For all
drying temperatures, it can be considered that after the first 1000 min of process,
the average moisture content varies slightly. Thus, we can state that the equilibrium
moisture content was reached at this time.
Fig. 1.7 Predicted and experimental average moisture content of ceramic brick as a function of
drying time (T = 100 °C)
Analyzing the graphs, it is noted that there is an agreement between the exper-
imental values and the predicted values by the model used, confirming that the
modeling used to find the average moisture content, as a function of drying time, is
effective.
1.3.3.3 Heating Process
Similar to the procedure adopted for the moisture content, to find the convective heat
transfer coefficients, at the different drying temperatures, a comparison between the
predicted and experimental brick vertex temperature (Eq. 1.4) was made, until it
reached a minimum error.
Figures 1.8 and 1.9 illustrate the brick temperature adjustment curves as a function
of time for drying at 50 and 100 °C, respectively.
Through analysis, it can be proved that, for drying at higher temperatures, the
brick reaches its equilibrium temperature in a shorter process time.
When evaluating the graphs, it is noted that there was a good agreement between
the experimental values and the values determined through the proposed model. The
adjustment efficiency was not as good as in mass transfer, but this was due to the
fact that the analytical model developed took into account only the heat transfer,
disregarding the simultaneous mass transfer effect and the energy to be used in the
phase change of water.
Therefore, even with a not so refined agreement between the experimental and
predicted brick temperatures, it can be said that the modeling used to estimate the
process parameters is effective.
Fig. 1.8 Predicted and experimental brick surface temperature as a function of drying time (T =
50 °C)
Fig. 1.9 Predicted and experimental brick surface temperature as a function of drying time (T =
100 °C)
1.3.3.4 Estimation of Transport Parameters
After gravimetric and thermal analysis, the process parameters were found for the
different drying conditions. After fitting of Eqs. 1.16 and 1.20 to experimental data
of average moisture content and temperature, the heat and mass transfer coefficients
were estimated. Table 1.9 summarizes the estimated values of convective heat and
mass transfer coefficients, with the respective errors obtained with Eqs. 1.21 and
1.22. In these equations, the number of experimental points is n = 110.
Table 1.9 Convective heat and mass transfer coefficients estimated from fitting of Eqs. 1.16 and
1.20 to experimental data
T (°C) hm (m/s) ERM (kg/kg)2 hc (W/m2 °C) ERT (–)
50 2.6500 × 10−7 0.000293 0.36985 0.823922
60 3.3266 × 10−7 0.000307 0.50538 0.375189
70 4.7300 × 10−7 0.000176 0.75000 0.525849
80 5.2783 × 10−7 0.000276 0.88250 0.792176
90 5.7216 × 10−7 0.000462 1.00000 0.539377
100 6.9816 × 10−7 0.000263 1.33333 0.689403

n
2
ERM = Mpred − Mexp (1.21)
i=1
n

θpred − θexp 2
ERT = (1.22)
i=1
θpred
Analyzing the convective heat and mass transfer coefficients as a function of

drying temperatures, it is noted that there is an increase in the value of these coef-
ficients with increasing drying temperature. Increasing the temperature implies an
increase in the drying and heating rates of the brick, which makes it possible to reach
its thermal and hygroscopic equilibrium conditions faster. The small values of the
heat transfer coefficient are equivalent to the free convection heat transfer condition.
1.4 Concluding Remarks
From the studies performed, it can be concluded that:

(a) The drying process at high temperatures takes place in a shorter process time.
(b) Parameters for third-degree polynomial functions describe well the behavior of
volume and surface area during the drying process.
(c) At high temperatures, the volumetric variation was 20.57% while the surface
area varied by 5.83%. This point explains that the drying process was done
correctly as the integrity of the brick shape was maintained. It is important to
evaluate the behavior of the brick shape during drying, as this can make process
control and therefore avoid possible defects in the parts.
(d) The mathematical modeling developed taking into account the dimensional
variations during the drying process was considered satisfactory.
(e) The convective heat and mass transfer coefficients increased with the evolution
of the drying temperature.
Acknowledgments The authors thank CNPq, CAPES, FINEP (Brazilian Research Agencies), and
PIBIC/CNPq-UFCG scientific initiation undergraduate program for the financial support, and the
researchers cited in the text, who helped in the improvement of the investigation made.
References
Almeida, G.S., Silva, J.B., Silva, C.J., Swarnakar, R., Neves, G.A., Lima, A.G.B.: Heat and mass
transport in an industrial tunnel dryer: modeling and simulation applied to hollow bricks. Appl.
Thermal Eng. 55, 78–86 (2013)
Almeida, G.S., Tavares, F.V.S., Lima, W.M.P.B., Lima, A.G.B.: Energetic and exergetic analysis of
the clay bricks drying in an industrial tunnel dryer. Def. Diff. Forum 369, 104–109 (2016)
Araújo, M.V., Pereira, A.S., Oliveira, J.L., Brandão, V.A.A., Brasileiro Filho, F.A., Silva, R.M.,
Lima, A.G.B.: Industrial ceramic brick drying in oven by CFD. Mater 12(10), 1612–1634 (2019a)
Araújo, M.V., Santos, R.S., Silva, R.M., Nascimento, J.B.S., Santos, W.R.G., Lima, A.G.B.: Drying
of industrial hollow ceramic brick: a numerical analysis using CFD. Def. Diff. Forum 391, 48–53
(2019b)
Araújo, M.V., Santos, R.S., Silva, R.M., Lima, A.G.B.: Drying of industrial hollow ceramic brick:
analysis of the moisture content and temperature parameters. Def. Diff. Forum 380, 72–78 (2017a)
Araújo, M.V., Delgado, J.M.P.Q., Lima, A.G.B.: On the use of CFD in thermal analysis of industrial
hollow ceramic brick. Diff. Found. 10, 70–82 (2017b)
Brito, M.K.T.: Theoretical study of heat and mass transfer in the drying of ceramic bricks with
parallelepiped shape. Master’s dissertation in Mechanical Engineering, Federal University of
Campina Grande, Campina Grande, Brazil (2016). (In Portuguese)
Brito, M.K.T., Almeida, D.B.T., Lima, A.G.L., Rocha, L.A., Lima, E.S., Oliveira, V.A.B.: Heat and
mass transfer during drying of clay ceramic materials: a three-dimensional analytical study. Diff.
Found. 10, 93–106 (2017)
Brooker, D.B., Bakker-Arkema, F.W., Hall, C.W.: Drying and Storage of Grains and Oilseeds. AVI
Book, New York (1992)
Cabral Jr., M., Motta, J.F.M., Almeida, A.S., Tanno, L.C.: Clay for red ceramics. Industrial rocks
and minerals. CETEM 2(1), 747–770 (2008). (In Portuguese)
Callister Jr., W.D.: Materials Science and Engineering: An Introduction, 7th edn. Wiley, USA (2007)
Callister Jr., W.D., Rethwisch, D.G.: Fundamentals of Materials Science and Engineering: An
Integrated Approach, 3rd edn. Wiley, USA (2008)
Cavalcanti, M.S.L.: Development of ceramic masses for sanitary stoneware using flat glass residue
as a flux in partial replacement to feldspar, Doctoral Thesis in Process Engineering, Federal
University of Campina Grande, Campina Grande, Brazil (2010). (In Portuguese)
Farias, V.S.O., Silva, W.P., Silva, C.M.D.P.S., Delgado, J.M.P.Q., Farias Neto, S.R., Lima, A.G.B.:
Transient diffusion in arbitrary shape porous bodies: numerical analysis using boundary-fitted
coordinates. In: Delgado, J.M.P.Q., Barbosa de Lima, A.G., Silva, M.V. (eds.) Numerical Analysis
of Heat and Mass Transfer in Porous Media, vol. 27, pp. 85–119. Springer, Heidelberg, Germany
(2012)
Farias, V.S.O., Silva, W.P., Silva, C.M.D.P.S., Rocha, V.P.T., Lima, A.G.B.: Drying of solids with
irregular geometry: numerical study and application using a three-dimensional model. Heat Mass
Transfer 49(5), 695–709 (2013)
Lima, A.G.B., Delgado, J.M.P.Q., Santos, I.B., Santos, J.P.S., Barbosa, E.S., Silva, C.J.: GBI method:
A powerful technique to study drying of complex shape solids. In: Delgado, J.M.P.Q., Barbosa
de Lima, A.G. (eds.) Transport Phenomena and Drying of Solids and Particulate Materials, vol.
48, pp. 25–431, Springer International Publishing, Heidelberg, Germany (2014)
Lima, A.G.B., Silva, J.B., Almeida, G.S., Nascimento, J.J.S., Tavares, F.V.S., Silva, V.S.: Clay
products convective drying: foundations, modeling and applications. In: Drying and Energy
Technologies, vol. 63, pp. 43–70. Springer, Heidelberg, Germany (2015)
Lima, E.S., Lima, W. M.P.B., Lima, A.G.B., Farias Neto, S.R., Silva, E.G., Oliveira, V.A.B.:
Advanced study to heat and mass transfer in arbitrary shape porous materials: Foundations,
phenomenological lumped modeling and applications In: Delgado, J.M.P.Q., Lima, A.G.B. (eds.)
Transport Phenomena in Multiphase Systems, 93, pp. 181–217. Springer International Publishing,
Heidelberg, Germany (2018)
Lima, W.M.P.B.: Heat and mass transfer in porous solids with complex geometry via concentrated
analysis: modeling and simulation. Master,s dissertation in Mechanical Engineering, Federal
University of Campina Grande, Campina Grande, Brazil (2017)
Macedo, R.F.: Continuous drying of bentonite clay in an industrial rotary dryer: modeling, simu-
lation and experimentation. Master’s dissertation in Mechanical Engineering, Federal University
of Campina Grande, Campina Grande, Brazil (2016)
Oliveira, M.C., Bernils, M.F.: Environmental technical guide for the white ceramics and coatings
industry. In: CETESB—Companhia de Tecnologia de Saneamento Ambiental, São Paulo (2006).
(In Portuguese)
Rodrigues Neto, A., Mota, J.A.: Local productive arrangements in the red ceramic industry: a case
study in Brazil Northeastern. Rev. Econ. NE. 47(1), 127–142 (2016). (In Portuguese)
Santos, J.P.S.: Drying of ceramic materials with complex shape: a theoretical study via CFX.
Doctoral Thesis in Process Engineering, Federal University of Campina Grande, Campina Grande,
Brazil (2018)
Santos, R.S., Farias Neto, S.R., Lima, A.G.B., Silva Jr., J.B., Silva, A.M.V.: Drying of ceramic
bricks: thermal and mass analysis via CFD. Diff. Found. 25, 133–153 (2020)
SEBRAE (Serviço Brasileiro de Apoio às Micro e Pequenas Empresas). Red Ceramics: Overview of
the market in Brazil. http://www.bibliotecas.sebrae.com.br/chronus/ARQUIVOS_CHRONUS/
bds/bds.nsf/b877f9b38e787b32594c8b6e5c39b244/$File/5846.pdf. Accessed 13 Jan 2019
Silva, A.A., Nascimento, J.J.S., Lima, A.G.B: Analytical study of ceramic tiles drying using the
Galerkin-based integral method and Dirichlet boundary condition Rev. Eletrônica Mater. Process.
(UFCG) 4(2), 48–55 (2009). (In Portuguese)
Silva, A.M.V.: Drying of industrial ceramic blocks: Modeling, simulation and experimentation.
Doctoral thesis in Process Engineering, Federal University of Campina Grande, Campina Grande,
Brazil (2018)
Silva, J.B.: Simulation and experimentation of the drying of holed ceramic bricks. Doctoral Thesis
in Process Engineering, Federal University of Campina Grande, Campina Grande, Brazil (2009).
(In Portuguese)
Silva, V.S.: Heat and mass transfer in complex shaped materials via the lumped analysis method.
Case study: drying of ceramic materials. Doctoral Thesis in Process Engineering, Federal
University of Campina Grande, Campina Grande, Brazil (2016). (In Portuguese)
Silva, J.B., Almeida, G.S., Lima, W.C.P.B., Neves, G.A., Lima, A.G.B.: Heat and mass diffusion
including shrinkage and hygrothermal stress during drying of holed ceramics bricks. Def. Diff.
Forum 312–315, 971–976 (2011)
Silva, W.P., Farias, V.S.O., Neves, G.A., Lima, A.G.B.: Modeling of water transport in roof tiles by
removal of moisture at isothermal conditions. Heat Mass Transfer 48(5), 809–821 (2012)
Silva, V.S., Delgado, J.M.P.Q., Lima, W.M.P.B., Lima, A.G.B.: Heat and mass transfer in holed
ceramic material using lumped model. Diff. Found. 7, 30–52 (2016)
Strumillo, C., Kudra, T.: Drying: Principles, Science and Design. Gordon and Breach Science
Publishers, New York (1986)
Tavares, F.V.S., Farias Neto, S.R., Barbosa, E.S., Lima, A.G.B., Silva, C.J.: Drying of ceramic
hollow bricks in an industrial tunnel dryer: a finite volume analysis. Int. J. Multiphys. 8(3),
297–312 (2014)
Chapter 2
Vegetable Fiber Drying: Theory,
Advanced Modeling and Application
J. F. Brito Diniz, A. R. C. de Lima, I. R. de Oliveira, R. P. de Farias,

F. A. Batista, A. G. Barbosa de Lima, and R. O. de Andrade
Abstract This chapter aims to study the drying of sisal fibers. The interest in this type
of material is related to its high mechanical performance. Several important topics
such as theory, experiments, lumped and distributed mathematical modeling, and
technological applications of fibers are presented and discussed. Emphasis is given
to advanced distributed modeling that describes the heat and mass transfer in a wet
fiber bed during drying. The model includes different effects such as bed porosity,
fiber and bed moisture, coupling between heat and mass transport, and conduc-
tion, convection, and evaporation heat transfer. Results of fiber drying and heating
kinetics, temperature distribution, and water vapor concentration in the fibrous bed
are presented, compared with experimental data and analyzed.
J. F. Brito Diniz
Department of Mathematics, Federal University of Campina Grande, Av. Aprígio Veloso 882,
Bodocongó, 58429-900 Campina Grande, PB, Brazil
e-mail: jacqueline@mat.ufcg.edu.br
A. R. C. de Lima · I. R. de Oliveira · A. G. B. de Lima (B) · R. O. de Andrade
Veloso 882, Bodocongó, 58429-900 Campina Grande, PB, Brazil
I. R. de Oliveira
e-mail: rodrigues.iran@hotmail.com
R. O. de Andrade
e-mail: anakel_alimentos@hotmail.com
R. P. de Farias
Department of Agriculture Science, State University of Paraiba, Catolé do Rocha, PB 58884-000,
Brazil
e-mail: rp.eng.tec@gmail.com
F. A. Batista
Department of Physics, State University of Paraiba, R. das Baraúnas, 351, Campina Grande, PB
58429-500, Brazil
e-mail: chicoalves13@hotmail.com
https://doi.org/10.1007/978-3-030-47856-8_2
32 J. F. Brito Diniz et al.
Keywords Drying · Sisal fiber · Experimental · Simulation · Finite-Volume
2.1 Introduction
Vegetable fibers are structural tissues of plants. It is a body consisting of fibers (solid)
and pores (filled with fluid) as illustrated in Fig. 2.1.
The main chemical components of vegetable fibers are polar substances such as
cellulose, hemicellulose (or polyoses), and lignin, with lower percentages of other
components such as pectin, proteins, wax, inorganic salts, and other water-soluble
substances. Its chemical composition varies slightly according to cultivation region,
soil type, and climatic conditions (Silva 2003).
Vegetable fiber is made up of several elemental fibers strongly bonded together by
a resinous material consisting primarily of lignin. Each elemental fiber is essentially
a composite in which rigid cellulose microfibrils are encased in an amorphous matrix
of lignin and hemicellulose. Lignin acts as a resinous material, uniting microfibrils,
Fig. 2.1 Longitudinal

micrographs of untreated
sisal fiber obtained by
Scanning Electron
Microscope (SEM): a 100×
magnification and b 200×
magnification
2 Vegetable Fiber Drying: Theory, … 33
while hemicellulose acts as an interface between cellulose microfibril and lignin

(Silva 2003). The structure of an elemental plant fiber consists of a thick wall formed
by several microfibril spirals along the fiber axis, having a lumen in the center.
There are several types of vegetable fibers such as caroá, curauá, pineapple leaf,
juta, and sisal. Sisal is a plant of the cactaceae family with the scientific name Agave
Sisalana Perrine, being cultivated in semi-arid regions, being resistant to aridity and
intense sun. The main and best-known product of sisal is biodegradable yarn.
The cycle of transformation of sisal into natural yarn begins at 3 years of plant life
or when its leaves reach about 150 cm in length. Plant growth depends, among other
factors, on water availability: The plant stores water in the rainy season (winter) to
consume it in the dry season (summer). Its useful life is 6–7 years, and the leaves are
cut every 6 months. Sisal can produce between 200 and 250 leaves before flowering,
each leaf measuring 6–10 cm wide, 150–200 cm long, and containing approximately
700–1400 bundles of fiber ranging in length from 0.5 to 1.0 m. The leaf of sisal
consists of a structure composed of approximately 4% fiber, 1% film (cuticle), 8% dry
matter, and 87% water. Except fiber, these materials are considered processing waste,
being used as organic fertilizer, animal feed, and by the pharmaceutical industry
(Martin et al. 2009; Wei and Meyer 2014).
The sisal fiber extraction process, which consists in the elimination of the pulp
from the fibers, can be done manually, by maceration or by a mechanical process
called decorticating (Silva 2008). In the decorticating process, the sisal leaves are
crushed by passing between two blunt-bladed wheels (defibrillator), so that only the
fibers remain (Silva 2008). In the Brazilian northeastern, the defibration is performed
through a machine called “agave engine”.
Benefited or industrialized, the sisal fiber generates more than half a million
direct or indirect jobs through its service chain, which begins with the activities
of crop maintenance, harvesting, leaf cutting, fiber shredding and processing, and
finally with industrialization and varied use (Martin et al. 2009). It has been used
in handicrafts, baling fodder, and ropes of various uses. Sisal is also used in the
production of upholstery, paste for the cellulose industry, the production of tequila,
decorative rugs, medicines, biofertilizers, animal feed, organic fertilizer, and sacks.
Fibers can also be used in the automotive industry, replacing fiberglass.
In recent years, with increasing awareness of environmental preservation and
pollution control, interest in the use of natural fibers in polymer composite mate-
rials has increased significantly. In this context, the use of vegetable fibers as rein-
forcement in polymer composites, with the objective of totally or partially replacing
synthetic fibers, has received attention from the researchers. This is because vegetable
fibers have important advantages such as low cost, low density, high specific strength
and stiffness, and low abrasiveness to process equipment are biodegradable, non-
toxic, non-polluting, which reduces environmental problems. They also come from
renewable sources and are available worldwide (Cruz et al. 2011; Melo Filho et al.
2013; Nóbrega et al. 2010; Zhou et al. 2014). However, plant fibers are very suscep-
tible to humidity and temperature, which strongly affect their mechanical properties,
especially when used as reinforcement in polymeric materials.
Because it is a lignocellulosic fiber, light and non-toxic, with high modulus and
specific resistance, costing about ten times lower than fiberglass (inorganic fiber),
causing less abrasion damage to equipment and molds, sisal can have its commercial
value multiplied if used as reinforcement in polymer composites (Angrizani et al.
2006; Barreto et al. 2011).
The use of sisal fiber in high performance composites requires study of the
mechanical behavior of the fibers. There is a large discrepancy between the values
reported in the literature for tensile strength and elastic modulus of sisal fiber. The
variability in the properties of these fibers can be attributed to three main factors: test
parameters and conditions, plant characteristics, and the cross-sectional measurement
method. Among the parameters or test conditions that may influence the mechanical
properties of the fibers, we can mention the precision of the instruments, the fiber
length, the test speed, the types of claws used, and the sensitivity of the equipment
itself. The characteristics of the plants themselves include the origin of the plant, age,
type of processing (extraction process) as well as its microstructure. The measure-
ment of the cross-section may also cause variation in the measurement of mechanical
properties due to the indefinite shape of the section and the variation itself along the
fiber (Silva 2008).
2.2 Drying of Sisal Fibers
Sisal fibers when extracted from plants are moist, which requires drying them for
later use in different applications.
Drying is a thermodynamic process whereby a body’s moisture is reduced and its
temperature increased by supplying energy. It involves complex phenomena of heat
and mass transfer, momentum, and dimensional variations (Lima et al. 2016). The
control of the drying process is of fundamental importance to determine the ideal
drying conditions, minimizing product losses, and energy consumption.
According to Ferreira et al. (2012), the cellulose polysaccharide chains are more
tightly arranged with the removal of water during drying and thus the microfibrils
come together in the dry state as a result of increased packaging. Fiber voids are
progressively closed with drying and cannot be completely reopened with rehu-
midification. A direct consequence of reduced absorption is the decrease in fiber
dimensional variation between the dry and saturated state. Thus, we have a greater
dimensional stability of the fiber.
Moisture transport from the interior to the material surface may occur as a liquid
and/or vapor, depending on the type of product and the percentage of moisture
present. The diffusion process should occur in a controlled way, avoiding high mois-
ture and temperature gradients within the material that may affect material prop-
erties. Thus, understanding the mechanisms involved in diffusion is a fundamental
requirement in the study of solutions that minimize such problems.
2.2.1 Experimental Study
In this work, the phenomena of heat and mass transport in fibrous bodies (sisal fibers)
were investigated. Agave sisalana variety sisal fibers with average moisture content
of 11.2% (db) were used. The fibers were submitted to oven drying with forced air
circulation at 70 °C. Figure 2.2 illustrates the sisal fibers used in the experiment.
Table 2.1 contains the fiber and drying air information.
During the drying process, moisture loss was measured by taking the sample
from the oven and periodically weighing (predefined intervals) using a 0.1 g precision
digital electronic device, and the surface temperature was measured using an infrared
thermometer. In the experiment, measurements were taken every 5 min until the mass
had minimal variation (about 30 min), after 10, 15, 20, 25, and 30 min. Then, the
measurements were changed every 60 min until the constant mass was reached.
Fig. 2.2 Sisal fibers used in

the experiments
36
Table 2.1 Experimental parameters of air and fibrous medium

Air Fibrous medium Process time
RH (%) T (°C) v (m/s) 2R1 (m) 2R1 (m) 2R1 (m) M o (db) M eq (db) T o (o C) T f (o C) t (h)
6.89 70 0.07 0.1 0.05 0.1 0.11148 0.02015 31.5 67.3 5.7
J. F. Brito Diniz et al.
Following, the sample was dried for 24 h to obtain the equilibrium mass and then for
a further 24 h at 105 °C to obtain the dry mass.
2.2.2 Theoretical Study
To describe (theoretically) the moisture and heat transfer within a fibrous medium
and to analyze the effects of certain parameters on their mechanical properties, it
is necessary that these transport phenomena within the fibrous medium be well
represented by a mathematical model. Therefore, it is important to fully insert all
effects within mathematical models so that the physical phenomenon can be described
with great realism, and to increase the reliability of the results obtained.
Analytical and numerical solutions to the transient diffusion problem for various
geometries have been reported in the literature; however, there are few studies related
to transient and three-dimensional problems, particularly those related to plant fibers
and incorporating the effect of porosity inside the fibrous medium.
2.2.2.1 Lumped Modeling
To describe the drying behavior of the fibrous media (sisal fibers) and to predict it
under different operating conditions, it is necessary to model the drying process. For
this, mathematical models are used in an attempt to predict the drying and heating
kinetics, which, as a rule, predominantly follow a falling rate period.
Several empirical, semi-empirical, and theoretical models have been proposed
to describe the drying process. Theoretical models take into account only internal
resistance, while semi-empirical and empirical models (thin-layer drying models)
take into account only external resistance to heat and moisture transfer between
material and air (internal resistance is insignificant). Currently, there are few models
that represent the drying of fibrous bodies, for this, the following models have been
proposed:
(a) Drying model
M = c1 exp(−k1 t) + c2 exp(−k2 t) + c3 exp(−k3 t) (2.1)
(b) Heating model
T = c1 log2 [(k1 t + k2 )c2 · (k3 t + k4 )c3 ] (2.2)

Fig. 2.3 Geometric

configuration of the physical
problem
where M is the average moisture content on dry basis, T is the temperature, and
t corresponds to the process time. The ci and ki parameters of the proposed thin-
layer models were obtained by nonlinear regression analysis by the Quasi-Newton
method using the STATISTICA 7.0 software. In addition, some statistical parameters
(correlation coefficient and variance) were determined for each proposed model.
2.2.2.2 Advanced Distributed Modeling
Governing Equations
This section presents the mathematical models required for the development of heat
and moisture (vapor) transport simulations in porous solids, with particular reference
to plant fibers. The entire mathematical formulation was developed in a fibrous region
in the form of a parallelepiped, according to Figs. 2.2 and 2.3.
(a) Vapor diffusion equation
The porous media consists of a series of rigid and inert fibers. Water vapor is free to
diffuse between the voids of the fiber bed (interfiber) and to be sorbed or desorbed
by the fiber (intrafiber). In addition, changes in fiber bed volume due to moisture
absorption/desorption may be neglected.
To describe the water vapor concentration in the fiber bed throughout the process,
it was considered: (a) that the vapor diffusion through the voids and across the fibers
is proportional to the concentration gradient in the usual way. The diffusion through
the pores will in many cases be greater than through the fibers, but even so, both
processes can be represented by assuming that the vapor in the fiber is always in
equilibrium with the surrounding air vapor and that the absorption isotherm has a
linear behavior, given by Eq. (2.5); (b) that moisture absorption or desorption through
the voids inside the fiber.
The mass and heat conservation equations will be expressed in terms of a unit
volume of the air-fiber mixture. Water vapor accumulates in the volume element
in both voids (interfiber) and fibers (intrafiber). Thus, the differential equation that
describes the phenomenon of vapor diffusion is as follows:
∂C ∂M
∇ · ε D ∇C = ε + (1 − ε)ρs (2.3)
∂t ∂t
where ε is the porosity of the fibrous medium, D is the diffusion coefficient, M is

the amount of moisture absorbed per unit mass of fiber, ρs is the fiber density, C is
the water vapor concentration in the voids (inter fibers), and t is the time.
(b) Heat conduction equation
Changes in heat flux in the element arise from various processes: heat conduction
into or out of the element, water phase change (sorption or desorption), changes in
temperature of the solid and gaseous phases. The contribution due to the last cause
is small and will be neglected.
To determine the change in the temperature of the fiber volume element, it was
considered: (a) heat conduction through air and fibers; (b) the heat released when
moisture is absorbed by the fibers.
Thus, the differential equation that describes the heat diffusion phenomenon is as
follows:
∂T ∂M
ρ · cP = ∇ · (K ∇T ) + h s ρ (2.4)
∂t ∂t
where cp is the specific heat, K is the thermal conductivity of the material, h s is the
enthalpy, and T is the temperature. In Eq. (2.4), the assumption that air energy is
negligible compared to fiber is used.
An important point to note is that both the vapor diffusion Eq. (2.3) and the energy
Eq. (2.4) involve M (fiber moisture). This shows that the two processes, moisture
transfer and heat transfer, are coupled, so in general, one process cannot be considered
without considering the other simultaneously.
(c) Equilibrium equation
According to Crank (1975), one can always consider that the fiber comes into
balance with its immediate surroundings. In addition, it is possible to assume linear
dependence on temperature and moisture content and write:
M = α + σ C − βT (2.5)
where M is the amount of moisture absorbed per unit mass of fiber in kgvapor /kgdry fiber ,
C is the concentration of water vapor in the voids (interfibers) expressed in kg/m3 ,
T is the temperature in °C, and α, σ and β are constants. It is just a reasonable
approximation over small ranges of moisture and temperature.
The average value of the quantity of interest Φ can be obtained by a weighted
average using the volume of each control volume as follows:
1
Φ= ∫ ΦdV (2.6)
VV
where Φ = C, T, or even M (Eq. 2.5) and V is the volume of the fibrous medium.
Considering a three-dimensional solid with vapor distribution C = C (x, y, z),

temperature T = T (x, y, z), and moisture M = M (x, y, z), the transient equations
of vapor diffusion (2.3) and heat conduction (2.4) in Cartesian coordinates are given
by:

∂C ∂ ∂C ∂ ∂C ∂ ∂C
[ε + (1 − ε)ρs σ ] = D + D + D + SC
∂t ∂x ∂x ∂y ∂y ∂z ∂z
(2.7)
and

∂T ∂ ∂T ∂ ∂T ∂ ∂T
ρ(cP + h s β) = K + K + K + ST (2.8)
∂t ∂x ∂x ∂y ∂y ∂z ∂z
where
∂M ∂C ∂T
=σ −β (2.9)
∂t ∂t ∂t
D = ε D (2.10)
∂T
S C = (1 − ε)ρs β (2.11)
∂t
and
∂C
S T = h s ρσ (2.12)
∂t
In the models, the following initial and boundary conditions were used:
• Initial condition:
C(x, y, z, t = 0) = Co ; (Mass transfer) (2.13)
T (x, y, z, t = 0) = To . (Heat transfer) (2.14)
• Boundary conditions for mass transfer:

∂C
−D = h m C − Ceq , ∀(x = R1 , y, z, t > 0); (2.15)
∂ x x=R1

∂C
−D = h m C − Ceq , ∀(x, y = R2 , z, t > 0); (2.16)
∂ y y=R2

∂C
−D = h m C − Ceq , ∀(x, y, z = R3 , t > 0). (2.17)
∂z z=R3
• Boundary conditions for heat transfer:

∂ T
−K = h c T − Teq , ∀(x = R1 , y, z, t > 0); (2.18)
∂ x x=R1

∂ T
−K = h c T − Teq , ∀(x, y = R2 , z, t > 0); (2.19)
∂y y=R2

∂ T
−K = h c T − Teq , ∀(x, y, z = R3 , t > 0). (2.20)
∂z z=R3
Numerical Procedure
Often a diffusive problem is so complex and contains intense nonlinear equations that
it cannot be solved by analytical solutions. However, it can be solved by numerical
methods. The numerical method consists of replacing a continuous domain by a
discrete domain and the partial differential equation is replaced by several algebraic
equations, one for each control volume of the discrete domain. One of the main
advantages of this method is the possibility of finding numerical solutions for the
diffusion equation for the most diverse situations, such as non-homogeneous and
non-isotropic medium, variable volume and diffusivity, and any geometry and shape
of the body (Maliska 2004). There are several numerical methods reported in the
literature.
The Finite-Volume Method (FVM) does not present problems of instability or
convergence, ensuring that in each discretized volume, the property under study
obeys the conservation law, giving a conservative characteristic. It is one of the most
used in the discretization of partial differential equations. This method works with
control volumes, thus preserving the finite-volume level. Therefore, FVM is widely
used in solving problems involving heat and/or mass transfer, and fluid flow (Maliska
2004).
In the finite-volume method, any continuous quantity can be approximated by
a discrete model composed of a set of continuous step or linear functions, defined
under a finite number of subdomains. Subdomains are called the control volumes
and the nodal points are well known as centroid of the control volume. In this
method, the partial differential equation that governs the phenomenon is numeri-
cally discretized by integrating it into elementary volumes and time, thus obtaining
Fig. 2.4 Scheme used to exploit the inherent symmetry condition of the parallelepiped: a domain,
b highlight to 1/8 of the parallelepiped, and c new domain
a system of algebraic equations, which must be solved by specific mathematical

techniques.
In order to obtain the numerical solution of the diffusion equation for a
parallelepiped-shaped porous material, the diffusion process takes into account the
following assumptions:
• The thermophysical and mechanical properties are constant;
• The diffusion coefficient is constant throughout the diffusion process;
• The solid is homogeneous and isotropic;
• There is symmetry in each central plane of the solid;
• The only mechanism of water transport within the solid is diffusion;
• Convective boundary conditions at the solid surface, with moisture content and
temperature depending on position and time;
• The field of moisture content and temperature inside the body is uniform at the
beginning of the process;
• Convective mass and heat transfer coefficients are constant for all faces of the
solid.
Because the geometric shape of the parallelepiped is regular, one can use the
symmetry condition and numerically solve the diffusive problem for only one
symmetrical part of the domain, such as studying only the region illustrated in
Fig. 2.4c.
Figure 2.5 illustrates the discretized domain used for discretization of the
governing equation. The numerical solution of the diffusion equation for a paral-
lelepiped was obtained considering a fully implicit formulation. This formulation
was chosen because it presents no instability or convergence problems.
Fig. 2.5 Discretized

three-dimensional domain
with 27 types of control
volumes
Considering Fig. 2.5, and integrating Eq. (2.7) into space and time, the following
result is obtained for a control volume P:

CP − CP0
∂C C ∂C ∂C ∂C
[ε + (1 − ε)ρs σ ] x y z = DeC − Dw y z + DnC − DsC x z
t ∂x e ∂x w ∂y n ∂ y s

∂C
∂C
+ DfC − DbC x y + S C x y z (2.21)
∂z f ∂z b
where superscript zero means that the term must be evaluated at time t prior to
the time of interest, whereas terms without superscript are evaluated at the time of
interest. The subscripts “e”, “w”, “n”, “s”, “f”, and “b” mean the east, west, south,
north, front, and back boundaries, respectively, of a considered control volume, P is
the nodal point, centered on this control volume, and N, S, E, W, F, and B refer to
the neighbors to the north, south, east, west, front, and back, respectively (Figs. 2.5
and 2.6).
From the analysis of Figs. 2.5 and 2.6, the following derivatives for Eq. (2.21) are
obtained:

∂C CE − CP
= (2.22)
∂x e δxe

∂C CP − CW
= (2.23)
∂ x w δxw
Fig. 2.6 Internal control

volume of nodal point P and
its neighbors

∂C CN − CP
= (2.24)
∂ y n δyn

∂C CP − CS
= (2.25)
∂ y s δys

∂C CP − CB
= (2.26)
∂z b δz b

∂C CF − CP
= (2.27)
∂z f δz f
Substituting Eqs. (2.22)–(2.27) in Eq. (2.21) and arranging terms, we have for the
internal control volumes the following algebraic equation:
Ap C P = Ae C E + Aw C W + An C N + As C S + Af C F + Ab C B + B (2.28)
where
x y z y z y z x z
Ap = [ε + (1 − ε)ρs σ ] + DeC + DwC + DnC
t δxe δxw δyn
x z x y x y
+ DsC + DfC + DbC (2.29)
δys δz f δz b
y z
Ae = DeC (2.30)
δxe
y z
Aw = DwC (2.31)
δxw
x z
An = DnC (2.32)
δyn
x z
As = DsC (2.33)
δys
Fig. 2.7 Scheme used to identify the symmetry condition in the parallelepiped (new domain)
x y
Af = DfC (2.34)
δz f
x y
Ab = DbC (2.35)
δz b
x y z 0
B = [ε + (1 − ε)ρs σ ] CP + S C x y z (2.36)
t
Equation (2.28) has important physical significance. The coefficients Ae , Aw , An ,
As , Af , and Ab represent the conductance between point P and its neighbors. The
term CP0 represents the influence of the value of variable C at the previous time on
its value at the present time. In this equation, V = x y z is the volume of the
infinitesimal element considered in Fig. 2.6.
Equation (2.28) is applied to all points within the computational domain except
boundary points, where boundary conditions must be incorporated into the formu-
lation. In this case, volumes adjacent to the body surface, called boundary control
volumes, are used. For such volumes, the integration of the conservation equation
is preceded, as described above, considering the existing boundary conditions. For
example, in the new domain under study (Fig. 2.4c), considering the symmetry condi-
tion, it is found that the mass flux in the west, back, and south boundaries is zero, in

other words, Cw = 0, Cb = 0, and Cs = 0 (Fig. 2.7).
Consequently, for the proposed discretization, with boundary condition
of the third type, it is sufficient to impose h mw = h mb = h ms =
0, (where h mw = h mb = h ms = h m ).
Similarly, to what was obtained for the vapor diffusion equation as applied to the
internal control volumes, the following algebraic equation for the heat transfer is
obtained:
Ap TP = Ae TE + Aw TW + An TN + As TS + Af TF + Ab TB + B (2.37)
where
Fig. 2.8 Two control volumes with transport coefficients DPC e DEC
ρ(cP + h s β) x y z y z y z x z x z
Ap = + K eT + K wT + K nT + K bT
t δxe δxw δyn δys
x y x y
+ K fT + K bT (2.38)
δz f δz b
y z
Ae = K eT (2.39)
δxe
y z
Aw = K wT (2.40)
δxw
x z
An = K nT (2.41)
δyn
x z
As = K sT (2.42)
δys
x y
Af = K fT (2.43)
δz f
x y
Ab = K bT (2.44)
δz b
ρ(cP + h s β) x y z 0
B= TP + S T x y z (2.45)
t
The discretization of the diffusion equation requires knowledge of the D C values

not only at the nodal point, but at the east, west, north, south, front and back faces
of each control volume, as illustrated in Fig. 2.8.
The value of DeC is the value of the property at the interface of the nodal points.
So, it is the value of D C on the common face between P and E. Such value is given
by:
DEC DPC
DeC = (2.46)
(1 − f d )DPC + f d DEC
where
dP
fd = (2.47)
dP + dE
where dP e dE are the distances from the interface “e” to the nodal points P and E,
respectively.
Considering a uniform mesh, we have that f d = 1/2, since in this case dP = dE .
Thus, Eq. (2.46) results in:
2DEC DPC
DeC = (2.48)
DEC + DPC
The average value of C can be obtained by a weighted average using each control
volume as follows (Eq. 2.6):
1
npx−1 npy−1 npz−1

C= Ci jk Vi jk (2.49)
V i=2 j=2 k=2
with

npx−1 npy−1 npz−1

V = Vi jk (2.50)
i=2 j=2 k=2
where V is the volume of the solid, i, j, and k define the position nodal point, in the

control volume considered, Vi jk is the volume value of this elemental volume, npx
− 2, npy − 2, and npz − 2 define the number of control volumes along the x, y, and
z directions, respectively. In the case of a uniform mesh, it’s given:
one-dimensional approach is described as:

Vi jk = x y z (2.51)
To solve the systems of algebraic equations generated by Eqs. (2.7) and (2.8), a
computer code using Mathematica® software was developed. In it, the systems of
linear equations are iteratively solved using the Gauss–Seidel method. It was assumed
that the numerical solution converged when, starting from an initial condition, the
following criterion was met at each nodal point in the computational domain at a
certain time:
n+1
Φ − Φ n ≤ 10−8 (2.52)
where Φ can be C or T, and n represents the nth iteration at each time point. This
criterion from the physical and numerical point of view is sufficiently precise to
guarantee the physical realism of the obtained results. To obtain the results it was
considered a numerical mesh of 20 × 20 × 20 nodal points and a t = 20 s. These
parameters were obtained after a mesh and time step refining was performed.
A program operation flowchart in block diagram form is shown in Fig. 2.9.
Estimation of Process Parameters
(a) Estimation of transport coefficients
With Eqs. (2.1) and (2.2) adjusted, “data capture” moments were established
throughout the process in which the average moisture content and temperature could
be determined so that the distribution of these points was approximately uniform.
Subsequently, these equations were used in the computer code to adjust the diffusive
and convective transport coefficients.
Transport coefficients were obtained by varying their values to minimize the
sum of quadratic deviations between predicted and experimental results. Deviations
between experimental and calculated values and variance were obtained as follows:

n
2
ERMQ = Φi,Num − Φi,Exp (2.53)
i=1
ERMQ
S̄ 2 = (2.54)
n−n

where n is the number of experimental points and n number of adjusted parameters

(number of degrees of freedom).
The initial value of the convective heat transfer coefficient
used
during the adjust-
ment was obtained using the correlations for the Nusselt N̄u , Reynolds (Re), and
Prandtl numbers (Incropera and De Witt 2002), applied to a plane plate as follows:
N̄uk
h c, j = (2.55)
Rj
where R j can be R1 or R2 or R3 (Fig. 2.2), and
1 2 /
1 3
N̄u j = 0.664Re j / Pr (2.56)
Fig. 2.9 Computational algorithm diagram

being
ρv R j
Re j = (2.57)
μ
with validity range (5 × 105 < Re ≤ 1 × 108 ).

The equation used to obtain the initial convective mass transfer coefficient
calcu-

lated for air was obtained using the correlations for Sherwood numbers Sh and
Schmidt (Sc), as follows (Incropera and De Witt 2002):
ShDAB
h m, j = (2.58)
Rj
where DAB is the diffusivity of water vapor in the air, and the Sherwood number
given by:
Sh j = 0.664Re j / Sc1/ 3
1 2
(2.59)
To obtain the apparent density of the samples, we used the following equation:
m fiber
ρsample = (2.60)
Vsample
The equations used to obtain the thermal conductivity and the specific heat
calculated for the sample are given as follows:
ksample = (1 − ε)k(fiber) + εk(air) (2.61)
and
cp,sample = (1 − ε)cp,(fiber) + εcp,(air) (2.62)
(b) Estimation of equilibrium equation parameters
Considering the equilibrium equation, Eq. (2.5) can also be written as follows:
M = a1 + a2 T (2.63)
where a1 = α + σ C e a2 = −β.
With the values of T eq and M eq for each experimental condition, a linear fit of
Eq. (2.63) to the experimental data was performed using the Quasi-Newton numerical
method using the Statistica® Software, with a convergence criterion of 0.000099,
from which we obtained the values of a1 and a2 parameters.
Table 2.2 Thermophysical and process parameters of the sample and fiber used in the simulation
for T = 70 °C
C o (kgvapor /m3 ) C eq (kgvapor /m3 ) ρ(sample) (kg/m3 ) ρ(fiber) (kg/m3 )
0.04125 0.01381 81.956 1450.00
cp,(sample) (J/kg K) cp,(fiber) (J/kg K) k(sample) (W/m K) k(fiber) (W/m K)
961.617968 149.65 0.03141034 0.067
On the other hand, the equation of state for an ideal gas is given by:
P = ρair · R · T (2.64)
where P is the atmospheric pressure, ρ is the density, R is the particular gas constant
(atmospheric air), and T is the drying temperature. Thus, air density within the fibrous
medium can be determined as follows:
P
ρair = (2.65)
R·T
To calculate the equilibrium water vapor concentration in the fibrous medium
(between the fibers), consider the following formula:
Ceq = ρair · UA (2.66)
where UA is the air absolute humidity in voids, obtained from the temperature and
relative humidity of the drying air. So, using the data from C eq and M eq and the value
of β obtained from the adjustment (Eq. 2.63), there is a system of equations with
two unknowns, which allows obtaining the α and σ parameters.
Thermophysical Properties of Materials
Table 2.2 presents some thermophysical properties and process parameters of the
fibrous medium for the drying experiment. These data were used in the simulation.
Table 2.3 presents some thermophysical properties and process parameters of the
drying air at atmospheric pressure for the experiment. These data were used to obtain
the parameters of Table 2.4 and the transport coefficients reported in Table 2.7.
Table 2.4 presents some calculated transport parameters. These data were used to
determine the transport coefficients reported in Table 2.7.
Table 2.3 Thermophysical and process parameters of drying air at atmospheric pressure for T =
70 °C
ρair (kg/m3 ) k (W/m K) μ (N s/m2 ) UA UAsat (kgvapor/ kgdry air )
(kgvapor/ kgdry air )
1.020411 0.028260 19.96557 × 10−6 0.01353746 0.2765

DAB m2 /s cp (kJ/kg K) hs (kJ/kg) Pr Sc
31.1693 × 1.033492 2333.26 0.73016 0.627739
10−6
Table 2.4 Transport

Dimensionless parameters
parameters calculated for the
experimental test in T = Rex Re y Rez
70 °C 127.7713 63.8856 127.7713
Nux Nu y Nuz
6.75860 4.77905 6.75860
Shx Sh y Shz
6.42655 4.54425 6.42655
2.2.3 Results
2.2.3.1 Lumped Analysis
From the analysis of the experimental data obtained, it was observed that the moisture
content decreases with time. In general, the drying rate increases with higher drying
air temperature and lower air relative humidity. Therefore, increasing the drying air
temperature resulted in a shorter processing time.
The surface temperature of the fibrous medium varied during the drying process
and reached thermal equilibrium faster at the highest drying temperature. Since the
surface temperature of the fiber rises during drying, the process occurs at a falling
drying rate, i.e., the migration rate of water from the fiber to its surface is less
than the water removal rate from the surface by the heated air. The fiber temperature
increases as the drying rate decreases. Similar results have been reported for different
researchers (Zhou et al. 2014; Santos et al. 2017).
It is noticed that at the end of the process, the drying rate tends to zero when
the moisture content approaches the hygroscopic equilibrium condition and the fiber
temperature stabilizes, that is, the fiber approaches its thermal equilibrium.
All details of the results and statistical parameters obtained with the model
adjustments to the experimental data are presented in Tables 2.5 and 2.6.
Figure 2.10 shows the fitted curves for the average moisture content of the samples
versus drying time.
Table 2.5 Parameters of Eq. (2.1) obtained after adjustment to experimental data of sisal fiber
moisture content
T (°C) Parameters
c1 k 1 (min−1 ) c2 k 2 (min−1 ) c3 k 3 (min−1 )
70 0.779910 0.031757 0.022230 0.000215 0.011298 0.243766
R (kg/kg)2 Proportion of Loss function
variance (kg/kg)2 (kg/kg)2
0.99995 0.99989 0.000001574
Table 2.6 Parameters of Eq. (2.2) obtained after adjustment to experimental data of sisal fiber
temperature
T (°C) Parameters
c1 (°C) k 1 (min−1 ) c2 (–) k 2 (–) c3 (–) k 3 (min−1 ) k 4 (–)
70 0.536510 0.000406 −5.85983 0.006903 8.947182 13.39565 3.234171
R (°C)2 Proportion of Loss
variance function
(°C)2 (°C)2
0.99737 0.99474 6.887782641
__
T = 70o C Model: M = c1 exp(-k1 t) + c2 exp(-k2 t) + c3 exp(-k3 t)
__
M = (0.077991) exp[-(0.031757) t]+(0.02223) exp[-(0.000215) t]+(0.011298) exp[-(0.243766) t]
0.12
0.10
0.08
M (kg/kg)
0.06
0.04
0.02
0.00
0 100 200 300 400 500
t (min)
Fig. 2.10 Average moisture content of the sample during drying at 70 °C. Experimental (ooo) and
predicted (__)
T s = 70oC Model: T = c1 log2[(k1 t + k2)c2 (k3 t + k4 )c3]

T = (0.53651) log2{[(0.000406) t + (0.006903)] (-5.8598) [(13.3956) t + (3.23417)](8.94718)}
70
60
50
40
T (ºC)
30
20
10
0
0 100 200 300 400 500
t (min)
Fig. 2.11 Sample surface temperature during drying at 70 °C. Experimental (ooo) and predicted
(__)
Figure 2.11 shows the curves of the fiber surface temperature versus drying time.
From the analysis of Tables 2.5 and 2.6 and Figs. 2.10 and 2.11, it can be seen that
a good fit was obtained, with correlation coefficient R above 0.988, in all cases.
2.2.3.2 Equation Equilibrium Analysis
Based on the methodology presented before, we obtained the following equilibrium

equation:
M = 0.044702 + 2.217337C − 0.000784T (2.67)
Equation (2.67) describes the linear dependence of temperature (T ), water

vapor concentration (C), and moisture content (M), fundamental for the coupling
between the vapor diffusion equation and the heat conduction equation. A correlation
coefficient of 0.99 was obtained in this regression.
2.2.3.3 Distributed Analysis
Drying and Heating Kinetics
In this topic will be presented the results of drying and heating kinetics, and distri-
bution of moisture content and temperature inside the fibrous medium, for drying air
Table 2.7 Initial values of the transport coefficients used during the nonlinear regression (T =
70 °C)
Parameters

h mx (m/s) h my (m/s) h mz (m/s)
4.00622 × 10−3 5.66564 × 10−3 4.00622 × 10−3

h cx W/m2 K h cy W/m2 K h cz W/m2 K
3.81996 5.40224 3.81996
Table 2.8 Parameters Estimated transport coefficients for the drying air temperature T = 70 °C
Parameters

h mx (m/s) h my (m/s) h mz (m/s) h cx W/m2 K h cy W/m2 K h cz W/m2 K
5.0622 × 21.6564 × 5.0622 × 10−4 5.538942 7.833248 5.538942
10−4 10−4
2 2
D (m2 /s) α m2 /s ERMQM (kg/kg)2 S M (kg/kg)2 ERMQT (°C)2 S T (°C)2
1.612 × 3.9855592 × 0.0000722468 7.52571 × 967.74872 9.976791
10−6 10−7 10−7
Fig. 2.12 Comparison between numerical and experimental values of the average moisture content
of the fibrous medium as a function of time (T = 70 °C)
temperature of 70 °C. Later, on Tables 2.7 and 2.8 will be presented and discussed the
values of the diffusive and convective transport coefficients obtained after comparing
the predicted data with the experimental data for the experiment performed.
Figure 2.12 presents the comparison of the numerical and experimental values of
the average moisture content (on dry basis) of the fibrous medium as a function of
Fig. 2.13 Comparison between numerical and experimental values of the fibrous medium surface
temperature as a function of time (T = 70 °C)
time for the air temperature of 70 °C. From the analysis of this figure, we can see
that data of there is a good agreement between the numerical and experimental the
average moisture contents throughout the drying process.
The temperature behavior of sisal fibers during drying was described by Eq. (2.4).
The properties of the fibrous medium, which are thermal conductivity (k) and specific
heat (cp ) were obtained using Eqs. (2.61) and (2.62), respectively.
On the surface of the fibrous medium occurs both convective heat transport and
heat transfer associated with moisture evaporation. Taking into account only the
convective heat transport on the surface of the fibrous medium, the boundary condi-
tion of third kind was considered, in which the heat flux on the surface of the
fibrous medium is proportional to the difference between the surface temperature
of the fibrous medium and the drying air temperature (equilibrium temperature).
The proportionality constant hc (convective heat transfer coefficient) was obtained
applying the best square error technique between the numerical and experimental
data of fiber temperature during drying at 70 °C. The best value of hc corresponds to
the lowest value of S̄ 2 .
Figure 2.13 shows the comparison of numerical and experimental values of the
fibrous medium surface temperature as a function of time for the temperature of
70 °C. From the analysis of this figure, we can note that there is good agreement
between numerical and experimental surface temperature values in the first 4000 s
of process.
Since the surface temperature of the fiber rises during drying, the process occurs at
a falling drying rate. The fiber temperature increases as the rate of drying decreases.
It can be seen in Fig. 2.13 that at the end of the process, the drying rate tends to
a) t = 200 s b) t = 700 s c) t = 8000 s
Fig. 2.14 Water vapor concentration distribution (kgvapor /m3 ) in the plane yz at x = 0.025 m (R1 /2)
to a drying air temperature of 70 °C
zero when the moisture approaches the equilibrium moisture content and the fiber
temperature stabilizes, that is, the fiber approaches its equilibrium thermal.
Analyzing the result, it can be stated that the model used to describe the heating
kinetics of the fibrous medium, considering constant volume and transport parameters
can be considered satisfactory, even if a discrepancy between the simulated and
experimental data is perceived from t = 4000 s. This discrepancy may have been
caused by errors in the temperature measurement process during the experiments or
even by the measuring device itself.
These differences observed between the simulated results and the experimental
data of the temperature after the process 4000 s may also indicate that the convective
heat coefficient hc from this time should be lower than in the initial moments. In
this case, the hypothesis of hc variable throughout the process would be a more
appropriate choice.
Water Vapor Concentration and Temperature Distributions
Figures 2.14 and 2.15 show the distribution of water vapor concentration and temper-
ature inside the fibrous medium, analyzed in the planes x = 0.025 m (R1 /2), for three
times 200 s, 700 s, and 8000 s, respectively. It is important to remember that all
results are plotted to 1/8 of the fibrous body volume, due to the symmetry that exists
in the physical problem and in the geometry of the sample.
By analyzing these figures, we can see that water vapor concentration presented
the highest results in the central regions of the body at any time. The decrease in
vapor concentration over time at any position was also noted, tending toward its
equilibrium value for sufficiently long drying times (Fig. 2.12).
a) t = 200 s b) t = 700 s c) t = 8000 s
Fig. 2.15 Temperature distribution (°C) in the plane yz at x = 0.025 m (R1 /2) to a drying temperature
of 70 °C
Temperature has the lowest results in the central regions of the body at any time.
The temperature also increases over time in any position, tending to its equilibrium
value for sufficiently long drying times. This shows that heat flux occurs from the
surface to the center of the material, in contrast to the moisture flux that occurs from
the center to the surface of the material.
Estimation of Transport Coefficients (D, hm and hc )
The mass diffusion coefficient measures the tendency of water molecules to migrate
from one region of high concentration to another of lower concentration. The higher
the diffusion coefficient, the faster the diffusion of one species relative to another.
This coefficient is directly related to the temperature and moisture content.

The initial convective transport coefficients h c and h m were obtained using
Eqs. (2.55) and (2.58), respectively. From these initial values, an optimization process
was performed to obtain the ideal values of the convective coefficients, as described
earlier. Table 2.7 gives the obtained values of these parameters.
Estimation of the transport coefficients h c , h m , and D was made by minimizing
the sum of the squares of the residues, as mentioned earlier. Table 2.8 summarizes
the obtained values of these coefficients as well as relative error and variance for the
experimental test.
In general, the numerical results showed a good agreement with the experimental
data of moisture content and temperature of sisal fibers submitted to drying. The small
errors and variances indicate that the methodology used to estimate the transport
coefficients is satisfactory.
Specifically, with respect to the mass diffusion coefficient (D), it can be said that
it is a multiplication of the vapor diffusion coefficient inside the fibrous medium by
the bed porosity that is, D = ε D . Since the porosity of the medium ε > 0.91, it can
be noted that the drying of the fibrous medium resembles the drying of individual
fibers. This in fact is almost true and can be proved by the value of the D which
is smaller than the DAB (Table 2.3) for the experimental test. This indicates that the
vapor flux inside the fibrous medium is more difficult than in the air outside the
fibrous medium, as expected.
Comparison between the mass diffusivities of porous materials reported in the
literature becomes difficult due to the lack of specific studies of these materials.
In general, it is important to note that differences in mass diffusion coefficient can
be attributed to the different factors, such as geometric considerations, calculation
method, initial and equilibrium moisture contents, physical structure of the material
used, and porosity of the material and boundary conditions.
2.3 Conclusions
In this chapter, the physical problem of simultaneous heat and mass transfer in a paral-
lelepiped porous bed has been studied. Due to the great importance of plant fibers,
emphasis is given to drying of sisal fibers. A transient three-dimensional mathe-
matical modeling, written in Cartesian coordinates was proposed, and its numerical
solution based on the finite-volume method is presented and discussed. Results of
the drying and heating kinetics and the vapor concentration and temperature distri-
butions inside the fiber bed at different times of the process are presented, compared
with experimental data and discussed.
From the obtained results it can be concluded that: (a) The proposed lumped
models can satisfactorily be used to describe the drying process of sisal fibers,
considering that they presented good agreement with the experimental data, with
correlation coefficient greater than 0.988; (b) the finite-volume method proved to
be adequate to predict the phenomenon of heat and mass transfer within the fibrous
medium; (c) drying of sisal fibers occurred at a falling drying rate; (d) there is a
difference in water vapor concentration and temperature between the central region
and the surface of the fibrous medium; (e) the largest water vapor concentration and
temperature gradients are located in the regions near the vertices of the fiber porous
bed. Since these regions are in more intense contact with the drying air, fibers located
in these regions are more susceptible to deformation and thermal effects.
Acknowledgments The authors thank CNPq, FINEP and CAPES (Brazilian Research Agencies),
and the Federal University of Campina Grande (Brazil) for financial support.
References
Angrizani, C.A., Vieira, C. A.B., Zattera, A.J., Freire, E., Santana, R.M.C., Amico, S.C.: Influence
of sisal fiber length and its chemical treatment on the properties of polyester composites. In:
17º CBECIMat—Brazilian Congress of Materials Science and Engineering, Foz do Iguaçu, PR,
Brazil (2006). (In Portuguese)
Barreto, A.C.H., Rosa, D.S., Fechine, P.B.A., Mazetto, S.E.: Properties of sisal fibers treated by
alkali solution and their application into cardanol-based biocomposites. Compos. Part A: Appl.
Sci. Manufac. 42(5), 492–500 (2011)
Crank, J.: The Mathematics of Diffusion. Oxford University Press, London (1975)
Cruz, V.C.A., Nóbrega, M.M.S., Silva, W.P., Carvalho, L.H., Lima, A.G.: B: An experimental
study of water absorption in polyester composites reinforced with macambira natural fiber.
Materialwiss. Werkstofftech. 42(11), 979–984 (2011)
Ferreira, S.R., Lima, P.R.L., Silva, F.A., Toledo Filho, R.D.: Effect of sisal fiber humidification on the
adhesion with portland cement matrices. Rev. Matéria 17(2), 1024–1034 (2012). (In Portuguese)
Incropera, F.P., De Witt, D.P.: Fundamentals of Heat and Mass Transfer. Wiley, New York, USA
(2002)
Lima, A.G.B., Silva, J.B., Almeida, G.S., Nascimento, J.J.S., Tavares, F.V.S., Silva, V.S.: Clay prod-
ucts convective drying: Foundations, modeling and applications. In: Delgado, J.M.P.Q., Barbosa
de Lima, A.G. (eds.) Drying and Energy Technologies. Series: Advanced Structured Materials,
vol. 63, 63edn, pp. 43–70. Springer, Heidelberg (Germany) (2016
Maliska, C.R.: Computational Heat Transfer and Fluid Mechanics, p. 453. LTC, Rio de Janeiro,
Brazil (2004)
Martin, A.R., Martins, M.A., Mattoso, L.H.C., Silva, O.R.R.F.: Chemical and structural characteri-
zation of sisal fibers from Agave Sisalana variety. Polímeros: Ciência e Tecnologia 19(1), 40–46
(2009). (In Portuguese)
Melo Filho, J.A., Silva, F.A., Toledo Filho, R.D.: Degradation kinetics and aging mechanisms on
sisal fiber cement composite systems. Cem. Concr. Compos. 40, 30–39 (2013)
Nóbrega, M.M.S., Cavalcanti, W.S., Carvalho, L.H., Lima, A.G.B.: Water absorption in unsaturated
polyester composites reinforced with caroá fiber fabrics: modeling and simulation. Materialwiss.
Werkstofftech 41(5), 300–305 (2010)
Santos, D.G., Lima, A.G.B., Costa, P.S.: The effect of the drying temperature on the Moisture
removal and mechanical properties of sisal fibers. Def. Diff. Forum 380, 66–71 (2017)
Silva, J. S.: Drying and Storage of Agricultural Products. Aprenda Fácil, Viçosa,) 560 p. (2008).
(In Portuguese)
Silva, R.V.: Polyurethane Resin Composite Derived from Castor Oil and Vegetable Fibers. Doctoral
Thesis in Science and Materials Engineering. University of São Paulo, São Carlos, SP, Brazil
(2003) (In Portuguese)
Wei, J., Meyer, C: Improving degradation resistance of sisal fiber in concrete through fiber surface
treatment. Appl. Surf. Sci. 289, 511–523 (2014)
Zhou, F., Cheng, G., Jiang, B.: Effect of silane treatment on microstructure of sisal fibers. Appl.
Surf. Sci. 292, 806–812 (2014)
Chapter 3
Foam-Mat Drying Process: Theory
and Applications
E. R. Mangueira, A. G. Barbosa de Lima, J. de Assis Cavalcante,

N. A. Costa, C. C. de Souza, A. K. F. de Abreu, and A. P. T. Rocha
Abstract The duck egg is an ideal product to increase human nutrition because
it has a large amount of protein and vitamins. This chapter focuses on the foam-
mat drying technique applied to duck egg white and yolk. The aim is to obtain
powder of these materials after drying. Herein, different topics related to founda-
tions, experiments, and lumped underling are presented and discussed. Drying exper-
iments with and without emulsifiers to obtain stable foam were performed based on
the complete factorial experimental design. The idea is to assist researchers, engi-
neers, and academics in the understanding of this important topic related to food
preservations.
E. R. Mangueira · J. de Assis Cavalcante · N. A. Costa · C. C. de Souza

Department of Chemical Engineering, Federal University of Paraiba (UFPB), 58051-900 João
Pessoa, PB, Brazil
e-mail: ezia.rodrigues@hotmail.com
J. de Assis Cavalcante
e-mail: josy_cavalcante@yahoo.com.br
N. A. Costa
e-mail: nagelalves@hotmail.com
C. C. de Souza
e-mail: christian.carlos.sousa@gmail.com
A. G. B. de Lima (B)
Veloso, 882, Bodocongó, Campina Grande 58429-900, PB, Brazil
A. K. F. de Abreu
Department of Technology and Development, Federal University of Campina Grande (UFCG),
Sumé, PB 58540-000, Brazil
e-mail: amandak_20@hotmail.com
A. P. T. Rocha
Department of Food Engineering, Federal University of Campina Grande (UFCG), Campina
Grande 58429-900, PB, Brazil
e-mail: ana_trindade@yahoo.com.br
https://doi.org/10.1007/978-3-030-47856-8_3
62 E. R. Mangueira et al.
Keywords Foam-mat drying · Egg white · Egg yolk · Experimental · Theoretical
3.1 Drying Theory of Porous Materials
3.1.1 Fundamentals
Drying is one of the oldest processes used by humans in food preservation. In general,
it is a process in which water is removed from the product, involving simultaneous
heat and mass transfer, and phase change of the water present in the food. In this
process, a large amount of water is eliminated, consequently reducing weight of the
product and the water activity that affects microbial growth, enzymatic reactions,
and other reactions of chemical and physical reactions (Gava 2008).
Two of the main factors governing drying are the removal of moisture from the
product surface and the migration of moisture inside the product. The rate of moisture
removal from the surface of the product is a function of both the surface area of the
product exposed to air and the ability of the air to remove water of the surface (drying
potential). The larger the surface area of the product, the larger the heat and mass
exchange area with the airflow, facilitating the removal of water. In this step, the
driving force related to water removal is directly related to the difference between
the water vapor pressure at the material surface, the water vapor pressure in the air
passing through the dryer. When the moisture is removed from the concentration
gradient is created internally in the product, causing a migratory process of moisture
from the center to the product surface (Fioreze 2004).
The migration of moisture from the interior to the surface of the product depends
on the particle size, its internal structure, and the driving force for this migration
(concentration gradient). The larger the particle, the greater the distance to be trav-
eled by heat from surface to center and by moisture from center to surface of the
product to be evaporated. Different products have different internal structures, facil-
itating or hindering moisture migration, according to their porosity and the positive
and negative charges of the carbon chains of the product. Increased driving force
for water migration can be observed by increasing temperature and/or decreasing
relative humidity of the drying air. This increases drying rate and the differences in
concentrations between the inner and surface of the product (Fioreze 2004).
In convective drying process, the water vapor present at the surface of the wet
porous material is removed by air flow, either in natural or forced convection.
For successful drying of biological products, it is well known that several variables
must be taken into account during the process. The main variables are: air relative
humidity; air temperature; air velocity; initial moisture of the product; final moisture
of the product; product shape; and product type (Fioreze 2004).
Some products, when dried, keep their physical and nutritional characteristics
intact and return to their natural appearance or undergo few changes when rehumid-
ified. This characteristic makes the drying process a viable way of preserving food
for human consumption (Cornejo et al. 2003; Mayor and Sereno 2004).
3 Foam-Mat Drying Process: Theory and Applications 63
Fig. 3.1 Typical drying

curve of a wet porous
material
The drying process has evolved from the use of solar energy to current techniques,
including but not limited to tray drying, tunnel drying, spray drying, rotary drying,
freeze drying, osmotic dehydration, extrusion, fluidized bed drying, and microwave
and radiofrequency use (Vega-Mercado et al. 2001). Therefore, there are several
types of dryers; however, the choice of an appropriated method depends on several
factors, among which stand out: product type, dryer availability, drying cost, and
purpose of the dehydrated product (Sagar and Kumar 2010).
When a wet porous material is subjected to the drying process, it can lose water at
a constant velocity throughout the process. As drying progresses under fixed condi-
tions, the rate of water removal decreases (Meloni 2003). This can be seen in Fig. 3.1
which shows the relationship of product moisture content with time in a typical drying
curve. The importance of studying the drying curves of a wet porous product is that
they indicate the rate of water removal at any time measured from the beginning of
the process. A higher or lower slope of the curve indicates the ease or difficulty of
removing water during the drying process (Meloni 2003).
Drying curves can help in choosing a desirable drying time, with the aim of
obtaining the product with the required moisture, and thus increasing a good quality
product.
The A–B section of the curve represents the initial stage of drying when the solid is
heated or cooled and goes from the initial temperature T0 to the wet-bulb temperature
T bu . This stretch is called the stabilization period, in which the surface conditions of
the solid balance with those of the drying air. In general, this stage is described by a
short period and, in general, is negligible of the total drying cycle (Ordonéz 2005).
During this time the drying rate may increase or decrease under the effect of drying
temperature.
In B–C section, the drying rate and product temperature become constant. From
this point, the temperature increases and the drying rate drops rapidly. At this stage,
liquid water evaporates at the surface of the product in the same rate as the liquid
water moves inside it. The surface of the solid remains wet and at a temperature close
to the wet-bulb temperature of the drying air. This stage is known as the constant
drying rate period and continues until it reaches the critical moisture that corresponds
to the point C in Fig. 3.1 (Fellows 2000).
Fig. 3.2 Typical drying rate

curves
The C–D section is called the first falling drying rate period. It occurs when
the velocity of water migration from the interior of the product to the surface is
reduced, and therefore the partial pressure of water vapor at the surface of the product
decreases progressively, and it begins to dry. In this period, the drying rate is limited
mainly by the velocity of moisture movement within the solid, reducing the effects
of external factors, especially air velocity. At this stage, water is entrapped in the
structure of the moisture, and its movement through the dehydrated product is very
slow. Therefore, for the drying rate to be significant, it is necessary to increase the
temperature of the product to provide sufficient desorption heat and to raise the water
vapor pressure inside of the material (Ordonéz 2005). The D–E stretch is well known
as the second-rate period, where the product dries to reach the equilibrium moisture
content (hygroscopic equilibrium condition).
Variations in product moisture content overtime during the drying process give
rise to the drying rate curve (Fig. 3.2). The drying curve is linked to heat and mass
transfer phenomena (Strumillo and Kudra 1986).
In the initial drying period, the solid and its surface are covered by a liquid layer.
The constant drying rate period considers the mass transfer resistance and the limiting
factors of the drying rate are the external conditions and the gaseous boundary layer
at the surface of the product. In the falling drying rate period, the amount of moisture
that reaches the surface of the material decreases gradually. As a result, the water
vapor partial pressure on the material surface also decreases and the drying rate
is controlled by the moisture transport that depends on the moisture concentration
gradient inside the material (Mangueira 2017). In general, the falling drying rate
period is almost always the only one observed for the drying of agricultural and food
products.
3.1.2 Mathematical Modeling in Drying
The study of drying kinetics aims at understanding the behavior of the product during
the process and the prediction of drying time. On the one hand, drying experiments are
of great importance, on the other hand, process modeling plays important role in the
development and optimization of dryers, as well as enabling process standardization
and the reduction of exhaustive drying tests, and predicting the drying behavior of
various materials quickly.
Predicting the falling drying rate is more complex than the constant drying rate
and encompasses not only external heat and mass transfer mechanisms but also
internal mechanisms in the product. The complexity of phenomena during drying
leads researchers to propose numerous theories and multiple empirical formulas
to predict the drying rate adequately. These theories can be summarized as being
derived from two other theories: diffusional theory and capillary (Park et al. 2007).
Diffusional theory is based on Fick’s law, which expresses mass flow rate per unit
area as proportional to the water concentration gradient within the product. It is
a model used for the falling drying rate period. However, the analytical solution
of Fick’s diffusional model requires that boundary conditions be known and that
the effective means diffusivity be specified. These limitations, in addition to the
requirement of knowing the material geometry, often lead searchers to use empirical
or semi-empirical models.
Semi-theoretical models are generally derived from the simplification of a solution
in series of Fick’s second law (Doymaz 2005).
The empirical method is used for drying analysis using experimental data, which
can be determined in laboratory and in the use of dimensionless analysis (Gouveia
et al. 2002). This method is generally based on drying external conditions such as
temperature, relative humidity, and drying-air velocity (Carlesso et al. 2007), without
providing information on energy or mass transport within the product.
From the drying data, it is possible to study the drying kinetics, with the aid of the
drying characteristic curve of the product. In fact, to adequately product the drying,
it is necessary to know the initial moisture content of the product to be drier, the
relationship of water with the solid structure, and the mechanism of water migration
from inside the material to its surface (Park et al. 2001).
Some empirical and semi-empirical mathematical models are summarized in
Table 3.1. These models can be fitted to experimental data by nonlinear regres-
sion using appropriately statistical software (Doymaz 2005; Biazus 2006; Marques
Table 3.1 More common

Name Model References
empirical and semi-empirical
models used to describe the Henderson and RU = a exp(−Kt) Park et al. (2002)
drying process Pabis
Midilli et al. RU = a exp(−Kt n ) + Midilli et al. (2002)
bt
Page RU = exp(−Kt n ) Zhang and
Litchfield (1991)
Page (modified) RU = a exp(−Kt n ) Mangueira (2017)
Newton RU = exp(−Kt) Liu et al. (1997)
2009). In Table 3.1, RU = X/X o is the moisture content ratio of the product; t is the
time; K is the drying coefficient; and a, b, and n are constants.
3.2 Foam-Mat Drying
3.2.1 General Foundations
Foam-mat drying is a technique used to obtain powdered food products. In this tech-
nique, liquid or semi-liquid foods are transformed into stable foams by the addition or
not of foaming agents (which is intended to keep the foam stable during the process)
and incorporation of air, nitrogen, or other gases in blenders or other foam generation
equipment (Brennan 1994).
Foam is a colloidal dispersion in which gas is dispersed in a continuous liquid
phase. The dispersed phase is referred to as the internal phase and the continuous
phase is called the external phase (Baniel et al. 1997). Based on the ratio of dispersed
phase to continuous phase, the foams can be classified into polyhedral foam and
diluted bubbling foam. In polyhedral foams, the proportion is large, resulting in a
large number of bubbles. As the number of bubbles increases, they push themselves
to form a honeycomb structure. Egg white foam and beer foam are good examples
of polyhedral foam. In diluted foams, the proportion is small; therefore, individual
bubbles retain their spherical shape. Chocolate mousse is a good example of diluted
bubbling foams (Prins 1988). The gas phase (usually air) is incorporated as evenly
distributed small particles. The idea is to the texture and appearance of the product
(Narchi et al. 2009).
The foams have thin, flat, and liquid films or lamella between bubbles. The cover-
slips meet at a point called the plateau border (Fig. 3.3). As described in Fig. 3.3, gas
bubbles are confined to the structures formed by the foam and plateau border cover-
slips. Other foam characteristics depend on the air interface that determines foam
Fig. 3.3 Schematic representation of a foam structure

stability. The use of viscous liquids for foaming results in stable foaming. The foam
texture is also influenced by proteins and surfactants as they help in the formation of
stable foam (Vernon-Carter et al. 2001).
The mechanical strength of the lamella determines the stability of the foam along
with its air/water interface properties. If viscous liquids are used for foam production,
they would produce more stable foams due to increased lamella elasticity (Dickinson
1998).
Foam increases drying efficiency because it increases surface area and the heat
and mass transfer. In addition, capillarity through the foam pores facilitates moisture
loss. This makes drying in a foam mat approximately three times faster than drying
in a similar liquid layer (Muthukumaran et al. 2008; Rajkumar et al. 2007). Foam
thickness directly influences drying time, but this effect is greater for foods that are
dehydrated in solid form (Kadam et al. 2010).
After production, the foam is spread as a thin sheet or mat and exposed to hot
airflow to be dried until the desired moisture content. Drying is performed at relatively
low temperatures to form a thin porous layer which is disintegrated to produce a free-
flowing powder. The larger surface area exposed to the drying air is the main cause
of accelerated moisture removal (Brygidyr et al. 1977). During drying, moisture
can be reduced to a level ranging from 1 to 5%, which prevents microbial and
enzymatic deterioration. In addition to a substantial reduction in weight and volume, it
minimizes packaging, storage, and transportation costs (Falade and Solademi 2010).
Foam-mat drying is used in heat-sensitive foods as it requires lower dehydra-
tion temperatures and drying time due to a larger surface area exposed to air, and
consequently, a faster drying rate, thus accelerating the water removal process and
obtaining an easily rehydrated porous product (Karim and Chee-Wai 1999; Rajkumar
et al. 2007).
This technique has some advantages over other liquid drying techniques, such as
simpler technique, lower operating cost and allows the use of lower temperatures,
which better preserves the taste and nutritional value. According to Franco et al.
(Franco 2015), the powder produced by this method is easily reconstituted, presenting
characteristics of texture, color, taste, and nutritional composition very similar to
the original material. This consequently increases the commercial possibilities of
obtaining dehydrated products by the method, especially for heat-sensitive foods.
The main disadvantages of this technique are related to the need for a large drying
surface area to meet high production rates, which increases the investment cost
(Francis 2000). Furthermore, additives can modify the taste, aroma, and color char-
acteristics of the food. In addition, a lack of foam stability may occur during heating
or drying processes (Karim 1999), thus some variables such as the chemical nature
of the raw materials, soluble solids, type, and concentration of foaming agent have
influenced the foam stability (Hart et al. 1963).
3.2.2 Different Methods for Foam Formation
The quantity and quality of the foam produced is determined by the different foaming
techniques. The most common foaming methods are whipping, shaking, and bubbling
(Dehghannya et al. 2018).
3.2.2.1 Whipping or Beating
Whipping is a process that involves adding a large amount of air to a known amount
of liquid to generate foam (Lomakina and Mikova 2006). This can be accomplished
using various devices such as mixers and homogenizers. These devices can mix a
variety of food materials including fruits, vegetables, and liquids. In this process,
the stirring air gets entrapped in a liquid. The amount of air entrapped in a liquid
increases with increasing agitation. Incorporation of air into the liquid initially results
in large bubbles, which upon further agitation are reduced to a smaller size, providing
a homogeneous foamy structure to the food material. The final size of the air bubble
depends on the stirring speed, equipment design, and rheological properties of the
liquid. This technique is widely applied in the food processing sector and also for
the basic study of foam (Dehghannya et al. 2018).
3.2.2.2 Shaking
In this method, the foam is generated by vigorous stirring of the liquid. The volume of
foam produced by this method depends on the magnitude and frequency of agitation,
and the shape and size of the container, temperature, type, and concentration of
foaming agent (Arzhavitina and Steckel 2010). This method is slower compared to
the whipping or bubbling method, as under similar agitation conditions they produce
less foam volume (Lomakina and Mikova 2006).
3.2.2.3 Bubbling or Sparging
In this method, gas is injected into a known amount of liquid through small openings
(Arzhavitina and Steckel 2010), where bubbles of uniform size are produced. The
size of the bubbles can be controlled by adjusting the size of the opening through
which air is injected. The volume of foam produced depends on the amount of liquid
and foaming agent. In this method, the liquid can be completely foamed if a large
amount of air is injected (Mounir 2017).
3.2.3 Foaming Agents
Food foams are composed of air and liquid and sometimes it is necessary to use
an active agent on the surface (Kinsella 1981). A foaming agent is a surfactant that
facilitates foaming when present in small amounts. The foaming agent reduces the
surface tension between two liquid materials or between a solid and liquid material
that results in foam generation.
A good foaming agent must be able to stabilize the foam adequately and rapidly
at low concentrations; effectively function over a wide range of pH values and
ability to perform effectively in the presence of foam inhibitors such as fat, flavoring
substances, and alcohol (Zayas 1997). The most commonly used foaming agents are
egg albumin, milk protein, soy protein, and gelatin.
3.2.3.1 Egg Albumin
Egg albumin is a natural protein found in eggs with good foaming properties
(Sangamithra et al. 2015). By rapidly beating the egg albumin, the air/liquid inter-
face is denatured and interact with each other to form a stable film (Lomakina and
Mikova 2006). Therefore, the whipping time required by egg albumin is compara-
tively shorter compared to other foaming agents. This implies that egg white proteins
could be adsorbed faster at the air–liquid interface and more rapidly denatured than
other proteins (Townsend and Nakai 1983).
3.2.3.2 Whey Protein
Whey protein is obtained from the dairy industry as a byproduct during cheese
production (Tariq et al. 2003). This is one of the main sources of protein in industrial
foods because of its properties, which include its use as an emulsifier, its nutritional
content, and its ability to form gel and stable foam (Broch et al. 2014). Due to the
higher solubility of whey protein in water and on its surface, whey protein has the
ability to form a high-quality foam (Sangamithra et al. 2015).
Whey protein has the ability to retard oxidation reactions in dry food materials.
Furthermore, whey protein has a greater ability to bind flavored compounds, making
it highly conducive to working with vegetables with sensitive and volatile constituents
(Zhang et al. 2017).
3.2.3.3 Soy Protein
Soy protein can be obtained by removing soy oil at a lower temperature. Isolated soy
protein is a highly purified form of protein, with a minimum protein content of 90%
(Nishinari et al. 2014). Isolated soy protein has many functional properties such as
solubility, water and fat absorption, water retention capacity, viscosity, foaming or
whipping, emulsification, and gelling (Liu et al. 1958).
3.3 Applications: Drying of Egg White and Yolk of Duck

Egg
3.3.1 Material Preparation
Duck eggs were purchased from the popular commerce of the city of João Pessoa,
Paraíba, Brazil. Following, they were cleaned and sanitized with chlorinated water
(50 ppm) according to the industrial and sanitary inspection of products regulation
of animal origin (Mapa 2005). After washing, the duck eggs were broken, and the
egg white and yolk were separated manually. Then, they were weighed and beaten
in a food mixer to obtain the foam.
3.3.2 Experimental Planning
Experimental planning is used in basic and technological research, where many

factors can be varied at the same time, and the analysis of variance (ANOVA) is used
to determine which factors are statistically significant. The analysis of the signifi-
cance of the parameters can also be performed using the F-test values, which can
be obtained by the ratio between the quadratic means associated with the regression
and the residuals. The use of the central point allows to add a third level for each
factor, thus enabling the factorial study using the response surface methodology, as
well as quantifying the significance of possible curvature and errors associated with
individual effects and interactions between them.
For the accomplishment of the experiments, a complete factorial experimental
design was carried out 23 + 3 central points, with the input variables for the egg
white one: temperature (50, 60, and 70 °C), agitation rate (6, 7, and 8 levels), and
stirring time (4, 5, and 6 min), and for the yolk, the input variables were temperature
(50, 60, and 70 °C), emulsifier concentration (Emustab®) (7, 10, and 13%),. and
stirring time (4, 5, and 6 min). The following output variables were considered: final
moisture of the product and drying time (min) for both.
Tables 3.2 and 3.3 present the coded and actual values of the independent vari-
ables and the matrix of the complete factorial experimental design for egg white,
respectively. Tables 3.4 and 3.5 present the coded and actual values of the indepen-
dent variables and the matrix of the complete factorial experimental design for the
yolk, respectively.
The complete factorial experimental design methodology was used aiming the
proposition of statistical models able to adequately predict the characteristics of the
Table 3.2 Coded and real

Independent variables Levels
values of the independent
variables for the egg white −1 0 1
vag (level) 6 7 8
t ag (min) 4 5 6
T (°C) 50 60 70
vag —stirring rate; t ag —stirring time; T —temperature
Table 3.3 Matrix of

Experiment Independent variables
complete factorial
experimental design 23 + 3 vag (level) t ag (min) T (°C)
central points for the egg 1 (−1) 6 (−1) 4 (−1) 50
white
2 (1) 8 (−1) 4 (−1) 50
3 (−1) 6 (1) 6 (−1) 50
4 (1) 8 (1) 6 (−1) 50
5 (−1) 6 (−1) 4 (1) 70
6 (1) 8 (-1) 4 (1) 70
7 (−1) 6 (1) 6 (1) 70
8 (1) 8 (1) 6 (1) 70
9 (0) 7 (0) 5 (0) 60
10 (0) 7 (0) 5 (0) 60
11 (0) 7 (0) 5 (0) 60
Table 3.4 Coded and actual

Independent Levels
values of independent
variables for the yolk variables −1 0 1
t ag (min) 4 5 6
C (%) 7 10 13
T (°C) 50 60 70
t ag —stirring time; T —temperature; C—emulsifier concentration
powder obtained after the foam-mat drying of the egg white and the yolk. Statistical
analysis was performed using the Statistica® 12 software, where the obtained data
were interpreted by analysis of variance (ANOVA), for the comparison of arithmetic
means, calculating the main effects and interactions of the variables on the obtained
responses.
Table 3.5 Matrix of

Experiment Independent variables
complete factorial
experimental design 23 + 3 C (%) t ag (min) T (°C)
central points for the yolk 1 (−1) 7 (−1) 4 (−1) 50
2 (1) 13 (−1) 4 (−1) 50
3 (−1) 7 (1) 6 (−1) 50
4 (1) 13 (1) 6 (−1) 50
5 (−1) 7 (−1) 4 (1) 70
6 (1) 13 (−1) 4 (1) 70
7 (−1) 7 (1) 6 (1) 70
8 (1) 13 (1) 6 (1) 70
9 (0) 10 (0) 5 (0) 60
10 (0) 10 (0) 5 (0) 60
11 (0) 10 (0) 5 (0) 60
3.3.3 Experiment of Foam-Mat Drying
The foam obtained after beating using the Arno Deluxe Planetary Mixer SX80 was
placed in aluminum trays (Fig. 3.4) and set was placed in the oven at a constant
temperature of 50, 60, and 70 °C. At regular time intervals, the trays were weighed
Fig. 3.4 Foam of a egg

white and b yolk of the duck
egg arranged in a tray
a)
b)
on a semi-analytical digital scale, accurate to ±0.01 g until they reached constant

weight. The dried material was removed from the tray with the aid of spatulas, packed
in polyethylene bags, and closed.
In this stage, we studied the drying kinetics of the egg white and yolk, where
the experiments were performed according to the complete factorial design 23 + 3
central points as described in Table 3.1. After completion of drying, some empirical
models were fitted to the experimental moisture content data.
3.3.4 Analysis of Results
3.3.4.1 Duck Egg White
Duck egg white has good air incorporation capacity where the addition of a foaming
and/or stabilizing agent is not required to produce a stable foam. This is due to the
action of its proteins, which move through the aqueous phase and are spontaneously
absorbed by the liquid–gas interface where the viscoelastic film is subsequently
formed. The result of protein adsorption is related to reduction in surface tension,
which improves the foaming ability, as well as the ability to encapsulate and retain
incorporated air (Davis and Foegeding 2007).
Table 3.6 shows the results of moisture content (X f ) and drying time (t f ) for the
egg white of the duck at the end of foam-mat drying process.
Figures 3.5, 3.6, and 3.7 show the drying kinetics for the duck egg white foam at
temperatures of 50, 60, and 70 °C, respectively. Figures 3.8, 3.9, and 3.10 illustrate
Table 3.6 Moisture content values on dry basis and drying time at the end of drying of the duck
egg white
Experiment Independent variables Dependent variables
vag (level) t ag (min) T (°C) X f (db) t f (min)
1 (−1) 6 (−1) 4 (−1) 50 0.1475 250
2 (+1) 8 (−1) 4 (−1) 50 0.4559 250
3 (−1) 6 (+1) 6 (−1) 50 0.0596 250
4 (+1) 8 (+1) 6 (−1) 50 0.0689 250
5 (−1) 6 (−1) 4 (+1) 70 0.1182 150
6 (+1) 8 (−1) 4 (+1) 70 0.4158 110
7 (-1) 6 (+1) 6 (+1) 70 0.0623 110
8 (+1) 8 (+1) 6 (+1) 70 0.0461 180
9 (0) 7 (0) 5 (0) 60 0.0224 180
10 (0) 7 (0) 5 (0) 60 0.1810 210
11 (0) 7 (0) 5 (0) 60 0.1896 130
Fig. 3.5 Drying curves of duck egg white foam at a temperature of 50 °C
the specific water mass flowrate (ṁ ) as a function of drying time, obtained for each
experiment performed.
After analysis of these figures, it can be observed that the drying curves presented
both constant (approximately) and falling drying rate period. It can be observed
that there was a variation in the drying time for the different temperatures, being
the drying at 50 °C the longest, not exceeding 250 min, and the fastest, using the
Fig. 3.8 Specific drying rate of duck egg white during foam-mat drying at temperature of 50 °C
temperature of 70 °C, drying approximately 180 min. This is due to the higher
heat and mass transfer between air and foam layer, which proves that temperature
positively influences the drying of egg white and that drying occurs with moderate
velocity even at low temperatures.
In addition, it was found that both levels and stirring time affect the moisture
reduction of the product, especially at low temperatures. This implies that the domi-
nant variable in the low-temperature foam-mat drying process is the heat and mass
exchange area available in the product. However, at high temperatures, it is the
temperature of the drying air that determines the phenomenon behavior. Obviously,
in both cases, the drying-air potential is directly related to the relative humidity and
the drying-air velocity (in the constant drying rate period).
Pereira (Pereira 2015), in his studies on chicken egg white drying, reports values
for the drying time, of approximately 360 min at temperatures of 50, 60, and 70 °C.
From some mathematical models reported in Table 3.1, nonlinear regressions
were made to the experimental data. For each drying condition, Table 3.7 shows the
results of the statistical parameters obtained with this procedure. The best-fit model
Table 3.7 Statistic parameters of the modified Page’s model after fitting to the experimental data
for the drying of the duck egg white at 50, 60, and 70 °C
Experiment Parameters
X 0 (db) K (min−1 ) a (–) n (–) R2 (–) S (–)
1 6.1017 0.0010 0.9878 1.4886 0.9988 0.0051
2 9.7615 0.0138 1.0394 1.0477 0.9945 0.0219
3 5.6573 0.0009 0.9599 1.4450 0.9965 0.0119
4 5.7980 0.0008 0.9678 1.5687 0.9984 0.0072
5 6.0155 0.0027 0.9766 1.5177 0.9988 0.0044
6 8.9434 0.0055 0.9872 1.3774 0.9994 0.0016
7 4.4871 0.0027 0.9681 1.5458 0.9981 0.0056
8 3.9617 0.0028 0.9684 1.5619 0.9983 0.0070
9 2.9781 0.0043 0.9822 1.3707 0.9976 0.0095
10 2.9775 0.0023 0.9774 1.4369 0.9969 0.0126
11 3.1212 0.0070 0.9955 1.2698 0.9979 0.0060
(modified model Page’s) was chosen taking into consideration the statistical analysis
(coefficient of determination above 0.99 and estimation errors less than 0.01).
The graph showing the result predicted by the Modified Page’s model and the
experimental dimensionless moisture content at 50, 60, and 70 °C are illustrated in
Figs. 3.11, 3.12, and 3.13, respectively.
Fig. 3.11 Comparison between predicted (modified Page’s model) and experimental results of the
moisture content ratio during the foam-mat drying process of the duck egg white at 50 °C
3.3.4.2 Duck Egg Yolk
For the production of duck egg yolk foam, the Emustab® emulsifier (Sousa 2017)
was required. In studies realized by Negreiros (Negreiros 2016) related to foam-mat
drying chicken egg yolk, the egg white was used as emulsifier. In the duck egg yolk,
it was not possible to produce the foam using the egg white because, despite the
emulsifying characteristic of the duck egg yolk, this product has a high-fat content,
which makes the formation of foam difficult.
Table 3.8 shows the results of moisture content (X f ) and drying time (t f ), for the
duck egg yolk at the end of drying process.
Figures 3.14, 3.15, and 3.16 show the drying kinetics for the duck egg yolk foam
at temperatures of 50, 60, and 70 °C, respectively. Figures 3.16, 3.17, and 3.18
illustrate the specific water mass flowrate (ṁ ) as a function of time, obtained for
each experiment performed.
After analysis of these figures, it can be observed in Figs. 3.14, 3.15, and 3.16 that
the drying curves present approximately constant and falling drying rate periods. It
can also be observed that there was a variation in the drying time for the different
temperatures, being the drying at 50 °C the longest, occurring in approximately
450 min, and the fastest, using the temperature of 70 °C, in a drying time approxi-
mately 250 min, almost half of drying realized at 50 ° C. With this, it was possible
to prove the influence of temperature on foam-mat drying process. Approximate
drying time values were found by Negreiros (Negreiros 2016) in their studies related
to foam-mat drying of chicken egg yolk at the same temperatures. The experiments
show a good reproducibility in the behavior of the drying curve to the center point
cited in Table 3.5 (Experiments 9–11).
Table 3.8 Moisture content values on dry basis and drying time at the end of drying for duck egg
yolk
Experiment Independent variables Dependent Variables
C (%) t ag (min) T (°C) X f (db) t f (min)
1 (−1) 7 (−1) 4 (−1) 50 0.0144 450
2 (+1) 13 (−1) 4 (−1) 50 0.1406 450
3 (−1) 7 (+1) 6 (−1) 50 0.0058 450
4 (+1) 13 (+1) 6 (−1) 50 0.0024 390
5 (−1) 7 (−1) 4 (+1) 70 0.0008 210
6 (+1) 13 (−1) 4 (+1) 70 0.1400 180
7 (−1) 7 (+1) 6 (+1) 70 0.0124 250
8 (+1) 13 (+1) 6 (+1) 70 0.0065 210
9 (0) 10 (0) 5 (0) 60 0.0842 290
10 (0) 10 (0) 5 (0) 60 0.0223 290
11 (0) 10 (0) 5 (0) 60 0.0866 250
Fig. 3.14 Drying curves of duck egg yolk foam at a temperature of 50 °C
Figures 3.17, 3.18, and 3.19 show the specific drying rates for the duck egg yolk
at temperatures of 50, 60, and 70 °C, respectively. From the analysis of these figures,
we state the existence of both constant and falling drying rate periods.
Now, as reported for duck egg white, for some mathematical models reported
in Table 3.1, nonlinear regression was made to the experimental data. The results
Fig. 3.17 Specific drying rate of duck egg yolk during foam-mat drying at temperature of 50 °C
presented in Table 3.9 are only of the model with statistically significant fitting
(modified Page’s model).
The graphs showing the result predicted by the Modified Page’s model and the
experimental dimensionless content at 50, 60, and 70 °C are shown in Figs. 3.20,
3.21, and 3.22, respectively.
3.4 Final Considerations
In this chapter, the physical problem of foam-mat drying has been addressed. Special
attention is given to egg white and yolk, which are protein-rich foods. Here, the
theoretical (via grouped models) and experimental (observed in experimental design)
approaches are made with the aim of obtaining powder product.
Table 3.9 Statistic parameters of the modified Page’s model after fitting the experimental data for
the drying of the duck egg yolk at temperature of 50, 60, and 70 °C
Experiment Parameters
X 0 (db) K (min−1 ) a (–) n (–) R2 (–) S (–)
1 0.8338 0.0026 0.9877 1.1945 0.9992 0.0041
2 1.1588 0.0042 1.0002 1.0556 0.9985 0.0061
3 0.8095 0.0027 0.9634 1.2139 0.9975 0.0131
4 0.8370 0.0013 0.9686 1.3740 0.9985 0.0078
5 0.8616 0.0040 0.9678 1.3419 0.9979 0.0086
6 1.1551 0.0072 0.9951 1.1194 0.9992 0.0024
7 0.7836 0.0061 0.9832 1.2222 0.9992 0.0036
8 0.8348 0.0036 0.9848 1.3750 0.9994 0.0027
9 1.0756 0.0047 0.9844 1.1253 0.9994 0.0023
10 0.9976 0.0042 0.9765 1.1962 0.9989 0.0044
11 1.0133 0.0081 0.9987 1.0961 0.9983 0.0063
moisture content ratio during the foam-mat drying process of duck egg yolk at 50 °C
From the obtained results, it can be concluded that:

(a) For the duck egg white, the drying-air temperature, the stirring rate, and the
stirring time influenced the final moisture content of the obtained powder. For
the duck egg yolk, the drying-air temperature, Emustab® concentration and
stirring time influenced the final moisture content. Verifying that the higher the
temperature the shorter the drying time.
(b) The drying curves for both duck egg white and yolk showed approximately
constant and falling drying rate. The modified Page’s model was the empirical
model with best fit to the experimental data.
(c) Duck egg white foams dried at 50 and 70 °C were considered to be egg white
powder only for a stirring time greater than 5 min (moisture content, X < 8%).
For the duck egg yolk, yolk powder was obtained in all experimental conditions.
(d) The production of the duck egg powder obtained with the foam-mat drying
process proved to be a viable alternative. A batch averaged time at 3 h for the
egg white and 5 h for the egg yolk were obtained.
Acknowledgments The authors are grateful for the financial support provided by CNPq, CAPES,
and FINEP (Brazilian Research Agencies). We also acknowledge scientific support from the authors
mentioned in this chapter.
References
Arzhavitina, A., Steckel, H.: Foams for pharmaceutical and cosmetic application. Int. J. Pharm.
394(1–2), 1–17 (2010)
Baniel, A., Fains, A., Popineau, Y.: Foaming properties of egg albumen with a bubbling apparatus
compared with whipping. J. Food Sci. 62(2), 377–381 (1997)
Biazus, J.P.M.: Optimization of zea mays malt drying. Food Sci. Technol. 26(4), 787–792 (2006)
Brennan, J. G.: Food Dehydration: A Dictionary and Guide, 189 p. Buttenvorth-Heinemann, Oxford
(1994)
Broch, A., Jena, U., Hoekman, S.K., Langford, J.: Analysis of solid and aqueous phase products
from hydrothermal carbonization of whole and lipid-extracted algae. Energies 7(1), 62–79 (2014)
Brygidyr, A., Rzepecka, M., Mcconnell, M.: Characterization and drying of tomato paste foam by
hot air and microwave energy. Can. Inst. Food Sci. Technol. J. 10(4), 313–319 (1977)
Carlesso, V.O., Berbert, P.A., Silva, R.F., Detmann, E.: Evaluation of thin mat drying models of
yellow passion fruit seeds. Braz. J. Seeds 29(2), 28–37 (2007)
Cornejo, F.E.P., Nogueira, R.I., Wilberg, V.C.: Drying as a method of preserving fruit. Rio
de Janeiro: Embrapa (2003). http://www.ctaa.embrapa.br/upload/publicacao/doc54-2003.pdf.
Accessed October (2019)
Davis, J.P., Foegeding, E.A.: Comparisons of the foaming and interfacial properties of whey protein
isolate and egg white proteins. Colloids Surf., B 54(2), 200–210 (2007)
Dehghannya, J., Pourahmad, M., Ghanbarzadeh, B., Ghaffari, H.: Heat and mass transfer modeling
during foam-mat drying of lime juice as affected by different ovalbumin concentrations. J. Food
Eng. 238(June), 164–177 (2018)
Dickinson, E.: Proteins at interfaces and in emulsions Stability, rheology and interactions. J. Chem.
Soc. Faraday Trans. 94(12), 1657–1669 (1998)
Doymaz, I.: Drying behaviour of green beans. J. Food Eng. 69(2), 161–165 (2005)
Falade, K.O., Solademi, O.J.: Modelling of air drying of fresh and blanched sweet potato slices.
Int. J. Food Sci. Technol. 45(2), 278–288 (2010)
Fellows, P.: Food Processing Technology. Principles and Practice, 2 edn, p. 562. CRC Press, New
York (2000)
Fioreze, R.: Principles of Drying Biological Products, vol. 229. University Publisher/UFPB, João
Pessoa (2004)
Francis, F.J.: Encyclopedia of Food Science and Technology, vol. 12907, 2nd edn. Wiley, New York
(2000)
Franco, T.S.: Dehydration of yacon juice by the foam mat method. Doctoral Thesis in Food
Engineering. Federal University of Paraná, Curitiba, Brazil (2015). (In Portuguese)
Gava, A.J.: Food Technology: Principles and Applications. Nobel, São Paulo (2008)
Gouveia, J.P.G., Moura, R.S.F., Almeida, F.A.C., Oliveira, A.M.V., Silva, M.M.: Evaluation of
cashew drying kinetics through experimental design. Braz. J. Agri. Environ. Eng. 6(3), 471–474
(2002)
Hart, M.R., Graham, R.P., Ginnette, L.F., Morgan Jr., A.I.: Foam-mat drying requires stiff, stable
foams. Food Technol. 17(10), 90–92 (1963)
Kadam, D.M., Wilson, R.A., Kaur, S.: Determination of biochemical properties of foam-mat dried
mango powder. Int. J. Food Sci. Technol. 45(8), 1626–1632 (2010)
Karim, A.A., Chee-Wai, C.: Characteristic of foam prepared from starfruit (Averrhoa carambola
L.) puree by using methyl cellulose. Food Hydrocolloids 13(2), 203–210 (1999)
Kinsella, J.: Functional properties of proteins: possible relationships between structure and function
in foams. Food Chem. 7, 273–288 (1981)
Liu, K., Johnson, L. A., Knapp, H.: Soybeans as Functional Foods and Ingredients. In: Soyfoods, L.,
KeShun (eds.) Chapter 1: Soybeans as a Powerhouse of Nutrients and Phytochemicals, pp. 1958–
2053. Champaign: AOCS Press (2004)
Liu, Q., Martins, M.D., Bakker-Arkema, F.W.: Stochastic modelling of grain drying: Part 1:
experimental investigation. J. Agri. Eng. Res. 66(4), 267–273 (1997)
Lomakina, K., Mikova, K.: A study of the factors affecting the foaming properties of egg white—a
review. Czech J. Food Sci. 24(3), 110–118 (2006)
Mangueira, E.R.: Study of duck egg (foam mat drying). Master´s dissertation, in Chemical Engineer.
Federal University of Paraiba, João Pessoa (2017). (In Portuguese)
Mapa, M.D.: Regulation of industrial and sanitary inspection of animal origin product (2005)
Marques, G.M.R.: Drying of sugarcane juice in foam mat and sensory evaluation of the product.
Dissertation (Master in Food Engineering)—State University of the Southwest of Bahia,
Itapetinga, Brazil (2009). (In Portuguese)
Mayor, L., Sereno, A.M.: Modelling shrinkage during convective drying of food materials: a review.
J. Food Eng. 61(3), 373–386 (2004)
Meloni, P.L.S.: Dehydration of Fruits and Vegetables. Frutal Institute (2003). http://www.eteavare.
com.br/arquivos/20_1959.pdf. Accessed October (2019)
Meloni, P.L.S.: Dehydration of Fruits and Vegetables, p. 87. Frutal Institute, Fortaleza (2003)
Midilli, A., Kucuk, H., Yapar, Z.A.: New model for single-layer drying. Dry. Technol. 20(7), 1503–
1513 (2002)
Mounir, S.: Foam Mat Drying. In: Prabhat, K., Nema, B.P.K., Mujumdar, A.S. (eds.) Drying
Technologies for Foods-Fundamentals and Applications. CRC Press, New York (2017)
Muthukumaran, A., Ratti, C.; Raghavan, V.G.S.: Foam-mat freeze drying of egg white and mathe-
matical modeling. Part I: optimization of egg white foam stability. Dry. Technol. 26(4), 508–512
(2008)
Narchi, I., Vial, C., Djelveh, G.: Effect of protein–polysaccharide mixtures on the continuous
manufacturing of foamed food products. Food Hydrocolloids 23, 188–201 (2009)
Negreiros, J.K.S.: Study of the kinetics of drying of egg in a foam mat (foam-mat drying) and the
characterization of the obtained product. 63 p. Final course report (Undergraduate in Chemical
Engineering), Federal University of Paraíba, João Pessoa, Brazil (2016). (In Portuguese)
Nishinari, K., Fang, Y., Guo, S., Phillips, G.O.: Soy proteins: a review on composition, aggregation
and emulsification. Food Hydrocolloids 39, 301–318 (2014)
Ordonéz, J.A.: Food Technology, vol. I. Artmed, Porto Alegre (2005)
Park, K.J., Yado, M.K.M., Brod, F.P.R.: Drying study of sliced Bartlett pear (Pyrus sp.). Food Sci.
Technol. 21(3), 288–292 (2001)
Park, S.K., Shanbhag, S.R., Dubin, A.E., De Bruyne, M., Wang, Q., Yu, P., Shimoni, N., D’Mello, S.,
Carlson, J.R., Harris, G.L., Steinbrecht, R.A., Pikielny, C.W.: Inactivation of olfactory sensilla
of a single morphological type differentially affects the response of Drosophila to odors. J.
Neurobiology. 51(3), 248–260 (2002)
Park, K.J., Antonio, G.C., Oliveira, R.A., Park, K.J.B.: Process concepts and drying equip-
ment. Campinas, 121 p. (2007). http://www.feagri.unicamp.br/ctea/manuais/concproceqsec_07.
pdf. Accessed October (2007). (In Portuguese)
Pereira, T.S.: Foam-mat drying study of white egg. Master´s dissertation in Agri-industrials Systems,
Federal University of Campina Grande, Pombal, Brazil (2015). (In Portuguese)
Prins, A.: Principles of foam stability. In: Dickinson, E., Stainsby, G. (eds.) Advances in Food
Emulsions and Foams, pp. 91–122. Elsevier, London (1988)
Rajkumar, P., Kailappan, R., Viswanathan, R., Raghavan, G.S.V., Ratti, C.: Foam mat drying of
alphonso mango pulp. Dry. Technol. 25(2), 357–365 (2007a)
Rajkumar, P., Kailappan, R., Viswanathan, R., Raghavan, G.S.V.: Drying characteristics of foamed
alphonso mango pulp in a continuous type foam mat dryer. J. Food Eng. 79, 1452–1459 (2007b)
Sagar, V.R., Kumar, S.P.: Recent advances in drying and dehydration of fruits and vegetables: a
review. J. Food Sci. Technol. 47(1), 15–26 (2010)
Sangamithra, A., Venkatachalam, S., John, S.G., Kuppuswamy, K.: Foam mat drying of food mate-
rials: a review. J. Food Process. Preserv. 39(6), 3165–3174 (2015).https://doi.org/10.1111/jfpp.
12421
Sousa, C.C.: Definition of parameters for foam-mat drying of anas platyrhynchos domesticus egg
white and yolk. João Pessoa, 54 p. Final course report (Undergraduate in Chemical Engineering),
Federal University of Paraíba, João Pessoa, Brazil (2017). (In Portuguese)
Strumillo, C., Kudra, T.: Drying: Principles. Applications and Design. Gordon and Breach Science
Tariq, M.R., Sameen, A., Khan, M.I., Huma, N., Yasmin, A.: Nutritional and therapeutic properties
of whey. Ann. Food Sci. Technol. 14(1), 19–26 (2003)
Townsend, A.A., Nakai, S.: Relationships between hydrophobicity and foaming characteristics of
food proteins. J. Food Sci. 48(2), 588–594 (1983)
Vega-Mercado, H., Gongora-Nieto, M.M., Barbosa-Canovas, G.V.: Advances in dehydration of
foods. J. Food Eng. 49(4), 271–289 (2001)
Vernon-Carter, E.J., Espinosa-Paredes, G., Beristain, C.I., Romero-Tehuitzil, H.: Effect of foaming
agents on the stability, rheological properties, drying kinetics and flavour retention of tamarind
foam-mats. Food Res. Int. 34(4), 587–598 (2001)
Zayas, J.F.: Functionality of Proteins in Food. Chapter 5: Foaming Properties of Proteins, pp. 122–
134. Springer, Heidelberg (1997)
Zhang, Q., Litchfield, J.B.: An optimization of intermittent corn drying in a laboratory scale thin
layer dryer. Dry. Technol. 9, 383–395 (1991)
Zhang, M., Bhandari, B., Fang, Z.: Handbook of Drying of Vegetables and Vegetable Products.
CRC Press, Boca Raton (2017)
Chapter 4
Drying Process of Jackfruit Seeds
T. M. Q. de Oliveira, R. A. de Medeiros, V. S. O. Farias, W. P. da Silva,

C. M. R. Franco, and A. F. da Silva Júnior
Abstract This chapter presents the application of an analytical solution for the
diffusion equation in cylindrical coordinates, considering a boundary condition of
the third kind. This diffusive model was used to verify the influence of the presence
of the seed coat in jackfruit seeds on the mass transfer at the product surface and on
the drying time. For this, jackfruit seeds were dried with and without the seed coat at
60 and 70 °C. In order to obtain the optimal values of effective mass diffusivity and
Biot number, the analytical solution was coupled to an optimizer developed from
an inverse method. A program was developed in Fortran language to execute the
optimizer coupled to the analytical solution. The results showed that the seed coat
had a strong influence on the drying time and on the Biot number, indicating that the
boundary condition of the third kind is the most suitable for the drying simulation
of this type of product.
T. M. Q. de Oliveira · R. A. de Medeiros
Postgraduate Program in Natural Sciences and Biotechnology, Federal University of Campina
Grande, Olho D’Água da Bica, S/N, Cuité, PB 58175-000, Brazil
e-mail: tham.iresmabel@hotmail.com
R. A. de Medeiros
e-mail: raquel.medeiros113@gmail.com
V. S. O. Farias · C. M. R. Franco · A. F. da Silva Júnior (B)
Physics and Mathematics Department, Federal University of Campina Grande, Olho D’Água da
Bica S/N, Cuité, PB 58175-000, Brazil
e-mail: aluiziofsj.ces@gmail.com
V. S. O. Farias
e-mail: vera.solange6@gmail.com
C. M. R. Franco
e-mail: celiafranco_m@hotmail.com
W. P. da Silva
Physics Department, Federal University of Campina Grande, Av. Aprígio Veloso 882 Bodocongó,
Campina Grande, PB 58429-900, Brazil
e-mail: wiltonps@uol.com.br; cleidedps@gmail.com
https://doi.org/10.1007/978-3-030-47856-8_4
90 T. M. Q. de Oliveira et al.
Keywords Diffusion equation · Analytical solution · Mass transfer · Seed coat ·

Optimization
4.1 Introduction
Jackfruit (Artocarpus heterophyllus Lam.) is a species widely cultivated in the Asian

continent and in tropical climate areas, including Brazil. Its fruits reach an average
of 3.5 kg to a maximum of 25 kg and are composed of arils with yellowish and sweet
pulp and brown seeds wrapped in a hard shell (Swami et al. 2012).
Jackfruit pulp has high nutritional value and is rich in sugars, mainly sucrose,
fructose, and glucose, as well as minerals, dietary fiber, carboxylic acids, and
vitamins. Due to the great versatility of its use as food, it can be eaten fresh or
processed by adding sugar or another component into products such as jams and
cakes (Anaya-Esparza et al. 2018).
Another very important component is the seeds, which represent about 10–15%
of the total weight of the fruit and stand out for having high amounts of protein,
fiber, minerals, and fatty acids (Pacheco et al. 2015; Tulyathan et al. 2002). Its great
technological value directly influences its economic potential, which is linked to
the wide possibility of use in biotechnology, especially as a food source. It can be
eaten cooked, candied, in flour form, and used as preparation and/or meal enrichment
ingredients or as a substitute for people with dietary restrictions (Anaya-Esparza et al.
2018).
The seed when kept fresh has favorable conditions for rapid deterioration, causing
loss and damage. Therefore, the drying of these seeds to obtain the flour has been
widely used as an alternative to increase the useful life and expansion of technological
applications, especially in the food industry. Due to its nutritional content consisting
of 78% carbohydrates, 11.2% protein, and 0.99% lipids, it is being implemented as
an enrichment strategy in the development of cappuccinos, breads, and meatballs
(Tulyathan et al. 2002; Landim et al. 2015; Santos 2012; Spada et al. 2018).
Although drying is one of the most commonly used preservation techniques, it is
known that its use requires a large expenditure of energy, in addition to modifying
the nutritional and sensory properties of the product, resulting in financial losses for
industries. With a view to reducing costs and obtaining a good quality product, the
description of drying kinetics through mathematical simulation is a strategy that can
be used to predict variables such as time, temperature, and dryer types best suited
for use in the processing of the studied product (Gan and Poh 2014).
In addition to the variables often studied in the drying process such as temperature,
pressure, and air velocity, product constituents such as shells can influence important
process parameters. However, most studies available in the literature do not analyze
the influence of such elements on the thermo-physical parameters of drying.
Doymaz and Pala (Doymaz and Pala 2003) performed the drying of corn grains
with and without ethyl oleate pretreatment at 55, 65, and 75 °C. One of the models
used to predict drying kinetics and to determine effective water diffusivity was a
4 Drying Process of Jackfruit Seeds 91
simplification of the solution of the diffusion equation in spherical coordinates (only

the first term was considered). In addition, a boundary condition of the first kind
was imposed. Although these simplified models fit the experimental data well, the
influence of product constituents (such as the seed coat) on the surface resistance
to mass transfer should be evaluated. However, this is only possible by assuming a
boundary condition of the third kind.
A similar study was performed by Leite et al. (Leite et al. 2019) with germinated
seeds of jackfruit. In this research, germinated seeds of jackfruit were dried at 55,
65, and 75 °C with air velocities of 1.0 and 1.3 m s−1 . For the description of drying
kinetics, 12 empirical models were tested. To determine the effective diffusivity of
water, the same simplification of the diffusive model used by Doymaz and Pala
(Doymaz and Pala 2003) was adopted. Since the boundary condition was again of
the first kind, it was not possible to evaluate the influence of the seed coat on mass
transfer at the product surface.
In order to analyze the effect of seed coat presence on the drying process param-
eters, four treatments were carried out (drying at 60 and 70 °C of seeds with and
without seed coat). An analytical solution for the diffusion equation in cylindrical
coordinates for the two-dimensional case, assuming a boundary condition of the third
kind, was considered to describe the processes.
4.2 Methodology
4.2.1 Experiments
The study was carried out using “soft” and “hard” jackfruit varieties obtained at
the local market of the city of Cuité, Paraiba, Brazil, pre-selected according to
physiological integrity and absence of mechanical damage to the fruit.
The technological processes of the experiment were carried out at the Food Tech-
nology Laboratory of the Federal University of Campina Grande—UFCG, Campus
of Cuité, Brazil. The seeds used in the drying process were obtained through fruit
disinfection, pulping, characterized by pulp and seed separation, and washing of the
seed in drinking water. In addition, to remove the shell (seed coat), the jackfruit seeds
were immersed in boiling water for about 1 min to facilitate the process. Then these
seeds were placed on a stainless steel sieve to remove surface water, and the shells
were removed with the help of a knife, as shown in Fig. 4.1. Immediately after, the
seeds with and without seed coat were placed separately in a sealed plastic container
and subjected to the drying process.
An oven previously stabilized at 60 and 70 °C was used for drying. The samples
were divided into four treatments reproduced in triplicate: T1—Jackfruit seeds with
seed coat submitted to 60 °C, T2—Jackfruit seeds without seed coat submitted to
60 °C, T3—Jackfruit seeds with seed coat submitted to 70 °C, and T4—Jackfruit
seeds without seed coat submitted to 70 °C. In each treatment, the samples were
Fig. 4.1 Seed shell removal

with a stainless steel knife
Fig. 4.2 Jackfruit seeds

without the seed coat
arranged in baskets for the
drying process
placed in baskets with mass previously measured on a semi-analytical scale, as shown

in Fig. 4.2. The masses of the samples were measured before drying began (time t
= 0), and then at intervals of 2, 5, 10, 20, and 30 min and 1 hour (h), 2 h, and 3 h
until they reached equilibrium. Then, the samples were dried in an oven previously
stabilized at 105 °C for 24 h to obtain the dry mass. The moisture content of the
samples ranged from 1.069 to 1.321 (dry basis, d.b.) for the seeds with seed coat and
from 0.977 to 1.35 (d.b.) for the seeds without seed coat.
4.2.2 Mathematical Modeling
In the present study, the liquid diffusion model for water migration in a product with
finite cylinder geometry was considered adequate to describe thin-layer drying of
jackfruit seed. This is a widely accepted model in the literature (Pacheco-Aguirre
et al. 2014; Silva Júnior et al. 2018; Arunsandeep and Chandramohan 2018; Chayjan
and Kaveh 2014). In addition, as the objective of this study was to analyze the
influence of the presence of the seed coat on the mass transfer at the product surface,
a boundary condition of the third kind was assumed.
4.2.2.1 The Model
The analytical solution of the diffusion equation will be presented for the finite
cylinder, where the diffusive process is subject to the following hypotheses: (1)
the cylinder must be considered homogeneous and isotropic; (2) the distribution
of moisture content within the cylinder must have radial symmetry and must be
initially uniform; (3) the conditions of the drying medium remain the same throughout
the process; (4) the only water transport mechanism inside the cylinder is liquid
diffusion; (5) dimensions of the cylinder do not vary during diffusion; (6) the effective
diffusivity does not vary during the process; and (7) the boundary condition is of the
third kind.
For the previously established hypotheses, the diffusion equation has analytical
solution for several simple geometries, among which is the finite cylinder geometry.
It is noteworthy that a finite cylinder can be obtained by intersecting two even simpler
solids: the infinite cylinder and the infinite wall, as shown in Fig. 4.3a.
In order to present the analytical solution of the diffusion equation for the geometry
of a finite cylinder of radius R and length L, such geometry is outlined as shown in
Fig. 4.3b.
The three-dimensional diffusion equation in cylindrical coordinates (r, y, ) is given
by:

∂X 1 ∂ ∂X 1 ∂ ∂X ∂ ∂X
= rD + 2 D + D (4.1a)
∂t r ∂r ∂r r ∂θ ∂θ ∂y ∂y
For a symmetrical diffusion with respect to the r- and y-axes, only the radial
and axial flows were considered and, therefore, the flow in the angular direction was
neglected. Thus, for the cylindrical geometry shown in Fig. 4.3b, the two-dimensional
diffusion equation can be written as follows:
(a) (b)
Fig. 4.3 a Intersection of an infinite cylinder and an infinite wall; b Finite cylinder of radius R and
length L

∂X 1 ∂ ∂X ∂ ∂X
= rD + D (4.1b)
∂t r ∂r ∂r ∂y ∂y
In Eq. (4.1b), r is defined relative to the central axis of the cylinder and, together
with the y-coordinate, defines the position of a point (r, y) within the solid to be
studied. Also, in this equation, D is the effective mass diffusivity, X is the moisture
content on dry basis, and t is the time.
The boundary condition is of the third kind, which is expressed by imposing
equality between the internal (diffusive) flow on the surface of the finite cylinder and
the external (convective) flow in the vicinity of this surface:
∂ X (r, y, t)
−D = h X (r, y, t)r =R − X eq (4.2)
∂r r =R
and
∂ X (r, y, t)
−D = h X (r, y, t) y=±L/2 − X eq (4.3)
∂y y=±L/2
4.2.2.2 Exact Solution
For a homogeneous and isotropic cylinder of radius R and length L with uniformly
distributed initial moisture content X i and equilibrium moisture content X eq , the
solution X(r, y, t) of Eq. (4.1b) for the boundary conditions defined by Eqs. (4.2) and
(4.3) can be obtained by separating the variables (Luikov 1968; Crank 1975) and
results in:

r
∞
∞
y
X (r, y, t) = X eq + (X i − X eq ) An,1 Am,2 J0 μn,1 cos μm,2
n=1 m=1
R L/2

μ2n,1 μ2m,2
× exp − + Dt (4.4)
R2 (L/2)2
As mentioned earlier, this solution considers the idea that a finite cylinder can be
obtained by intersecting two even simpler solids: an infinite cylinder of radius R and
an infinite wall of thickness L.
Returning to Eq. (4.4), it should be noted that X(r, y, t) is the moisture content on
dry basis at a cylinder position (r, y) at time t, and D is the effective mass diffusivity.
Also, with respect to Eq. (4.4), the coefficients An,1 and Am,2 are defined as follows:
2Bi1
An,1 = (4.5)
J0 (μn,1 )(Bi21 + μ2n,1 )
and
2Bi2 (Bi22 + μ2m,2 )1/2

Am,2 = (−1)m+1 (4.6)
μm,2 (Bi22 + Bi2 + μ2m,2 )
In Eqs. (4.5) and (4.6), variables referring to the terms of the second member will
be defined later. On the other hand, the expression for the average moisture content
at time t is given as follows:

1
X (t) = X (r, y, t)d V (4.7)
V
The solution of the diffusion equation for the mean value in a finite cylinder at
time t is obtained by substituting Eq. (4.4) in Eq. (4.7), which results in:
∞
∞

μ2n,1 μ2m,2
X (t) = X eq + (X i − X eq ) Bn,1 Bm,2 exp − + Dt (4.8)
n=1 m=1
R2 (L/2)2
where X̄ (t) is the average moisture content on dry basis at time t.

The coefficient Bn,1 is defined as follows:
4Bi21
Bn,1 = (4.9)
μ2n,1 (Bi21 + μ2n,1 )
where Bi1 is the Biot number for the infinite cylinder and is given by
hR
Bi1 = (4.10)
D
The coefficient Bm,2 is defined as follows:
2Bi22
Bm,2 = (4.11)
μ2m,2 (Bi22 + Bi2 + μ2m,2 )
and in this expression Bi2 is the Biot number referring to the infinite wall, given by
the expression
h(L/2)
Bi2 = (4.12)
D
In Eqs. (4.2), (4.3), (4.10), and (4.12), h is the convective mass transfer coefficient,
and, in the presented solution, the same value of h was imposed to all external surfaces
of the cylinder.
In Eqs. (4.5), (4.8), and (4.9), μn,1 are the roots of the characteristic equation for
the infinite cylinder and are calculated by the following transcendental equation:
J0 (μn,1 ) μn,1
= (4.13)
J1 (μn,1 ) Bi 1
where J 0 and J 1 are Bessel functions of the first-order type 0 and 1, respectively.
In Eqs. (4.6), (4.8), and (4.11), μm,2 are the roots of the characteristic equation
for the infinite wall and are calculated by the following transcendental equation:
μm,2
cot μm,2 = (4.14)
Bi 2
From the foregoing, Eqs. (4.4) and (4.8) can be used to determine X(r, y, t) and
X̄ (t) for any Biot numbers of interest. In the present study, aiming at the compu-
tational implementation of Eq. (4.8), the first 20 roots of Eqs. (4.13) and (4.14)
were calculated. The choice of this number of roots is based on the study by Silva
et al. (2012), which points out the relationship between the number of terms in the
series (Eq. 4.8) and the Biot number. Note that for each term in this series, a root
for transcendental Eqs. (4.13) and (4.14) is required. A detailed description of the
obtaining of these roots will be presented in the section related to computational code
development.
It is worth noting that the Biot number is a widely used parameter in the literature
to determine if the internal resistance to mass flow is relevant (Incropera et al. 2012).
Such resistance may be considered negligible if Bi < 0.1. In this case, the moisture
distribution inside the product becomes uniform during the process.
Equation (4.8) can be rearranged to express the moisture ratio, which is defined
as follows:
∗ X (t) − X eq
X = (4.15)
X i − X eq
In this study, the experimental data obtained for drying kinetics were used in the
dimensionless form using Eq. (4.15).
4.2.2.3 Optimization Procedure
A program in the Fortran language was developed on the Windows platform. Equa-
tion (4.8), which presents the average moisture content for any time instant, was
implemented in this program. However, to obtain the average moisture content
through Eq. (4.8), it is necessary to find the roots of the transcendental equations,
which in turn depend on Bessel functions and Biot numbers.
The input data of the computational code are the experimental data, initial moisture
content, equilibrium moisture content, and the length and radius of the cylinder. Once
input data are provided, the developed optimizer begins the process of determining the
Biot numbers Bi1 and Bi2 for the infinite cylinder and the infinite wall, respectively,
and the effective water diffusivity.
For each value of the Biot numbers supplied by the optimizer, it is necessary to
calculate the roots μn,1 and μm,2 . For the calculation of μn,1 , the code proceeds as
follows: the Bessel functions of order 0 and 1 are calculated for each n, considering
80 terms of the factorial in the expression. Then their values are replaced in the
transcendental equation and, after that, the Secant method with an accuracy of 10−12
is used to calculate these roots. Thus, the value of μn,1 is obtained and, consequently,
by Eq. (4.13), the value of Bi1 is obtained for each n.
For the calculation of μm,2 , the Newton Method with an accuracy of 10−16 is
applied to Eq. (4.14). Thus, for each m, the respective value of μm,2 is obtained.
The optimizer used in the present work was developed in order to obtain the
optimal values of parameters D, Bi1 , and Bi2 . This optimizer was developed through
an inverse method, which initially requires the user to provide initial values for the
three parameters. These values are then corrected to minimize an objective function,
which in this case is chi-square, defined as:

Np
exp 2 1
χ =
2
Xi − X̄ isim (D, Bi1 , Bi2 ) , (4.16)
i=1
σi2
exp
where X i is the i-th experimental point; X̄ isim (D, Bi1 , Bi2 ) is the average value of
exp
X obtained by the analytical solution at the same time as X i ; σi is the standard
deviation of the experimental average moisture content at point i; D is the effective
mass diffusivity; and Np is the number of experimental points. In the present work,
all σi were considered equal to 1.
Once all the necessary elements for the determination of the value of χ 2 are
obtained, the next step is to adjust the initial values of the parameters Bi1 , Bi2 , and
D, by minimizing the chi-square. For this, the optimizer follows the following steps:
First, with the initial user-supplied parameter data, the optimizer calculates the
first value for chi-square.
Second, the optimizer starts looking for ranges where the optimal values for the
parameters Bi1 , Bi2 , and D are found. Initially, with the Bi2 and D parameter values
fixed, the algorithm corrects the initial Bi1 parameter value by adding 0.1% to the
current value (if the optimal value is higher) or subtracting 0.1% from the current
value (if the optimal value is lower). At each correction of parameter Bi1 , a new value
for χ 2 is calculated and compared with the previous one. This process is repeated
until the χ 2 value is higher than the previous
one. Finally,
it is considered that the
optimal value of Bi1 is within the interval Bik−11 , Bi k
1 , where the indices k and k −
1 represent the iterations where the chi-square increases and the previous iteration,
respectively.
Third, once the range containing the optimal value for the parameter is found, the
midpoint is calculated, which will divide the range into two new ranges. Then, the
chi-square at the midpoints of the two new intervals obtained is calculated, and the
choice of the best midpoint is made by decreasing the chi-square. This process is
repeated until the chi-square can no longer be minimized.
In each iteration, the second and third steps should be applied to each parameter.
At the end of each iteration, the optimizer checks the relative error of each parameter.
The optimization process is terminated when the relative error of each parameter is
less than 10−16 . This error is calculated by the following formula:

Pcurrent − Pprevious
E rel = , (4.17)
Pprevious
where E rel denotes the relative error, Pcurrent is the parameter value in the current
iteration, and Pprevious is the parameter value in the previous iteration.
In the optimizations performed, no significant differences were observed between
Bi1 and Bi2 . Thus, the values of these parameters were considered equal to a single
value Bi.
4.3 Results Analysis
The physical parameter optimization processes were performed using the analyt-
ical solution presented in Sect. 4.2. The results of these processes are presented in
Table 4.1.
It is possible to notice the influence of the presence of the seed coat also on the
drying time by observing the graphs shown in Fig. 4.4. From the observed drying
times, it can be concluded that the drying of the samples with the presence of seed
coat at temperatures of 60 and 70 °C lasted about 66% longer than the drying of the
samples without seed coat. Thus, the energetic cost for seed processing with seed
coat is high, being justified only if these seeds have relevant nutritional indicators.
Figure 4.5 shows the drying kinetics for the four treatments performed.
By analyzing the kinetics for seed with seed coat, one can observe the influence
of temperature. On the other hand, this influence is not observed on the kinetics for
seeds without seed coat. However, further studies are necessary considering other
Table 4.1 Values obtained for the parameters of the drying process of jackfruit seeds with and
without the presence of the seed coat
Temperature/Presence of Dw (m2 m−1 ) h (m m−1 ) Bi R2 χ2
seed coat
60 °C/present 6.46 × 10−7 6.21 × 10−6 8.84 × 10−2 0.991 3.64 × 10−2
60 °C/absent 6.21 × 10−8 1.32 × 10−4 19.01 0.998 4.15 × 10−3
70 °C/present 7.99 × 10−7 7.99 × 10−6 9.19 × 10−2 0.998 6.92 × 10−3
70 °C/absent 6.43 × 10−8 1.28 × 10−4 18.85 0.999 2.04 × 10−3
(a) (b)
(c) (d)
Fig. 4.4 Fits obtained for samples with seed coat at temperatures of a 60 °C and b 70 °C and for
samples without seed coat at temperatures of c 60 °C and d 70 °C
Fig. 4.5 Simulation of

drying kinetics for the four
treatments
temperatures in order to analyze whether this influence is dominated by the presence

of the seed coat.
Figure 4.6 presents simulations of the moisture distribution inside the seeds for
the four treatments.
As can be seen, the simulations presented in Fig. 4.6 correspond to the half of the
cylinder that represents the seeds. It is also possible to notice a very small moisture
gradient. This phenomenon may be related to the high resistance observed through
(a) (b) (c)
Fig. 4.6 Simulation of moisture distribution for treatment at 60 °C with seed coat at times: a t =
30.72 min, b t = 120 min, and c 330.20 min
the Biot number presented in Table 4.1. This resistance causes a kind of “brake” to
the water flow, resulting in the uniformity of moisture inside the product.
By comparing Figs. 4.6 and 4.7, it can be observed that the seed coat is what
determines the existence of moisture gradients inside the product, since the gradients
(which were small in Fig. 4.6) increase in Fig. 4.7. This phenomenon can also be
observed when comparing the simulations for 70 °C, presented in Figs. 4.8 and 4.9.
By comparing the simulations of 60 and 70 °C, one can note an influence of
temperature on the distribution of moisture inside the product. Moreover, in simu-
lations for the time near 120 min, gradient is observed only in the drying at 60 °C.
In the simulation for drying at 70 °C, a uniform distribution of moisture inside the
product is noted.
The influence of the seed coat on the moisture distribution inside the product
observed in the simulations for drying at 60 °C is also seen in Figs. 4.8 and 4.9.
Moreover, when comparing the simulations for drying at 60 and 70 °C of the samples
(a) (b) (c)
Fig. 4.7 Simulation of moisture distribution for treatment at 60 °C without seed coat at times: a t =
30.36 min, b t = 120.1 min, and c 330 min
(a) (b) (c)
Fig. 4.8 Simulation of moisture distribution for treatment at 70 °C with seed coat at times: a t =
30.40 min, b t = 120.70 min, and c 330.60 min
(a) (b) (c)
Fig. 4.9 Simulation of moisture distribution for treatment at 70 °C without seed coat at times: a t =
30.24 min, b t = 120.20 min, and c 330.50 min
without seed coat, there are slight differences between the moisture distributions. This
can also be observed through the kinetics presented in Fig. 4.5.
In this chapter, the effect of the presence of the seed coat in jackfruit seeds on the
process parameters was studied. It was concluded that the presence of this element
contributed to the increase in drying time and influenced the resistance of the product
surface to mass transfer. The proposed model adequately described the drying kinetics
of seeds with and without seed coat. Moreover, from the values obtained for the Biot
number, the most appropriate boundary condition for describing the drying of this
type of seed is that of the third kind. Finally, the methodology used in this chapter
can be applied to describe the drying of other seeds in order to verify the influence
of their seed coat on the process parameters.
Acknowledgments Prof. Wilton would like to thank CNPq (Conselho Nacional de Desen-
volvimento Científico e Tecnológico) for his research grant (Process Number 301708/2019-3;
PQ-1A).
References
Anaya-Esparza, L.M., González-Aguilar, G.A., Domínguez-Ávila, J.A., Olmos-Cornejo, J.E.,

Pérez-Larios, A., Montalvo-González, E.: Effects of minimal processing technologies on jackfruit
(Artocarpus heterophyllus Lam.) Qual. Paramet. Food Biopro. Technol. 11, 1761–1774 (2018)
Arunsandeep, G., Chandramohan, V.P.: Numerical solution for determining the temperature and
moisture distributions of rectangular, cylindrical, and spherical objects during drying. J. Eng.
Phys. Thermophys. 91(4), 895–906 (2018)
Chayjan, R.A., Kaveh, M.: Physical parameters and kinetic modeling of fix and fluid bed drying of
terebinth seeds. J. Food Process. Preserv. 38, 1307–1320 (2014)
Crank, J.: The Mathematics of Diffusion, 414 p. Clarendon Press, Oxford, UK (1975)
Doymaz, I., Pala, M.: The thin-layer drying characteristics of corn. J. Food Eng. 60, 125–130 (2003)
Gan, P.L., Poh, P.E.: Investigation on the effect of shapes on the drying kinetics and sensory
evaluation study of dried jackfruit. Int. J. Sci. Eng. 7, 193–198 (2014)
Incropera, F.P., De Witt, D.P., Bergman, T.L., Lavine, A.S.: Fundamentals of Heat and Mass Transfer.
LTC, Rio de Janeiro (2012). (In Portuguese)
Landim, L.B., Bonomo, R.C.F., Reis, R.C., Silva, N.M.C., Veloso, C.M., Fontan, R.C.I.: Kibbeh
formulation with jackfruit flour. J. Health Sci. 14, 87–93 (2015). (In Portuguese)
Leite, D.D.F., Queiroz, A.J.M., Figueirêdo, R.M.F., Lima, L.S.L.: Mathematical drying kinetics
modeling of jackfruit seeds (Artocarpus heterophyllus Lam.), vol. 50, pp. 361–369. Agronomic
Science Magazine (2019). In Portuguese
Luikov, A.V.: Analytical Heat Diffusion Theory, 685 p. Academic Press, Inc. Ltd, London (1968)
Pacheco, C.S.V., Ferreira, A.N., Rocha, T.J.O., Tavares, I.M.C., Franco, M.: Use of the jackfruit
seed for obtaining endoglucanase from aspergillus niger by solid state fermentation. J. Health
Sci. 14, 25–29 (2015). (In Portuguese)
Pacheco-Aguirre, F.M., Ladrón-González, A., Ruiz-Espinosa, H., García-Alvarado, M.A., Ruiz-
López, I.I.: A method to estimate anisotropic diffusion coefficients for cylindrical solids:
application to the drying of carrot. J. Food Eng. 125, 24–33 (2014)
Santos, D. B. French bread development with the addition of jackfruit flour (Artocarpos integrifólia
L.). Biosph. Encycl. 8, 597–602 (2012). (In Portuguese)
Silva Júnior, A.F., Silva, W.P., Farias, V.S.O., Silva, C.M.D.P.S., Lima, A.G.B.: Description of
osmotic dehydration of banana slices dipped in solution of water and sucrose followed by
complementary drying using hot air. In: Transport Phenomena in Multiphase Systems: Advanced
Structured Materials, 1 edn, pp. 273–304. Springer International Publishing (2018)
Silva, W.P., Farias, V.S.O., Neves, G.A., Lima, A.G.B.: Modeling of water transport in roof tiles by
removal of moisture at isothermal conditions. Heat Mass Transf. 48, 809–821 (2012)
Spada, F.P., Silva, P.P.M., Mandro, G.F., Margiotta, G.B., Spoto, M.H.F., Canniatti-Brazaca,
S.G.: Physicochemical characteristics and high sensory acceptability in cappuccinos made with
jackfruit seeds replacing cocoa powder. PLoS One 13, 1–12 (2018)
Swami, S.B., Thakor, N.J., Haldankar, P.M., Kalse, S.B.: Jackfruit and its many functional compo-
nents as related to human health: a review. Compr. Rev. Food Sci. Food Saf. 11, 565–576
(2012)
Tulyathan, V., Tananuwong, K., Songjinda, P., Jaiboon, N.: Some physicochemical properties of
jackfruit (Artocarpus heterophyllus Lam) seed flour and starch. Sci. Asia 28, 37–41 (2002)
Chapter 5
Spouted Bed Drying of Fruit Pulps:
A Case Study on Drying of Graviola
(Annona muricata) Pulp
F. G. M. de Medeiros, I. P. Machado, T. N. P. Dantas, S. C. M. Dantas,

O. L. S. de Alsina, and M. F. D. de Medeiros
Abstract The spouted bed dryer with inert particles has been researched as an alter-
native for the drying fruit pulps in order to obtain powdered products. Depending on
the composition and physical properties of the pulps, the dryer is subject to agglom-
eration and accumulation problems that can be minimized by the addition of drying
adjuvants, especially carbohydrates, such as maltodextrin; sources of proteins, such
as whey protein and milk itself. In this work, the advantages of the spouted bed dryer,
regarding its mixing capacity, temperature uniformity, high heat and mass transfer
rates, and reduced processing time are emphasized. A review of the fundamentals of
the spouted bed is presented in this chapter, as well as the relevant and recent works
related to drying fruit pulps in the spouted bed, addressing the use of adjuvants and the
impact of the process on phytochemicals present in fruits and other vegetables. The
chapter is concluded with the presentation of a case study on the drying of graviola
fruit pulp with the addition of milk in the spouted bed dryer, where the results related
F. G. M. de Medeiros (B) · I. P. Machado · S. C. M. Dantas · M. F. D. de Medeiros (B)

Department of Chemical Engineering, Federal University of Rio Grande do Norte, Av. Senador
Salgado Filho, 3000, Natal, RN 59078-970, Brazil
e-mail: fabio.medeiros@USherbrooke.ca
M. F. D. de Medeiros
e-mail: mariadefatima@eq.ufrn.br; mfatimadmedeiros@gmail.com
I. P. Machado
e-mail: machadoizap@gmail.com
S. C. M. Dantas
e-mail: suzianidantas@gmail.com
T. N. P. Dantas
Federal Institute of Education, Science and Technology of Rio Grande do Norte, Campus Currais
Novos, R. Manoel Lopes Filho, 773, Currais Novos, RN 59380-000, Brazil
e-mail: thaysenpires@gmail.com
O. L. S. de Alsina
Department of Chemical Engineering (retired), Federal University of Campina Grande, R.
Aprigio Veloso, 743, Campina Grande, PB 58429-140, Brazil
e-mail: odelsia@uol.com.br
https://doi.org/10.1007/978-3-030-47856-8_5
106 F. G. M. de Medeiros et al.
to production, thermal efficiency, product characteristics, and process modeling are

presented with intermittent pulp feeding.
Keywords Spouted bed dryer · Graviola pulp · Phytochemicals · Process modeling
5.1 Introduction
Brazil is the third-largest fruit producer in the world and ranks among the leading
exporters of several tropical such as pineapple, papaya, mango, oranges, melons,
and others (Altendorf 2017). However, due to the perishable condition of fruits, the
development of efficient post-harvest processing strategies is a major concern of the
food industry, in order to avoid food waste. According to FAO (FAO 2019), 20–30%
of world’s fruits and vegetables’ production goes to waste between the post-harvest
and retail levels.
For many years, drying has been regarded as an efficient conservation method and
a versatile post-harvest processing alternative for fruits and other highly perishable
materials (Zhang et al. 2020; Souza da Silva et al. 2019). The lowering of mois-
ture content on dried fruit is a key parameter for extending products’ shelf life and
maintaining a stable fruit products’ supply chain, since low water activity on dried
products is related to reduced microorganism growth and delayed enzymatic process,
which leads to higher storage stability (Rocha et al. 2011; Karam et al. 2016).
The growing market demand for natural-based products has been pushing the food
industry toward innovative product-oriented technologies in order to take full advan-
tage of the dietary and phytochemical values of fruits (Belwal et al. 2018; Demirkol
and Tarakci 2018). In this sense, the versatility of dehydration as a processing tech-
nique is highlighted on a new product-development point of view. From ready-to-eat
and ready-to-drink products (Dantas et al. 2019; Cappato et al. 2018) to food ingredi-
ents (Correia et al. 2017; Moraes et al. 2017), dried fruit products have been attracting
attention and space on the food industry.
The choice of drying method is, therefore, of utmost importance, since the impact
of the heat and mass transfers during the dehydration process are directly related
to the final composition and quality aspects of the dried product (Demirkol and
Tarakci 2018). In addition to the industrially popular spray dryer and freeze dryer,
the spouted bed dryer with inert particles is an alternative drying technique that allows
the production of powdered matrices from liquid and paste-like foods (Dantas et al.
2018). Combining operation flexibility with lower costs, when compared to the spray
dryer, several studies have demonstrated the efficiency of the spouted bed drying for
the production of high-quality powdered products (Rocha et al. 2011; Medeiros et al.
2002; Lucas et al. 2018).
5 Spouted Bed Drying of Fruit Pulps … 107
5.2 Fundamentals of Spouted Bed Drying
The spouted bed technique was reported for the first time by Mathur and Gishler
(1955), when the authors investigated the performance of this unconventional tech-
nique for the drying of wheat grains. In that original work, the authors reported that
the vigorous air and particles circulation through the system facilitated the removal
of water from the wheat grains, when compared to traditional fluidized bed dryers.
In the late 1960s, the Leningrad Institute of Technology successfully applied the
spouted bed dryer with inert particles for the drying of solutions. The authors reported
that the spouted bed drying of organic dyes, salt and sugar solutions, and chemical
reagents resulted in quality fine powders (Mathur and Epstein 1974).
Several designs have been proposed for processing suspensions and pastes in a
spouted bed dryer (Costa et al. 2006; Passos et al. 1997; Pallai et al. 2007), but the
conventional dryer is composed of a cylindrical vessel (drying column or drying
chamber) with a conical base with an inlet orifice for air injection (Fig. 5.1). Inert
particles are used as drying support for the feed suspension. A thin layer of material
is accumulated around the particles, covering them, and, after drying, the powders
are separated from the particles due to the friction of the particles’ bed and carried
by the inlet air (Araújo et al. 2015).
The spouted bed drying system is initiated with inlet air injection at the conical
base of the dryer’s chamber. When air flow is sufficient to pneumatically move the
inert particles, an upward movement is noticed and the inert particles are carried to
Fig. 5.1 Schematic representation of a conventional spouted bed dryer. (1) Air blower; (2) Air
valve; (3) Heater; (4) Temperature sensor; (5) High-density polyethylene bed; (6) Control panel;
(7) Cylindrical column; (8) Lapple cyclone; (9) Outlet air temperature and humidity sensors; (10)
Digital thermo-hygrometer and anemometer; (11) Powder collector
levels above the bed, forming a high-porosity spouting region. A low-porosity region
is formed in the annular section of the drying chamber by the downward movement of
the inert particles. The particles then return to the conical base and are carried again
into the spouting region, in a cyclic movement (Delgado and Lima 2014; Nascimento
et al. 2015).
The feed pastes and suspensions may be drip-fed or sprayed through a nozzle onto
the moving and spouting particles bed, which allows for an increased contact surface
area. The inlet feed is usually performed on the top of the drying chamber, since
studies have shown that this leads to higher processing stability and lower material
accumulation inside the system (Costa et al. 2006; Freire et al. Freire et al. 2011).
The study of the fluid dynamic behavior of the spouted bed dryer with inert parti-
cles, taking into account the presence of the feed suspension in the bed is extremely
relevant, although neglected by many authors. The fluid dynamic behavior influences
the process operation conditions, which can be optimized for greater production effi-
ciency, absence of instability, more economical process, and better product quality.
Among the factors that influence the fluid dynamic behavior of inert particles in the
spouted bed, the minimum spouting air velocity, the stable spouting air velocity, and
the maximum pressure drop are worth to highlight (Vieira et al. 2004). In addition
to the parameters of the inlet drying air, the geometric configuration of the dryer, the
physical characteristics and composition of the suspensions, and properties of the
inert material are also responsible for influencing the process stability (Nascimento
et al. 2015; Moreira da Silva et al. 2019).
The heat transfer in the spouted bed is carried out by conduction in the inert
particles and convection of the hot drying air. The heat and mass transfers promote
the drying of the material accumulated in the thin layer around the inert particles
which progressively become fragile and friable. These characteristics of the dried
material allow it to be removed, in the powder form, by the successive collisions to
which the inert particles are subjected. The powder is then carried by the inlet air
and collected in separation cyclone. In a spouted bed drying system, removal rates
should be high enough to avoid agglomeration and mass accumulation inside the
drying chamber (Freire et al. 2011; Sousa et al. 2019).
The inert particles’ collision energy is also affected by a number of variables,
including the solid circulation rates, the ratio between paste/suspension inlet feed
and the inert particles load in the bed and the drying rate. The solids circulation rate
determines the time required for a complete drying cycle: from particle coating to
dried film removal. The increasing drying rate favors increased dried film friability
and positively affects the process. The paste/suspension inlet feed rate should be
carefully controlled to prevent bed collapse caused by fluid dynamic instability,
particle growth, or agglomeration. The material inlet feeding rate must be low or
moderate, resulting in low production of dry products, compared to the spray dryer,
and is therefore an important limitation of this drying technique (Freire et al. 2012;
Santos et al. 2015; Benelli et al. 2013b).
In addition, the high pressure drop through the inert particles bed, the high air
flow necessary for maintaining spouting stability, the difficult process scaling up, the
strong adhesion of the dry powder to the equipment walls and the particle agglom-
eration, which is related to the composition of the paste/suspension feed, are among
the main limitations involved with the spouted bed drying process (Pallai et al. 2007;
Bacelos et al. 2007).
Despite said limitations, the spouted bed drying technique has several advan-
tages, which are responsible for attracting interest from research and development
sectors, such as promoting good mixture between the particles and the fed suspen-
sion, minimal friction, temperature uniformity throughout the bed and elevated heat
and mass transfer coefficients. In addition, the spouted bed drying process presents
high drying rates due to the large surface contact area between the inert particles and
the drying gas, that results in reduced processing times, which is indicated for heat-
sensitive products, such as phytochemicals (Pallai et al. 2007; Pablos et al. 2018;
Niksiar and Nasernejad 2017; Niksiar et al. 2013).
5.3 Spouted Bed Drying of Fruit Pulps
Drying is one of the most commonly used techniques for handling foods with high
moisture content, such as fruits and vegetables (Zhang et al. 2020; Kumar et al.
2014). The drying of fruits and fruit pulps on a spouted bed dryer is a simpler and
cost-reduced alternative technology, when compared to traditional freeze or spray
drying (Rocha et al. 2011; Medeiros et al. 2002).
Over the last three decades, several studies have described the drying of fruit
pieces and fruit pulps using a spouted bed dryer with inert particles. Such studies have
mainly focused on the influence of feed composition (Rocha et al. 2011; Medeiros
et al. 2002; Larrosa et al. 2015; Braga and Rocha 2013), drying parameters (Fujita
et al. 2013; Nascimento et al. 2019; Sales et al. 2019), powder production and quality
parameters (Lucas et al. 2018; Benelli et al. 2013a, b; Braga and Rocha 2013; Braga
and Rocha 2015), and use of drying carriers (Dantas et al. 2019; Fujita et al. 2013;
Butzge et al. 2015, 2016; Rocha et al. 2018).
Medeiros et al. (2002) investigated the influence of the composition of fruit pulps,
using mango pulp as a model formulation, on the fluid dynamics and powder produc-
tion efficiency for spouted bed drying. In this study, the composition of the fruit pulps
was adjusted in relation to the contents of reducing sugars, starch, pectin, lipids, fibers,
water, and total acidity. The authors reported that the fiber content of modified fruit
pulps did not influence the fluid dynamic behavior of the drying system. Other carbo-
hydrates, on the other hand, were related to instabilities on the spouted bed dryer:
reducing sugars promoted instability of the bed, while starch and pectin accounted
for higher spouting stability. In addition, the authors reported that lipids, starch, and
pectin concentrations positively influence the powder production efficiency.
These results were further confirmed by Rocha et al. (2011) have also reported
that while high reducing sugars concentrations were related to spouting stability,
fruit pulps with higher concentrations of starch and lipids promoted a more stable
fluid dynamic regime of the spouting bed. In addition, the authors also verified that,
despite a significant sharp decrease on pressure drop just after the pulp feeding
into the drying chamber, pressure drop increased as the drying process reached a
stable regime. Moreover, authors also highlighted that the powder retention inside
the drying chamber, due to inadequate powder removal rates, may also influence the
fluid dynamics of the spouting bed.
In a recent study, Nascimento et al. (2019) reported the obtention of dried
bacaba fruit powder by spouted bed drying. The authors reported the optimiza-
tion on processing conditions in order to obtain a high yielding and quality dried
product. Authors investigated the influence of temperature, maltodextrin concentra-
tion (as a drying carrier) and drying air velocity on the drying yield, moisture content,
anthocyanins, and phenolic compounds retention.
In this study, the authors reported findings that agree with Costa et al. (2015),
who investigated the spouted bed drying of açaí fruit pulp: increased temperature
is related to lower moisture content on the dried product and maltodextrin concen-
trations around 20% increased process production and phytochemicals retention. In
addition, both studies have suggested that there must be a balance between drying
temperature (>70 °C) and drying air velocity in order to avoid further degradation
on nutritional and bioactive components of fruit pulps.
Braga and Rocha (2015) evaluated the spouted bed drying of pure blackberry
pulp and milk-added blackberry pulp. In addition, they also evaluated the impact of
maltodextrin, casein, and palm oil as composition-modulators on the performance
of the spouted bed drying of blackberry pulp. The authors reported that despite the
modifications on protein and lipid content of the pulp composition, the drying of pure
blackberry pulp was not possible on the spouted bed dryer, since the pulp feeding
was responsible for significant instability that resulted in bed collapse due.
The use of milk as a drying carrier, on the other hand, was reported successful
in this study. The authors described that the addition of 25% (v/v) of whole milk
in the paste formulation yielded a high-quality (around 3% moisture, 77 mg/100 g
anthocyanins, and 19% protein) product and increased fluid dynamic stability.
In a recent study by our research group, Dantas et al. (2019) reported the drying
of acerola pulp (Malpighia emarginata DC) using milk and milk whey protein as
drying carriers. The authors analyzed the influence of these diary adjuvants on both
the fluid dynamics and the final product quality of dried acerola-based powders. It was
reported that the addition of 1% whey protein to the acerola pulp jeopardize spouted
bed drying due to high pressure drop on the spouting bed that led to instability and
collapse.
On the other hand, confirming the results previously reported by Braga and Rocha
(2013, 2015), the use of milk as a drying carrier for fruit pulps was successful. Dantas
et al. (2019) used a model formulation in which the drying carrier corresponded to
50% of the total solids on the final composition, and reported that the addition of milk
powder increased the production yield, prevented spouting instability and allowed
the most efficient processing in terms of the equipment thermal requirements. On
product quality parameters, the authors also reported that the use of milk as a drying
adjuvant increased calcium content on the final product and permitted a high ascorbic
acid retention (around 70%) after thermal processing.
5.4 Phytochemicals on Spouted Bed Dried Fruit Powders
Over the last decade, the growing awareness for the benefits of health-promoting
diets has led the food industry toward research and development strategies in order
to take full advantage of the functional potential of fruits and vegetables (Cappato
et al. 2018; Willett et al. 2019). Studies have shown that fruits play a major role in
the balanced diets due to their vast phytochemical and fiber contents, which have
protective properties against several diseases (Siriamornpun et al. 2012; Habauzit
and Morand 2012).
Phytochemicals are naturally occurring extra-nutritional plant metabolites, such
as vitamins, phenolic acids, flavonoids, that can be related to biological activities in
the human organism (Chang et al. 2016; Fang and Bhandari 2017). In fact, the bioac-
tive performance of several groups of phytochemicals has already been documented.
Anti-inflammatory activity of blueberries (Grace et al. 2019), wound-healing prop-
erties of strawberries and blackberries (Van de Velde et al. 2019), neuroprotective
effects of camu–camu (Myrciaria dubia HBK McVaug) (Azevêdo et al. 2016) and
antioxidant potential of acerola (Malpighia emarginata DC) (Cruz et al. 2019) have
been consistently reported.
Despite the several health benefits related to these bioactive components, the
potential of such phytochemicals is still in the verge of exploitation. In addition to
their occurrence in small quantities in fruits (Kris-Etherton et al. 2002), their avail-
ability for the final consumer is limited due to the seasonal aspect of fruit production,
as well as the low storage stability, which is usually associated with these compounds
(Karam et al. 2016).
Studies have shown that drying of fruits can, in addition to extending products’
shelf life, help stabilizing the phytochemical contents of the dried powders (Correia
et al. 2017; Moraes et al. 2017). Naturally sensitive, these bioactive compounds may
be affected by a number of processing, storage, and delivery conditions, such as pH
variations, temperature, presence of light, and oxygen (Patras et al. 2010), which
may alter their molecular structure and compromise the biological functionality.
In this sense, the use of the spouted bed drier has been regarded as an effective
alternative for dealing heat-sensitive materials (Lucas et al. 2018; Alves et al. 2016),
due to the possibility of milder operation conditions and the use of drying adjuvants
that may act as a protection for the labile components (Dantas et al. 2019; Costa
et al. 2015). Some aspects of the impact of spouted bed drying on the phytochemicals
found on fruit pulps will be discussed as follows, which focus on total phenolics,
anthocyanins, and ascorbic acid.
5.4.1 Impact of Spouted Bed Drying on the Phytochemicals

Content
5.4.1.1 Total Phenolic Compounds
The known potential for promoting health benefits has drawn much attention
for increasing the presence of phenolic compounds on the human diet. Phenolic
compounds are plant secondary metabolites structured around benzene rings with
hydroxyl substituents (Lin et al. 2016). The anti-inflammatory, cardio- and neuro-
protective properties, antioxidant and chemo-preventive activities of phenolic
compounds can be related to several biological mechanisms, some of them still
not fully described on the literature, that involve radical scavenging and inactivation,
metal-ion chelation and single oxygen quenching (Oliveira et al. 2016; Sauceda et al.
2018).
Studies have shown that the biological activities of polyphenols are concentration-
dependent (Heleno et al. 2015), which highlights the drying strategy as an effec-
tive way of producing polyphenol-rich products that increase these phytochemi-
cals’ concentration and stability while maintaining functionality (Correia et al. 2017;
Hoskin et al. 2019). The total phenolic content was evaluated on spouted bed dried
pepper and aromatic extracts (Benelli et al. 2013a, b), camu–camu (Fujita et al. 2013),
bacaba fruit (Nascimento et al. 2019), cubiu fruit (Sales et al. 2019) and vegetable
pastes (Larrosa et al. 2015).
Camu–camu (Myrciaria dubia HBK McVaugh) is a small, round Amazonian fruit
known for its high nutritional and nutraceutical value. It is known for its high contents
of phytochemicals (phenolic compounds, β-carotene, vitamin C) and micronutrients
(potassium, iron, phosphorus, amino acids) (Akter et al. 2011). Fujita et al. (2013,
2015) conducted studies on the impact of spouted bed drying on the physico- and
phytochemical characteristics of camu–camu pulp. In addition, the research group
also evaluated the impact of other drying techniques (spray drying and freeze drying)
on the biological activities of camu–camu phytochemicals.
The drying of camu–camu pulp was carried in a classical conical base spouted
bed dryer, using high-density polyethylene (HDPE) for the inert particles bed. In
this study, different temperatures (60, 80, 95, and 110 °C) were evaluated in order to
assess the final impact on the products’ quality. Freeze drying of camu–camu pulp
was performed for comparison reasons (Fujita et al. 2013). Authors reported a high
concentration of phenolic compounds on the fresh camu–camu pulp (81.6 ± 6.5
milligrams of equivalent gallic acid per gram of dried sample [mg GAE/g DW]) and
the average impact of the drying process on the phenolic content of camu–camu pulp
was around 33–42%, but the increasing temperature did not statistically affect the
phenolic results. In fact, although temperature-sensitive, the increase in temperature
was followed by a reduction in processing time, which may have compensated the
losses (Vega-Gálvez et al. 2012).
In a follow-up study, the authors investigated the biological activities of dried
camu–camu (Fujita et al. 2015). Although the drying technique reported in this
study was spray drying, the authors indicated that the presence of several phenolic
compounds such as gallic acid, syringic acid, ellagic acid, quercetin, and myricetin on
the camu–camu pulp and dried powders were linked to anti-diabetic and antimicrobial
activities, and cellular regeneration properties on planaria models.
Cubiu (Solanum sessiliflorum Dunal) is an Amazonian fruit of the Solanaceae
family, which is known by the indigenous communities in the Amazonia forest for its
health-promoting benefits (Andrade Júnior et al. 2012). The biological activities asso-
ciated with the phytochemicals from the cubiu fruit range from hypoglycemic and
hypocholesterolemic control, anti-genotoxic, and antioxidant activities (Hernandes
et al. 2014). Sales et al. described the drying of the cubiu pulp on a lab-scale spouted
bed dryer in order to evaluate the influence of the drying temperature on the degra-
dation of the phenolic compounds (Sales et al. 2019). The authors investigated the
influence of two drying temperatures (50 and 70 °C) in the total phenolic content
of cubiu pulp dried without the addition of drying carriers. The reduction in the
total phenolic content from the dried cubiu pulp was temperature-dependent. In this
case, the degradation of the phenolic compounds increased from 33.54 to 59.12%
following the increase in temperature.
Studies have shown that the use of drying carriers may help to reduce the degra-
dation of phenolic compounds, as well as other phytochemicals, during spouted bed
drying of fruit pulps. The use of such drying adjuvants will be discussed in the
following section.
5.4.1.2 Anthocyanins
Anthocyanins are water-soluble flavonoid pigments found in tubers, flowers, and

fruits. Chemically, the anthocyanins are known for their particular structure of an
aromatic ring bonded to an oxygen-containing heterocyclic ring and linked to a third
aromatic structure. As pigments, this group of bioactive compounds is responsible
for the red, blue, and purple colors, while as nutraceuticals, the anthocyanins are
linked to several health benefits (Frank et al. 2003).
The low bioavailability of anthocyanins is related to their low stability in food
systems (Khoo et al. 2017). Several factors such as temperature, pH variations,
oxygen, and light exposure, type of solvent and co-pigment, contact with degrading
enzymes, metal ions, and some antioxidant agents are responsible for affecting the
molecular stability of these compounds and jeopardizing their functionality (Laleh
et al. 2006; Castañeda-Ovando et al. 2009). On the other hand, recent studies have
shown that drying is an effective way of increasing anthocyanins stability (Correia
et al. 2017; Moraes et al. 2017; Roopchand et al. 2013).
In addition, the in vivo and in vitro biological activities related to the anthocyanins
content on dried powders have also been documented, and studies report the pres-
ence of hypoglycemic (Roopchand et al. 2012; Grace et al. 2009), anti-inflammatory
(Esposito et al. 2014), cardio-protective (Bell and Gochenaur 2006), and anticar-
cinogenic (Wang et al. 2009) activities, among others. The anthocyanins content was
evaluated on spouted bed dried grapes (Butzge et al. 2015), bacaba fruit (Nascimento
et al. 2019), açai fruit (Lucas et al. 2018; Costa et al. 2015), blueberries (Feng et al.
1999), blackberries (Braga and Rocha 2015) and purple flesh sweet potato (Liu et al.
2015).
Lucas et al. (2018) compared the impact of three drying processes (spouted bed
drying, freeze drying, and spray drying) on the production of açai powder without
the addition of drying adjuvants. On a physicochemical point of view, the authors
reported that the moisture content of spouted bed dried açai powder (4.75 ± 0.21%)
did not differ statistically from the moisture of the spray dried samples (4.75 ±
0.22%). Medeiros et al. (2002) have previously indicated that, with the proper tuning
on operation conditions, the spouted bed obtained products can meet the overall
quality parameters of spray dried powders, with lower production costs.
When it comes to the phytochemical content, the anthocyanins content was consid-
erably affected according to the chosen drying method. The authors reported that the
total anthocyanins content on spouted bed dried açai powders (1.36 ± 0.02 mg/g)
represented a 30% lower degradation of these phytochemicals, when compared to
the powders obtained by spray drying (0.53 ± 0.04 mg/g) (Lucas et al. 2018). While
the constant agitation of the spouted bed may provide a higher contact with oxygen
(Oliveira et al. 2016), the temperature required for the spouted bed process was lower,
when compared to spray drying (90 °C and 210 °C, respectively), which may explain
the higher retention on the spouted bed dried samples (Braga and Rocha 2015).
Regarding the pigments’ color stability, the authors (Lucas et al. 2018) also
reported that the spray dried samples presented the highest total color difference
(E; 16.28 ± 0.30), while the E for the spouted bed dried samples did not differ
from the freeze dried samples (11.79 ± 0.47 and 12.22 ± 0.26, respectively).
5.4.1.3 Ascorbic Acid
Ascorbic acid, or vitamin C, is a water-soluble vitamin found in fruits and vegetables.

Essential micronutrient, the bioactive capacity of vitamin C is well-documented in the
literature, being related to strengthening of the immune system, antioxidant activities,
skin health promotion, scurvy, cancer, and chronical diseases prevention (Manela-
Azulay et al. 2003; Pullar et al. 2017). Vitamin C is a particularly heat-sensitive
compound, and evaluating the impact of the drying processes on the degradation of
this phytochemical is a key parameter for assessing the overall quality and efficiency
of the process (Kamiloglu et al. 2016; Santos and Silva 2008).
Fujita et al. (2013) investigated the impact of the spouted bed drying process on
the vitamin C content on the camu–camu fruit pulp. In that occasion, the authors
determined that the ascorbic acid retention on the dried powders was temperature-
dependent. Despite the lower drying period associated with the higher temperatures,
the sensitivity of the vitamin C to the increasing temperature was more significant
and the retention varied from 55 to 36%, when temperature increased from 60 to
110 °C.
The spouted bed drying of Tommy-variety mango pulp was described by Cunha
et al. (2006) and the authors also evaluated the impact of the drying process on the
ascorbic acid content. The authors described that the degradation of vitamin C was
both temperature- and time-dependent. In the continuous process described in that
study, authors reported that by the increasing of processing time, the accumulated
mass on the spouted bed dryer was submitted to longer periods of exposure to temper-
ature and oxygen, which are degrading factors for the ascorbic acid. However, authors
highlighted that a freeze-drying process was performed for comparison purposes and
the degradation of vitamin C on freeze dried samples were around 50%, while the
degradation after spouted bed reached 65%. In this sense, the hypothesis was that in
addition to temperature, other deleterious factors also contributed to the degradation
of ascorbic acid.
5.4.2 Use of Drying Carriers
Feed composition plays a major role on the efficiency of the spouted bed drying
process. Studies have shown that the chemical composition is directly related to the
glass transition temperature of the inlet feed, which may be responsible for altering
the heat and mass transfer phenomena on the drying process. The presence of high
concentrations of reducing sugars (glucose, fructose, lactose), for example, shows
a negative effect on both powder production and the products’ quality parameters
(Medeiros et al. 2002; Braga and Rocha 2015; Souza et al. 2009).
Drying carriers have been used in the spouted bed drying process in order to
alter the feed composition and improve both the process efficiency and the final
products’ quality (Souza and Oliveira 2012). Maltodextrins, cyclodextrins, protein
sources (whey protein, collagen, plant proteins), modified starch, and milk are some
examples that have been mentioned in the literature as effective drying carriers for
increasing powder production, solubility, and storage stability (Dantas et al. 2019;
Butzge et al. 2016, 2015; Rocha et al. 2018; Costa et al. 2015).
The combination of the adequate drying carriers and drying processing conditions
may result in the encapsulation of the phytochemicals found on the fruit pulps. For
encapsulation, the drying carrier is used in order to build a protective coat around the
targeted compounds, in this case, the phytochemicals, which will be less exposed to
deleterious agents (pH, moisture, temperature, light) and, hence, increasing storage
stability (Correia et al. 2017; Fang and Bhandari 2017; Fang and Bhandari 2010).
Studies have shown that the spouted bed dryer is an alternative for producing encap-
sulated products, which are usually core-shell type large microcapsules formed by
coating mechanisms favored by the fluid dynamics of the spouted bed process (Jono
et al. 2000; Baracat et al. 2008).
Milk has been used as an alternative drying carrier in order to produce ready-to-
consume dried powders. The use of milk powder and reconstituted milk in formu-
lations for spouted bed drying has been reported for acerola fruit (Dantas et al.
2019) and blackberries (Braga and Rocha 2013). In both cases, the use of the drying
carriers helped in increasing the phytochemicals retention on the dried powders by
protecting these compounds from further degradation due to the thermal processing.
Dantas et al. (2019) reported that the use of milk powder yielded a 72.9% of ascorbic
acid retention on acerola fruit formulations, while Braga and Rocha (2013) described
a 14% degradation on the anthocyanins content on the blackberry dried powders.
Maltodextrin is a versatile form of hydrolyzed starch and it is frequently used as
a drying carrier in order to modulate both the feed composition, process efficiency,
and final powder characteristics. Souza and Oliveira (2012). Several are the reported
benefits of maltodextrin as a drying carrier, such as high solubility, mild residual
flavor, high glass transition temperature, and low hygroscopicity. In addition, authors
have reported increased encapsulation efficiency and production under storage when
maltodextrin is used (Zhang et al. 2018; Ballesteros et al. 2017; Vidović et al. 2014).
Costa et al. (2015) reported that maximum anthocyanins retention on the spouted
bed drying of açai fruit pulp was achieved when 20% maltodextrin was used as
drying carrier, 65 °C of air temperature, and air velocity corresponding to 1.25-times
the minimum spouting air velocity. The same operation conditions were used by
Nascimento et al. (2019) to produce bacaba fruit powder. The authors reported that
using 20% maltodextrin resulted in anthocyanins and phenolic compounds retention
around 90% and 80%, respectively.
5.5 Spouted Bed Drying of Graviola (Annona muricata)

Pulp: A Case Study
The studies regarding the spouted bed drying of fruit pulps carried out by the research
groups at the Federal University of Rio Grande do Norte (UFRN) and the Federal
University of Campina Grande (UFCG), in partnership with the State University of
Campinas (UNICAMP) and the University of Tiradentes (UNIT) have successfully
evolved in the last 20 years (Conrado et al. 2019).
Based on the studies at UNICAMP (Braga and Rocha 2013, 2015), the UFRN
research group developed work on the spouted bed drying of graviola fruit (Annona
muricata) using milk and albumin as drying carriers, which presented promising
results for processing efficiency and production yields (Machado et al. 2015;
Machado 2015; Dantas and Machado 2015). In a follow-up study, Dantas et al.
(2018; Dantas 2018) investigated the influence of the physical properties of graviola
fruit mixtures and the operational conditions (drying carriers concentration and
temperature) on the modeling of mathematical equations that described the powder
production and the drying behavior on the spouted bed dryer, taking into account the
intermittent feeding strategy.
From the mixtures’ physical properties and the material accumulation data, several
mathematical models were proposed in order to describe the powder production and
the outlet air temperature behaviors. Such models were validated with the previous set
of experimental data from Machado (2015), with satisfactory adjusts to the predicted
variables. This case study is comprised of the relevant data gathered during the
development of a master (Machado 2015) and a doctoral (Dantas 2018) thesis, which
describes the drying of graviola fruit pulp and mixtures with milk in a spouted bed
dryer.
5.5.1 Fundamentals
Graviola (Annona muricata L.) is a popular fruit grown in all tropical regions, native
from the Caribbean, Central and South America, and valued for its pleasant char-
acteristics: moderate, aromatic acidity, juicy pulp, and distinct flavor (Quek et al.
2013). The fruits of the graviola are oval, large, and wide, about 10–30 cm long, and
can weigh up to 4.5 kg (Nwokocha and Williams 2009). The edible pulp of the fruit
corresponds to about 67.5% of the total fruit mass (Badrie and Schauss 2010). When
it reaches physiological maturity, the graviola completes ripening within six days,
which makes the graviola fruit extremely perishable (Oliveira et al. 2019).
Among the enzymes found in the graviola fruit, pectinesterase stands out, a more
heat resistant enzyme, which can lead to geleification and precipitation of pectin in
pulps and graviola juices and polyphenol oxidase. This enzyme is responsible for
darkening the fruit pulp (Badrie and Schauss 2010).
Studies on the presence of compounds with phytochemical and pharmacological
properties are being carried out and reveal the existence of new acetogenins in all
parts of the graviola fruit. Among the pharmacological properties, the following stand
out: cytotoxicity and anti-leishmanicide activity of the fruit pericarp; antiviral ability
against the herpes-causing HSV-1 virus; anticarcinogenic and genotoxic effects (exis-
tence of acetogenins with antitumor property); activity for healing injuries and
antimicrobial capacity (Coria-Téllez et al. 2018). Antibacterial activities against
Staphylococcus aureus, Stapylococcus epidermidis, Propionibacterium acne, and
Pseudomonas aeruginosa were also found positive (Pai 2016).
Due to the fruit’s fragility and ease of suffering injuries, graviola is usually indi-
cated for processing, being used in the manufacture of juices, nectars, syrups, shakes,
sweets, jams, ice cream, powders, and flakes (Quek et al. 2013; Gratão et al. 2007). In
parallel with the growth of fruit production, there has been an increase in consump-
tion of fruit-based beverages in recent years. In these preparations fruits are usually
associated with dairy compounds such as milk and whey protein. The development
of these flavored dairy foods becomes an alternative that adds functional and more
attractive value to the product (Moura et al. 2015).
Considering the characteristics of graviola fruit and the importance of the study
of drying this fruit minimizing the use of additives and incorporating nutritional
ingredients that act as agents that enable the good performance of the process, the
drying of the graviola pulp with addition of milk in a spouted bed dryer with inert
particles was investigated (Machado 2015). The effects of milk concentration on
the mixture, drying air temperature, intermittent feeding time and air flow on yield,
production rate, powder moisture, drying rate, and thermal efficiency, as well as the
impact of the process on the physicochemical characteristics and physical properties
of mixtures reconstituted by post rehydration were assessed. This study was expanded
(Dantas et al. 2018; Dantas 2018) investigating the influence of the physical properties
of graviola pulp + milk mixtures and temperature in order to generate mathematical
equations and models for the prediction of recovered powder and the spouted bed
dryer behavior, based on mass and energy balances, using intermittent feeding.
5.5.2 Materials and Methods
5.5.2.1 Materials
Graviola pulp (GP) was obtained by manual depulping of ripe fresh graviola fruits
acquired in the local market (Natal, Brazil). The fruit pulp was processed with a
domestic blender and sieved through a nylon cloth (0.5 mm) in order to further
remove any parts of peels and seeds. The GP was then frozen to −20 °C until use.
Pasteurized whole milk was obtained from the local market.
High-density polyethylene (HDPE) particles were used for the inert bed. The parti-
cles were characterized through the mean diameter (as a sphere of equal volume) and
density by liquid-phase picnometry. The inert bed apparent density was calculated
as the ratio between the inert load mass (2.5 kg) and the apparent volume of the bed.
The porosity of the static bed (ε) was estimated according to Eq. 5.1. All measures
were taken in triplicate.
ρap = (1 − ε)ρinert (5.1)
where ρap is the apparent density of the inert bed, ε is the porosity of the static bed,
and ρinert is the density of the inert particles.
5.5.2.2 Drying Apparatus
The spouted bed dryer used in this work is similar to the apparatus shown in Fig. 5.1.
The dryer was composed of a stainless steel cylindrical column (72 cm height, 18 cm
diameter) with a conical base (60° angle, 13 cm height, 3 cm inlet air diameter)
and a Lapple-type cyclone (40 cm height, 10 cm diameter, 5 cm overflow, 2.5 cm
underflow).
The inlet air was supplied by a 7 hp centrifugal blower (model CR-6, IBRAM-
Weq, Brazil) and heated by a set of 2 kW electrical resistances. The mixtures inlet
feed was atomized using a twin-fluid nozzle coupled with a peristaltic pump. A low
power compressor supplied the atomization air.
A digital thermo-hygrometer, digital anemometer, digital K-type thermocouple
thermometers, and a U-type manometer were used to measure the air temperature
and relative humidity, air flow, air temperature in the cyclone outlet and in the drying
chamber walls, and the bed pressure drop, respectively.
Table 5.1 Study variables of the full 24 factorial experimental design

Value X L (%) Tge (°C) tinter (min) v ∗ /vjm
−1 30 70 10 1.2
0 40 80 12 1.35
+1 50 90 14 1.5
Legend: X L —milk concentration; Tge —inlet air temperature; tinter —intermittent feeding time;
v∗ /vjm —ratio between inlet air velocity and minimum spouting air velocity
5.5.2.3 Experimental Design and Drying Conditions
A full 24 factorial design with three repetitions on the central point (total 19 exper-
iments) was used to investigate the influence of milk concentration (X L ; %), inter-
mittent feed time (tinter ; min), drying temperature (Tge ; °C), and ratio between inlet
air velocity and minimum spouting air velocity (v∗ /vjm ) on the drying yield (Y; %),
powder moisture (Upo ; %), powder production rate (Wpo ; g/min), drying rate (K; g/s),
and process thermal efficiency (EFF; %). The levels for each one of the four study
variables are shown in Table 5.1.
After the operation conditions were set, the feeding was initiated at a rate of 7.0
± 0.8 mL/min using a twin-fluid atomizer nozzle. Six feeding cycles of 6 min were
performed, while the intermittent feeding time was defined as the interval between
the stop after 6 min feeding and the start of a new feeding cycle. Throughout the
drying experiments, outlet air temperature and humidity were measured every 2 min.
After the six feeding cycles, the inert particles were weighted in order to assess the
amount of fruit powder not entrained and accumulated within the bed.
5.5.2.4 Samples Characterization
GP samples and GP + milk mixtures were characterized for soluble solids, density
and viscosity. Soluble solids (SST; °Brix) measures were performed by direct read
in a digital refractometer (model Smart-1, Atago, USA). The density was assessed
by picnometry at 25 °C, according to AOAC method 952.22 (AOAC 2006). For
viscosity, the rheological data of all samples were taken by a digital viscosimeter
(model DV-II + Pro, Brookfield Engineering, USA), for 300 mL samples. Reads
were performed in 5 min. Total acidity (ATT) was determined by titration and results
were expressed as citric acid equivalents (g/100 g) (AOAC 2006).
5.5.2.5 Drying Yields
Drying yield (Y; %) was calculated as total solids recovery. It was defined as the
ratio between the total solids content on the powdered samples (recovered at the
cyclone outlet) and the total solids content on the initial sample formulations (GP +
milk), according to Daza et al. (2016). For the spouted bed drying experiments, the
powder production data was used to adjust a linear model and determine the powder
production rate (Wpo ; g/min).
5.5.2.6 Powder Characterization
For the dried powders, samples were assessed for pH, moisture content, water activity,
total titratable acidity, solubility, and reconstitution time. Samples pH was deter-
mined using a digital potentiometer (model Tec-5, Tecnal, Brazil), water activity
was determined using a digital dew point hygrometer Aqualab® (model series 3 TE,
Decagon Devices, USA) at room temperature (23 °C). Moisture was assessed by the
gravimetric method at 70 °C (Tontul et al. 2018).
Solubility was assessed according to Rocha et al. (2011). Samples (1 g) were
mixed with 100 mL of distilled water, stirred for 5 min, and centrifuged (3000 rpm,
5 min). Supernatant aliquots (20 mL) were transferred to Petri dishes and dried at
70 °C to constant weight. Solubility was calculated as percentage of material soluble
in the supernatant (%).
Reconstitution time was evaluated by dissolving the powdered samples in
distilled water under constant stirring until the initial soluble solids content of the
non-processed mixture was achieved and no agglomerated material was observed.
5.5.2.7 Thermal Efficiency
The thermal efficiency of the spouted bed drying process was evaluated based on
energy and mass balances and calculations according to Passos et al. (2004) and
Saldarriaga et al. (2015). The overall thermal efficiency (EFF; %) was defined as
the ratio between the energy (heat) used in the drying process for water evaporation
(Q evap ) and the energy (heat) provided by the inlet drying air flow (Q inlet ), calculated
according to Eqs. 5.2–5.4.
Q evap (kJ/s) = Wevap × Λ (5.2)

Q inlet (kJ/s) = Winlet × Cp × Tge − Tea (5.3)
EFF (%) = Q evap /Q inlet × 100 (5.4)
where Wevap is the evaporated water molar flow (kmol/s), Λ is the enthalpy of vapor-
ization of water (kJ/kmol), Winlet is the inlet air molar flow (kmol/s), Tge is the inlet
air temperature (°C), and Tea is the room temperature (°C).
5.5.2.8 Mathematical Modeling
For constructing a mathematical model of the spouted bed drying of graviola

pulp + milk mixtures, further drying experiments were performed, as described
in Sect. 5.2.2. The sample mixtures of graviola pulp + 30% milk (GP-30M),
graviola pulp + 40% milk (GP-40M), and graviola pulp + 50% milk (GP-50M)
were dried at three different temperatures (60, 70 and 80 °C) using two different
inert particles for the dryer’s bed, polypropylene (PP) and high-density polyethylene
(HDPE). The intermittent feeding period defined for the experiments was 4 min. The
physicochemical composition of the sample mixtures can be found in Table 5.2.
The physical properties of mixtures and inert particles, as a function of the compo-
sition of materials and the temperature of the drying process, considered for the
definition of the equation describing the production of graviola-based powders in
the spouted bed dryer were viscosity, surface tension, density, contact angle, adhe-
sion work, fat concentration, and reducing sugars concentration. The Vaschy–Buck-
ingham theorem was applied in order to mathematically represent the inlet flow of
the mixtures.
The energy balance of the process was constructed based on the outlet air temper-
ature, the mathematical model for powder production (powder removal from the
dryer), the operational conditions of the drying process, the correlations for drying
rates, and the dryer wall temperature. The mathematical model for the energy balance,
based on the first law of Thermodynamics, considering the powder accumulation
inside the dryer, can be written as Eq. 5.5.
dTgs Wge cpge Tge + Wpe cppe Tpe − Wgs cpgs Tgs − cppo Tgs Wpo − kH v − Q̇
=
dt m g cpgs + m pi cppi + m j cp j Tgs + Mcppo
(5.5)
where Tgs is the temperature of the outlet air flow (°C), Wge is inlet air mass flow
(g/s), cpge is the specific heat of the inlet air flow (J/g K), Tge is the temperature of
the inlet air flow (°C), Wpe is the mixture inlet mass flow (g/s), cppe is the specific
heat of the mixture inlet flow (J/g K), Tpe is the temperature of the mixture inlet
flow (°C), Wgs is the outlet air mass flow (g/s), cpgs is the specific heat of the outlet
air flow (J/g K), cppo is the specific heat of the product powder (J/g K), Wpo is the
Table 5.2 Physicochemical

Parameter GP-30M GP-40M GP-50M
composition of the graviola
pulp + milk sample mixtures Reducing 3.45 ± 0.21 2.75 ± 0.17 2.07 ± 0.13
sugars (%)
Fat (%) 0.94 ± 0.08 1.25 ± 0.10 1.56 ± 0.11
Water 12.42 ± 0.98 11.94 ± 0.95 11.63 ± 0.87
content (%)
Legend: GP-30M—graviola pulp + 30% milk; GP-4M—graviola
pulp + 40% milk; GP-50M—graviola pulp + 50% milk
Table 5.3 Inert particles

Properties Results
characterization results
Real density (g/cm3 ) 0.875 ± 0.468
Mean diameter (cm) 0.320 ± 0.050
Apparent density (g/cm3 ) 0.537
Static bed porosity 0.386
powder production rate (g/s), k is the drying rate (g/s), H v is the enthalpy of water
vaporization (J/g), Q̇ is the heat lost to the spouted bed dryer surroundings (J/s), m g
is the outlet air flow mass (g), m pi is the inert particles mass load (g), cppi is the
specific heat of the inert particles (J/g K), and t is time (s).
The procedure for estimating the unknown parameter of the model, the heat lost
to the dryer surroundings (Q), was based on minimizing the objective function of
the least square technique using the heuristic method of optimization PSO (Particle
Swarm Optimization), an algorithm developed by Kennedy and Eberhart (1995) and
also known as a particle swarm method (Prata et al. 2009).
5.5.3 Results and Discussion
5.5.3.1 Inert Material Characterization
The results for the inert HDPE particles are presented in Table 5.3. From the charac-
teristic curve of the inert particle bed, which represents the pressure drop in the bed
due to the air surface velocity inside the column, the minimum spouting air velocity
0.8 m/s and stable spouting pressure drop of 319.37 Pa were determined. In order
to work under stable fluid dynamic conditions, we chose to work in an air velocity
range between 20 and 50% above the minimum spouting air velocity found for the
bed without adding the mixtures of GP and milk.
5.5.3.2 Characterization of Graviola Pulp and Sample Formulations
Table 5.4 shows the physicochemical characterization of graviola pulp and the sample
formulation with the addition of 30% (GP-30M), 40% (GP-40M), and 50% (GP-
50M) of pasteurized whole milk, prior to the spouted drying.
According to Brazilian legislation (BRASIL 2000), the graviola pulp should
present minimum values for total soluble solids of 9 °Brix, pH 3.5, total acidity
of 0.6 g/100 g, and total solids of 12%. The results found in this study, where the
graviola pulp was obtained without water addition, meet the legislation parameters.
All found values are above the minimum required.
Canuto et al. (2010) analyzed the GP produced in the Brazilian state of Pará and
found values of 88.1%, 12 °Brix, and 3.7 for moisture, total soluble solids, and pH,
Table 5.4 Physicochemical characterization of graviola pulp and graviola pulp + milk sample
formulations
Parameter GP Milk GP-30M GP-40M GP-50M
Moisture (%) 82.4 ± 0.9 87.60 ± 0.35 85.33 ± 0.49 85.55 ± 0.14 85.73 ± 0.64
SST (°Brix) 15.7 ± 0.34 12.99 ± 0.06 12.89 ± 0.07 11.76 ± 0.30 9.69 ± 0.16
pH 4.13 ± 0.02 6.57 ± 0.02 4.17 ± 0.08 4.22 ± 0.08 4.47 ± 0.02
ATT 0.77 ± 0.04 ND 0.53 ± 0.04 0.48 ± 0.02 0.46 ± 0.04
Legend: GP—graviola pulp; GP-30M—graviola pulp + 30% milk; GP-40M—graviola pulp +
40% milk; GP-50M—graviola pulp + 50% milk; SST—total soluble solids; ATT—total titratable
acidity; ND—not detected
respectively. Marcellini and Cordeiro (2003) presented results of analysis of graviola

fruits produced and marketed in the Brazilian state of Sergipe: 88.3% moisture, 12.21
°Brix for soluble solids, pH 4.36 and 0.578 g/100 g of total acidity. The GP charac-
terized in the present study contains less water, higher concentration of soluble solids
and acidity, and pH among the values cited by the authors. It is important to mention
that the in natura pulps present variations in their physicochemical characteristics
due to variations in the physiological conditions of the fruit.
The addition of milk with lower concentration of soluble solids and higher mois-
ture content results in wetter mixtures with lower soluble solids content than natural
GP. Since milk presents a basic character, its addition elevates the pH of the GP +
milk mixtures compared to that of fruit pulp, and consequently lowers the acidity
(Table 5.4).
5.5.3.3 Drying Process Performance
The matrix for the full 24 factorial experimental design and the results observed in the
spouted bed drying of GP + milk formulations are presented in Table 5.5. In all drying
experiments, the fluid dynamic conditions of the spouted bed dryer remained stable,
without instabilities or bed collapse. However, in most experiments, low powder
production was observed, which can be related to the accumulation of dried material
in the dryer walls and the retention of powder in the inert bed (20.7 ± 5.7 g, on
average)
For all experiments, the powder production data as a function of time were
linearized and the correlation coefficients presented good adjusts (>0.90). The
angular coefficient for all the adjusted linear models represents the powder production
rates. Figure 5.2 illustrates the linear adjusted models representing the cumulative
powder production for experiments carried out with intermittent feeding time of
10 min. The other experiments presented similar behavior. These results are compat-
ible with those reported by previous authors (Dantas et al. 2019; Braga and Rocha
2015; Souza Júnior 2012).
Table 5.5 Full 24 factorial design and responses for the spouted bed drying of graviola pulp +
milk formulations
Run X L (%) Tge (°C) tinter (min) v ∗ /vjm Y (%) Upo (%) Wpo (g/min) K (g/s) EFF
(%)
1 −1 (30) −1 (70) −1 (10) −1 (1.2) 14.28 6.39 0.078 0.083 38.49
2 1 (50) −1 (70) −1 (10) −1 (1.2) 24.54 5.48 0.181 0.142 60.38
3 −1 (30) 1 (90) −1 (10) −1 (1.2) 3.90 6.98 0.018 0.056 20.22
4 1 (50) 1 (90) −1 (10) −1 (1.2) 17.32 6.17 0.099 0.091 27.86
5 −1 (30) −1 (70) 1 (14) −1 (1.2) 4.70 9.99 0.024 0.092 44.65
6 1 (50) −1 (70) 1 (14) −1 (1.2) 34.17 6.72 0.142 0.100 45.43
7 −1 (30) 1 (90) 1 (14) −1 (1.2) 5.16 6.00 0.021 0.084 29.41
8 1 (50) 1 (90) 1 (14) −1 (1.2) 10.98 5.39 0.036 0.081 33.62
9 −1 (30) −1 (70) −1 (10) 1 (1.5) 16.97 7.49 0.105 0.094 41.80
10 1 (50) −1 (70) −1 (10) 1 (1.5) 42.65 6.24 0.303 0.102 55.07
11 −1 (30) 1 (90) −1 (10) 1 (1.5) 10.95 5.43 0.069 0.116 22.40
12 1 (50) 1 (90) −1 (10) 1 (1.5) 33.96 4.40 0.203 0.070 19.87
13 −1 (30) −1 (70) 1 (14) 1 (1.5) 32.47 7.11 0.143 0.045 16.86
14 1 (50) −1 (70) 1 (14) 1 (1.5) 30.44 5.74 0.155 0.098 49.83
15 −1 (30) 1 (90) 1 (14) 1 (1.5) 10.06 5.26 0.055 0.067 16.82
16 1 (50) 1 (90) 1 (14) 1 (1.5) 36.28 4.18 0.151 0.066 21.99
17 0 (40) 0 (80) 0 (12) 0 (1.35) 20.72 6.32 0.087 0.083 33.39
18 0 (40) 0 (80) 0 (12) 0 (1.35) 15.97 7.27 0.067 0.104 29.33
19 0 (40) 0 (80) 0 (12) 0 (1.35) 17.44 5.85 0.089 0.081 28.71
Legend: X L —milk concentration; Tge —inlet air temperature; tinter —intermittent feeding time;
v ∗ /vjm —ratio between inlet air velocity and minimum spouting air velocity; Y —powder production
yield; Upo —powder moisture; Wpo —powder production rate; K—drying rate; EFF—thermal
efficiency
As presented in Table 5.5, the moisture content of the powdered samples varied
from 4.18 to 9.99%. Lower moisture values are noted for tests performed at the
highest temperature. These results corroborate the values found by Souza (2009) for
the spouted bed drying mixtures of mango, umbu, and seriguela pulps (4.4–7.5%).
The powder production rates ranged from a minimum of 0.018 g/min in Run 3 to a
maximum of 0.303 g/min in Run 10 with yields of 3.9% and 42.5%, respectively. By
analyzing the responses for the full 24 factorial experimental design, the influence of
the independent variables (study factors) on the moisture content, powder production
rate and yields can be verified in the Pareto diagrams (Fig. 5.3), at a confidence level
of 95%.
As shown in Fig. 5.3a, none of the study variables, alone or combined with the
other variables, presented significant effects on the moisture content, although it is
noticeable in the Pareto diagram the trend for higher temperatures to produce powders
Fig. 5.2 Representative behavior of powder production for the spouted bed drying of graviola pulp
+ milk formulations, at intermittent feeding time of 10 min
with lower moisture contents. These results can be justified by the low feeding flow
of the mixture, kept virtually constant.
In Fig. 5.3b, c are illustrated the Pareto diagrams for the powder production
rate and drying yield, respectively. For the powder production rate, all study factors
independently have significant effects on the response. The effects of air flow and
solid concentration are positive and of greater intensity, while inlet air temperature
and intermittent feeding time negatively influence the powder production. These
results are compatible with phenomenological observations of the process and with
the literature. The positive effect of milk concentration is justified by its fat content
(Medeiros et al. 2002) and high glass transition temperature.
The negative effect of the inlet air temperature on the powder production rate
is cited by several authors. With the inert bed heated above the glass transition
temperature of the dehydrated fruit pulp, the film adhered to the surface of the inert
material. It behaves like a rubber-like material with hygroscopic characteristics, and
its compromised detachment only occurs due to the action of shock and friction of
inert material (Collares et al. 2004; Hofsetz et al. 2007). When the mixture feeding
is suspended for a longer period and the air temperature is high, the bed becomes
more heated and the glass transition temperature of the dehydrated pulp is achieved
resulting in powder adherence and compromising powder production (Souza 2009).
Higher air flow rates promote higher solid circulation rate and frequency of shocks
between the inert particles, facilitating detachment of adhered film. Figure 5.3c
shows that only the air flow showed a significant and positive effect on drying yield.
The effects of milk concentration and inlet air temperature were almost significant,
positive and negative, respectively, as expected since yield is a function of powder
production. In the calculation of yield, the moistures of the fed mixture and the
powder produced are included. The moisture of the mixtures has undergone small
variations that depended on the characteristics of the processed graviola pulp. On
Fig. 5.3 Pareto diagrams for

the influences of the study
variables on the drying
responses: a moisture
content, b powder production
rate, c drying yields
the other hand, the moisture of the inlet air flow (not controlled in the experiments)
and the temperature interfere in the moisture of the recovered powder. In a combined
way, these variables ended up interfering in the yield and nullifying the statistical
significance of the other variables. These interactions justify why the other operating
variables presented statistically less significant and lower intensity effects on yield,
although with the same trend observed in the powder production rate.
Since none of the independent variables presented significant effects on the powder
moisture content, statistical models were adjusted to the experimental data of the
powder production rate and drying yield, and they are represented in Eqs. 5.6–5.7.
For the powder production rate, effects that did not present statistical significance
were eliminated from the models. For yield, the “almost significant” effects of inlet
air temperature (Tge ) and v∗ /vjm ratio was considered in the models.
Wpo = 0.109 + 0.044 × X L − 0.033 × Tge − 0.025 × tinter + 0.040 v∗ /vjm (5.6)
Y = 20.155 + 8.24 × X L − 4.476 × Tge + 6.171 v∗ /v jm (5.7)
where X L —milk concentration; Tge —inlet air temperature; tinter —intermittent

feeding time; v∗ /vjm —ratio between inlet air velocity and minimum spouting air
velocity; Y—powder production yield; Wpo —powder production rate.
The adjusted models for both the powder production rate and yield have a reason-
able quality of agreement with the experimental data. The determination coeffi-
cients indicate a satisfactory adjustment between the values observed and predicted
by the correlations (R2 > 0.80). However, F tests for both regression models and
lack of fit tests indicate that both models are statistically significant and that there
is a satisfactory adjustment of the first-order model to experimental observations.
Figure 5.4 illustrates the satisfactory adjust between the experimental data and the
values predicted by the adjusted regression models.
5.5.3.4 Drying Rates and Thermal Efficiency
Before analyzing the behavior of drying rates and thermal efficiency of the spouted
bed drying in the processing of GP + milk formulations, it is necessary to evaluate
the temperature and humidity conditions of the outlet air flow, as these variables
were used in the mass and energy balances and calculation of the drying and heat
exchange rates and, consequently, in determining the thermal efficiency of the dryer.
Figure 5.5 illustrates the experimental data of air humidity (Fig. 5.5a) and temper-
ature (Fig. 5.5b) for the dryer outlet air flow, for a representative set of experimental
conditions. This set of conditions includes the behavior observed in all experiments.
In all curves, the same behavior reported by Dantas (2013) is observed, tempera-
ture oscillations due to discontinuation of the feeding flow (intermittent feed). These
oscillations become more evident in the tests with longer intermittent feeding times
and greater flow of air, represented by the v∗ /vjm ratio.
Fig. 5.4 Experimental data versus adjusted mathematical models for powder production rate (a) and
yield (b)
Fig. 5.5 Representative experimental behavior of air humidity a and temperature b of the spouted
bed dryer’s outlet air flow
As shown in Fig. 5.5, the behavior of air humidity is the same observed for
temperature, with alternating oscillations as a function of the intermittent feeding time
of GP + milk formulations. It is also observed that oscillations are attenuated when
the intermittent feeding time is shorter. There is also a small influence of the inlet air
temperature on the air humidity at the dryer’s outlet air flow. The air leaves the dryer
with lower humidity content when drying occurs at higher temperatures. However,
an important effect of the initial air humidity is observed, which corresponds to the
humidity of the air fed to the dryer. Coincidentally, in experiments carried out at 90 °C,
the fed air was much drier. This variable may have interfered more significantly in
the air humidity curve along the drying process.
The drying rates are subjected to variations of the initial air humidity (not
controlled in this work), since they were calculated from the mass and energy balances
for the inlet and outlet air flows. On the other hand, the GP + milk formulations feed
flow also suffered mild variations (7.0 ± 0.8 mL/min) due to the physical properties
(density and viscosity) of the sample formulations. Figure 5.6 illustrates, at the same
scale, the feeding and drying rates of a representative set of experiments.
The drying rate results presented in Table 5.5 represent an average of the drying
rates observed during the feeding periods, since the drying rate was almost null during
the periods when feeding was suspended. The results regarding the drying rates are
consistent with those found by other authors (Souza Júnior 2012; Dantas 2013)
and can predict the condition of constant drying rate with continuous pulp/mixture
feeding, as cited by Moraes Filho (2013).
The drying rates are subject to variations in the initial air humidity (not controlled).
The heat exchange rates used for water evaporation during the drying process and
the heat exchange rates lost to the dryer surroundings were calculated and are shown
in Fig. 5.7.
Figure 5.7 shows the same oscillatory behavior verified for the other variables
previously analyzed, resulting from the intermittent feeding of the GP + milk
formulations. The heat exchange rates used for water evaporation follow the same
behavior as drying rates, and present lower values than the energy lost to the dryer’s
surroundings (Fig. 5.7a, b).
It is important to highlight the gap in the peaks of each curve and the most
pronounced heat losses in the period in which the feed is suspended, when the heat
spent on evaporation is minimal. As a result, the heat exchange rates lost fluctuate
less over the drying process. Considering that the mixture feeding flow was constant
in all experiments, an analysis of the results demonstrates that the dryer operates
above the thermal conditions necessary to enable the evaporation rates required in
the drying process. In addition to the temperature, the air flow required to maintain
the stability conditions of the spouting bed with high circulation rate of solids and
sufficient friction for the breakup of the adhered dried film extrapolates the thermal
demands of the drying process.
In the conditions illustrated in Fig. 5.7c, the behavior is different from that
observed in Fig. 5.7a, b. It is observed that the peaks in heat exchange rates spent
on evaporation coincide with the heat losses. Oscillatory behavior is maintained
in these conditions, being less evident in the heat losses data, with a tendency to
become constant. Heat losses to the dryer surroundings are in a range lower than
those observed in Fig. 5.7a, b, which can be justified by the concomitant conditions
of lower temperature and inlet air flow to the dryer.
The drying rates ranged from a minimum of 0.046 g/s in Run 13 to a maximum
of 0.142 g/s in Run 2 (Table 5.5). For Run 2 the high evaporation rate may be due to
the high mixture feeding flow. Regarding the dryer’s thermal efficiency, the values
observed in Table 5.5 are low and, for the most part, below 50% as expected. The
Runs 2, 13, and 15 presented the highest and lowest thermal efficiencies, 60.80%,
16.86%, and 16.82%, respectively.
Figure 5.8 shows the Pareto diagrams for the responses drying rate (Fig. 5.8a) and
thermal efficiency (Fig. 5.8b) in relation to the study factors.
From the analysis of Fig. 5.8, it is verified that none of the study factors, alone
or combined, had statistically significant effects on the drying rates. This result
was expected and agrees with other results found in the literature (Dantas 2013;
Fig. 5.6 Representative experimental behavior of feeding and drying rates for a Run 3, b Run 6,
and c Run 7
Fig. 5.7 Representative experimental behavior of the heat exchange rates used on water evaporation
during the drying process (Q evap ) and the heat exchange rates lost to the dryer’s surroundings (Q p )
for a Run 3, b Run 6, and c Run 7
Fig. 5.8 Pareto diagrams for the influences of the study variables on the drying responses: a drying
rate, b thermal efficiency
Bacelos 2005) which shows the strong dependence on drying rates with the mixture
feeding flow. As in this study, except for the variations due to the control difficulties,
the mixture feeding flow was virtually constant, and the effects of the other study
variables were not statistically significant.
Regarding the dryer thermal efficiency, only the variable intermittent feeding
time showed no significant effect. The effects of temperature and inlet air flow are
negative, with the temperature presenting the highest intensity, which was expected
and agrees with the previous discussion on extrapolation of these operating variables.
The concentration of milk also interfered significantly and positively on dryer thermal
efficiency. The influence of this study factor may be attributed to the higher inlet water
flow to be evaporated since the higher concentration of milk means a lower percentage
of solids in the feeding mixture. As previously mentioned, milk contains a lower
solids content when compared to graviola pulp. In addition, the higher fat content
in the inlet feeding mixture facilitates the particles’ flowability and bed stability,
which can also imply better use of thermal potential for water evaporation. Some
interactions between the variables also had significant effects on thermal efficiency,
as observed in the Pareto diagram (Fig. 5.8b).
Since none of the study factors presented significant effects on the drying rate, a
mathematical model was adjusted only to the experimental data of thermal efficiency
(Eq. 5.8). Non-significant effects from study factors and variables interactions were
not considered in the model, which presented good adjust to the experimental data
(R2 = 0.892).
EFF = 33.50 + 5.18 × X L − 10.05 × Tge − 3.50 × v∗ /vjm − 3.37 × X L × Tge

+ 3.19 × Tge × tinter + 3.22 × X L × tinter × v∗ /vjm (5.8)
Figure 5.9 shows the relation between the experimental data for the dryer thermal
efficiency and the predicted values by the adjusted mathematical model, representing
the satisfactory agreement between them.
5.5.3.5 Powder Characterization
For the physicochemical characterization of dried powder, the experimental condi-

tions that presented the highest yields were chosen. Therefore, Run 10 (X L = 50%,
Tge = 70 ◦ C, tinter = 10 min, v∗ /vjm = 1.5, Y = 42.65%), Run 13 (X L = 30%,
Tge = 70 ◦ C, tinter = 14 min, v∗ /vjm = 1.5, Y = 32.47%), and Run 16 (X L = 50%,
Tge = 90 ◦ C, tinter = 14 min, v∗ /vjm = 1.5, Y = 36.28%) were selected. The results
for moisture content, water activity (aw ), total titratable acidity, and solubility of the
dried powders are presented on Table 5.6.
Moisture content and water activity are important parameters for food conser-
vation. The moisture content represents the total water present in the food matrix,
while water activity represents the free or available water content in the food matrix
to be used on microbial, enzymatic, and biochemical reactions (Nóbrega et al. 2015;
Fig. 5.9 Experimental data versus adjusted mathematical model for the dryer thermal efficiency

Parameter Run 10 Run 13 Run 16
characterization of the dried
graviola pulp + milk on Moisture 5.68 ± 0.61 7.17 ± 0.09 4.41 ± 0.32
selected high-yielding content (%)
conditions aw 0.331 ± 0.001 0.375 ± 0.003 0.274 ± 0.007
ATT 3.22 ± 0.13 4.46 ± 0.02 3.81 ± 0.02
(g/100 g)
Solubility 64.18 ± 0.19 70.20 ± 1.38 66.52 ± 0.21
(%)
Legend: aw —Water activity
Casciatori et al. 2015). The range established for dried and stable foods, from a
microbiological point of view, is aw < 0.6 and moisture content below 25% (Dantas
et al. 2019; Moraes et al. 2017). The powders obtained here are within the desirable
ranges in relation to the two parameters. Dantas et al. (Dantas et al. 2019) reported
similar values for moisture content (5.28–7.04%) and water activity (0.362–0.374)
for spouted bed dried acerola pulp using milk powder and concentrated whey protein
as drying carriers.
Regarding the total acidity (expressed in g citric acid/100 g), comparing the results
of the powders (Table 5.6) with those of the natural mixtures (Table 5.4), it is observed
that the powders are more acidic, which was expected due to water evaporation. There
Fig. 5.10 Dried powders

and water reconstituted
mixtures for a Run 13 and
b Run 16
is also the highest acidity of the powder produced from the drying of the mixtures
with 30% milk, due to the higher concentration of the fruit with acid characteristic.
Solubility is an important physical property that can be defined as the ability of
the solute (dried powders) to remain in homogeneous mixture with water (Borges
et al. 2016). The powders presented high solubility, with values close to those found
by Souza (Souza 2009) for the mixtures of siriguela, umbu, and mango with the
addition of starch, pectin, and palm fat, 60.15 and 67.82%. The solubility results are
comparable to those reported by Dantas et al. (2019) for spouted bed dried acerola
pulp (61.5–75.4%), and higher than those reported by Correia et al. (2017) for spray
dried blueberry extract using vegetal proteins as drying carriers (28.1–52.4%)
Figure 5.10a, b display the images of the powders obtained in Runs 13 e 16,
respectively, and the reconstituted mixtures obtained by rehydration with water. As
observed, the reconstituted mixtures are homogeneous and very similar to natural
mixtures.
Table 5.7 shows the results for the physicochemical attributes of GP + milk
mixtures prior to drying and the reconstituted mixtures from the rehydration of the
powders obtained in Runs 10, 13, and 16.
The pH of the reconstituted mixture remained close to that of the fresh mixtures,
and in the acid foods classification range. No relevant changes were verified between
the physicochemical attributes of initial GP + milk mixtures and the water recon-
stituted powders. The minor variations can be attributed to the eventual losses on
volatile and other heat-sensitive components due to the drying process (Souza 2009;
Borges et al. 2016), which may not be noticeable, from a sensory point of view, in
face of the physicochemical results presented here.
Table 5.7 Physicochemical attributes of graviola pulp + milk mixtures and reconstituted powders
Parameter In natura Reconstituted
GP-30M GP-50M Run 10 Run 13 Run 16
SST (°Brix) 12.89 ± 0.07 11.76 ± 0.30 12.59 ± 0.33 12.99 ± 0.07 10.91 ± 0.16
pH 4.17 ± 0.08 4.22 ± 0.08 4.48 ± 0.02 4.04 ± 0.06 4.43 ± 0.106
ATT 0.53 ± 0.04 0.48 ± 0.02 0.496 ± 0.000 0.775 ± 0.131 0.543 ± 0.022
Reconstitution – – 80 120 90
time (s)
Legend: GP-3M—graviola pulp + 30% milk; GP-50M—graviola pulp + 50% milk; SST—total
soluble solids; ATT—total titratable acidity
Powders with 50% milk were reconstituted faster than powder with 30% milk.
It can be noted from Fig. 5.10 that the powder with 50% milk presents a looser
aspect, different from the powder with 30% milk, which apparently presents more
agglomerate.
5.5.3.6 Density and Rheological Attributes
For a more detailed evaluation of the effect of milk addition, the study of the rheo-
logical behavior of the in natura GP and GP + milk mixtures at room temperature
was performed. Also, the rheogram of the reconstituted mixture from Run 10 was
obtained. Figure 5.11 shows viscosity curves as a function of viscosimeter rotation.
Both the GP and GP + milk mixtures in different concentrations, and the recon-
stituted mixture (Run 10) presented the same rheological behavior. They behave
as non-Newtonian fluids (n < 1) with pseudoplastic characteristics, since viscosity
decreases with increasing the rotation speed of the viscosimeter.
Fig. 5.11 Rheograms of samples of graviola pulp (GP), graviola pulp + 30% milk (GP-30M),
graviola pulp + 40% milk (GP-40M), graviola pulp + 50% milk (GP-50M) and water reconstituted
Run 10 powder
Table 5.8 Rheological attributes of graviola pulp + milk mixtures

Sample n μ (cP) 30 rpm μ (cP) 60 rpm ρ (g/cm3 )
GP 0.483 1080 963.9 1.015
GP-30M 0.359 535.9 395.9 1.019
GP-40M 0.395 539.9 427.9 1.023
GP-50M 0.374 567.9 264.4 1.029
Reconstituted Run 10 0.356 304.9 205 1.048
Milk 1.000 1.65 1.65 1.032
Legend: GP—graviola pulp; GP-30M—graviola pulp + 30% milk; GP-40M—graviola pulp +
40% milk; GP-50M—graviola pulp + 50% milk; μ—apparent viscosity; ρ—density; n—fluid
flow index; cP—centipoise
Table 5.8 shows the values of the apparent viscosity of the unprocessed (GP, GP-
30M, GP-40M, and GP-50M) and water reconstituted mixtures (Run 10) for 30 and
60 rpm, as well as fluid flow index and density of samples.
The values of the apparent viscosity for the rotations of 30 and 60 rpm are compat-
ible with those reported by Medeiros et al. (Medeiros et al. 2002) for tropic fruit
pulps. The apparent viscosities of GP-50M to 30 rpm is higher than that of the Run
10 reconstituted mixture; however, as the viscosimeter rotation increases (60 rpm)
the values become closer. The specific mass (density) of the Run 10 reconstituted
mixture is higher which can be attributed to possible changes in its composition, or
changes in the physicochemical characteristics caused by the heating process. The
density of mixtures increases with the concentration of milk which is justified by the
higher density of milk.
5.5.3.7 Mathematical Modeling of the Spouted Bed Drying of Graviola

Pulp with Intermittent Feeding
Based on experimental results and using the correlations for predicting physical
properties as a function of temperature and milk concentration, the relationship
between the powder production rate (Wpo ) and the reducing sugar and fat contents is
represented by Eq. 5.9 (Dantas 2018).
−2.44 2.29 −6.13
−6 η m rs Wad
Wpo =3.04 × 10 × × ×
ρ 1/3 × σ 1/2 × m fat
1/6 m fat σ
× (m fat × σ )0.5 (5.9)
where Wpo is the powder production rate (g/s), η is the apparent viscosity (Pa s), ρ
is density (g/cm3 ), m fat is the fat content (g), m rs is the reducing sugars content (g),
σ is the superficial tension (mN/cm), Wad is the adhesion work (mN/cm).
Evaluating the relationship between powder production and apparent viscosity, it

was noticed that the influence on this response due to the change in the inert type is
much more evident in conditions in which this property has lower values, resulting
from the increase in temperature and the highest percentage of milk in the mixture.
In the condition of lower concentration of milk and, consequently, higher viscosity,
the type of polymeric material did not interfere so intensely.
The relationship between powder recovery and density is centered on the variation
of milk concentration, in which mixtures with a higher percentage of this ingredient
resulted in larger densities and consequently higher powder production. There was
little influence of process temperature on the variation of this physical property.
The relationship between powder recovery and surface tension indicates that
tensions with lower values implicated higher yields, which is related to increased
temperature and percentage of milk in the mixture.
There was an important increase in powder production with the increase in the
variables of milk concentration and drying temperature, when drying was performed
with HDPE, in these cases there was a reduction in the values of the adhesion work,
which indicates that this inert was best suited for drying these materials.
For graviola pulp mixtures with lower percentage of milk, the large amount of
reducing sugars resulted in lower powder production during the drying process in
the spouted bed dryer. However, in mixtures with a greater amount of milk, due to
the increase in the fat concentration, there was a reduction in adhesion forces and
the significant increase in product recovery (Araújo et al. 2015; Benelli et al. 2013b;
Braga and Rocha 2013).
By evaluating the adjust quality of Eq. 5.9 to the experimental data, it was found
that 95.23% of Wpo variation is explained by the regression model, which indi-
cates that it satisfactorily represents the experimental data. The adhesion work and
surface tension have the greatest influence on the estimation of the powder produc-
tion (Eq. 5.9), a fact observed by the higher values of exponents for these properties,
when compared to the other terms. This reflects the importance of the interaction
between fluid and the inert particle used in the spouted bed dryer.
For the validation of powder production adjusted model (Eq. 5.9), data from
Machado (2015) (Table 5.5) on the production of graviola pulp + milk powders
were used. The mixtures of graviola pulp + milk (30–50%) were dried at 70–90 °C
using HDPE. The experimental data and curves adjusted by the model (Eq. 5.9) are
illustrated in Fig. 5.12.
In order to evaluate the application of the adjusted model based on the mass and
energy balances given by Eq. 5.5, the value of heat lost to the dryer surroundings
(Q) was considered constant, determining an average value for each experiment. The
determined results for heat lost to the dryer surroundings were equal to 203.71 ±
4.69 W, 232.88 ± 3.72 W, and 281.63 ± 5.85 W, for experiments carried out at 60 °C,
70 °C, and 80 °C, respectively.
These values agree with those reported by Machado (2015). In this work, the
authors found that 267 and 222 W corresponded to the heat losses for the processing
of graviola + milk mixtures with 30% milk and 50% processed at 70 °C, respectively.
Using these experiments for validation of Eq. 5.5 and Q = 232.88 W, the adjusted
Fig. 5.12 Experimental data for graviola + milk powder production (Machado 2015) versus
adjusted model (Eq. 5.9)
Fig. 5.13 Experimental data for graviola + milk (Machado 2015) versus adjusted model for heat
loss (Eq. 5.5)
models can be found on Fig. 5.13. The deviations observed for these simulations
were 2.35% and 4.82% for Figs. 5.13a and 5.13b, respectively.
As observed in the curves adjusted to the experimental data, the model was able to
predict the behavior of air temperature at the outlet of the dryer in these experiments.
The most evident deviations observed in Fig. 5.13b are due to the difficulty faced
in controlling the feeding flow of the mixture in this experiment, in which in some
periods of intermittent feeding, the flow of the paste distanced itself from the predicted
mean.
5.5.4 Final Comments
The spouted bed dryer presented stable fluid dynamic behavior with uniform produc-
tion rates although some tests presented low yield and large amount of material
retained in bed and adhered to the walls of the equipment.
All process variables presented significant effects on the powder production rate,
with positive of milk concentration and air flow, and negative effects of tempera-
ture and intermittent feeding time. For yield, the important positive effect was air
flow. None of the process variables had a significant effect on powder moisture;
however, drier powders were obtained at higher air temperature. The first-order statis-
tical models adjusted to the data of the production rate and yield were shown to be
significant and useful for predictive purposes.
The analytical resolution of the equations obtained by Vaschy–Buckingham
theorem generated an empirical equation capable of predicting the behavior of the
graviola pulp + milk powder production rate, considering process variables and
physical properties of the mixtures. This model was used in the energy balance,
in determining the air temperature at the outlet of the dryer, considering the accu-
mulation of material in the drying system. The model described by the differential
equations adapted to the intermittent feeding condition considering the accumula-
tion of mass in the dryer bed was able to describe the phenomena of heat and mass
transfer occurred during the spouted bed drying of graviola pulp + milk under stable
operation.
The heat exchange analysis demonstrated that the dryer operated under conditions
that extrapolated the drying thermal requirements. The first-order statistical model
adjusted to thermal efficiency data was significant and useful for predictive purposes.
The obtained graviola + milk powders presented moisture and water activity
in the indicated range for dry foods, short reconstitution time, and high solubility
compatible with the literature. The reconstituted mixtures presented physicochemical
and rheological characteristics close to those of the unprocessed mixture, which
demonstrates the low impact of the process on the dehydrated product.
5.6 Conclusions
Considering the most recent data reported on the drying of fruit pulps, it is perceived
the current importance of research that seeks to enable the production of fruit powders
through low impact technologies on the product. The current search for products rich
in bioactive compounds and the consumption of healthier foods is an incentive to
investigate drying methods that promote the production of high added value food
components. The spouted bed dryer used in the drying of fruit pulps has presented
promising results mainly with regard to the use of adjuvants such as milk that
promotes the enrichment of the product without compromising sensory characteris-
tics, and the rehydration capacity in water. Low performance problems are related
to powder production or thermal efficiency need to be reevaluated by reusing the
thermal potential of exhaust gas and techniques that will favor powder recovery.
Studies on process modeling with intermittent feeding correlated with the composi-
tion and physical properties of fruit pulp are important and need to be expanded and
validated with data from other fruits.
Acknowledgments Fábio Medeiros was supported by Coordenação de Aperfeiçoamento de

Pessoal de Nível Superior (CAPES, Brazil), grant number 88882.375732/2019-01. The authors
would like to thank the Federal University of Rio Grande do Norte (UFRN) for the technical
support. We also acknowledge scientific support from the authors mentioned along this chapter.
References
Akter, M.S., Oh, S., Eun, J.B., Ahmed, M.: Nutritional compositions and health promoting phyto-
chemicals of camu-camu (Myrciaria dubia) fruit: a review. Food Res. Int. 44, 1728–1732 (2011).
https://doi.org/10.1016/j.foodres.2011.03.045
Altendorf, S.: Major Tropical Fruits Market Review 2017. FAO, Rome (2019). http://www.fao.org/
economic/est/est-commodities/tropical-fruits/en/
Alves, N.N., Messaoud, G.B., Desobry, S., Costa, J.M.C., Rodrigues, S.: Effect of drying technique
and feed flow rate on bacterial survival and physicochemical properties of a non-dairy fermented
probiotic juice powder. J. Food. Eng. 189, 45–54 (2016). https://doi.org/10.1016/j.jfoodeng.2016.
05.023
Andrade Júnior, M.C., Andrade, J.S.: Physicochemical changes in cubiu fruits (Solanum sessil-
iflorum Dunal) at different ripening stages. Food Sci. Technol. 32,250–254 (2012). https://doi.
org/10.1590/s0101-20612012005000049
AOAC: Official Methods of Analysis of AOAC International, 20th edn. AOAC InternationalAr-
lington, USA (2006)
Araújo, A.D.A., Coelho, R.M.D., Fontes, C.P.M.L., Silva, A.R.A., Costa, J.M.C., Rodrigues, S.:
Production and spouted bed drying of acerola juice containing oligosaccharides. Food Bioprod.
Process. 94, 565–571 (2015). https://doi.org/10.1016/j.fbp.2014.08.005
Azevêdo, J.C.S., Borges, K.C., Genovese, M.I., Correia, R.T.P., Vattem, D.A.: Neuroprotective
effects of dried camu-camu (Myrciaria dubia HBK McVaugh) residue in C. elegans. Food Res.
Int. 73, 135–141 (2016). https://doi.org/10.1016/j.foodres.2015.02.015
Bacelos, M.S., Passos, M.L., Freire, J.T.: Effect of interparticle forces on the conical spouted bed
behavior of wet particles with size distribution. Powder Technol. 174, 114–126 (2007). https://
doi.org/10.1016/j.powtec.2007.01.023
Bacelos, M.S., Spitzner Neto, P.I., Silveira, A.M., Freire, J.T.: Analysis of fluid dynamics behavior
of conical spouted bed in presence of pastes. Dry. Technol. 23, 427–453 (2005). https://doi.org/
10.1081/DRT-200054116
Badrie, N., Schauss, A.G.: Soursop (Annona muricata L.). In: Watson, R., Preedy, V. (eds.) Bioactive
Foods in Promoting Health, 1st edn, pp. 621–643. Academic Press, Cambridge, USA (2010)
Ballesteros, L.F., Ramirez, M.J., Orrego, C.E., Teixeira, J.A., Mussatto, S.I.: Encapsulation of
antioxidant phenolic compounds extracted from spent coffee grounds by freeze-drying and spray-
drying using different coating materials. Food Chem. 237, 623–631 (2017). https://doi.org/10.
1016/j.foodchem.2017.05.142
Baracat, M.M., Nakagawa, A.M., Freitas, L.A.P., Freitas, O.: Microcapsule processing in a spouted
bed. Can. J. Chem. Eng. 82, 134–141 (2008). https://doi.org/10.1002/cjce.5450820117
Bell, D.R., Gochenaur, K.: Direct vasoactive and vasoprotective properties of anthocyanin-rich
extracts. J. Appl. Physiol. 100, 1164–1170 (2006). https://doi.org/10.1152/japplphysiol.00626.
2005
Belwal, T., Devkota, H.P., Hassan, H.A., Ahluwalia, S., Ramadan, M.F., Mocan, A., Atanasov, A.G.:
Phytopharmacology of Acerola (Malpighia spp.) and its potential as functional food. Trends.
Food. Sci. Technol. 74, 99–106 (2018). https://doi.org/10.1016/j.tifs.2018.01.014
Benelli, L., Souza, C.R.F., Oliveira, W.P.: Quality changes during spouted bed drying of Pepper-
Rosmarin extract. Can. J. Chem. Eng. 91, 1837–1846 (2013a). https://doi.org/10.1002/cjce.21907
Benelli, L., Souza, C.R.F., Oliveira, W.P.: Spouted bed performance on drying of an aromatic plant
extract. Powder Technol. 239, 59–71 (2013b). https://doi.org/10.1016/j.powtec.2013.01.058
Borges, K.C., Azevedo, J.C., Medeiros, M.F.D., Correia, R.T.P.: Physicochemical characterization
and bioactive value of tropical berry pomaces after spouted bed drying. J. Food. Qual. 39, 192–200
(2016). https://doi.org/10.1111/jfq.12178
Borges, K.C., Bezerra, M.D.F., Rocha, M.P., Silva, E.S.D., Fujita, A., Genovese, M.I., Correia,
R.T.P.: Fresh and Spray Dried Pitanga (Eugenia uniflora) and Jambolan (Syzygium cumini) Pulps
are Natural Sources of Bioactive Compounds with Functional Attributes. J. Probiotics Heal. 4,
e1000145 (2016). https://doi.org/10.4172/2329-8901.1000145
Braga, M.B., Rocha, S.C.S.: Drying of milk-blackberry pulp mixture in spouted bed. Can. J. Chem.
Eng. 91, 1786–1792 (2013). https://doi.org/10.1002/cjce.21918
Braga, M.B., Rocha, S.C.S.: Spouted bed drying of milk–blackberry pulp: analysis of powder
production efficiency and powder characterization. Dry. Technol. 33, 933–940 (2015). https://
doi.org/10.1080/07373937.2014.999372
BRASIL: IN n° 1-7/01/2000. Brasília, MAPA, Brazil (2000). http://www.agricultura.gov.br/ass
untos/vigilancia-agropecuaria/ivegetal/bebidas-arquivos/in-no-1-de-7-de-janeiro-de-2000.doc/
view. (In Portuguese)
Butzge, J.J., Godoi, F.C., Rocha, S.C.S.: Spouted bed drying efficiency of bovine hydrolyzed
collagen. Brazilian. J. Food. Technol. 19, e2015010 (2016). https://doi.org/10.1590/1981-6723.
1015
Butzge, J.J., Hanao, F.H., Godoy, F.C., Rocha, S.C.S.: Drying of the hydrolyzed collagen-grape
pulp mixture in a spouted bed: analysis of the efficiency of obtaining powder and the incorpora-
tion of anthocyanins in the final product. In: XX Brazilian Congress of Chemical Engineering,
pp. 6281–6288, São Paulo, Editora Blücher (2015). https://doi.org/10.5151/chemeng-cobeq2014-
1801-17486-147533. (In Portuguese)
Canuto, G.A.B., Xavier, A.A.O., Leandro, C.N., Benassi, M.T.: Physical and chemical charac-
terization of fruit pulps from Amazonia and their correlation to free radical scavenger activity.
Rev. Bras. Frutic. 32, 1196–1205 (2010). https://doi.org/10.1590/S0100-29452010005000122.
(In Portuguese)
Cappato, L.P., Ferreira, M.V.S., Moraes, J., Pires, R.P.S., Rocha, R.S., Silva, R., Neto, R.P.C.,
Tavares, M.I.B., Freitas, M.Q., Rodrigues, F.N., Calado, V.M.A., Raices, R.S.L., Silva, M.C.,
Cruz, A.G.: Whey acerola-flavoured drink submitted Ohmic Heating: Bioactive compounds,
antioxidant capacity, thermal behavior, water mobility, fatty acid profile and volatile compounds.
Food Chem. 263, 81–88 (2018). https://doi.org/10.1016/j.foodchem.2018.04.115
Casciatori, F.P., Laurentino, C.L., Zanelato, A.I., Thoméo, J.C.: Hygroscopic properties of solid
agro-industrial by-products used in solid-state fermentation. Ind. Crops. Prod. 64, 114–123
(2015). https://doi.org/10.1016/j.indcrop.2014.11.034
Castañeda-Ovando, A., Pacheco-Hernández, M.L., Páez-Hernández, M.E., Rodríguez, J.A., Galán-
Vidal, C.A.: Chemical studies of anthocyanins: a review. Food Chem. 113, 859–871 (2009).
https://doi.org/10.1016/j.foodchem.2008.09.001
Chang, S.K., Alasalvar, C., Shahidi, F.: Review of dried fruits: phytochemicals, antioxidant effica-
cies, and health benefits. J. Funct. Foods 21, 113–132 (2016). https://doi.org/10.1016/j.jff.2015.
11.034
Collares, F., Finzer, J.R., Kieckbusch, T.: Glass transition control of the detachment of food pastes
dried over glass plates. J. Food Eng. 61, 261–267 (2004). https://doi.org/10.1016/S0260-877
4(03)00098-0
Conrado, L.S., Silva, O.S., Dantas, T.N.P., Silva, F.H.S., Cavalcante, J.A., Silva, G.F., Moraes,
C.M., Lima, A.S., Medeiros, M.F.D., Alsina, O.L.S.: Particulate systems research in the Brazilian
Northeast: Campina Grande, Natal, João Pessoa and Aracaju. In: Freire, J.T., Ferreira, M.C.,
Freire, F.B., Maia, G.D. (eds.) An Overview on Particulate Systems in Brazil, 1st edn, pp. 223–253.
Federal University of São Carlos, São Carlos (2019)
Coria-Téllez, A.V., Montalvo-Gónzalez, E., Yahia, E.M., Obledo-Vázquez, E.N.: Annona muricata:
a comprehensive review on its traditional medicinal uses, phytochemicals, pharmacological activ-
ities, mechanisms of action and toxicity. Arab. J. Chem. 11, 662–691 (2018). https://doi.org/10.
1016/j.arabjc.2016.01.004
Correia, R., Grace, M.H., Esposito, D., Lila, M.A.: Wild blueberry polyphenol-protein food ingredi-
ents produced by three drying methods: comparative physico-chemical properties, phytochemical
content, and stability during storage. Food Chem. 235, 76–85 (2017). https://doi.org/10.1016/j.
foodchem.2017.05.042
Costa, E.F., Freire, F.B., Freire, J.T., Passos, M.L.: Spouted beds of inert particles for drying
suspension. Dry. Technol. 24, 315–325 (2006). https://doi.org/10.1080/07373930600564563
Costa, R.G., Andreola, K., Mattietto, R.A., Faria, L.J.G., Taranto, O.P.: Effect of operating condi-
tions on the yield and quality of açai (Euterpe oleracea Mart.) powder produced in spouted bed.
LWT—Food Sci. Technol. 64, 1196–1203 (2015). https://doi.org/10.1016/j.lwt.2015.07.027
Cruz, R.G., Beney, L., Gervais, P., Lira, S.P., Vieira, T.M.F.S., Dupont, S.: Comparison of the
antioxidant property of acerola extracts with synthetic antioxidants using an in vivo method with
yeasts. Food Chem. 277, 698–705 (2019). https://doi.org/10.1016/j.foodchem.2018.10.099
Cunha, R.L., de la Cruz, A.G., Menegalli, F.C.: Effects of operating conditions on the quality of
mango pulp dried in a spout fluidized bed. Dry. Technol. 24, 423–432 (2006). https://doi.org/10.
1080/07373930600611869
Dantas, S.C.M., Pontes Júnior, S.M., Medeiros, F.G.M., Santos Júnior, L.C., Alsina O.L.S.,
Medeiros, M.F.D.: Spouted-bed drying of acerola pulp (Malpighia emarginata DC): effects of
adding milk and milk protein on process performance and characterization of dried fruit powders.
J. Food. Process. Eng. 42, 1–13 (2019). https://doi.org/10.1111/jfpe.13205
Dantas, T.N.P., Machado, I.P., Medeiros, M.F.D.: Study of powder production and accumulation
during the spouted bed drying of graviola pulp and milk with intermittent feeding. In: XXXVII
Brazilian Congress of Particulate Systems, pp 1883–1892, São Paulo, Edgar Blücher Press (2015).
https://doi.org/10.5151/ENEMP2015-SE-737. (In Portuguese)
Dantas, T.N.P., Moraes Filho, F.C., Souza, J.S., Oliveira, J.A., Rocha, S.C.S., Medeiros, M.F.D.:
Study of model application for drying of pulp fruit in spouted bed with intermittent feeding and
accumulation. Dry. Technol. 36, 1349–1366 (2018). https://doi.org/10.1080/07373937.2017.140
2785
Dantas, T.N.P.: Evaluation of the data drying fruit pulp suspensions in spouted bed with intermittent
feeding. Master’s dissertation in Research and Development in Regional Technologies, Federal
University of the Rio Grande do Norte (2013). https://repositorio.ufrn.br/jspui/handle/123456
789/15840. (In Portuguese)
Dantas, T.N.P.: The influence of physical properties of soursop and additive on spouted bed drying
in intermittent feed. Doctoral Thesis in Chemical Engineering, Federal University of Rio Grande
do Norte (2018). https://repositorio.ufrn.br/jspui/handle/123456789/25449. (In Portuguese)
Daza, L.D., Fujita, A., Fávaro-trindade, C.S., Rodrigues, J.N., Granato, D., Genovese, M.I.: Effect
of spray drying conditions on the physical properties of Cagaita (Eugenia dysenterica DC) fruit
extracts. Food Bioprod. Process. 97, 20–29 (2016). https://doi.org/10.1016/j.fbp.2015.10.001
Delgado, J.M.P.Q., Lima, A.G.B.: Transport Phenomena and Drying of Solids and Particulate
Materials, vol. 48. Springer, Heidelberg, Germany (2014)
Demirkol, M., Tarakci, Z.: Effect of grape (Vitis labrusca L.) pomace dried by different methods on
physicochemical, microbiological and bioactive properties of yoghurt. LWT—Food Sci. Technol.
97, 770–777 (2018). https://doi.org/10.1016/j.lwt.2018.07.058
Esposito, D., Chen, A., Grace, M.H., Komarnytsky, S., Lila, M.A.: Inhibitory effects of wild blue-
berry anthocyanins and other flavonoids on biomarkers of acute and chronic inflammation in vitro.
J Agric. Food Chem. 62, 7022–7028 (2014). https://doi.org/10.1021/jf4051599
Fang, Z., Bhandari, B.: Spray Drying of Bioactives. In: Roos, Y.H., Livney, Y.D. (eds.) Engineering
Foods for Bioactives Stability and Delivery, 1st edn, pp. 261–284. Springer Nature, New York
(2017)
Fang, Z., Bhandari, B.: Encapsulation of polyphenols—a review. Trends Food Sci. Technol. 21,
510–523 (2010). https://doi.org/10.1016/j.tifs.2010.08.003
FAO.: The State of Food and Agriculture—Moving forward on food loss and waste reduction.
Rome, FAO (2019). Available from: http://www.fao.org/policy-support/tools-and-publications/
resources-details/en/c/1242090/
Feng, H., Tang, J., Mattinson, D.S., Fellman, J.K.: Microwave and spouted bed drying of frozen
blueberries: the effect of drying and pretreatment methods on physical properties and retention
of flavor volatiles. J. Food Process. Preserv. 23, 463–479 (1999). https://doi.org/10.1111/j.1745-
4549.1999.tb00398.x
Frank, T., Netzel, M., Strass, G., Bitsch, R., Bitsch, I.: Bioavailability of anthocyanidin-3-glucosides
following consumption of red wine and red grape juice. Can. J. Physiol. Pharmacol. 81, 423–435
(2003). https://doi.org/10.1139/y03-038
Freire, J.T., Ferreira, M.C., Freire, F.B.: Drying of solutions, slurries and pastes. In: Epstein, N.,
Grace, J. (eds.) SPouted Spout-Fluid Bed, 1st edn, pp. 206–221. Cambridge University Press,
Cambridge (2011)
Freire, J.T., Ferreira, M.C., Freire, F.B., Nascimento, B.S.: A review on paste drying with inert parti-
cles as support medium. Dry. Technol. 30, 330–341 (2012). https://doi.org/10.1080/07373937.
2011.638149
Fujita, A., Borges, K., Correia, R., Franco, B.D.G.M., Genovese, M.I.: Impact of spouted bed drying
on bioactive compounds, antimicrobial and antioxidant activities of commercial frozen pulp of
camu-camu (Myrciaria dubia Mc. Vaugh). Food Res. Int. 54, 495–500 (2013). https://doi.org/10.
1016/j.foodres.2013.07.025
Fujita, A., Sarkar, D., Wu, S., Kennelly, E., Shetty, K., Genovese, M.I.: Evaluation of phenolic-linked
bioactives of camu–camu (Myrciaria dubia Mc. Vaugh) for antihyperglycemia, antihypertension,
antimicrobial properties and cellular rejuvenation. Food Res. Int. 77, 194–203 (2015). https://doi.
org/10.1016/j.foodres.2015.07.009
Grace, M.H., Ribnicky, D.M., Kuhn, P., Poulev, A., Logendra, S., Yousef, G.G., Raskin, I., Lila,
M.A.: Hypoglycemic activity of a novel anthocyanin-rich formulation from lowbush blueberry,
Vaccinium angustifolium Aiton. Phytomedicine 16, 406–415 (2009). https://doi.org/10.1016/j.
phymed.2009.02.018
Grace, M.H., Xiong, J., Esposito, D., Ehlenfeldt, M., Lila, M.A.: Simultaneous LC-MS quantifi-
cation of anthocyanins and non-anthocyanin phenolics from blueberries with widely divergent
profiles and biological activities. Food Chem. 27, 336–346 (2019). https://doi.org/10.1016/j.foo
dchem.2018.10.101
Gratão, A.C.A., Silveira, V., Telis-Romero, J.: Laminar flow of soursop juice through concentric
annuli: friction factors and rheology. J. Food. Eng. 78, 1343–1354 (2007). https://doi.org/10.
1016/j.jfoodeng.2006.01.006
Habauzit, V., Morand, C.: Evidence for a protective effect of polyphenols-containing foods on
cardiovascular health: An update for clinicians. Ther. Adv. Chronic Dis. 3, 87–106 (2012). https://
doi.org/10.1177/2040622311430006
Heleno, S.A., Martins, A., Queiroz, M.J.R.P., Ferreira, I.C.F.R.: Bioactivity of phenolic acids—
metabolites versus parent compounds: a review. Food Chem. 173, 501–513 (2015). https://doi.
org/10.1016/j.foodchem.2014.10.057
Hernandes, L.C., Aissa, A.F., Almeida, M.R., Darin, J.D.A.C., Rodrigues, E., Batista, B.L., Barbosa,
F., Mercadante, A.Z., Bianchi, M.L.P., Antunes, L.M.G.: In vivo assessment of the cytotoxic,
genotoxic and antigenotoxic potential of maná-cubiu (Solanum sessiliflorum Dunal) fruit. Food
Res. Int. 62, 121–127 (2014). https://doi.org/10.1016/j.foodres.2014.02.036
Hofsetz, K., Lopes, C.C., Hubinger, M.D., Mayor, L., Sereno, A.M.: Changes in the physical
properties of bananas on applying HTST pulse during air-drying. J. Food. Eng. 83, 531–540
(2007). https://doi.org/10.1016/j.jfoodeng.2007.04.003
Hoskin, R.T., Xiong, J., Esposito, D.A., Lila, M.A.: Blueberry polyphenol-protein food ingredients:
the impact of spray drying on the in vitro antioxidant activity, anti-inflammatory markers, glucose
metabolism and fibroblast migration. Food Chem. 280, 187–194 (2019). https://doi.org/10.1016/
j.foodchem.2018.12.046
Jono, K., Ichikawa, H., Miyamoto, M., Fukumori, Y.: A review of particulate design for pharma-
ceutical powders and their production by spouted bed coating. Powder Technol. 113, 269–277
(2000). https://doi.org/10.1016/S0032-5910(00)00310-7
Kamiloglu, S., Toydemir, G., Boyacioglu, D., Beekwilder, J., Hall, R.D., Capanoglu, E.: A review
on the effect of drying on antioxidant potential of fruits and vegetables. Crit. Rev. Food Sci. Nutr.
56, S110–S129 (2016). https://doi.org/10.1080/10408398.2015.1045969
Karam, M.C., Petit, J., Zimmer, D., Baudelaire, D.E., Scher, J.: Effects of drying and grinding in
production of fruit and vegetable powders: A review. J. Food. Eng. 188, 32–49 (2016). https://
doi.org/10.1016/j.jfoodeng.2016.05.001
Karam, M.C., Petit, J., Zimmer, D., Djantou, E.B., Scher, J.: Effects of drying and grinding in
production of fruit and vegetable powders: A review. J. Food. Eng. 188, 32–49 (2016). https://
doi.org/10.1016/j.jfoodeng.2016.05.001
Kennedy, J., Eberhart, R.: Particle swarm optimization. Proc. IEEE Int. Conf. Neural Networks 4,
1942–1948 (1995). http://dx.doi.org/10.1109/ICNN.1995.488968
Khoo, H.E., Azlan, A., Tang, S.T., Lim, S.M.: Anthocyanidins and anthocyanins: colored pigments
as food, pharmaceutical ingredients, and the potential health benefits. Food Nutr. Res. 61,
e1361779 (2017). https://doi.org/10.1080/16546628.2017.1361779
Kris-Etherton, P.M., Hecker, K.D., Bonanome, A., Coval, S.M., Binkoski, A.E., Hilpert, K.F., Griel,
A.E., Etherton, T.D.: Bioactive compounds in foods: Their role in the prevention of cardiovascular
disease and cancer. Am. J. Med. 113, 71–88 (2002). https://doi.org/10.1016/S0002-9343(01)009
95-0
Kumar, C., Karim, M.A., Joardder, M.U.H.: Intermittent drying of food products: A critical review.
J. Food. Eng. 121, 48–57 (2014). https://doi.org/10.1016/j.jfoodeng.2013.08.014
Laleh, G.H., Frydoonfar, H., Heidary, R., Jameei, R., Zare, S.: The Effect of light, temperature,
pH and species on stability of anthocyanin pigments in four berberis species. Pakistan J. Nutr. 5,
90–92 (2006https://doi.org/10.3923/pjn.2006.90.92
Larrosa, A.P.Q., Cadaval, T.R.S., Pinto, L.A.A.: Influence of drying methods on the characteristics
of a vegetable paste formulated by linear programming maximizing antioxidant activity. LWT—
Food Sci. Technol. 60, 178–185 (2015). https://doi.org/10.1016/j.lwt.2014.08.003
Lin, D., Xiao, M., Zhao, J., Li, Z., Xing, B., Li, X., Kong, M., Li, L., Zhang, Q., Liu, Y., Chen,
H., Qin, W., Wu, H., Chen, S.: An overview of plant phenolic compounds and their importance
in human nutrition and management of type 2 diabetes. Molecules 21, e1374 (2016). https://doi.
org/10.3390/molecules21101374
Liu, P., Mujumdar, A.S., Zhang, M., Jiang, H.: Comparison of three blanching treatments on the
color and anthocyanin level of the microwave-assisted spouted bed drying of purple flesh sweet
potato. Dry. Technol. 33, 66–71 (2015). https://doi.org/10.1080/07373937.2014.936558
Lucas, B.F., Zambiazi, R.C., Costa, J.A.V.: Biocompounds and physical properties of açaí pulp
dried by different methods. LWT—Food Sci. Technol. 98, 335–340 (2018). https://doi.org/10.
1016/j.lwt.2018.08.058
Machado, I.P., Delmiro, T.M., Machado, A.K.T., Medeiros, M.F.D.: Spouted bed drying of graviola
and milk mixture: evaluation of the effects of operating variables on production parameters, drying
rate and thermal efficiency. In: XXXVII Brazilian Congress of Particulate Systems, pp. 1756–
1765, São Paulo, Edgar Blücher Press (2015). https://doi.org/10.5151/ENEMP2015-SE-642. (In
Portuguese)
Machado, I.P.: Thermal evaluation and performance of the drying process of graviola and milk
mixtures in a spouted bed dryer. Master’s dissertation in Chemical Engineering, Federal University
of Rio Grande do Norte (2015). https://repositorio.ufrn.br/jspui/handle/123456789/19691. (In
Portuguese)
Manela-Azulay, M., Mandarim-de-Lacerda, C.A., Perez, M.A., Filgueira, A.L., Cuzzi, T.: Vitamin
C. An Bras Dermatol 78, 265–272 (2003). https://doi.org/10.1590/S0365-05962003000300002.
(In Portuguese)
Marcellini, P.S., Cordeiro, C.E.: Physicochemical and sensory comparison of atemóia with pine
cone and graviola produced and marketed in the state of Sergipe. Alim. Nutr. 14, 187–189 (2003).
http://serv-bib.fcfar.unesp.br/seer/index.php/alimentos/article/view/857. (In Portuguese)
Mathur, K.B., Epstein, N.: Spouted Beds. Academic Press Inc., New York, USA (1974)
Mathur, K.B., Gishler, P.E.: A study of the application of the spouted bed technique to wheat drying.
J. Appl. Chem. 5, 624–636 (1955). https://doi.org/10.1002/jctb.5010051106
Medeiros, M.F.D., Rocha, S.C.S., Alsina, O.L.S., Jerônimo, C.E.M., Medeiros, U.K.L., Mata,
A.L.M.L.: Drying of pulps of tropical fruits in spouted bed: Effect of composition on dryer
performance. Dry. Technol. 20, 855–881 (2002). https://doi.org/10.1081/DRT-120003767
Moraes Filho, F.C.: Evaluation of the use of models for pastes and suspensions drying in spouted
bed with continuous feeding. Master’s dissertation in Research and Development in Regional
Technologies, Federal University of the Rio Grande do Norte (2013). https://repositorio.ufrn.br/
jspui/handle/123456789/15843. (In Portuguese)
Moraes, F.P., Gonçalves, A.C., Veríssimo Miguel, T.B., Borges, K.C., Correia, R.T.P.: Freeze Dried
Acerola (Malpighia emarginata) Pulp and Pomace: Physicochemical Attributes, Phytochemical
Content and Stability during Storage. J. Food. Ind. 1, 17 (2017). https://doi.org/10.5296/jfi.v1i1.
11795
Moreira da Silva, C.A., Ferreira, M.C., Freire, F.B., Freire, J.T.: Analysis of the dynamics of paste
drying in a spouted bed. Dry. Technol. 37, 876–884 (2019). https://doi.org/10.1080/07373937.
2018.1471699
Moura, S.C.S.R., Vissotto, F.Z., Ruffi, C.R.G., Alves Júnior, P.: Physical and rheological properties
of fruit products. Brazilian J. Food. Technol. 19, e2015086 (2016). https://doi.org/10.1590/1981-
6723.8615. (In Portuguese)
Nascimento, L.D., Corumbá, L.G., Rocha, S.C.S., Taranto, O.P., Costa, C.M.L., Faria, L.J.G.:
Fluid-dynamics evaluation in a conical spouted bed and characterization of foxtail millet seeds.
Particuology 23, 75–81 (2015). https://doi.org/10.1016/j.partic.2015.01.009
Nascimento, R.A., Andrade, E.L., Santana, E.B., Paixão Ribeiro, N.F., Costa, C.M.L., Faria, L.J.G.:
Bacaba powder produced in spouted bed: An alternative source of bioactive compounds and
energy food product. Brazilian J. Food. Technol. 22, 1–15 (2019). https://doi.org/10.1590/1981-
6723.22918
Niksiar, A., Nasernejad, B.: Activated carbon preparation from pistachio shell pyrolysis and gasifi-
cation in a spouted bed reactor. Biomass Bioenergy 106, 43–50 (2017). https://doi.org/10.1016/
j.biombioe.2017.08.017
Niksiar, A., Sohrabi, M., Rahimi, A.: A model for the dynamics of spouted bed dryers. Dry. Technol.
31, 295–307 (2013). https://doi.org/10.1080/07373937.2012.729768
Nóbrega, E.M., Oliveira, E.L., Genovese, M.I., Correia, R.T.P.: The impact of hot air drying on
the physical-chemical characteristics, bioactive compounds and antioxidant activity of acerola
(Malphigia emarginata) residue. J. Food Process. Preserv. 39, 131–141 (2015). https://doi.org/
10.1111/jfpp.12213
Nwokocha, L.M., Williams, P.A.: New starches: Physicochemical properties of sweetsop (Annona
squamosa) and soursop (Anonna muricata) starches. Carbohydr. Polym. 78, 462–468 (2009).
https://doi.org/10.1016/j.carbpol.2009.05.003
Oliveira, E.N.A., Santos, D.C., Santos, Y.M.G., Oliveira, F.A.A.: Agroindustrial use of graviola
(Annona muricata L.) for the production of liqueurs: sensory evaluation. J. Biotechnol. Biodivers.
7, 281–290 (2019). https://doi.org/10.20873/jbb.uft.cemaf.v7n2.alvesoliveira. (In Portuguese)
Oliveira, S.M., Brandão, T.R.S., Silva, C.L.M.: Influence of drying processes and pretreatments on
nutritional and bioactive characteristics of dried vegetables: a review. Food. Eng. Rev. 8, 134–163
(2016). https://doi.org/10.1007/s12393-015-9124-0
Pablos, A., Aguado, R., Tellabide, M., Altzibar, H., Freire, F.B., Bilbao, J., Olazar, M.: A new
fountain confinement device for fluidizing fine and ultrafine sands in conical spouted beds. Powder
Technol. 328, 38–46 (2018). https://doi.org/10.1016/j.powtec.2017.12.090
Pai, B.M.: Anti-microbial efficacy of soursop leaf extract (Annona muricata) on oral pathogens: an
in-vitro study. J. Clin. Diag. Res. 10, ZC01–ZC04 (2016). https://doi.org/10.7860/JCDR/2016/
18329.8762
Pallai, E., Szentmarjay, T., Mujumdar, A.S.: Spouted bed dryer. In: Mujumdar, A.S. (ed.) Handbook
of Industrial Drying, 3rd edn, pp. 389–410. CRC Press, Boca Raton (2007)
Passos, M.L., Massarani, G., Freire, J.T., Mujumdar, A.S.: Drying of pastes in spouted beds of
inert particles: design criteria and modeling. Dry. Technol. 15, 605–624 (1997). https://doi.org/
10.1080/07373939708917249
Passos, M.L., Trindade, A.L.G., d’Angelo, J.V.H., Cardoso, M.: Drying of black liquor in spouted
bed of inert particles. Dry. Technol. 22, 1041–1067 (2004). https://doi.org/10.1081/DRT-120
038579
Patras, A., Brunton, N.P., O’Donnell, C., Tiwari, B.K.: Effect of thermal processing on anthocyanin
stability in foods; mechanisms and kinetics of degradation. Trends Food Sci. Technol. 21, 3–11
(2010). https://doi.org/10.1016/j.tifs.2009.07.004
Prata, D.M., Schwaab, M., Lima, E.L., Pinto, J.C.: Nonlinear dynamic data reconciliation and param-
eter estimation through particle swarm optimization: application for an industrial polypropylene
reactor. Chem. Eng. Sci. 64, 3953–3967 (2009). https://doi.org/10.1016/j.ces.2009.05.028
Pullar, J.M., Carr, A.C., Vissers, M.C.M.: The roles of vitamin C in skin health. Nutrients 9: e866
(2017). https://doi.org/10.3390/nu9080866
Quek, M.C., Chin, N.L., Yusof, Y.A.: Modelling of rheological behaviour of soursop juice concen-
trates using shear rate–temperature–concentration superposition. J. Food. Eng. 118, 380–386
(2013). https://doi.org/10.1016/j.jfoodeng.2013.04.025
Rocha, S.C.S., Souza, J.S., Alsina, O.L.S., Medeiros, M.F.D.: Drying of tropical fruit pulps: Spouted
bed process optimization as a function of pulp composition. Dry. Technol. 29, 1587–1599 (2011).
https://doi.org/10.1080/07373937.2011.585442
Rocha, S.F., Müller, T., Castro, J.V.O., Lima, H.Z., Pinto, L.A.A. Protein content maximization of
vegetable paste by incorporation of whey through the linear programming: drying and rehydration
evaluation. J. Food. Sci. Technol. 55, 2541–2551 (2018). https://doi.org/10.1007/s13197-018-
3174-2
Roopchand, D.E., Krueger, C.G., Moskal, K., Fridlender, B., Lila, M.A., Raskin, I.: Food-compatible
method for the efficient extraction and stabilization of cranberry pomace polyphenols. Food Chem.
141, 3664–3669 (2013). https://doi.org/10.1016/j.foodchem.2013.06.050
Roopchand, D.E., Kuhn, P., Poulev, A., Oren, A., Lila, M.A., Fridlender, B., Raskin, I.: Biochemical
analysis and in vivo hypoglycemic activity of a grape polyphenol-soybean flour complex. J. Agric.
Food Chem. 60, 8860–8865 (2012). https://doi.org/10.1021/jf300232h
Saldarriaga, J.F., Grace, J., Lim, C.J., Wang, Z., Xu, N., Atxutegi, A., Aguado, R., Olazar, M.:
Bed-to-surface heat transfer in conical spouted beds of biomass-sand mixtures. Powder Technol.
283, 447–454 (2015). https://doi.org/10.1016/j.powtec.2015.05.046
Sales, M.L.F., Cavalcante, L.A., Silva, O.C., Aum, Y.K.P.G.: Evaluation of the influence of the
operational conditions of spouting bed drying on the maintenance of the phenolic components of
cubiu. In: Andrade, D.F. (ed.) Processos Químicos e Biotecnológicos, vol. 1, 1st edn, pp. 13–19.
Belo Horizonte, Editora Poisson (2019). (In Portuguese)
Santos, K.G., Francisquetti, M.C.C., Malagoni, R.A., Barrozo, M.A.S.: Fluid dynamic behavior in
a spouted bed with binary mixtures differing in size. Dry. Technol. 33, 1746–1757 (2015). https://
doi.org/10.1080/07373937.2015.1036284
Santos, P.H.S., Silva, M.A.: Retention of Vitamin C in drying processes of fruits and vegetables—a
review. Dry. Technol. 26, 1421–1437 (2008). https://doi.org/10.1080/07373930802458911
Sauceda, A.E.Q., Sayago-Ayerdi, S.G., Ayala-Zavala, J.F., Wall-Medrano, A., de la Rosa, L.A.,
González-Aguilar, G.A., Álvarez-Parrilla, E.: Biological Actions of Phenolic Compounds. In:
Yahia, E.M. (ed.) Fruit and Vegetable Phytochemicals: Chemistry and Human Health, 2nd edn,
pp. 125–138. Wiley, Hoboken, USA (2018)
Siriamornpun, S., Kaisoon, O., Meeso, N.: Changes in colour, antioxidant activities and carotenoids
(lycopene, β-carotene, lutein) of marigold flower (Tagetes erecta L.) resulting from different
drying processes. J. Funct. Foods. 4, 757–766 (2012). https://doi.org/10.1016/j.jff.2012.05.002
Sousa, R.C., Ferreira, M.C., Altzibar, H., Freire, F.B., Freire, J.T. Drying of pasty and granular
materials in mechanically and conventional spouted beds. Particuology 42, 176–183 (2019).
https://doi.org/10.1016/j.partic.2018.01.006
Souza, C.R.F., Donida, M.W., Rocha, S.C.S., Oliveira, W.P.: The role of colloidal silicon dioxide in
the enhancement of the drying of herbal preparations in suspended state. Chem. Eng. Commun.
196, 391–405 (2009). https://doi.org/10.1080/00986440802359543
Souza, C.R.F., Oliveira, W.P.: Drying of phytochemical preparations in a spouted bed: perspectives
and challenges. Dry. Technol. 30, 1209–1226 (2012). https://doi.org/10.1080/07373937.2012.
692746
Souza da Silva, E., Rupert Brandão, S. C., Lopes da Silva, A., Fernandes da Silva, J.H., Duarte
Coêlho, A.C., Azoubel, P.M.: Ultrasound-assisted vacuum drying of nectarine. J. Food. Eng. 246,
119–124 (2019. https://doi.org/10.1016/j.jfoodeng.2018.11.013
Souza, J.S.: Drying of tropical fruit pulp mixture in spouted bed. Doctoral Thesis in Research and
Development in Regional Technologies, Federal University of the Rio Grande do Norte (2009).
https://repositorio.ufrn.br/jspui/handle/123456789/15892. (In Portuguese)
Souza Júnior, F.E.: Drying of process acerola waste in spouted bed: Study of fluid dynamics and
analyze of performance of the dryer. Master’s dissertation in Research and Development in
Regional Technologies, Federal University of the Rio Grande do Norte (2012). https://reposi
torio.ufrn.br/jspui/handle/123456789/15831. (In Portuguese)
Tontul, I., Eroğlu, E., Topuz, A.: Convective and refractance window drying of cornelian cherry
pulp: effect on physicochemical properties. J. Food Process. Eng. 41, 1–8 (2018). https://doi.org/
10.1111/jfpe.12917
Van de Velde, F., Esposito, D., Grace, M.H., Pirovani, M.E., Lila, M.A.: Anti-inflammatory and
wound healing properties of polyphenolic extracts from strawberry and blackberry fruits. Food
Res. Int. 121, 453–462 (2019). https://doi.org/10.1016/j.foodres.2018.11.059
Vega-Gálvez, A., Ah-Hen, K., Chacana, M., Vergara, J., Martínez-Monzó, J., García-Segovia, P.,
Lemus-Mondaca, R., Di Scala, K.: Effect of temperature and air velocity on drying kinetics,
antioxidant capacity, total phenolic content, colour, texture and microstructure of apple (var.
Granny Smith) slices. Food Chem. 132, 51–59 (2012). https://doi.org/10.1016/j.foodchem.2011.
10.029
Vidović, S.S., Vladić, J.Z., Vaštag, Ž.G., Zeković, Z.P., Popović, L.M.: Maltodextrin as a carrier
of health benefit compounds in Satureja montana dry powder extract obtained by spray drying
technique. Powder Technol. 258, 209–215 (2014). https://doi.org/10.1016/j.powtec.2014.03.038
Vieira, M.G.A., Donida, M.W., Rocha, S.C.S.: Adhesion of an aqueous polymeric suspension to
inert particles in a spouted bed. Dry. Technol. 22, 1069–1085 (2004). https://doi.org/10.1081/
DRT-120038580
Wang, L.S., Hecht, S.S., Carmella, S.G., Yu, N., Larue, B., Henry, C., McIntyre, C., Rocha, C.,
Lechner, J.F., Stoner, G.D.: Anthocyanins in black raspberries prevent esophageal tumors in rats.
Cancer Prev. Res. 2, 84–93 (2009). https://doi.org/10.1158/1940-6207.CAPR-08-0155
Willett, W., Rockström, J., Loken, B., Springmann, M., Lang, T., Vermeulen, S., Garnett, T., Tilman,
D., DeClerck, F., Wood, A., Jonell, M., Clark, M., Gordon, L.J., Fanzo, J., Hawkes, C., Zurayk,
R., Rivera, J.A., De Vries, W., Sibanda, L.M., Afshin, A., Chaudhary, A., Herrero, M., Agustina,
R., Branca, F., Lartey, A., Fan, S., Crona, B., Fox, E., Bignet, V., Troell, M., Lindahl, T., Singh, S.,
Cornell, S.E., Srinath Reddy, K., Narain, S., Nishtar, S., Murray, C.J.L.: Food in the anthropocene:
the EAT–lancet commission on healthy diets from sustainable food systems. Lancet 393, 447–492
(2019). https://doi.org/10.1016/S0140-6736(18)31788-4
Zhang, L., Liao, L., Qiao, Y., Wang, C., Shi, D., An, K., Hu, J.: Effects of ultrahigh pressure and
ultrasound pretreatments on properties of strawberry chips prepared by vacuum-freeze drying.
Food Chem. 303, 125386 (2020). https://doi.org/10.1016/j.foodchem.2019.125386
Zhang, L., Zeng, X., Fu, N., Tang, X., Sun, Y., Lin, L.: Maltodextrin: a consummate carrier for
spray-drying of xylooligosaccharides. Food Res. Int. 106, 383–393 (2018). https://doi.org/10.
1016/j.foodres.2018.01.004
Chapter 6
Osmo-convective Dehydration of Fresh
Foods: Theory and Applications
to Cassava Cubes
T. R. Bezerra Pessoa, A. G. Barbosa de Lima, P. C. Martins, V. C. Pereira,

T. C. O. Alves, E. S. da Silva, and E. S. de Lima
Abstract This chapter focuses on the hybrid process of osmotic dehydration and
convective air drying of foods. Emphasis has been done to cassava cubes (Manihot
esculenta Crantz.). The fresh cassava cubes had a water activity content of about
0.954, 60.45% moisture on a wet basis, 2.27% sucrose, and 0.13% sodium chloride on
a wet basis. Herein, the kinetics of osmotic dehydration of cassava cubes were studied
under an optimized operating condition of the convective drying kinetics of fresh
and osmotically dehydrated cassava cubes which were evaluated at different drying
conditions. Under mathematical point of view, different lumped approaches are used
to estimation of average effective mass diffusivities (moisture and solids). Transient
results of moisture loss, solids gain, sodium chloride, and sucrose incorporation, and
moisture content are presented, compared with experimental data, and discussed.
T. R. Bezerra Pessoa (B) · P. C. Martins · V. C. Pereira · T. C. O. Alves

Department of Food Engineering, Federal University of Paraiba, João Pessoa, PB 58051-900,
Brazil
e-mail: thayzepessoa1@yahoo.com
P. C. Martins
e-mail: pierre@ct.ufpb.br
V. C. Pereira
e-mail: vitor_ufpb@hotmail.com
T. C. O. Alves
e-mail: thalitaaoliveira@gmail.com
A. G. B. de Lima · E. S. de Lima
Veloso, 882, Bodocongó, Campina Grande, PB 58429-900, Brazil
E. S. de Lima
e-mail: limaelisianelima@hotmail.com
E. S. da Silva
Department of Civil and Environmental Engineering, Federal University of Paraíba, João Pessoa,
PB 58051-900, Brazil
e-mail: elsonsaneamento33@gmail.com
https://doi.org/10.1007/978-3-030-47856-8_6
152 T.R. Bezerra Pessoa et al.
The hybrid process has generated a dry product with 11% moisture, 16.89% sucrose,
and 5.94% sodium chloride on a dry basis at better operation conditions. The product
obtained from the cassava cubes hybrid process can be used in the food production
at cassava base.
Keywords Osmotic dehydration · Cassava · Drying · Hybrid drying process
6.1 Introduction
6.1.1 Drying Fundamentals
Water is a major constituent of fresh food. It is intimately related to most of the

physicochemical changes taking place in food. This constituent is vital in maintaining
the quality and extending the shelf life of the food materials (Li et al. 1998). Since
water activity is the thermodynamic measure of chemical potential, it can be used
to determine the state of water in a solution or in a solid (Lewicki 2004). The water
content is considered one of the most critical quality parameters, which influences
the microbial growth and sensory attributes (texture, appearance, and flavor) of fresh
foods (Hills et al. 1990). In this context, reduction in water content improves food
materials stability and extends their shelf life. Drying is one of the most frequently
used preservation methods of fresh foods, particularly vegetables, fruits, and meats
that contain high water concentration. Drying provokes increases in the concentration
of solids in food by removing water either by evaporation or sublimation (Kudra 2004;
Koyuncu et al. 2007). Different drying methods have been applied in the industry
to remove water from foods, such as spray drying, fluidized bed drying, foam-mat
drying, microwave drying, osmotic dehydration convective drying, etc. The drying
kinetics measurement and modeling can provide better insights into physical and
chemical processes that take place when food materials undergo drying. Such insights
provide reliable determination of drying time, help meet quality specifications, and
lead to better energy conservation (Feng et al. 2014).
Osmotic dehydration produces foods with an intermediate moisture content,
whose shelf life is relatively short, and it can improve sensory characteristics (color,
taste, texture, and others) of them; this drying technique has been used for many
researches (Assis et al. 2018; Pessoa et al. 2017; Mierzwa and Kowalski 2016; Corrêa
et al. 2017; Kumar et al. 2017). Convective drying is a very simple water removal oper-
ation applied to wet porous solids that has better moisture removal results and prod-
ucts with longer storage and consumption times under ambient conditions (Mercali
et al. 2010; Isquierdo et al. 2013; Yadav and Singh 2014).
Hybrid drying technologies are being developed to better preserve the natural
food quality, better control of the residual moisture content, and to enhance drying
efficiency (Feng et al. 2014). Despite the importance of the single drying process, the
hybrid process plays an important role in this area. The use of combined processes
aims to use the advantages of each technique of a particular preservation method
6 Osmo-convective Dehydration of Fresh … 153
transformation of raw materials into differentiated products that can improve their
use in formulations and consumption. Thus, osmotic dehydration associated with
convective drying of fresh foods represents a combined process of moisture reduc-
tion techniques that can provide products with better color and texture stability and
longer shelf life. This new product should exhibit differentiated sensory character-
istics from only convection dried material due to incorporation or solute loss during
osmotic dehydration and increased storage time (24–48 months) at ambient condi-
tions promoted by convective drying, which may increase its acceptance and expand
its commerce and consumer market (Castro et al. 2018; Pessoa et al. 2011).
6.1.2 The Focus of This Work
Brazil is one of the world’s largest cassava producers (Manihot esculenta Crantz),
occupying the third position in the world ranking (Chicherchio 2014). This vegetable
is a shrub, perennial plant, from Euforbiaceas family and dicots class. It has tuberous
roots, which has high starch content in its composition. It is the only species of its
genus commercially cultivated, aiming at the production of tuberous roots rich in
starch (Fialho and Vieira 2011). There are several products that can be obtained from
the cassava root. In the human food, it is consumed cooked, fried, and in other forms
(Chicherchio 2014).
6.2 Application: Hybrid Drying of Cassava Cubes
6.2.1 The Raw Material
6.2.1.1 Samples Preparation
Experimental tests were performed with cassava (Manihot esculenta Crantz)

purchased from local commerce in João Pessoa, Paraíba state, Brazil. The cassava
was peeled by hand until the peel was completely removed and the root was cut with
a 2.5 × 2.5 × 2.5 cm3 cube slicer. For osmotic dehydration, solutions were prepared
with 56% w/w solute, 46% w/w sucrose, and 10% w/w sodium chloride. Concentra-
tions of the solutions were verified through a benchtop refractometer. The previously
weighed cassava cubes were placed in screw-capped 250 mL glass jars along with
the osmotic solution. The material: solution ratio of 1:15 was used to ensure that the
solution concentration remained constant throughout the process. Vials containing
the samples were brought to a refrigerated digital shaker bench incubator (model
LS4900-TZH, Alpax, Brazil) for 190 min at 52 °C and 180 rpm. Figure 6.1 shows
the raw material and devices used in the experiments.
Fig. 6.1 Fresh material, aluminum cutter, and incubator
6.2.1.2 Samples Physical and Chemical Characterization
The characterization experiments (moisture content, water activity, sodium chloride

content, and non-reducing sucrose sugars) of the cassava cubes in natura and dehy-
drated osmotically were performed in triplicate. Moisture content was determined by
the gravimetric method using heat, which is based on the weight loss of the material
when heated to 70 °C in a vacuum oven until it reaches constant weight, according
to the AOAC methodology (AOAC 1995). For water activity, the LabMaster equip-
ment (NOVASINA, Switzerland) was used at 25 °C. Sodium chloride content was
obtained by the Mohr method, based on titration with silver nitrate, using potassium
chromate as an indicator (Jeffery et al. 1989). Non-reducing sucrose sugars were
determined by the Lane-Eynon method, consisting of the complete reduction of the
cupric ions of Fehling’s reagent reducing to cuprous ions under the action of heat in
alkaline medium (Lane and Eynon 1923).
6.2.2 Osmotic Dehydration Tests
6.2.2.1 Experimental Procedure
The samples were taken from the incubator at 15, 30, 45, 60, 75, 90, 110, 130, 150,
180, 240, 300, 360, 420, and 480 min that correspond to 8 h of operation. In the test
was observed the behavior of the mass transfer process between the solid and the
solution. After removal, they were drained on stainless steel mesh to remove excess
dehydrating solution and weighed. Thereafter, triplicate determinations of moisture
content, sucrose, and sodium chloride were performed. The osmotic dehydration
kinetics were studied by monitoring moisture loss (PU), solids gain (GS), and incor-
porations of sodium chloride (INaCl) and sucrose (ISac). Figure 6.2 illustrates the
samples before osmotic dehydration process.
Fig. 6.2 Fresh material and fresh cassava cubes inside osmotic solutions
6.2.2.2 Theoretical Procedure
The osmotic dehydration kinetics was theoretically studied using the Azuara’s model
(1992). The authors developed an empirical model based on a mass balance that can
be used for different geometries (without geometric constraint) including cube. The
processes can be performed at short time intervals, as the model does not require
that the equilibrium point has actually reached for the mass transport parameter
prediction. Starting from a mass balance in the material that undergoes dehydration,
the following equations are obtained for moisture loss, total solids gain, and sodium
chloride and sucrose incorporations:
S1 t(ML∞ ) t(ML∞ )
MLt = = 1 (6.1)
1 + S1 t S1
+t
S2 t(SG∞ ) t(SG∞ )
SGt = = 1 (6.2)
1 + S2 t S2
+t
S3 t(NaCl∞ ) t(NaCl∞ )
NaClt = = 1 (6.3)
1 + S3 t S3
+t
S4 t(Suc∞ ) t(Suc∞ )
Suct = = 1 (6.4)
1 + S4 t S4
+t
where MLt is the moisture loss fraction at any time; SGt is the solid gain fraction
at any time; NaClt is the sodium chloride incorporation at any time; Suct is the
sucrose incorporation any time; ML∞ is the moisture loss fraction at equilibrium
condition; SG∞ is the solid gain fraction at equilibrium condition; NaCl∞ is the
sodium chloride incorporation fraction at equilibrium condition; Suc∞ is the sucrose
incorporation fraction at equilibrium condition; S1 is a constant related to the water
diffusion rate out from product; S2 is a constant related to the rate of solids diffusion
in the product; S3 is a constant related to the rate of sodium chloride incorporation
in the product; and S4 is a constant related to the rate of sucrose incorporation in the
product. Rewriting Eqs. 6.1, 6.2, 6.3, and 6.4, in the linear form we obtain
t 1 t
= + (6.5)
MLt S1 ML∞ ML∞
t 1 t
= + (6.6)
SGt S2 SG∞ SG∞
t 1 t
= + (6.7)
NaClt S3 NaCl∞ NaCl∞
t 1 t
= + (6.8)
Suct S4 Suc∞ Suc∞
Crank (1975) obtained a simplified equation for the Fick’s physics–mathematical

model, considering a small process time, transient regime, diffusion in a semi-infinite
medium, constant osmotic solution concentration, and external resistance to mass
transfer negligible. This model is represented by the following equations:

MLt DeffML t 1/2
=2 (6.9)
ML∞ π L2

SGt DeffSG t 1/2
=2 (6.10)
SG∞ π L2

NaClt DeffNaCl t 1/2
=2 (6.11)
NaCl∞ π L2

Suct DeffSuc t 1/2
=2 (6.12)
Suc∞ π L2
where DeffML is the effective moisture loss diffusivity; DeffSG is the effective solids
gain diffusivity; DeffNaCl is the effective sodium chloride incorporation diffusivity;
DeffSuc is the effective sucrose incorporation diffusivity, and L is the characteristic
dimension.
Replacing Eqs. 6.9, 6.10, 6.11, and 6.12 in the Eqs. 6.5, 6.6, 6.7, and 6.8, respec-
tively, four simple expressions are obtained to calculate the effective diffusivity of
moisture loss, solids gain, sodium chloride incorporation, and sucrose incorporation
at different times, as follows:
mod 2
πt S1 L
ML∞
DeffML = · exp (6.13)
t 4 1 + SML t
ML∞
2
πt S2 L SG∞mod
DeffSG t = · exp (6.14)
4 1 + SSG t SG∞
2
πt NaCl∞mod
S3 L
DeffNaCl = · exp (6.15)
t 4 1 + SNaCl t
NaCl∞
2
πt S4 L Suc∞mod
DeffSuc t = · exp (6.16)
4 1 + SSuc t Suc∞
where ML∞mod is the moisture loss value at equilibrium condition obtained by Eq. 6.1;
SGmod mod
∞ is the solids gain value at equilibrium condition obtained by Eq. 6.2; NaCl∞
is the sodium chloride incorporation value at equilibrium condition obtained by
Eq. 6.3; Sucmod
∞ is the sucrose incorporation value at equilibrium condition obtained
exp
by Eq. 6.4; ML∞ is the moisture loss value at equilibrium condition obtained experi-
exp
mentally; SG∞ is the solids gain value at equilibrium condition obtained experimen-
exp
tally; NaCl∞ is the sodium chloride incorporation value at equilibrium condition
exp
obtained experimentally, and Suc∞ is the sucrose incorporation value at equilibrium
condition obtained experimentally.
Applying Eqs. 6.9, 6.10, 6.11, and 6.12 for a cubic geometry, considering the
characteristic dimension L as the edge of the cube, and replacing them in Eqs. 6.1,
6.2, 6.3, and 6.4, respectively, we obtain the following equations:
mod 3
2
π S1 L 3 ML∞
DeffML = · exp (6.17)
4t 3
1
1 + S1 t ML∞
mod 3
2
π S2 L 3 SG∞
DeffSG = · exp (6.18)
4t 3
1
1 + S2 t SG∞
mod 3
2
π S3 L 3 NaCl∞
DeffNaCl = · exp (6.19)
4t 3
1
1 + S3 t NaCl∞
mod 3
2
π S4 L 3 Suc∞
DeffSuc = · exp (6.20)
4t 3
1
1 + S4 t Suc∞
Thus, the general average effective diffusivity obtained from the transport of
materials (water outflow, total solids input, sodium chloride, and sucrose) during of
cassava cube can be calculated by using Eq. 6.21, as follows:

N
(Deff )i
i=1
Deff = (6.21)
N
where Deff is the average effective diffusivity in time; Deff is the effective diffusivities
for each time and N is the number of data used.
The mean relative error (E) was calculated using Eq. 6.22 to evaluate whether the
model was or not predictive (E < 10%).
100
Vexp − Vpre
E= (6.22)
N i=1
Vexp
where Vexp is the experimental value, Vpre is the predicted value, and N is the number
of experimental points.
6.2.3 Convective Drying Tests
6.2.3.1 Experimental Procedure
Drying tests were performed at different temperatures with fresh cassava cubes
osmotically dehydrated. The process was carried out in a convective fixed bed dryer
with perpendicular air flow. Figure 6.3 shows the convective drying equipment.
The drying air temperatures chosen were 50, 60, and 70 °C using constant velocity
(1.35 m/s) and absolute humidity (0.060 kg water/kg solid) conditions of the drying
air. Prior screening of the air velocity profile was performed using a hot wire
anemometer (model AK833, China) and the temperature and relative humidity in
the drying chamber using a portable thermo-hygrometer with probe (model AK625,
brand AKSO). Figure 6.4 illustrates these devices.
Convective drying kinetics was obtained by experimental measurements of the
mass of the cassava cubes as a function of the drying time, with 60 min intervals until
Fig. 6.3 Convective dryer

used in the experiments
Fig. 6.4 Anemometer and

thermo-hygrometer
the final drying period. Drying air conditions were monitored during the experiments
and the tests were performed in triplicate.
The drying analysis was performed through the experimental curves of the mois-
ture content as a function of the time and the drying rate as a function of the mois-
ture content. Drying curves were expressed with moisture content on a dry basis,
according to literature (Moyers et al. 1999).
The average final moisture content data of the cassava cubes (fresh dried and
osmotically dehydrated) at three drying air temperatures were subjected to variance
analysis at a significance level of 5% and Tukey test mean comparison by using
STATISTICA® software (STATSOFT 1997).
According to Montgomery (Montgomery 2008), variance analysis, also known as
ANOVA, is an approach used to compare various interest groups. It seeks to assess
if there are considerable differences between the investigated groups.
The Tukey test is based on an amplitude distribution of the T function. It is used to
calculate the minimum significant difference and comparing it with the means differ-
ence obtained for each treatment, assuming a statistical significance level (Nogueira
2007).
6.2.3.2 Transport Parameter Estimation
The average effective moisture diffusivity of cassava cubes exposed to convective

drying was obtained through the Fick’s model simplified by Crank (1975), consid-
ering uniform initial moisture distribution, absence of thermal effect in mass transfer,
and applied to an infinite flat plate and long drying times. For a cube, all sides were
considered of equal dimension; thus, the solution of the Fick’s model applied to a
cube will be given as follows:
3
M − Me 8 π 2 Defft L sample
= exp − ∴ L= (6.23)
M0 − Me π2 (2L)2 2
where Defft represent the effective diffusivity, M is the average moisture content, Me
is the equilibrium moisture content, M0 is the initial moisture content, t is the time, L
corresponds to the characteristic length (half the thickness on each side of the cube).
6.2.4 Results and Analysis
6.2.4.1 Physicochemical Characterization of Cassava
The physicochemical characterization of Manihot esculenta crants in natura was

carried out according to the referenced methods in Sect. 2.1.2. Table 6.1 presents the
results obtained.
The cassava roots consist basically of water and sucrose, according to results in
Table 6.1. The chemical composition of this material consisted of 60.45% moisture,
2.27% sucrose, and 0.13% sodium chloride. The water activity value found in the
cassava root is above the minimum water activity values for the development of
pathogenic microorganisms; thus, this raw material is not microbiologically stable
(Chirife and Favetto 1992).
Luna et al. (2013) presented results for the moisture (35.31%) of raw cassava roots
well different from those obtained in this work. These differences may be related to
variations in soil moisture. Maieves (2010) evaluated the moisture content of cassava
tubers at various harvest times and concluded that the roots collected in February
showed higher moisture than those collected in the month of May. He says that roots
grown in sandy soils have an average moisture of 60% (wet basis).
The values of non-reducing sugars in sucrose obtained in this research differ from
those found by Aguiar et al. (2014), which obtained higher values, about 3.94% in
the root of the frozen Mandiocaba variety. Differences in sugar content vary with the

Analysis Fresh cassava cubes average valuesa
characterization of the fresh
cassava cubes Water activity 0.954 ± 0.00
Moisture (w.b. %)b 60.45 ± 0.03
Sucrose (%) 2.27 ± 0.19
Sodium chloride (%) 0.13 ± 0.02
a Mean value ± standard deviation
b Wet basis
Fig. 6.5 Moisture loss and

total solids gain kinetics in
the osmotic dehydration of
cassava cubes in ternary
solution
harvest period. Couto (2013) observed that there was a decrease in the total sugar
content in cassava roots harvested later. The plant’s development cycle consists of five
physiological phases and in the first phase it needs more energy, producing a higher
sugar concentration. Rinaldi et al. (2015) studied the effect of different freezing forms
on cassava roots and concluded that the use of this conservation process causes less
changes in the structure of the raw material, prolonging the conservation of its initial
nutritional characteristics.
Valduga et al. (2011) found significant differences in the sodium levels of five
cassava cultivars (BRS Rosada, Casca Roxa, BRS Dourada, BRS Egg Yolk, and
Saracura) harvested at 8 months after planting. The cultivar Casca Roxa showed a
significant content of sodium chloride 0.19% (dry basis); this value was close to
what was obtained in this work (0.13%). The authors concluded that the chemical
composition of cassava is specific not only for each cultivar, but also depends, mainly,
on associated genetic factors.
6.2.4.2 Osmotic Dehydration Process
Drying Kinetics in the Optimal Condition
After different experimental tests of osmotic dehydration of cassava cubes were

chosen the best drying condition for the study. Optimum conditions obtained in
ternary solution of sucrose, sodium chloride, and water were 52 °C, 56% w/w solute,
10% w/w sodium chloride, 190 min and 180 rpm. The kinetic parameters result from
the osmotic dehydration of cassava cubes are presented through the moisture loss
curves and solids gains shown in Fig. 6.5.
From the analysis of Fig. 6.5, in the early stages of operation (first 15 min) the
highest gradients of moisture loss and solids gain occurred. After this period, the
solids gain almost reached equilibrium after 30 min of operation. Moisture loss
continued to increase until reaching a maximum value of 24.89% and stabilized
after 180 min of operation. An unexpected event occurred after 360 min of osmotic
dehydration of the cassava cubes. There was a small decline in moisture loss and a
sudden increase in the solids gain of samples, whose parameters were re-established
in values equal to 22.7 and 16.45% for moisture loss and solids gain, respectively.
The solids gain stabilized before the moisture loss probably due to lower internal
mass transfer resistance of the solutes (sucrose and salt) as compared to moisture.
The behavior of the mass transfer rates of moisture and solutes between the cassava
cubes and the hypertonic osmotic solution may be associated with the chemical and
physical characteristics of these solutes. Junqueira et al. (2017) have reported that
high molecular weight solutes such as sucrose are responsible for increasing moisture
loss in the dehydrated product and promote low solids gain. The sucrose promotes
an increase in the viscosity of the osmotic solution, which may lead to the formation
of a barrier on the vegetable surface, limiting its impregnation in the product (Pereira
et al. 2006). However, low molecular weight solutes provide a higher solid gain when
compared to high molecular weight solutes because they are able to penetrate into
the food cell, increasing their concentration in the product (Junqueira et al. 2017;
Pereira et al. 2006; Ruiz-López et al. 2011; Sritongtae et al. 2011). Considering the
above reports, sucrose was probably responsible for the greater moisture loss, and
sodium chloride by the solids gain in the dehydration process of cassava cubes in
ternary solutions.
High moisture loss and solids gain rates in the early hours of the osmotic dehy-
dration process of guava were reported by Castro et al. (2018). Similar results were
found by Silva et al. (2012), when studying the osmotic dehydration of acerola.
According to Ramya et al. (2014), the early stages of osmotic dehydration play an
important role because the transport phenomena are faster, causing greater impact
on the process progress.
Results of moisture loss and solids gain similar to those found in this research
were found by Alam et al. (2013) when using binary solution of sodium chloride and
water. They found a final value of 28.42% of moisture loss and 11.24% for the solids
gain in osmotic dehydration of onion under the conditions 25 °C, 6 h of process
and concentration salt of 25 °Brix in the solution. However, when using a ternary
solution with 55 °Brix sucrose and 15 °Brix of salt, under these same conditions
of temperature and time, the moisture loss increased to 48.08% and the solids gain
increased slightly to 13.53%. According to these authors, an increase in moisture
loss and solids gain occurs as the concentration of the solution increases.
Figure 6.6 shows the diffusion profile over time of sucrose and sodium chlo-
ride incorporations for osmotic dehydration of cassava cubes in ternary solution of
sucrose, sodium chloride, and water.
The analysis of the results shown in Fig. 6.6 indicated that the kinetics of sucrose
and sodium chloride incorporation presented the same behavior. Sucrose and salt
gain occurred more intensely in the first 15 min of the process when it had already
incorporated approximately 3% and 1%, respectively. Then, we noticed a slower
gain of these two response variables in a time interval of up to 180 min. From 180
to 300 min of process, there was again an increase in sucrose and sodium chloride
incorporations, rising to 6% and 3%, respectively. At 300 min, stability in mass
transfer rates was observed for all incorporations. At the end of the experiment, the
incorporations were approximately 9% for sucrose and 4% for sodium chloride.
Fig. 6.6 a Sucrose and b Sodium chloride incorporations kinetics in the osmotic dehydration of
cassava cubes in ternary solution
In the study of osmotic dehydration kinetics of cassava slices in ternary solution,

Carmo et al. (2017) found that in the early hours of the process, the presence of a
high concentration of sugars provided a rapid mass transfer, leading to greater gain
of soluble solids. The sugars balance condition was reached from 200 min with a
final value of 10%.
Similar results were found by Aires et al. (2016) and Castro et al. (2014) for
guava osmotic dehydration, and by Borsato et al. (2010) for apple osmotic dehydra-
tion. Araújo et al. (2014) studying the process of osmotic dehydration of carrots in
temperature of 50 °C, 240 min and solution concentration of 50 °Brix, found solids
incorporation values using sucrose solution, similar to this research, of 22.13%.
However, Hadipernata and Ogawa (2016) studying potato osmotic dehydration at
20 °C in 8 h with 20% solution concentration, obtained in their research a smaller
sucrose gain of 1.75%, only.
Mercali (2009), when studying mass transfer kinetics in banana fruit, reported a
high rate of sodium chloride incorporation at the beginning of the dehydration process
followed by lower rates in the final stages of the process. Vázquez-Vila et al. (2009)
also observed that solids gain using sodium chloride solution at 17.22 and 26% w/w at
25.35 and 45 °C increased at the beginning of the carrot osmotic dehydration process.
Silva Júnior et al. (2015) observing that the incorporation of solids in dehydrated
green beans with sodium chloride solution increased at the beginning of the process.
Further, the authors found that the effective diffusivity of the solid increased with
the increase of sodium chloride concentration in the solution from 20 to 26.5%.
Regarding the stabilization time of the transfer rate of soluble solids, sucrose, and
sodium chloride, Mayor et al. (2006), similarly to the information obtained in this
research, found that the balance occurred around 5 h in pumpkin osmotic dehydration
in sodium chloride solutions between 5 and 25% w/w, at 12.25 and 38 °C with times
from 0 to 9 h. Kumar et al. (2017) found a solid incorporation content of 4.20%
by employing sodium chloride solution in osmotically dehydrated chayote cubes.
The conditions used were temperature 35 °C, process time 180 min, 10% sodium
Fig. 6.7 Osmotically

dehydrated cassava cube
chloride concentration, and 1:6 ratio between fruit and solution. Figure 6.7 illustrates
the cassava cube osmotically dehydrated on the specific condition.
Moisture and Total Solids Effective Diffusivities Estimation
The determination of the moisture and solutes mass transport parameter in the osmotic
dehydration of cassava cubes was carried out using the empirical model proposed by
Azuara et al. (1992). Initially, a linear regression related to moisture loss, solids gain,
and sucrose and sodium chloride incorporations as a function of time, represented
by t/ML, t/SG, t/NaCl, and t/Suc was performed. Figure 6.8 presents the linearized
experimental results of these parameters for the determination of parameters of the
(Eqs. 6.5–6.8).
From the analysis of the analyses of Fig. 6.8, we can see that the model used
satisfactorily represented the experimental data for the four studied variables (in these
linear regressions the correlation coefficients (R2 ) were varied from 0.943 to 0.999).
From the results of the fitted parameters, it was possible to determine diffusivities
of moisture, solids gain, sucrose, and sodium chloride for osmotic dehydration of
cassava cubes in the desired optimum condition. The values of these parameters are
presented in Table 6.2.
By analyzing Table 6.2, the Azuara et al. (1992) model presented relative mean
error (E) ranging from 3.4 to 22.2%, and determination coefficients (R2 ) close to
1.00 for all parameters indicating a good fit to the experimental data.
According to Table 6.1, the constants of sodium chloride (S3 ) and sucrose (S4 )
incorporations and the effective diffusion coefficient showed similar values, indi-
cating that these two solutes were incorporated with the same velocity into the dehy-
drated cassava cubes. This fact probably occurred due to the material structure as well
as the competition between the fluxes of the two solutes during the process. Since
the molecular weight of the salt is lower than the sucrose, it spontaneously enters the
plant cell, resulting in a reduction in the sucrose mass transfer coefficient. Further,
the total solid gain velocity constant (S2 ) was higher than the moisture loss constant
Fig. 6.8 Comparison between the experimental and theoretical (Azuara et al. 1992) results of the
moisture loss, solids gain, and sodium chloride and sucrose incorporations as a function of time
(S1 ). The absorption rate of total solids in the osmotically dehydrated cassava cubes
was about 63% higher than the water outlet velocity, resulting in the higher average
effective diffusivity of the total solids in relation to moisture effective diffusivity.
This behavior is probably related to the amount, type, and concentration of solutes
used in the osmotic solution and the operating temperature.
Comparison between the effective diffusivity data cited in the literature is a
complicated task due to the different estimation methods and various models
employed, associated with changes in the chemical composition of the food and
its physical structure. In addition, effective diffusivity varies throughout the process
and the osmotic moisture gradient is not constant (Azoubel and Da Silva 2008;
Mercali et al. 2011).
The effective diffusivities values for moisture and solids transport obtained in this
research were of the order of 10−8 m2 /s, in which the average value of these transport
parameters for osmotic dehydration of cassava cubes was 1.88 × 10−8 m2 /s. Values
from the same order of magnitude were obtained for several osmotically dehydrated
vegetables such as carrot (Sutar and Prasad 2011), mango (Arias et al. 2017) nectarine
(Rodríguez et al. 2013), and banana (Góis et al. 2010).
Table 6.2 Fitted parameters

Variables Parameters Value
of the Eqs. 6.5–6.8 in the
best-operating conditions Moisture loss T (min) 360
MLmod
∞ (%) 27.967
S1 8.265 × 10−4
R2 0.995
E (%) 8.407
Deff (m2 /s) 1.99 × 10−8
Solids gain t (min) 360
SGmod
∞ (%) 12.923
S2 22.521 × 10−4
R2 0.999
E (%) 3.389
Deff (m2 /s) 2.77 × 10−8
Sodium chloride incorporation t (min) 480
NaClmod
∞ (%) 4.489
S3 1.883 × 10−4
R2 0.966
E (%) 15.678
Deff (m2 /s) 1.36 × 10−8
Sucrose incorporation t (min) 480
Sucmod
∞ (%) 9.573
S4 1.802 × 10−4
R2 0.943
E (%) 22.224
Deff (m2 /s) 1.40 × 10−8
∞ = value of the moisture loss at equilibrium obtained by the

MLmod
∞ = value of the solids gain at equilibrium obtained by
model; SGmod
∞ = value of the sodium chloride incorporation
the model; INaClmod
at equilibrium obtained by the model; ISucmod∞ = value of the
sucrose incorporation at equilibrium obtained by the model
Arias et al. (2017) and Rodríguez et al. (2013) associated the high diffusion coef-
ficients with the temperature used in the osmotic dehydration process. Escobar et al.
(2007) explained that high values of diffusivities are due to the effect of measure-
ments that cause cell death of plant tissue before osmotic pretreatment, facilitating
mass transfer. The authors cite as an example bleaching. Maldonado et al. (2008)
justified that high diffusion coefficients are linked to high moisture loss values.
Góis et al. (2010) reported that the differences in the order of magnitude of diffu-
sivities probably derive from the type of geometry used in the material. Allali et al.
(2008) and Corzo et al. (2008) stated that the magnitude of effective moisture diffu-
sivity for food materials varies in the range of 10−8 to 10−12 m2 /s. This variation is
explained by the type of experimental analysis, composition and physiology of the
food and the method of data treatment.
Azarpazhooh and Ramaswamy (2012) observed that the effective moisture and
solid diffusivities in osmotic dehydration of apple cylinders reached maximum values
at temperatures of 50 °C and 50 °Brix solution concentration, close to the results
presented in this work for osmotic dehydration of cassava cubes. Assis et al. (2017)
found that the higher temperature (60 °C) promoted higher diffusion of water and
solute in the osmotic dehydration process of apple cubes. This behavior was also
observed by Abbasi Souraki et al. (2012) in osmotically dehydrated green beans
ranging from 30 to 50 °C.
Lower diffusivity results (order 10−9 m2 /s) were obtained by Rodríguez et al.
(2017) in plum osmotic dehydration. Assis et al. (2017) in osmotically dehydrated
apple cubes, Singh et al. (2008) for pretreated carrot cubes in sodium chloride
solution, Hamedi et al. (2018) on osmotic dehydration of ultrasound-assisted agar
gel cylinders, and Azarpazhooh and Ramaswamy (2012) analyzing osmotically
dehydrated apple cylinders.
Cassava cubes were dehydrated in ternary solution of sucrose, salt, and water
at high concentration (56% w/w) combined with high temperature (52 °C). High
temperatures increase the solubility of solutes and cause changes in plant cell struc-
ture, increasing the diffusion rate of sodium chloride and sucrose into the cassava
cube compared to water diffusion. Several authors have observed solid diffusivity
values greater than water diffusivity in osmotic dehydration of vegetables (Arias
et al. 2017; Azarpazhooh and Ramaswamy 2012; Assis et al. 2017; Hamedi et al.
2018; Zúñiga and Pedreschi 2012). Assis et al. (2017) found lower values of water
diffusivity in relation to total solids in osmotic dehydration of apple cubes in sucrose
and sorbitol solution, at temperatures ranging from 25 to 60 °C. They report that the
sucrose solution has high viscosity due to the high molecular weight of the solute,
making it difficult to transport water between the product and the solution.
Arias et al. (2017) found lower effective moisture diffusivity values in sleeves at
50 °C by increasing the sucrose solution concentration from 45 to 60 °Brix. They
explained that this behavior is due to the fact that the more dilute the solution can
penetrate better into tissues, as opposed to concentrated solutions that are more
viscous and can form a sucrose surface layer, making it difficult for water to escape
from the material. Similarly, Assis et al. (2017) found lower values of water diffusivity
compared to solids in the osmotic dehydration of apple cubes in sucrose and sorbitol
solution, at temperatures ranging from 25 to 60 °C. They proved that the type of
osmotic agent used, as well as its molecular weight, influenced the diffusion of
water, obtaining smaller diffusivities when the osmotic dehydration was performed
with sucrose solution. The authors explained that sucrose solution is more viscous
than sorbitol and that sucrose has higher molecular weight, making it difficult to
transport water between the product and the solution.
Hamedi et al. (2018) observed higher values of solid diffusivity in relation to water,
in the osmotic dehydration of an agar gel cylinder, in sucrose solution in an ultrasonic
Fig. 6.9 Dimensions of

moisture as a function of
time for drying process of in
natura and osmotically
dehydrated cassava cubes at
various process temperatures
bath (100% power). The authors explained that increasing the concentration of the
osmotic solution resulted in greater absorption of solids in the sample due to the
increased osmotic pressure gradient between the solution and the dehydrated product.
Finally, we state that migration rates of total solids and moisture content, as
shown in Fig. 6.6, and demonstrate that total solid gain reaches equilibrium more
rapidly in relation to moisture loss in cassava cubes. This indicates a greater diffi-
culty in migrating water from the solid matrix to the surrounding osmotic solution
as compared to its transfer of solutes (sucrose and salt) into the solid. Other consid-
erations, such as the higher amount of moisture in migration, the synergistic effect
of salt for the penetration of sucrose in the vegetal membrane, and others, can clarify
this difference of values between the average effective diffusivities of total solids and
humidity.
6.2.4.3 Convective Drying Process
Drying Kinetics for Cassava Cubes Dried in Natura and Osmotically

Dehydrated
Figure 6.9 shows the dimensionless moisture content as a function of time for two
different drying physical situations: dried in natura and osmotically dehydrated
cassava cubes at the various drying air temperatures.
By comparing the curves for the two sample types it is evident that the shortest
drying time was detected for the dried samples without pretreatment. The in natura
cassava cube dried at 70 °C presented the shortest drying time (≈12 h), and the
osmotically dehydrated cassava cubes at the three temperatures had equal drying
times, totaling 24 h of process, twice from the in natura sample time dried at 70 °C.
Castiglioni et al. (2013) reported that the shortest convective drying time of cassava
fibrous mass was reached at the highest temperature studied at 67 °C.
Analyzing Fig. 6.9 for drying kinetics of fresh material dried at 50 and 60 °C,
a similar trend is observed. However, by checking the drying curves separately for
the fresh sample at 50 and 70 °C and 60 and 70 °C, another type of behavior was
observed, as the temperature increased, the curve became sharper.
This, the time required to reduce the moisture content to an almost equilibrium
condition is reduced too, as stated above. On the other hand, more than 50% of the
moisture of fresh cassava cubes was removed during the first 5 h of drying at 70 °C,
and during the first 8 h for drying at 50 and 60 °C. The remaining water content
was eliminated over a comparatively longer period. This probably occurred due to
the shrinkage of the cube with the corresponding pore reduction that increased the
resistance of water transport during the drying process (Pereira et al. 2009).
Osmotically dehydrated samples took longer drying times when compared to
fresh samples at three temperatures. It was observed that the moisture of the osmoti-
cally dehydrated material decreased rapidly at higher temperatures, generating more
pronounced curves by increasing this parameter. More than 50% of moisture of the
osmotically pretreated materials at the three temperatures analyzed were removed
within the initial 10 h of the drying process.
Pavkov et al. (2011) observed a similar result when studying the drying kinetics
of osmotically dehydrated nectarine seeds at 60 °C. Kowalski and Łechtańska (2015)
also reported similar behavior when comparing the drying time for fresh beet and
osmotically dehydrated in 25% NaCl solution at 65 °C.
The authors reported that the longer drying time in the dehydrated material was
due to the crystallization of sucrose contained in the beet, and the impregnation of the
solutes on the food surface. The substances acted as a barrier to moisture output from
the product. However, Kowalski and Mierzwa (2011) stated that vegetables submitted
to the osmotic dehydration process should dry out faster than fresh vegetables due
to their lower moisture content. Osidacz and Ambrosio-Ugri (2013) found that the
osmotically dehydrated eggplant in 10% NaCl solution achieved a shorter drying
time at 70 °C compared to in nature eggplant dried at the same temperature.
The drying rates of in natura and osmotically dehydrated cassava cubes as a func-
tion of time for all drying condition are presented in Fig. 6.10. This figure reveals that
there is no constant drying rate period for both types of materials studied, and that
the entire drying process occurs in the decreasing rate period, being represented by
the first and second phase of the falling drying rate with internal migration control of
moisture. Several authors have also observed this behavior for various types of vegeta-
bles, such as Akoy (2014), Cabrera et al. (2016), Kek et al. (2013), and Rayaguru
and Routray (2012).
In the period of decreasing rate, it gradually decreases due to decreased evapora-
tion of water inside the material; the process is controlled by the moisture migration
mechanism inside the material, so that a dry layer begins to form on the product
surface. After the removal of bound moisture from the food, the phase change of
the various types of intrinsic moisture in the food occurs, which are bound to the
components by physical and chemical forces (Pavkov et al. 2011).
The influence of selected drying air temperature levels and sample type on drying
kinetics is clearly visible in the images shown in Fig. 6.6. By comparing the drying
Fig. 6.10 Drying rate as a function of moisture content of in natura and osmotically dehydrated
cassava cubes at various process temperatures
rate for both sample types at all temperatures analyzed. It should be noted that
the highest drying rates were achieved in fresh materials due to their higher initial
moisture content compared to osmotically dehydrated samples. Kaya et al. (2016)
researching the drying of fresh and osmotically pretreated Kiwui found a higher
drying rate in fresh samples at higher temperatures. They justified this behavior, as
due to the high moisture value of the fresh samples and explained that the increase
in the temperature difference between the drying air and the product accelerates
the water migration. The larger temperature difference between drying air and fresh
cubes increased the convective heat transfer coefficient, influencing the heat and mass
transfer rates. Several authors have reported similar results for the drying of fresh
and osmotically dehydrated fruits such as figs (Babalis and Belessiotis 2004; Gupta
and Patil 2014; Sacilik and Elicin 2006; Togrul 2005).
The impregnation of sucrose and sodium chloride in dehydrated material during
osmotic pretreatment of cassava cubes was probably responsible for the decrease
in the drying rate. Similar results were verified by several authors in their studies
with the drying of osmotically pretreated vegetables, such as Pavkov et al. (2011)
for nectarine seeds, Osidacz and Ambrosio-Ugri (2013) for eggplant, Dionello et al.
(2009) for pineapple, Kaya et al. (2016) for carrots, Andrés et al. (2007) for mango
and Sanjinez Argandoña et al. (2005) for guava, Azoubel et al. (2009) for cashew
nuts, Guiné (2006) and Park et al. (2002) for pear, Korsilabut et al. (2010) for melon,
Riva et al. (2005) for apricot, Sankat et al. (1996) for bananas, and Singh and Gupta
(2007) for carrots.
Dionello et al. (2009) working with drying fresh pineapple and dehydrated in
solutions of sucrose and invert sugar explained that the low humidity rates found in
the osmotically dehydrated samples occurred due to the concentration of the osmotic
solution and the type of solute used in it. Lower molecular weight solutes such as
glucose and fructose found in invert sugar penetrate more easily than sucrose into the
tissues of the top layer of the vegetable, entering more intensely to make it difficult
to draw water inside the food, thus reducing the drying rate.
Andrés et al. (2007) and Sanjinez Argandoña et al. (2005) found that the presence
of sucrose molecules in pretreated mango and guava tissue, respectively, increased
the internal resistance to water diffusion.
Pavkov et al. (2011), studying drying of nectarine seeds in natura and osmotically
dehydrated, explained that the difference between the partial pressures of water
molecules on the surface of the fresh material and in moist air is greater. Such
behavior promotes a high convective mass transfer coefficient at the surface of the
material, generating faster evaporation and increased drying rate. The reduction in
moisture of the osmotically pretreated sample generates a decrease between the
partial pressures of water molecules on the material surface and in the moist air
during the drying process. As the solute concentration in the plant tissue increases,
the effective moisture diffusivity decreases, this increasing the drying time of the
osmotically dehydrated sample.
The parameters that characterize the convective drying of the cassava cubes in
natura and osmotically dehydrated are presented in Table 6.3. The humidity of both
types of samples was obtained dynamically, weighing the cubes until reaching a
constant weight in the convective drying process. The parameter studied was the
drying air temperature, which ranged from 50 to 70 °C.
As stated earlier, there was no constant drying rate period for both types of
materials. It can be seen from Table 6.3, through the transition moisture content
(M tr ) values, that there were two periods of decreasing drying rate with internal
moisture migration control, before that osmotically dehydrated and fresh cassava
cubes reach the final moisture content (M f ). The times for the 1st stage and the 2nd
stage correspond to the periods of the first and second phase of the decreasing rate,
respectively.
Table 6.3 shows that the in natura samples reached equilibrium moisture content
in a shorter time than the osmotically dehydrated samples, as shown in Fig. 6.10.
According to this table, the moisture contents found for the fresh and osmotically
dehydrated cassava cubes at all temperatures analyzed were below 13% on a wet
basis. These values are within the values established by Standard Resolution RDC
No. 23 of December 14, 2005 (Brazil 2005). This regulation establishes tolerance
limits for starch products derived from cassava root, which require moisture values
of less than 14% and 15% on a wet basis for starch and tapioca, respectively.
172
Table 6.3 Characterization of convective drying of cassava cubes in natura and osmotically dehydrated
Sample T (°C) M a0 M tr M af t tr 1st stage (h) t 2nd stage (h) T otal time (h)
(d.b.) (w.t.) (d.b). (w.t.) (d.b.) (w.t.)
In natura 50 1.38 0.58 1.11 0.53 0.07 0.065 1 20 21
60 1.67 0.63 1.09 0.52 0.06 0.060 2 18 20
70 1.88 0.65 1.00 0.50 0.05 0.051 2 10 12
Osmotically dehydrated 50 0.74 0.43 0.57 0.36 0.15 0.128 1 23 24
60 0.76 0.43 0.57 0.36 0.11 0.102 1 23 24
70 0.98 0.49 0.60 0.37 0.09 0.081 2 22 24
T = Temperature; M 0 = Initial moisture content; M tr = Transition moisture content; M f = Final moisture content; t = Time
a Total average value in triplicate in the dry and wet basis, tr = transition time
T.R. Bezerra Pessoa et al.
Table 6.4 Fitted parameters of the Fick’s model at different convective drying condition
Temperature (°C) Parameter (Deff × 1010 m2 /s) in natura cube Osmotically dehydrated cube
50 5.45 2.75
60 5.83 3.61
70 9.85 4.82
From Table 6.3, we can see that the equilibrium moisture content of the fresh dried
cubes was almost 50% lower than cubes dried by hybrid process. This fact occurred
due to the high concentration of solids incorporated in the material during the osmotic
dehydration step, forming an obstacle for water outlets in the convective drying step.
The in natura cube dried at 70 °C reached the lowest equilibrium moisture content
(5.11% on wet basis). A similar result was obtained by Pornpraipech et al. (2017)
during drying process of cassava rectangular slices at 80 °C. However, Lugo et al.
(2018) found 12% final moisture content for dry cassava at 70 °C in a hybrid drying
system.
Correa et al. (2017) observed lower equilibrium moisture content values in fresh
dried samples and higher samples in osmotically dehydrated samples in sucrose solu-
tion when drying pineapple at 70 °C assisted by ultrasound. They justified that drying
at high temperatures probably caused the caramelization of the incorporated sugars,
establishing additional barriers to the outflow of water from the solid pineapple
matrix. As in this paper, other authors studying the drying of fresh and osmotically
pretreated products also found lower final moisture content values in fresh products
(Osidacz and Ambrosio-Ugri 2013; Kaya et al. 2016; Singh and Singh Hathan 2016).
In general, it is observed in Table 6.3 that the drying times of the in natura dried
cubes were also shorter than the drying times of the osmotically pretreated cubes at
the same temperatures, decreasing with increasing temperature. However, for osmot-
ically dehydrated cassava cubes, the total time was equal at the three temperatures.
These results agree with those obtained by Kaya et al. (2016), who observed longer
drying times in osmotically dehydrated carrot slices in sucrose and sodium chlo-
ride solution at 35 °C, while studying the drying of fresh and osmotically pretreated
carrots. Garcia-Noguera et al. (2010) found drying times of 612 and 891 min for
strawberries dried in natura and osmotically dehydrated previously (50% sucrose
solution), respectively.
Moisture Effective Diffusivity Estimation
In this research, the simplified diffusional model (Fick’s 2nd Law) was fitted to
experimental data of convective drying of fresh and osmotically dehydrated cassava
cubes for long drying times, without considering shrinkage. The aim was to estimate
the moisture diffusion coefficient.
Table 6.5 Variance analysis for final moisture content of in natura cassava cubes
Final moisture content
Source SS DF MS p-Value* Fc F tab
Samples 1.0860 2 0.5430 1.1460 1.1460 6.94
Temperatures 2.8152 2 1.4076 2.9708 2.9708 6.94
Error 1.8952 4 0.4738
Total 5.7964 8
SS = sum of squares; DF = degrees of freedom; MS = mean square; F c = Calculated F; F tab =
Tabulated F; *Statistically significant at p < 0.05 level
Table 6.4 presents the values of the effective moisture diffusivity obtained in this
non-linear regression as applied to convective drying at temperatures 50, 60, and
70 °C.
According to Table 6.4, an increase of the effective moisture diffusivity with
increased drying temperature for the two samples analyzed was observed. Fresh
samples showed higher effective diffusivity values than osmotically dehydrated
samples due to the higher initial moisture content. The results obtained are in agree-
ment with those reported in the literature (Singh and Gupta 2007; Aires et al. 2018;
Ruiz-López et al. 2010).
The osmotically dehydrated cassava cubes presented lower diffusivity values due
to their lower initial moisture content and high concentration of incorporated solids
during the drying process. Osmotic pretreatment resulted in a reduction of free water
in these samples, contributing to the reduction of the mass transfer rate in convective
drying.
Aires et al. (2018) and Zuñiga and Pedreschi (2012) reported that solids gain can
cause the formation of a barrier, making it difficult to mass transfer within the product
during convective drying.
Dehghannya et al. (2018) observed that potato cubes pretreated in solutions with
higher sucrose concentrations (50 and 70%) showed lower effective moisture diffu-
sivity values than samples pretreated in solutions with lower sucrose concentrations
(10 and 30%), after convective drying; they explained that the use of this high solute
concentration in osmotic solutions caused changes in potato texture, which in turn
made it difficult to remove moisture from the product. According to Dehghannya
et al. (2015), osmotic solutions in high concentration can degrade the texture of the
vegetable and stop the moisture diffusion during drying.
Determination of the Best Drying Condition
The determination of the best drying condition was based on the moisture content of
the product and the operating time for both types of samples, according to the data
presented in Table 6.5.
Table 6.6 Tukey test for

Temperatures (°C) Average final moisture content1
comparison of averages final
moisture content of cassava 50 12.79(a)
cubes and dried by hybrid 60 10.22(ab)
process
70 8.05(b)
1 Means followed by the same lowercase letter in the same column
do not differ from each other by the Tukey test at 5% probability
According to Table 6.4, it is observed that for the fresh material, the drying time
at 70 °C was shorter compared to the other drying times of fresh samples dried at
50 and 60 °C. However, in terms of final moisture content, there is a proximity of
the results obtained for fresh samples at the three temperatures analyzed. Thus, an
analysis of variance (ANOVA) was performed at a significance level of 5%, to verify
if there was a significant difference between the values of these parameters at the
three temperatures.
According to the analysis of variance for final moisture content of the fresh
samples shown in Table 6.5, it can be seen that there was no significant difference
between samples and temperatures (p > 0.05), with calculated F values lower than
the tabulated F. Thus, the best drying condition for fresh cassava cubes was at 70 °C,
as it presented a shorter drying time (12 h).
The Tukey test was used to verify the differences between the average final mois-
ture content of the subjected to hybrid process (osmo-convective drying) cassava
cubes at the three temperatures analyzed, as shown in Table 6.6.
By Tukey test, the average final moisture content of the products at temperatures
between 50 and 60 °C and 60 and 70 °C showed no significant difference. However,
between 50 and 70 °C, there was a significant difference, so the temperature of 60 °C
was chosen for convective drying of the osmotically dehydrated cassava cubes.
As a final comment, despite the importance of the statistical methodology applied
here in aiming to obtain the best convective drying condition of in natura and osmot-
ically dehydrated cassava cubes, this is a food product. In this case, new statistical
tests taking account nutritional aspects of the dried cassava cubes are strongly recom-
mended, in order to obtain the best drying conditions based on the final moisture
content, energy consumed nutritional and sensory parameters.
6.2.4.4 Evaluation of the Product Obtained by the Hybrid Process
To verify some changes that the hybrid process (osmotic dehydration and convective
drying) can provoke on the final product, the physical–chemical characterization
of this material was carried out, comparing the results with the physical–chemical
information obtained for the cubes only dried at 60 °C and in natura cubes.
Table 6.7 presents the chemical composition results of the cassava cubes in natura
and osmotically dehydrated and dried at 60 °C.
Table 6.7 Composition of

Parameter In natura Cassava Cassava cubes
cassava cubes in natura and
cubes dried at 60 °C
osmotically dehydrated and
dried at 60 °C Water activity 0.954 ± 0.00 0.232 ± 0.00
Sucrose (g/100 g m 5.745 ± 0.60 16.894 ± 0.42
s)
Sodium chloride 0.340 ± 0.05 5.946 ± 0.06
(g/100 g m s)
Mean value ± standard deviation
The hybrid moisture reduction process (combination of osmotic dehydration and

convective drying) produced a material with desirable shelf life, as it reduced the
water activity value for values below 0.6, which prevents the pathogenic microor-
ganisms’ growth that is responsible to deteriorate the food (Chirife and Favetto 1992).
The values of water activity close to those presented by the osmotically dehydrated
and dried cubes were found by Silva et al. (2013). These authors found water activity
value of 0.180 in tapioca flour. Vieira et al. (2010) found a water activity value of
0.310 for sweet biscuits prepared with 15% cassava starch. The water activity reduc-
tion is more pronounced during convective drying, because the free water in food
is evaporated, reducing the water vapor pressure, which acts on the food (Moreno
et al. 2010). During the osmotic dehydration process, the reduction in water activity
occurs slowly, because diffusion phenomena occur in an aqueous medium.
Sodium is an alkali metal that constitutes approximately 40% of salt, i.e., in
mean, 1 g salt contains 0.4 g of sodium (He and Macgregor 2010). The sodium value
(2,136 mg) found in 100 g of the osmotically dehydrated and dried cassava cube at
60 °C is close to the daily nutrient reference values established in Standard RDC nº
360, on December 23, 2003. This standard reports the nutritional values of packaged
foods and establishes 2,400 mg sodium as the daily nutrient reference value (Brazil
2003). The 2,136 mg value represents 89% sodium in a food portion. The maximum
sodium limit recommended by the World Health Organization (WHO) is 2 g per day
(Sarno et al. 2013). Then, the sodium content found in 100 g of the osmotically dried
cassava cube at 60 °C exceeded the maximum sodium limit recommended by WHO.
According to the data in Table 6.7, sucrose in the osmotically dehydrated cube,
and dried at 60 °C showed a value three times greater than its initial value. However,
sodium chloride showed a higher incorporation power than sucrose, showing a 17-
fold increase in its initial value.
Solutes with a higher molecular weight such as sucrose have lower mass diffusiv-
ities due to its high molecule size, allowing less mobility in food materials through
existing pores and free spaces of plant tissues.
Sugars are generally hydrophilic, uncharged molecules that exhibit slow diffusion
rates (Ruiz-López et al. 2011; Agnieszka and Andrzej 2010; Udomkun et al. 2015).
Udomkun et al. (2015) observed high concentrations of glucose, fructose, and lower
sucrose contraction value in osmotically pretreated and dried papaya cubes. They
explained that this fact may be related to the solute lower molecular weight of glucose
and fructose that penetrate more easily in the vegetable’s superficial layer. Brandão
et al. (2003) found higher sucrose concentrations in osmotically dehydrated and
sun-dried mangabas when compared to the mangaba in natura.
In this chapter, the drying process of food has been studied. Emphasis is given to the
hybrid drying process (combination of osmotic dehydration and convective drying)
as applied to cassava cubes. The study encompasses two analyses: experimental and
theoretical (used to process parameters estimation). Herein transient results of the
moisture loss solid gain and sodium chloride and sucrose incorporation along the
process are presented.
From the obtained results it can be concluded that
(a) The fresh cassava cubes showed 60.45% moisture (wet basis), 2.27% sucrose,
and 0.13% sodium chloride.
(b) The study of osmotic dehydration kinetics in the optimized condition showed
that the moisture loss reached equilibrium in 180 min of process, the total solids
gain in 30 min, and the incorporation of sodium chloride and sucrose in 300 min.
(c) The highest values of the osmotic dehydration kinetics study parameters were
24.90% moisture loss, 16.46% solids gain, 8.87% sucrose incorporation, and
4.07% sodium chloride.
(d) The average effective moisture diffusivities, solid gain, incorporation of sodium
chloride and sucrose presented results equal to 1.99 × 10−8 m2 /s, 2.77 × 10−8
m2 /s, 1.36 × 10−8 m2 /s, and 1.40 × 10−8 m2 /s, respectively.
(e) Convective drying of fresh cassava cubes presented shorter drying times than
previously osmotically dehydrated cassava cubes due to the presence of sucrose
on the outer surface of the cubes making it difficult to remove moisture from
the inside of the material.
(f) The entire convective drying process of the fresh and osmotically dehydrated
cubes at 50, 60, and 70 °C occurred during the falling moisture migration rate.
(g) The fresh samples in convective drying showed higher drying rates than the
osmotically pretreated material in sucrose solution and sodium chloride.
(h) The convective drying temperatures that produced a material with lower final
moisture content was 70 °C for fresh cassava cubes and 60 °C for osmotically
dehydrated cassava cubes.
(i) The average effective moisture diffusivities obtained through the simplified Fick
model for the convective drying of cassava cubes varied from2.75 × 10−10 m2 /s
(Osmotically dehydrated cube at 50 °C) to 9.85 × 10−10 m2 /s (in natura cube
at 70 °C).
(j) Cassava cubes dehydrated osmotically and dried at 60 °C showed 11% humidity,
16.89% sucrose, and 5.94% sodium chloride on a dry basis
(k) The good results obtained with the cassava cubes after submitted to the hybrid
process of osmotic dehydration and convective drying proved that it can be used
in food production as raw material for the development of new cassava-based
products.
Acknowledgments The authors thanks to CNPQ, CAPES and FINEP (Brazilian Research
Agencies) for their financial support.
References
Abbasi Souraki, B., Ghaffari, A., Bayat, Y.: Mathematical modeling of moisture and solute diffusion
in the cylindrical green bean during osmotic dehydration in salt solution. J. Food Process. Preserv.
90(1), 64–71 (2012)
Agnieszka, C., Andrzej, L.: Rehydration and sorption properties of osmotically pretreated freeze-
dried strawberries. J. Food Eng. 97(2), 267–274 (2010)
Aguiar, R., Cunha, R.L., Cunha, E.F.M., Rego, J.Y.N.: Chemico-physical characterization of
mandiocaba roots. In: Proceedings of the Scientific Initiation Seminar and 2nd Post-graduation
Seminar of Embrapa East Amazon, pp. 1–4, Embrapa, Belém (2014). (In Portuguese)
Aires, J.E.F., Silva, W.P., Aires, K.L.C.A.F., Júnior, A.F.S., Castro, D.S., Silva, C.M.D.P.S.: Guava
osmotic dehydration: description by two-dimensional diffusion models considering shrinkage
and variations in process parameters. Int. J. Food Eng. 12(6), 527–536 (2016)
Aires, J.E.F., Silva, W.P., Aires, K.L.C.A.F., Júnior, A.F.S., Silva, C.M.D.P.S.: Convective drying
of osmo-dehydrated apple slices: kinetics and spatial behavior of effective mass diffusivity and
moisture contente. Heat Mass Transfer 54(4), 1121–1134 (2018)
Akoy, E.O.M.: Experimental characterization and modeling of thin-layer drying of mango slices.
Int. Food Res. J. 21(5), 1911–1917 (2014)
Alam, M.M., Islam, M.N., Islam, M.N.: Effect of process parameters on the effectiveness of osmotic
dehydration of summer onion. Int. Food Res. J. 20(1), 391–396 (2013)
Allali, H., Marchal, L., Vorobiev, E.: Blanching of strawberries by ohmic heating: effects on the
kinetics of mass transfer during osmotic dehydration. Food Bioproc, Technol. 3, 406–414 (2008)
Andrés, A., Fito, P., Heredia, A., Rosa, E.M.: Combined technologies for development of high-
quality shelf-stable mango products. Dry. Technol. 25(11), 1857–1866 (2007)
AOAC (Association of Official Analytical Chemists): Official Methods of Analysis. 16th edn.
Washington, USA (1995)
Araújo, P.M., Fonseca, J.R.L., Magalhães, M.M.A., Medeiros, M.F.D.: Drying of carrosts in slices
with osmotic dehydration. Afr. J. Biotechnol. 13(30), 3061–3067 (2014)
Arias, L., Perea, Y., Zapata, J.E.: Kinetic of the mass transfer process in the osmotic dehydration of
mango (Mangifera indica L.) var. Tommy Atkins as function of the temperature. Inform. Tecnoló.
28(3), 47–58 (2017)
Assis, F.R., Morais, R.M.S.C., Moraes, A.M.M.B.: Mathematical modelling of osmotic dehydration
kinetics of apple cubes. J. Food Process. Preserv. 41(3), 1–16 (2017)
Assis, F.R., Morais, R.M.S.C., Morais, A.M.M.B.: Osmotic Dehydration combined with freeze-
drying of apple cubes and comparison with microwave drying and hot air drying. Adv. Food Sci.
Eng. 2(1), 39–47 (2018)
Azarpazhooh, E., Ramaswamy, H.S.: Modeling and optimization of microwave osmotic dehydra-
tion of apple cylinders under continuous-flow spray mode processing conditions. Food Bioproc.
Technol. 5, 1486–1501 (2012)
Azoubel, P.M., Da Silva, F.O.: Optimisation of osmotic dehydration of “Tommy Atkins” mango
fruit. Int. J. Food Sci. Technol. 43(7), 1276–1280 (2008)
Azoubel, P.M., El-Aouar, A.A., Tonon, R.V., Kurozawa, L.E., Antonio, G.C., Murr, F.E.X., Park,
K.J.: Effect of osmotic dehydration on the drying kinetics and quality of cashew apple. Int. J.
Food Sci. Technol. 44(5), 980–986 (2009)
Azuara, E., Beristain, C.I., Garcia, H.S.: Development of a mathematical model to predict kinetics
of osmotic dehydration. J. Food Sci. Technol. 29(4), 239–242 (1992)
Babalis, J.S., Belessiotis, G.V.: Influence of drying condition on the drying constants and moisture
diffusivity during the thin layer drying of figs. J. Food Eng. 65(6), 449–458 (2004)
Borsato, D., Moreira, I., Silva, R.S.S.F., Bona, E., Nóbrega, M.M., Pina, M.V.R., Moreira, M.B.:
Simulation of the multicomponent diffusion during the osmotic dehydration of apple: determi-
nation of the diffusion coefficients by the simplex method, Semina: Ciências Agrárias, 31(2),
391–404(2010). (In Portuguese)
Brandão, M.C.C., Maia, G.A., Lima, D.P., Parente, E.J., Campello, C.C., Nassu, R.T., Feitosa, T.,
Sousa, P.H.M.: Physical and chemical, microbiological and sensorial analysis of mango fruits
submitted to osmotic-solar dehydration. Rev. Braz. Frutic. 25(1), 38–41 (2003). (In Portuguese)
Brazil. Ministry of Agriculture, Livestock and Supply. Normative Instruction n° 23, December 14,
2005. Approves the Technical Regulation on Identity and Quality of Starchy Products derived
from cassava root. Official Journal of the Federative Republic of Brazil, Brasília, p. 5 Section 1
Brazil. Ministry of Health. National Health Surveillance Agency. Standard no. 360, December 23,
2003. Technical regulation on nutritional labeling of packaged foods, 9 p. Ministry of Health,
National Health Surveillance Agency, Brasília (2003)
Cabrera, E., Sanjuán, N., Panadés, G., Cruz, L.: Influence of osmotic pretreatment on the convective
drying of guava. Int. Food Res. J. 23(4), 1623–1628 (2016)
Carmo, A.S., Alves, T.C.O., Martins, P.C.: Study of the kinetics of osmotic dehydration of manioc
slices. Rev. Braz. Agrotecnol. 7(2), 266–272 (2017). (In Portuguese)
Castiglioni, G.L., Silva, F.A., Caliari, M., Soares Júnior, M.S.: Mathematical modeling of drying
process of fibrous mass of cassava. Rev. Braz. de Engenharia Agrícola e Ambiental 17(9), 987–994
Castro, D.S., Nunes, JS., Júnior, A.F.S., Aires, J.E.F.A., Silva, W.P., Gomes, J. P.: Influence of
temperature on the process of dehydration osmotic pieces of guava, Rev. Geintec 4(5)1413–
1423(2014). (In Portuguese)
Castro, D.S., Silva, W.P., Gomes, J.P., Aires, J.E.F., Aires, K.L.C.A.F., Junior, A.F.S.: Development
and sensory evaluation of osmotically dehydrated guava. Braz. J. Food Technol. 21(e2016013),
1–8 (2018). (In Portuguese)
Chicherchio, C.L.S.: Cassava and major derivatives. In: CONAB. Perspectives for Agriculture:
Crop Data 2014/15, pp. 106–117. CONAB, Brasília (2014)
Chirife, J., Favetto, G.J.: Some physico-chemical basis of food preservation by combined methods,
Food Res. Int., Oxford 25(5), 389–396 (1992)
Corrêa, J.L.G., Rasiab, M.C., Muletc, A., Cárcelc, J.A.: Influence of ultrasound application on
both the osmotic pretreatment and subsequent convective drying of pineapple (Ananas comosus).
Innovative Food Sci. Emerg. Technol. 41, 284–291 (2017)
Corzo, O., Bracho, N., Alvarez, C.: Water effective diffusion coefficient of mango slices at different
maturity stages during air drying. J. Food Eng. 87(4), 479–484 (2008)
Couto, E.M.: Characterization of Cassava cultivars from the semi-arid region of Minas Gerais in
four harvest seasons. Doctoral Thesis in Food Sciences, Federal University of Lavras, Lavras,
Brazil (2013). (In Portuguese)
Crank, J.: The Mathematics of Diffusion, 2nd edn. Clarendon, Oxford (1975)
Dehghannya, J., Gorbani, R., Ghanbarzadeh, B.: Effect of ultrasound-assisted osmotic dehydration
pretreatment on drying kinetics and effective moisture diffusivity of Mirabelle plum. J. Food
Proces. Preserv. 39(6), 2710–2717 (2015)
Dehghannya, J., Bozorghi, S., Heshmati, M.K.: Low temperature hot air drying of potato
cubes subjected to osmotic dehydration and intermittent microwave: drying kinetics, energy
consumption and product quality indexes. Heat Mass Transf. 54(4), 929–954 (2018)
Dionello, R.G., Berbert, P.A., Molina, M.A.B., Pereira, R.C., Viana, A.P., Carlesso, V.O.: Assess-
ment of convective drying models for fresh and osmo-dehydrated pineapple rings. Food Sci.
Technol. 29(1), 232–240 (2009). (In Portuguese)
Escobar, M.P., Galindo, F.G., Wadso, L., Najera, J.R., Sjoholm, I.: Effect of long-term storage and
blanching pre-treatments on the osmotic dehydration kinetics of carrots (Daucus carota L. cv.
Nerac). J. Food Eng. 81(2), 313–317 (2007)
Feng, L., Zhang, M., Adhikari, B.: Effect of water on the quality of dehydrated products: a review of
novel characterization methods and hybrid drying technologies. Dry. Technol. 32(15), 1872–1884
(2014)
Fialho, J.F., Vieira, E.A.: Cassava in the Cerrado: Technical Guidelines/Technical Editors, 2 edn.
Embrapa Cerrados, Planaltina, Brazil (2011)
Garcia-Noguera, J., Oliveira, F.I.P., Gallão, M.I., Weller, C.L., Rodrigues, S., Fernandes, F.A.N.:
Ultrasound-assisted osmotic dehydration of strawberries: effect of pretreatment time and
ultrasonic frequency. Dry. Technol. 28(2), 294–303 (2010)
Góis, J.L.C.X., Costa, A.K.L., Filho, R.S.F.: Study of osmotic dehydration of banana apple (Musa
acuminata Colla × Musa balbisiana Colla, AAB Group), Instituto Federal de Educação, Ciência
e Tecnologia do Rio Grande do Norte, IFRN, pp. 1–8 (2010). (In Portuguese)
Guiné, R.P.F.: Moisture diffusivity in pears: Experimental determination and derivation of a
mathematical prediction model. Int. J. Food Sci. Technol. 41(10), 1177–1181 (2006)
Gupta, S.V., Patil, B.N.: Convective drying of osmo-dehydrated sapota slices. Int. J. Agricult. Food
Sci. Technol. 5(4), 219–226 (2014)
Hadipernata, M., Ogawa, M.: Mass transfer and diffusion coefficient of d-Allulose during osmotic
dehydration. J. Appl. Food Technol. 3(2), 6–10 (2016)
Hamedi, F., Mohebbi, M., Shahidi, F., Azarpazhooh, E.: Ultrasound-assisted osmotic treatment of
model food impregnated with pomegranate peel phenolic compounds: mass transfer, texture, and
phenolic evaluations. Food Bioproc. Technol. 11(5), 1061–1074 (2018)
He, J.F., Macgregor, G.A.: Reducing population salt intake worldwide: from evidence to imple-
mentation. Prog. Cardiovasc. Dis. 52(5), 363–382 (2010)
Hills, B.P., Takaca, S.F., Belton, P.S.: A new interpretation of proton NMR relaxation time
measurements of water in food. Food Chem. 37(2), 95–111 (1990)
Isquierdo, E.P., Borém, F.M., Andrade, E.T., Corrêa, J.L.G., Oliveira, P.D., Alves, G.E.: Drying
kinetics and quality of natural coffee. Trans. ASABE 56(3), 1003–1010 (2013)
Jeffery, G.H., Basset, J., Mendham, J., Denney, R.C.: Vogel’s textbook of Quantitative Chemical
Analysis, 5th edn. Longman Scientific & Technical, England (1989)
Junqueira, J.R.J., Correa, J.L.G., Mendonça, K.S.: Evaluation of the shrinkage effect of sweet potato.
J. Food Process. Preserv. 41(3), 1–10 (2017)
Kaya, A., Aydin, O., Kolayli, S.: Influence of osmotic dehydration on drying kinetics of carrot. J.
Thermal Sci. Technol. 36(2), 155–162 (2016)
Kek, S.P., Chin, N.L., Yusof, Y.A.: Simultaneous time-temperature-thickness superposition theo-
retical and statistical modelling of convective drying of guava. J. Food Sci. Technol. 51(12),
3609–3622 (2013)
Korsrilabut, J., Borompichaichartkul, C., Duangmal, K.: Effect of invert sugar on the drying kinetics
and water mobility of osmosed-air dried cantalupe. Int. J. Food Sci. Technol. 45(7), 1524–1531
(2010)
Kowalski, S., Łechtańska, J.M.: Drying of red beetroot after osmotic pretreatment: kinetics and
quality considerations. Chem. Process Eng. 36(3), 345–354 (2015)
Kowalski, S.J., Mierzwa, D.: Influence of preliminary osmotic of carrot (Daucus Carota L.). Chem.
Process Eng. 32(3), 185–194 (2011)
Koyuncu, T., Tosun, I., Pinar, Y.: Drying characteristics and heat energy requirement of cornelian
cherry fruits (Cornus mas L.). J. Food Eng. 78(2), 735–739 (2007)
Kudra, T.: Energy aspects in drying. Dry. Technol. 22(5), 917–932 (2004)
Kumar, A., Islam, S., Dash, K.K., Sarkar, S.: Optimization of process parameters for osmotic
dehydration of chayote cubes by response surface methodology. Int. J. Agr. Environ. Biotechnol.
10(6), 725–737 (2017)
Lane, H., Eynon, L.: Determination of reducing sugar by means of Fehling’s solution with methylene
blue as internal indicatior. J. Soc. Chem. Ind., London 42, 32T–37T (1923)
Lewicki, P.P.: Water as the determinant of food engineering properties: a review. J. Food Eng. 61(4),
483–495 (2004)
Li, S., Dickinson, L.C., Chinachoti, P.: Mobility of “unfreezable” and “freezable” water in waxy
corn starch by 2H and 1H NMR. J. Agr. Food Chemistry 46(1), 62–71 (1998)
Lugo, P.J.M., Padilla, K.A.M., Gallo, R.T., Fandiño, J.M.M., Vasquez, R.D.G.: Experimental evalua-
tion of venezuelan cassava drying by using a hybrid air heating system. Rev. Chilena de Ingeniería
26(2), 329–338 (2018)
Luna, A.T., Rodrigues, F.F.G., Costa, J.G.M., Pereira, A.O.B.: Physical-chemical study, microbial
and bromatological of Manihot esculenta Crantz (mandioca). Rev. Inter.: Saúde, Humanas e
Tecnolo 1(3), 1–11(2013). (In Portuguese)
Maieves, H.A.: Physical, physical chemical and technological potential of new Cassava cultivars.
Master’s dissertation in Food Engineering, Food Engineering College, Federal University of Santa
Catarina, Florianópolis, Brazil (2010). (In Portuguese)
Maldonado, S., Santapaola, J.E., Singh, J., Torrez, M., Garay, A.: Cinética de la transferencia de
masa durante la deshidratación osmótica de yacón (Smallanthus sonchifolius). Food Sci. Technol.
28(1), 251–256 (2008)
Mayor, L., Moreira, R., Chenlo, F., Sereno, A.M.: Kinectcs of osmotic dehydration of pumpkin
with sodium chloride solutions. J. Food Eng. 74(2), 253–262 (2006)
Mercali, G.D.: Study of mass transfer in banana osmotic dehydration (Musa sapientum, shum.).
Master’s dissertation in Chemical Engineering, Federal University of the Rio Grande do Sul,
Porto Alegre, Brazil (2009). (In Portuguese)
Mercali, G.D., Kechinski, C.P., Coelho, J.A., Tessaro, I.C., Marczak, L.D.F.: Study of mass transfer
during the osmotic dehydration of blueberry. Braz. J. Food Tecnol. 13(2), 91–97 (2010). (In
Portuguese)
Mercali, G.D., Kechinski, C.P., Coelho, J.A., Tessaro, I.C., Marczak, L.D.F.: Study of mass transfer
during the osmotic dehydration of blueberry. Braz. J. Food Technol. 13(2), 91–97 (2011). (In
Portuguese)
Mierzwa, D., Kowalski, S.J.: Ultrasound-assisted osmotic dehydration and convective drying of
apples: process kinetics and quality issues. Chem. Process Eng. 37(3), 383–391 (2016)
Montgomery, D.E.: Introduction to Statistical Quality Control, Sixt edn. Wiley, New York (2008)
Moreno, A., León, D., Giraldo, G., Rios, E.: Estudio de la cinética fisicoquímica del mango
(Mangiferia indica L. Var. tommy Atkins) tratado por métodos combinados de secado, DYNA,
77(162), 75–84 (2010)
Moyers, C.G., Baldwin, G.W.: Psychrometry, evaporative cooling and solids drying. In: Perry,
R.H., Green, D.W. (eds.) Perry’s Chemical Engineers’ Handbook, 7 th edn, pp. 12-1–12-90, Mac
Graw-Hill, Nova York (1999). (CD-ROM)
Nogueira, M.C.S.: Agronomic Experimentation I-Concepts, Planning and Statistical Analysis.
Esalq, Piracicaba (2007). (In Portuguese)
Osidacz, R.C., Ambrosio-Ugri, M.C.B.: Physicochemical quality of eggplant dehydrated with varied
pretreatments. Acta Scient. Technol. 35(1), 175–179 (2013)
Park, K.J., Bin, A., Pedro, R.B.F.: Drying of pear dAnjou with and without osmotic dehydration. J.
Food Eng. 56(1), 97–103 (2002)
Pavkov, I., Babić, L., Babić, M., Radojčin, M., Stojanović, C.: Effects of osmotic pre-treatment on
convective drying kinetics of nectarines halves (Pyrus persica L.). J. Process. Energy Agr. 15(4),
217–222 (2011)
Pereira, L.M., Ferrari, C.C., Mastrantonio, S.D.S., Rodrigues, A.C.C., Hubinger, M.D.: Kinetic
aspects, texture, and color evaluation of some tropical fruits during osmotic dehydration. Dry.
Technol. 24(4), 475–484 (2006)
Pereira, L.M., Carmello-Guerreiro, S.M., Hubinger, M.D.: Microscopic features, mechanical and
thermal properties of osmotically dehydrated guavas. LWT Food Sci. Technol. 42(1), 378–384
(2009)
Pessoa, T., Amaral, D.S., Duarte, M.E.M., Cavalcanti Mata, M.E.R.M., Gurjão, F.F.: Sensory assess-
ment of passed guavas obtained by combined techniques of osmotic dehydration and drying. Holos
4(27), 137–147 (2011). (In Portuguese)
Pessoa, T., Silva, D.R.S., Duarte, M.E.M., Cavalcanti Mata, M.E.M.R., Gurjão, F.F., Miranda,
D.S.A.: Physical and physicochemical yam sticks of submitted to osmotic dehydration in saline.
Holos 7(33), 30–38 (2017)
Pornpraipech, P., Khusakul, M., Singklin, R., Sarabhorn, P., Areeprasert, C.: Effect of temperature
and shape on drying performance of cassava chips. Agr. Nat. Resour. 51(5), 402–409 (2017)
Ramya, H.G., Kumar, S., Kumar, M.: Mass exchange evaluation during optimization of osmotic
dehydration for oyster mushrooms (Pleurotus sajor-caju) in salt-sugar solution. J. Appl. Nat. Sci.
6(1), 110–116 (2014)
Rayaguru, K., Routray, W.: Mathematical modeling of thin layer drying kinetics of stone apple
slices. Int. Food Res. J. 19(4), 1503–1510 (2012)
Rinaldi, M.M., Vieira, E.A., Fialho, J.F., Malaquias, J.V.: Effect of different freezing forms on
cassava roots. Braz. J. Food Thechnol. 18(2), 93–101 (2015). (In Portuguese)
Riva, M., Campolongo, S., Leva, A.A., Maestrelli, A., Torreggiani, D.: Structure-property
relationships in osmo-air dehydrated apricot cubes. Food Res. Int. 38(5), 533–542 (2005)
Rodríguez, M.M., Arballo, J.R., Campañone, L.A., Cocconi, M.B., Pagano, A.M., Mascheroni,
R.H.: Osmotic dehydration of nectarines: influence of the operating conditions and determination
of the effective diffusion coefficients. Food Bioproc. Technol. 6(10), 2708–2720 (2013)
Rodríguez, M.M., Arballo, J.R., Campañone, L.A., Mascheroni, R.H.: Analysis of operating condi-
tions on osmotic dehydration of plums (Prunus Domestica L.) and 3D-numerical determination of
effective diffusion coefficientsAnalysis of operating conditions on osmotic dehydration of plums
(Prunus Domestica L.) and 3D-numerical determination of effective diffusion coefficients. Int.
J. Food Eng. 13(11), 1–13 (2017)
Ruiz-López, I.I., Huerta-Mora, I.R., Vivar-Vera, M.A., Martínez-Sánchez, C.E., Herman-Lara, E.:
Effect of osmotic dehydration on air-drying characteristics of chayote. Dry. Technol. 28(10),
1201–1212 (2010)
Ruiz-López, I.I., Ruiz-Espinosa, H., Herman-Lara, E., Zárate-Castillo, G.: Modeling of kinetics,
equilibrium and distribution data of osmotically dehydration carambola (Averrhoa carambola
L.) in sugar solutions. J. Food Eng. 104(2), 218–226 (2011)
Sacilik, K., Elicin, A.K.: The thin layer drying characteristics of organic apple slices. J. Food Eng.
73(3), 281–289 (2006)
Sanjinez-Argandoña, E.J., Cunha, R.L., Menegalli, F.C., Hubinger, M.D.: Evaluation of total
carotenoids and ascorbic acid in osmotic pretreated guavas during convective drying. Italian
J. Food Sci. 17(3), 305–314 (2005)
Sankat, C.K., Castaigne, F., Maharaj, R.: The air drying behaviour of fresh and osmotically
dehydrated banana slices. Int. J. Food Sci. Technol. 3(2), 123–135 (1996)
Sarno, R.M., Levy, R.B., Bandoni, D.H., Monteiro, C.A.: Estimated sodium intake for the Brazilian
population, 2008-2009. Rev. Saúde Pública 47(3), 571–578 (2013)
Silva Júnior, A.F., Aires, J.E.F., Cleide, K.LC.A.F.A., Silva, M.D.P.S., Farias, V.S.O.: Effects of salt
concentration on osmotic dehydration of green bean. J. Agr. Stud. 3(1), 60–78 (2015)
Silva, M.A.C., Silva, Z.E., Mariani, V.C., Darche, S.: Mass transfer during the osmotic dehydration
of West Indian cherry. LWT, Food Sci. Technol. 45(2), 246–252(2012)
Silva, P.A., Cunha, R.L., Lopes, A.S., Pena, R.S.: Characterization of tapioca flour obtained in Pará
state, Brazil. Ciencia Rural 43(1), 185–191 (2013). (In Portuguese)
Singh, B., Gupta, A.K.: Mass transfer kinetics and determination of effective diffusivity during
convective dehydration of pre-osmosed carrot cubes. J. Food Eng. 79(2), 459–470 (2007)
Singh, B., Singh Hathan, B.: Convective dehydration kinetics and quality evaluation of osmo-
convective dried beetroot candy. Italian J. Food Sci. 28(4), 669–682 (2016)
Singh, B., Panesar, P.S., Nanda, V.: Osmotic dehydration kinetics of carrot cubes in sodium chloride
solution. Int. J. Food Sci. Technol. 43(8), 1361–1370 (2008)
Sritongtae, B., Mahawanich, T., Duangmal, K.: Drying of osmosed cantaloupe: effect of polyols on
drying and water mobility. Dry. Technol. 29(5), 527–535 (2011)
STATSOFT. Statistica for Windows, Tulsa, USA (1997)
Sutar, P.P., Prasad, S.: Modeling mass transfer kinetics and mass diffusivity during osmotic
dehydration of blanched carrots. Int. J. Food Eng. 7(4), 1–20 (2011)
Togrul, H.: Simple modeling of infrared drying of fresh apple slices. J. Food Eng. 71, 311–323
(2005)
Udomkun, P., Argyropoulos, D., Nagle, M., Mahayothee, B., Müller, J.: Sorption behaviour of
papayas as affected by compositional and structural alterations from osmotic pretreatment and
drying. J. Food Eng. 157, 14–23 (2015)
Valduga, E., Tomicki, L., Witschinski, F., Colet, R., Peruzzolo, M., Ceni, G.C.: Evaluation of
acceptability and mineral components of different cassava cultivars (Manihot esculenta Crantz)
after cooking. Alimentos e Nutrição Araraquara 22(2), 205–210 (2011). (In Portuguese)
Vázquez-Vila, M.J., Chenlo-Romero, F., Moreira-Martínez, R., Pacios-Penelas, B.: Dehydration
kinetics of carrots (Daucus carota L.) in osmotic and air convective drying processes. Span. J.
Agr. Res. 7(4), 869–875 (2009)
Vieira, J.C., Montenegro, F.M., Lopes, A.S., Pena, R.S.: Physical and sensorial quality of sweet
cookies with cassava starch. Ciência Rural 40(12), 2574–2579 (2010)
Yadav, A.K., Singh, S.V.: Osmotic dehydration of fruits and vegetables: a review. J. Food Sci.
Technol. 51(9), 1654–1673 (2014)
Zúñiga, R.N., Pedreschi, F.: Study of the pseudo-equilibrium during osmotic dehydration of apples
and its effect on the estimation of water and sucrose effective diffusivity coefficients. Food
Bioproc. Technol. 5(7), 2717–2727 (2012)
Chapter 7
Heat Transfer in a Packed-Bed Elliptic
Cylindrical Reactor: Theory,
Heterogeneous Transient Modeling,
and Applications
A. S. Pereira, R. M. da Silva, R. S. Santos, A. G. Barbosa de Lima,

R. O. de Andrade, W. M. P. B. de Lima, and G. S. de Lima
Abstract This chapter focuses on the study of heat transfer in packed-bed elliptic
cylindrical reactor. Based on the local thermal non-equilibrium, a heterogeneous
mathematical model was developed. The transient model is composed for one solid
phase and another fluid phase, in which the balance equation for each constituent,
written in elliptic cylindrical coordinates, is applied separately, and the proposed
model includes different phenomena such as geometry of the particles and reactor,
bed porosity, fluid velocity, conduction, and convection heat transfer between the
solid particles and fluid flowing inside the bed, and heat generations in the involved
A. S. Pereira (B)
Federal Institute of Education, Science and Technology Baiano - IFBaiano, Highway BR 420,
Rural Zone, Santa Inês, BA Zip Code: 45320-000, Brazil
e-mail: antonildo.pereira@ifbaiano.edu.br
R. M. da Silva
Federal Institute of Education, Science and Technology of Paraíba, IFPB, R. Tranqüilino Coelho
Lemos, 671, Dinamérica, Campina Grande, PB Zip Code: 58432-300, Brazil
e-mail: rodrigo.silva@ifpb.edu.br
R. S. Santos
Rural Federal University of the Semi-Arid, Av. Francisco Mota, 572, Mossoró, RN Zip Code:
59625-900, Brazil
e-mail: rosilda.santos@ufersa.edu.br
A. G. B. de Lima (B) · R. O. de Andrade · W. M. P. B. de Lima · G. S. de Lima
Veloso, 882, Bodocongó, Campina Grande, PB Zip Code: 58429-900, Brazil
R. O. de Andrade
e-mail: romario_andrade@hotmail.com
W. M. P. B. de Lima
e-mail: wan_magno@hotmail.com
G. S. de Lima
e-mail: gustavosantoslima@gmail.com
https://doi.org/10.1007/978-3-030-47856-8_7
186 A. S. Pereira et al.
phases. Application has been done to a specific geometry of the reactor with aspect
ratio 2.
Keywords Heat transfer · Fixed-bed reactor · Two-phase model · Simulation
7.1 Introduction
The study of heat transfer in porous media (structure composed by connected and
for unconnected voids and solid material) has been an important topic of researches
around the world. This morphology is present both in nature, as in most of the
Chemical Engineering unitary operations, such as filtration, distillation, absorption
and adsorption, drying and catalytic reactions in fixed and fluidized beds (Freire
2004). On catalytic reactions, fixed-bed tubular reactors are often used in industry to
promote such highly exothermic or endothermic heterogeneous gas-solid reactions.
However, in order to have a realistic and safety design of such equipment, theoretical
and experimental studies, and the development of accurate mathematical models,
based on cold (or heated) flow experiments, must be performed.
The models of porous media heat transfer can be divided into two groups: (a)
pseudo-homogeneous—where there is no distinction between the phases, and the
solid–fluid mixture heat transfer occurs in the same temperature at each location
of the bed (local thermal equilibrium) and (b) heterogeneous model—where each
phase has its own heat transfer dynamics, and there is a parameter that coupling
the heat transfer between the phases (local thermal non-equilibrium). These models
can be further subdivided into 1D, 2D, or 3D models according to the analyzed
geometry. Each model may present variations due to the considered simplifying
assumptions; however, the heterogeneous model is the most accurate and realistic
under the physical point of view.
Heat transfer studies in fixed-bed reactors are still limited to simple cylindrical
geometries, pseudo-homogeneous model, and variations in some system thermo-
physical properties of the involved materials. Therefore, this chapter aims to realize
a study of the heat transfer in a fixed-bed reactor with elliptic cylindrical geometry
and applying a two-phase mathematical model (heterogeneous model).
7.2 Porous Media and Packed-Bed Reactors
7.2.1 Porous Media
For a material to be considered as a porous medium it must be checked whether it

contains relatively small voids, generally called pores, within the solid or semi-solid
matrix. The pores usually are filled by a fluid, such as air, water, or a fluid mixture,
moreover, they must be permeable, i.e., these fluids may penetrate the porous medium
7 Heat Transfer in a Packed-Bed Elliptic … 187
Fig. 7.1 Particle filling state, initial (left) and final (right), after compression sintering and /or
heating
through one face and emerge on another face, or migrate from the volume interior to
surface due to the action of some external agent, such as heat pressure or concentration
gradients.
Porous media can be classified according to structure as granular or fibrous. Gran-
ules are usually formed by a set of particles or grains, spherical or not, arranged
regularly or randomly, and represent the vast majority of porous media. Fibers are
formed by a set of very long inclusions, called fibers, that can be natural or synthetic,
straight or curved, being randomly arranged or in regular distributions. Examples
of porous media are particle beds, porous rocks, fibrous cluster such as tissues and
filters, and extremely small microspore-containing catalytic particles (Mendes 1997).
Figure 7.1 illustrates a porous medium consisting of particles with different shapes
and dimensions, uncompressed, and compressed by pressure and/or heating.
Except for metal structures, dense rocks, and some plastics, on a microscopic
scale, solids can be considered porous media materials (Dullien 1992). Having
adequate models to predict the behavior of the momentum, mass, and heat transport
phenomena inside of porous media can be fundamental in the scientific, technolog-
ical, and industrial areas, such as the fixed-bed reactors. The ability to model the
porous medium behavior under different conditions allows to accelerate the devel-
opment and to improve the efficiency of processes involving porous media and thus,
to allow economic and environmental gains.
It is difficult to precisely describe the porous media geometry due to its complex
structure. In theory, this material can be specified by analytical equations that
define the shape and pores dimensions. For practical purposes, it is impossible to
fully describe these equations and, therefore, some geometric approximations are
considered, obtaining characteristics very close to the real ones.
As described in Eq. (7.1), the porosity is the ratio of void volume (V v ), which
are the zones not occupied by the solid material and the total volume of the porous
medium (V T ) which is the sum of the void volume and the solid particle volumes
(Dullien 1992).
VV
ϕ= (7.1)
VT
Fig. 7.2 Distribution of

particles in a porous bed
Thus, porosity indicates the void volume percentage in relation to the total volume;
Fig. 7.2 can assist in the understanding of these parameters.
The Eq. (7.2) shows a relationship between porosity and density of the bed (bulk
density) that contain particle and fluid:
m total
ρbed = (7.2)
Vtotal
where the total mass is the sum of solid and fluid mass, as follows:
m total = (1 − ϕ)(SH)ρs + ϕ(SH)ρf (7.3)
where ρ s and ρ f are, respectively, the particle and fluid densities, and
Vtotal = (SH)Vtotal = (SH) (7.4)
Inserting Eqs. (7.3) and (7.4) in Eq. (7.2), the available volume to flow is defined
as
ρbed − ρs
ϕ= (7.5)
ρf − ρs
Another way to determine the porous medium is by using the packing factor (PF),
which represents the actual fraction occupied by the particles. The mathematical
expression for this purpose is

N · VP
ϕ = 1 − (PF) = 1 − (7.6)
Vtotal
where N is the effective particle number, V p is the particle volume, and V total is the
unit cell volume (porous media).
The particle geometric characteristics: shape, size, and distribution influence the
behavior of the unconsolidated porous media. The bed porosity increases as the
particle shape is very different from a spherical shape, thus, the sphericity is less
than 1. Given this, many works report the use of an equivalent diameter for the
particles.
The equivalent diameter (d p ) is defined as the sphere diameter with the same
particle volume (McCabe et al. 1985). It can be determined by the ratio d p = 6/Ap ,
if the specific surface area (Ap ), particle surface area divided by particle volume, is
known. The Ap represents the contact area between the solid and the fluid phase,
which is a very important parameter in some processes. An equivalent nominal
diameter may also be obtained by sieving if an equivalent diameter measurement is
not available. This mathematical expression for the diameter is most commonly used
for particles with shape closer to the spherical. For particles with regular or irregular
geometry, a sphericity factor β is defined by
1/3
VP
β= (7.7)
Vsc
where the values of this factor differ for particles of different shapes. In Eq. (7.7),
V p and V sc , respectively, represent the particle and circumscribed sphere volumes,
as shown in Fig. 7.3 (Curray and Griffiths 1955).
In many applications, the bed particles do not have a uniform diameter, but a
size distribution. Thus, it is common to determine an average value for the particle
diameter (equivalent particle diameter). The consequence of this approach is that a
Fig. 7.3 Relationship

between particle volume and
circumscribed sphere volume
Fig. 7.4 Scheme of an

unconventional fixed-bed
reactor
real bed with various particle sizes distribution will be represented by a bed formed
by spherical particles with the same equivalent diameter.
7.2.2 Chemical Reactors
7.2.2.1 Reactor Fundamentals
Chemical reactors are equipment in which chemical reactions occur. They can be
found in two basic types, tanks or tubes, aiming to maximize the generation of
desired products with higher added value; produce the highest yield at the lowest cost;
generate intermediates chemical products for new processes, and to generate profits,
operating within pre-established safety (controlled), according to environmental
legislation (Fábrega 2012).
The ideal reactors (for which a specific mathematical model is developed from
pre-established conditions and predict properly the physical phenomena behavior
when realistic conditions are applied) and non-ideal reactors (for which treatment
and specific mathematical function due to reaction and/or reactor peculiarities are
required) have been reported in the literature. Batch, tubular, and mixing are the three
main types of ideal reactors. Figure 7.4 illustrates a schematic of a fixed-bed reactor
with fluid inlet and outlet, the particle packing, and the fluid flow direction in the
bed.
7.2.2.2 Reactors Modeling
Due to the development of computers and the availability of industrial simulators, it is

not recommended to expand the reactor scale without first developing any modeling
as simple as it may be, to have a better knowledge of the equipment and process
behavior. Modeling can vary from the fundamental, which can use simpler differential
equations by separately evaluating each mechanism that influences the process, to

later add more information from the same mechanisms to the model, providing a
more complex reactor simulation, or it can be based on pilot experimentation to
adjust the model effective parameters (Froment and Hofmann 1987).
The reactor to be adequately controlled must be very well known and, therefore,
a model that describes its behavior as operating with great accuracy is necessary.
On the other hand, applications involving a dynamic model usually require a large
computational effort with direct impact on the processing time. In addition, to the
development of models with high prediction potential, it is necessary to consider the
difficulty in their solution, both in computational terms and in the availability of the
necessary (Bunnell et al. 1949).
The simulation of chemical reactors had large use in recent years. These simula-
tions have served several purposes: reactor design, reactor start and stop strategies,
determination of desired and hazardous operating conditions for process control, and
optimization, using sometimes detailed and heterogeneous models.
The heat transfer related catalytic bed models can be divided into heteroge-
neous model (solid phase + fluid phase) also known as two-phase model and single
model (pseudo-homogeneous). Each model may also present variations due to the
used assumptions. For example, in a tubular reactor, one-dimensional models do
not consider radial gradients of temperature or concentration, grouping all resis-
tance to heat transport on the wall. The two-dimensional consider the existence of a
non-planar radial profile of temperatures and concentrations, which presupposes the
knowledge of the effective radial thermal conductivity, and the film coefficient on
the wall (Giordano 1991).
Performance analyses of different two-dimensional models (pseudo-
homogeneous and heterogeneous) show that the pseudo-homogeneous model
is consistent having a simpler computational solution and programming than
the other models. In the two-phase model (solid + fluid), each phase has its
own dynamics of heat transfer, which is physically more realistic. Nevertheless,
few scientists have studied this model for inherent modeling reasons, which are
considerably more complicated solution of the energy equations for the solid and
fluid phases, experimental difficulty in determining the solid–fluid heat transfer
coefficient required for heterogeneous model, and the difficulty in spot temperature
measurement for each phase.
7.3 Heat Transfer in Fixed-Bed Elliptical Reactor

via Two-Phase Model
7.3.1 Physical Problem and Geometry
The packed-bed elliptical reactor studied in this research is illustrated in Fig. 7.5.
The reactor bed is percolated by a heated fluid (fluid 1), which exchanges heat with
Fig. 7.5 Scheme of a packed-bed elliptical cylindrical reactor
the particles, and the system is cooled at the wall by fluid 2 which has a temperature
less than the inlet fluid temperature. Fluid 1 flows in the laminar regime.
This physical problem with the use of pseudo-homogeneous model has been
studied by Oliveira et al. (2004), Silva Filho et al. (2013), Silva et al. (2017, 2018);
however, based on the heterogeneous model no works have been reported in the
literature.
The system geometric shape proposed in this chapter suggests the use of a partic-
ular coordinate system that best fits this geometry and, consequently, will lead to
greater efficiency and confidence of the results (Lima 1999). In this case, the elliptic
cylindrical coordinate system is most appropriate.
Thus, a change of variables is a natural requirement. The general relations between
the Cartesian coordinate system (x, y, z) and the elliptical cylindric coordinate system
(τ, φ, z) are given as follows (Magnus et al. 1966):
x = L cosh τ cos φ (7.8)
y = L senh τ sen φ (7.9)
z=z (7.10)
whereL is the ellipse focal length, mathematically calculated by the expression

L = L 22 − L 21 , where L 1 and L 2 are the ellipse minor and major axes, respectively
(Fig. 7.5). To obtain the desired transformation, consider the following variables:
ξ = cosh τ (7.11)
η = cos φ (7.12)
Thus, the substitution of these variables ξ and η in Eqs. (7.8)–(7.9) provides

the direct relationships between the two coordinate systems. Thus, the following
relationships are obtained for x, y, and z, in terms of ξ and η:
x = Lξ η (7.13)

y=L 1 − η2 ξ 2 − 1 (7.14)
z=z (7.15)
The domain of validity of variables ξ, η, and z in the elliptic cylindrical system

are 1 ≤ ξ ≤ L 2 /L, 0 ≤ η ≤ 1, and 0 ≤ z ≤ H .
The elimination of variable φ, in the Eqs. (7.8) and (7.9), generating the xy plan
curves (Fig. 7.6), characterized by the parameters ξ = ξ0 (constant). The surfaces
Fig. 7.6 Representative

scheme of the elliptic
cylindrical coordinate
system in ξ η and xy planes
ξ0 > 1 are revolution ellipsoids with center in origin. The generated ellipses have
the same focus. The two-ellipse focus are located along the x-axis at the points (x =
±L, y = 0). The surface ξ = 1 it is a straight line that joins the origin (z = 0) and
the focal point (z = +L).
According to Figs. 7.5 and 7.6, when L 2 → L 1 , the elliptic cylinder tends to a
circular cylinder with diameter of 2L 1 . Thus, at the limit when the interfocal distance
tends to zero, the elliptical coordinate system is reduced to the cylindrical: Lξ → r
and η → cos θ, when ξ → ∞, where r and θ are the cylindrical coordinates.
7.3.2 Governing Equations
The transient energy equations (in terms of temperature) for the fluid and solid phases
in the Cartesian coordinate system are, respectively (Nield and Bejan 1992):
• Fluid phase
∂ Tf DP
ϕ ρcp f + ρcp f v · ∇Tf = + ϕ∇ · (K f ∇Tf ) + μψ + ϕ q̇f + h(Ts − Tf ) (7.16)
∂t Dt
• Solid phase
∂ Ts
(1 − ϕ)(ρc)s = (1 − ϕ)∇ · (K s ∇Ts ) + (1 − ϕ)q̇s + h(Tf − Ts ) (7.17)
∂t
where f and s refer to the fluid and solid phases, respectively, T is the temperature,
t is the time, v is the fluid average velocity, ϕ is the media porosity, ρ is the density,
cp is the specific heat at constant pressure, K is the thermal conductivity, μψ is the
viscous dissipation term, P is the pressure, q̇ internal energy generation per volume
unit, and h is the specific heat transfer coefficient by convection, between the solid
and fluid phases.
The first term of Eq. (7.16) represents the transient transfer of energy; and the
second term, the convective heat transport, and where the relation of Dupuit–Forch-
heimer v = ϕV, V the fluid velocity was used. The third term represents the substan-
tive derivative of pressure, the fourth term is the conduction heat transport, the fifth
term corresponds to viscous dissipation, the sixth term is the internal energy gener-
ation, and the seventh term represents the convection heat exchange between the
solid and fluid phases. The first term of Eq. (7.17) represents the transient transfer
of energy and the second term represents the conductive heat flux through the solid.
The third term represents the heat generation inside the solid, and the fourth term
refers to the heat exchange between the solid and fluid phases, by convection.
Some values of h can be obtained indirectly (Polyaev et al. 1996). One of the
correlations for a porous particle bed is given by Dixon and Cresswell (1979):
h = asf h sf (7.18)
where hsf is the convective heat transfer coefficient to both phases and afs is the
specific surface area, given by the relationships between the total area to heat transfer
and the particle bed volume. For example, to a spherical particle bed this parameter
is given as follows:
asf = 6(1 − ϕ)/dP (7.19)
where d P is the particle diameter and the parameter hsf is given as follows:
1 dP dP
= + (7.20)
h sf Nusf K f β Ks
where β is the sphericity of the porous bed particles obtained by (see Eq. 7.7):
1/3
a2
β= (7.21)
b2
being a and b positive real numbers that determine the particle dimensions and shape
(see Fig. 7.3). The Nusselt number Nusf can be obtained by the following expression
(Handley and Heggs 1968):
1 1
Nusf = (0.225/ϕ)Pr 3 Rep3 (7.22)
valid for particle Reynolds numbers ReP > 100. In this equation, Pr is the Prandtl
number. Another correlation for Nusselt number is given as follows (Wakao and
Kaguei 1982):
1
Nusf = 2.0 + 1.1Pr 3 Re0.6
p (7.23)
Equation (7.23) is valid for low values of ReP . In this case, predictions of Nusf
vary between 0.1 and 12.4 (Miyauchi et al. 1981; Wakao et al. 1976; Wakao and
Kaguei 1979). Several other authors, such as Alazami and Vafai (2000), Grangeot
et al. (1994), Saito and Lemos (2005), Quintard et al. (1997), Quintard and Whitaken
(2000) and Nield (2002) have reported alternative expressions for determining the
parameters hsf and asf .
Considering viscous dissipation and the substantive derivative of pressure negli-
gible, the general conservation equation applied for the fluid and solid phases for a
generic variable Φ and writing in any coordinate system (Maliska 1995) are given
by

∂ Φ ∂ Φ ∂ Φ ∂ Φ
ϕ(ρcP )f + (ρcP )f U + (ρcP )f V + (ρcP )f W =
∂t J ∂ξ J ∂η J ∂z J

∂ ∂Φ ∂Φ ∂Φ
α11 ϕ J Γ Φ + α12 ϕ J Γ Φ + α13 ϕ J Γ Φ
∂ξ ∂ξ ∂η ∂z

∂ ∂Φ ∂Φ ∂Φ
+ α21 ϕ J Γ Φ + α22 ϕ J Γ Φ + α23 ϕ J Γ Φ
∂η ∂ξ ∂η ∂z

∂ ∂Φ ∂Φ ∂Φ qf
+ α31 ϕ J Γ Φ + α32 ϕ J Γ Φ + α33 ϕ J Γ Φ + ϕ + h(Φs − Φf )
∂z ∂ξ ∂η ∂z J
(7.24)
and

∂ Φ ∂Φ Φ ∂Φ Φ ∂Φ
α31 (1 − ϕ)J Γ + α32 (1 − ϕ)J Γ + α33 (1 − ϕ)J Γ
∂z ∂ξ ∂η ∂z
qs h
+(1 − ϕ) + (Φf − Φs ) (7.25)
J J
where J represents the Jacobian, determined mathematically as follows:
∂x
∂x ∂x
∂ξ ∂η ∂z
∂y ∂y ∂y
J −1 = ∂ξ ∂η ∂z (7.26)
∂z
∂z ∂z
∂ξ ∂η ∂z
The coefficients α ij , on the Eqs. (7.24) and (7.25) are determined by the following
relations:
a
α11 = (7.27)
J2
d
α12 = α21 = (7.28)
J2
b
α22 = (7.29)
J2
e
α13 = α31 = (7.30)
J2
c
α33 = (7.31)
J2
f
α23 = α32 = (7.32)
J2
where
2 2 2
∂ξ ∂ξ ∂ξ
a = + + (7.33)
∂x ∂y ∂z
2 2 2
∂η ∂η ∂η
b = + + (7.34)
∂x ∂y ∂z
2 2
∂z ∂z 2 ∂z
c = + + (7.35)
∂x ∂z ∂y

∂ξ ∂η ∂ξ ∂η ∂ξ ∂η
d = + + (7.36)
∂x ∂x ∂y ∂y ∂z ∂z

∂z ∂ξ ∂z ∂ξ ∂z ∂ξ
e = + + (7.37)
∂x ∂x ∂y ∂y ∂z ∂z

∂z ∂η ∂z ∂η ∂z ∂η
f = + + (7.38)
∂x ∂x ∂y ∂y ∂z ∂z
For the elliptic cylindrical coordinate system, the determination of the Jacobian
inverse provides as a result:

−1 L 2 ξ 2 − η2
J
=− (7.39)
ξ 2 − 1 1 − η2
In the general equation (Eqs. 7.24 and 7.25), the terms containing α ij with i = j are
the diffusive terms referring to the non-orthogonality of the mesh. Thus, checking the
orthogonality of the adopted coordinate system becomes an important requirement.
In this case, the necessary and sufficient conditions for a coordinate system to be
orthogonal are (McRobert 1967):

∂x ∂x ∂y ∂y ∂z ∂z
+ + =0 (7.40)
∂ξ ∂η ∂ξ ∂η ∂ξ ∂η

∂x ∂x ∂y ∂y ∂z ∂z
+ + =0 (7.41)
∂η ∂z ∂η ∂z ∂η ∂z

∂x ∂x ∂y ∂y ∂z ∂z
+ + =0 (7.42)
∂z ∂ξ ∂z ∂ξ ∂z ∂ξ
It can be verified that all these conditions are satisfactory for the elliptic cylindrical
coordinate system. Then, the coefficients d , e and f are null, and Eq. (7.24) will be
reduced as follows:

∂ Φ ∂ Φ ∂ Φ ∂ Φ
ϕ(ρcP )f + (ρcP )f u ξ + (ρcP )f u η + (ρcP )f u z =
∂t J ∂ξ J ∂η J ∂z J

∂ ∂Φ ∂ ∂Φ ∂ ∂Φ qf h
α11 ϕ J Γ Φ + α22 ϕ J Γ Φ + α33 ϕ J Γ Φ + ϕ + (Φs − Φf ) (7.43)
∂ξ ∂ξ ∂η ∂η ∂z ∂z J J
Substituting Eqs. (7.27), (7.29), (7.31), and (7.39) in Eq. (7.24) and rearranging
the terms, where Φ = T and Γ Φ = K f , we obtain for the fluid phase, the following
equation:
⎡ 2 2 2
⎤ ⎡ 2 2 2
⎤ ⎡ 2 2 2
⎤
∂ ⎣ ϕ ρcp f L ξ − η Tf ⎦ ∂ ⎣ ρcp f L ξ − η u ξ Tf ⎦ ∂ ⎣ ρcp f L ξ − η u η Tf ⎦
+ +
∂t ξ 2 − 1 1 − η2 ∂ξ ξ 2 − 1 1 − η2 ∂η ξ 2 − 1 1 − η2
⎡ 2 2 2
⎤
∂ ⎣ ρcp f L ξ − η u z Tf ⎦ ∂ ξ2 − 1 ∂T f ∂ 1 − η2 ∂T f
+ = ϕ Kf + ϕ Kf
∂z ξ 2 − 1 1 − η2 ∂ξ 1 − η2 ∂ξ ∂η ξ2 − 1 ∂η
⎡ ⎤
2 2 2 L 2 ξ 2 − η2
∂ ⎣ L ξ −η ∂ Tf ⎦
+
∂z
ϕ K f
∂z
+ ϕqf + h(Ts − Tf ) (7.44)
ξ 2 − 1 1 − η2 ξ 2 − 1 1 − η2
Considering u z u ξ and u z u η , the Eq. (7.44) assumes the way:

⎡ ⎤ ⎡ ⎤
∂⎣ ϕ ρc ξ − η ρc ξ − η
⎦ + ∂ ⎣ p f
2 2 2 2 2 2
L T L u T
p
f
f z f
⎦=
∂t ∂z
ξ 2 − 1 1 − η2 ξ 2 − 1 1 − η2

∂ ξ2 − 1 ∂ Tf ∂ 1 − η2 ∂ Tf
ϕ Kf + ϕ Kf
∂ξ 1 − η2 ∂ξ ∂η ξ2 − 1 ∂η
⎡ ⎤
∂ ⎣ L 2 ξ 2 − η2 ∂ Tf ⎦ L 2 ξ 2 − η2
+ ϕ K f ∂z + [ϕqf + h(Ts − Tf )]
∂z ξ 2 − 1 1 − η2 ξ 2 − 1 1 − η2
(7.45)
Similarly, for the energy equation applied to the solid phase, and substituting
Φ = T and Γ φ = K s , we obtain
⎡ ⎤
∂ ⎣ (1 − ϕ) ρcp s L 2 ξ 2 − η2 Ts ⎦ ∂ ξ2 − 1 ∂ Ts
= (1 − ϕ)K s
∂t ξ 2 − 1 1 − η2 ∂ξ 1 − η2 ∂ξ
⎡ ⎤
∂ 1 − η 2 ∂ Ts ∂ L ξ
2 2
− η 2
∂ Ts ⎦
+ (1 − ϕ)K s + ⎣ (1 − ϕ)K s ∂z
∂η ξ2 − 1 ∂η ∂z ξ −1 1−η
2 2

L 2 ξ 2 − η2
+ [(1 − ϕ)qs + h(Tf − Ts )]
ξ 2 − 1 1 − η2
(7.46)
Fig. 7.7 Scheme showing

the heat exchanges
considered in the boundary
for the solid and fluid phases
Since Eqs. (7.45) and (7.46) are second order in space and first order in time
differential equations, their solution requires at least two boundary conditions for
each direction and one initial condition. Moreover, it is an elliptical equation, making
it necessary to define these boundary conditions along the entire boundary of the
considered domain. Thus, considering Fig. 7.7, the following initial and boundary
conditions are given:
(a) Prescribed temperature condition at the reactor inlet:
T (ξ, η, z = 0, t) = T0 (7.47)
(b) Parabolic condition at reactor output:
∂T
(ξ, η, z = H, t) = 0 (7.48)
∂z
(c) Symmetry conditions:
∂T
(ξ = 1, η, z, t) = 0 (7.49)
∂ξ
∂T
(ξ, η = 0, z, t) = 0 (7.50)
∂η
∂T
(ξ, η = 1, z, t) = 0 (7.51)
∂η
(d) Reactor wall conditions

It is considered that in the reactor wall heat diffusive and convective fluxes (only for
the fluid phase) occur on the inner side of the wall that equals the diffusive heat flux
at the reactor wall, which is equal to the convective heat flux, at the external side of
the reactor wall. Thus, can be written as

k ξ 2 − 1 ∂ T
q =− + h win (TP − Twin ) = h wext (Twext − Tm ) =
L ξ 2 − η2 ∂ξ
(ξ =ξin )

kwr ξ − 1 ∂ T
2
− (7.52)
L ξ 2 − η2 ∂ξ
(ξ =ξext )
where ξ in = L 2 /L on the surface (Fig. 7.5) and the subscript wr means the reactor
wall location.
7.3.3 Numerical Treatment of Heat Transport Equations
It is well known by the scientific community that physical problems related to trans-
port phenomena (energy, linear momentum, and mass) have a high complexity and
inevitably are governing by partial differential equations. To obtain an analytical
solution to problems of this insignificance, when it is achieved, will require labo-
rious and rigorous mathematical treatment, with severe considerations. Thus, the use
of numerical techniques emerges as an alternative for the interpretation and solution
of the physical problem with great consistence and realism.
The advance in the study of physical problems involving computer simulation,
as well as the speed of computer processing today, has significantly increased the
search for the analysis of such problems through numerical solutions. There are
several numerical methods that are being used by the scientific community. In this
chapter, we will use the finite-volume method, which has as its basic principle the
transformation of partial differential equations into elementary algebraic equations.
The fundamental concept of the finite-volume method is that any continuous quantity
can be approximated by a discrete model, consisting of a set of continuous functions,
defined in a finite number of subdomains, so-called control-volumes, with nodal
points located in the centroid of them (Patankar 1980; Maliska 1995).
Figure 7.8 illustrates the computational domain used to represent the physical
domain in the fixed-bed elliptic cylindrical reactor, where there is symmetry in the
four quadrants (see Figs. 7.5 and 7.6). In Fig. 7.8, the control-volume is associated
with the nodal point P and the lines ξ and η constants defining the contour. The points
F, T, N, S, E, and W are the neighboring nodal points (top, bottom, north, south,
east, and west, respectively).
Considering the control-volume outlined in Fig. 7.8, it is possible to make the
discretization of Eqs. (7.45) (fluid phase) and (7.46) (solid phase) by integrating
each term in volume and time. Assuming a fully implicit formulation and the WUDS
Fig. 7.8 Numerical mesh control-volume in the elliptical cylindric coordinate system
scheme as a spatial interpolation function for the convective and diffusive fluxes
over the control-volume, after rigorous mathematical treatment we obtain the energy
equations for both phases in the discretized form, as follows.
• Fluid phase
APf TPf = AEf TEf + AWf TWf + AN f TNf + ASf TSf + AFf TFf + ATf TTf + A0Pf TP0f + Bf
(7.53)
where

L 2 ξf2 − ηf2 ϕ K ff βff
A Ff = − (0.5 − αf )ρff cPff u z ξ η (7.54)
ξf2 − 1 1 − ηf2 δz f

L 2 ξt2 − ηt2 ϕ K tf βtf
ATf = + (0.5 + αt )ρtf c P u z ξ η (7.55)
ξ 2 − 1 1 − η2 δz t tf
t t

1 − η2 ϕ K ef βef
AEf = 2 e ξ z (7.56)
ξe − 1 δηe

1 − ηw2 ϕ K wf βwf
AWf = 2 ξ z (7.57)
ξw − 1 δηw
⎧
⎨ (ξn2 −1) ϕ K nf βnf
ηz, Internal points.
A Nf = (1−ηn2 ) δηn (7.58)
⎩
0, Boundary points.

ξs2 − 1 ϕ K sf βsf
A Sf = ηz (7.59)
1 − ηs2 δηs

L 2 ξ 2 − η2 ϕ 0 ρf0 cP0f ξ ηz
A0Pf = (7.60)
1 − η2 ξ 2 − 1 t
APf = AEf + Awf + ANf + ASf

L 2 ξf2 − ηf2 ϕ K ff βff
+ + (0.5 + αf ff Pff z ξ η
)ρ c u
ξf2 − 1 1 − ηf2 δz f

L 2 ξt2 − ηt2 ϕ K tf βtf
+ − (0.5 − αt )ρtf cPtf u z ξ η + SMf
ξt2 − 1 1 − ηt2 δz t
ϕρ c
L 2 ξ 2 − η2 f Pf
+ t + a sf sf ξ ηz
h (7.61)
1 − η2 ξ 2 − 1
⎧
⎪
⎪ (ξn2 −ηP2 )
⎪
⎪ Lηz
⎪
⎪ (1−ηP2 )
⎪
⎪ ⎡ ⎛ ⎞ ⎤ , Boundary points.
⎪
⎪

⎨ ⎝1+ Kf + hwinf + Kf U + hwinf δξn ⎠

SMf = ⎢ ⎥

K wr h wextf h wextf δξn
K U
⎪ ⎢ ⎛ ⎞ wr ⎥
⎪ ⎣ ⎦

⎪
⎪ KfU
⎪
⎪ ⎝ h winf + δξn ⎠
⎪
⎪
⎪
⎪
⎩
0, Internal points
(7.62)
⎧
⎪
⎪ (ξn2 −ηP2 ) ηz
⎪
⎪ L
(1−ηP2 )
⎪
⎪
⎪
⎪ ⎡⎛ ⎞⎤, Boundary points.
⎪

⎪
⎪ ⎝1+ K f + h winf + K f U + h winf δξn ⎠
⎪
⎪ ⎢ δξn

⎥
⎨ ⎢
K wr h wextfh wextf
K wr U ⎥
⎛ ⎞
Bf = ⎣ ⎦

(7.63)
⎪
⎪ ⎝h winf + K f U ⎠
⎪
⎪
δξn
⎪
⎪
⎪
⎪
⎪
⎪ L 2 ξ 2 − η2
⎪
⎪ [ϕ q̇f + asf h sf TS )]ξ ηz, Internal points.
⎩ 1 − η2 ξ 2 − 1
⎪
• Solid phase
APs TPs = AEs TEs + Aws Tws + ANs TNs + ASs TSs + AFs TFs + ATs TTs + A0Ps TP0s + Bs
(7.64)
where

1 − ηe2 (1 − ϕ)K es βes
AEs = 2 ξ z (7.65)
ξe − 1 δηe

1 − ηw2 (1 − ϕ)K ws βws
A ws = 2 ξ z (7.66)
ξw − 1 δηw
⎧
⎨ 0, Internal points.
A Ns =
⎩ (1−η
ξn −1) (1−ϕ)K ns βns
2 (7.67)
ηz, Boundary points.
( n2 ) δηn

ξs2 − 1 (1 − ϕ)K ss βss
A Ss = ηz (7.68)
1 − ηs2 δξs

L 2 ξf2 − ηf2 (1 − ϕ)K fs βfs
AFs = ξ η (7.69)
ξ 2 − 1 1 − η2 δz f
f f

L 2 ξt2 − ηt2 (1 − ϕ)K ts βts
ATs = ξ η (7.70)
ξt2 − 1 1 − ηt2 δz t

L 2 ξ 2 − η2 1 − ϕ 0 ρs0 cP0s ξ ηz
A0Ps = (7.71)
1 − η2 ξ 2 − 1 t

L 2 ξ 2 − η2
(1 − ϕ)ρs cPs
APs = AEs + Aws + ANs + ASs + AFs + ATs + t
+ asf h sf + SMs (7.72)
1 − η2 ξ 2 − 1
⎧
⎪
⎪ (ξn2 −ηP2 )
⎪
⎪
Lηz
(1−ηP2 )⎞
⎪
⎪ ⎡⎛ ⎤ , Boundary points.
⎪

⎨ ⎜ K KU ⎟
⎢ ⎝1+ K wr
s +
h wexts δξn ⎠ ⎥
s
SMs = ⎢
⎢
⎥
⎥ (7.73)
⎪
⎪ ⎢ ⎛ ⎞
⎥
⎪
⎪ ⎣ ⎜ KsU ⎟ ⎦
⎪
⎪
⎝ δξ
n
⎠
⎪
⎩
0, Internal points.
⎧
⎪
L ( 1−η
⎪ ξn2 −ηP2 )
⎪
⎪ ηz
⎪
⎪ ( P2 )
⎪
⎪ ⎡% & ⎤ , Boundary points.
⎪

⎪
⎪ s + KsU
⎪
⎨ ⎢
1+ KKwr h wexts δξn
⎥
Bs = ⎣ % & ⎦
KsU
⎪
⎪
⎪
⎪
δξn
⎪
⎪
⎪
⎪ L 2 ξ 2 − η2
⎪
⎪ [(1 − ϕ)q̇s + asf h sf Tf )]ξ ηz, Internal points.
⎪
⎩ 1 − η2 ξ 2 − 1
⎪
(7.74)
The coefficients AK , K = P, represent the components of diffusive and convective

heat transfer from the neighboring points toward the P point. The effects of the vari-
able T in on previous time its value in the present time are computed in the coefficient
A0P . These effects are gradually reduced as the process tends to steady-state condi-
tion. The applications of Eqs. (7.53) and (7.64) are restricted to the computational
domain.
Nodal points on the domain contour are not into the set of linear algebra equations
to solve. After the system of equations has been solved, the estimation of the variable
T is performed in these nodal points. For example, for symmetry axes, it is assumed
that the conduction heat flux leaving the point adjacent to the symmetry point is equal
to the conduction heat flux arriving at these points, as illustrated in Fig. 7.9.
These points can be mathematically expressed for the fluid phase, for example,
as follows.
% & % &
Kf 1 − η2 ∂ T Kf 1 − η2 ∂ T
− = − (7.75)
L ξ 2 − η2 ∂η L ξ 2 − η2 ∂η
e w
Thus, by discretizing Eq. (7.75) and rearranging the common terms, the
temperature at the nodal points in η = 0, is given by
⎡ ⎛ ⎞⎤ ⎛ ⎞
(1−ηw2 )
K fw K fw (1−ηw2 )
⎢ ⎜ (ξP −ηw ) ⎟⎥
δηw 2 2 ⎜ δηw (ξP −ηw ) ⎟
2 2
TEf = ⎢ ⎜ ⎟⎥ ⎜
⎣1 + ⎝ 1−η2 ⎠⎦TPf − ⎝ 1−η2 ⎠TWf
⎟ (7.76)
K fP ( e) K fP ( e)
δηe (ξP2 −ηe2 ) δηe (ξP2 −ηe2 )
Fig. 7.9 Schematic

representation of a symmetry
point on face η = 0
The representative equation for determining the fluid phase temperature in the
inner wall of the porous bed (see Fig. 7.7) is given by

KfU h win δξn
Tm + TPf +
Kf
K wr
+
h win
h wext
+
h wext δξn

K wr U
Twinf = (7.77)
KfU win δξn
1 + K wr + h wext + h wext δξn +
Kf h win h
K wr U
7.4 Application: Heat Transfer in an Elliptic Cylindrical

Reactor Filled with Spheroidal Particles
In this chapter, as an application will be considered the heated air flow percolating a
bed of prolate spheroidal particles in the local thermal equilibrium condition and in
steady state. The reactor wall is cooled by water at room temperature T m .
The thermophysical and geometrical parameters used in the simulation can be
seen in Table 7.1.
In the software Mathematica® a computational code was developed to solve
the set of discretized equations, using Gauss–Seidel solution method, considering a
convergence criterion of 10−9 . All results were obtained using a mesh with 20 × 20
×20 control-volumes obtained after some refinements.
Table 7.1 Thermophysical and geometrical parameters used in the simulation

Reactor Air (fluid phase) Particles (solid phase)
L 1 (m) L 2 (m) k f (W/m hwext (W/m2 K) ρ f (kg/m3 ) k s (W/mK) b (m) a (m)
K)
0.05 0.10 2.47 × 2.69 1.09488 5.64 2.5 × 2.0 ×
10−3 10−3 10−3
H (m) K wr (W/mK) uz (m/s) cpf (J/kg K) μf (kg/m ρ s (kg/m3 ) cps (J/kg ϕ
s) K)
0.20 401 0.10 1000 2.025 × 487 5500 0.44
10−5
T m (°C) T 0 (°C) β
30 70 0.85
The results presented here take into account the dimensionless temperature
profiles (T − T m )/(T 0 − T m ) in different xy planes (z/H = 0.0833, 0.5277 and
0. 9722) and on the yz(x/L = 0.0) and xz(y/L = 0.0) planes. Percolating fluid has the
convection heat transfer coefficient (h wint ) calculated by correlations involving the
particle Reynolds number (Beek 1975), as follows:
2ρu z ϕdp
Rep = (7.78)
3μ(1 − ϕ)
The Colburn factor (JH ) and the Stanton number (St ) both for heat transfer are
given as follows (Incropera and De Witt 1992):
JH = 2.06Re−0.575
p (7.79)
and
JH
St = (7.80)
Pr 2/3
Since that the Stanton number is defined by
h
St = (7.81)
ρV cP
we can write
h wint = St ρu z ϕcp (7.82)
Figures 7.10, 7.11, 7.12 illustrate the dimensionless temperature distribution in

the xy plane at different axial positions for the solid and fluid phases. Figures 7.13,
(a) Fluid phase, z/H= 0.0833. (b) Solid phase z/H = 0.0833.
(c) Fluid phase, z/H = 0.5277. (d) Solid phase, z/H = 0.5277.
(e) Fluid phase, z/H = 0.9722. (f) Solid phase, z/H = 0.9722.
Fig. 7.10 Dimensionless temperature distribution within a fixed-bed elliptic cylindrical reactor
filled with prolate spheroidal particles (hwint = 1.03 × 10−4 W/m2 K)
7.14, 7.15 illustrate the dimensionless temperature distribution in the xz and yz planes
for the solid and fluid phases.
Considering the inner wall of the reactor, it can be observed that an increase in
the heat transfer coefficient on the inner wall of the reactor (hwint ) from 1.03 × 10−4
W/m2 K to 40 W/m2 K does not cause significant changes in the temperature field
for both phases inside the reactor. Major changes can be seen in the region near the
outlet (z/H = 0.9722) on the surface (x = L 2 ).
Radial dimensionless temperature gradients are high at the reactor inlet due to the
thermal inlet effects. As the axial position increases along the reactor, these radial
gradients decrease. It can be seen at any axial position along the bed that the radial
dimensionless temperature gradients are slightly most affected by larger for the fluid
phase than the solid phase, and that the region near the reactor surface is more affected
by the cold wall.
(a) Fluid phase, z/H = 0.0833. (b) Solid phase z/H = 0.0833.
(e) Fluid phase, z/H = 0.9722 (f) Solid phase, z/H = 0.9722.
Fig. 7.11 Dimensionless temperature distribution within fixed-bed elliptical cylindric reactor filled
with prolate spheroidal particles (hwint = 2.0 W/m2 K)
In this chapter, the physical problem of heat transfer and fluid flow in a particle-filled
fixed-bed has been studied. Emphasis is given to elliptical cross-sectional reactors.
A transient mathematical modeling written in elliptic cylindrical coordinates
applied to the particulate and fluid phases was proposed, and its numerical solution,
which is based on the finite-volume method, is presented.
Results of temperature distribution within the reactor at different planes have been
presented and discussed. From the results obtained, the following conclusions are
given:
(a) Under the physical point of view the heterogeneous mathematical model proved
to be satisfactory for the study of heat transfer in fixed-bed reactor with an elliptic
cylindrical geometry;
(b) The temperature distribution of the phases indicates that heat flux occurs from
the center toward the reactor wall (angular and radial directions) and in the axial
direction from the inlet to the outlet region;
(a) Fluid phase, z/H = 0.0833. (b) Solid phase z/H = 0.0833.
(e) Fluid phase, z/H = 0.9722. (f) Solid phase, z/H = 0.9722.
Fig. 7.12 Dimensionless temperature distribution within fixed-bed elliptic cylindrical reactor filled
with prolate spheroidal particles (hwint = 40 W/m2 K)
(c) Axial temperature gradients are most relevant in the region near the reactor inlet;
(d) Radial temperature gradients are larger near the reactor wall;
(e) The temperature distribution within the reactor was higher for solid phase as
compared to the fluid phase;
a) Fluid phase (y/L=0.0). b) Fluid phase (x/L=0.0).
c) Solid phase (y/L=0.0). d) Solid phase (x/L=0.0).
Fig. 7.13 Dimensionless temperature distribution of the fluid and solid phases inside the elliptic
cylindrical reactor (hwint = 1.03 × 10−4 W/m2 K)
cylindrical reactor (hwint = 2.0 W/m2 K)
cylindrical reactor (hwint = 40 W/m2 K)
Acknowledgments The authors thank to FINEP, CAPES and CNPq (Brazilian Research Agencies)
for financial support to this research, and also to the researchers for their referenced studies which
helped in improving the quality of this work.
References
Alazmi, B., Vafai, K.: Analysis of variants within the porous media transport models. J. Heat Transf.
122(2), 303–326 (2000)
Beek, W.J., Muttzall, K.M.K.: Transport Phenomena. Wiley, London (1975).
Bunnell, D.G., Irvin, H.B., Olson, R.W., Smith, J.M.: Effective thermal conductivities in gas-solid
systems. Ind. Eng. Chem. Res. Dev. 41(9), 1977–1981 (1949)
Curray, J.K., Griffiths, J.C.: Sphericity and roundness of quartz grains in sediments. Bull. Geol.
Soc. Am. 66, 1075–1096 (1955)
Dixon, A.G., Cresswell, D.L.: Theoretical prediction of effective heat transfer parameters in packed
beds. AIChE J. 25(4), 663–676 (1979)
Dullien, F.A.L.: Porous Media: Fluid Transport and Pore Structure, 2nd edn. Academic Press, San
Diego, USA (1992)
Freire, J.T.: Heat and mass dispersion in flows through porous media. J. Porous Media 7(2), 143–153
(2004)
Froment, G.F., Hofmann, H.P.K.: Design of fixed-bed gas-solid catalytic reactors. In: Carberry, J.J.,
Varma, A. (eds.) Chemical Reaction and Reactor Engineering. Marcel Dekker, Inc., New York
(1987)
Fábrega, F.M.: Calculus of Reactor I. Report. Pitágoras de Jundiaí College, 1st ed. Jundiaí, Brazil
(2012)
Giordano, R.C.: Modeling and optimization of natural gas steam reforming. Doctoural Thesis,
Escola Politécnica, University of São Paulo, São Paulo, Brazil (1991). (In Portuguese)
Grangeot, G., Quintard, M., Whitaker, S.: Heat transfer in packed beds: interpretation of experiments
in terms of one- and two-equation models. Heat Transfer 1994. Inst. Chem. Eng., Rugby, 5,
291–296 (1994)
Handley D, Heggs P.J.: Momentum and heat transfer mechanisms in regular shaped packings, Trans.
Inst. Chem E, 46: paper T251 (1968)
Incropera, F.P., De Witt, D.P.: Fundamentals of Heat and Mass Transfer, 3 edn. LTC—Livros
Técnicos e Científicos Editora S.A., Rio de Janeiro (1992). (In Portuguese)
Lima, A.G.B.: Diffusion Phenomena in Prolate Spheroidal Solids. Studied Case: Drying of Banana.
Doctoral thesis in Mechanical Engineering, State University of Campinas, Campinas, Brazil
Magnus, W., Oberhettinger, F., Soni, R.P.: Formulas and Theorems for the Special Functions of
Mathematical Physics, 3rd edn. Springer, Berlin (1966)
Maliska, C.R.: Heat Transfer and Computational Fluid Mechanics. LCT-Livros Técnicos e
Científicos Editora S. A, Rio de Janeiro (1995). (In Portuguese)
McCabe, W.L., Smith, J.C., Harriot, P.: Unit Operations of Chemical Engineering, 4th edn. McGraw
- Hill International Editions, New York, USA (1985)
McRobert, T.M.: Spherical Harmonics: An Elementary Treatise on Harmonic Functions with
Applications. Pergamon Press, Oxford (1967)
Mendes, N.: Heat and moisture prediction models for building porous elements. Doctoral Thesis,
Federal University of Santa Catarina, Florianópolis, Brazil (1997). (In Portuguse)
Miyauchi, T.S., Furusaki, S., Morooka, S., Ikeda, Y.: Transport Phenomena and Reaction in Catalyst
Beds. In: Drew, T.B., Cokelet, G.R., Hoopes Jr., J. W., Vermeulen, T. (eds.) Advances in Chemical
Engineering, vol. 11, 276–449. Academic Press, New York (1981)
Nield, D.A.: A note on the modeling of local thermal non-equilibrium in a structured porous medium.
Int. J. Heat Mass Transf. 45(21), 4367–4368 (2002)
Nield, D.A., Bejan, A.: Convection in Porous Media. Springer, New York (1992)
Oliveira, L.G.: Heat transfer in packed bed cylindrical-elliptical reactor: thermal-fluid dynamics
and geometric aspects. Doctoral thesis in Process Engineering, Federal University of Campina
Grande, Campina Grande, Brazil (2004). (In Portuguese)
Patankar, S.V.: Numerical Heat Transfer and Fluid Flow. Hemisphere Publishing Corporation, New
York (1980)
Polyaev, V.M., Mozhaev, A.P., Galitseysky, B.A., Lozhkin, A.L.: A study of internal heat transfer
in nonuniform porous structures. Expt. Therm. Fluid Sci. 12, 426–432 (1996)
Quintard, M., Kaviany, M., Whitaker, S.: Two-medium treatment of heat transfer in porous media:
numerical results for effective properties. Adv. Water Resour. 20, 77–94 (1997)
Quintard, M. Whitaker, S.: Theorical Analysis of Transport in Porous Media. In: Vafai, K. (ed.)
Handbook of Heat Transfer in Porous Media, pp. 1–52. Marcel Dekker, Inc., New York (2000)
Saito, M.B., de Lemos, M.J.S.: Interfacial heat transfer coefficient in nonequilibrium convective
transport in porous media. Int. Comm. Heat Mass Transf. 32(5), 666–676 (2005)
Silva, R.M., Lima, A.G.L., Oliveira, L.G., Araújo, M.V., Santos, R.S.: Transient heat transfer in a
packed-bed elliptic cylindrical reactor: a finite-volume approach. Def. Diff. Forum 380, 79–85
(2017)
Silva, R.M., Lima, A.G.B., Pereira, A.S., Machado, M.C.N., Santos, R.S.: Unsteady state heat
transfer in packed-bed elliptic cylindrical reactor: theory, advanced modeling and applications.
In: Delgado, J.M.P.Q, Lima, A.G.B (eds.) Transport Phenomena in Multiphase Systems, vol. 93,
pp. 139–179. Springer International Publishing AG, Cham (2018)
Silva Filho, A.A., Silva de Almeida, J.P., Lima, A.G.B.: Heat transfer inside elliptic cylindrical
reactor: effect of bed porosity. Def. Diff. Forum, 336, 97–102 (2013)
Wakao, N., Kaguei, S.: Effect of fluid dispersion coefficients on particle-to-fluid heat transfer
coefficients in packed beds. Chem. Eng. Sci. 34, 325–336 (1979)
Wakao, N., Kaguei, S.: Heat and Mass Transfer in Packed Beds. Gordon and Breach Science
Wakao, N., Tanaka, K., Nagai, H.: Measurement of particle-to-gas mass transfer coefficients from
chromatographic adsorption experiments. Chem. Eng. Sci. 31, 1109–1113 (1976)

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Advanced Structured Materials

More information about this series at http://www.springer.com/series/8611

ISSN 1869-8433 ISSN 1869-8441 (electronic)

1 Clay Ceramic Materials: From Fundamentals and Manufacturing

3 Foam-Mat Drying Process: Theory and

5.5.3 Results and Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . 122

A. G. Barbosa de Lima, J. M. P. Q. Delgado, L. P. C. Nascimento,

Keywords Drying · Brick · Experimental · Simulation · Lumped model

A. G. B. de Lima (B) · L. P. C. Nascimento · E. S. de Lima · A. M. V. Silva · J. V. Silva

1.1 Ceramic Materials

Following, the ceramic industry underwent major developments, now based on

1.1.2 Fundamental Concepts

1.1.3 The Ceramic Industry and Clay Products

occurrence of mineral resources, abundance of natural gas, expanding market, and

Table 1.1 Types and characterization of red ceramics (Silva 2009)

considered as dispersed mineral systems in which particles below 2 µm in diameter

1.1.4 Red Ceramic Product Manufacturing Process

Fig. 1.1 Manufacturing flowchart of red ceramic pieces

materials, mechanical forming, thermal processing, and shipping. The following

1.1.4.1 Extraction and Preparation of Raw Materials

1.1.4.2 Mechanical Forming

1.1.4.3 Thermal Processing

1.2 The Drying Process

1.2.1 General Principles

Drying can be explained as a thermodynamic process responsible for the partial

A more detailed discussion of drying theories can be found in the literature

1.2.2 The Mathematical Modeling of the Drying Process

The main objective of an appropriated drying modeling is to mathematically describe

1.3 Lumped Model Application: Drying of Clay Ceramic

The focus is to develop a phenomenological mathematical modeling and its analyt-

1.3.1 The Experimental Data

Fig. 1.3 Hollow brick with dimensions

M = A1 exp(k1 t) + A2 exp(k2 t) (1.3)

where t is given in minutes. The A1 , A2 , k 1 , and k 2 parameters were estimated using

where t is given in minutes. Parameters B1 , B2 , K 1 , and B3 were estimated using

1.3.2 Phenomenological Mathematical Modeling

To predict the drying process was developed an advanced and phenomenological

50 0.576178 −0.004711 0.482232 −0.004711 0.997676745 0.995358888

50 −546.0430 283.1605 0.42554 101.18296 0.960840804 0.923215051

(a) Brick is composed of liquid water and solid matter;

1.3.2.1 Geometric and Dimensional Analysis

Vf = aV aH R3 (brick holes volume) (1.5)

V = (R1 R2 R3 ) − (8Vf )(brick volume) (1.6)

S = (2R1 R3 ) + (2R2 R3 ) + 2[(R1 R2 ) − (8aH aV )] + 8[(2aH R3 ) + (2aV R3 )]

where in Eqs. 1.5, 1.6, and 1.7:

aV = (R2 − 2a1 − 3a3 )/4 (height of a hole) (1.8)

aH = (R1 − 2a2 − a4 )/2 (width of a hole) (1.9)

1.3.2.2 Mass Transfer Analysis

where the coefficients a k are specified according to drying conditions.

1.3.2.3 Heat Transfer Analysis

where the coefficients bk are specified according to drying conditions.

1.3.3 Results Analysis

1.3.3.1 Dimensional Variations

50 −0.000862 1.76499 −1099.66 1,381,400 0.98227288 96.486

50 −0.000126 0.259821 −163.671 371,912 0.99130038 98.268

Statistica® software also provides graphs of the estimated functions compared to

1.3.3.2 Drying Process

a 1 = b1 0.15 0.20 0.29 0.21 0.17 0.06

a 2 = b2 95.11 48.35 47.31 39.10 44.57 88.20

a 3 = b3 0.0005 0.0006 0.0005 0.0006 0.0008 0.0009

a 4 = b4 −218.45 −128.91 −85.22 −44.78 −83.38 −194.00

a 5 = b5 −51.82 −14.11 −25.59 −21.74 −27.83 −34.53

a 6 = b6 1829.10 1471.72 1935.06 1545.75 1109.26 1322.77