Chemical Engineering Research and Design 1 4 6 ( 2 0 1 9 ) 78–86

Contents lists available at ScienceDirect

Chemical Engineering Research and Design

journal homepage: www.elsevier.com/locate/cherd

Drying of Maltodextrin solution in a vacuum spray

dryer

Fernanda de Melo Ramos a,∗ , Job Ubbink b , Vivaldo Silveira Júnior a ,

Ana Silvia Prata a
a Department of Food Engineering, Faculty of Food Engineering, State University of Campinas, P.O. Box 6121,
13083-862 Campinas, SP, Brazil
b Food Science and Nutrition Department, California Polytechnic State University, San Luis Obispo, CA 93442, USA

a r t i c l e i n f o a b s t r a c t

Article history: New drying strategies that use low temperatures can have a significant impact on the
Received 25 September 2018 improvement of food quality, in particular regarding the retention of flavor compounds,
Received in revised form 11 March bioactives and other thermosensitive components. The vacuum spray dryer (VSD) is a spray
2019 dryer that operates with a low-pressure drying chamber, which consequently reduces the
Accepted 24 March 2019 increases the thermodynamic driving force for water removal and allows drying at sig-
Available online 1 April 2019 nificantly reduced temperatures. In order to understand the process behavior and define
operational strategies, a mathematical model that encompasses mass and energy balances
Keywords: was validated with experimental measurements of pressure and temperature during drying
Drying modelling of large chained maltodextrin (dextrose equivalent = 10). Results from experiments carried
Energy balance out in a pilot VSD present a good fit with the proposed model and confirmed its underlying
Maltodextrin assumptions. In addition, comparative analyses were performed regarding physical aspects
Glass transition of particles produced by VSD and by conventional spray dryer (SD) in the same equipment,
Spray drying but without vacuum. Under the tested conditions, VSD particles presented a higher moisture
Vacuum content (8%) and smaller time of wettability than SD particles. The morphological changes
were caused by the vacuum and can be interesting for technological applications.
© 2019 Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.

1. Introduction
Spray drying is a process that transforms a liquid raw material into
dried particles by atomizing the solution into a hot drying medium
(Keshani et al., 2015). The atomization produces very small droplets
that are able to efficiently evaporate the water in the very short res-
idence time in the drying chamber. However, as a result of the high
temperatures that are typically above 130 ◦ C, degradation reactions can
be induced in thermo-sensitive compounds such as vitamins, flavors
or lipids, resulting in decreased quality of the product even after a few
seconds of exposure (Anandharamakrishnan et al., 2007; Belingheri
et al., 2015; Fu and Etzel, 1995; Ixtaina et al., 2015; Jafari et al., 2008;
Menshutina et al., 2010; Mestry et al., 2011; Tonon et al., 2009; Tsotsas,
2012; Wijlhuizen et al., 1979; Zare et al., 2012). In addition, in conven-
tional spray drying, the materials are exposed to high levels of oxygen,
owing to the large amounts of air used in the drying process and the
turbulent flow characteristics in the drying chamber.
In this context, new drying strategies that use low temperatures
and avoid the use of air can have a positive impact on the retention
of bioactive compounds. An electrostatic spray-dryer, for example, by
polarity differences is claimed to promote the migration of polar com-
pounds, such as the solvent and the carrier, to the outer surface of the
droplet, improving the active compound retention. The external avail-
ability of water favors the evaporation process requiring lower inlet
temperatures. The patent claims that inlet temperature ranges from
25 ◦ C to 110 ◦ C (Sobel et al., 2016). Similar technology was launched by
®
Fluid Air, known as PolarDry , and tests have been done to potential
products.

∗
Corresponding author.
E-mail addresses: fernandalp29@hotmail.com (F. de Melo Ramos), jubbink@calpoly.edu (J. Ubbink), vivaldo@unicamp.br (V. Silveira
Júnior), asprata@unicamp.br (A.S. Prata).
https://doi.org/10.1016/j.cherd.2019.03.036
0263-8762/© 2019 Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.
 Chemical Engineering Research and Design 1 4 6 ( 2 0 1 9 ) 78–86 79

Nomenclature

Acronyms
C.V. Control volume
dm/dt Mass accumulate in the system over the time
Ṁinlet Mass flow rate of the inlet streams [kg/s]
Ṁoutlet Mass flow rate of the outlet streams [kg/s]
F Feed solution stream [kg/s]
Ai Atomization air stream (inlet) [kg/s]
Ao Air stream carrying the water evaporated (out-
let) [kg/s]
P Product stream [kg/s]
Gi Mass flow rate of atomization dry air in the inlet
of dryer [kg dry air/s] Fig. 1 – Global scheme of streams in the VSD.
Go Mass flow rate of dry air in the outlet of dryer
[kg dry air/s]
XF Mass fraction of water present in the feed solu-
In the same way, the vacuum spray dryer introduced in this study
tion [kg water/ kg feed solution]
is a drying technology under development (Ramos et al., 2016a, 2016b)
XP Mass fraction of water present in the product
that combines the advantages of the atomization, by increasing the sur-
[kg water/ kg product]
face area to improve the heat transfer, with the same strategy used for
Yi Absolute humidity of the atomizing air at the freeze-drying process, i.e., the reduction of the pressure inside the dry-
inlet [kg water/ kg dry air] ing chamber for decreasing the evaporation temperature of the water.
Yo Absolute humidity of the air at the outlet [kg of This combination of factors enables the processing of sensitive prod-
water/ kg dry air] ucts in a reduced time comparatively to freeze drying processes and
HF Enthalpy of the feed solution [J/s] under conditions that minimize product degradation.
Hi Enthalpy of the atomization air (inlet) [J/s] The operation principle of a VSD can be subdivided into three steps
HP Enthalpy of the product [J/s] that take place inside the drying chamber under vacuum, as shown in
Ho Enthalpy of the outlet air [J/s] the control volume (C.V.) around the nozzle (Fig. 1).
The first step, described as contact, occurs when the feed solution
Ha Enthalpy of the air stream (dry air (g) + water
enters in contact with the atomization air, in co-current flow, still inside
vapor (v)) [J/s]
the atomizing nozzle. The two stream entering in the system are those
Hstream Enthalpy of the stream containing solids [J/s]
from the feed solution and from the atomization air. Contrary to con-
Q Heat flow from the environment to the system ventional spray drying processes, the VSD’s chamber is not fed with
[J/s] a hot air stream and, as the only air that flows into this dryer is the
Cpg Specific heat of the air at the inlet and outlet compressed air used in the atomization, the low pressure inside the
streams [kJ/kg ◦ C] chamber can be maintained.
Cpv Specific heat of vaporization [kJ/kg ◦ C] Secondly, in the expansion step, the droplets of the feed solution
Cps Specific heat of the solids [kJ/kg ◦ C] are exposed to the low pressure inside the drying chamber. If its vapor
Cpw Specific heat of the liquid water [kJ/kg ◦ C] pressure of the water in the droplets is higher than the water vapor
pressure inside the chamber, part of the water molecules in the liquid
 Latent heat of vaporization [kJ/kg]
phase will evaporate driven by the mass gradient, since the vapor is not
Ta Air temperature [◦ C]
saturated. Subsequently, for continuing the evaporation of the liquid,
Tref Reference temperature (Tref = 0 ◦ C)
the latent heat of vaporization must be supplied by the internal energy
Ts Temperature of the product [◦ C] of the liquid. As the consequence, the evaporating droplet will reach
Tw Liquid water temperature [◦ C] the wet bulb temperature. With the established temperature gradient
Pw Partial pressure water vapor [kPa] (Tvapor –Twet bulb ), the evaporation step achieves a steady state that will
Pt Total pressure of the system [kPa] continue while there is excess of the water phase in the droplet. During
Ps Saturation vapor pressure [kPa] the evaporation step, a water content gradient in the drying droplet
ϕ Relative humidity [%] will be formed. Under certain conditions, a crust may be formed, with
Tg Glass transition temperature of the system [◦ C] kinetics depending on the glass transition of the material and the water
Tg,m Glass transition temperature of the dry matrix content dependence of the diffusion coefficient of water (Parker and
Ring, 1995). This crust, when formed, helps to avoid the sticking of the
[◦ C]
material to the wall of the dryer (Adhikari et al., 2007a) but also hinders
Tg,w Glass transition temperature of the water [◦ C]
the migration of the water phase to the surface because of the low rates
Qs Weight fraction solids in system [kg solids/ kg
of diffusion of water at low water contents (Räderer et al., 2002). All
total] these steps occur simultaneously inside of the drying chamber.
Qw Weight fraction water in system [kg water/ kg For spray drying, the basic phenomena include numerous aspects
total] of fluid mechanics, heat and mass-transfer, particle technology, and
kGT Gordon-Taylor coefficient materials science (Chen, 2004) and a number of models are available
in the literature whether as looking for the droplets drying kinetics
(Huang et al., 2003; Mezhericher et al., 2010; Woo et al., 2008) or flow
fields of the drying agent/particles (Kieviet, 1997; Langrish et al., 2004;
Zbiciński, 1995). Both aspects can be solved using discrete approxima-
tions Eulerian-Lagrangian by computational fluid dynamics (CFD) due
in part to the complexity of the gas and particle flow patterns and in
part to the overall complexity of the spray drying process (Kuriakose
and Anandharamakrishnan, 2010; Langrish, 2009).
80 Chemical Engineering Research and Design 1 4 6 ( 2 0 1 9 ) 78–86
Fig. 2 – Scheme of process and instrumentation of the vacuum spray dryer (VSD).
An alternative approach is coarse-scale modeling that can deter-
mine in a relatively simple manner the processes conditions to be used
for short-chamber spray dryers based on a limited number of well-
chosen assumptions (Langrish, 2009). The heat and mass transfer rates
from the droplets to the gas phase are estimated, assuming well-mixed
conditions inside the chamber as well as equilibrium between the gas
and particles in the outlet.
Drying in a vacuum spray dryer is an expensive technology. A
detailed and quantitative understanding of the process is therefore
needed to optimize process parameters and reduce the costs of a poten-
tial commercial technology. For this reason, we perform experiments
in the laboratory on pilot scale, which we corroborate with a modeling
approach. In the present work, a coarse-scale approach was used to
develop a mathematical model based on overall mass and energy bal-
ances in the spray dryer. This model was validated through the drying
of a maltodextrin solution by the vacuum spray drying process.
2. Experimental design
A VSD model equipment was developed based on previ-
ous studies of Ramos et al. (2016a, 2016b) and consists in a
sequence of vacuum pumps (0.3–0.9 kW), with rotary vanes,
adapted to a cylindrical-cone chamber to promote low pres-
sure condition, as shown in Fig. 2. A double fluid atomizer
(Labmaq, Brazil) is located at the top of the drying chamber
and a small amount of air is supplied from a compressor MSV
6 (Schulz, Brazil) to allow the atomization. The stainless steel
drying chamber is 200 mm in diameter and 680 mm tall. The
cyclone has a total height of 540 mm and its largest diameter is
95 mm. The system instrumentation used three temperature
sensors (resistance thermometers) to measure the air temper-
ature at several spots in the system (TT 101 to 103 in Fig. 2).
Inside the vacuum line, a pressure sensor (PCG-750, Agilent
Technologies) was placed to monitor the vacuum level (PT101
in Fig. 2). In this setup a relative humidity and temperature
sensor (RHT-WM, Novus, Brazil) is located (MT101 and TT 103
respectively in Fig. 2).
A solution of 40% w/w of maltodextrin DE 10 (MOR-REX
DE 10, Ingredion, Brazil) was prepared by dissolving the mate-
rial in deionized water at 25 ◦ C for 24 h. The atomization of
the maltodextrin solution was performed using a peristaltic
pump (Masterflex, United States) with atomization airflow of
1.2 m3 /h at a pressure of 94.24 kPa and a temperature of 26.9 ◦ C.
The pressure inside the chamber was kept around at 27 kPa.
After that, a flow rate of 0.008 g/s was used, for 3 repetitions.
Data of these trials are reported in this work. During the exper-
iments, temperature and relative humidity data were acquired
every 30 s using an Arduino-Radiuíno platform and software
Scada BR for the data acquisition by a computer.
The same solution was dried in conventional spray dryer
(MSD 1.0 model, Labmaq, Ribeirão Preto, Brazil) in order to
compare particles produced by the two techniques. The flow
rate of the drying air was 81 m3 /h, the air pressure was 4 bar,
the compressed air flow rate was 2.4 m3 /h, and the feed rate
was 0.0007 m3 /h. The temperature of the drying air was set at
190 ◦ C.
2.1. Characterization of the powders
2.1.1. Moisture content and water activity
The moisture content of the dried powders was determined
gravimetrically at 105 ◦ C ± 5 ◦ C until constant weight following
the official AOAC method (AOAC, 2006). Each powder replicate
was tested in triplicate.
Water activity (aw ) of the particles was measured at 25 ◦ C
in triplicate by a water activity analyzer (AquaLab Series 3TE,
Decagon, Pullman, USA).
2.1.2. Scanning electron microscopy (SEM)
The samples were coated under vacuum with gold in a
Sputter-Coater EMITECH unit (K450, Kent, UK). The thickness
of gold layer is estimated to be 200 Å.
The micrographs were obtained in a scanning electron
microscope with Energy Dispersive X-ray Detection (SEM: Leo
440i, EDS: 6070, SEM/EDS: LEO Electron Microscopy/ Oxford,
Cambridge, England). The analyses were performed with an
accelerating voltage of 5 kV and a 50 pA beam current to obtain
the micrographs.
2.1.3. Particle size distribution and mean diameter
Size distribution and mean diameter of powders were deter-
mined by light scattering technique using laser diffraction
(Mastersizer Hydro 2000 MU, Malvern Instruments Ltd.,
 Chemical Engineering Research and Design 1 4 6 ( 2 0 1 9 ) 78–86
Malvern, UK). The mean diameter was determined based on
the mean diameter of a sphere of the same volume, the
Brouckere diameter (D43 ) (Eq. (1)). The samples were analyzed
by wet method, with dispersion in 99.5% ethanol.
 4
ni .di
D[4,3] = 
3
ni .di
where, di is the average particle diameter and ni is the number
of particles.
2.1.4. Wettability
Samples of each powder (∼1 g) were spread on the surface of
a beaker containing 100 mL of distilled water at 25 ◦ C without
stirring in order to determine the wettability of the powders
(Fuchs et al., 2006). The time spent for immersing or wetting
the last particle of powder was used as wettability response of
the samples.
2.1.5. Tapped density
Tapped density in g. cm−3 was determined by measuring the
volume occupied by 2 g of powder sample in a 50 ml gradu-
ated cylindrical glass tube (24 mm diameter, 198 mm height) at
room temperature (Goula and Adamopoulos, 2004) after tap-
ping the bottom of cylinder for ten times on a hard surface
with interval of two seconds between each beat. The tapped
density was calculated as ratio between mass to volume. This
analysis was performed in triplicate.
3. Model development
3.1. Mass balance
˙ psychometric correlations for the environmental air, entering
The general mass balance, in mass flow rate (M), for the VSD
can be written as:
dm  
= Ṁinlet − Ṁoutlet
dt
The model is solved using overall mass and energy bal-
ances, and the C.V. chosen for the study of the process was
the drying chamber (Fig. 1). Thus, one can find in the inlet, the
feed solution stream (F) and atomizing air stream (Ai ), and in
the outlet, the air stream carrying the water evaporated (Ao )
and the product stream (P). No chemical reactions occur in the
material and the mass of product accumulated outside of the
control volume (Figs. 1 and 2) was considered to be negligible
(dm/dt = 0). Thus, the general mass balance in the VSD can be
described as:
(F + Ai ) = (P + Ao ) [kg/s]
Inside the chamber, the medium consists of three phases:
solid (s), liquid (l) and gas (g). The stream Ai is a moist air
stream, and it is constituted by water vapor (v) and dry air (G).
The G streams, in the inlet (i) and in the outlet (o) of the dryer,
are exactly the same. Then, the mass balance for the water
component, in wet basis, can be described as:
(FXF + Gi Yi ) = (PXP + Go Yo )
For the solid components, we have:
F (1 − XF ) = P (1 − XP )
81
3.2. Energy balance
The general energy balance in the VSD can be obtained by an
enthalpy balance in each stream in the C.V.. In this way, the
energy balance becomes:
(1)
(FHF + Gi Hi ) = (PHP + Go Ho ) (6)
However, this process can be not completely adiabatic,
as some heat exchange between the system and its neigh-
borhood occurs. A term of the losses or gain in enthalpy
is therefore inserted in the balance equation. The gain can
occurs if the temperature inside the chamber is very low,
resulting in a heat flow from the environment to the chamber,
and thus:
(FHF + Gi Hi + Q) = (PHP + Go Ho ) (7)
whereby Q is the energy supplied to the drying chamber. For
the air stream (dry air (g) + water vapor (v)), the enthalpy may
generically be stated by the equation:
    
Ha = Cpg Ta − Tref + Y  + Cpv Ta − Tref (8)
where, the specific heat of the air was calculated at the cor-
respondent temperature of the stream (Jumah et al., 1996)
and for Cpg the value of 1.04 kJ kg−1 C−1 at the inlet and
outlet streams was used. The specific heat of vaporization,
Cpv , was estimated as 1.8 kJ kg−1 C−1 , and the latent heat of
vaporization, ␭, was taken at wet bulb temperature as 2500 kJ
kg−1 (Zhang et al., 2011) Ta is the air temperature (in ◦ C) and
Tref = 0 ◦ C is the reference temperature.
The air absolute humidity (Y) was estimated using the
with the temperature of the air in the following equation (Keey,
1978; Strumillo and Kudra, 1986):
(2)
Y = 0.622Pw /(Pt − Pw ) (9)
where, Pw is partial pressure water vapor and Pt is the total
pressure of the system. In the inlet stream the pressure was
94.24 kPa, whereas in the outlet stream was 29.33 kPa.
At the inlet of the dryer, the air temperature (Ta ) was
26.94 ◦ C and the relative humidity was 44.68%. Firstly, the max-
imum vapor pressure at the inlet air temperature, i.e., the
saturation vapor pressure (Ps ), needed to be calculated. One
way of calculating it was through the Antoine equation, one
version of which is (Langrish, 2009):
 3816.44

Ps (Pa) = 133.3 exp 18.3036 − (10)
(3) T (◦ C) + 229.02
The partial pressure of water vapor divided by the sat-
uration vapor pressure is the relative humidity(ϕ), which is
commonly expressed in %. Therefore, using the Eqs. (9)–(11),
we have that the saturation pressure and the partial pressure
water vapor was calculated as 3.53 and 1.57 kPa respectively.
Pw
ϕ= . 100% (11)
Ps
(4)
In the outlet stream, the air temperature (Ta ) was 26.86 ◦ C
and the relative humidity was 14.8%. Consequently, using Eqs.
(9)–(11) we have that the saturation pressure and the partial
(5) pressure water of vapor was calculated as 3.52 and 0.52 kPa
82 Chemical Engineering Research and Design 1 4 6 ( 2 0 1 9 ) 78–86
Table 1 – Characterization of the streams.
Parameters Inlet
Feed solution
ṁ [g/s] 0.008
Xi [kg water/ kg total] 0.600
Y [kg water/kg dry air] – 0.0106
where ṁ =mass flow of the stream.
respectively. Thus, the absolute humidity values in the inlet
and outlet conditions was calculated as 0.0106 and 0.0112 kg
water vapor/kg dry air respectively.
The enthalpy of the stream containing solids (F and P) is
given by sum of the enthalpy of water and solids and can be
described, in a generic way, by the equation:
ˆ     ization of the feed and the time to water evaporation is thus
Hstream = Cps Ts − Tref (1 − Xi ) + Cpw Tw − Tref (Xi ) (12)
For the specific heat of solids, Cps , a value of 1.5 kJ kg−1
C−1 was used (Frías et al., 2001) and the specific heat of
liquid water, Cpw is 4.18 kJ kg−1 C−1 (Baik et al., 2001). The
enthalpy was calculated in the correspondent temperature of
the stream (i.e., 24 ◦ C (F stream) and 26.9 ◦ C (P stream)). Ts is
the temperature of the product, ◦ C, considered in equilibrium
with Tw , the liquid water temperature, ◦ C.
4. Results and discussion
Drying process normally involves high temperatures which
causes sensorial and nutritional changes in food products
and convective air to accelerate the heat and mass transfer
and which consequently increments the oxygen supply. Both
parameters are harmful for thermo-labile and oxidable prod-
ucts as vitamins, colorants and oils.
Also, at these conditions, a high energy consumption is
required due to the latent heat supply for water evaporation,
the sensible heat for heating the air and the energy require-
ments for blowers. For example, in a conventional spray dryer,
about 3900 W of energy-input is required to process 1 kg/s of
a 40% w/w solution using 15 kg/s of dry airflow (0.01 kg water
vapor/kg dry air). From this amount, 85% of the energy is used
to heat the air stream (m.Cp .dT) up to the inlet temperature
of the spray dryer (200 ◦ C). High temperatures are required
by considering the small residence time of the particles in
the path of the spray dryer, which is around 4 s (Birchal and
Passos, 2005). However, when observing the water withdrawal
potential of a stream of dry air, which is ideally the adiabatic
saturation limit, it is seen that air exits with about 60% of its
water saturation capacity, indicating that this energy portion
can be optimized by reducing the temperature or the air flow
employed.
In the VSD developed in this work, auxiliary air is not
employed for that the drying occurs and due to significant
reduction of the amount of oxygen in the chamber, the
quality of products prone to oxidation can be improved. Dry-
ing can account for 60–70% of the total energy consuming
of a process (Bahu, 1991) and therefore the evaluation of
drying systems regarding sustainability beyond the require-
ments of product quality have a strong interest to allow its
implementation.
Outlet
Air inlet Product Air outlet
0.359 0.003 0.359
– 0.079 –
– 0.0112
Some discussions in the literature consider the energy sav-
ing of vacuum systems as much inferior to convective dryers
(Motevali et al., 2014, 2011). The main reason for that, as for
freeze-dryers, is the thickness of the product layer that lim-
its the diffusion of water through the material, increasing
the processing time. However, in the VSD, the exposed area
is higher than in conventional vacuum drying due to atom-
significantly reduced. On the other hand, conventional spray
dryer has a blower and a heater, which, for the MSD 1.0 model
(Labmaq, Ribeirão Preto, Brazil) that we employed together
add up to 4000 W of power. The vacuum system used in this
work has three vacuum pumps which consume less than half
(1500 W) of this energy.
While we recognize that this prototype has some limita-
tions, it turns out that these are mainly related to the design
parameters of the dryer, and not to the intrinsic physics of the
process. The drying process could be conducted even without
external energy source. As part of furthering the innovation
of this equipment, the prototype developed in this work is
being improved taking into account the results and analysis
reported in this article. Our current results however already
show that for the mass flow as applied here (0.008 g/s), the
VSD uses about 25% less energy (102.6 J/ kg) in comparison
with a conventional spray dryer (424.2 J/ kg). The total energy
involved by a SD is higher than that used for VSD due to the
heating of the flow air. Of course, a higher thermal input would
allow greater transfer of energy to the system, providing better
conditions for water evaporation and favoring an increase of
the flow rate of the solution. Thus, even with additional heat
supplied to the process to improve the flow rate, the VSD can
not be considered more energy expensive than conventional
SD.
All values of incoming and outgoing stream in the drying
chamber required by the mass balance were experimentally
determined and these values are presented in Table 1.
The energy balance developed considers that one part
of the heat required to evaporate the water is supplied by
the environment. The parameters used and results from this
energy balance developed can be seen in Table 2.
In the literature, a limited number of studies (Aoyama et al.,
2009; Islam et al., 2017, 2016; Kitamura et al., 2009; Ramos et al.,
2016a, 2016b; Semyonov et al., 2011) are published with dry-
ers based on the vacuum principle. Several groups employed
infrared heaters installed near the atomizer (Aoyama et al.,
2009; Kitamura et al., 2009) to supply energy through electro-
magnetic waves as auxiliary source of heat for evaporation. In
another study (Islam et al., 2017, 2016) superheated steam at
200 ◦ C was used. All the groups circulated hot water at 50 ◦ C
inside the chamber jacket to increase the temperature of the
inner wall of the chamber and prevent the sticking of materi-
als to the wall. Our study is different in this respect, as there
 Chemical Engineering Research and Design 1 4 6 ( 2 0 1 9 ) 78–86
Table 2 – Energy parameters of inlet and outlet stream in VSD.
Parameters Inlet
Gi F Q
h [kJ/kg] 55.1 74.6
H [J/s] 19.78 0.59
T [◦ C] 26.9 24
a
Calculated value from energy balance.
Fig. 3 – State diagram of maltodextrin DE-12. The state
diagram is composed of the ice melting line Tm , the boiling
line Tb , the glass transition line Tg and the glass transition
temperature of the maximally cryo-concentrated state Tg’ .
Tb is plotted atmospheric pressure (101.35 kPa;
conventional spray drying) and a pressure of 3.5 kPa
(vacuum spray drying). As maltodextrins do not show a
clear crystallization limit, the solubility line, commonly
plotted for simple carbohydrate-water systems, is omitted.
The approximate process routes for conventional and
vacuum spray drying are indicated by the dashed arrows,
which represent the sample trajectory from the initial
solution at 0.4 w/w maltodextrin content to the final
powder with a water content of 0.08 w/w. The state
diagram is compiled using data from Kilburn et al. (2005).
was no external way of supplying vaporization heat to the sys-
tem, not even in the feed solution that was processed at room
temperature.
In a schematic state diagram (Fig. 3), the pathway for the
process vacuum operated as well as the pathway that repre-
sent the evaporation of the water in the conventional process
are indicated by dotted lines.
The dried sample is a model product, consisting of pure
maltodextrin with a dextrose equivalent (DE) of 10 and a glass
transition temperature in the dry state of 164 ◦ C (Kilburn et al.,
2005). These characteristics enable a more efficient drying by
reducing the sticking of the material to the wall of the spray
dryer when compared to carbohydrates of lower molecular
weight. Sticking occurs when the viscosity of the material
is sufficiently low, i.e., in the early stages of the drying, and
the empirical parameter to quantify the propensity to stick-
ing, the so-called, sticky point, was shown to be related to
the glass transition temperature (Tg ) of the material to be
dried (Roudaut et al., 2002). The Tg , in turn, is influenced
by both the molecular weight of the material and its water
content.
83
Outlet
Go P
– 56.6 46.0
0.09a 20.31 0.14
– 26.9 26.9
The dependence of the glass transition temperature on the
water content can be modeled by the Gordon-Taylor equation
(Gordon and Taylor, 1952):
T g,m .Q s + kGT .Q w .T g,w
Tg = (13)
T g,m + kGT .T g,w
where, Tg , Tg,m , Tg,w : glass transition temperature of system,
dry matrix and water, Qs , Qw : weight fraction solids and water
in system, kGT : Gordon-Taylor coefficient, and for maltodex-
trin corresponds to 7.3.
Equation (13) is conventionally used to fit the water con-
tent dependence of the glass transition temperature of food
materials to determine the end point for drying. If the glass
temperature of one component is increased, the glass transi-
tion temperature of the system is increased as well, implying
in that the amount of water that needs to be removed is lower
to reach the glassy state. In addition, the drying is aided by
the high solids content of the feed, which further limits the
amount of water that needs to be removed during the drying
operation. The current material is therefore not very sensitive
to sticking that often occurs in spraying towers and that is
due to the high product’s outlet temperature relative to its Tg .
Such more sensitive materials remain in the rubbery state at
the end of the drying (Adhikari et al., 2007a, 2007b, 2004).
The critical condition for any spray drying process is the
water content below which the powder is in the glassy state at
either the outlet temperature of the dryer or the storage or the
storage temperature of the powder. For a storage temperature
of 25 ◦ C, the powder is at the glass transition for a weight frac-
tion water of 0.103 (wet basis). For any water content below this
value, the maltodextrin powder will thus be in the glassy state.
As the powder after drying in the VSD attained at water con-
tent of 0.079 kg water/kg product, the powder is in the glassy
state after drying. We conclude that the current vacuum spray
process is able to dry solutions and dispersions to a sufficient
extent to allow the production of physically-stable powders,
notwithstanding that its water content is higher than that
which is normally obtained using a conventional spray dryer
(water weight fraction in the range of 0.04) (Fang and Bhandari,
2012), can be considered stable. While the water content of the
current powder prepared by VSD is low enough for the powder
to be in the glassy state, it is still higher than what is usually
considered to be optimal in case oxidation sensitive bioactives
are encapsulated in the maltodextrin matrix. A further lower-
ing of the water content should is definitely be possible using
our process, the goal of our research is however to demon-
strate that we could obtain a powder in the glassy state using
the VSD, not to fully optimize powder stability in the light of
the stability of a potential encapsulant.
The powder obtained in VSD was apparently more porous
(Fig. 4b) when compared to the equivalent powder obtained in
conventional spray dryer using the same nozzle and solution
of maltodextrin in the same concentration.
84 Chemical Engineering Research and Design 1 4 6 ( 2 0 1 9 ) 78–86
Fig. 4 – SEM micrographs of particles obtained by spray
dryer and vacuum spray dryer.
The conventional spray drying process implies an inten-
sive moisture evaporation at the surface of droplets, and the
heat of evaporation of water is responsible to keep the droplets
at the wet bulb temperature until the evaporation of water is
significantly restricted by low diffusion rates at the low mois-
ture crusty formed at the particle surface. The driving force
for water removal in this process is much higher than in VSD
and the evaporation process impacts on the development of
the particle morphology.
In the case of spray drying, the high pressures gener-
ate inside of particles can produce particles that inflate
(Fig. 4a) significantly producing smooth and spherical sur-
faces (Oakley, 1997). Under vacuum, the particles will also
puff and porous channels are formed, which is a well-known
phenomenon occurring in freeze–dried materials and can be
attributed to the expansion of air and water vapor at sub-
ambient pressures (Motevali et al., 2014). But we hypothesize
that two more reasons are responsible for the observed behav-
ior. In VSD, the water vapor is more evenly released due the
longer time took to form the surface crust in contact with the
drying environment. This can reduce the resistance to mass
transfer close to the particle surface as the water diffusion
coefficient is very low in the crust. This effect is reinforced
by the migration rate of water from the matrix being more
homogeneous due to the lower driving force for heat and mass
transfer, further reducing the internal pressure. Another fac-
tor that could have an influence is that the water removal
becomes more difficult over time due to an increased vis-
cosity linked to the low temperatures, which is additionally
be responsible to restrain the formed structure from inflating
(Fig. 4b). The difference between the driven force between the
Table 3 – Moisture content, water activity, wettability, apparent density and mean diameter of the powders produced in
conventional SD and VSD.
Equipment Moisture content (%) Water activity (aw )
Spray dryer 1.13 ± 0.22a 0.043 ± 0.006a
Vacuum spray dryer 7.88 ± 0.09b 0.381 ± 0.003b
Different letters indicate statistically significant differences between the samples produced in the different types of equipment (p ≤ 0.05).
Fig. 5 – Particle size distributions for the particles produced
in VSD and conventional spray dryer.
processes, conventional spray dryer and VSD, is an important
factor to be understood for explaining the differences between
the structures formed.
Results of moisture content, water activity, wettability,
apparent density and mean diameter obtained for the par-
ticles produced in the SD and VSD are shown in Table 3.
Particles produced by VSD were significantly different from
those obtained with SD. Wettability is the time required for
water to imbibe to the particles until they sediment. The wet-
tability of VSD particles was approximately 7 times lower than
the particles from SD (Table 3). This is most likely related to
the porous structure formed by these particles in VSD, which
can be represented by their higher apparent density. The mean
diameter of particles can contribute with this effect, because
smaller particles tends to be together and hinder the water
hydration.
In principle, the mean diameter of particles produced by
atomization depends on the type of atomizer (Filkova and
Mujumdar, 1995). However, even though the same atomizer
was used, particles produced by VSD were larger (159 ␮m) than
SD particles (88 ␮m) – Table 3. However, as can be seen in Fig. 5,
the size distribution occurs in two peaks. The first one, in about
20 ␮m, represents the size of VSD particles that, as expected,
presented some morphological alterations as compared to SD
particles (50 ␮m). The peak at 500 ␮m refers to the recovered
powder from the wall of the VSD. The particles recovered from
the wall of the drying chamber in this process were larger.
For SD, the size measurement was done only on particles col-
lected in the cyclone. These observations are consistent with
the morphology of the particles shown in Fig. 4. The value of
the polydispersity index (PDI) indicates the degree of unifor-
mity of the distribution. For VSD particles, the value obtained
was 17.2 while for powders obtained by SD it was 3.46, which
confirms the less uniform size distribution for VSD particles.
We discard the possibility of agglomeration, because at the
final moisture content (7%) reached at the end of vacuum dry-
ing process, the water activity of 10 DE maltodextrin is 0.65.
Wettability (s) Apparent density (g/cm3 ) Mean diameter (␮m)
1341.00 ± 28.00b 0.286 ± 0.016a 87.68 ± 13.68a
192.00 ± 20.07a 0.412 ± 0.004b 159.51 ± 4.78b
 Chemical Engineering Research and Design 1 4 6 ( 2 0 1 9 ) 78–86
Agglomeration would only be important if relative humidity
of drying environment (45%) were higher than 65%.
5. Conclusion
A conventional spray dryer was adapted to be operated under
vacuum and was evaluated by the drying of atomized droplets
of a DE 10 maltodextrin solution. We adopted a coarse-grained
mathematical model to account for the heat and mass bal-
ances in this system, and we validated it with data of pressure
and temperature acquired on line. The results show that the
proposed mathematical model represents the process well.
As the vacuum drying process takes place without external
source of heat, the saves VSD energy when compared with
freeze drying and conventional spray drying processes. Also,
as the process does not involve an air stream, the oxygen
availability inside the chamber is reduced. This should bring
significant benefits in the drying of oxygen sensitive bioactive
compounds. Because the lack of an external heat source, only
a very low amount of solution could be processed. Notwith-
standing, the drying kinetics in the VSD are sufficiently fast to
enable the conversion of the maltodextrin DE 10 solution into
an amorphous powder in the glassy state at the end of the
drying process. The powder characteristics of both processes
were significantly different, and the VSD particles showed a
porous aspect contributing with their wettability. However,
the effect of internal pressure of the chamber on the particles
characteristics warrants further exploration. The evaluation
of the moisture content and water activity of atomized mate-
rial during the process may help to design a new dryer that
allows to optimize direct correlating with the product quality.
Acknowledgement
This study was financed in part by the Coordenação de
Aperfeiçoamento de Pessoal de Nível Superior – Brasil (CAPES)
– Finance Code 001.
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