Professional Documents
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BY:
(2020-2024)
APPROVAL SHEET
This Project Work entitled “Overview of membrane technology and its applications in
fruit juice processing” by Abhiram Kalluri, Mankala Karthik, G C S Vignesh, Manish Saini,
Jithesh Kumar and Harish H R, are approved for partial fulfilment of the second-year,
Bachelor of Technology in Chemical Engineering, Department of Chemical Engineering,
NIT-Andhra Pradesh.
Supervisor (s):
________________________
________________________
Examiners:
________________________
________________________
Chairman:
________________________
Date: ____________
Place: ____________
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DECLARATION
We declare that this written submission represents my ideas in my own words and where
others' ideas or words have been included, I have adequately cited and referenced the original
sources. I also declare that I have adhered to all principles of academic honesty and integrity
and have not misrepresented or fabricated or falsified any idea/ data/ fact/ source in my
submission. I understand that any violation of the above will be cause for disciplinary action
by the Institute and can also evoke penal action from the sources which have thus not been
properly cited or from whom proper permission has not been taken when needed.
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CONTENTS
1. Approval Sheet
2. Declaration
3. Abstract
process-------------------------------------------------------------------------- 19
13.Bibliography ------------------------------------------------------------------26
14.Acknowledgements 27
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ABSTRACT
Membrane technology encompasses the related scientific and engineering approaches for the
transport or rejection of components, species, or substances through or by the membranes.
The concept of membrane-based separation has been introduced since the 18th century and
regarded to have advantages over most conventional separation processes, e.g., distillation,
adsorption, and absorption.
In the process of fruit juice clarification, the main intention is to increase the shelf life of the
juice, keeping in mind the natural flavour and nutritious components of the juice. Membrane
technology has evolved as an efficient and cost-effective alternative to the traditional thermal
processing of fruit juices, that comes at a cost of the depletion of natural flavour as well as
degradation of nutrients from the juice.
However, the biggest challenge in the membrane technology is the fouling of membranes
which greatly effects the rate of separation as well as he quality of desired product and the
cost of replacement of membranes.
This Mini Project is intended for the study of Membrane technology, the classification of
membranes, their working principle and driving forces responsible, the fabrication of ceramic
and polymer membranes and the effects of different membrane characteristics on the
separation process and henceforth, the applications of different membranes in various
industrial processes. Different membrane separation methods, including Microfiltration,
Ultrafiltration, Nanofiltration and Reverse Osmosis for the clarification/ concentration of fruit
juices have also been studied.
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CHAPTER 1
INTRODUCTION
A membrane is a thin barrier that permits the transport of certain species across it from one
fluid to another, under the influence of a driving force across the membrane, allowing the
passage of one or more desired components in a mixture.
The stream that enters the membrane is called feed-stream, the fluid that passes through the
membrane is known as the permeate while the fluid that contains the retained components is
named retentate or concentrate.
The driving force for any mass transfer operation is the difference of Chemical Potential,
which depends upon the difference of Pressure, Temperature, Concentration, Electric
Potential difference, etc.
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1.1. MASS BALANCES OVER MEMBRANE
Assuming that no chemical reaction takes place and the mass balance is carried out at steady
state, the overall mass balance equation can be represented as:
Since, at steady state, Accumulation = 0, the mass balance equation can be written as:
ṅ f = ṅ p + ṅr
Where, ṅ f is equal to total molar flow rate in feed stream, ṅ p is the total molar flow rate in
product stream and ṅr is the total molar flow rate in retentate stream.
If x i is the mole fraction of component i, the mass balance equation for a single component
can be given as:
ṅ f xi , f =ṅ ρ x i , p + ṅ r x i , r
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CHAPTER 2
LITERATURE REVIEW
Various experiments have been done by using both ceramic and polymer membranes of
different geometric structures as well as morphologies for the processing of fruit juices in
order to increase the shelf life of a fruit juice keeping its nutritious value in mind. In the
contemporary world, a high population means a large demand of food. Considering the case
of fruit juices, the most critical raw material, the corresponding fruit needs to be produced.
However, it is obvious that, it is not possible to produce a particular fruit throughout the year
unless genetically modified, which could have other consequences. Keeping in mind to retain
the natural genetic character of a fruit as well as to address the demand of fruit juices of a
particular juice throughout the year, the shelf life of the fruit juice needs to be extended,
which could be possible either by thermal processing or by membrane separation.
The advantages of membrane separation over that of thermal processing has been further
discussed in this project report. There is a large variety of membranes currently available for
different purposes. However, choosing the most suitable membrane for a particular process is
the most critical part in obtaining the highest optimization and feasibility in a particular
process. Therefore, the choice of the membrane could only be done once we come to know
about the characteristics of a membrane as well as anticipate the possible challenges that we
could face while carrying out a particular separation process.
The project report focusses on the scrutiny of all such membranes that could be the best fit
for clarification of different kinds of fruit juices as well as about various parameters affecting
the process and the possible measures that could be taken in order to achieve highest quality
product as well as most feasible processing technology.
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CHAPTER 3
Chemical potential is the main driving force that governs membrane separation process.
Since chemical potential cannot be measured easily, other driving forces such as pressure
gradient, concentration gradient and electric potential difference are taken as reference
that govern the membrane separation process.
Reverse
Osmosis(RO)
Nanofiltration
Membrane Dialysis
Separation Concentration
gradient
Gel permeation
chromatography
Electroosmosis
Electric Potential
Difference
Electrodialysis
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The above flowchart depicts the classification of membrane separation process based on
different driving forces.
Pressure gradient drives many day-to-day basis membrane separation processes such as
Reverse osmosis, Microfiltration, Ultrafiltration, Nanofiltration etc.
Concentration gradient drives membrane separation processes such as dialysis and gel
permeate chromatography.
a. Dialysis: dialysis is the process of removing excess water, solutes, and toxins from the
blood in people whose kidneys can no longer perform these functions naturally.
b. Gel permeation chromatography: Gel permeation chromatography is a type of size-
exclusion chromatography, that separates analytes on the basis of size, typically in
organic solvents. The technique is often used for the analysis of polymers.
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b. Electrodialysis: Electrodialysis is used to transport salt ions from one solution through
ion-exchange membranes to another solution under the influence of an applied
electric potential difference. This is done in a configuration called an electrodialysis
cell.
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CHAPTER 4
CLASSIFICATION OF MEMBRANES:
Membranes can be classified into different categories: Geometry, Structure and Material, in
the following ways as shown in the flowchart:
Cylindrical porous
Symmetric/Isotropic
Porous
Membranes
Asymmetric/Anisotropic
Composite Membranes
Membranes
Flat Membranes
CLASSIFICATION
OF MEMBRANES Based on Geometry
Tubular Membranes
Polymeric Membranes
Based on material
Ceramic Membranes
On the basis of structure, membranes are broadly classified into two types:
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dissolved into the membrane, then diffuse and finally desorbs from the
membrane
On the basis of geometry, membranes are broadly classified into two types:
On the basis of material, membranes are broadly classified into two types:
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membranes have been widely used in various gas separation applications mainly due
to their high-performance regarding permeation and selectivity.
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CHAPTER 5
There are several methods for the preparation ceramic membranes such as slip casting,
extrusion, pressing, etc. The following steps generally summarize the preparation procedure:
Suspension preparation: Where the starting powders are mixed with a suitable
binding liquid.
Forming: This includes shaping of the prepared suspension according to some
predetermined method.
Heat treatment: This means using high temperatures to bind the membrane
particles through a sintering process.
The fabrication of composite membranes is done by coating the membrane support then
firing as illustrated:
A few methods adopted for the fabrication of ceramic membranes are Solid State Method,
Tape Casting method, Slip Casting method, Pressing method, Extrusion method etc.
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5.2. POLYMERIC MEMBRANE FABRICATION:
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Fig: Interfacial Polymerization Process
The unique features of these fibrous membranes are controllable aspect ratios. The
morphology of the nano/microfibers, or both, can be achieved by optimizing the
following factors:
Solution viscosity
Environmental conditions
Applied electric potential
Flow rate of the solution
The fiber size, shape, and morphology are needed to identify or finalize the
porosity, pore size distribution, hydrophobicity, and surface morphology of the
electrospun fibrous membranes.
There are various other novel ways adopted in the manufacture of polymer
membranes such as track etching, stretching etc.
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CHAPTER 6
Membrane processes employ a barrier layer that allows water to permeate or pass through it
but rejects or retards other components from going along with that filtrate. In the case of
microfiltration and ultrafiltration, distinct pores in the polymer allow for water to flow
through the barrier but retard/reject the passage of species larger than the pores. Reverse
osmosis barrier layers do not have distinct pores but do allow water to diffuse through the
barrier layer and reject most of the dissolved ions in the mixture. Since heat is not used to
affect the separations, the components in the mixture are less likely to suffer thermal
degradation. Membranes are replacing diatomaceous earth filtration (DE), multimedia
filtration, centrifugation, extraction, rotary vacuum filters, evaporation and distillation and
other unit operations that have been used to make products. Cold sterilization of beverages,
pharmaceuticals and milk take advantage of the membrane systems. Most of the membrane
products commercially available have a polymeric barrier layer however ceramic membranes
with distinct pores have been used in demanding conditions and are finding use in new
applications. Ceramic membranes have pore sizes that classify them as microfiltration and
ultrafiltration filters.
Membrane products are well known for producing potable water in municipal plants and
seawater desalination. However, what is not appreciated is how much membrane technology
is used in industrial applications around the world. Membranes achieve separations without a
phase change and the absence of applying heat can be advantageous to some applications.
The ability to remove water from a process stream or effluent has shown to be an effective
way of concentrating valuable components of an aqueous stream. At times the membrane
facility may not be large compared to a municipal plant but the value to the system and
process may be critical for overall economic viability. Sometimes, the water available to an
industrial facility may not meet the requirements of the application and membranes can be
used to improve the quality so that the process can be run. Or perhaps the discharge from the
processes is too great and a reduction step is needed that can be facilitated by membranes. At
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times, the concentration of the solution may not be desirable and an easy, efficient means of
adjusting the concentration may be in order by using membranes. Finally, membranes are
used in Membrane Bioreactors (MBR) for waste treatment in food and dairy, pharmaceutical
and other facilities.
Applications include:
Membrane processes have found a great variety of applications in which their use has
improved products, recovered valuable components, added stability to the mixture, enhanced
the aesthetics of the solutions and contributed to the economics of the processes.
Microfiltration, ultrafiltration, reverse osmosis and nanofiltration each offer different
separation options for industrial applications that will continue to grow in their use.
Among the very numerous applications on an industrial scale, a few of the main separations
which represent the latest advances in food processing, are reported.
Clarification of fruit, vegetable and sugar juices by microfiltration or ultrafiltration allows the
flow sheets to be simplified or the processes made cleaner and the final product quality
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improved. Enzymatic hydrolysis combined with selective ultrafiltration can produce
beverages from vegetable proteins.
Also, membrane processes have been popular in the separation of bacteria and viruses from
water in the wastewater treatment processes
The applications of membrane technology are manifold. Membranes are not only used
for filtration, extraction, and distillation, they can also be applied for gas storage in biogas
plants or act as catalysts in syntheses.
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CHAPTER 7
This Mini Project is focused upon the study of fruit juice clarification using Membrane
separation processes. However, the project has been limited to case study and acquiring
information from research articles and printed text material due to the time period available
for the project after being brought into knowledge about the same, constraining the data only
to previously published material instead of experimental collection.
Thermal processing remains the most widely employed method for shelf-life extension and
food preservation and concentration. However, industrial thermal treatments may have
negative impacts on nutritious components.
The advantages of these membrane processes over traditional methods are lower thermal
damage to product, increase in aroma retention, less energy consumption, and lower
equipment costs.
Raw fruit juice contains lower molecular weight components like sugar, acid, salt, flavour,
and aroma compounds. It additionally contains noteworthy measure of macromolecules
(100–1000 ppm) for example, polysaccharides (pectin, cellulose, hemicellulose, and starch),
dimness shaping segments (suspended solids (SSs), colloidal particles, proteins, and
polyphenols) and so forth. Therefore, in order to store for longer periods for commercial use,
the juice needs to be clarified.
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Clarification is necessary for the removal of such macromolecules. In traditional processes,
enzyme treatment of raw juice is being performed with the help of enzymes (pectinase and
amylase) for reducing the pectic substances and starch content followed by addition of fining
agents. The main function of the fining agents such as gelatine, bentonite etc. is to enhance
the settling of formed flocs. This enzymatic treatment helps in reducing the turbidity and
viscosity and thereby makes the clarification process easier.
The suspended solids, colloidal particles, proteins etc. are removed by conventional filtration.
To facilitate the filtration process, filter aids are used. The above-mentioned traditional
methods to clarify fruit juice are batch processes and are highly labour-intensive and time-
consuming. Also, one major concern is the incomplete removal of additives (fining agents
and filter aids) from product juice which can affect the taste of juice.
Thermal evaporation is one of the most conventional techniques for fruit juice concentration.
Despite its economic feasibility and technology, it does exhibit some disadvantages when
applied to fruit juices. Even under vacuum, operating temperatures are still high enough to
bring about significant deterioration in the product juice such as degradation of colour, loss of
nutritional characteristics, and the development of a “cooked” taste. For example, lipids and
ascorbic acid can be oxidized, amino acids and sugars can undergo browning reaction, and
pigments, especially anthocyanin, carotenoids, and chlorophyll, can be degraded. Due to high
temperatures of evaporation, loss of aroma compounds occurs in fruit juices.
Hence, compared to these traditional methods, energy saving membrane operations such as
microfiltration (MF) and ultrafiltration (UF), represent a valid alternative for the clarification
of additive-free high-quality fruit juices with natural fresh taste.
Membrane processes, commonly used for fruit juice clarification are Microfiltration (MF),
Ultrafiltration (UF), Nanofiltration (NF), Reverse Osmosis (RO), Electrodialysis,
Pervaporation, Osmotic Distillation etc. A few of the following have been discussed below:
a. Microfiltration (MF): In the fruit juice processing industry, the main purpose of MF is
mainly clarification to remove suspended solids (SS), fat and high molecular weight
proteins. Microfiltration (MF) membranes are normally of average pore size between
0.1 and 10 µm.
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b. Ultrafiltration (UF): UF is essentially utilized for fractionation, fixation and filtration.
UF is utilized to clear up a wide assortment of natural juices by evacuating polluting
influences, for example, yeast, molds, microscopic organisms and colloids, together
with proteins, tannins and polysaccharides, which all confers stability to the last item.
c. Nanofiltration (NF): NF can be utilized to in part demineralization, and in addition to
concentration. In the juice processing industry, NF can be used to concentrate useful
bioactive compounds from fruit juices e.g., lycopene in case of watermelon juice.
One of the main problems of using of membranes for clarifying or concentrating fruit juices
is membrane fouling and concentration polarization. Concentration polarization is reversible
fouling while pore blocking is mostly irreversible. Concentration polarization and pore
blocking results in flux decay with the process time, thus reducing the permeability of the
membrane or making a thin layer over the membrane surface. Membrane fouling controls the
frequency of cleaning, the lifetime of the membrane, area needed for separation which
ultimately determines the costs, design and operating parameters of membrane plants.
Pre-treatment methods before juice clarification can reduce the particulate suspended
materials in the juice, resulting in improvement of flux and attainment of higher
concentration factors. The first step for pre-treatment for clarification of citrus juices using
membrane separation is pectin removal with the help of enzymes. The most used method for
pre-treatment of juices to remove pectin is enzymatic treatment by pectinase. More than 95%
recovery of the product can be achieved by UF of such depectinised juices.
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A few other flux enhancing techniques to diminish fouling layer and pore blocking in juice
processing include ultrasonic vibration, periodic backwashing with air or N2, and
backwashing by pulsating flow etc.
a. Effect of operating parameters in permeate flux: Permeate flux decline with time due
to concentration polarization and fouling remains a major hindrance in fruit juice
processing using membrane methods. Most researchers have found that an increase in
temperature have a positive effect in flux enhancement in fruit juice clarification
processes. High values of pressure helped in maintaining a high level of flux during
reverse osmosis concentration of fruit juices. A trend of declining permeate flux is
generally observed with an increase of volumetric concentration factor in case of fruit
juice concentration processes.
b. Effect of pre-treatment in permeate flux and juice quality: Over the years, enzymatic
treatment has been widely used as a pre-treatment in juice processing industries.
Researchers have shown that Enzymatic pre-treatment helps in maintaining a higher
flux level in case of clarification/concentration of citrus juices by reducing the juice
viscosity and pectic materials. Depectinisation also helps in reducing the juice
turbidity which ultimately enhances permeate flux.
Other factors affecting the fruit juice clarification include pore size distribution, mode of
filtration (e.g., dead end filtration, crossflow filtration) etc.
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CHAPTER 8
Throughout the case study, the team has explored about various types of membranes, and
observed the following:
1. Tubular membranes have been less prone to fouling as compared to flat plate
membranes, due to the cross-flow mode of filtration.
2. Although, polymer membranes are cheaper, ceramic membranes provide great
mechanical, thermal as well as chemical stability and hence compatible with a myriad
of applications.
3. There are numerous applications of membrane technology in the food processing
industry, such as extraction of casein and fat from milk, increasing the shelf life of
fruit juices by clarification process, removal of bacteria, viruses and colloidal particles
of harmful pollutants such as microplastics etc. for potable and safe drinking water, in
which membrane technology had a promising scope of a highly efficient as well as
affordable way to obtain the desired product and also making the further processing of
retentate much easier and feasible.
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CHAPTER 9
During the study, relationships between the synthesis of membranes, their structure, surface
properties, and performance have been wetted upon. We saw that remarkable progress has
been made in the fabrication of membranes for various applications such as water treatment,
food processing etc.
Coming to the focus area, i.e., fruit juice processing, significant development has happened
over the time to retain the quality of fruit juices, along with the elements that could
potentially reduce the shelf life of the fruit juices. However, juices with high acidic character,
high concentration of dissolved particulates or microbial contents are still a challenge to be
handled as they increase the rate of fouling and concentration polarization in the membrane.
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CHAPTER 10
BIBLIOGRAPHY
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ACKNOWLEDGEMENTS
The knowledge and experience acquired by the group though the project work is priceless.
We are highly indebted to the relentless efforts put by our faculty, mentors and classmates,
extending their selfless efforts for the successful completion of this mini project for the
academic year 2021-22.
We are thankful to our supervisor, Dr. Vinoth Kumar Raja, Head, Dept. of Chemical
Engineering, for the guidance and supervision throughout the period of project.
We thank Ms. S L Sandhya Rani, Ph.D. Scholar, Dept. of Chemical Engineering, for her
help and guidance in providing the basic insight about the focus area as well as in guiding our
path for finding relevant reference material for the same.
We are grateful to our Faculty, Department of Chemical Engineering, and laboratory staff
who have delivered their support for the collection of necessary information and in nurturing
our knowledge about the assigned focus area, as well as in helping us in learning about the
respective lab equipment available in the institute for the same.
We profusely render our gratitude to our parents and our friends for their tireless support in
helping us succeed in the completion of mini project.
Sincerely,
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