MODERN SEPARATION TECHNIQUES

[Link]- I Semester Chemical Engineering

Dr. BASAVARAJ R J

Asst. Professor in Chemical Engineering

basavarajarj@[Link]
Students group ID: rvcemasters@[Link]
R V College of Engineering, Bengaluru-560 059
 MODERN SEPARATION TECHNIQUES

Faculty Name: Dr. Basavaraja R J

Subject code : 14HCE153 IA Marks :
50

No. of Lecture Hours / Week : 04 Exam Hours : 03

No. of Practical Hours / Week : --- No. of Tutorial : 02 Hours/
Week
Total No. of Lecture Hours : 52 Exam Marks : 100

SYLLABUS

Introduction: Review of conventional processes, Recent advances in

separation techniques based on size, surface properties, ionic properties and
other special characteristics of substances, Process concept, Theory and
equipment used in cross flow filtration, cross flow electro filtration, dual
functional filter, Surface based solid -liquid separations involving a second
liquid, Sirofloc filter.
• Separation can be defined as an operation by
which a mixture is resolved in to its components.
• Separation processes play vital role in process
industries.
• With out separation processes no industry can
exist.

Separations are carried out based on differences in properties such

as size, shape, mass, or chemical affinity between the constituents of
a mixture, and are often classified according to the particular
differences they use to achieve separation.
• Every Industrial Process is designed to produce
economically a desired product from a variety of
starting materials through a succession of
treatment steps.

IMPUTRITIES BY PRODUCT

PURFIED COMBINED
PRODUCT DOWN
CHEMICAL /
STREAM
UPSTREAM BIOCHEMICAL
PROCESS
PROCESS RAW TREATMENT
MATERIAL

PRODUCT
RAW
MATERIALS
Typical Chemical Process
Physical Treatment before reaction step is required for
preparing the raw material – upstream processing or pre
treatment step.
The raw material undergo a number of physical
treatment steps to put them in the form in which they
can be treated chemically.

Chemical Processes
• Iron pyrites ore is dried in rotary kiln and ground to
– 200 mesh for sulfur and sulfur dioxide production.

• Calcium carbide is pulverized for the production of

acetylene.

• Phosphate rock ground for production of elemental

phosphorous, phosphorous pentoxide and phosphoric
acid.
• Lime stone is pulverized, classified, treated in flotation
cell for the beneficiation of limestone.

• Clay and limestone are pulverized for cement

manufacture.

• Rice bran is palletized before extraction

 Schematic representation of a Separation Process

Separating
agent

Product stream

Feed Separating
stream Device
By product stream
• One or more feed with two or more species enter the
unit
• Two or more products of different compositions leave
the unit
• A separating agent is required for the separation
– Energy separating agent
– Mass separating agent
•Often separating agents will cause formation of second
phase of matter.
•A separation is accomplished if the generated phase has a
different composition from the feed.
 Primary Basis for Separation
• Any separation depends on the use of one or more differences in
properties of components
• Greater the differences in properties, easier is the separation by
that method
– Vapor Pressure-distillation
– Diffusivity and Solubility-reverse Osmosis
– Molecular Size-ultra Filtration
 Separation factor
• Proposed as a measure of degree of separation obtainable for particular
mixture and a separation technique

• For a binary mixture it is the ratio of the concentration ratio of A and B

in one phase to that in other

αij = xi1 / xj1 = ki / kj

xi2 /xj2
ki- equilibrium ratio

• Vapour liquid system-relative volatility

• liquid-liquid system-selectivity
• unity-no separation possible
• larger the value greater the separation
• separation factor is quite large-separation possible in a single stage
 Classification of Separation Processes
• Separation may be achieved by chemical, mechanical and
physical/diffusion methods

• Chemical method ordinarily destroys the original substance

and hence used rarely.

• The mechanical /Physical / Diffusion methods are further

classified as equilibrium separation process, rate governed
separation process and mechanical separation processes.
• Petroleum industry is one of the earlier examples

• Development of new separation processes and equipments

helped the growth of antibiotic industry and nuclear
industry

• Recent times challenging problems of separation have

come in the field of waste treatment, pollution control,
production of ultra pure fluids and food preservation.

• Beverages processing, production of pharmaceuticals,

harmones, enzymes, vaccines and other biologicals.
 Equilibrium Processes
PROCESS FEED AGENT PRODUCT PRINCIPLE EXAMPLE

EVAPORATION L H L+V DIFFERENCES IN CONCENTRATION OF

VOLATILITY SOLUTIONS
DISTILLATION L&OR V H L+V DIFFERENCES IN PETROLEUM
VOLATILITY PRODUCTS,ALCOHOL
ABSORPTION G L( NV) L+V PREFERENTIAL RECOVERY OF CO2,SO2
SOLUBILITY
STRIPPING L G(NC) L+V DIFFERENCES IN REMOVAL OF LIGHT
VOLATILITY HYDROCARBONS
LIQUID L L(IMM) L+L PREFERENTIAL PENCILLIN RECOVERY
EXTRACTION SOLUBILITY
LEACHING OR S L L+S PREFERENTIAL RECOVERY OF
WASHING SOLUBILITY MINERALS FROM ORE
CRYSTALLIZATION L H(REMOVAL) L+S DIFFERENCES IN SUGAR,CITRIC ACID
SOLUBILITY
DRYING S H S+V DIFFERENCES IN FOOD DEHYDRATION
VOLATILITY
ADSORPTION G(OR)L S L(OR)G DIFFERENCES IN DRYING OF
CHEMICAL GASES,DECOLOURATION
AFFINITY OF SOLNS.
ION EXCHANGE L S( RESIN) L+S ELECTRICAL WATER SOFTENING
CHARGE
+ADSORPTION
FREEZE DRYING FROZEN H S+V SUBLIMATION OF DEHYRATION OF FOOD
WATER WATER
 Rate Governed Processes
PROCESS FEED AGENT PRODUCT PRINCIPLE EXAMPLE

DIALYSIS L M SELECTIVE L+L DIFFERENCE IN ARTIFICIAL

DIFFUSIONAL RATE KIDNEY

ELECTRO L M +[Link] L+L DIFFERENCE IN DESALINATION OF

DIALYSIS IONIC MOBILITY BRACKISH WATER

ULTRA L+ M+PRESSURE GRADIENT L+L DIFFERENCE IN PROTEIN

FILTRATION COLLOID PERMEABILITIES CONCENTRATION

REVERSE L M+PRESSURE GRADIENT L+L DIFFERENCE IN DESALINATION OF

OSMOSIS COMBINED SEA WATER
SOLUBILITIUES AND
DIFFUSIVITIES IN
MEMBRANES

GAS PERMEATION G M+PRESSURE GRADIENT G DIFFERENCE IN GAS REVOCERY/

SOLUBILITIES AND PURIFICATION OF
TRASPORT RATE HYDROGEN
THRO’MEMBRANES

THERMAL G(OR)L [Link] G(OR) L DIFFERENCE IN SEPARATION OF

DIFFUSION RATE OF THERMAL ISOTOPES
DIFFUSION
 Mechanical Processes
PROCESS FEED AGENT PRODUCT PRINCIPLE EXAMPLE

FILTRATION L+S FILTER L+S SIZE Separation of

MEDIUM+ Solids form Slurry
PRESSURE

SETTLING L+S GRAVITY L+S DIFFERENCE IN Clarification of

DENSITY Solutions
CENTRIFUGING L+S(OR)L CENTRIFUGA L+S(OR)L DIFFERENCE IN Recovery of
L FORCE DENSITY Insoluble Products
CYCLONE G+S(OR)L INERTIAL G+S(OR)L DIFFERENCE IN Recovery of
SEPARATION FORCE DENSITY Insoluble Products
ELECTROSTATIC G+S(FINE ELECTRICAL G+S CHARGE ON Dust Removal
PRECIPITATION FIELD FINE SOLID from Stack Gasses
PARTICLES
 Electro-dialysis

At the cathode
2e- + 2 H2O → H2 (g) + 2 OH-
while at the anode
H2O → 2 H+ + ½ O2 (g) + 2e- or 2 Cl- → Cl2 (g) + 2e-
 Direct and Indirect methods

• Direct method:
Only energy is added or removed- [Link] ,
evaporation, crystallization-Product is obtained in a
single stage.

• Indirect method :
Involves addition of foreign substance- [Link] ,
absorption, adsorption-Product is obtained in a second
operation.
 Choice of Separation Processes

The criteria for choice for recovery of products depends on

1. Nature of the Feed (Gas Liquid or Solid)
2. Concentration of Product in the Feed
3. Physical and Chemical Characteristics of the desired product
4. Impurities in the feed
5. Intended use of the product
6. The minimal acceptance standard of purity
7. Marketability of the product.
 Selected Separation Processes

1. Filtration
2. Distillation
3. Extraction
4. Crystallization
5. Evaporation
6. Supercritical Extraction
7. Gel Electrophoresis
8. Chromatography Separations
9. Gel Filtration
[Link] Separation Processes
 Distillation
Removal of liquid mixtures in to their components by
vaporization.

The property exploited is the relative volatility.

More the relative volatility between the components to be

separated easier will be the [Link] the relative volatility
difficult will be the separation.

Azeotropic system.

Simple distillation, Continuous distillation, steam distillation,

extractive distillation, azeotropic distillation.

Packed column distillation, plate column distillation.

Steam distillation.
 Filtration :
Used for heterogeneous mixtures.

The general problem of the separation of solid particles

from liquids can be solved by using a wide variety of
methods, depending on the types of solids,the
proportion of solid to liquid in the mixture,viscosity of
the solution,and other factures.

In filtration,a pressure difference is setup that causes

the fluid to flow through small holes in a screen or cloth
which block the passage of large particle;these in
turn,buildup on the cloth as a porous cake.
Different filtration includes
Batch filtration, continuous filtration, vacuum filtration,
pressure filtration .
 Extraction
Removal of active ingredient from mixture using a solvent.

Liquid-liquid extraction is also called as solvent extraction. Solid

liquid extraction is called leaching.

Extraction and leaching exploits the differences in solubility of

solutes in different [Link] solubility is expressed as
distribution coefficient or selectivity.

Used to recover heat sensitive material from solution.

Penicillin G is an antibiotic which is recovered from fermentation

broths by counter current solvent extraction.

Two component system three component system.

Extract, raffinate.
Solutropic system.
 Extraction

Solvent extraction is a method for separating a

substance from one or more others by using a solvent. It
relies on variations in the solubilities of different
compounds in different substances. In most cases, the
substance to be extracted, which may be a solid, a liquid
or a gas, is dissolved in a liquid, along with other
substances, and a liquid solvent is used for the extraction
— this is sometimes called liquid-liquid extraction.

The technique may also be applied to solid materials that

contain compounds that need to be extracted. This
method is widely used in industry, and in the laboratory
for refining, isolating and purifying a variety of useful
compounds.
 Extraction

A solvent will be chosen that does not mix with the

compound in which the substance of interest is currently
dissolved, so that, when left undisturbed, they will form two
separate layers, as with oil and water.

It is also important that the compound to be extracted should

have greater solubility in the solvent that has been added,
and that this should not dissolve any unwanted substances
in the original mixture. Once added, the two liquids may be
shaken together for a time then allowed to stand for a while,
so that they separate out.

The choice of solvent to be used will depend on the

chemical and physical properties of all the substances in the
mixture. The process may need to be carried out in several
stages, using different solvents.
 Liquid-Liquid Extraction
Liquid-liquid extraction (also known as solvent extraction) involves the
separation of the constituents (solutes) of a liquid solution by contact with
another insoluble liquid. Solutes are separated based on their different
solubilities in different liquids. Separation is achieved when the
substances constituting the original solution is transferred from the original
solution to the other liquid solution.

The Figure showed a feed liquid

(the "first" liquid) containing the
desirable compound that is to be
separated together with other
compounds. Then an immiscible
extraction liquid (the "second"
liquid) is added and mixed with the
feed liquid through agitation. The
species re-distribute themselves
between the 2 liquid phases.
Agitation of the 2 phases is
continued until equilibrium, and
then agitation is stopped and the
liquids are allowed to settle until
both phases are clear. The 2
phases can then be separated.
 Crystallization

Removal of solids from solutions by super saturating the

solution.

The super saturation may be carried out by cooling, by

vaporizing a portion of the solvent, adiabatic evaporation or by
adding a third component which will reduce the solubility of
solute.

Tank crystallizers, agitated batch crystallizers, continuous

crystallizers, vacuum crystallizers.
 Evaporation
Removal of major portion of liquid from solution by boiling the
solution.

Major portion of solvents used in extraction are recovered by

evaporation.

Solution is heated in evaporators by using steam in [Link]

liquid evaporated is collected at the top ,condensed and collected if
vapor is the useful product.

The solution leaving at the bottom is a thick solution.

 Evaporation, Contd..
The solids enter with the solution dose not evaporate because they
do not have sufficient vapor pressure.

The liquid portion of the feed is divided in to two portions but the
the solid that enters goes only to the bottom stream.

Economy, Single effect,multiple effect, once through, circulation

evaporators. Natural convection, forced [Link] film
falling film evaporators,vapor recompression evaporators.
 Super Critical Extraction
• The basic principle of SCE is that when the feed material is
contacted with a supercritical fluid then the volatile substances
will partition into the supercritical phase.
• After the dissolution of soluble material the supercritical fluid
containing the dissolved substances is removed from the feed
material.
• The extracted component is then completely separated from
the SCF by means of a temperature and/or pressure change.
• The SCF is then recompressed to the extraction conditions and
recycled.
 Advantages of SCE

• Thermally labile compounds can be extracted with minimal

damage as low temperatures can be employed by the
extraction.
• Dissolving power of the SCF is controlled by pressure and/or
temperature.
• SCF is easily recoverable from the extract due to its volatility.
• Non-toxic solvents leave no harmful residue.
• High boiling components are extracted at relatively low
temperatures.
• Separations not possible by more traditional processes can
sometimes be effected.
 Disadvantages of SCE

• Elevated pressure required

• Compression of solvent requires elaborate recycling

measures to reduce energy costs

• High capital investment for equipment

 Enriching section

Stripping section

Distillation column
 Major process steps in Downstream processing in a typical
Bioprocess Industry

Extra
Supernatant Recovery Purification cellular
products

Intra
Solid-liquid
Fermenter Recovery Purification cellular
separation
products

Cells Cell rupture

Cell products Cell debris

 Bio processes

• Media preparation-The formation of media to be used

in culturing the process organism during the
development of the inoculum and in the production
fermenter.
• Sterilization_Sterilization of the medium, fermenter and
ancillary equipment,development of Inocula for
industrial fermentations.

• Production of active,pure culture in sufficient quantity

to inoculate the production vessel.

• The growth of the organism in the production

fermenter under optimum conditions for product
formation.
• Preparation of reactants-upstream process

• Optimization of conditions in reactor to maximize

process yield

• Recovery of product-down stream process

After successful fermentation or enzyme reactions,
desired products must be separated and purified

This final step is commonly known as downstream

processing or bioseparations.

This can account for up to 60 percent of the total

production costs,excluding the cost of raw materials.
The fermentation products can be
The cells themselves (biomass)
Components within the fermentation broth
( extra cellular)
Those trapped in cells( intracellular)

Examples of Bio processing Products

Type Products
Cell itself Bakers yeast,single cell protein
Extra cellular Alcohols,organic acids,amino acids
Intracellular Recombinant DNA proteins
Bio separation processes make use of many separation
techniques commonly used in chemical process
industries
However, Bio separations have distinct characteristics
which are not common in the traditional separations of
chemical processes.
Some of the unique characteristics of bioseparation
products are
The products are in dilute concentration in aqueous
medium
The products are usually temperature sensitive
There is a great variety of products to be separated

The products can be intracellular,often as insoluble

inclusion bodies
The physical and chemical properties of products are
similar to contaminants

Extremely high purity and homogeneity may be needed

for human health care

These characteristics of bioseparation products limit

the use of many traditional separation technologies and
also require the development of new methods
• The upstream and down stream processes are
mainly the separation processes.
• The separation processes accounts for 50-90% of
the capital investment
• Separation itself may be main function of an entire
process
Common downstream processes used in Bio
processing are

Solid liquid separations – Filtration,centrifugation

Extraction and Leaching

Evaporation

Distillation

Crystallization

Adsorption

Drying
 Cross flow filtration

Principle of cross flow filtration

Cross flow filtration is different from dead end filtration in which the feed is
passed through a membrane or bed, the solids being trapped in the filter
and the filtrate being released at the other end. Cross-flow filtration gets its
name because the majority of the feed flow travels tangentially across the
surface of the filter, rather than into the filter.
 Cross flow filtration

In crossflow filtration, the feed is passed across

the filter membrane (tangentially) at positive
pressure relative to the permeate side. A
proportion of the material which is smaller than
the membrane pore size passes through the
membrane as permeate or filtrate; everything
else is retained on the feed side of the
membrane as retentate.

With crossflow filtration the tangential motion of

the bulk of the fluid across the membrane causes
trapped particles on the filter surface to be
rubbed off. This means that a crossflow filter can
operate continuously at relatively high solids
loads without blinding
Advantages:
•A higher overall liquid removal rate is achieved by the prevention of filter cake
formation
•Process feed remains in the form of a mobile slurry, suitable for further processing
•Solids content of the product slurry may be varied over a wide range
•It is possible to fractionate particles by size
Crossflow filtration vs Dead-end filtration
　
Filtration modes can be divided by crossflow filtration and dead-end
filtration depending the flow direction on membrane surface.
In crossflow filtration, feed moves parallel to the filter medium to
generate shear stress to scour the surface (Fig. 1a). Extra energy is
required to generate crossflow, but cake layer thickness can be
controlled. Pseudo steady-state may exist, where scouring effect and
particle deposition find a balance and cake layer hardly grows. This
filtration mode is particularly effective when feed water carries high
level of foulants such as suspended solids and macromolecules. All
MBR processes and most of wastewater filtrations are adapting
crossflow modes.

In dead-end filtration, no crossflow exits and feed moves toward the

filter medium. All the particles that can be filtered by filter settle on the
filter surface. Since the filtration is not sustainable forever without
removing accumulated solids, backwashing is performed periodically
and/or filter medium is replaced. This filtration mode is particularly
effective when feed water carries low level of foulants. Many surface
water filtrations, pretreatment for seawater RO, and tertiary filtrations
are adapting dead-end modes.
Assignment

• Theory and equipment used in cross flow filtration

• cross flow electro filtration, dual functional filter

• Surface based solid -liquid separations involving a second

liquid, Sirofloc filter.

• surface properties, ionic properties and other special

characteristics of substances used in se