MODERN SEPARATION TECHNIQUES

M.Tech- I Semester Chemical Engineering

Dr. BASAVARAJ R J
Asst. Professor in Chemical Engineering
basavarajarj@rvce.edu.in
Students group ID: rvcemasters@gmail.com
R V College of Engineering, Bengaluru-560 059

MODERN SEPARATION TECHNIQUES

Faculty Name: Dr. Basavaraja R J
Subject code : 14HCE153
50
No. of Lecture Hours / Week : 04
No. of Practical Hours / Week : --Total No. of Lecture Hours : 52

IA Marks :
Exam Hours : 03
No. of Tutorial : 02 Hours/
Week
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

UPSTREAM
PROCESS

RAW
MATERIAL

CHEMICAL /
BIOCHEMICAL
TREATMENT

COMBINED
PRODUCT

DOWN
STREAM
PROCESS

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
manufacture.

are

pulverized

Rice bran is palletized before extraction

for

cement

Schematic representation of a Separation Process

Separating
agent

Product stream
Feed
stream

Separating
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

ij = 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

EVAPORATION

L+V

DIFFERENCES IN
VOLATILITY

CONCENTRATION OF
SOLUTIONS

DISTILLATION

L&OR V

L+V

DIFFERENCES IN
VOLATILITY

PETROLEUM
PRODUCTS,ALCOHOL

ABSORPTION

L( NV)

L+V

PREFERENTIAL
SOLUBILITY

RECOVERY OF CO2,SO2

STRIPPING

G(NC)

L+V

DIFFERENCES IN
VOLATILITY

LIQUID
EXTRACTION

L(IMM)

L+L

PREFERENTIAL
SOLUBILITY

PENCILLIN RECOVERY

LEACHING OR
WASHING

L+S

PREFERENTIAL
SOLUBILITY

RECOVERY OF
MINERALS FROM ORE

CRYSTALLIZATION

H(REMOVAL)

L+S

DIFFERENCES IN
SOLUBILITY

SUGAR,CITRIC ACID

DRYING

S+V

DIFFERENCES IN
VOLATILITY

FOOD DEHYDRATION

G(OR)L

L(OR)G

DIFFERENCES IN
CHEMICAL
AFFINITY

DRYING OF
GASES,DECOLOURATION
OF SOLNS.

ION EXCHANGE

S( RESIN)

L+S

ELECTRICAL
CHARGE
+ADSORPTION

FREEZE DRYING

FROZEN
WATER

S+V

ADSORPTION

SUBLIMATION OF
WATER

EXAMPLE

REMOVAL OF LIGHT
HYDROCARBONS

WATER SOFTENING

DEHYRATION OF FOOD

Rate Governed Processes

PROCESS

FEED

AGENT

PRODUCT

PRINCIPLE

EXAMPLE

DIALYSIS

M SELECTIVE

L+L

DIFFERENCE IN
DIFFUSIONAL RATE

ELECTRO
DIALYSIS

M +ELE.FIELD

L+L

DIFFERENCE IN
IONIC MOBILITY

DESALINATION OF
BRACKISH WATER

L+
COLLOID

M+PRESSURE GRADIENT

L+L

DIFFERENCE IN
PERMEABILITIES

PROTEIN
CONCENTRATION

REVERSE
OSMOSIS

M+PRESSURE GRADIENT

L+L

DIFFERENCE IN
COMBINED
SOLUBILITIUES AND
DIFFUSIVITIES IN
MEMBRANES

DESALINATION OF
SEA WATER

GAS PERMEATION

M+PRESSURE GRADIENT

DIFFERENCE IN
SOLUBILITIES AND
TRASPORT RATE
THROMEMBRANES

GAS REVOCERY/
PURIFICATION OF
HYDROGEN

G(OR) L

DIFFERENCE IN
RATE OF THERMAL
DIFFUSION

SEPARATION OF
ISOTOPES

ULTRA
FILTRATION

THERMAL
DIFFUSION

G(OR)L

TEMP.GRADIENT

ARTIFICIAL
KIDNEY

Mechanical Processes
PROCESS

FEED

AGENT

PRODUCT

PRINCIPLE

EXAMPLE

FILTRATION

L+S

FILTER
MEDIUM+
PRESSURE

L+S

SIZE

Separation of
Solids form Slurry

SETTLING

L+S

GRAVITY

L+S

DIFFERENCE IN
DENSITY

Clarification of
Solutions

CENTRIFUGING

L+S(OR)L

CENTRIFUGA
L FORCE

L+S(OR)L

DIFFERENCE IN
DENSITY

Recovery of
Insoluble Products

CYCLONE
SEPARATION

G+S(OR)L

INERTIAL
FORCE

G+S(OR)L

DIFFERENCE IN
DENSITY

Recovery of
Insoluble Products

ELECTROSTATIC
PRECIPITATION

G+S(FINE

ELECTRICAL
FIELD

G+S

CHARGE ON
FINE SOLID
PARTICLES

Dust Removal
from Stack Gasses

Electro-dialysis

At the cathode
2e- + 2 H2O H2 (g) + 2 OHwhile at the anode
H2O 2 H+ + O2 (g) + 2e- or 2 Cl- Cl2 (g) + 2e-

Direct and Indirect methods

Direct method:
Only energy is added or removed- Eg.Distillation ,
evaporation, crystallization-Product is obtained in a
single stage.

Indirect method :
Involves addition of foreign substance- Eg.Extraction ,
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
10.Membrane 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 separation.Less 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 solvents.The 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 calendrias.The
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 convection.Climbing 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

measures to reduce energy costs

High capital investment for equipment

elaborate

recycling

Distillation column

Stripping section

Enriching section

Major process steps in Downstream processing in a typical

Bioprocess Industry
Supernatant

Fermenter

Solid-liquid
separation

Recovery

Recovery

Cells

Cell rupture

Cell products

Cell debris

Purification

Purification

Extra
cellular
products
Intra
cellular
products

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
processing are

processes

used

in

Bio

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