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SEPARATION METHODS

Objectives
Explain the role of separations
operations in industrial chemical
process
Explain what constitutes the separation
of a chemical mixture and enumerates
general separation techniques
Explain the use of external fields to
separate chemical mixtures
Introduction
Early civilization techniques:
- Extracts metal from ores
- Perfume from flower
- Dyes from plant
- Evaporation of sea water to obtain salt
- Distill liquor

Introduction
Chemist use chromatography to
separate complex mixtures quantitatively
Chemical engineers concerned with
the manufacture of chemicals using large
scale separation methods
Chemical Processes
Conducted:
Batchwise
Continuous
Semi-continuous

Key operations in chemical process
involved:
- Reaction Processes
- Separation Processes
Mechanism of Separation
Mixture of homogenous phase
Mixture of two or more immiscible
phases

Feed
PERMEATE
RESIDUE
Caustic Scrubber
FURNAC
E
MEMBRANE
HYDROGEN
LIQUIDS
COOLING
Sieve
Dryer
Light
Hydrocarbons
Heavier
Hydrocarbons
EXAMPLE: SEPARATION PROCESS
Mechanism of Separation
Mixing of chemical is spontaneous,
increase entropy and randomness.
Separation of chemicals requires the uses
of energy.
Separation includes:
- Separation of component A from mixture in
homogenous phase
- Separation of component A from mixture in
different phases

Mechanism of Separation

If two or more immiscible phases exist
mechanical separation is preferable
E.g: Centrifuge, pressure reduction,
electric/magnetic field






Basic of separation

Types of Separation Process
1) Separation by phase addition or
creation
2) Separation of barrier
3) Separation by solid agent
4) Separation by external field or gradient
- Centrifugation
- Thermal diffusion
- Electrophoresis
- Electrodialysis
Phase creation process
Involve the creation of a second phase
that is immiscible with the feed.
Accomplished by energy or pressure
reduction.
Suitable for mixture that have tendency
to vaporize.
E.g: Evaporation, sublimation,
crystallization, distillation.
Phase addition processes
For separation of homogenous, single phase
mixture, a second immiscible phase must be
developed.
This is achieved by:
- Creation of energy separating agent (ESA)
- Mass separating agent (MSA)
When 2 immiscible fluid phases are contacted,
intimate mixing of the 2 phases is important in
enhancing mass transfer rates.
After phase contact, employing gravity and/or
enhanced techniques completed the
separation process.
Cont
Disadvantages of MSA:
- Need additional separator to recover
MSA
- Need for MSA make up
- Possible contamination of the product
- More difficult design procedure
Eg: Extractive distillation, liquid-liquid
extraction, leaching
Separation by Barrier
Includes the use of microporous and
nonporous membrane as semipermeable
barriers
Membrane are fabricated from polymer,
natural fiber, ceramic, metal etc.
Microporous membrane separation occur
at different diffusion rate
Nonporous separation based on the
solubility

Cont
Hydrogen removal in refineries, ammonia plants, and olefin
units.
Separation by Solid Agent
Process that use solid mass-separating
agents.
Solid normally in the form of a granular
material or packing. E.g: activated
carbon, aliminium oxide, silica gel, or
calcium aluminosilicate zeolite.
Example of process: Adsorption,
Chromatography, & Ion Exchange.

Generalized downstream
processing


Bioseparation
Techniques
Liquid-solids separations (dewatering,
concentration, particle removing) @
Recovery
Solute-solute separations (Isolation,
Purification)
Solute-liquid separations (Polishing)
RIPP Scheme

Bioseparation Techniques
Stage Objective(s) Typical Unit
Operations
Recovery
(separation of
insolubles)
Remove or collect cells,
cell debris
Reduce volume
Filtration, sedimentation,
extraction, adsorption,
centrifugation
Isolation Remove materials having
properties widely different
from those of target
product
Reduce volume
Extraction, adsorption,
ultrafiltration,
precipitation
Purification Remove remaining
impurities, which typically
are similar to those of
target product
Chromatography, affinity
methods, precipitation
Polishing Remove liquids
Convert product to
crystalline form (not
always possible)
Drying, crystallization

Example of bioseparation
fermentation
Cell removal and
concentration
Cell disruption
Removal of cell
debris
Protein
precipitation or
aqueous two-
phase extraction
lyophilization
dialysis
Solvent
precipitation
Chromatographic
purification
ultrafiltration
Separation and purification of intracellular
enzymes

Rules of thumb
Remove the most plentiful impurities first
Remove the easiest-to-remove impurities
first
Make the most difficult and expensive
separations last
Select processes that make use of the
greatest differences in the properties of
the product and its impurities
Select and sequence processes that
exploit different separation driving forces

Cyclodextrin
Remove the most plentiful impurities
first: CD-agent complex
Remove the easiest-to-remove
impurities first: unused starch, linear
dextrins, glucose, maltose, etc

Make the most difficult and
expensive separations last:
CD crystals

Select processes that make use of the
greatest differences in the properties of the
product and its impurities: decanol and CD
Select and sequence processes
that exploit different separation
driving forces

Example 1
You have been given a task to purify the erythromycin antibiotic
from fermentation broth. The information on erythromycin is given
below. What do you think the most likely unit operations that
should be used for the isolation and purification of
erythromycin? Justify the reasons for the selection of the unit
operations.
Information on erythromycin
Formula : C
37
H
67
NO
13
,

Molecular weight : 733.94
Form : Salts with acids, Melting point : 56 C
UV max : 280 nm, pKa : pH 8.8
Freely soluble in alcohols, acetone, chloroform, acetonitrile,
ethyl acetate. Moderately soluble in ether, ethylene
dichloride, amyl acetate. Hydrated crystals from water,
melting point 135-140 C. Resolidifies with second melting
point 190-193 C

Solution
Erthromycin has limited solubility in water but is
soluble in several solvents, including amyl
acetate. Since the solubility of amyl acetate is
low, isolation could be performed by a liquid-liquid
extraction of erythromycin using water-amyl
acetate system. For the extraction, it would be
desirable to raise the pH of the aqueous phase above
the pKa of erythromycin of 8.8, so that the secondary
amino group is converted from the positively charged
from the neutral free base form. For the purification step,
crystallization is a good choice, since hydrated crystals
have been obtained from water.