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 MEMBRANE

HYDROGEN
PERMEATE

Light
Hydrocarbons
RESIDUE

Sieve
Dryer
Feed

FURNACE
COOLING

Caustic Scrubber LIQUIDS

EXAMPLE: SEPARATION PROCESS Heavier

Hydrocarbons

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

 Bioseparation Techniques
Stage Objective(s) Typical Unit Operations

Recovery • Remove or collect cells, Filtration, sedimentation,

(separation of cell debris extraction, adsorption,
insolubles) • Reduce volume centrifugation
Isolation • Remove materials having Extraction, adsorption,
properties widely different ultrafiltration,
from those of target precipitation
product
• Reduce volume
Purification • Remove remaining Chromatography, affinity
impurities, which typically methods, precipitation
are similar to those of
target product
Polishing • Remove liquids Drying, crystallization
• Convert product to
crystalline form (not
always possible)

 Example of bioseparation
Separation and purification of intracellular
enzymes
fermentation
lyophilization

Cell removal and

concentration dialysis

Cell disruption Solvent

precipitation
Removal of cell
debris Chromatographic
purification
Protein
precipitation or ultrafiltration
aqueous two-
phase extraction
 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 easiest-to-remove
impurities first: unused starch, linear
Remove the most plentifuldextrins,
impurities
glucose, maltose, etc
first: CD-agent complex
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

Make the most difficult and
that exploit different separation
expensive separations last:
driving forces
CD crystals

 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 : C37H67NO13, 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