CHAPTER 1

INTRODUCTION TO SEPARATION
PROCESSES
012-7027484/Ext-2040
nooraina@unikl.edu.my
ASSESMENT METHODS
Tests 20%
Assignments 20%
Final Examination 60%
Total 100%

Test 1 : Week 6 or week 7

Test 2 : Week 11 to week 13
Introduction
Separation process developed in the early
civilizations include:
Evaporation of seawater to obtain salt
Perfumes from flowers
Dyes from plants
 General Separation Technique:

Product 1
Feed mixture to be Product 2
Separation
separated
Process Product N-1
Product N
Ex. Simple Separation Technique:
Sand in water

Sludge/sediment in water
Mechanism of Separation
Separation by Phase Addition (heat or depressurize)
or Creation (add solvent, liquid absorbent)
Separation by Barrier (semipermeable membrane)
Separation by Solid Agent Use particles (reaction,
absorbent film, direct absorption, chromatography)
Separation by External Field or Gradient
(Use electric field, magnetic field, gravity (Hall effect,
electrophoresis, mass spec)
A) Separation by Phase Addition or Creation
For a single-phase solution feed mixture is a homogeneous,
single-phase solution (gas, liquid or solid), second separable
phase must be developed (created by energy separating
agent (ESA) and/or mass separating agent (MSA)).
ESA: Involves heat transfer or transfer of shaft work (Eg.
Creation of vapor from a liquid phase by reducing the
pressure).
MSA: May be partially immiscible with one or more mixture
components and may be miscible with liquid mixture but
may selectively alter partitioning of species between liquid
and vapor phases.
 The second phase is created by an energy-separating
agent (ESA) or added a mass-separating agent (MSA).
(MSA) (add solvent, liquid absorbent)
(ESA) Heat added or heat removed
Other separating agent such as pressure reduction
and work transfer.
 Separations that use an (ESA) are generally preferred, an
(MSA) can make possible a separation that is not feasible
with an (ESA).

Disadvantages of the use of an MSA are:

1.Need for an additional separator to recover the MSA for
recycle.
2.Need for MSA makeup.
3.Possible contamination of the product with the MSA.
4.More difficult design procedures.
 Phase 1 Phase 1

Feed Phase Feed

Phase
Creation Addition
Phase 2 Phase 2

(E.S.A) M.S.A
(M.S.A)
 Ex: Partial condensation or vaporization
( When the feed mixture includes species that differ
widely in their tendency to vaporize and condense)

Vapor Initial or feed phase

vapor or Liquid
Created phase
Liquid orCooling vapor or Liquid
vaporor heating Separating Agent
Heat transfer
liquid (ESA)

e.g : Recovery of H2 and N2 from NH3 by partial condensation

and high pressure phase separation.
 Ex: Liquid liquid extraction
(when distillation is impractical, especially
Separate compounds based when the mixture to be separated is
on their relative solubilities
L temperature-sensitive and/or more than about
in two different immiscible
liquids, usually water and an
100 distillation stages would be required)
organic solvent. It is an MSA
extraction of a substance Initial or feed phase
from one liquid into another liquid
liquid phase.
Created phase
liquid
L
Separating Agent
Liquid solvent
(MSA)
L

e.g : Recovery of aromatics.

B) Separation by Barriers
Use of microporous and non-porous membrane as
semipermeable barriers.
Microporous membrane: separation is affected by
rate of species diffusion through the pores.
For nonporous membrane: separation is controlled
by differences in solubility in the membrane and
rate of species diffusion.
 Concentration gradient
Impermeable membrane
Transfer of solvent in opposite
direction by imposing
pressure > osmotic pressure
Concentration gradient
Porous membrane

0.02-10 um Microporous membrane

1-20 nm Species transported is

evaporated, separate
azeotropic mixture

Pressure driving force,

nonporous polymer
Surfactant containing
mixtures at the
interface between two
fluid phase.
B) Separation by Solid Agents
Solid in form of granular material or packing is used
as an adsorbent or acts as an inert support for a
thin layer of adsorbent by selective adsorption of
chemical reaction with species in the feed.
Active separating agent eventually becomes
saturated and need to be replaced or regenerated.
B) Separation by External Field or Gradient
External fields can take advantage of differing degrees of response of
molecules and ions to force fields.
Feasibility of Separation Method

Case 1: Separation of air into oxygen-rich and nitrogen-rich

products by distillation.

The normal boiling points of O2 (183C) and N2 (195.8C) are

sufficiently different that they can be separated by
distillation, but elevated pressure and cryogenic
temperatures (-150C to absolute zero) are required.
At moderate to low production rates, they are usually
separated at lower cost by either adsorption (i.e. silica gel
(N2))or gas permeation through a membrane .
 Case 2: Separation of m-xylene from p-xylene by distillation.

The close normal boiling points of m-xylene (139.3C) and

pxylene (138.5C) make separation by distillation impractical.
However, their widely different melting points of 47.4C for
m-xylene and 13.2C for p-xylene make crystallization as the
separation method of choice.
 Case 3: Separation of benzene and cyclohexane by distillation.
The normal boiling points of benzene (80.1 C) and cyclohexane
(80.7C) preclude a practical separation by distillation. Their
melting points are also close, at 5.5C for benzene and 6.5C for
cyclohexane, making crystallization also impractical. The method
of choice is to use distillation in the presence of phenol (normal
boiling point of 181.4C), which reduces the volatility of benzene,
allowing nearly pure cyclohexane to be obtained.
The other product, a mixture of benzene and phenol, is readily
separated in a subsequent distillation operation.
 Case 4: Separation of isopropyl alcohol and water by distillation.

The normal boiling points of isopropyl alcohol (82.3C) and water

(100.0 C) seem to indicate that they could be separated by
distillation. However, they cannot be separated in this manner
because they form a minimum-boiling azeotrope at 80.4C and 1 atm
of 31.7 mol% water and 68.3 mol% isopropanol.
A feasible separation method is to distill the mixture in the presence
of benzene, using a two-operation process. The first step produces
almost pure isopropyl alcohol and a heterogeneous azeotrope of the
three components. The azeotrope is separated into two phases, with
the benzene-rich phase recycled to the first step and the water-rich
phase sent to a second step, where almost pure water is produced by
distillation, with the other product recycled to the first step.
Case 5: Separation of penicillin from water in a fermentation broth by
evaporation of the water.

Penicillin has a melting point of 97 C, but decomposes before

reaching the normal boiling point. Thus, it would seem that it could
be isolated from water by evaporation of the water. However,
penicillin and most other antibiotics are heat-sensitive, so a near-
ambient temperature must be maintained. Thus, water evaporation
would have to take place at impractical, high vacuum conditions. A
practical separation method is liquidliquid extraction of the penicillin
with n-butyl acetate or n-amyl acetate.