Chapter 1 Introduction To Separation

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UNIT OPERATIONS II
Chapter 1: Separation Methods

: Introduction to separation
Apinan Soottitantawat
apinan.s@chula.ac.th
Separation Methods: Objectives
• Explain the role of separation operations in an industrial chemical
process
• Explain
E l i what h t constitutes
tit t the
th separation
ti off a chemical
h i l mixture
i t and
d
enumerate the five general separation techniques
• Explain the use of an energy-separating agent (ESA) and/or a mass-
separating agent (MSA) in a separation operation
• Explain how separation are made by phase creation or phase addition
and list the many separation operations that use these two techniuqes
• Explain how separations are made by introducing selective barriers and
list several separation operations that utilize this technique
• Explain the use of external field to separate chemical mixtures
• Calculate component material balances around a separation operation
based on specifications of component recovery (split ratios or split
fractions) and/or product purity
• Use the concept of key component and separation power to measure the
degree of separation between two key components
• Make a selection of feasible separation operation based on factors
involvingg the feed,, products,
p , property
p p y differences among g chemical
components, and characteristics of different separation operations
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Introduction to Separations
The goal of a separations process is to purify solutions.

To do this we must cause differential transport of species or conversion of species so that
the purer mixtures can be collected. Most separations processes involve differential
transport.
Examples:
Separation of blood
Purification of drugs
P ifi ti off A
Purification Au, Si
Si, GaAs
G A
Refining of crude oil
DNA testing
Purification of organics
g
Purification of water
Smog control
mixed separated
However, mixing is inherent in nature: The increase in entropy associated with the
randomness of a mixture lowers the Gibbs free energy.
Therefore, to “unmix” a solution we must overcome the entropic driving force to mix.
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Why Separate?
There are many reasons for wanting pure substances. Some of these reasons include:
• Need for pure material in engineering application (semiconductors)
• Preparation of raw materials into their components
• Need for pure material for materials processing
• Need to remove toxins or inactive components from solution (drugs)
• Need for ultrapure samples for testing
• Need for analysis of the components of the mixture (DNA testing)
Based on these motivations for separations, we can divide separations up into three main areas:
A l ti l Separations
Analytical S ti P
Preparative
i S Separations
i I d t i l Separations
Industrial S ti
• small scale • small scale • large scale
• quantitative analysis • materials for R&D • economical
Example: Example: Example:

Chromatography Centrifugation Distillation
The list of different existing separations methods is limitless. Therefore

we will emphasize the fundamentals of separations.
separations
Note: 50 to 90 percent of capital investment in chemical plant is for separations equipment.
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Background Material for Separations
The fundamentals that we will apply to study separations in this

course involve:
i l
1. Materials and energy balances: conservation of energy and matter
2. Thermodynamics: phase equilibrium and solution thermodynamics
(Chapter 2)
3. Transport
p p
phenomena ((Chapter
p 3; not emphasized)
p )
4. Chemical reaction kinetics: rate of conversion of one species to another
(not emphasized)
For the most part our analysis of various separations processes will
focus on using phase equilibrium and materials and energy
balances.
balances
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Mass and Energy Balances
Balance Equation
Input + generation – Output =
Accumulation
Control
Vol me
Volume
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Mass and Energy Balances
For non-reacting systems Generation = 0
For systems operated at steady state

Accumulation = 0
Mass and Energy Balances reduce to

Input = Output
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Basic Description of Operations
Separations processes can be run in various modes of operation:
• Batchwise: no flows
• Continuous: continuous flows in and out of separators
• Semicontinuous: pauses in flows.
Operations are classified as key operations and auxiliary operations

• Key Operation: involves reaction or separations
Examples:
l distillation,
di ill i leaching,
l hi reactor
• Auxiliary Operation: involves no change in chemical composition
Examples: pumps, heaters, compressors
Block Flow Diagrams indicate:

•Key Operations by rectangles and
•Flows and Streams by lines
Process Flow Diagrams indicates processes by:

•Realistic symbols of process equipment
•Including auxiliary operations
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Basic Description of Operations
Block Flow Diagram Process Flow Diagram
S1 P1
T t l condenser
Total d
Distillation Distillation
Reflux drum
Overhead vapor
1 Reflux
F Distillate
2
Feed Feed Stage
Boilup
Stripping section stages N
Partial reboiler
Bottoms
P2 S2
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Examples of Industrial Chemical Processes
Refinery for converting crude oil into a variety of marketable products

Production of chemicals (HCl, Ethanol, …..)
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Example of Industrial Chemical Processes
Example: Recovery of hydrocarbons from wet natural gas (wng)

These types of separations generally exploit the differences in volatility to cause a
separation
methane
C2+ ethane
Feed: wng
C2+/abs
C3+
absorber
i-butane
n-butane C4 C4+
C5+ propane
Notice that this pprocess involves a train of separators:

p
This is common in industrial processes.
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Example: Recovery of hydrocarbons from wet natural gas (wng)

These types of separations generally exploit the differences in volatility to cause a
separation
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Example: Hydration of ethylene to ethanol
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Mechanism of Separations
• UNMIXING is not a spontaneous process in nature

A process requiring no external driving force
Reduces randomness and thus decrease the entropy of the system
• Separations involve nonspontaneous processes
• Usually the mixture to separate is a homogeneous, single phase:

Iff not, then
h often
f one willill phase
h separate first
fi
• gravity
• centrifugation
• filtration
filtration.
Product 1
Feed Product 2
S L
S, L,V
V {ci} Product 3
Differ in concentrations,
Separator: Causes different chemical may differ in phase state
components to move to different spatial
l ti
locations to
t be
b collected
ll t d as more pure
mixtures: Differential Transport.
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Separation Technology
Homogeneous mixture
A
A
B
B
C
D C
Homogeneous mixture
A
A
B
B
C
D C/D
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Homogeneous mixture
A
A/B
B
C
D C/D
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Separation
p of the mixture ((A/B/C/D))
would be easier if the components in the
mixture
i t exist
i t in
i different
diff t phases.
h
Phases
Solid
Liquid
Gas/Vapor
p
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Thermodynamics of Separations
Remember that there is an “infinite” driving force associated with

removing the last impurity atom from a pure substance:
ΔSM
Δ SB G’
ΔS A
G' B 0
G' A 0
GA
GB
0 XB 1
0 XB 1
Since the
Si h driving
d i i force
f to mix
i will
ill eventually
ll equall the
h driving
di i
force we introduced to cause the separation the extent of
separation will be limited by thermodynamics equilibrium!
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Rate of Separations
Although the extent of a separation is determined by thermodynamics, the rate of

separations
ti is
i limited
li it d by
b the
th differential
diff ti l rate
t att which
hi h the
th different
diff t species
i are moved.
d
That is:
The Rate of Separation is limited by Mass Transport.
Limits: Extent = Thermodyanmics

Rate = Transport
In this course we will generally focus on the thermodynamic fundamentals

governing separations. Transport issues will be addressed, but not a focus.
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Properties for mass transfer driving force
The ability to separate depends on how the different properties of

the
h components can be b usedd to cause diff
different rates off diffusion.
diff i
The important properties are..
Molecular Properties
-Molecular weight -Polarizability
-van
van der Waals volume Dielectric constant
-Dielectric
-van der Waals area -Electric Charge
-Molecular shape (acentric factor) -Radius of Gyration
-Dipole
Dipole moment
Thermodynamic and Transport Properties

-Vapor pressure
-Solubility
-Adsorptivity
Diffusivity
-Diffusivity
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Main Separations Techniques
Two ways of creating a second phase involve either

Phase
increasing or lowering the temperature or pressure
C
Creation
ti
(Energy-separating agent: ESA)Æ heat or depressurize
Phase
Addition Add solvent or absorber (Mass-separating agent: MSA).
Barrier Use membrane (semipermeable membrane)

Separation
Solid Agent Use particles (reaction, adsorbent film, direct adsorption,

Separation chromatography)
Separation Use electric field, magnetic field, gravity (Hall effect,

by gradient electrophoresis mass spec)
electrophoresis,
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Phase Addition
A
A/C + B =
B/C
Phase I Phase II
Mass-separating
i agent (MSA)
( SA)
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Phase Creation
A
A/C =
C
E
Energy-separating
ti agentt (ESA)
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Phase Creation
A
A/C =
C
E
Energy-separating
ti agentt (ESA)
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Phase Creation or Addition
Phase I Phase II
A B
Interface
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Gas Liquid
A B
Interface
Absorption
(MSA: Liquid absorbent)
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Gas Liquid
A B
Interface
Stripping
pp g
(MSA: Stripping vapor)
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Liquid Liquid
A B
Interface
Extraction
(MSA: liquid solvent)
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Liquid Solid
A B
Interface
Leachingg
(MSA: liquid solvent): liquid-solid extraction
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liquid
A liquid A+C
solid solid
B+C B
Leachingg
(MSA: liquid solvent): liquid-solid extraction
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liquid
A+C
liquid
A+C solid
C
Q
Crystallization
y
(ESA: Heat transfer)
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Most Common • Phase Creation

• Phase Addition
Gaining popularity • Barrier Separation
• Solid Agent separations
Often in labs • Separation by gradient
All five techniques rely on the ability to enhance the rate of mass
transfer of certain species relative to others to effect a spatial
separation
p of components.
p
Thus, all separations processes must introduce a thermodynamic driving force
to overcome the decrease in the entropy of the system as the components are
separated.
The rate of separation is governed by mass transfer, while the extent of

separation
ti isi limited
li it d by
b thermodynamic
th d i equilibrium
ilib i
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Separation by Barrier
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Separation by Solid Agent
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Separation by External Field or Gradient
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Separation by External Field or Gradient
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Common Industrial Separation Methods
Separation Phase of Separation Developed or Separation

Method the feed agent added phase principle
Equilibrium L and/or V Pressure V or L difference
reduction or
flash heat transfer
in volatility
Distillation L and/or V Heat transfer V or L difference
or shaft work
in volatility
Gas V Liquid L difference
absorbent
Absorption in volatility
Stripping L Vapor stripping V difference
agent
in volatility
l l
Extractive L and/or V Liquid solvent V and L difference
and heat
Distillation t
transfer
f
in volatility
Azeotropic L and/or V Liquid V and L difference

entrainer and
Distillation heat transfer
f
in volatility
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Separation Phase of Separation Developed Separation

Method the feed agent or added principle
phase
Liquid-liquid L Liquid Second Difference in
Extraction solvent liquid solubility
solub l ty
Crystalli- L Heat Solid Difference in

zation transfer solubility or
mp
m.p.
Gas V Solid Solid difference in
adsorption adsorbent adsorbabililty
Liquid
d L Solid
ld Solid
ld difference
d ff in
adsorption adsorbent adsorbabililty
Membranes L or V Membrane Membrane difference

ff in
permeability
and/or
solubility
Separation Phase of Separation Developed Separation

Method the feed agent or added principle
phase
Supercritical L or V Supercritical Supercritical Difference
extraction solvent fluid
flu d in solubility
Leaching S Liquid L Difference
solvent in solubility
Drying S and L Heat V Difference
transfer in volatility
Selecting Separation Method
The development of a separation process requires

the selection of:
n Separation methods
o ESAs and/or MSAs
p Separation equipment
q Optimal arrangement or sequencing of the equipment
r Optimal operating temperature and pressure for the equipment
Selection of separation method largely depends of
feed condition –
} Vapor: partial condensation, distillation, absorption, adsorption, gas
permeation (membranes)
} Liquid: distillation, stripping, LL extraction, supercritical extraction,
crystallization, adsorption, and dialysis or reverse osmosis
(membranes)
} Solid: if wet → drying, if dry →leaching
Measures of Separation
ni(1) The Split Fraction is the ratio of the amount of

S li Fraction:
Split F i SFi = ( F )
ni component in a product stream to the feed stream.
ni(1) SFi ,k
Split Ratio: SRi = (2 ) = The Split Ratio is the ratio of the amount of
ni (1 − SFi ,k ) component in two product streams.
Number of moles of i
Ci(1)
Ci(2 ) SRi The separation power is the a ratio of split ratios.
Separation Power: SPi , j = =
C (j1) SR j A Separation Power near 1 indicates a poor separation.
C (j2 )
Concentration
Note: SPi,j only indicates the desired separation and not whether it is achievable. In order to verify
if the desired separation is achievable, the design of the operation, thermodynamic relations,
transport properties, etc., needs to be evaluated.
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Selection of Feasible Separation Techniques
Important Factors
• Feed Conditions (composition, flow rates, T, P, state, …)
• Product conditions (purity/recovery, T, P, state)
• p y Differences ((molecular,, thermodynamic,
Property y ,
transport)
• Characteristics of Separation Operation (scale
(scale-up;
up; stages;
T, P, state requirements; size limitation; energy
requirements; …)
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Selection of Feasible Separation Techniques
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Study Question: Chapter 1 Separation Methods
Section 1.1:
1. What are the two key process operations in chemical engineering?
2. What are the main auxiliary process operations in chemical engineering? ?
3. What is the difference between a block flow diagram and a process flow
diagram?
4 Why
4. Wh d do almost
l t allll iindustrial
d t i l chemical
h i l processes contain
t i separation
ti
operations?
5. Why is the espresso machine a good example of a product design based
on chemical engineering?
Section 1.2:
1. Is the separation of a mixture a spontaneous, natural process?
2 What are the five general separation techniques and what do they all have
2.
in common?
3. Why is mass transfer a major factor in separation processes?
4 What limits the extent to which the separation of a mixture can be
4.
achieved?
5. List at least five property differences that can exploited to develop a
p
separation p
process.
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Section 1.3:
1 What are the two agents that can be used to create a second phase in the
1.
separation of a chemical mixture?
2. What is the most common method used to separate two fluid phases?
3 List five separation operations that use an ESA and five that use an MSA
3. MSA.
4. Give three disadvantages of using an MSA.
5. What is the most widely used industrial separation operation?
6. What is extractive distillation? How does it differ from distillation and when
should it be considered?
7. What is the difference between absorption and stripping?
8. What is liquid-liquid
q q extraction, when should it be considered, and how does it
differ from supercritical-fluid extraction and leaching?
9. What is the basic requirement for removing liquid from a wet solid by
evaporation?
10. Why is crystallization important in the semiconductor industry?
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Section 1.4:
1 How does the mechanism of separation for a microporous membrane differ
1.
from that of a nonporous membrane?
2. Why can't osmosis be used to separate a liquid mixture?
3. How do reverse osmosis and dialysis y differ? What do they
y have in common?
4. How does gas permeation differ from pervaporation?
5. Why are membrane separations important in the human body?
Section 1.5:
1. In the separation of a mixture, how does the action of a membrane differ from
that of a solid adsorbent?
2. What is the difference between adsorption and absorption?
3. Adsorption requires that the adsorbed chemicals be separated from the
adsorbent to regenerate it and prepare it for reuse. How do pressure-swing
adsorption and thermal-swing adsorption differ in the means of regeneration?
Section 1.6:
4. What is the difference between dialysis and electrodialysis?
5. How does field-flow fractionation work from a fluid mechanics standpoint? Can
th flow
the fl field
fi ld b
be tturbulent?
b l t? If not,
t why
h not?
t?
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Section 1.7:
1 The degree of separation in a separation operation is often specified in terms of
1.
component recoveries and/or product purities. How do these two differ?
2. For a separation operation, is it possible to specify the recovery of a feed
component
p and the mole ((or mass)) fraction of that same component
p in one of
the products?
3. Is the component split fraction the same as the component recovery? If not,
how do theyy differ?
4. What is the difference between the split fraction and split ratio?
5. What is a key component? What is a multicomponent product?
6. Using an aqueous sulfuric acid solution in an example, explain the differences
among compositions in terms of molarity, molality, and normality.
Section 1.8:
7. What factors of a separation operation influence the degree of separation?
8. What is the separation power? ?
Section 1.9:
9. When selecting a separation method, what factors are important?
10 What
10. Wh t five
fi separation
ti operations
ti are the
th mostt technologically
t h l i ll mature?t ?
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Chapter 1 Introduction To Separation

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Chapter 1: Separation Methods

The goal of a separations process is to purify solutions.

Example: Example: Example:

The list of different existing separations methods is limitless. Therefore

The fundamentals that we will apply to study separations in this

For non-reacting systems Generation = 0

For systems operated at steady state

Mass and Energy Balances reduce to

Operations are classified as key operations and auxiliary operations

Block Flow Diagrams indicate:

Process Flow Diagrams indicates processes by:

Block Flow Diagram Process Flow Diagram

Feed Feed Stage

Refinery for converting crude oil into a variety of marketable products

Example: Recovery of hydrocarbons from wet natural gas (wng)

Notice that this pprocess involves a train of separators:

Example: Recovery of hydrocarbons from wet natural gas (wng)

Example: Hydration of ethylene to ethanol

• UNMIXING is not a spontaneous process in nature

• Separations involve nonspontaneous processes

• Usually the mixture to separate is a homogeneous, single phase:

Remember that there is an “infinite” driving force associated with

Although the extent of a separation is determined by thermodynamics, the rate of

The Rate of Separation is limited by Mass Transport.

Limits: Extent = Thermodyanmics

In this course we will generally focus on the thermodynamic fundamentals

The ability to separate depends on how the different properties of

Thermodynamic and Transport Properties

Two ways of creating a second phase involve either

Barrier Use membrane (semipermeable membrane)

Solid Agent Use particles (reaction, adsorbent film, direct adsorption,

Separation Use electric field, magnetic field, gravity (Hall effect,

Most Common • Phase Creation

The rate of separation is governed by mass transfer, while the extent of

Separation Phase of Separation Developed or Separation

Azeotropic L and/or V Liquid V and L difference

Separation Phase of Separation Developed Separation

Crystalli- L Heat Solid Difference in

Membranes L or V Membrane Membrane difference

Separation Phase of Separation Developed Separation

 The development of a separation process requires

ni(1) The Split Fraction is the ratio of the amount of

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For non-reacting systems Generation = 0

For systems operated at steady state

The development of a separation process requires