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DISTILLATION
Mass transfer process of separation based on
distribution between the vapor and liquid phases.
ABC
Distillate
(D)
Feed
(F)
Vapor rate
(V)
bottoms
3
ABSORPTION AND DISTILLATION
BOTH involve mass transfer & equilibrium
Differences
1) All components in the mixture transfer during
distillation (this complicates equilibrium calculations).
Vap/Liq Equilibrium = All components exist in both phases
Gas/Liq Equilibrium = Only 1 component exists in both phases
2) Addition of heat is required for distillation
3) Degrees of freedom for distillation of a binary mixture (2
components)
F=CP+2 = 22+2= 2
(Absorption has 3 degrees of freedom)
4) Only 1 feed stream in distillation (2 in absorption/stripping)
INTRODUCTION TO MULTICOMPONENT
DISTILLATION
• Most of the distillation processes deal with
multicomponent mixtures
• Multicomponent phase behaviour is much more complex than
that for the binary mixtures
• Rigorous design requires computers
• Short cut methods exist to outline the scope and limitations
of a particular process
MULTICOMPONENT DISTILLATION
As in binary mixtures calculations of equilibrium stages
usage multi component mixtures also requires
material balances for each component overall and
for each stage
one enthalpy balance overall and one for each stage
complex phase Equilibria
DEGREES OF FREEDOM IN MCD
variables No. to be specified
Feed rate (F) 1
Feed composition 3
Quality of feed 1
Distillate 1
Bottom product 1
Reflux ratio 1
Reflux condition 1
Optimum feed plate 1
Total 10 (= C+6)
PHASE EQUILIBRIA IN MULTICOMPONENT
MIXTURES
Distribution Coefficient or K factors
K's = fn(T, P, comp)
Ki = yie/xie
If Dalton’s law and Roult’s law hold then
Ki = P
i
’/P
We can Use Relative volatility for each component
in system instead of K's
Relative volatility for each component based on
one base component key
I
IJ
J
m
m
o =
VAPOR LIQUID EQUILIBRIUM
Bubble point
Dew point
*
,
,
1.0
i
i j i
i
i j i
y
x
y
x
o
o
=
=
¿
¿
*
,
,
1.0
/
/
i
i i j
i
i i j
x
y
x
y
o
o
=
=
¿
¿
MULTI COMPONENT FLASH DISTILLATION
Vaporizing a definite fraction of liquid
Evolved vapor in equilibrium with residual
liquid
Separate vapor from liquid and then
condense
No reflux
FLASH DISTILLATION
GOVERNING EQUATIONS
1
Fi
Di Bi
x f
y x
f f
÷
= ÷
1
1
Di Fi
i
Bi Bi
y x
K f
x f x
 
= = + ÷

\ .
1 1
1
( 1) 1
Nc Nc
Fi
Bi
i i
i
x
x
f K
= =
= =
÷ +
¿ ¿
DISTILLATION COLUMN DESIGN
FRACTIONATION OR COLUMN DISTILLATION
DISTILLATION COLUMN DESIGN
DISTILLATION COLUMN DESIGN
Tools: Material balance
Energy balance
Thermodynamic equilibrium
Bubble point / dew point summation
Specifications: Purity
Recovery
In multi component separation involving n species,
n1 columns are needed to totally separate all n
species
Computers usually used because of the large
number of variables (T,P, composition, flow rates)
and because iterative solution is necessary
Two different Methods are commonly used to
specify computer input
I. specify feed condition, desired separation
between 2 components, and reflux ratio
II. specify feed condition, no. of stages, and
reflux ratio
KEY COMPONENTS
Light key : designated by L
Heavy key : designated by H
Only KEY components are present in
significant amounts in both Distillate and
Bottom
Usually, L & K are adjacent in rank order of
volatility. This is called a "sharp" separation
DISTRIBUTED AND UNDISTRIBUTED
COMPONENTS
• Components that are present in both the distillate and
the bottoms product are called distributed components
 The key components are always distributed components
• Components with negligible concentration (<10
6
) in one
of the products are called undistributed
A B C D E G
key
components
heavy nondistributed components
(will end up in bottoms product)
light nondistributed components
(will end up in the overhead product)
FENSKE EQUATION FOR MULTICOMPONENT
DISTILLATIONS
Assumption: relative volatilities of components remain constant
throughout the column
1
ln
ln
,
,
,
,
,
min
÷
(
¸
(
¸
=
HK LK
HK D
HK B
LK B
LK D
x
x
x
x
N
o
LK – light component
HK – heavy component
) (
) (
) (
,
T K
T K
T
HK
LK
HK LK
= o
x
N+1
y
N
x
1
y
o
1
N
Total Reboiler
FENSKE EQUATION FOR MULTICOMPONENT
DISTILLATIONS
) (
) (
) (
,
T K
T K
T
HK
LK
HK LK
= o
Choices for relative volatility:
B
T
1) Relative volatility at saturated feed condition
) (
,
, F
F
HK LK
T
HK LK
o o =
2) Geometric mean relative volatility
) ( ) (
, ,
, B
B
D
D
HK LK
T T
HK LK HK LK
o o o =
3
,
) ( ) ( ) (
, , ,
B
B
D
D
F
F
HK LK
T T T
HK LK HK LK HK LK
o o o o =
NON KEY COMPONENT DISTRIBUTION FROM
THE FENSKE EQUATION
(
(
¸
(
¸
=
+
HK B
HK D N
HK i
i B
i D
x
x
x
x
,
, 1
,
,
,
min
o
HK
i
HK i
K
K
=
,
o
(
¸
(
¸
· +
(
¸
(
¸
· ·
=
+
+
HK B
HK D N
HK i
HK B
HK D N
HK i i F
i D
Bx
Dx
Bx
Dx
Fx
Dx
,
, 1
,
,
, 1
, ,
,
min
min
1 o
o
MINIMUM REFLUX RATIO ANALYSIS
•Maximum ratio which require infinite no. of
trays for desired separation
•
•At the minimum reflux ratio condition
invariant zones occurs above and below the
feed plate, where the number of plates is
infinite and the liquid and vapour compo
sitions do notchange from plate to plate
• Unlike in binary distillations, in
multicomponent mixtures these zones
are not necessarily adjacent to the feed
plate location
y
x
z
f
z
f
x
B
x
D
y
1
y
B
x
N
MINIMUM REFLUX RATIO ANALYSIS
* Relative volatility of each component has to be the same for each invariant zone
* Constant molar overflow
* α
i
=K
i
/K
ref
(Usually K
ref
=K
HK
)
The operating line equations for each section of the column become:
Underwood method
B i m i
REF
i
m i
D i n i
REF i
n i
Bx y
K
L
y V
Dx y
K
L
Vy
, , 1 ,
, , 1 ,
÷ =
+ =
+
+
o
o
rectifying section
stripping section
B i m i
REF
i
m i
D i n i
REF i
n i
Bx y
K
L
y V
Dx y
K
L
Vy
, , 1 ,
, , 1 ,
÷ =
+ =
+
+
o
o
rectifying section
stripping section
In the invariant zones: · +
= =
, , 1 , i n i n i
y y y
B i i
REF
i
D i i
REF i
Bx y
K
L
V
Dx y
K
L
V
, ,
, ,
=


.

\

÷
=


.

\

÷
·
·
o
o
( )
( ) A
x
VK L
x
y
D
V
A
x
VK L
x
y
D
V
i
B i
i
REF
i
B i
i
i
i
D i i
REF i
D i i
i
÷
=
÷
= ÷
÷
=
÷
=
·
·
o
o
o
o
o
o
o
o
, ,
,
, ,
,
Underwood method
Minimum reflux ratio analysis
¿ ¿
¿ ¿
÷
= ÷ = ÷
÷
= =
·
·
A
x
B
V
y
D
V
A
x
D
V
y
D
V
i
B i
i
i
i
D i i
i
o
o
o
o
,
,
,
,
We are looking for a condition where
this is correct. In general there are
multiple solutions
But consider the following
) 1 (
, ,
q F
A
x
B
A
x
D V V
i
B i
i
i
D i i
÷ =
÷
+
÷
= ÷
¿ ¿
o
o
o
o
Underwood method
Minimum reflux ratio analysis
) 1 (
, ,
q F
A
x
B
A
x
D V V
i
B i
i
i
D i i
÷ =
÷
+
÷
= ÷
¿ ¿
o
o
o
o
In other words:
A
x
B
A
x
D
A
x
B
A
x
D q F
B D B D
÷
+
÷
+
÷
+
÷
= ÷
2
, 2
2
2
, 2 2
1
, 1
1
1
, 1 1
) 1 (
o
o
o
o
o
o
o
o
Under Underwood conditions: A=Ā,
i
i
o o =
¿
÷
=
÷
+
÷
= ÷
A
x
A
x
A
x
q
i
F i i F F
o
o
o
o
o
o
,
2
, 2 2
1
, 1 1
) 1 (
Underwood method
Minimum reflux ratio analysis
MINIMUM REFLUX RATIO ANALYSIS
¿
÷
= ÷
i
HK i
i F HK i
A
x
q
,
, ,
) 1 (
o
o
¿
÷
= = +
i
HK i
i D HK i
m
A
x
D
V
R
,
, ,
1
o
o
For a given q, and the feed composition
we are looking for A satisfies this equation
(usually A is between α
LK
and α
HK.
Once A is found, we can calculate the
minimum reflux ratio
Underwood method
GILLILAND CORRELATION: NUMBER OF IDEAL
PLATES AT THE OPERATING REFLUX


.

\

+
÷
=
+
÷
1 1
min
D
Dm D
R
R R
f
N
N N
Kirkbride equation: Feed stage location
206 . 0
2
,
,
,
,
(
(
¸
(
¸


.

\



.

\

=
D
B
x
x
x
x
N
N
HK D
LK B
LK F
HK F
S
R
R S
N N N + =
Complete short cut design:
FenskeUnderwoodGilliland method
Given a multicomponent distillation problem:
a) Identify light and heavy key components
b) Guess splits of the nonkey components and compositions
of the distillate and bottoms products
c) Calculate
d) Use Fenske equation to find N
min
e) Calculate distribution of non key components
f) Use Underwood method to find R
Dm
g) Use Gilliland correlation to find actual number of ideal stages
given operating reflux
h) Use Kirkbride equation to locate the feed stage
HK LK ,
o
RIGROUS METHODS
Two broad categories
1. Equilibrium methods
2. Rate based models
Equilibrium methods solve MESH equation simultaneously
Rate based method solve mass and heat transfer equations in terms of
available driving force
MESH equations
M Material balance equations
Total material balance:
Component i balance:
1 1
( ) ( ) 0
n n n sn n sn n
L V F L L V V
÷ +
+ + ÷ + ÷ + =
1 1 1 1 , , ,
. ( ). ( ). 0
n n n n n i n sn n i n sn n i n
L x V y F z L L x V V y
÷ ÷ + +
+ + ÷ + ÷ + =
E Equilibrium relations
S summation of mole fractions
and
H Heat (Enthalpy) balance
, , , , , , 1
. . (1 ). 0
MG i n i n i n i n MG i n i n
E K x y E y
÷ ÷ +
÷ + ÷ =
,
1
i n
i
y =
¿
,
1
i n
i
x =
¿
1 , 1 1 , 1 , , ,
. ( ). ( ). 0
n L n n V n n F n sn n L n sn n V n n
L H V H F H L L H V V H Q
÷ ÷ + +
+ + ÷ + ÷ + ÷ =
RATE BASED MODEL
Consider that murphee efficiency of plates
varies from plate to plate
A simulation program RATEFRAC available
in ASPEN PLUS
EQUIPMENT AND COLUMN SIZING
In order to have stable operation in a distillation column, the
vapor and liquid flow must be managed.
Requirements are:
vapor should flow only through the open regions
of the tray between the downcomers
liquid should flow only through the downcomers
liquid should not weep through tray perforations
liquid should not be carried up the column entrained in the vapor
vapor should not be carried down the column in the liquid
vapor should not bubble up through the downcomers
SINGLE PASS SIEVE TRAY
TRAY DECK
MULTIPLE PASS TRAYS
Single Pass Two Pass Four Pass
TRAY HYDRAULICS
Types of trays
1. Sieve plates
2. Bubblecap plates
3. Valve plates
Types of trays
In order to get a preliminary sizing for
distillation column, we need to obtain values
for
the tray efficiency
the column diameter
the pressure drop
the column height
Stage efficiency analysis
Step 1: Thermodynamics data and methods to predict equilibrium
phase compositions
Step 2: Design of equilibrium stage separation
Step 3: Develop an actual design by applying the stage efficiency analysis
to equilibrium stage design
Stage efficiency analysis
In general the overall efficiency will depend:
1) Geometry and design of contact stages
2) Flow rates and patterns on the tray
3) Composition and properties of vapour and
liquid streams
Stage efficiency analysis
L
in
,x
in
L
out
,x
out
V
out
,y
out
V
in
,y
in
Local efficiency
1
*
1
+
+
÷
÷
'
=
n n
n n
mv
y y
y y
E
Actual separation
Separation that
would have been
achieved on an
ideal tray
What are the sources of inefficiencies?
For this we need to look at what actually happens
on the tray
Stage efficiency analysis
Depending on the location on the tray
the point efficiency will vary
high concentration
gradients
low concentration
gradients
stagnation points
The overall plate efficiency can
be characterized by the Murphree
plate efficiency:
1
*
1
+
+
÷
÷
=
n n
n n
mV
y y
y y
E
When both the vapour and liquid
phases are perfectly mixed the plate
efficiency is equal to the point
efficiency
mv mV
E E =
Point efficiency
Stage efficiency analysis
In general a number of
empirical correlations exist
that relate point and plate
efficiencies
c e
L
Pe
t D
Z
N
2
=
Peclet number
length of liquid
flow path
eddy diffusivity residence time of liquid
on the tray
Stage efficiency analysis
In addition we need to take in account effects of
entrainment
Entrained liquid droplets
Dry Murphree efficiency can be corrected for the
entrainment effects by Colburn equation:


.

\

÷
+
=
¢
¢
1
1
mV
mV
a
E
E
E
entrainment fraction =
entrained liquid/gross liquid flow
Stage efficiency analysis
Finally the overall efficiency of the process defined as
l theoretica
actual
O
N
N
E =
TRAY DIAMETER
U C C F F F C
F F foam factor C
F for
A
A
F
A
A
for
A
A
D
V M
f U
A
A
where
A
A
flood
L V
V
ST F HA F
ST F F
HA
h
a
HA
h
a
h
a
T
vapor
flood
d
V
d
=
÷ 
\

.

=
=

\

.

= ÷
= > =

\

.

+ s s
=
÷

\

.

¸
(
¸
(
(
(
(
=
µ µ
µ
o
t µ
1 2
0 2
20
1 0 0 10 5 0 5 0 06 0 10
4
1
0 1
/
.
. . . . .
: . ( typical value )
0.50
PRESSURE DROP
TRAY COLUMN HEIGHT
Column Height =
# actual stages x tray spacing + space
allowance for feed/draws + sump + top
volume
Tray spacing for most applications is 1824
inches
REBOILERS
Circulating Pump
Heating
Medium
Forced Circulation
Top Tray
Heating
Medium
Vertical Thermosiphon
Top Tray
Bottoms Product
Bottoms Product
Reboilers
Heating
Medium
Kettle
Top Tray
Heating
Medium
Horizontal Thermosiphon
Top Tray
Bottoms Product
Bottoms Product
Reboilers
FEED DISTRIBUTORS
THE “REAL” WORLD
Fouled Structured Packing Damaged Valve Tray
THE “REAL” WORLD
Plugged Distributor Tray “Blanking” Strips
VALVE TRAY DECK
MAJOR TRAY DAMAGE
FOULING RESISTANT DESIGN
FOULED BUBBLE CAP TRAY
GAMMA SCAN TECHNOLOGY
D
i
s
t
a
n
c
e
f
r
o
m
t
o
w
e
r
t
o
p
T
r
a
y
N
u
m
b
e
r
Tower Scan
CLOSE BOILING OR AZEOTROPIC MIXTURE
Binary mixtures having nearly equal to 1
Separation difficult even of ideal mixtures
Third component is used
Two types:
I. Extractive distillation
II. Azeotropic distillation
EXTRACTIVE DISTILLATION
non volatile solvent is used
Associate with one of the
component and increase
Solvent selectivity:
ability to enhance the
separation of key
component
AZEOTROPIC DISILLATION
Entrainer is added
Entrainer forms an low
boiling azeotrope with
one component
CRUDE OIL DISTILLATION
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