Mass Transfer Design

CCB2053

Dr Sintayehu Mekuria Hailegiorgis

Department of Chemical Engineering

Distillation Process

Multicomponent Distillation

CCB2053

Lesson outline
Flash distillation of multicomponent mixtures
Approximate Shortcut Methods for Multicomponent
Distillation

Estimate number of equilibrium stages

using an empirical correlation:- relates actual number of
stages to:
1. number of stages at total reflux
2. minimum reflux ratio
3. actual reflux ratio

Estimate feed location with an empirical correlation

Lesson outcome
At the end of the session, the students are able to:
Estimate the number of theoretical stages used in
multicomponent distillation to achieve the desired
separation.
Able to estimate the feed tray location in multicomponent
distillation process.

Recap of Pervious lesson

Multicomponent distillation

Multicomponent distillation - terminology

Key Components

Distributed components
Non-distributed light and heavy non-key components

Equilibrium data in multi component distillation

Boiling point,
dew point and

CCB2053

Flash distillation of multicomponent mixtures

For flash distillation, the process flow is shown in the figure below
Defining,
V, yi

Separator

F, xiF
Heater

Expansion
valve

L, xi

f = V/F and
1- f = L/F

Making a component i balance,

the following equation can be
obtained:

yi

x
f 1
xi iF
f
f

(3.90)

Where: yi is the composition of i in the vapor, in equilibrium with xi in the

liquid after vaporization. From equilibrium,

yi = Kixi = KCixi, where i = Ki/KC, the Eq.(3.90) becomes;

yi K C i xi

x
f 1
xi iF
f
f

(3.91)

Solving for xi and summing for all components,

xi

xiF
1.0
f K C i 1 1

(3.92)

This is solved by trial and error method first assume the temperature if the fraction f
vaporized has been set.
When the xi values add up to 1.0 the proper temperature has been chosen.
The composition of the vapor can be obtained from yi = KCixi or by a material
balance.

Approximate Shortcut Methods for

Multicomponent Distillation in a Fractional
distillation
Estimate number of equilibrium stages
using an empirical correlation
relates actual number of stages to:

1. number of stages at total reflux

2. minimum reflux ratio
3. actual reflux ratio

Estimate feed location with an empirical

correlation

Total Reflux for Multicomponent Distillation

1. Minimum stages for total reflux - Fenskes equation
Fenskes equation for binary mixture to find the minimum number of
theoretical stages, N m can also apply for multicomponent distillation.
When applies to the heavy key, H and the light key, L, it becomes;

Nm

xLD D
xHW W
log

x
D
xLW W
HD

log L.av

(3.93)

Where: xLD is mole fraction of light key in distillate, xLW is mole fraction in
bottoms, xHD, is mole fraction of heavy key in distillate and xHW is mole
fraction in bottoms.
the average value of L,av for the light key is calculated from LD at the top
temperature (dew point) of the tower and LW at the bottom temperature:

 L,av LD LW

(3.94)

Since the distribution of the other component is not known, the distillate
dew point and bottom boiling point estimation is partially trail and error
method.

2. Distribution of Non-key Components at Total Reflux

The Fenske equation is not restricted to the two key components.
Once Nmin is known, Fenske equation can be used to calculate mole
fractions for all non-key components
To determine the distribution and concentration of non-key components in
the distillate and bottoms at total reflux Eq. (3.93) can be rearranged and
written for any other component i as follows:

xiD , D
xHD
N
i ,av m
xiW , W
xHW W

(3.95)

These concentrations of the non-key components determined at total reflux

can be used as approximations with the finite and minimum reflux ratios.

Minimum Reflux Ration for Multicomponent

Distillation
In binary distillation, minimum reflux ratio, Rm is the reflux that requires an
infinite number of trays to achieve the desired separation.
In binary distillation, only one pinch point occurs at the feed plate where the
number of steps become infinite as shown below.

Location of pinch-point
zones at minimum reflux

In multicomponent system, two pinch point occurs:

One above the feed plate
The other below the feed plate as shown below

Pinch
point

stage between the feed stage and the rectifying

section pinch point remove heavy components
from the distillate
The heavy components concentrations change from
plate to plate and reduced to near zero when the
pinch point (or invariant zone) is reached.

stage between the feed stage and the stripping section pinch point
remove light components from the bottoms
The light components concentrations change from plate to plate and
reduced to near zero when the pinch point (or invariant zone) is reached
The rigorous plate-by-plate stepwise procedure for calculating Rm is trial and
error and can be extremely tedious for hand calculation.

Underwood Equation - Minimum Reflux

Underwoods shortcut method for calculating Rm provides a reasonable
accurate value.
It uses constant average values and assumes constant flows in both
sections of the tower
The two equations to be solved to determine the minimum reflux
ratio, Rm are;

i xiF
1 q
i
i xiD
Rm 1
i

(3.96)

(3.97)

 The values for xiD for each component in the distillate in Eq.(3.97) are
supposed to be the values at Rm.

However, to start with the estimation, an approximate values obtained

for total reflux using Fenkes method can be used.
Since may vary with temperature, the average value of for the top
temperature and bottom temperature as calculated in Fenske equation can
be used.
To solve for Rm, the value of in Eq.(3.96) is first obtained by trial and
error method.
The value of lies between the values of the light key and the
heavy key.
Using the value of , the value of Rm can be obtained directly.

Gilliland Correlation
Correlation for Actual Number of Stages at Finite Reflux Ratio
Gilliland - empirically relate N at finite R to Nmin and Rmin

Procedure to use the Gilliland correlation:

1. Calculate Nmin from the Fenske equation
2. Calculate Rmin from Underwood equation
3. Choose actual R

Gilliland correlation

y=

x=

R Rm
R 1

Figure 7-3 Gilliland correlation as modified by Liddle (1968);

Reprinted with permission from Chemical Engineering, 75(23), 137 (1968), copyright 1968, McGraw-Hill.

From Separation Process Engineering, Third Edition by Phillip C. Wankat

(ISBN: 0131382276) Copyright 2012 Pearson Education, Inc. All rights reserved.

Gilliland Correlation
Calculate the actual number of stages by using
the Gilliland correlation
1 54.4 X X 1
N N min
Y
1 exp
0.5
N 1
11 117.2 X X

where

R Rmin
X
R 1

(3.98)

(3.99)

 An alternative method is the empirical correlation of Erbar and

Madox which is similar to Gilliland correlation;
It is used to estimate the theoretical number of stages
required for an operating reflux ratio, R and is an
approximate method.
As shown in the Figure below, the operating reflux ratio, R
is correlated with the minimum Rm obtained using the
Underwood method, the minimum number of stages, Nm
obtained using the Fenske method and the number of stages
at the operating, R.

Estimate of feed plate location

Kirkbride had devised an approximate method to estimate the number of
theoretical stages above and below the feed which can be used to estimate
the feed stage location as presented below.

x
Ne
log
0.206 log HF
Ns
xLF

W xLW

D xHD

(3.100)

Where Ne is the number of theoretical stages above the feed

plate and Ns is the number of theoretical stages below the
feed plate.

Example
The liquid of 100mol/h at the boiling point is feed to a distillation tower at 405.3
kPa. The composition of the feed is as follows: n-butane (xA = 0.40),
n-pentane (xB= 0.25), n-hexane (xC = 0.20), n-heptane (xD = 0.15). The feed is to
be fractionated so that 90% n-pentane (B) is recovered in the distillate and 90%
of the n-hexane (C) in the bottoms. Calculate the following
a.
b.
c.
d.
e.

f.

Moles per hour and composition of the distillate and bottoms

Top temperature (dew point) of distillate and boiling point of bottoms.
Minimum stage for total reflux and distribution of other non-key
components in the distillate and in the bottom.
Minimum reflux ratio using Underwood methods
Number of theoretical stages at operating reflux ratio R of 1.5Rm using the
Erbar and Madox correlation
Location of the feed tray using the method of Kirkbride

Solution
a. Moles per hour and composition of the distillate and bottoms

Material balance for each component need to be made

Choice of key components:
n-pentane (B) light component, L
n-hexane (C) heavy component, H
For the over all balance
F =D + W
For Component B light key balance
FxBF = DyBD + WxBW
0.25(100) =25 = DyBD + WxBW

Since 90% of B is in the distillate,

DyBD = (0.9)*25 = 22.5
Hence,

WxBW = 2.5

For Component C, heavy key balance

FxCF = DyCD + WxCW

0.2(100) =20 = DyCD + WxCW

Also 90% of C is in the bottom,
DyCW = (0.9)*20 = 18.0
Hence,

DxCD = 2.0

For the first trail it is assumed that no component D (heaver than

the heavier key, (C) is in the distillate and no light A in the bottoms.
Hence, mole A in the distillate is;
DyAD = 100*(0.4) = 40
Also moles D in bottom is
WyDW = 100*(0.15) = 15
This values are tabulated as shown below;

b. Top temperature (dew point) of distillate and boiling point of bottoms

For the top temperature (dew point) of distillate, a value of 67oC will be
estimated for the first trial. The K values are read from the graph and the
values are calculated
Using Eqs. (3.88) and (3.89), the following values are calculated;
(3.88)
yi 1
yi

yi
xi

K


1
C
i

(3.89)

The calculated value of KC is 0.2627, which corresponds very closely to 67oC

therefore,

it is the final temperature of the dew point.

For the bubble point of the bottom, a temperature of 135oC is assumed for the
first trial and Eqs. (3.86) and (3.87) are used for the calculation

yi Ki xi KC i xi 1
yi

i xi
( i xi )

(3.86)
(3.87)

A second trial is made using 132oC that gives the final temperature as shown below

The calculated value is 1.144, which is the value at 1320C.

c.

Minimum stage for total reflux and distribution of other non-key

components in the distillate and in the bottom.

in this case, the proper values of the light key L (n-pentane ) to use in
EQ.(3.94) is

L,av LD LW

(3.94)

 LD = 2.5 (T = 67oC at the top of the column)

LW = 2.04 (T = 132oC at the bottom of the column)
Then,

L ,av

LD LW

2.5 * 2.04

2.258
Substituting in to Eq.(3.93)

x D

xHW W
log LD

x
D
x
W
HD
LW

Nm
log L.av

log 0.349 * 64.5

0.507 * 35.5

0.031* 64.5
0.070 * 35.5
log( 2.258)

5.404 theoretica l stages (4.404 theoretica l trays )

 The distribution or composition of the other components can be

calculated using Eq.(3.95)
DxiD
DxHD
N
i ,av m
xiW , W
WxHW

(3.95)

For component A, the average value to use is

A,av AD AW 6.73 * 4.348
5.409

x AD , D
DxHD
N
A, av m
x AW , W
WxHW
5.409

5.404

64.5 * 0.031
35.5 * 0.507

(a)

1017

making an over all balance on A

FxAF = 40 = DxAD + WxAW

(b)

 Substituting DxAD = 1017WxAW from Eq.(b) to Eq.(a) and solving

WxAW = 0.039, DxAD = 39.961
For the distribution of component D ,

D,av DD DW

0.385 * 0.530 0452

xDD , D
N m DxHD
D , av
xDW , W
WxHW
0.452

5.404

645 * 0.031
0.001521
355 * 0.507

making an over all balance on D

FxDF = 15 = DxDD + WxDW
SOLVING

DxDD = 0.023; WxDW = 14.977

 The revised bottom and top compositions are as follows;

Minimum reflux ratio using the Underwood methods;

In this case the temperature to use to determine the value of
i is the average between the top of 67oC and the bottom of
132oC, i.e.,
67 + 132=99.5

The Ki obtained from Ki vs T diagram and the i values and

distillate and feed compositions to use in Eq.(3.96)and (3.97) are
as follows

Substituting into Eq. (3.96) with q=1 for feed at the boiling point

i xiF
1 q
i
1 1 0

5.20(0.40) 2.30(0.25) 1.0(0.20) 0.467(0.15)

5.2
2.3
1.0
0.467

This is trial and error, so a value of = 1.21 will be used for the
first trial ( must be between 2.3 and 1.00). This and other trials
are shown below.

The final value = 1.2096 is substituted into eqn. (3.97) to solve

for Rm.

i xiD
Rm 1
i
5.20(0.40) 2.30(0.25)
1.0(0.20)
0.467(0.15)

5.2 1.2096 2.3 1.2096 1.0 1.2096 0.467 1.2096

Rm 0.395

Number of theoretical stages at operating reflux ratio R of

1.5Rm using the Erbar and Madox correlation

R 1.5Rm 1.5 * 0.395

0.593
R
0.593

0.3723
R 1 0.953 1
Rm
0.395

0.2832
Rm 1 0.395 1
Using this two values, from Figure
of Erbar-Maddox correlation

Nm
5.4
0.49
N 11
N
N

Therefore, 11 theoretical stages are in the tower. This gives 111(reboiler),or 10 theoretical trays.

Location of the feed tray using the method of Kirkbride

Using Eq.(3.100)
x
Ne
log
0.206 log HF
Ns
xLF

xLW

xHD

0.20 35.516 0.0704 2

0.206 log

0
.
25
64
.
484
0
.
310

0.07344

Hence

Ne
10 0.0 3 7 4 4 1.84
Ns

N e 1.84 N s
N e N s N 11
1.84 N s N s 2.84 N s 11
N S 5 and N e 6
Hence, the feed is entered at the 6th tray.