DESIGN OF A PACKED

DISTILLATION COLUMN


NAME : Abeyrathna D.K.M.R.P
INDEX NO : 100007E
DATE OF SUB : 04/08/2014
Ethanol and Butyl Acetate mixture

i
CONTENTS
TERMINOLOGY .................................................................................................................................... iii
1 PROBLEM ........................................................................................................................................ 1
2 DESIGN CALCULATION .............................................................................................................. 2
2.1 Packing Material ........................................................................................................................ 2
2.2 Vapour pressure of gas .............................................................................................................. 4
2.3 Construction of Q line ............................................................................................................... 6
2.4 Mass balance for rectification section ....................................................................................... 6
2.5 Mass balance for stripping section ............................................................................................ 9
2.6 Flow rates and compositions calculation ................................................................................. 11
2.7 Rectifying Section ................................................................................................................... 15
2.7.1 Density Calculation .......................................................................................................... 15
2.7.2 Viscosity Calculation ....................................................................................................... 17
2.8 Stripping Section ..................................................................................................................... 19
2.9 The column height ................................................................................................................... 21
2.10 Feed tray location .................................................................................................................... 21
2.11 Heat load .................................................................................................................................. 22
2.11.1 Condenser heat load ......................................................................................................... 22
2.11.2 Reboiler heat load ............................................................................................................. 22
3 SUMMARY .................................................................................................................................... 24
4 REFERENCES ............................................................................................................................... 25


List of Table
Table 3.1 Details of selected packing ....................................................................................................... 2
Table 3.2 Details of packing materials ..................................................................................................... 2
Table 3.3 Saturated pressure of Ethanol & Butyl acetate in different temperatures ................................ 4
Table 3.4 Equilibrium data for composition ............................................................................................ 5
Table 3.5 Density calculation data ......................................................................................................... 16
Table 3.6 Viscosity data ......................................................................................................................... 17
Table 3.7 Parameter values of rectifying section ................................................................................... 17
Table 3.8 Parameters values of stripping section ................................................................................... 21

ii

List of Figures
Figure 3.1 Rectifying section ................................................................................................................... 6
Figure 3.2 Stripping section ..................................................................................................................... 9
List of Graphs
Graph 3.1 Composition graph of Ethanol ................................................................................................ 7
Graph 3.2 Equilibrium curve of Ethanol Butyl acetate mixture .............................................................. 8
Graph 3.3 Temperature-composition diagram of ethanol ...................................................................... 13
Graph 3.4 Composition marked Temperature-composition diagram of ethanol ................................... 14
Graph 3.5 Flooding curve ....................................................................................................................... 18





iii
TERMINOLOGY
x mole fraction of heptane in liquid phase (With suffixes F-feed, D-distillate, W-Bottom product)
y mole fraction of heptane in vapor phase (With suffixes F-feed, D-distillate, W-Bottom product)
R
min
Minimum reflux ratio
R Operating reflux ratio
y
n
Mole fraction of heptane in vapor stream leaving upwards the n
th
theoretical stage
x
n
Mole fraction of heptane in liquid stream leaving downwards the n
th
theoretical stage
D Distillate flow rate (kmol/hr)
F Feed flow rate (kmol/hr)
W Bottom product flow rate (kmol/hr)
L Downwards liquid stream flow rate in rectifying section (kmol/hr)
G Upwards vapor stream flow rate in rectifying section (kmol/hr)
L Downwards liquid stream flow rate in stripping section (kmol/hr)
G Upwards vapor stream flow rate in stripping section (kmol/hr)
L
w
* Liquid mass flow rate along the column (kg/hr)
V
w
* Vapor mass flow rate along the column (kg/hr)

v
Vapor density (kg/m3)

L
Liquid density (kg/m3)
F
p
Packing factor (m-1)

L
Kinematic viscosity of liquid (Ns/m2)
c Latent heat of condensing vapor at condensor (kJ/kg)

L
Latent heat of evaporating liquid at reboiler (kJ/kg)
Qc Condensor heat load
Q
R
Reboiler heat load













1

1 PROBLEM
Design a distillation column with a total condenser and a partial reboiler for the following separation.
Data:
System : Ethanol- butyl acetate
Operating pressure :1 bar
Feed rate : 130kmol/hr
Feed condition : saturated liquid
Feed composition : 62mol% ethanol
Distillate composition : 97mol% ethanol
Bottom product composition : 5mol% ethanol
Column type : Packed column
Packing type : Intalox saddles

Select a suitable packing material, packing size, pressure drop across packing or percentage of
flooding and a reflux ratio. Obtain an appropriate HETP value HTU from the literature and determine
the Number of ideal stages required the column height and the diameter of the column, feed tray
location and the Condenser and Reboiler heat loads.
The report should include detail calculation, graphical constructions, data used for the calculation,
assumptions made and the references. Mechanical design and construction are not required. Mc-Cabe
and Thiele method, Ponchan - Savarit method or HTU-NTU method can be used. All the important
information should be summarized in the last page of the report.

2

2 DESIGN CALCULATION
2.1 Packing Material
The distillation is supposed to be done at 1 bar pressure.The packing is selected as pressure drop is
reduced.The pressure drop has to be maintained to keep the column below the flooding condition.
There two packing method for packed distillation which random and structured packing. According to
the given data we need to use Intalox saddles type packing material. Intalox saddles type is used in
random packing method. So we have to use random packing method for our distillation process. In
intalox saddles type has different type raw material such as ceramic, metal, plastic and carbon.
Many plastic type reacts with butyl acetate. As well as some temperature condition are affects for
plastic. There for we can ignore plastic type. Weight of column increase due to ceramic. Weight of
ceramic is higher than metal. So metal is good for packing material. Some metal saddles are reacted
with ethanol and butyl acetate. Stainless steel, Hastelloy saddles can be used. But that material cost is
very high and consider the availability in market most intalox saddles types are ceramic. Therefore use
ceramic intalox saddle for packing material.

Material : ceramic intalox saddle

Table 2.1 Details of selected packing
Name Intalox Saddles
Material Ceremic
Size (mm) 38
Bulk density (kg/m3) 625
Specific Surface area (a) (m2/m3) 194
Packing Factor (F
p
)(m-1) 170
HETP 0.60 - 0.75




Table 2.2 Details of packing materials
3





































4

2.2 Vapour pressure of gas
Saturated vapour pressure can be calculated using below equation.
Limits of this equations can be use;
For Ethanol: 159.05K to 514K
For Butyl Acetate: 199.65K to 574.5K [3]

Component C
1
C
2
C
3
C
4
C
5
Ethanol 122.82 -9253.2 -14.99 1.05E-05 2
Butyl Acetate 73.304 -7122.3 -7.1424 2.89E-06 2

Table 2.3 Saturated pressure of Ethanol & Butyl acetate in different temperatures
Temperature(
0
C)
Vapour Pressure(mmHg)
Ethanol Butyl acetate
78.37
760 151
80 807 161
85 978 195
90 1177 235
95 1408 281
100 1675 334
105 1982 395
110 2334 465
115 2733 544
120 3186 634
125 3698 735
126 3806 760

From Raoults law

Applying Raoults law for Ethanol & Butyl acetate;

From Daltons Law;

In the mixture, only contain Ethanol and Butyl Alcohol


5

Therefore,

From Daltons law;

Values of

and

can be calculated for each temperature using equation

Consider the vapour pressure values at 80
0
C.

-
-

)

Table 2.4 Equilibrium data for composition












Temperature(
0
C)
Vapour Pressure(mmHg) Mole Fraction
Ethanol Butyl acetate X
Ethanol
Y
Ethanol
78.37 760 151 1.00 1.00
80 807 161 0.93 0.98
85 978 195 0.72 0.93
90 1177 235 0.56 0.86
95 1408 281 0.42 0.79
100 1675 334 0.32 0.70
105 1982 395 0.23 0.60
110 2334 465 0.16 0.48
115 2733 544 0.10 0.35
120 3186 634 0.05 0.21
125 3698 735 0.01 0.04
126 3806 760 0.00 0.00
6




2.3 Construction of Q line




Feed condition is saturated liquid.




2.4 Mass balance for rectification section
Assumption
Constant molar overflow
Reflux is at its boiling point



Material balance for the system boundry
V = L + D-------------------------------------(1)
For m.v.c.( Ethanol)
V L
Figure 2.1 Rectifying section
7

V

. y
n+1
= L. x
n
+ D. x
D
---------------------------(2)
From (1) and (2)



Operating line equation for the rectification section (Top Operating Line)

) ( .x
R 1
1
.x
R 1
R
y
D n 1 n
A

Gradient of the operating line = (R/(R+1))
Intercept = x
D
/(R+1)
Operating line intersects, y = x line at ( x
D
, x
D
)




0.00
0.10
0.20
0.30
0.40
0.50
0.60
0.70
0.80
0.90
1.00
0.00 0.10 0.20 0.30 0.40 0.50 0.60 0.70 0.80 0.90 1.00
M
o
l
e

f
r
a
c
t
i
o
n

o
f

E
t
h
a
n
o
l

i
n

v
a
p
o
u
r


Mole fraction of Ethanol in Liquid
q line
top operating line

D n 1 n
.x
D L
D
.x
D L
L
y

Graph 2.1 Composition graph of Ethanol

8

Top operating line equation in minimum reflux




D
min
n
min
min
1 n
.x
R 1
1
.x
R 1
y

R
actual
is in between 1.2R
min
and 1.5R
min
.
Let assume R
actual
= 1.3R
min
=1.30.2963=0.3852
=>

D
actual
n
actual
1 n
.x
R 1
1
.x
R 1
y

actual
R

00 7 . 0 .x 278 . 0 y
n 1 n

0.00
0.10
0.20
0.30
0.40
0.50
0.60
0.70
0.80
0.90
1.00
0.00 0.10 0.20 0.30 0.40 0.50 0.60 0.70 0.80 0.90 1.00
A
x
i
s

T
i
t
l
e

Axis Title
Graph 2.2 Equilibrium curve of Ethanol Butyl acetate mixture
9


Number of Theoretical plates required for the separation = No. of steps 1
=7-1
= 6
2.5 Mass balance for stripping section


Material balance for the system boundary;

For the m.v.c. (Ethanol)

Bottom Operating Line
(B)
m
.x
W L
W
m
.x
W L
L
1 m
y

From graph
Figure 2.2 Stripping section
10

Gradient=

11

2.6 Flow rates and compositions calculation
F : 130kmol/hr
X
F
: 0.62
X
D
: 0.97
X
W
: 0.05

Mass balance for the system


Mass balance for ethanol

From (1) & (2)

From bottom operating line;

12


13


75
76
77
78
79
80
81
82
83
84
85
86
87
88
89
90
91
92
93
94
95
96
97
98
99
100
101
102
103
104
105
106
107
108
109
110
111
112
113
114
115
116
117
118
119
120
121
122
123
124
125
126
127
128
129
130
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
B
o
i
l
i
n
g

p
o
i
n
t
(
C
)

Mole fraction
Ethanol in liquid
Ethanol in Vapor
Graph 2.3 Temperature-composition diagram of ethanol
14

75
76
77
78
79
80
81
82
83
84
85
86
87
88
89
90
91
92
93
94
95
96
97
98
99
100
101
102
103
104
105
106
107
108
109
110
111
112
113
114
115
116
117
118
119
120
121
122
123
124
125
126
127
128
129
130
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
B
o
i
l
i
n
g

p
o
i
n
t
(
C
)

Mole fraction
Ethanol in liquid
Ethanol in Vapor
Graph 2.4 Composition marked Temperature-composition diagram of ethanol
15

2.7 Rectifying Section
The composition of the gas and liquid streams vary along the column and so the mass flow rates and
the stream densities for gas and liquid also vay along the column. Therefore for the rectifying section,
the average composition of the feed and the distillate has been considered to determine the mass flow
rates and the densities.
Ethanol molar fraction at feed = 0.62
Ethanol molar fraction at distillate = 0.97
Molar mass of Ethanol= 46.06844 kg/kmol
Molar mass of Butyl Acetate=116.16 kg/kmol
Average temperature value of rectifying section =

Average composition for rectifying section taken at as X= 0.780 and Y = 0.945
Molar mass in feed=
Molar mass in Distillate
Average molar mass

Mass fraction of A=



Mass fraction of Ethanol M
Ethanol
=

11616
= 0.5844
Mass fraction of Butyl acetate M
Butyl acetate
= 1- M
Ethanol

= 1-0.5844
= 0.4156

Mass fraction of Ethanol M
Ethanol
=

11616
= 0.8720
Mass fraction of Butyl acetate M
Butyl acetate
= 1- M
Ethanol

= 1-0.8720
= 0.128

2.7.1 Density Calculation
Density of organic compound

[2]
Where C
1,
C
2,
C
3,
C
4
are constant and T is temperature.




16

Table 2.5 Density calculation data
Constants Ethanol Butyl acetate
C
1
1.6288 0.67794
C
2
0.27469 0.2637
C
3
514 575.4
C
4
0.23178 0.29318
Temperature(
0
C) Densities(mol/dm
3
)
83.5 15.835 7.017
104 15.348 6.819

Density of Ethanol at

= 729.4937 Kg.m
-3

Density of Butyl acetate at

= 815.0947Kg.m
-3

For Vapour region

By Doltons law

Where,

is partial pressure of ethanol

To calculate density of ethanol at this temperature and pressure, we can calculate as follow

11616

17

Mass flow rate of vapor stream

= V kmol/hr x Average molar mass kg/kmol

= 6742.8575
Mass flow rate of liquid stream

= L kmol/hr x Average molar mass kg/kmol

= 1875.0641

2.7.2 Viscosity Calculation
Liquid Viscosity can be represent by function of temperature. Where C
1,
C
2,
C
3,
C
4
are constant and T is
temperature. [3]

Table 2.6 Viscosity data
Constants Ethanol Butyl acetate
C
1
7.875 -17.488
C
2
781.98 1478.2
C
3
-3.0418 0.91828
C
4
- -
C
5
- -
Temperature(
0
C) Viscosity(Pa.s)
83.5 4.072*10
-4
3.5427*10
-4

104 3.049*10
-4
2.9765*10
-4

Table 2.7 Parameter values of rectifying section


Average molar mass

6742.8575

1875.0641







18

Graph 2.5 Flooding curve
The pressure drop inside the packed column determines the maximum possible gas velocity through
the packed column. There is a maximum value for the gas velocity at a given pressure drop which
further increment of gas velocity causes flooding. So the safety margin we provide to save the column
from flooding determines the pressure drop we maintain within the column. For a selected pressure
drop, the correlation to determine the internal gas velocity are illustrated in the figure below. Now the
above calculated internal liquid and gas flow rates can be used to determine the allowed gas phase
velocity that inside the column without flooding.





























19

for the rectifying section,

=>

18750641

F
LV
= 0.1195
For random packing the pressure drop will not normally exceed 80 mm of water per meter of packing
height. At this value the gas velocity will be about 80 per cent of the ooding velocity (Sinnott, 2005).
However the recommended pressure drop for packed column distillation to keep in a safer region from
flooding is between 40-80 mm of water column per meter of packing height (Sinnott, 2005). So let us
consider 60 mm water column pressure drop per meter of packed height for our design.
Therefore using the pressure correlation closer to 60 mm water/m in Graph 3.5 above, the relevant K4
value for the rectifying section is 1.8.
:.

But the total mass flow rate in vapor stream of the rectifying section is supposed to be 6742.8575 kg/hr
according to the above calculation.
So if the column diameter is D,
Column cross section area

D
rectifying
= 1.6827 m

2.8 Stripping Section
Similarly as above, the average composition of the feed and the residue has been considered to
determine the mass flow rates and the densities of vapor and liquid streams of the stripping section.
Ethanol molar fraction at feed = 0.62
Ethanol molar fraction at distillate = 0.05
Therefore average molar fraction of Ethanol in rectifying section = (0.62 + 0.05)/2 = 0.335
Molar mass in feed=
Molar mass in Distillate
Average molar mass

Average temperature value of stripping section =

Average composition for stripping section taken at as X= 0.245 and Y= 0.620
20

Mass fraction of Ethanol in liquid M
Ethanol
=

11616
= 0.13549
Mass fraction of Butyl acetate in liquid M
Butyl acetate
= 1- M
Ethanol

= 1-0.13549
= 0.86451
Mass fraction of Ethanol in vapour M
Ethanol
=

11616
= 0.4676
Mass fraction of Butyl acetate in vapour M
Butyl acetate
= 1- M
Ethanol

= 1-0.4676
= 0.5324
Density of Ethanol at

=707.0584 Kg.m
-3

Density of Butyl acetate at

= 792.095 Kg.m
-3

11616

Mass flow rate of vapor stream

= V kmol/hr x Average molar mass kg/kmol

= 12732.2822
Mass flow rate of liquid stream

= L kmol/hr x Average molar mass kg/kmol

= 17315.9224

21


Table 2.8 Parameters values of stripping section

Average molar mass

12732.2822

17315.9224
for the rectifying section,

=>

173159224

F
LV
= 0.0279
Similarly as in rectifying section, a pressure drop of around 60mm water column per meter has been
assumed. Therefore using the pressure correlation closer to 60 mm water/m in figure 3 above, the
relevant K4 value for the rectifying section is 2.9.
:.

But the total mass flow rate in vapor stream of the rectifying section is supposed to be 12732.2822
kg/hr according to the above calculation.
So if the column diameter is D,
Column cross section area

D
Stripping
= 1.5446 m
2.9 The column height


2.10 Feed tray location
According to stages counting figure feed location should be between two & three stages from the top.
Feed tray location=
22

2.11 Heat load
2.11.1 Condenser heat load
The total condensor is used in the vapor stream leaving the top most column to totally convert it into
liquid form. So the resultant liquid will consist of the same composition as the vapor which was
subjected to condensation and the condensor heat load will be the latent heat required to condense this
vapor stream up to its dew point.
Flow rate of the vapor stream of the rectifying section (G) = kmol/hr
As we have 97% Ethanol and 3% butyl acetate in this stream,

Component

(kJ/kmol)

(K)

(K)
Ethanol 38600 514 351.37
Butyl acetate 35893.44 575.4 399

So latent heat of the Ethanol (
1
) =

38842.668 kJ/kmol
latent heat of the Butyl acetate (
2
) =

39264.243kJ/kmol
Average latent heat () = 38842668 39264243
Therefore condensor heat load (Qc) = V x
=
=4335009.784kJ/hr
=

=1202.78kW

2.11.2 Reboiler heat load
Component

(kJ/kmol)

(K)

(K)
Ethanol 38600 514 351.37
Butyl acetate 35893.44 575.4 399

So latent heat of the Ethanol (
1
) =

34765.765 kJ/kmol
latent heat of the Butyl acetate (
2
) =

3kJ/kmol

23

Average latent heat () = 3
Therefore Reboiler heat load (Q
R
) = V' x
=
=4983215.651kJ/hr
=

=1384.167kW






























24

3 SUMMARY
Column type =Packed column
Packing material = 38 mm ceremic Intalox Saddles
Pressure drop across packing=60mm H
2
O/m
Reflux ratio =0.3852
Number of theoretical plates =6
Column Height =
Column diameter = 1.6827 m m for rectifying section
= 1.5446 m m for stripping section
Feed entering location=
Condensor heat load = 1202.78kW
Reboiler heat load = 1384.167kW


25

4 REFERENCES

[1] R. H. Don W.Green, "Vapor Pressure of Inorganic and Organic Liquids," in Perry's Chemical
Engineers' Hand Book, The Mc-Graw-Hill companies, 2008, pp. 2-56 to 2-60.
[2] R. H. P. Don W. Green, "Densities of Inorganic and Organic Liquids," in Perry's Chemical
Engineers' Handbook, Eighth Edition, MC-Graw Hill, 2008, pp. 2-98 and 2-100.
[3] R. H. P. Don W. Green, "Viscosity of Inorganic and Organic Liquids," in Perry's Chemical
Engineers' Handbook, Eighth Edition, Mc-Graw Hill, 2008, pp. 2-427 and 2-429.
[4] R. Sinnott, Coulson & Richardsons' Chemical Engineering Series-Chemical Engineering Design,
Oxford: Elsevier Butterworth-Heinemann, 2005.
[5] S. B. Thakore and B. Bhatt, Introduction to Process Engineering and Design, New Delhi: Tata
McGraw-Hill Education, 2007.
[6] L. AceChemPack Tower Packing Co., "Random & Structured Ceramic Packing," 2000. [Online].
Available: http://www.tower-packing.com/Dir_ceramic_packing.htm.