CHAPTER 2

DESIGN OF DISTILLATION COLUMN

2.1 Distillation Column

Distillation is a method used to separate the components of a liquid solution, which

depends upon the distribution of these various components between a vapor and a
liquid phase. All components are present in both phases. The vapor phase is created
from the liquid phase by vaporization at the boiling point.

Characteristics in chosen types of distillation column are requirement of

separation objective satisfied with this distillation column, the cost of construction and
simplicity in design. The design of a distillation column can be divided into the following
steps:

i. Specify the degree of separation required; set product specifications.

ii. Select the operating conditions: batch or continuous; operating pressure.
iii. Select the type of contacting device: plates or packing.
iv. Determine the stage and reflux requirements: the number of equilibrium stages.
v. Size of the column: diameter, number of real stages.
vi. Design the column internals: plates, distributors, packing support.
vii. Mechanical design: vessel and internal fittings.

2-1
Table 2.1 shown the condition in inlet and outlet streams of distillation column (Dc 3)

Table 2.1: Condition in inlet and outlet streams of distillation column (Dc 3)
Molar Flow Mass Flow Temperature ( C) Pressure(kpa)
Rate (kmol/m3) Rate(kg/m3)
Feed 197.1 32950 294 820
Distillate 132.4 20260 274.2 600
Bottom 64.65 12690 347.2 600

Figure 2.1 shows the condition in inlet and outlet streams of distillation column.

Vn

Distillate,D
Ln
Feed,F

Bottom,B
Figure 2.1 : Condition in inlet and outlet streams of distillation column(Dc 3)

2-2
2.2 Chemical Design of Distillation Column

2.2.1 Key components

Before commencing the column design, the two ‘keys’ components between which it is
desired to make the separation must be selected. The light key will be the component to
be kept out of the bottom product. It has small boiling point and more volatile. The
heavy key is the component to be kept out of the top product. It has large boiling point
and less volatility. Specifications will be set on the maximum concentrations of the keys
in the top and bottom products. The keys are known as ‘adjacent keys’ if they are
adjacent in a listing of the components in order of volatility. While ‘split keys’ is where
some other component lies between them in the order; they will usually be adjacent.

In this design purposes, the light key and the heavy key were determined. The
light key in this column is decene (C10H20) whilst the heavy key in the column is
tetradecene (C14H28) which is the product.

2.2.2 Minimum number of stages

Fenske (1932) equation can be used to calculate minimum number of stages required
at total reflux. Bottom and top stream temperature is calculated by the use of Antoine
equation and Roult’s Law in order to get value of average relative volatility. Those
equations are fairly applied for multicomponent systems.

Minimum number of stages (Fenske) is given as:

 x  x 
log  LK   HK 
 xHK  D  xLK  B
Nm  Eqn (2.1)
log  a

2-3
xLK,D  mol faction of light key in distillate
xHK, D  mol fraction of heavy key in distillate
xHK, B  mol fraction of heavy key in bottom stream
xLK, B  mol fraction of light key in bottom stream
αa  Average relative volatility of light key

2.2.3 Average relative volatility a ,

It is in need to identify the light and heavy key to determine average relative volatility.
Water is needed to recover much at distillate; therefore it is a light key.  a can be
determined by knowing top and bottom column temperature.

2.2.4 Determination of Bubble point Tbp and dew point Tdp

Trial and error procedure is required to calculate Tdp and Tbp by the use of Antoine
Equation. The temperature must satisfy the following criteria:
Dew point:  x   y / K  1.0
i i i

Bubble point:  y   K x  1.0

i i i

In w hich:
Pi
K
P
Pi is saturation pressure at any guess temperatur e that satisfied the criteria.

The vapor pressure can be calculated by using Antoine equation:

b
LogPi  a  Eqn (2.2)
T c

Where : Pi = Vapor pressure in mmHg

T = Temperature in Celcius
a,b and c = Constant values of Antoine Equation

2-4
 Table 2.2 shown the constant values of Antoine Equation for each component
while Table 2.3, Table 2.4 and Table 2.5 shown the variable at top, bottom and feed
column of distillation column.

Table 2.2 : Constant values of Antoine Equation for each component

Comp A B C
Decene(c10h20) 6.9103 1501.872 197.578
Dodecene(c12h24) 6.97522 1619.862 182.271
Tetradecene(c14h28) 7.02005 1745.001 170.475

a) Dew Point calcution (at the top column)

Temperature = 286.5 C and Operating pressure = 600 kPa

Table 2.3: Variable at top column

Component Pi(mmHg) ki Yi = xd ∑xi = ∑yi /ki
Decene(c10h20) 6423.307 1.427284 0.5458 0.382405
Dodecene(c12h24) 3308.79 0.735226 0.4531 0.616273
Tetradecene(c14h28) 1590.224 0.353354 0.0009 0.002547
Total 1.0000 1.001225

Since the value of ∑yi /ki is close to 1.0, therefore this temperature is acceptable.

b) Bubble Point calcution (at the bottom column)

Temperature = 347.2 C and Operating pressure = 600 kPa

Table 2.4: Variable at bottom column

Component Pi(mmHg) ki xw = x b ∑yi = ∑kixi
Decene(c10h20) 5348.346 1.188424 0 0
Dodecene(c12h24) 2679.851 0.595473 0.0037 0.006773
Tetradecene(c14h28) 1251.981 0.278195 0.9963 0.987073
Total 1.0000 0.993846

Since the value of ∑kixi is close to 1.0, therefore this temperature is acceptable

2-5
 c) Bubble Point calcution (at the feed column)
Temperature = 317.2 C and Operating pressure = 820 kPa

Table 2.5 : Variable at feed column

Component Pi(mmHg) ki xw = x d ∑yi = ∑kixi
Decene(c10h20) 9835.264 1.599098 0.3668 0.586549
Dodecene(c12h24) 5395.911 0.877312 0.3056 0.268106
Tetradecene(c14h28) 2765.956 0.449712 0.3275 0.147281
Total 1.0000 1.001936

Since the value of ∑kixi is close to 1.0, therefore this temperature is acceptable

2.2.5 Relative volatility

The relative volatility, , of two components can be expressed as the ratio of their K
values :

 = KLK / KHK Eqn (2.3)

Where KLK = Light key component

KHK = Heavy key component

Table 2.6 and Table 2.7 shown relative volatilities at top and bottom of the
distillation column while Table 2.8 shown average relative volatilities at top and bottom
column.

Top Column (dew point)

Table 2.6: Relative volatilities at top column

Component ki i
LK Decene(c10h20) 1.427284 4.039248
Dodecene(c12h24) 0.735226 2.080708
HK Tetradecene(c14h28) 0.353354 1

2-6
Bottom Column (bubble point)

Table 2.7: Relative volatilities at bottom column

Component ki i
LK Decene(c10h20) 3.163737 3.193312
Dodecene(c12h24) 1.830521 1.847633
HK Tetradecene(c14h28) 0.990739 1

Average Velocity;

Table 2.8: Average relative volatilities at top and bottom column

Component α (top) α (bottom) α (mean)
Decene(c10h20) 4.039248 3.193312 3.61628
Dodecene(c12h24) 2.080708 1.847633 1.96417
Tetradecene(c14h28) 1 1 1

2.2.6 Minimum number of stages

The determination of the minimum number of stages of this Distillation Column, Nm by

using the Frenske Equation (Reference : Coulson and Richardson, Volume 6, 1999)
 x   x  
log   LK   HK  
  x HK  d  x LK  b 
Nm = Eqn (2.4)
log  LK

 0.5458  0.9963 
Log   
 0.0009  0.0037 
Nm =
log 3.61628
log(163297.4549)
Nm =
log( 3.61628)
Nm = 9.337872
= 10 stages

2-7
2.2.7 Minimum reflux ratio

Reflux ratio can be calculated using Underwood equation:

 i x i ,d
 i   = Rm + 1 Eqn (2.5)

Where,  i = the relative volatility of component i with respect to some reference

component, usually the heavy key
R m = the minimum reflux ratio
Xi,d = concentration of component i in the tops at minimum reflux

And  is the root of the equation:

x,
 ii i f = 1 – q
xi,f = the concentration of component I in the feed, and q depends on the
condition of the feed
q = 1(assume as feed is at tis boiling point)

The value Ө of must lie between the values of the volatility of the light and heavy keys,
and goind by trial and error method.

Therefore,

x,
 ii i f =1-1

x,
 ii i f =0

x,
 ii i f = 3.555828 x0.3668 1.95083x0.3056 1x0.3275
3.555828  

1.950832  

1
=0

The value of Ө is 1.234834.

2-8
Table 2.9 exposed the variable to calculate minimum reflux ratio of distillation
column 3.

Table 2.9: Variables to calculate minimum reflux ratio

Component Composition at
Relative volatilities ,αi
distillate,xi,d
Decene(c10h20) LK 0.5458 4.039248
Dodecene(c12h24) 0.4531 2.080708
Tetradecene(c14h28) HK 0.0009 1

 i xi , d
 = Rm + 1
i 

 i xi , d
 =
4.039248 x0.5458

2.0850708 x0.4531

1x0.0009
= Rm + 1
i  4.039248  1.247742 2.0850708  1.247742 1  1.247742

The minimum reflux ratio

Rm +1 =0.896844
Rm = 0.472808

The operating reflux ratio is normally set between 1.2Rmin and 1.5Rmin. In this case,
1.5Rmin is chosen,

R = 1.3 Rmin
= 1.3(0.896844)
= 1.165897

Relation between reflux ratio and stages

Rm 0.9707
= = 0.538298
R m  1 0.9707  1

Specimen calculation, for R= 2.0

R 2
= = 0.67
(R  1) 3

2-9
From figure Erbar – Maddox correlation relating number of stages to reflux ratio, see
Appendic 2.1

Nm
= 0.54
N
Therefore,
Nm
N
0.54
10
 = 19 stages
0.54
Number of stages including reboiler is 19 stages.

2.2.8 Overall column efficiency

A quick estimate of the overall column efficiency can be obtained from correlation given
by O’Connell (1946)
E0  51  32.5 log(  a  a ) Eqn (2.6)

Where,  a = average relative volatility of the light key

 a = the molar average liquid viscosity, mNs/m2

Viscosity at average temperature

Ttop = 286.5 C = 559.65 K
Tbottom = 347.2 C = 620.35 K
Taverage = (547.55 + 620.35) = 583.95 K

Viscosity of components at average temperature, 583.95 K:

1 1
Log (μ) = Vis A (  )
T VisB

2-10
Table 2.10 shown values of calculated viscosity for decene, dodecene and tetradecene.

Table 2.10: Values of calculated Viscosity for each component

Component xw= xf mean

VisA VisB Viscosity(mNs/m2)
viscosity
Decene(c10h20) 0.3668 518.37 277.8 0.102946 0.037761
Dodecene(c12h24) 0.3056 615.67 310.07 0.114268 0.03492
Tetradecene(c14h28) 0.3275 697.349 336.13 0.128029 0.041929
total 0.11461

From the previous calculation, relative volatility of light key is:

 a = 3.73261

Therefore, overall column efficiency,

E0  51  32.5 log(  a  a )
= 51 – 32.51log (0.11461x 3.61628)
= 62.43171 %

The minimum number of stages is 19, and overall column efficiency is 62.63463 %.
Consider reboiler and condenser as a stage, therefore, number of real stages is:

Number of ideal stages

E0 
Number of real stages

(19  1)
Number of actual stages = = 28.37697 = 29 stages
0.6243171

Therefore, number of real stages = 29 stages

2-11
In order to find the feed point location, an estimate can be made by using the Fenske
equation to calculate the number of stages in the rectifying and stripping section
separately, but this requires an estimate of the feed-point temperature. As an
alternative approach is to use the empirical equation given by Kirkbride (1944) as a
matter

N   x  x b,LK 
2
Log  r  = 0.206 log  B  f ,HK   
 Ns   D  x f ,LK  x
 d,HK

 
  Eqn (2.7)

Where, Nr = number of stages above the feed, including any partial condenser

Ns =number of stages below the feed, including the reboiler

x f ,HK =concentration of the heavy key in the feed

x f ,LK = concentration of the light key in the feed

x d,HK = concentration of the heavy key in the top product

x b,LK = concentration of the light key if in the bottom product

B = molar flow of bottom product

D =molar flow of top product

N   64.65  0.3275  0.0037 2 

Log  r  = 0.206 log      = - 0.0404
 Ns   132.4  0.3668  0.0009  

 Nr 
  = 1.50897
 Ns 
Where actual number of stages is 14,
Nr  Ns = 29
0.9111Ns + Ns = 29
1.9111 Ns = 29
Ns = 11.55853 = 12

Therefore, the feed is at stages 12 from the bottom column.

2-12
2.2.9 Column Sizing

An approximation of column size started once the number of real stages is known. This
procedure includes plate spacing and column diameter.

a) Plate spacing

The overall height of the column will depend on the plate spacing. Plate spacing range
from 0.5 to 1.0 m is normally used. Its spacing depends on column diameter and
operating condition.

b) Column diameter

The principal factor that determines the column diameter is the vapor flow rate. The
equation given below, which is based on the well-known Souders and Brown equation,
Lowenstein (1961), can be used to estimate the maximum allowable superficial vapor
velocity, and hence the column area and diameter:
1/ 2
 ( L   V 
uv  (0.1710l t  0.27lt  0.047) 
2

 V  Eqn (2.8)
Where, u v = maximum allowable vapor velocity, based on the gross (total)
Column cross-sectional area, m/s
l t =plate spacing, (range 0.5 m – 1.0m)

The column diameter can be calculated using equation:

4 Vw
Dc =
 v u v

Where, Vw = the maximum vapor rate, kg/s

c) Column area
Column area can be calculated using equation:

Dc 2
Area 
4
Where Dc = Column diameter,m2

2-13
2.2.10 Flooding velocity

The flooding condition fixes the upper limit of vapour velocity. A high vapour velocity is
needed for high plate effiencies and the velocity will normally be between to 70 – 90 %
of that cause the flooding.

For this design, the value is between 80 -85% of the dlooding velocity should be used
(Sinnot 2006)
Flooding velocity can be estimated from the correlation given by Fair (1961):

ρL  ρV
U f  Ki Eqn (2.9)
ρV

where, Uf = flooding vapour velocity, m/s, based on the net column cross-sectional
area
Ki = a constant obtain from figure 11.27

The liquid-vapour flow factor, FLV in figure 11.27 is given by:

LW V
FLV  Eqn (2.10)
VW L

where LW = liquid mass flow rate, kg/s

VW = vapour mass flow rate, kg/s

2-14
2.2.11 Calculation for density

a) Top product

Liquid density,ρl
ρL = 516.1kg/m3

Table 2.11 shown values of vapour density for all components at top product of
distillation column.

Table 2.11: Values of vapour density for components at top product

Mw Ptop Tstp Pstp Vstp Density,

Component Ttop (K)
(kg/kmol) (kPa) (K) (kPa) (m3/kmol) ρv
Decene
140 547.55 600 273 100 22.4 18.69692
(c10h20)
Dodecene
168 547.55 600 273 100 22.4 22.43631
(c12h24)
Tetradecene
196 547.55 600 273 100 22.4 26.17569
(c14h28)

Mw Tstp Pop
Vapour density, ρv= x x
Vstp Top Pstp Eqn (2.11)

140 273 600

For decene, ( ρv )  x x  18.69692 kg/m3
22.4 547.55 100
For total vapour density, ρv =  (ρv)(xd)

= 20.39423 kg/m3

2-15
b) Bottom product

Liquid density,ρl
ρL = 477.9kg/m3

Table 2.12 shown values of vapour density for all components at bottom product of
distillation column.

Table 2.12 : Values of vapour density for components at bottom product

Mw Tbottom Pbotto, Vstp Density,

Component Tstp(K) Pstp(kPa)
(kg/kmol) (K) (kPa) (m3/kmol) ρv

Decene(c10h20) 140 620.35 600 273 100 22.4 16.50278

Dodecene(c12h24) 168 620.35 600 273 100 22.4 19.80334

Tetradecene(c14h28) 196 620.35 600 273 100 22.4 23.10389

Mw Tstp Pop
Vapour density, ρv=  
Vstp Top Pstp

140 273 600

For decene, ( ρv)  x x  16.50278 kg/m3
22.4 620.35 100

For total vapour density, ρv =  (ρv)(xd)

= 23.09168 kg/m3

2-16
 2.2.12 Calculation for Relative Molar Mass (RMM)

Table 2.13 shown molecular weight and mole fractions for every component at top,
bottom and feed column of distillation column.

Table 2.13: Molecular weight and mole fractions for each component
Molecular Feed Mol Top (D) mol Bottom (B) mol
Component
Weight, MW Fraction, XF Fraction, XD Fraction, XB
Decene(c10h20)
140 0.3668 0.5458 0
Dodecene(c12h24)
168 0.3056 0.4531 0.0037
Tetradecene(c14h28)
196 0.3275 0.0009 0.9963
1.0000 1.0000 1.0000

RMM of Feed = 0.3668 (140) + 0.3056 (168) + 0.3275 (196)

= 166.8828 kg / kmol

RMM of Top Product = 0.5458 (140) + 0.4531 (168) + 0.0009 (196)

= 152.7092kg / kmol

RMM of Bottom Product = 0 (140) + 0.0037 (168) + 0.9963 (196)

= 195.8964kg / kmol

Hence, after calculations are made, values of RMM at feed, top and bottom
column is shown at Table 2.14.

Table 2.14: Value of RMM at feed, top and bottom column

Relative Molar Mass(RMM) (kg / kmol)

Feed RMMf Top (D) RMMd Bottom (B) RMM b
Total 166.8828 152.7092 195.8964

2-17
2.2.13 Maximum allowable vapour density

Maximum allowable vapour density

1/ 2
 ( L   V 
uv  (0.1710l  0.27lt  0.047) 
2
t 
 V  Eqn (2.8)
Where , Ii = plate spacing = 0.50 m

Therefore,
1/ 2
 ( L   V 
uv  (0.1710l  0.27lt  0.047) 
2
Top : t 
 V 
516.1  20.39423 1/2
= ( - 0.171 x 0.52+0.27 x 0.5 – 0.047)( )
20.39423
= 0.22564 m/s
1/ 2
 ( L   V 
uv  (0.1710l t  0.27lt  0.047) 
2
Bottom: 
 V 
477.9  23.09168 1/2
= ( - 0.171 x 0.52+0.27 x 0.5 – 0.047)( )
23.09168
= 0.200819m/s

2.2.14 Flooding velocity

Maximum vapour rate:

DxRM 132.4 x152.7092
VW  
3600 3600

= 5.616305

Maximum liquid rate :

BxRM 64.65 x195.8964
LW  
3600 3600

= 3.517973

2-18
The liquid- vapour flow factor, FLV is given by :

LW V
FLV  Eqn (2.12)
VW L

Therefore,

FLV top

3.51797 20.39423
FLV  x  0.123164
5.61263 516.1
FLV bottom

3.51797 23.09168
FLV  x  0.13769
5.61263 477.9
From the Figure flooding velocity, the value of top and bottom for Ki can be
determined, see Appendic 2.2

Therefore, at spacing, II = 0.5 m , for FLV(top) = 0.123164, the value of Ki = 0.08 while
for FLV(bottom) = 0. 13769, the value of Ki =0.07

Flooding velocity can be estimated from correlation given by Fair (1961) :

ρL  ρV
U f  Ki
ρV
Eqn (2.13)
Therefore,

516.1  20.39423
Top Uf = 0.08 = 0.398922 m/s
20.39423

477.9  23.09168
Bottom Uf = 0.07 = 0.310659 m/s
23.09168

For design, a value of 80 to 85 per cent of the flooding velocity should be used.

Top Uf = 0.398922 m/s (0.85) = 0.339084 m/s

Bottom Uf = 0.310659m /s (0.85) = 0.26406 m/s

2-19
2.2.15 Maximum volumetric flow-rate

To operating reflux ratio is normally set between 1.2Rmin and 1.5Rmin. for this case,
1.3Rmin is chosen.

R = 1.3 Rmin
= 1.3(0.896844)
= 1.165897

Vm (RMM )
Maximum volumetric flow-rate =
V

i) Above the feed point

Vapor flow rate will be:

Vn  D(R  1)
Where: D = Distillate molar flowrate
R = Reflux ratio
So,
Vn = 132.4(1.165897+ 1)
= 286.7648 kmol/h

Liquid down flow will be:

Vn = L n  D

L n = Vn  D
= (186.7648 – 132.4) kmol/h
= 154.3648 kmol/h

ii) Below the feed point

Liquid flow rate will be:

L m = Ln  F

2-20
Where: F = feed molar flowrate
Hence; Lm = 154.3648 + 197.31
= 351.4648 kmol/h

Vapor flow rate will be:

Vm = L m  W
Where: W = bottom molar flowrate
Hence; Vm = 351.4648 – 64.65
= 286.8148 kmol/h

Therefore, maximum volumetric flow rate:

V n ( RMM ) 279.3442 (152.7092)

Top = = = 0. 609747 m3/s
V 20.39423 x3600

V m ( RMM ) 279.3942(195.8964)
Bottom = = = 0.67588 m3/s
V 23.09168 x3600

2.2.16 Net area required

volumetric flowrate
Net required, An=
flooding velocity

0.609747
Top = = 1.649818 m2
0.352238

0.67588
Bottom = = 2.371148 m2
0.277669

2-21
2.2.17 Column cross-sectioned area

The equation used to calculate column cross-secioned,Ac is :

Dc 2
Area 
4 Eqn (2.14)

As first trial, take downcomer area,A d as 12% of total clolum cross-sectional area.
Therefore, downcomer Area,Ad = 0.12Ac

An = Ac – Ad
An = Ac – 0.12Ad
An = (1-0.12)Ac
An = 0.88Ac

An
Therefore, Ac  0.88
4

1.649818
Top = =2.043432m2
0.88

2.371148
Bottom = =2.908599m2
0.88

Downcomer area, Ad=0.12Ac (at 12%)

Top = 0.12Ac
= 0.12 (1.874793)
= 0.245212 m2

Bottom = 0.12Ac
= 0.12 (2.694486)
= 0.349032m2

2-22
2.2.18 Column diameter

4 Ac
Dc =
v
Eqn (2.15)

The column diameter, Dc is :

4(2.14343)
Top = = 1.612679 m


4(2.90859)
Bottom = = 1.92402 m


2.2.19 Liquid flow pattern,

L m (RMM )
Maximum volumetric liquid rate =
L Eqn (2.16)

351.4648kmol / h(195.8964)kmol / h 1h
= x
477.9kg / m
3
3600s

= 0.040019 m3/s

2-23
2.2.20 Weir Dimensions

Provisional plate design

Column diameter, D C = 1.92402m

Column area, A C = 2.908599m2

Down comer area, A d = 0.12 x 2.694486 m2 (at 12%)
= 0.349032m2
Net area, A n = AC  Ad
= 2.908599 – 0.349032
= 2.559567m2
Active area, A a = A C  2A d
= 2.9028599 – (2 x 0.349032)
= 2.210535m2
Hole area, Ah = 0.221054m2 (take 10% of Aa as first trial)

a) Weir Length

Ad 0.349032
x 100% = x 100% = 12%
AC 2.908599

From figure relation between downcomer area and weir length, see Appendix 2.6
Iw
= 0.75
Dc

Iw = 0.75 x 1.92402
= 1.443015 m

Take weir height, hw = 50mm

Hole diameter, dh = 5mm
Plate thickness = 5mm

Area of 1 hole,

dh 2 (0.005 ) 2
A lh = = =1.963 x 10-5 m2
4 4

2-24
Number of holes per plate,
Ah 0.221054
Nh  = =11253.63 holes (approximately 10254 holes)
A lh 1.963x10 5

b) Check weeping (Enough vapour to prevent liquid flow through hole)

Lm(RMM )
Minimum liquid rate, Lw =
3600 s
351.4648kmol / h(195.8964kg / kmol)
=
3600s
= 19.12519kg/s
Minimum liquid rate = 0.7 x 18.72139kg/s (at 70% turn-down ratio)
= 13.38763kg/s

c) Weir liquid crest

The height of the liquid crest over the weir can be estimated using the Francis weir
formula. For a segmental down comer this can be written as:
2/3
 L 
h ow = 750 w 
 l (l w ) 
Where, lW = weir length
Lw = liquid flow rate, kg/s
L =liquid density
2/3
 19.12519kg / s 
Maximum h ow = 750 3
 = 68.71631 mm liquid
 477.9kg / m (1.443015 m) 
2/3
 13.38763kg / s 
Minimum h ow = 750 3
 = 54.17412 mm liquid
 477.9kg / m (1.443015m) 

At minimum rate, clear liquid depth,

h ow  h w = (54.17412 + 50) mm liquid = 104.17412mm liquid

From the Figure Weep-point correlation (Eduljee, 1959)],see Appendix 2.5

When h ow  h w =104.17412
K 2 = 31
2-25
 d) Weep point

The lower limit of the operating range occurs when liquid leakage through the plate
holes becomes excessive is known as weep point. The vapor velocity at the weep point
is the minimum value for stable operation. Minimum vapor velocity through the holes
based on the holes area can be calculated using Eduljee (1959) equation:

K 2  0.9(25.4  dh )
Uh (min) 
( v )1/ 2 Eqn (2.17)

Where, Uh =minimum vapor velocity through the holes based on the holes area
dh = hole diameter, mm
K 2 = a constant, dependent on the depth of clear liquid on the plate,
Obtain from figure weep-point correlation, see Appendix 2.5

K 2  0.9(25.4  d h )
U h (min) 
(  v )1 / 2 Eqn (2.18)
31  0.9(25.4  5)
=
(23.09128) 1 2
= 2.630385m/s

mimmumvaporrate
Actual minimum vapor velocity =
Ah

0.7(0.67588m 3 / s)
=
0.221054 m 2
= 2.14028m/s

So, minimum operating rate will be below the weep point.

2-26
 1. Plate pressure drop

a) Dry plate drop

The pressure drop through the dry plate can be estimated using expression derived for
flow through orifices:
2
U  
h d  51 h  v
 C o  L Eqn (2.19)

Where, Uh = velocity through the holes

C o = orifice coefficient
volumetric flow rate
Uh =
hole area, A h

0.67588 m3 / s
Uh = = 3.057542m/s
0.221054 m2

For plate thickness/hole diameter = 5 mm/5 mm = 1

Ah 0.221054m2
 x100% = 10 %
Aa 2.21054m2

So, orifice coefficient value can be obtained from figure discharge coefficient, see
Appendix 2.8
C o = 0.84
Therefore, dry plate drop:
2
 2.630385m / s  23.09168kg / m 3
hd  51  3
= 159.7019 mm liquid
 0.84  525.9852 kg / m

b) Residual head
Residual head can be calculated using Hunt et al (1955) equation:

12.5x10 3
hr 
L

12.5 x103
hr  =26.1561mm liquid
477.9

2-27
 c) Total pressure drop

The total plate drop is:

h t  hd  (h w  how )  hr

ht  159.7019  (104.1741)  26.1561

h t  290.0322 mm liquid

2.2.21 Down comer liquid back-up

Down comer pressure loss:

hap  h w  10mm

hap  50mm  10mm = 40 mm

Where, h ap is the height of the bottom edge of the apron above the plate.

Area under apron,

A ap  hap (l w ) = 40 x 10-3 m (1.443015m) =0.057721m2 (less than Ad=0.349032m)

Where A ap is the clearance area under down comer.

As this is less than A d , thus equation can be used to calculate the head loss in down
comer hdc
2
 L 
h dc  166  wd 
 L A m  Eqn (2.20)
Where, h dc = head loss in down comer, mm

L wd = liquid flow rate in down, kg/s

A m = either the down comer area Ad or the clearance area under the

down comer A ap ; whichever is the smaller

2
 19.12519 
hdc  166  = 4.172324 mm liquid
 (477.9)(0.057721) 

2-28
Back-up in the down comer, ( h b ),

hbc = hw + how + ht + hdc

hbc = 104.1741 + 290.0322+ 4.172324
hbc = 398.3786 mm liquid or 0.398 m

Down comer residence time

Ad xhbc xpl 0.349032 x398.3786 x477.9

tr = = = 3.4745s
LWD 19.12519

2.2.22 Check entrainment

Entrainment can be estimated from the correlation given by Fair (1961). The
percentage flooding is given by:
Un actual velocity (based on net area)
% flooding 
Uf
3
Uf 0.658394m / s
Un = = = 0.26406 m/s
An 2.559567m2
0.26406m / s
% flooding = x100 = 66.19354%
0.398922m / s

From figure 11.29  value = 0.0065

 value is below 0.1, so column diameter which is proposed earlier is acceptable.

2-29
2.2.23 Perforated area

From figure relation between angle subtended by chord, chord height and chord length,

see Appendix 2.7

lw 1.388887mm
At   0.76
Dc 1.851849mm
 c = 100
Angle subtended at plate edge by unperforated strips = (180 –99) = 800

a) Mean length, unperforated edge strips,

80
= (Dc –0.05) x  x
180
81
= (1.92402 – 50 x10-3) m x  x
180
= 2.617679m

b) Area of unperforated edge strips,

= (50 x 10-3) m x (2.6176799 m)

= 0.130884m2

c) Area of calming zones,

= 2 x 0.05 (lw – 2 x 50x10-3) m2

= 2 x 0.05 (1.443015– 2 x 50x10-3) m2
= 0.149302m2

d) Total area available for perforation, Ap :

Ap = Active area – (Area of unperforated edge + Area of calming zones)

= 2.908599 m2 – (0. 130884 + 0.149302) m2
= 1.93035m2

2-30
 Ah 0.221054
= = 0.114515
Ap 1.93035

From figure Relation between hole area and pitch, see Appendix 2.9
lp
= 2.90 (satisfactory, range normally within 2.5 to 4.0)
dh

2.2.24 Column height

Column diameter = 1.92402m

Column height = number of stage x tray spacing
= 29 x 0.5
= 14.5

Rule of thumb: Add 1.2 m at top of column for vapour phase and 1.8 m for reboiler
return.

Therefore, column height = 14.5 + 1.2+ 1.8

= 17.5 m

2-31
Table 2.15 shows summary of the chemical process design for distillation column

Table 2.1: Summary of the chemical process design for distillation column

ITEMS VALUES UNITS

Column Diameters, Dc 1.92402 m

Column Height, Hv 17.5 m

Column Area, Ac 2.908599 m2

Number of Plates 29 Units

Plate Spacing, Il 0.5 m

Plate Thickness 5 mm

Plate Pressure Drop, ht 290.0322 mm liquid

Downcomer Area, Ad 0.349032 m2

Net area, An 2.559567 m2

Active Area, Aa 2.210535 m2

Hole Area, Ah 2.559567 m2

Hole Diameter,Ah 0.221054 mm

Number of Holes 10254 units

Weir Length. lw 1.388887 m

Weir Height, hw 50 mm

Residence Time, tr 3.4745 s

2-32
2.3 Mechanical Design of Distillation Column

Total column height = tray spacing x no. of stages

= 0.5 m x 29
= 14.5 m
Internal diameter, Dc = 1.92402 m
Operating pressure, Top column = 600 kpa , 6 bar
Bottom column = 600 kpa , 6 bar
Take column operating at = 6 bar
Material of column = Carbon steel
Operating temperature = 347.2 oC
Tray temperature = Sieve tray (29 trays equally spaced)
Material of tray = Carbon steel
Disengagement space = 3000 mm
= 3m
Insulation column = Mineral wool 75 mm thick
Design stress = 79 N/mm2 (for carbon steel at 347.2 oC)

2.3.1 Pressure Design

Take design as 10% above operating pressure,

= 6 bar x 1.1

1.01325 x105 N / m2 (1m)2

= 6barx x
1.01325bar (1000mm)2
= 6.6 bar
= 0.66 N/mm2

2-33
2.3.2 Minimum wall thickness

Minimum thickness required for pressure loading, (t),

PxD c
tm =
2 des  P Eqn (2.21)

0.66 N / mm2 (1.92402mm)

=
2(79 N / mm2 )  (0.66 N / mm2 )
= 8.070759mm (approximately 8 mm)

Actual minimum wall thickness,

tam = tm + corrosion allowance

= 8.070759 + 2
= 10.070759 (approximately 10mm)

A much thicker wall required at column base to withstand wind and weight load. Allow 2
mm for corrosion; 5mm, 7 mm, and 9 mm.
Thus, for further calculation take t = 10 mm.

2.3.3 Weight loads

a) Dead weight of vessel

Wv  240Cv Dm H v  0.8Dm  tx10 -3 Eqn (2.22)

where, W V = total weight of shell , excluding internal fitting such as plates

CV = a factor to account for the weight of manways and internal support. (In
this case for distillation column, CV = 1.15)
Dm = mean diameter of vessel (DC + t x 10-3)
HV = height or length between tangent lines
Tm = wall thickness
= 10 m

2-34
 Dm = (1. 92402 + 10 x 10-3m)
= 2.02402m
Hv = 14.5 m
Wv = 240(1.15)(2.02402 x (14.2 + 0.8(2.02402)) 10 x 10-3
Wv = 90.0467 kN

b) Weight of plates

Plate area

D 2
Plate area = = 2.908599m²
4
1.2 is factor fir contacting plates, steel including typical liquid loading in kN/m²
Weight of plate = 1.2 kN/m² x 2.908599= 3.490319kN
Weight of 29 plates = 29 x 490319kN = 101.2192kN

c) Weight of insulation

Mineral wool density = 130 kg/m³

Approximate volume of insulation = π x DC x HV x (75 x 10-3) m
= π (1.92402) (13) (75 x 10-3) m
= 6.574232 m³

Weight of insulation = 6.574232 x 130 x 9.81

= 8384.118 N
= 8.384118 kN
Double this value to allow for fitting = 16.76824 kN

d) Total weight

Total weight,W t = 90.0467 + 101.2192 + 16.76824

= 208.0342 kN

2-35
2.3.4 Wind loading

Take dynamic wind pressure as 1280 N/m2

Fw = Dynamic wind pressure x mean diameter includes insulation
Mean diameter includes insulation = DC  D t  75  x103
c

= 1..92402  1.92402 10  75  x10

3
 3.62402m

Fw = 1280 N/m 3 x3.62402m  4.638746 Nm

Bending moment at bottom tangent line:

 x2 
M x  Fw   Eqn (2.23)
2
14.52 
M x  4638.746  
 2 
M x  487.6481kNm

2.3.5 Analysis of stresses

At bottom tangent line:

a) Pressure stresses

PD
L = Eqn (2.24)
4t

where P = operating pressure (0.11 N/mm²)

D = column diameter (1.0m)
t = thickness (10mm)

PD
L =
4t
0.661924.02
L =
410
 L = 31.74633N/mm2

2-36
 PD
h = Eqn (2.25)
2t
0.66(1924.02)
h=
210
 h = 63.49266N/mm2

b) Dead weight stress

WV
w = Eqn (2.26)
 ( Dc  t )t

60.0467x103
w =
 (1924.02  10)10
 w = 0.001482 N/m2
1.481838N/mm2

c) Bending Stresses

M  Dc 
b =   t Eqn (2.27)
IV  2 
where M = bending moment at bottom tangent line

IV =

64
D 0
4
 Di
4
 Eqn (2.28)

where IV = bending stress

Do = DC  2t  1944.02 mm


IV =
64
1944.02 4

 1944.024  2.84x1010 mm4

Thus;
487.6481x103  1924.02 
b =   10 
 
10
2.84 x10 2
 b =  16.68271N/mm2
The resultant longitudinal stress is:  z   L   W   b
 Z (upwind) = 46.9472N/mm2
 Z (downwind) = 13.58178N/mm2

2-37
The greatest difference between the principal stresses will be on the downwind side:
 h   z  77.07445 N/mm2; much below than design stress

The value of differences between the principal stresses is well below the maximum
allowable design stress.

2.3.6 Elastic stability

Critical buckling stress,

 t 
 C = 2 x104   Eqn (2.29)
 o
D
where ν = 0.3 and E = 193000 N/mm² include a high factor of safety,

 10 
 C = 2 x104   N/mm2
 1.94402 
 C = 1028.796 N/mm2

Therefore, a critical buckling stress is 1028.796 N/mm².

When the vessel is not under pressure (where the maximum stress occur):

Maximum stress = σw + σh
= 1.481838 + 16.68271
= 18.16455 N/mm²

The maximum stress is well below the critical buckling stress. Therefore, design is
satisfactory.

2-38
2.3.7 Design for the skirt support

Material of construction for skirt support is SS 304.

Design stress = 79 N/mm²
Liquid Density = 447.9 kg/m3
Young modulus = 193000 N/mm²

The maximum dead weight load on the skirt will occurs when the vessel is full of liquid.

 
Approximate weight = xDc ( H V )  x L ( g ) Eqn (2.30)
4 
 
Approximate weight = (1.92402m) 2 (14.5m)  x (447.9kg/m 3 ) (9.81)
4 
= 197.6694kN

Dead weight of vessel = 208.0342 kN

Total weight = Vessel dead weight + Approximate weight
Total weight = 208.0342 + 197.6694kN
= 405.7036 kN

Wind loading from previous calculation = 4.638746 kN

Take skirt support as 1 m height,

Bending moment at base skirt:

Bending moment at base of skirt = Wind loading x (column height + skirt height)2
2
Bending moment at base of skirt = 4.638746 kN x (14.5 m + 1m)² /2
= 710.3079kNm

2-39
 a) Stress analysis of skirt base

The resultant stresses in the skirt support will be:

σ S (tensile) = σ bs – σ ws
σ S (compressive) = σ bs + σ ws

where, σ bs = bending stress in the skirt

σ ws = dead weight stress in the skirt
and;

4M s
 bs = Eqn (2.31)
 ( Ds  t s )t s Ds

where, Ms = maximum bending moment, evaluated at the base of the skirt

(due to the wind, seismic and eccentric load)
Ds = inside diameter of the skirt, at the base
ts = skirt thickness
Therefore;

4 x 710.3079 x 103 x103

 bs =
 1924.02  101924.02x10
 bs = 24.30132 N/mm2

b) Dead weight stress in the skirt

W
 ws = Eqn (2.32)
 ( Ds  t s )t s Ds

197.6694x103
 ws (test) =
 (1924.02  10)10

=3.252912 N/mm2

2-40
 405.7036 x103
 ws (operating) =
 (1924.02  10)10

= 6.67639 N/mm2

Maximum  s (compressive);

 bs   ws = 30.97771N/mm2

Maximum  s (tensile):

 bs   ws = 21.04841N/mm2

Skirt thickness should be under the combination of wind and dead weight load. The
following design criteria are not exceeded:

s (tensile) < fs J sin s

ts
s (compressive) < 0.125 E sin  s
Ds
Take J as 1 and sin 90 = 1.

fs J sin s = 79 N/mm2.

Young modulus, E for SS 304 is 193000 N/mm2

ts
0.125 E sin  s = 112.0969 N/mm2
Ds

Therefore,
s (tensile) < fs J sin s
21.0484 N/mm2 < 79 N/mm2.

ts
s (compressive) < 0.125 E sin  s
Ds
30.9777N/mm2 < 112.0969N/mm2

Both criteria are satisfied; add 2 mm to allow for corrosion. Hence, thickness = 10 mm.

2-41
2.3.8 Base Rings and Anchor Bolts

Assume pitch circle diameter,Db = 1.6 m

Circumference of bolt circle, Db = 1600
= 5026.548 mm
According to Scheiman (Coulson Richardson Chemical engineering volume 6, page
848),
Bolt stress design, f b = 79 N/ mm2
Recommended spacing between bolts = 600 mm
5027
Minimum number bolt required, Nb = (4.55)
600
= 8.378

Bending moment at base skirt, Ms = 385 kNm

Total weight of vessel, W = 208.0342 kN

1  4M s 
Area of bolt, Ab =   W  (4.56)
Nb fb  Db 
1  4(385000) 
=   208034.2 
12(79)  1.6 
= 1872.955 mm2

Ab x 4
Bolt root diameter, d = (4.57)

1872.955 x 4
=

= 48.8304 mm

Total compressive load on the base ring per unit length,

 4M s W 
Fb =    (4.58)
Ds
2
Ds 

 4 (385000) 208034.2 
=  
  (1.924)
2
 (1.924) 
= 278.689 kN/m
By assuming that a pressure of 5 N/mm2 is one of the concrete foundation pad, f c

2-42
 Fb 1
Minimum width of the base ring, L b = x 3 (4.59)
f c 10
278689
=
5 x 10 3
= 55.7378 mm
With this minimum width, can get actual width
Use M56 bolts (BS 4190:1967) root area = 1120 mm2, Figure 13.30, page 849,
Chemical Engineering Volume 6, 1996.
Actual width required = Lr + ts + 50 (4.60)
= 102 + 20 + 50
= 172 mm
Actual bearing pressure on concrete foundation
Fb
f'c = (4.61)
actual width
278.689
=
172
= 1.6203 N/mm2
0.5
3f 
Actual minimum base thickness, tb = Lr  c  (4.62)
 fr 
Where , fc= actual bearing pressure on base, N/mm2
fr= allowable design stress in the ring material, typically 140 N/mm 2

3(1.6203)
Therefore, tb = 102
140
= 19.0061 mm
 19 mm

Chair dimension for bolt size M42. Skirt to be welded flush with outer diameter of
column shell.

2-43
Table 2.16 shows summarized Results of Mechanical Design

Table 2.16 Summarized Results of Mechanical Design

Column Type Pressure Vessel

Column Material Stainless Steel 304
Operating pressure, Po 0.66 N/mm2
Design Pressure, Pi 0.6 N/mm2
Design Temperature, TD 347.2 oC
Operating Temperature, To 347.2 oC
Column Diameter, Dc 1924.02 mm
Outer Diameter, Do 1944.02 mm
Colum Height,Hv 17.5 m
Wall thickness,t 10 mm
Insulation Material Mineral wool
Insulation Thickness 75 mm
Skirt Thickness 1
Design Stress,f 79N/mm2
Crown Radius, Rc 1924.02 mm
Knuckle Radius, Rk 115.441 mm
Dead weight of vessel, W v 90.0467 kN
Weight of a plate, W p 3.490319kN
Weight of 29 plates,W p 101.2192kN
Weight of insulation, W I 8.384118 kN
Total weight 208.0342 kN
Young’s Modulus 193000 N/mm2

2-44
2.4 References

J. M. Coulson, J. F. Richardson, 1977. Chemical Engineering,3rd Editon. Volume

Two.The Pergamon Press.

Robert H. Perry, Don W. green, 1998.Perry’s Chemical Engineer’s Handbook, 7th

Edition, McGraw-Hill.

R. K Sinnot,1996. Coulson & Richardson’s Chemical Engineering, Chemical

Engineering Design, Volume Six, Butterworth Heinemann.

James, M. Douglas, 1988. Conceptual Design of Chemical Processes, McGraw-Hill

Book Company.

Martyn S. Ray and David, W. Johnston,1989. Chemical Engineering, Design

Project: A Case Study Approach, Gordon and Breach Science Publishers

Carl R. Branan, 1994. Rules of Thumb for Chemical Engineers, Gulf Publishing
Company

Micheal J. Barber, 1985. Handbook of Hose, Pipes, Couplings and Fittings, 1st
Edition, The Trade & Technical Press Limited

Robinson, C.S, and Gilliland, E.R, 1950. Elements of Fractional Distillation,

McGraw-Hill.

Kister, H. Z,1992, Distillation Design, McGraw-Hill

Billet, R, 1979. Distillation Engineering, Heydon Publishing

King, C. J,1992. Separation Processes, 2nd Edition, McGraw-Hill.

Lockett, M. J, 1986. Distillation Tray Fundamentals, Cambridge University Press

2-45
Normans, W. S, 1961. Absorption, Distillation and Cooling Towers, Longmans

Oliver, E. D. 1966, Diffusional Separation Process, John-Wiley.

Smith, R, 1995. Chemical Process Design, McGraw-Hill

Van Winkle, M, 1967. Distillation, McGraw-Hill.

Louis Gary Lamit, 1981. Piping Systems: Drafting and Design, Prentice-Hall, Inc.

2-46
Appendices

APPENDIX 2.1

2-47
APPENDIX 2.2

APPENDIX 2.3

2-48
APPENDIX 2.4

APPENDIX 2.5
APPENDIX 2.6

2-49
APPENDIX 2.7

APPENDIX 2.8

2-50
APPENDIX 2.9

2-51
2-52