m
m


 
m
  

› A Distillation Column is used to separate a
mutilcomponent liquid mixture into distillates and
bottoms due to differences in their boiling points.
› They are of following two types based upon
construction.
› Tray Column
› Packed Column
    


› Plate column are designed to handle wide range of
liquid flow rates without flooding.
› For large column heights, weight of the packed
column is more than plate column.
› Man holes will be provided for cleaning in tray
Columns. In packed columns packing must be
removed before cleaning.
› When large temperature changes are involved as in
the distillation operations tray column are often
preferred.
› Random-Packed Column generally not designed with
the diameter larger than 1.5 m and diameters of
commercial tray column is seldom less than 0.67m.
½   
› ½ieve trays are selected due to following main
reasons.
› High capacity.
› High Efficiency .
› Lowest Cost per unit area than all other types with
the downcomer.
› Good flexibility in operation(Turndown ratio).
m
 ½ 
m
  


› Calculation of Minimum Reflux Ratio Rm.
› Calculation of optimum reflux ratio.
› Calculation of theoretical number of stages.
› Calculation of actual number of stages.
› Calculation of diameter of the column.
› Calculation of weeping point.
› Calculation of pressure drop.
› Calculation of the height of the column.
› Calculation of thickness of the shell & Head.
m
  

3    
d



d
 



 


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%
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( 


 )*   +
Y
  
   
YY 0.0005 650 44.217 0.022
Y 0.8451 16.6 1.13 0.954

0.1362 2.43 0.165 0.0225
 0.0182 0.0085 0.00578 1.05*10-5
™K*Xf 0.9998

$,d,$!&
(







 
 



 
-.,,-
Πm  
  


 !  
Colburn method is used to fine out the minimum
reflux ratio i.e.
Rm = (1/ (Įlk-1)*[(XlkD/XlkR)² Įlk(XlkD/XlkR)] (1)
Where
Xlkn= [rF/ (1+rF)*(1+™ĮXhF)] (2)
Xhkn= (XlkR/rF) (3)
Where ™ĮXhf for every component heavier than
the
heavy key
In Our case the component heavier than the
heavy key is residues
Œ
For that Į= (0.0011/2.78)=0.0004
½o that ™ĮXhf = 0
rF=(XlkF/XhkF) =6.22
Įlk = (17.9/2.8) = 5.85
XlkD=0.9987 and XhkD=0.0016
Then XlkR = [6.22/ (1+6.22)] =0.861 (By 2)
XhkR= (0.862/6.24)=0.138 (By 3)
Rm = 0.22 (By 1)
u   


 !  
Reflux Ratio = R=1.5*Rmin (1.2----1.5)
R = 1.5 * 0.22 = 0.33
Ln = R * D
Ln = 69.23 Kgmole/hr
Vn = Ln+D
= 276.6 Kgmole/hr
As, the feed is at its boiling point, q = 1
Lw = Ln+qF
= 305.41Kgmole/hr
Vw = Ln ± B
= 276.6 Kgmole/Kgs
è  


 ½

*sing Fenske¶s equation

Nm + 1 = Log [(Xl/Xh)d (Xh/Xl)s] / Log (Įlk)ave

Nm + 1 = Log [(0.9978/0.0016)d (0.879/0.115)s]

Log ((Į5.29)ave)

Nm = 6
J 
 " ½

› Ideal number of ½tages can be found by Lewis
Matheson Method.
› Average Temperature = 213.61 oC = 416.5 oF
› Relative Volatilities are

Y
 
YY 144.34
Y 5.237

1
 0.00948
J
BELOW THE FEED PLATE:
The ½OL Equations are
Y m = Lw*(Xm+1 / Vw) - W*(Xw / Vw)
Ym,ODCB = 1.106Xm+1-0.00068
Ym,TDI = 1.106*Xm+1-0.119
Ym,RE½ = 1.106*Xm+1-0.01564
And other equations are
Yi = (ai*Xi)/™(ai*Xi)
For every component
J
comp Xb a*Xb Yb X1 a*X1 Y1

ODC 0.005 0.026 0.028 0.026 0.136 0.124

B 18
TDI 0.879 0.879 0.97 0.96 0.958 0.875

Res 0.115 0.001 0.001 0.014 0.000 0.000

09 2 8 14 13
™ 0.999 0.906 1 0.999 1.09 1
J
--- X5 a*X5 Y5 X6 a*X6 Y6 X7
--- 0.803 4.207 0.958 0.844 4.421 0.969 0.8
5
--- 0.182 0.182 0.041 0.141 0.141 0.030 0.1
3
--- 0.013 0.0003 0.000 0.013 0.000 0.000 0.0
2 1
--- 0.999 4.389 1 0.999 1 1 0.9
9

The plate 7 has composition very close to the feed

plate so it is considered as feed plate.
J
ABOVE THE FEED PLATE:
The ROL equations are
Y n+1 = Ln*(Xn+1 / Vn) + D *(xD / Vn)
Y n,ODCB = (0.248 * X n+1) + 0.748
Y n,TDI = (0.248 * X n+1) + 0.0012
Y n,COCl2 = ( 0.248* X n+1) + 0.00045
J
Comp X7 a*X7 Y7 X8 a*X8 Y9
COCl2 0.000 0.0000 0.000 0.000 0.002 0.000
5 15 45 14 0 45
ODCB 0.853 0.9244 0.96 0.857 4.488 0.966

TDI 0.132 0.0755 0.036 0.142 0.142 0.030

Res 0.013 0.0001 0.000 0.000 4.9*10 1.04*0

7 3 13 52 ^-6 ^-6
™ 0.992 1 0.997 1 4.633 0.997
J
--- Y14 X15 a*X15 Y15 X16 a*X16 Y16
--- 0.0005 2.6*1 0.00 0.00 3.1*1 0.00 0.00
3 0- 4 05 0^ 45 58
5 -5
--- 0.992 0.98 5.14 0.99 0.99 5.19 0.99
3 8 4 1 3 7
--- 0.005 0.011 0.01 0.00 0.08 0.00 0.00
6 3 3 8 2
--- 0 0 0 0 0 0 0
--- 0.999 1 5.16 0.99 1 5.02 1.00

The Plate 16 has nearly same composition as that of

the top product so it is the last plate from top to
bottom.
x
   

The efficiency of the column is given by the following
empirical relation
Eo = 51 - 32.5 Log (µa * Įa)
Where
ȝa = Average viscosity of the feed = 0.1156
Įa = Average relative volatility of light to heavy
key = 5.29
Then,
Eo = 65%
  
 ½

'
/
 01  
23(,4
.
!
Actual number of stages = Ideal number of stages/Eo
= 15/0.65
Actual number of stages = 23
½ieve Trays are used.
ÿ #
 m

Top Condition Bottom Conditions

Ln =69.23Kgmole/hr Lm = 305.41 Kgmol/hr

Lw =10178.45 Kgs/hr Lw = 59226.02 Kg/hr
Vn = 276.6 Kgmole/hr Vm = 276.6 Kgmol/hr
Vw =40687.85 Kgs/hr Vw = 53641.04Kg/hr
M aver. = 147.01 M aver=193.923Kg/Kgmol
Kg/Kgmol T = 252.22oC
T = 160oC Liquid density = dL = 1202
Liq density = dL = 1306 Kg/m3
Kg/m3 Vapor density = dV = 4.5
Vap density = dV = 4 Kg/m3 Kg/cm3
ÿ
› Flooding Velocity:
Flv=(Lw/Vw)(dv/dl)^0.5
Flv = 0.0675
From figure11.27, Coulson and Richardson, 6th Ed.
At 18 inch spacing or 0.457 m
K1 = 0.08
*c = 0.952 m/s (By above equation)
Let, flooding = 80%
*c* = 0.8 * 0.952
= 0.762 m/s
ÿ
› Maximum volumetric flow rate of vapors :
qv = Vw /dv = 3.31 m3/s
› Net area required:
An = qv / *c*== 4.33 m2
› Column Cross sectional Area:
Column area = Ac = An / 0.88 = 4.92 m2
› Diameter:
Diameter =Dc = (4*Ac/3.14) 0.5= 2.5m
The calculated diameter at the top of column is 2.2 m.
ÿ
› Downcomer Area:
Ad = 0.12*Ac = 0.59 m2
› Net Area:
An = Ac ± Ad= 4.33 m2
› Active Area:
Aa = Ac-2Ad = 3.74 m2
› Hole Area:
Ah = 0.11*0.579= 0.41 m2(by trial)
Lets take,
› Weir height = hw = 50mm
› Plate thickness = 5mm
› Hole diameter = dh = 5mm

›
£ $  
› Weir Length:
Factor (Ad/Ac)*100 = 12 At (Ad / Ac) * 100 = 12
From Graph b/w (Ad/Ac)*100 vs. lw / Dc on page #
572 by ³Coulson and Richardson¶s´, 6th Ed.
lw / Dc = 0.77
lw = 1.92 m
› Weir Liquid Crest:
Maximum liquid rate = Lw = 59226.05/3600
= 16.45Kgs/sec
Minimum liquid rate)= Lw*=16.45*0.7
(at 70% turn down) =11.5kgs/sec
how =750*(Lw/dl*lw)2/3
max how =27.778mm
min how = 21.88
› At minimum liquid rate,
hw + how = 50 + 21.88
=71.88 mm
From graph 11.30, page # 571,´Coulson and
Richardson´ Vol. 6
At hw + how =71.88 mm
K2 =30.6 mm
› Weep point:
*h(min) = [K2-0.9(25.4-dl)]/dv0.5
= [30.6-0.9(25.4-5)]/4.50.5
=5.76 m/s
Actual *h(min) based on active hole area is given as:
Actual *h(min) = 0.7*(Vw/dv)*A h
= (0.7*53641.04)/(4.5*3600*0.41)
= 5.65 m/s
As, actual minimum velocity is less than *h(min) , so
we change the hole area so that Actual *h (min)
becomes well above *h(min) .
› Another Trial For Hole Area:
Aa = 3.74 m2
Ah=0.08*3.74=0.3m2

½o, Actual *h(min) = 7.72 m/sec

½ince Actual *h(min) is well above *h (min) so our

new trial is correct
3  

 m
› Dry Plate Pressure Drop:
Maximum vapor velocity through holes
*h(max) = Vm / dv*An
= 11.037 m/s
(Ah / Aa) * 100 = (0.23/2.87)*100
=8.02
From figure 11.34,6th Ed. ³Coulson and Richardson¶s´
At (Ah/Aa)*100=8.02, When Plate thickness to plate dia
ratio is 1.
Then, Co = 0.83
hd = 51 (*h / Co)2 (dv/dl)
= 33.76 mm liquid
› Residual Drop:
hr = 12.5*1000/dl
= 10.4 mm liquid
› Total Plate Pressure Drop:
ht= hd + hr + (hw +how)
= 33.76 + 10.4+ 71.88
= 116.04 mm liquid
› ¨Pt = 9.81*10-3*(ht)*dl
= 9.81*10-3*116.04*1202
=1368.3Pa = 1.36 KPa = 0.1973 psi
33 
  

› Downcomer Liquid backup/ Liquid height in
downcomer:
Let, hap= hw-10
=40 mm = 0.04m
Area under apron = hap*lw
= 0.04*1.92
= 0.0768m2
As Aap is less than Ad = 0.59m2
hdc=166*(Lw/dl*Aap)2
=166*(59226.02/1202*3600*0.0768)2
=5.27mm
› Hb = ht + hdc + (hw + how)
= 116.04 + 5.27+ (71.88)
=193.2 mm=0.2m
½ince, Hb < 0.5*(tray spacing +weir height)
0.200<0.253
½o, tray spacing is acceptable.
› Residence Time:
tr = Ad * hbc * dl
Lw
tr = 0.59 * 0.20* 1202 = 8.26 sec
16.45
As residence time is greater than 3 sec, so satisfactory
3Π
 
 
*v = (*n / *c)* 100
Where
*n = Vw/(dv*An)
= 0.764 m/s
*v = (0.764/0.952)*100
= 80.3 % (Our Assumption is correct.)
Flv = 0.0675
From Graph 11.29, 6th Ed. ³Coulson and Richardson´
Fractional entrainment= ȥ = 0.052
As, entrainment is less than 0.1, process is satisfactory
3u  ½    
› *se ½ectional Construction. The Plates are
supported on a ring welded around the vessel wall,
and on the beams about 50mm wide. Allow 50mm
wide claming zones.
lw/Dc = 1.92/3.3
= 0.77
Ԧ = 104o
› Angle subtended at plate edge by
unperforated strip = 180o ± 104o
= 76o
› Length of unperforated edge strips :
(2.5 ± 50*10-3)  *76 = 3.25 m
180
Area of unperforated edge strip =Au = 50*10-3*3.25
= 0.162 m2
Mean length of Claming Zone:
(2.5-50*10-3)*½in(76o/2) = 1.508m
Area of calming zone = Acz = 2*50*10-3*1.508
= 0.15m2
Total area available for perforations:
Ap = Aa ± (Au + Acz) = 3.42 m2
Ah/Ap = 0.3/3.42 = 0.087
From Graph 11.33, 6th Ed., Coulson and Richardson
lp/dh = 3.2 (satisfactory i.e. b/w 2.5²4.0)
Hole Pitch: lp/dh = 3.2, lp=16mm Triangular
Number Of Holes per plate:
Number Of Holes = Total hole area = 9307
Area of one hole
3è   

No. of plates = 23
Tray spacing = 0.457 m
Distance between 23 plates = 10.5 m
Top clearance = 0.5 m
Bottom clearance = 0.5 m
Tray thickness = 5 mm/plate
Total thickness of trays = 0.005* 23= 0.115 m
Total height of column = 10.5+ 0.5 + 0.5 + 0.115
Ht = 11.6m
3J   
  
½HELL:
Diameter of the tower =Dc = 2500 mm = 2.5 m
Working/Operating Pressure = 1.01325 bar =101325 Pa
Design pressure = 1.1×Operating Pressure
= 1.1×101325 = 1.11*105Pa
Working temperature = 525.22 ºK
Design temperature = 1.1*525.22=577.7 ºK
½hell material = ½tainless steel,Type:317
Permissible tensile stress (ft) = 540 MN/m2
Elastic Modulus (E) = 210000 MN/mm2
Insulation material = Diatomaceous earth
Maximum Working Temperature=650oF
Insulation thickness = 2´= 50.8 mm
Density of insulation = 288 kg/m3
HEAD - TORI½PHERICAL DI½HED HEAD:
Material = ½tainless steel,Type:317
Allowable tensile stress = 540 MN/m2
½*PPORT ½KIRT:
Height of support = 5000 mm = 5 m
Material ± Carbon ½teel
3x  

½  


Considering the vessel as an internal pressure vessel.
ts = ((P×Rc)/ ((ft×J)- 0.6P)) + C
Where ts = thickness of shell, mm
P = design pressure, Pa
Rc = diameter of shell, m
ft = permissible/allowable tensile stress, MN/m2
C = Corrosion allowance,3 mm
J = Joint factor
ts = 3.26 mm
Taking the thickness of the shell = 6 mm (standard)
3  m

Type: Torispherical head:
Thickness of head = th = (P×Rc×0.885)/ (ft×J-0.1P)
P =internal design pressure, Pa
Rc = radius of shell, m
th = (111457.5×1.25×0.885)/ (540E+06×1-
0.1*111457.5)
= 3.23mm
Including corrosion allowance take the thickness of
head = 3 mm
th = ((111457.5×1.25×0.885)/ (420*106×1.00)) + C
= 3.23 mm
Thickness of shell=8mm (½tandard)
½    ½ 
m
  
%m u3
½PECIFICATION ½HEET
›Identification:
Item Distillation column
Item No. D-310
No. required 1
Tray type ½ieve tray
›Function: ½eparation of ODCB from TDI and
Reaction Residues.
›Operation: Continuous
› Material handled:

Feed Top Bottom

Quantity 36453.6Kg/h 30843.8Kg/ 5586Kg/hr
r hr
Compositi 84.51% 99.78% 0.5%
on of
ODCB
Temp. 194oC 160oC 252.22oC
 › Design data:

No. of tray=27 Active holes = 9307

Pressure = 101.32 KPa Weir height = 50 mm
Height of column = Weir length = 1.92 m
13.47m Reflux ratio = 0.33:1
Diameter of column Tray spacing =0.457m
=2.5m Active area = 3.74 m2
Hole size = 5 mm Flooding = 80.3 %
Pressure drop per tray = Entrainment=5.2%
1.36 KPa
Tray thickness = 5 mm
 

› condenser is a two-phase flow heat exchanger in
which heat is generated from the conversion of
vapor into liquid (condensation) and the heat
generated is removed from the system by a
coolant.
› Types of Condensers:
½team Turbine Exhaust Condensers/surface
condensers
1. Plate Condensers
2. Air-Cooled Condensers
3. Direct Contact Condensers
4. ½hell & tube type
 ½    

   
Four Condenser Configuration are Possible
› Horizontal with condensation in shell side and cooling
medium in the tubes.
› Horizontal with condensation in tube side cooling
medium in shell side.
› Vertical with condensation in the shell.
› Vertical with condensation in the tubes.
Horizontal shell side and vertical tube side are the
most commonly used types of condensers. In this
process we have used the horizontal with
condensation in shell side & cooling medium in tube.
m
 ½ 
 

%
u3Œ
› Heat Balance.
› Assumed Calculations.
› Calculations Of Heat Transfer Coefficients.
› Calculations Of Pressure Drops.
 &
T1=160C
T2=160C

t2=60C t1=30C

› Vapor: Qvap = mHv

Qvap = 11202300KJ/hr
› Water: Q = wCp( t2- t1)
w = 88907.14 Kg/hr
› LMTD: LMTD = (T2 - t1) - (T1- t2) = 114.34oC
Ln (T2 - t1)
(T1- t2)



  

Assume Design overall coefficient =*D = 850 W/m2 oC
Heat Transfer area: A=Q /(*D*LMTD)=32.017m2
Tube Lay out & size: Length = 2.4m , Passes = n=2
OD, BWG, pitch(Pt) = 19mm, 16 BWG,
24mm Triangular pitch.
Out side surface area per linear ft =a"t = 0.06m2
No. of tubes = Nt = A/ (a´t.L) = 222
½hell side: From the nearest count on Table 9, ³Process
Heat Transfer by Kern´
ID = 0.438m , No. Of Tubes=Nt=224
½uppose Baffle spacing=B = 0.8m and Passes = 1
   
 
   

› Cold Fluid: tube side (water)
› Flow area: at = Nt*a"t = 0.0224m2
144*n
› Mass velocity: Gt = w/at= 3969068.75Kg/hr.m2
Velocity : V = Gt/3600*ȡw= 1.1 m/s
From Graph 25 On Kern
hi = 5678.3W/m2.oC

hio = hi*ID
OD
hio = 4692 W/m2.oC
Hot fluid: shell side (Vapors)
› Flow area:as = ID*C*B C=Pt-do =24mm
144*Pt
as = 0.073m2
› Mass velocity:Gs =W/as =557367.94Kg/hr.m2
› Loading: G"=W/L*Nt2/3= 394.2 Kg/hr. m
Assume ho = 2000W/m2.oC
tw = ta + ho (Tv - ta) =85C
(hio + ho)
tf = tw + Tv = 122.5C
2
ho = 1750 W/m2.oC
Clean Overall Coefficient:
*C = hio*ho = 1274.6 W/m2.oC
hio+ho
› Dirt Factor: Rd = (*d-*c)/(*d**c) = 0.00039
(½atisfactory)
m  
 

 m
› ½hell ½ide: De = 0.014 m(Table 10, Kern)
› Res = De*Gs = 197018.2
u
f = 0.1728 (From Graph 26 Kern)
s =0.004
› No. Of Crosses: N + 1= (L/B) =3
› ¨Ps = __f*Gs2*Ds*(N + 1) =24.3KPa
2*5.22*1010*De*s
› Tube ½ide: water
› Ret = 26226.6 f = 0.037
› ¨Pl = _f*Gt2*L*n_______ = 3.2KPa
5.22*1010*D*s*Ët

› ¨Pr= 4nV2 =4.84KPa

s*2g¶

› ¨Pt= ¨Pr+ ¨Pl=8.04KPa

½    ½  

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 9;
   

› Reboilers are heat exchangers provided at the

bottom of the fractionator to generate the stripping
vapors stream.
› Classification:
1. Forced circulation reboiler.
2. Kettle reboiler.
3. Fired reboiler.
4. Thermosiphon reboiler.
½      
› The best choice is the kettle reboiler due to
following main reasons.
› High residence time.
› Rate of vaporizations is very high (about
90%) of the feed.
› The viscosity of the system is not very high
› Comparatively less costly under above
conditions .
m
 ½ 
   %

33u
› Heat Balance.
› Assumed Calculations.
› Calculation of heat transfer coefficients.
› Calculation of Pressure Drops.
 &
› Hot Fluid: Thermal fluid (Dimethyle ½iloxane)
› Cold Fluid: Bottoms (87.5%TDI)
› Vapor load:53641.04Kg/hr
› Heat duty:1.12*107KJ/hr
› Flow rate of Dimethyle ½iloxane=W=
247422.47Kg/hr
› LMTD:62.13oC

         
 
)   0



  

› Let *D=596 W/m2oC
A=Q/(*D*LMTD)=83.8m2
› Tube specification:19mm OD, 24mm Triangular
Pitch, 16BWG
› No.Of Tubes=Nt=(83.8/3*0.06)=465
Corrected *D=(Q/a¶1*Nt)=103 Btu/hr.ft2.oF
From Table 10(Kern) By the Nearest Count
Nt=506
› Diameter Of tube Bundle=Db=(OD)*(n/C)1/2.21
Db=0.6m Where C=0.249
› ½hell Dia.=1.08m (Ratio Of Bundle to ½hell Dia is 1.8)
   
 
   

›  
   !"#
› Flow Area=at=0.0002m2/tube
at = (a¶t*Nt/n) = 0.0506 m2
› W=Q/Cp*ǻT=247422.47Kg/hr
› Gt = W/at = 1358.27Kg/m2.hr
V= (Gt/3600*ȡ)=1.82m/sec
hi=1567.2 W/m2.C
hio=hi*(ID/OD)=1295 W/m2.C
   

Assume ho=1703.5 W/m2.C
tw=ta + (hio/ho+hio)*(Ta-ta)
tw= 279.33C
ǻtw = 27.11C From graph 11.5(Kern) ho>1703.5 W/m2.C
so use
ho=1703.5 W/m2.C
*c=ho*(hio/(ho+hio)) = 736 W/m2.C

Dirt Resistance=Rd=(*c-*d)/(*c**d)
= 0.00032m2C/W
(½atisfactory)
  

 m

›  
› Ret = (Gt*D/ȝ )
Ret= 50000
f=0.0026, s=0.672
› ǻPt = (f*Gt*L*n/5.22*1010 * D*s)
ǻPt = 9.16KPa
› ǻPr = (4/s) *( n) * (V2/g´)
ǻPr = 13.5KPa
› ǻPT = ǻPt + ǻPr
ǻPT = 22.6KPa
›   Negligible
½    ½    
%
33u
› Identification:
Item name:Reboiler
Item no.:E-113
Type: Kettle Reboiler
No. Required = 1
› Function:
To Vaprize The bottom Product Of Distillation Column
› Heat Duty = 1.12*107KJ/hr
›  
Fluid handled: Dimethyle ½iloxane
Flow rate = 247422.47 Kg/hr
Pressure = 202 Kpa
Temp. = 326 oC to 304 oC
Tubes: OD:19mm,16BWG
506 tubes each 3 m long
2 passes
24 mm triangular pitch
pressure drop = 22.6 KPa
›  
Fluid handled :Bottoms Of Distillation Column
Vapor Load= 53641.04Kg/hr
½hell: 1.08 m diameter
1 pass
Pressure drop = Negligible
Temperature= 252.22oC
* ThermalFluid (Dimethyle ½iloxane)

› *D assumed = 596 W/m2.oC

› *c calculated = 736 W/m2oC
› Calculated dirt factor = Rd = 0.00032 m2oC/W
› Allowable dirt factor = Rd = 0.0006 m2oC/W