Chapter # 05 Equipment design

5.6 DESIGN OF DISTILLATION COLUMN

In industry it is common practice to separate a liquid mixture by distillating the

components, which have lower boiling points when they are in pure condition
from those having higher boiling points. This process is accomplished by partial
vaporization and subsequent condensation.

5.6.1CHOICE BETWEEN PLATE AND PACKED COLUMN:

Vapour liquid mass transfer operation may be carried either in plate column
or packed column. These two types of operations are quite different. A selection
scheme considering these factors fewer than four headings.

i) Factors that depend on the system i.e. scale, foaming, fouling factors,
corrosive systems, heat evolution, pressure drop, liquid holdup.
ii) Factors that depend on the fluid flow moment.
iii) Factors that depends upon the physical characteristics of the column and
its internals i.e. maintenance, weight, side stream, size and cost.
iv) Factors that depend upon mode of operation i.e. batch distillation,
continuous distillation, turndown, intermittent distillation.

The relative merits of plate over packed column are as follows:

i) Plate column are designed to handle wide range of liquid flow rates
without flooding.
ii) If a system contains solid contents, it will be handled in plate column,
because solid will accumulate in the voids, coating the packing
materials and making it ineffective.

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iii) Dispersion difficulties are handled in plate column when flow rate of
liquid are low as compared to gases.
iv) For large column heights, weight of the packed column is more than
plate column.
v) If periodic cleaning is required, man holes will be provided for cleaning.
In packed columns packing must be removed before cleaning.
vi) For non-foaming systems the plate column is preferred.
vii) Design information for plate column are more readily available and
more reliable than that for packed column.
viii) Inter stage cooling can be provide to remove heat of reaction or solution
in plate column.
ix) When temperature change is involved, packing may be damaged.

5.6.2 Distillation Column Design Steps

Designation of design basis

Operating conditions
Determination of equilibrium stages
Size of the column
Design of plate

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5.6.3 Designation of Design Basis:

Feed mol Bottom mol
Components Top mol fraction
fraction fraction
H2 0.4647 0.8472

CH4 0.0112 0.0205

C 2 H6 0.0110 0.0200

C 3 H8 0.0127 0.0232

C4H10 0.0247 0.0451

C5H12 0.0252 LK 0.0433 0.003

C6H14 0.0482 HK 0.0006 0.106

C7H16 0.1290 0.286

C 6 H6 0.1594 0.353

C6H5--CH3 0.1020 0.226

C6H11--CH3 0.0073 0.016

C5H9--CH3 0.0044 0.010

5.6.4 OPERATING CONDITIONS:

Operating Pressure 15.2 atm
Streams Temperature
Feed 125 oC
Top Stream 48 oC
Bottom stream 250 oC
Reflux stream 40 oC

5.6.4 DETERMINATION OF EQUILIBRIUM STAGES:

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Equilibrium data at operating conditions

Determination of minimum reflux ratio
Determination of minimum number of stages
Determination of ideal stages

Equilibrium data at operating condition:

RELATIVE
Components K-VALUES
VOLATILITY
H2 __
CH4 16.400 51.250
C 2 H6 5.500 17.188
C 3 H8 3.200 10.000
C4H10 1.200 3.750
C5H12 0.560 1.750
C6H14 0.320 1.000
C7H16 0.130 0.406
C 6 H6 0.080 0.250
C6H5--CH3 0.182 0.569
C6H11--CH3 0.102 0.320
C5H9--CH3 0.218 0.680

Minimum Reflux Ratio:

By using Coulburn method,

1 X dL X
R AB dH
min
( AB 1) X nL X nH

Upper pinch Temperature

1
Tn T p (TB TP )
3
1
48 ( )(250 48)
3

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=115.33 oC

Lower pinch Temperature

1
T Tp (TB TP )
3
2
48 ( )(250 48)
3

= 182.667 oC

Light Key composition in Upper pinch

rf
X nL
(1 r f )(1 X fn )

Where;
rf = ratio of composition of light key to heavy key in the liquid part of feed.
I = relative volatility of components with respect to heavy key.
Xfhi = composition of heavier than heavy key components in the feed stream.

Now;
For components heavier than heavy key
Components Mol. Fractions Xfn
C7H16 0.129 0.406 0.052
C 6 H6 0.159 0.250 0.040
C6H5--CH3 0.102 0.569 0.058
C6H11--CH3 0.007 0.320 0.002
C5H9--CH3 0.004 0.680 0.003

Xfn = 0.155

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X fL
rf
X fH

0.0252
rf = 0.52
0.0482
rf
X nL
(1 r f )(1 X fn )

0.52
=0.296
(1 .52)(1 0.155)

X nL
X nH
rf

0.296
= 0.569
0.52

Now using this equation,

1 X dL X
R AB dH
min
( AB 1) X nL X nH

1 0.0433 0.0006
1.75
(1.75 1) 0.296 0.569

=1.947

Optimum Reflux Ratio ranges from (1.1 1.5)*R min.

I choose the optimum reflux ratio, by plotting the graph b/w total annual cost and
reflux ratio. (Given in appendix)
reflux ratio taken is 2.92

Minimum Number of Stages:

By using Fenskes Equation;

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X X
ln LK HK
X HK d X LK b
Nm
ln LK

0.0433 0.106
ln
0.0006 d 0.003 b

ln 1.75

=14 plates with reboiler

Number of Ideal Stages:

Using Erbar - Maddox graph (fig 11.11 C&R Vol. 6)

N + partial condenser 24

N 23

Actual Number of Stages and Feed Location:

Plate Efficiency:
Using OConnell method (Coulson Vol.6)

E 51 32.5 log( a a )

Where;
a = average viscosity of liquid, mNs/ m2
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a = Relative volatility of light key

a = 0.1712 m Ns/ m2
So,
E 51 32.5 log(0.1712 * 1.75)

= 68.02 %
Actual number of stages (N actual)

N actual = N ideal / Eo
= 23/0.68
= 34 (excluding partial condenser)

Feed location
By, using kirkbridge Equation;

ND B x fHK xbLK
2

log 0.206 log

x dHK

NB D x fLK

ND 139.271 0.048 0.003 2

log 0.206 log
NB 169.211 0.025 0.0006

ND
2.13
NB

N D 2.13 N B

N total N D N B

34 2.13 1 N B

N B 11

So feed is entering at 11th plate from bottom.

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5.6.5 TRAY DESIGN

Molar Flow Rate of Streams:

Feed, F 308.48 kg mol/hr

Top Product, D 169.21 kg mol/hr

Bottom product, W 139.27 kg mol/hr

Reflux, Ln 494.10 kg mol/hr

Vapour Flow Rate:

in rectifying section, Vn 663.30 kg mol/hr

in stripping section, Vm 513.11 kg mol/hr

Liquid Flow Rates:

in rectifying section, Ln 494.10 kg mol/hr

in stripping section, Lm 652.38 kg mol/hr
Lm/W 4.68

Physical Conditions:
Top Bottom

Vapour Density, kg/m3 8.78 34.36

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Liquid density, kg/m3 504.6 796.3

Vapour flow rate, m3/sec 0.9486 0.1875

Liquid flow rate, m3/sec 0.0122 0.0102

Vapour & Liquid velocities can be found by using following formulae respt.

Vm avg Molwt
Vapour flow rate = V 3600

Lm avgMolwt
Liquid flow rate = V 3600

Diameter of Column:

V
1/ 2

2
u v 0.171l t 0.27l t 0.047 L V


Where;
Uv = maximum allowable vapour velocity, based on the gross (total)
Column cross-sectional area, m/s,
lt = plate spacing, m, (range 0.5 --1.5)

Plate Spacing = 0.5 m

Now, by putting values in above formula we get vapour velocity as under,

Top Bottom
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Vapour velocity, m/s 0.34 0.213

Now,
Diameter of column can be calculated as,

4VW
DC
V uV

Where;
Vw is the maximum vapour rate, kg/sec
By putting values we get as,

Column Diameter, Dc 1.05 m

We based our design on bottom diameter.

So, I take diameter = 3.5 ft

1.067 m

Tray Design:

Tower application or service Product finishing

Tower inside Diameter 1.067 m
Tray type Cross flow
Tray spacing 0.508 m
No. of down comers / tray 1

Caps Data:

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4 in standard cap size is selected for 3.5 ft column, so that

all data about cap becomes fixed.

Cap OD = 4 in =0.1016 m
Cap ID =0.0984 m
Pitch 600(triangular)
Spacing 0.03175 m
No. of rows/tray 8
Inside Height above tray 0.1000 m
No. of slots/cap, Ns (selected from table) 51
Height of slot, Hs, 0.0381 m
Width of slot, ws 0.003175 m
skirt Height, s 0.00635 m

Shroud ring height, hsr 0.00635 m

Riser OD. 0.06985 m
ID. 0.06667 m
Riser height above tray floor 0.08255m

Down Flow Area, Adf;

It ranges from 10 20 % of tower area.
Thus for 15% of tower area 0.134 m2

Liquid Distribution Area, Ala;

It ranges 8 20 % of tower area.

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And for 16 % of tower area 0.143 m2

End Wastage, Aew;

It ranges from 7 22 % of tower area

And for 15 % of tower area 0.134m2

No. of caps /tray;

AC Adf Ala Aew
NC
ac
0.894 0.134 0.143 0.134
NC
0.0081
= 60 caps

Areas:
D 2
Area =
4

D 2
Total cap area = N C
4

Cap inside cross-sectional area, ac 0.007606 m2

Total cap inside cross-sectional area/tray, Ac 0.456 m2

Riser inside cross-sectional area/cap, ar 0.00349 m2

Total riser inside cross-sectional area/tray, Ar, 0.209 m2

Riser outside cross-sectional area/cap, aro, 0.003832 m2

Total riser outside cross-sectional area/tray, Aro,0.229 m2

2
Annular area per cap. a a
4
d ci d ro2 0.003773 m2
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Total annular area/tray, Aa 0.226 m2

Reversal area / cap,ar, 0.00399 m2

Total reversal area/tray 0.2394 m2

Slot area/ cap,as, (Ns*Hs*Ws) 0.00617 m2

Total slot area / tray , As, 0.37 m2

Tray Details:

Length of outlet weir Iw,

Usually taken from 60 80 % of diameter
of column
I take 75% of diameter of column 0.80025 m

Height of weir above tray floor, hw(2.5 3.5 in.) 0.0762 m

Height of top of cap slots (depends on Hs)
above tray floor 0.0508 m

Static slot submergence or seal, hss, 0.0381 m

Height of bottom of Down comer
above tray floor 0.06985 m
Riser slot seal 0.0508 m

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Performance of Tray:

Top Bottom

Residence time in downcomer;

down comer area, Ad (Using graph b/w

Weir length and down comer area)0.134 m2 0.134 m2
effective height of down comer ,hde
hde = St +hw/12 0.5842 m 0.5842 m
time= (Ad*hde) / Vl 6.5 sec 8.0 sec

Slots:
1 2
v 3 V 3
hs 32
l v N C N S wS

Where;
hs = slot opening, or pressure drop through slot, in. liquid.
V = total vapour flow through tray, ft3/sec

Nc = number of caps per tray

Ns = number of slots per cap
Ws = width of slot (rectangular), in.

slot opening, hs 0.042 m 0.0236 m

Maximum slot velocity(12.1/g)1/2 4.98 m/sec 2.5 m/sec
Minimum slot velocity (3.4/g)1/2 1.418 m/sec 0.71 m/sec
Super facial slot velocity, uo= V/As 2.56 m/sec 0.052 m/sec

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Pressure Drop:

Caps:
Top Bottom
Riser Pressure Drop, hr;
2.09
d 1 V
hr 0.111 r V 2
L A
r

Where;
dr = dia of riser 2.625 in 2.625 in
L = density of liquid 31.43 lb/ ft3 49.6 lb/ ft3
v = density of vapour 0.547 lb/ ft3 2.14 lb/ ft3
V = volumetric flow rate 33.5 ft3/sec 6.622 ft3/sec
Ar = total riser area 2.25 ft2 2.25 ft2

By solving equation,
hr = Pressure drop (in in of liquid) 0.079 in 0.058 in
Reversal and Annulus Pressure Drop, hra;

1.71
0.68 2a r2 1 V
hra V 2
L a a
x c A
r
Where;
ar = inside riser area = in2 5.41 5.41
ax = Reversal area = in2 6.185 6.185

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ac = inside area of cap = in2 11.79 11.79

By solving equation,
hra = Pressure drop (in in of liquid) 0.086 0.062

Rectangular Slot Dry pressure Drop, hs' ;

1.73
0.163 1 V
h'S dC V 2
L AS

Where:
dc = diameter of cap = in 3.874 3.874
As = total area of slot = ft2 3.983 3.983
By solving equation,
hs = Pressure drop (in in of liquid) 0.0368 0.026

Total dry pressure drop;

hC' hr hra hS' (Inches of liquid) 0.1918 0.146

V V a S 2
Wet cap pressure drop, (in of liquid) =
AS L a a

Where;
as = area of slot /cap = in2 9.56 9.56
aa = annular area/ cap = in2 5.85 5.85

V V aS 2
0.36 0.31
AS L aa

From graph (fig 8-115 Ludwig, vol. 2, p 167)

The values of Cw are.
Cw 0.18 0.14
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hc= hc/Cw 1.065 1.042

hcmax = hr+hra+(Hs+s) 1.915 1.87

Since hc is less than hc,max., cap is O.K. and not blowing under the shroud
ring.

Height of Liquid over Weir; Top Bottom

First calculate,
Lg/ (lw) 2.5 17.32 14.48
And
lw/D 0.75 0.75
Where;
Lg = flow rate of liquid in gallons/min
lw =length of weir = ft

Using graph (fig 8-104 Ludwig, vol. 2, p 159)

Factor,Fw 1.09 1.075
Lg
hOW 0.092 FW (In) 1.762 1.54
lW

Liquid gradient /2:

Mean tray width = (dc + lw)/2
= (3.5+2.625)/2 3.0625 ft =0.934 m

Assumed Liquid Depth, h1

h1 = hw + how+ (/2) assume 4.862 in 4.65 in

Lg/mean tray width (gallon/min. ft) 63.14 52.79

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Uncorrected /no. of Rows (inches) 0.02 0.02

V0 (v) 1/2 1.401 1.0066

From graph Cv (fig 8-113 Ludwig, vol.2)1.06 0.97

Where;
= liquid gradient in inches of liquid
Vo = Superficial velocity based on column area (ft/sec)
3.482 0.688
Cv = correction factor for uncorrected liquid gradient
No. of rows = 8

Corrected /2 (inches of liquid) 0.112 0.0805

Total Pressure Drop/Tray :( in inches of liquid)

ht =hc +hss +how +/2

Where;
hc (inches of liquid) 1.065 1.042
hss (inches of liquid) 1.5 1.5
how (inches of liquid) 1.762 1.54
/2 (inches of liquid) 0.112 0.0805

ht = hc + hss + how + /2 4.439 4.1625

Total Pressure Drop/Tray (in inches of water)

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3.007 2.85

Range for pressure drop is 2- 4 in of water /tray

So pressure drop is with in the range
Pressure drop for trays (in in. of water)
For 23 plate above, and 11 plate below 69.161 31.35
(mm of Hg) 129.22 58.572

Downcomer Pressure Drop:

Down comer friction loss plus underflow loss, hdu

2
Lg
hdu 0.56 0.0399 in 0.0249 in
449 Ad

in mm of Hg 0.07455 0.04652

Where;
Ad = down comer area in ft2

Liquid height in down comer:

Hd = hw + how + hd + ht + 0.2077 m 0.1957 m

Hd < St which is in range.

Free Height in Downcomer:

F = St + hw - Hd 0.389 m 0.40 m

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Throw over weir:

tw = 0.8 [ how* F]1/2 108.9 mm 99.9 mm

Dynamic Slot Seal:

hds = hss + how + /2 85.69 mm 79.26 mm

Liquid Entrainment:

volflowrate
Vf 1.51 m/sec 0.299 m/sec
Ac 2 Ad
Where:
Vf = Superficial velocity based on active area m/sec

Calculate:
1
27.3 V 2
10.75V F 3.52 2.047
St L V

From graph, (fig 8-116 Ludwig, vol. 2, p 169)

We / (how + hss +hs ) 0.5 0.025

And

We in Kg/min m2 0.0624 0.0025

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Entrainment in Kg/min (We *(Ac 2Ad))0.39 0.157

Entrainment ratio 0.0078 0.00306

The value of entrainment is low, so spacing is quite good.

Height of Column:

Height of column ( 20 inches tray spacing)

Hc = (N actual 1) St + H
= (34 1) 0.508 + 1.918
= 18.75 m

SPECIFICATION SHEET OF DISTILLATION

COLUMN D-270

Identification:
Item Distillation column
Item No. T-102
No. required 1
Tray type Bubble cap tray
Function: Separation of Light H.C from Heavy H.C
Operation: Continuous
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Material handled

Feed Top Bottom

Quantity 308..48 Kgmol/hr 169.211 kgmol/hr 139.27 Kgmol/hr

Compositions
Light key 2.52 % 4.3 % 0.30 %
Heavy key 4.82 % 0.06 % 10.6 %
Temperature 125 oC 48o C 250 oC

Design Data

Pressure = 15.2 atm Reflux ratio = 2.92:1

No.of trays = 34 Cap size = 0.1016m
Diameter of column= 1.067 m No. of Caps/tray = 60

Shell thickness = 11.887mm Weir length = 0.80025 m

Corrosion allowance=2.0mm Weir height =76.2 mm

Tray spacing = 0.508 m Down comer area =0.134 m2
Height of column = 18.75 m Overall efficiency = 68%

Top Bottom

Pressure drop/tray = 3.007 2.85 in. of water

Entrainment ratio = 0.0078 0.00306

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