DESIGN OF DISTILLATION COLUMN

CHAPTER No.9
DESIGN OF DISTILLATION
COLUMN
In industry it is common practice to separate a liquid mixture by distilling 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.

9.1 DISTILLATION:-
“Process in which a liquid or vapor mixture of two or more substances is separated
into its component
fractions of desired
purity, by the
application and
removal of heat”.

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9.2 TYPES OF DISTILLATION COLUMNS

There are many types of distillation columns, each designed to perform specific types of
separations, and each design differs in terms of complexity.
 Batch columns
 Continuous columns

Batch Columns
In batch operation, the feed to the column is introduced batch-wise. That is, the column is
charged with a 'batch' and then the distillation process is carried out. When the desired
task is achieved, a next batch of feed is introduced.

Continuous Columns
In contrast, continuous columns process a continuous feed stream. No interruptions occur
unless there is a problem with the column or surrounding process units. They are capable
of handling high throughputs and are the more common of the two types. We shall
concentrate only on this class of columns.

9.3 CHOICE BETWEEN PLATE AND PACKED

COLUMN
Vapor liquid mass transfer operation may be carried either in plate or packed column.
These two types of operation are quite different. The relative merits of plate over packed
column are as follows:

1-Plate column are designed to handle wide range of liquid flow rates without flooding.
2-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.
3-Dispersion difficulties are handled in plate column when flow rate of liquid are low as
compared to gases.
4-For large column heights, weight of the packed column is more than plate column.
5-If periodic cleaning is required, man holes will be provided for cleaning. In packed
columns packing must be removed before cleaning.

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6-For non-foaming systems the plate column is preferred.

7-Design information for plate column is more readily available and more reliable than
that for packed column.
8-Inter stage cooling can be provided to remove heat of reaction or solution in plate
column.
9-When temperature change is involved, packing may be damaged.

Our mixture which is to be processed is “Acrylonitrile, Acetonitrile”. I’ve selected plate

column because:
1-System is non-foaming.
2-Temperature is high i.e. 80C.

CHOCE OF PLATE TYPE

There are three main types, sieve tray, bubble cap, valve tray. I’ve selected sieve tray
because:
1-They are lighter in weight and less expensive. It is easier and cheaper to install.
2-Pressure drop is low as compared to bubble cap trays.
3-Peak efficiency is generally high.
4-Maintenance cost is reduced due to the ease of cleaning.

9.4 SELECTION CRITERIA OF TRAYS

Cost

Cost of plate depends upon material of construction used.

For mild steel, the ratio of cost between plates is

Sieve plate : valve plate : bubble-cap plate

3 : 1.5 : 1.0.
Capacity

Sieve tray > valve tray > bubble-cap tray

Operating Range:-
It is the range of liquid and vapor flow rates which must be above the weeping
conditions and below the flooding conditions. Operating range flexibility comparison is
Bubble cape tray > Valve tray > Sieve tray

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For good design, sieve plate gives satisfactory operating range.

Pressure drop

Bubble-cap tray > valve tray > sieve tray

Choice of Tray Type (Sieve Tray)

 Sieve plates are lighter in weight and less expensive. It is easier and cheaper to
install.
 Pressure drop is low as compared to bubble cap trays.
 Maintenance cost is reduced due to ease of cleaning.
 If properly designed, sieve tray gives desired separation

9.5 MAIN COMPONENTS OF DISTILLATION

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COLUMNS
Column internals such as trays/plates and/or packing which are used to enhance
component separations.

 A reboiler to provide the necessary vaporization for the distillation process. The
liquid removed from the reboiler is known as the bottoms product or simply,
bottoms.
 A condenser to cool and condense the vapor leaving the top of the column. The
condensed liquid that is removed from the system is known as the distillate or top
product.
 A reflux drums to hold the condensed vapor from the top of the column so that
liquid (reflux) can be recycled back to the column. The condensed liquid is stored
in a holding vessel known as the reflux drum. Some of this liquid is recycled back
to the top of the column and this is called the reflux.

A schematic of a typical distillation unit with a single feed and two product streams is
shown above.

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9.6 FACTORS AFFECTING DISTILLATION

COLUMN OPERATION
Vapor Flow Conditions
Adverse vapor flow conditions can cause:
 Foaming
 Entrainment
 Weeping/dumping
 Flooding

Foaming
Foaming refers to the expansion of liquid due to passage of vapor or gas. Although it
provides high interfacial liquid-vapor contact, excessive foaming often leads to liquid
buildup on trays. In some cases, foaming may be so bad that the foam mixes with liquid
on the tray above. Whether foaming will occur depends primarily on physical properties
of the liquid mixtures, but is sometimes due to tray designs and condition. Whatever the
cause, separation efficiency is always reduced.

Entrainment
Entrainment refers to the liquid carried by vapor up to the tray above and is again caused
by high vapor flow rates. It is detrimental because tray efficiency is reduced: lower
volatile material is carried to a plate holding liquid of higher volatility. It could also
contaminate high purity distillate. Excessive entrainment can lead to flooding.

Weeping/Dumping
This phenomenon is caused by low vapor flow. The pressure exerted by the vapor is
insufficient to hold up the liquid on the tray. Therefore, liquid starts to leak through
perforations. Excessive weeping will lead to dumping. That is the liquid on all trays will
crash (dump) through to the base of the column (via a domino effect) and the column will
have to be re-started. Weeping is indicated by a sharp pressure drop in the column and
reduced separation efficiency.

Flooding
Flooding is brought about by excessive vapor flow, causing liquid to be entrained in the
vapor up the column. The increased pressure from excessive vapor also backs up the
liquid in the down comer, causing an increase in liquid holdup on the plate above.
Depending on the degree of flooding, the maximum capacity of the column may be
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severely reduced. Flooding is detected by sharp increases in column differential pressure

and significant decrease in separation efficiency.

Reflux Conditions
Minimum trays are required under total reflux conditions, i.e. there is no withdrawal of
distillate. On the other hand, as reflux is decreased, more and more trays are required.

Feed Conditions
The state of the feed mixture and feed composition affects the operating lines and hence
the number of stages required for separation. It also affects the location of feed tray.

State of Trays and Packings

Remember that the actual number of trays required for a particular separation duty is
determined by the efficiency of the plate. Thus, any factors that cause a decrease in tray
efficiency will also change the performance of the column. Tray efficiencies are affected
by fouling, wear and tear and corrosion, and the rates at which these occur depends on the
properties of the liquids being processed. Thus appropriate materials should be specified
for tray construction.

Column Diameter
Vapor flow velocity is dependent on column diameter. Weeping determines the minimum
vapor flow required while flooding determines the maximum vapor flow allowed, hence
column capacity. Thus, if the column diameter is not sized properly, the column will not
perform well.

9.7 DESIGNING STEPS OF DISTILLATION

COLUMN

 Calculation of Minimum Reflux Ratio Rm.

 Calculation of optimum reflux ratio.
 Calculation of theoretical number of stages.

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 Calculation of actual number of stages.

 Calculation of diameter of the column.
 Calculation of weeping point.
 Calculation of pressure drop.
 Calculation of thickness of the shell.
 Calculation of the height of the column.
Process Condition:-

Process Design:-
Temperature of feed = 80o C
Temperature of top product = 75o C
Temperature of bottom product = 98o C

COMPONENTS FEED DISTILLATE BOTTOM

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XF XD XW
Acrylonitrile .93 .98 .011
Acetonitrile .04 .00004 .94
Acrolein .02 .02 .005
Water .002 .00002 .05

Heaviest Key Component = Water

Light Key Component = Acetonitrile
Relative Volatility
Acrylonitrile = 2.85
Water = 1
Calculation of Minimum Reflux Ratio Rm
Using Underwood equation,
α A xfA α B xfB
  1 q
αA  θ αB  θ

As feed is entering as vapors so, q = 0

By trial,  = 1.88

α A xfA α B xfB
  R m 1
Using eq. of min. reflux ratio,
αA  θ αB  θ
putting all values Rm = 2.5
Actual Reflux Ratio:-
The rule of thumb is:
R = (1.2 ------- 1.5) Rmin
R = 1.3 Rmin
R = 3.25
Calculation of Minimum no. of Plates:-
The minimum no. of stages Nmin is obtained from Fenske relation which is,

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N min 
log     
XB XC
XC D XB B

log α BC  ave
Nmin = 6
Theoretical no. of Plates:-
Gilliland related the number of equilibrium stages and the minimum reflux ratio and the
no. of equilibrium stages with a plot that was transformed by Eduljee into the relation ;

N  N min   
0.566
 .751   R  Rmin
N 1 R  1 
  

From which the theoretical no. of stages to be,

N= 20.
One plates is removed for reboiler, so N = 20-1 = 19
Location of feed Plate:-
The Kirkbride method is used to determine the ratio of trays above and below the feed
point.


   xLK  B 
2

log
ND 
 . 206 log B  xHK   
  D xLK   xHK  D  
 NB   
From which,
Number of Plates above the feed tray = ND = 12
Number of Plates below the feed tray = NB = 7
Calculation of actual number of stages:-
Tray Efficiency:

Average temperature of column = 75+98/2 = 87oC

Feed viscosity at average temperature = L = 0.30 Cp

= 0.6
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From equation , overall efficiency of column = 60%

So, No. of actual trays = 19/0.6 = 33
Location of feed point = 7/0.6 = 12
Determination of the Column Diameter:-

Top Conditions Bottom Conditions

Ln= 1210 kgmol/hr Lm = 1496 kgmol/hr

Vn = 1486 kgmol/hr Vm = 1486 kgmol/hr

Average Mol Wt = 53 kg/kgmol Average Mol wt = 40 kg/kgmol

T = 353 K T = 390 K

Liquid density = dl = 807 kg/m³ Liquid density = dl = 787 kg/m³

Vapour density = dv = 2.01 kg/m³ Vapour density dv = 1.71 kg/m³

Flow Parameter: (For Stripping Section)

0.5
L  ρ v 
FLV   m  
 Vm  ρ L 

FLV = Liquid Vapor Factor = 0.05

Capacity Parameter:

Assumed tray spacing = 18 in.

From Fig (24) of Appendix-B, sieve tray flooding capacity,
Csb(18) = 0.080 m/Sec
Surface tension of system =  = 26.3 dynes/Cm

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0.2
 
Corrected Csb = Csb(18)   = 0.084m/Sec
 20 
0.5
ρ ρ 
Now Vnf = Csb  L V  = 1.57 m/Sec
 ρV 

Maximum volumetric flow rate of vapour at bottom:

Vw
qv 
dv

= 8.25m3/sec

Net area required

qv
An  
Uc

= 6.9 m2
Total area required AT = An +Ad = 0.9 AT
An = 6.9 m2
Down comer area = Ad = 0.10 AT
π
AT = D2 = 7.7 m2
4

D=3m
Flow Parameter: (For Rectifying section)
0.5
L  ρ v 
FLV   m  
 Vm  ρ L 

FLV = Liquid Vapor Factor = 0.04

Capacity Parameter:

Assumed tray spacing = 18 in.

From Fig (24) of Appendix-B, sieve tray flooding capacity,
Csb(18) = 0.079 m/Sec

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Surface tension of system =  = 27.3 dynes/Cm

0.2
 
 
Corrected Csb = Csb(18)  20  = 0.103 m/Sec
0.5
ρ ρ 
Csb  L V 
Now Unf =  ρV  = 1.49 m/Sec

Maximum volumetric flow rate of vapour at top:

Vw
qv 
dv
= 9.88 m3/sec

Net area required

qv
An  
Uc
= 8.8 m2
Total area required AT = An +Ad = 0.9 AT
An = 8.8 m2
Down comer area = Ad = 0.10 AT
AT = π D2 /4= 9.6 m2
D = 3.3 m
Now as diameter of Striping and Rectifying section varies les than 10% so there is no
need of varying diameter of column
Tray Selection:-

Number of Tray Passes

For one pass design that the liquid flow rate does not exceed 7 to 13 gpm/in of outlet
weir .
At this preliminary point in the calculation assume that the weir length is 0.8 times the

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tower diameter

So weir length = 0.8(2.504) m = 98 inch

For bottom section

= Ln * Ma/dl * 3600
= 334 gal/min
= 334 gal/min / 98 in
= 3.41 gpm / in
For top section

= Ln * Ma/dl * 3600
= 349 gal/min
= 349 gal/min / 98 in
= 3.56 gpm/in
As both top and bottom liquid flow rates are between 7 - 13 gpm/ in so We have
selected single cross flow sieve tray with segmental down comer. For this type of tray
Other Tray Specs
Down comer area = Ad = 0.10 AT = 0.77 m2
Weir length = Lw = 0.8 DT = 2.504 m
Selected weir height hw = 1.5 in. =0.0381 m
Hole diameter = 3/16’’ = 4.75 mm 0.00475=
Assumed tray spacing = 18 in.
Tray Hydraulics

Active Area:
Aa = At-2Ad
= 6.16 m2

Hole Area:
12% of Aa
Ah = 0.12 * 6.16
= 0.74m2
Flooding checking:
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F = (Vf / Vnf)*100
Vf = qv/An
Vf = 1.19 m/sec
F = 76 %
Tray Pressure Drop

Ht =Hd + ( Hw + How ) + Hr

(a) Hw = 38 mm

(b) Dry Tray Pressure Drop

Hd = 51 (Uh/Co) 2 (rV /rL)

Hd = Dry tray drop.

Uh = Hole velocity = Qv/Ah

QV
Uh = = 8.95 m/sec
Ah

Using Fig. 11.34 of Coulson 6. We find “Co “

Co = Orifice Coefficient = 0.83
2
U   rV 
Hd = 51  h   
 CO   rL 

= 14.67 mm

(c) Weir Crest

How = 750 ( Lw/rL* Lw) 2/3

Lw = weir length

Lw = .8DT
Lw = 2.504 m

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How = 25 mm

(d) Residual Head ( Hr)


12.5  10e3 
Hr =  
 = 15.9 mm
 r L 

So,

Ht =Hd + ( Hw + How ) + Hr

= 14.67 + 38 + 25 + 15.9

= 90 m

Total Pressure Drop:

 Pt = (9.81  10e-3) Ht  r L

= 9.81  10e-3  90  787

= 690 Pa = 0.69kPa

Total Pressure drop across all Trays = 0.69  33 = 20kPa

Estimation of Weep point:

K2 - [ 0.90 - (25.4 - dh)

Uh(min) 
 ρ V  0.5

HW =38 mm

HOW = 25 mm

HW + HOW = 38+25 = 63 mm

From graph,

K2 = 30.5

Uh(min) = 3.99 m/s

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Actual Min. Vapour Velocity  Uh(min)

So there will be no Weeping.

Calculation of Entrainment

As FLV = 0.05 and F = 76%

From Figure 11.29 of coulson 6, we calculate
 = 0.043
 = Fractional Entrainment factor
Since  < 0.1, so now process is satisfactory

Total no. of holes

 Ah 
Total no. of holes = 
 ah 

dh = 4.762 mm
ah = (3.14  .004762)/ 4 = 1.77  10-4 m2
Total no. of holes = 0.7392/1.77  10-4 = 4176

Pitch calculation

At lw / Dc = 0.8, graph b/w angle subtended by chord & chord length:

θc = 108°
Angle subtended at plate edge by unperforated edge strip = 180 – 108= 72°

Length of unperforated edge strips = (D– hw)  *72 / 180

= 3.9 m
Area of unperforated edge strip =Au = hw*3.9

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= 0.15 m2
Area of calming zone = Acz = 2*hw*(lw-2*hw)
= 0.18 m2
Total area available for perforations = Ap = Aa – (Au + Acz)
= 5.83 m2
K = 0.905 for Equilateral Triangular Pitch
So
0.7392/5.83 = 0.905(0.0047/hole pitch)2
Hole Pitch = 0.01256 m
Check
Pitch to Hole Diameter ratio = 0.01256/0.00476
= 2.63
( Correct )it should between 2 and 4
So our selection of equilateral triangular pitch is right.
Downcomer Liquid backup/ liquid height in downcomer:
Let, hap= hw-10
= 38.1 mm = 0.015m
Area under apron = hap*lw
Aap = 0.015*
= 0.037 m2
As Aap is less than Ad = 0.59m2
2
 Lw 
h dc  166   
 d l  Aap 
 
=10.82 mm
H D  H t  H dc  (ho  how )

=113.89 mm=0.11 m
Since,
HD < 0.5*(Tray spacing +Weir height)
0.11 < 0.375
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So, tray spacing is acceptable.

Residence Time:
Ad  hbc  d l
tr 
Lw

= 13 sec
As residence time is greater than 3 sec, so satisfactory.

Height of Distillation Column

No. of plates = 33
Tray spacing = 0.4572 m
Distance between 33 plates = 0.4572  33 = 13 m
Top clearance = 0.5 m
Bottom clearance = 0.5 m
Tray thickness = 4.75 mm/plate
Total thickness of trays = 0.00475  33 = 0.15675 m
Total height of column = 13 + 0.5 + 0.5 + 0.15675 = 14 m

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9.8 NOMENCLATURE OF DISTILLATION COLUMN

Aa = Active area (m2)

Ad = down comer area (m2)
Ah = hole area (m2)
An = Net area (m2)
Ada = area under down comer apron (m2)
C = corrosion allowance (in/year)
Csb(20) = capacity parameter for liquids ( = 20 dynes/cm)
Csb = Capacity parameter of liquid
D = Diameter of tower (m)
Df = flow width normal to liquid flow (m)
Dh = hole diameter (m)
e = total entrainment (Kg/sec)
F = feed (Kgmol/hr)
F* = Design % loading
HF = Enthalpy of feed (J/Kgmol K)
HB(l) = Enthalpy of bottom (J/Kgmol K)
HD(L) = Enthlpy of the distillate (J/Kgmol K)
ha = head loss due to created liquid (cm)
hf = froth height on tray (cm)
had = had loss due to down comer apron (cm)
hdc = height of clear liquid in down comer (cm)
hw = weir height (cm)
how = height of liquid crest over weir (cm)
ho = head loss due to bubble formation (cm)
J = weld efficiency factor
L = liquid flow rate (Kg/hr)
Lw = weir length (m)

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Nm = min. no. of plates

Pdry = dry pressure drop (cm)
PT = total pressure drop (cm)
QL = Liquid flow rate (Kg/m3)
Qv = Vapour flow rate (Kg/ m3)
Qc = condenser duty (J/ m3)
QR = Rebotr duty (J/hr)
QP = Areatio factor
Rh = Hydraluic radius of aerated mass (m)
Reh = Modified Reynold No.
Rm = Min. reflux ration
R = operational reflux ratio
Tm = thickness of shell (mm)
Uh = vapour velocity through holes (m/sec)
Vm = vapour flow rate at bottom (Kgmol/hr)
WF = mass flow rate of feed (Kgmol/hr)
WB(r) = bottoms (Kg/hr)
W D(r) = mass flow rate distillate (Kg/hr)
Unf = flooding velocity based upon net area (m/sec)
Vd = down comer liquid velocity (m/sec)
 = relative volatility
rL = density of liquid (Kg/m3)
rv = density of vapor (Kg/m3)
average = average viscosity of feed (Cp)
 = fractional entrainment factor
 = relative froth density
 = surface tension (J/N2)
 = liquid gradient

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9.9 SPECIFICATION SHEET:

Identification
Item Distillation Column
Item # D-108
Type Sieve Tray
No. of item 3
Function
The separation of Acrylonitrile
Design data
No. of trays 33
Operating Pressure 132 kPa
Operating Temperature 98 oC
Tray spacing 0.45m
Tray thickness 4.75 mm
Height 14 m
Diameter 3m
Reflux ratio 3.25
Hole size and Arrangement 4.75mm equilateral triangular pitch
Liquid density 787 Kg/m3
Vapor density 1.71 Kg/m3
Material of Construction Stainless stell 18Cr/8Ni Ti stabilized

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