(8.3) Distillation Column

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Design of Distillation Column


Distillation:
In process industries , it is often desired to separate the components of liquid mixture . the
easiest way is to carry out this separation is by distillation .this unit operation makes use of the
difference in the boiling or the relative volatilities of the components. Distillation is considered
to be the preferred separation technique if the relative volatility difference between the two key
components (that are required to be separate from each other ) is greater than 1.2

Selection of the Distillation Column:


Batch and Continuous Columns.
Distillation columns may be batch or continuous, based on the feed is introduced.
In batch columns, a batch of feed is charged and operating carried out till the desired degree of
separation is achieved. The material removed and the next batch is charged. These columns are
suitable for very low throuputs and for system where very high purity is required. Continuous
columns process continuous feed streams. The are widely used in industries for high throuputs.
Here we are concerned with the later type of operation.

Vacuum Distillation Column


I have selected the continuous vacuum distillation column because.

For heat sensitive material (gasoline)


Relative volatility of components is increased
To avoid thermal decomposition of A.G.O (T<350C)
Energy economical process.

Selection of Vacuum System:


Steam jet ejector

Vacuum pumps

Simple design , with no moving parts and


practically no wear.
Lowest capital cost among vacuum
producing devices.

High power requirement.


Low operating cost but high capital
investment .

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Simple repair and maintenance


Offers the largest throuput capacity of any
vacuum producing devices,
Can handle more than 1000,000 ft3 /min of
process fluid.
Preferred when steam is available.

Hard to repair and maintain.


Capacity range varies depending upon type
of pump.
Can handle overload in capacity at the cost
of power

Several devices are available for producing vacuum at a chemical process plant. Each has its own
advantages and disadvantages , among these ejectors are workhorses. The simples and probably
most widely used vacuum producer is the steam jet ejector.

Ejectors Offer a Range of Attraction:

Simply design with no moving parts and particularly no wear.


Can be mounted in any orientation
Can be fabricated of virtually any metal
No special start up or shut down procedure required
Can handle condensable loads and corrosive vapors
Simple repair and maintenance .

Steam Jet Ejector:


Steam jet ejectors are designed to convert the pressure energy of a motivating fluid to a
velocity energy to entrain suction fluid ant then to recompress the mixed fluid by converting
velocity energy back in to the pressure energy. This is based on the theory that a properly
designed nozzle followed by a properly designed throat or venture will make economically make
use of high pressure fluid to compress from a low pressure region to a high pressure. This change
from pressure head to velocity head is the basis of the jet vacuum principle.

Ejectors Range:
Ejectors range from single stage up to six stage units, and can be either condensing or noncondensing types. The numbers of ejector stages required are usually determined by the economy
of the ejectors and the level of vacuum required. Vacuum ranges for each stage are as follows.:
1st stage
2nd stage
3rd stage
4th stage
5th stage
6th stage

810mmHgA-30mmHgA
130mmHgA-3mmHgA
25mmHgA-0.8mmHgA
4 mmHgA-75microns Hg A
0.4 mmHgA-10 microns HgA
0.1 mmHgA-3 microns HgA

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Fig .
8.1

Fig .
8.2

Ejector Performance Curve:


This curve is used to find out the required water or steam flow rate to create the desired suction
pressure in the upstream of the motive fluid.

Tray and Packed Column:


The performance of a distillation column depends upon the intimate contact of liquid
and vapor steams. Two configurations are widely used in this respect. These are the plate and the
packed columns. A general comparison of the two configuration is made below.
1. Packed columns are continuous contacting units. On the other hand , vapor liquid contact
in a tray column occurs only at discrete location i.e., on the trays.

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2. The liquid and vapor streams never reach equilibrium in a packed column. In a tray
column, the steams leaving any stage are assumed to be in the equilibrium.
3. Packed columns can operate over a relatively wide range of vapor flow rates. On the
other hand , plated columns offer wide operating range with respect to the liquid flow
rates.
4. Packed columns cannot work efficiently under stressed condition of temperature and
pressure.
5. Liquid distribution can be a problem in packed columns and cause channeling.
6. For diameters less than about 0.6 m , a plate column cannot be constructed. Therefore a
packed column has to be used.
7. Design information for plate column is more readily available and more reliable.
8. If the system contains solid contents, a plated column is preferred. The solids can
accumulate in the voids of the packing and choke them .
9. For large column heights, weight of the plate column is much smaller as compared to that
of a packed column.
10. For cleaning of packed column, packing must be removed.

In petroleum refining , the distillation columns are plate columns. This selection has
the following aspects.
1. The distillation columns in petroleum refining are complex columns. Actually , they are
fractionators , and multiple products are obtained from a single column as side streams .
the side streams are often steam-stripped to meet the flash point specification and the
overlapping standards of two fractions. The resultant vapor streams are again introduced
in to the column. Hence , a distillation column in a petroleum refinery has a number of
streams going into and out of the system. These inlets and outlets are easy to locate at
discrete points in a tray column, but difficult for a packed column.
2. Because of the multiple inlet and outlet streams, the liquid and vapor flow rated widely
very inside the column. A packed column is not suitable for such a condition.
3. To avoid problems like flooding and entrainment because of the variable liquid and vapor
flow rated , inter stage cooling or heating is often required. Sometimes, pump-arrounds
are also used for this purpose. this provision can only be made in a plate column.
Keeping in mind the above factors, the column selected for the current design is a plate
column.

Tray Selection:

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Three basic types of trays are used in plate columns. These are sieve trays, bubble cap
trays, and valve trays. The trays selected for the column are sieve trays. The supporting
factors are.
1. They are light weight and the cheapest available, and easiest to fabricated and install.
2. They have higher capacity and lower pressure drop than other tray types
3. Sufficient design data is available
4. The maintenance cost is lower because of the ease of cleaning.

Fig
-8.3

Component Of Distillation Column:


Major components of distillation system are.

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1. The distillation column itself , as a tray or packed column where the vapor and liquid
streams are brought in contact with each other, and the separation occurs.
2. A reboiler to provide the heat required for vaporization.
3. A condenser to remove the heat from the system and condenses the vapors leaving from
top of the column.
4. A reflux drum to hold the condensed liquid after the separator and provide continuous
liquid reflux to the column.

Design Of Distillation Column:


The design steps for a column design are:

Calculation of Minimum number of stages. Nmin

Calculation of Minimum Reflux Ratio Rm.

Calculation of Actual Reflux Ratio.

Calculation of theoretical number of stages.

Calculation of actual number of stages.

Calculation of diameter of the column.

Calculation of weeping point, entrainment, etc

Calculation of pressure drop.

Calculation of the height of the column.

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Fig
8.4

From Material Balance We Have:


Component

Feed
Fraction
xf

(table- 8.1)
Bottom

Top

Fraction

Fraction

xb

xd

C1,C2

.039

.0001

C3

.042

.0089

I-C4

.048

.032

N-C4

.047

.0238

Gasoline

.313

.439

Napthta (LK)

.326

.058

.455

Atm gas oil(HK)

.186

.942

.0013

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Water

92

.04

Selection Of Key On The Basis Of Relative Volatility.


C1,C2

= lighter than lighter key

C3

= lighter than lighter key

i-C4

= lighter than light key

n-C4

= lighter than light key

gasoline = lighter than light key


naphtha = light key
unconverted. A.G.O = heavy key

Nature Of Feed:
Feed is entering in column as a saturated liquid at T=1050C and P=305kpa
Components
C1,C2
C3
i-C4
n-C4
Gasoline
Naphtha
U.A.G.O

Xf

Ki
0.039
0.042
0.048
0.047
0.313
0.326
0.186

Table

Ki*Xf
60
13
6
5
1.07
0.111
1.315 E-5

0.115648
0.321437
0.340852
0.208026
0.33628
0.042272
2.42E-06

By bubble point Xf*Ki=1.10; it is verified that feed is entering at saturated liquid. ref: (col V6
page 498.)

Estimation Of Top Temperature:


By dew point calculation , (Ki/Xd)=1
T=90

P=13 kpa

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Components
C1,C2
C3
i-C4
n-C4
Gasoline
Naphtha
U.A.G.O
Water

93

Xd

Ki

Ki/Xd

.0001
.0089
.032
.0238
.439
.455
.0013
.04

147.5
32
18
17
22.1923
2.2077
0.0014

1.62E-05
9.59E-04
3.92E-03
3.04E-03
1.75E-02
2.06E-01
8.25E-01
0.25E-02

15
Table

Hence by dew point calculation (Ki/Xd)=1.2 app . it is verified the top temperature

Estimation Of Bottom Temperature:


By bubble point calculation Xw*Ki=1
Components
Naphtha
Un.A.G.O

T=200C and P=30 kpa

Xw
0.058
0.942

Ki

Xw*Ki
13.025
0.094866667

Table8.4

0.8597041
0.0893334

Hence by bubble point calculations the bottom temperature is verified. Xw*Ki=0.8912

Calculation Of Minimum Number Of Stages:


The minimum no. of stages Nmin is obtained from Fenske relation which is
Nmin + 1 =

ln[(xLK/xHK)D/(xLK /xHK)B]
ln (LK/HK) average

To find average geometric relative volatility of light key to heavy key:

Lk / Hk avg Lk / Hk D Lk / Hk B 0.5
Lk / Hk
Lk / Hk
so

1 .5

5.3

Average geometric relative volatility = 3.01

Nmin +1=8.77/1.12
Nmin = 7

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Calculation Of Minimum Reflux Ratio rm


Using Underwood equation
As feed is entering as saturated liquid so,
q=1
= 1.225

By

trial,

(root of equation)

Using

equation of minimum reflux ratio

Putting all values we get,


Rm = 0.3

Actual Reflux Ratio:


The rule of thumb is
R = (1.2---------1.7)Rmin
R = 1.7 Rmin
R = 0.5

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

0.75 1 R Rmin

N 1
R

Nmin = 6

N N min

Rmin = 0.3
R(actual)= 0.5

0.566

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From which the theoretical no of stages to be


N= 15

Calculation of Actual Number of Stages:


Overall Tray Efficiency: (OConnells equation)


Eo 51 32.5 log avg . avg

ref: Coulson V6 page 550


avg =average relative volatility of light key component =3.01
avg = molar average liquid viscosity of feed evaluated at average temperature of column
Average temperature of column = (200+90)/2 = 145 oC
Feed viscosity at average temperature = avg =0.0057 mNs/m2
So

Eo = 54.0%

Then,
No. of actual trays = 15/0.54 = 28
Total # of actual trays=28+1=29

Calculation Of Feed Plate:


The Kirk bride method is used to determine the ratio of trays above and below the feed point.

ref Coulson V6 page 526


where Nr = number of stages above the feed, including any partial condenser,
Ns = number of stages below the feed, including the reboiler,
B = molar flow bottom product,
D = molar flow top product,
xf,HK = concentration of the heavy key in the feed,
xf,LK = concentration of the light key in the feed,
xd,HK = concentration of the heavy key in the top product,

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

XLk(f)=.38

B=345.5kmol/hr

XLk(B)=.058

D=1209kmol/hr

XHk(B)=.0013
XHk(f)=.184
From which,
Number of Plates above the feed tray=Nr = ND = 10
Number of Plates below the feed tray=Ns = NB = 19
So feed is entering at plate 11 from top

Top And Bottom Condition


Top conditions
Ln=604kmol/hr
Ln=Lm=58769.9kg/hr
Vn=Ln+D=1813kmole/hr
Vn=Vm=176405kg/hr
T=90C=364K
,P=13kpa
v(top)=5.77kg/m3
L(top)=601.6kg/m3
M.w=97.3kg/kmole

Bottom conditions
Lw=Ln+F=2382kmole/hr
Vw=Lw-W=2036.35kmole/hr
Lm=Lw=284562kg/hr
Vm=Vw=196805kg/hr
T=200C=473K ,P=30kps
v(bottom)=5.68kg/m3
L(bottom)=756.6kg/m3
M.W=119kg/kmole
Table 8.5

Determination Of The Column Diameter:


Flow Parameter:
FLV

L
n
Vn

v

L

0.5

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Lm=Ln=284562kg/hr
Vm=Vn=196805kg/hr
v=5.68kg/m3
L=756.5kg/m3
FLV = Liquid Vapor Factor = 1.25
Assumed tray spacing = 35 inch (0.91 m)
Net vapor velocity at flooding.

From Fig (11.27) Coulson and Richardson vol-6, sieve tray


K1 = 0.03(/.02)0.5
Surface tension of Mixture = = 2.5*10-3 N/m
K1=0.062
v=5.68kg/m3
L= 756.5kg/m3
uf=Vnf=.062*11.4= 0.706 m/sec
Assume 80% of flooding then
vn= 0.8Vnf
So, actual vapor velocity,
vn= 0.565 m/sec
Net column area used in separation is
An = Qv/vn
Volumetric flow rate of vapors = Qv
QV

Vm
V 3600

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Qv=196805/(5.68*3600)= 9.6m3/s
Now, net area = Qv/vn = 17m2
Assume that down comer occupies 15% of cross sectional Area (Ac) of column thus:
Ac = An + Ad
Where, Ad = down comer area
Ac = An + 0.15(Ac)
Ac = An / 0.85
Ac=20 m2
So Diameter of Column Is
Ac =(/4)D2

Dc =

4 Ac

Dc = 5meter = 16ft
(based upon bottom conditions)
in the similar way we calculate the top diameter which come out to be 4.43m.so we will
decrease the perforated area for uniform diameter of 5m

Provisional Plate Design :


Column Diameter Dc= 5 m
Column Cross-sectional Area(Ac) = 20 m2
Down comer area Ad = 0.15Ac =3 m2
Net Area (An) = Ac - Ad =17 m2

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Active area Aa=Ac-2Ad = 14 m2


Hole area Ah take 10% Aa = 0.1 14
=1.4 m2
To find Weir length
Ad / Ac = 3 / 20 = 0.15
From figure 11.31 Coulson & Richardson 6th volume 4th edition page 573
Lw / dc = 0.80
Lw = 5*0.80
Iw=Lw = 4 m
Weir length should be 60 to 85% of column diameter which is satisfactory
Take weir height, hw= 25 mm (25mm-75mm)
Hole diameter, dh = 5 mm

(5mm-25mm)

Plate thickness = 5 mm

Check Weeping:

where uh = minimum vapour velocity through the holes(based on the hole area), m/s,
dh = hole diameter, mm,
K2 = a constant, dependent on the depth of clear liquid on the plate

The vapor velocity at weeping point is the minimum velocity for the stable operation.
In order to have K2 value from fig11.30 Coulson & Richardson 6th volume 4th edition we
have to 1st find how(depth of the crest of liquid over the weir)
where how is calculated by following formula:
how=750{[Lm/lw*l]2/3}
Maximum liquid rate Lm= 284562/3600=79 kg/sec
Minimum Liquid Rate At 80% turn down ratio

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= 63.2Kg/sec
Iw=4m
l=756kg/m3
At Maximum rate ( how)= 63 mm Liquid
At Minimum rate (how) = 54.6 mm Liquid
hw + how = 25 + 54.6 = 79 mm Liquid
from fig 11.30, Coulson and Richardson Vol.6
K2 = 28
So, putting the value for Umin we will have.
U (min) = 3.5 m/sec
Now maximum volumetric flow rate (vapors) Base = 9.6 m3/sec
Ah=1.4m2
At 80% turn down ratio
Actual minimum vapor velocity

Fig
8.5

= minimum vapor rate / Ah


= 5.5 m/sec
So minimum vapor rate will be well above the weep point.
Now we well calculate the pressure drop (P.D)

Plate Pressure Drop (P.D):


Consist of dry plate P.D (orifice loss), P.D due to static head of liquid and residual P.D (bubbles
formation result in energy loss + froth formed in operating plates)
ht=hd+(hw+how)+hr

Dry Plate Drop (hd):

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Max. Vapor velocity through holes (Uh) =


Maximum Volumetric Flow Rate / Hole Area=
9.6/1.4= 6.8 m/sec
Perforated area Ap (active area) =14 m2
Ah/Ap = 0.100
From fig. 11.34 (Coulson & Richardson 6th volume
4th edition) for
plate thickness/hole diameter = 1.00
We get,

Co = 0.84
hd = 25 mm Liquid

Residual Head (hr):


hr = (12.5*103 / L)

L =756kg/m3

so hr = 16.5 mm Liquid

Fig
-8.6

Total Pressure Drop


ht=25+(25+54)+16.5
ht = 131.35 mm liquid
Total column pressure drop Pa, (N/m2)
P = (9.81*10-3) htL = 890Pa = 0.890 kPa=0.1psi
And allowable p.d is 0.1 psi per tray.

Down Comer Liquid Backup :


Caused by P.D over the plate and resistance to flow in the down comer itself.

hb = (hw+ how) + ht + hdc


The main resistance to flow in down comer will be caused by constriction in the down comer
outlet, and head loss in the down comer can be estimated using the equation given as,

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where Lwd is the liquid flow rate in down comer, kg/sec(79kg/sec)


l=765.5 kg/m3
and Aap is the clearance area under the down comer, m2
Aap =hap* Lw
Where hap the height of bottom edge of apron above the plate.
hap = hw (5 to 10 mm)
hap = 20 mm
so,
Area under apron Aap = (20/1000)*4 = 0.085
As this is less than area of down comer Ad (3m2)so using Aap values in above formula for hdc
So,
hdc = 205mm
As a result,
hb = (hw+how)+ht+hdc
= 404 mm=0.404
hb < (Tray spacing + weir height)

that is

0.404 < 0.467

So tray spacing is acceptable

Check Residence Time:


Sufficient residence time should be allowed in the down comer for the entrained vapors to
disengage from liquid stream to prevent aerated liquid being carried under the down comer.
tr =Ad hbc L/L(max)
Ad=3m2

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hbc=0.404m
l=756kg/m3
Lmax=79kg/sec
tr = 12 sec
It should be > 3 sec. so, result is satisfactory

Check Entrainment:
(un) actual velocity (based on net area) = (max volumetric flow rate at base Vm / net area An)
un=9.6/17=0.565m/sec
(un) actual velocity = 0.565 m/sec
Velocity at flooding condition Uf = 0.706 m/sec
So Percent flooding =un/ uf = 0.80 = 80%
Liquid flow factor FLV = 1.25
From fig. 11.29 Coulson & Richardson 6th volume 3rd edition
fractional entrainment can be found out.
Fractional entrainment () factor = 0.0025
Well below the upper limit of () which is 0.1. Below this the effect of entrainment on
efficiency is small.

No. Of holes.
Area of 1 Hole=ah = (/4) Dhole2
= 0.00002 m2
Area of N Holes =Ah= 1.4 m2
So,
Number OF Holes=Ah/ah = 7000

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Height of distillation column:


Height of column Hc= (Nact-1) Hs+ H+ plates thickness
No. of plates = 29
Tray spacing Hs = 0.90 m
H=top clearance + bottom clearance.
H=1.5+1.5 m
Total thickness of trays = 0.005*29 = 0.34 m
So,
Height of column = (29-1)*0.90+ 3+0.34
= 29 meters

Fig 8.7

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Specification sheet
Identification:
Item
No. required:
Tray type:

vacuum Distillation column


1
Sieve tray

Function:
separation of gasoline and
Operation:

naphtha from unconverted A..G.O


Continuous

Table 8.6
No. of tray= 29

Active holes = 7000

Pressure = 15Kpa

Weir height = 25 mm

Height of column = 29 m

Weir length = 4 m

Diameter of column=5m

Reflux ratio = 0.5

Pressure drop per


tray=0.899Kpa=0.1psi

Tray spacing =0.91 m

Hole size = 5mm

Active area = 14 m2

Tray thickness = 5 mm

Flooding Percent =80 %

Entrainment = 0.025 %

Residence time=12 sec

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