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DISTILLATION POINTS TO REMEMBER

1. Dis tillation columns carry out phys ical s eparation of liquid chemical components from a
mixture by
a. A combination of trans fer of he at energy (to vaporize lighte r components)
b. Mas s trans fe r betwee n the liquid and vapor phas es .
2. Simple Rules of Vapor Liquid Equilibrium
a. Vapor pre s sure of liquid depends on temperature.
b. Heat input rais e s vapor pres s ure of liquid.
c. A liquid boils whe n its vapor pres s ure equals the s ys tem pres s ure.
d. Higher the vapor pre s s ure lowe rs the boiling point.
e. Volatile liquids have high vapor pres s ure.
f. The vapor pres s ure and hence the boiling point of a liquid mixture depends on the
relative amounts of the compone nts in the mixture.
3. Dis tillation is the mos t common s eparation technique. Dis tillation is energy intens ive
proces s. It has large he ating and cooling load. It can contribute to 30-60% of plant
operating cos ts
4.
a. Fractionation is a unit that has both a re boiler to supply heat at the bottom and a
condens er to take heat out from the top. This is normally calle d dis tillation.
b. Abs orption is a unit that has no method at the top of the tower to take heat out. An
exte rnal liquid is s upplied from outs ide the s ys tem to abs orb material from the
vapor.
c. Stripping is a unit that has an exte rnal s tream (gas or s te am) s upplied from
outs ide the sys tem to s trip light mate rial from the liquid. It may have a re boiler at
the bottom of the towe r to put heat in.
5. In oil and gas proces s ing s harp s eparation of a product of high purity is not so common.
Example LPG is not a pure compone nt.
6. The equilibrium compos itions of the components in a liquid mixture vary with
temperature at a fixed pres sure. Whe n a liquid with mole fraction of A=0.4 (point A) is
heated, its concentration remains cons tant until it reaches the bubble-point (point B). It
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starts to boil. The vapors evolve d during the boiling has the
equilibrium compos ition given by point C.
7. Relative Volatility of component 1 and 2 in a mixture is
given by- Relative Volatility = [y1/x1] / [y2/x2] , Where -y
is the compos ition in vapor phas e and x is the compone nt in
liquid phas e at a particular press ure and temperature .
8. A typical dis tillation major components and bas ic ope ration
a. A re boiler to provide the neces s ary he at of
vaporization for the distillation proce s s .
b. A condens er to cool and conde ns e the vapor le aving the top of the column.
c. A reflux drums to hold the conde ns ed vapor from the top of the column s o that
liquid (reflux) can be re cycled back to the column to e nhance clos e s e paration.
d. The fe e d is introduced us ually somewhere near the middle of the column to a tray
known as the fe e d tray.
e. The fe e d tray divides the column into a top (e nriching or re ctification) s e ction and
a bottom (s tripping) s ection.
f. The liquid (from fe ed and conde nsing vapors on the re ctification s ection) fe e d
flows down the column.
g. Heat is s upplie d to the re-boiler to generate vapor.The liquid remove d from the
re boiler is known as the bottoms product or simply, bottoms .
h. The vapor moves up the column, and as it exits the top of the unit, it is coole d by
a conde ns e r.
i. The conde ns e d liquid is
collecte d in a ve s s e l known
as the reflux drum. Some of
this liquid is recycled back to
the top of the column and this
is calle d the reflux.
j. Part of the condens ed liquid
is removed from the reflux
drum (or from one of the
trays ) s ys te m is known as the
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dis tillate or top product.
k. Thus the dis tillate and the bottoms become the final products . For multi-
component dis tillation.
l. Certain products can be drawn from one of the trays and is calle d s ide draw off.
m. Each tray attains a e quilibrium tempe rature. A temperature profile takes place
along the dis tillation column, the highes t being at the bottom and the lowes t being
at the top.
9. Packed Column Vs Tray Column
Packed Column
Low pre ss ure drop
Good for vacuum s ervice
Le s s fle xibility for s ide draws
Good for corrosive s ervice
Ide al for small diameter
Not preferre d for high pres s ure
Not use d for Res ide nce time limitations
Us ually avoide d for low Liquid loading
Can handle very large liquid load
Requires s maller diameter column
Tray Column
High pre ss ure Drop
Not recomme nded for high vacuum service
Flexible for s ide draw
Expens ive for corros ive s ervice
Expens ive for s mall diameter
Good at high press ure
Good when high Residence time re quired
Good for low liquid loading
Cannot handle ve ry large liquid load
Requires larger diameter column
10. Dis tillation Calculation Methods
a. Stre am Specifications
b. Fe e d S pecifications (Temp, Pres s ure and Composition)
c. Variation in fe ed s pecifications .
d. Top product s pecification
e. Bottom product s pe cification
f. Side draw s pecification
g. Provide des ign margin while making calculation
h. Es timate the re covery re quire d
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11. Feed Condition
The thermal condition of the fee d determines the column internal flows .
a. If the fee d is below its bubble point, he at is ne eded to rais e it to where it can be
vaporize d. This he at must be obtained by conde nsing vapor ris ing through the
column, s o the liquid flow moving down the column increas e s by the e ntire amount
of the fe ed plus the conde ns e d material and the vapor flow upward is decreas e d.
Sub cooled Liquid - q>1 i.e. q=1+cp
L
(T
bp
-T
f
)/lambda
b. If the fee d e nters as s upe rheate d vapor, it will vaporize s ome of the liquid to
e qualize the enthalpy. In this cas e , the liquid flow down the column drops and the
vapor flow up is increas ed by the entire amount of the fee d plus the vaporized
material. Superheated Vapor - q<0, q=(-cp
V
*(T
f
-T
dp
)/lambda).
c. If the fee d is s aturated (liquid or vapor), no additional heat must be adde d or
s ubtracte d, and the fe ed adds dire ctly to the liquid or vapor flow.
i. Saturated Liquid (bubble point fee d), q=1
ii. Partially Vaporized 0 < q < 1, q is the fraction of the fee d that is liquid. It
can be found by doing a flas h calculation and the n q=(L/F)=(1-V/F)
iii. Saturated Vapor (dew point fee d), q=0
12. Thermodynamic Method
The s election of thermodynamic method is one of the most critical de cis ion a proces s
e ngineer makes in des ign. Ge neral guidelines are given in the s oftware. However, this is
not ade quate. Proce s s e ngineer mus t develop s kill in s ele cting thermodynamics method.
The following may be us e d as a guide line:
a. Us e S-R-K or P-R methods for mos t hydrocarbon s ervice. The improved
methods als o may be us e d. Both the methods are good for high pres s ure als o.
b. The s oftware may have inte raction parameters for methods like Wilson, NRTL,
Margules , etc. You may us e this for non-ideal s e rvices .
c. If experimental x-y data are available at one or more conditions, the data can be
re gres s ed us ing the mos t s uitable thermodynamic model.
d. For vacuum s ervices , vapor pres s ure (ideal) mode l can be cons idere d.
e. Us e s pecial methods for the given application s uch as Amines or Sour Water etc.
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13. Es timate us ing Short-cut methods
Fens ke-Underwood-Gillliland (FUG) Shortcut Method / Smith-Brinkley Method
a. Operating Pres s ure for Column - In ge neral lower the operating pres s ure, eas ie r
the s eparation. Howe ver, lower the pre s s ure, larger the column s ize. S ele ct
optimum pres s ure bas e d on expected temperature, utilitie s available, product
degradation, refrigeration re quirement etc.
b. Pres sure Drop - Initial e s timate on pre s sure drop may be done bas ed on 70 mm
water column for pres s ure drop in e ach tray and 40 mm water column per mete r
of packe d height for random packing.
c. Bas ed on the given fee d and product s pecifications , es timated re covery and K-
model s election, us e s hort-cut methods to calculate the following:
i. Minimum Reflux Ratio Underwoods Equation
ii. Minimum number of theoretical trays Fe ns kes Total Reflux Equation
iii. Reflux ratio Vs No. of trays Gilliland Empirical Correlation
iv. Ideal Fee d Location -
v. Expe cted temperature and duty.
vi. Bas ed on s hort-cut method, s elect the number of trays required, reflux
ratio and fee d tray location. This is the firs t es timate for rigorous method.
14. Rigorous Calculation Method
a. Sele ct the column operating pre ss ure at the top
b. Specify pres s ure drop for the conde ns er, may be 0.05 to 0.3 Kg/cm2, depending
on s ervice .
c. Sele ct number theoretical trays and fe ed location bas e d on res ults of s hort cut
method.
d. Spe cify minimum s pecification as per programme requirements . This include
re flux ratio and reflux rate, product purity, re boile r duty, top temperature, bottom
temperature etc.
e. For fas t conversion of column, s pecify product rate, reflux rate, re boiler duty etc.
f. Spe cify e s timated quantitie s of othe r paramete rs , if known.
g. Deve lop one precis e calculation.
h. Fine tune (optimize) on reflux ratio and fe ed-tray location.
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i. The numbe r of trays s elected from s hort-cut method may not be optimum.
There fore, develop few cas es with different number of trays .
j. Bas ed on all the s e cas es , s ele ct the cas e which s eems to be the optimum.
k. The theoretical number of trays can be converted to actual number of trays bas ed
on tray efficiency or can be converted to e quivale nt packe d he ight bas e d on HETP
value.
15. Tray Efficiency
a. Tray e fficiency vary from 30% to 100%, but mos t hydrocarbon s ervice, it is in the
range of 60% to 80%.
b. Various co-relations are cited in literature for calculating efficie ncy. However,
they are not very reliable.
c. In-hous e data bank, tray ve ndor information and publis hed experimental
information is more reliable for tray efficie ncy
16. HETP
a. HETP (Height Equivalent to a Theoretical Plate) values are us e d for calculating
total packe d height from the number of trays calculate d us ing s imulator.
b. HETP value is calculated bas e d on experience and vendor information.
c. While calculating the HETP, the liquid distribution for each be d plays a major role.
d. The typical value of HETP for mos t random packing is 300 mm to 800 mm. The
corre s ponding value for s tructural packing is s ome what lowe r. Smaller the
packing, lower the HETP value
e. The total packed height is divide d into number of be ds. Each be d may have
height equivale nt to 6 to 15 theoretical trays for random packing.
f. H/D Ratio for a random packed be d is limite d to 8. Ofte n bed height is res tricted
to 6 m. Higher packed height per be d is permitte d for s tructure packing.
17. Column Diameter and Height Calculation
a. Tray Column
i. Calculate total number of trays re quire d
ii. Calculate column diamete r bas ed on vapor and liquid flow rates . Preliminary
calculations can be done us ing simulator. Tray vendor will give accurate
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data. Tray diameter calculation de pends on tray s pacing. Therefore, s ome
optimization calculation may be required.
iii. Tray s pacing varies from 250 mm to 750 mm. Mos t hydrocarbon s ervice s
us e tray s pacing of 450 mm to
600 mm.
iv. Provide s pace of about 800 mm
to 1000 mm at the top of 1s t
tray for man-way.
v. Provide liquid le vel at column
bottom bas e d on res idence
time re quired. Note that liquid
dis appears due to bottom
product removal and due to vaporization
vi. Provide ade quate s pace betwee n HHLL and the las t tray for proper
s e paration of vapor and liquid.
vii. Column hydraulics s hall be s uch that normal operation is away from
e ntrainment, flooding, choking etc. Vapor flow velocity is de pende nt on
column diamete r. We eping determines the minimum vapor flow required
while flooding determine s the maximum vapor flow allowe d, he nce column
capacity. Thus , if the column diamete r is not s ized prope rly, the column will
not perform well. Not only will operational problems occur, the de sired
s e paration duties may not be achie ve d.
b. Packe d Column
i. Calculate HETP as des cribe d above. This includes s ele cting s ize of the
packing.
ii. Calculate total packed height above and be low the fe ed location.
iii. Divide the total packed height into number of beds s uch that each bed has
about 10 theoretical s tage s .
iv. Calculate column diameter us ing s imulator bas e d on hydraulics data and
packing s electe d. Specify pres s ure drop in the range of 25 mm wate r
column to 40 mm water column per meter of packe d height. This is finalized
after discus s ion with packing ve ndor.
v. Calculate overall column dimens ions as des cribed for tray column.
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18. Internals
a. Tray Column
i. Trays
ii. Chimney Tray
iii. Fee d Pipes
iv. Gas Dis tributor
v. Partition Plate
b. Packe d Column
i. Packing
ii. Distributor / Re distributors
iii. Support Plate
iv. Hold drum plate / be d limiters
v. Fee d Pipe
vi. Gas Dis tributor
19. Factors Affecting Distillation Column Operation / Performance
The performance of a dis tillation column is
determine d by many factors , for example:
a. Fee d Conditions
The s tate of the fe e d mixture and fe ed
composition affects the operating line s and
he nce the number of stages re quired for
s e paration. It als o affects the location of
fee d tray. During ope ration, if the deviations
from des ign s pecifications are exce s sive ,
the n the column may no longe r be able
handle the s e paration tas k. To overcome
the problems as s ociated with the fe ed, s ome column are de signed to have multiple
fee d points whe n the fee d is expe cted to containing varying amounts of components .
b. Reflux Conditions
As the reflux ratio is increas ed, the gradient of operating line for the rectification
s ection moves towards a maximum value of 1. Phys ically, what this me ans is that
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more and more liquid that is rich in the more volatile compone nts are being recycled
back into the column. Se paration then be come s better and thus le s s trays are nee ded
to achie ve the s ame de gre e of s e paration. Minimum trays are re quire d under total
re flux conditions, i.e. there is no withdrawal of dis tillate.
On the other hand, as reflux is decreas ed, the operating line for the rectification
s ection move s towards the equilibrium line. The pinch betwe en ope rating and
equilibrium line s becomes more pronounce d and more and more trays are re quire d.
This is e as y to verify us ing the McCabe-Thiele method. The limiting condition occurs
at minimum re flux ration, whe n an infinite number of trays will be re quire d to effect
s e paration. Mos t columns are de signed to ope rate betwee n 1.2 to 1.5 times the
minimum reflux ratio becaus e this is approximately the region of minimum operating
costs (more reflux me ans higher reboiler duty).
c. State of Trays and Packings
Remembe r that the actual number of trays re quire d for a particular s e paration duty is
determine d by the efficiency of the plate, and the packings if packings are us ed. Thus,
any factors that caus e a decre as e in tray efficiency will also change the performance
of the column. Tray efficiencies are affecte d by fouling, wear and tear and corros ion,
and the rates at which thes e occur depends on the propertie s of the liquids being
proce s s e d. Thus appropriate mate rials s hould be s pe cifie d for tray cons truction
d. Vapor Flow Conditions
Advers e vapor flow conditions can caus e
i. Foaming
Foaming refers to the expansion of liquid due to pas sage of vapor or gas.
Although it provide s high interfacial liquid-vapor contact, exces s ive foaming often
le ads to liquid buildup on trays . In s ome cas es , foaming may be so bad that the
foam mixes with liquid on the tray above. Whether foaming will occur de pe nds
primarily on physical properties of the liquid mixture s , but is sometime s due to
tray des igns and condition. Whateve r the caus e, s eparation efficiency is always
re duce d.
ii. Entrainment
Entrainment refers to the liquid carried by vapor up to the tray above and is again
caus ed by high vapor flow rates . It is detrime ntal be caus e tray efficie ncy is
re duce d: lower volatile material is carrie d to a plate holding liquid of higher
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volatility. It could als o contaminate high purity dis tillate. Exces s ive entrainme nt
can le ad to flooding.
iii. We eping / Dumping
This phenomenon is caus ed by low vapor flow. The pres s ure exerted by the vapor
is ins ufficie nt to hold up the liquid on the tray. There fore, liquid s tarts to leak
through pe rforations . Exces s ive wee ping will lead to dumping. That is the liquid
on all trays will cras h (dump) through to the bas e of the column (via a domino
effect) and the column will have to be re-s tarted. Wee ping is indicate d by a s harp
pres sure drop in the column and re duced s eparation efficiency.
iv. Flooding
Flooding is brought about by exces s ive vapor flow, caus ing liquid to be e ntrained
in the vapor up the column. The increas e d pres s ure from exce s sive vapor als o
backs up the liquid in the down comer, caus ing an incre as e in liquid holdup on the
plate above. De pending on the degre e of flooding, the maximum capacity of the
column may be s everely re duced. Flooding is dete cted by s harp incre as e s in
column differe ntial pre s s ure and s ignificant decreas e in s e paration efficie ncy.
v. Weather Conditions
Mos t dis tillation columns are open to the atmos phe re. Although many of the
columns are ins ulated, changing weathe r conditions can s till affect column
ope ration. Thus the re boiler mus t be appropriate ly size d to e ns ure that e nough
vapors can be ge nerate d during cold and windy s pells and that it can be turned
down s ufficiently during hot s easons . The s ame applie s to condens ers .
Thes e are s ome of the more important factors that can caus e poor dis tillation
column performance. Other factors include changing operating conditions and
throughputs , brought about by changes in ups tream conditions and change s in the
demand for the products . All the s e factors , including the as s ociated control
s ys tem, s hould be cons idere d at the des ign stages becaus e once a column is built
and installed, nothing much can be done to re ctify the situation without incurring
s ignificant cos ts .