DISTILLATION

Distillation is an operation for separating the components of mixture based on the

transfer of material from one homogeneous phase to another by vaporization. Mixtures
of miscible and volatile substances are vaporized into individual components or in some
cases into groups of components.
Principle of distillation is the distribution of the substances between the gas and
liquid phase, applied to cases where all components are present in both cases.
Since this depends on the nature of the substance there is no chance for alteration of
solvents as in the case of absorption, stripping etc.
A gas and liquid phase has been brought into contact for purpose of diffusional
interchange between them. The equipments for the gas liquid operations provide intimate
contact of the two fluids. The rate of mass transfer is directly dependent upon the
interfacial surface exposed between the phases and the nature and the degree of
dispersion of one fluid in the other,
Gas dispersed: Liquid is continuous phase, gas dispersed phase
Ex sparged and agitated vessels, tray towers in which the gas phase is dispersed into
bubbles or foams.
Liquid dispersed: Liquid is dispersed into thin films as drops.
Ex Wetted wall towers, sprays, venturi scrubber, packed towers.
Bubble point:
The temp. At which first bubble appears to boil from liquid state. At this point
yi = 1.0; But y = (m * x),
Where x = mole fraction in liquid.
y = mole fraction in vapor.
m = Vapour Pressure / Total Pressure.
Vary the temp. and find yi till it becomes equal to 1.0.
SIGNIFICANCE: This gives the bottom temp. in batch distillation.

Dew Point:
The temp. at which first drop condenses from Vapor State. At this point
xi = 1.0; But x = (y /m) ,
where x = mole fraction in liquid.
y = mole fraction in vapor.
m = Vapour Pressure / Total Pressure.
Vary the temp. and find yi till it becomes equal to 1.0
Bubble point & Dew point are the same for a pure compound i.e., equal to the boiling
point of that compound.
SIGNIFICANCE: This gives the top temp. in the distillation column.
Ex. Calculation of Bubble point & Dew point of 50 % Toluene & 50 % Water mixture.
Bubble point:
At temp of 104 C,
Antoine Eq: -ln (VP) = A B / (T+ C) where ABC are constant And T in Kelvin
Compnd mole Fracn A
B
C
Water
0.5
18.3036 3816.44 46.13
Toluene 0.5
16.0137 3096.52 53.67

v.p.
K
y=k*x
870.4755 1.166857 0.583429
624.3651 0.836951 0.418475
1.001904

Dew point:
At temp. of 105 C.
Compou
nd
Water
Toluene

mole
fraction
0.5
0.5

18.3036 3816.44 46.13

16.0137 3096.52 53.67

v.p.

901.2619 1.208126 0.413864

643.0765 0.862033 0.580024
0.993888

Relative volatility ():

For binary mixtures,
y * (1-x)
= --------------- ,
(1-y) * x

Vapour pressure of 1
= --------------------------Vapour pressure of 2

x=y/k

 is always found between the boiling point of the two compounds.

TYPES OF DISTILLATION:
1) Batch Distillation.
i)
With reflux.
a) Constant reflux.
b) Constant distillate product.
ii)
Without reflux (Simple Distillation) .
2) Continuous Distillation.
3) Steam Distillation.
4) Azeotropic Distillation.
5) Extractive Distillation.

1. Batch Distillation:
These are used when:
*
The compositions of the materials to be separated vary over wide ranges.
*
For small-scale operations.
*
When there is small amount of light or high boiling compound.
*
When more compounds are involved and pure cut to be done to avoid more no.
of columns.
Usually in Distillation column we have a Rectifying section & Stripping Section.
Rectifying section: Mainly from Vapor to Liquid. Similar to Absorption.
Stripping Section: Mainly from Liquid to Vapor . Similar to Stripping.
In Batch Distillation operations only rectifying or enriching section is present, as the
feed is the vapor.
i) Without reflux: (Simple Distillation):
There is no control and the distillate composition keeps on varying.
Gives more output & low boiler recovery but less percentage in the distillate
composition.
ii) Constant reflux ratio & variable product composition:
There is not much difference with that of with out reflux but still separation
between compounds is obtained.
Gives medium recovery & medium output & medium distillate composition.
iii) Variable reflux ratio & constant product composition:
The reflux ratio is changed to maintain the product composition constant.
Distillate composition is highest with low output & low recovery.
Ex. Almost all distillation in Company with Column & Reflux ratio.

Distillation
Method

Still comp. Receiver

A
Simple distillation 0.10
Constant reflux
0.13
Varying reflux
0.26

A
0.58
0.84
0.95

A %
Recovery
96.6
87.6
65.4

Steam Distillation:
Steam distillation is used for substance, which is;
1) High boiling.
2) Insoluble with Water.
The boiling point is at the temperature at which sum of the Vapour pressures becomes
equal to Total pressure.

Continuous Distillation:
Continuous feeding is done and continuously product & residue are withdrawn.

Azeotropic Distillation:
Azeotropic distillation is used when;
i)
The relative volatility between the two components is less, which requires high
reflux ratio.
ii)
The product of required purity cannot be obtained by ordinary fractionation.
In this method, a 3rd compound is introduced to the mixture (A & B , A is low boiling) so
that the 3rd component forms low boiling Azeotrope with A (the low boiling compound)
of the mixture and comes out as distillate product. Then the 3 rd component is separated by
means of Phase separator and returned back to the column. Thus A is separated from B.
3rd component used is called Entrainer.
While choosing the 3rd component care should be taken that
i)
It forms low boiling azeotrope and it is also insoluble with A so that the separation
between the two can be done with out any further process.
ii)
The compound should be cheap & quantity required should be less.
iii)
This component should not react with original components.
iv)
Latent heat of vaporization of the entrainer chosen should be less.

Extractive Distillation:
Extractive distillation is used when;
1
i)
The relative volatility between the two components is less, which requires high
reflux ratio.
ii)
The product of required purity cannot be obtained by ordinary fractionation.
In this method, a 3rd compound is introduced to the mixture (A & B, A is low boiling) so
that the 3rd component either forms high boiling Azeotrope with B (the high boiling
compound), or reduces the volatility of the high boiling compound thereby helping the
separation. Then the 3rd component is separated by means of distillation from the high
boiling component. Thus A is separated from B. 3rd component used is called Solvent.
While choosing the 3rd component care should be taken that
i)
It forms either high boiling azeotrope with high boiling compound or reduces the
volatility.
ii)
The compound should be cheap & quantity required should be less. It should have
less latent heat of vaporization.
iii)
This component should not react with original components.
iv)
Its relative volatility with A should be less.

PACKED BED COLUMNS

TYPES OF PACKINGS :
Random packings :
Random packings are used for providing better contacting surface area between gas
liquid or liquid liquid, compared to the hollow columns. The pressure drop in these are
more because of randomness in packing. The random packings are used are IMTP,
raschig rings Pall rings etc. The cost of these packings are less. These packings are
available in different siszes and different moc such as ceramic, MS,plastics, SS.
Structured PackingS :
Provides Less pressure drop and lower HETP compared to the random packing. Their
cost is higher (labourous job) these are mainly used in critical operation where very high
vacuum is a large no of theoretical stages are required.
TYPES OF DISTILLATION DEPENDING ON OPERATING PRESSURE :
Vacuum Distillation: 1

Distillation is carried out under vacuum conditions to reduce the boiling temp of for one
of the following reasons.
1) The relative volatility between the components generally increases the boiling temp
drops. This higher relative volatility improves the ease of separation, which lowers
the no of theoretical stages needed for given separation. If the no of theoretical stages
held constant, the reflux ratio required for same separation is reduced. In addition the
no of theoretical stages and the reflux ratio are maintained constant, product purity
will be increased.
2) Lower distillation temp is desirable when processing thermally sensitive products,
lower temp retard the undesirable reactions such as product decomposition,
polymerization or discoloration.
3) Separations can be achieved for components with very low vapour pressures or
compounds that degrade at temp near their boiling point.
4) Lower reboiler temp permit the use of less costly energy sources such as LPS, Hot
water. In case of LPS Latent is also more compare to MPS or HPS.
Pressure Distillation: Pressure Distillation is carried out to permit condensation of low boiling materials at
ambient temp. As the distillation pressure is increased the relative volatility will be
decreased so the separation will become more difficult. This will lead to the greater no of
theoretical stages for the same separation. Even though the capacity of a column
increases at higher Pressure due to the greater vapour density the no of theoretical stages
or reflux ratio required will be higher. Usually distillation column is designed at the
lowest operating pressure that is economically feasible.
OPERATION :
Packed Columns are used in the continuous contact of liquid and gas in
the cocurrent and countercurrent flow types, these are vertical
columns which have been filled with packing that provide large
interfacial area, liquid is distributed over and trickles down
through the packing exposing a large surface to contact the gas.
Desired properties of packing :
1) Provide large interfacial area between liquid and gas
2) The packing must permit the passage of large volumes of fluids through small tower
C/S without loading or flooding and with low pressure drop for the gas (void fraction
must be large)

For Random Dumped Packing :

Gas Phase pressure drop with packings is greater than with hallow pipe. And with
introduction of liquid from top will further increase the pressure drop.
Kozeny Carmon Equation: P = V U/( ^ 3)* { [ (1-)/Dp] 2} For Laminar Flow
Burke Plummer equation: P = U^2 g /Dp * {(1-)/ ^ 3} for turbulent flow.
Adding Kozeny & Plummer equation will give the Ergun Equation.
Kister and Gill equation to predict at flood for random dumped packings.
P (Flood) = .115 * F ^ 0.7

TYPES OF PACKING : Rasching rings (ceramic /metal )

Saddle Intalox (ceramic)
Saddle Berl (ceramic)
Pall ring (Plastic /Metal)
IMTP metal (intallox metal tower packing)
Liquid Hold up in packed Towers :Static Hold Up = Volume of Liquid per unit vol. of packing that remains after the flow
stops and the bed is drained. (Depends on packing surface area, roughness of packing,
contact angle)
Operating Hold up: Volume of liquid per unit vol. of packing that drains out of the bed after the gas and
liquid flows to the column are stopped.

PACKING SIZE VS RECOMMENDED LIQUID RATES: Packing size (inch)

Liquid rate (gam /ft 2)

1
1
2

25
40
55
70

Packing factors
(F)
chart
for
random dumped

5/8

3/4

packing
IMTP (metal)
Pall Ring(plastic)
Intallox
Saddle 200
(ceramic)

51
95
145

41
55
92

28
40
52

18
26
40

12
17
22

FLOW PATTERN IN A PACKED BED COLUMN :

Co-current Flow Operations : Single mass transfer stage is required. No conventional flooding limitations because
liquid hold up tends to decrease with increasing gas rate.
Because of higher allowable pressure drop the capacity of a given dia column is much
greater in co-current than the counter current flow operations. Gas liquid contact
intensity is greatly increased at higher flow rates. Thus the mass transfer rates can be
elevated in co-current flow.
These operations are used for following processes, where either absorption is with
reactions or the resistance for mass transfer is very less.
Ex: 1. Absorption of low concentrations of ammonia by dilute acids.
2. Removal of traces of H2S or CO2 by absorption into caustic soda solution.
Drying of Chlorine gas with recirculated sulfuric acid.
Counter-current Flow Operations : Provides the greatest efficiency because mass transfer driving forces are maximum at
both the ends.
This type of contacting is used in most of the operations.
Cross Flow Operations: Area for gas flow is different than the area for liquid flow. Thus cross flow operations
will permit higher gas rates and the use of higher gas to liquid flow ratios than a counter
currently operated column.
But the packing efficiency and mass transfer driving forces are reduced compared to
countercurrent flow.

GENERAL PROCEDURE FOR OPERATION OF A DISTILLATION

SYSTEM :1) Receive RM. in the distillation vessel.
2) Get the analysis of RM. to distill (understand the Components present in the Mass)
3) Open the vapour line valve, equalisation valve collection or Reflux and atm vent /
vacuum line valve.
4) Check the dew point of the low boiler to be distilled at the distillation Pressure(atm ,
vacuum)

5) The condenser utility should be such that the diff in dewpoint of low boiler and the
utility temp should be at least 10 C.
Start utility CTW /CHW/CHB.
6) Drain the limpet /jacket by opening passing steam trap / By pass valve to complete
the draining.
7) Once the steam starts coming from by pass valve / Trap that mean now the limpet
/jacket has been drained completely.
8) Continue heating the distillation mass initially the pressure gauge will show very low
pressure as most of the steam will be condensed immediately in side the limpet
/jacket to heat the RM.
9) After the distillation mass has been heated to sufficient temp for boil up the pressure
gauge will show relatively high pressure.
10) Check whether boiling of distillation mass is taking place or not in the sight glass of
the reactor /Check the vapour temp is raising.
11) Once the vapour condensation is started, Check the temp of the vent line /Vacuum
line, if it is cold then we can further increase the boil up. If it is warm then we can
bring down the temp by throttling the heating media valve.
12) Calculation of Boil up rate of the system.
If L= 2 (reflux) and D=1 (colln) and the collection rate is 400 Lit /Hr,
The boil up would be = 400 (2+1) = 1200 Lit /Hr.
13) If the boil up rate is lower than the expected values then check whether steam tarps
are working or not, open the by pass valve slightly, after opening the boil up is
satisfactory that means trap is not working.
14)Do the cut changeover as per SOP (when the vapour temp is constant at some fixed
pressure and there is no collection cut changeover is done)
15) Same is thing is repeated for the remaining cuts.

TROUBLE SHOOTING:
1. Pressure drop more :
The vapor line or equalization or vacuum line gets restricted.
2. Reactor pressure increases:
The column bottom reflux is not taking place through the reflux line but through the
vapor line.
3. Vacuum problems.
4. Boil ups:
Check for the steam condensate. Measure the steam condensate rate and check for the
boil up. Usually the latent heat is taken as 100 Kcal/Kg for organic compounds.
5. Sublimation problem :
For avoiding this, following solutions are there;
i)
Provide baroleg and avoid vacuum in collection tanks so that there will be no
sublimation.

ii)

Increase the pressure in the system there by sublimation temp. Increases and
thereby avoid sublimation.

10