A Lecture on Distillation

DISTILLATION

Distillation is defined as:

a process in which a liquid or vapour

mixture of two or more substances is
separated
into
its
component
fractions of desired purity, by the
application and removal of heat.

Distillation is based on the fact

that the vapour of a boiling mixture
will be richer in the components
that have lower boiling points.

DISTILLATION PRINCIPLE
Separation of components from a liquid
mixture via distillation depends on the
differences in boiling points of the
individual components. Also, depending
on the concentrations of the components
present, the liquid mixture will have
different boiling point characteristics.
Therefore, distillation processes depends
on the vapour pressure characteristics of
liquid mixtures.

RELATIVE VOLATILITY
Relative volatility is a measure of the differences in
volatility between 2 components, and hence their
boiling points. It indicates how easy or difficult a
particular separation will be. The relative volatility
of component i with respect to component j is
defined as
yi = mole fraction of component i in the vapour
xi = mole fraction of component i in the liquid
Thus if the relative volatility between 2
components is very close to one, it is an indication
that they have very similar vapour pressure
characteristics. This means that they have very
similar boiling points and therefore, it will be
difficult to separate the two components via
distillation.

CONT.
It is the ratio of the concentration
ratio of A & B in gas phase to that
of liquid phase.

y * /(1 y*) y * (1 x)

x /(1 x)
x(1 y*)

IDEAL SOLUTION RAOULTS LAW

For an ideal solution ,the equilibrium
partial pressure p* of a constituent
at a fixed temperature equals the
product of its vapor pressure p
when pure at this temperature and
its mole fraction in liquid.
P*A= PA x

BASIC DISTILLATION
EQUIPMENT
MAIN COMPONENT OF DISTILLATION COLUMN

Distillation columns are made up of several

components, each of which is used either to
transfer heat energy or enhance material
transfer. A typical distillation contains several
major components:
a vertical shell where the separation of
liquid components is carried out.
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.
a condenser to cool and condense the
vapour leaving the top of the column.

COLUMN REBOILERS
There are a number of designs of reboiler.
It is beyond the scope of this set of
introductory notes to delve into their
design principles. However, they can be
regarded as heat-exchangers that are
required to transfer enough energy to
bring the liquid at the bottom of the
column to boiling point. The following are
examples of typical reboiler types.

TYPE OF DISTILLATION
COLUMN
There
are
many
types
of
distillation
columns,
each
designed to perform specific
types of separations, and each
design
differs
in
terms
of
complexity.
One way of classifying distillation
column type is to look at how they
are operated. Thus we have:
batch and
continuous columns.

DISCRIPTION
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
most common of the two types. We shall
concentrate only on this class of columns.

TYPES OF CONTINUOUS
COLUMN
Continuous columns can
classified according to:

be

further

The nature of the feed that they are

processing,
Binary column - feed contains only two components
Multi-component column - feed contains more than
two components

The number of product streams they

have
Multi-product column - column has more than two
product streams.

CONT..
Where the extra feed exits when it is
used to help with the separation,
Extractive distillation - where the extra feed
appears in the bottom product stream
Azeotropic distillation - where the extra feed
appears at the top product stream

The type of column internals

Tray column - where trays of various designs are
used to hold up the liquid to provide better
contact between vapour and liquid, hence better
separation
Packed column - where instead of trays,
'packings' are used to enhance contact between
vapour and liquid

COLUMN
INTERNALS

TRAYS AND PLATES

The terms "trays" and "plates" are used
interchangeably. There are many types of
tray designs, but the most common ones
are :
Bubble cap trays
A bubble cap tray has riser or chimney fitted
over each hole, and a cap that covers the
riser. The cap is mounted so that there is a
space between riser and cap to allow the
passage of vapour. Vapour rises through the
chimney and is directed downward by the cap,
finally discharging through slots in the cap,
and finally bubbling through the liquid on the
tray.

BUBBLE CAP TRAY

CONT
Valve trays
In valve trays, perforations are covered by
liftable caps. Vapour flows lifts the caps, thus
self creating a flow area for the passage of
vapour. The lifting cap directs the vapour to
flow horizontally into the liquid, thus
providing better mixing than is possible in
sieve trays.

Sieve trays
Sieve trays are simply metal plates with holes
in them. Vapour passes straight upward
through the liquid on the plate. The
arrangement, number and size of the holes
are design parameters.

SIEVE TRAY

VALVE TRAY

LIQUID-VAPOUR FLOW
The next few figures show the direction of
vapour and liquid flow across a tray, and
across a column.
Each tray has 2 conduits, one on each
side, called downcomers. Liquid falls
through the downcomers by gravity from
one tray to the one below it. The flow
across each plate is shown in the diagram
A weir on the tray ensures that there is
always some liquid (holdup) on the tray
and is designed such that the the holdup
is at a suitable height, e.g. such that the
bubble caps are covered by liquid.

PACKINGS
Packings are passive devices that are
designed to increase the interfacial area for
vapour-liquid contact. The following pictures
show 3 different
These strangely shaped pieces are supposed
to impart good vapour-liquid contact when a
particular type is placed together in
numbers,
without
causing
excessive
pressure-drop across a packed section. This
is important because a high pressure drop
would mean that more energy is required to
drive the vapour up the distillation column.

TYPES OF DISTILLATION
There are
distillation.

different

Conventional distillation
Steam Distillation
Vacuum Distillation
Fractional Distillation
Azeotropic Distillation
Extractive Distillation

types

of

STEAM DISTILLATION
It is convenient technique for distilling
certain difficult-to-handle Materials. As
followChemicals having relatively high boiling points
at atmospheric pressure.
Chemicals that are likely to decompose even
at their atmospheric boiling points. e.g. fatty
acids.
Chemicals that pose hazards when distilled by
the application of direct heat. e.g Turpentine.

Steam distillation is practiced in coal

chemicals, fats and oils, petroleum,
petrochemicals, paper industries etc.

VACUUM DISTILLATION
It is normally referred to those distillation
which are carried out under vacuum.
Vacuum distillation has some benefits are as
under.
The volatility of the components generally rises
with the lowering of the boiling points. So that
required column height will be reduced. Required
lower reflux ratio.
Polymerization and thermal decomposition of
components can be prevented. The column
temperature is at its highest at the bottom
section
where
product
degradation,
polymerization can happen. So lower bottom
temperatures can generate less unwanted
chemical changes.

CONT..
There are some organic compounds that
are
thermally
unstable
even
at
temperature near their atmospheric
boiling points.
Separation under vacuum buys an
economy
in
reboiler
energy
requirement.So
less
costly
energy
sources like low pressure steam or waste
heat steam or hot water can be used

PACKINGS Vs TRAYS

A tray column that is facing throughput

problems may be de-bottlenecked by
replacing a section of trays with packings.
This is because:
packings provide extra inter-facial area for liquidvapour contact
efficiency of separation is increased for the same
column height
packed columns are shorter than trayed columns

Packed columns are called continuouscontact columns while trayed columns are
called staged-contact columns because of
the manner in which vapour and liquid are
contacted.

FACTOR AFFECTING
DISTILLATION OPERATION
The performance of a distillation column is determined
by many factors, for example:
feed conditions
state of feed
composition of feed
trace elements that can severely affect the VLE of
liquid mixtures
internal liquid and fluid flow conditions
state of trays (packings)
weather conditions
Some of these will be discussed below to give an idea
of the complexity of the distillation process .

DIFFICULTIES IN
DISTILLATION COLUMN
For stage or tray efficiency to be high the time of
contact should be long to permit the diffusion. In
order to provide long contact time the liquid pool
on each tray should be deep.so that bubbles of
gas will required a long time to rise through the
liquid.
But when gas bubble only slowly through the
opening on the tray the bubble are large & the
interfacial surface is small & much of it may even
pass over the tray without having contact the gas.
So, for high tray efficiency we required deep pool
of liquid & high gas velocities.

Cont.
This condition however leads to
number of difficulties.
flooding
Priming(foaming)
entrainment
weeping/dumping
Coning

ENTRAINMENT
When the gas velocities is relatively high, it
dispersed very thoroughly into liquid which
in turn is agitated into froth.this provide
large interfacial surface area. But at high
gas velocities, when the gas is disengaged
from the froth small droplets of liquid will
be carried by the gas to the tray above.
This is called entrainment. This will reduce
the concentration change brought about by
the mass transfer which lead to decrease
the tray efficiency.

FLOODING
Great liquid depth & high gas velocities both
result in high pressure drop for gas , flowing
through the tray.
With the large pressure diff. In the space
between the tray, the level of liquid leaving the
tray at relatively low pressure.
As the pressure diff. Increase due to increase
rate of flow of either gas or liquid the level in
down spot will rise further to permit the liquid to
enter the lower tray. Further increase in flow rate
the liquid will fill the entire space between the
trays.the tower is then flooded.

PRIMING
For liquid gas combination which tend to
foam excessively, high gas velocities may
lead to priming.
Here the foam persists throughout the
space between the tray and the liquid is
carried by the gas from one tray to another
tray.the liquid so carried recirculates
between trays & the added liquid-handling
load increase the gas pressure drop to lead
to flooding.

CONING, WEEPING &

DUMPING
If liquid rates are to low, the gas rising
through the openings of the tray may
push the liquid away (Coning) and contact
of gas & liquid is poor.
If the gas rate is to low, much of the liquid
may rain down through the openings of
the tray(Weeping) thus to failing to obtain
of complete flow over the tray.
At very low gas flow rate none of liquid
reaches the downspout.(Dumping)