Distillation

Lecture 01
DISTILATION
• INTRODUCTION
• PRINCIPLE OF DISTILLATION
• AFFECTING CONDITIONS
• TYPES OF DISTILLATION
COLUMNS
• BASIC DISTILLATION
EQUIPMENT AND
OPERATION
• BASIC OPERATION AND
TERMINOLOGY
DISTILLATION
• Physical separation process, and NOT a chemical
reaction.
• Distillation is a method of separating or purifying
liquids based on their different boiling points
• Distillationis a method of separating mixtures
based on differences in their volatilities in a boiling
liquid mixture.
• Distillation
of fermented solutions has been used
since ancient times to produce distilled beverages
with higher alcohol content.
DISTILLATION

• Commercially, it is used to
• separate crude oil;
• water is distilled to remove impurities, such as
salt from seawater;
• airis distilled to separate its components—
notably oxygen, nitrogen, and argon—for
industrial use.
DISTILATION
• Distillation
is favored over other separation
techniques such as crystallization or
membranes when;
• The relative volatility is greater than 1.2
• Products are thermally stable
• Large rates are desired
• No corrosion
• Precipitation or explosion issues are
present.
PRINCIPLE OF DISTILLATION

• The component with the lowest boiling point

vaporizes first, travels through the tubing and
then is condensed in the test tube that sits in the
cool water.
• The material that remains in the distilling flask is
known as the residue.
PRINCIPLE OF DISTILLATION

• The substance that travels through the tubing

and is later condensed in the test tube is known
as the distillate or condensate.
• The apparatus for distillation can be more
sophisticated than the one shown here.
Types of Distillation
• Simple distillation-use to separate mixtures of
liquids with significant difference in volatility
• Fractional distillation-used when components
of a mixture have close boiling points
 Simple Distillation Set up
• Distilling flask
• Distilling head
• Pocket
Thermometer
• Thermometer
• Condenser
• Cooling water in
• Cooling water
out
• Adapter
Fractional Distillation Set up
• 1.Distilling flask
• 2.Fractionating
column
• 3.Distilling head
• 4.Pocket
Thermometer
• 5.Thermometer
• 6.Condenser
• 7.Cooling water in
• 8.Cooling water out
• 9.Adapter
• 10.Receiving flas
 Types of Distillation

• Steam
distillation-the
process of
separating or
purifying a liquid
by passing steam
through it.
 Types of Distillation

• Vacuum
distillation-
distilling liquid at
low pressure so
that it boils at a
lower boiling
point
TYPES OF DISTILLATION
• Batch Distillation
• A mixture is distilled to separate it into its
component fractions before the distillation
still is again charged with more mixture and
the process is repeated.
• Ithas always been an important part of the
production of seasonal or low capacity and
high-purity chemicals.
• It is a very frequent separation process in the
pharmaceutical industry and in wastewater
treatment units.
TYPES OF DISTILLATION

• Continuous Distillation
• An ongoing distillation in which a liquid mixture
is continuously fed and separated fractions are
removed continuously as output streams from
distillation column during the operation.
• Produces at least two output fractions, including
at least one volatile distillate fraction and
bottoms (or residue) fraction
TYPES OF DISTILLATION

• Differs from batch distillation such that the

concentrations remain same over time.
• Can be run at a steady state for an arbitrary
amount of time.
• Requires building and configuring dedicated
equipment.
• The high investment cost restricts its use to
the large scale.
TYPES OF DISTILLATION
COLUMNS
• Continuous columns can be classified
according to:
• 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
TYPES OF DISTILLATION
COLUMNS
• The number of product streams
• Multi-product column - column has more
than two product streams 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.
BASIC DISTILATION UNIT
• The type of column internals
• Tray column
• 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.
BASIC
• DistillationDISTILATION
columns are made UNIT
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:
• Distillation Column.mp4
• Vertical shell
• A vertical shell where the separation of
liquid components is carried out
• column internals such as trays/plates and/or
BASIC DISTILATION UNIT
• Reboiler
• Provide the necessary vaporization for the
distillation process
• Condenser
• Cool and condense the vapour leaving the top
of the column
• Reflux drum
• Hold the condensed vapour from the top of the
column so that liquid (reflux) can be recycled
back to the column
 BASIC DISTILATION UNIT
• The vertical shell
houses the column
internals and
together with the
condenser and
reboiler, constitutes a
distillation column.
•A schematic of a
typical distillation
unit with a single
feed and two product
streams is shown
 BASIC OPERATION AND
• Feed TERMINOLOGY
• The liquid mixture that is to be processed.
• Introduced usually somewhere near the
middle of the column to a tray known as the
feed tray.
• Enriching or rectification – part of column
above the feed tray to top of column.
• Bottom (stripping) section – part of column
below the feed tray to the reboiler.
• The feed flows down the column where it is
collected at the bottom in the reboiler.
Distillation
• Column Internals
• Trays and Plates
• The terms "trays" and "plates" are used
interchangeably.
• 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
Distillation column Internals
Distillation

• Valve trays
• Perforations are covered by liftable caps.
• Vapour flows lifts the caps, thus 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.
Distillation
Valve trays
Distillation

• Sieve trays
• 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.
Distillation
Sieve trays
Distillation
• jDye of their efficiency, wide operating range,
ease of maintenance and cost factors, sieve
and valve trays have replaced the once highly
thought of bubble cap trays in many
applications.
Distillation
• Liquid and Vapour Flow in a Tray 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.
•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.
• Being lighter, vapour flows up the column and is forced to
pass through the liquid, via the openings on each tray. The
area allowed for the passage of vapour on each tray is called
the active tray area.
Distillation
Liquid and Vapour Flow in a Tray Column
Distillation
• Asthe hotter vapour passes through the liquid on the tray
above, it transfers heat to the liquid.
• In doing so, some of the vapour condenses adding to the
liquid on the tray.
• Thecondensate, however, is richer in the less volatile
components than is in the vapour.
• Additionally,because of the heat input from the vapour, the
liquid on the tray boils, generating more vapour. T
• his vapour, which moves up to the next tray in the column, is
richer in the more volatile components.
• This continuous contacting between vapour and liquid occurs
on each tray in the column and brings about the separation
between low boiling point components and those with higher
boiling points.
Distillation
• Tray Designs
• A tray essentially acts as a mini-column, each accomplishing a
fraction of the separation task. From this we can deduce that the
more trays there are, the better the degree of separation and that
overall separation efficiency will depend significantly on the design
of the tray. Trays are designed to maximise vapour-liquid contact by
considering the
• · liquid distribution and
• · vapour distribution on the tray.
• This is because better vapour-liquid contact means better separation
at each tray, translating to better column performance. Less trays
will be required to achieve the same degree of separation. Attendant
benefits include less energy usage and lower construction costs.
• There is a clear trend to improve separations by supplementing the
use of trays by additions of packings.
Distillation
• Packings
• Packings are passive devices that are
designed to increase the interfacial area for
vapour-liquid contact.
Distillation

• 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.
Distillation
• Packings versus Trays
• packings provide extra inter-facial area for liquid-
vapour contact
• efficiency
of separation is increased for the same
column height
• packed columns are shorter than trayed columns
• Packed columns are called continuous-contact
columns while trayed columns are called staged-
contact columns
• Because of the manner in which vapour and liquid
are contacted.
 BASIC OPERATION AND
TERMINOLOGY
• Heatis supplied to the reboiler to generate
vapour.
• The source of heat input can be any suitable
fluid, normally steam and the output streams
of other columns.
• The vapour raised in the reboiler is re-
introduced into the unit at the bottom of the
column.
• The liquid removed from the reboiler is known
as the bottoms product or simply bottoms.
 BASIC OPERATION AND
TERMINOLOGY
• The vapour moves up the column, and as it
exits the top of the unit, it is cooled by a
condenser.
• Thecondensed 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.
• The condensed liquid that is removed from
the system is known as the distillate or top
product.
AFFECTING CONDITIONS:

• Pressure and Temperature:

• Determines how good or how easy the
separation can be, since a different T /or P
can give you different equilibrium
conditions.
• Probably determining how theoretical
stages are needed, or moving towards/away
from an azeotropic point.
AFFECTING CONDITIONS:

• Feed condition
• Alter the vapor/liquid content or flow inside
the unit
• Influence the reboiler duty
• A saturated or subcooled liquid (feed), the
reboiler will need more heat to evaporate,
while the feed having some vapor phase or
is saturated vapor require less heat.
AFFECTING CONDITIONS:

• Reflux ratio:
• Determine the purity of the overhead
product by sacrifying distillate flow rate.
• Morereflux result in better separation, but
producing less distillate.
• Less reflux produce more distillate with
lower purity in the light component.
AFFECTING CONDITIONS:
• Reboiler duty:
• Determines the amount of heavy vapor
phase in the column.
• Also determines how much heavy
component is evaporated thus affecting the
heavy composition in the bottoms product.
• The reboiler, duty must be balanced to
generate enough vapor avoiding the
contamination of the overhead product with
heavy component.
 BASIC OPERATION AND
TERMINOLOGY

• Operation of Distillation column

Distillation