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Distillation

Distillation is a method for separating liquid mixtures through vaporization and condensation, involving steps to convert liquid to vapor and recover the liquid. Various distillation methods include simple, flash, fractional, and vacuum distillation, each suited for specific applications like purifying water or separating components in the petroleum industry. The document outlines the principles, construction, working, and applications of these methods, emphasizing their importance in producing high-purity substances and preventing contamination.

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0% found this document useful (0 votes)
14 views57 pages

Distillation

Distillation is a method for separating liquid mixtures through vaporization and condensation, involving steps to convert liquid to vapor and recover the liquid. Various distillation methods include simple, flash, fractional, and vacuum distillation, each suited for specific applications like purifying water or separating components in the petroleum industry. The document outlines the principles, construction, working, and applications of these methods, emphasizing their importance in producing high-purity substances and preventing contamination.

Uploaded by

Lubhanshu Sharma
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PPTX, PDF, TXT or read online on Scribd
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DISTILLATION

BY - HIMANI
INTRODUCTION
• Distillation is defined as the separation of the components of a liquid
mixture by a process involving vaporization and subsequent condensation
at another place.
• The distillation process involves two steps;
(a) converting a liquid into vapour phase and
(b) transferring the vapour to another place. and recovering the liquid by
condensation.
The feed liquid is known as distilland. The condensed liquid is known as
distillate or condensate.
If one component is volatile and others are non-volatile, it is possible to
separate volatile components from non-volatile components by distil-
lation.In such cases, distillation is considered as a separation or
purification method. When heat is supplied to a mixture, a more volatile
liquid evaporates readily than the less volatile liquid.
Contd…
Difference Between Distillation , Evaporation and Drying
Distillation operation is used when condensed vapour is required as a product.
Evaporation operation is used when the concentrated liquid residue is needed as a
product.
Drying operation is used when dried solid residue is required as a product.

CLASSIFICATION OF DISTILLATION METHODS


Simple distillation
Flash distillation
Fractional distillation
Azeotropic and extractive distillation
Distillation under reduced pressure
Steam distillation
Molecular distillation
Destructive distillation
Compression distillation
SIMPLE DISTILLATION
Applications:
(1) Simple distillation is used for the preparation of distilled water and water
for injection.
(2) Volatile and aromatic waters are prepared.
(3) Organic solvents are purified.
(4) A few official compounds are prepared by distillation. Examples are spirit
of nitrous ether and aromatic spirit of ammonia.
(5) Non-volatile solids are separated from volatile liquids
INDUSTRIAL SCALE
Contd…
Construction:
• A large metal still (made of stainless steel, copper, etc.) is used.
• A thermometer is attached to monitor the temperature of the liquid
• A sight glass (observation window) helps the operator check the liquid
level and process.
• The still is heated using steam.
• A condenser is attached, where cold water circulates to cool down the
vapor.
•The receiver collects the final distillate (purified liquid).
Contd…
Working:
1. The liquid to be distilled is filled into the still (½ to ⅔ of its volume).
2.To prevent bumping, small pieces of porcelain or porous material are added.
3.Steam heats the still, and the liquid starts boiling.
4.Vapors rise and move to the condenser.
5.In the condenser, vapors cool down and condense into liquid.
6. The distillate is collected in the receiver drop by drop.
7.The temperature remains constant at the boiling point of the liquid.
8. Distillation continues until only a small amount of liquid is left in the still

Usage:
Commonly used to produce distilled water, especially for injections or other
pharmaceutical uses
Preparation of Purified Water (BP) and
Water for Injection (BP) By Distillation

Water for Injection (WFI) is highly purified water used in the pharmaceutical
industry, especially for preparing medicines that are administered directly into the
body, such as injections. It must be free from contaminants like bacteria, endotoxins,
and other impurities.

PRINCIPLE
The principle involved in the preparation of water for injection by distillation is same as
that of the simple distillation. However, it is a special case for the following
reasons :-
1) Removal of Gases from Raw Water
• What it means: The water we use might have dissolved gases like carbon dioxide
(CO₂) or ammonia (NH₃).
• Why it’s important: These gases can contaminate the final distilled water

• Key point: Ammonia is especially harmful and must be removed to make pure water
for injection.
Contd…
(2) Avoid Carryover of Soluble Materials
• What it means: During boiling, tiny droplets of water can get carried with
the steam.
• Why it’s important: These droplets can contain dissolved impurities or
salts, which will spoil the purity of the final product.
• Key point: We want only pure steam, not droplets.
(3) Prevent Liquid Droplet Entrapment
• What it means: Sometimes liquid droplets get trapped in the steam rising
from the boiler.
• How it’s controlled: Baffles (metal plates) are used to block or catch these
droplets.
• Key point: These baffles clean the steam before it goes to the condenser.
Contd…
(4) Avoid Pyrogen Contamination
• What it means: Pyrogens are fever-causing substances (often from bacteria).

• Why it’s important: If the feed water contains pyrogens, they might get into
the distillate, making the water unsafe for injection.
• Key point: The system must prevent pyrogens from entering the final water.
(5) Prevent Hydrolysis and Volatile By-products
• What it means: If the concentration of solids in the boiler is too high, they
can react with water (hydrolysis).
• What happens then? This can produce volatile (easily evaporated)
substances, like hydrochloric acid (HCl) if chlorides are present.
• Key point: Such by-products contaminate the distillate and must be avoided.
Contd….
• CONSTRUCTION
The apparatus mainly has these parts:
1. Boiler / Still: • It’s a big chamber where water is boiled to make
steam.
2. Heating Coils: • These are coils inside the boiler that heat the water
using steam or electricity.
3. Multitubular Condenser: • It contains many tubes. Hot steam
passes through them and gets cooled down into water.
4. Water Inlet: • This is where the raw (feed) water enters the system.
5. Baffles: • These are plates that block any unwanted droplets or solid
particles from passing through with the steam.
6. Constant Level Device: • Maintains the same water level inside the
unit.
7. Gas Escape Opening: • Allows unwanted gases (like CO₂ or
ammonia) to leave so they don’t contaminate the final water.
8. Distillate Outlet:• The final clean water (distillate) comes out from here.
Contd…
Contd…
WORKING
1. Feed water enters from the bottom of the unit.
2. The water passes through the condenser tubes, where it gets preheated by hot
steam moving in the opposite direction.
3. This preheated water goes into the boiler, where it is boiled using heating coils.

4. As it boils, steam is produced. This steam contains only pure water—leaving


behind salts, bacteria, and other impurities.
5. The steam rises and passes through baffles, which stop any droplets or
impurities from going further.
6. The clean steam enters the multitubular condenser, where it cools down and
turns back into liquid water.
7. This condensed water is very pure—this is the Water for Injection (WFI).

8. Finally, this WFI is collected from the distillate outlet at the bottom.
Contd…
Advantages
• Very pure water is obtained.
• Removes gases, salts, and microbes.
• Uses heat efficiently (because feed water is preheated using steam from the
condenser
FLASH DISTILLATION
• Flash distillation is defined as a process in which the entire liquid mixture
is suddenly vaporized (flash) by passing the feed from a high pressure zone
to a low pressure zone.
• Flash distillation is also known as equilibrium distillation.
Principle : When a hot liquid mixture is allowed to enter from a high-pressure
zone into a low-pressure zone, the entire liquid mixture is suddenly
vaporised. This process is known as flash vaporisation. During this process
the chamber gets cooled. The individual vapour phase molecules of high
boiling fraction get condensed, while low boiling fraction remains as
vapour. This process requires certain amount of time. Therefore, the liquid
and vapour is kept in intimate contact until equilibrium is achieved. The
liquid fraction is collected separately. The vapour is separated from the
liquid and further allowed to condense.
Contd…
Construction:
The construction of a flash distillation apparatus is shown in Figure .It
consists of a pump, which is connected to a feed reservoir. Pump helps in
pumping the feed into the heating chamber which contains a suitable
heating mechanism. The other end of the pipe is directly introduced into
the vapour-liquid separator through a reducing valve. The vapour outlet is
provided at the top of the separator and liquid outlet is provided at the
bottom
Contd..
Contd…
Working :
The feed is pumped through a heater at a certain pressure, The liquid gets
heated, which enters the vapour-liquid separator through a pressure-
reducing valve. Due to the drop in pressure, the hot liquid. flashes, which
further enhances the vaporisation process. The sudden vaporisation induces
cooling. The individual vapour phase molecules of high boiling fraction
get condensed, while low boiling fraction remains as vapour. The mixture
is allowed for a sufficient time, so that vapour and liquid portions separate
and achieve equilibrium. The vapour is separated through a pipe from
above and liquid is collected from the bottom of the separator.
Uses :
Flash distillation is used for separating components, which boil at widely
different temperatures. It is widely used in petroleum industry for refining
crude oil
Contd…
Advantages : Flash distillation is a continuous process. It is used for
obtaining multi-component systems of narrow boiling range, especially in
oil refinery. Examples are petroleum ether 60, 80 etc.

Disadvantages : Flash distillation is not effective in separating


components of comparable volatility. It is not suitable for two component
systems. It is not an efficient distillation when nearly pure components are
required, because the condensed vapour and residual liquid are farfrom
pure.
DISTILLATION UNDER REDUCED PRESSURE
OR VACUUM DISTILLATION
• Distillation under reduced pressure may be defined as a distillation process
in which the liquid is distilled at a temperature lower than its boiling point
by the application of vacuum.
• Vacuum pumps, suction pumps, etc. are used to reduce the pressure on the
liquid surface. Distillation under reduced pressure is based on the principle
of simple distillation with some modifications.
Principle: Liquid boils when vapour pressure is equal to the atmospheric
pressure, i.e., pressure on its surface. If the external pressure is reduced by
applying vacuum, the boiling point of liquid decreases.Therefore, the
liquid boils at a lower temperature. This principle is illustrated using an
example of water. Water boils at 100 °C at an atmospheric pressure of
101.31 kPa (760 mm Hg). At 40 °C, the vapour pressure of water is
approximately 9.33 kPa (70 mm Hg). Hence, the external pressure is
reduced to 9.33 kPa (70 mm Hg) where water boils at 40 °C. The net result
is an increase in the rate of mass transfer into vapour.
Contd…
Assembling of apparatus : It consists of a double-neck distillation flask
known as Claisen flask .Thick walled glass apparatus with interchangeable
standard glass joints are used for vacuum distillation. In one of the necks
of the Claisen flask, a thermometer is fitted. The second neck prevents
splashing of the violently agitated liquid. Bumping occurs readily during
vacuum distillation. Placing a fine capillary tube in the second neck of the
flask can prevent bumping.The capillary tube is dipped in the boiling
liquid, so that a stream of air bubbles is drawn out. Water bath or oil bath is
used for heating.
The Claisen flask is connected to a receiver through a condenser.Vacuum
pump is attached through an adapter to the receiver. A small vacuum gauge
(manometer) should be inserted between the pump and the receiver.
Contd…
Contd…
Procedure : The liquid to be distilled is filled one-half to two-third volume
of the flask. Small pieces of porcelain are added to the liquid for
facilitating distillation and prevent bumping. The capillary tube and
thermometer are kept in place in the flask.The required vacuum is applied.
The contents are heated gradually. The temperature rises and liquid gets
vaporised rapidly due to vacuum. The vapour passes through the
condenser. The condensate is collected in the receiver. The temperature is
noted down, which would be less than the boiling point of the liquid.When
a large volume of a liquid is to be distilled under reduced pressure, it is
more convenient to distil comparatively small volumes at a time .
Disadvantages : In vacuum distillation, persistent foaming occurs.This
may be overcome by adding capryl alcohol to the liquid or by inserting a
fine air capillary tube in the second neck of the Claisen flask.The stream of
air is drawn in and breaks the rising foam. The above method is not
suitable for the preparation of semisolid or solid extracts.
Contd…
Application
Preventing degradation of active constituents: During extraction,
concentration and processing at higher temperatures, the active
constituents may undergo decomposition (inactivation). A few examples
are given below. Hence extraction and concentration should be done at a
lower temperature (<55 °C) under reduced pressure.
INDUSTRIAL SCALE
Contd..
Construction
• A vacuum still made of stainless steel or other strong metal.
• It has A sight glass to see the liquid level.
• A thermometer to check temperature.
• A drain pipe at the bottom.
• A connection to a vacuum pump to reduce pressure.
• A condenser to cool down the vapors.
• Two receivers to collect the distillate (liquid product)
Contd..
Working
1. The still is filled with the liquid to be distilled.
2. A vacuum pump creates low pressure (vacuum) inside the still.
3. The liquid is heated using steam.
4. Because of low pressure, the liquid boils at a lower temperature.
5. It vaporizes quickly, and vapors go to the condenser.
6. In the condenser, vapors turn back into liquid (condensate).
7. The distillate is collected in one of the receivers.
8. When one receiver is full, it is switched, and the second one starts
collecting—no need to stop the process.
Contd…
Why Use Vacuum Distillation?
• Useful for liquids that boil at very high temperatures.
• Prevents decomposition of heat-sensitive compounds.
• Saves energy as boiling occurs at a lower temperature.

Note
• A stirring device can be added for uniform heating.
• Capacity ranges from a few liters to thousands of liters depending on
industrial needs.
STEAM DISTILLATION
• Steam distillation is a method of distillation carried with the aid of steam and is
used for the separation of high-boiling substances from non-volatile impurities.
• High-boiling liquids cannot be purified by simple distillation, since the
constituents in the mixture tend to decompose at higher tempera-tures. In such
cases, steam distillation is employed. Steam distillation is used for the
separation of immiscible liquids.
• Principle: A mixture of immiscible liquids begins to boil when the sum of their
vapour pressures is equal to the atmospheric pressure. In case of a mixture of
water and turpentine, mixture boils below the boiling point of pure water,
though the turpentine boils at a much higher temperature than that of water.
For example, the boiling point of turpentine is about 160°C. But when it is
mixed with water and heated, the mixture boils at about 95.6°C. At this
temperature, the vapour pressure of water is 86.245 kPa (647 mm Hg) and that
of turpentine is 15.06 kPa (113 mm Hg). The sum of the vapour pressures is
101.31 kPa (760 mm Hg) which is normal atmospheric pressure. Thus, high
boiling substances may be distilled at a temperature much below its boiling
point, when water (steam) is used.
Contd…
Assembly of apparatus: The assembly of apparatus for steam distillation on
laboratory scale is shown in Fig. It consists of a metallic 'steam can' fitted with
a cork having two holes. Through one of the holes, a long tube is passed so as
to reach almost the bottom of the steam generator. This tube acts as a safety
tube, so that in case the pressure inside the steam generator becomes too much,
water will be forced out of it and the pressure will be relieved. Moreover, when
steam starts coming out from the safety tube, it indicates that the steam can is
almost empty. Through another hole, a bent tube is passed. The other end of the
bent tube is connected to the flask containing non-aqueous liquid (for example,
crude containing volatile oil) through a rubber bung.This tube should reach
almost the bottom of the flask.
Through the other hole of the rubber bung, a delivery tube is inserted Which
connects the flask and the condenser. The condenser is connected to a receiver
flask using an adaptor. Provisions are made to heat the steam can and flask.
STEAM DISTILLATION
Contd…
Procedure : The non-aqueous liquid is placed in the flask. A small quantity
of water is added to it. Steam can is filled with water. The steam generator
and the flask are heated simultaneously, so that a uniform flow of steam
passes through the boiling mixture.The heated. The steam carries the
volatile oil and passes into the condenser, which is cooled by cold water.
The condensed immiscible liquid is collected into the receiver.
Distillation is continued until all the non-aqueous liquid has been distilled.
In the receiver, water and organic liquid form two separate layers, which
can be easily separated using a separating flask.
Contd…
Applications :
(1) Steam distillation is used for the separation of immiscible liquids.
Example is toluene and water.
(2) This method is used for extracting most of the volatile oils such as clove,
anise and eucalyptus.
(3) It is useful in purification of liquid with high boiling point, for example
essential oil of almond.
(4) Camphor is distilled by this method.
(5) Aromatic waters are prepared by this method.
Advantages : Volatile oils can be separated at a lower temperature in steam
distillation, without any decomposition and loss of aroma. If a substance has
low volatility, it can be satisfactorily distilled, provided its molecular weight
is considerably higher than water.
Disadvantages : Steam distillation is not suitable when immiscible liquid
and water react with each other
INDUSTRIAL SCALE
Contd..
• Steam distillation is used to extract volatile oils (like turpentine oil) from plant materials
using steam. It’s especially useful for substances that might break down at high temperatures
if distilled directly.
• How the Equipment Works
• 1. Still/Boiler: • This is where the raw material (like plant leaves or wood
containing oil) is placed. • It has a perforated plate at the bottom to let steam pass
through the material.
• 2. Steam Supply: • Steam is passed into the still (from the side and the
jacket around it). • The steam heats the water and plant material, causing the volatile
oil to vaporize along with the steam.
• 3. Condenser: • The vapor (steam + oil) moves to a condenser, where it’s
cooled by cold water. • This causes the vapor to turn back into liquid.
• 4. Florentine Receiver: • The condensed liquid (oil + water) goes into a
Florentine receiver. • Since oil and water don’t mix, they separate into two
layers: • Oil (usually lighter) floats on top. • Water stays at the bottom.
• 5. Collection: • Oil is collected from the upper spout. •
Water is removed from the lower spout and can be reused.
Contd..
Why This Method?
• It prevents heat-sensitive oils from decomposing.
• Steam helps carry the oil without needing high temperatures.
• Separation is easy since oil and water form two layers after condensation.
Extra Notes:
If the oil’s density is close to water, it might not separate well. In such cases,
the whole mixture is collected and the oil is extracted using a solvent.
MOLECULAR DISTILLATION
Molecular distillation is defined as a distillation process in which each
molecule in the vapour phase travels mean free path and gets condensed
individually without intermolecular collisions on application of vacuum.
Molecular distillation is based on the principle of the simple distillation with
some modifications.. This is also called evaporative distillation or short
path distillation .
Principle : The substances to be distilled have very low vapour pressures.
Examples are viscous liquids, oils, greases, waxy materials and high
molecular weight substances. These boil at very high temperatures.In order
to decrease the boiling point of the liquids, high vacuum must be applied.
The vapour pressure above the liquid is much lower than that of the
saturated vapour in equilibrium. At very low pressure, the distance
between the evaporating surface and the condenser is approximately equal
to the mean free path of the vapour molecules. Molecules leaving the
surface of the liquid are more likely hit the condenser surface.
Contd…
Theory: The mean free path of a molecule is defined as the average
distance through which a molecule can move without coming into collision
with another.The mean path (2) can be expressed mathematically as:
Contd….
According to equation :
(a) Liquids having low viscosity and density possess long mean path.
Distillation is simple.
(b) Substances having high pressures possess low mean free path.
The mean free path can be increased by decreasing the viscosity (n), which
can be obtained at high temperature and low pressure. novolatile substances
may become volatile and distillation is possible.

It is necessary to design the equipment based on the requirement of the


molecular distillation.
1) The evaporating surface must be close to the condensing surface.
2) The molecular collisions should be minimized because they change the
direction of the path of molecules.
3) The liquid surface area must be as large as possible so that the vapour is
evolved from the surface only, but not by boiling. Thus this process is also
called evaporative distillation.
Based on the method of formation of the liquid
film, apparatus may be divided into two types:-
Falling Film Molecular Still or Wiped Film
Molecular Still
Principle: In this method, vaporisation occurs from a film of liquid flowing
down a heated surface under high vacuum. The vapour (molecules) travels
a short distance and strikes the condenser nearby. Each molecule is
condensed individually. The distillate is subsequently collected .
Construction- The vessel has a diameter of one metre The walls of the
vessel are provided with suitable means of heating jacket. Wipers are
provided adjacent to the vessel wall. Wipers are connected to a rotating
head through a rotor.The condensers are arranged very close to the wall
evaporating surface as shown in Figure Vacuum pump is connected to a
large diameter pipe at the centre of the vessel. Provisions are made for
collecting the distillate and the undistilled liquid residue at the bottom.
Contd..
Contd…
Working : The vessel is heated by suitable means.Vacuum is applied at the
centre of the vessel and wipers are allowed to rotate. The feed is entered
through the inlet of the vessel. As the liquid flows down the walls, it is
spread to form a film by PTFE (polytetrafluoroethylene) wipers, which are
moving at a rate of 3 metre per second. The velocity of the film is 1.5
metres per second. Since the surface is already heated, the liquid film
evaporates directly. The vapour (molecules) travels its mean free path and
strikes the condenser. The condensate is collected into a vessel. The residue
(undistilled or mean free path not travelled) is collected from the bottom of
the vessel and re-circulated through the feed port for further distillation.
Capacity is about 1000 litre per hour.
Contd….
Centrifugal Molecular Still
Principle : In this method, liquid feed is introduced into a vessel, which is
rotated at very high speed (centrifugal action). On account of heating,
vaporisation occurs from a film of liquid on the sides of the vessel. The
vapour (molecules) travels a short distance and gets condensed on the
adjacent condenser.Each molecule is condensed individually. The distillate is
subsequently collected.
Construction: The construction of a centrifugal molecular still is shown in
Figure . It consists of a bucket-shaped vessel having a diameter of about 1 to
1.5 metre. It is rotated at high speed using a Radiant heaters are provided
externally to heat the fluid in the bucket. Condensers are arranged very close
to the evaporating surface. Vacuum pump is connected to the entire vessel at
the top. Provisions are made for introducing the feed into the centre of the
bucket, for receiving the product and residue for re-circulation.
Contd…
Contd…
Working : Vacuum is applied at the centre of the vessel. The bucket
shaped vessel is allowed to rotate at high speed. The feed is introduced
from the centre of the vessel. Due to centrifugal action of the rotating
bucket, liquid moves outward over the surface of the vessel and forms a
film. Since, the radiant heaters heat the surface, the liquid evaporates
directly from the film. The vapour (molecules) travels its mean free path
and strikes the condenser. The condensate is collected into another vessel.
The residue is collected from the bottom of the vessel and is recirculated
through the feed port for further distillation.
Disadvantages: Construction and operation are more complicated
compared to falling film molecular still.
Contd…
Applications-
(1)Purification of chemicals such as tricresyl phosphate, dibutylphthalate
and dimethyl phthalate.
(2) More frequently used in the refining of fixed oils.
(3) Vitamin A is separated from fish liver oil.
(4)Free fatty acids are distilled at 100 °C. Steroids can be obtained
between 100 °C and 200 °C, while triglycerides can be obtained from 200
°C onwards.
FRACTIONAL DISTILLATION
• Fractional distillation is a process in which vaporisation of liquid mixture
gives rise to a mixture of constituents from which the desired one is
separated in pure form.
• This method is also known as rectification, because a part of the vapour is
condensed and returned as a liquid.This method is used to separate
miscible volatile liquids, whose boiling points are close, by means of a
fractionating column.
• Fractional distillation is different from simple distillation. In simple
distillation, vapour is directly passed through the condenser. In fractional
distillation the vapour must pass through a fractionating column in which
partial condensation of vapour is allowed to occur. In simple distillation,
condensate is collected directly into the receiver, while in fractional
distillation, condensation takes place in the fractionating col-umn, so that a
part of the condensing vapour returns to the still.
Contd…
• Principle- When a liquid mixture is distilled, the partial condensation of the vapour is
allowed to occur in a fractionating column. In the column, ascending vapour from the
still is allowed to come in contact with the condensing vapour returning to the still. This
results in enrichment of the vapour with the more volatile component. By condensing
the vapour and reheating the liquid repeatedly, equilibrium between liquid and vapour is
set up at each stage, which ultimately results in the separation of a more volatile
component.
OR
When you heat a mixture of liquids, some of it turns into vapor. In fractional distillation,
this vapor goes up through a special column. Inside the column: • Some
of the vapor cools down and turns back into liquid. • The rising vapor meets
the falling liquid.
• This helps separate the liquids: the one that boils more easily (the more volatile
one) stays in vapor form and rises higher.
By repeating this process again and again inside the column, you can separate liquids
with close boiling points, because the lighter (more volatile) liquid moves up, and the
heavier one stays lower.
Contd…
• Applications : Fractional distillation is used for the separation of miscible
liquids such as acetone and water, chloroform and benzene.
• Disadvantage : Fractional distillation cannot be used to separatemiscible
liquids, which form azeotropic mixtures.
• Advantages- Fractional distillation is easy to use . Highly effective and
efficient.
CONSTRUCTION
The fractionating column is inserted between the still and the condenser. A
provision is made for the supply of heat (usually a steam coil) at the
bottom of the column. At the top of column, a condenser is provided. The
column has a large area for providing sufficient flow conditions. The
broken lines across the column represent the contacting devices.
Contd…
Contd..
WORKING
The mixture to be distilled is fed to the boiler and heated usually by steam.
The sequence of events occurring in the fractionating column can be
illustrated using the following general example .
Consider a mixture of two miscible liquids A and B containing 20% of A
and 80% B. Liquid A (More Volatile Component, MVC) is having a lower
boiling point than B (Less Volatile Component, LVC). These liquids do not
produce constant boiling point mixture. The boiling point composition
curves of this mixture are shown in Figure.
Contd…
1. Start with a mixture: • A mixture of two liquids — A (more volatile)
and B (less volatile) is taken. • Example: 20% A and 80% B.
2. Heating in the distillation flask: • The mixture is heated in the boiler. •
When it starts boiling, the vapour contains more of the volatile
component A — about 60% A, even though the original liquid had only 20% A.
3. First condensation and re-vaporization: • This 60% A vapour
condenses on a cooler surface in the column.• It is then heated again (re-
vaporized). • This new vapour now contains 90% A (as shown in the
2nd stage in the diagram).
4. Second condensation and re-vaporization: • The 90% A vapour
condenses and is re-heated. • This time, it gives vapour containing
98% A (third stage in diagram).
5. Third condensation and final purification: • The 98% A vapour
condenses again, and after one more round of vaporization, it becomes almost pure
A (more than 98%). • This is now pure component A in vapour form.
6. Final collection: • The pure A vapour reaches the top of the column, where
it is condensed and collected as pure liquid A.
Contd…(Expln..)
Step 1: Initial Vaporization
• When you heat this mixture, both A and B vaporize, but since A is more volatile,
it forms a greater proportion of the vapour.
• From the graph:Liquid with 20% A → gives vapour with 60% A.
Why
• Because A boils more easily, more A molecules enter the vapour than B
molecules.
• So, vapour is always richer in A than the liquid it came from.
Step 2: First Condensation & Re-Vaporization
• The vapour (60% A) rises up and condenses on a cooler surface in the column.
• Now this condensed liquid (60% A) is reheated, causing it to vaporize again.
• From the graph:Liquid with 60% A → gives vapour with 90% A.
Why?
• Again, A is more volatile, so even in this 60% mixture, more A goes into vapour,
increasing A’s concentration to 90%
Contd…
Step 3: Second Condensation & Re-Vaporization
• The 90% A vapour condenses again on a higher tray and is reheated.
• From the graph:Liquid with 90% A → gives vapour with 98% A.
Step 4: Final Stage – Near Pure A
• This 98% A vapour is condensed and re-vaporized once more.
• It becomes almost pure A (above 98%).
• This vapour finally goes to the condenser at the top, where pure liquid A is
collected.
LSO
Contd…
• Construction
1. Boiler: • A large vessel at the base of the apparatus where the feed
mixture is heated.• Contains feed inlet, steam inlet, and outlet.
2. Feed Inlet: • Entry point for the liquid mixture to be separated.
3. Steam Inlet: • Provides steam to heat the feed mixture and assist in
vaporization.
4. Outlet: • Removes the remaining non-volatile components or residue after
distillation.
5. Fractionating Column: • Vertical column above the boiler filled with
trays or packing materials to enhance separation. • Allows rising
vapors and descending liquids to interact, promoting efficient fractionation.
6. Condenser: • Cools and condenses the vapor into liquid form. •
Positioned at the top of the fractionating column.
7. Divider:• Divides the condensed liquid into two parts: product and reflux.

8. Reflux Line: • Returns part of the condensed liquid back to the column
to improve separation efficiency.
Contd..
Working
1. The feed mixture is introduced into the boiler through the feed inlet.
2. Steam is supplied through the steam inlet to heat the mixture.
3. The mixture boils, forming vapors that rise through the fractionating
column.
4. As vapors ascend, they encounter descending liquid reflux, which creates
repeated condensation and vaporization cycles—this enhances separation
based on boiling points.
5. The more volatile components move higher and eventually reach the
condenser, where they are condensed into liquid.
6. The condensed liquid flows to the divider, where part is collected as
product and part is returned as reflux.
7. The less volatile components condense lower in the column or return to
the boiler as liquid, eventually exiting through the outlet.

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