Distillation
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.
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…
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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.
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..
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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.
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.
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.