OBJECTIVES

To know and understand the fundamental principles of distillation as a unit

operation

To have a grasp on the mechanisms of a basic distillation process

To learn and familiarize the applications of distillation in the industry

BASIC CONCEPTS

In the field of Chemical Engineering separation process is the transfer of

any mass that converts the substance mixture into distinctive product mixtures. In
some cases, a separation may fully divide the mixture into its pure constituents.
Separations are carried out based on differences in chemical properties, or physical
properties such as size, shape, mass, density, or chemical affinity, between the
constituents of a mixture, and are often classified according to the particular
differences they use to achieve separation.

In most cases one single difference is used to attain a desired separation;

however multiple processes are implemented in combination to attain the desired
solution. Apart from a few cases, compounds and elements are found naturally in an
impure state and these impure materials needs to be separated for purification.
There are a large number of types of separation processes, including distillation,
extraction, absorption, membrane filtration, and so on. Each of these can also be
used for purification, to varying degrees.

Distillation is the process of heating a liquid until it boils, then condensing

and collecting the resultant hot vapors. This process is used to separate a pure
liquid from a mixture of liquids. It works when the liquids have different boiling
points. (www.essentialchemistry.com)

Distillation was probably first used by ancient Arab chemists to isolate

perfumes. Vessels with a trough on the rim to collect distillate, called diqarus, date
back to 3500 BC.

Distillation is the oldest and the most universal process of chemical

technology and other branches of industry incorporating separation of mixtures. It
has substantial advantages over other processes applied in order to separate a
mixture, such as extraction, crystallization, semipermeable membranes, etc. As a
rule, it is the most cost-effective process, so it may be used for mixtures with very
diverse properties. This process is based on the fact that the composition of the
boiling liquid and that of the vapor over it differ. Thus, if the boiling temperature is
low, it is necessary to use low-temperature refrigerants and conduct the process at
a higher pressure. If it is high, high-temperature heat carriers or fire preheating
have to be used and the process is run under vacuum.

The following are the general types of distillation:

Simple distillation - In this process, the liquids are separated by

evaporating and capturing them at various points in their cooling cycle, and
then immediately channeled into a condenser. Simple distillation is used for a
mixture in which the boiling points of the components differ by at least 158F
(70C). It is also followed for the mixtures contaminated with nonvolatile
particles (solid or oil), and those that are nearly pure with less than 10
percent contamination.

Source: http://www.otec.ws/pure_water_products.html
Figure 2.1. Desalination of water process through simple distillation

Vacuum distillation This form of distillation relies on the basic principle

that boiling occurs when vapor pressure exceeds ambient pressure for a
liquid. The pressure above the liquid being distilled is reduced via vacuum to
below its vapor pressure, causing it to boil and rise through the column. This
may or may not require heating.

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 Figure 2.2. Vacuum Distillation in Petroleum Refining
Source: www.britannica.com
Fractional distillation Distillation process where chemical components
are separated into fractions based on their properties

Source: http://pythagorasandthat.co.uk
Figure 2.3. Fractional Distillation of Liquid Air to produce Nitrogen Gas

Steam distillation Distillation system used for temperature sensitive

materials or materials that begin eroding at sustained high temperatures. By
adding water or steam to the distillation process, the boiling temperatures of
the other substances are brought down, allowing lower temperatures to be
used.

2
 Source: http://herb-
education.eu/angoldvd/gi3.html
Figure 2.4. Extraction of Essential Oils through Steam Distillation

TYPES OF DISTILLATION COLUMNS

There are many types of distillation columns, each are designed to perform
specific types of separation, and each design differs in terms of complexity. One
way of classifying distillation column type is to look at how they are operated and
are as follows:

1. Batch Columns

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.

2. Continuous Columns

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.

Classification of continuous Columns

1. The nature of feed that they are processing

a. Binary Column feed contains only two components
b. Multi-component Column feed contains more than two
components
2. The number of product streams they have

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 a. Multi-product Column column has more than two product
streams
3. To where the extra feed exits when it is used to help with
the separation
a. Extractive distillation - where the extra feed appears in the
bottom product stream
b. Azeotropic distillation where the extra feed appears at the
top product stream
4. The type of column internals
a. Tray Column where trays of various designs are used to
hold up the iquid to provide better contact between vapour
and liquid, hence better separation
b. Packed Column where instead of trays, packings are used
to enhance contact time between vapour and liquid.

BASIC DISTILLATION EQUIPMENT AND OPERATION

Major Components of a Typical Distillation Column

1. Vertical Shell the separation of liquid components is carried out.

2. Trays/ Plates/ Packings used to enhance component separation
3. Reboiler - provide the necessary vaporization for the distillation
4. Condenser To cool and condense the vapour leaving the top of the column
5. Reflux Drum to hold the condensed vapour from the top of the column so
that a liquid (reflux) can be recycled back to the column.

BASIC OPERATION AND TERMINOLOGY

The liquid mixture that is to be processed is known as the feed and this is
introduced usually somewhere near the middle of the column to a tray known as the
feed tray. The feed tray divides the column into a top (enriching or rectification)

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section and a bottom (stripping) section. The feed flows down the column where it is
collected at the bottom in the reboiler.

Heat is supplied to the reboiler to generate vapour. The source of heat input
can be any suitable fluid, although in most chemical plants this is normally steam.
In refineries, the heating source may be 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.

The vapour moves up the column, and as it exits the top of the unit, it is
cooled by a condenser. The condensed 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.

Thus, there are internal flows of vapour and liquid within the column as well
as external flows of feeds and product streams, into and out of the column.

EQUIPMENTS USED AND MECHANISM

The following is an illustration of a simple distillation setup.

Source: http://chemistry.tutorvista.com/inorganic-
Figure 3.1. Apparatuses included in a Simple Distillation Setup
chemistry/distillation.html

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 For the mechanism of a simple distillation, imagine a mixture of three liquids,
A, B, and C. A has a boiling point of 86F; B has a boiling point of 104F; and C has a
boiling point of 122F.

The three-liquid mixture described above is added to a distillation flask.

The mixture in the flask is heated by a Bunsen burner. Liquid A begins to boil
when the temperature in the flask reaches 86F. It turns into a vapor at that
temperature, rises in the distilling flask, and passes out of the flask arm into the
condenser.

The condenser consists of a long tube surrounded by a larger tube. The

outer tube contains water, which enters near the bottom of the condenser and
leaves near the top. The water passing through the outer jacket of the condenser
cools the vapor passing through the inner tube. The vapor loses heat and
condenses. It flows out of the condenser and into a receiving container. The liquid
is now known as the distillate, or the product of the distillation.

Meanwhile, the temperature in the distilling flask has not changed, as

indicated by the thermometer in the mouth of the flask. Heat added to the liquid
mixture is used to vaporize liquid A, not to raise the temperature of the mixture.
That temperature will begin to rise only when liquid A has completely boiled away.
By watching the thermometer, therefore, an observer can know when liquid A has
been completely removed from the liquid mixture. At that point, the receiver
containing pure liquid A can be removed and replaced by a new receiver.

Once liquid A has boiled away, the temperature in the distilling flask begins
to rise again. When it reaches 104F, liquid B begins to boil away, and the sequence
of events observed with liquid A is repeated. Eventually, pure samples of A, B, and C
can be collected.

For the summary, the following is the sequence of events in distillation:

HEATING EVAPORATING COOLING

CONDENSING

GENERAL TYPES OF DISTILLATION COLUMNS

Packed Bed Distillation Column

Packed bed columns are often used to recover solvents. Differences in

concentration cause the less-volatile components to transfer from the vapor phase
to the liquid phase. The packing increases the time of contact, which increases the
separation efficiency. The exiting vapor contains the most volatile components,
while the liquid product stream contains the least volatile components.

6
 Copyright: Sulzer Chemtech Ltd., Switzerland
Figure 3.2. Packed Bed Columns used in an ethanolamine plant

Mechanism

The feed mixture contains components of different volatilities, and

enters the column approximately at the middle. After the feed mixture enters
the column liquid flows down the column through the packing
countercurrently and contacts the rising vapor stream. The liquid at the
bottom enters a reboiler. Two streams exit the reboiler; a vapor stream, which
returns to the column, and a liquid product stream. The vapor stream flows
upward through the packing, picks up the more volatile components, exits
the column, and enters a condenser. After the vapor condenses, the stream
enters a reflux drum, where it is split into an overhead product stream, known
as the distillate, and a reflux stream that is recycled back to the column.

Source: http://encyclopedia.che.engin.umich.edu
Figure 3.3. Parts of Packed Bed Distillation Column

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Plate or Tray Column

The plate, or tray column is the most widely used type of distillation column.
The number of trays, or stages in the column is dependent on the desired purity and
difficulty of separation. The number of stages also determines the height of the
column.

Copyright: Odfjell, Norway

Figure 3.4. 40-Tray Column used for mineral oils

Mechanism

The feed enters a plate column towards the middle of the column. After
the feed mixture enters the column liquid flows down the column and across
the trays in either crossflow or countercurrent flow. A reboiler at the bottom
separates the stream into a vapor stream that returns to the column and a
liquid product stream. The vapor stream flows upward through the trays, and
contacts the down-flowing liquid stream, allowing the separation to take
place. At the top of the column, the vapor is condensed in a condenser. The
condensed stream is split into an overhead product stream, known as the
distillate, and a reflux stream that returns to the top of the column.

8
 Source: http://encyclopedia.che.engin.umich.edu

Figure 3.5. Mechanism of Tray Column

COLUMN INTERNALS
For Tray and Plates
1. 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.
2. 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.
3. 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.

Packings

1. Random Packing
2. Grid Packing
3. Structured Packing

PACKING VS. TRAYS

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 A tray column that is facing throughput problems may be de-bottlenecked
by replacing a section of trays with packings. This is because:
1. packings provide extra inter-facial area for liquid-vapour contact
2. efficiency of separation is increased for the same column height
3. 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.

DISTILLATION PRINCIPLES
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.

VAPOR PRESSURE AND BOILING

The vapour pressure of a liquid at a particular temperature is the equilibrium
pressure exerted by molecules leaving and entering the liquid surface. Here are
some important points regarding vapour pressure:
1. energy input raises vapour pressure
2. vapour pressure is related to boiling
3. a liquid is said to boil when its vapour pressure equals the surrounding
pressure
4. the ease with which a liquid boils depends on its volatility
5. liquids with high vapour pressures (volatile liquids) will boil at lower
temperatures
6. the vapour pressure and hence the boiling point of a liquid mixture
depends on the relative amounts of the components in the mixture
7. distillation occurs because of the differences in the volatility of the
components in the liquid mixture

THE BOILING POINT DIAGRAM

The boiling point diagram shows how the equilibrium compositions of the
components in a liquid mixture vary with temperature at a fixed pressure. Consider
an example of a liquid mixture containing 2 components (A and B) - a binary
mixture. This has the following boiling point diagram.
The boiling point of A is that at which the mole fraction of A is 1. The boiling
point of B is that at which the mole fraction of A is 0. In this example, A is the more
volatile component and therefore has a lower boiling point than B. The upper curve
in the diagram is called the dew-point curve while the lower one is called the
bubble-point curve.

The dew-point is the temperature at which the saturated vapour starts to

condense.

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 The bubble-point is the temperature at which the liquid starts to boil

This difference between liquid and vapour compositions is the basis for
distillation operations.

APPLICATIONS

General Applications

Distillation is a powerful tool both for the identification and the

purification of organic compounds. The boiling point of a compound is one of
the physical properties used to identify it. Distillation is used to purify a compound
by separating it from a non-volatile or less-volatile material. When different
compounds in a mixture have different boiling points, they separate into individual
components when the mixture is carefully distilled.

Specific Applications

Laboratory Scale Applications

Distillation has long been used as the separation process in the

chemical and petroleum industries because of its reliability, simplicity, and
low-capital cost. It is employed to separate benzene from toluene,
methanol or ethanol from water, acetone from acetic acid, and many
multicomponent mixtures.

Sample Application with Illustration

Distillation is commonly used to separate ethanol - the alcohol in alcoholic

drinks - from water.

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Source:http://www.bbc.co.uk/schools/gcsebitesize/science/aqa/crudeoil/crudeoilrev2.
shtml
Figure 4.1. Heating water and ethanol mixture

Source:http://www.bbc.co.uk/schools/gcsebitesize/science/aqa/crudeoil/crudeoilrev2.
shtml
Figure 4.2. Evaporation and Condensation of ethanol

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Source:http://www.bbc.co.uk/schools/gcsebitesize/science/aqa/crudeoil/crudeoilrev2.
shtml
Figure 4.3. Total separation of ethanol from water

Industry scale applications

Distillation is widely used in industry, for example in the manufacture

and purification of nitrogen, oxygen and the rare gases. However, one
of its best known uses is the refining of crude oil into its main fractions,
including naphtha, kerosene and gas oil.

Sample Applications with Illustration

Source:http://www.essentialchemicalindustry.org/processes/distillation.html
Figure 4.4. Fractional Distillation of Crude Oil

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 Source: http://allcars.pw.html/
Figure 4.5. Distillation of Water for Injection

Other Fields of Application

a. Pharmaceutical
b. Food Processing
c. Oil Refining
d. Cosmetics
e. Production of Various Chemicals

TRIVIAS

1. Alchemists believed that distillation released the essence or spirit of a

substance.

Stradamus (Circa 1550)

Figure 5.1. Ancient alchemists performing distillation

2. Jabir B. Hayyan described distillation using an alembic in the 8th century.

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 Source: http://www.montgomerydistillery.com/our-process/distilling/
Figure 5.2. Arabic Distillation

3. Whiskey and whisky are both made from grain. Whiskey is the usual American
spelling, especially for beverages distilled in the U.S. and Ireland. Whisky is
the spelling for Canadian and Scotch distilled beverages

Source: http://www.askmen.com/
Figure 5.3. Famous alcoholic drink, Jack Daniels and Tennessee Whiskey

4. It was a Persian doctor, Avicenna (980-1037), who was the first to obtain the
oil from flowers, known as attar, by distillation. Before this revelation,
perfumes were derived from the bark of twigs and shrubs in the form of
resins. His works were faithfully followed by other chemists, soon becoming
general practice.

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 Source: http://www.crytalinks.com/
Figure 5.4. Persian Doctor Avicenna

REFERENCES

http://www.bbc.co.uk/schools/gcsebitesize/science/edexcel_pre_2011/oneearth/fuels
rev1.shtml
http://www.scienceclarified.com/everyday/Real-Life-Chemistry-Vol-2/Distillation-and-
Filtration-Real-life-applications.html
http://science.jrank.org/pages/2122/Distillation-Applications.html
http://www.essentialchemicalindustry.org/processes/distillation.html
http://orgchem.colorado.edu/Technique/Procedures/Distillation/Distillation.html
http://www.slideshare.net/kumarsachin3801/distillation-column
http://www.mitaoe.ac.in/different-types-list-of-separation-processes-in-chemical-
engineering
http://www.montgomerydistillery.com/our-process/distilling/
http://www.encyclopedia.com/topic/distillation.aspx
http://science.jrank.org/pages/2122/Distillation-Applications.html#ixzz41ecusn7b
http://www.buzzle.com/articles/types-of-distillation.html
http://encyclopedia.che.engin.umich.edu/Pages/SeparationsChemical/DistillationCol
umns/DistillationColumns.html
http://articles.compressionjobs.com/articles/oilfield-101/2710-distillation-columns-
towers-column-control-?start=1

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