UNIT

OPERATION:

Riczel Mariz A. Balitaan | ChE-3202

  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

A unit operation is any part of potentially multiple-step process which can be

considered to have a single function. Separation process is one of example of a unit operation.
(www.britannica.com)

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

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 the components differ by at least 158°F (70°C). 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.

Source: www.britannica.com
Figure 2.2. Vacuum Distillation in Petroleum Refining

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 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.

Source: http://herb-education.eu/angoldvd/gi3.html

Figure 2.4. Extraction of Essential Oils through Steam Distillation

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 The following is an illustration of a simple distillation setup.

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

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

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 86°F. 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

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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 104°F, 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.

Copyright: Sulzer Chemtech Ltd., Switzerland

Figure 3.2. Packed Bed Columns used in an ethanolamine plant

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  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

 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.

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 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.

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

Figure 3.5. Mechanism of Tray Column

 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.

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 Sample Application with Illustration

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

from water.

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

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

Stradamus (Circa 1550)

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 Figure 5.1. Ancient alchemists performing distillation

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

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 Daniel’s 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

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 from the bark of twigs and shrubs in the form of resins. His works were faithfully
followed by other chemists, soon becoming general practice.

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

Distillation, by definition, is the process of heating a liquid until it boils, then condensing
and collecting the resultant hot vapors. This unit operation is under the category of liquid-liquid
separation. In the process of performing separation of components, there must be a certain
difference regarding the properties of the participating components. Difference in volatility and
boiling point are the common properties that govern the process of distillation. The separation
process under the principle of distillation may require one or more property difference based on
the complexity of the process to be performed.

The process of distillation, as provided by the information presented, is in a series of

events throughout the process namely: heating, evaporating, cooling and condensing. Heating
is the first process wherein a mixture is heated until a certain temperature where the most
volatile component will start evaporating. In the process of the evaporation, the vapour of the
most volatile component is then directed to the condenser where it is cooled. Cooling of this
vapour is due to the “cold” water entering the other layer of the condenser. The last process is
condensing wherein the separated component goes back to its liquid form after being cooled in
the condenser. This sequence of events for a simple distillation may form a loop if the mixture
contains more than two components.

Distillation, as a unit operation, covers a wide range of applications in the industry. Its
most common and known application is the cracking of crude oil. In this process, large bonds of
hydrocarbons which are composed by crude are broken into fractions through their difference in
boiling points. Distillation can also be used in purifying and identifying unknown components
which is essential to the industry. Other fields of application include pharmaceutical where, for
example, distillation can be used in preparing Water for Injection (WFI). Food processing also

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uses the process of distillation. Alcoholic beverages are common products this unit operation.
Distillation is also used in the process of formulating cosmetic products. Deionized water, as a
product of distillation, is commonly used as a solvent for the said formulation. The application
of distillation process in not limited within the aforementioned fields. Distillation has its
complexity based on the desired output to be produced. It can be done in multiple processes or
in a single process depending on the raw materials as well as the equipment.

http://www.bbc.co.uk/schools/gcsebitesize/science/edexcel_pre_2011/oneearth/fuelsrev1.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

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WHAT: “DRAW IT WITH A TWIST”

RULESand REGULATIONS
1.The class will be divided in two teams.
2.Each group will be asked to prepare 3 words for the other group to guess.
3.The team will choose one member to draw out the word.
4.To draw an illustration of a distillation setup or any apparatus included to is not allowed.
5.Here’s the twist, “the team member to lead the guessing game is not allowed to use
his/her hands to draw”.
6. 30 seconds is allotted to guess every word. If the playing team failed to reveal the
corresponding word, the score will be given to the other group.
7. The team with the most number of points will be considered as the DISTILLATION
CHAMPIONS.

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