CLB20804 Mass Transfer 1 - Assignment Distillation Page |1

NAME : SITI HAJAR MOHAMED

STUDENT ID : 55213114225

SECTION : L02-T01

LECTURER : MADAM AZYYATI BINTI JOHARI

CLB20804 Mass Transfer 1 - Assignment Distillation Page |2

TABLE OF CONTENTS

No. Contents Pages

1. Cover page 1

2. Table Contents 2

3. Introduction 3

4. Differential / Batch Distillation 46

5. Flash / Equilibrium Distillation 78

6. Continuous Distillation with reflux binary system 9 12

7. Comparison between Batch, Flash and Continuous 13 - 14

Distillation

8. Factors enhance purity / productivity of product 15 16

9. References 17 - 18
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INTRODUCTION

i) Definition of Distillation

Distillation is a process of separating the component substances from a liquid mixture by

selective evaporation and condensation. Distillation may result in essentially complete separation

(nearly pure components), or it may be a partial separation that increases the concentration of

selected components of the mixture. In either case the process exploits differences in

the volatility of mixture's components. (Wikipedia)

ii) Type of Distillation

a. Differential / Batch Distillation

b. Flash / Equilibrium Distillation

c. Continuous Distillation

d. Azeotropic Distillation
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QUESTION: DRAW COMPLETE DIAGRAM FOR EACH UNIT & SYMBOLS, AND

DESCRIBE PROCESS OF RESPECTED DISTILLATION.

1) Differential / Batch Distillation

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Based on above batch distillation diagram which refers to distillation in batches, where a

mixture is distilled to separate it into its component fractions before the distillation still and again

charged with more mixture and the process is repeated. This is in contrast with continuous

distillation where the feedstock is added and the distillate drawn off without interruption. Batch

distillation has always been an important part of low capacity and high-purity chemicals and very

frequent separation process in the pharmaceutical industry.

Heating an ideal mixture of two volatile substances A and B (with A having the higher

volatility, or lower boiling point) in a batch distillation setup until the mixture is boiling results

in a vapor above the liquid which contains a mixture of A and B. The ratio between A and B in

the vapor will be different from the ratio in the liquid: the ratio in the liquid will be

determined by how the original mixture was prepared, while the ratio in the vapor will be

enriched in the more volatile compound, A (due to Raoult's Law). The vapor goes through the

condenser and is removed from the system. This in turn means that the ratio of compounds in the

remaining liquid is now different from the initial ratio (i.e., more enriched in B than the starting

liquid). The result is that the ratio in the liquid mixture is changing, becoming richer in

component B. This causes the boiling point of the mixture to rise, which in turn results in a rise

in the temperature in the vapor, which results in a changing ratio of A : B in the gas phase (as

distillation continues, there is an increasing proportion of B in the gas phase). This results in a

slowly changing ratio A : B in the distillate. If the difference in vapor pressure between the two

components A and B is large (difference in boiling points), the mixture in the beginning of the

distillation is highly enriched in component A, and when component A has distilled off, the

boiling liquid is enriched in component B.

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The simplest and most frequently used batch distillation configuration is the batch

rectifier, including the pot still. The batch rectifier consists of a pot (or reboiler), rectifying

column, a condenser, some means of splitting off a portion of the condensed vapor (distillate)

as reflux, and one or more receivers. The pot is filled with liquid mixture and heated. Vapor

flows upwards in the rectifying column and condenses at the top. Usually, the entire condensate

is initially returned to the column as reflux. This contacting of vapor and liquid considerably

improves the separation. Generally, this step is named start-up. The first condensate is the head,

and it contains undesirable components. The last condensate is the feints and it is also

undesirable, although it adds flavor. In between is the heart and this forms the desired product.

The head and feints may be thrown out, refluxed, or added to the next batch of mash/juice,

according to the practice of the distiller. After some time, a part of the overhead condensate is

withdrawn continuously as distillate and it is accumulated in the receivers, and the other part is

recycled into the column as reflux. Owing to the differing vapor pressures of the distillate, there

will be a change in the overhead distillation with time, as early on in the batch distillation, the

distillate will contain a high concentration of the component with the higher relative volatility.

As the supply of the material is limited and lighter components are removed, the relative

fraction of heavier components will increase as the distillation progresses. The other simple

batch distillation configuration is the batch stripper. The batch stripper consists of the same parts

as the batch rectifier. However, in this case, the charge pot is located above the stripping column.

During operation (after charging the pot and starting up the system) the high boiling constituents

are primarily separated from the charge mixture. The liquid in the pot is depleted in the high

boiling constituents, and enriched in low boiling ones. The high boiling product is routed into the

bottom product receivers. The residual low boiling product is withdrawn from the charge pot.
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2) Flash / Equilibrium Distillation

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Based on above flash distillation diagram where the process begins when the salt water

enters a bundle of tubes which are located in the vapor space of the preheat chamber. The water

then flows into a heater consisting of a bundle of tubes which are heated externally by steam.

Here, the water is heated to 100 C, but it does not boil because the pressure is above 1 atm. The

hot sea water then enters a flash chamber which is kept under reduced pressure. The vapors

which are flashed off are then condensed on the tubes carrying the incoming flow of cold sea

water. The distillate and the remaining salt water are then restored to atmospheric pressure by

pumps. Condensing the water by heat exchange with the incoming flow in one of the economical

advantages of this process.

The multiple stage evaporators is able to produce more distillate per unit of heating steam

because the flashing occurs in more than one stage since the flashed vapors are used to heat the

incoming water. For example, using a four stage evaporator, the temperature of the evaporating

salt water is reduced by 10 C and the incoming temperature of the incoming salt water is

increased by the same amount. Instead of the remaining salt water being discharged at 60 C

after only one evaporator, it exits at 30 C after four units. The amount of heating steam required

is only one-fourth of that required for a single unit operation.

In the vapor-reheat process, the vapors in the flash chambers are condensed on a spray or

film of cold distilled water. No metal tube separates the two. As a result, the distilled water

gradually heats up and increases in volume. The hot distillate is then passed through a liquid-

liquid heat exchanger and transfers the heat to an immiscible oil that it is in direct contact with.

The oil then transfers this heat to the incoming sea water. This process has been varied slightly

by some by using a solid rock bed rather that oil.

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3) Continuous Distillation With Reflux Binary System

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Based on above continuous distillation with reflux binary system diagram, the principle

for continuous distillation is the same as for normal distillation. When a liquid mixture is heated

so that it boils, the composition of the vapor above the liquid differs from the liquid composition.

If this vapor is then separated and condensed into a liquid, it becomes richer in the lower boiling

components of the original mixture. This is what happens in a continuous distillation column. A

mixture is heated up, and routed into the distillation column. On entering the column, the feed

starts flowing down but part of it, the components with lower boiling points, vaporizes and rises.

However, as it rises, it cools and while part of it continues up as vapor, some of it (enriched in

the less volatile component) begins to descend again. The diagram also showed a simple

continuous fractional distillation tower for separating a feed stream into two fractions, an

overhead distillate product and a bottoms product. The lightest products (those with the lowest

boiling point or highest volatility) exit from the top of the columns and the heaviest products

(the bottoms, those with the highest boiling point) exit from the bottom of the column. The

overhead stream may be cooled and condensed using a water-cooled or air-cooled condenser.

The bottoms reboiler may be a steam-heated or hot oil-heated heat exchanger, or even a gas or

oil-fired furnace.

In a continuous distillation, the system is kept in a steady state or approximate steady

state. Steady state means that quantities related to the process do not change as time passes

during operation. Such constant quantities include feed input rate, output stream rates, heating

and cooling rates, reflux ratio, and temperatures, pressures, and compositions at every point.

Unless the process is disturbed due to changes in feed, heating, ambient temperature, or

condensing, steady state is normally maintained. If the feed rate and feed composition are kept

constant, product rate and quality are also constant. Even when a variation in conditions occurs,
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modern process control methods are commonly able to gradually return the continuous process

to another steady state again. Since a continuous distillation unit is fed constantly with a feed

mixture and not filled all at once like a batch distillation, a continuous distillation unit does not

need a sizable distillation pot, vessel, or reservoir for a batch fill. Instead, the mixture can be fed

directly into the column, where the actual separation occurs.

Another example continuous distillation with reflux binary system is when a liquid

mixture is heated so that it boils, the evolved vapor will have a higher concentration of the more

volatile (i.e., lower boiling point) components than the liquid mixture from which it evolved.

Conversely, when a vapor mixture is cooled, the less volatile components tend to condense.

Condensation a number of times and each time becomes richer in the more volatile component.

The part of the feed liquid that did not vaporize on entering the column, flows downward and is

heated by contacting the upward flowing hot vapor until it is partially vaporized. The resulting

vapor flows upward and the residual liquid is enriched in the less volatile components and flows

downward. As the liquid continues to flow downward, it undergoes partial vaporization a

number of times and each time becomes richer in the less volatile component. The distillation

trays in the column are designed to facilitate the intimate contacting of upward flowing vapor

with downward flowing liquid.

The overhead vapor that exits the top of the column is rich in the more volatile

component of the column feed and the bottoms liquid which exits the bottom of the column is

rich in the less volatile component of the column feed. Heat is required to provide the multiple

occurrences of partial vaporization in a distillation column. The required heat is applied to the

bottom of a distillation column in a number of ways, the most common being the transfer of heat

from a reboiler. Similarly, cooling is required to provide the multiple occurrences of partial
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condensation that also occur in a distillation column. The required cooling is most usually

provided by a condenser used to cool and condense the overhead vapor into a liquid and then

returning part of the cool condensed liquid to the top of the column as reflux. The overhead

condenser may be water-cooled or air-cooled. The bottoms reboiler may be a heat

exchanger heated by steam or hot oil, or it might be a fuel-fired furnace. The location of the feed

entry can vary from one design to another and is selected to provide optimum result at McCabe

Thiele method. (Citizendium)

A continuous distillation column is kept in a steady state or approximate steady state. In

the context of continuous distillation, that means that the feed rate, output product

rates, refluxrate, heating and cooling rates, temperatures, pressures, and compositions at every

point within the column are essentially kept constant during operation. It also means that the

column is material-balanced and heat-balanced (i.e., the material inputs equal the material

outputs, and the heat inputs equal the heat outputs). If a variation in conditions does occur,

modern process control equipment is usually able to gradually return the system to a steady state

again.
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QUESTION: COMPARE ALL OF THESE 3 TYPES OF DISTILLATION UNIT

Differential / Batch Flash / Equilibrium Continuous Distillation With

Distillation Distillation Reflux Binary System

SIMILARITIES 1. The process of distillation involves the separation of mixture to pure substance.
2. The process of distillation is related to pressure,P (in Pascal) and temperature,T (in
Kelvin) to separate the mixture.
3. The process of distillation consists of mixing and separate two different component
with different volatility.

DIFFERENCES 1. Mixture is distilled to 1. No such heat,q (in 1. Separation in which a

separate it into its Watts) is loss to mixture is continuously
component fractions surrounding (system is in (without interruption) fed
before the distillation still thermal equilibrium). into the process and
is again charged with 2. A single-stage operation separated fractions are
more mixture and the where a liquid mixture is removed continuously as
process is repeated. partially vaporized, vapor output streams.
2. Process involves no produced and residual 2. Complete separation or
reflux and no stages, not liquid are in equilibrium, partial separation of a liquid
needed to distillate two which are then separated feed mixture into
substances. and removed. components or fractions by
3. Liquid is removed 3. Vapor is in Ideal Gas selective boiling
when the process of one state. (or evaporation) and
batch completed. condensation.
3. Separation two or more
components or mixtures.
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APPLICATIONS 1. Major uses of 1. Used to remove salt 1. Very frequent used in the
distillation in the food (NaCl) from sea water to chemical process industries
industry are for get fresh water. and in large quantities of
concentrating essential 2.Desalination of brackish liquids have to be distilled.
oils, flavours and water or ocean water by 2. Used in industries of
alcoholic beverages, Multi-Stage the natural gas
pharmaceutical industry Flash Distillation. processing, petrochemical p
and in the deodorization roduction, coal tar
of fats and oils. processing, liquor
production, liquified
air separation, hydrocarbon
solvents production and also
in petroleum refineries.
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QUESTION: EXPLAIN SOME FACTORS THAT WOULD ENHANCE THE PURITY /

PRODUCTIVITY OF PRODUCT.

To improve the purity or productivity of product, the tower is normally provided inside

with horizontal plates or trays, or the column is packed with a packing material. Next, the purity

of the top product can be improved by recycling some of the externally condensed top product

liquid as reflux. Increasing the reflux ratio will increase and improve the purity of product and

also the separation. When reflux ratio is increased, the amount of reflux increases. Reflux

represents cooled, condensed top product returned to the tower top and, as such it is being

reprocessed. Thus, the top product will therefore be purer. In addition, decreasing the condenser

pressure control of a distillation tower can increased the productivity of product. Later, to

enhance the productivity of product, the temperature of distillation column should be increased.

Lastly, increase in boil up rate will result in only a moderate increase in the purity of the bottoms

product.
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REFERENCES

1. Geankoplis, C. J., Transport Processes and Separation Process Principles. Pearson Education

International, USA. p.706, (2003).

2. Krishna, H. J., Introduction to Desalination Plant, Texas Water Development. (1989).

3. Kister, H. Z., Distillation Operation. McGraw-Hill Professional Publishing Co., New York.

(1990).

4. McCabe, W. L., and Smith, J. C., and Harriott, P., Unit Operations of Chemical Engineering,

6th Ed, McGraw-Hill Publishing Co., New York. (2011).

5. Seader, J. D., and Henley, E. J., Separation Process Principles. John Wiley & Sons, Danvers,

MA, p. 359-387. (1998).

6. Mujtaba, I. M., Batch Distillation Design and Operation, Series on Chemical Engineering,

Vol.3.

7. https://en.m.wikipedia.org/wiki/McCabe-Thiele_Method . McCabe Thiele Method

(Wikipedia), retrieved from 30 September 2015.

8. https://encyclopedia2.thefreedictionary.com/distillation+column Distillation Column (The

Free Dictionary), retrieved from 29 September 2015.

9. https://en.wikipedia.org/wiki/Batch_distillation Batch Distillation (Wikipedia), retrieved from

21 October 2015.

10. https://en.wikipedia.org/wiki/Continuous_distillation Continuous Distillation (Wikipedia),

retrieved from 19 October 2015.

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11. http://www.separationprocesses.com/Distillation/DT_Chp03.htm Flash (Equilibrium)

Distillation (Distillation), retrieved from 19 October 2015.

12. https://en.wikipedia.org/wiki/Flash_evaporation Flash Evaporation (Wikipedia), retrieved

.from 20 October 2015.

13. http://www.rpi.edu/dept/chem-eng/Biotech-Environ/Environmental/desal/flash.html Flash

Distillation (Biotech-Environment), retrieved from 22 October 2015.

14. Perry, J. H., and Don, W. G., Perrys Chemical Engineers Handbook, 7th Ed, McGraw-Hill

Inc., New York, NY. (1997).

15. http://en.citizendium.org/wiki/Continuous_distillation Continuous Distillation (Citizendium),

retrieved from 22 October 2015.