CHAPTER 1

1.1 INTRODUCTION

The function of distillation is to separate, by vaporization, a liquid mixture of

miscible and volatile substances into individual components or, in some cases , into
groups of components; of liquid air into nitrogen, oxygen, argon ;and of crude
petroleum into gasoline, kerosene, fuel oil, and lubricating stock are examples of
distillation. Suppose there are two components, A and B. Both of these components
are found in both phases. There are four variables: pressure, temperature, and
concentration of component A in the liquid and vapor phases (the concentrations of
component B are unity less those of concentrations of A). If the pressure is fixed, only
one variable, e.g, liquid-phase concentration, can be changed independently and
temperature and vapor-phase concentration follow.

Flash (equilibrium) distillation is a single-stage continuous operation where a

liquid mixture is partially vaporized, the vapor produced and the residual liquid are in
equilibrium, which are then separated and removed.

Flash distillation (sometimes called "equilibrium distillation") is a single stage

separation technique. A liquid mixture feed is pumped through a heater to raise the
temperature and enthalpy of the mixture. It then flows through a valve and the pressure is
reduced, causing the liquid to partially vaporize. Once the mixture enters a big enough
volume (the "flash drum"), the liquid and vapor separate. Because the vapor and liquid
are in such close contact up until the "flash" occurs, the product liquid and vapor phases
approach equilibrium.
Simple flash separations are very common in industry, particularly petroleum refining.
Even when some other method of separation is to be used, it is not uncommon to use a
"pre-flash" to reduce the load on the separation itself.
Flash calculations are very common, perhaps one of the most common Ch.E.
calculations. They are a key component of simulation packages like Hysis, Aspen, etc.
When designing a flash system it is important to provide enough disengaging space in
the drum. Drums can also be designed as cyclone separators.

1
 The distillation performed on a laboratory scale often uses batches of the liquid
mixture whereas industrial distillation processes are generally continuous, requiring a
constant composition of the mixture to be maintained. For a mixture of liquids, the
distillation process is dependent on Dalton’s law and Raoult’s law. As per Raoult’s law,
the partial pressure of a single liquid component in an ideal liquid mixture equals the
product of the vapor pressure of the pure component and its mole fraction. According to
Dalton’s law of partial pressures, the total pressure exerted by a mixture of gases is equal
to the sum of the partial pressures of all the constituent gases. when a mixture of a
liquids is heated, the vapor pressure of the individual components increases the total
vapor pressure. Therefore, the mixture cannot have multiple boiling points at a given
composition and pressure.
There are different types of distillation which includes:
 Simple distillation
 Fractional distillation
 Steam distillation
 Vacuum distillation
 Air sensitive vacuum distillation
 Short path distillation
 Zone distillation.

In this experiment, we are concerned with flash distillation

Flash distillation is one of the simplest separation processes. A liquid stream containing
several components is partially vaporized in a "flash drum" at a certain pressure and
temperature. This results in two phases: a vapor phase, enriched in the more volatile
components, and a liquid phase, enriched in the less volatile components. The fluid is
pressurized and heated and is then passed through a throttling valve or nozzle into the
ash drum. Because of the large drop in pressure, part of the fluid vaporizes. The vapor is
taken overhead, while the liquid drains to the bottom of the drum, where it is withdrawn.
The system is called "flash distillation because the vaporization is extremely rapid after
the feed enters the drum. Because of the intimate contact between liquid and vapor, the
system in the ash chamber is very close to an equilibrium stage.

2
1.2 AIMS AND OBJECTIVES
1. To determine the relative volatility (α) of ethanol in water.
2. To determine the number of theoretical plates of distillation column using Mc
Cabe and Thiele method.

1.3 SIGNIFICANCE OF EXPERIMENT

Flash distillation can be used in the following process:
1. Petroleum distillation in which you separate different chemicals that make up
petroleum.
2. Lighter hydrocarbons (such as propane and butane, typically used ingas lighters)
are taken from stages high up in the distillation column.
3. Dissemination of sea water.
4. Separation of atmosphere into unique elements such as oxygen, nitrogen and
argon.
5. Perfumes and food flavorings are obtained from herbs and plants through
distillation.
6. Fermented products such as alcoholic beverages are purified with the help of this
method.

3
 CHAPTER TWO
2.1 THEORETICAL BACKGROUND

Flash distillation is a special operation within distillation, where a liquid mixture is

heated up and fed – with constant flowrate – into a distillation equipment. The resulting
vapor and liquid phases enter a phase separator – an equilibrium chamber – and are
drained separately. During the operation, the total pressure and temperature of the
system, as well as the compositions of the two phases in equilibrium remain constant
over time. One implementation of this operation is shown in Figure 1.

The mixture to be separated is fed from the feed tank (1) by a pump (2) through a
heat exchanger (3) at pressure P3. Here, it is heated above the boiling point it would
have at P5, the pressure inside the phase separator (5). The pressure of the mixture is
then decreased by flowing it through a valve (4), so that it partially evaporates and yields
a vapor and liquid phase with equilibrium compositions.
Based on Figure 1, the following balance equations can be obtained: mass balance
F L V (Eq.1) component balance:
Fx Lx Vy F (Eq.2)
All necessary calculation can be carried out by using balance equations (Eq.1) and
(Eq.2). The balance equations are valid whether using molar flows or mass flows.
FxFV; y
L; x P3 > P5
Another implementation of flash distillation is feeding a mixture of quantity F and
composition xF into a heated tank, yielding a liquid phase of quantity L and composition
x, and a vapor phase of quantity V and composition y (which is the equilibrium
composition for liquid phase composition x). (Eq.1) and (Eq.2) apply in this case as well,
thus all results are calculated with the same methods. This second implementation
requires a startup period, which will be explained in detail later.

4
Flash ("equilibrium distillation") is a single stage separation technique. A liquid mixture
feed is pumped through a heater to raise the temperature and enthalpy of the mixture. It
then flows through a valve and the pressure is reduced, causing the liquid to partially
vaporize. Once the mixture enters a big enough volume (the "flash drum"), the liquid and
vapor separate. Because the vapor and liquid are in such close contact up until the "flash"
occurs, the product liquid and vapor phases approach equilibrium.
Simple flash separations are very common in industry, particularly petroleum refining.
Even when some other method of separation is to be used, it is not uncommon to use a
"pre-flash" to reduce the load on the separation itself.
Flash calculations are very common, perhaps one of the most common Ch.E.
calculations. They are a key component of simulation packages like Hysis, Aspen, etc.
When designing a flash system it is important to provide enough disengaging space in
the drum. Drums can also be designed as cyclone separators.

5
 CHAPTER THREE
3.1 DESCRIPTION OF APPARATUS
The following are the apparatus used during the experiment.
ROUND BOTTOM FLASKS: they are the types of flasks having a spherical bottoms
used as a laboratory glassware, mostly for chemical or biochemical work. They are
typically made of glass for chemical inertness and in modern days, they are usually made
of heat-resistant borosilicate glass. They are used for heating or boiling liquid,
distillation. It was used during the experiment to heat the mixture of ethanol and water.

Fig 3.1.1
CONDENSER: It is a device or unit used to condense vapor into liquid.

Fig 3.1.2

HEATING MANTLE: It is also known as isomantle, is a piece of laboratory equipment

used to apply heat to containers as an alternative to other forms of heated bath.

Fig 3.1.3
MEASURING CYLINDER: It is also known as graduated or mixing cylinder. It is a
common piece of laboratory equipment used to measure the volume of a liquid. It has a
narrow cylindrical shape each marked line on the graduated cylinder represents the
amount of liquid that has been measured. It was used during the experiment to measure
the volume of ethanol, water and the condensate.
6
 Fig 3.1.4
BEAKER: A beaker is a cylindrical container used to store, mix and heat liquids in
laboratories. Most are made of glass, but other non-corrosive materials, such as metal
and heat-resistant plastic, are also used. Beakers usually have a flat bottoms and a lip
around the top (beak) use for pouring solution easily. It was used to take and mix the
fluid to be used( ethanol and water).

d
Fig 3.1.5 Beaker

HOSE: It is a tubular section or hollow cylinder, usually but not necessarily of circular
cross-section, used mainly to convey substances which can flow liquids and gases
(fluids), slurries, powders and masses of small solids. It aids the flow of water during the
experiment.

3.2 EXPERIMENTAL PROCEDURE

7
 The alcohol percentage in the ethanol given was measured. 50ml of water and
100ml of ethanol was measured and mixed thoroughly and the alcohol percentage was
also measured using and alcohol meter.
The feeds (water and ethanol) was charged into the round bottom flask 50ml of water
and 100ml of ethanol. The vessel was connected to the distillation column and the
mixture was heated to its boiling point, the temperature used in this experiment was 80 oc.
The vapor was passed through a condenser which condensed the vapor. As the vapor
condensed, the condensate was collected and the volume and the alcohol percentage was
measured at the interval of 5minutes.

8
CHAPTER FOUR
4.1EXPERIMENTAL RESULTS
Initial alcohol content – 72%
Volume of alcohol used – 100ml
Volume of water used – 50ml
Temperature used – 800C
Alcohol content in solution (alcohol + water) = 69%
S/N TIME Volume Volume of Mole Mole Alcohol
(minutes) of remaining fraction in fraction in Content
condensat liquid (ml) vapour liquid recovered
e (ml) phase (Y) phase (X) (%)
1 5 0 100 0 1 0
2 10 10 90 0.10 0.9 10
3 15 28 62 0.31 0.69 28
4 20 26 36 O.42 0.58 26
5 25 23 13 0.64 0.36 23
6 30 16 -3 1.23 0.23 16
Table 4.1.1 Data obtained for the flash distillation of Ethanol and Water
CALCULATION FOR MOLE FRACTION IN VAPOUR PHASE(Y)
0
1. Y = 100 =0

10
2. Y = 100 =0.10

28
3. Y = 90 =0.31

26
4. Y = 62 =0.42

23
5. Y = 36 =0.64

16
6. Y = 13 =1.23

CALCULATION FOR MOLE FRACTION IN LIQUID PHASE (X)

X=1-Y
1) X = 1 - 0 = 1
9
2) X = 1 – 0.10 = 0.9

3) X = 1 – 0.31 = 0.69

4) X = 1 – 0.42 = 0.58

5) X = 1 – 0.64 = 0.36

6) X = 1 – 1.23 = -0.23

CALCULATION FOR RELATIVE VOLATILITY

y (1−x )
α¿ x(1− y )

0(1−1)
1. α¿ 1(1−0) = 0
0.1(1−0.9)
2. α¿ 0.9(1−0.1) = 0.012
0.31(1−0.69)
3. α¿ 0.69(1−0.31) = 0.202
0.42(1−0.58)
4. α¿ 0.58(1−0.42) = 0.524
0.64(1−0.36)
5. α¿ 0.36(1−0.64) = 3.16

Using Mc Cabe and Thiele method

The values of X ranges from 0 to 1.

The values of X assumed are: 0, 0.2, 0.4, 0.6, 0.8, 1

αX
Using equation Y = 1+(α −1) X

α = 3.16

For X= 0
3.16 X 0
Y = 1+(3.16−1)0 = 0

For X= 0.2
3.16 X 0.2
Y = 1+ ( 3.16−1 ) 0.2 = 0.44

For X= 0.4

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 3.16 X 0.4
Y = 1+ ( 3.16−1 ) 0.4 =0.68

For X= 0.6
3.16 X 0.6
Y = 1+ ( 3.16−1 ) 0.6 =0.83

For X= 0.8
3.16 X 0.8
Y = 1+ ( 3.16−1 ) 0.8 =0.93

For X= 1
3.16 X 1
Y = 1+(3.16−1)1 =1

The new table becomes:

S/N X(mol) Y(mol)

1 0.0 0.0
2 0.2 0.44
3 0.4 0.68
4 0.6 0.83
5 0.8 0.93
6 1.0 1.0
Table 4.1.2 Data obtained for the flash distillation of Ethanol and Water using the
relative volatility

Plot the graph of X(mol) against Y(mol)

The distillate recovered for this experiment (D) was 50ml

To get 87% purity, XD = 0.36

L = 100ml
L 100
Also, RD = D = 50 = 2

To find the Intercept using the Top Column Equation =

11
 R 1
Yn = R +1 Xn+1 + R +1 XD

1 1
Intercept = R +1 XD = 2+ 1 × 0. 36= 0.12

The rectifying section operating line was joined from 0.12 to the XD line.

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4.2DISCUSSION OF RESULT

The results and calculations have shown the following;

For separation to be achieved, relative volatility must be greater or equal to unit. For the
more volatile component, volatility increases above 1 and separation becomes easier. For
an ideal system the volatility is numerically equal to the vapor pressure of the pure
component.

13
CHAPTER FIVE
5.1 CONCLUSION
Being able to perform experiments on the flash distillation column was very
useful task as it provides practical experience in using the theoretical knowledge
acquired in the unit operation class throughout the semester.

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 5.2 RECOMMENDATION
In view of the outcome of the experiment, the following recommendations were
made:
 Water supply should be available and reliable.
 The readings should be taken when the system is stabilized.

15
REFERENCES

1. McCabe, W.L; Smith.J.C. and Harrortt,P.(2001). Unit operation of

Chemical Engineering (6th Edition, Singapore)
2. Perry, R.H and Green D.W(1997) Chemical Engineers’Handbook
(Seventh Edition). McGraw Hill. New York.
3. Douglas, J.F; Gasiorek, J.M. and swaffied, J.A. (1995). Fluid mechanics
(3rd Edition). Addition Wesley Longman limited, England.
4. Chemical Engineering Manual (University of Ilorin).
5. Standards of the Tubular Exchanger Manufacturers Association
(TEMA), 9th edition, 2009
6. EN 13445-3 "Unfired Pressure Vessels - Part 3: Design", Section 13
(2012)
7. ASME Boiler and Pressure Vessel Code, Section VIII, Division 1, Part
UHX

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