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DISTILLATION

Distillation is the mass transfer separation technique of preferential separation of the more
volatile component(s) from the less volatile ones by partial vaporization of the feed followed
by condensation of the resulting vapour phase. For a greater degree of separation to be
achieved, a multistage contact arrangement is setup between the liquid and vapour phases
in a suitable equipment known as the Distillation column.

The most important parts of a distillation unit as shown in the diagram below are (a)
A column having trays or a packing and suitable internals (b) A reboiler (which supplies
heat energy to the system), and (c) a condenser (to condense the resultant vapour
phase back to liquid for collection)

Figure 1: Schematic of a typical distillation column


During distillation in a distillation column, an intimate contact between the descending liquid
phase and the ascending vapour phase occurs on the trays or on the packing surface and
exchange of mass takes place between the liquid and the vapour phases. The more volatile
components move from the liquid phase to the vapour phase while the less volatile
component move from the vapour phase to the liquid phase as the vapour rises up the
distillation column.
There is need to at this point, point out a major difference between distillation and
evaporation which also entails separation of a mixture by vaporizing the mixture and
separating the mixture into liquid and vapour phases. Whereas in evaporation a solvent is
removed essentially in its pure form from its liquid mixture with solute(s), in distillation, all
the components are present in both phases and are not really absolutely separated albeit the
concentration of the components in the phases vary as already described above with the
more volatile component(s) having a higher concentration in the vapour phase coming out
from the top of the column (known as top product or distillate) while the less volatile
component(s) will have a higher concentration in the liquid phase coming from the bottom of
the column (known as bottom product)
Table 1: A few examples of separation of liquid mixtures by distillation

N.B: -do- connotes same as above (e.g. petrochemical in the above table)

VAPOUR LIQUID EQUILIBRIUM


Many processes in chemical engineering such as distillation do not only involve a single phase
but a combination of two immiscible phases, or a stream containing both gas and liquid. It is
very important to recognize and be able to calculate when these phases are
in equilibrium with each other, and how much is in each phase. The distribution of the
components to be separated by distillation in the two phases is governed by the vapour
liquid equilibrium relationship of the system. Separation of a mixture by distillation is based
on equilibrium distribution between the liquid and the vapour phases.
More specifically, there are three important criteria for different phases to be in equilibrium
with each other:
1. The temperature of the two phases is the same at equilibrium.
2. The partial pressure of every component in the two phases is the same at
equilibrium.
3. The Gibbs free energy of every component in the two phases is the same at
equilibrium.

Single Component Phase Equilibrium


If there is only a single component in a mixture, there is only a single possible temperature
(at a given pressure) for which phase equilibrium is possible. For example, water at standard
pressure (1 atm) can only remain in equilibrium at 100C. Below this temperature, all of the
water condenses, and above it, all of the water vaporizes into steam.

At a given temperature, the unique atmospheric pressure at which a pure liquid boils is called
its vapor pressure. If the atmospheric pressure is higher than the vapor pressure, the liquid
will not boil.
Multiple-Component Phase Equilibrium: Phase Diagrams
We deal often with equilibrium of mixtures. When a mixture begins to boil, the vapor
does not, in general, have the same composition as the liquid. Instead, the substance with
the lower boiling temperature (or higher vapor pressure) will have a vapor concentration
higher than that with the higher boiling temperature, though both will be present in the
vapor. A similar argument applies when a vapor mixture condenses.
The concentrations of the vapor and liquid when the overall concentration and one of the
temperature or pressure are fixed can easily be read off of a phase diagram. In order to
read and understand a phase diagram, it is necessary to understand the concepts of bubble
point and dew point for a mixture.
Bubble Point and Dew Point
In order to be able to predict the phase behavior of a mixture, scientists and engineers
examine the limits of phase changes, and then utilize the laws of thermodynamics to
determine what happens in between those limits. The limits in the case of gas-liquid phase
changes are called the bubble point and the dew point.
The names imply which one is which:

1. The bubble point is the point (a set of conditions of temperature and pressure) at
which the first drop of a liquid mixture begins to vaporize.
2. The dew point is the point (a set of conditions of temperature and pressure) at which
the first drop of a gaseous mixture begins to condense.

If you are able to plot both the bubble and the dew points on the same graph, you come up
with what is called a Pxy or a Txy diagram, depending on whether it is graphed at constant
temperature or constant pressure. If it is graphed at constant temperature, we get a Pxy
phase diagram and if the Vapor-Liquid Equilibrium (VLE) data is plotted at constant pressure,
we get a Txy phase diagram. The "xy" implies that the curve is able to provide information on
both liquid and vapor compositions.

Txy and Pxy diagrams


The easier of the two diagrams to calculate (but sometimes harder to grasp intuitively) is the
Pxy diagram, which is shown below for an idealized Benzene-Toluene system:
In order to avoid getting confused about what you're looking at, think: what causes a liquid
to vaporize? Two things should come to mind:

Increasing the temperature


Decreasing the pressure
Therefore, the region with the higher pressure is the liquid region, and that
of lower pressure is vapor, as labeled. The region in between the curves is called the two-
phase region.
We can determine, given the mole fraction of one component and a pressure, whether the
system is gas, liquid, or two-phase, which is critical information from a design standpoint.
For example, if the Benzene composition in the Benzene-Toluene system is 40% and the
pressure is 25 mmHg, the entire mixture will be vapor, whereas if the pressure is raised to
50 mmHg it will all condense. The design of a flash evaporator at 20oC would require a
pressure between about 30 and 40 mmHg (the 2-phase region).
We can also determine the composition of each component in a 2-phase mixture, if we
know the overall composition and the vapor pressure. First, start on the x-axis at the overall
composition and go up to the pressure you want to know about. Then from this point, go
left until you reach the bubble-point curve to find the liquid composition, and go to the right
until you reach the dew-point curve to find the vapor composition. See the below diagram.
This method "works" because the pressure must be constant between each phase while the
two phases are in equilibrium. The bubble and dew compositions are the only liquid and
vapor compositions that are stable at a given pressure and temperature, so the system will
tend toward those values.
Another useful rule is the lever rule which can be used to calculate the percentage of all the
material that is in a given phase (as opposed to the composition of the vapor). The lever rule
equation is given thus;
2
% = 1
1 + 2

1
% = 2
1 + 2
Another form of the lever rule is given as;

= 3

Where,
represents the overall composition of the component A in the feed mixture.
The phase whose percent you're calculating is simply the one which you are
going away from for the line segment in the numerator; for example, D2 is going from the
point of interest to the vapor phase, so if D2 is in the numerator then you're calculating
percent of liquid.
Txy diagrams have entirely analogous rules, but just be aware that the graph is "reversed"
somewhat in shape. It's somewhat harder to calculate even in an ideal case, requiring an
iterative solution, but is more useful for isobaric (constant-pressure) systems and is worth
the effort. The extreme ends of the txy diagram are the boiling temperatures of pure
toluene (xb = 0) and benzene (xb = 1) at 760 mmHg.

CALCULATION OF VAPOUR LIQUID EQUILIBRIUM DATA FOR AN IDEAL BINARY SYSTEM


Vapour-liquid Equilibria of ideal solutions is described using Raoults law. The equilibrium
partial pressures of components A and B in a binary liquid mixture is given according to
Raoults law as shown below;
= 4
= (1 ) 5
The total pressure: = + = + (1 ) 6
Where, and are the equilibrium partial pressures of A and B in the vapour;
and are the vapour pressures of A and B at the given temperature.
The mole fraction of A in the vapour is given by;

= = 7

and can be evaluated from the Antoines equation for evaluating the vapour pressures
of substances at a given temperature. The Antoines equation is presented below;

ln = 8
+
With in mm Hg and in 0C. The parameters , and are known as the Antoines
equation constants and have unique values for any particular chemical substances. The values
of these constants for various compounds are available in literature such as Perrys Chemical
engineering handbook.
The above equations can be used to obtain the bubble point curve (T-x), dew point curve (T-
y) and equilibrium curves (y-x) for any given binary system if the pressure is fixed. The
combination of the bubble point curve (T-x) and dew point curve (T-y) make up the Txy
diagram as already depicted above. Same also applies for obtaining the bubble point curve
(P-x), dew point curve (P-y) and equilibrium curves (y-x) for any given binary system if the
temperature is fixed. The procedure basically involves;
a) Find the vapour pressures of A and B ( ) at any reasonably chosen
temperature T( < < ). represent the boiling points of
components A and B respectively.
b) The total pressure P being known, calculate from equation 6 and from equation
7
c) Repeat steps (a) and (b) above at other reasonably chosen temperatures T( < <
) to obtain a set of values of T, and with which The T-x and T-y curves can be
plotted to obtain the Txy diagram and a y-x plot will give the equilibrium curve for the
binary system. This procedure is illustrated in example 1.
Also, to obtain the Pxy diagram at a constant or fixed temperature;
a) Evaluate from the Antoines equation using the fixed value of
temperature.
b) Choose reasonable values of 0 < < 1 and evaluate P using equation 6 and
using equation 7. This will result in a set of P, and values with which the
Pxy diagram can then be obtained.
Bubble Point and Dew Point with Raoult's Law
Key concept
When calculating either a bubble point or a dew point, one quantity is key, and this is
the overall composition, denoted with the letter z. This is to distinguish it from the single-
phase composition in either the liquid or the gas phase. It is necessary to distinguish
between them because the composition of the two phases will almost always be different at
equilibrium.
It is important to remember that the dew and bubble points of a multi-component mixture
are limits. The bubble point is the point at which a very small amount of the liquid has
evaporated - so small, in fact, that in essence, the liquid phase composition remains the
same as the overall composition. Making this assumption, it is possible to calculate the
composition of that single bubble of vapor that has formed.
Similarly, the dew point is the point at which a very small amount of the vapor has
condensed, so that the gas phase composition remains the same as the overall composition,
and thus it is possible to calculate the composition of the single bubble of liquid.

Bubble Point
Let us first consider how to calculate the bubble point (at a constant temperature) of a
mixture of 2 components A and B, assuming that the mixture follows Raoult's Law under all
conditions. To begin, write Raoult's Law for each component in the mixture. Recall equ. 7

= =

For component B, we also have

= =

We can add these two equations together and multiply through by P to get,
) = +
( +

Now since and are mole fractions with A and B being the only components of the
= 1 . In addition, recall that since we are considering the bubble point,
mixture, +
the liquid composition is essentially equal to the overall composition. Therefore =
= . Note that this is only true at the bubble point.
Hence we have the following equation valid at the bubble point for an ideal equilibrium:

= + 9
Therefore, if the temperature and overall composition are known, the bubble pressure can
be determined directly. P represents the bubble point pressure, and can be
calculated from the Antoines equation using the given temperature.
If the pressure is held constant and the bubble point temperature is required, it is necessary
to calculate the temperature by an iterative method. The temperature dependence is
contained in the Antoine equation for vapor pressure of each component. One method to
solve for the temperature is to:
1. Guess a temperature
2. Use the guess and the Antoine equation to calculate the vapor pressure of each
component in the mixture.
3. Calculate an equilibrium pressure using the bubble point pressure equation.
4. If the calculated pressure does not equal the known pressure, it is necessary to
change the temperature and try again.
If there are more than two-components (multi-component mixtures), The Raoults law
equation for calculating the bubble point pressure becomes;
= ( ) 10
Summed over all components i.
Dew Point
The derivation of the dew point pressure equation for a two-component system under
Raoults law is similar to that for bubble point only that since we are dealing with dew point,
we eliminate the liquid phase compositions just as we did the vapor phase compositions when
dealing with the bubble point pressure.
The dew point pressure equation for a two-component system under Raoults law is given by
1
= + 11

For a multi component system having i components, we have that;
1
= ( ) 12

The procedure for determining the dew point temperature at a fixed pressure is similar to
that described for bubble point temperature and requires an iterative method with the major
difference in step 3 of the process in the sense that instead of using the bubble point pressure
equation (equ 9), we would use the dew point pressure equation (equ 11) to evaluate the
pressure which we would then compare with the fixed value to ascertain if our initial guess
of the temperature is correct.
Example 1
Cyclo-pentane (A) and benzene (B) form nearly ideal solutions.
The Antoines equation constant for Cyclo-pentane are A, B and C = 15.8602, 2589.2 and
231.36 respectively while those for Benzene are A, B and C = 15.9037, 2789.01 and 220.79
respectively.
a) Using the vapour pressure data given and assuming ideal behaviour, prepare the
bubble point curve, the dew point curve and the vapour-liquid equilibrium curves for
this binary at 1 atm total pressure.
b) If one kilomole of a two-phase mixture having 42 mole% A at 68oC and 1 atm total
pressure is allowed to separate into a liquid and vapour phase at 1 atm total pressure,
calculate the amounts and compositions of the two phases.
c) If an equimolar mixture of the compounds has a bubble point of 100 oC, calculate the
total pressure exerted at that temperature at equilibrium.

Solution
a) The bubble point and dew point values of a Cyclo-pentane Benzene mixture remains
within 49.2oC (boiling point of pure Cyclo-pentane at 1 atm) and 80oC (boiling point of
pure Benzene at 1 atm). The total pressure remains constant at 1 atm (760mm Hg)
In order to compute the T-x-y data with which we would obtain the T-x-y diagram, we
employ the procedure already outlined previously.
To start with, take T = 70oC. (Note that TA < T < TB as 49.2oC < 70oC < 80oC)

ln = 15.8602 2589.2/(231.36 + 70)


= 1434

ln = 15.9037 2789.01/(220.79 + 70)


= 551

Total pressure, = 760 = (1434) + (1 )(551)


= 0.237
Therefore at = 70oC and = 760 , the mole fraction of A in liquid at equilibrium
is, = 0.237.
1434
Mole fraction of A in the equilibrium vapour, = ( ) = 0.237 ( 760 ) = 0.447
So the bubble point of a liquid at equilibrium having 0.237 mole fraction of A at 1 atm total
pressure is 70oC. This is also the dew point of a vapour at equilibrium having 0.447 mole
fraction of A. So the data are = 70oC, = 0.237 and = 0.447
The bubble and dew points of liquids and vapours of other compositions are similarly
calculated to get a set of T-x-y data with which we plot the dew point curve (T-y), bubble point
curve (T-x) and equilibrium curve (x-y) as shown below. The experimental x-y data are also
shown. It is seen that the deviation from ideal behaviour is small. The system is nearly ideal.
(a) The calculated T-x-y data (Raoults law) for Cyclo-pentane benzene mixtures, and
(b) The experimental x-y data from Mayers, Ind. Eng. Chem. 48(1956) 1104

(b) The state of the feed (68oC; 1 atm; ZAF = 0.42) is represented by the point F that lies in
the two-phase region in the figure above. In order to find the compositions of the liquid and
vapour phases at equilibrium, we draw a horizontal line through F to meet the bubble point
curve at L and the dew point curve at V. The point where the line meets the bubble point
curve (T-x) gives the equilibrium composition of the liquid as = 0.294 and the point
where the line meets the dew point curve (T-y) gives the equilibrium composition of the
vapour as = 0.521
We have that the total amount of mixture = 1
=+ =1
Recalling equation 3, we have

=

By substituting the values of , and and solving the equations above
simultaneously, we find moles of liquid = 0.555 and moles of vapor =
0.445 .

(c) The equimolar composition at bubble point means = 0.5 = 0.5


At a temperature of 100oC, the vapour pressures are calculated using the Antoines
equation to give = 3120.2 = 1350.5

The equilibrium total pressure exerted above an equimolar mixture at 100oC is given by
= + (1 ) = (0.5)(3120.2) + (1350.5)(1 0.5) = 2235.3

Relative Volatility
The relative volatility of a component A in a mixture indicates the ease of its separation from
another component B. It is defined as the concentration ratio of the more volatile component
A in the vapour phase divided by the same ratio in the liquid phase.
It is usually denoted by . For a binary mixture,
/(1 )
= 13
/(1 )


= 14
1 + ( 1)
Equation 14 shows us that an algebraic equation can be established between and if the
relative volatility between A and B is known.
In order to separate a binary mixture using distillation process, there must be a substantial
difference in the volatilities of the components. Being that A is the more volatile component,
should be much greater than 1 if separation by distillation is to be effective. The higher
is than 1, the better the separation process by distillation.
The relative volatility in an ideal binary solution can be expressed in terms of the vapour
pressures of the components as shown below;
/(1 ) ( ) ( )
= = = 15
/(1 ) ( ) ( )

Batch Distillation
In batch distillation, the feed is charged to the still pot to which heat is supplied continuously
through a steam jacket or a steam coil. As the mixture boils, it generates a vapour richer in
the more volatiles. As the boiling continues, concentrations of more volatiles in the liquid
decrease. The vapour is led to a condenser and the condensate or top product is collected in
a receiver. At the beginning, the condensate will be pretty rich in the more volatiles, but the
concentrations of the more volatiles in it will decrease as the condensate keeps on
accumulating in the receiver.
In batch distillation, the condensate is usually withdrawn intermittently having products or
cuts of different concentrations.
Batch distillation is used when the feed rate is not large enough to justify installation of a
continuous distillation unit. It may also be used when the constituents greatly differ in
volatility.

A Batch Distillation set-up

When small amounts of products of varying compositions are required, a batch distillation
provides several advantages over the continuous distillation.
Batch distillation is versatile and commonly employed for producing biochemical, biomedical,
and/or pharmaceutical products, in which the production amounts are small but a very high
purity and/or an ultra-clean product is needed

Material Balance for Simple Batch distillation

Theoretical analysis of batch distillation is based on a differential mass balance because the
liquid and the vapour phase concentrations of the components change continuously as
distillation proceeds. Let, at any moment, the number of moles of liquid in the still be L having
a mole fraction x of the more volatile component (i.e. A) and let the moles of accumulated
condensate be D. Concentration of the equilibrium vapour is . Over a small time, the
change in the amount of liquid in the still is and the amount of vapor withdrawn is .
The following differential mass balance equations may be written:

Total Material balance: = 16


Component A balance: () = 17
= + = = ( ) 18
Equation 16 means that the total amount of vapor generated must be equal to the decrease
in the total amount of liquid. Similarly, equation 17 indicates that the loss in the number of
moles of A from the still because of vaporization is the same as the amount of A in the small
amount of vapor generated.
Putting = in equation 18 and rearranging we get,

= 19

If distillation starts with F moles of feed of concentration and continues till the amount of
liquid reduces to W moles ( = ), the above equation can be integrated to
give


= ln = 20

Equation 20 is the basic equation of batch data distillation and is called the Rayleigh
equation. If the vapour liquid equilibrium data (- ) are available in a tabular form, the
right side of equation 20 can be evaluated graphically. If an algebraic relation between
and is available, analytical integration may be possible. For example, if the relative
volatility of A in the binary mixture is constant as in ideal solutions, the relation
between and may be obtained from equation 14 and substituting for in equation 20
and integrating gives,


1 (1 ) 1
ln = = ln + 21
( 1) (1 ) 1
1 + ( 1)

The above integral can be expressed in a more convenient form by multiplying through by
( 1) and simplifying to get
(1 )
ln = . 22
(1 )
The average composition (, ) of the accumulated distillate (D) can be obtained by the
simple material balance.
= , + = + 23

Example 2
A charge of 50kmol of a mixture of Benzene and Chloro-benzene having 55mol% of the less
volatile is to be batch-distilled. (a) If 25 moles of the solution is vaporized and condensed as
the distillate, calculate the concentration of the accumulated distillate. (b) If the
concentration of the accumulated product is found to be 72mol% benzene, calculate its
amount. The relative volatility of benzene in the mixture is 4.15
Solution
Moles of feed, F = 50kmol;
Feed concentration of the more volatile component, = 1 0.55 = 0.45
(a) Distillate, D = 25 kmol, and W = 25 kmol , = ?; we will use equ. 22 to obtain
which will in turn be used in equ 23 to finally , .
50 0.45 50 (1 0.45)
ln = 4.15
25 25(1 )
Solving the above, we get = 0.218
Material balance: = , + 50 0.45 = 25 0.218 + 25 ,

, = 0.682

Composition of the distillate collected, = , = 0.682

(b) Given: = , = 0.72; = ?

Total material balance, 50 = + ;


Benzene balance, 50 0.45 = + 0.72
13.5
From the above two equations we get, =
0.72

Substituting in equation 22,


50 0.45 50(1 0.45)
ln =
13.5 13.5
(0.72 ) (0.72 )(1 )

13.5
Solving for we have, = 0.309; = 0.720.309 = 32.85

Amount of Distillate, = = 50 32.85 = 17.15


Recall, that we mentioned that if the vapour liquid equilibrium data (- ) are available in
a tabular form, the right side of equation 20 can be evaluated graphically, this will apply
especially if the equilibrium relationship between the phases is not known in terms of the
relative volatility thus making equation 22 irrelevant.
For the problem that the value of is specified with equation 22 not applying as the
equilibrium relationship in terms of relative volatility is not defined and the value of is to
be determined, a trial & error technique must be employed as follows

1
1) From the tabulated equilibrium data, evaluate the value of yA x
from the values of yA and
1
x for each corresponding value of x. Plot y x on the vertical axis against x. The area under
A
the plotted graph between xW and xF is the solution of the integral on the right hand side of
equation 20. However, as mentioned above, if the value of xW is not known and the value of
xD is specified then the integral cannot be integrated straight away and we would need to
apply a trial and error procedure

2) Make a first (1st) guess for the value of xW and calculate the value of the integration of Equ
20 according to the guessed value of xW

3) Then, the value of final W can be calculated from equation 20

4) Use the value of final W obtained from step 3 and the guessed value of xW made in 2,
combined with the given values of F and xF , to compute the values of Dcalc and
xD,calc (yD,av calc) using the combined pair of equation 23

5) Compare the value of xD,calc obtained from 4 with the given value of xD : if xD,calc = xD ,
the trial & error procedure is finished; however, if xD,calc xD , the new trial & error has to
be repeated, until we obtain the guessed value of xW that makes xD,calc = xD

The following Example illustrates the employment of the trial & error technique to solve the
batch distillation problem

Example Use the given equilibrium data of methanol (MeOH) and water for solving the simple
batch distillation problem with the following description:
A single-equilibrium-stage (or a simple) batch still pot is used to separate MeOH from water
The feed with the total amount of 50 moles of an 80 mol% MeOH is charged into the still
pot operated at 1 atm. The desired distillate concentration (xD ) is 89.2 mol% MeOH

Determine:
a) The total amount of the distillate collected (Dtotal )
b) The amount of material (liquid or waste) remained in the pot after the distillation has ended
(final W) and its corresponding concentration (final xw )

It is given that
F = 50 moles
xF = 0.80
xD,avg = 0.892

The equilibrium (y -x) data of MeOH is as summarised in the following Table

Methanol liquid ( ) (mol %) Methanol vapour ( ) (mol %)

0 0
2.0 13.4
4.0 23.0
6.0 30.4
8.0 36.5
10.0 41.8
15.0 51.7
20.0 57.9
30.0 66.5
40.0 72.9
50.0 77.9
60.0 82.5
70.0 87.0
80.0 91.5
90.0 95.8
95.0 97.9
100.0 100.0

In this Example, the unknowns are


Total D
Final W

Since one of the integral boundaries, is NOT known, a trial & error technique must be

employed to compute the integral

To start the calculations, the 1st guess with of 0.70 is used

1
From the given equilibrium data, the value of for each value of x can be summarised in
the following Table (note that interpolations are needed to obtain the values of y and
1
when the values of x are, e.g., 0.75, 0.65):

x y Y-x 1

0.80 0.915 0.115 8.69
0.75 0.895 0.145 6.89
0.70 0.871 0.171 5.85
0.65 0.845 0.195 5.13
0.60 0.825 0.225 4.44
0.50 0.780 0.280 3.57

1
Plotting a graph between x (X-axis) and (Y-axis) using the data in the Table above from,

= 0.70 (the dashed lines) to = 0.80, yields the following graph
(from Separation Process Engineering by Wankat, 2007)

0.70
From the resulting graph, 0.80 is in fact,the area under the curve from x = 0.70 to x

0.80
For this Example, the area under the curve is found to be - 0.7044
The value of final W (i.e. the liquid remained in the still pot) can then be calculated, using Equ
20 to obtain Final W = 24.72 mol

Thus, the total amount of the distillate can


be computed using the second part of Equ 23 to get = 25.28
The value of , can be calculated using the first part of Equ 23 to get , = 0.898
However, the desired value of , is 0.892 the calculated value is too high!

Thus, a new guess of is needed

With the new guess of of 0.60, we obtain the following (by performing similar calculations
as above):
Area under the curve from, = 0.60 = 0.80 is 1.2084
Final W = 50 exp (-1.2084) = 14.93
= F -W = 50-14.93 = 35.07
, = 0.885 (Too low!)
Hence, we need to make a new (the 3rd) guess for

With the 3rd guess of of 0.65, we obtain the following:


Area under the curve (from x = 0.65 to
y = 0.80) = 0.9710
Final W = 18.94
= 31.06
, = 0.891 (O.K. close enough!)

Since , = , when we use of 0.65, the which we seek is = 0.65

Batch Distillation with Rectification


One of the simplest and most frequently used batch distillation configuration is the batch rectifier,
including the alembic and 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 vapour (distillate) as reflux, and
one or more receivers.

The pot is filled with liquid mixture and heated. Vapour 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 vapour 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 flavour. 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 vapour 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.
Batch Distillation with rectification set-up

Multi-Stage Batch Distillation at Constant Reflux

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