Mass Transfer Operations I

Prof. Bishnupada Mandal

Department of Chemical Engineering
Indian Institute of Technology, Guwahati

Module - 5
Distillation
Lecture - 4
Batch and Steam Distillation

Welcome to the fourth lecture of module 5. Here, we are discussing distillation

operations.

(Refer Slide Time: 00:35)

So, let us have recap of our earlier lectures. In lecture 3, we discussed flash distillation,
and this flash distillation is very important particularly in petroleum refining; important
and frequently used in petroleum refining, and we have also taken the example of a
mixture of n-hexane and n-heptane. Today, we will discuss two more topics; one is batch
distillation and second is steam distillation.
(Refer Slide Time: 02:27)

So, let us consider batch distillation. This is a simple distillation, where a tank is charged
with the feet material, and which is fitted with the steam jacket, and it heated with a
steam coils. What happens? The vapor flows upward; then it goes to overhead, it is then
condensed, and then it is collected with a receiver, and then the remaining material
which is left in the tank is known as the residue. So, the composition which is collected
in the receiver, composition changes with time; this is small x D. The composition which
is obtained at the receiver is the average compositions of all the materials collected.

So this is a batch process, and this can be switched off every time as the operation is
done, and the cuts are taken out. So, this batch process is inherently; this is an unsteady
state process or we can say it is a dynamic process.
(Refer Slide Time: 04:59)

So this cannot be modeled at steady state say dynamic process, and this operation, it can
be done with or without reflux. Two methods can be followed with or without reflux.
When we consider with reflux, then we can use the total reflux or we can vary the reflux
as well. Here, we will consider now without reflux. So, this batch distillation operation, it
is very common in small capacities plant like pharmaceuticals, pharma industry,
specialty chemicals, or fine chemicals, and this can be also used for test runs for new
products, or this can be used for the continuous process where the frequent cleaning is
required. In that case, this operations can be done; the process which required frequent
cleaning.
(Refer Slide Time: 07:28)

Let us consider differential distillation of a binary mixture. So, we will consider binary
mixture a and b, and we will consider without reflux. When the batch distillation without
reflux is operated, the process is called differential distillation. Since there is no reflux,
the vapor which is producing from the still is assumed to be in equilibrium with that
liquid, which is the residue; vapor is in equilibrium with residue.

Now, let us take L is the number of moles of liquid in the still pot at any time t, and small
x is the mole fraction of more volatile component say A, and D is the moles of
condensate accumulated, y star is equal to concentration of the equilibrium vapor.
(Refer Slide Time: 10:23)

Now if we do the total material balance, the differential mass balance we will do. First,
we will do the total material balance is minus dL is dD; say this is equation 1. Now
component A balance we can write minus d of Lx would be equal to y star dD.

So, from this we can write minus L dx minus x dL would be equal to y star dD. So, this
is equation 2. Now if you use equation 1 in place of equation 2, we can write minus L dx
plus x dD is equal to y star dD. So, from this we can write minus L dx would be equal to
y star minus x dD; this is equation 3. Suppose and if we use equation 1 in this case; so, it
will be minus L dx would be y star minus x into dL. So, from this we can write dL by L
is equal to dx by y star minus x. So, this is equation 4.
(Refer Slide Time: 13:04)

Now if we consider F is equal to a moles of feed, Z F concentration of feed, and W is the

moles of residue, and also x w is the concentration of more volatile in the residue. Then
we can write from equation 4; this equation we can write, integral F to W dL by L would
be equal to integral Z F to x w dx divided by y star minus x. So, from this we can write
ln F by w would be equal to integral x w two Z F dx by y star minus x. So, this equation
is known as the Rayleigh equation, and this relates with the residue and the composition
relation.

(Refer Slide Time: 15:36)

So, ln F by w is equal to integral x w to Z F dx by y star minus x. So, in this equations
the right hand side if we have the equilibrium data in tabular form, suppose x and y star;
this data are available in tabular form, equilibrium data. Then graphical integration is
possible; graphical integration can be done. But if we have the relations between x and y
star, then numerical integration is possible; numerical integration we can do. Suppose, if
we take the relations y star is equal to alpha x divided by 1 plus alpha minus 1 into x.

So, if we use in this Rayleigh equations. So, it will be ln F by W would be equal to

integral x w to Z F dx divided by alpha x by 1 plus alpha minus 1 into x minus x, which
we can write 1 by alpha ln Z F by x w into 1 minus x w divided by 1 minus Z F plus ln 1
minus x w by 1 minus Z F. So, this can be written in more convenient form is ln F Z F by
W x w would be equal to alpha ln F by W 1 minus Z F by 1 minus x w. Say this is
equation 5, and this is equation 6, and this is the equation 7.

(Refer Slide Time: 19:03)

Now, the average composition y D average; so, this is y D. This can be obtained average
composition, that is, y D average of accumulated distillate can be obtained by material
balance. So, if we do the little balance F Z F is equal to D y D average plus W x w, and
then we can do the overall mass balance, F is equal to D plus W. So, from this, we can
calculate y D average.
(Refer Slide Time: 20:30)

Now, let us take an example to see how we can calculate the average concentration. A
liquid mixture of 150 mol containing 40 mol percent n-hexane and 60 mol percent n-
heptane, which is, B is subjected to batch distillation at a total pressure of 1 atmosphere
to vaporize one-third of the feed. The relative volatility of n-hexane in the mixture is
2.36. Calculate the following: What is the average composition of the distillate? If the
accumulated vapor is 90 percent n-hexane, what is the amount of distillate?

(Refer Slide Time: 21:24)

So, first we will try to calculate the average compositions of the distillate. It is given the
feed, which is F is equal to 150 mol, and the composition Z F which is 0.4; 40 mol
percent n-hexane, and for problem 1, it is given that to vaporize one-third of the feed. So,
feed is vaporized one-third; that means 150 into one-third. So, 50 mol is vaporized which
is D. From the total material balance if we look, F is equal to D plus W. So, 150 is equal
to 50 plus W; so, the W is 100 mol.

Now, you have to calculate y D average. So, let us use Rayleigh equations, which is ln F
Z F by W x w is equal to alpha ln F by W 1 minus Z F by 1 minus x w. Now putting the
values; if we put the values ln 150 into 0.4 divided by 100 x w is equal to 2.36 ln 150 by
100 1 minus 0.4 divide by 1 minus x w.

(Refer Slide Time: 23:58)

So, this we can write ln 0.6 by x w would be equal to 2.36 ln 0.9 by 1 minus x w. So,
after solving we can do trial and error method guessing x w from both sides. So, we can
get x w is equal to 0.315. Now we know that, F Z F is equal to D y D average plus W x
w. So, then we can use 150 into 0.4 would be equal to 50 into y D average plus 100 into
0.315. So, from this we can obtain y D average is equal to 0.57. So, this is the
composition of the distillate.
(Refer Slide Time: 25:53)

Now, let us do for second part b. So, it is given y D average is equal to x D which is 0.9,
and we have to calculate what is the value of distillate; amount of distillate? We know
from the total material balance, mass balance 150 is equal to D plus W; this is equation
1, and we can write the material balance; component balance is 150 into 0.4 would be W
x w plus D into 0.9. So, from these two relation we can write W x w plus 150 minus W
into 0.9, and from this we can get 60 is equal to W x W plus 150 minus 0.9 W, and from
this we can write W into 0.9 minus x w is equal to 75. So, W is equal to 75 divided by
0.9 minus x w.

(Refer Slide Time: 28:04)

Now if we use this w in place of Rayleigh equation, we know ln F Z F by W x w is equal
to alpha ln F by W 1 minus Z F by 1 minus x w. So, we can write l n 150 by 75 by 0.9
minus x w into 0.45 by x w is equal to 2.36 ln 150 by 75 divided by 0.9 minus x w into 1
minus 0.4 divided by 1 minus x w . So, if we simplify this will be ln 2 by 0.9 minus x w
into 0.5 by x w is equal to 2.36 ln 2 by 0.9 minus x w into 0.6 divided by 1 minus x w.
So if we solve this, then we can obtain x is equal to 0.206.

(Refer Slide Time: 30:26)

So, we know that W is equal to 75 divided by 0.9 minus x w. So, if we put 75 by 0.9
minus 0.206, which would be 108. So, this is this much mol of W. So, the amount of
distillate D is equal to F minus W from the total mol balance. So, it is 150 minus 108; so,
this is equal to 42 mol.
(Refer Slide Time: 31:18)

Let us consider another type of distillation which is steam distillation, particularly when
some liquid which are very high boiling and it has some contaminant of non volatile
components, which cannot be separated at normal distillation at atmospheric pressure.
So, first is high boiling component. High boiling liquid cannot be purified by normal
distillation at atmospheric pressure; because if we apply high temperature, there is a high
possibility of decomposing the material at high temperature.

So when the components are high boiling, then they are in general immiscible in water.
So, a separation at lower temperature can be possible by using steam distillation. So, it is
an operation where live steam each used for distillation with the mixture of high boiling
liquid with other components, which may be traces of impurities of non volatile
impurities or any other component, which are non volatile in nature. So, our target is to
recover the high boiling components, which has low volatility and low solubility in
water. Suppose component A which is high boiling, low volatility, low solubility in
water; and component C say is non volatile in nature.
(Refer Slide Time: 34:20)

So, this is shown in the figure. As we can see, the feed is taken in a tank and live steam is
injected through the sparger. Feed is taken in a still and then live steam is sparged from
the bottom. So, the vapor which will produce it will carried by the steam and it is
condensed. This is condenser. Vapor formed is carried along with the steam and
condensed at the top.

(Refer Slide Time: 35:54)

Now since, A has the less miscibility with water it will form two layers, and one layer is
water layer and target materials layer. Then it is separated. This two layers can be easily
separated, and another thing is that the energy required to heating the feed to its bubble
point, so energy we have to be supplied to heat the feed to its bubble point and to
vaporize A.

So if we use only live steam, say, there is a high chance of condensing the steam in the
steel to heat the material. So to avoid these, a still coil is used to provide the energy for
heating. So, a still coil is used for make up heat.

(Refer Slide Time: 38:06)

Now, what is the use of this steam distillation? Use importantly. This is used in food
industries for the removal of volatile materials, volatiles, and flavors from edible fats and
oils, separation of thermally unstable material and third, separation of ammonia and
VOCs volatile organic materials from waste water, and so on. There are so many
applications.
(Refer Slide Time: 39:38)

Now let us consider if we have a two immiscible liquids A and B, which is water and this
is boiled. So, vapor will generate. So, 3 phase system; so, phases 3, component 2. So, if
we apply here phase rule we can see F is equal to C minus P plus 2. So, this will be 2
minus 3 plus 2 is equal to 1. This is the degrees of freedom. So if the total pressure is
fixed, then the system is fixed.

(Refer Slide Time: 40:53)

Now two liquid phases exert its own vapor pressure at the prevailing temperature, and
this cannot be influenced by others. When the sum of the vapor pressure equals the total
pressure, then the mixture boils. So, we can write P A v plus P B v is equal to P t.
Therefore, y A should be P A v by P t; P A v and P B v are the vapor pressures of the
components, and P t is the total pressure, y B should be P B v by P t. So, these are the
vapor compositions.

Now by steam distillation as long as water is present, so the high boiling component A at
a temperature below its boiling point will vaporize and without using the vapor pressure.

(Refer Slide Time: 42:41)

This means as long as water present in the system, the high boiling component vaporizes
at a temperature below its normal boiling point. The disadvantage of the method: Large
amount of heat must be supplied to evaporate water simultaneously with the high boiling
component.
(Refer Slide Time: 44:39)

Now, if you take m A moles of component A which is high boiling to be vaporized, and
m B moles of steam required. Then, if the system operates in equilibrium we can write m
A by m B would be equal to P A v by P B v, which is P A v by P t minus P A v. So, from
this we can write m A would be m B P A v by P t minus P A v. But if the system does
not operate in equilibrium, then the partial pressure of A will be less than it is vapor
pressure; partial pressure of A should be less then P A v. So, in that case another factor
which is E is known as the vaporizing efficiency is used. So, P A would be E P A v.
Therefore, we can write m A would be m B E P A v divided by P t minus E P A v.

(Refer Slide Time: 47:12)

Now, let us take a very simple example. A 2 kg liquid mixture of A and C, which is non
volatile is to be steam distilled. Live steam at 110 degree centigrade is used at a flow rate
of 10 kg per hour. Assume A is immiscible with water. The vaporization efficiency is
0.9. Vapor pressure of water and component A at 110 degree centigrade are 1.4 bar and
0.1 bar respectively. Molecular weight of A is 200. Calculate the distillation time
required.

(Refer Slide Time: 47:53)

It is given that P A v is 0.1 bar and P B v is 1.4 bar. Molecular weight of component A is
200 and m A which is 2 by 200 is 2 kg mixture, which is equal to 1 into 10 to the power
minus 2 Kmol. So, m B is m A P B v by E P A v, which is equal to 1 into 10 to the
power minus 2 into 1.4 divided by 0.9 into 0.1, which is equal to 0.156 into 18, which is
equal to 2.8 k g. Now it is given that steam rate is equal to 10 k g per hour. Therefore,
time required is equal to 2.8 divided by 10 hour, which is equal to 16.8 minute.