DEPARTMENT OF CHEMICAL ENGINEERING

INDIAN INSTITUTE OF TECHNOLOGY

KANPUR

Che492-Unit Operations Laboratory 2

Experiment no.
Continuous Distillation
Instructors:

Dr. Siddhartha Panda

Dr. Deepak Kunzru

Name of TA:

Prashant Kr. Gupta

Date of experiment: 12/08/2013
Date of submission: 19/08/2013

Group No: 2
Roll no.
10059
10062
10067

INDEX

Name
Akshay Bansal
Akshit Gupta
Aman Jain

S.
No
1
2
3
4
5
6
7
8
9

Title

Page No.

Introduction
Objective
Theory
Utulities required
Procedure
Observation & calculation
Inferences
Precautions
References

3
4
4
5
5
5
9
9
9

INTRODUCTION
Continuous distillation, a form of distillation, is an on-going separation in which a mixture is continuously
(without interruption) fed into the process and separated fractions are removed continuously as output streams.

A distillation is the separation or partial separation of a liquid feed mixture into components or fractions by
selective boiling (or evaporation) and condensation. A distillation produces at least two output fractions. These
fractions include at least one volatile distillate fraction, which has boiled and been separately captured as a
vapor condensed to a liquid, and practically always a bottoms (or residuum) fraction, which is the least volatile
residue that has not been separately captured as a condensed vapor.
Each fraction may contain one or more components (types of chemical compounds). When distilling crude
oil or a similar feedstock, each fraction contains many components of similar volatility and other properties.
Although it is possible to run a small-scale or laboratory continuous distillation, most often continuous
distillation is used in a large-scale industrial process.

OBJECTIVE
To study Continuous Distillation in a Sieve plate column

THEORY
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 component(s) 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 component(s) with lower
boiling point(s), 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 "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 reboilermay 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 (location). Unless the process is disturbed due to changes in feed, heating,
ambient temperature, or condensing, steady state is normally maintained. This is also the main attraction of
continuous distillation, apart from the minimum amount of (easily instrumentable) surveillance; if the feed rate
and feed composition are kept constant, product
rate and quality are also constant. Even when a variation in conditions occurs, modern process control methods
are commonly able to gradually return the continuous process to another steady state again.

TERMINOLOGY
REFLUX
Reflux refers to the portion of the condensed overhead liquid product from a distillation tower that is returned
to the upper part of the tower the downflowing reflux liquid provides cooling and partial condensation of the
upflowing vapors, thereby increasing the efficacy of the distillation tower. The more reflux that is provided, the
better is the tower's separation of the lower boiling from the higher boiling components of the feed
Reflux Ratio is given by L/D
Where,
L is the flow rate of the liquid sent back to the column
D is the distillate flow rate.

Total Reflux
For, a column operating at Total Reflux (i.e. all of the distillate being sent back to the column)
L=V in both the enriching & stripping sections
y = x for all trays.
Thus the operating line of McCabe Thiele diagram coincides with the y = x line.

Finite Reflux ratio (R)

For the column being operated at some other reflux ratio R, the quality is given by:
q= Hg- Hf /(Hg-HL)
And the slope of this q-line is given by -> q/(q-1)
The enriching section operating line is given by-

It passes through

y = x = XD

The operating line of stripping section passes through the intersection of the enriching section operating line &
the q line.
The equation for enriching section operating line is given by -

A column with a high reflux ratio may have fewer stages, but it refluxes a large amount of liquid, giving a

wide column with a large holdup. Conversely, a column with a low reflux ratio must have a large number of
stages, thus requiring a taller column.

EXPERIMENTAL APPARATUS

Chemical engineering schematic of Continuous Binary Fractional Distillation tower. A binary distillation
separates a feed mixture stream into two fractions: one distillate and one bottoms fractions.

UTILITIES REQUIRED:

Distillation column made of glass having perforated plates

Ethanol-Water solution

pumps for feed and reflux

Refractometer for measuring the refractive index

Electricity Supply: 220 V AC

Floor Area Required: 2 m x 2 m.

PROCEDURE

We calibrated the rotameter with the given solution.

We obtained the calibration curve for refractive index Vs. Alcohol
percent.
We noted the composition of feed in the boiler and initial
conditions of setup such as temperature of feed and water flowing
in and water flowing out etc,. as per in data sheet given.
We started the reboiler heating, taking the initial reading of power
meter and cooling water in the condenser also.
We operated the system in total reflux and waited till steady state
is obtained. Distillate and bottom samples are taken
systematically and then we determined the refractive index and
specific gravity .
We noted the flow rate of distillate.
Now we operated the system under a reflux ratio higher than
minimum reflux ratio and obtained samples at steady state as
same procedure explained above.
We took readings of flow rate of, feed , distillate, product and
reflux.
The setup is shutdown and finally took the power reading at the
end of the experiment.
Quantity of sample collected from product stream is calculated
and note down for mass balance calculations. We came next day
to calculate the total amount of feed remain in re-boiler and its
refractive index. The amount of secondary feed consumed is also
noted.

OBSERVATIONS AND CALCULATION

Mole
fractio
n of
ethanol
0.10
0.20
0.32
0.42
0.47
0.61
0.63

Mole
fractio
n of
ethanol
0.430
0.620
0.700
0.750
0.800
0.900

Refractiv
e index
1.343
1.353
1.358
1.359
1.359
1.360
1.360

Speci
fic
gravit
y
0.873
0.845
0.830
0.820
0.810
0.804

Refractive index Vs mole fraction

1.365
1.360
1.355

f(x) = - 0.27x^4 + 0.7x^3 - 0.63x^2 + 0.24x + 1.32

R = 1

1.350
1.345
1.340
1.335
1.330
0.00

0.10

0.20

0.30

0.40

0.50

0.60

0.70

Specific gravity Vs mole fraction

0.900
f(x) = - 0.16x + 0.94
R = 0.98

0.850
Specific gravity

0.800
0.750
0.400

0.500

0.600

0.700

0.800

0.900

1.000

Mole fraction

Finding the Value of q :

Given Feed conditions, super cooled liquid we can calculate the value of q by following
expression:
q = 1 + Cpl(Tb Tf)/Hvap
Tb
= Boiling point of the mixture
Tf

= Freezing point of the mixture

C PL = Heat capacity of the mixture

Hvap= Latent heat of vaporization of the mixture
Given, refractive index = 1.356
From the graph of Refractive index vs mole fraction plotted above, we
find that at the mole fraction of ethanol in the feed is 0.238
0.24
Mol. Wt. of Ethanol = 46
Mol. Wt. of water = 18
Therefore, average mol. Wt. for the given composition = 0.24x46 + 0.76x18
= 24.72 g/mole
Calculating the weighted average of heat capacities of water and alcohol, we get
111.46*0.24 + 75.6*0.76 = 84.21 J/mole K
Tb

= 351.37*.24 + 373*.76 = 367.81 K

C PL

Tf

= 159*.24 + 273*.76 = 245.64 K

Hvap = 38.6*.24 + 40.68*.76 = 40.18 KJ/mole = 40180 J/mol

Putting these values in the equation obtains q = 1+84.21*(367.81245.64)/40180 =1.256
Slope of the q line is 1.256/(1.256-1) = 4.91 and Intercept of the y-axis
is
.24/(1-1.256)= .937

Calculation of R minimum
Relative volatility of mixture at given feed conditions is given as = .76/.24 = 3.2
approximately.
Rmin can be calculated by following expression ,where Zf = 0.24
Rmin

Condition
total reflux
Partail Reflux
1
Partail Reflux
2

= 1/zf( - 1) = 1/(.24*(3.2-1)) = 1.894

Weight of sample
26.932
26.884

Sp.gravity
0.807
0.802

Molefraction
0.85
0.88

26.912

0.805

0.80

26.897

0.803

0.80

26.914

0.805

0.81

26.934

0.807

0.81

Used scientific calculator equation solving function to solve the best

fitting curve in the fig.2
Molefractio
Condition
Refractive index
n
1.355
0.23
total reflux
1.345
0.11
Partail Reflux
1.340
0.08
1
1.346
0.12
Partail Reflux
1.346
0.12
2
1.347
0.13

Total Reflux:
Here R is infinite so y intercept of operating line is 0
And operating Line is y = x
xD
Observed
is 0.88 from table 4 given above.
x F = 0.24 and after steady the mole fraction in the bottoms is

xw

0.11
Now using McCabe-Thiele method to calculate theoretical No. of stages
No. of stage = 8
Efficiency=

( Theoretical no .of stages )100

Actual no . of stages
= 8*100/12 = 66.66%

Partial Reflux 1
Flow rate of reflux (R) = .152 ml/s = 9.12 ml/min
Flow rate of product (D) = .0425 ml/s = 2.55 ml/min
Reflux ratio = (R-D)/D = (9.12-2.55)/2.55 = 2.576
Observed

xD

is .8

By McCabe-Thiele method
No. of stages = 9
Efficiency=

( Theoretical no .of stages )100

Actual no . of stages
= 9*100/12 = 75%

Partial Reflux 2
Flow rate of reflux (R) = .165ml/s = 9.9 ml/min
Flow rate of product (D) = .0438ml/s = 2.628 ml/min
Reflux ratio = (R-D)/D = (9.9-2.628)/2.628 = 2.767
Observed

xD

is .81

By McCabe-Thiele method

No. of stages = 8
Efficiency=

( Theoretical no .of stages )100

Actual no . of stages
= 7*100/12 = 66.66%

Material Balance
(Mass in Mass out ) = Mass accumulating

Mass coming in:

Feed in = 1200ml
Density of feed = .24*.789 + .76*.9905 = .942g/ml
Mass coming in = 1200*.942 = 1130.568g

Mass coming out:

Product taken out = 225ml
Average density of product =
(.88*.789+.12*.9905 + .81*.789+.19*.9905 + .80*.789+.2*.9905)/3 =
0.823 gm/ml
Mass of product coming out = .823*225 = 185.23g
Mass of bottom = 970*(.13*.789+.87*.9905)= 935.4g

Mass accumulating:
Mass accumulating = 1130.568-935.4 = 195.2g

Energy Balance:
Latent heat of vaporization: - Ethanol:-38.6 K J/mol = 767.9 J/g,
Water: - 40.68 KJ/mol = 2146 J/g
Heat capacity: - Ethanol:-111.46 J/mol-K = 2.845 J/g-K
Water:- 75.6 J/mol-K =4.184 J/g-K
(Energy in Energy out) = (Energy accumulating + Energy loss)

Energy coming in:

Re-boiler energy input = (349.1-347.5)/ = 1.6 KWH = 5760 KJ
Energy coming in by feed = 0 (at reference temp)

Energy coming out:

Bottom heat cap. = 0.13*2.845+0.87*4.184 =4.01 J/g-K
Energy coming out by product = 225*0.823*(.8*2.845+.2*4.184)*(7628) = 27.67 KJ
Energy out by Condenser = (flow rate (ml/s)*density (g/ml)*Cp(J/gK)*T*time (s))
= (2.1*1000/60)*1*4.184*(31-28)*(180*60) = 4744

KJ

Energy loss:
Energy loss = 5760-4744 = 1016 KJ