RE-302

Batch Reactive Distillation

Batch: B6 (B)
Nitish Amnerkar
Sumit Diwakar
Abhishek Meena
Nilay Bhadade

17/02/2015
27/02/2015

12D020014
12D020028
12D020024
12D020006
Date of Experiment:
Date of Presentation:

Aim
To examine the potential of batch reactive distillation
in enhancing the reaction conversion

Motivation
Reactive distillation is especially useful for
equilibrium-limited reactions such as esterification
and ester hydrolysis reactions. Conversion can be
increased far beyond what is expected by the
equilibrium due to the continuous removal of reaction
products from the reactive zone. This helps reduce
capital and investment costs and may be important
for sustainable development due to a lower
consumption of resources.

Theory
Esterification used in the reaction is

CH3COOH + C4H9OH C4H9COOCH3 + H2O

law of mass action is given by, (K = equilibrium
Constant)
K=
According to Le Chateliers principle if we constantly
remove water from the reaction system equilibrium will
shift towards the product side. Removing of water is
done using continuously distillation.

Theory
Butanol, Butyl Acetate and water (in reaction system)
forms ternary azeotrope. This azeotrope is
heterogeneous and low boiling one, thus boiling point of
water is lowered to 87-90C. There is also a phase
separation (heterogeneous), organic phase comprises of
Butyl Acetate and Butanol and aqueous phase consist of
water which can be removed easily
To measure the extent of reaction, we measure the
amount of acetic acid remaining in the reaction mixture
by titrating the sample with standard NaOH solution in
presence of phenolphthalein indicator

Experimental Procedure
Take 440 g acetic acid and 550 g Butanol in both the reactors (R1
and R2) along with the 100 g of acidic resin which act as a
catalyst
Take samples from both reactor ( t = 0 readings)
Start the power supply to both the reactor and put the stirrer into
them (agitating speed 1000 rpm). Also start the water supply to
the condenser.
R1 is based on BRD while R2 is on conventional method, vapours
in R1 will rise and get condensate with phase separation
(heterogeneous azeotrope). Take samples from both aqueous
and organic phase
Collect samples from both the reactors and from aqueous and
organic phase every 10 minutes
Titrate the 1ml of collected samples against standard NaOH
solution to calculate the concentration in samples collected

Calculation
Sr.
no.

time
(min)

% conv. In
R1

% conv. In
R2

10

25.6756757 36.08108108

-0.405263158

20

52.2837838 50.94594595

0.025588007

30

67.7378378 59.86486486

0.116227108

40

78.0324324

0.137572735

50

85.2837838 68.78378378

0.193471716

60

92.1189189

0.156495716

67.2972973
77.7027027

Enhancement factor

Results
Temperature Vs Time
130
120
110
100
Temperature
90
80

R
1

70
60
50
40
30
20
0

10

20

30

40

Time

Graph 1

50

60

70

Results
Conversion Vs Time
100
90
80
70
60
Conversion

R
1

50
40
30
20
10

0
0

10

20

30

40

Time
Graph 2

50

60

70

Results
Cumulative Water Vs Time
70
60

Cumulative Water
50
40
30
20
10
0
0

10

20

30

40

Time
Graph 3

50

60

70

Results
Enhancement Factor Vs Time
0.3
0.2

Enhancement
Factor
0.1
0
0

10

20

30

40

50

60

70
R1

-0.1
-0.2
-0.3
-0.4
-0.5

Time

Graph 4

Error analysis
Error in measuring NaOH = 0.5gm
for preparing 1 N solute relative error = 0.025
Error in volumetric measurement =
dV1/V1+dV2/V2=10/210+10/340=0.077
Least count of burette while titration = 0.1mL
Least count of syringe in measurement of sample (1mL) =
0.1mL
For reactor 1 relative error =
(0.077)+(0.1+0.025)=0.202
For reactor 2 relative error =
(0.077)+(0.1+0.025)=0.202
Average enhancement factor (E) = 0.037
total relative error = 0.202+0.202 = 0.404
dE=0.4040.037=0.015

Conclusion
Enhancement factor = 31.5 %
Enhancement factor is greater than 1, which shows that
conversion is more in reactor 1 compare to that in reactor 2.
Hence Batch Reactive Distillation gives more yield for the
same input condition and eventually it is more energy and
cost effective.

Discussions
Le Chateliers principle: When a system at equilibrium is
subjected to change in concentration,temperature,volume or
pressure, then the system readjusts itself to counteract the
effect of the applied change and a new equilibrium is
established. In this case water is being removed at
equilibrium, so the reaction shifts in forward reaction to nullify
the effects of water loss.
Reaction temperature depends on the composition of the
mixture in the reactor and this composition is changing
continuously. Hence, the reaction temperature keeps changing
Azeotrope: An azeotrope is a mixture of two or more liquids
whose proportions cannot be altered by simple distillation. In
this case minimum boiling heterogeneous azeotrope is formed
which makes it possible to remove water through distillation
without much loss of acetic acid. It also condenses to form
separate organic and aqueous layer which can be easily
separated.

Discussions
If azeotrope is not heterogeneous then aqueous layer and
organic will be inseparable.
The high speed of agitation results in particle being
suspended and thus uniformly distributed in mixture and thus
helps in increasing the mass transfer coefficient between the
liquid and the catalyst.