Experiment 7 - Batch Reactor

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The key takeaways are that conductivity decreases over time as the concentration of sodium hydroxide decreases during the reaction, and that increasing the temperature increases the rate of reaction.

The conductivity decreases over time as the concentration of sodium hydroxide decreases during the reaction, forming more sodium acetate.

Increasing the temperature increases the rate of reaction because the particles collide more frequently and effectively at higher temperatures, requiring less activation energy for the reaction to proceed.

Abstract

This experiment is done to study the effects of temperature on


saponification reaction of ethyl acetate and sodium hydroxide in batch reactor. A
batch reactor is a reactor which the reactant is feed and left in the tank. The
product is only removed from the tank when the reaction is completed. In this
experiment, ethyl acetate and sodium hydroxide is mixed in the tank. The
temperature is manipulated and the time taken for the conductivity values to
achieve a steady state for each flow rate is monitored and recorded. From the
results obtained, it was found that as the temperature increases, the rate of
reaction increases. Overall, the conductivity increase with the increase of time
and temperature.
Introduction
A simple batch reactor is a reactor which the feed is charged via two holes in the
top of the tank. While the reaction is carried out, there is nothing else to be put
in or taken out from the tank until the reaction is completed. The tank is easily
heated or cooled by cooling jacket. Batch reactor has the advantage of high
conversion that can be obtained by leaving the reactant for a long period of time.
There are several factors that affect the rate of reaction in the batch reactor. For
this experiment, the objective is being study the effect of temperature on
saponification reaction of ethyl acetate and sodium hydroxide in a batch reactor.
Assumption made was the conductivity decreased with time but increased with
the increment of temperature.
Methodology:
First of all, 2.5L of 0.1M sodium hydroxide solution, 500mL of 0.1M sodium
acetate solution and 2.0L 0.1M ethyl acetate is prepared. Next to prepare
calibration curve, 100mL of deionised water is mixed with each set of chemical
mixture (a. 100mL NaOH for 0% conversion, 75mL NaOH + 25mL Na(Ac) for 25%
conversion, 50mL NaOH + 50mL Na(Ac) for 50% conversion, 25mL NaOH + 75mL
Na(Ac) for 75% conversion, and 100mL Na(Ac) for 100% conversion).
To perform reaction at 30C, the temperature is set at 30C for both
reactor and reactant. 1L of 0.1M ethyl acetate is added into the jacketed reactor
through the opening at the top of the reactor. The stirrer is switched on and set
at the minimum speed. Once the temperature is uniform, 1L of 0.1M NaOH is
added into the reactor and stop watch is started immediately. Then the product
is collected every 5mins and its conductivity is tested and recorded until its
conductivity remain constant. After that, the reactant in the reactor is drained
out. The steps are repeated by increase the reactor and reactants temperature
until 50C.
Result:

No
Conversion, % Conductivity
1
0
17.99
2
25
14.76
3
50
11.76
4
75
7.76
5
100
4.74
Table 1: Calibration data

Conversion versus Conductivity


120
100

f(x) = - 7.45x + 134.92


R = 1

80
Conversion (%)

60

Conversion, %
Linear (Conversion, %)

40
20
0
4

8 10 12 14 16 18 20
Conductivity

Graph 1: Calibration curve of conversion versus conductivity


According to the calibration curve, the higher the conductivity, the lower the
conversion. Conductivity is caused by the ionic solution such as sodium
hydroxide and sodium acetate. Sodium hydroxide has a higher conductivity
compared to sodium acetate. Therefore, when sodium hydroxide is used to
produce sodium acetate; the concentration of the strong sodium hydroxide ions
decreases, thus causing the conductivity to decrease as well. Based on the best
line obtained, the relationship between conversion and conductivity can be
expressed in the equation of

y=7.4476 x+134.92 .

No
.

Time
(min)

Conductiv
ity

Conversion,
%

15.00

23.21

13.12

37.21

10

12.30

43.31

15

11.77

47.26

20

11.06

52.55

25

10.92

53.59

30

10.81

54.41

35

10.81

54.41

Table 2: Data for reaction at 30C

Conversion / Conductivity versus Time


60.00
50.00
40.00
Conversion (%) / Conductivity

Conductivity

30.00

Conversion, %

20.00
10.00
0.00
0 10203040
Time (min)

Graph 2: Graph of Conversion/ Conductivity versus Time for the reaction at 30C

No
.

Time
(min)

Conductiv
ity

Conversion,
%

14.14

29.61

10.71

55.16

10

10.53

56.50

15

10.66

55.53

20

10.65

55.60

25

10.53

56.50

30

10.53

56.50

35

10.53

56.50

Table 3: Data for reaction at 50C

Conversion / Conductivity versus Time


60.00
50.00
40.00
Conversion (%) / Conductivity

Conductivity

30.00

Conversion, %

20.00
10.00
0.00
0 10203040
Time (min)

Graph 3: Graph of Conversion/ Conductivity versus Time for reaction at 50C

Based on graphs 2 and 3, as the reaction time increases the rate of conversion
increases until a state of equilibrium has achieved and the reaction has ended.
The graph also shows that the conductivity decreases over time. This supports
the theory that sodium hydroxide has a higher conductivity than sodium acetate
and when sodium hydroxide is reacted to form sodium acetate in the
saponification reaction, the conductivity decreases. The conductivity decreases
faster and the rate of conversion in graph 3 is higher than graph 2 because the
temperature is higher for the experiment in graph 3 than graph 2. A reaction in a
higher temperature occurs faster because as the temperature increases, the
particles vibrate and move faster, causing them to collide more with each other.
This causes a higher rate of effective collisions and minimum activation energy is
needed to get the reaction started.

Application of batch reactor in chemical process industries


There are many types of batch reactors in chemical process industries a
sequential batch reactor is one of those reactors in industries. It is used mostly in
water treatment.
Secondly is the FED batch reactor. It is mostly used in fermentation processes.
Thirdly is the semi-batch reactor which is operated with both continuous and

batch input outputs. That means a semi-batch reactor can also function as a
continuously stirred tank reactor. This type of reactor is used in chlorinations.
Way to improve efficiencies of batch reactor
Cleaning and maintenance should be regularly done to improve the efficiency of
batch reactors. Flushing out precipitations and cleaning reactors may allow
reactors to perform more efficiently without regular breakdowns and the total
life-span of a reactor can be increased.
Conclusion
As a conclusion, sodium hydroxide contributes stronger conductivity
compare to sodium acetate. Thus, as the time increase, the concentration of
sodium hydroxide decrease and the conductivity decrease. At the same time, the
concentration of sodium increase and cause the conversion increase. Besides, as
the temperature increase, the conversion increase as well.
There are a few suggested steps to obtain more accurate result. Firstly,
make sure the concentrations of the reactants are accurately prepared. Next,
make sure that the conductivity meter is well calibrated. Last but not least,
safety precaution must be followed such as wear glove while handling chemical.

References
1. Control and Monitoring of Chemical Batch Reactors; 2011; Fabrizio
Caccavale, Francesco Pierri, Mario Iamarino, Vincenzo Tufano; page 2
&page 3.
2. Element of Chemical Reaction Engineering; Forth edition; 2006; H. SCOTT
FOGLER , Ame and Catherine Vennema Professor of Chemical Engineering,
The University of Michigan, Ann Arbor; page 10
3. http://www.engin.umich.edu/~cre/asyLearn/bits/batch/index.htm

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