ABSTRACT

This experiments main purpose is to study the non-catalytic homogenous reaction in an

isothermal batch reactor. This experiment allows the study effect of temperature upon the
reaction of ethyl acetate and sodium hydroxide in a batch reactor. It also determines the reaction
rate constant, K for the saponification of both the solutions. Likewise, determines the activation
of energy, E for the same reaction.

INTRODUCTION
Batch reactors are utilized broadly as a part of industry at all scales. Batch reactors are tanks,
ordinarily gave unsettling and a technique for warmth exchange. This sort of reactor is
essentially utilized for moderately moderate responses of a few hours length of time, subsequent
to the downtime for filling and exhausting vast hardware can be critical. Agitation is utilized to
keep up homogeneity and to enhance heat exchange. Batch reactor is specifically designed for a
detailed study of this process. In this experiment, the change of sodium hydroxide, NaOH
concentration and conductivity is observed. By using the integral method of analysis, the
reaction is found to be second order reaction. The experimental activation energy is determined
as well if the experiment is conducted in different temperatures. The reaction chosen is the
saponification of ethyl acetate by sodium hydroxide. Saponification is a process that produces
soap. Technically it involves base that is NaOH to form sodium salt of a carboxylate.
CH 3COOC 2H5 NaOH CH 3COONa C2H5OH EtAc NaOH NaAc EtOH
Ethyl acetate sodium hydroxide

sodium acetate ethanol

MATERIALS AND METHODS

A 1L of 0.1M NaOH solution and 1L of 0.1M ethyl acetate solution were prepared. As well as
400ml of NaOH was prepared in two 500ml beakers. Then the burette was carefully filled with
0.1M hydrochloric acid, HCl (Standard Solution) using a 20ml measuring cylinder. This burette
was prepared for titration of the sample that will be collected in time. Once the burette was filled,
the valves V1-V2 was made sure that it was closed. As the water in the water bath was prepared,
the ethyl acetate solution was filled into the reactor consequently. After making sure that the
ON/OFF switches are at OFF point, the reaction temperature was set (ambient to 70 C)
accordingly by increasing, decreasing and set button of DTC. Then the electric supply was
connected to the set up. The set up was then switched on along with the heater and stirrer of the
bath. Once the constant temperature was reached, sodium hydroxide was filled into the same
reactor. Subsequently, the motor and stirrer of the reactor was switched on. Then at regular
intervals of 5 minute, 10ml of the reaction mixture was collected using a measuring cylinder.
Then the sample of reaction mixture was transferred to conical flask that contained 20ml 0.1M
HCl. instantly 3 to 5 drops of phenolphthalein was added as an indicator. The solution was then
titrated directly and subsequent solutions were titrated for next 4 intervals of 5 minutes till the
mixture reached equilibrium. When the experiment was over, all the feed flow was stopped by
closing the valves. The heater, stirrer of water bath and the stirrer of reactor were switched off.
The air pressure was also reduced to 0kg/cm 2 by using the pressure regulator and pressure gauge.
The reactor then was drained out.

RESULTS AND DISCUSSION

1.987
800ml
20ml
10ml
0.0825
0.0825
0.1

Real gas constant R

Working volume of reactor VR
Volume of HCl VHCl
Volume of sample VSAMP
Normality of NaOH in feed solution NNaOH
Normality of NaOH used for titration N1
Normality of HCl NHCl

Table 1: Titration volume according to time intervals and temperature

o
o
T( C) = 45 C
V1(ml)
29.5
31.5
31.6
31.3
31.2

Time [min]
5
10
15
20
25

o
Table 2: Conversion rate and rate reaction constant at temperature of 45 C

Time (min)

(min)

XA

[1-XA]

5
10
15
20
25

5
10
15
20
25

0.566
0.401
0.393
0.418
0.426

0.188
0.359
0.368
0.339
0.329

XA/ [1-XA]
2.8351
1.1169
1.0679
1.2330
1.2948

K
(L/mol.min)
44.1095
15.6982
10.3163
8.0837
6.5686

Table 3: Temperature and rate constants

4

T (K)

1/T (K)

lnK

318

3.144710-03

207.14

5.333

vs XA/[1-XA]
3
2.5
2

XA/ [1-XA]2

1.5
1
0.5
0
5

10

15

20

25

(min)

o
Figure 1: Changes in conversion factor according to reaction time at temperature 45 C
In this experiment, the solution ethyl acetate is not conductive whereas sodium hydroxide is
highly conductive. From this relation, the decrease in conductivity that occurs as the reaction
proceeds also indicates a decrease in sodium hydroxide concentration.
5

Since sodium hydroxide is being consumed over time, its concentration declines with time as per
Table 1. By using the integral method, can conclude that the overall reaction rate is second order.
However, the experiment shows inaccurate results in Figure 1. Moreover, the calculated reaction
rate constant and activation energy did not equal for the used temperatures. This is mainly due to
lack of precision in recording the conductivity. From the results obtained from Figure 1, which
settles that increasing the reaction temperature results in an increase in the reaction rate constant.

CONCLUSION AND RECOMMENDATION

The batch reactor study is carried out experimentally. The first objective of this study is to
determine the order of this saponification reaction. The second objective is to determine the rate
constant of the reaction which can be calculated. Based on the result that we obtained, the order
of saponification reaction can be determined. Furthermore, the rate of reaction can be calculated
from the slope of the graph in Figure1. The deviation of graph in Figure is due to the lateness of
addition of sample into hydrochloric acid, HCl that will quench the reaction between sodium
hydroxide and ethyl acetate. The deviation of graph between minute 0 to minute 10 is due to the
titration process in which he pink colour needs to obtain is not as light as needed. Furthermore,
through this experiment the reaction that was studied in order to improve the understanding and
gain hands on experience in reaction engineering in broad and batch reactors in specific. The
error percentage that resulted at the end of the calculations was found to be relatively high. This
is a result of human error factor.
Hence there are few recommendations regarding this study. The titration process should be done
slowly in order to get the first point in which the light pink of the sample is obtained. Then the
sample must be quickly added into the HCL to avoid any experimental error. When the burette
readings are taken, use white paper placed behind the measurements to read the readings.

REFERENCES
1. Kenneth A. ConnorsChemical Kinetics, the study of reaction rates in solution, 1991,
VCH Publishers
2. Levenspiel, O. (1999). Chemical Reaction Engineering (3rd Edition). John Wiley.
3.

APPENDICES
Sample Calculations
CA0 = NNaOH (mole/L)
CA0 = 0.1 mole/L

HCIO =

V HCl N HCl
(moles)
1000

HCIO =

0.02 0.1
=2 106 moles
1000

HCIR = HCIO-

V 1 N1
(mole)
1000

6
HCIR = (2 10 ) -

(0.0295)(0.0825)
=4.3375 107 mole
1000

CA =

HCIR
mole
1000(
)
V SAMP
L

CA =

4.3375 107
mole
1000=0.043375
0.01
L

C A C

XA =

XA =

K=

CA

0.10.043375
=0.5663
0.1

C A C
L
(
)
t C A C A mole min
0

K=

0.10.043375
L
=2.611
5 0.1 0.043375
mole min

1
L
(
)
Kt = S 1 C A mole min ;
0

S1: slope of vs XA/ [1-XA]

Kt =

1
L
=207.14
0.04828 0.1
mole min

10