Introduction

This batch reactor experiment was split into three parts which are calibration curve for
conductivity vs conversion, batch saponification reaction of ethyl acetate and sodium hydroxide
at room temperature and the effect of temperature on batch saponification reaction of ethyl
acetate and sodium hydroxide. In Part 1, the main objective is to plot the calibration curve to
determine the gradient which is the reaction order and y-axis intercept which is the rate constant
to be used as a baseline. In Part 2, the main objective is to determine the reaction rate constant by
plotting a graph of ln (dCA/dt) vs ln (CA) and finding the gradient which is the reaction order and
rate constant (k) which is the y-axis intercept value. In Part 3, the main objective is to determine
the effects of temperature on the extent of conversion and to determine the activation energy of
the reaction using the Arrhenius equation by plotting the graph of ln k vs 1/T.
Underlying Theory

The Batch reactor is a common reactor used in process industries. Its typically used in
process operations such as solids dissolution, product mixing, chemical reactions, batch
distillation, crystallization, liquid/liquid extraction and polymerization (Christopher, 2018).
Batch reactors are also typically used in fermentation process for beverage products and waste
water treatment (Razi, 2010). A typical batch reactor consists of a tank with an agitator and
integral heating/cooling system (Christopher, 2018).

The batch chemical process is a discontinuous process, which does not have inlet flow
and an outlet flow. Thus, the mass balance obeys the following statement:

𝑑𝑁𝑗
𝐺𝑒𝑛𝑒𝑟𝑎𝑡𝑖𝑜𝑛(𝐺𝑗 ) = 𝐴𝑐𝑐𝑢𝑚𝑢𝑙𝑎𝑡𝑖𝑜𝑛 ( )
𝑑𝑡

In this experiment, the reaction being conducted is the saponification of ethyl acetate Et
(Ac) and sodium hydroxide NaOH. The reaction is shown in following equation.

𝑁𝑎𝑂𝐻 + 𝐸𝑡(𝐴𝑐) → 𝑁𝑎(𝐴𝑐) + 𝐸𝑡𝑂𝐻

The conversion of component j in constant volume system can be determined using the
formula below:

(𝑁𝑗0 − 𝑁𝑗 )
𝑋𝑗 = 𝑁𝑗0

Where,
Nj0 = initial amount of j at t = 0
Nj = present amount at time t
 Below shown is the Arrhenius equation where ln (k) represents the y-axis, ln (A) the y-
𝐸
axis intercept and − which is the slope represented in graphical form.
𝑅
𝐸 1
ln(𝑘) = ln(𝐴) − ( )
𝑅 𝑇

Where,
E = Activation Energy (J/mol)
A = Arrhenius Constant
R = Universal Gas Constant (8.314 J/mol.K)
T = Absolute Temperature (K)
Description of Apparatus
The apparatus used in conducting our saponification reaction between ethyl acetate and
sodium hydroxide is the SOLTEQ batch reactor.

General Start Up Procedure

10 L or sodirum hydroxide (0.1M) and ethyl acetate (0.1M) was prepared in tank B1 and
B2. All valves were ensured to be closed except for bypass valve V3 and V6. The water
circulator was then filled with water and the power for the control panel was turned on. Stirrer
M1 was then turned on and the speed was adjusted to 200 rpm and then was switch off. Valves
V2 and V5 was then opened ready for experimentation.

Part 1: Calibration Curve for Conductivity vs Conversion

Five 100 mL beakers

pH Meter

1 L sodium hydroxide (0.1M)

1 L sodium acetate (0.1M)

1 L deionized water

100 mL measuring cylinder

Part 2: Batch Saponification Reaction of Ethyl Acetate and Sodium Hydroxide at Room
Temperature

SOLTEQ Batch Reactor

10 L of 0.1M sodium hydroxide
10L of 0.1M ethyl acetate
Stop Watch
Part 3: The Effect of Temperature on Batch Saponification Reaction of Ethyl Acetate and
Sodium Hydroxide

SOLTEQ Batch Reactor

10 L of 0.1M sodium hydroxide
10L of 0.1M ethyl acetate
Stop Watch

Experimental Method
The saponification reaction between ethyl acetate and sodium hydroxide was conducted
in three parts, the first part is the calibration curve for conductivity vs conversion, the second part
the batch saponification reaction of ethyl acetate and sodium hydroxide at room temperature and
the third part is the effect of temperature on batch saponification reaction of ethyl acetate and
sodium hydroxide.

Part 1: Calibration Curve for Conductivity vs Conversion

1 L of 0.1M sodium hydroxide, 1 L of 0.1M sodium acetate and 1 L of deionized water
was prepared. The calibration solutions were prepared in the following ratios, 0% conversion:
100mL NaOH, 25% conversion: 75mL NaOH + 25 mL Na(Ac), 50% conversion: 50mL NaOH
+ 50mL Na(Ac), 25mL NaOH + 75mL Na(Ac) and 100% conversion: 100mL Na(Ac) which
were all prepared in 100 mL beakers. After preparing the 5 solutions, a pH meter was inserted
into each beaker and was used to measure the conductivity of each solution mixture. Once the
readings were tabulated, the calibration curve of conductivity vs conversion was plotted and the
gradient and y-axis intercept was determined.
Part 2: Batch Saponification Reaction of Ethyl Acetate and Sodium Hydroxide at Room
Temperature
The general start up procedure as shown in description of apparatus was performed.
Pump P2 was switched on and valve V5 was opened. Reactor R1 was filled with 0.1M Et(Ac) to
1.5 L volume and then pump P2 was stopped. Pump P1 was then switch on and valve V2 was
opened to fill the reactor R1 with 0.1M NaOH until the solution reaches a total of 3 L volume
after which pump P1 was stopped. Stirrer M1 was switched on and the timer was immediately
started using a stop watch. The conductivity values were recorded at 1-minute intervals. The
experiment was stopped when the conductivity values became constant. Valve V8 was then
opened and the solution was drained from the reactor into waste tank B3. The graph of
conversion vs time was plotted and well as the graph of ln(dCA/dt) vs ln (CA) and the slope and
y-axis intercept was determined.

Part 3: The Effect of Temperature on Batch Saponification Reaction of Ethyl Acetate and
Sodium Hydroxide
The general start up procedure as shown in description of apparatus was performed. The
TIC-01 temperature controller was set to 40°C. The water circulator was then switched on and
the temperature was set 5°C higher than the desired reaction temperature and both the feed tanks
were allowed to reach to desired temperature. Once desired temperature is reached, pump P2 was
switched on and valve V5 was opened. 1.5L of 0.1M Et(Ac) was filled into the reactor then
pump P2 was stopped and valve V5 was closed. Pump P1 was then switched on and valve V2
was opened to fill the reactor with 1.5 L of 0.1M NaOH until the solution reaches 3L in total
then pump P1 was stopped and valve V2 was closed. Heater W1 and stirrer M1 was then
switched on and the stop watch was started immediately. The conductivity values were recorded
at 1-minute intervals. The experiment was stopped when the conductivity values became
constant and heater W1 was switched off. The experiment was repeated for reaction temperatures
of 50°C, 60°C and 70°C. The results were tabulated and for each temperature a graph of 1/CA vs
time was plotted and the slope and y-axis intercept was determined. The rate constant, k can be
determined from the slope for each different temperature. The graph of ln k vs 1/T was plotted
and the slope and y-axis intercept was determined. The activation energy (Ea) of the
saponification reaction and Arrhenius constant (A) can be determined using the Arrhenius
equation mentioned in the underlying theory section.

References

Christopher, Saints Burner. "Introduction for Batch Reactor Experiment." Scribd. Accessed
March 31, 2018. https://www.scribd.com/doc/231973043/Introduction-for-batch-reactor-
experiment.

Razi ,Fakhru’l-. "Application of Membrane-coupled Sequencing Batch Reactor for Oilfield

Produced Water Recycle and Beneficial Re-use." Bioresource Technology. April 30,
2010. Accessed March 31, 2018.
https://www.sciencedirect.com/science/article/pii/S0960852410006656.