ABSTRACT

The SOLTEQ Reactor Service Unit (Model: BP 150) was run with a Continuous Stirred Tank
Reactor (CSTR), to observe its system functionality and potential while experimenting its effects
on flow changes. The experiment was done to determine the rate constant from the data collected
and also to observe the temperature effects on the reaction, also primarily experimented to study
the dynamics of a CSTR during different stages of its continuous operation by conducting the
process of saponification reaction between sodium hydroxide and ethyl acetate in CSTR.
Ultimately the objective was to measure the conversion of ethyl acetate in saponification as a
function of design parameters in a continuous stirred tank reactor (CSTR). The reaction rate
constant shall also be determined.
Before the unit was set up for experiment, the conductivity calibration curve (Conversion vs.
Conductivity) was prepared, since the rate of reaction depends on both concentrations of Et(Ac)
and NaOH. The reaction kinetics and the rate law of process can be obtained from this curve.
The reactor unit, comes with an electronic instrumentation with digital indicators to monitor
continuously temperature and conductivity. The conductivity of the reaction mixture changed
with conversion and therefore the extent of the reaction was monitored by recording the
conductivity with respect to time. The calibration curve was used to relate conductivity data to
the concentration value. The conductivity measurement is necessary as it indicated the degree of
conversion of the saponification reaction. The experimental results were used, to determine the
effect of temperature on the reaction kinetics and the effect of residence time on the extent of
conversion, also to calculate the reactions activation energy using Arrhenius equation and to
study the residence time distribution (RTD) using step change input.
PROCEDURE
General Start-Up Procedures
1. Valves V3, V7 and V12 were kept open, and the rest of the valves were closed at first.
2. 30 Liters of salt solution, sodium chloride, NaCl 0.10 M was prepared.
3. Tank B2, was filled with the prepared NaCl 0.10 M solution.
4. The control panel was powered on.
5. Connect the water de-ionizer to the laboratory water supply. Open valve V9 and fill up
feed tank B1 with the de-ionized water. Close valve V9.
6. The water de-ionizer was connected to the laboratory water supply, then Valve V9 was
opened and tank B1was filled with the de-ionized water.
7. Open valves V2, V4 and V17. Switch on pump P2. Adjust valve V4 and V3 to obtain a
flow rate of approximately 200 ml/min at flow meter FI-02. Close valves V17 and switch
off pump P2.
8. Valves V2, V4 and V17 was opened and Pump P2 was switched on. Valves V4 and V3
was adjusted to an approximate flowrate of 200 ml/min on the flow meter FI-02. Valve
V17 was closed and Pump P2 was switched off.
9. Valves V6, V8 and V18 were opened and Pump P3 was switched on. Then Valves V8 and
V7 were adjusted to an approximate flowrate of 200 ml/min on the flow meter FI-01.
Valve V18 was closed and Pump 3 was switched off following that.
10. The unit was ready to run the experiment.

CSTR Setup procedure

1. All Valves V1 to V27 was closed.
2. CSTR Reactor R2 - Flexible hoses for port A to port C were connected as such:
i. Port A: connected to QI02
ii. Port B: connected to QI01
iii. Port C: connected to valve V27
3. Valves V25 and V27 was opened (to waste tank) for an overflow of working volume 3L.

General Shut-Down Procedures

1. Pumps P1, P2 and P3 were switched off.
2. The heaters were switched off.
3. The cooling water was kept to circulate through the reactor while the stirrer motor was
running allowing the water jacket to cool down to room temperature.
4. Since the equipment was not to be operated prolonger further, all the liquid from the unit
was drained out by opening valves V1, V5, V14, V20, V23, V24, V26, V27 (to waste
tank) and V33.
5. The control panel was powered off.
Procedure of Preparation of Calibration Curve for Conversion vs. Conductivity

1. The following solutions were prepared:

a) 1 liter of sodium hydroxide, NaOH (0.1 M)
b) 1 liter of sodium acetate, Na(Ac) (0.1 M)
c) 1 liter of deionized water, H2O

2. The conductivity and the concentration of NaOH for each conversion values were determined
by mixing the following solutions into 100 ml of deionized water:
a) 0% converted : 100 ml NaOH
b) 25% converted : 75 ml NaOH + 25 ml Na(Ac)
c) 50% converted : 50 ml NaOH + 50 ml Na(Ac)
d) 75% converted : 25 ml NaOH + 75 ml Na(Ac)
e) 100% converted : 100 ml Na(Ac)

REFERENCES
1. Danish M., Al Mesfer M. K. (2015). A Comparative Study of Saponification Reaction in
a PFR and CSTR. Research Journal of Chemical Sciences, 5(11), pp. 13 17.

2. Fogler H.S., Elements of Chemical Reaction Engineering, Prentice Hall Professional

Technical Reference, (2006)

3. Grau M.D., Nougues J.M. and Puigjaner L., Comparative Study of Two Chemical
Reactions with Different Behavior in Batch and Semibatch Reactors, Chem. Eng. J., 88,
225-232 (2002)

4. Bursali N., Ertunc S. and Akay B., Process Improvement Approach to Saponification
Reaction Using Statistical Experimental Design, Chem. Eng. Process., 45, 980-989
(2006)

5. Levenspiel O., Elements of Chemical Reaction Engineering, John Wiley and Sons, Third
Edition, 38-39 (1999)