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Continuos Stirred Tank Reactor Experiment
Continuos Stirred Tank Reactor Experiment
CONTINUOUS
STIRRED TANK
REACTOR
MODEL: BP 143
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CPE554 Universiti Teknologi MARA
OPERATING PROCEDURES
5. Check that there is sufficient water in the thermostat T1 tank. Refill as necessary.
6. Open cooling water valve V13 and let the cooling water flow through the condenser W1. (Only for
Experiment 2)
7. Adjust the overflow tube to give a working volume of 10 L in the reactor R1.
2. Switch off both pumps P1 and P2. Switch off stirrer M1.
3. Switch off the thermostat T1. Let the liquid in the reaction vessel R1 cool down to room
temperature.
5. Close valves V2, V3, V7 and V8. Open valves V4, V9 and V12 to drain any liquid from the unit.
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CPE554 Universiti Teknologi MARA
EXPERIMENTAL PROCEDURES
The reaction to be studied is the saponification reaction of ethyl acetate Et(Ac) and sodium hydroxide
NaOH. Since this is a second order reaction, the rate of reaction depends on both concentrations of Et(Ac)
and NaOH. However, for analysis purposes, the reaction will be carried out using equimolar feeds of Et(Ac)
and NaOH solutions with the same initial concentrations. This ensures that both concentrations are similar
throughout the reaction.
The following procedures will calibrate the conductivity measurements of conversion values for the reaction
between 0.1 M ethyl acetate and 0.1 M sodium hydroxide:
PROCEDURES:
2. Determine the conductivity and NaOH concentration for each conversion values by mixing the following
solutions into 100 ml of deionised water:
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CPE554 Universiti Teknologi MARA
It is advisable to carry out manual conversion determination on experiment samples to verify the
conductivity measurement values. The following procedures will explain the method to carry out back
titration on the samples. It is based on the principle of quenching the sample with excess acid to stop any
further reactions, then back titrating with a base to determine the amount of unreacted acid.
PROCEDURES:
3. Obtain a 50 ml sample from the experiment and immediately add the sample to the HCl in the flask to
quench the saponification reaction.
5. Titrate the mixture with NaOH solution from the burette until the mixture is neutralized. Record the
amount of NaOH titrated.
Unknown quantity:
Known quantities:
Volume of sample = Vs ml
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CPE554 Universiti Teknologi MARA
Calculations:
C NaOH, s
Volume of unreacted quenching HCl, V2 = V1 ml
C HCl,s
æ C ö
Conversion of NaOH in the reactor, X = çç1 - NaOH ÷÷ x100%
è CNaOH ,0 ø
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CPE554 Universiti Teknologi MARA
OBJECTIVE:
PROCEDURES:
2. Switch on both pumps P1 and P2 simultaneously and open valves V5 and V10 to obtain the
highest possible flow rate into the reactor.
3. Let the reactor fill up with both the solution until it is just about to overflow.
4. Readjust the valves V5 and V10 to give a flow rate of about 0.1 L/min. Make sure that both flow
rates are the same. Record the flow rate.
5. Switch on the stirrer M1 and set the speed to about 200 rpm.
6. Start monitoring the conductivity value at QI-401until it does not change over time. This is to
ensure that the reactor has reached steady state.
7. Record the steady state conductivity value and find the concentration of NaOH in the reactor and
extent of conversion from the calibration curve.
8. Open sampling valve V12 and collect a 50 mL sample. Carry out a back titration procedure to
manually determine the concentration of NaOH in the reactor and extent of conversion (Section
5.2).
9. Repeat the experiment (steps 5 to 9) for different residence times by adjusting the feed flow rates
of NaOH and Et(Ac) to about 0.15, 0.20, 0.25 and 0.30 L/min. Make sure that both flow rates are
the same.
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CPE554 Universiti Teknologi MARA
2. Plot a graph of conversion vs. residence time. The reactor’s residence time is defined as the
reactor volume divided by the total feed flow rates.
VCSTR
Residence time, t =
u0
3. For a second order equimolar reaction with the same initial reactants’ concentration ( CA0 = CB0 ) ,
the rate law is shown to be:
- r A = kC AC B = kCA2
FA 0 X
VCSTR =
- rA
FA 0 F0 (C A0 - C A )
VTFR = =
kCA2 kCA2
4. For different reactor residence times, calculate the value of the reaction rate constant, k and the
rate of reaction, -rA.
Reaction rate constant, k =
(C A0 - C A )
tC A2
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CPE554 Universiti Teknologi MARA
OBJECTIVE:
PROCEDURES:
2. Switch on both pumps P1 and P2 simultaneously and open valves V5 and V10 to obtain the
highest possible flow rate into the reactor.
3. Let the reactor fill up with both the solution until it is just about to overflow.
4. Readjust the valves V5 and V10 to give a flow rate of 0.20 L/min. Make sure that both flow rates
are the same. Record the flow rate.
5. Switch on the stirrer M1 and set the speed at about 200 rpm.
7. Start monitoring the conductivity value at QI-401 and temperature value at TI- 101 until they do not
change over time. This is to ensure that the reactor has reached steady state.
8. Record the steady state conductivity and temperature values and find the concentration of NaOH in
the reactor and extent of conversion from the calibration curve.
9. Open sampling valve V12 and collect a 50 mL sample. Carry out a back titration procedure to
manually determine the concentration of NaOH in the reactor and extent of conversion (Section
5.2).
10. Repeat the experiment (steps 7 to 10) for different reactor temperatures by setting the thermostat
temperature to 50, 60, 70, and 80 ºC. Make sure that the flow rates of both solutions are
maintained at 0.20 L/min.
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CPE554 Universiti Teknologi MARA
3. For different reactor temperatures, calculate the value of the reaction rate constant, k.
4. Plot the graph of ‘ln k’ vs ‘1/T’ and evaluate the slope and y-axis intercept.
5. Calculate the saponification reaction’s activation energy, E and Arrhenius constant, A from the
slope and intercept values using the Arrhenius equation.
-E
k (T ) = Ae RT , R = universal gas constant (8.314 J/mol.K)
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CPE554 Universiti Teknologi MARA
APPENDIX A
APPENDIX B
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APPENDIX C
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