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Continuous Stirred Tank Reactor: Operating & Experimental Manual
Continuous Stirred Tank Reactor: Operating & Experimental Manual
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OPERATING
MANUAL
&
EXPERIMENTAL
CONTINUOUS
STIRRED TANK
REACTOR
MODEL: BP 143
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OPERATING PROCEDURES
General Start-Up Procedures
1. Prepare the following solutions:
a) 40 L of sodium hydroxide, NaOH (0.1M)
b) 40 L of ethyl acetate, Et(Ac) (0.1M)
c) 1 L of hydrochloric acid, HCL (0.25M), for quenching
2. Ensure that all valves are initially closed.
3. Charge the feed vessels as follows:
a) Open the charge port caps for vessels B1 and B2.
b) Carefully pour the NaOH solution into vessel B1 and the Et(Ac) solution into vessel B2.
c) Close the charge port caps for both vessels.
4. Turn on the power for the control panel.
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.
8. Open valves V2, V3, V7, V8 and V11.
9. The unit is now ready for experiment.
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EXPERIMENTAL PROCEDURES
Preparation of Calibration Curve for Conversion vs. Conductivity
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.
NaOH + Et(Ac) Na(Ac) + EtOH
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:
1. Prepare the following solutions:
a) 1 liter of sodium hydroxide, NaOH (0.1 M)
b) 1 liter of sodium acetate, Et(Ac) (0.1 M)
c) 1 liter of deionised water, H2O
2. Determine the conductivity and NaOH concentration for each conversion values by mixing the following
solutions into 100 ml of deionised water:
a) 0% conversion : 100 ml NaOH
b) 25% conversion : 75 ml NaOH + 25 ml Et(Ac)
c) 50% conversion : 50 ml NaOH + 50 ml Et(Ac)
d) 75% conversion : 25 ml NaOH + 75 ml Et(Ac)
e) 100% conversion : 100 ml Et(Ac)
ANALYSIS AND DISCUSSION:
1. Record all data in the sample table in Appendix A.
2. Plot the calibration curve of conductivity vs conversion. Determine the slope and y-axis intercept.
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= CNaOH
mol/L
Volume of sample
= Vs
ml
= CNaOH,f
mol/L
= VHCl,s
ml
= CHCl,s
mol/L
= V1
ml
= CNaOH,s
mol/L
Known quantities:
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Calculations:
Conc. of NaOH entering the reactor, CNaOH,0
= (CNaOH,f)/2
= VHCl,s V2
ml
= (CHCl,s V3)/1000
mol
= n1
mol
= n2 / (Vs 1000)
mol/L
C
= 1 - NaOH x100%
C NaOH, s
C HCl,s
V1
CNaOH ,0
mol/L
ml
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VCSTR
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
VCSTR =
VTFR =
FA 0 X
- rA
FA 0
kCA2
F0 (C A0 - C A )
kCA2
(C A0 - C A )
tC A2
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(C A0 - C A )
tC A2
4. Plot the graph of ln k vs 1/T and evaluate the slope and y-axis intercept.
5. Calculate the saponification reactions activation energy, E and Arrhenius constant, A from the
slope and intercept values using the Arrhenius equation.
k (T ) = Ae
-E
RT
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APPENDIX A
SAMPLE TABLE FOR PREPARATION OF CALIBRATION CURVE
APPENDIX B
SAMPLE TABLE FOR EXPERIMENTS 1 & 2
Reactor volume = _____ L
Concentration of NaOH in feed vessel = _____ M
Concentration of Et(Ac) in feed vessel = _____ M
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APPENDIX C
PHYSICAL PROPERTIES OF COMPONENTS
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