LABORATORY MANUAL DECLARATION FORM Editted

LABORATORY MANUAL JULY 2010 REACTION ENGINEERING (CKB 20104)
LABORATORY REPORT GUIDELINES

REACTION ENGINEERING (CKB 20104)
Each experimental report should contain the following items in accordance to the numbering as listed:
1. COVER PAGE
Please insert the LABORATORY REPORT SUBMISSION FORM as the front cover.
DOWNLOAD FROM E LEARNING
2. TABLE OF CONTENTS
The table of content and number of pages should be in following format.
Note: Each page should be numbered.
Content Page Number
Summary
1.0 Results and Discussions
2.0 Conclusions
3.0 References
4.0 Tutorial
5.0 Appendices
3. SUMMARY
Give the summary (not more then half page) on the overall experimental report. Give brief
review on the objectives of the experiment, main experimental results and discussions which
are deemed significant and finally conclusions obtained from the work.
4. RESULTS AND DISCUSSIONS

Note: Refer to the respective experimental procedure (Analysis and Discussions sections)
to determine the extent of analysis and discussions required.
A. Record down and present each of the experimental data and findings in proper manner
B. Present the data either in Table, Graph, Histogram or Pie chart form as deemed suitable
with complete label and units.
C. Explanations of the referred table and figure must be presented below the table and figure.
1
Example Table:
Table 1: X vs. Y
Samples X (unit) Y (unit)
A
B
C
D
Example Graph:
2.0
1.8
1.6
1.4
Parameter Y (unit)
1.2
1.0
0.8
y = -0.7886x + 1.7986
0.6
0.4
0.2
0.0
0.0 0.5 1.0 1.5
Parameter X (unit)
Figure 1: Relationship between X and Y
D. Based on the experimental results, discuss on your findings and relate to your theory and
objective of experiment
7. CONCLUSIONS
A. Summary of the results to relate briefly the findings or results with the theory applicable to
the experimental
B. Suggest improvements in apparatus or measurement procedure, or even experimental
procedures for future work (if applicable).
C. Should be in one paragraph.
8. TUTORIAL
Tutorial are the questions as given in the laboratory procedures. All questions must be
answered as required or else marks would not be rewarded for this section.
NOTE: STUDENTS ARE GIVEN OPTION TO HANDWRITE THE CALCULATIONS
PART AS TASKED IN THE REPORT. HOWEVER THE OTHER PART OF THE
REPORT SHOULD BE TYPED.
2
9. REFERENCES
Details of published sources of material referred to or quoted in the text (including any lecture
notes and URL addresses of any websites used.).
REFERENCES SHOULD BE IN COMPLETE FORM AS GIVEN BELOW OR ELSE
MARKS WILL BE DEDUCTED FOR EACH ERROR.
A. The references should be in following format:
1. Books/Journals: Authors (editor), title, publisher, (year), chapter or page number
Example:
Smith J.M and Van Hess H.C., Introduction to Chemical Engineering
Thermodynamics, McGraw-Hill, New York, 2001, p229
2. Internet Website: Title of the information, year, source of data, [Online]. [Date
Accessed]. Available from World Wide Web
Example:
BP (British Petroleum). (2007) BP Statistical review of world energy. [Online].
[Accessed 19th January, 2008]. Available from World Wide Web:
http://bp.com/statisticalreview.
B. The references should be arranged according to the author name in alphabetical order
10. APPENDICES
All the raw data should be included here.
IMPORTANT NOTE:
1. LABORATORY REPORTS ARE MEANT TO BE GROUP TASKS. EACH MEMBER OF
THE GROUP IS REQUIRED TO CHOOSE 1 PART OF EACH SECTION TO BE
EXECUTED INDIVIDUALLY. THEREFORE ANY INFORMATION COPIED FROM
ANOTHER GROUP OR TAKEN DIRECTLY FROM OTHER SOURCES SUCH AS THE
INTERNET WITHOUT PROPER REFERENCES WILL NOT BE TOLERATED AND
THE REPORT WILL BE MARKED AS ZERO.
2. LABORATORY REPORT SHOULD BE SUBMITTED THE FOLLOWING WEEK (7
DAYS) AFTER THE EXPERIMENTAL IS CONDUCTED. ANY LATE SUBMISSIONS
WITHOUT AGREEMENT OF THE LECTURER WILL RESULT IN 50% DEDUCTIONS
OF THE OVERALL MARKS.
3. LABORATORY REPORT SHOULD BE SUBMITTED DIRECTLY TO THE LECTURER
IN CHARGE FOR DATE VERIFICATION
3
The Dean/Head of Campus

Universiti Kuala Lumpur
Malaysian Institute of Chemical and Bioengineering Technology (MICET)
Lot 1988, Vendor City Industrial Area
Taboh Naning, 78000 Alor Gajah
Malacca
Dear Sir,
SAFETY DECLARATION
I ………………………………..…………………………………………………………. ID No
………………………. declared that I have read and understood the safety rules and regulations in
UniKL MICET. I hereby agree to abide by all the rules and regulations as stated in the safety
guidelines.
2. I hereby understood the contents and agreed to any disciplinary action taken against me, if I do
not abide by the stated rules.
3. I am fully responsible for all my actions during laboratory sessions.
Thank you.
Yours faithfully,
……………………………….
Name:
ID No:
Subject Name and Code:
Date:
4
LABORATORY MANUAL
REACTION ENGINEERING
CKB 20104
JULY 2010
LIST OF EXPERIMENTS:
EXPERIMENT 1: BATCH REACTOR

Experiment A: The Batch Saponification of Ethyl Acetate
Experiment B: Effect of Temperature on the Batch Saponification
Reaction
EXPERIMENT 2: CONTINUOUS STIRRED TANK

REACTOR (CSTR)
Experiment A: Effect of RTD on the Reaction in a CSTR
Experiment B: The Effect of Temperature on the Reaction in a
CSTR
EXPERIMENT 3: PLUG FLOW REACTOR (PFR)

Experiment A: Effect of Residence Time on the Reaction in a PFR
Experiment B: Effect of Temperature on the Reaction in a PFR
EXPERIMENT 4: REACTOR TEST RIG (RTR)

Experiment A: Reactor Comparison Test
5
EXPERIMENT 1
BATCH REACTOR
OBJECTIVES
To measure the rate constant of the reaction between ethyl acetate and sodium hydroxide under
batch condition.
To study the liquid phase reaction kinetics in a batch reactor.
To study the effect of temperature on the reaction in CSTR
Keywords: Batch reactor; Kinetics; Saponification reaction; Activation energy
1.0 GENERAL DESCRIPTION
1.1 Description and Assembly

Before operating the unit and running experiments, you must familiarize yourself with
the unit’s components. Please refer to Figure 2 to understand the process. All glass
components of the QVF Batch Reactor unit are made of borosilicate glass with PTFE
gaskets.
1. Reactor (R1)
• Fused jacketed vessel with graduation, nominal capacity 10 L
• Bottom port for dead space reduced bottom outlet valve
• Jacket connections for heating agent
• Cover DN300 with connections for: Agitator
• Charge port with screw cap for feeding by hand
• Inlet for dosing vessel B1
• Vapour pipe with connection for distillate and vapour trap
• Conductivity and temperature sensor
2. Agitator (A1)
• Laboratory drive 230V / 50,60Hz
• 0.25 kW, 0-550 rpm, steplessly adjustable by hand
3. Dosing vessel (B1)

• 2,000 mL graduated cylindrical vessel with overflow pipe
4. Condenser (W1)
• Coil heat exchanger, area 0.3 m 2
• Max coolant pressure of 3 bars with allowable temperature difference of 130°C
5. Instrumentation
• Temperature measurement (TI-101)
• Conductivity measurement (QI-401)
6
Chemical engineering processes can be broadly divided into two types: batch processes
and continuous processes. In a batch process, input materials are placed in a reactor
and product is withdrawn some time later. This is typical of what is normally done in
chemistry laboratories. You will be studying for batch conditions the reaction between
an ester (ethyl acetate) and sodium hydroxide:
CH 3 COOC 2 H 5 + OH − → CH 3 COO − + C 2 H 5 OH
This type of reaction is called a saponification because of its importance in the
manufacture of soap.
The reaction is relatively slow and the changing ester concentration can be followed
quite easily by analyzing samples from the reaction mixture every few minutes. The
second order rate constant is determined in two different ways:
a) Integrated rate law method
Assuming the reaction to be a simple, irreversible, second order process, then

the rate law for a batch process may be written
d[ester ]
= k [ester ][OH ]
−
Rate = −
dt
Suppose that the concentrations of the ester and hydroxide are equal at the start
of the experiment and equal to CA0 mol/dm3, and that at some time t later, both
the ester and hydroxide concentration have fallen to CA. Therefore we obtain
−
dC A
dt
[ ]
= k [ester ] OH − = kC A
2
Separating the variables and integrating with appropriate boundary conditions,

c t
dC A 1 1
∫c C 2 ∫0 dt ⇒ C A − C A0 = kt
= k
o A
A plot of 1/CA against t should give a straight line with the gradient, k.
7
b) Half-life method
1 1 1  C − CA 
From − = kt can be rearranged to give k =  A0 
C A C A0 t  C A C A0 
Let t1/2 be the time taken for the concentration of ester to be halved, C A = C A0 / 2
then
1
k=
t 1/2 C A0
The time taken to halve the concentration of ester is inversely proportional to
the initial concentration. From plot of the ester concentration CA against t, it is
possible to determine t1 / 2 and hence the rate constant.
1.2 Safety Considerations
1. Students must not carry out laboratory work without the supervision of a lecturer.
2. Read operating instructions carefully, and make sure that you fully understand all
aspects of operation of the batch reactor unit.
3. Safety glasses must be worn at all times during these experiments – remember you
are in charge of all safety aspects.
4. For each experimental setting, allow 10 minutes for equilibrium conditions to be

established.
5. After each experiment, make sure that the reactor and tubing are cleaned properly.
Sodium hydroxide and ethyl acetate both are corrosive and can damage the tubing’s
and the reaction rig.
6. Dispose all liquids immediately after each experiment. Do not leave any reactants
or product in the feed or product vessels.
7. Wipe off any spillage on the ground or working bench.
8. Plastic gloves and eye shields must be worn when handling corrosive liquids, and
heat resistant gloves when adjusting steam valves.
9. All experiments involving a potential explosive hazard must be conducted behind

special shields.
10. When working with solvents etc., ensure that the apparatus is adequately vented.
11. All used solvent should be handed to the technician and not disposed into drains or
laboratory sinks.
12. Smoking is forbidden in all laboratories.
13. Safety helmets must be worn.
8
14. Services equipment (vacuum generators) must in no circumstances be started up by

students.
15. Gas cylinders, when in use, should be adequately strapped to bench and supported
in the upright position, away from sunlight or flames. Ensure that cylinders are
shut-off after use.
16. Before using any chemical, ensure that you are familiar with its hazards and with
emergency procedures.
17. If in doubt, ask the lecturer in charge.
18. If chemical spillage occurs, evacuate the laboratory in an orderly fashion.
19. Plug in all cables into appropriate sockets before switching on the main switch.
Inspect all cables for any damage to avoid electric shock. Replace if necessary.
20. Do not switch on the heater unless it is fully submerged in the liquid. Always
maintain liquid level above the height of the heater to avoid damage to the heater.
2.0 EXPERIMENTAL PROCEDURES
Experiment A:
The Batch Saponification of Ethyl Acetate
1. Prepare the following solutions:
a) 1 L of sodium hydroxide, NaOH (0.1 M)
b) 250 mL of ethyl acetate, Et(Ac) (0.1 M)
c) 250 mL of hydrochloric acid, HCl (0.1 M)
2. Pipette 200 mL of 0.1M ethyl acetate, Et(Ac) solution into a clean dry conical flask
3. Placed 200 mL of 0.1M sodium hydroxide (NaOH) into 500 ml beaker.
4. Label 11 clean conical flasks from 1 to 11 and pipette 20 mL of 0.1M hydrochloric acid,
HCl into each of them (Flask 1 to 11).
5. Place the mechanical stirrer in the sodium hydroxide (NaOH) solution.
6. Turn on the stirrer and quickly pour all of the ethyl acetate, Et (Ac) from the conical flask
into the NaOH beaker, starting the stopwatch at roughly the mid-point of addition.
7. After 5 minutes, withdraw by pipette 20 mL of the reacting mixture and pour into Flask 1,
noting the time at the mid-point of delivery.
8. Record the temperature of the reacting mixture in the beaker.
9. Titrate the content of Flask 1 with 0.1M sodium hydroxide, NaOH using two or three drops
of phenolphthalein as indicator. The color of the indicator will change from colorless
(acidic) to pink (basic).
9
10. Stop the titration once the change of indicator color is observed. Determine the amount of
NaOH needed.
11. Withdraw further samples at 10 (Flask 2), 15 (Flask 3), 20 (Flask 4), 25 (Flask 5), 30
(Flask 6), 35 (Flask 7), 40 (Flask 8), 50 (Flask 9), 60 (Flask 10) and 75 (Flask 11) minutes.
Repeat step 6 to 10.
12. Record the results in Appendix A
3.0 ANALYSIS AND DISCUSSIONS
3.1 Method of Calculations to determine concentration of NaOH
Let titre of NaOH as = Y mL
Therefore the number of moles of 0.1M NaOH used in the titration

0.1(Y)
= mol
1000
= acid neutralized in titration
We know the initial quantity of 0.1M acid

0.1(20)
= mol
1000
Therefore the amount of acid neutralized by sample

0.1(20 - Y)
= mol
1000
= moles of NaOH present in the sample
Thus, NaOH concentration in 20 mL sample from the reactor

= Ester concentration
0.1 (20 − Y )
= × mol / mL
1000 20
1. Plot a graph conversion vs time and discuss it thoroughly.
2. List down the problems encountered when running the experiment and suggest
methods of improvement.
3. Explain why it is vital to conduct certain chemical reactions in bench scale up
4.0 TUTORIAL
Determine the rate constant, k using both methods and compare both values as
explained previously:
a. Integrated rate law method
b. Half-life method
10
* In the half-life method, the initial concentrations (CA0) can be obtained straight
forward. From the experimental data, for example we observed the concentration at, t
= 10 min (CA), therefore from the graph (CA versus t) we can determined how long it
takes for that concentration to be halved (t 1/2). Repeat this procedure for other times
during the experiment to check that the rate constant, k is indeed consistent.
Experiment B:
Effect of Temperature on the Batch Saponification Reaction
5.1 General Start-Up Procedures

b) 9 L of ethyl acetate, Et (Ac) (0.1 M)
2. Ensure that all valves are initially closed.
3. Turn on the power for the control panel.
4. Open cooling water valve and let the cooling water flow through the condenser.
5. The unit is now ready for experiment.
5.2 General Shut-Down Procedures

1. Keep the cooling water valve open to allow the cooling water to continue flowing.
2. Switch off the pump and heating. Let the liquid in the reaction vessel cool down to
room temperature.
3. Switch off the stirrer.
4. Close cooling water valve.
5. Open bottom valve to drain any liquid from the unit.
6. Turn off the power for the control panel.
5.3 Experimental Procedures

1. Perform the general start-up procedures
2. Measure and carefully pour 3 L of 0.1 M ethyl acetate solution into the reactor R1
through the charge port on the vessel cover.
3. Then, measure and carefully pour 3 L of 0.1 M sodium hydroxide solution into the
reactor R1 through the charge port on the vessel cover.
11
4. Switch on the stirrer and set the speed to 300 rpm. Set the heating temperature T1
and T2 at 50°C.
5. Start the timer simultaneously.
6. At every 5-minute intervals, open sampling valve (at the bottom) and collect a 2 mL
sample. Carry out a conductivity measuring by using conductivity meter.
7. Record your conductivity value in the Appendix C.
8. End the experiment when the conductivity values do not change significantly over
time.
9. Repeat the procedure 1-8 with the temperature at 60°C.
10. Perform the general shut-down procedures.
7.0 ANALYSIS AND DISCUSSIONS
1. Use the sample table in Appendix C for data collection.
2. Plot a graph conversion vs time for different temperature and subsequently compare
the conversions for the different temperature. Discuss it thoroughly and include
explanations on the effect of temperature onto the reaction.
3. Discuss the advantages and disadvantages of using batch reactors in chemical

reaction
4. Describe an example of industrial applications other than saponification that

utilized batch reactors in its process.
7.0 TUTORIAL
1. For a second order reaction, the rate law is shown to be:

-rA = - dCA/dt = kCA2
CA t
∫
CA 0
dCA/ CA2 = -k ∫ dt
0
1/CA = kt + 1/CA0
Where CA0 is the initial concentration of reactant NaOH in the reactor.
i) For each temperature value, plot the graph of ‘1/CA’ vs time, t and evaluate
the slope and y-axis intercept.
ii) Determine the rate constant, k from the slope value for different temperature
values. Examine the change in the rate constant.
12
iii) Plot a graph of ‘ln k’ vs ‘1/T’ and evaluate the slope and y-axis intercept.
iv) Calculate the saponification reaction’s activation energy, E and Arrhenius

constant, A from the slope and intercept values using the Arrhenius
equation. (R = 8.3014 J/mol.K)
8.0 REFERENCES
1. Atkins, P.W. ‘Physical Chemistry’ (various ed.)
2. Smith, J.M. ‘Chemical Engineering Kinetics ‘(3rd ed.), McGraw-Hill, 1981
3. Frost, A.A. & Pearson, R.G. ‘Kinetics and Mechanics’ (2nd ed.), Wiley, 1961
4. Fogler, H.S., Elements of Chemical Reaction Engineering, 3rd edition, Prentice Hall Int. Series,
N.J. (USA), 1997.
5. Levenspiel, O., Chemical Reaction Engineering, 3rd edition, John Wiley and Sons, 1999
6. Astarita G., “Mass Transfer with Chemical Reaction”, Elsevier, 1967.
7. Model SOLTEC BP 141 Operating Manual, Solution Engineering Bhd, KL.
13
APPENDIX A
SAMPLE TABLE FOR EXPERIMENT A
Amount of Concentration of
Time Flask Conversion,
NaOH titred NaOH,
(min) Number X (%)
(mL) CNaOH (M)
5 1
10 2
15 3
20 4
25 5
30 6
35 7
40 8
50 9
60 10
75 11
14
APPENDIX B
TABLE OF CALIBRATION CURVE
Solution Mixtures
Concentration Conductivity
Conversion 0.1 M
0.1 M NaOH H2O of NaOH (M) (mS/cm)
Na(Ac)
0% 100 mL – 100 mL 0.0500 10.7
25% 75 mL 25 mL 100 mL 0.0375 9.7
50% 50 mL 50 mL 100 mL 0.0250 7.5
75% 25 mL 75 mL 100 mL 0.0125 5.6
100% – 100 mL 100 mL 0.0000 4.0
Plot the calibration curve of conductivity vs concentration of NaOH (M). Determine the slope and y-
axis intercept
15
APPENDIX C
TABLE FOR EXPERIMENT B
Volume of NaOH = _____ L

Volume of Et(Ac) = _____ L
Initial concentration of NaOH = _____ M
Initial concentration of Et(Ac) = _____ M
Time Temperature Conductivity Concentration of Conversion,

(min) (°C) (mS/cm) NaOH, CNaOH (M) X (%)
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100
105
110
115
120
16
EXPERIMENT 2
CONTINUOUS STIRRED TANK REACTOR (CSTR)

OBJECTIVES
To study liquid phase reaction kinetics in a CSTR
To determine the conversion at different residence time.
To study the effect of temperature on the reaction in CSTR.
Keywords: CSTR; residence time; Mixing; Saponification kinetics; Activation energy
1.1 Description & Assembly

components of the QVF Continuous Stirred Tank Reactor unit are made of borosilicate
3.3 glass with PTFE gaskets.
1. Reactor (R1)
• Fused jacketed vessel with graduation, nominal capacity 10 L
• Bottom port for dead space reduced bottom outlet valve
• Jacket connections for heating agent
• Cover DN300 with connections for:
Agitator
Charge port with screw cap for feeding by hand
Inlet for feed vessels B1 and B2
Vapour pipe
Integrated conductivity and temperature sensor
2. Agitator (A1)
• Laboratory drive 230V / 50,60Hz
• 0.11 kW, 50-700 rpm, steplessly adjustable by hand, max torque 60 Ncm
3. Feed vessels (B1/B2)

• 50 L graduated cylindrical vessels
4. Pumps (P1/P2)
• Centrifugal pumps
• Max suction height of 3 m
5. Condenser (W1)
• Coil heat exchanger, area 0.2 m2
• Max coolant pressure of 2 bar with allowable temperature difference of 150°C
6. Receiving vessel (B3)

• 100 L rectangular tank
17
7. Instrumentation
• Flow measurement (FI-301, FI-302)
• Temperature measurement (TI-101)
• Conductivity measurement (QI-401)
1. The unit must be operated under the supervision of an authorized staff who has
been properly trained to handle the unit.
2. All operating instructions supplied with the unit must be carefully read and
understood before attempting to operate the unit.
3. Feed stock which severely affects PTFE, PFA and borosilicate glass are not to be
used.
4. The system should not be subjected to shock, sudden impact, vibration, additional
load, or permanent external action of aggressive vapours.
5. Always check and rectify any leakages.
6. Do not touch the hot components of the unit.
7. Be extremely careful when handling hazardous, flammable or polluting materials.
8. Restore the system to operating conditions after any repair job.
9. Make sure the system is sufficiently ventilated when working at atmospheric

pressure.
10. Do not exceed the maximum cooling pressure of 2 bar (g) for the top condenser
(W3) and product cooler (W4).
11. Only a properly trained staff should be allowed to carry out any servicing.
Manufacturer's manual must always be observed.
12. Before any servicing, shut down the whole operation, let the system cool down and
be properly ventilated.
13. Do not use any coarse or abrasive cleaners on glass components.
14. Leaking couplings should be carefully retightened. Replace any gaskets or seals if
necessary.
18
Vent
V1 V6
Cooling
Water
B1 B2 W1 Cooling
Water
V13
HS
1
Q1
M 401
TI
101
V2 V7
FI FI
301 302
V5 V10 R1
V3 V8
V3
V11
V4 V9
P1 P2
M M V12
HS HS
2 3 B3 T1
12
2.0 OPERATING PROCEDURES
2.1 General Start-up Procedures

b) 30 L of ethyl acetate, Et(Ac) (0.1 M)
3. Charge the feed vessels as follows:
4. Open the charge port caps for vessels B1 and B2.
5. Carefully pour the NaOH solution into vessel B1 and the Et(Ac) solution into vessel
B2.
6. Close the charge port caps for both vessels.
8. Switch on the heating for the thermostat tank T1. Check that there is sufficient
water in the tank. Refill as necessary.
9. Open cooling water valve V13 and let the cooling water flow through the condensor
W1.
10. The unit is now ready to be used for an experiment.
1. Keep the cooling water valve V13 open to allow the cooling water to continue
flowing.
2. Switch off both pumps P1 and P2. Switch off the stirrer.
3. Switch off the pump and heating for the thermostat tank T1. Let the liquid in the
reaction vessel R1 cool down to room temperature.
4. Close cooling water valve V13.
5. Close valves V2 and V7. Open valves V4, V9 and V12 to drain any liquid from the
unit.
13
Experiment A:
Effect of RTD on the Reaction in a CSTR
3.1 OBJECTIVES:
• To carry out a saponification reaction between NaOH and Et(Ac) in a CSTR.
• To determine the effect of residence time on the extent of conversion.
3.2 PROCEDURES:
1. Perform the general start-up procedures.
2. Open valves V2, V5, V7, and V10.
3. Switch ON both pumps P1 and P2 simultaneously.
4. Let the reactor fill up with both solutions until it is just about to ¾ full.
5. Readjust the valves V5 and V10 to give a flow rate of about 100 mL/min. Make
sure that both flow rates are the same. Record the flow rate.
6. Switch ON the stirrer, M1 and set the speed to about 200 rpm.
8. Record the conductivity value at Q1-401 for every 5 minutes until it does not
change over time. This is to ensure that the reactor has reached steady state.
9. Find the concentration of NaOH in the reactor and extent of conversion from the
calibration curve.
time.
11. Repeat the experiment (steps 6 to 10) for different residence times by adjusting the
feed flow rates of NaOH and Et(Ac) to about 200 mL/min. Make sure that both
flow rates are maintained the same.
14
4.0 ANALYSIS AND DISCUSSION:
1. Use the table for data collection at Appendix B.
2. Plot a graph of conversion vs. time for the different residence time. The reactor’s
residence time is defined as the reactor volume divided by the total feed flow rates.
V
Residence time, τ = PFR
F0
Compare the conversion at the different residence time. Discuss the graph
thoroughly and explain how it can influence the rate of reaction
3. Discuss the advantages and disadvantages of using CSTR reactors in chemical

reaction.
4. Describe an example of industrial applications that utilized CSTR reactors in its

process.
5.0 TUTORIAL
1. For different reactor residence times, calculate the value of the reaction rate
constant, k and the rate of reaction, -rA.
15
EXPERIMENT B:
The Effect of Temperature on the Reaction in a CSTR
6.1 OBJECTIVES:
• To determine the effect of temperature on the extent of conversion.
6.2 PROCEDURES:
1. Perform the general start-up procedures.
2. Open valves V2, V5, V7, and V10.
3. Switch on both pumps P1 and P2 simultaneously.
4. Let the reactor fill up with both solutions until it is just about to ¾ full.
5. Readjust the valves V5 and V10 to give a flow rate of 200 mL/min. Make sure that
both flow rates are the same. Record the flow rate.
6. Switch ON the stirrer, M1 and set the speed at about 200 rpm.
7. Set the thermostat tank T1 temperature to 40°C. Wait until the desired temperature
is reached, then turn on the thermostat pump.
9. Record the conductivity value at Q1-401 for every 5 minutes until it does not
change over time. This is to ensure that the reactor has reached steady state.
10. Find the concentration of NaOH in the reactor and extent of conversion from the
calibration curve.
time.
12. Repeat the experiment (steps 6 to 11) for different reactor temperatures by setting
the thermostat temperature to 60°C. Make sure that the flow rates of both solutions
are maintained at 200 mL/min.
16
1. Use the sample table in Appendix B for data collection.
2. Plot a graph of conversion, X vs. reactor temperature, T.
3. Plot a graph of conversion vs. time for the different temperature. Compare the
conversion at the different temperature. Discuss the graph thoroughly and explain
how it can influence the rate of reaction
4. Discuss the advantages and disadvantages of using CSTR reactors in chemical

reaction.
5. Describe an example of industrial applications that utilized CSTR reactors in its

process.
8.0 TUTORIAL
1. For different reactor temperatures, calculate the value of the reaction rate constant,
k.
2. Plot the graph of ln k vs 1/T and evaluate the slope and y-axis intercept
3. Calculate the saponification reaction’s activation energy , E and Arrhenius constant,

A from the slope and intercept values using the Arrhenius equation.
9.0 REFERENCES
1. Levenspiel O., “Chemical Reaction Engineering”, John Wiley (USA), 1972.
2. Fogler H.S., “Elements of Chemical Reaction Engineering, 3rd Ed.”, Prentice Hall (USA),
1999.
3. Smith J.M., “Chemical Engineering Kinetics”, McGraw Hill (Singapore), 1981.
17
APPENDIX A
RESULTS FOR PREPARATION OF CALIBRATION CURVE
Solution Mixtures
Conversion 0.1 M 0.1 M
H2O of NaOH (M) (mS/cm)
NaOH Na(Ac)
0% 100 mL – 100 mL 0.0500 10.7
25% 75 mL 25 mL 100 mL 0.0375 9.7
50% 50 mL 50 mL 100 mL 0.0250 7.5
75% 25 mL 75 mL 100 mL 0.0125 5.6
100% – 100 mL 100 mL 0.0000 4.0
axis intercept.
18
APPENDIX B
RESULTS FOR EXPERIMENTS
Reactor volume = _____ L Flowrate = _____ mL/min

Concentration of NaOH in feed vessel = _____ M Temperature = _____ oC
Concentration of Et(Ac) in feed vessel = _____ M
Total flow
Flow rate of Flow rate of Concentration of
Temperature rate of Residence Conductivity Conversion,
Time NaOH Et(Ac) NaOH,
(°C) solutions, time, τ (min) (mS/cm) X (%)
(mL/min) (mL/min) CNaOH (M)
F0 (mL/min)
0
5
10
15
20
25
30
35
40
45
50
55
60
65
19
EXPERIMENT 3
PLUG FLOW REACTOR (PFR)
OBJECTIVES
To determine the effect of residence time on the conversion in a PFR.
To determine the effect of temperature on the conversion in a PFR.
Keywords: PFR, pulse input, step input, residence time

Before operating the unit and running experiments, students must familiarize
themselves with the unit’s components. Please refer to Figure 1 to understand the
process. All glass components of the QVF Plug Flow Reactor unit are made of
borosilicate 3.3 glass with PTFE gaskets.
1. Plug flow reactor (R1)

• Jacketed pipe with approximate capacity of 1.5 L
• Pipe length 15 m

• 60 L PE rectangular vessels with all necessary connections
2. Dosing vessels (HB1/HB2)

• 1 L cylindrical vessels with overflow port and bottom port
3. Pumps (P1/P2)
• Max delivery rate of 60 L/h and max delivery height of 8 m
4. Pre-heater (W1/W2)
• Max heating media pressure of 0.5 bar

6. Instrumentations
• Flow measurements (FI-301, FI-302, FI-303)
• Temperature measurements (TI-101, TI-102)
• Conductivity measurements (QI-401, QI-402)
20
1. The unit must be operated under the supervision of an authorized staff that has been
properly trained to handle the unit.
used.
load, or permanent external action of aggressive vapors.
5. Always check and rectify any leak.

pressure.
11. Only a properly trained staff shall be allowed to carry out any servicing.
12. Before any servicing, shut down the whole operation and let the system to cool
down and be properly ventilated.
necessary.
21
Vent
QI TI
402 102
V10
HB1 HB2
SR1
V1 V2 T1
W1 W2 TI QI
101 401
Injection
B1 B2 FI
301
FI
302
FI
303
B3
V11
V3 V4 V7 V8 V9
P1 P2
M M
V5 V6
HS HS Process Water
1 2
V12
22
2.1 General Start-Up Procedures for Experiments A & B
2. Prepare a 50 L solution of sodium chloride, NaCl (0.05 M).
3. Fill the feed vessel B1 with the NaCl solution.
4. Turn on the power for the contol panel.
5. Open the process water valve V12.
6. Open valve V1.
7. Switch on pump P1 and observe the flow of NaCl solution into the dosing vessel
HB1 and towards valve V8.
8. Make sure that the pipeline before valve V8 is filled with the salt solution. Bleed
any trapped air in the pipeline by using valve V8.
9. Allow the solution overflow in the dosing vessel HB1 into the feed vessel B1.
10. Open valve V9 and let the process water flow through the plug flow reactor SR1
until it empties into the receiving vessel B3. Close valve V9.
1. Switch off both pumps P1 and P2.
2. Switch off the thermostat T1.
3. Close the process water valve V12.
4. Open valves V3, V4, V5, V6, V7, V8 and V11 to drain all liquid from the unit.
23
EXPERIMENT A:
Effect of Residence Time on the Reaction in a PFR
3.1 OBJECTIVE
• To carry out a saponification reaction between NaOH and Et(Ac) in a PFR.
• To determine the reaction rate constant.
• To determine the effect of residence time on the conversion in a PFR.
3.2 PROCEDURES:
2. Open valves V7 and V8.
3. Allow both the NaOH and Et(Ac) solutions to enter the plug flow reactor SR1 and
empty into the receiving vessel B3.
4. Adjust valves V7 and V8 to give a flow rate of about 500 mL/min. Make sure that
5. Start monitoring the inlet (QI-401) and outlet (QI-402) conductivity values until
they do not change over time. This is to ensure that the reactor has reached steady
state.
6. Record both inlet and outlet steady state conductivity values. Find the concentration
of NaOH exiting the reactor and extent of conversion from the calibration curve.
7. Repeat the experiment (steps 4 to 7) for different residence times by reducing the
feed flow rates of NaOH and Et(Ac) to about 400, 300, 200, 100 and 50 mL/min.
Make sure that both flow rates are the same.
24

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.
V
Residence time, τ = PFR
F0
thoroughly and explain how it can influence the rate of reaction
7. Discuss the advantages and disadvantages of using PFR reactors in chemical

reaction.
8. Describe an example of industrial applications that utilized PFR reactors in its

process.
5.0 TUTORIAL
For a second order equimolar reaction with the same initial reactants’ concentration
(CA0 = CB0), the rate law is shown to be:
− rA = kC A C B = kC 2A = kC 2A0 (1 − X )2
dX dX
− rA = FA0 = F0 C A0
dV dV
F X dX F  X 
VPFR = 0 ∫ = 0  
kC A0 (1 − X )
0 2
kC A0  1 − X 
Where: X = extent of conversion
CA = exit concentration of reactant NaOH (M)
F0 = total inlet flow rate of solutions (mL/min)
CA0 = inlet concentration of reactant NaOH in the reactor (M)
For constant PFR volume, flow rate and initial concentrations, the reaction rate constant
is,
F0  X 
k=  
VPFR C A0  1 − X 
Subsequently, for different reactor residence times, calculate the value of the
reaction rate constant, k and the rate of reaction, -rA.
25
EXPERIMENT B
Effect of Temperature on the Reaction in a PFR
6.1 OBJECTIVE:
• To determine the effect of temperature on the conversion in a PFR.
6.2 PROCEDURES:
3. Allow both the NaOH and Et(Ac) solutions to enter the plug flow reactor SR1 and
empty into the receiving vessel B3.
5. Switch on the thermostat T1 and set the water temperature to 50°C.
6. Start monitoring the conductivity values at QI-401 & QI-402 and temperature
values at TI-101 & TI-102 until they do not change over time. This is to ensure that
the reactor has reached steady state.
7. Record both inlet and outlet steady state conductivity and temperature values. Find
the concentration of NaOH exiting the reactor and extent of conversion from the
calibration curve.
8. Repeat the experiment (steps 5 to 7) for different reactor temperatures by increasing

the thermostat temperature to 60, 70 and 80°C. Make sure that the flow rates of
both solutions are maintained at 200 mL/min.
7.0 ANALYSIS AND DISCUSSION
1. Use the sample table in Appendix B for data collection.
9. Plot a graph of conversion, X vs. reactor temperature, T.
3. Plot a graph of conversion vs. time for the different temperature. Compare the
conversion at the different temperature. Discuss the graph thoroughly and explain
how it can influence the rate of reaction
4. Discuss the advantages and disadvantages of using PFR reactors in chemical

reaction.
5. Describe an example of industrial applications that utilized PFR reactors in its

process.
26
8.0 TUTORIAL
1. For different reactor temperatures, calculate the value of the reaction rate constant,
k.
2. Plot the graph of ln k vs 1/T and evaluate the slope and y-axis intercept
3. Calculate the saponification reaction’s activation energy , E and Arrhenius constant,

A from the slope and intercept values using the Arrhenius equation.
9.0 REFERENCES
1999.
APPENDIX A
Solution Mixtures
NaOH Na(Ac)
0% 100 mL – 100 mL 0.0500 10.7
25% 75 mL 25 mL 100 mL 0.0375 9.7
50% 50 mL 50 mL 100 mL 0.0250 7.5
75% 25 mL 75 mL 100 mL 0.0125 5.6
100% – 100 mL 100 mL 0.0000 4.0
axis intercept.
27
APPENDIX C
SAMPLE TABLE FOR EXPERIMENTS A AND B
Reactor volume = _____ L

Concentration of NaOH in feed vessel = _____ M
Temperature (°C) Total flow Exit

Flow rate Flow rate Residence Inlet Outlet
rate of concentration Conversion,
No. of NaOH of Et(Ac) time, τ conductivity conductivity
solutions, of NaOH, X (%)
Inlet Outlet (mL/min) (mL/min) (min) (mS/cm) (mS/cm)
F0 (mL/min) CNaOH (M)
1
2
3
4
5
6
7
8
9
10
28
EXPERIMENT 4
REACTOR TEST RIG

OBJECTIVES
To compare the performance of single reactor, 3 CSTRs AND PFR.
Keywords: CSTR, PFR, Reactors in series; Conversion; Residence time distribution (RTD) studies
components of the QVF Reactor Test Rig unit are made of borosilicate 3.3 glass with
PTFE gaskets.
1. Reactor (R1)
• Jacketed cylindrical vessel, 4 L nominal capacity
2. Cascaded reactors (R2/R3/R4)

• Jacketed cylindrical vessel, 1 L nominal capacity each
3. Plug flow reactor (SR1)

• Jacketed pipe with approximate capacity of 3.0 L

• 100 L PE rectangular vessels with all necessary connections
5. Dosing vessels (HB1/HB2)

• 1 L cylindrical vessels with overflow port and bottom port
6. Pumps (P1/P2)
• max delivery rate of 60 L/h and max delivery height of 8 m
7. Pre-heater (W1/W2)
• max heating media pressure of 0.5 bar

9. Instrumentations
• Flow measurements (FI-301, FI-302, FI-303)
• Temperature measurements (TI-101, TI-102, TI-103, TI-104)
• Conductivity measurements (QI-401, QI-402, QI-403, QI-404)
29
1. The unit must be operated under the supervision of an authorized staff that has been
properly trained to handle the unit.
used.
load, or permanent external action of aggressive vapours.
5. Always check and rectify any leak.

pressure.
11. Only a properly trained staff shall be allowed to carry out any servicing.
12. Before any servicing, shut down the whole operation and let the system to cool
down and be properly ventilated.
necessary.
30
Vent
V22 V23 V24 M2 V25

HS
4
QI
404
M M3
HS
TI
5
104
M M4
HB1 HB2 HS T1
6
TI
103
M
QI
403
R2
M1 V16
HS
3 R3
TI
V1 V2
102 V17
M
QI
402 R4
SR1
W1 W2 V18
V11 V12 V13
QI TI
401 101 R1
V14
Injection
V15
FI FI FI
B1 B2 301 302 303
V19 V20 V21

V8 V9 V10
P1 P2 V27
V3 V4
M M V5 V6 Process Water
HS HS
V7
1 2 B3 V26
36
2.1 General Start-Up Procedures for Experiment

b) 100 L of ethyl acetate, Et(Ac) (0.1 M)
3. Fill the feed vessel B1 with the NaOH solution and feed vessel B2 with the Et(Ac)
solution.
5. Check that there is sufficient water in the thermostat T1 tank. Refill as necessary.
6. Open the process water valve V27.
8. Switch on both pumps P1 and P2. Observe the flow of NaOH and Et(Ac) solutions
into the dosing vessels HB1 and HB2, towards valves V10 and V9 respectively.
9. Make sure that the pipelines before valves V9 and V10 are filled with liquid. Bleed
any trapped air in the pipelines by using valves V9 and V10.
10. Allow both solutions to overflow in the dosing vessels HB1 and HB2 into the feed
vessels B1 and B2 respectively.
2.2 Selection of Reactors
Any one of the three reactors provided in the reactor test rig can be used for each of the
experiments. The following procedures will explain the steps needed to select a
particular reactor to run an experiment.
1. Ensure that all valves from V3 to V21 are closed.
2. For the plug flow reactor SR1:

a) Open valves V11 and V19.
b) Read the outlet conductivity value from QI-404 and temperature value from TI-
104.
3. For the single stage continuous stirred tank reactor R1:

a) Open valves V13, V14 and V20
b) Switch on the stirrer M1 and set the speed to 200 rpm.
c) For sampling, use valve V15.

37
d) Read the outlet conductivity value from QI-402 and temperature value from TI-
102.
4. For the 3-stage continuous stirred tank reactors R2, R3 and R4:
a) Open valves V12 and V21.
b) Switch on the stirrers M2, M3 & M4 and set the speed to 200 rpm each.
c) For sampling, use valves V16, V17 and V18 for the 1st, 2nd and 3rd CSTR
stage respectively.
d) Read the outlet conductivity value from QI-403 and temperature value from TI-
103.
1. Switch off both pumps P1.
2 Close the process water valve V27.
3. Open valves V3 to V21 and valve V26 to drain all liquid from the unit.
EXPERIMENT
Reactor Comparison Test
3.1 OBJECTIVE:
• To carry out a saponification reaction between NaOH and Et(Ac) using different
types of reactors.
• To compare the reaction conversion between different types of reactors.
• To determine the reaction rate constant.
3.2 PROCEDURES:
2. Select the desired reactor
4. Allow both the NaOH and Et(Ac) solutions to enter the selected reactor and empty
into the receiving vessel B3.
38
6. Start monitoring the inlet (QI-401) and outlet conductivity values of the reactor
until they do not change over time. This is to ensure that the reactor has reached
steady state.
7. Record both inlet and outlet steady state conductivity values. Find the concentration
of NaOH exiting the reactor and extent of conversion from the calibration curve.
8. Repeat the experiment (steps 5 to 7) for different residence times by adjusting the
feed flow rates of NaOH and Et(Ac) to about 200 and 300 mL/min. Make sure that
both flow rates are the same.
8. Close valves V9 and V10.
9. Repeat the experiment (steps 2 to 8) by selecting a different reactor.

2. Plot a graph of conversion vs. different residence time for the reactors. The
reactor’s residence time is defined as the reactor volume divided by the total feed
flow rates.
V
Residence time, τ = reactor
F0
thoroughly and explain how it can influence the rate of reaction.
3. Compare the 3 reactors and based on the experimental results, discuss which
configurations are the best for this reaction and state the reasons accordingly.
5.0 TUTORIAL
Single stage CSTR
1. For a second order equimolar reaction with the same initial reactants’ concentration
− rA = kC A C B = kC 2A
F X
VCSTR = A0
− rA
F X F (C − C )
VCSTR = A0 2 = 0 A0 2 A
kC A kC A
where: X = extent of conversion
39
Reaction rate constant, k =

(C A0 − C A )
τC 2A
Rate of reaction, − rA = kC 2A
3-stage CSTR’s in series

1. In the 3-stage CSTR in series, all of equal volume and same operating temperature,
the Damnköhler (Da) number for a second order reaction in a CSTR is defined
as Da = τkC A,in .
2. Calculate the following,
a) For the first reactor,

Da 1 = τkC A0
(1 + 2Da1 ) − 1 + 4Da1
X1 =
2Da1
C A1 = C A0 (1 − X 1 )
b) For the second reactor,

Da 2 = τkC A1
(1 + 2Da 2 ) − 1 + 4Da 2
X2 =
2Da 2
C A2 = C A1 (1 − X 2 )
c) For the third reactor,

Da 3 = τkC A2
(1 + 2Da 3 ) − 1 + 4Da 3
X3 =
2Da 3
C A3 = C A2 (1 − X 3 )
where: CA,i = concentration of NaOH in reactor I (M)
Xi = extent of conversion in reactor i
τ = reactor residence time (volume / total feed flow rates) (min)
k = reaction rate constant
Compare the above calculated results with the experimental values.
Plug flow reactor (PFR)

1. For a second order equimolar reaction with the same initial reactants’ concentration
− rA = kC A C B = kC 2A = kC 2A0 (1 − X )2
dX dX
− rA = FA0 = F0 C A0
dV dV
F0 X dX F  X 
VPFR = ∫
kC A0 0 (1 − X )2
= 0 
kC A0  1 − X 

where: X = extent of conversion

40
2. For constant PFR volume, flow rate and initial concentrations, the reaction rate
constant is,
F0  X 
k=  
VPFR C A0  1 − X 
6.0 REFERENCES
1999.
41
APPENDIX B
Solution Mixtures
NaOH Na(Ac)
0% 100 mL – 100 mL 0.0500 10.7
25% 75 mL 25 mL 100 mL 0.0375 9.7
50% 50 mL 50 mL 100 mL 0.0250 7.5
75% 25 mL 75 mL 100 mL 0.0125 5.6
100% – 100 mL 100 mL 0.0000 4.0
axis intercept.
42
APPENDIX C
TABLE FOR EXPERIMENT B
Reactor type = _____

Reactor volume = _____ L
Concentration of NaOH in feed vessel = _____ M
Temperature (°C) Total flow Exit

Flow rate Flow rate Residence Inlet Outlet
rate of concentration Conversion,
No. of NaOH of Et(Ac) time, τ conductivity conductivity
solutions, of NaOH, X (%)
Inlet Outlet (mL/min) (mL/min) (min) (mS/cm) (mS/cm)
F0 (mL/min) CNaOH (M)
1
2
3
4
5
6
7
8
9
10
43
37

LABORATORY MANUAL DECLARATION FORM Editted

Uploaded by

Document Information

Original Description:

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

LABORATORY MANUAL DECLARATION FORM Editted

Uploaded by

Copyright:

Available Formats

LABORATORY MANUAL JULY 2010 REACTION ENGINEERING (CKB 20104)

LABORATORY REPORT GUIDELINES

4. RESULTS AND DISCUSSIONS

Figure 1: Relationship between X and Y

The Dean/Head of Campus

3. I am fully responsible for all my actions during laboratory sessions.

EXPERIMENT 1: BATCH REACTOR

EXPERIMENT 2: CONTINUOUS STIRRED TANK

EXPERIMENT 3: PLUG FLOW REACTOR (PFR)

EXPERIMENT 4: REACTOR TEST RIG (RTR)

Keywords: Batch reactor; Kinetics; Saponification reaction; Activation energy

1.0 GENERAL DESCRIPTION

1.1 Description and Assembly

3. Dosing vessel (B1)

a) Integrated rate law method

Assuming the reaction to be a simple, irreversible, second order process, then

Separating the variables and integrating with appropriate boundary conditions,

1.2 Safety Considerations

4. For each experimental setting, allow 10 minutes for equilibrium conditions to be

7. Wipe off any spillage on the ground or working bench.

9. All experiments involving a potential explosive hazard must be conducted behind

12. Smoking is forbidden in all laboratories.

13. Safety helmets must be worn.

14. Services equipment (vacuum generators) must in no circumstances be started up by

17. If in doubt, ask the lecturer in charge.

18. If chemical spillage occurs, evacuate the laboratory in an orderly fashion.

2.0 EXPERIMENTAL PROCEDURES

3. Placed 200 mL of 0.1M sodium hydroxide (NaOH) into 500 ml beaker.

5. Place the mechanical stirrer in the sodium hydroxide (NaOH) solution.

8. Record the temperature of the reacting mixture in the beaker.

12. Record the results in Appendix A

3.0 ANALYSIS AND DISCUSSIONS

3.1 Method of Calculations to determine concentration of NaOH

Let titre of NaOH as = Y mL

Therefore the number of moles of 0.1M NaOH used in the titration

We know the initial quantity of 0.1M acid

Therefore the amount of acid neutralized by sample

Thus, NaOH concentration in 20 mL sample from the reactor

1. Plot a graph conversion vs time and discuss it thoroughly.

3. Explain why it is vital to conduct certain chemical reactions in bench scale up

a. Integrated rate law method

5.0 EXPERIMENTAL PROCEDURES

5.1 General Start-Up Procedures

2. Ensure that all valves are initially closed.

3. Turn on the power for the control panel.

5. The unit is now ready for experiment.

5.2 General Shut-Down Procedures

3. Switch off the stirrer.

4. Close cooling water valve.

5. Open bottom valve to drain any liquid from the unit.

6. Turn off the power for the control panel.

5.3 Experimental Procedures

5. Start the timer simultaneously.

7. Record your conductivity value in the Appendix C.

9. Repeat the procedure 1-8 with the temperature at 60°C.

10. Perform the general shut-down procedures.

7.0 ANALYSIS AND DISCUSSIONS

1. Use the sample table in Appendix C for data collection.

3. Discuss the advantages and disadvantages of using batch reactors in chemical

4. Describe an example of industrial applications other than saponification that

1. For a second order reaction, the rate law is shown to be:

iv) Calculate the saponification reaction’s activation energy, E and Arrhenius

Reactor volume = _ L Flowrate = _ mL/min