You are on page 1of 53

LABORATORY MANUAL (JAN 2015)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 FORMas 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

3.

1.0

Results and Discussion

2.0

Conclusions and Recommendations

3.0

Tutorial

4.0

References

5.0

Appendices

SUMMARY
Give the summary (not more than 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 Discussion 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

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

Example Table:
Table 1: X vs. Y
Samples
A
B
C
D

X (unit)

Y (unit)

Example Graph:

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 AND RECOMMENDATIONS


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.

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).

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

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 Statistical Review of World Energy, 2007,BP (British Petroleum),[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 and sample of calculations should be included here.
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.

IMPORTANT NOTE:
1.

Laboratory reports are meant to be group tasks.

2.

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
Internet without proper references will not be tolerated and the report will be marked as zero.

3.

Laboratory report should be submitted the following week (7 days) after the experimental is conducted.

4.

Any late submissions without agreement of the lecturer will result in 50% deductions of the overall
marks.

5.

Laboratory report should be submitted directly to the lecturer in charge for date verification.

APPENDIX
3

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

CHEMICAL PREPARATION
1. Ethyl acetate (CH3COOCH2CH3) (Liquid Phase)
Volume of ethyl acetate needed, V1 (L) from the original solution

mol
V2 (L)
L
V1 (L)
mol
10.10

L
M2

Where;
M2 = Desired molarity of Ethyl Acetate (mol/L) required in the experiment
V2 = Desired volume of Ethyl Acetate (mol/L) required in the experiment
2. Sodium Hydroxide (NaOH) (Solid Phase)
Weight of NaOH required for experiment, mNaoH

mol
g
MWNaOH
V2 (L)
L
mol

mNaOH (g) M 2
Where;

M2 = Desired molarity of NaOH (mol/L) required in the experiment


V2 = Desired volume of NaOH (mol/L) required in the experiment
Molecular weight of NaOH, MWNaOH = 40.0 g/mol

3. Hydrochloric acid (HCl) (Liquid Phase)


Volume of hydrochloric acid needed, V1 (L)from the original solution

V1 (L)

mol
V2 (L)
L
mol
1.0

M2

Where;
M2 = Desired molarity of HCl (mol/L) required in the experiment
V2 = Desired volume of HCl (mol/L) required in the experiment

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

LABORATORY MANUAL
REACTION ENGINEERING
CKB 20104
JANUARY 2015
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

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

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 a batch reactor.
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
units 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
6

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

4. Condenser (W1)
Coil heat exchanger, area 0.3 m2

Max coolant pressure of 3 bars with allowable temperature difference of 130C

5. Instrumentation
Temperature measurement (TI-101)
Conductivity measurement (QI-401)

Figure 1: Batch Reactor Unit


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 COOC2 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:

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

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

Rate

d ester

k ester OH
dt

Suppose that the concentrations of the ester and hydroxide are equal at the start of the experiment and
equal to CA0mol/dm3, and that at some time t later, both the ester and hydroxide concentration have
fallen to CA. Therefore we obtain

dCA
k ester OH kCA2
dt

Separating the variables and integrating with appropriate boundary conditions,


CA

t
dCA
1
1
C 2 k dt C C kt
C A0
0
A
A0
A

A plot of 1/CA against t should give a straight line with the gradient, k.

b)

Half-life method

1 C CA
1
1
k A0

kt

t
C
C
C
C

A A0
A0
From A
can be rearranged to give
Let t1/2 be the time taken for the concentration of ester to be halved,

C A C A0 / 2

, then

1
t1/2CA0

The time taken to halve the concentration of ester is inversely proportional to the initial concentration.
From plot of the ester concentration C Aagainst t, it is possible to determine t1 / 2 and hence the rate
constant.

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

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 tubings 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.
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 Lof sodium hydroxide, NaOH (0.1 M)

b)

250 mL of ethyl acetate, Et(Ac) (0.1 M)


9

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

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 200mL of 0.1M sodium hydroxide (NaOH) into 500 ml beaker.
4. Label 11 clean conical flasksfrom 1 to 11 and pipette 20 mLof 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. After5 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. 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. Stop the titration once the change of indicator color is observed. Determine the amount of NaOH
needed.
10. 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 70 (Flask 11) minutes. Repeat step 7 to 9.
11. Record the results in Appendix A.

3.0

ANALYSIS AND DISCUSSIONS


Method of Calculations to determine concentration of NaOH
Let titre of NaOH as

Y mL

The number of moles of 0.1M NaOH used in the titration = Acid neutralized in titration

0.1(Y )
mol
1000
=

0.1(20)
mol
1000
We know the initial quantity of 0.1M acid=
The amount of acid neutralized by sample= Moles of NaOH present in the sample

10

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

0.1(20 Y )
mol
1000
=
Thus, NaOH concentration in 20 mL sample from the reactor=Ester concentration =

20 Y
0.1

mol / mL
1000
20
=
1. Plot a graph conversion, Xvs.reaction time and discuss it thoroughly.
2. Determine the rate constant, k using both methods and compare both values as explained
previously:
a. Integrated rate law method

1
1

kt
CA CA0
A plot of 1/CA against t should give a straight line with the gradient, k.
b. Half-life method
* In the half-life method, the initial concentrations (C A0 = 0.05 M) can be obtained
straight forward. From the graph (CA versus t) we can determined how long it takes for
that concentration to be halved (t1/2 = Reaction time when concentration = 0.025 M).

4.0

1
t1/2CA0

TUTORIAL
Discuss why vital to conduct certain chemical reactions in bench scale up and subsequently discuss
its disadvantages.

5.0

EXPERIMENTAL PROCEDURES

Experiment B: Effect of Temperature on the Batch Saponification Reaction


1.

Prepare the following solutions:


a) 6 L of sodium hydroxide, NaOH (0.1 M)
b) 6 L of ethyl acetate, Et (Ac) (0.1 M)
11

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

2.

Ensure that all valves are initially closed.

3.

Turn on the power for the control panel.

4.

Check that there is sufficient water in the thermostat T1 tank. Refill as necessary.

5.

Open cooling water valve V5 and let the cooling water flow through the condenser W1.

6.

Switch on the thermostat T1 and set the water temperature to the desired temperature.

7.

The unit is now ready for experiment.

8.

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.

9.

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.

10.

Switch on the stirrer M1.

11.

Start the timer simultaneously.

12.

At every 5-minute interval, open sampling valve V1 (at the bottom) and collect a 10 mL
sample. Carry out a conductivity measuring by using conductivity meter.

13.

Record your conductivity value and temperature value from TI-101 in the Appendix C.

14.

End the experiment when the conductivity values do not change significantly over time.
Switch off the stirrer M1. Drain the reactor R1 by opening valve V1.

15.

Refilled the reactor with fresh solutions of 3 L of 0.1 M ethyl acetate and 3 L of 0.1 M
sodium hydroxide.

16.

Repeat the experiment (steps 1-8) for different reactor temperature by setting the
thermostat temperature tothe desired temperature.

17.

Perform the general shutdown procedures.

6.0 General Shutdown Procedures


1. Keep the cooling water valve V5 open to allow the cooling water to continue flowing.
2. Switch off the thermostat T1. Let the liquid in the reaction vessel R1 cool down to room
temperature.
3. Switch off the stirrer M1.
4. Close cooling water valve V5.Open bottom valve V1 to drain any liquid from the unit.
5. Turn off the power for the control panel.
2. ANALYSIS AND DISCUSSIONS
1. Use the sample table in Appendix C for data collection.
2. Find the concentration of NaOH in the reactor from the calibration curve.Subsequently calculate
the conversion, X based on the formula given in Appendix.

12

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

3. Plot a graph Conversion, X vs time, t forthe 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.
4. For a second order reaction, the rate law is shown to be:

rA

dCA
kCA2 AND
dt

Therefore

CA

dCA

CA0

CA2

k dt
t

1
1
kt
CA
CA0

where CA0 is the initial concentration of reactant NaOH in the reactor(0.05 M).
5. For each temperature value, plot the graph of 1/C A vs time, t and evaluate the slope and y-axis
intercept.
6. Determine the rate constant, k from the slope value for different temperature values. Examine
the change in the rate constant.
7. Plot a graph of ln k vs 1/T and evaluate the slope and y-axis intercept.

Ea

RT

From Arrhenius equation, k(T ) Aexp


In linear form ln k

Ea 1
ln A
R T

(R = 8.314 J/mol.K)

8. Calculate the saponification reactions activation energy, Ea and frequency factor, A from the
slope and intercept values using the Arrhenius equation.

8.0

TUTORIAL
1. Describe an example of industrial applications other than saponification that utilized batch
reactors in its process.
2. Discuss the advantages and disadvantages of using batch reactors in chemical reaction.

9.0
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.
13

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

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.

APPENDIX A
Table forExperiment A: The Batch Saponification of Ethyl Acetate
Time
(min)

Flask
Number

5
10
15
20
25
30
35
40
50
60
70

Concentration of
NaOH,
CNaOH (M)

Amount of
NaOH titred
(mL)

(From equation above)

Conversion,
X (%)
(Self calculate)

1
2
3
4
5
6
7
8
9
10
11

NOTE:
1. Formula to calculate conversion, X

CNaOH (0) CNaOH (t)


CNaOH (0)

x100% where CNaOH (0) 0.05M

APPENDIX B
Experiment B: Effect of Temperature on the Batch Saponification Reaction
TABLE OF CALIBRATION CURVE

14

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

Solution Mixtures
Conversion

Concentration
of NaOH (M)

Conductivity
(mS/cm)

0.1 M NaOH

0.1 M
Na(Ac)

H2O

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

NOTE
1. Plot the calibration curve of concentration of NaOH (M) (x-axis) vs conductivity (y-axis).
2. Determine the slope of the curve.
3. Use the calibration curve to determine the concentration of the experimental product (M) from the
pre-determined conductivity found during the experiment.

APPENDIX C
Table for Experiment B: Effect of Temperature on the Batch Saponification Reaction
Volume of NaOH

3L

Volume of Et(Ac)

3L
15

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

Initial concentration of NaOH =

0.05 M

Initial concentration of Et(Ac) =

0.05 M

Temperature

_____C

Time
(min)

Temperature
(C)

Conductivity
(mS/cm)

Concentration of NaOH,
CNaOH (M)
(From calibration curve)

Conversion,
X (%)
(Self calculation)

0
5
10
15
20
25
30
35
40
45
50
55
60
NOTE:
1. Obtain the concentration of NaOH for each of the reaction time from the measured conductivity
value based on the calibration curve (Appendix B).
2. Formula to calculate conversion, X

0.05 CNaOH (t)


0.05

100% where CNaOH (0) 0.05M

Continue:
Table for Experiment B: Effect of Temperature on the Batch Saponification Reaction
Volume of NaOH

3L

Volume of Et(Ac)

3L
16

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

Initial concentration of NaOH =

0.05 M

Initial concentration of Et(Ac) =

0.05 M

Temperature

_____ C

Time
(min)

Temperature
(C)

Conductivity
(mS/cm)

Concentration of NaOH,
CNaOH (M)
(From calibration curve)

Conversion,
X (%)
(Self calculation)

0
5
10
15
20
25
30
35
40
45
50
55
60
NOTE:
1. Obtain the concentration of NaOH for each of the reaction time from the measured conductivity
value based on the calibration curve (Appendix B).
2. Formula to calculate conversion, X

0.05 CNaOH (t)


0.05

100% where CNaOH (0) 0.05M

END EXPERIMENT 1

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.
17

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

To study the effect of temperature on the reaction in CSTR.


Keywords: CSTR; residence time; Mixing; Saponification kinetics; Activation energy
1.0

GENERAL DESCRIPTION
1.1

Description & Assembly


Before operating the unit and running experiments, you must familiarize yourself with the
units components. Please refer to Figure 1 to understand the process. All glass 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 150C


6. Receiving vessel (B3)
18

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

100 L rectangular tank


7. Instrumentation
Flow measurement (FI-301, FI-302)
Temperature measurement (TI-101)
Conductivity measurement (QI-401)
1.2

Safety Considerations
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.

19

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)


Vent

V1

V6

B1

Cooling
Water

B2

W1

Cooling
Water

V13
HS
1
Q1
401

TI
101

V2

V7
FI
301

FI
302

V5

V10

V3

R1

V8
V3

V11
V4

P1

V9

P2
M

HS
2

HS
3

V12

B3
Figure 2: Continuous Stirred Tank Reactor Unit

12

T1

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

2.0

OPERATING PROCEDURES
2.1

General Start-up Procedures


1. Prepare the following solutions:
a) 30 L of sodium hydroxide, NaOH (0.1 M)
b) 30 L of ethyl acetate, Et(Ac) (0.1 M)
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. Open valves V2, V7, and V11.
6. The unit is now ready to be used for an experiment.

2.2

General Shutdown Procedures


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 M1.
3. Switch off the thermostat T1. Let the liquid in the reaction vessel R1 cool down to
room temperature.
4. Close cooling water valve V13.
5. Open valves V4, V9 and V12 to drain any liquid from the unit.
6. Turn off the power for the control panel.

13

3.2

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

3.0

EXPERIMENTAL PROCEDURES

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.

To determine the reaction rate constant.

PROCEDURES:
1.

Perform the general start-up procedures.


2. Switch ON both pumps P1 and P2 simultaneously.
3. Open and adjust the valves V5 (Monitor at FI-301) and V10 (Monitor at FI-302) to
give a flow rate of about 200 mL/min. Both must be adjusted to equal flow rate.
4. Let the reactor fill up with both solutions until it is just about to 1/2 full.
5. Switch ON the stirrer M1.
6. Adjust the valves V5 and V10 to give the desired flow rate. Make sure that both
flow rates are maintained the same.
7. Start monitoring the conductivity value at QI-401.
8. Start the timer and record the conductivity value (QI-401) and both flow rates(FI301 and FI-302) when it has reached steady state (Conductivity value begin to
steadily decline with time).
9. Record the conductivity values and both flows rate for every 5 minutes until the
conductivity does not change over time. This is to ensure that the reactor has
reached steady state.
10.End the experiment when the conductivity values do not change significantly over
time.
11. Repeat the experiment (steps 6 to 10) for different residence times by adjusting the
feed flow rates of NaOH and Et(Ac).
12.Make sure that both flow rates are maintained the same.
13.Perform the general shut-down procedures.

14

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

4.0
1.

ANALYSIS AND DISCUSSION:


Use the table for data collection at Appendix B.
2. Find the concentration of NaOH in the reactor from the calibration curve. Subsequently
calculate the conversion, X based on the formula given in Appendix.
3. Plot a graph of conversion, X vs. reaction time, tfor the different flow rate. Discuss the
graph.
4. The reactors residence time is defined as the reactor volume divided by the average total
feed flow rates.

Residence Time,

VCSTR
F0

Subsequently calculate the average residence time,avg(NOTE: 1 FLOW RATE


PARAMETER GIVES 1 AVERAGE RESIDENCE TIME).
5. Compare the highest conversion, Xfor the different average residence time,avg(NOTE: 1
FLOW RATE PARAMETER GIVES 1 AVERAGE RESIDENCE TIME).Compare the
highest conversion, X at the different average residence time, avg. Discuss thoroughly
and explain how residence time can influence the rate of reaction.
6. Forthe different average reactor residence times, avg (NOTE: 1 FLOW RATE GIVES 1
AVERAGE RESIDENCE TIME), calculate the value of the reaction rate constant, k and
the rate of reaction, rA.

Reaction rate constant, k

A0

CA

avgC

2
A

AND Rate of reaction, - rA kCA2

avg

= Average residence time from 1 flow rate (min)

CA

= Exit concentration of reactant NaOH (M) (Note: Concentration of


NaOH at the highest conversion, X)

CA0

5.0

= Inlet concentration of reactant NaOH (M)(0.05M)

TUTORIAL
1. Discuss the advantages and disadvantages of using CSTR reactors in chemical reaction.
2. Describe an example of industrial applications that utilized CSTR reactors in its process.
15

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

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.


To determine the value of the reactions activation energy.
6.2

PROCEDURES:
1. Perform the general start-up procedures.
2. Check that there is sufficient water in the thermostat T1 tank. Refill as necessary.
3. Open cooling water valve V13 and let the cooling water flow through the condenser W1.
4. Switch on the thermostat T1 and set the water temperature to the desired temperature.
5. Switch ON both pumps P1 and P2 simultaneously.
6. Open and adjust the valves V5(Monitor at FI-301)and V10 (Monitor at FI-302)to give a
flow rate of about 200 mL/min. Both must be adjusted to equal flow rate.
7. Let the reactor fill up with both solutions until it is just about to 1/2 full.
8. Switch ON the stirrer M1.
9. Start monitoring the conductivity value at QI-401.
10. Start the timer and record the conductivity value at QI-401, temperature value at TI-101
and both flow rates (FI-301 and FI-302) when it has reached steady state (Conductivity
value begin to steadily decline with time).
11. Record the conductivity, temperature, both flow rate values for every 5 minutes until the
conductivity does not change over time. This is to ensure that the reactor has reached
steady state.
12. End the experiment when the conductivity values do not change significantly over time.
13. Repeat the experiment (steps 6 to 11) for different reactor temperatures by setting the
thermostat temperature to the desired temperature. Make sure that the flow rates of both
solutions are maintained at the original flow rate.
14. Perform the general shut-down procedures.

16

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

7.0 ANALYSIS AND DISCUSSION:


1. Use the sample table in Appendix B for data collection.
2. Find the concentration of NaOH in the reactor from the calibration curve.Subsequently
calculate the conversion, X based on the formula given in Appendix.
3. Plot a graph of conversion, X vs. reaction time, tfor the2 different temperatures.
4. Compare the highest conversion, X at the different temperature. Discuss it thoroughly and
explain how temperature can influence the rate of reaction, rA.
5. For different reactor temperatures, calculate the value of the reaction rate constant, k.

Reaction rate constant,k

A0

CA

avgC

2
A

= Average residence time from 1 flow rate (min)

CA

= Exit concentration of reactant NaOH (M) (Note: Concentration of


NaOH at the highest conversion, X)

CA0

= Inlet concentration of reactant NaOH (M)(0.05M)

6. Plot a graph of ln k vs 1/T and evaluate the slope and y-axis intercept.

Ea

RT

From Arrhenius equation, k(T ) Aexp


In linear form ln k

Ea 1
ln A
R T

(R = 8.314 J/mol.K)

6. Calculate the saponification reactions activation energy, E a and frequency factor, A from
the slope and intercept values using the Arrhenius equation.
8.0

TUTORIAL
1.

Discuss the advantages and disadvantages of using CSTR reactors in chemical


reaction.

2.

Describe an example of industrial applications that utilized CSTR reactors in


its process.

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

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

4. Astarita G., Mass Transfer with Chemical Reaction, Elsevier, 1967.


APPENDIX A
RESULTS FOR PREPARATION OF CALIBRATION CURVE

Solution Mixtures
Conversion

Concentration
of NaOH (M)

Conductivity
(mS/cm)

0.1 M
NaOH

0.1 M
Na(Ac)

H2O

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

NOTE
1. Plot the calibration curve of concentration of NaOH (M) (x-axis) vs conductivity (y-axis).
2. Determine the slope of the curve.
3. Use the calibration curve to determine the concentration of the experimental product (M) from
the pre-determined conductivity found during the experiment.

18

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

APPENDIX B
RESULTS FOR EXPERIMENTS
Reactor volume
Concentration of NaOH in feed vessel
Concentration of Et(Ac) in feed vessel

Time

Flow rate of
Temperature
NaOH, FNAOH
(C)
(mL/min)

=
=
=

10 L
_____ M
_____ M

Flow rate of
Et(Ac), FEt
(mL/min)

Flowrate
=
Temperature =
Total flow rate
of solutions,
F0 (mL/min),
= FNAOH + FEt
(Selfcalculation)

Residence
time, (min)
(Self
calculation)

_____ mL/min
_____ oC

Conductivity
(mS/cm)

Concentration of
NaOH,
CNaOH (M)
(From calibration
curve)

Conversion,
X (%)
(Self
calculation)

0
5
10
15
20
25
30
35
40
45
50
55
60
avg =
NOTE:
1. Obtain the concentration of NaOH for each of the reaction time from the measured conductivity value based on the calibration curve (Appendix B).
2. Formula to calculate conversion, X

0.05 CNaOH (t)


0.05

100% where CNaOH (0) 0.05M


19

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

RESULTS FOR EXPERIMENTS


Reactor volume
Concentration of NaOH in feed vessel
Concentration of Et(Ac) in feed vessel
Flow rate of
Temperature
Time
NaOH, FNAOH
(C)
(mL/min)

=
=
=

10 L
_____ M
_____ M

Flow rate of
Et(Ac), FEt
(mL/min)

Flowrate
=
Temperature =
Total flow rate
of solutions,
F0 (mL/min),
= FNAOH + FEt
(Selfcalculation)

Residence
time, (min)
(Self
calculation)

_____ mL/min
_____ oC

Conductivity
(mS/cm)

Concentration of
NaOH,
CNaOH (M)
(From calibration
curve)

Conversion,
X (%)
(Self
calculation)

0
5
10
15
20
25
30
35
40
45
50
55
60
avg =
NOTE:
1. Obtain the concentration of NaOH for each of the reaction time from the measured conductivity value based on the calibration curve (Appendix B).
2. Formula to calculate conversion, X

20

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

0.05 CNaOH (t)


0.05

100% where CNaOH (0) 0.05M

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
1.0

GENERAL DESCRIPTION
1.1

Description and Assembly


Before operating the unit and running experiments, students must familiarize
themselves with the units 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 (SR1)

Jacketed pipe with approximate capacity of 1.5 L

Pipe length 15 m

2. Feed vessels (B1/B2)


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)

Centrifugal pumps

Max delivery rate of 60 L/h and max delivery height of 8 m

EXPERIMENT 3

4. Pre-heater (W1/W2)
Coil heat exchanger, area 0.06 m2
20

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

Max heating media pressure of 0.5 bar


5. Receiving vessel (B3)
100 L rectangular tank
6. Instrumentations

Flow measurements (FI-301, FI-302, FI-303)

Temperature measurements (TI-101, TI-102)

Conductivity measurements (QI-401, QI-402)

1.2

Safety Considerations
1. The unit must be operated under the supervision of an authorized staff that 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 vapors.
5. Always check and rectify any leak.
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 shall be allowed to carry out any servicing.
Manufacturer's manual must always be observed.
12. Before any servicing, shut down the whole operation and let the system to cool
down and be properly ventilated.
21

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

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.

22

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

V1

B1

P1
M
HS
1

Figure 3: Plug Flow Reactor Unit


22

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

2.0

OPERATING PROCEDURES
2.1

General Start-Up Procedures for Experiments A & B


1. Prepare the following solutions:
a) 50 L of sodium hydroxide, NaOH (0.1 M)
b) 50 L of ethyl acetate, Et(Ac) (0.1 M)
2. Ensure that all valves are initially closed.
3. Fill the feed vessel B1 with the NaOH and feed vessel B2 with the Et(Ac) solution.
4. Turn on the power for the control panel.
5. Open valves V1 and V2.
6. Switch on pumps P1 and P2. Observe the flow of NaOH and Et(Ac) solutions into
the dosing vessels HB1 and HB2 towards valves V8 and V7.
7. Make sure that the pipelines before valves V7 and V8 are filled with solutions.
Bleed any trapped air in the pipelines by using valves V7 and V8.
8. Allow both the solutionsto overflow in the dosing vessels HB1 and HB2 into the
feed vessels B1and B2.
9. The unit is now ready for experiment.

2.3

General Shut-Down Procedures


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.
5. Turn off the power for the control panel.

13

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

3.0

EXPERIMENTAL PROCEDURES

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
1.

PROCEDURES:

Perform the general start-up procedures


2. Open valves V7 and V8 and adjust valves V7 (Monitor at FI-301)and V8 (Monitor
at FI-302) to give a flow rate of about 400 mL/min. Make sure that both flow rates
are the same.
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 the desired flow rate. Make sure that both flow
rates are the same.
5. Start monitoring the conductivity value at inlet (QI-401) and outlet (QI-402).
6. Start the timer and record both conductivity values (QI-401 and QI-402) and flow
rates (FI-301 and FI-302) when it has reached steady state (Conductivity value
begin to steadily decline with time).
7. Record the inlet and outlet conductivity values and both flow rates for every 5
minutes until the conductivity do not change over time. This is to ensure that the
reactor has reached steady state.
8. Repeat the experiment (steps 4 to 5) for different residence times by adjusting the
flow rates to the desired values. Make sure that both flow rates are the same.

14

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

4.0

ANALYSIS AND DISCUSSION:

1.

Use the table for data collection at Appendix B.


2. Find the concentration of NaOH in the reactor from the calibration curve. Subsequently
calculate the conversion, X based on the formula given in Appendix.
3. Plot a graph of conversion, X vs. reaction time, tfor the different flow rate. Discuss the
graph.
4. The reactors residence time is defined as the reactor volume divided by the average total
feed flow rates.

Residence Time,

VPFR
F0

Subsequently calculate the average residence time,avg (NOTE: 1 FLOW RATE


PARAMETER GIVES 1 AVERAGE RESIDENCE TIME).
5. Compare the highest conversion, Xfor the different average residence time,avg (NOTE:
1 FLOW RATE PARAMETER GIVES 1 AVERAGE RESIDENCE TIME). Compare the
highest conversion, X at the different average residence time, avg. Discuss thoroughly
and explain how residence time can influence the rate of reaction.
6. Forthe different average reactor residence times, avg (NOTE: 1 FLOW RATE GIVES 1
AVERAGE RESIDENCE TIME), calculate the value of the reaction rate constant, k and
the rate of reaction, rA.

Reaction rate constant, k

F0,avg

X
2
AND Rate of reaction, - rA kCA
VPFRCA0 1 X

F0, avg =

Average total inlet flow rate of solutions (mL/min)

CA

Exit concentration of reactant NaOH (M) (Note: Concentration of

NaOH at the highest conversion, X)

5.0

CA0

Inlet concentration of reactant NaOH (M)(0.05M)

Conversion (NOTE: Choose Highest Conversion X)

TUTORIAL
1.

Discuss the advantages and disadvantages of using PFR reactors in chemical


reaction.

2.

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


process.
15

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

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:
1. Perform the general start-up procedures.
2. Check that there is sufficient water in the thermostat T1 tank. Refill as necessary.
3. Open the process water valve V12.
4. Switch on the thermostat T1 and set the water to the desired temperature.
5. Open valves V7 and V8 and adjust valves V7(Monitor at FI-301)and V8(Monitor at
FI-302)to give a flow rate of about 400 mL/min. Make sure that both flow rates are
the same.
6. Allow both the NaOH and Et(Ac) solutions to enter the plug flow reactor SR1 and
empty into the receiving vessel B3.
7. Adjust valves V7 and V8 to give a flow rate of about 100 mL/min. Make sure that
both flow rates are the same.
8. Start monitoring the conductivity value at inlet (QI-401) and outlet (QI-402).
9. Start the timer and record both conductivity values (QI-401 and QI-402) flow rates
(FI-301 and FI-302), and temperatures ((TI-101 and TI-102) when it has reached
steady state (Conductivity value begin to steadily decline with time).
10. Record the conductivity, flow rates, and temperaturesfor every 5 minutes until they
do not change over time. This is to ensure that the reactor has reached steady state.
11. Repeat the experiment (steps 5 onwards) for different reactor temperatures by
increasing the thermostat temperature to the desired temperature. Make sure that the
flow rates of both solutions are maintained at 100 mL/min.

16

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

7.1

ANALYSIS AND DISCUSSION


1. Use the sample table in Appendix B for data collection.
2. Find the concentration of NaOH in the reactor from the calibration curve.Subsequently
calculate the conversion, X based on the formula given in Appendix.
3. Plot a graph of conversion, X vs. reaction time, tfor the2 different temperatures.
4. Compare the highest conversion, X at the different temperature. Discuss it thoroughly and
explain how temperature can influence the rate of reaction, rA.
5. For different reactor temperature, calculate the value of the reaction rate constant, k.

Reaction rate constant, k

F0,avg

VPFRCA0 1 X

F0

= Average total inlet flow rate of solutions (mL/min)

CA0

= Inlet concentration of reactant NaOH (M)(0.05M)

= Conversion (NOTE: Choose Highest Conversion X)

6. Plot a graph of ln k vs 1/T and evaluate the slope and y-axis intercept.

Ea

RT

From Arrhenius equation, k(T ) Aexp


In linear form ln k

Ea 1
ln A
R T

(R = 8.314 J/mol.K)

7. Calculate the saponification reactions activation energy, E a and frequency factor, A from
the slope and intercept values using the Arrhenius equation.
8.0

TUTORIAL
1.

Discuss the advantages and disadvantages of using PFR reactors in chemical


reaction.

2.

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


process.

9.0

REFERENCES
1. Levenspiel O., Chemical Reaction Engineering, John Wiley (USA), 1972.

17

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

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.
4. Astarita G., Mass Transfer with Chemical Reaction, Elsevier, 1967

APPENDIX A
RESULTS FOR PREPARATION OF CALIBRATION CURVE

Solution Mixtures
Conversion

Concentration
of NaOH (M)

Conductivity
(mS/cm)

0.1 M
NaOH

0.1 M
Na(Ac)

H2O

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

NOTE
1. Plot the calibration curve of concentration of NaOH (M) (x-axis) vs conductivity (y-axis).
2. Determine the slope of the curve.
3. Use the calibration curve to determine the concentration of the experimental product (M) from
the pre-determined conductivity found during the experiment.

18

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

RESULTS FOR EXPERIMENTS


Reactor volume
Concentration of NaOH in feed vessel
Concentration of Et(Ac) in feed vessel

Time
(min)

Temperature
(C)

=
=
=

Flow rate Flow rate


of NaOH, of Et(Ac),
FNAOH
FET
(mL/min) (mL/min)

1.5 L
_____ M
_____ M
Total flow
rate of
solutions,
F0 (mL/min)
= FNAOH + FET

Flowrate
=
Temperature =

Residence
time, (min)
(Selfcalculate)

(Self-calculate)

Inlet

Inlet
conductivity
(mS/cm)

_____ mL/min
_____ oC

Inlet
concentration
of NaOH,
CNaOH (M)
(from calibration
curve)

Outlet
Conversion,
concentration
Outlet
X (%)
of
NaOH,
Conductivity
(SelfCNaOH (M)
(mS/cm)
calculate)
(from calibration
curve)

Outlet

0
5
10
15
20
25
30
35
40
45
50
55
60
F0,avg =

avg =

NOTE:
1. Obtain the concentration of NaOH for each of the reaction time from the measured conductivity value based on the calibration curve (Appendix B).
2. Formula to calculate conversion, X

Inlet concentration of NaOH Outlet concentration of NaOH


100%
Inlet concentration of NaOH
19

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

RESULTS FOR EXPERIMENTS


Reactor volume
Concentration of NaOH in feed vessel
Concentration of Et(Ac) in feed vessel

Time
(min)

Temperature
(C)

=
=
=

Flow rate Flow rate


of NaOH, of Et(Ac),
FNAOH
FET
(mL/min) (mL/min)

1.5 L
_____ M
_____ M
Total flow
rate of
solutions,
F0 (mL/min)
= FNAOH + FET

Flowrate
=
Temperature =

Residence
time, (min)
(Selfcalculate)

(Self-calculate)

Inlet

Inlet
conductivity
(mS/cm)

_____ mL/min
_____ oC

Inlet
concentration
of NaOH,
CNaOH (M)
(from calibration
curve)

Outlet
Conversion,
concentration
Outlet
X (%)
of
NaOH,
Conductivity
(SelfCNaOH (M)
(mS/cm)
calculate)
(from calibration
curve)

Outlet

0
5
10
15
20
25
30
35
40
45
50
55
60
F0,avg =

avg =

NOTE:
1. Obtain the concentration of NaOH for each of the reaction time from the measured conductivity value based on the calibration curve (Appendix B).

X
2. Formula to calculate conversion, X

Inlet concentration of NaOH Outlet concentration of NaOH


100%
Inlet concentration of NaOH
19

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

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

1.0

GENERAL DESCRIPTION
1.1

Description and Assembly


Before operating the unit and running experiments, you must familiarize yourself with
the units components. Please refer to Figure 1 to understand the process. All glass
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

4. Feed vessels (B1/B2)

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)

Centrifugal pumps

max delivery rate of 60 L/h and max delivery height of 8 m

7. Pre-heater (W1/W2)
20

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

Coil heat exchanger, area 0.06 m2

max heating media pressure of 0.5 bar


8. Receiving vessel (B3)

100 L rectangular tank


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)


1.2

Safety Considerations
1. The unit must be operated under the supervision of an authorized staff that 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 leak.
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 shall be allowed to carry out any servicing.
Manufacturer's manual must always be observed.
12. Before any servicing, shut down the whole operation and let the system to cool
down and be properly ventilated.
21

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

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.

22

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)


Vent

V22

V23

M2

V24

V25

HS
4
QI
404

M3

M
HS
5

TI
104

M4

HB1

HS
6

HB2

QI
403

R2
M1
HS
3

V1

V2

W1

V17

R4
V18

V11

QI
401

R3

QI
402

SR1

W2

V16
TI
102

T1
TI
103

V12

V13

R1

TI
101

V14

Injection
V15

B1

FI
301

B2

FI
302

FI
303

V19
V8

P1

V3

P2

V4

HS
1

HS
2

V9

V20

V21

V10
V27

V5

V6
V7

B3

Figure 4: Reactor Test Rig


36

V26

Process Water

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

2.0

OPERATING PROCEDURES

2.1

General Start-Up Procedures for Experiment


1. Ensure that all valves are initially closed.
2. Prepare the following solutions:
a) 50 L of sodium hydroxide, NaOH (0.1 M)
b) 50 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.
4. Turn on the power for the control panel.
5. Open the process water valve V27.
6. Open valves V1 and V2.
7. 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.
8. 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.
9. Allow both solutions to overflow in the dosing vessels HB1 and HB2 into the feed vessels
B1 and B2 respectively.
10. The unit is now ready for experiment.

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 and V14.

b)

Switch on the stirrer M1.

c)

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.

c)

Read the outlet conductivity value from QI-403 and temperature value from TI-103.
37

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

2.3

General Shut-Down Procedure


1.

3.0

Switch off both pumps P1 and P2.


2.

Close the process water valve V27.

3.

Open valves V3 to V21 and valve V26 to drain all liquid from the unit.

4.

Turn off the power for the control panel.

EXPERIMENTAL PROCEDURES

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
1.

PROCEDURES:

Perform the general start-up procedures

Plug Flow Reactor, PFR


2.

Open valves V11 and V19.


3.

Open valves V9 (Monitor at FI-302) and V10 (Monitor at FI-303) and adjust
valves V9 and V10 to give a flow rate of about 200 mL/min. Make sure that both
flow rates are the same.

4.

Allow both the NaOH and Et(Ac) solutions to enter the selected reactor and
empty into the receiving vessel B3.

5.

Adjust valves V9 (FI-302) and V10 (FI-303) to give the desired flow rate. Make
sure that both flow rates are the same.

6.

Start monitoring the conductivity value at inlet (QI-401) and outlet (QI-404).

7.

Start the timer and record both conductivity values (QI-401 and QI-404) and
flow rates (FI-302 and FI-303) when it has reached steady state (Conductivity
value begin to steadily decline with time).

8.

Record the inlet and outlet conductivity and flow rate of the reactor for every 5
minutes until they do not change over time. This is to ensure that the reactor has
reached steady state.

9.

Repeat the experiment (steps 2 to 6) by selecting a different reactor.


38

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

Single stage continuous stirred tank reactor


1.

Open valves V13 and V14.


2.

Open valves V9 (Monitor at FI-302) and V10 (Monitor at FI-303) and adjust
valves V9 and V10 to give a flow rate of about 200 mL/min. Make sure that both
flow rates are the same.

3.

Allow both the NaOH and Et(Ac) solutions to enter the selected reactor and
empty into the receiving vessel B3.

4.

Switch on the stirrer M1.

5.

Adjust valves V9 (FI-302) and V10 (FI-303) to give the desired flow rate. Make
sure that both flow rates are the same.

6.

Start monitoring the conductivity value at inlet (QI-401) and outlet (QI-402).

7.

Start the timer and record both conductivity values (QI-401 and QI-402) and
flow rates (FI-302 and FI-303) when it has reached steady state (Conductivity
value begin to steadily decline with time).

8.

Record the inlet and outlet conductivity and flow rate of the reactor for every 5
minutes until they do not change over time. This is to ensure that the reactor has
reached steady state.

9.

Repeat the experiment (steps 2 to 6) by selecting a different reactor.

3-stage continuous stirred tank reactors


1.

Open valves V12 and V21.


2.

Open valves V9 (Monitor at FI-302) and V10 (Monitor at FI-303) and adjust
valves V9 and V10 to give a flow rate of about 200 mL/min. Make sure that both
flow rates are the same.

3.

Allow both the NaOH and Et(Ac) solutions to enter the selected reactor and
empty into the receiving vessel B3.

4.

Switch on the stirrer M2, M3 and M4.

5.

Adjust valves V9 (FI-302) and V10 (FI-303) to give the desired flow rate. Make
sure that both flow rates are the same.

6.

Start monitoring the conductivity value at inlet (QI-401) and outlet (QI-403).

7.

Start the timer and record both conductivity values (QI-401 and QI-403) and
flow rates (FI-302 and FI-303) when it has reached steady state (Conductivity
value begin to steadily decline with time).

8.

Record the inlet and outlet conductivity and flow rate of the reactor for every 5
minutes until they do not change over time. This is to ensure that the reactor has
reached steady state.
39

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

4.0

ANALYSIS AND DISCUSSION:


1. Use the sample table in Appendix B for data collection.
2. Find the concentration ofNaOH exiting the reactor from the calibration curve.
Subsequently calculate the conversion, X based on the formula given in Appendix.
3. Plot a graph of conversion, X vs. reaction time for each of the reactor.
4. Compare the graphs between the different typesof reactors and observe the relationship.
Based on the experimental results, discuss which configurations are the best for this
reaction and state the reasons accordingly.
5. Determine the following parameters:
a) Single stage CSTR

1.

The reactors residence time is defined as the reactor volume divided by the average total feed
flow rates.

Residence Time,

VCSTR
F
0

Subsequently calculate the average residence time,avg


2.

Calculate the value of the reaction rate constant, k and the rate of reaction, rA.

Reaction rate constant, k

A0

CA

avgC

AND Rate of reaction, - rA kCA2

2
A

avg

= Average residence time (min)

CA

= Exit concentration of reactant NaOH (M)


(Note: Concentration of NaOH at the highest conversion, X)

CA0

= Inlet concentration of reactant NaOH (M) (0.05M)

b) 3-stage CSTRs in series


1.

The reactors residence time is defined as the reactor volume divided by the average total feed
flow rates.

Residence Time,

VCSTR
F
0

Subsequently calculate the average residence time,avg


40

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

2.

Calculate the value of the reaction rate constant, k and the rate of reaction, rA.

Reaction rate constant, k

A0

CA

avgC

2
A

AND Rate of reaction, - rA kC A2

avg

= Average residence time (min)

CA

= Exit concentration of reactant NaOH (M)


(Note: Concentration of NaOH at the highest conversion, X)

CA0

= Inlet concentration of reactant NaOH (M) (0.05M)

3. In the 3-stage CSTR in series, all of equal volume and same operating
temperature, the Damnkhler (Da) number for a second order reaction in a
CSTR is defined as, Da = avgkCA0.Calculate the the Damnkhler (Da) number
and discuss its correlation to the highest conversion achieved in this experiment.

c) Plug flow reactor (PFR)


1. Calculate the value of the reaction rate constant, k and the rate of reaction, rA.

Reaction rate constant, k


CA

F0,avg

X
2
AND Rate of reaction, - rA kCA
VPFRCA0 1 X

= Exit concentration of reactant NaOH (M)


(Note: Concentration of NaOH at the highest conversion, X)

5.0

CA0

= Inlet concentration of reactant NaOH (M) (0.05M)

= Extent of conversion (NOTE: Choose Highest Conversion X)

F0,avg

= Average total inlet flow rate of solutions (mL/min)

TUTORIAL
1.

Write the differences between 3 reactors: Single CSTR, 3-stages CSTR and
Tubular(PFR) reactor.

2.
6.0

Discuss the advantages and disadvantages for each configuration.

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.
4. Astarita G., Mass Transfer with Chemical Reaction, Elsevier, 1967.
41

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

APPENDIX A
RESULTS FOR PREPARATION OF CALIBRATION CURVE

Solution Mixtures
Conversion

Concentration
of NaOH (M)

Conductivity
(mS/cm)

0.1 M
NaOH

0.1 M
Na(Ac)

H2O

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

NOTE
1. Plot the calibration curve of concentration of NaOH (M) (x-axis) vs conductivity (y-axis).
2. Determine the slope of the curve.
3. Use the calibration curve to determine the concentration of the experimental product (M) from the
pre-determined conductivity found during the experiment.

42

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

TABLE FOR EXPERIMENT


Reactor type

Concentration of NaOH in feed vessel =

Time
(min)

Temperature
(C)

PFR

Reactor volume

3L

_____ M

Concentration of Et(Ac) in feed vessel

_____ M

Flow rate Flow rate


of NaOH, of Et(Ac),
FNAOH
FET
(mL/min) (mL/min)

Total flow
rate of
solutions,
F0 (mL/min)
= FNAOH + FET

Residence
time, (min)
(Selfcalculate)

(Self-calculate)

Inlet

Inlet
conductivity
(mS/cm)

Inlet
concentration
of NaOH,
CNaOH (M)
(from calibration
curve)

Outlet
Conversion,
concentration
Outlet
X (%)
of
NaOH,
Conductivity
(SelfCNaOH (M)
(mS/cm)
calculate)
(from calibration
curve)

Outlet

0
5
10
15
20
25
30
35
40
45
50
55
60
F0,avg =

avg =

NOTE:
1. Obtain the concentration of NaOH for each of the reaction time from the measured conductivity value based on the calibration curve (Appendix B).

X
2. Formula to calculate conversion, X

Inlet concentration of NaOH Outlet concentration of NaOH


100%
Inlet concentration of NaOH
37

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

TABLE FOR EXPERIMENT


Reactor type

Concentration of NaOH in feed vessel =

Time
(min)

Temperature
(C)

Single-stage CSTR

Reactor volume

4L

_____ M

Concentration of Et(Ac) in feed vessel

_____ M

Flow rate Flow rate


of NaOH, of Et(Ac),
FNAOH
FET
(mL/min) (mL/min)

Total flow
rate of
solutions,
F0 (mL/min)
= FNAOH + FET

Residence
time, (min)
(Selfcalculate)

(Self-calculate)

Inlet

Inlet
conductivity
(mS/cm)

Inlet
concentration
of NaOH,
CNaOH (M)
(from calibration
curve)

Outlet
concentration Conversion,
Outlet
X (%)
of NaOH,
Conductivity
(SelfCNaOH (M)
(mS/cm)
calculate)
(from calibration
curve)

Outlet

0
5
10
15
20
25
30
35
40
45
50
55
60
F0,avg =

avg =

NOTE:
1. Obtain the concentration of NaOH for each of the reaction time from the measured conductivity value based on the calibration curve (Appendix B).

X
2. Formula to calculate conversion, X

Inlet concentration of NaOH Outlet concentration of NaOH


100%
Inlet concentration of NaOH
38

LABORATORY MANUAL (JAN 2015)REACTION ENGINEERING (CKB 20104)

TABLE FOR EXPERIMENT


Reactor type

Concentration of NaOH in feed vessel =

Time
(min)

Temperature
(C)

3-stage CSTRs

Reactor volume

1L

_____ M

Concentration of Et(Ac) in feed vessel

_____ M

Flow rate Flow rate


of NaOH, of Et(Ac),
FNAOH
FET
(mL/min) (mL/min)

Total flow
rate of
solutions,
F0 (mL/min)
= FNAOH + FET

Residence
time, (min)
(Selfcalculate)

(Self-calculate)

Inlet

Inlet
conductivity
(mS/cm)

Inlet
concentration
of NaOH,
CNaOH (M)
(from calibration
curve)

Outlet
Conversion,
concentration
Outlet
X (%)
of
NaOH,
Conductivity
(SelfC
(M)
NaOH
(mS/cm)
calculate)
(from calibration
curve)

Outlet

0
5
10
15
20
25
30
35
40
45
50
55
60
F0,avg =

avg =

NOTE:
1. Obtain the concentration of NaOH for each of the reaction time from the measured conductivity value based on the calibration curve (Appendix B).

X
2. Formula to calculate conversion, X

Inlet concentration of NaOH Outlet concentration of NaOH


100%
Inlet concentration of NaOH
39