LABORATORY

MODULE

PTT 248/4
REACTOR ENGINEERING
SEMESTER 2 (2014/2015)

Miss Nor Fauziah Binti Zainudin

Dr. Teoh Yi Peng
Mr. Mohd Qalani Che Kasim

Faculty of Engineering Technology

University Malaysia Perlis

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 CONTENT

CONTENT ii

CLEANLINESS AND SAFETY iii

EXPERIMENT 1 : INTRODUCTION TO REACTOR ENGINEERING 1

LABORATORY SAFETY AND ITS MACHINERIES

EXPERIMENT 2 : EFFECT OF FLOW RATE ON THE REACTION 4

IN A CONTINUOUS STIRRED TANK REACTOR
(CSTR)

EXPERIMENT 3 : EFFECT OF TEMPERATURE ON THE 11

REACTION IN A CONTINUOUS STIRRED TANK
REACTOR (CSTR)

EXPERIMENT 4 : DETERMINATION OF FLOWRATE 19

TEMPERATURE ON CONVERSION IN TUBULAR
REACTOR

EXPERIMENT 5 : DETERMINATION OF REACTION RATE 26

CONSTANT AND REACTION ORDER IN BATCH
REACTOR

EXPERIMENT 6 : DETERMINATION OF EFFECT OF 33

TEMPERATURE ON REACTION AND
REACTION’S ACTIVATION ENERGY FOR
BATCH REACTOR.

EXPERIMENT 7 : DETERMINATION OF STIRRING AND 41

TEMPERATURE EFFECTS ON CONVERSION
IN SERIES OF CONTINUOUS STIRRED TANK
REACTOR (CSTRs)

REFERENCES 48

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 CLEANLINESS AND SAFETY

CLEANLINESS

The Reaction Engineering Laboratory contains equipment that uses water or

chemicals as the fluid. In some cases, performing an experiment will inevitably allow
water/chemicals to get on the equipment and/or on the floor.

There are “housekeeping” rules that the user of the laboratory should be aware and
abide by. If no one cleaned up their working area after performing an experiment, the
lab would not be a comfortable or safe place to work in. Consequently, students are
required to clean up their area at the conclusion of the performance of an
experiment. Cleanup will include

 removal of spilled water (or any liquid) or chemicals

 wiping the table top on which the equipment is mounted

The lab should always be as clean as or cleaner than it was when you entered.
Cleaning the lab is your responsibility as a user of the equipment.

SAFETY
This is to serve as a guide and not as a comprehensive manual on safety. Every
staff/student has, at all time, a duty to care for Health and Safety of himself/herself
and of all people who may be affected by his/her action.

PROTECTIVE CLOTHING – Lab coat or Jackets MUST be worn all times. Rubber
gloves should be worn when handling corrosive materials, and heat-proof gauntlets
when discharging any equipments involving heat.

FOOTWARE – Wear fully covered shoes with strong grip.

EYE PROTECTION – Goggles must be used whenever necessary especially when

dealing with high pressure equipments.

iii
ELECTRICITY – Sometimes the floor may be wet. Therefore, care is essential.
Always switch off power before removing plugs from sockets.

CABLES AND HOSES – Cables must be suspended and not lying on the floor. All
cables and hoses should be routed to avoid walk-ways.

BROKEN GLASS – This should be disposed off in the glass bin, not in the usual
waste bin. Breakage should also be reported to the Instructor in charge.

INSTRUCTION SHEETS – Any appropriate instruction sheets should be studied

before starting the experiment. Particular attention should be given to the
recommended precautions, start up procedure and sequence of operation.

There should be NO EATING in the laboratory. Smoking is strictly prohibited in all

laboratories.

In case of emergency, report to the Instructor in charge or

doctor/ambulance/fire fighter from:

Hospital Tuanku Fauziah, Kangar 04-9763333

Bomba Perlis 04-9778827

SAFETY FIRST

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PTT 248/4 – Reactor Engineering Laboratory Module

EXPERIMENT 1
INTRODUCTION TO REACTOR ENGINEERING LABORATORY
SAFETY AND ITS MACHINERIES

1.0 OBJECTIVE

1.1 To identify applicable safety measures in performing the reactor engineering laboratory
practice.
1.2 To determine the necessary precautions prior to usage of reactor engineering learning
apparatus.

2.0 COURSE OUTCOME

CO1 : Ability to categorize design equation for most common industrial reactors and reactor
sizing.

3.0 INTRODUCTION TO LABORATORY SAFETY

The Engineering Laboratory contains equipment that use chemicals and water as the fluid. In
some cases, performing an experiment will inevitably allow water and chemicals to get on the
equipment and/or on the floor. Thus, the most basic practice in maintaining safe working
environment is to ensure that the workplace is well kept clean and organized at all times.

Laboratory users are required to clean up their work area at the end of the every experiment
performed. Cleanup will include, but not limited to, removal of spilled liquid and wiping the table
top on which the equipment is mounted. However, it is imperative that the lab should always be
kept clean as practicably possible, even during the experimental run.

Beside cleanliness, the use of personal protection equipment (PPE) is also vital to ensure one‟s
safety during the experimental run. PPE is considered as the last resort protection and should be
selected appropriately. PPE must be properly fitted, tested, cleansed, maintained and stored.
Comfortable PPE will ensure the efficiency of its usage towards protecting the users from specific
hazards.

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PTT 248/4 – Reactor Engineering Laboratory Module

PROTECTIVE CLOTHING – Lab coat or Jackets MUST be worn all times. Rubber gloves should
be worn when handling corrosive materials, and heat-proof gauntlets when discharging any
equipments involving heat.

FOOTWARE – Wear fully covered shoes with strong grip.

EYE PROTECTION – Goggles must be used whenever necessary especially when dealing with
high pressure equipments.

ELECTRICITY – Sometimes the floor may be wet. Therefore, care is essential. Always switch off
power before removing plugs from sockets.

CABLES AND HOSES – Cables must be suspended and not lying on the floor. All cables and
hoses should be routed to avoid walk-ways.

BROKEN GLASS – This should be disposed off in the glass bin, not in the usual waste bin.
Breakage should also be reported to the Instructor in charge.

INSTRUCTION SHEETS / LAB PROCEDURES – Any appropriate instruction sheets or lab

procedures should be studied before starting the experiment. Particular attention should be given
to the recommended precautions, start up procedure and sequence of operation.

3.0 REACTOR ENGINEERING LEARNING APPARATUS

The apparatus for the fluid mechanics laboratory is listed as follows:

i. Continuous-Stirred Tank Reactor
ii. Tubular Flow Reactor
iii. Batch Reactor
iv. Continuous-Stirred Tank Reactor in Series

4.0 EXPERIMENTAL PROCEDURES

1. Locate each reactor engineering apparatus provided in the laboratory.

2. Based on the physical appearance of the apparatus, assembly of equipment such as
pumps and tanks, and connections of piping, fittings and gauges at each apparatus:
a) Identify the necessary PPE to be utilized during the experimental run
b) Analyze all safety sign in the laboratory

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PTT 248/4 – Reactor Engineering Laboratory Module

c) Develop the general start-up and shutdown procedures as well as other necessary
precautions for the apparatus.

5.0 RESULTS AND DISCUSSIONS

1. Write the general lab procedures in Engineering Lab

2. Present your findings in section 4.0 (No.2) in a tabulated manner.
3. Discuss the first aid measures for each chemical that you will used in the laboratory (Refer
to Material Safety Data Sheet, MSDS).

6.0 CONCLUSION

Conclude your findings related to importance of laboratory safety.

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EXPERIMENT 2
EFFECT OF FLOW RATE ON THE REACTION IN A CSTR

1.0 OBJECTIVE
1.1 To carry out a saponification reaction between NaOH and Et(Ac) in a CSTR.
1.2 To determine the effect of flow rate on the extent of conversion.
1.3 To determine the reaction rate constant.

2.0 CORRESPONDING COURSE OUTCOME

CO 2 - Ability to analyze rate law and isothermal reactor design.

3.0 INTRODUCTION
The SOLTEQ® Reactor Basic Unit (CSTR) (Model: BP 400) has been designed for students‟
experiments on chemical reactions in liquid phase under isothermal condition. The unit comes
complete with a glass reactor, individual reactant feed tanks and pumps, temperature sensors and
conductivity measuring sensor. The reactor will enable students to conduct the typical
saponification reaction between ethyl acetate and sodium hydroxide among other types of
reaction.

4.0THEORY

4.1 CONTINUOUS-STIRRED TANK REACTOR

As with all continuous flow reactors, CSTRs are almost always operated at steady state. In
addition, the contents inside the reactor are assumed to be perfectly mixed. As a result, there is
no time or position dependence of the temperature, concentration or reaction rate inside the
CSTR. Therefore, all variables are the same at any point within the reaction vessel.

From the general mole balance equation,

Eq. (1)

So, the design equations for the continuous-stirred tank reactor.

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PTT 248/4 – Reactor Engineering Laboratory Module

Eq. (2)

Figure 1: Mole balance on a CSTR

4.2 CONVERSION IN CONTINUOUS-STIRRED TANK REACTORS

In chemical reactions, it is often that one of the reagents deplete before the others. When this
occurs, the reaction ceases, and thus this reagent is termed the limiting reagent. In most
instances, it is best to choose the limiting reagent as the basis of stoichiometric calculations.
Consider a general reaction

Eq. (3)

where the uppercase letters represent chemical species and the lowercase letters represent
stoichiometric coefficients (moles). Suppose that species A were to be the limiting reagent, we
then divide the reaction expression by the coefficient of species A, to obtain

Eq. (4)

Now that the other chemical species are on a “per mole of A” basis, we would then want to know
how far the reaction proceeds to the right, or how many moles of A are consumed to form one
mole of C. These can be determined by defining a parameter called conversion. The conversion
of chemical species A is simply the number of moles of A that have reacted per mole of A fed into
the system.

Eq (5)

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4.3 SAPONIFICATION OF ETHERS WITH SODIUM HYDROXIDE

Now that we understand the basic chemistry and chemical engineering involved in chemical
reactors, consider a chemical reaction between an ether and sodium hydroxide. This process is
also known as saponification. The reaction is reversible, and is described by

The acetic ether (ethyl acetate) molecules split into acetate ions and ethanol molecules,
consuming hydroxide ions provided by the sodium hydroxide in the process. The progress of the
reaction can thus be tracked accurately by the change in hydroxide ions. This can be observed by
the conductivity change in the reactor vessel, since the presence of hydroxide ions increase the
conductivity in a solution.

5.0 MATERIALS AND EQUIPMENT

5.1 Description of Apparatus

Figure 2: Unit construction for Single CSTR reactor

5.2 Description and Assembly

Before operating the unit and running experiments, students must familiarize
themselves with every components of the unit. Please refer to Figure 1 to
understand the process.

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PTT 248/4 – Reactor Engineering Laboratory Module

1. Reactor (R1)
3.0-L vessel made of borosilicate glass
Internal cooling coil
2 Cartridge type heaters ( 500 W)
Stainless steel impeller

2. Stirrer (M1)
Medium duty general purpose motor
Power: 24V d.c. / 75 W
Max. speed: 230 rpm, steplessly adjustable by hand
Max torque: 200 mNm

3. Feed tanks (B1, B2)

35-L cylindrical tank made of stainless steel

4. Pumps (P1, P2)

Diaphragm pumps
Max delivery rate: 3.785 LPM
Max pressure: 25 psi
Power: 12V d.c.

5. Instrumentation
Temperature measurement (TIC-101)
Flow measurement (FI-201, FI-202)
Conductivity measurement (QI-301)
5.3 Valves and Instruments List

Valves list:
Tag Location
V1 Drain valve for feed tank B1
V2 Inlet valve for pump P1
V3 By-pass valve from P1 to tank B1
V4 Needle valve for liquid flow regulating at FI 201
V5 Drain valve for feed tank B2
V6 Inlet valve for pump P2
V7 By-pass valve from P2 to tank B2
V8 Needle valve for liquid flow regulating at FI 202
V9 Drain valve for CSTR Reactor R1
V10 Sampling valve
V11 Inlet port for cooling water into reactor

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PTT 248/4 – Reactor Engineering Laboratory Module

6.0 PROCEDURES

6.1 Preparation of Calibration Curve for Conductivity vs. Conversion.

6.1.1 Prepare the following solutions:
a) 1 liter of sodium hydroxide (0.1 M)
b) 1 liter of sodium acetate (0.1 M)
c) 1 liter of deionised water, H2O

6.1.2 Determine the conductivity and NaOH concentration for each conversion value
by mixing the following solutions into 100 mL of deionised water.
0% conversion : 100 mL NaOH
25% conversion : 75 mL NaOH + 25 mL Na(Ac)
50% conversion : 50 mL NaOH + 50 mL Na(Ac)
75% conversion : 25 mL NaOH + 75 mL Na(Ac)
100% conversion : 100 mL Na(Ac)

6.1.3 Tabulate all data in the table of Appendix B1.

6.2 Start up

6.2.1. Ensure that all valves are initially closed except by-pass valves V3 and V7.

6.2.2. Fill feed tank B1 with the NaOH solution and feed tank B2 with the Et(Ac)
solution. Close the feed tanks.

6.2.3. Turn on the power for the control panel.

6.2.4. Adjust the overflow tube to give working volume of 1 liter in the reactor R1.

6.2.5. Open valves V2 and V6.

6.2.6. The unit is now ready for experiment.

6.3 Experiment Effect Of Flow Rate On The Reaction In A CSTR

6.3.1. Switch on both pumps P1 and P2 simultaneously and open valves V4 and V8
to obtain the highest possible flow rate into the reactor.

6.3.2. Let the reactor fill up with both the solution until it is just about to overflow.
Adjust the overflow tube to achieve level of the mixture solution which is 1 liter.

6.3.3. Set the flow rate of about 200 ml/min at both flow meters. Make sure that both
flow rates are the same. Set the temperature controller at 30oC

6.3.4. Switch on the stirrer and set the speed to about 200 rpm.

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6.3.5. Start monitoring the conductivity value until it does not change over time. This
is to ensure that the reactor has reached steady state.

6.3.6. Record the steady state conductivity value.

6.3.7. Repeat the experiment (steps 3 to 6) for different flow rates by adjusting the
feed flow rates of NaOH and Et(Ac) at 100 ml/min . Make sure that both feed
flow rates are the same.
6.3. 8. Switch off the main power switch and dosing pump.
6.3. 9. Drain chemicals in the reactor vessels and the waste tank.

7.0 RESULTS
7.1 Record all the results in appropriate tables.
7.2 Plot graph of conductivity vs. conversion, concentration NaOH vs. conversion.
7.3 Plot a graph of conversion vs. time.
7.4 Plot a graph of conversion vs. residence time.
7.5 For different flow rates, calculate the value of the reaction rate constant, k and the
rate of reaction, -rA.

8.0 DISCUSSION
8.1 Discuss the effect of flow rate on the conversion.
8.2 Discuss appropriate discussion regarding this experiment

9.0 CONCLUSION
9.1 Based on the experimental procedure done and the results taken draw some
conclusions to this experiment.

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APPENDIX A1: Physical Properties of Et(Ac) and NaOH.

Property Ethyl Acetate, Et(Ac) Sodium Hydroxide, NaOH

Formula CH3COOCH2CH3 NaOH

Appearance clear liquid white solid

Molecular weight 88.11 g/mol 40.00 g/mol

Normal boiling point 77.1°C 1390° C

Normal melting point -84.0°C 323°C

Density 0.8945 g/mL @ 25°C 2.1 g/mL

Refractive index 1.3274 @ 20°C –

APPENDIX B1: Sample Table for Preparation of Calibration Curve

Solution Mixtures
Concentration Conductivity
Conversion 0.1 M 0.1 M
H2O of NaOH (M) (mS/cm)
NaOH Na(Ac)
0% 100 mL

25% 100 mL
50% 100 mL

75% 100 mL
100% 100 mL

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EXPERIMENT 3
EFFECT OF TEMPERATURE ON THE REACTION IN A CSTR

1.0 OBJECTIVE
1.1 To determine the effect of temperature on the extent of conversion.
1.2 To determine the value of the reaction‟s activation energy.

2.0 CORRESPONDING COURSE OUTCOME

CO3 - Ability to analyze rate data and multiple reaction.

3.0 INTRODUCTION
The SOLTEQ® Reactor Basic Unit (CSTR) (Model: BP 400) has been designed for students‟
experiments on chemical reactions in liquid phase under isothermal condition. The unit comes
complete with a glass reactor, individual reactant feed tanks and pumps, temperature sensors and
conductivity measuring sensor. The reactor will enable students to conduct the typical
saponification reaction between ethyl acetate and sodium hydroxide among other types of
reaction.

4.0 THEORY

4.1 CONTINUOUS-STIRRED TANK REACTOR

As with all continuous flow reactors, CSTRs are almost always operated at steady state. In
addition, the contents inside the reactor are assumed to be perfectly mixed. As a result, there is
no time or position dependence of the temperature, concentration or reaction rate inside the
CSTR. Therefore, all variables are the same at any point within the reaction vessel.

From the general mole balance equation,

Eq. (1)
So, the design equations for the continuous-stirred tank reactor.

Eq. (2)

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PTT 248/4 – Reactor Engineering Laboratory Module

Figure 1: Mole balance on a CSTR

4.2 CONVERSION IN CONTINUOUS-STIRRED TANK REACTORS

In chemical reactions, it is often that one of the reagents deplete before the others. When this
occurs, the reaction ceases, and thus this reagent is termed the limiting reagent. In most
instances, it is best to choose the limiting reagent as the basis of stoichiometric calculations.
Consider a general reaction

Eq. (3)

where the uppercase letters represent chemical species and the lowercase letters represent
stoichiometric coefficients (moles). Suppose that species A were to be the limiting reagent, we
then divide the reaction expression by the coefficient of species A, to obtain

Eq. (4)

Now that the other chemical species are on a “per mole of A” basis, we would then want to know
how far the reaction proceeds to the right, or how many moles of A are consumed to form one
mole of C. These can be determined by defining a parameter called conversion. The conversion
of chemical species A is simply the number of moles of A that have reacted per mole of A fed into
the system.

Eq (5)

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PTT 248/4 – Reactor Engineering Laboratory Module

4.3 SAPONIFICATION OF ETHERS WITH SODIUM HYDROXIDE

Now that we understand the basic chemistry and chemical engineering involved in chemical
reactors, consider a chemical reaction between an ether and sodium hydroxide. This process is
also known as saponification. The reaction is reversible, and is described by

The acetic ether (ethyl acetate) molecules split into acetate ions and ethanol molecules,
consuming hydroxide ions provided by the sodium hydroxide in the process. The progress of the
reaction can thus be tracked accurately by the change in hydroxide ions. This can be observed by
the conductivity change in the reactor vessel, since the presence of hydroxide ions increase the
conductivity in a solution.

5.0 MATERIALS AND EQUIPMENTS

5.1 Description of Apparatus

Figure 6: Unit construction for Single CSTR reactor

5.2 Description and Assembly

Before operating the unit and running experiments, students must familiarize
themselves with every components of the unit. Please refer to Figure 1 to
understand the process.

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PTT 248/4 – Reactor Engineering Laboratory Module

1. Reactor (R1)

3.0-L vessel made of borosilicate glass

Internal cooling coil
2 Cartridge type heaters ( 500 W)
Stainless steel impeller
Ports for:
Stirrer (M1)
Inlet for feed vessels (B1, B2)
Sensors: conductivity (QI01) and temperature (TIC01)
Cooling coil
Venting port

2. Stirrer (M1)

Medium duty general purpose motor

Power: 24V d.c. / 75 W
Max. speed: 230 rpm, steplessly adjustable by hand
Max torque: 200 mNm

3. Feed tanks (B1, B2)

35-L cylindrical tank made of stainless steel

5. Pumps (P1, P2)

Diaphragm pumps
Max delivery rate: 3.785 LPM
Max pressure: 25 psi
Power: 12V d.c. 5.Instrumentation
Temperature measurement (TIC-101)
Flow measurement (FI-201, FI-202)
Conductivity measurement (QI-301)

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5.3 Valves and Instruments List

Valves list:
Tag Location
V1 Drain valve for feed tank B1
V2 Inlet valve for pump P1
V3 By-pass valve from P1 to tank B1
Needle valve for liquid flow regulating at FI
V4
201
V5 Drain valve for feed tank B2
V6 Inlet valve for pump P2
V7 By-pass valve from P2 to tank B2
Needle valve for liquid flow regulating at FI
V8
202
V9 Drain valve for CSTR Reactor R1
V10 Sampling valve
V11 Inlet port for cooling water into reactor

6.0 PROCEDURES
6.1 Preparation of Calibration Curve for Conductivity vs. Conversion.

6.1.1 Prepare the following solutions:

a) 1 liter of sodium hydroxide (0.1 M)
b) 1 liter of sodium acetate (0.1 M)
c) 1 liter of deionised water, H2O

6.1.2 Determine the conductivity and NaOH concentration for each conversion value
by mixing the following solutions into 100 mL of deionised water.

0% conversion : 100 mL NaOH

25% conversion : 75 mL NaOH + 25 mL Na(Ac)
50% conversion : 50 mL NaOH + 50 mL Na(Ac)
75% conversion : 25 mL NaOH + 75 mL Na(Ac)
100% conversion : 100 mL Na(Ac)

6.1.3 Tabulate all data in the table of Appendix B2.

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6.2 Start up

6.2.1. Ensure that all valves are initially closed except by-pass valves V3 and V7.

6.2.2. Fill feed tank B1 with the NaOH solution and feed tank B2 with the Et(Ac)
solution. Close the feed tanks.

6.2.3. Turn on the power for the control panel.

6.2.4. Adjust the overflow tube to give working volume of 1 liter in the reactor R1.

6.2.5. Open valves V2 and V6.

6.2.6. The unit is now ready for experiment.

6.3 Experiment: Effect Of Temperature On The Reaction In A CSTR

6.3.1 Switch on both pumps P1 and P2 simultaneously and open valves V4 and V8
to obtain the highest possible flow rate into the reactor.

6.3.2 Let the reactor fill up with both the solution until it is just about to overflow.

6.3.3 Adjust valves V4 and V8 to give a flow rate of about 100 ml/min at both flow
meters. Make sure that both flow rates are the same.

6.3.4 Switch on the stirrer M1 and set the speed to about 200 rpm.

6.3.5 Switch on the heater on the control panel. Set the temperature setpoint on the
TIC-101 to 30 °C. Allow the liquid temperature to rise to the setpoint and
remains constant.

6.3.6 Start monitoring the conductivity reading until it doesn‟t change over time.
This is to ensure that the reactor has reached steady state.

6.3.7 Record the steady state conductivity and temperature readings.

6.3.8 Repeat the experiment for different reactor temperature of 50oC. Make sure
that the flow rates of both solutions are maintained at 100 ml/min.
6.3.9 Switch off the main power switch and dosing pump. Stop the cooling water
flow.
6.3.10 Drain chemicals in the reactor vessels and the waste tank.

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7.0 RESULTS
7.1 Record all the results in appropriate tables.

7.2 Plot a graph of conductivity vs. conversion, conversion vs. reaction temperature, T.

7.3 Plot the graph of „ln k ‟ vs „1/T‟ and evaluate the slope and y-axis intercept.

7.4 Calculate the activation energy, E and Arrhenius constant, A from the slope and

intercept values using the Arrhenius equation.

8.0 DISCUSSION

8.1 Discuss the effect of temperature on reaction (reaction constant, activation energy,
Arrhenius constant) in a single CSTR.

9.0 CONCLUSION
9.1 Based on the experimental procedure done and the results taken draw some
conclusions to this experiment.

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APPENDIX A2: Physical Properties of Et(Ac) and NaOH.

Property Ethyl Acetate, Et(Ac) Sodium Hydroxide, NaOH

Formula CH3COOCH2CH3 NaOH

Appearance clear liquid white solid

Molecular weight 88.11 g/mol 40.00 g/mol

Normal boiling point 77.1°C 1390° C

Normal melting point -84.0°C 323°C

Density 0.8945 g/mL @ 25°C 2.1 g/mL

Refractive index 1.3274 @ 20°C –

APPENDIX B2: Sample Table for Preparation of Calibration Curve

Solution Mixtures
Concentration Conductivity
Conversion 0.1 M 0.1 M
H2O of NaOH (M) (mS/cm)
NaOH Na(Ac)
0% 100 mL

25% 100 mL
50% 100 mL

75% 100 mL
100% 100 mL

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EXPERIMENT 4
DETERMINATION OF FLOW RATE AND TEMPERATURE ON
CONVERSION IN TUBULAR REACTOR

1.0 OBJECTIVE
1.1 To observe and control the operation of a tubular reactor.
1.2 To determine the effects of flow rate and reaction temperature on conversion rate in a
tubular reactor.

2.0 CORRESPONDING COURSE OUTCOME

CO3 – Ability to analyze rate law and isothermal reactor design

3.0 INTRODUCTION
The tubular reactor, also known as the plug flow reactor (PFR) is a type of continuous flow
reactor commonly used in industrial processing. As with all continuous flow reactors, PFRs
are almost always operated at steady state. However, the PFR is often used gas-phase
reactions, unlike the batch and continuous-stirred tank reactors.
As the reactants flow down the length of the reactor in a PFR, they are continually
consumed. When modeling a tubular reactor, it is assumed that the concentration varies
continuously in the axial direction through the reactor. Subsequently, the reaction rate also
varies axially, since it is a function of concentration (except for zero-order reactions). Now,
consider a system which the flow field is modeled by that of a plug flow profile (uniform
velocity as in turbulent flow). Thus, there should be no radial variation in reaction rate, as
shown in Figure 1.

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4.0 THEORY

4.1 Conversion In Tubular Reactors

General mole balance equation :

There are two ways we can use to develop a design equation for the PFR; the first involves
differentiating the general mole balance equation with respect to volume V,

while the second method is by performing a mole balance on species j in a small volume ΔV (as
shown in Figure 2). For the second method, the differential volume will be chosen such that there
are no spatial variations in reaction rate within this volume.

Figure 2: Mole balance on species j in a differential volume ΔV

The generation rate, ΔGj would then be

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4.2 Saponification Of Ethers With Sodium Hydroxide

Now that we understand the basic chemistry and chemical engineering involved in chemical
reactors, consider a chemical reaction between an ether and sodium hydroxide. This process is
also known as saponification.

The acetic ether (ethyl acetate) molecules split into acetate ions and ethanol molecules,
consuming hydroxide ions provided by the sodium hydroxide in the process. The progress of the
reaction can thus be tracked accurately by the change in hydroxide ions. This can be observed by
the conductivity change in the reactor vessel, since the presence of hydroxide ions increase the
conductivity in a solution. As the conversion increases, the hydroxide ions depletes to form
ethanol, and this should be observed by a decrease in conductivity.

5.0 MATERIALS AND EQUIPMENTS

5.1 Description Of Apparatus

The Tubular Flow Reactor is used for demonstrating the basics of chemical processing in tubular
flow reactors. The apparatus is comprised of a stainless steel top to accommodate 2 glass feed
tanks, a workspace to mount the chemical reactor, a hot water reservoir and a process control
console. The stainless steel base of the console is fitted with 2 peristaltic pumps with speed
controls for feeding the reactants, one heater control and one stirrer control unit.
Two reactant tanks are provided with heating coils to bring reactants to reaction temperatures
before being dosed into a Y joint into the tubular reactor.

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6.0 PROCEDURES
6.1 Preparation of Calibration Curve for Conductivity vs. Conversion.
6.1.1 Prepare the following solutions:
a) 1 liter of sodium hydroxide (0.1 M)
b) 1 liter of sodium acetate (0.1 M)
c) 1 liter of deionised water, H2O

6.1.2 Determine the conductivity and NaOH concentration for each conversion value by
mixing the following solutions into 100 mL of deionised water.

0% conversion : 100 mL NaOH

25% conversion : 75 mL NaOH + 25 mL Na(Ac)
50% conversion : 50 mL NaOH + 50 mL Na(Ac)
75% conversion : 25 mL NaOH + 75 mL Na(Ac)
100% conversion : 100 mL Na(Ac)

6.1.3 Tabulate all data in the table of Appendix A3.

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6.2 General Start-up Procedures

6.2.1 Fill the chemical tanks until 80% full.
6.2.2 Fill the rear left tank with 0.1 M ethyl acetate solution and the rear right tank with
0.1 M sodium hydroxide solution.
Safety Caution : ALWAYS use the LEFT tank for the ethyl acetate solution, as
the pump for the left tank is specially designed for the chemical. Failure to do so
may result in damage to the other pump.
6.2.3 Connect the reactor tank‟s water inlet and outlet to a water supply and drain
respectively.
6.2.4 Fill the reactor tank with water until the tubular reactor is completely immersed in
water.
Safety Caution : Do not overfill the reactor tank, as the high pressure water supply
may damage the vessel’s seal.
6.2.5 Plug in the 3-pin plug into a power supply and switch on the power.
6.2.6 Switch on the mains power on the unit.
6.2.7 Ensure that the heater is set to 45°C.
6.2.8 Switch on the agitator/mixer, and set the speed to approximately 100rpm.
6.2.9 Switch on both pumps for the dosing tanks and set the speed for both to 40%.
6.2.10 Before conducting experiments, ensure that the hot water valves for all tanks are
fully closed.
6.2.11 If all components are working and in order, the system is ready for use.

6.3 Experiment 1: The Effect of Flow Rate on Conversion Rate.

6.3.1 Set the speed for both dosing pump to 30% and turn on both dosing pumps.
6.3.2 Take down the reading of conductivity and temperature at the entry and exit of the
reactor for every one minute until no conversion at the exit changes.
6.3.3 Repeat Step 6.3.1 and 6.3.2 for the speed of 50%.
6.3.4 Tabulate all data and calculate the conversion at each time interval in the table of
Appendix B3.

6.4 Experiment 2: The Effect of Reaction Temperature on Conversion Rate.

6.4.1 Turn on the heater.
6.4.2 Make sure hot water temperature reaches 45 oC.
6.4.3 Open all hot water valves.
6.4.4 Turn on the hot water pump and wait until temperature of the both chemical tanks
and the reactor reached 45oC
6.4.5 Start the both dosing pumps and start timer on the stopwatch.

23
PTT 248/4 – Reactor Engineering Laboratory Module

6.4.6 Take down the reading of conductivity and temperature at the entry and exit of the
reactor for every one minute until no conversion at the exit changes.
6.4.7 Turn off the both dosing pumps and the hot water pump.
6.4.8 Tabulate all data and calculate the conversion at each time interval in the table of
Appendix B3.

6.5 Maintenance And Safety Precautions

6.5.1 Read the safety instructions thoroughly before conducting the experiment.
6.5.2 Wear protective gloves and glasses when conducting the experiment.
6.5.3 Dispose of all unused chemicals in an appropriate manner after the experiment.
Under no circumstances should the chemicals be allowed to flow into the main
drains.
6.5.4 Should any of the chemicals come into contact with the body, rinse off immediately
with cold water.
6.5.5 Be alert and careful at all times when conducting the experiment.

6.6 General Shut Down Procedures

6.6.1 Switch off the main power switch.
6.6.2 Switch off the dosing pump.

7.0 RESULTS
7.1 Record all the results in the table (Appendix B3) for every reading taken by
conductivity and temperature meter.
7.2 Plot calibration curve graph. (Conductivity vs. conversion; concentration of NaOH
vs. conversion).
7.3 Plot a graph of conversion vs. time for all experiments.

8.0 DISCUSSION
8.1 Discuss the effect of flow rate and temperature on conversion and conversion rate
through appropriate graphs.

9.0 CONCLUSION
9.1 Based on the experimental procedure done and the results taken draw some
conclusions to this experiment.

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PTT 248/4 – Reactor Engineering Laboratory Module

APPENDIX A3: Sample Table for Preparation of Calibration Curve

Solution Mixtures
Concentration Conductivity
Conversion 0.1 M 0.1 M
H2O of NaOH (M) (mS/cm)
NaOH Na(Ac)
0% 100 mL

25% 100 mL

50% 100 mL
75% 100 mL

100% 100 mL

APPENDIX B3: Sample Table for Experiment 1 & 2

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PTT 248/4 – Reactor Engineering Laboratory Module

EXPERIMENT 5
Determination of Reaction Rate Constant and Reaction Order in Batch
Reactor

1.0 OBJECTIVES
1.1 To observe and control the operation of a batch reactor for saponification reaction
between Sodium Hydroxide and Ethyl Acetate.
1.2 To determine the reaction rate constant and reaction order in batch reactor.

2.0 CORRESPONDING COURSE OUTCOME

CO2 - Ability to analyze rate law and isothermal reactor design

3.0 INTRODUCTION
In the majority of industrial chemical processes, reactor is the key equipment in which raw
materials undergo a chemical change to form desired products. The design and operation
of chemical reactors is thus crucial to the whole success of an industrial process. Reactors
can take a widely varying form, depending on the nature of the feed materials and the
products. Understanding the behavior of how reactors function is necessary for the proper
design, control and handling of a reaction system. Two main types of reactors are batch
reactor and continuous flow reactor.
The Reactor Basic Unit (Batch Reactor) has been designed for students‟ experiments on
chemical reactions in liquid phase under isothermal and adiabatic conditions. The unit
comes complete with a glass reactor, constant temperature water circulating unit,
temperature and conductivity measurements. Student shall be able to conduct the typical
saponification reaction between ethyl acetate and sodium hydroxide.

26
PTT 248/4 – Reactor Engineering Laboratory Module

4.0 THEORY
4.1 Rate of Reaction and Rate Law.

The rate at which a given chemical reaction proceeds can be expressed in several ways. It
can be expressed either as the rate of disappearance of the reactants, or the rate of
formation of products. In the following reaction,

aA + bB  cC + dD [1-1]

A and B are the reactants, while C and D are the products. a,b,c,d are the stoichiometric
coefficients for the respective species.If species A is considered as the reaction basis, then
the rate of reaction can be represented by the rate of disappearance of A. It is denoted by
the symbol –rA . The numerical value of the rate of reaction, –rA is defined as the number of
moles of A reacting (disappearing) per unit time per unit volume, and has the typical unit of
mol/dm3.s.
Similarly, the rate of reaction can also be represented by the rate of disappearance of
another species, such as –rB and the rate of formation of a product, such as rC or rD . They
can be related in the following equation,
 rA  rB rC rD
   [1-2]
a b c d

4.2 Conversion
Using the reaction shown in Equation [1-1], and taking species A as the basis of calculation,
the reaction expression can be divided through by the stoichiometric coefficient of species A,
in order to arrange the reaction expression in the form,

b c d
A+ B  C+ D [2-1]
a a a

The expression has now put every quantity on a „per mole of A‟ basis.
A convenient way to quantify how far the reaction has progressed, or how many moles of
products are formed for every mole of A consumed; is to define a parameter called
conversion. The conversion XA is the number of moles of A that have reacted per mole of
A fed to the system,

moles of A reacted
XA  [2-2]
moles of A fed

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PTT 248/4 – Reactor Engineering Laboratory Module

Because the conversion is defined with respect to the basis of calculation (species A), the
subscript A can be eliminated for the sake of brevity and let X = XA .

4.3 General Mole Balance Equation

To perform a mole balance on any system, the system boundaries must first be specified.
The volume enclosed by these boundaries will be referred to as the system volume. In this
example, a mole balance will be performed on species j in a system volume, where species j
represents the particular chemical species of interest.

Fj0 Fj
Gj

Figure 2: Balance on the system volume.

A mole balance on species j at any instant in time, t, yields the following equation,

Rate of j Rate of j  Rate of j   Rate of j 

 into   out of   produced   accumulated 
    
 system   system  within system within system
       
 volume   volume   volume   volume 

in – out + generation = accumulation

dN j
Fj0 – Fj + Gj = [3-1]
dt

where Nj represents the number of moles of species j in the system at time t.

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5.0 MATERIALS AND EQUIPMENT

Figure 6: Unit construction for Batch reactor

Valves list:
Tag Location Initial position
V1 Drain valve for feed tank B1 Closed
V2 Inlet valve for pump P1 Closed
V3 By-pass valve from P1 to tank B1 Open
V4 Needle valve for liquid feed from pump P1 Closed
V5 Drain valve for feed tank B2 Closed
V6 Inlet valve for pump P2 Closed
V7 By-pass valve from P2 to tank B2 Open
V8 Needle valve for liquid feed from pump P2 Closed
Drain or sampling valve (batch reaction
V9 Closed
process)
V10 Valve for vacuum pump to jacket vessel Closed
V11 Valve for cooling water int reactor R1 Closed
V12 Drain valve for water bath tank B3 Closed
V13 Inlet valve for pump P3 Closed
V14 Hot water inlet valve Closed

6.0 PROCEDURES
6.1 Preparation of Calibration Curve for Conductivity vs. Conversion.
6.1.1 Prepare the following solutions:
a) 1 liter of sodium hydroxide (0.1 M)
b) 1 liter of sodium acetate (0.1 M)
c) 1 liter of deionised water, H2O

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PTT 248/4 – Reactor Engineering Laboratory Module

6.1.2 Determine the conductivity and NaOH concentration for each conversion value by
mixing the following solutions into 100 mL of deionised water.

0% conversion : 100 mL NaOH

25% conversion : 75 mL NaOH + 25 mL Na(Ac)
50% conversion : 50 mL NaOH + 50 mL Na(Ac)
75% conversion : 25 mL NaOH + 75 mL Na(Ac)
100% conversion : 100 mL Na(Ac)

6.1.3 Tabulate all data in the table of Appendix B4.

6.2 General Start-up Procedures

6.2.1 Fill the chemical tanks until full.
6.2.2 Fill the rear left tank with 0.1 M ethyl acetate solution and the rear right tank with
0.1 M sodium hydroxide solution.
Safety Caution : ALWAYS use the LEFT tank for the ethyl acetate solution, as
the pump for the left tank is specially designed for the chemical. Failure to do so
may result in damage to the other pump.
6.2.3 Plug in the industrial socket into a power supply and switch on the power.
6.2.4 Switch on the mains power on the control panel.
6.2.5 Switch on the agitator/mixer, and set the speed to approximately 200rpm.
6.2.6 Switch on both pumps for the chemical tanks on the control panel.
6.2.7 Before conducting experiments, ensure that the hot water valves for all tanks are
fully closed.
6.2.8 If all components are working and in order, the system is ready for use.

6.3 Experiment 1: Batch Saponification Reaction of Et(Ac) and NaOH

6.3.1 Ensure that all valves are initially closed except liquid feed needle valve of P1 and
P2.
6.3.2 Open inlet valves of P1, P2 and P3.
6.3.3 To begin a batch reaction experiment, turn on pump P1 and fully open liquid feed
needle valve of P1 to obtain highest possible flow rate into the reactor. Fill the
reactor with the NaOH to 800mL of volume. Stops pump P1.
6.3.4 Turn on pump P2 and fully open liquid feed needle valve of P2 to obtained highest
possible flow rate into the reactor. Fill the reactor with the Et(Ac) until solution
reaches a total of 1.6L. Stops pump P2.
6.3.5 Switch on the stirrer (record the conductivity reading at time, 0) and start the timer
immediately.

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PTT 248/4 – Reactor Engineering Laboratory Module

6.3.6 Record the conductivity values at 1 minute interval.

6.3.7 Stop the experiment when the conductivity values remain constant (i.e. steady
state condition).
6.3.8 Open drain valve and drain all the solution.

7.0 RESULT
7.1 Record all the results in appropriate tables.

7.2 Plot calibration curve graph. (Conductivity vs. conversion; concentration of NaOH
vs. conversion).

7.3 Plot a graph of conversion vs. time.

7.4 For an equimolar reaction with the same initial reactants‟ concentration (CA0 = CB0),
the rate law is shown to be:
dC A
 rA    kCαA
dt
 dC 
ln   A   ln k  α ln C A
 dt 

where CA is the concentration of NaOH in the reactor at time t. Plot a graph of „ln
(dCA/dt)‟ vs. „ln (CA)‟ and evaluate the slope and y-axis intercept.

7.5 Determine the order of the reaction, α and the rate constant, k from the slope and
intercept values.

8.0 DISCUSSION
8.1 Discuss the reaction rate constant and reaction order in batch reactor.

9.0 CONCLUSION
9.1 Based on the experimental procedure done and the results taken draw some
conclusions to this experiment.

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PTT 248/4 – Reactor Engineering Laboratory Module

APPENDIX A4: Physical Properties of Et(Ac) and NaOH.

Property Ethyl Acetate, Et(Ac) Sodium Hydroxide, NaOH

Formula CH3COOCH2CH3 NaOH

Appearance clear liquid white solid

Molecular weight 88.11 g/mol 40.00 g/mol

Normal boiling point 77.1°C 1390° C

Normal melting point -84.0°C 323°C

Density 0.8945 g/mL @ 25°C 2.1 g/mL

Refractive index 1.3274 @ 20°C –

APPENDIX B4: Sample Table for Preparation 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
25% 100 mL

50% 100 mL
75% 100 mL

100% 100 mL

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EXPERIMENT 6
Determination of Effect of Temperature on Reaction and Reaction’s
Activation Energy for Batch Reactor

1.0 OBJECTIVES
1.1 To observe and control the operation of a batch reactor for saponification reaction
between Sodium Hydroxide and Ethyl Acetate.
1.2 To determine the effect of temperature on the extent of conversion.
1.3 To determine the value of the reaction‟s activation energy.

2.0 CORRESPONDING COURSE OUTCOME

CO3 - Ability to analyze rate data and multiple reaction.

3.0 INTRODUCTION
In the majority of industrial chemical processes, reactor is the key equipment in which raw
materials undergo a chemical change to form desired products. The design and operation
of chemical reactors is thus crucial to the whole success of an industrial process. Reactors
can take a widely varying form, depending on the nature of the feed materials and the
products. Understanding the behavior of how reactors function is necessary for the proper
design, control and handling of a reaction system. Two main types of reactors are batch
reactor and continuous flow reactor.
The Reactor Basic Unit (Batch Reactor) has been designed for students‟ experiments on
chemical reactions in liquid phase under isothermal and adiabatic conditions. The unit
comes complete with a glass reactor, constant temperature water circulating unit,
temperature and conductivity measurements. Student shall be able to conduct the typical
saponification reaction between ethyl acetate and sodium hydroxide.

33
PTT248/4 – Reactor Engineering Laboratory Module

4.0 THEORY
4.1 Rate of Reaction and Rate Law.

The rate at which a given chemical reaction proceeds can be expressed in several ways. It
can be expressed either as the rate of disappearance of the reactants, or the rate of
formation of products. In the following reaction,

aA + bB  cC + dD [1-1]

A and B are the reactants, while C and D are the products. a,b,c,d are the stoichiometric
coefficients for the respective species.If species A is considered as the reaction basis, then
the rate of reaction can be represented by the rate of disappearance of A. It is denoted by
the symbol –rA . The numerical value of the rate of reaction, –rA is defined as the number of
moles of A reacting (disappearing) per unit time per unit volume, and has the typical unit of
mol/dm3.s. Similarly, the rate of reaction can also be represented by the rate of
disappearance of another species, such as –rB and the rate of formation of a product, such
as rC or rD . They can be related in the following equation,
 rA  rB rC rD
   [1-2]
a b c d

4.2 Conversion
Using the reaction shown in Equation [1-1], and taking species A as the basis of calculation,
the reaction expression can be divided through by the stoichiometric coefficient of species A,
in order to arrange the reaction expression in the form,

b c d
A+ B  C+ D [2-1]
a a a

The expression has now put every quantity on a „per mole of A‟ basis.
A convenient way to quantify how far the reaction has progressed, or how many moles of
products are formed for every mole of A consumed; is to define a parameter called
conversion. The conversion XA is the number of moles of A that have reacted per mole of A
fed to the system,

moles of A reacted
XA  [2-2]
moles of A fed

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PTT248/4 – Reactor Engineering Laboratory Module

Because the conversion is defined with respect to the basis of calculation (species A), the
subscript A can be eliminated for the sake of brevity and let X = XA .

4.3 General Mole Balance Equation

To perform a mole balance on any system, the system boundaries must first be specified.
The volume enclosed by these boundaries will be referred to as the system volume. In
this example, a mole balance will be performed on species j in a system volume, where
species j represents the particular chemical species of interest.

Fj0 Fj
Gj

Figure 2: Balance on the system volume.

A mole balance on species j at any instant in time, t, yields the following equation,

Rate of j Rate of j  Rate of j   Rate of j 

 into   out of   produced   accumulated 
    
 system   system  within system within system
       
 volume   volume   volume   volume 

in – out + generation = accumulation

dN j
Fj0 – Fj + Gj = [3-1]
dt

where Nj represents the number of moles of species j in the system at time t.

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PTT248/4 – Reactor Engineering Laboratory Module

5.0 MATERIALS AND EQUIPMENTS

5.1 Unit construction for Batch reactor

Figure 6: Unit construction for Batch reactor

Valves list:
Tag Location Initial position
V1 Drain valve for feed tank B1 Closed
V2 Inlet valve for pump P1 Closed
V3 By-pass valve from P1 to tank B1 Open
V4 Needle valve for liquid feed from pump P1 Closed
V5 Drain valve for feed tank B2 Closed
V6 Inlet valve for pump P2 Closed
V7 By-pass valve from P2 to tank B2 Open
V8 Needle valve for liquid feed from pump P2 Closed
V9 Drain or sampling valve (batch reaction process) Closed
V10 Valve for vacuum pump to jacket vessel Closed
V11 Valve for cooling water int reactor R1 Closed
V12 Drain valve for water bath tank B3 Closed
V13 Inlet valve for pump P3 Closed
V14 Hot water inlet valve Closed

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6.0 PROCEDURES
6.1 Preparation of Calibration Curve for Conductivity vs. Conversion.
6.1.1 Prepare the following solutions:
a) 1 liter of sodium hydroxide (0.1 M)
b) 1 liter of sodium acetate (0.1 M)
c) 1 liter of deionised water, H2O

6.1.1 Determine the conductivity and NaOH concentration for each conversion value by
mixing the following solutions into 100 mL of deionised water.

0% conversion : 100 mL NaOH

25% conversion : 75 mL NaOH + 25 mL Na(Ac)
50% conversion : 50 mL NaOH + 50 mL Na(Ac)
75% conversion : 25 mL NaOH + 75 mL Na(Ac)
100% conversion : 100 mL Na(Ac)

6.1.2 Tabulate all data in the table of Appendix B5.

6.2 General Start-up Procedures

6.2.1 Fill the chemical tanks until full.
6.2.2 Fill the rear left tank with 0.1 M ethyl acetate solution and the rear right tank with
0.1 M sodium hydroxide solution.
Safety Caution : ALWAYS use the LEFT tank for the ethyl acetate solution, as
the pump for the left tank is specially designed for the chemical. Failure to do so
may result in damage to the other pump.
6.2.3 Plug in the industrial socket into a power supply and switch on the power.
6.2.4 Switch on the mains power on the control panel.
6.2.5 Ensure that the heater is set to 30°C.
6.2.6 Switch on the agitator/mixer, and set the speed to approximately 200rpm.
6.2.7 Switch on both pumps for the chemical tanks on the control panel.
6.2.8 Before conducting experiments, ensure that the hot water valves for all tanks are
fully closed.
6.2.9 If all components are working and in order, the system is ready for use.

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PTT248/4 – Reactor Engineering Laboratory Module
6.3 Experiment : Effect of Temperature on Batch Saponification Reaction of
Et(Ac) and NaOH
6.3.1 Turn on the heater.
6.3.2 Set the setpoint of the temperature controller TIC-101 to 30 °C (or other desired
reaction temperature).
6.3.3 Set the setpoint of the temperature controller TIC-102 to about 5°C more than the
desired reaction temperature.
6.3.4 When the bath temperature is reached, open hot water inlet valve and switch on
hot water pump. Close liquid feed needle valve for P1 and P2 valves and run
pumps P1 and P2 to stir the feeds. Allow the temperatures in both feed tanks to
increase. If necessary, adjust the temperature controller setpoint in step 6.3.3
above to achieve feed temperature as near as possible to the desired reaction
temperature.
6.3.5 For different reaction temperature, adjust the setpoint of the temperature controller
in step 6.3.2 and 6.3.3 above accordingly.
6.3.6 Perform the feed pre-heating procedure above for the desired reaction
temperature.
6.3.7 To begin a batch reaction experiment, turns on pump P1 and open liquid feed
needle valve of P1 to obtain highest possible flow rate into the reactor. Fill about
800mL of the 0.1 M NaOH into the reactor. Stops pump P1 and close the liquid
feed needle valve of P1.
6.3.8 Turns on pump P2 and open liquid feed needle vale of P2 to obtained highest
possible flow rate into the reactor. Fill of the 0.1 M Et(AC) until reaction solution
reaches 1.6-L. Stops pump P2 and close the liquid feed needle valve of P2.
6.3.9 Switch on the reactor heater and the stirrer (record the conductivity reading at time,
0). Immediately start the timer.
6.3.10 Record the conductivity values at 1 minute interval.
6.3.11 Stop the experiment when the conductivity values remain constant (i.e. steady
state condition).
6.3.12 Switch off the reactor heater.
6.3.13 Open drain valve and drain all the solution from the reactor.
6.3.14 Repeat the experiment (steps 6.3.1 to 6.3.13) for different reaction temperatures of
50 and 60 °C.
6.3.15 After finish the experiment, keep the cooling water to continue flowing.
6.3.16 Switch off pumps P1, P2 and P3. Switch off the stirrer.
6.3.17 Switch off both reactor and hot water heaters. Let the liquid in the reaction vessel
to cool down to room temperature.
6.3.18 Turn off the power for the control panel.
6.3.19 Keep the solutions for subsequent experiment. Otherwise, drain all solutions.

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PTT248/4 – Reactor Engineering Laboratory Module

6.3.20 Dispose all liquids immediately after each experiment. Do not leave any solution or
waste in the tanks over a long period of time.
6.3.21 Wipe off any spillage from the unit immediately.

7.0 RESULT
7.1 Record all the results in appropriate tables.

7.2 For a second order reaction, the rate law is shown to be:
dC A
 rA    kC2A
dt
CA dC A t
CA0 C 2A  k 0 dt
1 1
 kt 
CA C A0

where CA0 is the initial concentration of reactant NaOH in the reactor. For each
temperature value, plot the graph of „1/CA‟ vs. time, t and evaluate the slope and y-
axis intercept.

7.3 Determine the rate constant, k from the slope value for different temperature
values. Examine the change in the rate constant.

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

7.5 Calculate the saponification reaction‟s activation energy, E and Arrhenius constant,
A from the slope and intercept values using the Arrhenius equation.

E
k (T )  Ae E / RT or ln k  ln A  (1 / T )
R

where E = activation energy [J/mol]

A = Arrhenius constant
R = universal gas constant = 8.314 J/mol.K
T = absolute temperature [K]

8.0 DISCUSSION
8.1 Discuss the effect of temperature on reaction and reaction‟s activation energy for
batch reactor.

9.0 CONCLUSION
9.1 Based on the experimental procedure done and the results taken draw some
conclusions to this experiment.

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PTT248/4 – Reactor Engineering Laboratory Module

APPENDIX A5: Physical Properties of Et(Ac) and NaOH.

Property Ethyl Acetate, Et(Ac) Sodium Hydroxide, NaOH

Formula CH3COOCH2CH3 NaOH

Appearance clear liquid white solid

Molecular weight 88.11 g/mol 40.00 g/mol

Normal boiling point 77.1°C 1390° C

Normal melting point -84.0°C 323°C

Density 0.8945 g/mL @ 25°C 2.1 g/mL

Refractive index 1.3274 @ 20°C –

APPENDIX B5: Sample Table for Preparation of Calibration Curve

Solution Mixtures
Concentration Conductivity
Conversion 0.1 M 0.1 M
H2O of NaOH (M) (mS/cm)
NaOH Na(Ac)
0% 100 mL
25% 100 mL

50% 100 mL

75% 100 mL

100% 100 mL

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PTT248/4 – Reactor Engineering Laboratory Module
EXPERIMENT 7
Determination of Stirring, Flow Rate and Temperature Effects On
Conversion in Series of Continuous Stirred Tank Reactor (CSTRs)

1.0 OBJECTIVES
1.1 To observe and control the operation of a continuous-stirred tank reactor in
series.
1.2 To determine the conversion in each of the reactors after the delay section.
1.3 To determine the effects of stirring, flow rate and temperature on conversion in a
series of CSTRs.

2.0 CORRESPONDING COURSE OUTCOME

CO2 - Ability to analyze rate law and isothermal reactor design.

3.0 INTRODUCTION
The continuous-stirred tank reactor (CSTR) is a type of continuous flow reactor commonly
used in industrial processing. The continuous-stirred tank reactor (CSTR) in series has
been designed to introduce students on the dynamic behavior of reactors in series. The
unit is based on the simplest classic case of a well mixed, multi-staged process operation
that basically consists of three reactors connected in series by piping. The solution in each
reactor is well stirred and the concentration can be measured. Sump tanks, feed pumps
and instrumentations are also provided with the unit.

4.0 THEORY

4.1 CONTINUOUS-STIRRED TANK REACTOR

As with all continuous flow reactors, CSTRs are almost always operated at steady state. In
addition, the contents inside the reactor are assumed to be perfectly mixed. As a result,
there is no time or position dependence of the temperature, concentration or reaction rate
inside the CSTR. Therefore, all variables are the same at any point within the reaction
vessel.

From the general mole balance equation,

Eq. (1)

So, the design equations for the continuous-stirred tank reactor.

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PTT248/4 – Reactor Engineering Laboratory Module

Eq. (2)

Figure 1: Mole balance on a CSTR

4.2 CONVERSION IN CONTINUOUS-STIRRED TANK REACTORS

In chemical reactions, it is often that one of the reagents deplete before the others. When
this occurs, the reaction ceases, and thus this reagent is termed the limiting reagent. In
most instances, it is best to choose the limiting reagent as the basis of stoichiometric
calculations. Consider a general reaction

Eq. (3)

where the uppercase letters represent chemical species and the lowercase letters
represent stoichiometric coefficients (moles). Suppose that species A were to be the
limiting reagent, we then divide the reaction expression by the coefficient of species A, to
obtain

Eq. (4)

Now that the other chemical species are on a “per mole of A” basis, we would then want to
know how far the reaction proceeds to the right, or how many moles of A are consumed to
form one mole of C. These can be determined by defining a parameter called conversion.
The conversion of chemical species A is simply the number of moles of A that have
reacted per mole of A fed into the system.

Eq (5)
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4.3 SAPONIFICATION OF ETHERS WITH SODIUM HYDROXIDE

Now that we understand the basic chemistry and chemical engineering involved in
chemical reactors, consider a chemical reaction between an ether and sodium hydroxide.
This process is also known as saponification. The reaction is reversible, and is described
by

The acetic ether (ethyl acetate) molecules split into acetate ions and ethanol molecules,
consuming hydroxide ions provided by the sodium hydroxide in the process. The progress
of the reaction can thus be tracked accurately by the change in hydroxide ions. This can
be observed by the conductivity change in the reactor vessel, since the presence of
hydroxide ions increase the conductivity in a solution.

5.0 MATERIALS AND EQUIPMENTS

5.1 DESCRIPTION OF APPARATUS

The Continuous-Stirred Tank Reactor in Series is used for demonstrating the basics of
chemical processing. The apparatus is comprised of a stainless steel top to accommodate
2 feed tanks, a workspace to mount the chemical reactor, a cooling/heating water
reservoir, dosing pumps and a process control console. The stainless steel base of the
console is fitted with 2 peristaltic pumps with speed controls for feeding the reactants while
the control console is fitted with a temperature control, conductivity meter and one stirrer
control unit. Two reactant tanks are provided with heating coils to bring reactants to
reaction temperatures before being dosed into a joint into the continuous stirred reactor.

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Figure 2: Unit construction for CSTR in series

A - Mains power switch B - Conductivity & temperature meters

C - Hot water pump D - Hot water tank
E - Ethyl acetate dosing tank F - Sodium hydroxide dosing tank
G - Reactor vessels H - Dosing pumps

6.0 PROCEDURES

6.1 Preparation of Calibration Curve for Conductivity vs. Conversion.

6.1.1 Prepare the following solutions:
a) 1 liter of sodium hydroxide (1.15%)
b) 1 liter of sodium acetate (2.4%)
c) 1 liter of deionised water, H2O

6.1.2 Determine the conductivity and NaOH concentration for each conversion value by
mixing the following solutions into 100 mL of deionised water.
0% conversion : 100 mL NaOH
25% conversion : 75 mL NaOH + 25 mL Na(Ac)
50% conversion : 50 mL NaOH + 50 mL Na(Ac)
75% conversion : 25 mL NaOH + 75 mL Na(Ac)
100% conversion : 100 mL Na(Ac)

6.1.3 Tabulate all data in the table of Appendix B6.

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6.2 Setup
6.2.1 Fill the hot water tank until 70% full.
6.2.2 Remove the flanges from the dosing tanks by unfastening the quick coupling
connections.
6.2.3 Fill the rear left tank with 2.5% ethyl acetate solution and the rear right tank with
1.15% sodium hydroxide solution. ALWAYS use the LEFT tank for the ethyl
acetate solution, as the pump for the left tank is specially designed for the
chemical. Failure to do so may result in damage to the other pump.
6.2.4 Reattach the flanges to the dosing tanks.
6.2.5 Before conducting experiments, ensure all valves are in correct configuration.

6.3 Experiment 1 : To determine the effects of stirring on conversion in a

series of CSTRs.
6.3.1 Switch on the mains power on the unit.
6.3.2 Set the pump speeds to 40%.Begin the experiment by switching on the dosing
pumps.
6.3.3 Then, for the first reactor, allow the chemicals to immerse the stirrer, then switch on
the stirrer and set the speed to approximately 300rpm (low speed).
6.3.4 Repeat step 6.3.3 for the 2 other reactors.
6.3.5 Once the chemicals pass the delay section and the conductivity and temperature
readings reach steady values, note down the readings.
6.3.6 Now, change the speed of all stirrers to high speed setting to 100 rpm.
6.3.7 Wait for approximately 15 minutes, and then take down the conductivity and
temperature readings.
6.3.8 Switch off the dosing tank pumps and stirrer motor after the experiment.
6.3.9 Compare the difference in conversion of reactants with and without the effects of
stirring.

6.4 Experiment 2 : To determine the effects of temperature on conversion

in a series of CSTRs.
6.4.1 Ensure that the heater is set to 45°C.
6.4.2 Switched on the hot water pump.
6.4.3 Wait until the water in the hot water tank and the chemical tanks reached 45°C.
6.4.4 Set the pump speeds to 40% and switch on the dosing pumps.

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6.4.5 For the first reactor, allow the chemicals to immerse the stirrer, then switch on the
stirrer and set the speed to approximately 100rpm (low speed).
6.4.6 Repeat step 6.4.4 for the 2 other reactors.
6.4.7 Once the chemicals pass the delay section and the conductivity and temperature
readings reach steady values, note down the readings.
6.4.8 Switch off the dosing tank pumps, stirrer motor, heater and hot water pump after
the experiment.
6.4.9 Switch off the mains power and power supply.
6.4.10 Drain chemicals in the reactor vessels and the waste tank.

7.0 RESULT
7.1 Record all the results in the table (Appendix B3) for every reading taken by
conductivity and temperature meter.
7.2 Plot a graph of conductivity vs. conversion for calibration curve.
7.3 Plot a graph of conversion vs. tank no. for different stirring speeds.
7.4 Plot a graph of conversion vs. tank no. for different temperatures.
7.5 Plot a graph of -dCA/dt vs. time

8.0 DISCUSSION
8.1 Discuss the effect of stirring speed on reaction and reaction rate.
8.2 Discuss the effect of temperature on reaction and reaction rate.

9.0 CONCLUSION
9.1 Based on the experimental procedure done and the results taken draw some
conclusions to this experiment.

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APPENDIX A6: Physical Properties of Et(Ac) and NaOH.

Property Ethyl Acetate, Et(Ac) Sodium Hydroxide, NaOH

Formula CH3COOCH2CH3 NaOH

Appearance clear liquid white solid

Molecular weight 88.11 g/mol 40.00 g/mol

Normal boiling point 77.1°C 1390° C

Normal melting point -84.0°C 323°C

Density 0.8945 g/mL @ 25°C 2.1 g/mL

Refractive index 1.3274 @ 20°C –

APPENDIX B6: Sample Table for Preparation of Calibration Curve

Solution Mixtures
Concentration Conductivity
Conversion 0.1 M 0.1 M
H2O of NaOH (M) (mS/cm)
NaOH Na(Ac)
0% 100 mL
25% 100 mL
50% 100 mL

75% 100 mL

100% 100 mL

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REFERENCES

1. Operations and Experimental Manual, Chemical and Process Engineering, Lotus

Scientific (M) Sdn. Bhd.
2. H.Scott Fogler. Elements of Chemical Reaction Engineering, 4 th ed., Prentice Hall
Inc. 2006.
3. Levenspiel, O., Chemical Reaction Engineering,John-Wiley, 3rd edition, 2001.
4. Davis, M.E, Davis, R.J. Fundamentals of Chemical Reaction Engineering,1st
edition,Mc Graw Hilll, 2002.
5. Smith J.M., “Chemical Engineering Kinetics”, McGraw Hill (Singapore), 1981.
Astarita G., “Mass Transfer with Chemical Reaction”, Elsevier, 1967.

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