SOLTEQ® LIQUID PHASED STIRRED TANK REACTOR (Model: BP 100)

1.0 INTRODUCTION

The SOLTEQ® Liquid Phased Stirred Tank Reactor (Model:

BP 100) has been designed for students’ experiments on
chemical reactions in liquid phase under isothermal condition.
The unit comes complete with a glass reactor, vapor condensor,
individual reactant feed tanks and pumps, temperature sensor
and conductivity measuring sensors. The reactor will enable
students to conduct the typical saponification reaction between
ethyl acetate and sodium hydroxide among other types of
reaction. Figure 1 illustrates the process flow diagram for the
continuous stirred tank reactor unit.

In the majority of industrial chemical processes, the 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 behaviour of how reactors function is
necessary for the proper control and handling of a reaction
system. Basically, there are two main groups of reactors, batch
reactors and continuous flow reactors.

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SOLTEQ® LIQUID PHASED STIRRED TANK REACTOR (Model: BP 100)

Condens
er
Stirrer

Adjustable Control
Overflow Panel
Tube
Reactor

Peristaltic Pump

Waste
Tank

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SOLTEQ® LIQUID PHASED STIRRED TANK REACTOR (Model: BP 100)

Figure 1: Process flow diagram for the continuous stirred tank reactor unit.

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SOLTEQ® LIQUID PHASED STIRRED TANK REACTOR (Model: BP 100)

2.0 GENERAL DESCRIPTION

2.1 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.

1. Reactor (R1)
4-L vessel made of borosilicate glass
(OD:150mm, ID:140mm, Length: 250mm)
Internal cooling coil
Cartridge type heater (1.5 kW)
Stainless steel impeller
Ports for:
Stirrer (M1)
Inlet for feed vessels (B1, B2)
Condenser (W2)
Sensors: conductivity (QT101) and temperature
(TIC101)
Cartridge heater (W1)
Cooling coil

2. Stirrer (M1)
Laboratory drive with LCD display
Power: 230VAC / 50-60 Hz / 75 W
Speed range: 80 – 2000 rpm, steplessly adjustable by
hand
Max torque: 30 Ncm

3. Feed tanks (B1, B2)

30-L cylindrical tank made of stainless steel

4. Waste tank (B3)

60-L rectangular tank made of stainless steel

5. Condenser (W2)
Coil heat exchanger made of stainless steel
Exchange area: 0.03 m2

6. Pumps (P1, P2)

Peristaltic Pump
Tubing size: #17
Max delivery rate: 800 ml/min
Power: 230VAC / 50 Hz

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SOLTEQ® LIQUID PHASED STIRRED TANK REACTOR (Model: BP 100)

7. Instrumentation
Temperature measurement and control (TIC101)
Conductivity measurement (QT101)

Please refer to the manufacturer’s manual for further

details on the component specifications, installation and
operation, safety requirements and servicing.

2.2 Valves List

Valves list:
Initial
Tag Description
position
V1 Drain valve for feed tank B1 Close
Inlet valve to reactor R1 from pump
V2 Close
P1
V3 Drain valve for feed tank B2 Close
Inlet valve to reactor R1 from pump
V4 Close
P2
Cooling water inlet to condenser
V5 Close
W2
V6 Vent valve for reactor R1 Open
V7 Drain valve for sampling Close
V8 Drain valve to waste tank B3 Close
V9 Drain valve from waste tank B3 Close
Control valve for water supply to
V10 Close
feed tank B2
Control valve for water supply to
V11 Close
feed tank B1
V12 Vent valve for condenser W2 Open

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SOLTEQ® LIQUID PHASED STIRRED TANK REACTOR (Model: BP 100)

2.3 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 affect 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. Only a properly trained staff shall be allowed to carry
out any servicing. Manufacturer's manual must always
be observed.
11. Before any servicing, shut down the whole operation
and let the system to cool down and be properly
ventilated.
12. Do not use any coarse or abrasive cleaners on glass
components.
13. Leaking couplings or fittings should be carefully
retightened. Replace any gaskets or seals if necessary.
14. Please fill the reactor with water before switch on the
heater.

2.4 Maintenance

1. After each experiment, drain off any liquids from the

reactor and make sure that the reactor and tubings are
cleaned properly. Flush the system with de-ionized water
until no traces of salt are detected.
2. Dispose all liquids immediately after each experiment.
Do not leave any solution or waste in the tanks over a
long period of time.

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SOLTEQ® LIQUID PHASED STIRRED TANK REACTOR (Model: BP 100)

3. Wipe off any spillage from the unit immediately.

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SOLTEQ® LIQUID PHASED STIRRED TANK REACTOR (Model: BP 100)

3.0 SUMMARY OF THEORY

3.1 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)

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, –r A 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,

−r A −r B r C r D
= = =
a b c d (2)

The chemical reaction rate is an intensive quantity and

depends on temperature and concentration. The reaction
rate equation (or the rate law) is essentially an algebraic
equation involving concentration.One of the most common
general forms of the rate law equation is shown to be,

−r A = k A C αA C βB (3)

where CA and CB are the individual reactants’

concentrations, each raised to the powers α and β ,
while kA is the reaction rate constant.

The order of a reaction refers to the powers to which the

concentrations are raised in the reaction rate law. In
Equation (3), the reaction is α order with respect to

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SOLTEQ® LIQUID PHASED STIRRED TANK REACTOR (Model: BP 100)

reactant A, and β order with respect to reactant B. The

overall order of the reaction, n is,

n=α+β (4)
3.2 Conversion

Using the reaction shown in Equation (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+ a B  a C+ a D (5)

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 =
moles of A fed (6)

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 .

3.3 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

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SOLTEQ® LIQUID PHASED STIRRED TANK REACTOR (Model: BP 100)

Figure 2: Balance on the system volume.

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

the following equation,
R a t e o f flo w
o f j in to
s y s tem
v o lu m e
¿
r ig h
¿
¿
¿
[ ] −
¿
R a t e o f flo w
o f j o u t o f
s y s tem
v o lu m e
¿
r ig h
¿
¿
¿
[ ] +
¿
R a t e o f g e n e ra tio n o f j
b y c he mi c a l re a c tio n
w i th in s y s te m
v o lu m e
¿
r ig h
¿
¿
¿
R a t e o f j
a c c u m u la te d
w i th in s y s te m
v o lu m e
¿
r ig h
¿
[ ¿ ] [ ¿ ] [ ¿ ] ¿
¿
¿

in – out + generation =accumulation

dN j
Fj0 – Fj + Gj = dt (7)

where Nj represents the number of moles of species j in the

system at time t. If all the system variables (e.g.
temperature and concentration) are spatially uniform
throughout the system volume, the rate of generation of
species j, Gj , is just the product of the reaction volume, V
and the rate of formation of species j, rj ,

Gj = r j V (8)

Suppose that the rate of formation of species j for the

reaction varies with the position in the system volume, the
total rate of generation within the system volume is the
integral of all the rates of generation in each of the
subvolumes,

Then
V
Gj = ∫ r j dV
(9)

Therefore, the general mole balance equation for any

chemical species j that is entering, leaving, reacting and/or
accumulating within any system volume V, is,

V dN j
F j0 −F j +∫ r j dV =
dt (10)

From this general mole balance equation, the design

equations for various types of industrial reactors such as
batch, semibatch and continuous flow reactors can be
developed. Upon evaluation of these design equations, the
time (batch) or reactor volume (continuous) necessary to

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SOLTEQ® LIQUID PHASED STIRRED TANK REACTOR (Model: BP 100)

convert a specified amount of reactants to products can

then be determined.

3.4 Continuous Stirred Tank Reactors

A type of reactor used very commonly in industrial

processing is a stirred tank operated continuously. It is
referred to as the continuous stirred tank reactor
(CSTR). The CSTR is normally run at steady state and is
usually operated so as to be quite well mixed. As a result of
mixing, the CSTR is generally modeled as having no spatial
variations in concentration, temperature, or reaction rate
throughout the vessel. Since the temperature and
concentration are identical everywhere within the reaction
vessel, they are the same at the exit point as they are
elsewhere in the tank. Thus, the temperature and
concentration in the exit stream are modeled as being the
same as those inside the reactor.

FA0
CA0
vo

–rA = (–rA)exit FA
CA
v

Figure 3: Continuous stirred tank reactor (CSTR).

When the general mole balance is applied to species A in a

CSTR operated at steady state (i.e. conditions do not
change with time), in which there are no spatial variations
in the rate of reaction, the resulting equation is,

dN A
= 0
dt
V
∫ r A dV = Vr A
F Ao −F A +Vr A = 0 (11)

The familiar form known as the design equation for a

CSTR is obtained,

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SOLTEQ® LIQUID PHASED STIRRED TANK REACTOR (Model: BP 100)

F A 0 −F A
V =
−r A (12)

Normally, conversion increases with the time the reactants

spend in the reactor. For continuous flow systems, this time
usually increases with increasing reactor volume.
Consequently, the conversion X is a function of reactor
volume V.

If FA0 is the molar flow rate of species A fed to a system

operated at steady state, the molar flow rate at which
species A is reacting within the entire system will be [FA0 X].
The molar feed rate of A to the system minus the rate of
reaction of A within the system equals the molar flow rate
of A leaving the system, FA . This is shown in mathematical
form as,

F A = F A 0 −F A 0 X = F A 0 (1−X ) (13)

The entering molar flow rate FA0 is just the product of the
entering concentration
C A0 and the entering volumetric
flow rate,
v0 ,

FA 0 = C A 0 v0 (14)

Combining Equation (13) and Equation (12) yields the

design equation with a conversion term for the CSTR,

F A 0 X = −r A V
FA 0 X
V =
(−r A )exit (15)

Since the exit composition from the reactor is identical to

the composition inside the reactor, the rate of reaction is
evaluated at the exit condition.

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SOLTEQ® LIQUID PHASED STIRRED TANK REACTOR (Model: BP 100)

4.0 OPERATING PROCEDURES

4.1 General Start-Up Procedures

1. Ensure the water supply is connected to the deionizer

(blue filter at the bottom of the equipment).
2. Ensure all valves are initially closed except V6 & V12.
3. Open V10 and V11. Allow the water supply to fill up half
of the tank B1 and B2 with deionized water. Temporary
shut off the water supply.
4. Prepare the following chemicals:
a) Dissolve 100g of NaOH pellets with 1L deionized
water
b) Prepare 247ml of Ethyl acetate.
c) 1 liter of hydrochloric acid, HCl (0.25 M), for
quenching
5. Pour the NaOH solution into tank B1 and ethyl acetate
into tank B2. Fill up both tanks with the water supply up
to the top of the yellow mark which is about 25L. Note
that 100g of NaOH in 25L of water is 0.1M and 247ml of
Ethyl acetate in 25L of water is also 0.1M.
6. Turn on the power for the control panel.
7. Adjust the overflow tube to give the desired working
volume, which is about 3L in the reactor R1.
8. Open valves V2 and V4.
9. The unit is now ready for experiment.

4.2 General Shut-Down Procedures

1. Keep the cooling water cooling water continue flowing

into the reactor, by opening valve V5.
2. Switch off both pumps P1 and P2. Switch off the stirrer
M1.
3. Switch off the heater. Let the liquid in the reaction
vessel R1 to cool down to room temperature.
4. Close the cooling water supply, by closing the valve V5.
5. Turn off the power for the control panel.
6. Open valves V1 and V3 to drain all solutions from feed
tanks B1 and B2. Otherwise, keep the solutions for
subsequent experiment.
7. Open valves V8 to drain any liquid from the reactor R1
into waste tank B3. Open valve V9 to drain all solutions
from waste tank B3.

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SOLTEQ® LIQUID PHASED STIRRED TANK REACTOR (Model: BP 100)

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SOLTEQ® LIQUID PHASED STIRRED TANK REACTOR (Model: BP 100)

5.0 EXPERIMENTAL PROCEDURES

5.1 Preparation of Calibration Curve for Conversion vs.

Conductivity

The reaction to be studied is the saponification reaction of

ethyl acetate, Et(Ac) and sodium hydroxide, NaOH. Since
this is a second order reaction, the rate of reaction depends
on both concentrations of Et(Ac) and NaOH. However, for
analysis purposes, the reaction will be carried out using
equimolar feeds of Et(Ac) and NaOH solutions with the
same initial concentrations. This ensures that both
concentrations are similar throughout the reaction.

NaOH + Et(Ac)  Na(Ac) + EtOH

The following procedures will calibrate the conductivity

measurements of conversion values for the reaction
between 0.1 M ethyl acetate and 0.1 M sodium hydroxide:

PROCEDURES:
1. Prepare the following solutions:
a) 1 liter of sodium hydroxide, NaOH (0.1 M). (1 liter of
(0.1M) sodium hydroxide contains 4g of sodium
hydroxide)
b) 1 liter of sodium acetate, Na(Ac) (0.1 M). (1 liter of
(0.1M) of sodium acetate contains 8.2g of sodium
acetate)
c) 1 liter of deionised water, H2O
2. Determine the conductivity and NaOH concentration for
each conversion values by mixing the following solutions
into 100 ml of deionised water:
a) 0% conversion : 100 ml NaOH
b) 10% conversion : 90 ml NaOH + 10 ml Na(Ac)
c) 20% conversion : 80 ml NaOH + 20 ml Na(Ac)
d) 30% conversion : 70 ml NaOH + 30 ml Na(Ac)
e) 40% conversion : 60 ml NaOH + 40 ml Na(Ac)
f) 50% conversion : 50 ml NaOH + 50 ml Na(Ac)
g) 60% conversion : 40 ml NaOH + 60 ml Na(Ac)
h) 70% conversion : 30 ml NaOH + 70 ml Na(Ac)
i) 80% conversion : 20 ml NaOH + 80 ml Na(Ac)
j) 90% conversion : 10 ml NaOH + 90 ml Na(Ac)
k) 100% conversion : 100 ml Na(Ac)

ANALYSIS AND DISCUSSION:

1. Record all data in the sample table in Appendix A.

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SOLTEQ® LIQUID PHASED STIRRED TANK REACTOR (Model: BP 100)

2. Plot the calibration curve of conductivity vs conversion.

Determine the slope and y-axis intercept.

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SOLTEQ® LIQUID PHASED STIRRED TANK REACTOR (Model: BP 100)

5.2 Back Titration Procedures for Manual Conversion

Determination

It is recommended to carry out manual conversion

determination on experiment samples to verify the
conductivity measurement values. The following
procedures will explain the method to carry out back
titration on the samples. It is based on the principle of
quenching the sample with excess acid to stop any further
reactions, then back titrating with a base to determine the
amount of unreacted acid.

PROCEDURES:
1. Fill up a burette with 0.1 M NaOH solution.
2. Measure 10 ml of 0.25 M HCl in a flask.
3. Obtain a 50 ml sample from the experiment and
immediately add the sample to the HCl in the flask to
quench the saponification reaction.
4. Add a few drops of pH indicator into the mixture.
5. Titrate the mixture with NaOH solution from the burette
until the mixture is neutralized. Record the amount of
NaOH titrated.

ANALYSIS AND DISCUSSION:

NaOH + HCl  NaCl + H2O

Unknown quantity:
Concentration of NaOH in the reactor = CNaOH
mol/L

Known quantities:
Volume of sample = Vs ml
Concentration of NaOH in the feed vessel =
CNaOH,f mol/L
Volume of HCl for quenching = VHCl,s ml
Concentration of HCl in standard solution =
CHCl,s mol/L
Volume of titrated NaOH = V1 ml
Concentration of NaOH used for titration =
CNaOH,s mol/L

Calculations:
Conc. of NaOH entering the reactor, CNaOH,0 =
(CNaOH,f)/2 mol/L

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SOLTEQ® LIQUID PHASED STIRRED TANK REACTOR (Model: BP 100)

Volume of unreacted quenching HCl, V2 =

C NaOH,s
C HCl,s× V1 ml
Vol. of HCl reacted with NaOH in sample, V3 =
VHCl,s – V2 ml
Moles of HCl reacted with NaOH in sample, n1 =
CHCl,s × V3 mol
Moles of unreacted NaOH in sample, n2 =
n1 mol
Conc. of unreacted NaOH in the reactor, CNaOH =
n2 / (Vs × 1000) mol/L
Conversion of NaOH in the reactor, X = ( 1 –
C NaOH
C NaOH,0 ) × 100%

5.3 EXPERIMENT 1: Effect of Residence Time on the

Reaction in a CSTR

OBJECTIVE:
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 as in Section
4.1.
2. Switch on both pumps P1 and P2 simultaneously and
open valves V2 and V4 to obtain the highest possible
flow rate into the reactor. Both pump speed can be set
at 200 rpm.
3. 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 ¾ reactor height, which is
about 195mm on the scale for 3L working volume.
Record the volume of the solution.
4. Adjust knob on the peristaltic pump P1 and P2 to give a
flow rate of about 0.10 l/min (refer calibration curve of
pump), which is about 30 rpm for both pumps. Make
sure that both flow rates are the same. Record the flow
rates.
5. Switch on the stirrer M1 and set the speed to about 200
rpm.

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SOLTEQ® LIQUID PHASED STIRRED TANK REACTOR (Model: BP 100)

6. Start monitoring the conductivity value at QT101 until it

does not change over time. This is to ensure that the
reactor has reached steady state.
7. Record the steady state conductivity value and find the
concentration of NaOH in the reactor and extent of
conversion from the calibration curve.
8. Repeat the experiment (step 4 to 7) for different
residence times by adjusting the feed flow rates of
NaOH and Et(Ac) to 0.15, 0.20, 0.25 and 0.30 l/min.
Make sure that both feed flow rates are the same.

ANALYSIS AND DISCUSSION:

1. Use the sample table in Appendix B for data collection.
2. Plot a graph of conversion vs. residence time. The
reactor’s residence time is defined as the reactor
volume divided by the total feed flow rates, v0.
V CSTR
τ =
Residence time, v0

3. For a second order equimolar reaction with the same

initial reactants’ concentration (
C A 0=C B 0 ), the rate law
is shown to be:
2
−r A = kC A C B = kC A
F A0 X
V CSTR =
−r A
F A0 X v 0 (C A 0 −C A )
V CSTR = 2
= 2
kC A kC A

where: X = extent of conversion

CA = exit concentration of reactant NaOH (M)
v0 = total inlet flow rate of solutions (ml/min)
C A0
= inlet concentration of reactant NaOH in
the reactor (M)

For different reactor residence times, calculate the value

of the reaction rate constant, k and the rate of reaction,
-rA.
(C A 0 −C A )
k = 2
Reaction rate constant, τC A

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SOLTEQ® LIQUID PHASED STIRRED TANK REACTOR (Model: BP 100)

Rate of reaction, −r A = kC 2A

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SOLTEQ® LIQUID PHASED STIRRED TANK REACTOR (Model: BP 100)

5.4 EXPERIMENT 2: Effect of Temperature on the

Reaction in a CSTR

OBJECTIVE:
To determine the effect of temperature on the extent of
conversion.
To determine the value of the reaction’s activation energy.

PROCEDURES:
1. Perform the general start-up procedures as in Section
4.1.
2. Switch on both pumps P1 and P2 simultaneously and
open valves V2 and V4 to obtain the highest possible
flow rate into the reactor. Both pump speed can be set
at 200 rpm.
3. 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 ¾ reactor height, which is
about 195mm on the scale for 3L working volume.
Record the volume of the solution.
4. Adjust knob on the peristaltic pump P1 and P2 to give a
flow rate of about 0.10 l/min (refer calibration curve of
pump), which is about 30 rpm for both pumps. Make
sure that both flow rates are the same. Record the flow
rates.
5. Switch on the stirrer M1 and set the speed at about 200
rpm.
6. Switch on the heater on the control panel. Set the
temperature setpoint on the TIC01 to 40 °C. Allow the
liquid temperature to rise to the setpoint and remains
constant.
WARNING: ONLY TURN ON THE HEATER WHEN IT IS
FULLY SUBMERGED IN WATER.
7. Start monitoring the conductivity value at QT101 until it
doesn’t change over time. This is to ensure that the
reactor has reached steady state.
8. Record the steady state conductivity and temperature
values and find the concentration of NaOH in the reactor
and extent of conversion from the calibration curve.
9. Repeat the experiment (steps 6 to 8) for different
reactor temperatures by setting the temperature
setpoint to 45 and 50 °C. Make sure that the flow rates
of both solutions are maintained at 0.1 l/min.

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SOLTEQ® LIQUID PHASED STIRRED TANK REACTOR (Model: BP 100)

ANALYSIS AND DISCUSSION:

1. Use the sample table in Appendix B for data collection.
2. Plot a graph of conversion, X vs. reaction temperature,
T.
3. For different reaction temperatures, calculate the
reaction rate constant, k.
(C A 0 −C A )
k = 2
Reaction rate constant, τC A

Plot the graph of ‘ln k’ vs ‘1/T’ and evaluate the slope

and y-axis intercept.
Calculate the activation energy, E and Arrhenius
constant, A from the slope and intercept values using
the Arrhenius equation:
E
− E/ RT ln k = ln A− (1/T )
k(T ) = Ae or R
where E = activation energy [J/mol]
A = Arrhenius constant
R = universal gas constant = 8.314 J/mol.K
T = absolute temperature [K]

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SOLTEQ® LIQUID PHASED STIRRED TANK REACTOR (Model: BP 100)

6.0 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.
4. Astarita G., “Mass Transfer with Chemical Reaction”, Elsevier,
1967.

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