BATCH LIQUID REACTOR

BATCH LIQUID
REACTOR

BATCH LIQUID REACTOR

1.0

INTRODUCTION
In the majority of industrial chemical processes, a reactor is the key item of equipment in
which raw materials undergo a chemical change to form desired products. The unit comes
complete with a glass reactor, constant temperature water circulating unit, temperature and
conductivity monitoring systems, and Data Acquisition System. Student shall be able to
conduct the well-known saponification reaction between ethyl acetate and sodium
hydroxide.
Objectives:

2.0

To prepare the calibration curve for conversion vs. conductivity

To study the batch saponification reaction of Ethyl Acetate and Sodium
Hydroxide

SUMMARY OF THEORY
BATCH STIRRED-TANK REACTOR (BSTR)
In batch reactions, there are no feed or exit streams and therefore the equation is simplified
into:
Rate of A
Rate of A
produced

accumulate d
within volume
within volume

element
element

(1)

The rate of reaction of component A is defined as:

rA

1 dN A

V dt by reaction

moles of A which
appear by reaction

unit unit
volume time

(2)

By this definition, if A is a reaction product, the rate is positive; whereas if it is a reactant

which is consumed, the rate is negative.
Rearranging equation (2),

-rA V
3.0

N A0

dX A
dt

METHODOLOGY
The unit consists of the followings:

(3)

BATCH LIQUID REACTOR

a)

Reactor
The reactor consists of a glass vessel with top and bottom plate made of stainless
steel. The reactor is vacuum insulated by an outer glass jacket. The reactor comes
with a cooling coil, a 1.0 kW heater, a temperature sensor and stirrer system.

b)

Feed Inlet System (Liquid Reactions)

For each liquid reactant, a 20-L feed tank, a pump, a needle valve and a flow
meter are provided. Each reactant is pumped from the feed tank to the appropriate
inlet port at the reactor top plate.

c)

Water Bath
The water bath system consists of a 25-L tank, 2x2.0kW cartridge heaters,
temperature sensor and controller, and a circulation pump.

d)

Product/ Waste Tank

A 50-L rectangular tank made of stainless steel is provided for collecting the
product or waste before being discharged.

e)

Control Panel
The control panel consists of all the necessary electrical components for
controlling the operations of the unit. Components mounted on the panel door are
all labeled for convenience. The control panel also houses the necessary modules
for data acquisition system.

f)

Data Acquisition System

The Data Acquisition System consists of a personal computer, ADC modules and
instrumentations for measuring the process parameters. A flowmeter with 0 to 5
VDC output signal is supplied for each feed stream. A temperature sensor and
temperature transmitter with 4 to 20 mA output signal are provided to measure the
reaction temperature. A conductivity sensor with controller are provided for
monitoring the reaction conversion. All analog signals from the sensors will be
converted by the ADC modules into digital signals before being sent to the
personal computer for display and manipulation. Figure 1 shows the process
diagram for Batch Liquid Reactor.

BATCH LIQUID REACTOR

BATCH LIQUID REACTOR

EXPERIMENTAL PROCEDURES
By studying the saponification reaction of ethyl acetate and sodium hydroxide to form
sodium acetate in a batch reactor, evaluate the rate data needed to design a production
scale reactor.
A process flow diagram of the reactor is shown in Figure 1. This reactor has a total volume
of approximately 3 litres. A scale is provided to determine the reactor volume.
a)

Preparation of the calibration curve for Conversion vs. Conductivity:

1.

2.
b)

Prepare the following solutions and determine the conductivity values for
each of them.
Conversion
[%]

Solutions

0.00

1-L of 0.05M NaOH

0.25

1-L of 0.075M NaOH + 1-L of 0.025M Sodium Acetate

0.50

1-L of 0.05M NaOH + 1-L of 0.05M Sodium Acetate

0.75

1-L of 0.025M NaOH + 1-L of 0.075M Sodium Acetate

1.00

1-L of 0.05M Sodium Acetate

Conductivity
[mS/cm]

Determine the slope and y-axis intercept from the plot of conversion vs.
conductivity.

Reactants Preparation
1.

Prepare 1 litre of 0.25 M standard HCl and 1 litre of 0.1 M standard NaOH.

2.

Prepare 0.1 M NaOH solution in feed tank T1 and 0.1 M Ethyl acetate in
feed tank T2.

3.

Confirm the concentration of your 0.1 M NaOH solution by titrating a small

amount of it with standard 0.25 M HCl using phenolphthalein as indicator.

4.

Ensure the concentration of the ethyl acetate solution using the following
procedure:
First, add 0.1 M NaOH solution to a sample of ethyl acetate solution such
that the 0.1 M NaOH solution is in excess to ensure all of the ethyl acetate
reacted. Let this mixture react overnight. On the following day, determine
the amount of unreacted NaOH by direct titration with standard 0.25 M
HCl. Record the ethyl acetate real concentration.

Note: All the experiments should be repeated at least twice to ensure reproducibility.

BATCH LIQUID REACTOR

Experiment A: Batch Saponification Reaction of Ethyl Acetate and Sodium Hydroxide

Procedure:
1.

To begin a batch reaction experiment, switch on pump P2 and start

pumping 1 litre of the 0.1 M Ethyl acetate into the reactor. Stop pump P2.

2.

Switch on pump P1 and start pumping 1 litre of the 0.1 M NaOH into the
reactor as quickly as possible. Stop pump P1 and close valve V1
simultaneously when the reaction volume reaches 2 litres. Switch on the
stirrer and set the speed at about 200 rpm. Immediately start the timer.

3.

Record the conductivity values at 1 minute interval in an appropriate table.

4.

Drain the reactor and flush with de-ionized water.

5.

Repeat steps 1 to 4 with different stirrer speed of 50, 100, 150 RPM.

6.

Switch off all switches when you are finished with the experiment. Drain off
all liquid from the reactor

Task: Determine the order of the reaction and the rate constant, k.
Note:
For operations with SOLDAS Data Acquisition System, refer to the DAS operating
procedure. In step 2, click the START button. Conductivity values will be recorded
automatically and a table will be generated.
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REFERENCES

5.0

Levenspiel, O., Chemical Reaction Engineering, John Wiley, 1972.

Fogler, H.S., Elements of Chemical Reaction Engineering, 3rd Edition, Prentice Hall PTR,
1999.
Smith, J.M., Chemical Engineering Kinetics, McGraw Hill, 1981.
Astarita, G., Mass Transfer with Chemical Reaction, Elsevier, 1967.
SAFETY & MAINTENANCE
1.

2.
3.

After each experiment, drain off any liquids from the reactor and make sure that
the reactor and tubings are cleaned properly. Flush with de-ionized water as
necessary. Note: NaOH and Ethyl acetate are corrosive and they may damage the
tubings and the rig in the long run.
Dispose all liquids immediately after each experiment. Do not leave any reactants
or product in the tank over a long period of time.
Wipe off any spillage from the unit immediately.

SAFETY PRECAUTIONS
1.

Always observe all safety precautions in laboratory.

BATCH LIQUID REACTOR

2.
3.
4.
5.
6.
7.

Always wear protective clothing, shoes, helmet and goggles throughout the
laboratory session.
Always run the experiment after fully understand the equipment and procedures.
Always plug in all cables into appropriate sockets before switching on the main
power on the control panel. Inspect all cables for any damage to avoid electrical
shock. Replace if necessary.
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.
Make sure that the stirrer assembly is secured properly. Avoid excessive load to
the electrical motor to prevent damage.
Inspect the unit, including tubings and fittings, periodically for leakage and worn
out. Leakage might cause damage to equipments by corrosive chemical in the long
run.