LAB1 Batch Reactor - Procedure

CHE506: REACTION ENGINEERING LABORATORY
LAB 1: BATCH REACTOR
Equipment Description
The unit operation consists of the followings:
a) Reactor
The reactor consists of a glass vessel with top and bottom plate made of stainless steel.
The reactor comes with a cooling coil, a 1.5 kW heater, a temperature sensor, stirrer
system, an overflow tube and a gas sparging unit.
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
top plate.
c) Product/ Waste Tank

A 50-L rectangular tank made of stainless steel is provided for collecting the product or
waste before being discharged.
d) 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.
Methodology
By studying the saponification reaction of ethyl acetate and sodium hydroxide to form sodium
acetate in a batch reactor, the rate data needed to design a production scale reactor can be
evaluated.
This reactor has a total volume of approximately 4 liters. A scale is provided to determine the reactor
volume.
Reactants Preparation Procedure
1. Prepare 0.1 M NaOH and 0.1 M Ethyl acetate solutions in two separate 20-liter feed tanks.
2. Confirm the concentration of your 0.1 M NaOH solution by titrating a small amount of it with
standard 0.1 M HCl using phenolphthalein as indicator. The concentration of ethyl acetate
solution, on the other hand, is evaluated in the following manner. First, add enough 0.1 M
NaOH solution to a sample of the feed solution such that the 0.1 M NaOH solution is in
excess to ensure all the ethyl acetate reacted. Let this mixture react overnight. On the
following day, determine the amount of unreacted NaOH by direct titration with standard
0.1 M HCl. Record the ethyl acetate real concentration.
3. Prepare 1 liter of quenching solution of 0.25 M HCl and 1 liter of 0.1 M NaOH for back
titration.
1
Batch Reaction Procedure
1. To begin a batch reactor experiment, adjust the overflow tube in the reactor to give a
desired working volume or 2.5 liters. Switch on pump P1 and start pumping 1.25 liters of
the 0.1 M Ethyl acetate from the feed tank into the reactor. Switch off pump P1. Switch on
the stirrer and set the speed in the mid-range. To set the reaction temperature, switch on
the heater and set the reaction temperature. Run the cooling water to maintain the desired
temperature.
2. Switch on the stirrer and set the speed in the mid-range (say 180 rpm). Switch on pump
P2 and start pumping 1.25 liters of the 0.1 M NaOH into the reactor. Stop the pump and
immediately start timing the reaction. Record start time, t0.
3. Quickly measure 25 ml of the 0.25 M HCl in a flask.
4. After 1 minute of reaction, collect a 100 ml sample by opening the sampling valve and
immediately add to the 25 ml of 0.25 M HCl prepared in step 3, and mix. The HCl will
quench the reaction between ethyl acetate and sodium hydroxide.
5. Titrate the mixture with the 0.1 M NaOH to evaluate the amount of unreacted HCl; this will
provide you with the information to determine the amount of NaOH in the feed solution
which has reacted.
6. Repeat steps 3 to 5 for reaction times of 5, 10, 15, 20, 25 and 30 minutes.
7. Repeat steps 1 to 6 for reaction temperatures of 30, 40 and 50 °C.
8. Plot C vs. T; r vs. T and r vs. C.
2
Maintenance
1. After each experiment, make sure that the reactor and tubing are cleaned properly. NaOH
and Ethyl acetate are corrosive and can damage the tubing and the reaction rig.
2. Dispose all liquids immediately after each experiment. Do not leave any reactants or
product in the tank.
3. Wipe off any spillage on the bench.
Safety Precautions
1. Plug in all cables into appropriate sockets before switching on the main switch. Inspect all
cables for any damage to avoid electric shock. Replace if necessary.
2. 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.
3. Make sure that the stirrer assembly is secured properly to avoid damage to the mechanical
seal.
4. Inspect all tubing periodically for leakage and worn out. Leakage might cause damage to
equipment by corrosive reactants.
3
Universiti Teknologi MARA
Back Titration Procedures for Manual Conversion Determination
It is advisable 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 àNaCl + 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

Universiti Teknologi MARA
Calculations:
Conc. of NaOH entering the reactor, CNaOH,0 = (CNaOH,f)/2 mol/L
C NaOH, s
Volume of unreacted quenching HCl, V2 = V1 ml
C HCl,s
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)/1000 mol
Moles of unreacted NaOH in sample, n2 = n1 mol
Conc. of unreacted NaOH in the reactor, CnaOH = n2 / Vs× 1000 mol/L
æ C ö
Conversion of NaOH in the reactor, X = çç1 - NaOH ÷÷ x100%
è CNaOH ,0 ø

LAB1 Batch Reactor - Procedure

Uploaded by

Copyright:

Available Formats

LAB1 Batch Reactor - Procedure

Uploaded by

Document Information

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

LAB1 Batch Reactor - Procedure

Uploaded by

Copyright:

Available Formats

CHE506: REACTION ENGINEERING LABORATORY

LAB 1: BATCH REACTOR

The unit operation consists of the followings:

b) Feed Inlet System (Liquid Reactions)

c) Product/ Waste Tank

Reactants Preparation Procedure

3. Quickly measure 25 ml of the 0.25 M HCl in a flask.

7. Repeat steps 1 to 6 for reaction temperatures of 30, 40 and 50 °C.

8. Plot C vs. T; r vs. T and r vs. C.

3. Wipe off any spillage on the bench.

Back Titration Procedures for Manual Conversion Determination

1. Fill up a burette with 0.1 M NaOH solution.

2. Measure 10 ml of 0.25 M HCl in a flask.

4. Add a few drops of pH indicator into the mixture.

ANALYSIS AND DISCUSSION:

Concentration of NaOH in the reactor = CNaOH mol/L

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

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

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)/1000 mol

Moles of unreacted NaOH in sample, n2 = n1 mol

Conc. of unreacted NaOH in the reactor, CnaOH = n2 / Vs× 1000 mol/L

You might also like