UNIVERSITY OF MINNESOTA DULUTH

DEPARTMENT OF CHEMICAL ENGINEERING

ChE 3211-4211

CONTINUOUS STIRRED TANK REACTOR

OBJECTIVE

The objective of this experiment is to measure the conversion of ethyl acetate in

saponification as a function of design parameters in a continuous stirred tank reactor (CSTR).
The reaction rate constant shall also be determined.

INTRODUCTION

The stoichiometry of the saponification reaction between NaOH and EtOAc is :

NaOH + EtOAc NaOAc + EtOH (1)

This reaction can be assumed to be second order overall, first order in each reactant, with
the following rate expression:

Rate = k 2 C N C E (2)

where k2 = second order rate constant and CN and CE are concentrations of NaOH and EtOAc,
respectively. The rate expression has the units [moles/(liter)(time)]. For these experiments, the
unit of time should be minutes.

REFERENCES

ChE 3611 Textbook, H.S. Fogler, "Elements of Chemical Reaction Engineering"

EQUIPMENT

1. 1 - 4 channel peristaltic pump for reactant feed and product withdrawal.

2. 2 Stopwatches.
3. Magnetic stirrer.

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 4. Reaction vessel, 180 mL tall form beaker.
5. Containers for reagents and products.
6. 10 mL Buret.
7. 50 mL E-flasks.
8. Volumetric flasks.
9. 100 and 10 mL graduated cylinders.
10. Pipets of assorted sizes.

CHEMICALS/MATERIALS

1. Potassium Acid Phthalate - 0.05 M

2. HCl - 0.05 M
3. NaOH - 0.05 M
4. EtOAc - 0.05 M

EXPERIMENTAL PROCEDURE

Refer to Figure 1 for a schematic of the CSTR apparatus. It consists of a 180 mL tall form
beaker on top of a magnetic stirrer. Reactants and products are pumped in and out of the reactor
using the same peristaltic pump.

Figure 1. Laboratory CSTR System.

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 Your experiment should include the following investigations. You should attempt to run the
reactor at room temperature (21EC) at five different pump rates in the range 6.7 to 1.5 mL/min,
and you should measure the conversion at each flow rate. If time permits, you should either
repeat an experiment, or try other flow rates.

The reaction is run under conditions where the initial concentrations of the reactants are
equal. Monitoring the reaction and its approach to steady state is done using a flow through
conductivity cell. In considering the approach to steady state - think about the space time at the
particular flow rate. Has the reactor been running for a "space time" since you last changed the
flow rate? (Is this the right question to ask?)

The reaction volume should be kept the same for each flow rate. Taking samples from the
reactor will reduce its volume. One way to maintain constant volume is to place the inlet of the
flow through conductivity cell at the liquid interface when the experiment is started. You may
think of another way. Once the cell is placed at the interface do not move it. The conductivity
meter should be set on RANGE E.

Before or during the first part of the experiment standardize the NaOH and HCl as outlined
below.

1. Standardize the sodium hydroxide using the acidimetric standard (potassium hydrogen
phthalate [KHP]) available on the bench. Pipet 5 mL of KHP into a 50 mL erlenmeyer
flask. Titrate the KHP with the NaOH using the supplied burette until the
phenophthalein end point (pink) appears (run a minimum of three titrations).

2. The concentration of HCl is determined using the NaOH standardized above. Pipet 5
mL of HCl into a 50 mL erlenmeyer flask. Titrate the HCl with the NaOH using the
supplied burette until the phenolphthalein end point (pink) appears (run a minimum of
three titrations).

3. Pipet 5 mL of HCl into each of several 50 mL erlenmeyer flasks (E-flasks) before the
experiment begins.

The suggested procedure is:

1. Measure 50 mL of each reactant using a graduated cylinder and add them to the
reactor. Fill each of the l Liter bottles, to the line, with the reactants and clamp them
in the constant temperature bath. Allow both the liquid in the reactor and in the
bottles to come to equilibrium with the bath temperature before starting the
experiment.

2. Start the magnetic stirrer under the reactor and set at a speed of at least 200 RPM.

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 3. Loosen the clamp holding the flow through conductivity cell and position the bottom
of the short section of plastic tubing just above the liquid interface close to the side of
the beaker. Clamp it in place. The product will be pumped out of the reactor through
the conductivity cell and into the product bottle.

4. Clamp the feed lines so the end of the Y connector is just above the liquid. Start and
run the pump at your highest chosen flow rate. See procedure for setting pump
parameters in Appendix A. Let the feed lines fill with reactants. Start the timer
when liquid begins to flow into the reactor.

5. Shortly after, there should be a reading on the conductivity meter. If a reading does
not appear, check to see that the bottom of the short section of plastic tubing on the
conductivity cell is positioned at the surface of the liquid in the reactor. Make sure the
product eventually drips into the product container.

6. While waiting for steady state to be reached, measure the flow rate delivered by the
pump by collecting the liquid from the product lines using a 100 mL (or other size)
graduated cylinder.

7. What is the space time at this flow rate?

8. Monitor the conductivity. Record it, the time, and reaction temperature at appropriate
intervals (2-5 minutes). Steady state is reached when the conductivity does not
change. Be sure to record the conductivity at the time a sample is taken.

9. Take two 5 mL samples from the reactor when the reaction is at steady state.
Discharge the sample into 5 mL of HCl to quench the reaction. Record the time at
which the samples are taken. Titrate the samples with NaOH to determine the
concentration of unreacted NaOH in the samples.

10. Change the pump to a new setting and repeat the procedure from step 5. Keep the
stopwatch going. Do not reset the time.

11. Samples should be titrated promptly.

12. When the experiment is finished, remove the tubing from the reactant bottles and raise
the flow through conductivity cell so it is above the liquid in the reactor. Increase the
pump speed to approximately 7.0 mL/min (maximum = 7.0 ml/min) to pump the
liquid out of the tubing. After the liquid is pumped out of the tubing, insert the tubing
and the inlet of the conductivity cell in deionized water and pump for one to two
minutes to rinse the tubing and cell. Remove the tubing and conductivity cell from the
deionized water and continue to pump until the tubing is free of liquid.

13. Remove the reactor (180 mL beaker) from the constant temperature bath and discard

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 the liquid into the waste container. Rinse the beaker with deionized water and reinsert
it into the constant temperature bath.

14. Turn off the pump and the conductivity meter.

SAFETY NOTES

1. Before starting the experiment, review the Material Safety Data Sheets (MSDS) on
NaOH, HCl, and EtOAc. The sheets can be found in the MSDS notebook located in
the laboratory.

2. Personal protective equipment shall include safety glasses. Disposable nitrile gloves
should be worn when handling NaOH solutions.

3. A small amount of NaOH spilled on the outside of glassware and/or equipment can
cause the glassware and equipment to be extremely slippery when wet. Be careful.

4. Pumping of hazardous chemicals will be conducted in this experiment. Check all

hoses and connections before starting the experiment. Secure the hoses entering the
product vessel so they do not slip out. If a spill occurs, turn off the pumps (if possible
without injury) and immediately get in touch with the Laboratory Services
Coordinator or faculty member.

WASTE DISPOSAL PROCEDURES

Collect all waste chemical solutions in the container marked with "CSTR waste solution"
and your lab period. At the end of each lab period or the end of the experiment, add sufficient
base (NaOH) to yield a phenolphthalein end point (pink) that does not disappear overnight. This
indicates the reaction has gone to completion and the waste can be disposed down the drain.
Why? Do not add too much base as the pH has to be less than 10 before it can be disposed down
the drain. Once the phenolphthalein end point stays pink and the pH is less than 10, contact the
lab services coordinator.

02/2013

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 APPENDIX A

Masterflex pump instructions

1. Turn the power switch on.

2. Check the motor direction. The green light next to the clockwise icon should be on.
If it is not, see the Lab Services Coordinator.

3. Check the mode selection. The green light next to "INT" should be on. If it is not, see
the Lab Services Coordinator.

4. Check the tubing size. The green light next to "13" should be on. If it is not, see the
Lab Services Coordinator.

5. Set the desired flow (mL/min)

Press the FLOW control. The display will flash the presently set flow rate for five
seconds, or until another control is pressed.

If a different flow rate is desired, proceed as follows. Press and hold the increment
or decrement control until the desired flow rate is displayed, then release control.

NOTE: The change in value will be in small increments at first, then gradually
increase in multiples as high as 50.

To exit the set flow rate mode, wait five seconds or press any other control, except
the increment and decrement control. The display will then display 0.0.

Warning:

Do not press the prime button. To purge the tubing quicker, change to a higher flow.
Maximum flow rate is 7.0 mL/min.

Do not press the "CAL" button. The pump has been calibrated.

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 Department of Chemical Engineering
Stockroom Checkout slip

Continuous Stirred Tank Reactor Experiment ChE 4211

Name: Date:
(print name)

Lab No.: Lab 1 Tuesday 12:00 - 4:50 PM Lab 2: Thursday 12:00 - 4:50 PM

Lab No.: Lab 3 Tuesday and Thursday morning (9:30 - 12:00 AM)
(circle one)

Equipment Out In Equipment Out In

12-50 mL E-flasks 10 mL grad. pipet
100 mL grad. cylinder 1-5 mL transfer pipet
10 mL grad. cylinder 2-Stopwatches
2-250 mL beakers 1-pipet bulbs
Digital thermometer 1-Finnpipette (1-5 mL)

Name:
(Signature)