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CPE554

Universiti Teknologi MARA

OPERATING PROCEDURES General Start-Up Procedures for Experiments 3 & 4 1) Ensure that all valves are initially closed except valves V4, V8 and V17. 2) Prepare the following solutions: a. 20 liter of sodium hydroxide, NaOH (0.1 M) b. 20 liter of ethyl acetate, Et(Ac) (0.1 M) c. 1 liter of hydrochloric acid, HCl (0.25 M), for quenching 3) Fill the feed tank B1 with the NaOH solution and feed tank B2 with the Et(Ac) solution. 4) Fill the water jacket B4 and pre-heater B5 with clean water. 5) Turn on the power for the control panel. 6) Open valves V2, V4, V6, V8, V9 and V11. 7) Switch on both pumps P1 and P2. Adjust P1 and P2 to obtain flow of approximately 300 ml/min at both flow meters FI-01 and FI-02. Make sure both flow rates are the same. 8) Allow both solutions to flow through the reactor R1 and overflow into the waste tank B3. 9) Open valves V13 and V18. Switch on pump P3 to circulate the water through pre-heater B5. Switch on stirrer motor M1 and set the speed to about 200 rpm to ensure homogeneous water jacket temperature. 10) For experiment 4, perform the following additional steps: a. Switch on the heaters. b. Open valve V19 to let the cooling water to flow through the cooling tubes. Adjust valve V19 to obtain reasonable cooling water flow in order to minimize the temperature overshoot at the TIC-01 during heater cut-off. c. Set the temperature setpoint on TIC-01 to the desired temperature. 11) The unit is now ready for experiment. General Shut-Down Procedures 1) Switch off both pumps P1, P2 and P3. Close valves V2 and V6. 2) Switch off the heaters. 3) Keep the cooling water circulating through the reactor while the stirrer motor is running to allow the water jacket to cool down to room temperature. 4) If the equipment is not going to be used for long period of time, drain all liquid from the unit by opening valves V1 to V19. Rinse the feed tanks with clean water. 5) Turn off the power for the control panel.

Exp/Plug Flow Reactor

CPE554

Universiti Teknologi MARA

EXPERIMENT PROCEDURES A. 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) b) 1 liter of sodium acetate, Na(Ac) (0.1 M) 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) 25% conversion : 75 ml NaOH + 25 ml Na(Ac) c) 50% conversion : 50 ml NaOH + 50 ml Na(Ac) d) 75% conversion : 25 ml NaOH + 75 ml Na(Ac) e) 100% conversion : 100 ml Na(Ac)
ANALYSIS AND DISCUSSION:

1. Record all data in the sample table in Appendix A. 2. Plot the calibration curve of conductivity vs conversion. Determine the slope and y-axis intercept. B. 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.

Exp/Plug Flow Reactor

CPE554

Universiti Teknologi MARA

ANALYSIS AND DISCUSSION: NaOH + HClNaCl + H2O

Exp/Plug Flow Reactor

CPE554

Universiti Teknologi MARA

EXPERIMENT 3: Effect of Residence Time on the Reaction OBJECTIVE: To carry out a saponification reaction between NaOH and Et(Ac). To determine the reaction rate constant. To determine the effect of residence time on the conversion. PROCEDURES: 1) Perform the general start-up procedures as in Section 4.2. 2) Open valves V9 and V11. 3) Allow both the NaOH and Et(Ac) solutions to enter the plug reactor R1 and empty into the waste tank B3. 4) Adjust P1 and P2 to give a constant flow rate of about 300 ml/min at flow meters FI-01 and FI-02. Make sure that both flow rates are the same. Record the flow rates. 5) Start monitoring the inlet (QI-01) and outlet (QI-02) conductivity values until they do not change over time. This is to ensure that the reactor has reached steady state. 6) Record both inlet and outlet steady state conductivity values. Find the concentration of NaOH exiting the reactor and extent of conversion from the calibration curve. 7) Optional: Open sampling valve V15 and collect a 50 ml sample. Carry out a back titration procedure to manually determine the concentration of NaOH in the reactor and extent of conversion (Section B). 8) Repeat the experiment (steps 4 to 7) for different residence times by reducing the feed flow rates of NaOH and Et(Ac) to about 250, 200, 150, 100 and 50 ml/min. Make sure that both flow rates are the same. ANALYSIS AND DISCUSSION:

Exp/Plug Flow Reactor

CPE554

Universiti Teknologi MARA

EXPERIMENT 4: Effect of Temperature on the Reaction. OBJECTIVE: To determine the effect of temperature on the conversion in a TFR. PROCEDURES: 1) Perform the general start-up procedures as in Section 4.2. 2) Open valves V9 and V11. 3) Allow both the NaOH and Et(Ac) solutions to enter the plug reactor R1 and empty into the waste tank B3. 4) Adjust P1 and P2 to give a constant flow rate of about 150 ml/min at flow meters FI-01 and FI-02. Make sure that both flow rates are the same. Record the flow rates. 5) Set the temperature setpoint at TIC-01 to 40C in Section 4.2 (10(c)). 6) Start monitoring the conductivity values at QI-01 & QI-02 and temperature value at TIC-01 until they do not change over time. This is to ensure that the reactor has reached steady state. 7) Record both inlet and outlet steady state conductivity values and the water jacket temperature. Find the concentration of NaOH exiting the reactor and extent of conversion from the calibration curve. 8) Optional: Open sampling valve V15 and collect a 50 ml sample. Carry out a back titration procedure to manually determine the concentration of NaOH in the reactor and extent of conversion (Section B). 9) Repeat the experiment (steps 5 to 8) for different reactor temperatures by increasing the temperature setpoint on TIC-01 to 45, 50, 55 and 60C. Make sure that the flow rates of both solutions are maintained at 150 ml/min. ANALYSIS AND DISCUSSION: 1. Use the sample table in Appendix C for data collection. 2. Plot a graph of conversion vs. reactor temperature.
Exp/Plug Flow Reactor 5

CPE554

Universiti Teknologi MARA

Exp/Plug Flow Reactor

CPE554

Universiti Teknologi MARA

Exp/Plug Flow Reactor