Saponification of Saponification of Ethyl acetate by Ethyl acetate by Sodium hydroxide in Sodium hydroxide in a Plug Flow Reactor a Plug Flow Reactor Lindsey Kato Lindsey Kato Shawna Togioka Shawna Togioka Luke Sugie Luke Sugie February 2, 2005 February 2, 2005
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Saponification of Ethyl Saponification of Ethyl acetate by Sodium acetate by Sodium
hydroxide in a Plug Flow hydroxide in a Plug Flow ReactorReactor
Luke SugieLuke SugieFebruary 2, 2005February 2, 2005
Overview
Project ObjectivesProject Objectives Project Planning and ExecutionProject Planning and Execution Background and Experimental MethodsBackground and Experimental Methods Results and ConclusionsResults and Conclusions Recommendations and Future WorkRecommendations and Future Work
Project Objectives
Develop reaction kinetic data for the Develop reaction kinetic data for the saponification of ethyl acetate by sodium saponification of ethyl acetate by sodium hydroxide.hydroxide.
1.1. Develop calibration curves for electric Develop calibration curves for electric conductivity cell, using known concentrations conductivity cell, using known concentrations of reactants and productsof reactants and products
2.2. Calibration of pump settings on Plug Flow Calibration of pump settings on Plug Flow Reactor (PFR).Reactor (PFR).
3.3. Ran Batch Reactor and PFR and gathered Ran Batch Reactor and PFR and gathered kinetic rate data kinetic rate data
• Knowledge of equipment, data collections and laboratory Knowledge of equipment, data collections and laboratory documentationdocumentation
Safety Coordinator – Luke SugieSafety Coordinator – Luke Sugie• Hazards of the Lab, chemical safety, MSDSHazards of the Lab, chemical safety, MSDS
Group: Background data collection and analysisGroup: Background data collection and analysis
Key Planning ElementsKey Planning Elements
1.1. Project Plan / Time TableProject Plan / Time Table
2.2. Learn about the lab, equipment, safety, hazardsLearn about the lab, equipment, safety, hazards
3.3. Calibration TestsCalibration Tests
4.4. Batch Reactor TestsBatch Reactor Tests
5.5. PFR TestsPFR Tests
6.6. AnalysisAnalysis
7.7. Oral PresentationOral Presentation
8.8. Written ReportsWritten Reports
Lessons LearnedLessons Learned
Some activities take longer than expectedSome activities take longer than expected Experiments don’t always run smoothly. Experiments don’t always run smoothly.
Must rethink the experimental design.Must rethink the experimental design.
Overall – Lab time was utilized and Overall – Lab time was utilized and original project plan didn’t need to be original project plan didn’t need to be altered.altered.
Preparation: calibrated atPreparation: calibrated at
beginning of every labbeginning of every lab
period.period.
Calibration curves were constructedCalibration curves were constructed
with different concentrations ofwith different concentrations of
reactants and products.reactants and products.
EquipmentEquipment
Constant Water BathConstant Water Bath-Batch Reaction-Batch Reaction
experiments doneexperiments doneat at 25°C25°C
-Reactants were -Reactants were submerged in thesubmerged in thebath to reach temp. bath to reach temp. and then put together and then put together for the experiment.for the experiment.
EquipmentEquipment
Plug Flow ReactorPlug Flow Reactor-Packed with small-Packed with small
~0.41 ~0.41 -Equimolar concentrations of -Equimolar concentrations of NaOH and Ethyl AcetateNaOH and Ethyl Acetate
were pumped into PFRwere pumped into PFR-Conductivity meter used to -Conductivity meter used to determine the composition determine the composition of the product stream. of the product stream. -Experiment finished once -Experiment finished once reaction reached equilibrium.reaction reached equilibrium.
ExperimentsExperiments
1.1. Testing was done on the PFR pumps to Testing was done on the PFR pumps to determine the resonance time for each pump determine the resonance time for each pump at different settings.at different settings.
2.2. Calibration curves were generated for the Calibration curves were generated for the conductivity meter for known concentrations of conductivity meter for known concentrations of reactants and products.reactants and products.
3.3. Batch reactions were done using equimolar Batch reactions were done using equimolar concentrations of reactantsconcentrations of reactants..
4.4. PFR experiments were done using equimolar PFR experiments were done using equimolar concentrations and approx. equal molar flows.concentrations and approx. equal molar flows.
• Bath was set to 25Bath was set to 25°C°C• Reactants were measured and put in bath Reactants were measured and put in bath
separately to heat.separately to heat.• Combined reactants and conductivity Combined reactants and conductivity
measurements taken at 5 and 10 second measurements taken at 5 and 10 second intervals.intervals.
• Batches were constantly stirred for the Batches were constantly stirred for the duration of the experiment.duration of the experiment.
PFR ExperimentsPFR Experiments
• Large quantities of equimolar mixture of Ethyl Large quantities of equimolar mixture of Ethyl acetate and NaOH were prepared and placed at acetate and NaOH were prepared and placed at the inlet for each pump.the inlet for each pump.
• The pumps were set so that the flow rates of The pumps were set so that the flow rates of each of the reactants would be equal.each of the reactants would be equal.
• Conductivity Meter was connected to the PFR at Conductivity Meter was connected to the PFR at the outlet and readings were taken during the the outlet and readings were taken during the experiment.experiment.
• Experiment was finished once the conductivity Experiment was finished once the conductivity reached a steady state.reached a steady state.
Measurements were taken with pure NaOH, 50-50% Measurements were taken with pure NaOH, 50-50% concentration NaOH and Sodium acetate, and pure concentration NaOH and Sodium acetate, and pure sodium acetate.sodium acetate.
y = 106167x + 7070
R2 = 1
0
2000
4000
6000
8000
10000
12000
14000
16000
0 0.01 0.02 0.03 0.04 0.05 0.06 0.07
Results – Batch ReactorResults – Batch Reactor
The kinetic rate constant is the initial slope at The kinetic rate constant is the initial slope at the start of the experiment.the start of the experiment.
The flow rate of the pumps was varied to five The flow rate of the pumps was varied to five different settings for data collection.different settings for data collection.
Rlug Flow Reactor Trialsy = 0.2431x
R2 = 0.6406
12
13
14
15
16
17
18
19
20
21
22
23
60 65 70 75 80 85 90
V/Vo (s)
XO
H/(
CO
Ho
*(1-
XO
H))
Results – Batch and Plug Flow ReactorResults – Batch and Plug Flow Reactor
• Batch Reactor showed a kinetic rate Batch Reactor showed a kinetic rate constant of ~0.19 L/mole-secconstant of ~0.19 L/mole-sec• Tests showed the rate constant to be 2 times Tests showed the rate constant to be 2 times
higher than literary value, but was consistent higher than literary value, but was consistent for all trials.for all trials.
• Plug Flow Reactor showed the kinetic rate Plug Flow Reactor showed the kinetic rate constant to be ~0.24L/mole-secconstant to be ~0.24L/mole-sec• The experimental value was 2.5 times higher The experimental value was 2.5 times higher
than the literary value.than the literary value.
Major ConclusionsMajor Conclusions
1.1. The kinetic rate constant for batch is 0.19 L/mole-The kinetic rate constant for batch is 0.19 L/mole-sec sec
2.2. The kinetic rate constant for a PFR is 0.24 L/mole-The kinetic rate constant for a PFR is 0.24 L/mole-sec.sec.
3.3. The literary value was 0.111 L/mole-secThe literary value was 0.111 L/mole-sec4.4. Discrepancies in the experiment and literature could Discrepancies in the experiment and literature could
be caused from slightly unequal concentrations, be caused from slightly unequal concentrations, incorrect molar flow rates, or conductivity incorrect molar flow rates, or conductivity calibration problems.calibration problems.
5.5. Reaction data showed characteristics of being Reaction data showed characteristics of being second order as theory predicted.second order as theory predicted.
Lessons LearnedLessons Learned
Some activities take longer than expectedSome activities take longer than expected Experiments don’t always run smoothly. Experiments don’t always run smoothly.
Must rethink the experimental design.Must rethink the experimental design.
Overall – Lab time was utilized and Overall – Lab time was utilized and original project plan didn’t need to be original project plan didn’t need to be altered.altered.
Future RecommendationsFuture Recommendations
• More careful research done early on, so More careful research done early on, so work in the lab could go more smoothly.work in the lab could go more smoothly.
• Run more trials on the PFR and batch to Run more trials on the PFR and batch to confirm data.confirm data.
• Plan out your lab times carefully and set Plan out your lab times carefully and set reasonable goals and be safe.reasonable goals and be safe.
ReferencesReferences
1.1. Bamford, C.H. and C.F.H. Tipper. 1970. Bamford, C.H. and C.F.H. Tipper. 1970. Comprehensive Chemical Kinetics v.10Comprehensive Chemical Kinetics v.10. Elsevier . Elsevier Publishing Company. New York. p.169.Publishing Company. New York. p.169.
2.2. Batch Reactor Kinetic Analysis. Jan 15, 2005. Batch Reactor Kinetic Analysis. Jan 15, 2005. www.csupomona.edu/~tknguyen/che435/Notes/P5www.csupomona.edu/~tknguyen/che435/Notes/P5-kinetic.pdf-kinetic.pdf
3.3. Levenspiel, Octave. 1998. Engineering Flow and Heat Levenspiel, Octave. 1998. Engineering Flow and Heat Exchange. Plenum Press. New York. p.128.Exchange. Plenum Press. New York. p.128.