Saponification Kato

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Saponification of Ethyl

acetate by Sodium
hydroxide in a Plug Flow
Lindsey Kato
Reactor
Shawna
Togioka
Luke Sugie
February 2, 2005

Overview
Project Objectives
Project Planning and Execution
Background and Experimental Methods
Results and Conclusions
Recommendations and Future Work

Project Objectives

1.

2.
3.

Develop reaction kinetic data for the


saponification of ethyl acetate by sodium
hydroxide.
Develop calibration curves for electric
conductivity cell, using known concentrations
of reactants and products
Calibration of pump settings on Plug Flow
Reactor (PFR).
Ran Batch Reactor and PFR and gathered
kinetic rate data

Project Planning

Roles & Responsibilities

Team Leader Lindsey Kato


Planning agenda, Assigning tasks and goals, presentation

Operations Coordinator Shawna Togioka


Knowledge of equipment, data collections and laboratory
documentation

Safety Coordinator Luke Sugie


Hazards of the Lab, chemical safety, MSDS

Group: Background data collection and analysis

Key Planning Elements


1.
2.
3.
4.
5.
6.
7.
8.

Project Plan / Time Table


Learn about the lab, equipment, safety, hazards
Calibration Tests
Batch Reactor Tests
PFR Tests
Analysis
Oral Presentation
Written Reports

Lessons Learned
Some activities take longer than expected
Experiments dont always run smoothly.

Must rethink the experimental design.


Overall Lab time was utilized and

original project plan didnt need to be


altered.

Background Information

Reaction:
Ethyl acetate+Sodium Hydroxide Sodium acetate+Ethanol
C2H5O2CCH3 + Na-OH CH3CO2Na + H3C-CH2-OH
Theory:
-rOH = -dCOH/dt = -dCEt-O-Ac/dt = k*COH*CEt-O-Ac
A second order bimolecular reaction.
Literature Value1,2:
kOH = 0.111 L/mole-sec at 25C
Irreversible reaction

Equipment
Conductivity Meter
Uses: measured
the conductivity
in the batch reactions
and PFR experiments
Preparation: calibrated at
beginning of every lab
period.
Calibration curves were constructed
with different concentrations of
reactants and products.

Equipment
Constant Water Bath
-Batch Reaction
experiments done
at 25C
-Reactants were
submerged in the
bath to reach temp.
and then put together
for the experiment.

Equipment
Plug Flow Reactor
-Packed with small
spherical balls
-Bed Void Fraction3, , of
~0.41
-Equimolar concentrations of
NaOH and Ethyl Acetate
were pumped into PFR
-Conductivity meter used to
determine the composition
of the product stream.
-Experiment finished once
reaction reached equilibrium.

Experiments
1.

2.

3.
4.

Testing was done on the PFR pumps to


determine the resonance time for each pump
at different settings.
Calibration curves were generated for the
conductivity meter for known concentrations of
reactants and products.
Batch reactions were done using equimolar
concentrations of reactants.
PFR experiments were done using equimolar
concentrations and approx. equal molar flows.

Batch Reactor Experiments


Bath was set to 25C
Reactants were measured and put in bath
separately to heat.
Combined reactants and conductivity
measurements taken at 5 and 10 second
intervals.
Batches were constantly stirred for the
duration of the experiment.

PFR Experiments

Large quantities of equimolar mixture of Ethyl


acetate and NaOH were prepared and placed at
the inlet for each pump.
The pumps were set so that the flow rates of
each of the reactants would be equal.
Conductivity Meter was connected to the PFR at
the outlet and readings were taken during the
experiment.
Experiment was finished once the conductivity
reached a steady state.

Key Equations
Batch Reactor
COH=CEt-O-Ac
Relationship:
1 = k*t + 1
COH
COHo
PFR
COH=CEt-O-Ac
Relationship:
1 * XOH = k*
COH 1- XOH

= V/vo (Space-time)

Results Conductivity Calibration


Measurements were taken with pure NaOH, 50-50%
concentration NaOH and Sodium acetate, and pure
sodium acetate.

Results Batch Reactor


The kinetic rate constant is the initial slope at
the start of the experiment.

Results Batch Reactor

Results - PFR
The flow rate of the pumps was varied to five
different settings for data collection.

Results Batch and Plug Flow Reactor

Batch Reactor showed a kinetic rate


constant of ~0.19 L/mole-sec

Tests showed the rate constant to be 2 times


higher than literary value, but was consistent
for all trials.

Plug Flow Reactor showed the kinetic rate


constant to be ~0.24L/mole-sec

The experimental value was 2.5 times higher


than the literary value.

Major Conclusions
1.
2.
3.
4.

5.

The kinetic rate constant for batch is 0.19 L/molesec


The kinetic rate constant for a PFR is 0.24 L/molesec.
The literary value was 0.111 L/mole-sec
Discrepancies in the experiment and literature could
be caused from slightly unequal concentrations,
incorrect molar flow rates, or conductivity
calibration problems.
Reaction data showed characteristics of being
second order as theory predicted.

Lessons Learned
Some activities take longer than expected
Experiments dont always run smoothly.

Must rethink the experimental design.


Overall Lab time was utilized and

original project plan didnt need to be


altered.

Future Recommendations
More careful research done early on, so
work in the lab could go more smoothly.
Run more trials on the PFR and batch to
confirm data.

Plan out your lab times carefully and set


reasonable goals and be safe.

References
1.

2.

3.

Bamford, C.H. and C.F.H. Tipper. 1970.


Comprehensive Chemical Kinetics v.10. Elsevier
Publishing Company. New York. p.169.
Batch Reactor Kinetic Analysis. Jan 15, 2005.
www.csupomona.edu/~tknguyen/che435/Notes/P5-k
inetic.pdf
Levenspiel, Octave. 1998. Engineering Flow and Heat
Exchange. Plenum Press. New York. p.128.

Questions?

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