Saponification

Saponification of Ethyl Acetate by
Sodium Hydroxide in a Continuous

Stirred Reactor (CSTR)
Kurt Spies
Trevor Carlisle
ChE 414 Winter 2005

Presentation Overview
Requested information
Project objectives
Planning and execution
Team member roles
Background and experimental methods
Procedure
Data/results
Conclusions
Recommendations
Requested Information
Information Contained
The procedures and results of the saponification
experiment
Audience
Peers
Supervisors
Educational Leaders
Objectives
1. Develop calibration curves for conductivity
2. Determine rate constant using batch reactor
3. Evaluate the CSTR reaction rate as a function of
residence time

Project Planning and Execution
Planning
Developed initial project plan
Only deviation included an additional lab session
Execution Lessons/Thoughts
Plan first lab session before entering the room
Prepare to put in sufficient out of lab time into
project to make lab time efficient
Team member roles
Trevor- Operations Manager
Responsible for the operation of the CSTR
accountable for data collection
In charge of making sure experiment is accurate and follows
correct procedures
Kurt- Team Leader/Safety Manager
Identify safety issues
Develop the safety plan
Monitor safe lab behavior
Develop project plan
Ensure lab work moves forward
Responsible for the operation of batch reactor
Background and Experimental
Methods
The Irreversible Reaction
Ethanol Acetate Sodium
Hydroxide Sodium
Acetate Ethyl
OH H C Na H O C NaOH H COOC CH
5 2 3 2 2 5 2 3
+ +
Logical Experimental
Organization
Calibration
Batch Experiment
CSTR Experiment
Conductivity Calibration
15.0
Sample Solution
Conductivity Probe
Digital Conductivity Meter
Calibration Procedure
Prepared and standardized 0.1M NaOH
Solution
Diluted solution to various concentrations
Fine-tuned conductivity using calibration
probe
Measured Conductivity of different solutions
Calibration Data/Results
y = 0.00440x
0
0.01
0.02
0.03
0.04
0.05
0.06
0.07
0 2 4 6 8 10 12 14 16
Conductivity [mS]
C
o
n
c
e
n
t
r
a
t
i
o
n

N
a
O
H

M
Calibration Conclusions
1) Calibration curves for conductivity cells
match well with a linear approximation

[concentration NaOH M] = 0.00440*[conductivity]
Batch Reactor
15.0
Sample Solution
Conductivity Probe
Digital Conductivity Meter
Hot Water Bath
Theoretical Batch Calculation
Alkaline Hydrolysis of Ethyl Acetate is a
second order reaction

To solve using graphical methods
B A
B A
A
C kC
dt
dC
dt
dC
r = = =
( )
|
|
.
|
\
|
+ =
|
|
.
|
\
|
0
0
0 0
ln ln
A
B
A B
A
B
C
C
kt C C
C
C
Experimental Batch Design
Three Experimental Types
Equal molar concentrations
Significant excess Sodium Hydroxide
Significant excess Ethyl Acetate
Erlenmeyer Flask
~100 mL solution
Hot water bath ~50
O
C
Mixed with conductivity probe
Equal Molar Concentrations
y = 0.1125x + 12.5
12.00
13.00
14.00
15.00
16.00
17.00
18.00
19.00
20.00
21.00
22.00
0 10 20 30 40 50 60
Time (sec)
1
/
C
a

[
L
/
m
o
l
]
Run 1
Run 2
Run 3
Run 4
Run 5
Run 6
Run 7
Run 8
Linear (Theorey)
Results
Experimental Rate Constant from Data

Theoretical Experimental Rate Constant from
Tsujikawa and Inoue

Theoretical Experimental Rate Constant from
Mata-Segreda

(
=
s mol
L
k 00163 . 0 119 . 0
exp
(
=
s mol
L
k
th
1125 . 0
(
=
s mol
L
k
th
122 . 0
High Concentration of Sodium
Hydroxide
y = 0.00680x + 1.39
1.000
1.200
1.400
1.600
1.800
2.000
2.200
2.400
2.600
0 10 20 30 40 50 60 70 80 90 100
Time (sec)
l
n
(
C
b
/
C
a
)
Run 1
Run 2
Linear (Theory)
High Concentration of Sodium
Hydroxide Results
Slope of experimental line excluding bottom points

m=k(C
B0
-C
A0
)=0.00760 (+/- 0.000129)

(
=
s mol
L
k 127 . 0
exp
High Concentration Ethyl
Acetate
y = 0.0338x + 2.77
2
2.5
3
3.5
4
4.5
5
5.5
0 10 20 30 40 50 60 70 80
Time (sec)
l
n
(
C
b
/
C
a
)
Run 1
Run 2
Run 3
Linear (Theory)
High Concentration of Ethyl
Acetate Results
Slope of experimental line only including reaction
region of first few points

m=k(C
B0
-C
A0
)=0.0374 (+/- 0.0044)

(
=
s mol
L
k 125 . 0
exp
What accounts for theoretical and
empirical differences?
Overall rate constant consistent with
theoretical data
Initial concentration different then planned
y = 0.1125x + 12.5
12.00
13.00
14.00
15.00
16.00
17.00
18.00
19.00
20.00
21.00
22.00
0 10 20 30 40 50 60
Time (sec)
1
/
C
a

[
L
/
m
o
l
]
Run 1
Run 2
Run 3
Run 4
Run 5
Run 6
Run 7
Run 8
Linear (Theorey)
The Continuous Stirred Tank Reactor
Theoretical CSTR Calculation
Second order mixed
flow reactor

Graphical Solution

( )
( )
2
0
2
0
1
A A
A
A
A A
X C
X
C
C C
k
= t
| | ) log( ) log( ) log( k C order reaction r
A A
+ =
Experimental Design for CSTR
Filled chemical reservoirs with equal
concentration sodium hydroxide and ethyl
acetate

Preformed experiment with different flow
rates with different concentrations
CSTR Data
y = 2x - 0.949
0.4
0.5
0.6
0.7
0.8
0.9
1
1.1
0.7 0.75 0.8 0.85 0.9 0.95 1
Log(Ca) [log(mol/L)]
L
o
g
(
-
r
a
)

[
l
o
g
(
m
o
l
/
L
-
H
r
)
]
Linear (Theory)
CSTR Results
The theoretical information for the CSTR should
be the same rate constant

Our experimental data contains considerable
noise and does not conform to any experimental
trend for determining the order of reaction

2 1125 . 0 =
(
= order l theoretica
s mol
L
k
th
CSTR Data
y = 27.9x
-0.977
0
2
4
6
8
10
12
0 1 2 3 4 5 6 7 8 9 10
tau (resonance time) [sec]
r
e
a
c
t
i
o
n

r
a
t
e

[
m
m
o
l
/
L
-
H
r
]
CSTR Data
Power (CSTR Data)
CSTR Results
Our experimental data can be approximated by a
inverse relationship

This makes sense because as the resonance
time increases the rate should approach that of
the batch reactor

| | | |
977 . 0
Re 9 . 27 Re

= Time sonance Rate action al Experiment
What accounts for theoretical and
empirical differences?
The CSTR reaction has significant noise in
the reaction and the order is difficult to
experimentally confirm
The flow rates for the CSTR feeds may not
be correctly calibrated

Experimental Conclusions
2) Batch reaction information suggests the reaction
rate constant is

3) Experimental data suggests the correlation
between resonance time and reaction rate is
(
=
s mol
L
k 00163 . 0 119 . 0
exp
| | | |
977 . 0
Re 9 . 27 Re

= Time sonance Rate action al Experiment
Recommendations
Leave more time for CSTR data collection
Flow rate calibrations
Solution prep
Temperature adjustment
Use volumetric glassware as much as
possible
Gather sufficient technical information about
experiment
Questions?...
References
Density of Water: Vapor Pressure of Water. Retrieved February 15, 2005 from the World Wide Web:
http://www.ncsu.edu/chemistry/resource/
H2Odensity_vp.html

Kinetics: Alkaline Hydrolysis of Ethyl Acetate. Retrieved January 29, 2005 from the World Wide
Web: Http://www.uni-regensburg.de/fakultaeten/nat_fak_IV/
organische_chemie/didaktik/keusch/chembox_etae_e.htm

Levenspiel, Octave. 1999. Chemical Reaction Engineering (3
rd
Ed). United States of America: John
Wiley & Sons Inc.

Segreda-Mata, Julio F., Hydroxide as General Base in the Saponification of Ethyl Acetate. Journal of
American Chemical Society, 124: 10: 2259-2262

Traceable Expanded Range Digital Conductivity Meter Instructions. Model VWR 23226-523. 2000
Control Company.

Tsujikawa, Hiroo, and Inoue, Hakuai. The Reaction Rate of Alkaline Hydrolysis of Ethyl Acetate.
Bulletin of the Chemical Society of Japan, 39: 1837-1842

Saponification

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Saponification of Ethyl Acetate by

Sodium Hydroxide in a Continuous

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