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Presentation Overview. Requested informationProject objectivesPlanning and executionTeam member rolesBackground and experimental methodsProcedureData/resultsConclusionsRecommendations . Requested Information. Information Contained The procedures and results of the saponification experimentAudiencePeers SupervisorsEducational Leaders.
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1. Saponification of Ethyl Acetate by Sodium Hydroxide in a Continuous Stirred Reactor (CSTR) Kurt Spies
Trevor Carlisle
ChE 414 Winter 2005
3. Requested Information Information Contained
The procedures and results of the saponification experiment
Audience
Peers
Supervisors
Educational Leaders Peers- for information about the process and success for possible experimental recreation
Supervisors- for information about how successful the lab was and to confirm the correct lab format was followed
Educational Leaders- to verify the education of senior engineers and to thoroughly test their understanding of the lab Peers- for information about the process and success for possible experimental recreation
Supervisors- for information about how successful the lab was and to confirm the correct lab format was followed
Educational Leaders- to verify the education of senior engineers and to thoroughly test their understanding of the lab
4. Objectives Develop calibration curves for conductivity
Determine rate constant using batch reactor
Evaluate the CSTR reaction rate as a function of residence time
5. 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
6. 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
7. Background and Experimental Methods The Irreversible Reaction
8. Logical Experimental Organization Calibration
Batch Experiment
CSTR Experiment
9. Conductivity Calibration
10. 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
11. Calibration Data/Results
12. Calibration Conclusions 1) Calibration curves for conductivity cells match well with a linear approximation
[concentration NaOH M] = 0.00440*[conductivity]
13. Batch Reactor
14. Theoretical Batch Calculation Alkaline Hydrolysis of Ethyl Acetate is a second order reaction
To solve using graphical methods
15. 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 ~50OC
Mixed with conductivity probe
16. Equal Molar Concentrations
17. Equal Molar ConcentrationsResults Experimental Rate Constant from Data
Theoretical Experimental Rate Constant from Tsujikawa and Inoue
Theoretical Experimental Rate Constant from Mata-Segreda
18. High Concentration of Sodium Hydroxide
19. High Concentration of Sodium Hydroxide Results Slope of experimental line excluding bottom points
m=k(CB0-CA0)=0.00760 (+/- 0.000129)
20. High Concentration Ethyl Acetate
21. High Concentration of Ethyl Acetate Results Slope of experimental line only including reaction region of first few points
m=k(CB0-CA0)=0.0374 (+/- 0.0044)
22. What accounts for theoretical and empirical differences? Overall rate constant consistent with theoretical data
Initial concentration different then planned
23. Equal Molar Concentrations
24. The Continuous Stirred Tank Reactor Add picture of TowerAdd picture of Tower
25. Theoretical CSTR Calculation Second order mixed flow reactor
Graphical Solution
26. Experimental Design for CSTR Filled chemical reservoirs with equal concentration sodium hydroxide and ethyl acetate
Preformed experiment with different flow rates with different concentrations
27. CSTR Data
28. 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
29. CSTR Data
30. 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
31. 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
32. 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
33. 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
34. Questions?...
35. 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 (3rd 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