PARAMETRIC STUDY ON THE EFFECTS OF CO-SOLVENT
(TETRAHYDROFURAN) IN THE PRODUCTION OF METHYL ESTER FROM THE SODIUM HYDROXIDE CATALYZED TRANSESTERIFICATION OF
Jatropha curcas L.
MARY BETH ABESCORO MAGAMPON
A THESIS SUBMITTED TO
THE FACULTY OF THE DEPARTMENT OF CHEMICAL ENGINEERING COLLEGE OF ENGINEERING AND AGRO-INDUSTRIAL TECHNOLOGY
UNIVERSITY OF THE PHILIPPINES LOS BAÑOS
IN PARTIAL FULFILLMENT OF THE REQUIREMENTS FOR THE DEGREE OF
BACHELOR OF SCIENCE IN CHEMICAL ENGINEERING
APRIL 2009
The thesis attached hereto, entitled “PARAMETRIC STUDY ON THE EFFECTS OF CO-SOLVENT (TETRAHYDROFURAN) IN THE PRODUCTION OF
METHYL ESTER FROM THE SODIUM HYDROXIDE CATALYZED TRANSESTERIFICATION OF Jatropha curcas L.” prepared and submitted
by Mary Beth Abescoro Magampon in partial fulfillment of the requirements for the degree of Bachelor of Science in Chemical Engineering, is hereby accepted.
___________________________ __________________________
Engr. Butch G. Bataller Prof. Myra G. Borines
Panel Member Panel Member
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Date Signed Date Signed
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Prof. Rex B. Demafelis Dr. Laura J. Pham
Adviser Co-adviser
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Date Signed Date Signed
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Dr. Jovita L. Movillon Chair
Department of Chemical Engineering
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Date Signed
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Dr. Arsenio N. Resurreccion Dean
College of Engineering and Agro-Industrial Technology University of the Philippines Los Baños
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Date Signed
ABSTRACT
Magampon, Mary Beth A., College of Engineering and Agro-Industrial Technology, University of the Philippines Los Baños, Laguna; April 2009. Parametric study on the effects of co-solvent (tetrahydrofuran) in the production of methyl ester from the sodium hydroxide catalyzed transesterification of Jatropha curcas L.
Adviser: Prof. Rex B. Demafelis Co-adviser: Dr. Laura J. Pham
This parametric study was carried out to determine the effects of co-solvent tetrahydrofuran in methyl ester production from Jatropha curcas L. and to obtain the best operating conditions for transesterification.
Three levels of study were done. The first level was varying the oil to catalyst ratio (1:0.1, 1:0.2, 1:0.3). The chosen best ratio in the first level was 1:0.2 which yields 99% methyl ester after one-hour reaction. In the second level of analysis, the mixing rate was varied (500rpm, 750rpm, 1000rpm). Among the three ratios, 1000 rpm showed the highest methyl ester yield that is 97% at 15 minutes reaction time. For the last level of analysis, the effect temperature was examined. The temperature was increased to 45°C and it yields 99% methyl ester at 15 minutes reaction time.
TABLE OF CONTENTS
Table of Contents v
List of Tables vii
List of Figures ix
Abstract 1
I. Introduction
1.1 Background of the Study 2
1.2 Significance of the Study 3
1.3 Objectives of the Study 5
1.4 Scopes and Limitations of the Study 5
1.5 Date and Place of the Study 6
II. Review of Related Literature
2.1 Biodiesel 7
2.2 Feedstocks of Biodiesel Production
2.2.1 Fats and Oils 8
2.2.2 Alcohol 9
2.2.3 Catalyst 9
2.2.4 Co-Solvent 10
2.3 Transesterification 11
2.4 Variables Affecting Transesterification
2.4.1 Free Fatty Acid 13
2.4.2 Mixing Rate 14
2.2.5 Completion of Reaction 14
2.5. Specifications of Biodiesel 15
2.6. General Parameters of Biodiesel 16
III. Materials and Methodology 3.1 Materials
3.1.1 Chemicals and Reagents 20
3.1.2 Equipment and Glasswares 20
3.2 Methodology
3.2.1 Refining Process of Jatropha curcas L. Oil 21 3.2.2 Pretreatment of Jatropha curcas L. Oil
3.2.2.1 Degumming 21
3.2.2.2 Acid Esterification 21
3.2.2.3 Neutralization 22
3.2.3 Base Transesterification 22
3.2.4 Phase Separation and Washing 23
3.2.5 Thin Layer Chromatography 24
3.2.6 Titrimetric Method 24
IV. Results and Discussion
4.1 Refining Process 26
4.2 Pretreatment Process
4.2.1 Degumming 27
4.2.2 Acid Esterification 28
4.2.3 Neutralization 30
4.3 Transesterification 31
4.3.1 Effect of Varying Catalyst Ratio 31
4.3.2 Effect of Varying Mixing Rate 38
4.3.3 Effect of Varying Temperature 44
4.4 Determination of the Mass Yield 46
V. Summary and Conclusion 49
VI. Recommendation 50
VII. References 51
VIII. Appendices
Appendix A – Sample Calculations 54
Appendix B – Thin Layer Chromatography 57
Appendix C – Titrimetric Method 58
Appendix C - BIOSOFT Quantiscan Program Results 59
Appendix D - Material Data and Safety Sheet 64
Lists of Tables
Table no. Title Page
1 ASTM D 6751-02 Biodiesel Specifications 15
2 Percent composition of Neutralized Jatropha curcas L. Oil 31 determined by the BIOSOFT Quantiacn program.
3 Time Profile of each component in 1:0.2 Oil to catalyst ratio 33 determined by using BIOSOFT Quantiscan program.
4 Time Profile of each component of 1:0.1 oil to catalyst ratio 34 determined by using BIOSOFT Quantiscan program.
5 Time profile of each component of 1:0.3 oil to catalyst ratio 36 determined by using BIOSOFT Quantiscan program.
6 Time Profile of each component for 750 rpm mixing rate ratio 39 determined by using BIOSOFT Quantiscan program.
7 Time profile of each component for 500rpm mixing rate ratio 40 determined by using BIOSOFT Quantiscan program.
8 Time profile of each component for 1000 rpm mixing rate ratio 41 determined by using BIOSOFT Quantiscan program.
9 Time Profile of each component for the ratio that used 45°C 44 temperature determined by using BIOSOFT Quantiscan program.
A.1 Amount of Reagents used in First Level of Analysis 56 (varying oil to catalyst ratio)
D.1 Net Area of each component in 1:0.1 oil to catalyst ratio 750rpm 59 Mixing rate and at room temperature determined by using
BIOSOFT Quantiscan program
D.2 Net Area of each component in 1:0.2 oil to catalyst ratio with 750rpm 60 Mixing rate and at room temperature determined by using
BIOSOFT Quantiscan program
D.3 Net Area of each component in 1:0.3 oil to catalyst ratio with 750rpm 60 mixing rate and at room temperature determined by using BIOSOFT Quantiscan program
D.4 Net Area of each component in 500rpm mixing rate 61 with 1:0.2 oil to catalyst ratio at room temperature determined
by using BIOSOFT Quantiscan program
D.5 Net Area of each component for 750rpm mixing rate 62 with 1:0.2 oil to catalyst ratio at room temperature determined
by using BIOSOFT Quantiscan program
D.6 Net Area of each component for 1000rpm mixing rate 62 with 1:0.2 oil to catalyst ratio at room temperature determined
by using BIOSOFT Quantiscan program
D.7 Net Area of each component for 1000rpm mixing rate 63 with 1:0.2 oil to catalyst ratio at 45°C temperature determined
by using BIOSOFT Quantiscan program
Lists of Figures
Figure no. Title Page
1 Transesterification Reaction Mechanism 11
2 Refined Jatropha curcas L. oil 26
3 Thin layer chromatogram of refined Jatropha curcas L. oil 26
4 Degumming of Jatropha curcas L. oil 27
5 Thin layer chromatogram of degummed Jatropha curcas L. oil 27
6 Acid Esterificatin Set-up 28
7 Separation set-up for Acid Esterification 29
8 Neutralization Set-up 30
9 Thin layer chromatogram of Neutralized Jatropha curcas L. Oil 30 10 Thin layer chromatogram of 1:0.2 oil to catalyst ratio for biodiesel 32
production using Jatropha curcas L. oil
11 Thin layer chromatogram of 1:0.1 oil to catalyst ratio for biodiesel 34 production using Jatropha curcas L. oil
12 Thin layer chromatogram of 1:0.3 oil to catalyst ratio for biodiesel 36 production using Jatropha curcas L. oil
13 Front view of 1:0.3 oil to catalyst ratio with soap formation 37
14 Top view of 1:0.3 oil to catalyst ratio with soap formation 37 15 Biodiesel of the three oil to catalyst ratios 37 16 % Methyl ester vs. Time for the three ratios 37 17 Thin layer chromatogram of 750 rpm mixing rate for biodiesel 39
production using Jatropha curcas L. oil
18 Thin layer chromatogram of 500 rpm mixing rate for biodiesel 40 production using Jatropha curcas L. oil
19 Thin layer chromatogram for 1000rpm for biodiesel production 41 using Jatropha curcas L. oil
20 Methyl ester produced from the three ratios of mixing rate 43
21 % Methyl ester yield vs Time of the three mixing ratios 43
22 Thin layer chromatogram of 45°C for biodiesel production using 44 Jatropha curcas L. oil
23 Methyl ester produced from two temperature ratios 45 24 % Methyl ester vs Time of the two temperature ratios 45 25 Settling set- up of the biodiesel and glycerol layers 47 26 Washing of the methyl ester layer with water 47 27 Methyl ester produced from the transesterification of 48
Jatropha curcas L. oil with 1:8:1:0.2 Oil to methanol to
tetrahydrofuran to sodium hydroxide ratio with 1000 rpm mixing rate at 45°C
D.1 Quantiscan Result of 1:0.1 Oil to Catalyst Ratio with 750rpm 59 Mixing rate and at room temperature
D.2 Quantiscan Result of 1: 0.2 Oil to Catalyst Ratio with 750 rpm 59 mixing rate at room temperature at 60 min
D.3 Quantiscan Result of 1: 0.3 oil to catalyst ratio with 750 rpm 60 mixing rate at room temperature at 60 min
D.4 Quantiscan result for 500rpm mixing rate with 1:0.2 oil to catalyst 61 ratio at room temperature at 60 min
D.5 Quantiscan result for 750rpm mixing rate with 1:0.2 oil to catalyst 61 ratio at room temperature at 60 min
D.6 Quantiscan Result for 1000rpm mixing rate with 1:0.2 oil to catalyst 62 ratio at room temperature at 60 min
D.7 Quantiscan Result for 1000rpm mixing rate with 1:0.2 oil to catalyst 63 ratio at 45°C temperature at 60 min
