Determination Of Optimal Conditions For Biodiesel Production From Jansa Seed Oil Using Lithium-Doped Catalysts
ABSTRACT
This study
presents an empirical analysis of biodiesel production from Jansa seed oil
using tranesterification process. Following the quest to achieve improved
economic viability and clean production process for biodiesel, lithium ion from
lithium carbonate was applied to improve the catalytic properties of calcium
oxide and magnesium oxide for biodiesel production. Oil produced from jansa
seed was characterized to determine its suitability for biodiesel production.
Based on the characterization, an appreciable oil weight or yield of 38.09% was
produced. Also, 0.493mgKOH/kg free fatty acid (FFA) content, 205.923 gKOH/kg
saponification value and 99.95% ester value which specified its great tendency
to be converted into methyl ester (biodiesel) were obtained. Li-CaO and Li-MgO
catalysts were prepared in diverse concentrations for use in biodiesel
production. Li-CaO-1.50 and Li-MgO-1.50 gave the optimal yield of 76 and 83%
volume of biodiesel. These were applied to study the effects of other process
parameters (reaction time, reaction temperature, agitation speed, and methanol
to oil molal ratio) and optimized using a matrix design. Li-CaO-1.50 gave the optimal yield at other
process conditions. A two level, five experimental design matrix was used for
transesterification studies for 32 experimental runs using Li-CaO as catalyst.
Set of conditions that gave the optimal yield were; catalyst concentration of 1.5 % weight, reaction time of 3 hours,
temperature of 600C, methanol and oil molal ratio of 12:1 and
agitation speed of 500 rpm respectively. All possible interactions, predicted and
actual values, final equation in terms of coded factors and interaction plots
were identified. Biodiesel blends from optimal yield of the metallic oxides of
the catalysts were formulated and characterized to further determine the
physicochemical properties (calorific value, anisidine point, API gravity,
diesel index, flash and fire points, cloud and pour points) which were within
the ASTM D6751 standard recommendations for use in compression ignition
engines. Scanning electron microscopy (SEM) was used to study the active sites
of the surface structure of the catalyst in relation to various modifications.
The sample indicated increased points of higher porosity as lithium
concentration increased (1.5, 2.0 and 2.5%) and less porosity at 0.5 and 1.0%
concentration. Gas chromatography (GC) and Fourier transform infrared
spectrometry (FTIR) of the jansa seed oil and biodiesel produced were carried
out. A total of 7 compounds were identified in the oil of which 4 were FFAs and
other 3 were biodiesel esters. For the biodiesel, a total of 12 compounds were
identified, of which 9 were methyl esters and 3 non esters, thus, producing
88.35% methyl ester concentration at optimal yield sample. Evidently, the same
functional groups identified in the jansa seed oil were present in the optimal
biodiesel yield sample which includes; the hydrocarbon group (as a basic
characteristics of bio-oil),a halide group and an ester group (as the basic
characteristics of biodiesel). Overall, the optimal products developed were
found to meet standard properties for biodiesel through free fatty acid methyl
ester (FAME) profile test and functional group validation. At such, Li-CaO, Li-MgO,
other similar materials should be adopted as catalyst for the production of
biodiesel to bridge the energy gaps.
TABLE OF
CONTENTS
Page
Cover Page
i
Title Page ii
Declaration ii
Dedication iv
Certification v
Acknowledgements vi
Table of Contents vii
List of Tables xi
List of Figures xii
Abstract xv
CHAPTER 1: INTRODUCTION
1.1
Background
of the Study 1
1.2
Statement
of Problem 2
1.3
Aim and
Objectives of Study
3
1.4
Scope of
Study 3
1.5
Justification
of Study
4
CHAPTER 2:
LITERATURE REVIEW
2.1 Catalysts and
Compositional Properties 5
2.2 Basic Solid Catalysts 5
2.2.1 MgO as Base Heterogeneous
Catalyst 6
2.2.2 CaO as a Base Heterogeneous
Catalyst 7
2.2.3 SrO as a Base Heterogeneous
Catalyst 8
2.2.4 Biodiesel Production with
Mixed Metal Oxide and Derivatives 8
2.2.5
Biodiesel Production with Transition Metal Oxide and Derivatives 9
2.2.6 Waste Material-Base
Heterogeneous Catalysts 11
2.3 Acidic Solid Catalysts 12
2.3.1 Acid-Base Solid Catalysts 13
2.4 Adoption
of the Catalysts for the Study
15
2.5 Summary of Literature
17
CHAPTER 3: MATERIALS AND METHODS
3.1 Materials 19
3.1.1 Glass Wares and other Consumables 19
3.1.2 Analytical Grade Reagents 19
3.1.3 Electronic Equipment 19
3.2 Methods 19
3.2.1 Sample Collection and Preparation 19
3.2.2 Oil Extraction (Soxhlet Method) 20
3.2.3 Oil Characterization 21
3.2.4 Catalyst Preparation 26
3.2.5 Effects of Process Parameters on the
Biodiesel Production 26
3.3 Design of Experiment for Biodiesel
Production 28
3.3.1 Fractional Factorial Design of Experiment
for Biodiesel Production 28
3.4 Biodiesel Blends Preparation and Characterization 31
3.5 Gas
Chromatography – Mass Spectrometry (GC-MS) Analysis of the
Raw
Oil and the Biodiesel 33
3.6 Fourier Transform Infra-Red Spectrometry
(FTIR) of Raw Oil and Biodiesel 33
3.7 Scanning Electron Microscopy (SEM) of the
Catalysts 34
CHAPTER 4: RESULTS AND DISCUSSION
4.1
Characterization Test Result of the Jansa seed Bio-Oil 35
4.2 Gas Chromatography Mass Spectrometry
(GC-MS) Analysis
Test
Results of the Jansa Seed Oil 36
4.3 Scanning
Electronic Microscopy (SEM) of the Lithium-Ions-Doped Metallic
Oxides
Catalysts for Biodiesel Production 39
4.4 Effects of the Process Parameters on the
Biodiesel Production Yield
using the Lithium-Doped CaO and MgO
Catalysts Variants 42
4.4.1 Effect of Catalyst Concentration Variation
on the Biodiesel Yield 43
4.4.2 Effect of Reaction Time Variation on the
Biodiesel Yield 44
4.4.3
Effect of Reaction Temperature Variation on the Biodiesel Yield 44
4.4.4 Effect of Agitation Speed Variation on the
Biodiesel Yield 45
4.4.5 Effect of Methanol and Sample Molal Ratio
Variation on the Biodiesel Yield
45
4.5 Results for Optimization Yield Studies
of the Biodiesel Production using the
Fractional Factorial Matrix Design 46
4.5.1 Predicted and Actual Values for Biodiesel
Production from the Jansa Seed Oil.
46
4.5.2 Analysis of Variance (ANOVA) for Quadratic
Model 48
4.5.3 Fit Statistics Results for the Biodiesel
Production from the Jansa Seed Oil 50
4.5.4 Results for the Coefficient in Terms of
Coded Factors for the Biodiesel
Production
50
4.5.5 Matrix Design Final Equation Developed in Terms of Coded Factors
for the Effects
of the Process Parameters on
Biodiesel Produced from the Jansa Seed Oil 51
4.6 Interactions of Significant Variables
and Process Factors on the
Biodiesel Yield
53
4.6.1 Results of the Predicted and the Actual Interactions of Variables 53
4.6.2 3-Dimensional (3D) Plots Interactions
Results of the Process Variables
with
the Biodiesel Yield. 53
4.7 Characterization of the
Developed Biodiesel from the Jansa Seed Oil 59
4.7.1
Physicochemical Characterization Test
Result of the Optimal Biodiesel
Yield
and the Blends from the Jansa Seed Oil. 59
4.7.2 Gas
Chromatography of the Optimal Biodiesel Yield from the Jansa Seed Oil 65
4.7.3
Fourier Transfer Infrared Test Results of the Optimal Biodiesel
Yield 68
CHAPTER 5: CONCLUSION AND RECOMMENDATIONS
5.1
Conclusion 69
5.1.1 Contributions to Knowledge of this Study 71
5.2 Recommendations 71
References
72
Appendices 81
LIST
OF TABLES
Page
3.1 Studied
range of each factor in actual and coded form for heterogeneous catalysts 29
3.2 Experimental design matrix for
transesterification studies catalyzed by
lithium-ions-doped calcium and
magnesium oxides 30
4.1 Physicochemical
properties of the jansa bio-oil 35
4.2
FFAs profile identified in Cussonia
bateri seed oil by GC 38
4.3 Fourier transform infrared spectrometry
(FTIR) analysis of raw jansa seed oil 39
4.4 Predicted and actual values for
biodiesel production from the jansa seed oil 47
4.5 ANOVA results for quadratic model for the
jansa seed oil biodiesel production
(Response 1: Biodiesel yield)
49
4.6 Fit Statistics result for the biodiesel
production 50
4.7 Results for the coefficients in terms of
the coded factors for the biodiesel
production 51
4.8 Methyl
esters identified in the optimal biodiesel yield by gas chromatography
67 4.9 FTTR analysis of the optimal biodiesel yield from the
jansa seed oil 68
LIST OF FIGURES
Page
2.1 Mechanism of SrO catalyst
transesterification adapted 8
2.2 Flow chart for biodiesel production from
heterogeneous catalyst (Lee et al.,
2015) 10
3.1 Soxhlet apparatus set-up for bio-oil
extraction from jansa seed 20
4.1 Gas
chromatography column over ramping schedule of the jansa seed oil 36
4.2 Gas chromatograph of Cussonia bateri
seed oil showing elution peaks of FFAs 37
4.3 Fourier transform infrared spectrometry
(FTIR) of oil jansa seed oil 39
4.4
Scanning electron microscopy of
lithium doped metal oxides 42
4.5 Variation of biodiesel yield with catalyst
variants for the initial biodiesel production 43
4.6
Effect of process conditions
variation on biodiesel yield
43
4.7
Effect of reaction time variation on
the biodiesel yield
44
4.8 Effect
of reaction temperature variation on the biodiesel yield 44
4.9 Effect of agitation speed variation on the
biodiesel yield
45
4.10 Effect of methanol and sample molal ratio
variation on the biodiesel yield 45
4.11 Predicted versus actual plots for the
biodiesel yield
53
4.12 3D plot of Catalyst concentration and
reaction temperature with biodiesel yield 54
4.13 3D plot of Catalyst concentration and
reaction time with biodiesel yield 54
4.14 3D plot of Catalyst concentration and
agitation speed with biodiesel yield 55
4.15 3D plot of Catalyst concentration and molal
ratio with biodiesel yield 55
4.16
3D plot of reaction temperature and
reaction time with biodiesel yield 56
4.17 3D plot of reaction temperature and
agitation speed for the biodiesel yield 57
4.18 3D plot of reaction temperature and molal
ratio for the biodiesel yield 57
4.19 3D plot of reaction time and agitation speed
with biodiesel yield
58
4.20 3D plot of reaction time and molal ratio
with the biodiesel yield 58
4.21
3D plot of agitation speed and molal
ratio with the biodiesel yield 59
4.22 Variations of specific gravity with the
fuel blends
59
4.23 Variations of kinetic viscosity with the
fuel blends
60
4.24 Variations of flash point with the fuel
blends
61
4.25 Variations of fire point with the fuel
blends
61
4.26
Variation of cloud point with the fuel
blends
62
4.27 Variations of pour point with the fuel
blends
62
4.28 Variations of free fatty acid with the fuel
blends
63
4.29 Variations of API gravity with the fuel
blends
63
4.30 Variations of anisidine value with the fuel
blends
64
4.31 Variation of diesel index with the fuel
blends
64
4.32 Variation of calorific value with the fuel
blends
65
4.33 Gas
chromatography column-oven ramping schedule of methyl ester (biodiesel)
analysis
66
4.34 Chromatogram of the optimal biodiesel
yield from the jansa seed oil showing elution
peaks of the methyl ester
67
4.35 Fourier transform infrared spectrometry
(FTIR) of the optimal biodiesel yield from
jansa seed oil
68
0.0
EKWUEME, I (2023). Determination Of Optimal Conditions For Biodiesel Production From Jansa Seed Oil Using Lithium-Doped Catalysts. Repository.mouau.edu.ng: Retrieved Apr 27, 2024, from https://repository.mouau.edu.ng/work/view/determination-of-optimal-conditions-for-biodiesel-production-from-jansa-seed-oil-using-lithium-doped-catalysts-7-2
INNOCENT, EKWUEME. "Determination Of Optimal Conditions For Biodiesel Production From Jansa Seed Oil Using Lithium-Doped Catalysts" Repository.mouau.edu.ng. Repository.mouau.edu.ng, 31 Aug. 2023, https://repository.mouau.edu.ng/work/view/determination-of-optimal-conditions-for-biodiesel-production-from-jansa-seed-oil-using-lithium-doped-catalysts-7-2. Accessed 27 Apr. 2024.
INNOCENT, EKWUEME. "Determination Of Optimal Conditions For Biodiesel Production From Jansa Seed Oil Using Lithium-Doped Catalysts". Repository.mouau.edu.ng, Repository.mouau.edu.ng, 31 Aug. 2023. Web. 27 Apr. 2024. < https://repository.mouau.edu.ng/work/view/determination-of-optimal-conditions-for-biodiesel-production-from-jansa-seed-oil-using-lithium-doped-catalysts-7-2 >.
INNOCENT, EKWUEME. "Determination Of Optimal Conditions For Biodiesel Production From Jansa Seed Oil Using Lithium-Doped Catalysts" Repository.mouau.edu.ng (2023). Accessed 27 Apr. 2024. https://repository.mouau.edu.ng/work/view/determination-of-optimal-conditions-for-biodiesel-production-from-jansa-seed-oil-using-lithium-doped-catalysts-7-2