Taeka Haileleul MSc Thesis

149 Pages·2015·2.23 MB·English

ADDIS ABABA UNIVERSITY

SCHOOL OF GRADUATE STUDIES
ADDIS ABABA INSTITUTE OF TECHNOLOGY
SCHOOL OF CHEMICAL AND BIO ENGINEERING

Vernonia
galamensis
Fatliquor Product Development from
Seed Oil via Modified Sulphitation Process

By
Senait Gebey ehu Nadew

DECEMBER, 2014
ADDIS ABABA, ETHIOPIA
ADDIS ABABA UNIVERSITY
SCHOOL OF GRADUATE STUDIES
ADDIS ABABA INSTITUTE OF TECHNOLOGY
SCHOOL OF CHEMICAL AND BIO ENGINEERING

Vernonia
galamensis
Fatliquor Product Development from
Seed Oil via Modified Sulphitation Process
A thesis Submitted to the Research and Graduate School of Addis Ababa
University, Addis Ababa Institute of Technology, School of Chemical and Bio
Engineering in partial fulfillment of the requirements for the attainment of
the Degree of Masters of Science in Chemical Engineering under Process
Engineering Stream.

By:Senait Gebeyehu Nadew
Advisor: Ato Gizachew Shif eraw (Assistant Professor)

DECEMBER, 2014
ADDIS ABABA, ETHIOPIA
ADDIS ABABA UNIVERSITY
SCHOOL OF GRADUATE STUDIES
ADDIS ABABA INSTITUTE OF TECHNOLOGY
SCHOOL OF CHEMICAL AND BIO ENGINEERING

Vernonia galamensis
Fatliquor Product Development from Seed
Oil via Modified Sulphitation Process
By

Senait Gebeyehu Nadew

Approved by the Examining Board:

Chairman Department’s Signature Date
Graduate Committee

Ato Gizachew Shiferaw

Advisor Signature Date

Ato Teshome Worku

Internal Examiner Signature Date

Ato Lelissa Daba

External Examiner Signature Date
Fatliquor Product Development from Vernonia galamensis Seed Oil via Modified Sulphitation Process
Acknowledgment

First of all I would like to thank the Almighty and merciful God for giving me the health,
strength, patience and calm throughout the entire situation and challenge that I faced for
successful completion of this thesis.
Next I wish to express my deepest gratitude to my advisor Ato Gizachew Shiferaw for his
invaluable comments and excellent supervision. I must also thank him for the appreciation and
encouragement showed towards me, which was very helpful and very much cherished.
I would also like to thank School of Chemical and Bio Engineering Laboratory staff members
especially Ato Hintsasilasie Seifu for his technical assistance during experimental work; Leather
Industry Developemt Institute staffs especially Ato Addisu Mamo, W/t Feruza Yimam, Ato
Binyam Afework, Ato Wondosen Mamuye, Ato Dereje Taddesse and Ato Petros A. for their
professional advice and support during experimental works; Adet Agricultural Research Center
exceptionally W/t Yeruke Tilahun, Ato Cherenet Alem and Ato Belayneh Mezgebu for the raw
material acquirement; and Bahir Dar University especially Ato Tsega Yenew and Ato Mulu Adera
for their technical assistance during experimental work.
My deepest gratitude also goes to my best friends especially Ato Michael Moreda for being
there and helpful in many ways.
My special thanks goes to my dearest family members exceptionally to my mother W/o
Achamyelesh Eshete, my aunt W/o Etenesh Eshete and my brother Ato Wasihun Desta for their
encouragement and support towards my thesis and academic career.

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Fatliquor Product Development from Vernonia galamensis Seed Oil via Modified Sulphitation Process
Table of Contents
Contents Page
Acknowledgement ........................................................................................................................... i
Table of Contents .............................................................................................................................ii
List of Tables ..................................................................................................................................vii
List of Figures ..................................................................................................................................x
Acronyms ....................................................................................................................................... xii
Abstract ......................................................................................................................................... xiii
1. Introduction ...................................................................................................1
1.1 Background............................................................................................................................ 1
1.2 Statement of the Problem..................................................................................................... 2
1.3 Objective of the Research ..................................................................................................... 3
1.3.1 General Objective ........................................................................................................... 3
1.3.2 Specific Objectives .......................................................................................................... 3
1.4 Significance of the Study ....................................................................................................... 4
1.5 Scope of the Study ................................................................................................................ 4
2. Literature Review ...........................................................................................5
2.1 Introduction........................................................................................................................... 5
2.2 Raw Materials for Fatliquor Production................................................................................ 6
2.2.1 Vernonia Seed Oil .......................................................................................................... 7
2.2.2 Sodium Bisulphite ......................................................................................................... 11
2.3 Fatliquor Production Technologies ..................................................................................... 12
2.3.1 Saponification Process .................................................................................................. 13
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Fatliquor Product Development from Vernonia galamensis Seed Oil via Modified Sulphitation Process
2.3.2 Sulphation Process........................................................................................................ 13
2.3.3 Sulphitation Process ..................................................................................................... 15
2.3.4 Modified Sulphitation Process...................................................................................... 16
2.4 Parameters Affecting Modified Sulphited Fatliquor Production ........................................ 18
2.4.1 Reaction Temperature .................................................................................................. 18
2.4.2 Amount and Concentration of Sodium Bisulphite........................................................ 18
2.4.3 Reaction Time ............................................................................................................... 19
2.4.4 Mixing Speed ................................................................................................................ 19
2.4.5 Oil to FAME Weight Ratio ............................................................................................. 19
2.4.6 Purity of Reactants........................................................................................................ 20
2.5 Properties and Specification of Sulphited Fatliquor ........................................................... 20
2.5.1 Physical Conditions ....................................................................................................... 20
2.5.2 Emulsion Characteristics............................................................................................... 21
2.5.3 Odor .............................................................................................................................. 21
2.5.4 Chemical Requirements................................................................................................ 21
2.6 Fatliquoring .......................................................................................................................... 23
3. Materials and Methods ................................................................................25
3.1 Materials.............................................................................................................................. 25
3.2 Equipments.......................................................................................................................... 25
3.3 Experimental Method ......................................................................................................... 27
3.3.1 Preparation of Vernonia Seed ...................................................................................... 27
3.3.2 Extraction of Vernonia Oil............................................................................................. 27
3.3.3 Purification of Crude Vernonia Oil................................................................................ 28

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Fatliquor Product Development from Vernonia galamensis Seed Oil via Modified Sulphitation Process
3.3.4 Characterization of Vernonia Oil .................................................................................. 29
3.3.5 Experimental Design for Fatliquor Production ............................................................. 33
3.3.6 Experimental Setup....................................................................................................... 36
3.3.7 Sulphited Fatliquor Production Procedure ................................................................... 37
3.3.8 Feed Material Requirement.......................................................................................... 37
3.3.9 Yield of Sulphited Fatliquor .......................................................................................... 38
3.3.10 Characterization of Sulphited Fatliquor ..................................................................... 38
3.4 Application of Sulphited Fatliquor on Leather and Determination of Physicochemical
Properties of Fatliquored Leather ............................................................................................. 43
3.4.1 Application of Fatliquor on Leather.............................................................................. 43
3.4.2 Visual Tests ................................................................................................................... 44
3.4.3 Physical Tests ................................................................................................................ 44
4. Results and Discussion ..................................................................................46
4.1 Vernonia Seed Preparation, Oil Extraction, Purification and Characterization .................. 46
4.1.1 Vernonia Seed Preparation........................................................................................... 46
4.1.2 Vernonia Oil Extraction ................................................................................................. 46
4.1.3 Vernonia Oil Purification............................................................................................... 46
4.1.4 Physicochemical Properties Of Purified Vernonia Oil .................................................. 47
4.2 Analysis of Sulphited Fatliquor Production ........................................................................ 51
4.2.1 Statistical Analysis on Factors Affecting Degree of Sulphitation.................................. 51
4.2.2 Effect of Sulphitation Reaction Process Variables........................................................ 57
4.3 Yield of Sulphited Fatliquor ................................................................................................. 66
4.4 Physicochemical Properties of Sulphited Fatliquor ............................................................ 68

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Fatliquor Product Development from Vernonia galamensis Seed Oil via Modified Sulphitation Process
4.4.1 Physical Conditions ....................................................................................................... 68
4.4.2 pH of Emulsion .............................................................................................................. 69
4.4.3 Total Active Ingredient ................................................................................................. 71
4.4.4 Unsaponifiable Matter.................................................................................................. 72
4.4.5 Total Alkalinity .............................................................................................................. 73
4.4.6 Total Sulphur as Sulphites ............................................................................................ 74
4.4.7 Total Ash ....................................................................................................................... 76
4.5 Application of Sulphited Fatliquor on Leather and Determination of Physicochemical
Properties of Fatliquored Leather ............................................................................................. 77
4.5.1 Visual Tests ................................................................................................................... 77
4.5.2 Physical Tests ................................................................................................................ 78
5. Preliminary Feasibility Study.........................................................................82
5.1 Process Description for Sulphited Fatliquor Production..................................................... 82
5.2 Material Balance ................................................................................................................. 84
5.3 Energy Balance .................................................................................................................... 90
5.4 Preliminary Equipment Specifications and Sizing ............................................................... 98
5.5 Total Capital Investment ................................................................................................... 102
5.6 Production Costs ............................................................................................................... 104
5.6.1 Raw Material Cost....................................................................................................... 104
5.6.2 Operating Labor .......................................................................................................... 104
5.6.3 Utilities Cost ................................................................................................................ 105
5.7 Financial Appraisal............................................................................................................. 106
6. Conclusion and Recommendation .............................................................. 110

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Fatliquor Product Development from Vernonia galamensis Seed Oil via Modified Sulphitation Process
6.1 Conclusion ......................................................................................................................... 110
6.2 Recommendation .............................................................................................................. 111
Reference....................................................................................................... 112
Appendices .................................................................................................... 116
Appendix A: Composition of Vernonia Oil .................................................................................. 117
Appendix B: Standard Specification of Sulphited Fatliquor........................................................ 120
Appendix C: Experimental Result ............................................................................................... 121
Appendix D: Calculation Part ...................................................................................................... 127
Appendix E: Production Capacities of Leather Factories ........................................................... 130
Appendix F: Technical Data ........................................................................................................ 131

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Fatliquor Product Development from Vernonia galamensis Seed Oil via Modified Sulphitation Process
List of Tables

Table 2.1: Physical and chemical properties of Vernonia oil .......................................................... 9
Table 2.2: Physical and chemical property of sodium bisulphite (solid and 40% solution) ......... 11
Table 2.3: Chemical properties requirement................................................................................ 22
Table 2.4: Quality requirement for the main type of leather (General data) .............................. 24
Table 3.1: Independent variables and levels used in the CCD for the fatliquor production ........ 34
Table 3.2: The complete experimental design matrix .................................................................. 35
Table 3.3: The weight of wet blue and amount of sulphited fatliquor used ................................ 44
Table 4.1: Moisture content determination for Vernonia seed ................................................... 48
Table 4.2: Physicochemical properties of purified Vernonia oil ................................................... 51
Table 4.3: Experimental and predicted values ............................................................................. 53
Table 4.4: ANOVA for the regression model equation and coefficients ...................................... 56
Table 4.5: Yield of sulphited fatliquor........................................................................................... 67
Table 4.6: pH of 10% emulsion of sulphited fatliquor .................................................................. 70
Table 4.7: Total active ingredient of sulphited fatliquor .............................................................. 72
Table 4.8: Unsaponifiable matter of sulphited fatliquor .............................................................. 73
Table 4.9: Total alkalinity of sulphited fatliquor ........................................................................... 74
Table 4.10: Total sulphur as sulphites (SO ) of sulphited fatliquor.............................................. 75
3
Table 4.11: Total ash content of sulphited fatliquor .................................................................... 76
Table 4.12: Visual evaluation of synthesized and controlled tests............................................... 78
Table 4.13: Summary of physical tests ......................................................................................... 79
Table 5.1: Comparisons of sulphited fatliquor technology characteristics .................................. 83

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