12 Finally Edited

Federal TVET Institute
Mechanical Division
Department of Automotive Technology
Assessment of Tribological Properties of Bio-Grease Lubricant
of Soybean oil using Sugarcane Filter Cake Oil with Wax as
Additive
A thesis submitted in partial fulfillment of the requirements for the award of the
degree of Master of Science in Automotive Management Technology
Master of Science in Automotive Technology
By
Tsegaye Wolde Tezho
Advisor: Prof. Pedro Dionisio Remedios C. (PhD.)
December 2020 G.C
Addis Ababa, Ethiopia

Federal TVET Institute
Mechanical Division
Department of Automotive Technology
Assessment of tribological properties of bio-grease lubricant of
Soybean oil using Sugarcane Filter Cake Oil with Wax as Additive
A thesis submitted in partial fulfillment of the requirements for the
Award of Degree of Master of Science in
Automotive Management Technology
By
Tsegaye Wolde Tezho…..ID/272/11
Approved by Board of Examiners

___________________________________ ______ _______
Chairman, Department Graduate Committee Signature Date
________________ _______ _______
Internal Examiner Signature Date
_________________ _______ _______
External Examiner Signature Date
_______________ ________ _______
Adviser Signature Date

Assessment of tribological properties of bio-grease lubricant of Soybean oil using sugarcane oil with wax as additive
CANDIDATE’S DECLARATION
A declaration, I declare that this thesis entitled “Assessment of tribological properties of bio-grease
lubricant of Soybean oil using sugarcane oil with wax as an additive” is my original work, and has
not been presented by any other person for an award of a degree in this or any other university.
Name: Tsegaye Wolde
Signature: ---------------------------------- Date: -----------------------------
Advisor; Prof. Pedro Dionisio Remedios C (PhD.)
Signature: ---------------------------------- Date: -----------------------------
Date of submission: December 2020 GC
Place: Federal TVEL Institute, Ethiopia
i
Acknowledgment
First of all, I would like to thanks the almighty God for everything. I am endlessly grateful to my advisor
Dr. Pedro Dionisio Remedios Castaneiras for all his guidance, comments, technical and moral advice
to make this thesis possible and to complete it on time. Besides, I would also like to thank my parents
for all their support. They help me to realize how important our education is, as well as how essential
it is to the rest of my life. I would like to thanks my friend, Habtamu D. Hailemichael, for all his editing,
gathering data, downloading files, moral advice. Also, I would like to thanks my friend Ambachew
Jachen, for preparing the laboratory materials.
Finally, I would like to thank all my friends for their advice and help throughout the thesis.
ii
Abstract
The purpose of this research thesis is to focus on the preparation of bio-grease lubricants using the
alternative additive of Sugarcane Filter Cake Oil with 50% Sugarcane Filter Cake Wax (SCW) instead
of traditional additive and Soybeans oil as a based oil to improve the tribological properties and it’s
analyzed. The research is conducting by using the experimental method and analyzing. This experiment
is use standard ways for each test per item. To meet the aim of this research thesis, ten samples of bio-
greases lubricant produced in different ratios of thickener and additive according to the factorial matrix.
Characteristics of greases for Performance like dropping point temperature, viscosity, wear, and
coefficient of friction (COF) were investigated. All the ten tested produced samples were inside of the
ranges of functionality but three of the product (Sample-1of 2.0% of LiOH, 2.2 % SCW and 22.5 min;
Sample-5 of 3.5 % LiOH, 3.5% SCW, and 22.5 min and Sample-10 of 5.0% of LiOH, 3.5% SCW, and
30 min) showed a very good set of characteristics. This is the attribute to the optimized concentrations
of hydroxide, SCW, and time of reaction. Especially sample-5 Composites of 5.0% LiOH, 3.5% SCW,
and 30 min exhibited the best performance with relatively from the ten samples of the produced; higher
dropping point of 130℃ and viscosity of 0.5 Pas, lowest wear of 0.0327g and COF of 0.0307.
Comparing with the mineral grease, sample-5 exhibited better performance in all characteristics except
for the dropping point temperature and comparing from the similar product Soybean as based oil but
used different additive. Therefore, these bio-greases can be used in different industrial machinery, for
heavy-duty vehicles and any heavy machinery to reduce the frictional force and wears.
iii
Table of Contents
CANDIDATE’S DECLARATION ...................................................................................................... i
Acknowledgment ............................................................................................................................ ii
Abstract .......................................................................................................................................... iii
List of figures ................................................................................................................................. vi
List of tables .................................................................................................................................. vii
List of abbreviations ...................................................................................................................... ix
Definition of key terms .................................................................................................................. ix
CHAPTER ONE ............................................................................................................................... 1
1. Introduction ................................................................................................................................. 1
1.1 Background of the thesis ........................................................................................................... 1
1.2 Statement of the Problem .......................................................................................................... 3
1.3 Objective of the thesis ............................................................................................................... 4
1.3.1 General objective ............................................................................................................ 4
1.3.2 Specific objective ............................................................................................................ 4
1.4 Scope of the thesis/ Delimitation of the thesis .......................................................................... 4
1.5 Limitation of the thesis ............................................................................................................. 4
1.6 Significance of the thesis .......................................................................................................... 5
1.7 Hypothesis................................................................................................................................. 5
1.8 Organization of the thesis ......................................................................................................... 5
CHAPTER TWO ............................................................................................................................ 6
2. Literature Review........................................................................................................................ 6
2.1 Overview ................................................................................................................................... 6
2.2 Elements of grease .................................................................................................................. 10
2.3 Physicochemical Characteristics of Vegetable oil. ................................................................. 18
2.4 Function of grease ................................................................................................................... 19
2.5 Lubricating grease Uses or Application .................................................................................. 20
2.6 The difference between lubricating grease and lubricating oil/ liquid ................................... 20
2.7 Characteristics of lubricating greases ..................................................................................... 22
2.8 Common types of greases and characteristics of grease ......................................................... 24
2.9 Factor affecting the quality of grease ...................................................................................... 26
iv
2.10 Tribological property of grease ............................................................................................. 26

2.11. Grease Manufacturing Methods ........................................................................................... 28
CHAPTER THREE ...................................................................................................................... 32
3. Design, Methods, and Materials ............................................................................................... 32
3.1 Overall Methodology .............................................................................................................. 32
3.2 Material selection and design of an experiment to conduct Lubricant Biogreases ................. 32
3.2.1 Material Selection ........................................................................................................ 32
3.2.2 Laboratory Equipments ................................................................................................ 33
3.2.3 Design of an experiment to conduct lubrication of bio grease .................................... 33
3.3 Methodology ........................................................................................................................... 36
3.3.1 Standard Experimental technique to produce lubricating grease ................................. 36
3.3.2 Experimental procedure used in this research to produced Bio-greases...................... 37
3.3.3 Method of processing and Analysis ............................................................................. 38
3.4 Grease characterization for performance ................................................................................ 38
CHAPTER FOUR ........................................................................................................................... 45
4 Result and Discussion ................................................................................................................ 45
4.1 Result ...................................................................................................................................... 45
4.1.1 Physiochemical properties of produced Biogreases .................................................... 45
4.1.2 Characteristics of lubricating greases or Performance of Grease characterization ...... 49
4.2 Discussion ............................................................................................................................... 61
CHAPTER FIVE ............................................................................................................................. 76
5. Conclusion, Recommendation, and Future work ...................................................................... 76
5.1 Conclusion...................................................................................................................... 76
5.2 Recommendation ............................................................................................................ 77
5.3 Future work .................................................................................................................... 77
BIBLIOGRAPHY ....................................................................................................................................... 78
APPENDIX /ANNEXES ............................................................................................................................ 81
Appendix 1 .................................................................................................................................... 81
Annexes 2...................................................................................................................................... 82
Annexes 3...................................................................................................................................... 87
Budget ........................................................................................................................................... 87
v
List of figures
Figure 2.1 Lubricating grease and bio lubricating greases…………………………………….…......7
Figure 2.2 Global industrial greases sales breakdown………………………………..…..….………8
Figure 2.3 Elements/ composition of greases………….………………………………………..…...11
Figure 2.4 The flow chart of the batch is processing to manufacturing greases……………..……...28
Figure 2.5 Continuous Process Flow chart of Continuous Process.…………………………..……..30
Figure 3.1 Flowchart of Experimental Factor…………………………………….…………………36
Figure 3.2 Flow chart of Experiments according to the matrix…………………….………………..37
Figure 4.1:- High amount of thickener and additive in the production of Bio-grease…..……...……46
Figure 4.2: Sample production of Soybean oil and SCW…..………………………………………..48
Figure 4.3 the chart show that the lubricant test………………………….………………………….49
Figure 4.4 the chart show that the lubricant test………………………….………………………….50
Figure 4.5 the chart show that the lubricant test..……………………………………………………51
Figure 4.6 the chart show that the lubricant test.…………….………….…………………………...52
Figure 4.7 the chart show that the lubricant test……………………………………………………..53
Figure 4.8 the chart show that the lubricant test………………….………………………………….54
Figure 4.9 the chart show that the lubricant test…………………………….……………….………55
Figure 4.10 the chart show that the lubricant test…………………………….………………….…..56
Figure 4.11 the chart show that the lubricant test……………………………...………………..……57
Figure 4.12 the chart show that the lubricant test…………..………………………………….…….58
Figure 4.13 The chart show that mineral grease lubricant test………………….……………………59
Figure 4.14 Contours of the estimated response surface for DPT……………………………………61
Figure 4.15 Pareto diagram Standardized for Dropping point temperature (DPT)…………………..62
Figure 4.16 Graph of mean effects for dropping point temperatures………………………...………63
Figure 4.17 Contours of the estimated response surface for viscosity…….………………………….65
Figure 4.18 Contours of the estimated response surface for wear……………………………………68
Figure 4.19 Contours of the estimated response surface for the coefficient of friction…….………..70
Figure 4.20 comparative results of the four characteristics of greases response variable………….....73
Figure 4.21 Comparative result of COF with the time interval of Biogrease and mineral greases..….74
Figure 4.22 Comparing two best testing result of bio-grease product with mineral grease…………....75
vi
Figure 1. Pareto diagram Standardized for viscosity…………………………………………………..82

Figure 2. Graph of mean effects for Viscosity…………………………………………………………82
Figure 3. Pareto diagram Standardized for wear………………………………………………………83
Figure 4. Graph of mean effects for wear……………………………………………………………..84
Figure 5. Pareto diagram Standardized for the coefficient of friction……….………………………..85
Figure 6. Graph of mean effects for the coefficient of friction……………………..…………………85
List of tables
List of table chapter two
Table 2.1 Comparative Toxicity of Base Oil…..………………………..……………..…..………….9
Table 2.2 Common types of Lubricant Thickeners …………………..…….…….….………………15
Table 2.3 common lubricants additives………………………….………………………………...…17
Table 2.4 Lubricating grease and lubricating oil………………………..…….……………..……….21
List of table chapter three
Table 3.1 value of specification of Soybeans oil………..……………………………….……….…..32
Table 3.2 factor level setting………….………………………………………………………….…..34
Table 3.3 Respond to the test…………………………….………………..………………..…….….34
Table 3.4 Factorial Experiment Design Table or Design Matrix (counting 2 replications and
center point runs)……………………………………………...…….……….……………..………...35
Table 3.5 Main methods and standard tests for lubricating greases…….………………….………...39
Table 3.6 Specification of the tribological (wear and COF) test machine…………………………….44
Table 4.1 Composition of materials and temperature for Soybeans Bio grease production………….45
Table 4.2 Soybeans grease Visual aspect of the ten samples produced in different ratio of additive and
thickeners …………………………………………………………………………………………......47
Table 4.3 Test result of bio-grease of the lubricant……………………………………..…………….49
Table 4.4 the first lubricant test ……………………….………………….………………………….49
Table 4.5 the Second lubricant test…………………………………...………………………………50
Table 4.6 the third lubricant test...……………………..…………….………………….……………51
Table 4.7 The fourth lubricant test..……………………..….....…….…………………..….………..52
Table 4.8 The fifth lubricant test…….…...………………...…….…………………………………..53
Table 4.9 the sixth lubricant test………………………...…………..……………………………….54
Table 4.10 the seventh lubricant test……………………….……….………………………………..55
vii
Table 4.11 the eight lubricant test….……………………….………………………………………..56

Table 4.12 the ninth lubricant test….……………………….……………………………………..…57
Table 4.13 The tenth lubricant test……..…………………….……………………………..………..58
Table 4.14 the mineral grease lubricant test...……………….………………………………………..59
Table 4.15 Independent variables and dependent (responses) variable testing result of produced bio-
greases value………………………………………………………………………………..…………60
Tables 4.16 Analysis of variance (ANOVA) for dropping point temperature………………..……….64
Table 4.17 Combination of factor levels to maximized DPT…………...…………………….………64
Table 4.18 the product of bio-greases versus the response factorials.............................................…...72
Table 1. Factorial experiment design or design matrix by using statgraphics the first experimental
design…………………………………………………………….……………………………………81
Table 2. Analysis of Variance (ANOVA) for Viscosity………………………………………………83
Table 3. Combination of factor level for viscosity……………………………………………………83
Table 4. Analyses of Variance (ANOVA) wear………………………………………………………84
Table 5. Combination of factor levels for wear…….…………………………………………………85
Table 6. Analysis of Variance Friction coefficient…………………………………………………….86
Table 7. Combination of factor levels….………………………………………………………….….86
Table 8 the overall required budget to do the thesis…………………..…………………………….…87
viii
List of abbreviations
SCW=Sugarcane Filter Cake oil with 50 Sugarcane Filter Cake Wax
COF= Coefficient of friction
ASTM= The America Society for Testing and Materials
Co2 = Carbon dioxide
LiOH= Lithium hydroxide
NaOH= Sodium hydroxide
KOH= Potassium hydroxide
Lab= Laboratory
JIS=Japanese Industrial Standards
NLGI= National Lubricating Grease Institute
CAGR= Compound annual growth rate
PAG= Polyalkylene glycols
CST= Centi-Stock
mm= millimeter
Definition of key terms
 Soybeans oil
 SCW=Sugarcane Filter Cake oil with 50 Sugarcane Filter Cake
 Tribological test (friction and wear)
ix
CHAPTER ONE
1. Introduction
1.1 Background of the thesis
In this chapter introduction of the overall background of the thesis will be explained. In the world,
in one or other ways the energy will be lost because of inappropriate use of materials. For instance
in mechanical processes due to friction and wears a large amount of energy is wasted. Perhaps,
energy loss caused due to friction and wear may be reduced but it’s not possible to eliminate the
loss.
A lubricant is divided into organic and inorganic materials that are used to reduce frictional losses,
minimizes wear; reduces heat transferring by the mechanical system such as metal joints, shafts,
and bearings; high thermal and oxidative stabilities; removes contaminant and improves efficiency
between two surfaces in case of contact and undergoes relative motion, preventing damage by
scoring; are employed to upgrade the durability and dependability; serviceability and service
efficiency of mechanisms; mechanics and equipment. It may be to find in the form of liquid,
grease, dry film, and coating (Ponnekanti & Prashant, 2015) (Pedro D, et al., 2018) (Bahari, 2017).
Lubricating grease, by change solid to semi-solid, is by dispersion of thickening agent in a liquid
lubricant or thickening agents are dispersed into the base oil (Ponnekanti & Prashant, 2015).
In addition to reducing friction and wear in the machine element being lubricated under various
operating status, allowing protections from corrosion by preventing the entrance of water and
contaminants. Its function used a sealant to prevent lubricant leakage dripping and throw-off, resist
viscosity changes with temperature and pressure, water-stable, and to keep out foreign materials.
It acts an important portion in saving energy and reducing carbon dioxide (CO2) emission by
improving the lubrication efficiency and prolonging the service life of machines (Umesh & Neetu,
2019) (Pedro D, et al., 2018)
The actual lubricating grease produced traditionally from petroleum (mineral) oil and synthetic oil
but for the last decade’s time produced from vegetable oil and animal fats synthetic bio-oils
commonly used thickeners are soaps and organic or inorganic soap thickeners. The petroleum
(mineral) oil-based greases lead the market in terms of the volume consumed, provide better
stability in extreme temperatures applications, and are less expensive in comparison to synthetic
oil-based greases but less durable compared form its (Ismail, 2014) (Ponnekanti & Prashant,
2015).
1
Most lubricants contain petroleum base stocks but which are harmful to the environment and
difficult to dispose of. In the United States, over 60% of the lubricants used are lost to the
environment (Umesh & Neetu, 2019) (Syahrullail, et al., 2014).
Synthetic-based lubricants cost approximately more than two or three times that for comparable
conventional mineral oil-based lubricants. As the availability of synthetic-based environmentally
acceptable lubricants increases, this cost differential is expected to decline. The relatively higher
cost of synthetic esters is somewhat mitigated by their high oxidative stability, which results in
longer lubricant life. This is particularly applicable to areas of the vessel that require more frequent
lubricant changes (e.g., engine oil, hydraulic fluid, stern tube-thruster fluid). Synthetic is
compatible with mineral oil, which reduces conversion costs, but similar to vegetable oils in that
their effectiveness at removing mineral oil deposits can cause filters to overload during the period
initially following lubricant conversion. Disposal costs are similar to those for vegetable oil-based
lubricants (Ryan & Brian, 2011).
Vegetable oil lubricants will perform properly if some mineral oil balance remains. Because the
overall formulations are less toxic, disposal costs are generally lower (Suhaila, et al., 2018).
Depending on the biodegradability of base fluid grease both mineral oil and synthetic are less than
vegetable oil average test and synthetic oil offer improved performance over vegetable oil but it’s
a very high price than vegetable oil. Because of this reason vegetable oil is much preferable to
mineral (petroleum) oil and synthetic oil (Ryan & Brian , 2011) (Ngassapa, et al., 2012).
Previously most lubricating greases are producing from petroleum (mineral) oil and Synthetic oil
but those materials are Substitution by Alternative lubricating greases which producing from
vegetable oil because those materials are own more side effect comparing to vegetable oil like
Soyabean (Umesh & Neetu, 2019) (Pedro D, et al., 2018).
Generally, in nature, all base oil has its toxicity but the differences are in the degrees of toxicity
and also in case of adding additive may increase toxicity. So the selection of additives is its great
role to increase/decreasing the toxicity of the greases (Ryan & Brian, 2011).
Therefore, because of this reason, this research selected Sugarcane Filter Cake Oil with Sugarcane
Filter Cake Wax (SCW) as an alternative additive because the traditional additive is increasing
some toxicity of greases.
Tribology, Its objectives controlling friction, reducing emission, shock absorption, decreasing
noise pollution, developing bio- and eco-lubrication, and improving quality of life. Or its science
2
that deals with the study of friction, wear, and lubrication between the surfaces in moving relative
to each other. It does not include the study of tribological properties of surfaces if they are not in
relative motion (Zhang, 2013).
1.2 Statement of the Problem
Previously most lubricating greases are produced from petroleum (mineral) oil and synthetic oil
but petroleum oil as base oil used for the production of lubricating greases is not environmentally
friendly, toxic, stringent regulations and its non-renewable substances and the production process
cost is high and Synthetic based lubricant is approximately more than two or three-time cost
comparing from petroleum base oil and it’s also the high cost of the production process. Also,
most of the greases that are produced from those base oil use traditional additives like Zinc
dithiophosphate (ZDDP), organic polymer, sulphonates, carbon graphite…etc. which increases the
toxicity of the lubricant.
Other materials that are used to produce greases by using a vegetable as base oil called greases.
Vegetable oils like Soybeans oil; which are low toxic; environmental friendly materials or low
pollution; highly biodegradability; low production process cost and its capability to contribute
towards the goal of energy independence and sustainability since are a renewable resource and use
traditional additive as an additive it's more increase toxicity and involves environmental impact.
Vegetables as base oil are selected in this research thesis and changing traditional additive by
alternative additive of Sugarcane Filter Cake Oil with 50% of Sugarcane Filter Cake Wax (SCW).
In this research thesis, the influence on tribological properties of bio-grease lubricant base
Soybeans oil, and the possibility using of an alternative additive (SCW) that can minimize the
toxicity of the lubricant grease (as substitution of traditional toxic additives in its manufacture)
were investigated.
3
1.3 Objective of the thesis

1.3.1 General objective
The general objective of this research thesis is to investigate the influence on tribological
properties of bio grease lubricant base Soyabeans oil, using Sugarcane Filter Cake Oil with 50%
of Sugarcane Filter Cake Wax as alternative additive.
1.3.2 Specific objective
I. To conduct the experimental matrix to study the influence of different factors over the
tribological properties (Friction & Wear) of Soybeans as a base oil and SCW as an
alternative additive.
II. To produce bio-grease soybeans oil as a base oil and SCW as an alternative additive, with
the different conditions of factors to be studied.
III. To investigate the influence on the tribological performance of bio grease lubricant of
Soybeans base oil with the alternative additive of SCW.
IV. To compare the result with one of the mineral oil.
1.4 Scope of the thesis/ Delimitation of the thesis
This research thesis is focused on producing grease by using Soybeans oil as a base oil and also to
improve tribological properties with the use of the alternative additive of SCW.
I. Design the experimental matrix to study the influence of different factors over the
tribological properties (Friction & wear) of Soybeans oil as a base oil and SCW as
an alternative additive.
II. Produce bio-grease soybeans oil as a base oil and SCW as an alternative additive,
with the different conditions of factors to be studied.
III. Investigate the influence on the tribological performance of bio- grease lubricant of
Soybeans with the alternative additive SCW.
1.5 Limitation of the thesis
 One of the main limitations of this research thesis is the budget and finding some materials
in the country. The other is due to the current Covid-19 virus; it has been difficult for the
experimental progress.
 Because of the limitation of the lab setup in FTVEI and even if the country of Addis Ababa
all the characteristics of greases for performance are not tested.
4
1.6 Significance of the thesis

The significance of this research thesis is to study the method of producing bio grease by using
vegetable oils (Soybeans oil) and improving the tribological properties using alternative additive
of Sugarcane Filter Cake Oil with 50% of Sugarcane Filter Cake Wax. It’s known that the grease
conception and the cost increase each year, especially on petroleum (mineral) oil-based lubricating
greases. Its product is unsafe for the environment; non-renewable material; toxic substance; lowest
biodegradability as compared to vegetable oil and synthetic ester oil. So depending on this, The
aim of the research replacing petroleum oil with biodegradable, non-toxic, and cheap bio grease
products from vegetable oil (soybean oils) and using an alternative additive of Sugarcane Filter
Cake Oil with 50% of Sugarcane Filter Cake Wax instead of traditional additives. Other than this,
the research will benefit entrepreneurs to create new jobs for society.
1.7 Hypothesis
If it is used SCW (one of the biodegradable and not toxic materials) as an alternative additive in
the grease base vegetable oil instead of the traditional toxic additives, the tribological properties
of bio- grease will not be affected, and will not increase its toxicity.
1.8 Organization of the thesis
This research thesis is organizing into five chapters, the first chapter introduction and describing
the may purpose of the thesis, the second chapter, literature reviews, the third chapter the
methodology of the thesis and the four-chapter Result and Discussion and the five chapter
Conclusion, Recommendation, and Future Work.
5
CHAPTER TWO
2. Literature Review
2.1 Overview
In this chapter, focus on the previous research conduct related to this thesis will be introduced. It
was starting from, lubricating grease, elements of grease (base oil, thickener, additive), types of
grease, factor affect types of grease, tribological properties of grease.
A lubricant is divided into organic and inorganic materials that are used to reduce frictional losses,
minimizes wear; reduces heat transferring by the mechanical system such as metal joints, shafts,
and bearings; high thermal and oxidative stabilities; removes contaminant and improves efficiency
between two surfaces in case of contact and undergoes relative motion, preventing damage by
scoring; are employed to upgrade the durability and dependability; serviceability and service
efficiency of mechanisms; mechanics and equipment. It may be to find in the form of liquid,
grease, dry film, and coating (Ponnekanti & Prashant, 2015) (Pedro D, et al., 2018) (Bahari, 2017).
Lubricating grease, by change solid to semi-solid, is by dispersion of thickening agent in a liquid
lubricant or thickening agents are dispersed into the base oil (Ponnekanti & Prashant, 2015).
In addition to reducing friction and wear in the machine element being lubricated under various
operating status, allowing protections from corrosion by preventing the entrance of water and
contaminants. Its function used a sealant to prevent lubricant leakage dripping and throw-off, resist
viscosity changes with temperature and pressure, water-stable, and to keep out foreign materials.
It acts an important portion in saving energy and reducing carbon dioxide (CO2) emission by
improving the lubrication efficiency and prolonging the service life of machines (Umesh & Neetu,
2019) (Pedro D, et al., 2018)
Approximately 98% of the petroleum grease have controlled the market until 2004. The definition
of grease by Japanese Industrial Standards (JIS) or American Society for Testing and Material
(ASTM) said: “A solid or semi-solid product of dispersion of a thickening agent in lubricating oil”
(Ismail, 2014). Other ingredients imparting special properties may be included:-
6
Figure 2.1 Lubricating grease and bio-lubricating greases (Ismail, 2014).

The function of lubricants, which include organic and inorganic materials adequate to reducing
friction, minimizing the wear of friction surfaces, and preventing damage by scoring, are employed
to upgrade the durability and dependability, serviceability, and service efficiency of mechanisms,
mechanics, and equipment. In addition to reducing friction and wear in the machine element being
lubricated under various operating status, protect rust and corrosion, prevent dirt water and other
contaminants from entering the part being lubricated (Umesh & Neetu, 2019) (Pedro D, et al.,
2018). The mineral oil-based greases lead the market in terms of the volume consumed, provide
better stability in extreme temperatures applications, and are less expensive in comparison to
synthetic and semi-synthetic oil-based greases but less durable compared to them. The synthetic
and semi-synthetic oil-based greases are expensive but employed in more severe or even quite
exotic applications. The mineral and synthetic oil-based greases continue to dominate the market
today and this situation is likely to continue as long as the crude oil is available at affordable prices.
The recent success of nuclear talks between Washington and Tehran in July 2015 may culminate
in the availability of Iranian crude to global consumers. The current crude oil prices at US$40a
barrel are already the lowest since March 2009. These factors might adversely affect the growth
of biodegradable oils-based lubricants and greases segment in the market.
The National Lubricating Grease Institute (NLGI) 2010 Grease Production Survey indicates that
about 93% (over 1 billion kilograms) of Sustainable Development total worldwide grease volumes
were mineral oil-based greases, followed by synthetic and semi-synthetic oil-based greases at
about 3% each. Biogrease made their entry in the NLGI survey for the first time with about 1%
market share. The NLGI 2012 Grease Production Survey indicates that only 0.42% of the total
reported production worldwide is based on biodegradable base oils. Frost and Sullivan report that
the mineral oil-based greases accounted for 40.4% of the global industrial grease market revenue
7
in 2012, while the synthetic and semi-synthetic oil-based greases amounted to 55.6% of the total
revenue mainly due to higher prices, with the remaining 3.9% revenue contributed by
environment-friendly greases. (Fig. below) (Umesh & Neetu, 2019) (Ryan & Brian , 2011).
Figure 2.2 Global industrial greases sales breakdown (Umesh & Neetu, 2019) (Ryan & Brian ,
2011).
Vegetable oil lubricants are more expensive than comparable mineral oil lubricants, as a
the function of both higher base oil costs, as well as higher costs for the base oil-compatible
additives. Although vegetable oil lubricants cost approximately double that of mineral base oils,
more recent information obtained through personal communication with a major lubricant supplier
suggests that the current cost premium for these lubricants maybe only 20% more. Changing from
a mineral to a vegetable oil lubricant is relatively simple, as vegetable oils and mineral oils are
compatible and vegetable oil lubricants will perform properly if some mineral oil residue remains.
Because the overall formulations are less toxic, disposal costs are generally lower; however, this
may not always be the case, as fewer disposal stations can accept spent biobased lubricants
(Algailani, 2015) (Ryan & Brian, 2011).
Generally, Synthetic esters are the most expensive class of environmentally acceptable lubricants.
Its based bio-lubricants cost approximately two or three times that of comparable conventional
mineral oil-based lubricants. As the availability of synthetic ester-based environmentally
acceptable lubricants increases, this cost differential is expected to decline. The relatively higher
cost of synthetic esters is somewhat mitigated by their high oxidative stability, which results in
longer lubricant life. This is particularly applicable to areas of the vessel that require more frequent
lubricant changes (e.g., engine oil, hydraulic fluid, stern tube-thruster fluid). Synthetic esters are
compatible with mineral oil, which reduces changeover costs, but similar to vegetable oils in that
their effectiveness at removing mineral oil deposits can cause filters to clog during the period
8
initially following lubricant changeover. Disposal costs are similar to those for vegetable oil-based
lubricants. In general, vegetable oil and synthetic ester base oils have low toxicity to marine
organisms. Water-soluble Polyalkylene glycols may demonstrate increased toxicity to aquatic
organisms by directly entering the water column and sediments rather than remaining on the water
column surface as sheen (Ryan & Brian, 2011).
Table 1.1 Comparative Toxicity of Base Oils (Ryan & Brian, 2011).
Lubricant base oil Base oil source Toxicity
Mineral oil Petroleum High
Synthetic Ester Synthesized from biological sources Low
Vegetable Oils Naturally occurring vegetable oils Low
The toxicity of petroleum-based oils is also dependent upon additives used in formulations and
metabolites produced in biodegradation. The use of additives is dependent on the choice of base
oil and the intended function of the lubricant. However, several of the more toxic compounds in
formulations are also the ones with poor degradability. The overall product toxicity may be
significantly reduced by switching to biologically-sourced base oil used in conjunction with low
toxicity additives. Biolubricants have several disadvantages in the use phase of the product life
cycle, including some bad odors if contaminants are present, high viscosity at low temperatures,
poor oxidative stability at high temperatures, although additives designed specifically for plant-
based lubricants eliminate stability issues related to extreme high and low temperatures. If
lubricants are untreated, it lacks oxidation stability and will have high pour points. There are some
challenges associated with the production of bio lubricant which includes the high cost and limited
availability of bio lubricant feedstock. Various factors are contributing to the cost of bio lubricant.
These factors include feedstock prices, plant capacity, feedstock quality, processing technology,
net energy balance nature of purification and its storage, etc. However, the two main factors are
the costs of feedstock and the cost of processing into bio lubricant. It has been found that the cost
of feedstock accounts for 75% of the total cost of lubricants and biofuels in general (Wendimu,
2016).
Depending on the biodegradability of base fluid grease both mineral oil and synthetic are less than
vegetable oil average test and synthetic esters oil offer improved performance over vegetable oil
but it’s a very high price than vegetable oil. Chemical stability of vegetable oil is low because the
9
consists of polyunsaturated acid contact but the stability can be increased by the chemical
modification of the oils to reduce the content of conjugated double bonds. Because of this reason
vegetable oil is much preferable to mineral (petroleum) oil and synthesis oil (Brentin, 2018) (Ryan
& Brian , 2011).
Since bio-lubricants outperform petroleum lubricants, less is required per application. Cost
benefits include reductions in environmental and safety penalties in the case of spills, and fewer
parts wear maintenance costs, and disposal fees (Yifeng , et al., 2015). Biolubricants:
 Evaporate slower than petroleum lubricants.
 Adhere better to metal surfaces.
They have several disadvantages in the use phase of the product life cycle, including
 Some bad odors if contaminants are present.
 High viscosity at low temperatures.
 Poor oxidative stability at high temperatures, although additives designed specifically for
plant-based lubricants eliminate stability issues related to extreme high and low
temperatures.
2.2 Elements of grease
To make the Lubricating greases are used three major components. Those components are base
oil, thickener, and additives. In the case of grease preparation, the content of base oil and additive
package are the mean elements. The thickener is often referred to as a sponge that holds the
lubricant. Greases are solid to semi-fluid of a fluid lubricant, thickener, and additive. The fluid
lubricants perform the actual lubrication that can be prepare from petroleum (mineral) oil,
synthesis oil, and/or vegetable oil. Greases are consist of two main structural components those
are a thickener agent and liquid or base fluid. Expressing on the figure below: typical composition
of lubricating greases contains 70-95wt. % based fluid (mineral oil, synthetic or vegetable oil), the
thickeners are 3-30wt. % (Ismail, 2014), and some literature review said 5-20wt. % (Bhupender ,
et al., 2014) (Ponnekanti & Prashant, 2015). At the instant in this research select the second interval
(5-20wt. %) but it’s made the greases solid final change into a small amount of the interval (2-5%)
of thickener. Thickener is (simple, complex, and non-soap), and 0-10wt. % additives (antioxidants,
corrosive inhibitors, anti-wear/extreme pressure, antifoam, and tackiness agents (Bhupender , et
al., 2014) (Ismail, 2014) (Ponnekanti & Prashant, 2015).
10
Figure 2.3 Elements/ composition of greases (Bhupender , et al., 2014) (Ismail, 2014) (Ponnekanti
& Prashant, 2015).
Lubricating greases are generally highly structured suspensions, consisting of thickener dispersed
in mineral or synthetic oil. Fatty acid soaps of lithium, calcium, sodium, aluminum, and barium
are most commonly used as thickeners. This component is added to increase the consistency of
greases, preventing loss of lubricant under operating conditions and avoiding the penetration of
contaminants, such as solid particles and water, without a significant reduction of the lubricating
properties, which mainly supplied by oil. The thickener forms an entanglement network, which
traps the oil and confers the appropriate rheological and tribological behavior to the grease. The
performance of lubricating grease depends on the nature of its components and the microstructure
achieved during its processing. Consequently, suitable structural and physical properties may be
reached from a proper selection of ingredients but, also, from process optimization, as previously
reported (Syahrullail, et al., 2014).
2.2.1 Base oil
Know day most of the greases are produced using of the mineral (petroleum) oil. The conception
of the people and supply are unbalanced because the crude oil has already come to end so other
alternative resources are necessary to use for the production of greases and also mineral oil is toxic,
lowest biodegradability, environmentally unsafe….etc. Base oil that is produced from vegetables
and synthetic oil is much better for different considerations. Base oils make up to 70-95% of the
total composition of the grease. Fundamentally the base oils can be divided into two types: (i)
Water miscible and (ii) non-water miscible. Glycols are completely water-soluble; the most
11
regularly used are mono propylene glycol or polyethylene glycol with an average molecular weight
of 200-1500. The advantage of these compounds is theirs resistance to aging and hydrolysis, still,
the major disadvantages are solubility in water and incompatibility with minerals base oils. Non-
water soluble base oils can be subdivided into two categories (i) vegetable oils and (ii) synthetic
esters. This class of compound usually has the same structure, and hence, identical physical and
chemical properties (Algailani, 2015) (Bhupender , et al., 2014) (Ismail, 2014).
2.2.1.1 Soybeans oil
Soybeans oil is using in this research as the base oils. It’s a vegetable oil extracted from the seeds
of the soybean (Algailani, 2015) (Divine & Anuanwen , 2020). It’s the largest product in the world
(Bahari, 2017). Vegetable oil lubricates are biodegradable, non-toxic, unlike conventional mineral-
based oils. The low-temperature study has also shown that most vegetable oils undergo cloudiness,
precipitation, pool flow, and solidification at-100 C upon long-term exposure to cold temperature
in sharp contrast to mineral oil-based fluids. Its life cycle assessment studies show environmental
benefits: lower energy production cost, reduced exposure to toxic chemicals, lower carbon dioxide
emissions during production, and supply chain sustainability. Soyabean oil as a biobased lubricant
is based on its good lubrication performance-enhanced lubricity, high viscosity index, low
evaporation loss, low flammability, higher flash and fire points. It provides a sustainable and
renewable option for a broad range of lubrication fluid applications requiring low toxicity and
readily biodegradable. Established uses include lubrication fluids in hydraulic cylinders,
metalworking machines, and moving surfaces where the lubricant is lost directly into the
environment. Improved thermal stability is now possible with the recent development of high oleic
soybeans. With the proper balancing of additives and manufacturing processes, performance may
be further enhanced for needs specific to railroad users (Brentin, 2018) (Delgado, et al., n.d.)
(Yusuf, 2018).
Soybeans used to reduced dependency on petroleum and association product price fluctuations for
raw materials; unlike fossil fuels, Soybeans are a renewable resource, so there’s always an ample
supply; soybeans take carbon dioxide (CO2) out of the atmosphere as they and add a little while
being processed into products. This contributes to better air quality and helps manufacturers meet
new CO2 emission regulations; products containing soybean oil are less likely to pollute and
contaminate waterways like petroleum equivalents; in many cases, soybeans derivatives are
replacing suspect carcinogens in products, without compromising performance (Lubricants, 2016).
12
2.2.1.1.1 Extraction of Base oil

Mostly, the name of the vegetable oils derived from the name of plants. There are common
methods used to extract the lubricating oil. Therefore; Soybean oils also followed this standard
method to extracting oil. These methods are common or similar to other vegetable oils extracted
(Ozioko, 2012).
2.2.1.1.2 Methods of base oil extraction
The quality of the oil depends on the type of extraction; the method of manufacturing Soybean
oil includes the collection of raw materials for the extraction and selection of extraction method.
Therefore, the methods of extraction of oil are different methods those are the old traditional
method and conventional method of extraction (Cheng, 2017) (Divine & Anuanwen , 2020)
(Ozioko, 2012). Let see step by steps:-
 Old traditional method
In terms of oil recovery and oil yield, the old traditional or informal wet extraction methods
used by rural communities around the globe are regarded as inefficient, often yielding below the
range of plant oil.
There are three major means of recovering oil from oleaginous materials of plant origin as wet
extraction (hot water or steam extraction), solvent extraction, and mechanical expression.
Concerning the wet extraction method proffered nine major operations that are involved in the
extraction of castor oil by the old traditional method namely, collection of seed pods, shelling of
the pods/winnowing, boiling the seeds to reduce moisture, grinding of seeds to form a paste,
mixing the paste with water/boiling to extract oil, scooping of oil and drying the oil by heating.
They evaluated the percentage yield and percentage oil recovery using the expressions
Where Moil =mass of oil (kg)

Mseed = mass of oilseed (kg)
X= oil content of oilseed
The old traditional method of extraction of seed oils as involving the roasting of seed kernels by
mortar and pestle or between two stones, mixing the crushed mass with water, cooking of the
mixed paste to obtain the oil by floating and skimming, and then drying of the oil by further
heating (Cheng, 2017) (Divine & Anuanwen , 2020) (Yusuf, 2018).
13
 Conventional methods
The conventional methods are the well-known and widely practiced methods of oil extraction
namely, solvent extraction and mechanical expression. Many seed oils are extracted by either of
the two methods or a combination of the two. This classification may also include rendering
though perhaps not as widely used. Regardless of extraction method, extracted and refined oil
must be evaluated for its physicochemical properties to determine its application or usage (Cheng,
2017) (Divine & Anuanwen , 2020) (Yusuf, 2018).
2.2.1.1.2.1 Solvent Extraction of soybeans oil
This method is a conventional method of oil extraction commonly applied to oilseeds with low
oil content (< 20%), like soybean. This method is considered as one of the most efficient methods
in vegetable oil extraction, with less residual oil left in the cake or meal (Ozioko, 2012).
Solvent extraction uses the solubility of oil and a nonpolar organic solvent to extract oil from
soybean flakes. Compared to the mechanical expelling process, solvent extraction can remove
about 0.5% of residual oil with less energy consumption and facility maintenance. Due to its
relatively higher oil recovery and energy efficiency, the development and application of solvent
extraction have expanded since the 1940s along with the early expansion of U.S Soybean
production. Hexane is the solvent most used for oil extraction, and it is the mix of isomers with
similar properties which is also called extraction hexane or commercial hexane. Compared to n-
hexane, extraction hexane has similar molecular weight and specific gravity, higher ignition and
flash temperature, lower melting point and boiling point. These properties increase the safety of
operating. Additionally, the extraction of hexane results in a slightly greater ability to extract
efficiently than n-hexane, due to the presence of various isomers. The raw material is placed in a
glass, vessel and soaked with a suitable solvent (petroleum, ether, or benzene). After the extraction,
the solids are separated from the liquid mixture. The latter is heated so that the more volatile
essential oils can be evaporated to be subsequently condensed (Divine & Anuanwen , 2020)
(Yusuf, 2018).
14
2.2.2 Thickener
The thickener in lubricating grease is the component that sets grease apart from lubricants.
Thickeners are molecules, polymers, or particles that are partially soluble in lubricating fluid; they
arrange themselves in such ways that impart a semi-solid consistency to the grease. Many different
types of chemical compounds can be used to thicken grease. Simple soaps are the most common
grease thickeners. Simple soap is the reaction product of an organic acid (long-chain or fatty
carboxylic acid) and an alkali metal to form an organic salt. The most common alkalis used are the
hydroxides from earth metals such as aluminum, calcium, lithium, sodium, and titanium (Ismail,
2014). Thus, simple soaps are most commonly based on salts lithium and calcium and less
commonly on salts of sodium, aluminum, and barium. Examples of simple soap thickeners include
lithium 12-hydroxystearate and calcium stearate. Complex soaps are also used widely as grease
thickeners. The terms refer to the combination of simple soap and a complexing agent. For
example, a lithium complex thickener typically contains lithium 12-hydroxystearate (simple soap)
and a salt of a shorter chain di-functional carboxylic acid, boric acid, or aromatic acid (complexing
agent). Complex thickeners are usually based on lithium, calcium, or aluminum compounds. In
some cases, dissimilar thickener types are combined in grease. This type of thickener system can
be referred to as a hybrid thickener or in some cases as a complex thickener (Cyriac, et al., 2016).
Grease can also be thickened with non-soap materials. Common non-soap thickeners include
polyuria, organophilic clay, fumed, silica, Fluoropolymer, and others. A typical polyuria thickener
is the reaction product of a di-isocyanate with mono and/or diamines (Ismail, 2014).
Table 2.2 Common types of Lubrication Thickeners (Ismail, 2014).
15
Complex grease is made when a complex soap is formed in the presence of base oil. Generally,
complex greases have good all-around properties and can be used in multipurpose applications.
The base oil and the composition of the thickening agent play an important role in grease
consistency.
In this research to conduct the research used as a thickener was selected that is available in
Ethiopian those were lithium hydroxide (LiOH). Lithium soap lubricating greases are very good a
property of those greases i.e. a smooth appearance and dropping points (Ismail, 2014) (Cyriac, et
al., 2016).
2.2.3 Additive
Any based oils such as mineral oil, synthetic oil, and vegetable oil products cannot satisfy the
requirement of high-performance lubricants without using modern additive technology. Additive
brings up the characteristic of an oxidative stabilizer for lubricating grease. It’s antifriction
between two different parts of the bearing, shaft, and metal joints in case of contacting each other.
Additives are synthetic chemical substances that can improve lots of different parameters of
lubricants. They can boost existing properties; suppress undesirable properties in the base fluids
(Bengtsson, 2015) (Delgado, et al., n.d.) (Ismail, 2014) (Umesh & Neetu, 2019).
A good lubricated has the best chance of reaching its maximum service life. Additives behave
excellent in water and good storage stability, good shear and oxidation stability, good Antiwear
and load-carrying capacity, and saltwater corrosions properties.
The table tells the common traditional lubricants used as an additive in the production of any types
of greases either mineral greases, synthetic greases, or vegetable greases of lubricant and their
functionalities (Bahari, 2017) (Lubricants, 2016).
16
Table 2.3 common lubricant additives (Bahari, 2017) (Lubricants, 2016).

No. Additives Type Compounds used Function
1 Extreme pressure Sulfur, Chlorine- Increase load-carrying ability Protect metal
(EP) phosphorous compounds, surfaces against cold welding
2 Antioxidant Hindered phenols Amines Prolong oil life by slowing oxidation
3 Antifoam Silicones Control foaming in fortified systems
4 Anticorrosion Petroleum sulfonates Form anticorrosion film
5 Detergent or Calcium sulphonates Prevent deposition of carbon
Dispersant
6 Alkalinity (TBN) Calcium carbonates, Neutralize acidic engines byproducts
Magnesium, sulphonates
7 Antiwear Zinc dithiophosphate Reduce wear
(ZDDP)
8 Pour point Methacrylate polymers Lower pour point
depressant
9 VI Improvers Organic polymers Improve VI
Anti-corrosions grease is used to prevent or reduce processes that lead to rust or corrosions. Anti-
wear grease must prevent wear by forming a strong surface film to reduce content between surfaces
to prevent heating as an outcome of extreme prevent, Anti-oxidant grease must prevent oxidation
which will lead to damage which in turn will admit impurities or gives rise to acidity. Viscosity
index improver additives will retain the viscosity of grease will break down at high engine
temperatures or when the engine has run too long (Bahari, 2017) (Lubricants, 2016).
2.2.3.1 Alternative additive Sugarcane Filter Cake Oil with Sugarcane wax
There are different types of traditional additive; those are described in table 2.4 used to produce
greases. Those different types of traditional additive are own characteristics and applications as
the mansion in table 2.4 but those additives use for grease production is own impact on the
environment and toxicity; therefore, in this research, this improves other new and alternative
additives. This alternative additive is Sugarcane Filter Cake oil wax: sugarcane oil and 50 %
Sugarcane filter cake wax. Its properties and characteristics are almost similar with the application
of traditionally used additives expect toxicity.
17
Sugarcane filter cake oil characteristics and its application that are similar to traditional additives
are high-viscosity greases for the lubrication of gears, high-viscosity oils for bearings, resistance
to heavy loads and impacts, anti-wear qualities, corrosion resistance, low evaporation index, and
besides that expressing from the above sugarcane are different applications those are water-
repellent, associated services, product benefits, and biodegradability. When depending on the
philosophy or the point of this research the product of greases is based on different point points:
performance, lifetime, and respect for the environment (Bengtsson, 2015) (Delgado, et al., n.d.)
(Umesh & Neetu, 2019).
2.3 Physicochemical Characteristics of Vegetable oil.
There are different types of physical and chemical properties of the oil, those physical properties
are Density, specific gravity, viscosity, refractive index, and chemical properties like Acid value,
Peroxide, Iodine value, Saponification value of soybean, sesame, safflower, groundnut, rice bran
oil were determined by the standard method. In this topic, some of the properties are described
some are described in other places.
2.3.1 Specific gravity
The specific gravity of oils was measured by using the specific gravity of the bottle at 25o C. The
bottle was filled with oil and weighted. After cleaning, the bottle was filled with distilled water
and weighed. The specific gravity was expressed in terms of the ratio of oil to water. Values for
essential oils vary between the limits of 0.696 and 0.96 at 15℃. In general, the specific
gravity is less than 1. Hence essential oil can be collected over (floating on) water (Gagandeep, et
al., 2019) (katkade, et al., 2018).
2.3.2 Boiling range
In the case of isolates and synthetics, the boiling range is an important criterion of purity
(Gagandeep, et al., 2019) (katkade, et al., 2018).
2.3.3 Iodine value
It’s an indication of the degree of unsaturation in the oils and fat and is a measure of vulnerability
to oxidation. The higher the iodine value, the more vulnerability of the oil to oxidation (Ngassapa,
et al., 2012). Iodine value was determined using the method as reported in AOAC methods Weight
out 0.2g of oil into 500 ml conical flask. Add 20 ml of chloroform and dissolve the oil completely.
Keep in dark for 30 min. Add 20 ml of KI solution and mix well. Titrate against 0.1 N Na 2S2O3
18
solution using starch as an indicator with vigorous shaking to extract iodine from the chloroform
layer (Gagandeep, et al., 2019) (katkade, et al., 2018).
2.3.4 Acid value
The acid value is the number of milligrams of potassium hydroxide (POH) required neutralizing
the free fatty acid present in one gram of oil Or the acid value (AV) represents the degradation of
the oil quality resulting from the hydrolysis of triacylglycerol as well as further decomposition of
hydroperoxide (Gagandeep, et al., 2019) (katkade, et al., 2018).
2.3.5 Saponification
The saponification value is the number of a milligram of potassium hydroxide KOH required to
neutralize the fatty acids present as a result of the complete hydrolysis of 1g fat. Accurately weigh
out 2g of oil into a 250ml of the conical flask, add 25ml of alcoholic KOH and dissolve the oil
completely. Connect the air condenser to the flask and boil for about 30min on a boiling water
bath. Cool to room temperature; add 2 drops of phenolphthalein indicator and mix. Titrant against
standard 0.5N HCL until (Gagandeep, et al., 2019) (katkade, et al., 2018).
2.3.6 The importance of Moisture and Temperature in Oil Extraction
Moisture increases the flow of oil through the pores of the press cake, hence reducing the amount
of oil entrained in the cake and increasing the oil yield mostly in mechanical expression. High
moisture content stops oil flow possibly because the structures of the finely milled particles have
been altered (high aggregation). Moisture lubricates the pulp during pressing and causes a slower
pressure increase and reduces oil yields. Temperature plays an active role in the seed treatment for
mechanical extraction and ensures an effective solvent process by heating the solvent which
hastens the extraction process. At the right temperature and moisture content, the individual oil
droplets unite to form a continuous phase and flow out maximizing oil yield (Gagandeep, et al.,
2019) (Ngassapa, et al., 2012).
2.4 Function of grease
The function of grease is to remain in contact with and lubricant moving surfaces without leaking
out under gravity or centrifugal action or be squeezed out under pressure. Its major practical
requirement is that it retains its properties under shear at all temperatures that it is subjected to
during use. At the same time, the grease must be able to flow into bearing through grease guns and
from spot to spot in lubricated machinery as needed, but not add significantly to the power required
to operate the machine, particularly at startup. Generally, the lubricating grease functions are
19
minimized friction and wear, protections from corrosion, rust prevention or preventing the
entrance of water and contaminants, used as a sealant and sealing, Resist viscosity changes with
temperature and pressure, to keep out foreign materials, Reducing carbon dioxide (CO2) emission,
cooling, load balancing, cleaning (Ismail, 2014) (Umesh & Neetu, 2019).
2.5 Lubricating grease Uses or Application
Grease and oil are not interchangeable. Grease is used when it is not practical or convenient to use
oil. The lubricant choice for a specific application is determined by matching the machinery design
and operating conditions with the desired lubricant characteristics.
Grease and oil are not interchangeable. Grease is used when it is not practical or convenient to use
oil. The lubricant choice for a specific is determined by matching the machinery design and
operating conditions with desired lubricant characteristics (Gunam , et al., n.d.). Grease is
generally used for:-
 Machinery that runs intermittently or is in storage for an extended period. Because grease
remains in place, a lubricating film can instantly form.
 Machinery that is not easily accessible for frequent lubrication also requires grease. High-
quality greases can lubricate isolated or relatively inaccessible components for extended
periods without frequent replenishing. These greases are also used in sealed-for-life
applications such as some electrical motors and gearboxes.
 Machinery operating under extreme conditions such as high temperatures and pressures,
shock loads, or slow speed under heavy load prefers the usage of greases compared to oils.
 Worn components are another suitable application for grease as grease maintains thicker
films in clearances enlarged by wear and can extend the life of worn parts that were
previously lubricated by oil.
2.6 The difference between lubricating grease and lubricating oil/ liquid
The fundamental difference between grease and liquid lubricant is the presence of the thickening
agent. The thickeners are usually metallic soaps, such as lithium, sodium, and calcium salts of
long-chain fatty acids. The thickener gives grease its characteristic rigidity or consistency which
is a measure of resistance to deformation by an applied force. The structure will flow under applied
stress, the magnitude of which will depend on the rigidity of the soap fiber network which is
governed by the forces holding the fibers together. Soap thickeners not only provide consistency
to grease, and they also affect desired properties such as water and heat resistance and pump-
20
ability. Thickener can also lower the coefficient of friction over that of the base oil. Among
lubricating greases, the lithium soap-based lubricating grease has been numerous due to the very
good properties of these greases, i.e., a smooth appearance, and a high dropping point. However,
calcium soap is more favorable for formulating food-grade grease. Calcium is not toxic and it is
common in all living systems and is essential to life. Besides, calcium thickener has also high
resistance to water wash-out (Ismail, 2014) (Lubricants, 2016) (Syahrullail, et al., 2014).
Based on its physical state, grease is classified as a semi-solid lubricant and Liquid lubricants are
lubricating oil semi-solid lubricant grease compound solid lubricant of Molybdenum, disulfide,
and graphite, etc. Grease vs. oil lubricant Advantages and Disadvantages (Syahrullail, et al.,
2014).
Table 2.4 Lubricating grease and lubricating oil (Syahrullail, et al., 2014)
No, Items Grease lubrication Oil lubrication
1 Feed device Grease sealed does not require Require a device that continuously
re-lubrication for an extended feeds oil(drip-feed, splash feed,
period. recirculation system)
2 Consumption Can be kept to the minimum Significant amount require
necessary.
3 Lubrication system Simple Complex
4 Leakage Unlikely because of its seal Possible if the sealing system is
forming characteristics. adequate
5 Use for high-speed Limited Yes.
application
6 Contaminate No. Continual removal by filtration or
removal adequate.
7 Cooling efficiency No cooling capacity High cooling capacity.
8 Friction loss Generally high, but torque Generally low
reduction can be achieved by
channeling in order bearings.
21
2.7 Characteristics of lubricating greases

There are different characteristics of grease tested method concerning about ASTM-D and IT
standard or the tribological performance of the product was studied on different tested machines
as per ASTM-D and IP standard test methods.
2.7.1 Dropping point
The dropping point is the temperature at which grease becomes fluid enough to drip through the
orifice of the test apparatus under conditions specified by ASTM D-566 and D-2265. In easier
terms, the dropping point is the temperature at which the grease no longer stays in place. It is an
indicator of the heat resistance of the grease. As grease temperature increases, penetration
increases until the grease liquefies and the desired consistency is lost. The dropping point indicates
the upper-temperature limit at which grease retains its structure, not the maximum temperature at
which grease may be used. Hence, the dropping point should not be confused with the melting
point of grease. Dropping point is a key test parameter for any grease specification as it shows how
well the test grease will perform under applied load at high temperature under actual operating
conditions. A numeric value is assigned to a grease composition representing the corrected
temperature at which the first drop of the material falls from the test cup and reaches the bottom
of the test tube. It’s possible until 260 oC (Bahari, 2017) (Ponnekanti & Prashant, 2015) (Umesh
& Neetu, 2019)
2.7.2 Cone penetration
The degree to which lubricating grease resists deformation under the application of force is known
as its consistency or hardness. It depends on the type and amount of thickener used and the
viscosity of its base oil. The consistency of lubricating greases is measured by cone penetration
test according to ASTM D-217 or ASTM D-1403. In the test, a cone of fixed dimensions and mass
is allowed to drop into a sample of grease in a standard cup at a standard temperature of 25ºC for
five seconds. The depth to which the cone penetrates the grease is measured in tenths of a
millimeter and is used to determine the NLGI grade of the grease. The softer the consistency,
Sustainable Development the higher is the penetration number The National Lubricating Grease
Institute classified greases according to their consistency as measured by the worked penetration.
The penetration of a cone of specified dimensions, mass, and finish was measured in tenths of a
millimeter. These cone penetration tests not only evaluate the consistency of lubricating greases
over the full range of NLGI numbers but also evaluate the consistency of stiff greases having
22
penetration numbers less than 85. The penetration values of samples increase with decreasing
thickener content. A slight chance of a parameter may result from the change in penetration values.
The NLGI consistency number alone is not sufficient for specifying the grease required by a
particular application. Besides consistency, structural and mechanical stability, apparent viscosity,
oxidation resistance can be tested to determine the suitability of grease to a specific application
(Ponnekanti & Prashant, 2015) (Umesh & Neetu, 2019) (Suhaila, et al., 2018).
2.7.3 Oxidation stability
Oxidation stability is the ability of grease to resist a chemical union with oxygen. The Jatropha
oil under normal conditions of temperature, moisture, and oxygen levels will remain stable. If
subjected to high temperatures in the presence of moisture and oxygen for a prolonged period,
degradation will take place. Zinc dialkyl dithiophosphate (ZDDP) is found commonly in
lubricating oil where it plays a role as both an antioxidant and an anti-wear additive. It extends the
life of the lubricant grease by inhibiting oxidation, thus minimizing base oil thickening, sludging,
and deposits, and reducing the friction between moving parts by surface adsorption (Bahari, 2017)
(Ponnekanti & Prashant, 2015) (Umesh & Neetu, 2019).
2.7.4 Temperature Effect
High temperatures accelerated oxidation or even carbonization where grease hardens or forms a
crust. If the temperature of grease is lowered enough, Pump ability suffers and machinery
operation may become impossible due to torque limitations and power requirements. As a
guideline, the base oil’s pour point is considered the low-temperature limit of grease (Bahari, 2017)
(Ponnekanti & Prashant, 2015) (Umesh & Neetu, 2019).
2.7.5 Pumpability
Pumpability is the ability of a grease to be pumped or pushed through a system. More practically,
pump ability is the ease with which pressurized grease can flow through lines, nozzles, and fittings
of grease-dispensing systems (Bahari, 2017) (Ponnekanti & Prashant, 2015) (Umesh & Neetu,
2019).
2.7.6 Water resistance
This test method is used to evaluate the ability of grease to adhere to a metal surface when
subjected to direct water spray. The results obtained from the use of this test method suggest
correlation in operations involving direct water spray impingement such as steel mill roll neck
bearing service (Ponnekanti & Prashant, 2015) (Umesh & Neetu, 2019).
23
2.7.7 Antiwear
The wear scar diameter was determined under the conditions including the speed of 1200 ± 60
rpm, the load of 40 ± 2 kgf (392 N), the temperature of 75 ± 1.7 °C, and test duration of 60 ± 1
min. In this method, a steel ball was rotated under the load against three stationary steel balls
having a surface that was lubricated by grease. After completion of the test, the diameter of the
stationary ball was measured to determine the wear preventive characteristic of grease in sliding
steel on steel application (Syahrullail, et al., 2014). In this method, we carried out two tests and
their average was taken as wear scar diameter in mm (Ponnekanti & Prashant, 2015) (Umesh &
Neetu, 2019).
2.7.8 Weld load or critical load
The weld load was carried out at 1456 rpm under room temperature. This standard is specified
procedure for the measurement of the load-carrying, antifriction and anti-wear property of
lubricating oils and fluids through the different testing machine. In this method, the weld load was
measured as kgf. It is a “gravitational metric” unit of force and is equivalent to the force exerted
on a mass of one kg in 9.806 m/s2. The advantage over Newton is it avoids the use of factor g
which is the acceleration due to gravity. In kgf, where f means only force and 1 kgf = 9.806 N
(Ponnekanti & Prashant, 2015).
2.7.9 Biodegradability
In this method, the ultimate biodegradability of the base oil is determined. Here, biodegradability
was measured by collecting the CO2 produced when the lube oil was exposed to microorganisms
under controlled aerobic aquatic conditions. This value was compared with the theoretical amount
of CO2 (Ponnekanti & Prashant, 2015) (Umesh & Neetu, 2019).
2.6.10 Toxicity
Bacterial toxicity of the base oil was determined by the modified method of the Algal inhibition
test. Here, instead of Algae, natural sewage Bacteria were used to determine the toxicity (Bahari,
2017) (Ponnekanti & Prashant, 2015) (Umesh & Neetu, 2019).
2.8 Common types of greases and characteristics of grease
They are eight different common types of greases are manufacturing to use for different purposes,
such as including wheel bearing grease, universal joint grease, chassis grease, extended lubrication
interval (ELI), multipurpose grease, extreme pressure grease (EP), and spindle grease
(Mohammed, 2013).
24
Those different types of greases are:-

2.8.1 Aluminum Complex Grease
Have good high-temperature characteristics, with a dropping point of approximately 500°F,
excellent water tolerance, good shear stability, and response very well to additive treatments that
enhance performance capabilities, such as oxidation and rust inhibition. Frequently used in
lubricating food machinery (Mohammed, 2013).
2.8.2 Bentone (Clay) Grease
Bentonite clay is treated with a polar activator that will give an electrical charge to the clay
particles, thus aligning them to hold the lubricating oil in suspension in a non-soap thickener,
grease structure. Not very compatible with other greases, since the electrical charge may be
destroyed and soften the grease beyond performance limits. This type of product is often called
No-Melt grease. Have good water resistance, low-temperature pumpability, and extremely high-
temperature applications where non-melting grease is required, the clay structure can aid in setting
up a self-forming oil seal where bearing seals are impossible to maintain such as in wheel bearings
on high-temperature kiln cars (Mohammed, 2013).
2.8.3 Calcium Grease
Among one of the first types of grease manufactured. Recently used largely; because they are
moderately priced. It is manufactured by using hydrated lime and fatty material. Calcium grease
must be used in a lower temperature environment since it is limited to approximately 150°F.
Higher temperatures may alter the grease structure. Has very good water tolerance (Mohammed,
2013).
2.8.4 Lithium (12-Hydroxy Stearate) Grease
Multi-purpose type grease with a buttery texture and dropping point above 350°F.It can be used
with occasional temperatures up to 300°F. Lithium grease has excellent resistance to water and
breakdown, or softening, by working. Pumpability is a very strong characteristic for this type of
grease. The term Multi-Purpose Grease is used because they combine, in a single product, desirable
characteristics normally found in each of several products. Almost 60% of the total grease market
is satisfied by this type of grease (Mohammed, 2013).
2.8.5 Lithium Complex Grease
25
A newer type of grease, showing many of the same characteristics as the simple lithium greases,
with improved performance in the area of high temperature, high speed bearing life. The dropping
point is approximately 500°F (Bahari, 2017) (Mohammed, 2013).
2.8.6 Polyurea grease
Greases are a fairly recent development that does not use a conventional soap thickener. This type
of grease has a high dropping point, approximately 470°F, has an ashless structure, excellent water
resistance, pumpability, and provides superb high temperature bearing life. Often used in electric
motors, alternators, and food machinery. Some Polyurea greases are very shear sensitive, that is,
they will soften in dispensing and harden in the bearings. Lighter consistency greases may give
better performance under these conditions. It’s the most important organic nonsoap thickener
(Mohammed, 2013).
2.8.7 Sodium Grease (Soda Soap)
Generally fibrous textured, stringy grease was used as a standard wheel bearing grease for many
years. Dropping points will vary between 300 – 400°F, and have good shear stability, Low-cost
grease that has good rust protection but very poor water resistance (Mohammed, 2013).
2.8.8 Grease Compatibility
When two greases are mixed, the resultant mixture often exhibits properties and performance
Characteristics that are markedly inferior to those of either grease by itself. Therefore, it is wise to
exercise caution in switching between types of grease that may have compatibility problems. The
system should be cleaned of all previous grease when making a switch between grease types. If it
is impossible to remove the previous grease type from the bearings, grease more frequently until
all traces of the previous grease have been flushed out of the bearing (Mohammed, 2013).
2.9 Factor affecting the quality of grease
There are different types of factors affecting the quality of greases the six factors that affecting the
qualities of greases. The life of a lubricant those are affects the qualities are oxidation, thermal
degradation, contamination, foaming, Demulsibility, air release (Bahari, 2017).
2.10 Tribological property of grease
The tribological study of different components in industrial applications has been a study of
interest over many years. Tribology is the study of friction, wear, and lubrication between the
surfaces moving relative to each other. The tribology does not include the study of tribological
properties of surfaces if they are not in relative motion. The interacting surfaces in relative motion
26
are accompanied by friction. Friction between the surfaces leads to the dissipation of energy
resulting in the loss of resources. The main cause of friction is adhesion and deformation. In
adhesive friction, the interacting surfaces are held together by the molecular binding force. The
friction due to the deformation is caused when a harder surface gets in between the asperities of
softer surfaces and deforms it. The main consequence of friction is wear. The wear leads to the
degradation of materials performance and wastage of materials also takes place. Excessive wear
eventually causes the materials to fail. The tribological study has implications in many industries
including mechanical, electrical, and even computer engineering. Being able to understand and
improve the way that materials interact will lead to improvements and advances in many fields
(Wani, et al., 2018).
2.10.1 Friction
It’s the resistive force generated between two surfaces interacting with each other. The frictional
force is a primary cause of loss of material between surfaces and can cause significant issues
depending on the situation. As mentioned in the previous section, the laws of friction were first
developed by Leonardo Da Vinci. These early laws were then further elaborated by Amontons.
Several years later after conducting his experiments, French physicist Charles Coulomb observed
that the frictional resistance among mating materials arose from the mechanical interlocking of
surface asperities. Many factors contribute to the level of frictional force, including geometry,
material properties, and environmental conditions. This thesis will focus on the analysis of
lubricated friction and dry friction. Lubricated friction describes the friction in which a lubricating
material is sandwiched between two moving surfaces. Dry friction describes the resistance of two
solid surfaces in relative contact with one another (Mohammed, 2013) (Shahabuddin, et al., 2013)
(Wani, et al., 2018).
2.10.2 Wear
The progressive loss of material among interacting surfaces is called wear. It occurs as a result of
mechanical and/or chemical interactions and can be accelerated by thermal means due to friction.
One contributing factor is the surface characteristics of the material. In addition to surface
asperities, the wear volume/rate will be a function of material hardness. The tribological study
focuses on analyzing the mechanisms which cause wear in the hopes of improving machine
performance. The mechanisms responsible for wear include abrasive, adhesive, fretting, and
tribochemical wear (Mohammed, 2013) (Shahabuddin, et al., 2013) (Wani, et al., 2018).
27
2.10.3 Lubricant
The addition of a film of material between two interacting surfaces to reduce the effects of friction
between them is referred to as lubrication. By adding a lubricant in between the moving surfaces,
not only can the friction be reduced but the wear and thermal energy as well. Besides, lubricants
can serve to remove wear particles from the surfaces thus improving the flow of motion and
reducing the chances of those particles causing abrasive damage. A lubricant can be in the form of
a liquid, solid, gas, or any combination thereof. The proper application and selection of a lubricant
can significantly prolong the life of mechanical components. Essentially, there are three different
modes of lubrication. Boundary, fluid film (hydrodynamic), and mixed lubrication
(elastohydrodynamic) (Mohammed, 2013) (Wani, et al., 2018).
2.11. Grease Manufacturing Methods
Manufacturing of grease is carried out either in pressurized vessels or open cooking kettles.
Greases can be made either by Batch Process or In-line/ Continuous Process.
Batch process and Continuous process
When comparing these two methods Batch process is preferable because it is more advantageous
over the Continuous process. The manufacture of lubricating greases has shown constant progress
with time. This holds for raw materials, equipment, processes, and formulations (Kuikka, 1999).
2.11.1 Batch process
2.11.1.1 Steps Involved During Batch Processes
Figure 2.4 The flow chart of the batch is processing to manufacturing greases (Kuikka, 1999).
28
Batch production is the most common manufacturing method. The steps of manufacturing include
the following:-
1. Bulk ingredients are metered or weighed into the processing reactor. For soap-based
greases made by saponification (the process of forming soap by splitting a fat with an
alkali), the fatty ingredient, alkali, and a portion of the oil are added to the reactor. By
heating (300 - 450°F) and mixing, the fat is converted to soap, and the soap is dispersed
throughout the mixture. This may be done in open kettles or closed pressure kettles. After
the completion of saponification and dehydration (removal of water), the remaining oil is
added to the batch to lower the temperature. Next, the grease is milled or homogenized.
2. This step of homogenization or milling is very important because it will produce a
uniform crystal and gel structure that will not change when the grease is used.
Homogenizing the grease will break down the solid particles or fibers and will disperse the
resultant small particles in the liquid. It also breaks up lumps, eliminates graininess, and
produces a smooth product. Homogenization of certain types of greases will stiffen the
grease producing lower penetration value. Homogenization can improve texture and
“brighten” grease’s appearance. In many cases, this homogenization process is carried out
at temperatures greater than 200°F (93°C).
3. After homogenization, the grease is further cooled, desecrated, and packaged. Of course,
it is understood that many different grease manufacturing methods are depending on the
type of grease and the manufacturer (Kuikka, 1999).
Advantages of Batch process
i. The batch process offers a great advantage over a continuous process, which includes
manufacturing operation in which flexibility is required in either a rate or mixture of
products.
ii. Batch process adjusts production either operating the flexibility on fewer shifts or
manufacturing a different product that is in higher demand e.g. Continuous distillation
column has an efficient range of products that are set by the hydraulic limitations of
flooding at the high end and weeping at the low end. Operations outside this limit are not
feasible.
iii. In the batch, process equipment can be reused.
iv. Process variables can be subjected to adjustments.
29
v. In batch process, multi-product operation can be done.

vi. Grease has a demand that changes over time or has seasonal variability. And this type of
variability is well suited to batch manufacturing.
vii. The cost required is less in the case of the batch process.
2.11.1.2 Continuous Process Flow chart of Continuous Process
Figure 2.5 Continuous Process Flow chart of Continuous Process (Kuikka, 1999).
The saponifiable material, lubricating oil & metal base flows into the inlet of the saponification
zone of the tubular reactor. In the saponification zone pressure is about 100-300 PSIG and
temperature up to 180°F.
The reactant stream is passed through the saponification zone at a velocity that is preferably
sufficient to maintain turbulent flow within the tubular reactor. Reactant mixture flow velocity is
sufficient for producing highly turbulent flow with Reynolds number in the range of about 4000
to 100000. Flow rates required for obtaining the degree of turbulence are generally within the
range of about 0.6-12.0ft 3/min. of the reaction mixture. For obtaining such high flow rates of
reactant mixture through saponification zone reactor outlet may be recycled to the reactor via
reactor inlet. It is desirable to minimize the water injected into the grease with the additives. The
temperature of the reaction mixture which comes out of the saponification zone is maintained in
the range of about 250-350°F. A temperature of about 350°F is sufficient to provide the necessary
30
amount of heat to such combined mixtures. The temperature of the combined mixture should not
exceed the melting point of the soap component of the grease.
Additional heat is imparted to the combined mixture is heating means to restore or increase
the temperature of the combined mixture to about 250°F and to prevent condensation of water.
The dehydration zone comprises a vertical cylindrical vessel having a volume sufficient to receive
combined mixture and water vapor and provide a residence time of about 1 to 20 minutes.
The dehydration zone is maintained under vacuum conditions. Due to such conditions all the
liquid water present in the combined mixture flash vaporizes. The grease mixture is recycled
continuously from the bottom of the dehydration zone with pressure up to 10-200 psi. Recycling
of the grease mixture is preferably carried out at a rapid rate such that the turnover
the rate in the dehydration zone is at least equivalent to about the average volume of grease
therein per minute. The recycling rate and average residence time in the dehydration zone are
sufficient to provide a soap conditioning period of at least about 5 minutes. By such conditioning,
the soap of grease mixture is reduced to a consistency that contributes to the desired consistency
for the product grease.
The base oil which is added to the grease mixture is at a lower temperature than that of the grease
mixture. This is done for cooling purposes. In case if additional cooling is desirable then the
grease may be passed through the cooler and the grease mixture may be recycled for obtaining
multiple passes (Kuikka, 1999).
31
CHAPTER THREE
3. Design, Methods, and Materials
3.1 Overall Methodology
This research thesis is focused on the preparation of bio-grease lubricants using the alternative
additive of Sugarcane Filter Cake Oil with 50% Sugarcane Filter Cake Wax (SCW) and Soybeans
oil as a based oil to improves the tribological properties and it will be analyzed. In general, the
overall methodology of this research thesis is in the experiment. These experiments are using
standard procedures for each test per item. It uses different steps; the first step is preparing the
samples of Soybeans as base oil instead of petroleum oil and Sugarcane Filter Cake oil with
Sugarcane Wax as an additive instead of a traditional additive. The second step is analyzing and
testing the tribological property (Resistance of Wear, Friction, and lubrication), Dropping point
temperature, and Viscosity of bio grease produced from the sample.
3.2 Material selection and design of an experiment to conduct Lubricant Biogreases
3.2.1 Material Selection
The materials that are used in this research thesis are Soybeans oil as the base oil, SCW as an
alternative additive, and Lithium Hydroxide as a thickener. Those sample materials except the
additives are bought from the market to improve the test but the additive that is used in this research
is SCW. It came from the “Las Tunas Energy Research Center” of Las Tunas University, Cuba.
This material that used the additive is characterized in this Research Center. As Base oil selected
for production of bio grease is Soybeans oil:
Table 3.1 Value of specification of Soybeans oil (BRAJENDRA, et al., 2005) (Ozioko, 2012).
No. Parameter Value
1 SAE Grade Soybeans crude oil
2 Flashpoint (OC) 310
3 Fire point (OC) 320
4 Pour point (OC) -7
5 Specific gravity (g/ml) 0.917
6 Viscosity at 400 (cst) 29.37
7 Viscosity at 1000 (cst) 8.08
8 Viscosity index 225
32
a) As Additive used in the thesis:-

 Sugarcane Filter Cake containing 50 % Sugarcane Filter Cake Oil and 50% Sugarcane
Filter Cake Wax.
b) The Thicker used in this thesis:-
 Lithium hydroxide (LiOH)
 Lithium greases have high water resistance and a dropping point of about 190 °C. It can
be used at temperatures up to 135 °C and extreme pressure and speed Machines. Lithium
greases have a smooth and buttery appearance with low fibrous content.
 Composite materials of LiOH (Monohydrate):- it's extra pure those are Carbonate (Li2O2),
Chloride (Cl), Sulphate (SO2), Calcium (Ca), and Sodium (Na).
3.2.2 Laboratory Equipments
 400 ml Beaker its heat resistant materials
 Oven
 Mixer or Rotor
 Infrared Thermometer (T oC) and Mercury thermometer
 Tachometer (RPM)
 Digital balance
 Caliper or Micrometer
 Viscosity tester (Rotary tester)
3.2.3 Design of an experiment to conduct lubrication of bio grease
The design of the experiment is the process of making lubricant of bio grease, at the beginning,
there are three inputs (factors) that will be considered to control the investigation. Those factors or
independent variables are Hydroxides (LiOH) (X1); Sugarcane Filter Cake Oil with 50%
Sugarcane Filter Cake Wax (X2) and Time of reaction (X3). We want to ascertain the relative
influence (importance) of each of these factors on the response of the dependent variables
(Dropping point temperature, Viscosity, Wear, Friction).
Independent variables vs Dependent variables
Hydroxides (LiOH)=X1 Experimental Friction

Sugarcane oil with wax=X2 process to obtain Wear
Time of reaction= X3 bio-grease Dropping point temperature
Viscosity
33
Definition of variables (Independent and Dependent)

Independent:-
X1=Hydroxides (LiOH)
X2= Sugarcane Filter Cake Oil with 50% Sugarcane Filter Cake Wax
X3=Time of reaction
Table 3.2 Factor level settings
Level
No. Factorials Min (-) Max (-) Units
1 Hydroxides(LiOH) 2 5 %
2 SCW 2 5 %
3 Time of reaction 15 30 Min
Dependent: -Friction coefficient; Wear, Dropping point temperature, Viscosity. = Y (X1, X2, X3)
Y1=Friction
Y2= Wear
Y3= Dropping point temperature and Y4= Viscosity
The characteristics of the greases for performances are analyzed depending on the ASTM standard.
From the reference and the previous research for some application of bio greases and grease
lubricants; In the case of used 1kg mass; the bio greases lubricant testing result of the coefficient
of friction and wear is more than 0.039 and 1.00mm respectively (Zuan, et al., 2017). In the case
of lithium as a thickener; for mineral greases the COF is 0.04 up to 0.10 and for wear between
0.15mm and 0.50mm; Dropping point temperature 190oC and also viscosity up to 3.00 Pascal
second (FLOREA & ANTONESCU, 2003) (Algailani, 2015). In general, table 3.3 show the ranks
of dependent variables or response factor that are expect testing result in this research thesis.
Table 3.3 Response of the test.
Level
No. Response Min (-) Max (-) Units
1 Friction coefficient, μ 0.03 0.098
2 Wear 0.10 0.50 gram
O
3 Dropping point temperature 80 >200 C
4 Viscosity 0.03 3.00 Pa.s
34
3.2.4 Factorial experimental design (2k)

Factorial design of experimental, the total amount of factors (independent variables) to be
investigated is k = 3 and 2 levels. So, 2k = 23 = 8 runs of experiments but to get the experimental
matrix with some center point design and selected by software analysis the best ten-run for the
experiment to save time and resources. In this way, it is obtained the experimental matrix shown
in table 3.4.
Full model running the full complement of all possible factor combinations means that we can
estimate all the main and interaction effects.
First, the entire necessary sample had been prepared for the test; Characterization of the samples,
by mixing the sample produced grease and by using the standard procedures conduct the research.
Table 3.4 Factorial experiment design table or design matrix by using stat graphics.
Hydroxides Sugarcane oil Time, Friction Wear, Dropping point Viscosity,
N0. (LiOH), % with wax, % min coefficient gram temperature, OC Pa.s
1 2.0 2.0 22.5
2 2.0 5.0 22.5
3 5.0 3.5 15.0
4 2.0 3.5 30.0
5 5.0 3.5 30.0
6 3.5 2.0 15.0
7 3.5 5.0 15.0
8 3.5 2.0 30.0
9 3.5 5.0 30.0
10 3.5 3.5 22.5
The table 3.4 show that the factorial experiment design table or design matrix found the value of
independent variable or Factors by using Statgraphics Software.
The dependent variables or the response variable, its values will be found for each experiment after
carried out the experimental test.
35
Diagraph of Experimental Factorials

Figures 3.1 shows that the flowchart of the design of experimental factorial which is prepared for
the experimental factor from the beginning of the input factor up to run the experiment according
to the design of the matrix of the experimental.
Figure 3.1 Flowchart of Experimental Factor

3.3 Methodology
The research thesis is conducted in the laboratory, which basses on laboratory experiments by
running the samples through different characterization equipment, before and after the treatment
of the sample.
3.3.1 Standard Experimental technique to produce lubricating grease
In case Grease formulation is achieved in three stages:-
Stage 1:- The mixture was boiled and stirred until saponification takes place with foaming.
Stage 2:- The saponification mixture was further boiled, stirred to dehydrate.
36
Stage 3:-The heater was turned off and a melted grease base was stirred and more oil added as a
finishing procedure. This is required to bring down the temperature of the grease to a safe storage
range to avoid separation.
3.3.2 Experimental procedure used in this research to produced Bio-greases.
Figure 3.2 Flow chart of the step of the experiments according to the matrix (Shahabuddin, et al.,
2013).
37
3.3.3 Method of processing and Analysis

The experiments are using standard procedures for each test per item. The experiments are two
different steps; the first step is prepared the samples of grease by using Soyabean oil as base oil
instead of petroleum oil and Sugarcane Filter Cake Oil with 50% Sugarcane Filter Cake Wax as
an additive instead of traditional additive and Lithium Hydroxide as a thickener. The second step
is involved analyzing and testing the tribological property (resistance of wear, Coefficient of
friction, and lubrication), dropping point temperature, and viscosity of bio grease produced from
the sample by the standard testing machine.
3.3.3.1 Analysis
The data analysis is based on the laboratory results. The grease made using different ratios of base
oil, Lithium hydroxide as a thickener, and the additive was tested for Dropping point lubricating
(ASTM D-566), Viscosity test lubricating greases, EP (Wear) (ASTM D-2266) (Bahari, 2017)
(Mohammed, 2013).
3.4 Grease characterization for performance
There are different characteristics of grease tested method concerning about ASTM-D standard or
the tribological performance of the product was studied on pin-on-disc machines as per ASTM-D
test methods.
Grease characterization was carried out in Addis Ababa University Information Technology
(AAiT), Federal Technic and Vocational Educational Institution (FTVEI) and in General Wingate,
Polytechnic College Physicochemical Department analyzed the samples of Soybeans oil and
Sugarcane Filter Cake Oil with 50% Sugarcane Filter Cake Wax and Lithium hydroxide greases.
Physicochemical properties and some characteristics such as dropping point temperatures,
viscosity, wear, and coefficient of friction of bio grease are tested.
38
Table 3.5 Main methods and standard tests for lubricating greases (ASTM D-2266) (Bahari, 2017)
(Mohammed, 2013).
Properties Norma ASTM D
Color Visual
Penetration work 25 60 strokes, 1/10 mm. ASTM D-217
Drop point temp, ASTM D-566
Alkali content ASTM D-128-98
Critical load, N. ASTM G-77
Wear ASTM G-77
Shear stability ASTM D1831
Oxidation stability ASTM D-942
The table 3.5 show that different types of ASTM D method testing standard of lubricating greases.
 In this research thesis no conducted all of greases performance but some of the characteristics
of the greases will be tested because of lab setup. The testing characteristics are:-
 Dropping Point Temperature ASTM D-566,
 The viscosity of lubricating greases,
 Wear STM D-2266 and
 Coefficient of friction.
3.4.1 Dropping point of lubricating grease ASTM D-566
Dropping point temperature is indicating that how much greases can resistance of heat. As grease
temperatures, the grease gets softer, until it liquefies and its rigidity or consistency is lost
(Mohammed, 2013) (Ponnekanti & Prashant, 2015) (Umesh & Neetu, 2019).
It is an indication of the type of thickener used, and a measure of the cohesiveness of the oil and
thickener of grease. The dropping point is an indicator of the heat resistance of the grease. As
grease temperature increases, penetration increases until the grease liquefies and the desired
consistency is lost. The dropping point is the temperature at which a grease becomes fluid enough
to drip. The dropping point indicates the upper-temperature limit at which a grease retains its
structure, not the maximum temperature at which a grease may be used. The test apparatus consists
of a grease cup with a small hole in the bottom, a test tube, two thermometers, a container, a stirring
39
device if required, and an electric heater. The rank of dropping point temperature is 80°C -200°C
and maybe more than 200°C (Ponnekanti & Prashant, 2015) (Umesh & Neetu, 2019).
3.4.2 Corrosion Resistance ASTM D-130
Corrosion resistance; means that the substance protects from damage caused by oxidization or
chemical reactions (Mohammed, 2013).
3.4.2.1. Copper corrosion ASTM D-130
The copper corrosion test provides a measure of the corrosiveness of the grease. This is done
introducing a sheet of copper polished in a certain amount of the fat to the temperature of
100, for three hours, then the copper foil is extracted, dried, and compared with standard
or standard sheets. This method consists of the immersion of a clean polished strip of copper
in a lubricant sample at 100°C for 3 hours. If desired, the test temperature and time maybe
varied from the standard conditions. At the end of the test, the strip is removed and cooled
(Mohammed, 2013) (Ponnekanti & Prashant, 2015).
3.4.3 Cone penetration of Lubricating Grease ASTM D-217
The consistency of lubricating grease characterizes the firmness or relative hardness of grease and
depends basically, the relationship between the thickener and the base oil. Consistency is an
an important factor in the Lubrication capacity, sealability, permanence in place, and ease with
which can be applied. The National Lubricating Grease Institute - NLGI, established a
classification of fats per their Consistency, which is determined experimentally by the
penetration produced by the fall of a cone Standard on a grease sample at 25℃ for five
seconds. Penetration is Expresses in tenths of millimeters and the greater the penetration the
less its consistency and therefore the Softer is fat. A slight chance of a parameter may result in a
change in penetration values. Besides consistency, structural and mechanical stability, apparent
viscosity, oxidation resistance can be tested to determine the suitability of grease to a specific
application (Mohammed, 2013) (Suhaila, et al., 2018) (Umesh & Neetu, 2019).
3.4.4 Water Resistance ASTM D-1831
In bio grease lubrication applications water contamination may cause the structure of the grease to
change. It may become softer or harder. It may adsorb water or reject it, and in some instances, it
may lose its adhesiveness or sealing capabilities. The use of fresh samples of process water from
the actual application(s) for which a lubricant is intended to be used is known to be critical in
determining the operating properties of lubricants. The differences in chemical composition,
40
contaminants, pH, and adsorbed gases in process waters versus the standard distilled water or
synthetic seawater specified in test methods can have a significant influence on the water resistance
and corrosion protection test results (DuradjiaV.N, 2016).
3.4.4.1 Water Spray-off ASTM D-4049
It evaluates the ability of lubricating grease to adhere to a metal surface when subjected to a direct
water spray under controlled conditions. The percentage of grease sprayed off a stainless-steel test
panel after a specified period is determined by weight. This method consists of subjecting an
evenly distributed layer of lubricant spread at a given thickness on a stainless-steel panel to water
spray-off. The lubricant is sprayed with water at a given temperature for 5 minutes at a prescribed
pressure. The panel is then air-dried and weighed. Spray-off resistance is reported as the mass
percent of lubricant removed by the water spray (Umesh & Neetu, 2019) (DuradjiaV.N, 2016).
3.4.4.2 Wet Roll Stability ASTM D-1831
This method consists of running the standard ASTM D-1831 roll stability test with the addition of
the presence of water. Process water such as that containing sugar cane juice may be used instead
of specified standard water. Visual inspection of the lubricant and its penetration change after
being subjected to roll shear, along with the presence of free water and its quantity, are determining
factors for the water-resistance characteristics of the lubricant (DuradjiaV.N, 2016).
3.4.5 Weld load or critical load
The weld load was carried out at 1456 rpm under room temperature. This standard is specified
procedure for the measurement of the load-carrying, antifriction and anti-wear property of
lubricating oils and fluids using the different testing machine (Ponnekanti & Prashant, 2015).
3.4.6 Oxidation stability
This is the ability of a grease to resist a chemical union with oxygen. The reaction of grease
with oxygen produces insoluble gum, sludge’s and lacquer-like deposits that cause sluggish
the operation increased wear, and reduction of clearances. Prolonged exposure to high
temperatures accelerate oxidation in greases. The oxidation stability of grease (ASTM D-
942) is the ability of the lubricant to resist oxidation. It is also used to evaluate grease stability
during its storage. The base oil in grease will oxidize in the same way as lubricating oil of a
similar type. The thickener will also oxidize but is usually less prone to oxidation than the
base oil. So, an anti-oxidant additive must be selected to match the individual grease. There
41
the primary function is to protect the grease during storage and extend the service life, especially
at high temperatures (Ponnekanti & Prashant, 2015) (Umesh & Neetu, 2019).
3.4.7 Extreme pressure/ Antiwear or Wear and Friction Measurement
3.4.7.1 Extreme pressure/ Antiwear or Wear resistance
The term “extreme pressure” lubrication is perhaps misleading since presumably the pressure per
unit area on the actual contacting surfaces does not change with loading, rather the increased
pressures result in the increased contact areas. In extreme pressure (EP) tests the lubricant is
subjected to loading which is increased in specified steps after each stroke. This increase in load
is continued until a load of where the lubricant fails. The lubricant failure is indicated by welding
the bottom of the three balls to the top ball. The load at which the weld is produced is the index of
the extreme pressure property of the lubricant. Equipment such as the Four-Ball EP and Four-Ball
Wear tester, to name only two, have played and continue to play a critical role in the development,
testing, and selection of lubricants (Alliston, 2016) (Dugić M, et al., 2013) (Mohammed, 2013)
(Wani, et al., 2018) (Zuan, et al., 2017).
Antiwear or Wear resistance
Wear is defined as surface damage of one or all solid surfaces in contact subject to relative motion.
Wear might have different patterns corresponding to various wear mechanisms. A surface can be
subject to more than one wear mechanism simultaneously. The process of wear can change
continuously in time or with changes in operational conditions. Wear is usually accelerated by
frictional heating using chemical and mechanical interactions (Algailani, 2015) (Alliston, 2016)
(Wani, et al., 2018).
Procedure
1) Immediately before testing, and before measuring or weighing, clean and dry the specimens.
Take care to remove all dirt and external matter from the specimens. Use nonchlorinated,
non-film-forming cleaning agents and solvents. Dry materials with open grains to remove
all traces of the cleaning fluids that may be entrapped in the material. Steel (ferromagnetic)
specimens having residual magnetism should be demagnetized. Report the methods used
for cleaning.
2) Measure appropriate specimen dimensions to the nearest 2.5 µm or weigh the specimens
to the nearest 0.0001 g.
42
3) Insert the disk securely in the holding device so that the disk is fixed perpendicular (90°)
to the axis of the resolution.
4) Insert the pinned specimen securely in its holder and, if necessary, adjust so that the
specimen is perpendicular (90°) to the disk surface when in contact, to maintain the
necessary contact conditions.
5) Add the proper mass to the system lever or bale to develop the selected force pressing the
pin against the disk.
6) Start the motor and adjust the speed to the desired value while holding the pinned specimen
out of contact with the disk. Stop the motor.
7) Set the revolution counter (or equivalent) to the desired number of revolutions.
8) Begin the test with the specimens in contact under load. The test is stopped when the
desired number of revolutions is achieved. Tests should not be interrupted or restarted.
9) Remove the specimens and clean off any loose wear debris. Note the existence of features
on or near the wear scar such as protrusions, displaced metal, discoloration, microcracking,
or spotting.
10) Remeasure the specimen dimensions to the nearest 2.5 µm or reweigh the specimens to
the nearest 0.0001 g, as appropriate.
11) Repeat the test with additional specimens to obtain sufficient data for statistically
significant results (Bahari, 2017).
3.4.8 Friction
Friction is the resistive force generated between two surfaces interacting with each other. The
frictional force is a primary cause of loss of material between surfaces and can cause significant
issues depending on the situation (Bahari, 2017) (Wani, et al., 2018) (Zuan A.M.S., 2017).
3.4.8.1 Tribometer
The experiments were carried out in the Federal Technical and Vocation Education Institute, was
analyzed the samples of Soybeans oil base oil and lithium as thickener from Ethiopia and SCW
samples come from the Energy Research Center of Las Tunas University from Cuba.
Test duration influence
After the first minutes, the wear begins, but during the test, the variation of friction coefficient is
small. This aspect is possible because the wear spot increase and at the same time load of the
43
contact pressure decrease. The lubricants have in these conditions a great influence (Trivedia H.K
& Bhatt D.V., 2017).
Table 3.6 Specification of the tribological (wear and COF) test machine (Shahabuddin, et al.,
2013).
Parameter Value Used in this thesis
Disc Diameter More than 110.0 mm 227.00mm
Pin Diameter 2.00-10.0 mm 8.00mm

Disc Speed Range 25 to 3000 rpm 2120rpm
Motor Tuscan; (2000 rpm, 1.5 kW) (2000 rpm, 1.5 kW
Load Range 0 KG to 30 KG 2kg
Electrical Input 220 Volt AC 50 Hz 220 Volt AC 50 Hz
3.4.8.2 Steps for friction and wear test
The performance of these friction and wear tests comprises the following steps:
Note: - In this research used to measures friction and wear by using the pin on disc tester machine.
 The research was used to calculate the frictions of the objects were by dividing the normal force
of the object by the frictional force.
 To measure the Wear are used caliper or micrometer for each of the steps.
In this research used steps were:-
1) First measured the height of the pin Specimen of the tester before connect to the specimen
holder.
2) Second, put the different ratios of produced grease into the disk of the pin disk tester.
3) Third, put the pinned specimen on the surface of the disk of the tester
4) Forth Put the load on the arm of the tester.
5) Start the motor and wet into 10 minute
6) Stop the machine and remove the pinned specimen
7) Measure again the height and subtract in the first result that is found in step one (Subtract
before the test and after test)
8) Repeat the steps from 1-7 for each 10 samples test.
9) Recorded the result for each test.
44
CHAPTER FOUR
4 Result and Discussion
4.1 Result
A total of ten (10) Biogreases samples were produced Soybeans oil from for each different
proportion of Lithium hydroxide as thickener and Sugarcane Filter Cake oil with 50% Sugarcane
Filter Cake Wax as additive. Put 110g of Soybean oil into a 400ml beaker and heated at 100 0C
for 15 minutes. Lithium hydroxide was added according to the experiment's different ratio. The
mixture is stirred and heated up to a temperature of 200 0C for 15-30 minutes depends on the time
ratio and then cooled to 100 0C. Sugarcane Filter Cake oil with Sugarcane filter cake Wax as
additive added depends on the experimental ratio for each different ratio. The stirring and heating
are continued at the temperature of 100 0C for the next 30 minutes and cooled to a room
temperature of 25 0C for 45 minutes and stored for future analysis. The basis for the preparation is
on two parameters which are percentage weight and temperature.
Tables 4.1 Composition of materials and temperature for Soybeans Bio grease production.
Grease formulation Soybeans
Mass of base oil 110g
Mass of thickener -2, +5 g
Mass of additive -2, +5 g
Mixing temperature 100 (0C)
Maximum reaction temperature 200 0C
The mixing temperature of additive 100 0C
Cooling period 45 min
Cooling temperature 25 0C
4.1.1 Physiochemical properties of produced Biogreases
First, the entire necessary samples of the product were produced by using the standard procedures
and by mixing the necessary materials to produce the grease.
4.1.1.1 Produced greases samples Appearance
Table 1 in appendix 1 shows that the first experimental design, its high amount of the percentage
of hydroxide as a thickener (5-20%) and the additive (5-10). As shown in figure 4.1 the greases
in case of the high amount of thickener and additive used in the production of grease affecting the
45
qualities of the bio grease product. The thickener was in the range of 5% to 20 % and also the
additive a ranging from 5% to 10 % in the production. The value of thickener and additive
depending on the range that is expressing in figure 2.5.
The first two productions were Semi-solid as compared to the others because of the usage of
smaller amounts of thickener and additive. But using the maximum amount of thickener and
additive in the range, the grease produced was solid and that is demonstrated in pictures 3a-6. Even
if halving the amount of the thickener to 10%, the results were not changed and the thickener
dominated the production. This fact is demonstrated in picture 3c. From the observation the figure
4.1 using a high amount of thickener and additive (11% and 8.25 respectively) will give the
unsuitable quality of grease. Therefore in this range, the product physical visual aspects of the
Soybeans oils base greases have appeared with different visual properties. So figure 4.1 show that
the Biogreases lubricants at high content of thickener and additive.
Figure 4.1:- In case of the high amount of thickener and additive in the production of Bio-grease
So in this research, the least amount of thickener and additive in the range of 2%-5% and 2%-5%
respectively were used. This is attributed to the usage of high consistency additive as compared to
the previous researches. The result of the product in visual aspect is put in the table below with
46
some descriptions and figure 4.2 shows the product produced in the least range of thickener and
additive.
Table 4.2 shows the visual aspect of the product of grease by used Soybean oil as the base oil,
Lithium Hydroxide as a thickener and Sugarcane Filter Cake oil with a 50% Sugarcane filter cake
Wax as additive. In the table showing the different products in different ratios and from the
products were three of them different from the others because they are hard comparing from the
mineral greases because it’s soft.
The third and the sixth products are mixing problems because of the time of reaction, the lithium
hydroxide is not mixed appropriately with the oil.
Table 4.2 Soybeans grease Visual aspect of the ten samples produced in different ratio of additive
and thickeners
No. Samples Description Visual aspect
1 Soybean Soft Brown
2 Soybean Soft Dark brown
3 Soybean Soft Golden
5 Soybean little Hard Golden
6 Soybean Hard Brown
9 Soybean Hard Dark brown
Total produced ten (10) samples of bio greases, by using of Soyabeans as base oils, as additive
Sugarcane Filter Cake Oil with 50% Sugarcane Filter Cake Wax and lithium hydroxide as a
thickener. From these ten (10) samples, three of the samples were different from the other product
and also comparing from the mineral grease; two of this product were the reaction problem and
hard but the other one was only little hard product comparing from each other and with the mineral
greases because the mineral grease is a soft material.
47
In the figure 4.2 show the last product of the samples and in this research tested different parameter
of performance of the product. The results were improved after the thickener and additive were
reduced up to (2-5%) for both cases. The product was produced as the expressing on table 3.4
factorial design matrix.
Figure 4.2: Sample production of Soybean oil and sugarcane filter cake oil with wax grease.
Comparing some of the product by the visual aspect
a) Number three and five in figure 4.2 are similar in additive and thickeners but different in
the time of reaction. The difference in the result is because of the different reaction times.
Having lower reaction time number three was not completely reacted unlike that of
number five which had a longer reaction time. Number five was completely reacted and it
was a little hard as compared to number three.
b) Number six and eight in figure 4.2 are similar in additive and thickeners but different in
the times of reaction. The difference in the result was because of different reaction times.
Having a lower reaction time number six was not completely reacted unlike that of
number eight which had a longer reaction time. Number eight was completely reacted
and it was soft as compared to number six.
48
4.1.2 Characteristics of lubricating greases or Performance of Grease characterization

4.1.2.1 Dropping point and viscosity
The ten samples of the product of Soybean oil and SCW bio grease dropping point temperature
(DPT) and viscosity @100 OC the experimental testing result.
Table 4.3 Test result of biogrease of the lubricant
Testing results 1 2 3 4 5 6 7 8 9 10
DPT OC 143 123 119 110 130 90 120 110 85 130
Viscosity @100OC Pa.s 0.50 0.32 0.40 0.24 0.50 0.30 0.16 0.18 0.60 0.55
4.1.2.2 Tribological test (Wear and Frictional test)

Result of Friction and Wear for bio grease from Soybean & SCW additive in Tribometer pin on
disc (Bronze on Cast Iron) test and mineral grease test.
 Test = 1 The pin on Disc Test: - Pin Bronze, Grease 1
Greases= Soybeans base oil
Mass= 2kg; Diameter of pin=8 mm and Initial length pin=41.16 mm and Final length of pin
Lf=41.00mm and Initial Weight pin Wi =16.3gram and Final weight of pin Wf= 16.235gram
Table 4.4 The first lubricant test at Normal force =50.66865N
No. T, sec Fr; N COF

COF
1 30 0.045498548
2.3054 0.06
2 60 1.8639 0.03678606
0.05
3 90 2.1582 0.042594385 0.04
4 120 2.0111 0.039690223 0.03 The pin on
5 150 2.0111 0.039690223 0.02 Disc Test
pin Bronze,
6 180 2.3544 0.046466602 0.01 grease 1
7 210 1.8639 0.03678606 0
0 100 200 300 400
8 240 1.962 0.038722168
Time, sec
9 270 2.5996 0.051306873
10 300 2.2563 0.044530494 Figure 4.3 The chart show that the lubricant test-1.
11 330 2.2563 0.044530494
49
The result of the coefficient of friction (COF); Wear (DW) and DL Wear length of the pin; T=time
and Fr=Friction force
COF 0.042418375
DW 0.06537745gram
DL= 0.16mm
 The above result shows that the results of the lubricant test on a pin on a disc testing
machine. In the case of test 1 by using produced grease 1.
 Test =2 The pin on Disc Test: - Pin Bronze, Grease 2
Mass= 2kg
The diameter of pin=8 mm
Initial length pin Li=41.10 mm and Final length of pin Li= 30.60mm
Initial Weight pin Wi =16.6gram and final weight of pin Wf= 16.396gram
Table 4.5 The Second lubricant test at Normal force =48.9519N

COF
1 30
4.1202 0.084168337 0.1
2 60 3.9731 0.081162325 0.09
0.08
3 90 4.1693 0.085170341 0.07
0.06
4 120 4.1693 0.085170341 0.05
0.04 The pin on Disc
5 150 4.2183 0.086172345 Test pin
0.03
6 180 4.4145 0.090180361 0.02 Bronze, grease 2
0.01
7 210 4.4636 0.091182365 0
8 240 4.1202 0.084168337 0 100 200 300 400
Time, sec
9 270 4.2674 0.087174349
10 300 4.3164 0.088176353
and Fr= Friction force.
50
COF 0.0869011
DW 0.204305gram
DL= 0.50 mm
machine. In the case of test-2 by using produced grease 2.
Mass= 2kg
Initial length pin=40.22 mm and Final length of pin Lf=39.70mm
Initial Weight pin Wi =16.1gram and Final weight of pin Wf=15.888gram
Table 4.6 The third lubricant test at Normal force =50.08005N

COF
1 30 0.06072478
3.0411
0.07
2 60 2.5506 0.05093046
0.06
3 90 2.8449 0.056807052
0.05
4 120 2.9920 0.059745348 0.04
The pin on Disc
5 150 2.7468 0.054848188 0.03 Test pin
6 180 2.8449 0.056807052 0.02 Bronze, grease
3
7 210 2.5996 0.051909892 0.01
0
8 240 2.8449 0.056807052 0 100 200 300 400
9 270 2.6487 0.052889324 Time, sec
10 300 2.7468 0.054848188
The result of the coefficient of friction (COF);

Wear (DW) and DL Wear length of the pin; T= time and Fr= Friction force.
51
COF 0.05582762
DW 0.212476712gram
DL= 0.52mm
machine. In the case of test-3 by using produced grease 3.

Mass= 2kg
Diameter of pin=8 mm
Initial length pin Li=40.14 mm and
Final length of pin Li= 39.95mm
Initial Weight pin Wi =16.00gram and
final weight of pin Wf= 15.922gram
Table 4.7 The fourth lubricant test at Normal force=50.7177N
No T, sec Fr; N COF

COF
1 30
3.3354 0.065764023 0.07
2 60 3.3354 0.065764023 0.06
3 90 2.943 0.058027079 0.05
4 120 3.1392 0.061895551 0.04
5 150 2.9921 0.058994197 Test pin
0.02 Bronze, grease 4
6 180 2.9921 0.058994197
0.01
7 210 2.9921 0.058994197
0
8 240 2.9921 0.058994197 0 100 200 300 400
9 270 3.1392 0.061895551 Time, sec
10 300 3.1392 0.061895551

Figure 4.6 The chart show that the lubricant test-4.
11 330 3.1392 0.061895551
The result of the coefficient of friction (COF); Wear (DW) and DL Wear Length of the pin; T=time
52
COF 0.061192
DW 0.159357534gram
DL= 0.39 mm
 The above result shows that the results of the lubricant test on a pin on disc testing
machine. In the case of test-4 by using produced grease-4.
Mass= 2kg
The final length of pin Li= 40.06mm
Initial Weight pin Wi =16.00gr and
Final weight of pin Wf= 15.967311275gr
Table 4.8 The sixth lubricant test at Normal force =49.49145N
No T, sec Fr; N COF

COF
1 30
1.4225 0.028741328 0.04
2 60 1.1282 0.022794846
0.035
3 90 1.4225 0.028741328 0.03
4 120 1.4715 0.029732408 0.025
0.02
5 150 1.1282 0.022794846 The pin on Disc
0.015 Test pin Bronze,
6 180 1.7167 0.03468781 0.01 grease 5
7 210 1.4715 0.029732408 0.005
0
8 240 1.6677 0.033696729
0 100 200 300 400
9 270 1.6677 0.033696729 Time, sec
10 300 1.7658 0.03567889
53
COF 0.030723489
DW 0.032688725 gram
DL= 0.08 mm
 The above result shows that the results of the lubricant test on the pin on disc testing
Mass= 2kg
The final weight of pin Wf= 15.946880822 gram
Table 4.9 The sixth lubricant test at Normal force=49.3443N
No Time Fr; N COF

COF
1 30 0.235 0.04672
0.06
2 60 0.19 0.037773
0.05
3 90 0.22 0.043738
0.04
4 120 0.205 0.040755
0.03 The pin on
5 150 0.205 0.040755 Disc Test
0.02 pin Bronze,
6 180 0.24 0.047714 grease 6
0.01
7 210 0.19 0.037773
0
8 240 0.2 0.039761 0 200 400
9 270 0.265 0.052684 Time, sec
10 300 0.23 0.045726
54
COF 0.043557
DW 0.053119 gram
DL= 0.13 mm
 The above result shows that the results of the lubricant test on the pin on the disc testing
Mass= 2kg
Final weight of pin Wf= 15.750966913g
Table 4.10 The seventh lubricant test at Normal force=49.68765N
No T Fr; N COF
COF
1 30
2.8939 0.058242843 0.07
2 60 3.2863 0.066140178
0.06
3 90 2.8449 0.057255676
0.05
4 120 3.0411 0.061204344
0.04
5 150 2.8449 0.057255676 The pin on
0.03 Disc Test pin
6 180 2.9920 0.060217177 0.02
Bronze, grease
7
7 210 2.9920 0.060217177 0.01
8 240 3.2373 0.065153011 0
0 100 200 300 400
9 270 2.5996 0.052319842
Time, sec
10 300 2.7958 0.056268509
11 330 3.1882 0.064165844
The result of the coefficient of friction

(COF); Wear (DW) and DL Wear length of the pin; T=time and Fr=Friction force.
55
COF 0.059858207
DW 0.049033087 gram
DL= 0.12 mm
 The above result shows the results of the lubricant test on the pin on the disc testing
machine. In the case of test-7 by using produced grease7.
Mass= 2kg
Table 4.11 The eight lubricant test at Normal force=49.88385N
No. Time Fr; N COF

COF
1 30 0.079646018
3.97305 0.09
2 60 3.8259 0.076696165 0.08
3 90 3.48255 0.069813176 0.07
0.06
4 120 3.48255 0.069813176 0.05
The pin on
5 150 3.28635 0.065880039 0.04
Disc Test
0.03 pin Bronze,
6 180 3.18825 0.063913471
0.02 grease 8
7 210 3.58065 0.071779744 0.01
0
8 240 3.4335 0.068829892
0 100 200 300 400
9 270 3.4335 0.068829892 Time, sec
10 300 3.67875 0.073746313
11 330 3.4335 0.068829892
The result of the coefficient of friction (COF); Wear (DW); DL Wear length of the pin; T=time and
Fr= Friction force.
56
COF 0.070707071
DW 0.069464gram
DL= 0.17mm
 The above result shows that the results of the lubricant test on the pin on the disc testing

Mass= 2kg
Table 4.12 The ninth lubricant test at Normal force=49.88385N
No. Time Fr; N COF

COF
1 30
3.18825 0.063913471 0.1
2 60 3.77685 0.075712881 0.09
0.08
3 90 3.67875 0.073746313
0.07
4 120 3.97305 0.079646018 0.06
0.05 The pin on
5 150 4.1202 0.08259587 0.04 Disc Test
6 180 4.0221 0.080629302 0.03 pin Bronze,
0.02 grease 9
7 210 4.3164 0.086529007 0.01
0
8 240 3.924 0.078662734 0 100 200 300 400
9 270 3.924 0.078662734 Time, sec
10 300 3.3354 0.066863324
57
COF 0.077321891
DW 0.073549631gram
DL= 0.18mm
 The above result shows that the results of the lubricant test on the pin on disc testing machine.
In the case of test-9 by using produced grease-9.
Mass= 2kg
Table 4.13 The tenth lubricant test at Normal force=49.8348N
No. Time Fr; N COF

COF
1 30
2.30535 0.046259843 0.05
2 60 1.91295 0.038385827 0.045
0.04
3 90 1.52055 0.030511811 0.035
4 120 1.6677 0.033464567 0.03
0.025 The pin on
5 150 1.4715 0.029527559 0.02 Disc Test pin
0.015 Bronze,
6 180 1.71675 0.034448819 grease 10
0.01
7 210 1.71675 0.034448819 0.005
0
8 240 1.71675 0.034448819 0 100 200 300 400
9 270 2.1582 0.043307087 Time, sec
10 300 1.81485 0.036417323
and Fr= fraction force.
58
COF 0.035433071
DW 0.044946997
DL= 0.11
 The above result shows that the results of the lubricant test on the pin on disc testing machine.
In the case of test -10 by using produced grease -10.
Greases= Mineral grease
Mass= 2kg
Initial length pin Li=34.93mm and
Initial Weight pin Wi =15.6gram and
Final weight of pin Wf= 15.48150337gram
Table 4.14 The mineral grease lubricant test at Normal force= 52.185N
No. Time Fr; N COF

COF
1 30
3.97305 0.076056338
2 60 4.26735 0.081690141 0.1
0.09
3 90 4.6107 0.088262911 0.08
4 120 3.77685 0.072300469 0.06 Test pin
0.05 Bronze, grease
5 150 3.59537 0.068826291 0.04 12 (mineral
0.03
one)
6 180 3.77685 0.072300469 0.02
0.01
7 210 3.87495 0.074178404 0
0 100 200 300 400
8 240 3.73761 0.071549296
Time, sec
9 270 3.56103 0.068169014
10 300 3.67875 0.070422535
11 330 3.7278 0.071361502 Figure 4.13 The chart show that the mineral lubricant
test-11.
The result of the coefficient of friction (COF);

Wear (DW); DL Wear length of the pin; T=time and Fr= Friction force.
59
0.074177193
COF
DW 0.118496628gram
DL= 0.29mm
 The above result shows that the results of the lubricant test on the pin on disc testing
machine. In the case of test 11 by using produced Mineral grease.
Finally
This tribological test shows the comparative result of all the ten product produced a testing result
with the mineral grease coefficient of friction and wear.
The table 4.16 show, all the testing result including independent variable and dependent (response)
variable result with a general explanation about the result.
Table 4.15 Independent variables and dependent (responses) variable testing result of produced
bio-greases value.
Hydroxides SCW, Time Wear DOT Viscosity
O
N0. (LiOH),% % (min) COF gram C Pa.s
1 2.0 2.0 22.5 0.042418375 0.06537745 143 0.50
2 2.0 5.0 22.5 0.086901075 0.20430453 123 0.32
3 5.0 3.5 15.0 0.05582762 0.21247671 119 0.40
4 2.0 3.5 30.0 0.061192193 0.15935753 110 0.24
5 5.0 3.5 30.0 0.030723489 0.03268872 130 0.50
6 3.5 2.0 15.0 0.043556841 0.05311918 90 0.30
7 3.5 5.0 15.0 0.059858207 0.04903309 120 0.16
8 3.5 2.0 30.0 0.070707071 0.06946354 110 0.18
9 3.5 5.0 30.0 0.077321891 0.07354963 85 0.60
10 3.5 3.5 22.5 0.035433071 0.044946997 130 0.55
Table 4.15 shows that the performance of the bio-grease after examining some of the characteristics
of the final tested results of the response or dependent variables with the independent variables. .
Before the shadows indicate that the result of the independent variable of the design matrix, found
using statgraphics software to make grease. After the shadow the result of the response of dependent
variables that found after produced and tested the characteristics of the grease.
60
The mineral grease date (the data is used to comparing from the ten samples of the product bio
greases).
Greases type Wear (gram) COF viscosity(Pa.s) DPT (OC)
Mineral Grease 0.118496628 0.074177193 0.45 181
4.2 Discussion
i) Dropping point temperature
Estimated response surface for DPT
As shown on the stat graphics analysis; the result of the DPT contours estimated surface response
on Soybean oil and Sugarcane Filter Cake Oil with 50% Sugarcane Wax greases. As a result of
contours estimated surface response, DPT output is dependent on three independent variables;
those are Hydroxide, Sugarcane Filter Cake Oil with 50% Sugarcane Wax (additive), and time of
reaction. The DPT output will depend on the independent variables ratios.
When in case of hydroxide increases the DPT will increase and the reverse is true. When the
additives increase the DPT output value will increase but comparing to other dependent variables
the additive effect is slowly increasing in DPT. The time of reaction also affects the DPT value
because in case of less time of reaction the product will not be mixed appropriately and that will
decrease the DPT output result. The point shown in figure 4.14 indicates the optimum condition
of the Dropping point temperature (thickener 3.5g and additive 3.5g) at the time reaction=22.5
minute.
Figure 4.14 Contours of the estimated response surface for DPT
61
Model for Dropping point temperature (DPT)

The model which indicates about standardized Pareto chart for Dropping point temperature is
shown in figure 4.15. It shows that the highest DPT effect is caused by the time of reaction is
doubled (time of reaction squared CC) and the lowest DPT effect is caused by the normal time of
reaction (C) and the next highest effect on DPT value is the interaction between B and C.
The model A= Hydroxide AA=Squared hydroxide
B=Sugarcane filter cake oil with Sugarcane filter cake wax (SCW)
C=Time of Reaction CC= doubled/Squared time of reaction
AB= interaction of Hydroxide and SCW
BC= interaction of Hydroxide and time of reaction
Figure 4.15 Pareto diagram Standardized for Dropping point temperature (DPT).
Mean effect of dropping point temperature

Figure 4.16 chart shows that the effect of the three independent variables on dropping point
temperatures which are the tested value or the response variable.
In the case of hydroxide; at the instant the hydroxide high the dropping point temperature also
high and it's down until the critical point the DPT will be going down but after the critical point
the value of hydroxide increases the DPT also increases. The factor of hydroxide that affecting the
dropping point temperature is related. When the additive in the product increases the DPT value
gradually increases but comparing with other independent variables the effect is no much between
minimum up to maximum. With the increasing time of reaction, the dropping point temperature
62
first increases up to the maximum critical point or until the turning point, and then it decreases
when the time of reaction increases.
Figure 4.16 Graph of mean effects for dropping point temperatures.

Analysis of variance (ANOVA) for dropping point temperature
The ANOVA table partitions the Dropping point temperature variability into separate pieces for
each of the effects. Then test the statistical significance of each effect by comparing its mean
square against an estimate of the experimental error. In this case, 0 effects have a P-value less than
0.05, indicating that they are significantly different from zero with a confidence level of 95.0%
but there are with a confidence level of 90.0%.
The R-Squared statistic indicates that the model, thus adjusted, explains 95.5854% of the
variability in Dropping point temperature. The adjusted R-squared statistic, which is more suitable
for comparing models with different numbers of independent variables, is 80.1343%. The standard
error of the estimate shows that the standard deviation of the residuals is 8.00625. The mean
absolute error (MAE) of 3.2 is the mean value of the residuals. The Durbin-Watson (DW) statistic
tests the residuals to determine if there is any significant correlation based on the order in which
the data is presented in the file. Since the P-value is greater than 5.0%, there is no indication of
serial autocorrelation in the residuals at the 5.0% level of significance.
R-squared = 95.5854 percent
R-squared (adjusted for g.l.) = 80.1343percent
The standard error of the est. = 8.00625
63
Mean absolute error = 3.2

Durbin-Watson statistic = 1.50944 (P=0.1350)
Lag 1 residual autocorrelation = 0.221685
Tables 4.16 Analysis of variance (ANOVA) for dropping point temperature
Source Sum of square Gl Media square F-ratio P-value
A:Hydroxide 224.133 1 224.133 3.5 0.2024
B:SCW 6.25 1 6.25 0.1 0.7844
C:Time Reaction 0.572727 1 0.572727 0.01 0.9333
AA 490.583 1 490.583 7.65 0.1096
AB 168.75 1 168.75 2.63 0.2462
BC 756.25 1 756.25 11.8 0.0753
CC 946.4 1 946.4 14.76 0.0615
Total Error 128.2 2 64.1
Total (corr.) 2904 9
Maximize Dropping point temperature

This table shows the combination of factor levels. Which is maximizes dropping point
temperatures over the indicated region. Use the window option dialog box to indicate the region
in which the optimization will take place. You can set the value of one or more factors to constant,
by setting the high and low limits on that value.
Optimize reply
Goal: maximize Dropping point temperature
Value optimal Dropping point temperature = 161.638 oC
Table 4.17 Combination of factor levels to maximized DPT
Factor Min Max optimal
Hydroxide =% 2 5 5
Sugarcane Filter Cake Oil with wax= % 2 5 5
Time of Reaction =minute 15 30 17.8177
64
ii) Viscosity
Estimated surface response for Viscosity

The viscosity of the Soybean oil base and sugarcane filter cake oil with wax additive Biogreases
lubricant results:-
This statgraphics analysis is the estimated surface response value of the viscosity test of Soybean
oil and Sugarcane Filter Cake Oil with 50% Sugarcane Wax greases. The result shows that the
estimated surface response value of viscosity is dependent on three independent variables; those
variables are Hydroxide, Sugarcane Filter Cake Oil with 50% Sugarcane Wax (additive), and time
of reaction. The ratio of the variables is affecting on the result of viscosity, when hydroxide
increase the viscosity will increase and Sugarcane oil with Wax increase the result value of
Viscosity will increase. The time of reaction also affects the viscosity value because of less reaction
time the product will not mix appropriately so it will decrease the value of viscosity. Therefore
high hydroxide and additive the value of viscosity will be increased. Therefore, the point shown
in figure 4.17 indicates the optimum condition of the viscosity (thickener 3.5g and additive 3.5g)
at the time reaction=22.5 minute.
Figure 4.17 Contours of the estimated response surface for viscosity.
65
Model for Viscosity

The model which indicates about standardized Pareto chart for viscosity is shown in appendix 2 in
figure 1. It shows the highest Viscosity effect is caused by as the time of reaction is doubled (time
of reaction squared CC) and the lowest Viscosity effect is caused by SCW and the next highest
effect on Viscosity value is the interaction between Hydroxide (B) and SCW (C).
B=Sugarcane Filter Cake oil with Sugarcane Filter Cake Wax (SCW)
Mean effect variables on viscosity
The chart in appendix 2 figure 2 shows that the effect of the three independent variables on
viscosity which are the tested value or the response variable.
In the case of hydroxide, the hydroxide's high viscosity also high. The factor of hydroxide that
affecting the viscosity is so high. When the additive in the product increases the viscosity value
will increase but comparing to the other the effect is so much between minimum up to maximum.
With the increasing time of reaction, the viscosity first increases up to the maximum critical point
or until the turning point, and then viscosity decreases when the time of reaction increases.
Analysis of variance (ANOVA) for viscosity
The ANOVA table partitions the Viscosity variability into separate pieces for each of the effects.
Then test the statistical significance of each effect by comparing its mean square against an
estimate of the experimental error. In this case, 6 effects have a P-value less than 0.05, indicating
that they are significantly different from zero with a confidence level of 95.0%. But there are with
a confidence level of 90.0%.
variability in Viscosity. The adjusted R-squared statistic, which is more suitable for comparing
models with different numbers of independent variables, is 98.3946%. The standard error of the
estimate shows that the standard deviation of the residuals is 0.02. The mean absolute error (MAE)
of 0.008 is the mean value of the residuals. The Durbin-Watson (DW) statistic tests the residuals
to determine if there is any significant correlation based on the order in which the data is presented
66
in the file. Since the P-value is greater than 5.0%, there is no indication of serial autocorrelation in
the residuals at the 5.0% level of significance. R-squared = 99.4649 percent
R-squared (adjusted for g.l.) = 98.3946 percent
Durbin-Watson statistic = 1.5 (P=0.8355)
Lag 1 residual autocorrelation = 0.25
Maximization of Viscosity
Table 3 in the appendix shows that the combination of factor levels. Which is maximizes viscosity
over the indicated region. Use the window option dialog box to indicate the region in which the
optimization will take place. You can set the value of one or more factors to constant, by setting
the high and low limits on that value.
Optimize reply
Goal: maximized Viscosity
Value optimal Viscosity= 0.921588 Pa.s
iii) Wear
Estimated surface response for Wear
The statgraphics analysis is showing the estimated surface response of the wear dependence on the
value of three independent variables: those variables are Hydroxide, Sugarcane Filter Cake Oil
with 50% Sugarcane Wax (additive), and the time of reaction. The ratio of those materials varies
in different reaction matrices. When the value of hydroxide increases the wear value will increases
which means the surface will be damage. The value of sugarcane oil with the wax increases, the
wear of the surface will be reduced. The time of reaction increases the wear also increases, the
value of hydroxide decreases the wear also decreases, and the amount of additive decreases as the
wear increases. Therefore, the point shown in figure 4.18 indicates the optimum condition of the
wear (thickener 3.5 and additive 3.5) at the time reaction=22.5 minute.
67
Figure 4.18 Contours of the estimated response surface for wear.

Model for Wear
The model which indicates about standardized Pareto chart for Wear is shown in appendix 2 in
figure 3. It shows the highest wear effect is caused by the interaction between Hydroxide and time
of reaction (BC) and the lowest wear effect is caused by SC and the next highest effect on wear
value caused by the interaction of square time of reaction (CC).
Mean effect variables on wear
The chart in appendix 2 figure 4 shows that the mean effect of three independent variables on the
output value or the response variables of the wear. In the case of increasing hydroxide, it will be
increases the effect of wear but hydroxide decreases the wear also decrease. In the case of the
additive; at the instant the additive high the wear value is high but the additive decreases gradually
until the critical point/turn point the wear will be going to decrease and after the critical point, the
value of the additive increases the wear also increases. In the case of the reaction of time, it
gradually increases the wear until it will arrive at the critical point but After the critical point or
turning point, the wear will be decreased when the time of reaction increases.
68
Analysis of variance (ANOVA) for wear

In the appendix, in table 4, the ANOVA shows that the partitions of the Wear variability into
separate pieces for each of the effects. Then test the statistical significance of each effect by
comparing its mean square against an estimate of the experimental error. In this case, 4 effects
have a P-value less than 0.05, indicating that they are significantly different from zero with a
confidence level of 95.0%.
variability in Wear. The adjusted R-squared statistic, which is more suitable for comparing models
with different numbers of independent variables, is 99.6165%. The standard error of the estimate
shows that the standard deviation of the residuals is 0.00408609. The mean absolute error (MAE)
of 0.000817218 is the mean value of the residuals. The Durbin-Watson (DW) statistic tests the
residuals to determine if there is any significant correlation based on the order in which the data is
presented in the file.
R-Squared = 99.9574 percent
R-squared (adjusted for g.l.) = 99.6165 percent
Durbin-Watson statistic = 0.000817218
Lag 1 residual auto correlation = -0.25
Minimization of wear
Appendix 2 in table 5 shows that the combination of factor levels. Which is minimize wear over
the indicated region. Use the window option dialog box to indicate the region in which the
optimization will take place. You can set the value of one or more factors to constant, by setting
Optimize reply
Goal: minimized wear
Value optimal Wear = -0.110272gram
69
iv) Friction
Estimated surface response for the coefficient of friction
The statgraphics analysis is showing that the estimated surface response of the coefficient of
friction depends on the value of three independent variables. Those different variables are;
Hydroxide, Sugarcane Filter Cake Oil with 50% Sugarcane Wax (additive), and time of reaction.
When the value of hydroxide decreases the COF will be decrease and decreasing SCW; the value
of COF increases. the value of hydroxide increases the COF value will increase, the surface also
will be damage. The value of SCW increase and the COF of the surface will be decreased. The
time of reaction increases the COF is increasing. Therefore, the point shown in figure 4.19
indicates the optimum condition of the COF (thickener 3.5 and additive 3.5) at the time
reaction=22.5 minutes.
Figure 4.19 Contours of the estimated response surface for the coefficient of friction.
Model for Coefficient of friction
The model which indicates about standardized Pareto chart for the Coefficient of friction is shown
in appendix 2 in figure 5. It shows the highest Coefficient of friction effect is caused by as the
SCW is doubled (BB) and the lowest Coefficient of friction effect is caused by Hydroxide and the
next highest effect on Coefficient of friction value caused by the interaction of Hydroxide and
Time of Reaction.
70

Mean effect variables on the Friction coefficient
The chart in appendix 2 figure 6 shows the chart shows that the three independent variables are on
the coefficient of friction, which is affected the product value or the responds variables.
The chart shows that the mean effect of three independent variables on the output value or the
response variables of the COF. In the case of increasing gradually hydroxide, will increase the
value of COF. In the case of the additive at the instant the additive is the minimum value the
coefficient of friction value is high but the additive increase gradually until the critical point/turn
point the COF will be decreased and after the critical point, the value of additive much increase
the COF also increases. In case of the reaction of time continuously increase the COF will increase
and the time of reaction is a great effect on COF.
Analysis of variance (ANOVA) for the Friction coefficient
Appendix 2 on table 6 ANOVA shows that the partitions of the variability of the coefficient of
Friction into separate pieces for each of the effects. Then test the statistical significance of each
effect by comparing its mean square against an estimate of the experimental error. In this case, 2
effects have a P-value less than 0.05, indicating that they are significantly different from zero with
a confidence level of 95.0%.
variability in the Friction coefficient. The adjusted R-squared statistic, which is more suitable for
comparing models with different numbers of independent variables, is 98.8467%. The standard
error of the estimate shows that the standard deviation of the residuals is 0.00160761. The mean
absolute error (MAE) of 0.000371262 is the mean value of the residuals. The Durbin-Watson
(DW) statistic tests the residuals to determine if there is any significant correlation based on the
order in which the data is presented in the file.
R-squared = 96.7821percent
R-squared (adjusted for g.l.) = 90.3462percent
Durbin-Watson statistic = 1.58264
Lag 1 residual auto correlation = 0.122896
71
Minimization of the coefficient of friction

Appendix 2 table 7 shows the combination of factor levels. Which is minimizes the coefficient of
friction over the indicated region. Use the window option dialog box to indicate the region in which
the optimization will take place. You can set the value of one or more factors to constant, by setting
Optimize reply
Goal: minimize the coefficient of friction
Value optimal = -0.110272
Greases vs Responses
The table shows the response of the dependent variables found after the experiment was conducted
and tested. It shows the comparative result of Wear, COF, Dropping point temperature, and
Viscosity.
Table 4.18 The product of bio greases versus the response factorials
Wear, wear, COF Viscosity, DPT DPT x
Grease O
mm g Pa.s C 10-3
type
1 0.16 0.06537745 0.042418375 0.5 143 0.143
2 0.50 0.204304531 0.086901075 0.32 123 0.123
3 0.52 0.212476712 0.05582762 0.4 119 0.119
4 0.39 0.159357534 0.061192193 0.24 110 0.11
5 0.08 0.032688725 0.030723489 0.5 130 0.13
6 0.13 0.053119178 0.043556841 0.3 90 0.09
7 0.12 0.049033087 0.059858207 0.16 120 0.12
8 0.17 0.069463541 0.070707071 0.18 110 0.11
9 0.18 0.073549631 0.077321891 0.6 85 0.085
10 0.11 0.044946997 0.035433071 0.55 130 0.13
11 Mineral 0.29 0.118496628 0.074177193 0.45 181 0.181
72
Finally
The overall result of tribological tested value
Finally as shown in figure 4.20 that the overall results of the four dependent variables or response
factors of each experiment after testing. This chart showing that the comparative results of the ten
sample products of biogreases with the mineral grease. Experimental results show the best two
(samples 5 and 10) of the products produced to have as good results as mineral grease. They are
better at wear resistance; they have a low value of COF and also the grease characteristics for the
performance of the sample (samples 5 and 10) are high viscosity value and high dropping point
temperature.
Chart Title
0.7
0.6
0.5
wear, g
0.4
COF
0.3 Viscosityx10-1,mPa.s x10
Drpping Point x 10-3
0.2
0.1
0
1 2 3 4 5 6 7 8 9 10 11
Figure 4.20 Comparative results of the four characteristics of Biogreases response values.
73
Analysis
Figure 4.21 shows that the results of coefficient of friction vs time interval of all the ten samples
of product produced by Soybeans as a base oil and an additive (Sugarcane Filter Cake Oil with
50% Sugarcane Filter Cake Wax) of bio greases and the mineral grease test. The chart states from
the ten sample productions, sample-5 has the lowest COF and even if comparing with one of the
mineral greases.
Experiment Pin Bronze with all Grease
0.14
The pin on Disc Test pin Bronze,

grease 1
0.12
grease 2
0.1 grease 3
grease 4
0.08
grease 5
COF

grease 6
0.06 The pin on Disc Test pin Bronze,
grease 7
grease 8
0.04
grease 9
0.02 grease 10
grease 11 (mineral one)
0
0 100 200 300 400
Time, sec
74
Figure 4.21 Comparative result of the coefficient of friction with the time interval of sample
greases with mineral greases.
Summary of the overall result of tribological (Wear and COF) tested.
Finally: out of the ten product samples, the sample of the two bio-greases (Samples 5 and 10) and
the result of the mineral greases are almost the same. Therefore the results of the bio-grease exhibit
low COF and Wear and it is an advantage it could give to promote its use. The extent of similarity
among the three results shown in figure 4.22.
Experiment Pin Bronze with all Grease

0.1
0.09
0.08
0.07
0.06
The pin on Disc Test pin
Bronze, grease 5
COF
0.05
0.04 Bronze, grease 10
0.03 Bronze, grease 11 (mineral one)
0.02
0.01
0
0 100 200 300 400
Time, sec
Figure 4.22 Comparing the two best testing results of bio-grease products with mineral grease.
75
CHAPTER FIVE
5. Conclusion, Recommendation, and Future work
5.1 Conclusion
This research thesis aims to study the preparation of bio-grease lubricants using the alternative
additive of Sugarcane Filter Cake Oil with 50% Sugarcane Filter Cake Wax (SCW) and Soybeans
oil as a based oil to improve the tribological properties. To meet the objective of the research thesis
ten samples of bio-greases lubricant were produced in different ratios of thickener and additive
according to the factorial matrix. Based on the results, the following conclusions have been drawn.
a) The Comparative result of Dropping Point Temperature of the mineral greases (181 0C) greater
than all the product materials of soybeans as base oil greases but the results were between the
expecting ranges (Min (-) =800C and Max (+) = >200 0C). From the testing products; the
minimum value of PDT value is 85OC and the maximum value is 143 OC. Three of the product
(Sample 1, 5, and 10 results are 1430C, 1300C, and 130 0C; respectively) are the highest value
was as sample-9 of 850C has the lowest value.
b) Some of the Viscosity testing results of the produced samples of greases are greater than one of
the minerals (0.45 Pa.s) grease and even from similar types of product of Soybean product but
different additive. All the testing results of the ten produced samples show that between the
ranges (Min (-) =0.03 Pa.s and Max =3.00 Pa.s). From the ten samples of the product; four of
the samples are the higher viscosity values and two least viscosity values. Especially sample-9
=0.60Pa.s is the maximum viscosity and the minimum viscosity is sample 7 =0.16 Pa.s.
c) The Wear testing result shows that each of the samples is inside of range or between the
expecting values. The expecting values are between 0.10 gram and 0.50 gram. From the ten
samples tested products four of them were significantly higher testing results. Most of the
products wear testing results are very good and effective comparing from the mineral greases
and also similar types (Soybean as base oil) of product testing result of greases but used different
additive, especially sample-5 (0.032688725 gram) and samples-10 (0.044946997gram) has the
minimum value of the wear and also it wears testing value also smaller than comparing from
the mineral greases (0.118496628gram).
d) The Coefficients of Friction testing results were between the ranges (Min (-) =0.03 and Max
(+) =0.098). The testing result of sample-5 (0.030723489) has the lowest value of COF
comparing to the other ten samples of the product and also from the mineral (0.074177193)
76
grease and also from the similar product of soybean grease but different additive. The next
lower COF is sample-10 of (0.035433071) has a smaller COF from the mineral (0.074177193)
grease.
e) By using Statgraphics software analyzed the optimized value of each of the response variables;
for DPT and Viscosity to maximize the values 161.64 OC and 0.92188 Pa.s respectively but for
Wear and COF to the minimum the values-0.110272gram and. -0.110272 respectively.
5.2 Recommendation
 Such a kind of based lubricant product in our country can be a starting point to develop a new
materials lubricant, environmentally friendly (with available row materials on the country),
which are helping to be minimized the pollutants and foreigner dependence produced in
Ethiopia.
 The new alternative additive SCW investigated in this thesis demonstrated good characteristics
for the production of bio grease lubricant in addition to being renewable. But it came from the
“Las Tunas Energy Research Center” of Las Tunas University, Cuba to use in this research. It’s
recommended for the entrepreneurs to simply produced from wasted sugarcane materials that
can be produced in any sugarcane factory in Ethiopia.
5.3 Future work
 The response variables result were good but for more, they need extra performance testing in
the future because of the limitation of laboratory access, other important performance
parameters are not measured. For the future important to check; Cone penetration of the
Lubricating Grease, Corrosion resistance, Critical load (four-ball test), Oxidation stability,
Copper strip test, Water Resistance, Temperature Effect, Pumpability, Biodegradability, Shear
testing, better to test.
 By using Statgraphics software analyzed the optimized value of each of the response variables
(DPT and Viscosity) to maximize the values but not produced and tested in optimized value,
for future producing and testing this optimized value possible to found better greases
performance.
 At the instant Jatropha Curcas as base oil one of the parts of the research but cannot be produced
and test because of the time limitation and lack of Jatropha availability, for the future using this
material conducting the research thesis good because next to soybean jatropha is preferable
characteristics for effective bio-grease.
77
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80
APPENDIX /ANNEXES
Appendix 1
This table shows the first experimental design, its high amount of the percentage of hydroxide as
a thickener (5-20%) and the additive (5-10). Because of the factor of affecting the product both are
substitute into the lowest value of additive present 2%-5% and hydroxide present in 2%-5%
Table 1. Factorial experiment design or design matrix by using statgraphics the first experimental
design.
Hydroxides Friction Dropping point
N0. (LiOH) SCW Time coefficient Wear temperature Viscosity
% % Min μm oC Pa.s
1 5.0 5.0 32.5
2 5.0 10.0 32.5
3 20.0 7.5 15.0
4 5.0 7.5 50.0
5 20.0 7.5 50.0
6 12.5 5.0 15.0
7 12.5 10.0 15.0
8 12.5 5.0 50.0
9 12.5 10.0 50.0
10 12.5 7.5 32.5
81
Annexes 2
Steps of calculating the coefficient of friction
Normal force Nf =m*a…… used this formal for all tested material of coefficient of friction.
When m= mass of the load in kg
a=acceleration due to gravity
Frictional force Fr=μNf
μ = Fr/Nf……… Coefficient of friction
4.2 Discussion: - some of the discussion parts included below with some explanations
i) Viscosity
Model for Viscosity
Figure 1. Pareto diagram Standardized for viscosity.

Mean effect variables on viscosity
Figure 2. Graph of mean effects for Viscosity.
82
Analysis of variance (ANOVA) for viscosity

Table 2. Analysis of Variance (ANOVA) for Viscosity
Source Sum of squares Gl Middle Square F-ratio P-value
A:Hydroxide
0.065333 1 0.065333 163.33 0.001
B:Sugarcane Filter Cake Oil
with wax 0.0196 1 0.0196 49 0.006
C:Time Reaction 0.031784 1 0.031784 79.46 0.003
AB 0.034133 1 0.034133 85.33 0.0027
BC 0.0784 1 0.0784 196 0.0008
CC 0.083782 1 0.083782 209.45 0.0007
Error total 0.0012 3 0.0004
Total (corr.) 0.22425 9
Maximization of Viscosity
This table shows the combination of factor levels. Which is maximizes viscosity over the indicated
Table 3. Combination of factor level for viscosity
Hydroxide 2 5 5
Sugarcane Filter Cake Oil with wax 2 5 5
Time of Reaction 15 30 29.0053
ii) Wear
Model for Wear
Figure 3. Pareto diagram Standardized for wear
83
Mean effect variables on wear
Figure 4. Graph of mean effects for wear.

Analysis of variance (ANOVA) for wear
Table 4. Analyses of Variance (ANOVA) wear
Source Sum of squares Gl Middle Square F-Ratio P-value
A:Hydroxide 0.002 1 0.001803 108 0.0611
B: SCW 2.51E-19 1 2.51E-19 0 1
C:Time Reaction 4E-04 1 0.000417 25 0.1257
AA 0.004 1 0.003592 215.11 0.0433
AB 0.006 1 0.006434 385.33 0.0324
AC 0.013 1 0.013363 800.33 0.0225
BB 4E-04 1 0.000393 23.53 0.1294
CC 0.004 1 0.004023 240.94 0.041
Error total 2E-05 1 1.67E-05
Total (corr.) 0.039 9
84
Minimization of wear
Tables 5. Combination of factor levels for wear
Hydroxide 2 5 2
Sugarcane Filter Cake Oil with w 2 5 2.00274
Time of Reaction 15 30 15
iii) Coefficient of friction

Model for Coefficient of friction
Figure 5. Pareto diagram Standardized for the coefficient of friction.

Mean effect variables on the Coefficient of Friction
Figure 6. Graph of mean effects for the coefficient of friction.
85
Analysis of variance (ANOVA) for the Friction coefficient

Table 6. Analysis of Variance Friction coefficient
Source Sum of square Df mean square F-Ratio P-Value
A:Hydroxide 4.25E-05 1 4.25E-05 1.29 0.3382
B:Sugarcane Filter
Cake Oil with w 0.000131 1 0.000131 3.99 0.1397
C:Time Reaction 0.000497 1 0.000497 15.1 0.0302
AB 0.000364 1 0.000364 11.05 0.0449
AC 0.000849 1 0.000849 25.8 0.0147
BB 0.001118 1 0.001118 33.97 0.0101
Total Error 9.87E-05 3 3.29E-05
Total (corr.) 0.003067 9
Minimization of the coefficient of friction

Tables 7. Combination of factor levels
Factor Min Max Optimal
Hydroxide 2 5 2
Sugarcane Filter Cake Oil with w 2 5 2.88855
Time of Reaction 15 30 15
86
Annexes 3
Budget
The overall required budget to do this Thesis
No. Item Specification Unit Quantity Unit cost Total cost birr
1 Based oil (Soybean) Litters pack 5 96 480
2 Additive cost Kg 1 800 800
3 Cost of chemical Gram pack 500 4400 4400
thickener
4 Cost of lab-testing 6200
5 lab-testing materials 2000
cost
6 Flash 64 GB Pcs 2 650 1300
7 lamination cost 3 320 960
8 Transport cost - - - - 3000
9 Internet cost - - - 3000
10 Additional cost 3000
Total 25,140 Birr
Cost
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Federal TVET Institute

Advisor: Prof. Pedro Dionisio Remedios C. (PhD.)

December 2020 G.C

Addis Ababa, Ethiopia

Approved by Board of Examiners

Chairman, Department Graduate Committee Signature Date

________________ _______ _______

Internal Examiner Signature Date

_________________ _______ _______

External Examiner Signature Date

_______________ ________ _______

Adviser Signature Date

Name: Tsegaye Wolde

Signature: ---------------------------------- Date: -----------------------------

Advisor; Prof. Pedro Dionisio Remedios C (PhD.)

Signature: ---------------------------------- Date: -----------------------------

Date of submission: December 2020 GC

Place: Federal TVEL Institute, Ethiopia

2.10 Tribological property of grease ............................................................................................. 26

Figure 1. Pareto diagram Standardized for viscosity…………………………………………………..82

Table 4.11 the eight lubricant test….……………………….………………………………………..56

1.3 Objective of the thesis

1.6 Significance of the thesis

Figure 2.1 Lubricating grease and bio-lubricating greases (Ismail, 2014).

Vegetable Oils Naturally occurring vegetable oils Low

2.2.1.1.1 Extraction of Base oil

Where Moil =mass of oil (kg)

Table 2.3 common lubricant additives (Bahari, 2017) (Lubricants, 2016).

2.7 Characteristics of lubricating greases

Those different types of greases are:-

v. In batch process, multi-product operation can be done.

a) As Additive used in the thesis:-

Hydroxides (LiOH)=X1 Experimental Friction

Definition of variables (Independent and Dependent)

3.2.4 Factorial experimental design (2k)

Diagraph of Experimental Factorials

Figure 3.1 Flowchart of Experimental Factor

3.3.3 Method of processing and Analysis

Pin Diameter 2.00-10.0 mm 8.00mm

4.1.2 Characteristics of lubricating greases or Performance of Grease characterization

4.1.2.2 Tribological test (Wear and Frictional test)

No. T, sec Fr; N COF

No. T, sec Fr; N COF

No. T, sec Fr; N COF

The result of the coefficient of friction (COF);

Greases= Soybeans base oil

No T, sec Fr; N COF

10 300 3.1392 0.061895551

No T, sec Fr; N COF

No Time Fr; N COF

The result of the coefficient of friction

No. Time Fr; N COF

Greases= Soybeans base oil

No. Time Fr; N COF

No. Time Fr; N COF

No. Time Fr; N COF

The result of the coefficient of friction (COF);

Figure 4.14 Contours of the estimated response surface for DPT

Model for Dropping point temperature (DPT)

Mean effect of dropping point temperature

Figure 4.16 Graph of mean effects for dropping point temperatures.

Mean absolute error = 3.2

Maximize Dropping point temperature

Estimated surface response for Viscosity

____________ _ _____

_____________ _ _____

_________ _