Prahav NakhaIe

1ahmay Nalawade
Harshada Salvi
OpIimisaIion o! earing
Grease ProducIion
For AuIomobile ahd Ehgihe ApplicaIioh !rom Noh-
Edible Oilseed Karah|a
Grease is a mixIure o! a !luid lubricahI, usually peIroleum oil ahd a
Ihickeher (soap) dispersed ih Ihe oil. 1he base oil (peIroleum) cah be
chahged by usihg Ihe biodegradable oils. OIher Iheh base oil, Ihickeher
may play ah imporIahI role ih Ihe mixIure. Soap Ihickehers are !ormed by
reacIihg meIallic hydroxide, or alkali, wiIh a !aI, !aIIy acid, or esIer. Sihce
Ihe peIroleum prices will ihcrease each year, usihg hoh edible oilseed
karah|a as base oil is Ihe besI soluIioh Io produce grease ih Ihe low cosI
ahd decrease polluIioh. Ah ehvirohmehIal !riehdly biogrease has beeh
!ormulaIed usihg karah|a oil as base oil ahd liIhium 12-hydroxy-sIearaIe as
Ihickeher. LiIhium complex greases are commohly speci!ied !or use ih high-
IemperaIure applicaIiohs, such as auIomobile wheel bearihgs ahd ehgihes.
1he usual Ihickeher sysIem ih liIhium complex grease cohsisIs o! Ihe liIhium
salIs o! 12- hydroxyl sIearaIe. lh Ihis sIudy, Ihe characIerisIics o! liIhium 12-
hydroxysIearaIe grease wiIh addiIives Io cohvehIiohal liIhium complex
grease were compared. 8iogrease cah be syhIhesized via Irahs-esIeri!icaIioh
reacIiohs. 1he makihg process o! Ihe bio grease was carried ouI ih a
reacIor developed.
Pranav NakhaIe
ObIaihed 8.E. (8ioIechhology) degree alohg wiIh 1ahmay A. Nalawade,
Harshada M. Salvi !rom K.l.1.'s College o! Ehgiheerihg,Kolhapur,lhdia.
1heir area o! ihIeresI is 8io-reacIor desighihg & iIs simulaIioh, Food
Processihg & iIs applicaIioh ih ExIruded Food ProducIs , Greeh
1echhology, Rehewable Ehergy Sources & iIs sIraIegies !or
CommercializaIioh.
978-3-8465-5411-1
Pranav NakhaIe
1anmay NaIawade
Harshada 5aIvi
OpIimisaIion o! earing Grease ProducIion
Pranav NakhaIe
1anmay NaIawade
Harshada 5aIvi
OpIimisaIion o! earing Grease
ProducIion
For AuIomobiIe and Fngine AppIicaIion !rom Non-
FdibIe OiIseed Karanja
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PROJECT TITLE:
2SWLPLVDWLRQRf Bearing Grease Production for Automobile and Engine Application from
Non-EGLEOH2LOVHHG.DUDQMD
AUTHORS:
Pranav Hemant Nakhate, Tanmay Ashok Nalawade, Harshada Mohan Salvi.
DECLARATION
We hereby declare that this submission is our own work and that to the best of our
knowledge and belief. It contains no material previously published or written by another person
nor material which to a substantial extent has been accepted for the award of any other degree or
diploma of the university or other institute of higher learning, except where due
acknowledgement has been made in the text.
Mr. Nakhate Pranav Hemant
Mr. Nalawade Tanmay Ashok.
Miss. Salvi Harshada Mohan.
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ACKNOWLEDGEMENT:
This few words of gratitude in any way describe our deeply felt indebtedness to the
successful completion of our project.
We are and shall always deeply obligate the unintimidated support and the guidance of
our beloved guide Mrs. Dabeer Seema. P., whose excellence in the field of knowledge and
constant inspiration helped us a lot in the discussions, problems and their solutions,
specifications, their analysis and various other things without which we would not have reached
the shores of success.
We avail this opportunity to thank our beloved HOD, Dr. Pillai M. M. for her help in
providing all the required facilities and encouraging us throughout.
We acknowledge with sense of obligation to our principal Dr. Mujumdar M. M. for his
valuable support and help in providing all the required facilities from the college. We would like
to thanks Prof. Dr. A.N. Pathak and Prof. Dr. D.J. Bose from Amity University Rajasthan
(AUR), for their support in the publication.
We would like to thank heartily to I.B.D.C., Baramati Pune for their support and help in
whole project. Also we would like to thank Mr. Bhapkar (lecturer, department of Mechanical
Engineering, K.I.T.`s college oI eng. Kolhapur.), Dr. Anekar (H.O.D., Chemical Engineering,
TKIT Warana Nagar), Mr. Deshpande (lecturer , Chemical Engineering, TKIT Warana Nagar).
We would like to note with gratitude the guidance and cooperation of all the departmental
teaching and non-teaching staff members and library department. Without their help and
coordination it would not have been possible to complete work successfully.
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INDEX
Sr No. Title Page No.
1 Abstract 2
2 Introduction 3
3 Justification 9
4 Grease Characteristics 15
5 Components of grease 20
6 Grease Type 22
7 Material 25
8 Methodology 28
9 Result and discussion 40
10 Material Balance and Costing 58
11 Comparative study 61
12 Conclusion 63
13 Future Aspects 64
14 References and Bibliography 65
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ABSTRACT
Grease is a mixture of a fluid lubricant, usually petroleum oil and a thickener (soap)
dispersed in the oil. The base oil (petroleum) can be changed by using the biodegradable oils.
Other then base oil, thickener may play an important role in the mixture. Soap thickeners are
formed by reacting metallic hydroxide, or alkali, with a fat, fatty acid, or ester. Since the
petroleum prices will increase each year, using non edible oilseed karanja as base oil is the best
solution to produce grease in the low cost and decrease pollution.
An environmental friendly biogrease has been formulated using karanja oil as base oil
and lithium 12-hydroxy-stearate as thickener. Lithium complex greases are commonly specified
for use in high- temperature applications, such as automobile wheel bearings and engines. The
usual thickener system in lithium complex grease consists of the lithium salts of 12- hydroxyl
stearate.
In this study, the characteristics of lithium 12-hydroxystearate grease with additives to
conventional lithium complex grease were compared. Biogrease can be synthesized via trans-
esterification reactions. The making process of the bio grease was carried out in a reactor
developed. The characterization of the produced bio grease was carried out using Penetration
Test, Dropping Test. It was found that the produced lithium biogrease of NLGI No. 2 can
be prepared for automobile and engine application. The produced grease was found to be cost
effective.
Key words: Karanja, Biogrease, lithium 12-hydroxy stearate.
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CHAPTER 1
INTRODUCTION
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Increasing industrialization, growing energy demand, limited reserves of fossil fuels and
increasing environmental pollution have jointly necessitated exploring some alternative
conventional Iuels. Fossil Iuels are the largest source oI energy Ior today`s vehicles and iI
tomorrow the Iuel well`s get exhausted, the total economy oI the 'Rapid Developing World will
collapse. Thus the need for their substitution is obligatory and the best substitute for this is
BIO-DIESEL.
Biodiesel is a clean burning alternative fuel produced from domestic, renewable
resources. Biodiesel and bio-grease is simple to use biodegradable, non toxic and essentially free
of sulfur and aromatics 1 % to 2% biodiesel as a lubricity additive. Biodiesel is a more attractive
alternative fuel to diesel engines because it is a renewable and non-polluted fuel that can be
produced from renewable resources like plants. Biodiesel emits low pollutants (except NOx)
than petroleum diesel. Most of the biodiesels and bio-greases are derived from edible and non
edible oil seeds like soy bean (Glycine max), sunflower ( Helianthus annuus) , karanja
(Pongamia pinnata) , jatropha (Jatropha Curcus) etc. Biodiesel is obtained from the process
called transesterification.
Transesterification of a vegetable oil was conducted as early as 1853, by scientists
E.DuIIy and J. Patrick, many years beIore the Iirst diesel became Iunctional. RudolI diesel`s
prime model, a single 10 ft (3m) iron cylinder with a flywheel at its base , ran on its own power
for the first time in Augsburg, Germany on August 10 , 1893 using peanut oil a biofuel. In
remembrance of this event, August 10 have been declared International Biodiesel Day.
(Mathidbu, 2011).
Grease is a semi fluid to solid mixture of a fluid lubricant, a thickener, and additives.
The fluid lubricant that performs the actual lubrication can be petroleum (mineral) oil, synthetic
oil, or vegetable oil. The thickener gives grease its characteristic consistency and holds the oil in
place. Common thickeners are soaps and organic or inorganic non soap thickeners. Soaps are the
most common emulsifying agent used and the type of soap depends on the conditions in which
the grease is to be used. Different soaps provide differing levels of temperature resistance
(relating to both viscosity and volatility), water resistance, and chemical reactivity. Powdered
solids may also be used, such as clay, which was used to emulsify early greases and is still used
in some inexpensive, low performance greases.( Samman, 2007).
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The majority of greases on the market are composed of mineral oil blended with a soap
thickener. Additives enhance performance and protect the grease and lubricated surfaces. Grease
has been described as a temperature-regulated feeding device, when the lubricant film between
wearing surfaces thins, the resulting heat softens the adjacent grease, which expands and releases
oil to restore film thickness.
Semi solid lubricant or grease is widely used in many lubrication systems, because it can
provide a simple lubrication system for bearing and gear. Grease is more adhesive than liquid
lubricant so it is easier to retain in the bearing. It has lower friction coefficients, improves sealing
and provides better protection against corrosion to the surfaces. Lubricating grease is
manufactured by the dispersion of a thickening agent in a liquid lubricant and it may also contain
additives that impart special properties. Typical grease contains base oil 75%95%, thickener
5%20%, and additives 020%. The most common additives found in grease are anti-oxidants to
prolong the life of grease, anti-corrosion agents to protect metal against attack from water or
corrosive elements, anti-wear agent and extreme pressure to guard against excessive wear due to
metal to metal contact.
A fundamental difference between a grease and liquid lubricant is the presence in of the
thickening agent. The thickeners are usually metallic soaps, such as lithium, sodium and calcium
salts of long chain fatty acids. Lithium soap based lubricating greases have been numerous due to
the very good properties of these greases, i.e., a smooth appearance, and a high dropping point,
but for formulating food-grade grease, calcium soap is favorable. For more environmentally
acceptable thickener, oleo-gels that can be prepared by dispersing sorbitan mono-stearate (SMS)
in castor can be used as a substitute for the metallic soap.
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 an applied stress, the
magnitude of which will depend on the rigidity of the soap fibre network which is governed by
the forces holding the fibres together. Soap thickeners not only provide consistency to grease, but
also affect desired properties such as water and heat resistance and pump-ability. It can also
lower the coefficient of friction over that of the base oil alone.
Lithium complex grease is marketed as a superior tier of performance versus lithium
simple soap grease. This superiority is a result of increased operating temperature limits, which
can be more than 100F (56C) higher than the simple lithium soap. Lithium complex thickened
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grease has maximum temperature limits superior to that of simple lithium grease, because the
thickener offers higher thermal degradation limits. According to the NLGI Lubricating Grease
Guide, the two types of lithium grease are quite similar, except in dropping point and in the heat
resistance which this indicates. When differentiating lithium greases in the NLGI Annual
Production Survey, a dropping point of 210C (410F) or above signifies the grease production
volume is attributed to the 'complex soap category. (Nadkarni, 2008)
Simple soap greases are widely used for general purpose applications where temperatures
do not exceed 130C (266F). Simple lithium soap greases based upon 12-hydroxystearic acid
have been regarded as one of the best performing low-temperature greases, while the complex
lithium soaps have been regarded as one of the best performing high-temperature greases.
Greases that claim operating temperature ranges exceeding 130C (266F) are typically
formulated with complex soaps. In this regard, complex greases are commonly referred to as
high-temperature greases because of the increase in dropping point that comes from the two-part
thickener system. The additive modification by incorporation of a boron ester bridges the gap
between these two types of grease. The lower soap content of simple soap grease offers less
resistance to flow at low temperature combined with the heat resistance of complex grease
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1.1 Problem statement:

Grease is a mixture from a fluid lubricant (usually petroleum oil and thickener soap).
Nowadays the petroleum price were increase each year, one of the factors because the decreasing
of oil reserve and the increasing of demand. Because of the increasing of raw material price, we
need to find the solution to produce grease in the low cost. Nowadays majority of developing
countries face water pollution. The major source of water pollution is oil (petroleum and waste
lubricants). Most of factories discard their waste into the river and sea. To rectify this situation
we propose to recycle the waste to produce grease. The aim of this research is to find the solution
that can reduce the water pollution and at the same time can use the waste to produce grease.
This project will benefit not only to the environment, but also the entrepreneur and society. In
this research grease will be produce by using used lubricant oil based on suitable method. The
product will be testing their viscosity by using viscometer, to know the quality and the best
method to produce grease.
Greases are employed where heavy pressures exist, where oil drip from the bearings is
undesirable, and/or where the motions of the contacting surfaces are discontinuous so that it is
difficult to maintain a separating lubricant film in the bearing. Grease-lubricated bearings have
greater frictional characteristics at the beginning of operation. Under shear, the viscosity drops to
give the effect of an oil-lubricated bearing of approximately the same viscosity as the base oil
used in the grease. (Nadkarni, 2008)
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1.2 Approach:

The project 'Biogrease production Irom edible oil seed karanja is under collaboration
with 'Indian Biodiesel Corporation, Baramati. The Ieedstock oil was provided by them. We
proceeded with production of biogrease from non edible oilseed karanja by doing the literature
review and checking the fatty acid content of various oils and experimented it by doing
production in a small scale oI about 50 ml oil in K.I.T`s college oI engineering, Kolhapur in
biotechnology department microbiology laboratory. We were successful in production of
biogrease in small scale and thus proceeded for the production of biogrease at large scale by
scaling up. The setup required for the production of grease was designed by our self. Six
different kind of grease were produced with varying additives. The produced grease was checked
for its properties such as dropping point test, penetration number and consistency tests. The
grease was rated as per the standard norms and NLGI no was given. The remaining test has been
done in Indian biodiesel corporation, Baramati. These results were compared with the standard
grease used for automobile and engine applications and concluded.
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CHAPTER 2
JUSTIFICATION AND LIKELY BENEFITS
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'Within Next 50 Years, All the Non-Renewable Sources Will Be Exhausted and World
Will Go Toward Stone Age, Again.!
Increasing industrialization, growing energy demand, limited reserves of fossil fuels and
increasing environmental pollution have jointly necessitated exploring some alternative
conventional fuels. Fossil fuels are the largest source of energy and if tomorrow the fuel gets
exhausted, total economy oI the 'Rapid Developing World will collapse. Thus the need Ior their
substitution is obligatory and the best substitute for this is BIO-DIESEL/BIO-GREASE.
Bio-grease is simple to use, biodegradable, renewable, non toxic, essentially free of
sulphur and aromatic non-polluted fuel that can be produced from renewable resources like
plants.
Due to the concern on the availability of fossil fuel reserves, attention has been given to
bio-grease production as an alternative to petrochemicals. The recent focus is to find oil bearing
plants that produce non-edible oils as the feedstock of biodiesel for biogrease production. Many
non-edible oil-seeds are being tried for the production of the biodiesel and bio grease. Some of
them are Jatropha, Karanja, Castor, Neem, Undi, Mahua etc. (Arjun B., 2008).
Vegetable oil has been used since a long time but has some disadvantages. In their natural
form it lacks of sufficient oxidative stability for lubricant use. Thus, the oil will oxidize quickly
during use, becoming thick and polymerizing to a plastic-like consistency. Chemical
modification of vegetable oils and/or the use of antioxidants can address this problem, but
increase the cost. Chemical modification could involve partial hydrogenation of the vegetable oil
and a shifting of its fatty acids. The challenge with hydrogenation is to determine at what point
the process is to cease. Full hydrogenation of oil can lead to solid products like margarine.
Depending on the needed liquidity and pour point of the oil, optimum hydrogenation is
determined. Recent advances in biotechnology have led to the development of genetically
enhanced oilseeds that are naturally stable and do not require chemical modification and/or use
of antioxidants.
Another negative aspect of vegetable oils is their high pour point (the temperature at
which oil loses fluidity and does not flow). This problem too can be addressed by winterization,
addition of chemical additives (pour point suppressants) and/or blending with other fluids
possessing lower pour points. Various synthetic oils can be used for this purpose (Mac Vean,
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2003). If a high degree of biodegradability is required, then biodegradable synthetic esters are
added to improve cold temperature properties. Thus, the production of bio grease from non
edible seeds can be an optimised and effectiveness in its efficiency by reducing its negative
aspects can be increased.
Karanja tree is a deciduous legume that grows up to about 50 to 80 feet tall and is native
to subtropical region. It is a viable non-toxic
alternative to jatropha. Being a legume, it fixes
nitrogen into the soil. The oil is non-edible due to
bitter tasting flaveroids. The plant has
pharmaceutical uses but is not poisonous like
jatropha. It is insect resistant and is used in press
cake as both insecticide and chicken feed. The seed-
oil contain sufficient amount of non-edible oil. It
contains fatty acid like stearic acid 2.48.9%. (Dr. Kumar Patil, 2010).
Karanja has been found the most suitable tree species for the reasons summarized below
(Gubitz, 1997).
1. It is the quick growing plant even in adverse land situations degraded and barren lands
under forest and non-forest, dry and drought prone areas, marginal lands and as agro
forestry crop.
2. It can be planted on fallow lands and along IDUPHUV field boundaries.
3. It can be available during the non-rainy season, which facilitates better collection and
processing.
4. The cost of plantation is very low.
5. It has multiple uses and after the extraction of oil, the oil cake left behind is excellent
organic manure retains soil moisture and improves land capability.
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The quality oil that is used for the production of bio-grease has a direct relationship with
the trans-esterification, a basic reaction in biodiesel and bio-grease production. Trans-
esterification of a vegetable oil was conducted as early as 1853, by scientists E.Duffy and J.
Patrick, many years before the Iirst diesel became Iunctional. RudolI diesel`s prime model, a
single 10 ft (3m) iron cylinder with a flywheel at its base , ran on its own power for the first time
in Augsburg, Germany on August 10 , 1893 using peanut oil a biofuel. In remembrance of this
event, August 10 have been declared International Biodiesel Day. (Mathidbu, 2011).
Oils having high free fatty acid (FFA) need a different treatment of the oil from that of
low FFA oils. Therefore, chemical analysis of the oil, with respect to unsaponifiable matter, free
fatty acid and composition of fatty acids becomes very important. (Satish Lele, 2006).
Interesterification has been the method most commonly employed for modification of
non traditional oils and fats. Vegetable oils are modified chemically by hydrogenation or
Interesterification. During Interesterification, fatty acid (FAs) is exchanged within and among
triacylglycerols (TAGs) until a thermodynamic equilibrium is reached. Interesterification is
carried out by using lipase as a catalyst on non-traditional oils like Neem, Karanja and Rice bran
oil to produce chemicals having entirely different properties. (G. A. Usmani and H. V. Patil,
2010)
2.1 Grease Background
Grease is a semi fluid of a fluid lubricant, a thickener, and additives. The function of
grease is to remain in contact with and lubricate moving surfaces without leaking out under
gravity or centrifugal action, or be squeezed out under pressure. Its major practical requirement
is that it should retain its properties under shear at all temperatures that it is subjected to during
use. (Boehringer 1999)
The fluid lubricant that performs the actual lubrication can be petroleum (mineral) oil,
synthetic oil, or vegetable oil. The thickener gives grease its characteristic consistency and is
sometimes thought oI as a 'three-dimensional Iibrous network or 'sponge that holds the oil in
place (John A. 1981). Common thickeners are soaps and organic or inorganic non soap
thickeners. The majority of greases on the market are composed of mineral oil blended with a
soap thickener. Additives enhance performance and protect the grease and lubricated surfaces.
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Grease has been described as a temperature-regulated feeding device: when the lubricant film
between wearing surfaces thins, the resulting heat softens the adjacent grease, which expands
and releases oil to restore film thickness. (Boehringer, 1999).
2.2 Properties
Thickener gives grease its physical character, consistency, desired properties such as
water and heat resistance. Thickeners are of two type soap based and non soap based. The soap
based thickener influences how a grease will flow, change shape, and age as it is mechanically
worked and at temperature extremes. The principal ingredients in creating soap are a fatty acid
and an alkali. Soap is created when a long-carbon-chain fatty acid reacts with the metal
hydroxide. The metal is incorporated into the carbon chain and the resultant compound develops
a polarity. The polar molecules form a fibrous network that holds the oil. Thus, a gel-like
material 'grease is developed. Viscosity oI the base oil aIIects thickness as well. Since soap
qualities are also determined by the fatty acid from which the soap is prepared, not all greases
made from soaps containing the same metals are identical. The name of the soap thickener refers
to the metal (calcium, lithium, etc.) from which the soap is prepared. (Boehringer, 1999) Non-
Soap Thickeners like Clay, Polyurea, Silicones, Silica, Pigments, Carbon Black can also be used.
(Samuel Pratt, 1996). To maintain quality and stability, some additives are also added to grease
like antioxidants, antirust, corrosion, inhibitor, polymers. (Dick Meijer, 1999)
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2.3 Applications suitable for grease

Grease and oil are not the same. 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 desired lubricant characteristics. Grease is generally used
for:
1. Machinery that runs from time to time or is in storage for an extended period of time.
Because grease remains in place, a lubricating film can instantly form.
2. Machinery that is not easily reached for frequent lubrication. High-quality greases can
lubricate isolated or relatively inaccessible components for extended periods of time
without frequent replenishing.
3. Machinery operating under extreme conditions such as high temperatures and pressures,
shock loads, or slow speed under heavy load. Under this situation, grease provides thicker
film that is required to protect and sufficiently lubricate, whereas oil films can be too thin
and can break..
2.4 Functional properties of grease
1. Functions to minimize leakage and to keep out contaminants. Because of its stability,
grease acts to prevent lubricant leakage and also to prevent entrance of corrosive
contaminants and strange materials. It also acts to keep seals effective (whereas oil would
simply seep away).
2. Oil lubrication requires an expensive system of circulating equipment and complex
maintenance devices. In comparison, grease is good quality of stiffness, is easily confined
with simplified, and less costly maintenance devices.
3. Holds solid lubricants in suspension. Finely ground solid lubricants, such as molybdenum
disulfide and graphite, are mixed with grease in high temperature service (over 315 C
[599 F]) or in extreme high-pressure applications. Grease holds solids in suspension
while solids will settle out of oils.
4. Fluid level does not have to be controlled and monitored.
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CHAPTER 3
GREASE CHARACTERISTICS
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3.1. Apparent viscosity

At start-up, grease has a resistance to motion, implying a high viscosity. However, as
grease is sheared between wearing surfaces and moves faster, its resistance to flow reduces. Its
viscosity decreases as the rate of shear increases. By contrast, oil at constant temperature would
have the same viscosity at start-up as it has when it is moving. (Boehringer 1992) To
differentiate between the viscosity of oil and grease, the viscosity of grease is referred to as
'apparent viscosity. Apparent viscosity is the viscosity oI a grease that holds only Ior the shear
rate and temperature at which the viscosity is determined.
3.2. Bleeding, migration
Bleeding is a condition when the liquid lubricant separates from the thickener. It is
induced by high temperatures and also occurs during long storage periods. Migration is a form of
bleeding that occurs when oil in grease migrates out of the thickener network under certain
conditions. For example, when grease is pumped though a pipe in a centralized lubrication
system, it may encounter a resistance to the flow and form a plug. The oil continues to flow,
migrating out of the thickener network. As the oil separates from the grease, thickener
concentration increases, and plugging gets worse. If two different greases are in contact, the oils
may migrate from one grease to the other and change the structure of the grease. From
(Boehringer 1992)
3.3. Corrosion and rust resistance.
This is the ability of grease to protect metal parts from chemical attack. The Natural resistance of
grease depends upon the thickener type. Corrosion resistance can be enhanced by corrosion and
rust inhibitors. (Nabil Fikri, 2008)
3.4. Consistency, penetration, and National Lubricating Grease Institute (NLGI)
numbers.
The most important feature of grease is its stiffness or consistency. Grease that is too stiff may
not feed into areas requiring lubrication, while grease that is too fluid may leak out. Grease
consistency depends on the type and amount of thickener used and the viscosity of its base oil.
Grease`s consistency is its resistance to deIormation by an applied Iorce. The measure oI
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consistency is called penetration. Penetration depends on whether the consistency has been
changed by handling or working. ASTM D 217 and D 1403 methods measure penetration of
worked and worked greases. To measure penetration, a cone of given weight is allowed to sink
into a grease for 5 seconds at a standard temperature of 25 C (77 F). The depth, in tenths of a
millimeter, to which the cone sinks into the grease, is the penetration. A penetration of 100
would represent solid grease while one of 450 would be semi fluid. The NLGI has established
consistency numbers or grade numbers, ranging from 000 to 6, corresponding to specified ranges
of penetration numbers. Table1 lists the NLGI grease classifications along with a description of
the consistency of each classification. (Nadkarni, 2008)
NLGI NO.
ASTM WORKED PENETRATION
0.1 MM (3.28 10 FT) AT 25 C (77
F) CONSISTENCY
000
446-475 Semi fluid
00
400-430 Semi fluid
0
255-385 Very soft
1
310-340 Soft
2
265-285 Common grease
3
220-250 Semi hard
4
175-205 Hard
5
130-160 Very Hard
6
85-115 Solid
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3.5. Dropping point.

Dropping point is an indicator of the heat resistance of grease. As grease temperature
rises, penetration increases until the grease liquefies and the desired consistency is lost. Dropping
point is the temperature at which grease becomes fluid enough to drip. The dropping point
indicates the upper temperature limit at which grease retains its structure, not the maximum
temperature at which grease may be used. A few greases have the ability to regain their original
structure after cooling down from the dropping point. (Nadkarni, 2008)
3.6. Evaporation.
The mineral oil in grease evaporates at temperatures above 177 C (350 F). Excessive oil
evaporation causes grease to freeze due to increased thickener concentration. Therefore, higher
evaporation rates require more frequent regarding lubrication. (Nabil Fikri, 2008)
3.7. Oxidation stability.
This is the ability of 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
operation, increased wear, and reduction of clearances. Extended hightemperature exposure
accelerates oxidation in greases. (Nabil Fikri, 2008)
3.8. High-temperature effects.
High temperatures damage greases more than they damage oils. Grease, by its nature,
cannot disperse heat by convection like circulating oil. Therefore, without the ability to transfer
away heat, extreme temperatures result in accelerates oxidation or even carbonization where
grease hardens or forms a shell. Effective grease lubrication depends on the grease's consistency.
High temperatures bring softening and bleeding, causing grease to flow away from needed areas.
The mineral oil in grease can flash, burn, or evaporate at temperatures above 177 C (350 F).
High temperatures, above 73-79 C (165-175 F), can dehydrate certain greases such as calcium
soap grease and cause structural breakdown. The higher evaporation and dehydration rates at
high temperatures require more frequent grease replacement. (Nabil Fikri, 2008)
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3.9. Low-temperature effects.

If the temperature of grease is lower enough, it will become so viscous that it can be
classified as hard grease. Pump ability and machinery operation may become impossible due to
torque limitations and power requirements. The temperature at which this occurs depends on the
shape oI the lubricated part and the power being supplied to it. As a guideline, the base oil`s Ilow
point is considered the low temperature limit of grease. (Nabil Fikri, 2008)
3.10. Texture. (Nabil Fikri, 2008)
Texture is observed when a small sample of grease is pressed between thumb and index
finger and slowly drawn apart. Texture can be described as:
1. Brittle: the grease ruptures or crumbles when compressed.
2. Buttery: the grease separates in short peaks with no visible fibers.
3. Long fiber: the grease stretches or strings out into a single bundle of fibers.
4. Resilient: the grease can withstand moderate compression without permanent
deformation or rupture.
5. Short fiber: the grease shows short break off with evidence of fibers.
6. Stringy: the grease stretches or strings out into long, fine threads, but with no visible
evidence of fiber structure.
3.11. Water resistance.
This is the ability of grease to hold up the effects of water with no change in its ability to
lubricate. Soap or water may suspend the oil in the grease, forming a mixture that can wash away
or, to a lesser extent, reduce lubricity by diluting and changing grease consistency and texture.
Rusting becomes a concern if water is allowed to contact iron or steel components.(Nabil Fikri,
2008)
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CHAPTER 4
COMPONENTS OF GREASE
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4.1. Soap Thickeners (Satish Lele, 2006)

Dispersed in its base fluid, a soap thickener gives grease its physical character. Soap
thickeners not only provide consistency to grease, they affect desired properties such as water
and heat resistance and pump ability. They can affect the amount of an additive, such as a rust
inhibitor, required to obtain a desired quality. The soap influences how a grease will flow,
change shape, and age as it is mechanically worked and at temperature extremes. Each soap type
brings its own characteristic properties to grease.
The principal ingredients in creating soap are a fatty acid and an alkali. Fatty acids can be
derived from animal fat such as beef tallow, lard, butter, fish oil, or from vegetable fat such as
olive, castor, soybean, or peanut oils. The most common alkalis used are the hydroxides from
earth metals such as aluminum, calcium, lithium, and sodium. Soap is created when a long-
carbon-chain fatty acid reacts with the metal hydroxide.
The metal is included into the carbon chain and the resultant compound develops a
polarity. The polar molecules form a fibrous network that holds the oil. Thus, a somewhat rigid
gel-like material 'grease is developed. Soap concentration can be varied to obtain different
grease thicknesses. Furthermore, viscosity of the base oil affects thickness as well. Since soap
qualities are also determined by the fatty acid from which the soap is prepared, not all greases
made from soaps containing the same metals are identical. The name of the soap thickener refers
to the metal (calcium, lithium, etc.) from which the soap is prepared From (Weiheim Wikey
VCH, 2001)
4.2. Additives (Satish Lele, 2006)
An additive that mix together to form grease is as surface protecting and effectively
improves the overall performance of grease. Additives such as Calcium carbonate, Detergents as
a surfactant, Acryl amide, Citrate and Zinc Borate are added to grease for high temperatures
(above 315 C or 599 F), extreme high pressure applications, and also to improve properties like
anti-oxidation, surface tension, avoid resistance. Incorporating solid additives requires frequent
grease changes to prevent accumulation of solids in components.
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CHAPTER 5
GREASE TYPE
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5.1. Calcium grease (Satish Lele, 2006)

Calcium or lime grease, the first of the modern production greases, is prepared by
reacting mineral oil with fats, fatty acids, a small amount of water, and calcium hydroxide. The
water modifies the soap structure to absorb mineral oil. Because of water evaporation, calcium
grease is sensitive to elevated temperatures. It dehydrates at temperatures around 79 C (175 F)
at which its structure collapses, resulting in softening and, eventually, phase separation.
Greases with soft consistencies can Greases with soft consistencies can dehydrate at
lower temperatures while greases with firm consistencies can lubricate satisfactorily to
temperatures around 93 C (200 F). In spite of the temperature limitations, lime grease does not
emulsiIy in water and is excellent at resisting 'wash out. Also, its manuIacturing cost is
relatively low. If calcium grease is prepared from 12-hydroxystearic acid, the result is hydrous
(waterless) grease. Since dehydration is not a concern, anhydrous calcium grease can be used
continuously to a maximum temperature of around 110 C (230 F).
Calcium complex grease is prepared by adding the salt calcium acetate. The salt provides
the grease with extreme pressure characteristics without using an additive. Dropping points
greater than 260 C (500 F) can be obtained and the maximum usable temperature increases to
approximately 177 C (350 F). With the exception of poor pump ability in high-pressure
centralized systems, where caking and hardening sometimes occur calcium complex greases
have good all-around characteristics that make them desirable multipurpose greases.
5.2. Sodium grease (Satish Lele, 2006)
Sodium grease was developed for use at higher operating temperatures than the early
hydrated calcium greases. Sodium grease can be used at temperatures up to 121 C (250 F), but
it is soluble in water and readily washes out. Sodium is sometimes mixed with other metal soaps,
especially calcium, to improve water resistance. Although it has better adhesive properties than
calcium grease, the use of sodium grease is declining due to its lack of flexibility. It cannot
compete with water resistant, more heat resistant multipurpose greases. However, it still
recommended for certain heavy duty applications and well sealed electric motors.
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5.3. Aluminum grease (Satish Lele, 2006)

Aluminum grease is normally clear and has a somewhat stringy texture, more so when
produced from high viscosity oils. When heated above 79 C (175 F), this stringiness increases
and produces a rubberlike substance that pulls away from metal surfaces, reducing lubrication
and increasing power consumption. Aluminum grease has good water resistance, good adhesive
properties, and inhibits rust without additives, but it tends to be short-lived. It has excellent
inherent oxidation stability but relatively poor shear stability and pumpability.
Aluminum complex grease has a maximum usable temperature of almost 100 C (212 F)
higher than aluminum soap greases. It has good water and chemical resistance but tends to have
shorter life in high temperature, high speed applications.
Greases are considered incompatible when the physical or performance characteristics of
the mixed grease fall below original specifications. In general, greases with different chemical
compositions should not be mixed. Mixing greases of
different thickeners can form a mix that is too firm to
provide sufficient lubrication or more commonly, a mix
that is too soft to stay in place.
Combining greases of different base oils can
produce a fluid component that will not provide a
continuous lubrication film. Additives can be diluted when greases with different additives are
mixed. Mixed greases may become less resistant to heat or have lower shear stability. If a new
brand of grease must be introduced, the component part should be disassembled and thoroughly
cleaned to remove all of the old grease. If this is not practical, the new grease should be injected
until all traces of the prior product are flushed out. Also, the first grease changes should be more
frequent than normally scheduled.
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CHAPTER 6
MATERIALS
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6.1. Base oil:

Crude oil oI Karanja seeds was supplied by Indian Bio-Diesel Corporation (IBDC),
Baramati, pune`. We used this Karanja oil as a base oil for the preparation of the Bio-
lubricant i.e. - Bio-grease.
Other crude oils like Palm oil, Castor oil, Neem oil, Cotton seed oil, were obtained from
BAWADEKAR ayurvedic material shop, Kolhapur`.
6.2. Chemicals and reagents*:
x Lipase from Porcine pancreas type II (Sigma)
x NaOH (0.1 N)
x Standard 1 N HCl
x Ethyl alcohol (95%)
x Phenolphthalein Indicator
x Lithium Hydroxide
x Citric acid
x Calcium carbonate
x Surfactant (Detergent)
x Polyacrylamide
x Buffer pH 6.7 (Phosphate buffer)
*Salts used are of brand HIMEDIA.
6.3. Instruments:
x ACCULAB Weight Balance
x ELICO LI 127 pH meter
x ELTEK Electric stirrer (230 V AC)
x Dropping point equipment
x Penetrometer
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6.4. Glasswares:
x Erlenmeyer flask (250ml and 500ml)
x Beakers (10ml, 50 ml, 100ml)
6.5. Other acsesories:
x Gas cylinder
x Stove
x 5 liter steel vessel
x 1 liter steel vessel
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CHAPTER 7
METHODOLOGY
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7.1. Reagent preparation:

A) 0.1 N NaOH:
For NaOH normality = molarity; hence for 1M (1N) solution we had to dissolve 40 g
NaOH in 1L water. Therefore for 0.1 N solution we dissolved 4 g in 1 L water. Then it was
standardized by titrating it with standard 1 N HCl solution with addition of phenolphthalein
indicator.
B) Phenolphthalein indicator:
0.5 gm of phenolphthalein was weighed and dissolved in 50% ethanol (ethyl alcohol)
solution consisting of 50ml ethanol and 50 ml water. We standardized it with addition of 0.1 N
NaOH drop wise until slight pink color appears. Then 1 N HCl was added drop wise to neutralize
the solution until pink color vanishes.
C) Phosphate buffer pH 6.7:
0.1 M potassium dihydrogen phosphate (KH
2
PO
4
) (Molecular weight 136.08) 6.9 gm/50
ml deionized water was added to 0.1 M Dipotassium phosphate/phosphoric acid (K
2
HPO
4
)
(Molecular weight 174.18) 13.4 gm/50 ml deionized water. Both solutions are mixed in
proportion to make pH 6.4 and final volume was adjusted to 100 ml with deionized water.
7.2. Extraction of pure base oil / lube oil from crude oil obtained fromkaranja:
Initially the oil was warmed gently on burner to lower the viscosity of the oil.
Immediately the oil, then, was filtered to remove the solid particles and organic material by using
double layered cheesecloth in a funnel. The organic and inorganic debris was removed. Then oil
was heated in a distillation flask to remove the water content of the oil. The heat applied for this
process was 130
0
C.
The same procedure was done with each base oils- Palm oil, Karanja oil, Cotton seed oil,
Castor oil, Neem oil.
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7.3. Estimation of properties of the base oil:

7.3.1. Total Free Fatty Acid Content:
Total free fatty acid content was fount out by titrametric method. A clean dry burette was
filled with 0.1 N standardized NaOH. 1 ml of oil was taken in the clean dry 50 ml flask. 5ml
95% ethanol was added to the flask. The mixture in the flask was heated on the burner to
dissolve the oil into ethanol. Immediately 2-3 drops of phenolphthalein indicator was added to
the flask and hot mixture was titrated against the 0.1 N NaOH in the burette. The end point
colorless to pink was observed. And reading on burette was noted dawn. The free fatty acid
content was obtained by formula (Satish Lele, 2006)-

We determined amount of total free fatty acid content of all base oils.
7.3.2. Other properties of oil:
Other properties of karanja oil like Viscosity of oil at 40
0
C, Viscosity of oil at 100
0
C,
Viscosity index and Pour point were analyzed by Nikhil analytical laboratory, Sangali`
7.4. Determination of activity of the lipase (Reginald, 1996):
x Theory-
Lipase activity was determined on emulsifier free system using Karanja oil as substrate.
The reaction was carried out in 10 ml conical Stoppard flask at 40
0
C by immersion in the water
bath with continuous shaking at 120 rpm.
One unit of lipase activity is defined as the amount which liberates 1 micromole (m) of
fatty acid per minute at 40
0
C.
Burette reading Normality of NaOH 56.1
Total free fatty acid content (%) =
Amount of oil sample taken 2
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7.6. Production of grease produced by soap based method (John J. Lorimor, 2009):
7.6.1. Trial for grease production:
A) Setup of grease producing assembly:
For trial experiment we developed a trial
setup for grease production. We fixed a 500 ml
beaker containing Castor oil on tripod stand for
developing oil bath. Castor oil was selected as oil of
oil bath because it has boiling point (313
0
C) greater
then that of the Karanja oil (150
0
C). We inserted 100
ml beaker into the 500 ml beaker. Few glass beads
were dropped into the 500 ml beaker to avoid air
pockets and bursting of the beaker. The oil quantity
in the 500 ml beaker for the oil bath was taken such
that it won`t spill out aIter inserting the 100 ml
beaker into it. We fixed the 100 ml beaker to the
burette stand with help of clips. We used burner for
heat source below the tripod stand. We used glass rod for stirring purpose. The following picture
shows the setup of the trial grease producing assembly
B) Production of grease in trial setup:
We took total 50 ml of karanja oil, from which we added
10 ml oil in the 100 ml beaker in the above mentioned assembly.
We prepared 12-Hydroxy stearate from 10 ml oil of the total 50
ml oil. We added that 12-Hydroxy stearate to 10 ml oil in the 100
ml beaker and allowed it to boil by giving heat through burner. Heat was applied to reach 80C
to melt the acid. The temperature was measured with the help of thermometer.
Trial production of grease
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Meanwhile we prepared anhydrous lithium hydroxide

(LiOH) dispersion of 10 ml oil of total 50 ml oil. At 90C, the
anhydrous lithium hydroxide dispersion was added slowly to
the kettle over 20 minutes. After all the lithium hydroxide
dispersion was added, 15 minutes further mix time was
completed at a higher mixing speed. Following the 15 minutes
mixing time, the mixing speed was reduced and full heat was
then applied to initiate the temperature ramp to the 150-195C
process maximum. Once the 150-195C temperature stage was
reached, heat was shut off and 15 minutes max additional mix
time was allowed before cooling oil at a slow rate. The batch
was cooled to below 150C then remaining 20 ml oil was added slowly with rigorous mixing to
achieve proper consistency of the grease.
By similar method we tried to produce grease with NaOH as a thickener. Only difference
was that, we did not produce dispersion of the NaOH, instead we added NaOH directly.
C) Preparation of 12-Hydroxy stearate:
12-Hydroxy stearate is soap. To produce this we combined 1gm LiOH and 10 ml oil in an
aqueous medium (5 ml water). With the vigorous stirring, we added dilute monohydrate LiOH
gradually to the dispersion of the oil in water heated to slightly below the boiling point.
D) Preparation of anhydrous lithium hydroxide (LiOH) dispersion:
The dispersion of LiOH was done to avoid reaction of the LiOH with water in the air.
LiOH when come in contact with air, it might cause harmful effect to the respiratory system of
the human being. The dispersion of LiOH in oil reduces the toxicity of the LiOH. 10 ml oil was
taken into the mortar. 1 gm of LiOH was added to it and grinded in oil vigorously with the help
of pestle.
Grease produced
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7.6.2. Scale up of grease production:

A) Setup of final grease producing assembly:
For large scale production of grease we
scaled up the above methodology. We used 5 liter
steel vessel instead of 500 ml glass beaker. We
replaced 50 ml glass beaker with 1 liter steel vessel.
We wanted to produce approximately grease of 500
ml oil of different types. For that we used I liter
steel vessel so that head space was 500 ml volume.
We used electric stirrer instead of glass rod for
proper stirring of the mixture. The stirrer was
equipped with speed controller so that we adjusted
the speed of stirrer approximately to 500-700 rpm.
The temperature was measured with the help of
thermometer.
B) Final Grease production:
Final large scale grease was produced by similar way
as explained above. Only difference was that the proportion of
oil, LiOH added. We produced main control grease which was
additive less. We also produced other four types of greases
containing four different additives for different purposes. The
purpose of producing such different grease with different
additives was to assess the effect of each individual additive in the grease. Finally we produced
the compete grease which have all the additives. This was produced purposefully to check the
combined effect of all the additives. The different proportions of additions of oil, LiOH and
additives are described in the table below.
Large scale Grease production assembly
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Sr.
No.
Grease
sample
Oil in
Soap
form
(ml)
Oil in
Dispers-
ion
form
(ml)
Total
amoun
t of
oil
used
(ml)
Additive/ s
Amount
of
additive/s
(gm)
1 Control grease 60 60 300 -- --
2 Sample 1 60 60 300 Acrylamide 1.5
3 Sample 1 60 60 300 Citrate 1.5
4 Sample 1 60 60 300 Calcium carbonate (CaCO
3
) 1.5
5 Sample 1 60 60 300 Surfactant 1.5
6 Final grease 100 100 500
Acrylamide, Citrate, CaCO
3
,
Surfactant
2.5 (Each)
7.7. PRODUCTION OF GREASE PRODUCED BY NON-SOAP BASED METHOD:
7.7.1. Use of Polysaccharide Gum acacia as a non soap
based thickener:
We tried to produce the grease from Karanja oil by
using gum acacia as a thickener. For that we added 4 am of gum
to the 100 ml of Karanja oil. We gave heat to this mixture. At
about 150
0
C temperature the oil start to boil and gum get
completely dissolved into the oil. We stopped the heating of mixture and allowed it to cool. The
mixture get semi solidified at temperature below to the temperature 90
0
C.
Gumacacia
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7.8. Characterisation of grease (Boehringer, 1999):

Part oI grease characterization was done by us at K.I.T.`s college oI engineering,
Kolhapur. Remaining part of grease characterization was done by Indian Biodiesel Corporation,
Baramati, Pune.
Grease characterization mainly include following tests-
x Dropping point
x Penetration number and consistency
x Apparent viscosity/ pump ability
x Corrosion
x Rust resistance
x Evaporation
x Heat resistance
x Oxidation resistance
x Leakage
x Water resistance
x Wear resistance
We perIormed two oI them in our college K.I.T.`s college oI engineering, Kolhapur,
which were Dropping point and penetration number.
A) Dropping point:
Grease was placed in a small cup of the dropping point
analyzing equipment. The cup was placed into the dropping point test-
tube and thermometer was adjusted in the test tube such a way that the
bulb of thermometer gets immersed into the grease. The tube was
hanged into the beaker containing oil stirred by electric stirrer. Whole
assembly was put on the electric heater. Heat was supplied. When a
drop of oil falls from the lower opening of the cup, the dropping point
of the grease was calculated using thermometer.
Dropping point analyzer
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B) Penetration number and consistency:

This test can be used to determine the mechanical stability of grease through prolonged
working. The test was carried out with the help of Penetrometer. The cup of Penetrometer was
filled with approximately 300 gm of grease such a way that there was no any single bubble in the
cup. With the help of Penetrometer stoke was give for 60 seconds. The readings on the scale of
Penetrometer were noted down.
The consistency was determined from standard National Lubricating Grease Institute
(NLGI) table for NLGI number.
=(Sukirno, 2007)
Standard NLGI table for NLGI number
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CHAPTER 8
RESULTS AND DISCUSION
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8.1. Estimation of properties of base oil karanja:

8.1.1. Total free fatty acid content of Karanja oil:
After titration we got the burette readings i.e. amount of NaOH required to neutralize the
acidity of the mixture in the flask due to free fatty acid content.
x Solution in Burette- 0.1 N NaOH
x Mixture in flask- 1 ml karanja oil + 5 ml ethanol + phenolphthalein indicator
x The end point was colorless to pink.
Sr.
No.
Burette reading
1 (ml)
Burette reading
2 (ml)
Burette reading
3 (ml)
Mean Burette reading
(MBR) (ml)
1 4.9 4.3 4.6 4.616
x Formula:
x Calculations:
Total free fatty acid content of the Karanja oil = 4.6160.156.1
12
= 12.62%
Burette reading Normality of NaOH 56.1
Total free fatty acid content (%) =
Amount of oil sample taken 2
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8.1.2. Other Properties of the Karanja oil:

The result was obtained from Nikhil Analytical Lab, Sangali. The following results
are according to the data given by Nikhil Analytical Lab.
Sr.no Parameters value
1 Appearance Brownish thick
2 Specific gravity 0.9369
3 Viscosity (40
0
C) 440.7 cP
4 Viscosity (100
0
C) 417 cP
5 Viscosity index 17
6 Free fatty acid 12.62%
7 Pour point 6.0
0
C
8 Texture Creamy
8.1.2. Discussion:
The major characteristics of Karanja oil considered in the process of grease production,
were free fatty acid content and viscosity. Both the properties were tried to increase during
grease production process.
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8.2. Selection of blending oil to increase the free fatty acid content:
8.2.1. Total free fatty acid content of Neem oil:
After titration we got the burette readings i.e. amount of NaOH required to neutralize the
acidity of the mixture in the flask due to free fatty acid content.
x Solution in Burette- 0.1 N NaOH
x Mixture in flask- 1 ml Neem oil + 5 ml ethanol + phenolphthalein indicator
x The end point was colorless to pink.
Sr.
No.
Burette reading
1 (ml)
Burette reading
2 (ml)
Burette reading
3 (ml)
Mean Burette reading
(MBR) (ml)
1 4.9 4.7 5.0 4.866
x Formula:
x Calculations:
Total free fatty acid content of the Neem oil = 4.8660.156.1
12
= 13.64 %
Burette reading Normality of NaOH 56.1
Total free fatty acid content (%) =
Amount of oil sample taken 2
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8.2.2. Total free fatty acid content of Castor oil:

After titration we got the burette readings i.e. amount of NaOH required to neutralize the
acidity of the mixture in the flask due to free fatty acid content.
x Solution in Burette- 0.1 N NaOH
x Mixture in flask- 1 ml Castor oil + 5 ml ethanol + phenolphthalein indicator
x The end point was colorless to pink.
Sr.
No.
Burette reading
1 (ml)
Burette reading
2 (ml)
Burette reading
3 (ml)
Mean Burette reading
(MBR) (ml)
1 1.0 1.1 1.0 1.0
x Formula:
x Calculations:
Total free fatty acid content of the Castor oil = 1.00.156.1
12
= 2.805 %
Burette reading Normality of NaOH 56.1
Total free fatty acid content (%) =
Amount of oil sample taken 2
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8.2.3. Total free fatty acid content of Cotton seed oil:

After titration we got the burette readings i.e. amount of NaOH required to neutralize the
acidity of the mixture in the flask due to free fatty acid content.
x Solution in Burette- 0.1 N NaOH
x Mixture in flask- 1 ml Cotton seed oil + 5 ml ethanol + phenolphthalein indicator
x The end point was colourless to pink.
Sr.
No.
Burette reading
1 (ml)
Burette reading
2 (ml)
Burette reading
3 (ml)
Mean Burette reading
(MBR) (ml)
1 1.5 1.2 1.0 1.233
x Formula:

x Calculations:
Total free fatty acid content of the cotton seed oil = 1.2330.156.1
12
= 3.459 %
Burette reading Normality of NaOH 56.1
Total free fatty acid content (%) =
Amount of oil sample taken 2
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x Calculations:
Time (hr.) 0 24 48 72 96
Amount of fatty acid liberated
10
-3
(mol/ml)
3.3 7.8 1.2 1.68 2.13
x Discussion:
The activity of lipase at the end of 96 hours is 2.13 mol/ml.
8.3.2. Effect of blending Neem oil with Karanja oil to improve properties of base oil
Karanja:
Due to blending and inter-esterification process the properties of the oil get increased.
Free fatty acid content, boiling point are some of them. The increased free fatty acid content was
determined by titrametric method. The blend after incubation period of 2 hr was titrated against
0.1 N NaOH.
A) Effect of variable proportion of the Karanja and Neem oil:
After titration we got the burette readings i.e. amount of NaOH required to neutralize the acidity
of the mixture in the flask due to free fatty acid content.
x Solution in Burette- 0.1 N NaOH
x Mixture in flask- 1 ml Blend (Karanja + Neem) of different proportion + 5 ml ethanol +
phenolphthalein indicator
x The end point was colourless to pink.
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Blend
(Karanja
+ Neem)
Burette reading
1 (ml)
Burette reading
2 (ml)
Burette reading
3 (ml)
Mean Burette reading
(MBR) (ml)
1+9 3.2 4.3 4.8 4.11
2+8 4.6 4.8 4.7 4.21
3+7 5.1 4.2 4.5 4.62
4+6 4.8 4.9 4.6 4.77
5+5 4.3 5.6 5.8 5.22
x Formula:

x Calculations:
Blend (Karanja
+ Neem)
1+9 2+8 3+7 4+6 5+5
Total free fatty
acid content
11.54 13.22 12.96 13.38 14.65
Burette reading Normality of NaOH 56.1
Total free fatty acid content (%) =
Amount of oil sample taken 2
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B) Effect of variable proportion of the lipase:

After titration we got the burette readings i.e. amount of NaOH required to neutralize the acidity
of the mixture in the flask due to free fatty acid content.
x Solution in Burette- 0.1 N NaOH
x Mixture in flask- 1 ml Blend (Karanja + Neem) of same proportion (1:1) + 5 ml ethanol +
phenolphthalein indicator
x The end point was colorless to pink.
Lipase
quantity
(ml)
Burette reading
1 (ml)
Burette reading
2 (ml)
Burette reading
3 (ml)
Mean Burette reading
(MBR) (ml)
0.25 4.3 4.8 4.7 4.5
0.5 4.5 4.2 4.3 4.33
1.0 4.5 4.3 4.5 4.43
1.5 5.8 4.9 4.9 5.22
2.0 4.5 4.3 5.5 4.77
x Formula:

Burette reading Normality of NaOH 56.1
Total free fatty acid content (%) =
Amount of oil sample taken 2
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Overall discussion of Inter-esterification process for increasing properties of base oil

Karanja:
The inter-esterification process was useful to increase the properties like free fatty acid
content of the base oil karanja. But the percentage of increase in the total free fatty acid content
was not sufficient. Considering increase in the cost of the grease due to inter-esterification
process, the output result was not effective. Thus, the inter-esterification process was not used in
the further process of our project. More research work should be done for the increase in the fatty
acid content of the oil for grease making process.
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8.4. Characterisation of grease produced:

8.4.1. General properties of the grease:
Sr. No. Type of grease Color Texture Fineness
1
Grease without additives
(Control)
Dark yellow Buttery Smooth
2 Grease with Acrylamide Brownish Buttery
Slight
rough
3 Grease with citrate Yellow brownish Buttery
Slight
rough
4 Grease with CaCO3 Brownish Buttery
Slight
rough
5 Grease with Surfactant Yellowish Buttery Smooth
6
Grease with all additives
(Final grease)
Yellow Buttery Smooth
8.4.1.2. Discussion:
The grease produced from Karanja oil has general properties which were very similar to
the market petroleum grease (Veedol AP3). Overall texture of the grease was smooth and buttery.
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8.4.2. Dropping point of the grease:

Sr. No. Type of grease D.P. (
0
C)
1 Grease without additives
(Control)
136
2 Grease with Acrylamide 128
3 Grease with Citrate 138
4 Grease with CaCO3 142
5 Grease with Surfactant 132
6 Grease with all additives
(Final grease)
130
Graphical representation of dropping point:

K
^
&

8.4.2.1. Discussion:
The dropping point of the grease was sufficiently increased due to addition of CaCO
3
.
The dropping point of the grease with only CaCO
3
was 142 which is almost equal to the market
petroleum grease (Veedol AP3).
8.4.3. Penetration number and consistency:
Sr. No. Type of grease Penetration no. NLGI no. Consistency
1 Control 232 3 Semi hard
2 Grease with Acrylamide 215 3 Semi hard
3 Grease with Citrate 225 3 Semi hard
4 Grease with CaCO3 137 5 Very hard
5 Grease with Surfactant 210 3 Semi hard
6 Final grease 269 2 Common grease
Graphical representation of penetration no.:

K

^
&

WE
^
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CHAPTER 9
MATERIAL BALANCE AND COSTING
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9.1. Material Balance:-

Material Balance is very important and integrated terminology in the process of
optimisation.
Whenever we go for the optimisation in laboratory scale or industrial scale, material
balances for the components used and product formed is important factor as it yields the product
formation ratio.
General Material Balance can be given as:-
In the case of grease production from non edible seed Karanja, there is no any mass out,
as well as any consumption of substrate for by-product formation.
Hence material balance for the grease production can be given as,
.
This is represented diagrammatically as
Discussion
The grease that we have produced from non edible oil seed Karanja does not contain any
contaminants or any wastage. Hence, we have obtained almost 100 % product yield from the
substrates i.e. components.
Base Oil Karanja = 500 ml
LiOH = 20 gm
CaCO3 = 2.5 gm
Acrylamide = 2.5 gm
Citrate 2.5 gm
Surfactant = 2.5 gm
Production of
almost 530 gm
of Grease
MASS OF SUBSTRATE IN = MASS OF TOTAL PRODUCT FORMED
Mass accumulation = mass in mass out + mass generation mass consumption
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9.2 Costing Of The Grease:-

The economy of any product produced is very important aspect in market point of view.
Hence costing of each and every component used must be considered and must be optimised in
order to reduce overall costing of product produced.
A) All Purpose PetroleumGrease. B) All Purpose Karanja Grease.
Base oil-
Karanja Oil 50 Rs/500 ml
Thickener-
Lithium Hydroxide 36 Rs/ 20 gm.
Others-
1) Surfactant 0.5 Rs / 2.5 gm
2) Acryl amide 5 Rs. / 2.5 gm
3) Citric acid 1.5 Rs / 2.5 gm.
4) CaCO3 - 1 Rs / 2.5 gm
TOTAL = 95 Rs. / 500 gm TOTAL = 93.5 Rs. / 500 gm
Discussion
The grease that we have produced from non edible oil seed Karanja is cheaper than that
of market grease. Hence the production process is cost effective, and this Bio-grease can be
introduced into the market.
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CHAPTER 10
COMPARISON FOR AUTOMOBIL AND ENGINE APPLICATION OF
BIOGREASE FROMKARANJA OIL WITH MARKET PETROLEUM GREASE
W

Property VEEDOL AP3 Karanja grease

Texture Smooth Smooth
NLGI No. 3 2
Penetration No. 250 269
Dropping Point 120 130
Colour Light yellowish Light yellowish
Fineness Smooth Smooth
Soap type Lithium Lithium
Prise 95 Rs/ 500 gm 93.5 Rs/ 500 gm
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CHAPTER 11
CONCLUSION
From this study of the properties of biogrease compared with standard properties of
market grease i.e. VEEDOL AP-3, making biogrease from non edible oilseed karanja as the base
oil, several conclusions can be summarized as follow:
The amount of lithium soap needed is 20 gm/ 500 gm of total weight to produce the
biogrease of NGLI No. 2 from karanja oil as the base oil. The free fatty acid content of Karanja
Oil is 12.62 %.Penetration No. of the biogrease is 269. Dropping point of the grease is 130.The
Price of the grease produced is almost 93.5 Rs / 500 gm, which is less than that of market grease,
which is the remarkable point,
More work is going on the different properties of grease for its characterisation at Amity
University Rajasthan, Jaipur, Rajasthan
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CHAPTER 12
FUTURE ASPECTS
The biogrease produced from non edible oilseed karanja is prepared from the traditional
soap thickener lithium hydroxide. By varying the concentration of lithium hydroxide the effect
can be studied on grease. Also other alternatives for lithium hydroxide can be used for trial such
as calcium 12- hydroxyl stearate which is less toxic than lithium hydroxide. The current costing
of the biogrease is almost equal to that of market grease. This costing can be further reduced by
finding alternative to lithium hydroxide and further optimization of process. Also biological
additives such as polymers, polysaccharides can be used.
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CHAPTER 13
REFERENCES AND BIBLOGRAPHY
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Vol. 2, Page No.- 541- 600.
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production of oleochemicals Irom non traditional oils ', Rasayan journal chem., Vol.3,
No.2 , Page No.- 354-358.
9) G. Fucks and V. V. Vainsntok, (Oct. 1992), 'chemistry and technology of fuels and oils,
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High-Temperature Capability of Lithium 12-Hydroxystearate Soap Thickened Grease, The
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12) Mac Vean, (June 2003), 'Plantas utiles del Peten, Universidad del Valle de Guatemala, Vol
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Engineering, Department of Biotechnology, Srinivasan College of Arts and Science,
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International. Headquarters, Vol No. 4, page no- 27-80.
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17) Samman, Nicolas, (February 2007), 'High Temperature Greases, NLGI Spokesman, Vol.
70(11), Page No. 14-23.
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No. 56- 89.
19) Satish Lele, (September 2006), 'Biodiesel and Jatropha Plantation, J-22 sector 7 Vashi
Navi Mumbai-400703, Vol No.- 5, Page No.- 354-566.
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Oil and Thickener Lithium Soap ,CIGR Journal, Fac. oI Engineering, University oI
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of Industrial Chemistry, Vol. 6, Page No.- 333- 410.
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