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Biogreases for Environment Friendly Lubrication

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 13

Biogreases for Environment

Friendly Lubrication
UMESH CHANDRA SHARMA1* AND NEETU SINGH2

ABSTRACT
Biogrease is an environmentally acceptable green lubricant formulated from
plant origin base oils, thickeners and performance additives for the
lubrication of industrial, automotive and other mechanisms. Biogreases
are attractive particularly to those applications in which the grease is lost
to the environment and cannot be collected for reclamation such as
agriculture and forest machinery, rail road and marine applications where
grease is lost to soil and water. The present article on bio-grease first gives
a basic definition of lubricant and grease followed by functions and history
of use of grease in human civilization. A survey of world grease market and
future estimates is given based on national lubricating grease institute
(NLGI) and Frost & Sullivan grease production survey and reports. A
discussion on three basic grease components with their sources, advantages
and disadvantages is given in tabular form. Need for biogreases and their
application areas are discussed. The bio-based content required in grease
for its labelling as a bio product is discussed. The article then presents the
chemical and structural differences between mineral and vegetable oils and
fats, limitations of vegetable oils in using them as base oil for lubricating
greases and different chemical methods to modify these oils for their potential
use as bio-lubricant and bio-grease. The laboratory method for production
of bio-grease from transesterified esters of vegetable oils using conventional
lithium or aluminium metal soaps is included. Finally, the important test
methods like consistency, dropping point, biodegradability, oxidation
stability, water washout resistance, operating temperature, etc. needed to
analyze the performance of a biogrease are discussed.

1
Department of Chemical Engineering, UIET, CSJM University, Kanpur-208024 (India)
2
Department of Chemical Engineering, Thapar University, Patiala-147004 (India)
*Corresponding author : E-mail : uc_sharma@hotmail.com
2 Environmental Sci. & Engg. Vol. 1: Sustainable Development

Key words: Base oil, Biogrease, Biolubricant, Bio-degradability,

Consistency, Dropping point, Oxidation stability, Vegetable
oil, Kyoto protocol, NLGI, Frost & Sullivan.

INTRODUCTION

A lubricant is a material that is applied to reduce friction and wear between

two surfaces which are in contact and undergo relative motion. It may be
in the form of liquid, grease, dry film and coating[1]. Lubricating grease is a
solid to semi-solid dispersion of a thickening agent in a liquid lubricant[2].
The mineral and synthetic oils are traditionally used as liquid lubricants
for the greases[3], but for last few decades the vegetable oils and animal
fats based synthetic bio-oils are gaining attention due to growing
environmental concerns[4]. Thickening agents provide a spongy matrix that
stores the liquid lubricant. When the grease is subjected to shearing,
mechanical shock, loading or other stresses, it releases oil, which flows
into the gaps between mechanical parts and does the actual lubrication
work [5].

Greases are used in various mechanical systems to reduce friction and

wear between moving components such as metal joints, shafts and bearings
[6]
in order to maintain their mobility under conditions of application [7].
Grease provides protection from corrosion by preventing entrance of water
and contaminants. Grease functions as a sealant to prevent lubricant
leakage, dripping and throw-off and to keep out foreign materials. Good
quality grease maintains its consistency during service and also acts to
keep deteriorated seals effective[8]. Greases play an important part in saving
energy and reducing carbon dioxide (CO2) emission by improving the
lubrication efficiency and prolonging the service life of machines[9].

HISTORY OF GREASE

Fig. 1: Egyptian workers pulling a heavy sledge over wet sand

The earliest record for use of lubricants and greases to reduce friction
by human civilization dates back to 2400 B.C. in a painted wall relief of an
Egyptian Pharaoh’s tomb where a worker standing on the front of the sledge
is seen pouring the water on sand for moving a large statue (Fig. 1.)[10].
Hittite chariots from another tomb dated to around 1400 B.C. are found
Biogreases for Environment Friendly Lubrication 3

lubricated on axle with a mixture of tallow and limestone that probably

seems to be an early form of grease (Fig. 2)[11].

Fig. 2: A Hittite chariot with its three occupants

The vegetable oils, animal fats and other bio-based materials kept wheels
and gears moving along smoothly for over 4,000 years[5] until the second
half of the 19th century when they were replaced by mineral oil and to a
lesser extent by synthetic oil based lubricant and greases[12]. Since 1859,
only the mineral oil based greases were manufactured[13]. Vegetable oil
based greases have been reported in literature as early as the 1940’s;
however, their practical applications appeared only in the 1960’s. The main
reasons for their limited applications appear to be their high prices, limited
performance and lack of support from government and environment
agencies[12]. Current century is witnessing the resurgence of greases made
from vegetable oils after a gap of around 150 years principally due to
uncertainties in crude oil prices, depleting oil reserves, excess production
of vegetable oils in many parts of the world, growing environmental
consciousness, drive for products based on renewable sources and stringent
legislative compliances[5].

GLOBAL MARKET FOR GREASE

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[2].

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 availability
of Iranian crude to global consumers. The current crude oil prices at US$40
a barrel are already the lowest since March 2009. These factors might
adversely affect the growth of biodegradable oils based lubricants and
greases segment in market.

The National Lubricating Grease Institute (NLGI) 2010 Grease

Production Survey indicates that about 93% (over 1 billion kilograms) of
4 Environmental Sci. & Engg. Vol. 1: Sustainable Development

total worldwide grease volumes were mineral oil based greases, followed
by synthetic and semi-synthetic oil based greases at about 3% each.
Biogreases made their entry in NLGI survey for the first time with about
1% market share [12]. The NLGI 2012 Grease Production Survey indicates
that only 0.42% of the total reported production worldwide is based on
biodegradable base oils[14]. Frost and Sullivan reports that the mineral oil
based greases accounted for 40.4% of the global industrial grease market
revenue 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
remaining 3.9% revenue contributed by environment friendly greases. In
2013, the total industrial grease market generated US$1,169.3 million and
it is expected to grow at a compound annual growth rate (CAGR) of 6.6%
between 2012 and 2019 (Fig. 3.)[2].

Fig. 3: Global industrial greases sales breakdown in 2012 and projections for 2019
(Data source: Frost and Sullivan, 2014)

GREASE STRUCTURE

Greases contain three basic components: base oil, thickener and additives.
Base oil can be a mineral oil, synthetic oil, or vegetable oil. Thickeners can
be inorganic (silica and bentonite clay) or organic (polyurea) materials or
metal soaps. The metal soap can be a reaction product of a metal-based
material (oxide, hydroxide, carbonate, or bicarbonate) and carboxylic acid
or its ester, or it can be added separately. Commonly used soap-type greases
are based on calcium, lithium, aluminium and sodium. The additives for
lubricating oils and greases are similar[15]. The various grease components
with their sources, advantages and disadvantages are given in Table 1.

NEED FOR BIO-BASED GREASES AND THEIR APPLICATION AREAS

Used lubricating oils and greases present a serious threat to biosphere on

account of their non-biodegradability and ability to contaminate the
environment[6]. Since 1970s, the negative environmental impacts of mineral
oil based lubricants and greases have been thoroughly studied by
Biogreases for Environment Friendly Lubrication 5

Table 1: Grease components with their source, advantages and disadvantages[5, 15]

Compone- Sources Examples Advantages Disadvantages

nt (wt.%)

Base oil Petroleum Petroleum fra- Thermal and oxidati- Depleting feedstock
(75-90%) ctions having an ve stability/Low cost / / Toxicity and envir-
average volati- High lubricity onmental issues /
lity lower than Supply and price
that of gas oils fluctuations
Vegetable oil Soybean/Sun- Good lubrication / Thermal and oxida-
flower/ Canola / Biodegradable tive instability / Hi-
Castor/Corn/ gh price
Cottonseed/ Pa-
lm oil/ Karanja/
Jatropha
Synthetic oil Diesters and po- Thermal, oxidative, Diesters may deg-
lyol esters/Poly- hydraulic and hydrol- rade elastomeric
glycols/Polyalp- ytic stability/Wide vis- seals / Polyol esters
haolefins (PAO) cosity range/Wide ope- are expensive / Poly-
rating temperature glycols may degrade
range/High lubricity/ seals and surface
Low volatility/Long coatings/High visco-
service life sity PAO oils have
varying degrees of
biodegradability
Fatty acids Simple metal Anti-corrosion proper- Limited tempe-
from vegeta- soaps (lithium ties / Water resistant / rature and perfor-
ble, animal or or aluminium) Easy availability mance range / Can
fish oils re- stiffen after exten-
acted with ded use
metal hydro-
xide
Simultaneous Complex metal High and low tempe- Can be water-sen-
reaction of an soaps (lithium, rature applications / sitive / May harden
alkali with a aluminium, or Wash and corrosion on overheating
fatty acid and calcium sulph- resistance / Ability to
an inor-ganic onate) carry high loads with-
or short-chain out requiring extreme
organic acid pressure additives

Thickener Natural or Organo-clay Heat resistance May form residues

(5-20%) synthetic cla- on extended use /
ys modified Incompatible with
with or-ganic most other grease
amines types
Reaction of Polyurea Little to no metal co- Difficult to manu-
amines with ntent/Resistance to facture / Toxic ingre-
diisocyanates water and oxidation / dients/Some types
(synthetic) Good for ball bearings are incompatible
and electric motors / with most other
Table 1: Contd...
6 Environmental Sci. & Engg. Vol. 1: Sustainable Development

Table 1: Contd...
Compone- Sources Examples Advantages Disadvantages
nt (wt.%)

Improved shear per- greases

formance, shelf life,
pumpability, rust pro-
tection and extreme
pressure performance
Flame pyro- Fumed silica High temperatures, Polar additives can
lysis of SiCl4 specialized applica- disrupt the silica
or arcvapori- tions (e.g., optical particle network
zation of qua- cable fillers)
rtz sand
Synthetic Zn dialkyl dithi- High pressure appli- Toxicity and envir-
o p h o s p h a t e s cations / Anticorrosion onmental effects/
(ZDDP)/Mo, Sb, applications Can accumulate in
or Pb dialkyl di- mechanisms and
thiocarbamates cause wear
(DTC)/Pb naph-
thenate
Synthetic, Bi naphthenate Less toxic and does not Active sulphur co-
used in conju- bioaccumulate/Extre- EP agents can incr-
nction with me pressure proper- ease wear scarring
organosulphur ties similar to Pb na- at high speeds
Additive compounds phthenate
(0-10%) Natural (gra- MoS2, graphite Friction reduction/ Particles can accu-
phite) or syn- High temperature and mulate in compon-
thetic (gra- high pressure applica- ents and cause wear
phite, MoS2) tions
Synthetic Dodecylene suc- Corrosion protection / Less effective in pre-
cinic acid and Metal-free/Inhibits venting corrosion on
other succinate sludge and varnish cast iron or lead
derivatives formation

researchers and debated among policy makers to draft environment

protection policies[16]. The level of customer awareness has also gone up
particularly in the last two decades. An average customer is now aware of
the negative effects that mineral and synthetic oil based lubricants and
greases exert on the environment and makes demand for bio-based products
to reduce this impact[17]. Here the main motivation for buying bio-based
lubricants and greases is to protect the environment[5]. These products are
biodegradable, cost effective, environmentally benign, renewable, non-toxic
and not bioaccumulative[14, 18-19]. In addition to these environmental
benefits, bio-based lubricants and greases have huge potential for
encouraging economic health of country’s rural communities by adding value
to commodities and are critical to national economy, security and
environment[20].

Biogreases receive impressively increased attention for lubrication of

Biogreases for Environment Friendly Lubrication 7

agriculture and forestry machinery, construction vehicles, rail curve, rail

flange, mining, waste water and sewage treatment, food industry and
marine applications. In all these applications there is a clear loss of
lubricating material where the grease eventually ends up either in soil or
water[2, 12, 14].

LEVEL OF BIO-BASED CONTENT FOR BIO-LABELLING OF GREASE

The bio-based content of lubricating greases is an indication of the

percentage of renewable hydrocarbon typically derived from plant or animal
sources[18]. Currently there is no globally accepted standard classification
for bio-lubricants and bio-greases. Though a few classifications have evolved
locally in Europe such as German certification “the blue angel” and swedish
standard “Lubricating grease: Requirements and Test Methods – SS
155470” [14]. The blue angel is a german certification for products and
services that have environment friendly features. Section 4.2 of Swedish
Standard SS 155470 signifies that the base fluid in the lubricating grease
should be biodegradable with minimal aquatic toxicity. A lubricating grease
conforming to SS 155470 is classified in one of three environmentally
adapted classes A, B, or C. Class A implies that the mass content of
renewable resources should be more than 65%. The content of renewable
resources in Class B should be more than 45%. Class C type lubricating
greases bear no such demands for a specific mass content of renewable
materials. Technically speaking, a more bio-degradable grease can be
formulated just by replacing the mineral oil with a vegetable oil. However,
a completely bio-based grease can only be formed when traditional
thickening agents (metallic soaps, phyllosilicates or polyurea compounds)
are substituted by other more environmentally acceptable thickeners[3].

DIFFERENCE BETWEEN MINERAL OIL, VEGETABLE OIL AND FAT

Fats and oils are water-insoluble, hydrophobic substances of vegetable,

land animal, or marine animal origin which consist predominantly of
glyceryl esters of fatty acids called triglycerides. Structurally, a triglyceride
is the reaction product of one molecule of glycerol (trialcohol) with three
molecules of fatty acids (carboxylic acids) to yield one molecule of a
triglyceride (ester) and three molecules of water (Fig. 4.)[21].

Both mineral and vegetable oils are characterized by long hydrocarbon

chains; vegeta-ble oils have polar ester groups (A) and unsaturated double
bonds (B) (Fig. 5.) [22] . Fats contain saturated or nearly saturated
hydrocarbon chains and are solid at room temperature. Oils, on the other
hand, have a higher degree of unsaturation and are liquid at room
temperature. Unsaturation here refers to number of carbon-carbon double
bonds in the carbon chains. The greater saturation corresponds to fewer
8 Environmental Sci. & Engg. Vol. 1: Sustainable Development

Fig. 4: Esterification of glycerol to form triglyceride

double bonds. The saturated oils with greater hydrogen content are
preferred over unsaturated oils for intended application as base lube oil
because of better performance at low temperatures and stability towards
oxidation[5].

Fig. 5: Structural differences between mineral and vegetable oils[22]

Vegetable oils differ from mineral oils in physicochemical as well as

tribological properties due to presence of triglyceride in its chemical
structure. Vegetable oils render non-flammable character owing to their
high flash and fire points over 300ºC. Other characteristics include good
lubricity, high viscosity indices, better viscosity-pressure performance,
superior thin film strength, lower coefficient of friction, lower volatility,
ability for adhering to metal surfaces, greater solubility for polar
contaminants and additive molecules, non-toxicity and high bio-
degradability[3, 5, 16, 20, 23].

DRAWBACKS OF VEGETABLE OILS

Vegetable oils have certain disadvantages like poor thermo-oxidative and

hydrolytic stability, low temperature performance, high pour points and
usually higher costs than mineral oil[3, 19-20, 23]. These drawbacks make
vegetable oils incapable for direct use as lubricant as compared to mineral
Biogreases for Environment Friendly Lubrication 9

oil based lubricants and greases. Vegetable oils can be chemically modified
by transesterification, epoxidation, enzyme catalyzed esterification and
estolide formation for their use as bio-lubricants and bio-greases[16].

LABORATORY PREPARATION OF BIO-BASED LUBRICATING

GREASES

Transesterified esters of vegetable oils formed using branched neopentyl

polyols (trimethylolpropane or neopentyl glycol or pentaerythritol) are used
as base oil in formulating bio-based grease using conventional lithium or
aluminium preformed metal soaps. Soap concentration is fixed at 10–15%
w/w in the final product. Preformed soap is thermo mechanically dispersed
in a batch reactor equipped with a high speed impeller rotating at a speed
of 70 rpm. In the first step, 60% of the total amount of base oil is charged
into an open vessel which is pre-heated up to 100ºC and 5% w/w (on dry
basis over the total formulation) of the soap is added slowly in the form of
aqueous solution up to neutralization. Then, 20% base oil and the remaining
soap are added and the temperature is raised to 200ºC. The mixture is
maintained at this temperature for one hour and afterward the remaining
20% base oil is added at 120ºC during cooling the mixture. Finally, the
homogenization of the grease is done at rotational speed of 5000 rpm for 15
minutes and is cooled to room temperature. The formulated grease is then
tested for its properties[16-17].

PERFORMANCE ANALYSIS OF A BIOGREASE

The test methods required to analyse the performance of a biogrease are

the same as those required to analyse the mineral or synthetic oil based
greases. These test methods include the consistency (NLGI grade), dropping
point, bio-degradability, load carrying capability, oxidation stability, texture
and structure, flow characteristics and pumpability, mechanical stability
and reversibility, bleeding characteristics, water washout, operating
temperature and rust and corrosion protection.

Consistency

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 D217 or ASTM D1403. 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 millimetre and is
used to determine the NLGI grade of the grease. The softer the consistency,
10 Environmental Sci. & Engg. Vol. 1: Sustainable Development

the higher is the penetration number. Table 2 below lists the NLGI
consistency numbers in order of increasing consistency[1, 8].

Table 2: NLGI grades with their corresponding penetration[1]

NLGI consistency number Worked penetration range at 25ºC

000 445-475
00 400-430
0 355-385
1 310-340
2 265-295
3 220-250
4 175-205
5 130-160
6 85-115

Dropping Point

Dropping point is the temperature at which grease becomes fluid enough

to drip through orifice of the test apparatus under conditions specified by
ASTM D 2265. In easier terms, dropping point is the temperature at which
the grease no longer stays in place. It is an indicator of the heat resistance
of 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[1, 8].

Biodegradability

The biodegradable lubricants decompose or transform in the environment

due to the action of microorganisms found in groundwater or soil. A
biodegradable lubricant is that which contains more than 10% by weight of
oxygen (O2) content. To analyse the biodegradability of grease, a quantity
of test grease is dissolved in a sample, which along with some reference
samples, is placed in a controlled environment and then inoculated with
standard specified bacteria. The biodegradability test runs for 28 days and
as bacteria consume biodegradable materials, they consume the O2 and
release CO2. After consuming all the nutrients in the sample, the bacteria
begin to die out and O2 consumption flattens out and then drops[18]. The
test grease must undergo 60% or more biodegradation expressed in terms
of theoretical CO2 in 28 days and 67% or more biodegradation expressed in
terms of theoretical O2 uptake in 28 days in laboratory testing[1].
Biogreases for Environment Friendly Lubrication 11

Oxidation Stability

The ability of grease to resist chemical reaction with O2 is termed as its

oxidation stability. Oxidation of grease produces insoluble gum, sludge and
lacquer-like deposits that cause sluggish operation, increased wear and
reduction of clearances. All these factors may lead to degradation of grease
which in turn will reduce the useful service life. Long exposure to high
temperatures accelerates oxidation in greases. Oxidized grease becomes
softer and appears darker. Methods of measurement of oxidation stability
include ASTM D942 and D5483[8].

Water Washout Resistance

The ability of lubricating grease to withstand the effects of water with no

change in its lubricity is called water washout resistance. A soap/water
lather may suspend the oil in the grease, forming an emulsion that can
wash away or reduce lubricity by diluting and changing grease consistency
and texture[1, 8]. Water washout resistance is measured using the laboratory
apparatus and technique described in ASTM D1264. The test method
involves packing a grease sample in a ball bearing which is then impinged
with a jet of water at the specified flow rate and temperature. The
percentage of test grease washed out in one hour is determined by weight.

Pumpability

Pumpability is the ability of lubricating grease to flow under pressure

through the lines, nozzles and fittings of a grease dispensing system. It is
best indicated by the apparent viscosity at moderate shear rate[1].

Operating Temperature

The operating temperature of grease is the range between the lowest

temperature where a lubricated device can be started up in an acceptable
manner and the highest temperature where lubrication is adequate. The
operating temperature of grease depends on its formulation (base fluid,
thickener, additives). The temperature is usually measured in the general
vicinity of the lubricated contact and not between loaded surfaces[1]. The
temperature limits for use of greases are determined by dropping point,
oxidation stability and stiffening at low temperatures[24].

High temperature harms grease more than it harms lubricating oil.

Grease being a semi-solid material cannot dissipate heat by convection
like lubricating oil and so have poor ability to dissipate heat. The excess
heat accumulated in grease results in accelerated oxidation or even
carbonization in which grease hardens or forms a crust. In addition, high
temperature induces softening and bleeding, causing grease to flow away
12 Environmental Sci. & Engg. Vol. 1: Sustainable Development

from needed areas. The mineral oil in grease can flash, burn or evaporate
at temperatures greater than 177ºC. At low enough temperature, the grease
becomes so viscous that it can be classified as hard grease. The pumpability
suffers and machinery operation may become impossible due to torque
limitations and power requirements. The pour point of base fluid has been
accepted as the low-temperature limit of grease[8].

CONCLUSIONS

The first oil crisis in 1973 followed by second oil crisis in 1979 shocked the
world oil consumers with supply and price fluctuations in petroleum
products. These two crises in quick succession alarmed the world powers
and caused them to look for alternatives of crude oil. Beginning from the
same decade, researchers started publishing their works on the negative
environmental impacts of mineral oil based lubricants and greases. The
1992 United Nations Framework Convention on Climate Change
(UNFCCC), later extended in 1997 Kyoto Protocol, helped raising the
awareness among the common people to protect the environment from
anthropogenic interference. The depleting crude oil reserves, fluctuations
in oil prices and negative environmental impacts of petroleum products
are causes of major concern for everyone involved. Today a wide range of
biogreases are available commercially with lower cost environment friendly
manufacturing processes. The biogreases can be used in all applications
conventionally requiring mineral oil based greases, but are particularly
advantageous to agriculture, forest machinery, rail road and marine
applications where the grease is finally lost to soil or water. Apart from
cost and environmental benefits, biolubricants and biogreases can help in
improving the economic health of rural communities.

REFERENCES

[1] Grease glossary (https://www.nlgi.org/grease-glossary).

[2] Shankar, S. (2014). Emerging trends in the industrial greases market. Journal of
Business Chemistry, 11(3): 143–149.
[3] Sánchez, R. et al. (2008). Effect of thermo-mechanical processing on the rheology
of oleogels potentially applicable as bio-degradable lubricating greases. Chemical
Engineering Research and Design, 86: 1073–1082.
[4] Honary, L. and James, W. (2011). Performance properties of bio-based rail curve
greases, arema annual conference, minneapolis,
[5] McGuire, N. (2014). Bio-based greases: Back to the future, Tribology and
Lubrication Technology, pp. 36–47.
[6] Pilusa, T.J. et al. (2013). Thermo-chemical extraction of fuel oil from waste
lubricating grease, Waste Management, 33(6): 1509–1515.
[7] (2008). Guide to oils and greases, Penrite Oil Company Pty. Ltd., Australia.
[8] Wright, J. Grease basics (http://www.machinerylubrication.com/Read/1352/grease-
basics)
[9] Xiaoqiang, F. (2014). Tribological properties of conductive lubricating greases.
Friction, 2(4): 343–353.
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