Note: Descriptions are shown in the official language in which they were submitted.
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ENVIRONMENTALLY FRIENDLY LUBRICANTS
FIELD OF THE INVENTION
This invention relates to environmentally friendly engine lubricant
compositions
suitable for internal combustion engines, and in particular for use in
gasoline-fueled and
diesel-fueled engines.
BACKGROUND OF THE INVENTION
Vegetable oil triglycerides are available for use in food products and
cooking.
Many such vegetable oils contain natural antioxidants such as phospholipids
and sterols
that prevent oxidation during storage. Triglycerides are considered the
esterification
product of glycerol with three molecules of carboxylic acids. The amount of
unsaturation
in the carboxylic acid affects the susceptibility of the triglyceride to
oxidze. Oxidation
can include reactions that link two or more triglycerides together through
reactions of
atoms near the unsaturation. These reactions may form higher molecular weight
material
which can become insoluble and discolored e.g. sludge. Oxidation can also
result in
cleavage of the ester linkage or other internal cleavage of the triglycerides.
The
fragments of the triglyceride from the cleavage, being lower in molecular
weight, are
more volatile. Carboxylic acid groups generated from the oxidation of
triglyceride make
the lubricant acidic. Aldehyde groups may also be generated. Carboxylic acid
groups
have attraction for oxidized metals and can solubilize them in oil promoting
metal
removal from some surfaces of lubricated metal parts.
Due to oxidation problems with natural triglycerides, most commercial
lubricants
are formulated from petroleum distillates which have lower amounts of
unsaturation
making them resistant to oxidation. Petroleum distillates require additives to
reduce wear
and oxidation, lower the pour point and modify the viscosity index (to adjust
either the
high or low temperature viscosity) etc. The petroleum distillates are
resistant to
biodegradation and the additives used to adjust certain characteristics (often
containing
metals and reactive compounds) further detract from the biodegradability of
the spent
lubricant.
Synthetic ester lubricants having little or no unsaturation in the carbon to
carbon
bonds are used in premium quality motor oils due to their desirable
properties. However
the acids and alcohols used to make synthetic esters usually are derived from
petroleum
distillates and are thus not from a renewable source. Synthetic lubricants are
also more
costly and less biodegradable than natural triglycerides.
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The finite supply of petroleum coupled with concern over the environmental
effects from spills and disposal of petroleum based lubricants has fueled
interest in the
use of vegetable oils as viable substitutes for lubricants. Vegetable oils
have the
advantages of having a high flash point and excellent lubricating properties,
while also
being biodegradable and renewable. However, vegetable oils also have
relatively poor ,
flow characteristics at low temperatures and relatively poor oxidative
stability which
prevent their uses in some of the more extreme environments.
The vast majority of efforts to produce vegetable oil lubricants have utilized
oils
high in natural oleic acid levels, such as safflower, sunflower, corn, soybean
and
rapeseed oils. These polyunsaturated oils have lower oxidative stability,
whereas fully
saturated oils tend to crystallize at low temperatures. Thus, the use of oils
with a high
preponderance of the monounsaturated fat, oleic acid, provides a reasonable
compromise
between these two extremes.
In order to provide engine lubricants based on vegetable oils, certain
standards
should be met, including specifications required by SAE (Society of Automotive
Engineers), API (American Petroleum Institute) and ILSAC (International
Lubricant
Standardization and Approval Committee). In particular, the SAE low
temperature
viscosity requirements have been difficult to meet in vegetable based oils.
Further, an
oil for use in internal combustion engines should also satisfy the most
current
requirements of the GF-3/API SL minimum performance standards, including a
gelation
index of less than about 12; high temperature TEOST (thermo-oxidative engine
oil
simulation) of total deposits of 45 mg maximum; remain homogeneous and
miscible
when mixed with SAE reference mineral oils; low volatility; phosphorous level
of 0.1%
maximum; and has to pass foam, filterability and ball rust test.
Therefore, there is a need for a vegetable oil-based lubricant that can be
used as
internal combustion engine oils of varying SAE viscosities that meet the
current GF-
3/API SL specifications and are at least about 60% biodegradable.
SUMMARY OF THE INVENTION
The above need is met by various embodiments of the invention. In some
embodiments, an environmentally friendly lubricant comprises a transesterified
triglyceride oil and a synthetic ester different from the triglyceride oil,
the lubricant
having a gelation index less than about 12 and being at least 60%
biodegradable. The
lubricant can be used as an automobile engine oil and may further include
viscosity
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index improvers and/or detergent inhibitor (DI) packages. The automobile
engine oil
may also include other additives, such as a pour point depressant,
antioxidant, friction
modifier, rust inhibitor, corrosion inhibitor and anti-foaming agent.
Additional
embodiments are explained in the following description.
BRIEF DESCRIPTION OF THE DRAWINGS
Figure 1 is a graph of gelation index (Gi) against the weight percent of
viscosity
modifier (VII) for various lubricants made in embodiments of the invention.
DESCRIPTION OF EMBODIMENTS OF THE INVENTION
Embodiments of the invention provide an environmentally friendly lubricant for
use under a variety of operating conditions in automobiles, trucks, vans,
buses, and off
highway farm, industrial, and construction equipment. Preferably, the oil is
at least
about 60% biodegradable according to ASTM D5864-95 and meets one or more of
the
current standards according to the Society of Automotive Engineers (SAE),
American
Petroleum Institute (API) and the International Lubricant Standardization and
Approval
Committee (ILSAC), which are incorporated by reference herein in their
entirety.
In the following description, all numbers disclosed herein are approximate
values, regardless whether the word "about" or "approximate" is used in
connection
therewith. They may vary by 1 percent, 2 percent, 5 percent, or, sometimes, 10
to 20
percent. Whenever a numerical range with a lower limit, RL and an upper limit,
RU, is
disclosed, any number falling within the range is specifically disclosed. In
particular, the
following numbers within the range are specifically disclosed: R=RL+k*(RU-RL),
wherein k is a variable ranging from 1 percent to 100 percent with a 1 percent
increment,
i.e., k is 1 percent, 2 percent, 3 percent, 4 percent, 5 percent,..., 50
percent, 51 percent, 52
percent,..., 95 percent, 96 percent, 97 percent, 98 percent, 99 percent, or
100 percent.
Moreover, any numerical range defined by two R numbers as defined in the above
is also
specifically disclosed.
The following are test properties, definitions and test methods used in the
description and examples that follow:
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Tahlp 1 ~_ Testinu Methods and Terminolo~v
Pro erties Test Method
Biode radabili ASTM D5864
Scannin Brookfield Viscosi ASTM D5133
Cold Crankin Stimulator CCS ASTM D5293
Gelation Index ASTM D5133-99
Gelation Tem erature ASTM D5133-99
Kinematic Viscosi ASTM D445
Determination of Yield StressASTM D4684-98
and Apparent
Viscosity of Engine Oils at
Low Temperature
MRV TP-1
Pour Point ASTM D97
Viscosity at High Shear Rate ASTM D4683
and High
Temperature by Tapered Bearing
Simulator
TBS
Viscosi Index ASTM D2270
Viscosi ASTM D445
Volatility at 371C (SimulatedASTM 6417
Distillation,
Flash Point
Evaporation % Wt. Loss (NOACK)ASTM D972
Definitions
ASTM stands for American Society for Testing and Materials which provides
standard protocols for material evaluation.
S Biodegradability is a measure of a lubricants biodegradability. ASTM D 5864
determines lubricant biodegradation. The test determines the rate and extent
of aerobic
aquatic biodegradation of lubricants when exposed to an inoculum under
laboratory
conditions. The degree of biodegradability is measured by calculating the rate
of
conversion of the lubricant to C02. A lubricant is classified as readily
biodegradable
when 60 percent or more of the test material carbon is converted to COZ in 28
days, as
determined using this test method. In some embodiments, the lubricants have a
biodegradability of at least 65%, 70%, 75%, 80%, 85%, 90%, or 95%.
BROOKFIELD VISCOSITY is viscosity, in centipoises, as determined on the
Brookfield viscometer. The operating principle for the Brookfield viscometer
is the
torque resistance on a spindle rotating in the fluid being tested. Although
Brookfield
viscosities are most frequently associated with low temperature properties of
gear oils
and transmission fluids, they are in fact determined for many other types of
lubricants.
COLD Cranking STIMULATOR (CCS) is an intermediate shear rate viscometer
and measures the resistance of an oil to engine cranking at low temperatures.
CCS is
controlled largely by the additives in the oil and the viscosity index of the
base oil.
GELATION INDEX is defined as the largest rate of change of viscosity increase
when slowly cooled from -5°C to the lowest test temperature. The
gelation index is a
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number indicating the oil's tendency to form a gelated structure in the oil at
colder
temperatures. Numbers above 6 indicate some gelation-forming tendencies.
Numbers
above 12 are of concern to engine makers. Numbers above 15 have been
associated with
field-failing oils. Gelation index is determined in accordance with ASTM D-
5133 ,
S which is incorporated by reference herein in its entirety. The gelation
index can be
measured by the Scanning Brookfield Technique in accordance with ASTM D5133.
In
this test, a tube of oil containing a rotor driven at 0.3 RPM is slowly cooled
at 1 °C per
hour for approximately two days, typically from -5 °C (23 °F) to
-45 °C (-40 °F). As the
sample is cooled, the viscosity is measured by the increasing torque generated
by a
spindle rotating in the oil at constant speed. A plot of the overall viscosity
curve is
generated. The gelation index is determined accordingly.
GELATION POINT also known as GELATION TEMPERATURE is defined as
the temperature at which the gelation index occurs. Gelation temperature is
determined
in accordance with ASTM D-S 133 , which is incorporated by reference herein in
its
entirety.
KINEMATIC VISCOSITY (KV) is viscosity now commonly reported in
centistokes (cSt), measured at either 40°C or 100°C.
YIELD STRESS AND Apparent LOW TEMPERATURE VISCOSITY (MRV
YS and MRV TP-1) measures the borderline pumping temperature for engine oils.
An
engine oil is held at 80°C in a mini-rotary viscometer and slowly
cooled at a
programmed cooling rate to a final test temperature, a low torque is applied
to the rotor
shaft to measure yield stress, then a higher torque is applied to determine
the apparent
viscosity of the sample.
POISE is the CGS unit of absolute viscosity. This is the shear stress (in
dynes per
square centimeter) required to move one layer of fluid along another over a
total layer
thickness of one centimeter at a shear rate of one centimeter per second.
Dimensions are
dyne-sec/cm2. The centipoise (cP) is 1/100 of a poise and is the unit of
absolute viscosity
most commonly used. Whereas ordinary viscosity measurements depend on the
force of
gravity on the fluid to supply the shear stress and are thus subject to
distortion by
differences in fluid density, absolute viscosity measurements are independent
of density
and are directly related to resistance to flow.
POUR POINT is a widely used low-temperature flow indicator defined as the
lowest temperature at which an oil or distillate fuel is observed to flow when
cooled
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under conditions prescribed by test method ASTM D97. The pour point is
3°C (5°F)
above the temperature at which the oil in a test vessel shows no movement when
the
container is held horizontally for five seconds.
TAPERED Bearing SIMULATOR (TBS) measures high temperature high shear
rate viscosity of motor oils, very high shear rates are obtained by using an
extremely
small gap between the rotor and stator wall.
VISCOSITY index (VI) measures the rate of change of viscosity with
temperature, determined by formula from the viscosities at 40°C and
100°C in
accordance with ASTM D567 (or D2270 for VI's above 100).
VISCOSITY is a measure of a fluid's resistance to flow. It is ordinarily
expressed
in terms of the time required for a standard quantity of the fluid at a
certain temperature
to flow through a standard orifice. The higher the value, the more viscous the
fluid.
Since, viscosity varies inversely with temperature, its value is meaningless
unless
accompanied by the temperature at which it is determined. With petroleum oils,
viscosity
is now commonly reported in Centistokes (cSt), measured at either 40°C
or 100°C
(ASTM Method D445 - Kinematic Viscosity).
VOLATILITY is a property of a liquid that defines its evaporation
characteristics. Of two liquids, the more volatile boils at a lower
temperature, and it
evaporates faster when both liquids are at the same temperature. The
volatility of
petroleum products can be evaluated by tests for Flash Point, Simulation
Distillation and
volatility weight loss (NOACK).
Generally, the environmentally friendly lubricant in accordance with
embodiments of the invention is a mixture of transesterified vegetable oil and
esters.
The lubricant has a gelation index of less than about 12. In some embodiments,
the
gelation index is less than about 10, less than about 8, less than about 6,
less than about
4, or less than about 2. Preferably, the lubricant meets one or more of the
current
standards of the Society of Automotive Engineers (SAE), American Petroleum
Institute
(API) and the International Lubricant Standardization and Approval Committee
(ILSAC)
and is at least about 60% biodegradable according to the ASTM D 5864 test
which
defines the lubricant as readily biodegradable. Various types of vegetable
oils may be
present in the lubricant. For example, the transesterified vegetable oil may
be a mixture
of transesterified corn, rapeseed, soybean, and sunflower oil. The
transesterified
vegetable oil is mixed with esters that lower the gelation index and improve
viscosity.
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Table 2 indicates various compositions of environmentally friendly lubricant
compositions in accordance with embodiments of the invention.
Table 2
Component Preferred More PreferredMost PreferredPossible
Range (wt.%)Range (wt.%)Range (wt.%)Range (wt.%)
Transesterified Tri 30 - 85 35 - 75 40 - 65 0.5 - 99.5
1 ceride
Synthetic Ester 10 - 30 12 - 25 15 - 20 0.5 - 99.5
Ester Type Viscosity 0 - 3 0.2 - 2.5 0.5 - 2 0.5 - 99.5
Index
Improver
Olefin Copolymer Type0 - 6 1- 5 2 - 4 0.5 - 99.5
Viscosity
Index Im rover
Dispersant/Inhibitor 8 - 16 10 - 12 S - 10 0.5 - 99.5
Package
Additives 0 - 5 0 - 2 1 - 2 0.5 - 99.5
Mineral Oil 0 - 40 5 - 30 10 - 25 0.5 - 99.5
In some embodiments, the environmentally friendly lubricant is a mixture of a
transesterified vegetable oil in an amount from about 30 to about 85%, more
preferably
from about 35 to about 75%, and most preferred from about 40 to about 65%; a
synthetic
ester in an amount from about 10 to about 30%, more preferred from about 12 to
about
25%, and most preferred from about 15 to about 20%. Optionally, an ester type
viscosity
index improver may be added in an amount from about 0.1 to about 3.0%, more
preferred from about 0.2 to about 2.5%, most preferred from about 0.5 to about
2%;
further, an olefin copolymer type viscosity index improver is optionally added
in an
amount from about 0.1 to about 6.0%, more preferred from about 1 to about 5%,
most
preferred from about 2 to about 4%. The environmental lubricant further
optionally
includes a dispersant/inhibitor package in an amount from about 8 to about
14%, more
preferred from about 10 to about 12%; and other additives, such as a pour
point
depressant, antioxidant, friction modifier, rust inhibitor, corrosion
inhibitor, and anti-
foaming agent, in the amount from about 0.1 to about 5%, more preferred from
about 0
to about 2%. The environmentally friendly lubricant is formulated to have a
gelation
index of less than about 12 and is at least about 60% biodegradable in the
ASTM D-
5864-95 biodegradability test. The environmentally friendly lubricant also
meets all
ILSAC GF-3/API SL bench tests.
In other embodiments, transesterified vegetable oils in the environmentally
friendly lubricant are in the amount from about 30 to about 85 wt%, more
preferably
from about 35 to about 75 wt%, and most preferred from about 40 to about 65
wt%.
Suitable transesterified vegetable oils include, but are not limited to those
described in
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the following U. S. Patents which are incorporated by reference herein in
their entirety:
6,420,322; 6,414,223; 6,291,409; 6,281,375; 6,278,006; 6,271,185; and
5,885,643.
For example, one such transesterified vegetable oil comprises a glycerol
polyol
ester having the following formula, as disclosed in U. S. Patent No.
6,278,006:
O
I I
CH2 - O C - R~
O
II
CH -O C-R2
O
I I
CH2-O C-R3
wherein Rl, R2, and R3 are aliphatic hydrocarbyl groups having from about 4 to
about 24 carbon atoms inclusive, wherein at least one of Rl, RZ, and R3 have a
saturated
aliphatic hydrocarbyl moiety having about 4 to about 10 carbon atoms
inclusive, and
wherein at least one of Rl, R2, and R3 have an aliphatic hydrocarbyl moiety
having from
about 12 to about 24 carbon atoms inclusive. These triglycerides are available
from a
variety of plants or their seeds and are commonly referred to as vegetable
oils. R1, RZ
and R3 may be different moieties or the same moiety.
Within the triglyceride formula are aliphatic hydrocarbyl groups having at
least
60 percent monounsaturated character and containing from about 6 to about 24
carbon
atoms. The term "hydrocarbyl group" as used herein denotes a radical having a
carbon
atom directly attached to the remainder of the molecule. The aliphatic
hydrocarbyl
groups include the following:
(1) Aliphatic hydrocarbon groups; that is, alkyl groups such as heptyl, nonyl,
undecyl, tridecyl, heptadecyl; alkenyl groups containing a single double bond
such as
heptenyl, nonenyl, undecenyl, tridecenyl, heptadecenyl, heneicosenyl; alkenyl
groups
containing 2 or 3 double bonds such as 8,11-heptadecadienyl and 8,11,14-
heptadecatrienyl. All isomers of these are included, but straight chain groups
are
preferred.
(2) Substituted aliphatic hydrocarbon groups; that is groups containing non-
hydrocarbon substituents which do not alter the predominantly hydrocarbon
character of
the group. Those skilled in the art will be aware of suitable substituents;
examples are
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hydroxy, carbalkoxy (especially lower carbalkoxy), and alkoxy (especially
lower
alkoxy). The term, "lower" denoting groups containing not more than 7 carbon
atoms.
(3) Hetero groups; that is, groups which, while having predominantly aliphatic
hydrocarbon character contain atoms other than carbon present in a chain or
ring
otherwise composed of aliphatic carbon atoms. Suitable hetero atoms will be
apparent to
those skilled in the art and include, for example, oxygen, nitrogen and
sulfur.
Naturally occurring triglycerides are vegetable oil triglycerides.
Transesterified
triglycerides may be formed by the reaction of one mole of glycerol with three
moles of
a fatty acid or mixture of fatty acids or by the chemical modification of a
naturally
occurring vegetable oil. Regardless of the source of the triglyceride oil, the
fatty acid
moieties are such that the triglyceride has a monounsaturated character of at
least about
60 percent, preferably at least about 70 percent and most preferably at least
about 80
percent. The transesterified triglyceride may also have a monounsaturated
character of
at least about 85, 90, or 95 %.
Preferred transesterified vegetable oils have relatively high oxidative
stability and
good low temperature viscosity properties. Oxidative stability is related to
the degree of
unsaturation in the oil and can be measured, e.g., with an Oxidative Stability
Index
instrument, Omnion, Inc., Rockland, Mass. according to AOCS Official Method Cd
12b-
92 (revised 1993). Oxidative stability is often expressed in terms of "AOM"
hours. For
example, oxidative stability of oils can range from about 40 AOM hours to
about 120
AOM hours or from about 80 AOM hours to about 120 AOM hours. The
transesterified
vegetable oils used in some embodiments have excellent low temperature
viscosity
properties. A higher viscosity index value indicates that the viscosity of the
oil changes
less with a change in temperature. In other words, the higher the viscosity
index, the
greater the resistance of the lubricant to thicken at low temperatures and
thin out at high
temperatures. Transesterified vegetable oils used in certain embodiments have
a pour
point from about 0 °C to about -30 °C. The vegetable oils are
liquid at room temperature
and have a melting point of about 6 °C or less.
The vegetable oils may be genetically modified such that they contain a higher
than normal oleic acid content. High oleic vegetable oils contain at least
about 60%
oleic acid. These high oleic oils have lower oxidative stability, whereas
fully saturated
oils tend to crystallize at low temperatures. Normal sunflower oil has an
oleic acid
content of 25-30 percent. By genetically modifying the seeds of sunflowers, a
sunflower
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oil can be obtained wherein the oleic acid content is from about 60 percent up
to about
90 percent. U. S. Patents No. 4,627,192 and No. 4,743,402 are herein
incorporated by
reference for their disclosure to the preparation of high oleic sunflower oil
and its
method of measuring the oleic acid content.
S High oleic vegetable oils can be high oleic safflower oil, high oleic corn
oil, high
oleic rapeseed oil, high oleic sunflower oil, high oleic soybean oil, high
oleic cottonseed
oil, high oleic lesquerella oil, high oleic meadowfoam oil and high oleic palm
olefin. A
preferred oil is the AGRI-PURE 560T"~ which is a transesterified high oleic
acid
sunflower oil with short saturated fatty acid esters. AGRI-PURE 560TM is a
synthetic
10 polyolester TAG base oil by CARGILL (Minneapolis, MN).
The specifications according to the manufacturer for AGRI-PURE 560TM are:
Table 3: AGRI-PURE 560T""
Property Agri-Pure Test Method
560
Viscosi at 40C 28.76 cSt ASTM D445
Viscosi at 100C 6.47 cSt ASTM D445
Viscosity Index 189 ASTM D2270
Noack volatility 3.5 % ASTM D6375-99A
Specific Gravity 0.924 g/ml ASTM D1298
Density 7.39 lbs/galBy conversion
Flash Point 247C ASTM D92
Oxidative Stability >1500 hrs ASTM D943 Dry
PDSC, 180C 38 minutes ASTM D6186-98
Biodegradability >95 % CEC L33-A-94
Biodegradability >80 % ASTM D5864-95
Additional preferred TAG base oils include a high oleic sunflower oil
available
as SUNYL 80T"" and a high oleic rapeseed oil available as RS-80T"~, both from
SVO
1 S ENTERPRISES (Eastlake, Ohio). Other high oleic oils include high oleic
sunflower oils
available from DOW, DUPONT, or Instituto de la Grasa, high oleic canola oils
from
CARGILL or DUPONT, high oleic soybean oils from DUPONT or MONSANTO, high
oleic corn oils from DUPONT, and high oleic peanut oils from MYCOGEN or the
University of Florida.
Non-genetically modified vegetable oils are sunflower oil, safflower oil, corn
oil,
soybean oil, rapeseed oil, meadowfoam oil, lesquerella oil, castor oil or
olive oil. It is to
be noted that olive oil is naturally high in oleic acid. The oleic acid
content of olive oil
typically ranges from about 65 to about 85 percent.
Any vegetable oil can be transesterified by the addition of a saturated ester,
preferably a short chain fatty acid or a polyol ester. This addition results
in random
esterification of the short chain fatty acids to the glycerol backbone of the
vegetable oil.
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In general, transesterification can be performed by adding a short chain fatty
acid ester to
a vegetable oil in the presence of a suitable catalyst and heating the
mixture. Esters of
short chain fatty acids include methyl esters and polyol esters. Methyl esters
can be
produced, for example, by esterification of fatty acids.
Polyol esters also can be used in the transesterification of vegetable oils.
As used
herein, "polyol esters" refers to esters produced from polyols containing from
two to
about 10 carbon atoms and from two to six hydroxyl groups. Preferably, the
polyols
contain two to four hydroxyl moieties.
Transesterification of a polyol ester with a vegetable oil results in the
short fatty
acid chains of the polyol and the long fatty acid chains of the TAG being
randomly
distributed among both the polyol and glycerol backbones. In one embodiment,
transesterified vegetable contain TAGs having a structure as defined above,
and/or a
non-glycerol polyol ester having the following structure:
O
OC-R4
O
~ I \OCI - Rs
R~
wherein R4 and Rs are independently aliphatic hydrocarbyl groups having from
about 4 to about 24 carbon atoms inclusive, wherein at least one of R4 and Rs
have a
saturated aliphatic hydrocarbyl moiety having about 4 to about 10 carbon atoms
inclusive, and wherein at least one of R4 and Rs have an aliphatic hydrocarbyl
moiety
having from about 12 to about 24 carbon atoms inclusive. These triglycerides
are
available from a variety of plants or their seeds and are commonly referred to
as
vegetable oils. R6 and R~ are independently a hydrogen, an aliphatic
hydrocarbyl moiety
having one to four carbon atoms, or the following formula:
O
I I
(CH2)x - O C - R8
wherein X is an integer of about 0 to about 6, and wherein R8 is an aliphatic
hydrocarbyl moiety having four to 24 carbon atoms.
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Methods to produce the above transesterified vegetable oils are disclosed in
U.
S. Patent No. 6,278,006, which is incorporated in its entirety herein. Other
triaglycerol
oils that may be used are disclosed in U. S. Patent Nos. 5,990,055 and
6,281,375, which
are incorporated by reference in their entirety. The transesterified vegetable
oil may
include the glycerol polyol ester (shown above) alone or the non-glycerol
polyol ester
(shown above) alone, or a mixture of both.
Vegetable oils tend to crystallize at low temperature because the triacyl
structures
tend to be quite regular and subject to packing. This causes the viscosity to
abruptly
increase at lower temperatures, resulting in the failure of gelation index
tests. To meet
the gelation index requirement of less than about 12 as specified by the GF-
3/API SL
bench test specification, a low gelation index saturated synthetic ester
(which is different
from the vegetable oil) is added. For example, from about 10 to about 30% of a
saturated synthetic ester was blended in the formulation. It was discovered
that the
synthetic ester, particularly saturated esters, lowered the gelation index
significantly.
1 S The synthetic ester may be a dibasic ester such as adipate, a sebacate
ester, a tribasic
ester such as trimethylol ethane (TME), a trimethylol propane (TMP) ester, or
a polyol
ester, such as pentaerythritol ester. Preferably, the gelation index of the
first ester added
to the transesterified triglyceride oil should be less than about 10, less
than about 8, or
less than about 6. In some embodiments, the first ester used to lower the
gelation index
of the lubricant has a gelation index of less than about 5, such as about 4 or
less, about 3
or less, about 2 or less, or about 1 or less.
Dibasic or dibasic acid esters are the products from a C4-C12 dicarboxylic
acid
(such as succinic, glutaric acid, adipic acid, and sebacic acid) reacting with
2 moles of
C1-Ci2 alcohols. One example is di(2-ethylhexyl)adipate. The dibasic ester
should have
a viscosity index of at least about 120 in order to function adequately.
Dibasic esters are
of the formula:
O O
II II
R1 O - C - (CH2)~ - C O R2
wherein R1 and RZ are a hydrocarbyl group having from about 1 to about 20
carbon
atoms and n is an integer from about 1 to about 20. A preferred dibasic ester
is
EMKAR.ATE 1130TM which is the diester of a C,o alcohol with sebacic acid by
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13
UNIQEMA PERFORMANCE CHEMICALS (New Castle, DE). Rt and RZ may be
different moieties or the same moieties.
Dibasic esters having similar characteristics as those in the following talbe
are
also useful:
Property Value
Flash Point, C 230 (closed
cup)
260 o en cu
Auto I ition Tem erature, 385
C
Densi , /ml 0.909
Pour Point, C -60
Kinematic Viscosity, 20.2 @ 40 C
cSt
4.8 100 C
Tribasic esters are the products from a C4-C~2 tricarboxylic acid reacting
with 3
moles of C1-CZO alcohols or made by a fatty acid condensing with a polyol (tri-
ol). The
tribasic ester should have a viscosity index of at least about 120 in order to
function
adequately. Tribasic esters are of the formula:
O
II
CH20-C- Rz
O
I I
R~ - C - CH2- OC R3
t O
I I
CH2 - OC R4
wherein Rl, R2, R3 and R4 are a hydrocarbyl group having from about 1 to about
20
carbon atoms. A preferred tribasic ester is EMKARATE 1550TM made by UNIQEMA
PERFORMANCE CHEMICALS (New Castle, DE). R1, R2, R3 and R4 may be
different moieties or the same moieties.
Other synthetic esters have the following formula:
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14
O
I I
CH2-O-C- R~
I O
I I
R4-C -CH2-OC-R2
I O
I I
CH2-OC-R3
wherein Rl, R2, R3, and R4 are a hydrocarbyl group having from about 1 to
about
carbon atoms. When R4 is CH3, the resulting synthetic ester is a trimethylol
ethane
ester. When R4 is CH3CHz, the resulting synthetic ester is a trimethylol
propane ester.
Other suitable synthetic esters include EMK.ARATE 1700TM which is a
pentaerythritol
ester of a CS-C~ alcohol, PRIOLUBE 3960TM, PRIOLUBE 3939TM, PRIOLUBE 1831TM
15 which are polymers made from a dimer acid with a di-alcohol by UNIQEMA
PERFORMANCE CHEMICALS (New Castle, DE.) Rl, R2, R3 and R4 may be different
moieties or the same moieties.
To increase the viscosity at higher temperatures, viscosity index improvers
were
added to the formulation. Generally speaking, there are two types of viscosity
modifier
20 (or viscosity index improver). One is the relative polar ester-type, such
as LUBRIZOL
7671TM, which is a long chain ester of malefic anhydride styrene copolymer
(see also,
LUBRIZOL 7764TM and LUBRIZOL 7783TM which are polymethacrylate copolymers).
The other is the non-polar hydrogenated olefin copolymer (OCP) type, such as
LUBRIZOL 7075TM, (also included are hydrogenated styrene-dime copolymers, such
as
INFINEUM SV 200TM and INFINEUM SV 150TM, etc.) which are amorphous
hydrocarbon polymers. Both of these viscosity modifiers were tested in the
formulations.
By combining polar and non-polar types of viscosity modifiers, a wide range of
viscosity grades of motor oils can be blended. Further, when blended with the
synthetic
esters, a motor oil is produced meeting the desired viscosity, gelation index
specifications, and other specifications needed to make a renewable,
environmentally
friendly engine lubricant.
A preferred polar ester-type viscosity modifier is LUBRIZOLT"' 7671 made by
LUBRIZOL (Wickliffe, OH). LUBRIZOLT"" 7671 is a polymethacrylate type
thickener
and also acts as a pour point depressant for vegetable oils. Other polar ester-
type
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viscosity modifiers include LUBRIZOLT"" 7764, LUBRIZOLT"" 7776, LUBRIZOLT""
7785, LUBRIZOLT"" 7786, from LUBRIZOL (Wickliffe, OH) which are
polymethacrylate copolymer viscosity index improvers.
Polar ester-type viscosity modifiers having similar properties as those in the
5 following table are also useful:
Pro a Value
Flash Point, 165
C
S ecific 0.90
Gravi
Viscosity, 8500 @ 40
cSt C
1500 100
C
A preferred non-polar hydrogenated olefin copolymer-type viscosity modifier is
the LUBRIZOL 7075TM Series made by LUBRIZOL (Wickliffe, OH). This series is
Lubrizol's next generation nondispersant olefin copolymer (OCP) viscosity
modifier.
Hydrogenated olefin copolymers are the most widely used type of viscosity
modifier for
10 passenger car motor oils and heavy-duty diesel engine oils. Developed in
the mid-1960s,
hydrogenated olefin copolymers differ mainly in molecular weight and the ratio
of
ethylene to propylene. These polymers effectively minimize viscosity
variations over
typical engine operating temperatures. They are cost-effective and are
suitable for
formulating nearly any mainline engine oil. The polymers provide a cost-
effective way
15 to meet the latest international and original equipment manufacturer (OEM)
specifications for passenger car and heavy-duty diesel engine oils.
Non-polar hydrogenated olefin copolymer-type viscosity modifiers having the
following characteristics may also be useful in embodiments:
Pro a Value
Flash Point, 190
C
S ecific 0.87
Gravi
Viscosi 825 100 C
, cSt
LUBRIZOL 7075DTM is a preferred olefin copolymer type viscosity modifier
from LUBRIZOL (Wickliffe, OH). Other olefin copolymer type viscosity modifiers
include the LUBRIZOL 7070TM series, 7077TM series, 7740TM series; INFINEUM
SV I4OTM, SV 14STM, SV2OOTM, SV2OSTM, SV3OOTM, SV3OSTM, (EXXONMOBIL, TX)
and PARATONETM 8900 series by (CHEVRON,CA).
The ester type viscosity modifiers contribute to the lowering of the gelation
index. Using LUBRIZOLT"" 7764 and LUBRIZOLT"" 7785, the maximum amount of
ester viscosity modifiers allowable in the formulation without failing the
gelation index
specification is from about 1.7 to about 2.0%, see Fig. 1. At this low
concentration of
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16
the ester type viscosity modifier alone, the viscosity grade of the formulated
oil is a SAE
30 grade or lower.
Ester type viscosity modifiers having the following characteristics may also
be
useful in embodiments:
Pro a Value
Flash Point, 161
C
S ecific 0.90
Gravi
Viscosity, 20.5 @ 100
cSt C
S The solubility of the hydrogenated olefin copolymer-type viscosity modifier
in
vegetable oil is about 4 to about 6 wt% due to the polarity difference. When
using the
hydrogenated olefin copolymer-type viscosity modifier alone, the formulation
of the
lubricant is a viscosity grade SAE 30 grade oil.
However, a combination of these two types of viscosity modifiers produces a
wide range of viscosity grades of motor oils. Further, when combined with the
vegetable
oil and the synthetic ester, a motor oil was produced meeting the desired
viscosity,
gelation index specifications, and other bench test specifications. The ester
type viscosity
index improver may be added in an amount from about 0 to about 3.0%, more
preferred
from about 0.2 to about 2.5%, most preferred from about 0.5 to about 2% and
the
hydrogenated olefin copolymer type viscosity index improver may be added in an
amount from about 0 to about 6.0%, more preferred from about 1 to about 5%,
most
preferred from about 2 to about 4%.
Other suitable conventional viscosity index improvers, or viscosity modifiers,
are
olefin polymers, such as polybutene, hydrogenated polymers and copolymers and
terpolymers of styrene with isoprene and/or butadiene, polymers of alkyl
acrylates or
alkyl methacrylates, copolymers of alkyl methacrylates with N-vinyl
pyrrolidone or
dimethylaminoalkyl methacrylate. These are used as required to provide the
viscosity
range desired in the finished oil, in accordance with known formulating
techniques.
Esters obtained by co-polymerizing styrene and malefic anhydride in the
presence
of a free radical initiator and thereafter esterifying the copolymer with a
mixture of C4-
C,8 alcohols, are also useful as viscosity modifying additives. The styrene
esters
generally are considered to be multi-functional premium viscosity modifiers.
The styrene
esters in addition to their viscosity-modifying properties also are pour point
depressants
and exhibit dispersancy properties when the esterification is terminated
before its
completion leaving some unreacted anhydride or carboxylic acid groups. These
acid
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17
groups can then be converted to amides by reaction with a primary amine. The
co-
polymerization of styrene with malefic anhydride creates a copolymer (SMA)
which has a
higher glass transition temperature than polystyrene and is chemically
reactive with
certain functional groups. Thus, SMA polymers are often used in blends or
composites
where interaction or reaction of the malefic anhydride provides for desirable
interfacial
effects. Some SMA polymers that are commercially available from ROHMAX USA
(Horsham, PA) include VISCOPLEXT"~ 2-360, VISCOPLEXT"" 2-500, VISCOPLEXT"" 3-
540, VISCOPLEXTM 4-671, and VISCOPLEXT"" 6-054.
One difference between mineral oil and vegetable oil is that the former is
predominantly non-polar hydrocarbons whereas the latter has polar ester
functional
groups. There is lack of dispersant/inhibitor (DI) packages formulated
specially for use
with the more polar vegetable oils. Therefore, conventional DI packages were
used in
embodiments of the formulation. In order to solubilize conventional DI
packages in
vegetable oil, about 10 to about 30% of API Group I to Group III mineral oils
or Group
IV poly-a-olefin (PAO) synthetic oils are blended with the vegetable oil to
lower the
polarity. The resulting oils are clear and homogeneous.
A dispersant/inhibitor additive package may be added to the lubricant to break
insoluble particles already formed and to inhibit the formation of particles.
Particles are
kept finely divided so that they can remain dispersed or colloidally suspended
in the oil.
The dispersant/inhibitor additive package is preferably in an amount from
about 6 to
about 18 wt%, more preferred from about 8 to about 16 wt%, and most preferred
from
about 10 to about 14 wt%.
Detergents and dispersants are polar materials that serve a cleaning function.
Detergents include metal sulfonates, metal salicylates and metal
thiophosphonates.
Dispersants include polyamine succinimides, hydroxy benzyl polyamines,
polyamine
succinamides, polyhydroxy succinic esters and polyamine amide imidazolines.
Detergents are generally combined with dispersant additives in crankcase oils.
Detergents chemically neutralize acidic contaminants in the oil before they
become
insoluble and fall out of the oil, forming a sludge. Neutral or basic
compounds are
created which can remain in suspension in the oil. Lubricating oils typically
contain
from about 2 to about 5 wt% of detergent.
Suitable ashless dispersants may include, but are not limited to, polyalkenyl
or
borated polyalkenyl succinimide where the alkenyl group is derived from a C3 -
C4 olefin,
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18
especially polyisobutenyl having a number average molecular weight of about
7,000 to
50,000. Other well known dispersants include the oil soluble polyol esters of
hydrocarbon substituted succinic anhydride, e.g. polyisobutenyl succinic
anhydride, and
the oil soluble oxazoline and lactone oxazoline dispersants derived from
hydrocarbon
S substituted succinic anhydride and di-substituted amino alcohols, post-
grafted polymers
of ethylenepropylene with an active monomer such as malefic anhydride which
may be
further reacted with alcohol or an alkylene polyamine, styrene-malefic
anhydride
polymers post-reacted with alcohols and amines and the like.
Dispersants typically contain a hydrocarbon chain attached to an amine or
alcohol-containing polar group. The hydrocarbon "tail" serves to solubilize
the molecule
in the lubricant base stock, while the polar group serves to attract the polar
contaminants
resulting from the lubricant breakdown. The dispersant forms millions of
micellar
structures in the lubricant base stock which contain a highly polar core and
disperse
enormous amounts of polar contaminants. These contaminants are products of
oxidation
which serve as precursors to varnish/carbon/sludge formation as well as
already-formed
varnish/carbon/sludge deposits. The dispersed contaminants are held in
"solution" in the
basestock while already-formed deposits are cleaned off the metal and
elastomer
surfaces. Both the suspended precursors and deposits readily pass through
commonly
used filters. Ultimately, when these cores are saturated, the dispersant can
no longer pick
up contaminants, so the oil must be drained. However, the oil is usually
drained well
before this happens.
Lubricant oxidation is a chain reaction caused by the reaction of the oxygen
in air
with the lubricant base stock. Oxidation results in the formation of high
molecular
weight oil-insoluble polymers. These can settle out as sludges, varnishes and
gums.
They also cause an increase in the viscosity of the lubricant. The function of
the
inhibitors is the prevention of the deterioration from the oxygen attack on
the lubricant.
The oxidation inhibitors function either to destroy free radicals (phenolics
or amines) or
to decompose the peroxides (amines or ZDDPs) which are involved in the
oxidation
mechanism. As a result, the lubricant retains its cleanliness and viscosity
allowing it to
function properly over its drain interval.
A preferred dispersant/inhibitor additive package is LUBRIZOL 9850UT"" from
LUBRIZOL (Wickliffe, OH), or LUBRIZOL 9850T"". The contents of DI packages are
generally a proprietary secret, but usually contain an antiwear agent, such as
ZDDP
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(Zinc dialkyl dithiophosphate); an antioxidant- phenolic and/or amine type
antioxidant; a
detergent (Mg and/or Ca sulfonate or phenate); a dispersant (polyisobutylene
succinamide); a corrosion inhibitor; a rust inhibitor, a friction modifier; an
anti-foaming
agent, etc. Other suitable dispersant/inhibitor additive packages for gasoline
and diesel
engine oils are ORONITET"' (CHEVRON, CA) and INFINEUMT"" (EXXON-MOBIL,
TX). GF-3 DI packages include, for example, OLOA 55007TM and OLOA 59029TM
(CHEVRON, CA), INFINEUM 5063T"", INFINEUM 3421TM, INFINEUM 3422TM
(EXXON-MOBIL, TX), and LUBRIZOL 20,000T-- and LUBRIZOL 20,OOOAT""
(LUBRIZOL, OH).
Dispersant/inhibitor additive packages having similar characteristics as those
listed below are also be useful:
Pro erty Value
Flash Point, 146-167
C
S ecific 0.96 - 0.97
Gravi
Viscosity, 1350-1400 @
cSt 40 C
100-125 100
C
The environmentally friendly lubricant may further include one or more
additives. Such additives include, but are not limited to antioxidants, pour
point
depressants, detergents, dispersants, friction modifiers, rust inhibitors,
corrosion
inhibitors and anti-foaming agents.
Typical antioxidants are aromatic amines, phenols, compounds containing sulfur
or selenium, dithiophosphates, sulfurized polyalkenes, and tocopherols.
Hindered
phenols are particularly useful, and include for example, 2,6-di-tert-butyl-p-
cresol
(DBPC), tert-butyl hydroquinone (TBHQ), cyclohexylphenol, and p-phenylphenol.
Example of amine-type antioxidants include phenyl-a-napthylamine, alkylated
diphenylamines and unsymmetrical diphenylhydrazine. Zinc dithiophosphates,
metal
dithiocarbamates, phenol sulfides, metal phenol sulfides, metal salicylates,
phospho-
sulfurized fats and olefins, sulfurized olefins, sulfurized fats and fat
derivatives,
sulfurized paraffins, sulfurized carboxylic acids, disalieylal-1,2,-propane
diamine, 2,4-
bis (alkyldithio)-1,3,4-thiadiazoles) and dilauryl selenide are examples of
useful
antioxidants. IRGANOX L-64 (Ciba Specialty Chemicals, Tarrytown, NY) provides
a
mixture of antioxidants that is particularly useful. Antioxidants are
typically present in
amounts from about 0.001 to about 10 weight %. In preferred embodiments, from
about
0.01% to about 3.0% of an antioxidant is added to the lubricant. U. S. Patent
Nos.
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5451334 and 5773391 further disclose additional antioxidants and are hereby
incorporated in their entirety by reference.
Pour point depressants (PPD) lower the pour point of petroleum products
containing wax by reducing the tendency of the wax to collect into a solid
mass. Pour
5 point depressants permit flow of the oil formulation below the pour point of
the
unmodified lubricant. Common pour point depressants include polymethacrylates,
wax
alkylated naphthalene polymers, wax alkylated phenol polymers and chlorinated
polymers. U. S. Patent Nos. 5451334 and 5413725 further disclose additional
pour point
depressants and are hereby incorporated in their entirety by reference.
10 Pour point depressants are used generally in amounts of from about 0.01 to
about
5 wt%, more typically from about 0.1 to about 1 wt%. Illustrative of pour
point
depressants which are normally used in lubricating oil compositions are
polymers and
copolymers of n-alkyl methacrylate and n-alkyl acrylates, copolymers of di-n-
alkyl
fumarate and vinyl acetate, alpha-olefin copolymers, alkylated naphthalenes,
copolymers
15 or terpolymers of alpha-olefins and styrene and/or alkyl styrene, styrene
dialkyl malefic
copolymers and the like. A preferred pour point depressant is ACRYLOID 3004
Oil
Additive available by ROHMAX USA (Horsham, PA) that uses the commercial name
VISCOPLEX 1-3004T"". The chemistry is based on polymethacrylate (PMA). Other
VISCOPLEX series 1 wax modifiers that can be used include VISCOPLEX 1-6004,
20 VISCOPLEX 1-331, and VISCOPLEX 1-600. The VISCOPLEX series 10, such as
VISCOPLEX 10-130, and 10-171 can also be used.
Suitable metal detergent additives are known in the art and may include one or
more of overbased oil-soluble calcium, magnesium and barium phenates,
sulfurized
phenates, and sulfonates (especially the sulfonates of C~6 -Cso alkyl
substituted benzene
or toluene sulfonic acids which have a total base number of about 80 to 300).
These
overbased materials may be used as the sole metal detergent additive or in
combination
with the same additives in the. neutral form; but the overall metal detergent
additive
should have a basicity as represented by the foregoing total base number.
Preferably
they are present in amounts of from about 3 to about 6 wt% with a mixture of
overbased
magnesium sulfurized phenate and neutral calcium sulfurized phenate (obtained
from C9
or C12 alkyl phenols).
Suitable anti-wear additives are oil-soluble zinc
dihydrocarbyldithiophosphates
with a total of at least S carbon atoms and are typically used in amounts from
about 1 to
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21
about 6 wt% by weight. Other anti-wear additives include dithiophosphates and
in
particular, zinc dialkyl dithiophosphates, metal sulfonates, metal phenate
sulfides, fatty
acids, acid phosphate esters and alkyl succinic acids. Anti-wear additives
adsorb on
metal, and provide a film that reduces metal-to-metal contact. In general,
anti-wear
additives include zinc dialkyldithiophosphates, tricresyl phosphate, didodecyl
phosphite,
sulfurized sperm oil, sulfurized terpenes and zinc dialkyldithiocarbamate.
Rust inhibitors protect surfaces against rust and include alkylsuccinic type
organic acids and derivatives thereof, alkylthioacetic acids and derivatives
thereof,
organic amines, organic phosphates, polyhydric alcohols, and sodium and
calcium
sulphonates. Rust inhibitors are employed in very small proportions such as
from about
0.1 to about 1 wt% with suitable rust inhibitors being exemplified by C9 -C3o
aliphatic
succinic acids or anhydrides such as dodecenyl succinic anhydride.
Anti-foam additives reduce or prevent the formation of a stable surface foam
and
are typically present in amounts from about 0.01 to about 1 wt%.
Polymethylsiloxanes,
1 S polymethacrylates, salts of alkylene dithiophosphates, amyl acrylate
telomer and poly(2
ethylhexylacrylate-co-ethyl acrylate) are non-limiting examples of anti-foam
additives.
Additionally, by mixing high and low viscosity mineral oils in the
formulation, it
was possible to prepare a full range of SAE grade motor oils. Viscosity of an
automotive
oil is classified in SAE (Society of Automotive Engineers) viscosity grades
represented
by numbers such as 30, 40, 50. The higher the number, the thicker the oil and
the greater
it's effectiveness in high temperature operations. Lower numbered oils that
are thinner
oils with low viscosity are used in cold climates as they flow more easily and
are
identified by a "W" mark next to the grade of oil on the package. Multigrade
oils SWxx,
lOWxx, 20Wxx, etc. are suitable for both low and high temperature conditions.
Lubricating oils made specifically for industrial use have their viscosity
classified by
ISO (international Organization for Standardization) grades.
To prepare a wide range of SAE grade motor oils, high and low viscosity
mineral
oils are added to the environmentally friendly lubricant. The SAE grade motor
oils that
can be achieved include OW-30, SW-30, 10W-30, and 10W-40. Mineral oils from
Group I to Group V are preferred. Preferred examples useful in the formulation
include:
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Tahle 4: Mineral Oils
Group Example Kin. Visc. 40C Kin. Visc. 100C VI
cSt cSt
II EXCEL 100-HCT""20.85 4.2 101
II EXCEL 230-HCT""42.5 6.4 100
II EXCEL 575-HCT""111 12.3 100
III Yubase 150NT"' 37.9 6.6 129
III Yubase 240NT"" 47.4 7.7 129
III CHEVRON UCB07RT""28.2 6.8 137
III SHELL XHVIT"" 47.3 8.2 ~ 148
EXCEL 100-HCT"", 230-HCT"", and 575-HCT"" are Group II mineral oils made by
PENNZOIL-QUAKER STATE COMPANY (Houston, TX). Yubase 150NT"" and 240NT"~
are Group III mineral oils made by Yukong (Seoul, Korea). CHEVRON UCB07RT"~ is
a
Group III mineral oil made by CHEVRON. SHELL XHVI T~~ is a Group III mineral
oil
made by Shell Chemical Company. Mineral oils are used generally in amounts of
from
about 0 to about 40 wt%.
The following examples exemplify embodiments of the invention. They do not
limit the invention as otherwise described and claimed herein. All numbers in
the
examples are approximate values.
EXAMPLE 1
Table 5A and Table 5B provide the formulations and physical properties of
lubricants using polar ester-type viscosity modifiers. Formulations A to C
used
LUBRIZOL 7764T"", which is a polymethacrylate copolymer, and formulations D to
F
used LUBRIZOL 7785T"~ which is a polymethacrylate copolymer dispersed in
vegetable
oil. The dispersant/inhibitor package was LUBRIZOL 9850UT"'. The pour point
depressant was Viscoplex 1-3004T"~. The mineral oil was Yubase 150NT"~ and the
synthetic ester was Emkarate 1130T"". The vegetable oil was AGRI-PURE 560T"".
Table 5A: Formulations A-F
Formulation A B C D E F
Component Description Wt Wt Wt Wt Wt Wt
% % % % %
Lubrizo17764T"'VII 1 1.5 2 0 0 0
Lubrizo17785T""VII 0 0 0 1 2 3
Lubrizo19850UT"'DI 12 12 12 12 12 12
Visco lex PPD 0.1 0.1 0.1 0.1 0.1 0.1
1-3004T""
Yubase 150NT""Group III 25 25 25 25 25 25
oil
Emkarate Dibase ester 20 20 20 20 20 20
1130T""
AGRI-PURE Modified vegetablebalancebalancebalancebalancebalancebalance
560T"" oil
Total wt% 100 100 100 100 100 100
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23
Table SB: Properties of Formulations A-F
Physical Properties A B C D E F
KV @ 100C, 8.79.32 10.028.79 10.2511.36
cSt
KV @ 40C, cSt 43 46.3 49.5 43.4 50.864.7
VI 187190 195 I 1_95171
87
Gelation Index 5.78.2 10.5 10 20.925.7
The gelation index (Gi) for formulations including LUBRIZOL 7764T"" and
LUBRIZOL 7785TM were plotted against the weight percent of viscosity modifier
(VII)
as shown in Figure 1. This graph indicates that when the amount of viscosity
modifier
was higher than about 2.2 wt % and about 1.2 wt % of LUBRIZOL 7764T"" and
LUBRIZOL 7785T"', respectively, formulations failed the GF-3/API SL
specification of
the gelation index maximum of 12. When using less than 2.2 wt % of LUBRIZOL
7785T"" the formulations passed the gelation index, but the finished oils were
limited to
the SAE 30 viscosity grade. Similarly, using lower than 1.2 wt % of LUBRIZOL
7764T~"
gave formulations that passed the gelation index of 12, but the finished oils
were limited
to the SAE 20 viscosity grade.
EXAMPLE 2
The following formulations in Table 6A were prepared using an olefin copolymer
type viscosity modifier, LUBRIZOL 7075DT"~ in place of the polar-ester type
viscosity
modifier used above. The physical properties of these formulations are
provided in Table
6B. The formulations were clear and homogeneous at ambient temperature.
However,
when attempting to measure the gelation index in formulations G and H
according to the
ASTM D 5133 procedure, the viscosity modifier was found to separate and stick
to the
wall of the test cell during the chilling process, whereas formulation I
stayed clear and
homogeneous. This suggested that the formulation using the olefin copolymer
type
viscosity modifier, LUBRIZOL 7075DT"", may be limited to about 0 to about 6 wt
% in
the formulation.
Table 6A: Formulations G-I
Formulation G H I
Components Description Wt% Wt% Wt%
Lubrizo17075DT"'VII 6.3 7.98 3.94
Lubrizo19850UT""DI 12 12 12
Visco lex 1-3004T""PPD 0.1 0.1 0.1
Excel 100-HCT"" Group II oil 0 25 0
Excel 230-HCT"" Group II oil 25 0 0
Excel 575-HCT"" Group II oil 0 0 25
Emkarate 1130T""Dibase ester 20 20 20
AGRI-PURE 560T""Modified vegetablebalance balance balance
oil
Total wt% 100 100 100
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24
TahlP 6R~_ Prnnerties of Formulations C~-1
Ph sical Pro erties G H I
KV 100C, CST 10.3 10.3 10.3
KV @ 40C, CST 54.6 51.9 55.9
VI 179 192 174
CCS @ -25C 2390 1830 3270
CCS @ -30C N/A 1027 6060
MRV TP-1 @ -35C 9100 6600 14100
MRV YS @ -35C 0 0 0
Scanning Brookfield Temp.
@30,000 cp. N/A N/A -31.9C
@ 40,000 cp. N/A N/A -34C
Gelation Index N/A N/A 6
Gelation Temp., C N/A N/A -12
Formulation I is an SAE 30 grade lubricant. It is possible to raise the
viscosity of
Formulation I to SAE 40 grade by increasing the non-biodegradable heavy oil,
such as
S Excel 575-HC, which would decrease the biodegradability of the formulation.
EXAMPLE 3
Table 7A represents blends using a combination of the ester-type and the
olefin
copolymer type viscosity modifiers in a base oil comprising Group III mineral
oils
(Yubase 150NT"" and Yubase 240NT""), a dibasic ester, and modified vegetable
oil
(AGRI-PURE 560T""). Table 7B discloses the physical properties of the oils in
Table 7A.
These formulations pass the GF-3/API SL gelation index specification of less
than about
12 and meet other physical properties of a SAE SW-30 grade oil.
Table 7A: Formulations J-L
Formulation J K L
Component Description wt % wt % wt
Lubrizo17785T""VII 1 0 0
Lubrizo17764T""VII 0 1.7 1.7
Lubrizo17075DT"'VII 3.28 1.89 1.4
Lubrizo19850UT""DI 12 12 12
Visco lex I-3004T""PPD 0.1 0.1 0.1
Yubase 150NT""Group III Oil 25 25 0
Yubase 240NT"'Group III Oil 0 0 25
Emkarate 1130T""Dibase Ester 20 20 20
AGRI-PURE 560T"'Vegetable Oil balance balance balance
Total wt% 100 100 ~ 100
Table 7B: Properties of Formulations J-L
Physical Properties Test Method J K L
KV @ 100C D-445 10.3 10.5 10.53
KV @ 40C D-445 51.8 52.9 53.52
VI D-2270 193 194 191
Pour Point,C D-5950 -47C -47C -45C
CCS @ -30C D-5293 3540
CCS @ -25C D-5293 2050 2090 2230
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Physical Properties Test Method J K L
HTHS Viscosity, cP @ D-4683 3.42 3.37 3.37
150C
MRV TP-1 @ -35C D-4684 9800 10400
MRV YS @ -35C D-4684 0 0
MRV TP-1 @ -30C D-4684 3800 4600 4800
MRV YS @ -30C D-4684 0 0 0
Scanning Brookfield Temp.D-S 133
@30,000 cP -31.5C -33.4C -31.4C
@ 40,000 cP -32.6C -34.1C -32.2C
Gelation Index D-5133 10.4 10.4 10.9
Gelation Temp., C D-5133 -31C -34C -32.2C
NOACK volatility,Wt % D-5800 N/A 7.8 N/A
Loss
off at 700C ( Sim. Dist.)D-2687 N/A S.1 ~N/A
EXAMPLE 4
Formulation K was submitted to independent testing laboratories for ASTM D-
6335 Thermo-Oxidation Engine Oil Simulation Test (TEOST), and ASTM D-5864-95
5 Biodegradability tests were performed at BfB Oil Research in Belgium.
Results are
shown in Table 8. TEOST may be useful in determining the piston deposit
control
capability of the motor oil. According to the GF-3/API SL specification the
total deposit
in TEOST is 45 mg maximum. According to the ASTM D-5964-95 biodegradability
test, if the carbon dioxide released is higher than 60% (within 28 days) , the
material is
10 qualified as easily biodegradable.
Table 8: Formula K
Test Test MethodK
TEOST, Total D-6335 11.6
Deposit mg
Biodegradability D 5864-9562%
EXAMPLE 5
To reduce the cost of the lubricants, Group III mineral oils in Example 3 can
be
1 S replaced by Group II mineral oils, such as Excel HC or Exxon HC (hydro-
conversion)
oils. Table 9A discloses formulations, in which the different viscosity grades
of Group II
oils were used alone or in combination to make wide viscosity ranges of motor
oils.
Table 9B shows the properties of the formulations. To enhance the oxidative
stability,
additional antioxidants (i.e. Irganox L-64T"") can be added to the formulation
as
20 illustrated in the formulation Q . Formulation R replaces the Irganox L-
64T"" with
NAUGALUBE MOLYFM 2543T"~ (Crompton Corporation, Middlebury, CT) which is a
multifunctional friction modifier, anti-wear, and antioxidant additive.
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Table 9A: Formulations M-R
Formulation M N O P Q R
SAE Grade OW-30 5W-30 10W-30IOW-4010W-4010W-30
Components Description wt wt wt wt wt wt
% % % % %
DI, Lz 9850UDI 12 12 12 12 12 12
Viscoplex PPD 0.1 0.1 0.1 0.1 0.1 0.1
I- 3004
Lz 7764 VII 1.7 1.2 1.1 1.7 1.7 0
Lz 7075D VII 3.3 1.5 0 3.3 3.3 3.3
Excel 100-HCGroup II Oil 25 10 0 0 0 25
Excel 575-HCGroup II Oil 0 20 30 30 29.5 0
Irganox L-64Antioxidant 0.5
Emkarate Dibase ester 20 20 20 20 20 20
I 130
Naugalube Friction modifier 0.5
Mol FM 2543 Antioxidant
Cargill AP-560Modified vegetablebalancebalancebalancebalancebalancebalance
oil
Total wt% 100 100 100 100 100 100
~ ~ ~ ~ ~
Table 9B: Properties of Formulations M-R
Physical PropertiesM N O P Q R
SAE Grade OW-30 5W-30 10W-30 10W-4010W-40IOW-30
KV @ 100C 10.03 10.15 10.28 13.42 13.5 9.9
KV @ 40C 49.3 54.8 57.8 77.7 78.8 55.6
VI 196 176 168 177 176 165
Pour Point,C -45 -51 -33 -45 < -50 <-54
CCS @ -30C 3220
CCS @ -25C 2860 4260 3550
CCS @ -20C 2160 2330 2510 2020
HTHS Viscosity,3.27 3.37 3.43 4 4.08 3.4
cP
150C
MRV TP-1 @ 17,600
-40C
MRV YS @ -40C 0
MRV TP-I @ 14,000 17,800
-35C
MRV YS @ -35C 0 0
MRV TP-1 @ 7,600 11,30010,000
-30C
MRV YS @ -30C 0 0 0
Scanning Brookfield
Tem .
@30,000 cP -33.8C -31.7C -33.2C -27.7C-30.5C-28.7C
@ 40,000 cP -35.1C -32.4C -36.5C -29.4C-31.4C-30.4C
Gelation Index9.4 8.4 7.8 7.3 8.4 6.2
Gelation Temp.,-34 -33 -25 -7 -32 -10
C
NOACK volatility,Wt12.8 9.29 6.66 7.2 7.2 8.2
Loss
off at 700C 9.8 4.7 3.1 3.7 6.1 5.1
( Sim.
Dist.
EXAMPLE 6
The formulation Q was submitted to PerkinElmer Automotive Research
Laboratory (San Antonio, TX) for high temperature TEOST MHT-4 Thermo-Oxidation
Engine Oil Simulation test, Homogeneity and Miscibility (H&M) test, Foam
sequence I,
II, and III test, High Temperature Foam test, EOFT (Engine Oil Filterability
test), and
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EOWTT (Engine Oil Filterability/water tolerance test). In the H&M test, the
tested oil
shall remain homogeneous and miscible when mixed with SAE reference oils.
Table 10
discloses the results. According to ASTM D 4485-99b, the oil meets the bench
test of
API SL minimum performance standard.
Table 10: Formula Q
Description of the Test Test MethodTest ResultGF-3 Limit
H&M (Homogeneity & Miscibility)FTM-3470.1non-separationnon-separation
Test
TEOST MHT 4, D 6335M / /
Total Deposit ( Rod + 21.6 mg 45 mg (max)
Filter)
Foam Test GF-3 D 892 / /
Sequence I , foaming/setting 0/0 10 max./0
Sequence II , foaming/setting 0/0 50 max./0
Sequence III, foaming/setting 0/0 10 max./0
High Temperature Foam D 6082 /
Test
Foam Tendency 20 ml 100 ml(max)
Foam Stability 0 ml 0
EOFT (Engine Oil FilterabilityGM 9099P / /
Test),
Flow Reduction 24.82 50 (max)
EOWTT (Engine Oil Filterability/WaterGM 9099P / /
Tolerance Test
with 0.6% water 19.69 50 (max)
with 1.0% water 15.53 50 (max)
with 2.0% water 17.05 SO (max)
with 3.0% water 12.36 50 (max)
Gelation Index D 5133 8.4 12 (max)
EXAMPLE 7
The R formulation was tested by a modified ASTM Sequence VI B Fuel
Economy test in a Ford V-8 4.6 L engine mounted on a dynamometer as follows:
1. The engine was drained of existing oil and a 6-qt. quantity of test oil was
run for 10 minutes with a fresh filter.
2. The engine was allowed to drain and a new oil filter and another 6 quarts
of test oil was installed.
3. The engine was then started and an aging cycle was initiated 10 seconds
later.
1 S 4. The aging cycle was designed to mimic that of the sequence VI B aging
with the following parameters: 1500 rpm, 71.4 ft. lbs. torque (load) for 7320
seconds, 18.9 ft. lbs. torque for 1920 seconds, 71.4 ft. lbs. torque for 100
seconds
(total aging 9340 seconds), 212°F coolant temperature, and 220°F
oil
temperature.
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5. At completion of the aging cycle, the highway cycle was conducted after
exactly 5 minutes of a 600 rpm idle with no load.
6. Following the highway cycle, a metro (city) cycle was initiated after
exactly 5 minutes of a 600 rpm idle with 0 load.
7. Following the metro cycle, the engine was stopped and test oil was
drained and samples were taken at that time. Cooling water temperatures (4000
gallon
engine water tank) were consistent on each day of testing at 83°F.
Vapor pressure, fuel
specific gravity and relative humidity were recorded and entered into the
dynamometer
prior to each day's test sequence.
The Highway cycle consisted of a 300 second cycle programmed as follows:
minimum rpm: 850, maximum rpm 1840, load varied from: 5 to 28 ft. lbs. The
Metro
cycle consisted of a 504 second, low rpm and load cycle programmed as follows:
minimum rpm: 560, maximum rpm: 1320, load varied from: 0 to 40 ft. lbs.
Emissions
readings were taken beginning at the onset of each programmed test cycle and
ran for
the entire duration of each.
The results show that as compared with a reference oil and a commercial 10W-30
oil, the R formulation reduced the emission, especially, the hydrocarbon
exhaust gas as
shown in Table 11.
Tahle 11: Formula R
Metro Hydrocarbon, CO C02 02
ppm % %
Reference Oil 590 0.90 12.91 1.71
Commercia110W30 308 1.20 12.89 1.50
Formula R 162 1.10 13.65 1.52
Highway
Reference Oil 141 1.10 13.22 1.14
Commercia110W30 207 1.00 13.21 1.18
Formula R 93 1.20 13.90 1.16
4-Hour Aging
Reference Oil 117 0.90 13.40 0.94
Commercia110W30 238 0.83 13.28 1.13
Formula R 111 0.86 ~ 14.08~
1.09
EXAMPLE 8
Table 12 represents a range of SAE grade lubricant oils formulated from blends
using a combination of the ester-type and the olefin copolymer type viscosity
modifiers
in a base oil comprising a blend of Group II mineral oils (Excel 100-HCT"" and
Excel
575-HCT""), a dibasic ester, and CARGILL modified vegetable oil, AGRI-PURE
560T"".
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The dispersant/inhibitor additive package was Oloa 55007 and the pour point
depressant
was Viscoplex 1-3004. Table 12 discloses the physical properties of the oils
in Table 12.
These formulations pass API SL gelation index specification of less than about
12 and
meet other physical properties for their appropriate SAE grade.
Table 12A: Formulations S-V
Formulation S T U V
SAE Grade OW-30 5W-30 10W-3010W-40
Components Description wt % wt wt wt
% %
Lz 7764 VII 1.70 1.70 1.00 1.70
Lz 7075F VII 3.50 3.50 2.40 3.80
Excel 100-HC Group II Oil 20.00 15.00 0.00 0.00
Excel 575-HC Group II Oil 0.00 5.00 30.00 29.00
Cargill AP560Modified vegetable45.54 45.54 37.34 36.24
oil
Emkarate 1130Dibase ester 20.00 20.00 20.00 20.00
Oloa 55007 DI 9.16 9.16 9.16 9.16
Viscoplex PPD 0.10 0.10 0.10 0.10
1-3004
Total wt % 100.0% 100.0%100.0%100.0%
Table 12B: Properties of Formulations S-V
Physical Properties S T U V
SAE Grade OW-30 5W-30 10W-30 10W-40
KV 100C , cSt 9.62 10.0 10.9 13.1
KV 40C, cSt 43.3 46.1 61.4 72.9
VI 215.8 211.6 171 181
CCS -35C, cP 5420 6541
CCS -30C, cP 3013 3290 6650 6734
CCS -25C, cP 3530 3650
Scanning Brookfield
Temp.
@30000 cP -34.9C-34.5C -30.5C -30.7C
@40000 cP -36.5C-35.9C -31.7C -31.4C
GELATION INDEX 10.4 9.6 5.8 8.9
GELATION TEMP. -34C -34C -33C -32C
EXAMPLE 9
Table 13 represents a range of SAE grade lubricant oils formulated from blends
using a combination of the ester-type and the olefin copolymer type viscosity
modifiers
in a base oil comprising a blend of Group II mineral oils (Excel 100-HCT"" and
Excel
575-HCT""), a dibasic ester, and modified vegetable oil (AGRI-PURE 560T"").
The
dispersant/inhibitor additive package was Lubrizol 20000 and the pour point
depressant
was Viscoplex 1-3004. Table 13B discloses the physical properties of the oils
in Table
13A.
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Table 13A: Formulations W-Z
Formulation W X Y Z
SAE Grade OW-30 SW-30 10W-3010W-40
Components Description wt wt wt wt
% % %
Lz 7764 VII 2.60 1.40 1.00 1.60
Lz 7075F VII 1.40 1.40 1.00 2.50
Excel 100-HC Group II Oil 25.00 5.00 0.00 0.00
Excel 575-HC Group II Oil 2.00 20.00 30.00 30.00
Cargill AP560Modified vegetable36.90 40.10 35.90 33.80
oil
Emkarate 1130Dibase ester 20.00 20.00 20.00 20.00
Lubrizo120000DI 12.00 12.00 12.00 12.00
Viscoplex PPD 0.10 0.1_0 0.10 0.10
1-3004
Total wt % 100.0%100.0%100.0%100.0%
~ ~
Table 13B: Properties of Formulations W-Z
Physical Properties W X Y Z
SAE Grade OW-30 SW-30 10W-30 10W-40
KV 100C , cSt 11.1 10.9 11.2 13.2
KV 40C, cSt 51.9 58.69 61.7 75.2
VI 212 182 176 179
CCS -35C, cP 5671 10390
CCS -30C, cP 5160 6650 6734
CCS -25C, cP 3530 3650
EXAMPLE 10
5 Table 14 represents a SW-30 SAE grade lubricant oil formulation using a
combination of the ester-type and the olefin copolymer type viscosity
modifiers in a base
oil comprising a blend of Group II mineral oils (Excel 100-HCT"" and Excel 575-
HCT""), a
dibasic ester, and modified vegetable oil (AGRI-PURE 560T""). The
dispersant/inhibitor
additive package was Lubrizol 20000 and the pour point depressant was
Viscoplex 1-
10 3004. To enhance performance, an extra antioxidant was added. This
formulation
passed all API SL bench test requirements. Table 14 also discloses the
physical
properties of the formulation.
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Table 14: Formulation and Physical Properties of Formulation AA
Formulation
SAE Grade SW-30
Components Description wt
Lz 7764 VII 1.30
Lz 7075F VII 1.2
Excel 100-HC Group II Oil 5
Excel 575-HC Group II Oil 19
Cargill AP560 Modified vegetable40.40
oil
Emkarate 1130 Dibase ester 20.0
Lubrizol 20000A DI 12.00
Viscoplex 1-3004 PPD 0.1
Irganox L-64 ' Antioxidant 1.0
Total wt % 100.00%
Physical Properties
Kin. Vis @ 100C 10.94
cSt
@ 40C 59.09
cSt
VI 180
CCS -35C 12160
cP
CCS -30C 6180
cP
TBS@ 150C 3.5
Brookfield Temp
@ 30,000 cP -31.2C
@ 40,000 cP -32C
Gelation Index 8.3
Gelation Temp. -32C
MRV TP-1 @ -35C 15900
cP
MRV YS @ -35C 0
Pour Point ~ ~ ~ -52C
EXAMPLE 11
The formulation AA was submitted to PerkinElmer Automotive Research
Laboratory (San Antonio, TX) for high temperature TEOST MHT-4 Thermo-Oxidation
Engine Oil Simulation test, Homogeneity and Miscibility (H&M) test, Foam
sequence I,
II, and III test, High Temperature Foam test, EOFT (Engine Oil Filterability
test),
EOWTT (Engine Oil Filterability/water tolerance test), Gelation Index, NOACK
Volatility, Volatility Loss, Phosphorous and Ball Rust Test. In the H&M test,
the tested
oil shall remain homogeneous and miscible when mixed with SAE reference oils.
Table
discloses the results. According to ASTM D 4485-99b, the oil meets the bench
test of
the ILSAC GF-3/API SL minimum performance standard and passed all API-SL bench
tests requirements.
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Table 15: Formula AA
Description of the Test Test MethodTest ResultGF-3/API SL
Limit
H&M (Homogeneity & Miscibility)FTM-3470.1non-separationnon-separation
Test
TEOST MHT 4, D 6335M / /
Total Deposit ( Rod + 20.6 mg 45 mg (max)
Filter)
Foam Test GF-3 D 892 / /
Sequence I , foaming/setting 0/0 10 max./0
Sequence II , foaming/setting 5/0 50 max./0
Sequence III, foaming/setting 0/0 10 max./0
High Temperature Foam D 6082 / /
Test
Foam Tendency 20 100 ml(max)
Foam Stability 0 0
EOFT (Engine Oil FilterabilityGM 9099P / /
Test),
Flow Reduction 15.07 50 (max)
EOWTT (Engine Oil Filterability/WaterGM 9099P / /
Tolerance Test
with 0.6% water 22.12 50 (max)
with 1.0% water 12.17 50 (max)
with 2.0% water 13.9 50 (max)
with 3.0% water 15.63 50 (max)
Gelation Index D S 133 12 (max)
8.3
NOACK, Volatility % wt D 972 15 max
loss 7.1 I
Volatility Loss at 371F D 6417 10% max
3.20%
Phosphorous, wt% D 4951 0.1% max
0.093
Ball Rust Test, Average ~D 6557 ~ 100 min
Gray Value 134
The formulation AA was also submitted for ASTM Sequence 111F engine tests.
The Sequence IIIF Test is a fired-engine, dynamometer lubricant test for
evaluating
automotive engine oils for certain high-temperature performance
characteristics,
including oil thickening, sludge and varnish deposition, oil consumption, and
engine
wear. The Sequence IIIF Test utilizes a 1996 model Buick 3800 Series II, water-
cooled,
4-cycle, V-6 engine as the test apparatus. The Sequence IIIF test engine is an
overhead
valve design (OHV) and uses a single camshaft opeating both intake and exhaust
valves
via pushrods and hydrualic valve lifters in a sliding-follower arrangement.
The engine
uses one intake and one exhaust valve per cylinder. Introduction is handled by
a
modified GM port fuel injection system setting the Air-to-Fuel ratio at 15:1.
The test
engine is overhauled prior to each test, during which critical engine
dimensions are
measured and rated or measured parts (pistons, camshaft, valve lifters, etc).
The
Sequence IIIF Test consists of a 10-minute operational check, followed by 80
hours of
engine operaton at moderately high speed, load, and temperature conditions.
Following
each 10-hour segment, and the 10-minute operational check, oil samples are
drawn from
the engine. The kinematic viscosities of the 10-hour segment samples are
compared to
the viscosity of the 10-minute sample to determine the viscosity increase of
the test oil.
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The Sequence IIIF Test is operated at the test states in Table 16 during the
80
hour portion of the test. Table 17 discloses the results. According to ASTM
Sequence
IIIF engine tests, the oil meets the bench test of the ILSAC GF-3/API SL
minimum
performance standard and passed all API-SL bench tests requirements.
S Table 16: Test states of Sequence IIIF testing
Parameter Set Point
Engine Speed 3600 r/min
Engine Load 200 N-m
Oil Filter Block Temperature 155 C
Coolant Outlet Temperature 122 C
Fuel Pressure 365 kPa
Inlet Air Temperature 27 C
Inlet Air Pressure 0.05 kPa
Inlet Air Dew Point 16.1 C
Exhaust Back Pressure 6 kPa
Engine Coolant Flow 160 L/min
Breather Tube Coolant Flow 10 L/min
Engine Oil Cooler Flow 12 L/min
Air-to-Fuel Ratio 15.0 : 1
Breather Tube Coolant Outlet 40 C
Temperature
Table 17: Formula AA
Description of the Test Test Result GF-3/API SL
Limit
Viscosity Increase (KV 40C) 156.10 % 275 % max
Weighted Piston Skirt Vanish9.59 9.0 min
Rating
Weighted Piston Deposit Rating6.19 4.0 min
Hot Struck Piston Rings 0 None Allowed
Cam plus Lifter Wear, Average,16.7 20 max
pm
Oil Consumption L 1.83 5.2 max
Number of Cold Struck Rings 0 N.R.
Average Oil Ring Plugging, 0 N.R.
%
EXAMPLE 12
To reduce the cost of the lubricants, a less expensive dibase ester, Esterex
A41,
was used. Table 18 discloses a prototype formulation for an SW-30 SAE grade.
Other
grades are also easy to formulate with the less expensive dibase ester. Other
less
expensive dibase esters include Esterex NP 451 and NP 471. Table 18 further
shows the
properties of the formulation.
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Table 18: Formulation and Physical Properties of Formulation AB
Formulation AB
SAE Grade SW-30
Components Description wt
Lz 7764 VII 1.30
Lz 7075F VII 1.3
Excel 575-HC Group II Oil 25
Cargill AP560 Modified vegetable40.30
oil
Esterex A41 Dibase ester 20.0
Lubrizol 20000 DI 12.00
Viscoplex 1-3004 PPD 0.1
Total wt % 100.00%
Physical Properties
Kin. Vis @ 100C 10.5
cSt
@ 40C 56.1cSt
VI 179
CCS -35C 5210
CCS -30C 10270
TBS@ 150C 3.32
Brookfield Temp
@ 30,000 cP -30.3C
@ 40,000 cP -31.4C
Gelation Index 8.1
Gelation Temp. -32C
MRV TP-1 @ -35C 15000
cP
MRV YS @ -35C 0
Pour Point <-50C
NOACK, wt% loss
As demonstrated above, embodiments of the invention provide an
environmentally friendly lubricant that meets API SL bench test
specifications, and is
overall at least 60% biodegradable in ASTM D-5864-95 biodegradability testing.
Additional characteristics and advantages provided by embodiments of the
invention are
apparent to those skilled in the art.
While the invention has been described with respect to a limited number of
embodiments, the specific features of one embodiment should not be attributed
to other
embodiments of the invention. No single embodiment is representative of all
aspects of
the inventions. In some embodiments, the compositions may include numerous
compounds and/or characteristics not mentioned herein. In other embodiments,
the
compositions do not include, or are substantially free of, one or more
compounds and/or
characteristics not enumerated herein. Variations and modifications from the
described
embodiments exist. For example, the environmentally friendly lubricant need
not be a
mixture within the compositions given above. It can comprise any amount of
components, so long as the properties desired in the environmentally friendly
lubricant
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are met. It should be noted that the application of the environmentally
friendly lubricant
composition is not limited to lubricants for automobiles; it can be used in
any
environment which requires an environmentally friendly lubricant, such as a
trucks, vans
or buses. It is noted that the methods for making and using the
environmentally friendly
5 lubricant composition are described with reference to a number of steps.
These steps can
be practiced in any sequence. One or more steps may be omitted or combined but
still
achieve substantially the same results. The appended claims intend to cover
all such
variations and modifications as falling within the scope of the invention.
What is claimed is:
