Note: Descriptions are shown in the official language in which they were submitted.
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TITLE
CONTROLLED RELEASE OF ADDITIVE GEL(S)
FOR FUNCTIONAL FLUIDS
Field of the Invention
The present invention relates to a delivery system for providing one or more
functional fluids with desired additives. The invention further relates to the
systems
use in lubricant technology.
Sackground of the Invention
Modem mechanical equipment such as a transmission, hydraulic, engine or
gear all require a functional fluid to possess a number of different
properties. These
properties allow the equipment to operate in a range of equipment
environments,
including various regimes of soot/sludge formation, friction, corrosion,
thermal
decomposition, oxidation, extreme pressure and wear. In many instances these
different properties are unique to a component of the mechanical device. The
unique properties may depend on chemical interactions between additives (for
example, synergistic effects or antagonists competing for same reactive
sites),
component design, as well as the materials used. Consequently, a number of
functional fluids are required to lubricate various components within the
mechanical
equipment. Having a number of functional fluids may result in difficulties
such as
in handling or storage and confusion of application for the operator.
Confusion of
application may result in improper use resulting in equipment down time.
Furthermore, functional fluids degrade over time through use. The additives
in the functional fluids deplete or change over the lifetime of the fluid in
an engine
or other mechanical device. Replenishment of additives in a functional fluid
by a
slow release additive package in the form of a gel is disclosed in US Patent
Application 2004/0014614. Other time release additives include coatings or
polymers as disclosed in U.S. Patent Application 2004/0154304A1; and U.S.
Patents
4,075,098; and 4,066,559.
Accordingly, it is desirable to provide a delivery system for additives and a
method of lubricating a mechanical device with the delivery system. The
delivery
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system and method of lubricating allows for improved storage or handling of
functional fluids as well as reduced confusion of application. The present
invention
provides a delivery system and a method of lubricating capable of improving at
least
one of replenishing additives in a lubricating oil, storage and handling of
functional
fluids.
Summary of the Invention
The invention provides a method for lubricating a comprising:
(a) employing a first functional fluid, wherein the first functional fluid is
selected from the group consisting of an oil of lubricating viscosity, a gear
oil
including automotive and/or industrial, a manual transmission oil, an
automatic
transmission oil, a hydraulic fluid, an engine oil, a two cycle oil, a
metalworking
fluid and an axle fluid;
(b) contacting the first functional fluid with a delivery system wherein the
delivery system has the desired additives to be released imparting the desired
properties into the first functional fluid which is for lubricating a
mechanical device;
(c) releasing the desired additives from the delivery system into the first
functional fluid resulting in the first fnnctional fluid changing into a
second
functional fluid selected from the group consisting of a gear oil, a manual
transmission oil, an automatic transmission oil, a hydraulic fluid, an engine
oil, a
two cycle oil, a metalworking fluid and an axle fluid, with the proviso that
the
second functional fluid is different from the first functional fluid.
In another embodiment the invention is a method for lubricating a
mechanical device comprising:
(a) employing one or more delivery systems, wherein the delivery systems
may be the same, similar, different or combinations thereof and wherein the
composition of the delivery systems depends on the desired additives to be
added
into a first functional fluid or to change the first functional fluid into a
second
functional fluid;
(b) contacting the first functional fluid with one or more delivery systems
wherein the functional fluid may be of more than one type, and wherein the
delivery
systems comprises at least one additive comprising detergents, dispersants,
acids,
bases, over based detergent, succinated polyolefins, viscosity modifier(s),
friction
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modifier(s), detergent(s), cloud point depressant(s), pour point
depressant(s),
demulsifier(s), flow improver(s), anti static agent(s), dispersant(s),
antioxidant(s),
antifoam(s), corrosion/rust inhibitor(s), extreme pressure/antiwear agent(s),
seal
swell agent(s), lubricity aid(s), antimisting agent(s), or mixtures thereof;
resulting in changing the first functional fluid into the second functional
fluid
when the delivery systems are contacted with the first functional fluid.
The present invention provides a process for supplying one or more desired
additives to a functional fluid by contacting the functional fluid with the
additized
controlled release gel.
Detailed Description
In one embodiment the invention provides a method for lubricating a
mechanical device comprising the methods disclosed above.
The delivery system comprises at least one of liquids, solids, a controlled
release additive gel, capsules (for example melamine or urea formaldehyde
microencapsulation polymers), polymer bags (e.g. linear low density
polyethylene),
perforated sheets, baffles, injectors, polymers which are oil-permeable at
elevated
temperatures (as defined in US Patent 4,066,559), particles which are oil-
insoluble
but oil wettable (as defined in US Patent 5,478,463), oil-soluble solid
polymers
capable of functioning as viscosity improvers (as defined in US Patent
4.014,794),
or mixtures thereof. Typically the oil-soluble solid polymers are delivered
from
within an oil filter, but any means by which the delivery systenl can be
brought into
contact with the functional fluid can be used e.g., container/delivery device
within
the oil pan, or within a fluid by-pass loop.
In accordance with one embodiment of the present invention, a controlled
release additive gel is provided for a fluid conditioning device(s). The
present
invention provides a process for supplying one or more desired additives to a
functional fluid by contacting the functional fluid with the additized
controlled
release gel.
The present invention of a delivery system can be used in any fluid
conditioning device including internal combustion engines which include mobile
and stationary applications; hydraulic systems; automatic transmissions; gear
boxes
which include manual transmissions and differentials (e.g. front and rear
drive axles
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and industrial speed increasers or reducers); metalworking fluids; pumps;
suspension
systems; other lubricated mechanical systems; and the like. The fluid
conditioning
devices that can use the additive gel include, internal combustion engines,
stationary
engines, generators, diesel and/or gasoline engines, on highway and/or off
highway
engines, two-cycle engines, aviation engines, piston engines, marine engines,
railroad engines, biodegradable fuel engines and the like; lubricated
mechanical
systems such as gear boxes, automatic transmissions, differentials, hydraulic
systems and the like.
In one preferred embodiment, the first functional fluid is not a gear oil
because difficulties may be encountered transforming the gear oil into a
second
functional fluid. The reason for this is believed to be the presence of
excessive
amounts of antiwear/ EP agent additives based on sulphurised olefins. In some
instances where the amount of sulphurised olefin is reduced it may be possible
to
change a first functional fluid derived from a gear oil into a different
second
functional fluid.
The functional fluid becomes diminished and depleted of its additives over
time. The additive delivery system is specifically formulated to meet the
desired
performance requirements of the functional fluid system and to condition the
fluid.
The present invention provides for the use of an additive delivery system to
increase
the performance of the functional fluid by replenishing the depleted desired
additives or introducing new desired additives to the functional fluid. Thus
the
functional fluid can add and/or maintain consistent performance over the
functional
fluid's life because the device should perform closer to optimum for a longer
period
of time.
The functional fluids useful to be readditized through the additized delivery
system include gear oil, transmission oil, hydraulic fluid, engine oil, two
cycle oil,
metalworking fluid and the like. In one embodiment the preferred functional
fluid is
an engine oil. In another embodiment the preferred functional fluid is a gear
oil. In
another embodiment the preferred functional fluid is a transmission fluid. In
another
embodiment the preferred functional fluid is a hydraulic fluid.
In one embodiment the additive delivery system dissolves into the functional
fluid by contacting the additive delivery system with the functional fluid in
the
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system. The additive delivery system is positioned anywhere the additive
delivery
system will be in contact with the functional fluid. In one embodiment, the
additive
delivery system is positioned anywhere that the circulating functional fluid
contacts
the additive delivery system. In one embodiment the functional fluid is an
engine oil
and the additive delivery system is positioned in the engine oil system which
includes the lubricating system, filter, drain pan, oil bypass loop, canister,
housing,
reservoir, pockets of a filter, canister in a filter, mesh in a filter,
canister in a bypass
system, mesh in a bypass system, oil lines and the like. In one embodiment the
functional fluid is a gear oil and the additive delivery system is located in
the gear
system which includes oil drain pan, sump, filters, a full flow or bypass oil
line,
lines, loop and/or filter, canisters, mesh, other spaces within the device in
which a
delivery system might be contained and the like. In one embodiment the
functional
fluid is transmission fluid and the additive delivery system is located in the
transmission system which includes the space such as a hole within a
transmission
magnet, the oil pan, oil lines, lines, canisters, mesh and the like. In one
embodiment
the additive delivery system is located in the engine oil line, which includes
a full
flow filter, a by-pass filter, the oil pan, and the like. In one embodiment,
the
functional fluid is a hydraulic fluid and the additive delivery system is
located in the
hydraulic cylinder, sump, filter, oil lines, pan, full flow or by pass oil
loop, line
and/or filter, canister, mesh, other spaces in the system and the like.
One or more locations in a line, loop and/or the functional fluid system can
contain the additive delivery system. Further, if more than one additive
delivery
system for the functional fluid is used the additive delivery system can be
identical,
similar and/or a different additive delivery system composition.
In one embodiment the method for lubricating a mechanical device
comprises employing one or more additive delivery systems in a container.
In one embodiment the properties imparted by the desired additives include
dispersancy, antioxidancy, corrosion inhibition, wear prevention, scuffing
prevention, pitting prevention including micro and macro pitting, friction
modifying
properties including increased and/or decreased friction coefficients,
detergency,
viscosity control using viscosity modifiers, foam control or mixtures thereof.
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In one embodiment the mechanical device comprises axles, gear boxes,
automatic transmissions, manual transmissions, differentials or mixtures
thereof.
In one embodiment of the invention the first functional fluid is changed into
the second functional fluid different from the first functional fluid.
Changing the
first functional fluid into the second functional fluid may be attained by
releasing the
desired additives from a delivery system in an amount sufficient to provide a
different ratio of additives.
The first functional fluid may be changed into the second functional fluid by
adding and/or modifying the ratio of additives in the first functional fluid.
Modifying the ratio of additives by the addition the desired additives is
obtained by
adding or contacting the first functional fluid with a delivery system
composition of
the desired additives. The desired additives controlled released into the
first
functional fluid resulting in the first functional fluid changing into the
second
functional fluid. The change from the first functional fluid to the second
functional
fluid occurs when the desired additives are released from the delivery system
and
providing the desired properties to the second functional fluid.
In one embodiment the first functional fluid is a manual transmission fluid
additized with a sufficient amount of an antiwear agent/extreme pressure agent
and
other additives including dispersants and/or detergent to form the second
functional
fluid, an axle fluid.
In one embodiment the functional fluid system comprises additive delivery
systems suitable for forming a functional fluid for an axle. The compositions
of the
additive delivery systems suitable forming a functional fluid for an axle
and/or gear
oil in one embodiment contains reduced amounts of a sulfurized olefin antiwear
agent in the presence of a sulfonate detergent. In another embodiment the
functional
fluid for an axle and/or gear oil contains reduced amounts of sulfonate
detergent in
the presence of a sulfurized olefin antiwear agent. In another embodiment the
sulfonate detergent in the delivery system is substantially retained, thus
reducing the
amount of detergent in a functional fluid for an axle and/or gear oil. In one
embodiment, it is desirable that the sulfonate detergent in the delivery
system does
not release in a gear oil applications.
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In one embodiment the line, loop and/or the functional fluid system contains
two or more different additive delivery systems located at two or more
locations.
The different compositions of the additive delivery systems provide the first
functional fluid with desired additives to be control released to change to a
second
functional fluid that lubricates the mechanical device.
In one embodiment, the mechanical device contains two or more first
functional fluids which are contacted with one or more, for example two or
three
additive delivery systems. After contacting the additives delivery systems,
the first
functional fluids are changed into second functional fluids (which can be the
same or
different depending on the delivery systems) with two or more compositions
that are
employed to provide appropriate lubricating properties to various components
within
the mechanical device.
In one embodiment the mechanical device comprises one first functional
fluid contacting multiple delivery systems resulting in changing the first
functional
fluid into multiple second functional fluids.
In one embodiment the mechanical device comprises multiple first functional
fluids contacting multiple delivery systems resulting in changing the first
functional
fluids into multiple second functional fluids.
In one embodiment it is desirable to provide a container to hold the additive
delivery system, such as a housing, a canister or a structural mesh anywhere
in the
functional fluid system, for example, a canister within a bypass loop of a
stationary
gas engine for power generation. The necessary design feature for the
container is
that at least a portion of the additive delivery system is in contact with the
functional
fluid.
In one embodiment the delivery system is a controlled release gel. The gel
comprises;
i.) at least two additives selected from the group comprising
detergents, dispersants, acids, bases, over based detergent,
succinated polyolefins or mixtures thereof wherein the selected
additives when combined form a gel;
ii.) optionally at least one additive comprising viscosity modifier(s),
friction modifier(s), detergent(s), cloud point depressant(s), pour
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point depressant(s), demulsifier(s), flow improver(s), anti static
agent(s), dispersant(s), antioxidant(s), antifoam(s), corrosion/rust
inhibitor(s), extreme pressure/antiwear agent(s), seal swell agent(s),
lubricity aid(s), antimisting agent(s), or mixtures thereof.
The additive gel needs to be in contact with the functional fluid. In one
embodiment the additive gel is in contact with the functional fluid in the
range of
about 100% to about 1% of the functional fluid in the system, in another
embodiment the additive gel is in contact with the functional fluid in the
range of
about 75% to about 25% of the functional fluid in the system and in another
embodiment the additive gel is in contact with the functional fluid in the
range of
about 50% of the functional fluid in the system. As the flow rate decreases
there is
less dissolution of the additive gel and as the flow rate increases there is
greater
dissolution of the additive gel.
In one embodiment, the additive gel is positioned in the functional fluid
system so that the additive gel and/or spent additive gel can easily be
removed, and
then replaced with a new and/or recycled additive gel.
The additive gel is added to the system by any known method depending on
the total amount of gel that is desired to be released over time, the desired
form of
the additive gel (e.g. stiffness, consistency, homogeneity and the like), the
desired
overall dissolution of the gel, the desired release rates of a specific
component, the
desired mode of operation and/or any combinations of the above.
The release rate of the additive gel is determined primarily by the additive
gel formulation. The release rate is also dependent on the mode of addition of
the
additive gel, the location of additive gel, flow rate of the functional fluid,
the form of
the additive gel (e.g., stiffness, consistency, homogeneity and the like) and
the like.
The additive gel is positioned in a location desirable for the specified and
desirable
dissolution rate of the additive gel components.
The additive gel's formulation may be composed of one or more components
that selectively dissolve or a portion of one or more components remain till
the end
of its service life or combinations thereof. In general, the components in
category ii
will typically dissolve faster than the components in i) as defined above.
This
allows a desired component(s) ii) as defined above to be selectively released
into the
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functional fluid while other components remain undissolved or less dissolved.
Thus
depending on the fluid conditioning device and its functional fluid, the gel
would
contain the desired component(s) in category ii to dissolve into the
functional fluid
to replace or introduce the desired additive.
In one embodiment, it has been found that the gel slowly dissolves its
component additive parts into the functional fluid when exposed to heated
fluid with
no or limited flow over the surface of the gel. The rate of dissolution of
additive gel
under these conditions is controlled to be slow, and because the gel dissolves
into its
component additives, it effectively achieves slow and selective release of the
desired
additives into the functional fluid. If exposure to the hot fluid is continued
beyond
the point that certain additive(s) are selectively released, the gel will
continue to
dissolve over time so that the other additives, i.e. b i) components, continue
to be
released. These release rates can be optimized, using the parameters described
above, so that the desired gel component(s) are released over a substantial
portion to
all of the functional fluid's useful life.
The gel can be used as is, without an inert carrier or a non additive matrix,
such as a polymeric membrane or complicated mechanical systems needed in
earlier
systems for achieving controlled release of additives over time.
The gel is a mixture of two or more additives from category i component that
when combined form a gel and further contain at least one additive from
category ii
components. The gel exists in a semi-solid state more like a solid than a
liquid, see
Parker, Dictionary of Scientific and Technical Terms, Fifth Edition, McGraw
Hill,
1994. See, also, Larson, "The Structure and rheology of Complex Fluids",
Chapter 5, Oxford University Press, New York, New York, 1999, each which is
incorporated herein by reference. The rheological properties of a gel can be
measured by small amplitude oscillatory shear testing. This technique measures
the
structural character of the gel and produces a term called the storage modulus
which
represents storage of elastic energy and the loss modulus which represents the
viscous dissipation of that energy. The ratio of the loss modulus/storage
modulus,
which is called the loss tangent, or "tan delta", is >1 for materials that are
liquid-like
and <1 for materials that are solid-like. The additive gels have tan delta
values in
one embodiment of about < 0.75, in another embodiment of about < 0.5 and in
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another embodiment of about < 0.3. The gels have tan delta values in one
embodiment of about < 1, in one embodiment of about < 0.75, in one embodiment
of
about <0.5 or in one embodiment of about <0.3.
The additive gel contains a combination of gelling additives of i) components
in the range of about 0.01% to about 95%, in one embodiment in the range of
about
0.1% to 80% and in another embodiment in the range of about 1% to about 50% of
the total weight of the gel.
The additive gel contains a combination of optional additives of the ii)
components in the range of about 0.1% to about 95%, in one embodiment in the
range of about 0.1% to 90%, in another embodiment in the range of about 0.1%
to
about 80%, and in another embodiment in the range of about 0.5% to about 50%
of
the total weight of the additives and/or base oil of the delivery system (i.e.
excluding
the weight of the mechanical device).
In accordance with the present invention, any delivery system formed from
the combination of two or more additives comprising detergents, dispersants,
acids,
bases, over based detergents, succinated polyolefins, and the like can be used
to
make the additive gel. The additive gel comprises at least two additives
selected
from the group including detergents, dispersants, acids, bases, over based
detergent,
succinated polyolefins or mixtures thereof wherein such selected additives
when
combined form a gel. Further in one embodiment the additive gel includes
combining dispersants, or combining a dispersant and an acid, or combining a
dispersant and a base, or a dispersant and an over based detergent, and the
like.
In one embodiment, a category of gel which finds particular use are those in
which gellation occurs through the combination of an overbased detergent and
an
ashless succinimide dispersant. In one embodiment, the ratio of the detergent
to the
dispersant is from about 10:1 to about 1:10, in another embodiment from about
5:1
to about 1:5, form about 4:1 to about 1:1 and in another embodiment from about
4:1
to about 2:1. In addition, the TBN of the overbased detergent which
participates in
the gel-forming matrix, is normally at least 200, more typically at 300-1,000
and
most typically 350 to 650. Where mixtures of overbased detergents are used, at
least
one should have a TBN value within these ranges. However, the average TBN of
these mixtures may also correspond to these values.
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The dispersant includes dispersants; ashless type dispersants such as
Mannich dispersants; polymeric dispersants; carboxylic dispersants; amine
dispersants, high molecular weight (Cn wherein n< 12) esters and the like;
esterfied
maleic anhydride styrene copolymers; maleated ethylene diene monomer
copolymers; surfactants; emulsifiers' functionalized derivatives of each
component
listed herein and the like; and combinations and mixtures thereof. In one
embodiment the preferred dispersant ispolyisobutenyl succinimide dispersant.
The dispersants includes ashless-type dispersants, polymeric dispersants,
Mannich dispersants, high molecular weight (Cn wherein n >12) esters,
carboxylic
dispersants, amine dispersants and combinations thereof. The dispersant may be
used alone or in combination.
The dispersant includes but is not limited to an ashless dispersant such as a
polyisobutenyl succinimide and the like. Polyisobutenyl succinimide ashless
dispersants are commercially-available products which are typically made by
reacting together polyisobutylene having a number average molecular weight
("Mn") of about 300 to 10,000 with maleic anhydride to form polyisobutenyl
succinic anhydride ("PIBSA") and then reacting the product so obtained with a
polyamine typically containing 1 to 10 ethylene amino groups per molecule.
Ashless type dispersants are characterized by a polar group attached to a
relatively high molecular weight hydrocarbon chain. Typical ashless
dispersants
include N-substituted long chain alkenyl succinimides, having a variety of
chemical
structures including typically:
Ri R,
O
H
n )-N /N NH2
0 R2 n
and/or
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O 0
R, R,
N-[R2NH]x-R2N
O 0
wherein each R' is independently an alkyl group, frequently a polysiobutyl
group
with a molecular weight of 500-5000, and Ra are alkenylene groups, commonly
ethylene (C2H4) groups. Succinimide dispersants are more fully described in
U.S.
Patent 4,234,435 which is incorporated herein by reference. The dispersants
described in this patent are particularly effective for producing delivery
systems in
accordance with the present invention.
The Mannich dispersant are the reaction products of alkyl phenols in which
the alkyl group contains at least about 30 carbon atoms with aldehydes
(especially
formaldehyde) and amines (especially polyalkylene polyamines). Mannich bases
having the following general structure (including a variety of different
isomers and
OH OH
CH2-NH-{R2-NH]x-R2-NH-CH2
I I .
i
Rl Rl
the like) are especially interesting.
and/or
R~ Ri
H
H2C-~N N NH2
n ~ ~ R2 1 n
\OH
Another class of dispersants is carboxylic dispersants. Examples of these
"carboxylic dispersants" are described in Patent U.S. Patent 3,219,666.
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Amine dispersants are reaction products of relatively high molecular weight
aliphatic halides and amines, preferably polyalkylene polyamines. Examples
thereof
are described, in U.S. Patent 3,565,804.
Polymeric dispersants are interpolymers of oil-solubilizing monomers such
as decyl methacrylate, vinyl decyl ether and high molecular weight olefins
with
monomers containing polar substituents, e.g., amino alkyl acrylates or
acrylamides
and poly-(oxyethylene)-substituted acrylates. Examples of polymer dispersants
thereof are disclosed in the following U.S. Patents: 3,329,658, and 3,702,300.
Dispersants can also be post-treated by reaction with any of a variety of
agents. Among these are urea, thiourea, dimercaptothiazoles, carbon disulfide,
aldehydes, ketones, carboxylic acids, hydrocarbon-substituted succinic
anhydrides,
nitriles, epoxides, boron compounds, and phosphorus compounds.
Dispersants can be used alone or in combination. The dispersant is present
in the range from about 0 wt % or 0.01 wt % to about 95 wt % gel, in another
embodiment in the range from about 1 wt % to about 70 wt % gel, and preferably
in
another embodiment in the range from about 5 wt % to about 50 wt % total
weight
of the additives and/or base oil of the delivery system.
The detergents include overbased sulfonates, phenates, salicylates,
carboxylates, overbased calcium sulfonate detergents which are commercially-
available, overbased detergents containing metals such as Mg, Ba, Sr, Na, Ca
and K
and mixtures thereof and the like.
Detergents are described, for example, in U.S. Patent 5,484,542 which is
incorporated herein by reference. The detergents may be used alone or in
combination. Detergents are described, for example, in U.S. Patent 5,484,542
which
is incorporated herein by reference.
The detergents may be used alone or in combination. The detergents are
present in the range from about 0 wt % or 0.01 wt % to about 99 wt %, in one
embodiment in the range from about 1 wt % to about 70 wt % and in another
embodiment in the range from about 5 wt % to about 50 wt % total weight of the
additives and/or base oil of the delivery system.
Typically the additive gel further contains at least one desired additive for
controlled release into the functional fluid. The additive gel desired
components
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include viscosity modifier(s), friction modifier(s), detergent(s), cloud point
depressant(s), pour point depressant(s), demulsifier(s), flow improver(s),
anti static
agent(s), dispersant(s), antioxidant(s), antifoam(s), corrosion/rust
inhibitor(s),
extreme pressure/antiwear agent(s), seal swell agent(s), lubricity aid(s),
antimisting
agent(s), and mixtures thereof; resulting in a controlled release gel that
over time
releases the desired additive(s) into a functional fluid when the gel is
contacted with
the functional fluid. The desired additive component is further determined by
the
functional fluid formulation, performance characteristics, function and the
like and
what additive is desired to be added for depleted additives and/or added new
depending on the desired functions.
Antioxidants include alkyl-substituted phenols such as 2, 6-di-tertiary butyl-
4-methyl phenol, phenate sulfides, phosphosulfitrized terpenes, sulfurized
esters,
aromatic amines, diphenyl amines, alkylated diphenyl amines and hindered
phenols,
bis-nonylated diphenylamine, nonyl diphenylamine, octyl diphenylamine, bis-
octylated diphenylamine, bis-decylated diphenylamine, decyl diphenylamine and
mixtures thereof.
The antioxidant function includes sterically hindered phenols and includes
but is not limited to 2,6-di-tert-butylphenol, 4-methyl-2,6-di-tert-
butylphenol, 4-
ethyl-2,6-di-tert-butylphenol, 4-propyl-2,6-di-tert-butylphenol, 4-butyl-2,6-
di-tert-
butylphenol 2,6-di-tert-butylphenol, 4-pentyl-2-6-di-tert-butylphenol, 4-hexyl-
2,6-
di-tert-butylphenol, 4-heptyl-2,6-di-tert-butylphenol, 4-(2-ethylhexyl)-2,6-di-
tert-
butylphenol, 4-octyl-2,6-di-tert-butylphenol, 4-nonyl-2,6-di-tert-butylphenol,
4-
decyl-2,6-di-tert-butylphenol, 4-undecyl-2,6-di-tert-butylphenol, 4-dodecyl-
2,6-di-
tert-butylphenol, 4-tridecyl-2,6-di-tert-butylphenol, 4-tetradecyl-2,6-di-tert-
butylphenol, methylene-bridged sterically hindered phenols include but are not
limited to 4,4-methylenebis(6-tert-butyl-o-cresol), 4,4-methylenebis(2-tert-
amyl-o-
cresol), 2,2-methylenebis(4-metyl-6-tert-butylphenol), 4,4-methylene-bis(2,6-
di-
tertbutylphenol) and mixtures thereof.
Another example of an antioxidant is a hindered, ester-substituted phenol,
which can be prepared by heating a 2,6-dialkylphenol with an acrylate ester
under
based conditions, such as aqueous KOH.
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Antioxidants may be used alone or in combination. The antioxidants are
typically present in the range of about 0 wt % or 0.01 wt % to about 95 wt %,
in one
embodiment in the range from about 0.01 wt % to 95 wt %, and in another
embodiment in the range from about 1 wt % to about 70 wt % and in another
embodiment in the range from about 5 wt % to about 60 wt % total weight of the
additives and/or base oil of the delivery system.
The extreme pressure/anti-wear agents include a sulfur or chlorosulphur EP
agent, a chlorinated hydrocarbon EP agent, or a phosphorus EP agent, or
mixtures
thereof. Examples of such EP agents are amine salts of phosphorus acid acid,
chlorinated wax, organic sulfides and polysulfides, such as benzyldisulfide,
bis-
(chlorobenzyl) disulfide, dibutyl tetrasulfide, sulfurized sperm oil,
sulfurized methyl
ester of oleic acid sulfurized alkylphenol, sulfitrized dipentene, sulfurized
terpene,
and sulfurized Diels-Alder adducts; phosphosulfurized hydrocarbons, such as
the
reaction product of phosphorus sulfide with turpentine or methyl oleate,
phosphorus
esters such as the dihydrocarbon and trihydrocarbon phosphate, i.e., dibutyl
phosphate, diheptyl phosphate, dicyclohexyl phosphate, pentylphenyl phosphate;
dipentylphenyl phosphate, tridecyl phosphate, distearyl phosphate and
polypropylene substituted phenol phosphate, metal thiocarbamates, such as zinc
dioctyldithiocarbamate and barium heptylphenol diacid, such as zinc
dicyclohexyl
phosphorodithioate and the zinc salts of a phosphorodithioic acid combination
may
be used and mixtures thereof.
In one embodiment the antiwear agent/extreme pressure agent comprises an
amine salt of a phosphorus ester acid. The amine salt of a phosphorus ester
acid
includes phosphoric acid esters and salts thereof; dialkyldithiophosphoric
acid esters
and salts thereof; phosphites; and phosphorus-containing carboxylic esters,
ethers,
and amides; and mixtures thereof.
In one embodiment the phosphorus compound further comprises a sulfur
atom in the molecule. In one embodiment the amine salt of the phosphorus
compound is ashless, i.e., metal-free (prior to being mixed with other
components).
The amines which may be suitable for use as the amine salt include primary
amines, secondary amines, tertiary amines, and mixtures thereof. The amines
include those with at least one hydrocarbyl group, or, in certain embodiments,
two
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or three hydrocarbyl groups. The hydrocarbyl groups may contain about 2 to
about
30 carbon atoms, or in other embodiments about 8 to about 26 or about 10 to
about
20 or about 13 to about 19 carbon atoms.
Primary amines include ethylamine, propylamine, butylamine,
2-ethylhexylamine, octylamine, and dodecylamine, as well as such fatty amines
as
n-octylamine, n-decylamine, n-dodecylamine, n-tetradecylamine, n-
hexadecylamine,
n-octadecylamine and oleylamine. Other useful fatty amines include
commercially
available fatty amines such as "Armeen " amines (products available from Akzo
Chemicals, Chicago, Illinois), such as Armeen C, Armeen 0, Armeen OL, Armeen
T, Armeen HT, Armeen S and Armeen SD, wherein the letter designation relates
to
the fatty group, such as coco, oleyl, tallow, or stearyl groups.
Examples of suitable secondary amines include dimethylamine,
diethylamine, dipropylamine, dibutylamine, diamylamine, dihexylamine,
diheptylamine, methylethylamine, ethylbutylamine and ethylamylamine. The
secondary amines may be cyclic amines such as piperidine, piperazine and
morpholine.
The amine may also be a tertiary-aliphatic primary amine. The aliphatic
group in this case may be an alkyl group containing about 2 to about 30, or
about 6
to about 26, or about 8 to about 24 carbon atoms. Tertiary alkyl amines
include
monoamines such as tert-butylamine, tert-hexylamine, 1-methyl-l-amino-
cyclohexane, tert-octylamine, tert-decylamine, tert-dodecylamine, tert-
tetradecylamine, tert-hexadecylamine, tert-octadecylamine, tert-
tetracosanylamine,
and tert-octacosanylamine.
Mixtures of amines may also be used in the invention. In one embodiment a
useful mixture of amines is "Primene 81R" and "Primene JMT." Primene 81R
and Primene JMT (both produced and sold by Rohm & Haas) are mixtures of C11
to C 14 tertiary alkyl primary amines and C 18 to C22 tertiary alkyl primary
amines
respectively.
Suitable hydrocarbyl amine salts of alkylphosphoric acid of the invention
may be represented by the following formula:
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7
R3-0 ' P / O" R\ i+ / Rs
R4-O/ H /
R5
wherein R3 and R4 are independently hydrogen or hydrocarbyl groups such as
alkyl
groups; for the phosphorus ester acid, at least one of R3 and R4 will be
hydrocarbyl.
R3 and R4 may contain about 4 to about 30, or about 8 to about 25, or about 10
to
about 20, or about 13 to about 19 carbon atoms. R5, R6 and R7 may be
independently hydrogen or hydrocarbyl groups, such as alkyl branched or linear
alkyl chains with 1 to about 30, or about 4 to about 24, or about 6 to about
20, or
about 10 to about 16 carbon atoms. These R5, R6 and IC groups may be branched
or
linear groups, and in certain embodiments at least one, or alternatively two
of R5, R6
and IC are hydrogen. Examples of alkyl groups suitable for R5, R6 and R7
include
butyl, sec-butyl, isobutyl, tert-butyl, pentyl, n-hexyl, sec-hexyl, n-octyl, 2-
ethylhexyl, decyl, undecyl, dodecyl, tridecyl, tetradecyl, pentadecyl,
hexadecyl,
heptadecyl, octadecyl, octadecenyl, nonodecyl, eicosyl groups and mixtures
thereof.
In one embodiment the hydrocarbyl amine salt of an alkylphosphoric acid
ester is the reaction product of a C14 to C18 alkylated phosphoric acid with
Primene
81RTM (produced and sold by Rohrn & Haas) which is a mixture of Cll to C14
tertiary alkyl primary amines.
Similarly, hydrocarbyl amine salts of dialkyldithiophosphoric acid esters of
the invention used in the rust inhibitor package may be represented by the
formula:
R3---p S R7 ' Rs
P N +/
R4 \ H /I
R5
wherein the various R groups are as defined above, although typically both R
groups
are hydrocarbyl or alkyl. Examples of hydrocarbyl amine salts of
dialkyldithiophosphoric acid esters include the reaction product(s) of hexyl,
heptyl
or octyl or nonyl, 4-methyl-2-pentyl or 2-ethylhexyl, isopropyl
dithiophosphoric
acids with ethylene diamine, morpholine, or Primene 81RTM, and mixtures
thereof.
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In one embodiment the dithiophosphoric acid may be reacted with an
epoxide or a glycol. This reaction product is further reacted with a
phosphorus acid,
anhydride, or lower ester. The epoxide includes an aliphatic epoxide or a
styrene
oxide. Examples of useful epoxides include ethylene oxide, propylene oxide,
butene
oxide, octene oxide, dodecene oxide, styrene oxide and the like. In one
embodiment
the epoxide is Propylene oxide. The glycols may be aliphatic glycols having
from 1
to about 12, or from about 2 to about 6, or about 2 to about 3 carbon atoms.
The
dithiophosphoric acids, glycols, epoxides, inorganic phosphorus reagents and
methods of reacting the same are described in U.S. Patent numbers 3,197,405
and
3,544,465. The resulting acids may then be salted with amines. An example of
suitable dithiophosphoric acid is prepared by adding phosphorus pentoxide
(about
64 grams) at about 58 C over a period of about 45 minutes to about 514 grams
of
hydroxypropyl O,O-di(4-methyl-2-pentyl)phosphorodithioate (prepared by
reacting
di(4-methyl-2-pentyl)-phosphorodithioic acid with about 1.3 moles of propylene
oxide at about 25 C ). The mixture is heated at about 75 C for about 2.5
hours,
mixed with a diatomaceous earth and filtered at about 70 C. The filtrate
contains
about 11.8% by weight phosphorus, about 15.2% by weight sulfur, and an acid
number of 87 (bromophenol blue).
The EP / antiwear agent can be used alone or in combination.
In one embodiment the EP / antiwear agent may be in the delivery system
from about 0 wt % or 0.05 wt % to about 10 wt % or about 0.1 wt % to about 5
wt
%.
The EP / antiwear agents are present in the range of about 0 wt % to about 20
wt %, in one embodiment in the range from about 0.25 wt % to about 10 wt % and
in another embodiment in the range from about 0.5 wt % to about 25 wt % total
weight of the additives and/or base oil of the delivery system.
The antifoams include organic silicones such as poly dimethyl siloxane, poly
ethyl siloxane, polydiethyl siloxane, polyacrylates and polymethacrylates,
trimethyl-
triflouro-propylmethyl siloxane and the like.
The antifoams may be used alone or in combination. The antifoams are used
in the range of about 0 wt % to about 20 wt %, in one embodiment in the range
of
about 0.02 wt % to about 10 wt % and in another embodiment in the range of
0.05
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wt % to about 2.5 wt % total weight of the additives and/or base oil of the
delivery
system.
The viscosity modifier provides both viscosity improving properties and
dispersant properties. Examples of dispersant-viscosity modifiers include
vinyl
pyridine, N-vinyl pyrrolidone and N,N'-dimethylaminoethyl methacrylate are
examples of nitrogen-containing monomers and the like. Polyacrylates obtained
from the polymerization or copolymerization of one or more alkyl acrylates
also are
useful as viscosity modifiers.
Functionalized polymers can also be used as viscosity modifiers. Among the
common classes of such polymers are olefin copolymers and acrylate or
methacrylate copolymers. Functionalized olefin copolymers can be, for
instance,
interpolymers of ethylene and propylene which are grafted with an active
monomer
such as maleic anhydride and then derivatized with an alcohol or an amine.
Other
such copolymers are copolymers of ethylene and propylene which are reacted or
grafted with nitrogen compounds. Derivatives of polyacrylate esters are well
known
as dispersant viscosity index modifiers additives. Dispersant acrylate or
polymethacrylate viscosity modifiers such as AcryloidTM 985 or ViscoplexTM 6-
054,
from RohMax, are particularly useful. Solid, oil-soluble polymers such as the
PIB
(polyisobutylene), methacrylate, polyalkystyrene, ethylene/propylene and
ethylene/propylene/1,4-hexadiene polymers and maleic anhydride-styrene
interpolymer and derivatives thereof, can also be used as viscosity index
improvers.
The viscosity modifiers are known and commercially available.
The viscosity modifiers may be used alone or in combination. The viscosity
modifiers are present in the range of about 0 wt % to 20 wt %, in one
embodiment in
the range from about 0.25 wt % to about 10 wt % and in another embodiment in
the
range from about 0.5 wt % to about 2.5 wt % total weight of the additives
and/or
base oil of the delivery system.
The friction modifiers include organo-molybdenum compounds, including
molybdenum dithiocarbamates, and fatty acid based materials, including those
based
on oleic acid, including glycerol mono oleate (GMO), those based on stearic
acid,
and the like.
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In one embodiment, the friction modifier is a phosphate ester or salt
including a monohydrocarbyl, dihydrocarbyl or a trihydrocarbyl phosphate,
wherein
each hydrocarbyl group is saturated. In several embodiments, each hydrocarbyl
group contains from about 8 to about 30, or from about 12 up to about 28, or
from
about 14 up to about 24, or from about 14 up to about 18 carbons atoms. In
another
embodiment, the hydrocarbyl groups are alkyl groups. Examples of hydrocarbyl
groups include tridecyl, tetradecyl, pentadecyl, hexadecyl, heptadecyl,
octadecyl
groups and mixtures thereof.
In one embodiment, the phosphate salts may be prepared by reacting an
acidic phosphate ester with an amine compound or a metallic base to form an
amine
or a metal salt. The amines may be monoamines or polyamines. Useffizl amines
include those amines disclosed in U.S. Patent 4,234,435 at Col. 21, line 4 to
Col. 27,
line 50.
Useful amines include primary ether amines, such as those represented by
the formula, R"(OR')X NHZ, wherein R' is a divalent alkylene group having
about 2
to about 6 carbon atoms; x is a number from one to about 150, or from about
one to
about five, or one; and R" is a hydrocarbyl group of about 5 to about 150
carbon
atoms.
The phosphate salt may be derived from a polyamine. The polyamines
include alkoxylated diamines, fatty polyamine diamines, alkylenepolyamines,
hydroxy containing polyamines, condensed polyamines, arylpolyamines, and
heterocyclic polyamines.
The metal salts of the phosphorus acid esters are prepared by the reaction of
a metal base with the acidic phosphorus ester. The metal base may be any metal
compound capable of forming a metal salt. Examples of metal bases include
metal
oxides, hydroxides, carbonates, borates, or the like. Suitable metals include
alkali
metals, alkaline earth metals and transition metals. In one embodiment, the
metal is
a Group IIA. metal, such as calcium or magnesium, Group IIB metal, such as
zinc, or
a Group VIIB metal, such as manganese. Examples of metal compounds which may
be reacted with the phosphorus acid include zinc hydroxide, zinc oxide, copper
hydroxide or copper oxide.
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In one embodiment, the friction modifier is a phosphite and may be a
monohydrocarbyl, dihydrocarbyl or a trihydrocarbyl phosphite, wherein each
hydrocarbyl group is saturated. In several embodiments each hydrocarbyl group
independently contains from about 8 to about 30, or from about 12 up to about
28, or
from about 14 up to about 24, or from about 14 up to about 18 carbons atoms.
In
one embodiment, the hydrocarbyl groups are alkyl groups. Examples of
hydrocarbyl
groups include tridecyl, tetradecyl, pentadecyl, hexadecyl, heptadecyl,
octadecyl
groups and mixtures thereof.
In one embodiment, the friction modifier is a fatty imidazoline comprising
fatty substituents containing from 8 to about 30, or from about 12 to about 24
carbon
atoms. The substituent may be saturated or unsaturated, preferably saturated.
In one
aspect, the fatty imidazoline may be prepared by reacting a fatty carboxylic
acid
with a polyalkylenepolyamine, such as those discussed above. A suitable fatty
imidazoline includes those described in US Patent 6,482,777.
The friction modifiers can be used alone or in combination. The friction
reducing agents are present in the range of about 0 wt % to 10 wt %, or from
about
0.25 wt % to about 10 wt %, or from about 0.5 wt % to about 2.5 wt % total
weight
of the additives and/or base oil of the delivery system.
The anti-misting agents include very high (>100,000Mn) polyolefins such as
1.5 Mn polyisobutylene (for example the material of the trades name Vistanex
), or
polymers containing 2-(N-acrylamido), 2-methyl propane sulfonic acid (also
known
as AMPS ), or derivatives thereof, and the like.
The anti-misting agents can be used alone or in combination. The anti-
misting agents are present in the range of about 0 wt % to 10 wt %, or from
about
0.25 wt % to about 10 wt %, or from about 0.5 wt % to about 2.5 wt % total
weight
of the additives and/or base oil of the delivery system.
The corrosion inhibitors include alkylated succinic acids and anhydrides
derivatives thereof, organo phosphonates and the like. The rust inhibitors may
be
used alone or in combination. The rust inhibitors are present in the range of
about 0
wt % to about 90 wt %, and in one embodiment in the range from about 0.0005 wt
% to about 50 wt % and in another embodiment in the range from about 0.0025 wt
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% to about 30 wt % total weight of the additives and/or base oil of the
delivery
system.
The metal deactivators include derivatives of benzotriazoles such as
tolyltriazole, N,N-bis(heptyl)-ar-methyl-lH-benzotriazole-l-methanamine, N,N-
bis(nonyl)-ar-methyl-lH-Benzotriazole-l-methanamine, N,N-bis(decyl)ar-methyl-
1H-Benzotriazole-l-methanamine, N,N-(undecyl)ar-methyl-lH-benzotriazole-l-
methanamine, N,N-bis(dodecyl)ar-methyl-1H-Benzotriazole-l-methanamine N,N-
bis(2-ethylhexyl)-ar-methyl-lH-Benzotriazole-l-methanamine and mixtures
thereof.
In one embodiment the metal deactivator is N,N-bis(1-ethylhexyl)ar-methyl-lH-
benzotriazole-l-methanamine;1,2,4-triazoles, benzimidazoles, 2-
alkyldithiobenzimidazoles;2-alkyldithiobenzothiazoles; 2-N,N-dialkyldithio-
carbamoyl)benzothiazoles;2,5-bis(alkyl-dithio)-1,3,4-thiadiazoles such as 2,5-
bis(tert-octyldithio)-1,3,4-thiadiazole 2,5-bis(tert-nonyldithio)-1,3,4-
thiadiazole, 2,5-
bis(tert-decyldithio)-1,3,4-thiadiazole, 2,5-bis(tert-undecyldithio)-1,3,4-
thiadiazole,
2,5-bis(tert-dodecyldithio)-1,3,4-thiadiazole, 2,5-bis(tert-tridecyldithio)-
1,3,4-
thiadiazole, 2,5-bis(tert-tetradecyldithio)-1,3,4-thiadiazole, 2,5-bis(tert-
octadecyldithio)-1,3,4-thiadiazole, 2,5-bis(tert-nonadecyldithio)-1,3,4-
thiadiazole,
2,5-bis(tert-eicosyldithio)-1,3,4-thiadiazole and mixtures thereof; 2,5-
bis(N,N-
dialkyldithiocarbamoyl)-1,3,4-thiadiazoles; 2-alkydithio-5-mercapto
thiadiazoles;
and the like.
The metal deactivators may be used alone or in combination. The metal
deactivators are present in the range of about 0 wt % to about 90 wt %, or
from
about 0.0005 wt % to about 50 wt %, or from about 0.0025 wt % to about 30 wt %
total weight of the additives and/or base oil of the delivery system.
The demulsifiers include polyethylene and polypropylene oxide copolymers
and the like. The demulsifiers may be used alone or in conlbination. The
demulsifiers are present in the range of about 0 wt % to about 90 wt %, or
from
about 0.0005 wt % to about 50 wt %, or from about 0.0025 wt % to about 30 wt %
total weight of the additives and/or base oil of the delivery system.
The lubricity aids include glycerol mono oleate, sorbitan mono oleate and the
like. The lubricity additives may be used alone or in combination. The
lubricity
additives are present in the range of about 0 wt % to about 90 wt %, or from
about
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0.0005 wt % to about 50 wt %, or from about 0.0025 wt % to about 30 wt % total
weight of the additives and/or base oil of the delivery system.
The flow improvers include ethylene vinyl acetate copolymers and the like.
The flow improvers may be used alone or in combination. The flow improvers are
present in the range of about 0 wt % to about 90 wt %, or from about 0.0005 wt
% to
about 50 wt %, or from about 0.0025 wt % to about 30 wt % total weight of the
additives and/or base oil of the delivery system.
The cloud point depressants include alkylphenols and derivatives thereof,
ethylene vinyl acetate copolymers and the like. The cloud point depressants
may be
used alone or in combination. The cloud point depressants are present in the
range
of about 0 wt % to about 90 wt %, or from about 0.0005 wt % to about 50 wt %,
or
from about .0025% to about 30 wt % total weight of the additives and/or base
oil of
the delivery system.
The pour point depressants include alkylphenols and derivatives thereof,
ethylene vinyl acetate copolymers and the like. The pour point depressant may
be
used alone or in combination. The pour point depressant are present in the
range of
about 0 wt % to about 90 wt %, or from about 0.0005 wt % to about 50 wt %, or
from about 0.0025 wt % to about 30 wt % total weight of the additives and/or
base
oil of the delivery system.
The seal swell agents include organo sulfur compounds such as thiophene, 3-
(decyloxy)tetrahydro-1, 1-dioxide, phthalates and the like. The seal swell
agents
may be used alone or in combination. The seal swell agents are present in the
range
of about 0 wt % to about 90 wt %, or from about 0.0005 wt % to about 50 wt %,
or
from about 0.0025 wt % to about 30 wt % total weight of the additives and/or
base
oil of the delivery system.
Optionally, other components can be added to the delivery system includes
base stock oils, inert carriers, dyes, bacteriostatic agents, solid
particulate additives,
and the like so long as these components do not have a detrimental effect on
the
delivery system.
When the delivery system is a gel, typically the gel contains small amounts
(about 5-40 wt %) of base stock oils, which include but are not limited to
mineral-
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based, synthetic (including Fischer-Tropsch gas-to-liquid synthetic procedure
as
well as other gas-to-liquid oils) or mixtures thereof.
Optionally, an inert carrier can be used if desired. Furthermore, other active
ingredients, which provide a beneficial and desired function can also be
included in
the gel. In addition, solid, particulate additives such as the PTFE, MoS2 and
graphite can also be included.
Optionally, dyes can be used and include halo-alkanes and the like. The dyes
may be used alone or in combination. The dyes are present in the range of
about 0
wt % to about 90 wt %, or from about 0.0005 wt % to about 50 wt %, or from
about
0.0025 wt % to about 30 wt % total weight of the additives and/or base oil of
the
delivery system.
Optionally, bacteriostatic agents can be used and include formaldehyde,
gluteraldehyde and derivatives, kathan and the like. The bacteriostatic agents
may
be used alone or in combination. The bacteriostatic agents are present in the
range
of about 0 wt % to about 90 wt %, or from about 0.0005% to about 50 wt %, or
from about 0.0025% to about 30 wt % total weight of the additives and/or base
oil of
the delivery system.
The components are mixed together sequentially or all together to form a
mixture. After mixing of the components of the gel, a cure may be required in
order
for gelation to occur. If a cure is required, it is typically done in the
range of about
20 C to about 165 C for about 1 min to about 60 days, or about 50 C to
about 120
C for about 1 to about 24 hours, or about 85 C to about 115 C for about 4 to
about
12 hours.
Specific Embodiment
For all the examples the components listed in each example in the
specification were mixed together to form the gel. The gels were cured at
about
100 C for about 8 hours.
Example 1 Controlled Release of Antiwear Agent in Manual Transmission Fluid
Antiwear agents such as amine salts of a phosphorus acid esters are well
known as being suitable for a gear oil, transmission fluid or axle fluid.
Controlled release of an antiwear agent can be accomplished using a gel
composed of
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a. about 45 wt % of an overbased detergent,
b. about 10 wt % of a 2000 MW polyisobutenyl succan;
c. about 15 wt % of a succinimide dispersant, and
d. about 30 wt % of an amine salt of a phosphorus ester acid.
A manual transmission fluid is passed over the controlled release gel
containing the antiwear agent. The resulting composition contains an
acceptable
amount of antiwear agent to allow the fluid to be used as an axle fluid.
A FZG scuffing test is carried out on the manual transmission fluid (MTF)
and the manual transmission fluid containing antiwear agent from the
controlled
release gel (MTFGAW). The FZG scuffing test is carried out using "AlO" type
gears of about 10mm face width, at a pitchline velocity of about 16.6 m/s in
reverse
direction and at about 120 C (test also referred to as A10/16.6R/120 test).
The
results obtained are shown in Table 1.
Table 1
Sample Load Stage Fail
MTF 5
MTFGAW 7
The results indicate that the controlled release gel is capable of modifying a
lubricant designed for one mechanical device and providing desired additional
additives to provide a lubricant with a different composition with acceptable
properties in another mechanical device requiring a different lubricant
additive
composition.
