Title of Invention

ANTI-SEIZE COMPOSITION IN SOLID FORM

Abstract The invention discloses An anti-seize composition comprising: a solid anti-seize lubricant selected from the group consisting of metallic powders or flakes, non-metallic lubricants, and metal oxides, hydroxides and fluorides; and a carrier having said anti-seize lubricant dispersed therein, said carrier selected from the group consisting of grease, oil, polymeric matrix, wax having a viscosity of less than 44 cSt (200 SUS) at 100°F (37°C), naphthenic petroleum oil having a viscosity of less than 66 cSt (300 SUS) at 100°F (37°C) and having an API gravity at 60°F (15°C) from 23 to 25, said carrier being present in an amount to render said composition non-flowable at temperatures greater than 120°F (50°C), wherein said composition is dispensable at room temperature without the application of heat and has a Mil-907-E breakaway torque of less than 250 foot-pounds (12KPa).
Full Text ANTI-SEIZE COMPOSITION IN SOLID FORM
BACKGROUND OF THE INVENTION
Field of the Invention
[0001] The present invention relates to lubricant compositions useful for preventing
seizing of threaded fasteners. More particularly, the present invention relates to anti-seize
lubricant compositions in non-flowable or solid form, which can be packaged in a convenient
pocket-sized applicator dispenser.
Brief Description of Related Technology
[0002] U.S. Patent No. 5,498,351 (Heffling) claims a process for making anti-seize
lubricant compositions, and sets forth compositions of this type which include naphthenic oil,
lubricating grease, graphite, silicon fluid, and metal flake/oil suspension (65% aluminum flake
and 35% oil). The compositions described are not in a solid form, but are generally formed as
paste-like consistencies and are typically applied by dipping or brushing techniques.
[0003] Henkel Loctite Corporation has sold many flowable anti-seize lubricant
compositions. For instance, C5-A Copper Anti-Seize is a suspension of copper and graphite in a
high-quality grease, which protects metal parts from rust, corrosion, galling, and seizing at
temperatures to 1800°F (982°C), and tested to MIL(PRF)-A-907-E; Nickel Anti-Seize is a
copper-free product, recommended for stainless steel and other metal fittings to prevent
corrosion, seizing, and galling in harsh, chemical environments, and temperatures to 2400°F
(1315°C); Moly Paste is a low friction product, which lubricates press fits, protects during break-
in and under high static loads up to 750°F (400°C); Silver Grade Anti-Seize is a temperature-
resistant, petroleum-based inert lubricant compound fortified with graphite and metallic flake,
which will not evaporate or harden in extreme cold or heat and is for use in assemblies up to
1600°F (871 °C); Heavy Duty Anti-Seize is a metal free product, which provides excellent
lubricity, outstanding lubrication to all metals including stainless steel, aluminum, and soft
metals up to 2400°F (1315°C); Marine Grade Anti-Seize is formulated to protect assemblies
exposed directly or indirectly to fresh and salt water; Marine Grade Anti-Seize works well in
high humidity conditions, and has excellent lubricity, superior water wash-out and water spray
resistance, and prevents galvanic corrosion, protects in temperatures from -29°C to 1315°C (-
20T to 2400°F); Graphite-50 Anti-Seize is an electrically conductive, non-metallic product,
which is temperature resistant up to 900°F (482°C); Moly-50 Anti-Seize is a thread lubricant,
which is temperature resistant to 750T (400°C) and provides excellent lubricity; Zinc Anti-Seize
protects aluminum and ferrous surfaces from seizure and corrosion up to 750°F (400°C); Food
Grade Anti-Seize prevents seizure, galling, and friction in stainless steel and other metal parts up
to 750°F (400°C); N-1000 High Purity Anti-Seize is a copper-based product, which is suitable
for long-term, stainless steel applications and high-nickel, alloy bolting; N-5000 High Purity
Anti-Seize is a nickel-based product, which lubricates and protects Class 1,2 and 3 power plant
hardware and is recommended for highly corrosive environments to 2400°F (1315°C); High
Performance N-5000 High Purity Anti-Seize is also a nickel-based product, which provides
maximum lubricating and anti-seize properties for Class 1,2 and 3 power plant hardware.
Temperature resistant to 2400°F (1315°C); N-7000 High Purity Anti-Seize is a metal-free
product which provides high levels of purity and excellent lubricating properties for Class 1,2
and 3 power plant hardware; and White Hi-Temp Anti-Seize is a non-metallic product which
protects against high temperature seizing and galling of mated metal parts, up to 2000°F
(1093°C), while demonstrating excellent lubricity and use on various metals, such as copper,
brass, cast iron, steel and all alloys including stainless steel.
[0004] Recently it has become popular to place or to formulate certain adhesives,
sealants, coatings and related products in a solid, stick-like form for easy transport and ready
application by the end user. Examples of such products include "Semi-Solid Compositions for
Removing Cured Product" (such as is described in International Patent Publication No. WO
01/92430), "Semi-Solid One- or Two-Part Compositions" (such as is described in International
Patent Publication No. WO 01/92434), "Semi-Solid Primer Compositions" (such as is described
inlnternational Patent Publication No. WO 01/92435), "Spreadable Adhesive Compositions and
Applicators for Use Therewith" (such as is described in International Patent Publication No. WO
01/91915) and "Polymerizable Compositions in Non-Flowable Forms" (such as is described in
International Patent Publication No. WO 00/25628). All of these examples of solid adhesives,
sealants and coatings and related products in a solid or semi-solid form are intended to be
dispensed from a lipstick-type dispenser in which a mechanism at the base of the dispenser
advances the solid or semi-solid product through an opening at the opposite end of the dispenser.
[0005] International Patent Publication No. WO 00/44528 describes a solid anti-galling
agent that includes an anti-seize agent, hard waxes of long chain esters and alcohols having free
carboxyiic acid groups, such as candelilia or carnauba vegetable waxes, a moderate to high
viscosity petroleum oil of 110 to 1320 cSt (500 to 6,000 SUS), and surfactant, such as
propoxylated myristyl alcohol or dodecylbenzene sulfonic acid. The surfactant is included at 15
to 25% and is apparently required to maintain the homogeneity of the components and to soften
and/or wet the hard waxes used therein. Such formulations are believed to be commercial
products of LA-CO Industries, Inc., Elk Grove Village, IL. which markets an E-Z Break Twist-
Stick, Copper Grade, anti-seize formulation.
[0006] Other commercial anti-seize formulations in semi-solid form are available. For
example, AS-201 Stick is a semi-solid anti-seize formulation offered by Dyna Systems, Dallas,
TX. This product is offered in a twist-up holder, but is a relatively soft semi-solid which retards
retractability back into the container. Furthermore, the product is described as having storage
and handling limitation of less than about 50°C (120°F). Kar Products of Des Plaines, IL,
markets a Kar Anti-Seize Stick. The stick is made from aluminum complex grease, paraffin
wax, microcrystalline wax, aluminum powder and copper powder. The stick is a hard wax-based
formulation, which is not typically amenable to good spreadability over substrate surfaces. Hard
waxes also tend to crumble or crack, which also causes poor spreadability.
[0007] There is a need for an anti-seize composition in solid form having sufficient
spreadability to evenly coat substrate surfaces while having dimensional stability to be stored
and retractably dispensed from a container. More particularly, there is a need in the art for a
non-flowable anti-seize formulation having dimensional stability up to and exceeding 50°C
(120°F) so that it may be used in a variety of industrial settings.
SUMMARY OF THE INVENTION
[0008] The present invention satisfies a product profile, which confers anti-seize
properties up to a temperature of 1800°F or greater onto parts on which the inventive formulation
is applied. The anti-seize stick formulation has dimensional stability of up to 120°F (50°C) or
greater, for instance 130°F (55°C) or greater, indicating that the formulation supports its own
weight and does not change shape under gravitational forces. Moreover, the anti-stick
formulation of the present invention is not so hard, often having a penetration value less than 400
dmm, as to retard even spreadability. Desirably, the anti-seize composition of the present
invention includes one or more anti-seize lubricants, a matrix material, such as a polymeric
material, a grease and an oil, such that the above desirable properties are satisfied.
[0009] In one aspect of the present invention, an anti-seize composition includes, but is
not limited to, a solid anti-seize lubricant selected from the group consisting of metallic copper,
metallic nickel, metallic aluminum, metallic lead, metallic zinc, graphite, calcium oxide, calcium
carbonate, calcium fluoride, calcium stearate, lithium, molybdenum disulfide, boron nitride,
barium sulfate, or combinations thereof and a carrier for dispersing the lubricant. The carrier
includes grease, oil and a matrix material. The matrix material is a polymeric material, for
instance a hydroxy or amine modified aliphatic hydrocarbon polymeric material having a melting
point from 76°C to 93°C (170°F to 200°F). The carrier is present in an amount to render the
composition dimensionally stable and non-flowable at temperatures greater than 50°C (120°F).
Moreover, the composition is dispensable at room temperature without the application of heat
and has an unworked ASTM D 217 penetration at 25°C from 20 to 100 tenths of a millimeter.
Optionally, a wax, for instance a refined paraffin wax with a viscosity of less than 44 cSt (200
SUS) at 37°C (100°F) may also be included.
[0010] In another aspect of the present invention, an anti-seize composition having a
MIL(PRF)-A- 907E breakaway torque of less than 11.97 Kpa (250 foot-pounds) includes, but is
not limited to. a solid anti-seize lubricant and a carrier dispersing lubricant where the
composition is dispensable and spreadabie at room temperature without the application of heat.
The carrier includes, but is not limited to, grease, oil and a matrix material. The matrix material
is a polymeric material, for instance a hydroxy or amine modified aliphatic hydrocarbon
polymeric material having a melting point from 76°C to 93°C (170°F to 200°F). The carrier is
present in an amount to render the composition dimensionally stable and non-flowable at about
room temperature or greater. Optionally, a wax, for instance a refined paraffin wax with a
viscosity of less than 44 cSt (200 SUS) at (37°C)100°F, may also be included.
[0011] In yet another aspect of the present invention, an anti-seize composition is
provided which includes, but is not limited to, a solid anti-seize lubricant selected from the group
consisting of metallic copper, metallic nickel, metallic aluminum, metallic lead, metallic zinc,
graphite, calcium oxide, calcium carbonate, calcium fluoride, calcium stearate, lithium,
molybdenum disulfide, boron nitride, barium sulfate, or combinations thereof and a carrier which
is a solid at room temperature or greater and having the lubricant dispersed therein. The
carrier includes a grease, a naphthenic petroleum oil having a viscosity of less than 66 cSt (300
SUS) at 37°C (100°F) and having an API gravity at 15°C (60°F) from 23 to 25, and a polymeric
material, for instance, a hydroxy, amide or amine modified aliphatic hydrocarbon polymeric
material having a melting point from 76°C to 93°C (170T to 200°F). The composition is
dispensable at room temperature without the application of heat. Optionally, a wax, for instance,
a refined paraffin wax with a viscosity of less than 44 cSt (200 SUS) at 27°C (100°F), may also
be included.
[0012] The present invention also contemplates a method of making the non-flowable
anti-seize composition, as well as a method of using the non-flowable anti-seize composition
[0013] The present invention also contemplates an article of manufacture. In this
embodiment there is included a dispensing container for housing and dispensing a non-flowable
anti-seize composition. The container includes a generally elongate hollow body having first and
second ends, with one of the ends having a dispense opening. The container houses the non-
flowable anti-seize composition.
[0014] It is surprising to be able to manufacture an anti-seize formulation, such as one
that performs along the lines of one or more of the Loctite anti-seize products described above in
a solid, yet spreadable, form, because much of the anti-seize compositions are non-polar, liquid
hydrocarbons, whereas the polymeric materials used in the inventive anti-seize compositions are
solids, which are more polar in nature. The polarity difference inherently renders the two types
of materials physically incompatible and the liquid nature of the one and the solid nature of the
other also adds to their incompatibility.
(0015] The present invention overcomes these issues of incompatibility by mixing the
two types of materials at elevated temperature conditions sufficient to render the mixture a
substantially homogenous flowable mass.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] FIG. 1 is a perspective view of a lipstick-type dispenser container with a dispenser
cap.
(0017] FIG. 2 is a perspective view of a lipstick-type container showing the anti-seize
composition of the present invention contained therein.
[0018] FIG. 3 is a perspective view of a dispenser container showing a notched rim at the
dispense opening.
[0019] FIG. 4 shows a dispense container having a concave section at its dispense
opening for receiving geometrically complimentary parts.
[0020] FIG. 5 shows a dispense container having both a concave section and a notched
section at its dispense opening rim.
[0021] FIG. 6 is a perspective view of a dispensing container showing the dispense
opening being concave.
[0022] FIG. 7 is a perspective view of a container and cap showing the dispense opening
defined by slotted apertures.
[0023] FIG. 8 shows a perspective view of a container and cap having the dispense
opening defined by generally circular apertures.
[0024] FIG. 9 is a perspective view of a dispense container and cap showing the dispense
opening having a concave surface portion and slotted apertures therein.
[0025] FIG. 10 is a perspective view of a cap for a dispense container with one end being
concave.
[0026] FIG. 11 shows a top view of the cap of FIG. 10 showing elongate apertures for
dispensing compositions.
DETAILED DESCRIPTION OF THE INVENTION
[0027] The anti-seize compositions of the present invention are non-flowable and
dimensionally stable, i.e., they are capable of existing in a self-supporting mass without
migrating at temperatures of at least 70°F (21°C), desirably 120°F (49°C) up to at least 130°F
(55°C). In practical applications, these compositions are provided in an applicator such that they
can be conveniently dispensed to the desired location, such as by a pocket-sized or hand-held
lipstick-type container, which can be easily carried by a mechanic or maintenance worker for use
as needed. Such a dispenser, within which is dispensed on the inventive anti-seize composition,
solves many problems, such as spillage in the environment in which it is used, which can be
particularly problematic where sensitive parts are present and susceptible of contamination or
when migration of an anti-seize composition is generally undesirable.
[0028] The present invention provides anti-seize compositions in a spreadable, yet
dimensionally stable and solid form. The inventive compositions are based on an oil, a grease, a
matrix material, such as a polymeric matrix material, and a high melting point metal powder
(such as copper powder), and/or graphite. These different constituents are further described
hereinafter. Optionally, the inventive formulation may also include a wax, particularly a refined
paraffin wax with a viscosity of less than 44 cSt (200 SUS) at 37"C (100°F).
[0029] The inventive solid anti-seize lubricant composition includes anti-seize lubricants,
which are high melting point particles, such as powders or flakes. Useful high melting point
particles include those having an average melting point temperature above 500°F (260°C).
Desirably, the average melting point is greater than 1000°F (540°C) or higher, for example
greater than 1600°F (870°C). Useful, solid anti-seize lubricants include, but are not limited to,
metallic powders or flakes, non-metallic lubricants, and metal oxides, hydroxides and fluorides.
Non-limiting examples of metallic powders or flakes include copper, nickel, aluminum, lead,
zinc, chromium, cobalt, manganese, molybdenum, and steel, such as stainless steel. Non-
limiting examples of non-metallic lubricants include graphite, molybdenum disulfide, boron
nitride, polyethylenefluoroethylene (PTFE), mica, and/or talc. Non-limiting examples of metal
oxides, hydroxides and fluorides include calcium oxide, calcium fluoride, zinc oxide, titanium
dioxide, magnesium oxide, calcium hydroxide, barium oxide and/or tin oxide.
[0030] The solid anti-seize lubricants are generally powdered or flaked materials that are
ground or formed into a small or fine particle size. Generally, particles sizes are in the micron-
sized ranges. Particles sizes of less than 150 microns (or 100 mesh) are useful. Average
particles sizes of 100 microns or less (or 150 mesh or greater) are also useful. Desirably, the
average particle size is less than about 10 microns to 60 microns.
[0031] Grease is a mixture of a fluid lubricant, usually petroleum oil or synthetic oil, and
a thickener, usually soap, dispersed in the lubricant. Soap thickeners may formed by reacting,
i.e., saponifying, a metallic hydroxide, or alkali, with a fat, fatty acid, or ester. The type of soap
used depends on the grease properties desired. Calcium (lime) soap greases are highly resistant
to water, but unstable at high temperatures. Sodium soap greases are stable at high temperatures,
but wash out in moist conditions. Lithium soap greases resist both heat and moisture. Mixed-
base soap is a combination of soaps, offering some of the advantages of each type. A complex
soap is formed by the reaction of an alkali with a high-molecular-weight fat or fatty acid to form
soap, and the simultaneous reaction of the alkali with a short-chain organic or inorganic acid to
form a metallic salt (the complexing agent). Complexing agents usually increase the dropping
point of grease. Lithium, calcium, and aluminum greases are common alkalis in complex-soap
greases. Non-soap thickeners, such as clays, silica gels, carbon black, and various synthetic
organic materials are also used in grease manufacture.
[0032] Greases useful in forming the anti-seize composition of the present invention
include calcium, sodium, lithium, aluminum, bentonite clay and silica containing greases.
Polymer thickened greases, such as polyurea greases are also useful. Desirably, the grease is a
calcium/lithium grease having from 5 to 10 weight percent lithium/calcium thickener combined
with a base oil having a viscosity from 66 to 77 cSt (300 to 350 Saybolt Universal Seconds
(SUS)) at 50°C (100°F). Such a grease also has a consistency or penetration useful for the anti-
seize composition of the present invention.
[0033] Consistency or penetration of grease is a measure of the consistency of grease,
utilizing a penetrometer. Penetration is reported as the tenths of a millimeter (penetration
number) that a standard cone, acting under the influence of gravity, will penetrate the grease
sample under test conditions prescribed by test method ASTM D 217. Standard test temperature
is 25°C (77°F). The higher the penetration number, the softer the grease. Undisturbed
penetration is the penetration of a grease sample as originally received in its container.
Unworked penetration is the penetration of a grease sample that has received only minimal
handling in transfer from its original container to the test apparatus. Worked penetration is the
penetration of a sample immediately after it has been subjected to 60 double strokes in a standard
grease worker; other penetration measurements may utilize more than 60 strokes. Block
penetration is the penetration of block grease (grease sufficiently hard to hold its shape without a
container). Desirably, greases with ASTM D 217 worked or unworked penetrations from about
200 to about 400 mm at 77°F (25°C) are useful with the practice of the present invention. More
desirably, greases with ASTM D 217 worked or unworked penetrations from 250 to 350 mm at
77°F (25°C) are useful with the practice of the present invention.
[0034] The National Lubricating Grease Institute (NLGI) number is a series of
penetration numbers classifying the consistency range of lubricating greases, based on the
ASTM D 217 cone penetration number. The NLGI grades are in order of increasing consistency
(hardness). Desirably, the grease used with the practice of the present invention has a NLGI
grade from about 0 to about 3, or an ASTM D 217 worked penetration from 220 to
385 mm at 77°F (25°C). More desirably, the grease used with the practice of the
present invention has a NLGI grade of 2, or an ASTMD217 worked penetration from
265 to 295 mm at 77°F (25°C).
[0035] Harder greases, such as block greases, which are solid and can maintain their
shape at room temperature, or other greases with higher NLGI grades or lower penetration
values, may not result in good spreadability, i.e., an even coating without gaps on a substrate that
is easily applied by simply rubbing the composition over the substrate, of the anti-seize
composition. Softer greases may improve spreadability, but may result in poor dimensional
stability of a solid anti-seize composition.
[0036] The anti-seize composition further includes an oil to control, in part, the
spreadability of the composition. Useful oils include petroleum oils; mineral oils; synthetic oils,
such as silicone oils, ester-based oils, olefin-based oils, glycol oils, and the like; vegetable oils,
such as castor oil, coconut oil, corn oil, cotton seed oil, linseed oil, palm oil, and the like; and
animal oils, such as fish oils, sperm oil, and the like.
[0037] Desirably, the oil is a severely hydrotreated, naphthenic oil derived from
petroleum. Useful severely hydrotreated, naphthenic oils include oils having a viscosity of 18 to
66 cSt (80 to 300 SUS) at 37°C (100°F) and an API gravity of 22 to 26 at 15°C (60°F). More
desirably, the severely hydrotreated, naphthenic oils include oils having a viscosity of 22 to 25
cSt (100 to 110 SUS) at 37°C (100°F) and an API gravity of 24.5 to 25.5 at 15°C (60°F).
[0038] The anti-seize composition also includes a polymeric matrix. The polymeric
matrix includes an organic material which generally has a melting point or softening point range
in the range of 150°F (65°C) to 500°F (260°C), more desirably from 180°F (82°C) to 300°F
(150°C). Polymeric matrix materials useful in the present invention may be selected from
polyamides, polyacrylamides, polyimides, polyhydroxyalkylacrylates, urea-urethanes, hydroxy
or amine modified aliphatic hydrocarbons (such as castor oil-based rheological additives), liquid
polyester-amide-based rheological additives and combinations thereof. Of particular utility are
hydroxy or amine modified aliphatic hydrocarbons and liquid polyester-amide-based rheological
materials having a melting point of 170°F to 200°F (76°C to 93°C).
[0039] Non-limiting examples of hydroxyl, amide or amine modified aliphatic
hydrocarbons include THIXCIN R, THIXCIN GR, THIXATROL ST and THIXATROL GST
available from Rheox Inc., Hightstown, N.J. These modified aliphatic hydrocarbons are castor
oil based materials. The hydroxyl modified aliphatic hydrocarbons are partially dehydrated
castor oil or partially dehydrated glycerides of 12-hydrostearic acid. These hydrocarbons may be
further modified with polyamides to form polyamides of hydroxyl stearic acid. Certain of the
THIXCIN products include metallic additives, as well. Desirably, the hydroxy, amide or amine
modified aliphatic hydrocarbon is THIXCIN R.
[0040] Liquid polyester-amide based rheolgical additives include THIXATROL TSR,
THIXATROL SR and THIXATROL VF rheological additives available from Rheox Inc.,
Hightstown, N.J. These rheological additives are described to be reaction products
polycarboxylic acids, polyamines, alkoxylated polyols and capping agents. Useful
polycaboxylic acids include sebacic acid, poly(butadiene) dioic acids, dodecane dicarboxylic
acid and the like. Suitable polyamines include diamine alkyls. Capping agents are described as
being monocarboxylic acids having aliphatic unsaturation.
[0041] The present invention includes the polymeric matrix, such as the above-
mentioned hydroxyl, amide or amine modified aliphatic hydrocarbons, often in amounts of 2%
to 20% by weight of the total composition. When present in these amounts, the non-flowability
characteristics of a composition can be obtained with minimal undesirable effects, such as loss of
anti-seize lubrication or spreadability characteristics. The constituents of the anti-seize
composition should be heated, such as when the anti-seize lubricants and the polymeric matrix
are mixed together. For instance, it is desirable to heat the mixture to 100°C (212°F) to improve
the retractability of the end use anti seize product.
[0042] The polymeric matrix materials of the present invention desirably have a particle
size less than about 100 microns, although other particle sizes are useful. Desirably, the average
particle size is less than 50 microns.
[0043] Another polymeric matrix useful herein includes polyamide materials. One such
polyamide has a melting point of 260°F (127°C) and is commercially available as a non-reactive
free flowing powder under the tradename DISPARLON 6200, from King Industries Specialties
Company, Norwalk, CT. Other polyamides include DISPARLON 6100 and 6500.
[0044] Another polymeric matrix useful herein includes a combination of an alkali metal
cation and the reaction product of (a) a polyfunctional isocyanate and an hydroxy and an amine;
or (b) a phosgene or phosgene derivative, and a compound having 3 to 7 polyethylene ether units
terminated at one end with an ether group and at the other end with a reactive functional group
selected from an amine, an amide, a thiol or an alcohol; or (c) a monohydroxy compound, a
diisocyanate and a polyamine. When the reaction product described in (c) is employed it is
generally formed by first reacting a monohydroxy compound with a diisocyanate to form a
mono-isocyanate adduct, and subsequently reacting the mono-isocyanate reaction product with a
polyamine in the presence of an alkali metal salt and aprotic solvent, as described in U.S. Patent
No. 4,314,924. A commercially available version of the reaction product described in (c) is
believed to be BYK-410, from BYK-Chemie, Wallingford, CT. BYK-Chemie describes this
reaction product as a urea-urethane.
[0045] Useful isocyanates for forming the reaction product(s) of the additive include
polyisocyanates such as phenyl diisocyanate. toluene diisocyanate, 4,4'-diphenyl diisocyanate.
4,4'-diphenylene methane diisocyanate, dianisidine diisocyanate, 1,5-naphthalene diisocyanate,
4,4'-diphenyl ether diisocyanate, p-phenylene diisocyanate, 4,4'-dicyclo-hexylmethane
diisocyanate, l,3-bis-(isocyanatomethyl) cyclohexane, cyclohexylene diisocyanate,
tetrachlorophenylene diisocyanate, 2,6-diethyl-p-phenylenediisocyanate, and 3,5-diethyl-4,4'-
diisocyanatodiphenylmethane. Still other polyisocyanates that may be used are polyisocyanates
obtained by reacting polyamines containing terminal, primary and secondary amine groups or
polyhydric alcohols, for example, the alkane, cycloalkane, alkene and cycloalkane polyols such
as glycerol, ethylene glycol, bisphenol-A, 4,4'-dihydroxy-phenyldimethylmethane-substituted
bisphenol-A, and the like, with an excess of any of the above-described isocyanates.
[0046] Useful alcohols for reacting with the polyisocyanates also include polyethyl
glycol ethers having 3-7 ethylene oxide repeating units and one end terminated with an ether or
an ester, polyether alcohols, polyester alcohols, as well as alcohols based on polybutadiene. The
specific type of alcohol chosen and the molecular weight range can be varied to achieve the
desired effect Generally, monohydroxy compounds, straight or branched chain aliphatic or
cyclic primary or secondary alcohols containing C5.25, and alkoxylated derivatives of these
monohydroxy compounds are useful.
[0047] Phosgene and phosgene derivatives, such as bischloroformates, may be used to
make the reaction product of the additive (c). These compounds are reacted with a nitrogen-
containing compound, such as an amine, an amide or a thiol to form the adduct Phosgenes and
phosgene derivatives may also be reacted with an alcohol to form the reaction product.
[0048] The alkali metal cations are usually provided in the form of a halide salt For
example, sodium, potassium and lithium halide salts are useful. In particular, sodium chloride,
sodium iodide, sodium bromide, potassium chloride, potassium iodide, potassium bromide,
lithium chloride, lithium iodide, lithium bromide and combinations thereof may be employed.
[0049] The reaction products of additive (c) of the present invention are usually present
in and added to the composition with an alkali metal salt, in a solvent carrier. The solvents are
desirably polar aprotic solvents in which the reaction to form the reaction product was carried
out. For example, N-methyl pyrrolidone, dimethylsulfoxide, hexamethylphosphoric acid
triamide, N,N-dimethylformamide, N,N,N',N'-tetramethylurea, N,N-dimethylacetamide, N-
butylpyrrolidone, tetrahydrofuran and diethylether may be employed.
[0050] One particularly desirable additive is the combination of a lithium salt and a
reaction product which is formed by reacting a monohydroxy compound with a diisocyanate
compound to form a mono-isocyanate first adduct, which is subsequently reacted with a
polyamine in the presence of lithium chloride and 1 -methy-2-pyrrolidone to form a second
adduct. A commercially available additive of this sort is sold by BYK Chemie, Wallingford, CT
under the tradename BYK 410. This commercially available additive is described by BYK-
Chemie product literature as being a urea urethane having a minor amount of lithium chloride
present in a 1-methyl-2 pyrrolidone solvent.
[0051] Amines which can be reacted with phosgene or phosgene derivatives to make the
reaction product include those which conform to the general formula R11-NH2, where R11 is
aliphatic or aromatic. Desirable aliphatic amines include polyethylene glycol ether amines.
Desirable aromatic amines include those having polyethylene glycol ether substitution on the
aromatic ring.
[0052] For example, commercially available amines sold under the tradename
JEFF AMINE by Huntsman Corporation, Houston, Texas, may be employed. Examples include
JEFFAMINE D-230, JEFFAMINE D-400, JEFFAMINE D-2000, JEFFAMINE T-403,
JEFFAMINE ED-600, JEFFAMINE ED-900, JEFFAMINE ED-2001, JEFFAMINE EDR-148,
JEFFAMINE XTJ-509, JEFFAMINE T-3000, JEFFAMINE T-5000, and combinations thereof.
where R may be an aliphatic or aromatic, substituted or unsubstituted, hydrocarbon or
heterohydrocarbon, substituted or unsubstituted, having C1-36.
[0058] Alcohols useful in forming the reaction product with the phosgene or phosgene
derivatives include those described above.
[0059] Waxes useful as an optional component in the inventive compositions include
petroleum waxes, vegetable waxes, insect waxes, animal waxes and synthetic waxes. Waxes
may be characterized by a number of physical properties, including melting point and hardness
(or penetration). Penetration of a wax is a measure of the hardness of the wax, utilizing a
penetrometer. Penetration is reported as the depth, in tenths of millimeter or dram, to which a
standard needle penetrates the wax under conditions described in test method ASTM D 1321.
Prior to penetration, the wax sample is heated to 17°C (30°F) above its congealing point, air
cooled, then conditioned at a test temperature in a water bath, where the sample remains during
the penetration test. The test temperature may be controlled at different values depending upon
the particular wax to be analyzed. For softer or unrefined waxes ASTM D 937 prescribes the use
of a cone instead of a needle.
[0060] Petroleum wax includes a range of relatively high-molecular-weight hydrocarbon:
(approximately C16 to C50), is solid at room temperature, and is derived from higher boiling
petroleum fractions. Three basic categories of petroleum-derived or shale-oil-derived waxes
include paraffin (crystalline) wax, microcrystalline wax and petrolatum wax. Paraffin waxes are
produced from the lighter lube oil distillates, generally by chilling the oil and filtering the
crystallized wax. Paraffin waxes have a distinctive crystalline structure and have a melting point
range generally between 48°C (118°F) and 71°C (160°F). Paraffin wax is macrocrystalline and
is composed of 40-90 wt % normal alkanes with a remainder of C18-C36 isoalkanes and
cycloalkanes. Fully refined paraffin has less than 1 wt %; crude scale, 1-2 wt %, and slack
[64742-61-61], above 2 wt %. Paraffin wax is a petroleum-derived wax usually consisting of
high-molecular-weight normal paraffins; distinct from other natural waxes, such as beeswax and
carnauba wax (palm tree), which are composed of high-molecular-weight esters, in combination
with high-molecular-weight acids, alcohols, and hydrocarbons. Refined paraffin waxes are low
oil, or low liquid paraffin, content waxes, generally with an oil content of 1.0 weight percent or
less, under conditions prescribed by test method ASTM D 721. Fully refined paraffin waxes
generally have even lower oil content of 0.5 weight percent or less under the same conditions.
[0061] Microcrystalline waxes are produced from heavier lube distillates and residua
usually by a combination of solvent dilution and chilling. They differ from paraffin waxes in
having poorly defined crystalline structure, darker color, higher viscosity, and higher melting
points which typically range from 63°C (145°F) to 93°C (200°F). Microcrystalline waxes
contain more branched and cyclic compounds than paraffin waxes and also vary more widely
than paraffin waxes in their physical characteristics. Microcrystalline waxes can be somewhat
ductile, but are also often brittle and crumble easily.
[0062] Petrolatum waxes (CAS Registry No. 8009-0-8) are derived from heavy residual
lube stock by propane dilution and filtering or centrifuging. They are microcrystalline in
character, semisolid at room temperature and consist predominantly of saturated crystalline and
liquid hydrocarbons having carbon numbers greater than C25.
[0063] Useful insect and animal waxes include, but are not limited to, beeswax,
spermaceti wax, Chinese wax, wool wax, and shellac wax. The major components of beeswax
(CAS Registry No. 8012-89-3) are esters of C30 and C32 alcohols with C16 acids, free C25 to C31
carboxylic acids, and C25 to C31 hydrocarbons. Beeswax typically has a melting point of 60 to
70°C, a penetration (hardness) of 20 dmm at 25°C (ASTM D1321). Spermaceti wax (CAS
Registry Nos. 8002-23-1 and 68910-54-3) is derived from the sperm whale and has a melting
point of 42 to 50°C. Chinese wax (CAS Registry No. 8001-73-8) is formed on branches of ash
trees {Fraximus chinensis) from the secretion of the coccus insect {Coccus ceriferus). It is a hare
wax with a melting point of 80 to 84°C. Wool wax (CAS Registry No. 68815-23-6) or lanolin
wax (CAS Registry No. 68201-49-0) is extracted from sheep's wool and has a melting point of
36 to 43°C. Shellac wax is obtained from the lac of a scale insect (Coccus laced) that feeds on
certain trees in southern Asia and has a melting point of 79 to 82°C.
[0064] Useful vegetable waxes include, but are not limited to, carnauba wax, candelilla
wax, Japan wax, ouricury wax, rice-bran wax, jojoba wax, castor wax, bayberry wax, and soy
bean wax. Carnauba wax (CAS Registry No. 8015-86-9) is produced from fronds of a palm tree.
The major components of carnauba wax are aliphatic and aromatic esters of long-chain alcohols
and acids, with smaller amounts of free fatty acids and alcohols, and resins. Carnauba wax is
very hard with a penetration of about 2 dmm at 25°C and has a melting point of 83 to 86°C.
Candelilla wax (CAS Registry No. 8006-44-8) is produced from shrubby spurges (Euphorbia
antisyphilitica) native to southwest Texas and Mexico. The major components of candelilla wax
are hydrocarbons, esters of long-chain alcohols and acids, long-chain alcohols, sterols, and
neutral resins, and long-chain acids. Typically, candelilla wax has a melting point of 67 to 70°C
and a penetration of 3 dmm at 25°C. Japan wax (CAS Registry No. 8001-39-6) is derived from
the berries of a small tree native to Japan and China cultivated for its wax. Japan wax is
composed of triglycerides, primarily tripalmitin.Japan wax typically has a melting point of 48 to
53°C. Ouricury wax (CAS Registry No. 68917-70-4) is a brown wax obtained from the fronds
of a palm tree which grows in Brazil and has a melting point of
79 to 84°C. Rice-bran wax (CAS Registry No. 8016-60-2) is extracted from crude rice-bran oil
and has a melting point of 75 to 80°C. The wax is primarily composed of esters of lignoceric
acid, behenic acid, and C22-C36 alcohols. Jojoba wax (CAS Registry No. 61789-91-1) is obtainec
from the seeds of the jojoba plant. Castor wax (CAS Registry No. 8001-78-3) is catalytically
hydrogenated castor bean oil. Bayberry wax (CAS Registry No. 8038-77-5) is obtained from the
surface of the berry of the bayberry (myrtle) shrub. The wax is made up primarily of lauric,
myristic, and palmitic acid esters. The wax has a melting point of 45 to 49°C.
[0065] Useful mineral waxes include, but are not limited to, montan wax, peat wax,
ozokerite wax and ceresin wax. Montan wax (CAS Registry Nos. 8002-53-7) is derived by
solvent extraction of lignite. The wax components of montan is a mixture of long chain (C24-
C30) esters, long-chain acids, and long chain alcohols, ketones, and hydrocarbons. Crude montan
wax from Germany typically has a melting point of 76 to 86°C. Peat waxes are much like
montan waxes and are obtained from peat and has a melting point of 73 to 76°C. Ozokerite wax
(CAS Registry No. 001-75-0) was originally a product of Poland, Austria and the former USSR
where it was mined and has a melting point of 74 to 75°C. Ceresin wax (CAS Registry No.
8001-75-0) originally was a refined and bleached ozokerite wax.
[0066] Synthetic waxes include, but are not limited to, polyethylene waxes, polyethylene
oxide waxes, polyfluoro wax, polypropylene waxes, polytetra fluoro ethylene waxes, a-olefin
waxes, carbowaxes and halowaxes. Polyethylene waxes (CAS Registry No. 8002-72-4) are
obtained polymerization of polyethylenes or by Fischer-Tropsch synthesis. The waxes have
melting points ranging from 45-106°C. These waxes may also be chemically modified to vary
properties, such as acid number. Polymerized a-olefins can be produced to have wax-like
properties and are sold as synthetic waxes. The polymerization process yields highly branched
materials, with broad molecular weight distributions. Carbowaxes (CAS Registry Nos. 9004-74-
4 and 25322-68-3) are high molecular weight polyethylene glycols. Halowaxes (CAS Registry
Nos. 1321-65-9, 1335-87-1, 1335-88-2, 12616-35-2, 12616-36-3, 25586-43-0, 57817-66-7 and
58718-67-5) are chlorinated naphthalenes.
[0067] Desirably, the wax used in the anti-seize composition is a paraffin wax. More
desirably, the wax is a refined or fully refined paraffin wax derived from petroleum or shale oil.
Moderately soft waxes are also useful. For example, waxes, including paraffin waxes, with a
needle penetration (ASTM D 1321) of 8 to 30 dmm at 77°F (25°C) are useful. More desirably,
waxes, including paraffin waxes, with a needle penetration (ASTM D 1321) of 10 to 25 dmm at
77°F (25°C) are also useful. The use of such moderately soft waxes, as contrasted to harder
waxes, is believed to improve the spreadability of the anti-seize composition. The use of softer
waxes may result in an anti-seize composition not having adequate dimensional stability, i.e., a
flowable composition as contrasted to a non-flowable composition.
[0068] Thickeners, plasticizers, pigments, dyes, diluents, fillers, and other agents
common to the art can be employed in any reasonable manner to produce desired functional
characteristics, providing they do not significantly interfere with the anti-seize functionality.
[0069] Generally, the inventive anti-seize compositions include a solid anti-seize
lubricant in an amount from 10 to 60 weight percent on a total composition basis, and a carrier
in an amount from 10 to 30 weight percent on a total composition basis. More specifically, in
one aspect of the invention, the composition may include as the solid anti-seize lubricant,
graphite present from 10 to 30 weight percent on a total composition basis and copper present
from 10 to 30 weight percent on a total composition basis, and as the carrier, a polymeric
matrix present from 10 to 30 weight percent on a total composition basis, grease present from
10 to 40 weight percent on a total composition basis, and oil present from 20 to 60 weight
percent on a total composition basis. Desirably, the composition includes graphite present from
20 to 22 weight percent on a total composition basis, copper present from 16 to 18 weight
percent on a total composition basis, polymeric matrix present from 11 to 17 weight
percent on a total composition basis, grease present from 12 to 20 weight percent on a total
composition basis, and oil present from 25 to 40 weight percent on a total composition basis.
[0070] The anti-seize stick formulations of the present invention may be prepared by
placing the oil constituent and the grease constituent in a vessel and mixing these constituents of
the formulation. Desirably, these constituents are mixed at 1000 rpm under slightly elevated
temperature conditions, for example 80°C to 100°C. The matrix material may then be added,
while maintaining the temperature at 80°C to 100°C. The actual temperature used may vary
depending upon the melting point of the matrix material. After the matrix material has been
added, metallic powder and/or graphite may be added with the mixing speed increased to 1500
rpm. The so-formed anti-seize formulation is dispensed into lipstick-type dispensers while hot.
The dispensers are then allowed to cool to create the anti-seize stick formulations of the present
invention. The matrix material may be preheated to the above-described temperatures before its
addition.
[0071] One method for preparing a solid anti-seize composition includes the steps of (1)
selecting a grease with an ASTM D 217 penetration at 25°C from 200 to 400 tenths of a
millimeter; (2) selecting a naphthenic petroleum oil with a viscosity of less than 66 cSt (300
SUS) at 37°C (100°F) and with an API gravity at 15°C (60°F) from 23 to 25; (3) mixing the
grease and the oil to form a combined oil/grease composition; (4) adding and mixing into the
oil/grease composition a solid anti-seize lubricant selected from the group consisting of metallic
copper, metallic nickel, metallic aluminum, metallic lead, metallic zinc, graphite, calcium oxide,
calcium carbonate, calcium fluoride, calcium stearate, lithium, molybdenum disulfide, boron
nitride, barium sulfate, or combinations thereof; and a polymeric matrix and optionally a refined
paraffinic wax, which has a viscosity of less than 44 cSt (200 SUS) at 37°C (100°F), to form the
anti-seize composition. The method may further include the steps of heating polymeric matrix
and/or wax or the oil/grease composition to at least 80°C; maintaining the composition at least
80°C while mixing; and cooling the composition to
room temperature to solidify the composition. The method may further include the steps of
adding the composition at least 80°C into a dispensing container having a generally elongate
hollow body and having first and second ends, with one of said ends defining a dispense bottom
to releasably holding the composition, followed by cooling the composition to room temperature
to solidify the composition within the container.
[0072] The present invention also contemplates and article of manufacture which
includes the above-mentioned non-fiowable composition in a dispenser or applicator. Desirably
the dispenser is a pocket-size, lipstick-type dispenser which can be carried by the mechanic or
maintenance worker without fear of spillage or contamination of sensitive parts and used as
needed. The dispenser typically is generally elongate in shape and designed to mechanically
advance the composition through a dispense opening. The dispense opening can be defined as
the entire perimeter of the container wall or it can be smaller apertures located on the end surface
of the container. The perimeter or aperture which defines the dispense opening can be smooth,
notched or wavy, such as in a sinusoidal wave. Additionally, a portion of the dispense end of the
container can be concave to accommodate a threaded member or tubular body which requires
application of the composition.
[0073] Alternatively, the dispense end of the container may have a dispense opening
which is defined by apertures such as slots or holes on the top surface. These apertures can be
combined with other features described above, such as the concave surface or perimeter for
accommodating threaded members or other cylindrical parts.
[0074] The container is generally fitted with a cap which fits over and around the
container walls. The cap can also be designed at its closed end to have the concave portion
and/or apertures as defined previously.
[0075] At the container end opposite, i.e., the bottom end of the container, the dispense
opening is proximally located a mechanism for mechanically advancing the anti-seize
composition. These mechanisms are generally well known in the art and include a pusher means
which can include a knob located at the bottom of the container which when turned in one
direction advances the anti-seize composition contained therein to the dispense opening and
when turned in the other direction moves the anti-seize composition in the opposite direction.
[0076] The article of manufacture can be more particularly described referring to FIGs.
1-11. FIG. 1 shows dispense container 10 having a generally elongate tubular shape defined by
wall 20 and having a dispense end defined by perimeter 21. Cap 50 as shown is designed for
closingly engaging tubular wall 20 by fitting thereover.
[0077] Composition 30 is shown in FIG. 1 within container 10. FIG. 2 shows
composition 30 being advanced above perimeter 21 using knurled knob 40, which was turned to
advance the composition. Turning knob 40 in the opposite direction causes composition 30 to
descend back within the container.
[0078] FIG. 3 shows container 10 having a dispense perimeter defining the opening
being notched. Such a design could alternatively be sinusoidal or have other geometric shape
which can be tailored to the type of surface on which the composition is to be applied. For
example, FIG. 4 shows container 10 having opposed concave surfaces in its perimeter 23 for
accommodating parts having rounded surfaces such as a bolt, screw or rod-like parts. FIG. 5
shows a combination of opposed concave surfaces in perimeter 24 in combination with
oppositely opposed geometric portions of the same perimeter.
[0079J FIG. 6 shows container 10 having a large portion of its perimeter 25 having
opposed concave portions.
[0080] FIG. 7 shows container 10 having a dispense end with end surface 65 and
elongate apertures 70 through which the composition is dispensed.
[0082] FIG. 9 shows container 10 having an end surface 66 in which aperture 72 are both
elongate and concave since they follow the geometry of the end surface 66. Cap 51 for this
container fits around perimeter 80 and may be designed with or without apertures. In Figures 10
and 11, the design with apertures is shown, where cap 51 has elongate apertures which can be
opened or closed by closure means, not shown, and which can be fitted over perimeter 80.
[0083] The following non-limiting examples are intended to further illustrate the present
invention.
EXAMPLES
[0084] Non-flowable anti-seize compositions were prepared in accordance with the
formulations set forth below.
[0085] The compositions were prepared by placing a naphthenic oil and lithium/calcium
grease in a vessel and mixing these constituents of the formulation at 1000 rpm. While mixing,
these constituents were heated to 92 °C (200°F). Polymeric matrix, THIXCIN R, was then
added while the temperature and mixing were maintained. While mixing, metal and/or non-
metal powder was then added, followed by the addition of the synthetic graphite. Mixing
continued for 10 minutes. The so-formed anti-seize formulations were dispensed into lipstick-
type dispensers while hot. The dispensers were then allowed to cool to create the anti-seize stick
formulations of the present invention.
[0087] Composition B performed much like LOCTITE Copper (C5-A) Anti-Seize
Lubricant in terms of anti seize properties and average breakaway torque, and even showed
improved % water washout and % oil separation, which were 4 and 2.15, respectively, for
LOCTITE Copper (C5-A) Anti-Seize Lubricant.
[0088] Compositions A. 1 and A.2 performed much like LOCTITE Silver grade (767)
Anti-Seize Lubricant. Compositions A.l and A.2 were tested on 3/8"-16xl, 18-8 stainless steel
bolts, with matching 18-8 stainless steel nuts and washers on an Inconel 600 high temperature
block. Both nut and bolt threads were evenly coated with the anti-seize compositions A.l or A.2.
The nut was run on the end of the bolt to form an assembly, which was tightened with a Snap-On
torque wrench to 2.500 KPa (360 in-lbs). and exposed to the specified temperature for 24 hours.
Then the assembly was allowed to cool to room temperature. The nuts were loosened and
breakaway and prevailing torque were measured.
We claim:
1. An anti-seize composition comprising:
a solid anti-seize lubricant selected from the group
consisting of metallic powders or flakes, non-metallic
lubricants, and metal oxides, hydroxides and fluorides; and
a carrier having said anti-seize lubricant dispersed therein,
said carrier selected from the group consisting of grease,
oil, polymeric matrix, wax having a viscosity of less than
44 cSt (200 SUS) at 100°F (37°C), naphthenic petroleum oil
having a viscosity of less than 300 SUS at 100°F (37°C) and
having an API gravity at 60°F (15°C) from 23 to 25, said
carrier being present in an amount to render said composition
non-flowable at temperatures greater than 120°F (50°C),
wherein said composition is dispensable at room
temperature without the application of heat and has a Mil-
907-E breakaway torque of less than 250 foot-pounds (12KPa).
2. The composition of Claim 1, wherein said solid
anti-seize lubricant is selected from the group consisting of
copper, nickel, aluminum, lead, zinc, chromium, cobalt,
manganese, molybdenum, steel, and combinations thereof.
3. The composition of Claim 1, wherein said solid
anti-seize lubricant is selected from the group consisting of
metallic copper, metallic nickel, metallic aluminum, metallic
lead, metallic zinc, graphite, calcium oxide, calcium
carbonate, calcium fluoride, calcium stearate, lithium,
molybdenum disulfide, boron nitride, barium sulfate, and
combinations thereof.
4. The composition of Claim 1, wherein said solid
anti-seize lubricant is selected from the group consisting of
graphite, molybdenum disulfide, boron nitride,
polyethylenefluoroethylene (PTFE), mica, talc, and
combinations thereof.
5. The composition of Claim 1, wherein said solid
anti-seize lubricant is selected from the group consisting of
zinc oxide, titanium dioxide, magnesium oxide, calcium
hydroxide, barium oxide, tin oxide, and combinations thereof.
6. The composition of Claim 1, wherein said solid
anti-seize lubricant has a particle size of less than 150
microns.
7. The composition of Claim 1, wherein said grease is
calcium grease, sodium grease, lithium grease, aluminum
grease, or combinations thereof.
8. The composition of Claim 1, wherein said grease has
an ASTM D 217 penetration at 25°C from 200 to 400 mm and an
ASTM D 217 worked penetration at 25°C from 220 to 385 mm.
9. The composition of Claim 1, wherein said grease is
a number two grease.
10. The composition of Claim 9, wherein said grease is
a calcium-lithium grease.
11. The composition of Claim 1, wherein said oil is a
naphthenic petroleum oil having a viscosity of 18 to 66 cSt
(80 to 300 SUS) at 100°F (37°C) and having an API gravity at
60°F (15°C) from 22 to 26.
12. The composition of Claim 1, wherein said polymeric
matrix is a polymeric material selected from the group
consisting of polyamides, polyacrylamides, polyimides,
polyhydroxyalkylacrylates, urea-urethanes, hydroxy or amine
modified aliphatic hydrocarbons, liquid polyester-amide-based
rheological additives or combinations thereof.
13. The composition of Claim 1, wherein said polymeric
matrix is a hydroxy or amine modified aliphatic hydrocarbon
polymeric material having a melting point from 170°F (77'C)
to 200°F (93°C).
14. The composition of Claim 1, wherein said polymeric
matrix is a hydroxy modified aliphatic hydrocarbon having an
unworked ASTM D 217 penetration at 25°C from 20 to 100 dmm.
15. The composition of Claim 1, wherein said solid
anti-seize lubricant is- present from 10 to 60 weight percent
on a total composition basis, and said carrier polymeric
matrix is present from 10 to 30 weight percent on a total
composition basis.
16. The composition of Claim 1, wherein said wax is
paraffin wax, petrolatum wax, microcrystalline wax, animal
wax, vegetable wax, synthetic wax, or combinations thereof.
17. The composition of Claim 1, wherein said wax is
refined paraffinic wax.
18. The composition of Claim 17, wherein said refined
paraffinic wax is a soft wax.
19. The composition of Claim 17, wherein said refined
paraffinic wax has an ASTM D1321 needle penetration at 25°C
from 10 to 30 dmm.
20. A method for preparing a solid anti-seize
composition comprising:
selecting a grease with an ASTM D 217 penetration at
25°C from 200 to 400 mm;
selecting a naphthenic petroleum oil with a viscosity of
less than 300 SUS at 100°F (37°C) and an API gravity at 60°F
(15°C) from 23 to 25;
mixing said grease and said oil to form a combined
oil/grease composition;
adding and mixing into said oil/grease composition (a) a
solid anti-seize lubricant; and (b) a polymeric matrix to
form said solid anti-seize composition.
21. The method of claim 20, further comprising:
heating said matrix material or said oil/grease
composition to a temperature from 80°C to 100°C;
maintaining said anti-seize composition at the
temperature of 80°C to 100°C while mixing;
adding said solid anti-seize composition at the
temperature of 80°C to 100°C into a dispensing container
having a generally elongate hollow body and having first and
second ends, with one of said ends defining a dispense bottom
to releasably hold the composition; and
cooling said composition to room temperature to
solidify said composition.
22. The composition of claim 1, wherein said anti-seize
composition is dimensionally stable up to 130°F (54°C).


The invention discloses An anti-seize composition comprising: a solid anti-seize lubricant
selected from the group consisting of metallic powders or flakes, non-metallic lubricants,
and metal oxides, hydroxides and fluorides; and a carrier having said anti-seize lubricant
dispersed therein, said carrier selected from the group consisting of grease, oil, polymeric
matrix, wax having a viscosity of less than 44 cSt (200 SUS) at 100°F (37°C), naphthenic
petroleum oil having a viscosity of less than 66 cSt (300 SUS) at 100°F (37°C) and having
an API gravity at 60°F (15°C) from 23 to 25, said carrier being present in an amount to
render said composition non-flowable at temperatures greater than 120°F (50°C), wherein
said composition is dispensable at room temperature without the application of heat and has
a Mil-907-E breakaway torque of less than 250 foot-pounds (12KPa).

Documents:

478-kolnp-2004-abstract.pdf

478-kolnp-2004-assignment 1.1.pdf

478-kolnp-2004-assignment.pdf

478-kolnp-2004-claims.pdf

478-kolnp-2004-correspondence 1.1.pdf

478-kolnp-2004-correspondence.pdf

478-kolnp-2004-description (complete).pdf

478-kolnp-2004-drawings.pdf

478-kolnp-2004-examination report 1.1.pdf

478-kolnp-2004-examination report.pdf

478-kolnp-2004-form 1.pdf

478-kolnp-2004-form 18 1.1.pdf

478-kolnp-2004-form 18.pdf

478-kolnp-2004-form 3 1.1.pdf

478-kolnp-2004-form 3.pdf

478-kolnp-2004-form 5 1.1.pdf

478-kolnp-2004-form 5.pdf

478-kolnp-2004-gpa 1.1.pdf

478-kolnp-2004-gpa.pdf

478-kolnp-2004-granted-abstract.pdf

478-kolnp-2004-granted-claims.pdf

478-kolnp-2004-granted-description (complete).pdf

478-kolnp-2004-granted-drawings.pdf

478-kolnp-2004-granted-form 1.pdf

478-kolnp-2004-granted-specification.pdf

478-kolnp-2004-reply to examination report 1.1.pdf

478-kolnp-2004-reply to examination report.pdf

478-kolnp-2004-specification.pdf


Patent Number 243333
Indian Patent Application Number 478/KOLNP/2004
PG Journal Number 41/2010
Publication Date 08-Oct-2010
Grant Date 06-Oct-2010
Date of Filing 12-Apr-2004
Name of Patentee HENKEL CORPORATION
Applicant Address 1001 TROUT BROOK CROSSING, ROCKY HILL, CT
Inventors:
# Inventor's Name Inventor's Address
1 PATEL PRAKASH S 11 EASTING'S WAY, SOUTH BARRINGTON, IL 60010
2 ATTARWALA SHABBIR 36 BANKS ROAD, SIMSBURY, CT 06070
PCT International Classification Number C10M 103/00
PCT International Application Number PCT/US2002/33142
PCT International Filing date 2002-10-17
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 60/330,722 2001-10-29 U.S.A.
2 60/386,420 2002-06-07 U.S.A.