US2983680A - Lubricating greases thickened with mixtures of lithium fatty acid soaps and lithium dilinoleate - Google Patents

Lubricating greases thickened with mixtures of lithium fatty acid soaps and lithium dilinoleate Download PDF

Info

Publication number
US2983680A
US2983680A US663587A US66358757A US2983680A US 2983680 A US2983680 A US 2983680A US 663587 A US663587 A US 663587A US 66358757 A US66358757 A US 66358757A US 2983680 A US2983680 A US 2983680A
Authority
US
United States
Prior art keywords
lithium
grease
fatty acid
dilinoleate
acid
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
US663587A
Inventor
George W Eckert
Paul R Thomas
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Texaco Inc
Original Assignee
Texaco Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Texaco Inc filed Critical Texaco Inc
Priority to US663587A priority Critical patent/US2983680A/en
Application granted granted Critical
Publication of US2983680A publication Critical patent/US2983680A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M5/00Solid or semi-solid compositions containing as the essential lubricating ingredient mineral lubricating oils or fatty oils and their use
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06Metal compounds
    • C10M2201/063Peroxides
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/121Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
    • C10M2207/123Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms polycarboxylic
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/129Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of thirty or more carbon atoms
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/22Acids obtained from polymerised unsaturated acids
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/281Esters of (cyclo)aliphatic monocarboxylic acids
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/282Esters of (cyclo)aliphatic oolycarboxylic acids
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/283Esters of polyhydroxy compounds
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/286Esters of polymerised unsaturated acids
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/34Esters having a hydrocarbon substituent of thirty or more carbon atoms, e.g. substituted succinic acid derivatives
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/06Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
    • C10M2215/064Di- and triaryl amines
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/06Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
    • C10M2215/064Di- and triaryl amines
    • C10M2215/065Phenyl-Naphthyl amines
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/06Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
    • C10M2215/067Polyaryl amine alkanes
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00Metal present as such or in compounds
    • C10N2010/02Groups 1 or 11
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10Semi-solids; greasy

Definitions

  • This invention relates to improved lubricating greases, and more particularly to lithium base greases containing the lithium soap of an unsaturated fatty acid dimer.
  • improved lithium base greases are obtained by employing as the thickening agent a mixture of a lithium soap of a monomeric higher fatty acid and the lithium soap of dilinoleic acid.
  • lubricating greases are obtained by employing this combination of lithium soaps having superior shear stability and other advantages as compared with greases obtained from lithium soaps of the conventional fatty acids as .the sole thickening agent.
  • the use of a saponifiable material comprising a mixture of monomeric higher fatty acid and dilinoleic acid permitsthe grease preparation to be carried out by the convenient low temperature method, wherein the grease mixture is maintained at a temperature below the melting point of the soap during both the saponification and dehydration steps.
  • Dilinoleic acid is considered to have the formula:
  • trimer may also contain minor amounts of other materials, such as other unsaturated acid polymers, as impurities. Such a product may be employed directly in the preparation of the lithium soap.
  • the monomeric high molecular weight fatty acid materials employed for forming the other soap component of these greases are those employed conventionally in grease making, suitably fatty acids containing about 12 to 32 carbon atoms per molecule and their glycerides or other esters.
  • the preferred materials of this character are substantially saturated fatty acids containing about 14-22 carbon atoms per molecule and the glycerides or other esters thereof, such as myristic acid, palmitic acid, stearic acid, tallow, and hydrogenated fish fatty oils.
  • the lithium soap of the high molecular weight conventional fatty acids and the lithium soap of dilinoleic acid are employed in a ratio of about 1:2 to about 2:1 by weight. With higher proportions of the conventional lithium soap the shear stability of the grease falls ofi rapidly, whereas with higher proportions of the dimer acid soap the yield becomes unsatisfactory, a grease struc- Z ture being unobtainable with the dimer acid soap alone.
  • the two soaps are preferably employed in a. ratio of about 1:1 by Weight, with sufiicient of the mixture employed to give a grease consistency. Ordinarily the grease will contain from about 5 to about 50 percent by weight of the combined soaps.
  • the grease may contain a small excess of free alkali, preferably from about 0.2 to about 1.0 percent by weight of lithium hydroxide.
  • a small excess of free alkali preferably from about 0.2 to about 1.0 percent by weight of lithium hydroxide.
  • the oleaginous liquids employed in these greases may be any oils suitable for use in grease making generally, such as mineral oils obtained by any of the conventional refining processes in the lubricating oil viscosity range, preferably those having viscosities from about seconds Saybolt Universal at F. to about 225 seconds at 210 F.
  • various synthetic oils may be employed with advantage, such as high molecular weight ethers, esters, and silicone polymer oils.
  • Particularly suitable synthetic esters are dicarboxylic acid esters, such as, for example, di-Z-ethylhexyl sebacate, di(secondary amyl) sebacate, and di-2-ethylhexyl azelate.
  • the greases may also contain various additives of the usual types employed in lubricating greases, such as corrosion inhibitors, oxidation inhibitors. antiwear agents, etc.
  • they contain an oxidation inhibitor, which may suitably be an oxidation inhibitor of the amine type, such as diphenylamine, phenyl naphthylamine or tetramethyl diamino diphenyl methane.
  • the grease preparation may be carried out by any suitable grease making procedure. It is preferably carried out by the method involving saponification in situ, wherein a mixture of dilinoleic acid and conventional saponifiable material as described above is saponified in a portion of the lubricating oil employed as the liquid base, preferably in a mineral oil. Following the saponification, the saponification mass is heated at a higher temperature, such as a temperature in about the range 300-350 F., to dehydrate, and the main portion of the oleaginous liquid component and any additives employed are mixed in while the grease is allowed to cool.
  • a higher temperature such as a temperature in about the range 300-350 F.
  • Example I A grease was prepared having the following composition in percent by weight:
  • Mineral lubricating oil Remainder The mineral lubricating oil was a refined naphthene base distillate oil having a Saybolt Universal viscosity of about 312 seconds at 100 F.
  • the lithium stearate was obtained by saponification of a commercial triple-pressed stearic acid having a neutralization number of 201, a saponiiication number of 211, an iodine number of 2 and a titer of 54.6 C.
  • the lithium dilinoleate was obtained by saponification of a commercial dilinoleic acid having an apparent molecular weight of about 600, a neutralization number of 183, a saponification number of 188, an iodine number of 73 and a hydroxyl number of 6.
  • the grease preparation was carried out in the following manner: A laboratory grease kettle was charged with with 245 grams of stearic acid, 245 grams of the dimer mass was maintained at 310 F. and 500 grams more Dropping point, F. 376 Penetration, AST M, at 77 F.:
  • Miniature penetration- Original 70 After test 189 The dynamic shear test is conducted in an apparatus consisting of a perforated piston reciprocating within a closed cylinder maintained at a constant temperature.
  • the grease of this invention gave an increase of 119 points in miniature penetration, which the severe conditions of this test. This represents a 'very considerable improvement in shear stability over greases thickened with lithium stearate alone, which break down to liquid or semi-liquid products under these conditions.
  • Example II Another grease was prepared having the following composition in percent by weight:
  • the grease of the above example containing 0.5 percent of excess lithium hydroxide, had a dropping point above 500 F. and softened only two points upon working, in addition to having excellent oxidation resistance and resistance to water washing.
  • This grease also maintained good lubrication under actual service conditions in the torque breakdown machine test, giving no leakage from a Federal Precision ball bearing rotated at 1750 r.p.m. upon a shaft for 3 hours at 80 F. to 250 F. s
  • a shear stable and substantially water insoluble lubricating grease composition consisting essentially of a lubricating oil thickened to a grease consistency with a mixture in about a 1:2 to 2:1 ratio by weight of a lithium soap of a high molecular weight fatty acid and lithium dilinoleate.
  • the grease composition of claim 1 wherein the said lithium soap of high molecular weight fatty acid is the lithium soap of a substantially saturated fatty acid containing 14-22 carbon atoms per molecule.
  • a shear stable and substantially water insoluble lubricating grease composition consisting essentially of a mineral lubricating oil thickened to a grease consistency by about 5 to 50 percent by weight of a mixture in about a 1:1 ratio by weight of lithium stearate and lithium dilinoleate and containing about 0.2-1.0 percent by weight of excess lithium hydroxide.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)

Description

States George W. Eckert, Wappingers Falls, and Paul R. Thomas, Beacon, N.Y., assignors to Texaco Inc., a corporation of Delaware No Drawing. Filed June 5, 1957, Ser. No. 663,587
6 Claims. (Cl. 252-421) This invention relates to improved lubricating greases, and more particularly to lithium base greases containing the lithium soap of an unsaturated fatty acid dimer.
In accordance with this invention, improved lithium base greases are obtained by employing as the thickening agent a mixture of a lithium soap of a monomeric higher fatty acid and the lithium soap of dilinoleic acid. We have found that lubricating greases are obtained by employing this combination of lithium soaps having superior shear stability and other advantages as compared with greases obtained from lithium soaps of the conventional fatty acids as .the sole thickening agent. In addition, the use of a saponifiable material comprising a mixture of monomeric higher fatty acid and dilinoleic acid permitsthe grease preparation to be carried out by the convenient low temperature method, wherein the grease mixture is maintained at a temperature below the melting point of the soap during both the saponification and dehydration steps.
Dilinoleic acid is considered to have the formula:
It is obtained by the heat polmerization of linoleic acid acid or of the methyl ester or glyceridc of linoleic acid, followed by hydrolysis. The polmerization may be carried out as described, for example, in US. 2,482,761, by heating an unsaturated fatty acid material comprising linoleic acid as the chief polyunsaturated fatty acid component at about 260-360 C. for about 3-8 hours under a steam pressure of about 80-400 pounds per square inch. The unpolymerized fatty acids are then removed by distillation under reduced pressure. The product obtained in this manner consists chiefly of the linoleic acid dimer in admixture with small amounts, up
to about percent based on the weight of the product,
of the trimer. "It may also contain minor amounts of other materials, such as other unsaturated acid polymers, as impurities. Such a product may be employed directly in the preparation of the lithium soap.
The monomeric high molecular weight fatty acid materials employed for forming the other soap component of these greases are those employed conventionally in grease making, suitably fatty acids containing about 12 to 32 carbon atoms per molecule and their glycerides or other esters. The preferred materials of this character are substantially saturated fatty acids containing about 14-22 carbon atoms per molecule and the glycerides or other esters thereof, such as myristic acid, palmitic acid, stearic acid, tallow, and hydrogenated fish fatty oils.
The lithium soap of the high molecular weight conventional fatty acids and the lithium soap of dilinoleic acid are employed in a ratio of about 1:2 to about 2:1 by weight. With higher proportions of the conventional lithium soap the shear stability of the grease falls ofi rapidly, whereas with higher proportions of the dimer acid soap the yield becomes unsatisfactory, a grease struc- Z ture being unobtainable with the dimer acid soap alone. The two soaps are preferably employed in a. ratio of about 1:1 by Weight, with sufiicient of the mixture employed to give a grease consistency. Ordinarily the grease will contain from about 5 to about 50 percent by weight of the combined soaps. With particular advantage, the grease may contain a small excess of free alkali, preferably from about 0.2 to about 1.0 percent by weight of lithium hydroxide. We have found that such an excess of lithium hydroxide in these greases produces both improved yields and increased dropping points, dropping points of 500 or higher being obtained with an excess of about 0.5 percent or more of lithium hydroxide.
The oleaginous liquids employed in these greases may be any oils suitable for use in grease making generally, such as mineral oils obtained by any of the conventional refining processes in the lubricating oil viscosity range, preferably those having viscosities from about seconds Saybolt Universal at F. to about 225 seconds at 210 F. For certain purposes, such as for producing greases suitable for high temperature operations, various synthetic oils may be employed with advantage, such as high molecular weight ethers, esters, and silicone polymer oils. Particularly suitable synthetic esters are dicarboxylic acid esters, such as, for example, di-Z-ethylhexyl sebacate, di(secondary amyl) sebacate, and di-2-ethylhexyl azelate.
The greases may also contain various additives of the usual types employed in lubricating greases, such as corrosion inhibitors, oxidation inhibitors. antiwear agents, etc. Preferably, they contain an oxidation inhibitor, which may suitably be an oxidation inhibitor of the amine type, such as diphenylamine, phenyl naphthylamine or tetramethyl diamino diphenyl methane.
The grease preparation may be carried out by any suitable grease making procedure. It is preferably carried out by the method involving saponification in situ, wherein a mixture of dilinoleic acid and conventional saponifiable material as described above is saponified in a portion of the lubricating oil employed as the liquid base, preferably in a mineral oil. Following the saponification, the saponification mass is heated at a higher temperature, such as a temperature in about the range 300-350 F., to dehydrate, and the main portion of the oleaginous liquid component and any additives employed are mixed in while the grease is allowed to cool.
The following examples are illustrative of the lubricating greases of this invention.
Example I A grease was prepared having the following composition in percent by weight:
Lithium stearate -a 12.5 Lithium dilinoleate 12.5 Phenyl alpha naphthylamine 0.5 Mineral lubricating oil Remainder The mineral lubricating oil was a refined naphthene base distillate oil having a Saybolt Universal viscosity of about 312 seconds at 100 F.
The lithium stearate was obtained by saponification of a commercial triple-pressed stearic acid having a neutralization number of 201, a saponiiication number of 211, an iodine number of 2 and a titer of 54.6 C. The lithium dilinoleate was obtained by saponification of a commercial dilinoleic acid having an apparent molecular weight of about 600, a neutralization number of 183, a saponification number of 188, an iodine number of 73 and a hydroxyl number of 6.
The grease preparation was carried out in the following manner: A laboratory grease kettle was charged with with 245 grams of stearic acid, 245 grams of the dimer mass was maintained at 310 F. and 500 grams more Dropping point, F. 376 Penetration, AST M, at 77 F.:
Worked, 60 strokes 332 Worked, 100,000 strokes 354 Dynamic water resistance test, percent loss Norma-Hoffman oxidation test, 210 F., 100 hours, pressure drop, lbs. Dynamic shear test:
Miniature penetration- Original 70 After test 189 The dynamic shear test is conducted in an apparatus consisting of a perforated piston reciprocating within a closed cylinder maintained at a constant temperature.
'The results given in the table were obtained in the test carried out at a temperature of 225 F., with the piston reciprocated at 49 strokes per minute for eight hours.
As shown by the data, the grease of this invention gave an increase of 119 points in miniature penetration, which the severe conditions of this test. This represents a 'very considerable improvement in shear stability over greases thickened with lithium stearate alone, which break down to liquid or semi-liquid products under these conditions.
Example II Another grease was prepared having the following composition in percent by weight:
Lithium stearate 9.9 Lithium dilinoleate 9.9 Phenyl alpha naphthylamine 0.5 Excess LiOH I v 0.5 Mineral lubricating oil Remainder The mineral lubricating Mind the saponifiable materials employed were the same as those described in Example I. The grease preparation was carried out in the same manner as described in Example I except that the,
dehydration was carried out at 325 F.
The product obtained was a brown, uniform grease of slightly stringy texture which gave the following tests.
is considered only a moderate amount of softening under 4 Dropping point, F. 500+? Penetration, ASTM, at 77 F.:
Unworked 358 Worked 360 Dynamic water resistance test, percent loss 0 Norma-Hoffman oxidation test, 210 F., 100
hours, pressure drop, lbs. 2 Torque breakdown machine test, -250 F.,
rating Good As shown by the data, the grease of the above example, containing 0.5 percent of excess lithium hydroxide, had a dropping point above 500 F. and softened only two points upon working, in addition to having excellent oxidation resistance and resistance to water washing. This grease also maintained good lubrication under actual service conditions in the torque breakdown machine test, giving no leakage from a Federal Precision ball bearing rotated at 1750 r.p.m. upon a shaft for 3 hours at 80 F. to 250 F. s
Obviously many modifications and variations of the invention, as hereinbefore set forth, may be made without departing from the spirit and scope thereof and, therefore, only such limitations should be imposed as are indicated in the appended claims.
We claim:
1. A shear stable and substantially water insoluble lubricating grease composition consisting essentially of a lubricating oil thickened to a grease consistency with a mixture in about a 1:2 to 2:1 ratio by weight of a lithium soap of a high molecular weight fatty acid and lithium dilinoleate.
2. The grease composition of claim 1 wherein the said lubricating oil is a mineral lubricating oil.
3. The grease composition of claim 1 wherein the said soaps are employed in a ratio of about 1:1 by weight.
4. The grease composition of claim 1 wherein the said lithium soap of high molecular weight fatty acid is the lithium soap of a substantially saturated fatty acid containing 14-22 carbon atoms per molecule.
5. The grease composition of claim 1 wherein'the said composition contains about 0.5-1.0 percent by weight of excess lithium hydroxide.
6. A shear stable and substantially water insoluble lubricating grease composition consisting essentially of a mineral lubricating oil thickened to a grease consistency by about 5 to 50 percent by weight of a mixture in about a 1:1 ratio by weight of lithium stearate and lithium dilinoleate and containing about 0.2-1.0 percent by weight of excess lithium hydroxide.
References Cited in the file of this patent UNITED STATES PATENTS 2,555,104 Ashley et a1. May 29, 1951 2,585,321 ,Butcosk Feb. 12, 1952 2,699,428 Lux et al. Ian. 11, 1955 2,710,838 'Morway et a1. June 14, 1955 2,737,497 Wasson et a1. Mar. 6, 1956 2,883,342 Sprouleet al. Apr. 21, 1959 FOREIGN PATENTS 736,921 Great Britain Sept. 14. 1955

Claims (1)

1. A SHEAR STABLE AND SUBSTANTIALLY WATER INSOLUBLE LUBRICATING GREASE COMPOSITION CONSISTING ESSENTIALLY OF A LUBRICATING OIL THICKNED TO A GREASE CONSISTENCY WITH A MIXTURE IN ABOUT A 1:2 TO 2:1 RATIO BY WEIGHT OF A LITHIUM SOAP OF A HIGH MOLECULAR WEIGHT FATTY ACID AND LITHIUM DILINOLEATE.
US663587A 1957-06-05 1957-06-05 Lubricating greases thickened with mixtures of lithium fatty acid soaps and lithium dilinoleate Expired - Lifetime US2983680A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US663587A US2983680A (en) 1957-06-05 1957-06-05 Lubricating greases thickened with mixtures of lithium fatty acid soaps and lithium dilinoleate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US663587A US2983680A (en) 1957-06-05 1957-06-05 Lubricating greases thickened with mixtures of lithium fatty acid soaps and lithium dilinoleate

Publications (1)

Publication Number Publication Date
US2983680A true US2983680A (en) 1961-05-09

Family

ID=24662469

Family Applications (1)

Application Number Title Priority Date Filing Date
US663587A Expired - Lifetime US2983680A (en) 1957-06-05 1957-06-05 Lubricating greases thickened with mixtures of lithium fatty acid soaps and lithium dilinoleate

Country Status (1)

Country Link
US (1) US2983680A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2157207A1 (en) * 1970-11-18 1972-05-25 Esso Research and Engineering Co , Lmden, NJ (V St A ) Grease
US5948736A (en) * 1998-08-25 1999-09-07 Toxco, Inc. Dust free lithium hydroxide
US6653262B2 (en) * 2001-12-27 2003-11-25 Toxco, Inc. Dust free lithium hydroxide

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2555104A (en) * 1949-11-25 1951-05-29 American Cyanamid Co Aluminum soap compositions and greases containing them
US2585321A (en) * 1952-02-12 High-temperature grease
US2699428A (en) * 1949-12-19 1955-01-11 Witco Chemical Corp Oil soluble soap of polycarboxylic acids
US2710838A (en) * 1952-01-09 1955-06-14 Exxon Research Engineering Co Thixotropic lubricating grease containing polycarboxylic acid soap
GB736921A (en) * 1952-10-16 1955-09-14 Exxon Research Engineering Co Lithium greases
US2737497A (en) * 1952-01-02 1956-03-06 Exxon Research Engineering Co Non-inflammable hydraulic fluid
US2883342A (en) * 1956-03-22 1959-04-21 Exxon Research Engineering Co Lithium greases containing excess lithium hydroxide

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2585321A (en) * 1952-02-12 High-temperature grease
US2555104A (en) * 1949-11-25 1951-05-29 American Cyanamid Co Aluminum soap compositions and greases containing them
US2699428A (en) * 1949-12-19 1955-01-11 Witco Chemical Corp Oil soluble soap of polycarboxylic acids
US2737497A (en) * 1952-01-02 1956-03-06 Exxon Research Engineering Co Non-inflammable hydraulic fluid
US2710838A (en) * 1952-01-09 1955-06-14 Exxon Research Engineering Co Thixotropic lubricating grease containing polycarboxylic acid soap
GB736921A (en) * 1952-10-16 1955-09-14 Exxon Research Engineering Co Lithium greases
US2883342A (en) * 1956-03-22 1959-04-21 Exxon Research Engineering Co Lithium greases containing excess lithium hydroxide

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2157207A1 (en) * 1970-11-18 1972-05-25 Esso Research and Engineering Co , Lmden, NJ (V St A ) Grease
US5948736A (en) * 1998-08-25 1999-09-07 Toxco, Inc. Dust free lithium hydroxide
US6653262B2 (en) * 2001-12-27 2003-11-25 Toxco, Inc. Dust free lithium hydroxide

Similar Documents

Publication Publication Date Title
US2468099A (en) High-temperature grease
US2528373A (en) Alkenyl succinic acid grease
US2810695A (en) Lubricating grease compositions containing polyethylene
US2450220A (en) Texture-stable lithium base grease
US2450254A (en) Lithium base grease and method of preparing the same
GB655011A (en) Lubricating grease
US3068175A (en) Process for preparing complex calcium salt-calcium soap grease
US2983680A (en) Lubricating greases thickened with mixtures of lithium fatty acid soaps and lithium dilinoleate
US2641577A (en) Lithium-calcium lubricating grease composition
US3117087A (en) Method of making greases
US2612473A (en) Lubricating grease compositions
US2491028A (en) Lubricating grease compositions
US3009878A (en) Lubricating greases prepared from epoxy fatty acid materials
US2491054A (en) Lubricating grease
US2854410A (en) Soap-thickened lubricating greases containing an alcohol-substituted amide
US2967826A (en) Calcium soap grease containing lithium hydroxide
US2953528A (en) Lubricating grease thickened with lithium soap of styrenated fatty acid
US2721844A (en) Lithium soap-synthetic base instrument grease
US2626898A (en) Process for preparing alkali metal greases
US2690429A (en) Grease compositions containing an aryl oxy alkyl salt as a stabilizer
US3072571A (en) Calcium base greases containing chlorinated bicycloheptene compounds
US2916452A (en) Method for preparing lithium base greases involving quenching
US2751351A (en) Complex ester base lubricating grease compositions
US3271311A (en) Lubricant
US2892777A (en) Process for preparing improved synthetic ester based grease compositions