US2976242A - Lubricating grease compositions - Google Patents

Lubricating grease compositions Download PDF

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Publication number
US2976242A
US2976242A US498743A US49874355A US2976242A US 2976242 A US2976242 A US 2976242A US 498743 A US498743 A US 498743A US 49874355 A US49874355 A US 49874355A US 2976242 A US2976242 A US 2976242A
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Prior art keywords
grease
acid
molecular weight
acids
acetic acid
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US498743A
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English (en)
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Arnold J Morway
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ExxonMobil Technology and Engineering Co
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Exxon Research and Engineering Co
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Priority to US498743A priority Critical patent/US2976242A/en
Priority to GB5482/56A priority patent/GB778567A/en
Priority to DEE12078A priority patent/DE1054631B/de
Priority to FR1148917D priority patent/FR1148917A/fr
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    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M5/00—Solid or semi-solid compositions containing as the essential lubricating ingredient mineral lubricating oils or fatty oils and their use
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C—CHEMISTRY; METALLURGY
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C—CHEMISTRY; METALLURGY
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    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/04—Ethers; Acetals; Ortho-esters; Ortho-carbonates
    • C—CHEMISTRY; METALLURGY
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    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
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    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
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    • C10M2207/122—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms monocarboxylic
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    • C10M2207/129—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of thirty or more carbon atoms
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    • C10M2207/141—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings monocarboxylic
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    • C10M2207/142—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings polycarboxylic
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    • C10M2207/144—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings containing hydroxy groups
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/06—Thio-acids; Thiocyanates; Derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/06—Thio-acids; Thiocyanates; Derivatives thereof
    • C10M2219/062—Thio-acids; Thiocyanates; Derivatives thereof having carbon-to-sulfur double bonds
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/08—Thiols; Sulfides; Polysulfides; Mercaptals
    • C10M2219/082—Thiols; Sulfides; Polysulfides; Mercaptals containing sulfur atoms bound to acyclic or cycloaliphatic carbon atoms
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/10—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/10—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring
    • C10M2219/102—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring containing sulfur and carbon only in the ring
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/10—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring
    • C10M2219/104—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring containing sulfur and carbon with nitrogen or oxygen in the ring
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/10—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring
    • C10M2219/104—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring containing sulfur and carbon with nitrogen or oxygen in the ring
    • C10M2219/106—Thiadiazoles
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
    • C10M2229/02—Unspecified siloxanes; Silicones
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
    • C10M2229/04—Siloxanes with specific structure
    • C10M2229/05—Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/02—Groups 1 or 11
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/04—Groups 2 or 12
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/14—Group 7
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/16—Groups 8, 9, or 10
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10—Semi-solids; greasy

Definitions

  • This invention relates to novel organo-metallic complexes or compounds with coordinated valences and to compositions containing the same. More particularly, the present invention pertains to soap-salt complexes comprising a metal salt of acetic acid, a metal salt of medium molecular weight carboxylic acid, and a metal soap of high molecular weight carboxylic acid, to methods for preparing the soap-salt complexes and to cmpositions containing them.
  • the invention relates to compositions consisting of or containing dehydrated and baked complexes or coordinated compounds consisting of a metal salt of acetic acid, a metal salt of a medium molecular weight carboxylic acid containing from about 3 to carbon atoms, and a metal soap of a high molecular weight monocarboxylic acid containing from about 12 to 30 carbon atoms and preferably 18 to 22 carbon atoms, in which the mol ratio of acetic acid to the other acids employed exceeds 4, and in which the difference in number of carbon atoms per molecule between the average of the high molecular weight carboxylic acids and the average of the medium molecular weight carboxylic acids is at least 7.
  • compositions of the invention include novel and improved lubricating greases, lubricating oils, gear oils, filter oils, etc.
  • grease compositions containing the complexes of the invention have been found to have excellent extreme pressure and structural stability properties as well as other desirable grease characteristics.
  • soap-salt complexes as grease thickeners is well known in the art.
  • the complex materials used heretofore consisted of combinations of metal soaps of high molecular weight carboxylic acids having from 12 to 30 carbon atoms and metal salts of low molecular weight carboxylic acids containing from 1 to 6 carbon atoms per molecule.
  • the commonly known grease-making, high molecular weight fatty acids, saturated or unsaturated, containing from about 12 to 22 carbon atoms have been employed in conjunction with such low molecular weight carboxylic acids as acetic, propionic, alkoxy propionic, and the like to form the complex grease thiekeners of the prior'art. Normally.
  • novel compounds which are true complexes can be prepared by employing a metal salt of acetic acid, at least one metal salt of a medium molecular weight carboxylic acid, and at least one metal salt of a high molecular weight carboxylic acid.
  • the difference in' average number of carbon atoms per molecule between the high and the medium molecular weight carboxylic acid should be at least 7 and the average saponification value of the carboxylic acids, other than acetic acid should be within the range of about 290 to 450 and preferably at least 320.
  • carboxylic acids containing from about 3 to 10 and preferably 6 to 9 carbon atoms per molecule are designated as the medium molecular weight carboxylic acids. Those having from 6 to 9 carbon atoms are preferred. If it is desirable to use a polycarboxylic acid as the medium molecular weight acid in accordance with this invention, its saponification number must be reckoned on the basis of its molar equivalence in monocarboxylic acid. The equivalent saponification number is the quotient of milligrams equivalent weight of KOI-I (or 56,100) and gram equivalent of the acid. Suitable carboxylic acids coming within this definition are exemplified by the following:
  • Pentanoic a Hexanoic (caproic) Heptanoic (enanthic) Octanoic (caprylic) Nonanoic (pelargonic) Decanoic (capric) Branched chain saturated aliphatic acids:
  • Aromatic mono-and poly-carboxylic acids and anhydrides a
  • Furoic Thiophene carboxylic Mixed as well as single medium molecular weight carboxylic acids may be employed in accordance with the foregoing statements about the average carbon atom spread and average minimum saponification number of the high and medium molecular weight carboxylic acids. Similarly, commercial mixtures of medium molecular weight carboxylic acids can also be utilized to prepare the novel complexes.
  • the Oxo acids useful for the purposes of the present invention can be prepared by means of the well known Oxo synthesis. This process involves the oxona-tion or carbonylation of olefins with carbon monoxide and hydrogen at elevated temperatures of about 300 to 400 F. and pressures of about 2500 and 4000 p.s.i.g. in the presence of a group VIII catalyst, preferably cobalt.
  • a group VIII catalyst preferably cobalt.
  • Patent No. 2,632,021 the Oxo process and the nature of the reaction products, e.g. 0,; x0 products, are disclosed in detail. The preparation of acids from the 0x0 reaction products is described in US. Patent No. 2,537,577 and U3. Patent No.
  • the C Oxo acids can be derived from butylene, for example, and the C Oxo acids from the C olefins produced by polymerizing propylene alone or with some butylene.
  • High molecular weight monocarboxylic acids containing from about 12 to 30, preferably from 18 to 22, carbon atoms are useful for the purposes of this invention. These acids may be derived from saturated or unsaturated naturally occurring or synthetic fatty material. The fatty acids normally used in the manufacture of conventional greases, particularly the more saturated acids, are preferred. Examples of such acids include lauric, myristic, palrnitic, stearic, mono-hydroxy stearic, di-hydroxy stearic, poly-hydroxy stearic and arachidic acids and the hydrogenated fish oil and tallow acids, which contain chiefiy stearic acid. However, unsaturated acids such as oleic, ricinoleic and similar acids may also be used.
  • the average saponification value of a mixture of the high molecular weight carboxylic acids useful for the purposes of the present invention should not be more than about 280 and is preferably not more than about 220.
  • the acetic acid employed in the present invention can be either glacial acetic acid or an aqueous solution of acetic acid.
  • concentration of acid in the solution may vary from about 60 to 99.9 wt. percent, and is preferably about 80 wt. percent.
  • the presence of a salt of acetic acid in the complex is an essential part of the present invention, but the use of a'substituted acetic acid having 2 carbon atoms per molecule is not excluded, where such modification may be desirable.
  • chloro-acetic acid, glycolic acid, thioglycolic acid, glycine, or oxalic acid may be used to modify the structure of a grease made in accordance with the invention.
  • the metal component of the complexes of the invention is used in a form which can combine chemically with carboxylic acids to form salts or soaps; Ordinarily the metal hydroxide is used.
  • the choice of metal component depends to a certain extent on the use to which the multiple salt and soap complex of the inventionis to be put.
  • the alkaline earth metal hydroxides or carbonates such as those of calcium, barium and strontium are useful for many purposes of the invention. Calcium hydroxide is especially preferred. These metals afford the greatest advantages when their complexes, with mol ratios of acetic to the medium and high molecular weight acids above 5 :1, are used as grease thickeners, since they result in the production of greases having outstanding load carrying characteristics and structural stability during storage and at high temperatures even without the use of conventional extreme pressure and stabilizing agents.
  • the alkaline earth metals differ in this respect from the alkali metals, i.e. sodium, potassium and lithium. Soapsalt complexes having a high alkali metal content and which consist of the combination of acids, mol ratios and carbon atom spreads of this invention, yield greases.
  • metals having two valences when more than one metal salt or soap is used in the complex, one of them may be an alkali metal, for example, lithium.
  • metals useful for the purposes of this invention are magnesium and zinc.
  • copper, iron, nickel or cobalt may be used.
  • the preferred class of metals are the alkaline earth metals and zinc; and the preferred metal in that clas is calcium.
  • the metallic constituents of the salts and soaps may be any one or more of the metals set forth above. Though the metals may be either the same or different, in most cases the salts and soaps contain the same metal. If it is desired to incorporate a monovalent metal, e.g. lithium, into the composition along with a divalent metal, e.g. calcium, the monovalent metal should be in the salt of medium molecular weight carboxylic acid, particularly if it is a dicarboxylic acid.
  • a monovalent metal e.g. lithium
  • a divalent metal e.g. calcium
  • the proportion of acetic acid by weight should exceed that of the sum of medium and high molecular weight carboxylic acids; and the combination of the medium and high molecular weight acids should be selected so that the carbon atom spread, that is the difference in the average number of carbon atoms per molecule, between the high and the medium molecular weight carboxylic acids is at least about 7, preferably 7 to 15, and the average equivalent saponification value of the medium and high molecular weight carboxylic acids be within the range of about 290 to 450, and preferably above 320.
  • the mol ratio of acetic to the higher molecular weight carboxylic acids can be lower than 5:1 and at least 4:1; but it is particularly preferred to be higher than 5 :1 and most particularly between 7:1 and 25:1, in order to get the maximum benefit of a high content of combined metal per unit weight of the composition and therefore to get maximum utility for extreme pressure application.
  • the soap-salt complexes containing a metal salt of acetic acid, at least one metal salt of a medium molecular weight carboxylic acid having from about 3 to 10 carbon atoms, mid at least one metal soap of a high molecular weight carboxylic acid having 12 to 30 carbon atoms may be incorporated in a wide variety of liquid and semiliquid materials of natural or synthetic origin to improve the utility of these materials.
  • the mineral or synthetic lubricating oil should have a viscosity within the range of about 50 to 2000 SUS at 100 F. and 30 to 150 SUS at 210 F., a pour point of about +20 to 75 F., a
  • oils include synthetic lubricating oils of the hydro- 16 carbon, hydrocarbon polymer, ester, complex ester, formal, mercaptal, polyalkylene oxide, silicone or similar types. Synthetic oils such as di-Z-ethylhexyl sebacate, di-C Oxo, azelate and other branched chain simple esters of dicarboxylic acids can be used, as well as com- 20 plex esters prepared from glycols, dicarboxylic acids, and alcohols or monocarboxylic acids.
  • the metal soap-salt complexes of the invention may be prepared by coneutralization of a mixture of the carboxylic acids with suitable bases, particularly the hydroxides and/or carbonates of the metals desired.
  • the coneutralization step may be carried out in situ in the liquid menstruum to which the complex compound is to be applied in actual use.
  • the mixed acids may be coneutralized in a portion or all of a lubricating oil which then forms the dispersant of the complex and is thereby gelled to a grease.
  • the coneutralization may be carried out in other dispersants or solvent fluids, the characteristics of which are to be modified by the complex compound.
  • This coneutraliza- I tion method of preparation is particularly desirable in cases in which the salts and soap have the same metal constituent.
  • the coneutralized material is heated to a temperature above about 400 F., preferably 450 to 550 F., in order to dehydrate it and to form the baked complex.
  • this heating step is carried out in a liquid dispersant, the latter should have a boiling point above 400 F. or heating should be carried out under pressure.
  • the coneutralization method of preparation is not nec- '45 essary as long as the metal salts and soap are present when heating to the complex forming temperatures.
  • the complex compounds of the invention may also be prepared by separately preforming at least a portion of the acetic acid salt, the medium molecular weight carboxylic acid salt, and the high molecular weight carboxylic acid soap, intimately mixing the preformed ma terials, and baking the resulting mixture under complex forming conditions. This method is especially useful when different metals are employed as bases for the salts and soap.
  • the complex compounds of the invention when prepared in a liquid dispersant or solvent may be isolated from their dispersions or solutions by solvent extraction of the dispersing medium in a solvent in which the complex is insoluble.
  • Suitable solvents include most of the hydrocarbon solvents, acetone, etc.; the proper choice depending on the solubility characteristics of the liquid menstruum used to disperse the complex.
  • stearic acid and o-phthalic acid were charged to a fire heated kettle, and the mixture was warmed to 135 F.
  • This grease having the formulation listed below in Table I, was prepared by the method described above with, respect to the preparation of Grease A, except that C 2 weight acid.
  • the acetic acid and the medium molecular if OX0 acld'was gmployed as the medium molecular weight weight carboxylic acid employed are then added to, the, 65
  • carboxylic acid and lauric acid was employed as the high molecular Weight carboxylic acid.
  • the 10 drated lime and benzoic acid were charged to a fire heated grease batch was held at this temperature for 10 minutes kettle and mixed together while heating to 135 F. and then cooled to 275 F. with stirring.
  • the phenyl Acetic acid was then added, and heating continued to alpha naphthylamine was added to the grease batch, and 510 F. Heating was then discontinued, and the grease cooling was continued to 180-200 F. The resulting cooled to 250 F. while continuing to agitate.
  • At this grease composition was then pumped to a Gaulin homogetemperature phenyl alpha naphthylamine was added, and nizer, homogenized at 6000 p.s.i., filtered and packaged. the grease batch further cooled to 180 F. while mixing.
  • the grease product was Gaulin homogenized at 5000 Grease N F p.s.i., filtered and packaged. All of the mineral lubricating oil, hydrated lime, and stearic acid were charged to a fire heated. kettle and Grease No' I warmed to 150 F. While mixing. The isobutyric acid and This grease was prepared by the method substantially acetic acid were then added as a mixture and heating was as described in the preparation of Grease No. H. continued until the temperature reached 430-450 F.
  • Appearance se l S il form 7 Dropping Point F.) 500+ 500+ 500+ 500+ 500+ 500+ 500+ 500+ 500+ 500+ 500+ 500+ 500+ 500+ P711&l;latl0n5 (77 Fmm.
  • composition was prepared by the method substantially as described in the preparation of Composition N0. A, except that no acetic acid was employed.
  • Buosatisfactory grease composition was obtained by employing the calcium salt of. furoic acid in combination with the normally grease forming metal soaps oflhigh molecular weight carboxylic acids e.g. ,stearic acid, in the grease thickener.
  • compositionNo lubricating grease compositionspcan bejrepareld from a thickener comprising the calcium salt of'furoicac'i calcium salt of acetic acid, and the calcium soap of stearic acid.
  • the complex thickener resulting from this combination of acids gives an excellent stable grease product having a high load carrying capacity. 7
  • Composition No. C illustrates that greases can be prepared from a thickener comprising sodium furoate and sodium stearate, but they show little load carrying capacity. This grease, for example, failed the Timken test at a 20 lb. load.
  • EXAMPLE III The use of commercial mixtures of medium molecular weight acids, e.g. Neo Fat 360 which is composed of 60 wt. percent caprylic acid and 40 wt. percent of capric acid, is exemplified by this experiment.
  • the grease was prepared by the method described in the preparation of Composition A, of Example II.
  • caprylic acid 00% caprylic acid; 40% capric acid; sap. value (mg. ROE/gm.)- 355 6.
  • EXAMPLE IV The mineral lubricating oil, hydrated lime, stearic acid and citric acid were charged to a fire heated kettle and warmed to 135 F. while stirring. The acetic acid is then added, and the ingredients further heated to 500 F. The grease batch is cooled to 250 F. While agitating, and the phenyl alpha naphthylamine added. The grease is further cooled to below about 180 F. and then Gaulin homogenized at 6500 p.s.i.
  • This grease was prepared by the method substantially as described in the preparation of Grease .No. 1 with the exception that 1.0 wt. percent rather than 2.0 wt. percent of citric acid was employed.
  • the mineral lubricating oil, hydrated lime, stearic acid and phthalic anhydride were charged to a fire heated grease kettle and thoroughly mixed while warming to F. At this temperature the aqueous solution of acetic acid (80 wt. percent of acetic acid) was added, and heating was continued to 510 F. The heating was then discontinued, and the grease cooled to 250 F. with stirring. Phenyl alpha naphthylamine was then added, and the grease batch was further cooled to 180 F. The grease was then Gaulin homogenized, filtered and package The formulation and properties of the final grease composition are tabulated in Table V below:
  • EXA MPLE VI A lubricating grease containing a grease thickener prepared with hydroxy -bi1ZOiC acid as the medium weight carboxylic acid constituent was prepared by the method described above in preparing Grease H of Example 1, except that hydroxy benzoic acid rather than benzoic 13 acid was employed as the medium molecular weight carboxylic acid.
  • the present invention relates to soap-salt complexes comprising a metal salt of acetic acid, a metal salt of a medium molecular weight carboxylic acid containing from about 3 to 10 carbon atoms, and a metal soap of a high molecular weight carboxylic acid containing from about 12 to 22 carbon atoms.
  • the preferred soap-salt complexes of the invention also have a carbon atom spread between the high and medium molecular weight carboxylic acid of at least 7 and an average saponification value of acids, other than acetic acid of between about 290 to 450.
  • the mol ratio of acetic acid to the medium and high molecular weight carboxylic acids is between about 4:1 to 40:1.
  • the mol ratio of medium to high molecular weight acids will be about 0.521 to 10:1, preferably about 1:1 to 9:1.
  • Lubricating grease compositions of this invention contain complex thickeners prepared from about 4 to 20 wt. percent, preferably 8 to 12 wt. percent of acetic acid, from about 0.5 to 8 wt. percent, preferably 2 to 4 wt. percent of the medium molecular weight carboxylic acid; and from about 0.5 to 10 wt. percent, preferably 1 to 5 wt. percent of the high molecular Weight carboxylic acid, the above weight percentages being based on the total weight of the grease composition. Ordinarily, a major proportion of acetic acid will be employed in amounts up to or higher than twice the combined weight percentages of the other two acids.
  • the metal hydroxide and/or carbonate employed, e.g. lime will be employed in amounts from about 5 to 12 wt. percent, based on the total weight of the grease composition.
  • compositions prepared in accordance with the invention may contain various conventional additives, such as oxidation inhibitors, metal deactivators, corrosion preventatives, extreme pressure agents, dyes, deodorants, etc. as will be understood by those skilled in the art.
  • a lubricating grease composition which comprises a lubricating oil thickened to grease consistency within the range of 5 to 40 wt. percent of a complex of a metal salt of acetic acid, a metal salt of a medium molecular weight carboxylic acid containing from about 3 to 10 carbon atoms, and a metal soap of a high molecular weight carboxylic acid containing from about 12 to 22 carbon atoms, wherein the mol ratio of acetic to the other carboxylic acids is at least 4:1, the mol ratio of medium to high molecular weight acids is in the range of 0:5:1 to 10:1 the average difference in number of carbon atoms per molecule between the high and the medium molecular weight carboxylic acids is at least 7, the metal constituent of said soaps and salts is selected from the group consisting of alkaline earth metals and zinc, and said complex is prepared at a temperature in the range of 400 to 550 F.
  • a lubricating grease composition which comprises a mineral lubricatnig oil thickened to grease consistency within the range of 5 to 40 wt. percent of a complex prepared at a temperature in the range of 400 to 500 F. of a calcium salt of acetic acid, a calcium salt of caprylic acid and a calcium soap of hydrogenated fish oil acid, wherein the mol ratio of said acetic acid to said caprylic acid and said hydrogenated fish oil acid is about 5:1 and the mol ratio of said caprylic acid to said hydrogenated fish oil acid is about 6:1.
  • the method of preparing a lubricating grease composition which comprises dispersing a metal base, a medium molecular weight carboxylic acid containing from about 3 to 10 carbon atoms and a high molecular weight carboxylic acid containing from 12 to 22 carbon atoms in a dispersing proportion of a mineral lubricating oil, heating the dispersion to a temperature of about to F., adding acetic acid to the dispersion, and heating the resulting mixture to a temperature of about 400 to 550 F., the mol ratio of acetic to the other carboxylic acids being at least 4:1, the mol ratio of the medium to the high molecular weight acids being in the range of 0.5 :1 to 10:1, the metal constitutent of said metal base being selected from the group consisting of alkaline earth metals and zinc and the total amount of soaps and salts in said composition being in the range of 5 to 40 wt. percent.
US498743A 1955-04-01 1955-04-01 Lubricating grease compositions Expired - Lifetime US2976242A (en)

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US498743A US2976242A (en) 1955-04-01 1955-04-01 Lubricating grease compositions
GB5482/56A GB778567A (en) 1955-04-01 1956-02-22 Metal soap-salt complexes, and lubricating grease compositions containing them
DEE12078A DE1054631B (de) 1955-04-01 1956-03-12 Schmierfett und Verfahren zu seiner Herstellung
FR1148917D FR1148917A (fr) 1955-04-01 1956-03-21 Compositions de graisse lubrifiante

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Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3155619A (en) * 1962-02-12 1964-11-03 Sinclair Research Inc Complex lubricant
US3155618A (en) * 1960-04-05 1964-11-03 Socony Mobil Oil Co Inc Lubricant
US3216937A (en) * 1962-12-07 1965-11-09 Exxon Research Engineering Co Lubricant for marine diesel engines
US3223627A (en) * 1963-03-22 1965-12-14 Exxon Research Engineering Co Lubricating compositions containing metal salt of benzoic acid
US3223632A (en) * 1963-03-22 1965-12-14 Exxon Research Engineering Co Lubricating compositions containing metal salt of a bicyclo carboxylic acid
US3250709A (en) * 1964-08-31 1966-05-10 Exxon Research Engineering Co Mixed salt lubricants containing asphalt to eliminate haze
US3278431A (en) * 1963-09-27 1966-10-11 Exxon Research Engineering Co Lubricant
US3385792A (en) * 1965-11-05 1968-05-28 Exxon Research Engineering Co Lubricants containing mixed metal salt of fatty acid and diphenols
US3389084A (en) * 1965-10-29 1968-06-18 Exxon Research Engineering Co Lubricating grease containing odd and even-numbered fatty acids
US3466245A (en) * 1967-07-31 1969-09-09 Gulf Research Development Co Method of preparing calcium soap-calcium salt greases
US4130609A (en) * 1977-12-23 1978-12-19 Acf Industries, Inc. Staged accelerator pump
US20120302472A1 (en) * 2010-02-02 2012-11-29 Fuchs Petrolub Ag Lubricating Greases Containing Lignosulfonate, The Production Thereof, and the Uses Thereof
WO2013079559A1 (fr) * 2011-11-28 2013-06-06 Shell Internationale Research Maatschappij B.V. Composition de graisse
JP2014122282A (ja) * 2012-12-21 2014-07-03 Showa Shell Sekiyu Kk グリース組成物
CN104164278A (zh) * 2014-08-05 2014-11-26 中国石油化工股份有限公司 一种烧结机弹性滑道专用润滑脂组合物及制备方法
CN104164288A (zh) * 2014-08-05 2014-11-26 中国石油化工股份有限公司 一种复合钛基轴承润滑脂组合物及制备方法
CN104450086A (zh) * 2014-11-21 2015-03-25 苏州东辰林达检测技术有限公司 一种精密仪器用防霉润滑脂及其制备方法
CN104789304A (zh) * 2015-04-28 2015-07-22 天津市金海利油脂有限公司 一种烃基润滑脂及其制备方法

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Cited By (26)

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Publication number Priority date Publication date Assignee Title
US3155618A (en) * 1960-04-05 1964-11-03 Socony Mobil Oil Co Inc Lubricant
US3155619A (en) * 1962-02-12 1964-11-03 Sinclair Research Inc Complex lubricant
US3216937A (en) * 1962-12-07 1965-11-09 Exxon Research Engineering Co Lubricant for marine diesel engines
US3223627A (en) * 1963-03-22 1965-12-14 Exxon Research Engineering Co Lubricating compositions containing metal salt of benzoic acid
US3223632A (en) * 1963-03-22 1965-12-14 Exxon Research Engineering Co Lubricating compositions containing metal salt of a bicyclo carboxylic acid
US3278431A (en) * 1963-09-27 1966-10-11 Exxon Research Engineering Co Lubricant
US3250709A (en) * 1964-08-31 1966-05-10 Exxon Research Engineering Co Mixed salt lubricants containing asphalt to eliminate haze
US3389084A (en) * 1965-10-29 1968-06-18 Exxon Research Engineering Co Lubricating grease containing odd and even-numbered fatty acids
US3385792A (en) * 1965-11-05 1968-05-28 Exxon Research Engineering Co Lubricants containing mixed metal salt of fatty acid and diphenols
US3466245A (en) * 1967-07-31 1969-09-09 Gulf Research Development Co Method of preparing calcium soap-calcium salt greases
US4130609A (en) * 1977-12-23 1978-12-19 Acf Industries, Inc. Staged accelerator pump
US20120302472A1 (en) * 2010-02-02 2012-11-29 Fuchs Petrolub Ag Lubricating Greases Containing Lignosulfonate, The Production Thereof, and the Uses Thereof
WO2013079559A1 (fr) * 2011-11-28 2013-06-06 Shell Internationale Research Maatschappij B.V. Composition de graisse
US9290715B2 (en) 2011-11-28 2016-03-22 Shell Oil Company Grease composition
CN103958653A (zh) * 2011-11-28 2014-07-30 国际壳牌研究有限公司 润滑脂组合物
CN103958653B (zh) * 2011-11-28 2018-04-03 国际壳牌研究有限公司 润滑脂组合物
RU2637123C2 (ru) * 2011-11-28 2017-11-30 Шелл Интернэшнл Рисерч Маатсхаппий Б.В. Композиция консистентной смазки
KR102127029B1 (ko) 2012-12-21 2020-06-26 쉘 인터내셔날 리써취 마트샤피지 비.브이. 그리스 조성물
JP2014122282A (ja) * 2012-12-21 2014-07-03 Showa Shell Sekiyu Kk グリース組成物
KR20150099565A (ko) * 2012-12-21 2015-08-31 쉘 인터내셔날 리써취 마트샤피지 비.브이. 그리스 조성물
US20150315509A1 (en) * 2012-12-21 2015-11-05 Shell Oil Company Grease copositions
CN104164288A (zh) * 2014-08-05 2014-11-26 中国石油化工股份有限公司 一种复合钛基轴承润滑脂组合物及制备方法
CN104164278A (zh) * 2014-08-05 2014-11-26 中国石油化工股份有限公司 一种烧结机弹性滑道专用润滑脂组合物及制备方法
CN104450086B (zh) * 2014-11-21 2017-09-12 深圳市合诚润滑材料有限公司 一种精密仪器用防霉润滑脂及其制备方法
CN104450086A (zh) * 2014-11-21 2015-03-25 苏州东辰林达检测技术有限公司 一种精密仪器用防霉润滑脂及其制备方法
CN104789304A (zh) * 2015-04-28 2015-07-22 天津市金海利油脂有限公司 一种烃基润滑脂及其制备方法

Also Published As

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DE1054631B (de) 1959-04-09
FR1148917A (fr) 1957-12-18
GB778567A (en) 1957-07-10

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