US2446177A - Silicone grease and method of preparation - Google Patents

Silicone grease and method of preparation Download PDF

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Publication number
US2446177A
US2446177A US600777A US60077745A US2446177A US 2446177 A US2446177 A US 2446177A US 600777 A US600777 A US 600777A US 60077745 A US60077745 A US 60077745A US 2446177 A US2446177 A US 2446177A
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silicone
grease
parts
soap
lithium stearate
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US600777A
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George M Hain
William A Zisman
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Priority to FR962224D priority Critical patent/FR962224A/fr
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Priority to US600777A priority patent/US2446177A/en
Priority to GB5604/48A priority patent/GB652754A/en
Application granted granted Critical
Publication of US2446177A publication Critical patent/US2446177A/en
Priority to DED5800A priority patent/DE850047C/de
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    • 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
    • C10M169/00Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/02Mixtures of base-materials and thickeners
    • 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
    • C10M2205/00Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/026Butene
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    • 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
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    • 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
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    • 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
    • C10M2207/14Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings
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    • 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
    • C10M2207/14Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings
    • C10M2207/142Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings polycarboxylic
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    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/16Naphthenic acids
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    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/04Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
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    • 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
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    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/26Amines
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    • C10M2229/00Organic 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
    • C10M2229/04Siloxanes with specific structure
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    • C10M2229/00Organic 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
    • C10M2229/04Siloxanes with specific structure
    • C10M2229/041Siloxanes with specific structure containing aliphatic substituents
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    • C10M2229/00Organic 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
    • C10M2229/04Siloxanes with specific structure
    • C10M2229/042Siloxanes with specific structure containing aromatic substituents
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    • C10M2229/00Organic 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
    • C10M2229/04Siloxanes with specific structure
    • C10M2229/043Siloxanes with specific structure containing carbon-to-carbon double bonds
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    • C10M2229/00Organic 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
    • C10M2229/04Siloxanes with specific structure
    • C10M2229/044Siloxanes with specific structure containing silicon-to-hydrogen bonds
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    • C10N2010/00Metal present as such or in compounds
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    • C10N2010/00Metal present as such or in compounds
    • C10N2010/02Groups 1 or 11
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    • C10N2010/00Metal present as such or in compounds
    • C10N2010/04Groups 2 or 12
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    • C10N2010/00Metal present as such or in compounds
    • C10N2010/06Groups 3 or 13
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    • C10N2020/00Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01Physico-chemical properties
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    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/08Resistance to extreme temperature
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    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/12Inhibition of corrosion, e.g. anti-rust agents or anti-corrosives
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    • C10N2040/00Specified use or application for which the lubricating composition is intended
    • C10N2040/02Bearings
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    • C10N2040/00Specified use or application for which the lubricating composition is intended
    • C10N2040/12Gas-turbines
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    • C10N2040/00Specified use or application for which the lubricating composition is intended
    • C10N2040/12Gas-turbines
    • C10N2040/13Aircraft turbines
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    • C10N2050/00Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10Semi-solids; greasy
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    • C10N2070/00Specific manufacturing methods for lubricant compositions

Definitions

  • This invention relates to lubricating compositions and to a method for their preparation.
  • the invention accordingly, comprises the lubricating compositions or greases having the properties and the relation of components which will be exemplified in the compositions hereinafter described and the method of preparing such compositions which method of preparation involves the several steps and relation of one or more of such steps with respect to each of the others thereof and will be exemplified in detail in the processes hereinafter described and illustrated, and the scope of the invention will be indicated in the claims.
  • organo-silicon compounds One class of organo-silicon compounds is illustrated by polymeric compositions of the following general structure:
  • R, R1, R2, R3, R4 and R5 represent any alkyl, aryl, alkaryl or arallq l radicals, which compounds are available in the form of more or less viscous, oil-like fluids and, in general, are water-white and characterized by such properties as great thermal stability and high viscosity index.
  • Relatively common compounds of this type are dimethyl silicone, diethyl silicone, ethyl methyl silicone, di-phenyl silicone, di-tolyl silicone, phenyl tolyl silicone, methyl phenyl silicone, ethyl phenyl silicone and alkyl aryl silicone polymers.
  • dimethyl silicone polymer having a viscosity of about centistokes, one of the most common fluids corresponding to the above general formula, has no inherent rust inhibiting valuesuch as that possessed by many hydrocarbon oils and it will be found that it is not a boundary lubricant and seizure will occur in bearings employing it as a lubricant.
  • suitable alkali-metal fatty acid soap such as lithium stearate
  • a concentration of about 2 per cent in a hydrocarbon fraction of relatively low boiling range for example, about 100 to 440 F.
  • heating the mixture to the solvation temperature of the soap and maintaining it at substantially such temperature a gel structure will result.
  • the silicone fluid which must be one which is miscible with the hydrocarbon fraction, is added, agitated to form a homogeneous mix and the petroleum fraction removed to
  • the general property which the hydrocarbon fraction should have is that it be relatively low-boiling and that it be miscible with the silicone fluid to be used as the grease base.
  • the solvent should preferably have a boiling range well below that of the silicone oil,,for example 100 below that of the oil and it should have no heavy ends. However, the boiling range of the solvent should be high enough to approach the solvation temperature of the soap which is generally close to its melting temperature.
  • hydrocarbon solvents having boiling ranges of about 300 to 400 F. are suitable at atmospheric pressure or low boiling point solvents can be used at 300-400 F. under pressure.
  • Such hydrocarbon fractions or mutual solvents are benzene, petroleum ether, naphthas, deodorized kerosene and, generally; those hydrocarbon fractions used as insecticide carrying oils are useful in that they have the right boiling temhaving a silicone fluid as a base can be prepared with any desired soap concentration.
  • Example I 1 Lithium stearate, 2 parts, was dispersed in 100 parts by weight of a petroleum fraction having a boiling range of 300 to 400 F. (100 F. flash point naphtha) and the mixture heated to about 300 and maintained at that temperature until the lithium stearate had gone into solution to form a thick gel. Twenty-two (22) parts by weight of phenyl silicone (Dow-Corning 700 serles) having a viscosity of about 100 centistokes at 25 C. was added to the lithium soap-petroleum fraction gel at the elevated temperature and the mass'mixed to a uniform consistency.
  • phenyl silicone Dow-Corning 700 serles
  • Example III of the mixture in the bomb had developed, the I pressure was released and the petroleum ether allowed to evaporate off to leave behind a smooth homogeneous grease comprising about 15 per cent of lithium soap in dimethyl silicone.
  • Example IV Four (4) parts of lithium stearate were dispersed in 30 parts of Stoddard Solvent and the mixture heated to 150 C. in an open vessel to complete solvation of the soap. When a maximum thickening had been attained, approxiperature of about 200 to 250 F. in a vessel under a reduced pressure of 10 millimeters of mercury in order to assist in the removal of the petroleum fraction. The product, upon the removal of the petroleum fraction, was a stable grease of very smooth consistency having a soap concentration of about 9 per cent. I
  • Balancing ingredients such as corrosion inhibitors
  • Example V Three (3) parts of lithium stearate were dispersed in 35 parts of deodorized kerosene (boiling range 425-475 F.) and the mixture heated to 250 C. to effect solvation of the soap therein. Upon the formation of a thick gel, there were eflect solvation of the soap.
  • Example VI with the result that a very thick gel was left in the vessel.
  • 20 parts of diethyl and dimethyl silicone polymer (1-1 by weight) were added and the total mixture agitated and held at 150 C. until a completely homogeneous mix was formed.
  • the mix was then poured into a shallow pan and held at a temperature of about 125 C. in a current of warm air until all of the solvent had been removed before it was allowed to cool.
  • Example VII Lithium stearate, 6 parts, was dispersed in about 200 parts by weight of a petroleum traction having a boiling range of 300 to 400 F. (100 flash naphtha) and the mixture heated to about 300 and maintained at that temperature until the lithium stearate had gone into solution to form a thickened gel. As pointed out in connection with other examples, the completion 01' this stage is identifiable as the point at which maximum thickening of the solution occurs. Fortytwo (42) parts by weight of a mixture of phenyl silicone polymer and ethyl silicone polymer (approximately 1-1 by weight) were added to the gel after evaporating off from the gel part of the solvent used for solvating the soap. The
  • compositions of these examples thus contemplate using more than 70 parts of the silicone polymer blended with less than 30 parts of the lithium stearate.
  • the method of preparing. silicone-base grease compositions in accordance with the invention comprises blending a soap with the silicone fluid by employing a relatively low-boiling petroleum or hydrocarbon fraction as a mutual solvent for bringing the soap into colloidal solution in the base fluid.
  • a relatively low-boiling petroleum or hydrocarbon fraction as a mutual solvent for bringing the soap into colloidal solution in the base fluid.
  • silicone fluid used as a base for the grease be compatible with the petroleum fraction 6 l i and that the latter has no heavy ends.
  • composition is made up almost entirely of the ingredients recited and these ingredients are the main and characterizin ones, but this expression does not exclude the presence of minor amounts of other ingredients which are commonly employed in lubricating compositions or which are merely inert. Such added ingredients would not change the essential character of the composition.
  • a lubricant consisting essentially of, an organo-silicon polymer as a base fluid blended with a minor amount of lithium stearate to produce a stable grease.
  • a lubricating composition consisting essentially of. as a base fluid, more than 70 parts of an alkyl silicone polymer having a viscosity of about centistokes at 26 C. blended with less than 30 parts of lithium stearate to produce a stable grease.
  • a lubricating composition consisting essentially of, as a base fluid. more than 70 parts of an aryl silicone polymer having a viscosity of about 100 centistokes at 25 C. blended. with less than 30 parts of lithium stearate to produce a stable grease.
  • a lubricating composition consisting essentially of, as a base fluid, more than 70 parts of a mixed alkyl-aryl silicone polymer having a viscosity of aboutlOO centistokes at 25 C. blended with less than 30 parts of lithium's'tearate to produce a stable grease.
  • a lubricating composition consisting essentially of. as a base fluid, about 85 parts of dimethyl silicone having a viscosity of about 100 centistokes at 25 C. blended with about 15 parts of lithium stearate to produce a stable grease.
  • a lubricating composition consisting essentially of, as a base fluid, about 85 parts of diphenyl silicone polymer having a viscosity of about 100 centistoks at 25 C. blended with about 15 parts of lithium stearate to produce a stable grease.
  • a silicone-base grease consisting essentially of, dispersing about 2 parts of lithium stearate in about 100parts of a petroleum fraction which boils in the range of about 200 to 400 F., heating said dispersion of lithium stearate in said petroleum fraction to about 300 F. to produce solvation of the lithium stearate therein to form a solution of about 2 per cent concentration, adding to the solution thus obtained about 20 parts of a silicone fluid which is miscible with said petroleum fraction, maintaining said mixture at about 'solvation temperature until homogeneity is attained, and removing the petroleum fraction by evaporation to leave a residue of a stable grease containing about 12 per cent of lithium stearate dispersed, in the silicone base fluid, I i

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)
US600777A 1945-06-21 1945-06-21 Silicone grease and method of preparation Expired - Lifetime US2446177A (en)

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Application Number Priority Date Filing Date Title
FR962224D FR962224A (it) 1945-06-21
US600777A US2446177A (en) 1945-06-21 1945-06-21 Silicone grease and method of preparation
GB5604/48A GB652754A (en) 1945-06-21 1948-02-25 Silicone greases and method of preparation
DED5800A DE850047C (de) 1945-06-21 1950-09-21 Abschmierfette

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Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2508741A (en) * 1948-04-12 1950-05-23 Texas Co Lubricating grease composition
US2551931A (en) * 1948-09-29 1951-05-08 Dow Corning Polysiloxane grease and method of preparation
US2599917A (en) * 1950-01-25 1952-06-10 Dow Corning Siloxane lubricants
US2599984A (en) * 1949-02-07 1952-06-10 Dow Corning Lubricant consisting of copolymeric siloxanes substituted with methyl, phenyl, and halogenated-aryl radicals
US2616850A (en) * 1949-11-22 1952-11-04 Standard Oil Co Grease preparation
US2642395A (en) * 1952-02-08 1953-06-16 Dow Corning Siloxane boundary lubricants
US2652364A (en) * 1951-12-29 1953-09-15 Shell Dev High-temperature grease compositions
US2654710A (en) * 1951-06-22 1953-10-06 California Research Corp Polysiloxane-aluminum soap greases
US2677661A (en) * 1950-02-21 1954-05-04 Standard Oil Dev Co Bentonite greases
US2681313A (en) * 1950-02-20 1954-06-15 California Research Corp Alkyl orthosilicate and alkoxysiloxane base grease compositions
US2684944A (en) * 1952-06-02 1954-07-27 Standard Oil Co Lithium polyorgano siloxane polymer grease compositions
US2693449A (en) * 1948-08-13 1954-11-02 George M Hain Silicone greases
US2756212A (en) * 1956-07-24 Siloxyglycol
US2758981A (en) * 1952-10-29 1956-08-14 Exxon Research Engineering Co Corrosion preventive composition
US2826551A (en) * 1954-01-04 1958-03-11 Simoniz Co Nontangling shampoo
US2861950A (en) * 1955-02-28 1958-11-25 Theodore A Renshaw Method for grease manufacture utilizing fused metallic soaps
US3047497A (en) * 1960-08-15 1962-07-31 Gen Electric Greases thickened with metal salts of carboxyalkylpolysiloxanes
US3047499A (en) * 1960-08-15 1962-07-31 Gen Electric Grease compositions
US3120184A (en) * 1960-04-22 1964-02-04 Universal Match Corp Pyrotechnical devices and methods of making the same

Families Citing this family (3)

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DE943188C (de) * 1953-04-30 1956-05-17 Standard Oil Dev Co Schmiermittel
DE1001793B (de) * 1955-04-26 1957-01-31 Goldschmidt Ag Th Metallseifenhaltige Abschmierfette
GB2506974A (en) * 2012-08-14 2014-04-16 Dow Corning Lubricant compositions

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US2274674A (en) * 1940-04-05 1942-03-03 Clarence E Earle Lubricant containing a lithium compound
US2274673A (en) * 1940-04-05 1942-03-03 Clarence E Earle Lubricating composition
US2350906A (en) * 1938-05-20 1944-06-06 Frank S Busser Lubricant grease
US2351280A (en) * 1942-07-16 1944-06-13 Cities Service Oil Co Lubricant
US2354171A (en) * 1942-06-23 1944-07-18 Cities Service Oil Co Lubricant
US2362767A (en) * 1942-06-03 1944-11-14 Cities Service Oil Co Lubricants
US2375007A (en) * 1943-04-15 1945-05-01 Shell Dev Antifoaming composition
US2407037A (en) * 1939-10-21 1946-09-03 Frank J Sowa Lubricant and process of lubricating surfaces therewith

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US2350906A (en) * 1938-05-20 1944-06-06 Frank S Busser Lubricant grease
US2407037A (en) * 1939-10-21 1946-09-03 Frank J Sowa Lubricant and process of lubricating surfaces therewith
US2274674A (en) * 1940-04-05 1942-03-03 Clarence E Earle Lubricant containing a lithium compound
US2274673A (en) * 1940-04-05 1942-03-03 Clarence E Earle Lubricating composition
US2362767A (en) * 1942-06-03 1944-11-14 Cities Service Oil Co Lubricants
US2354171A (en) * 1942-06-23 1944-07-18 Cities Service Oil Co Lubricant
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Cited By (19)

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Publication number Priority date Publication date Assignee Title
US2756212A (en) * 1956-07-24 Siloxyglycol
US2508741A (en) * 1948-04-12 1950-05-23 Texas Co Lubricating grease composition
US2693449A (en) * 1948-08-13 1954-11-02 George M Hain Silicone greases
US2551931A (en) * 1948-09-29 1951-05-08 Dow Corning Polysiloxane grease and method of preparation
US2599984A (en) * 1949-02-07 1952-06-10 Dow Corning Lubricant consisting of copolymeric siloxanes substituted with methyl, phenyl, and halogenated-aryl radicals
US2616850A (en) * 1949-11-22 1952-11-04 Standard Oil Co Grease preparation
US2599917A (en) * 1950-01-25 1952-06-10 Dow Corning Siloxane lubricants
US2681313A (en) * 1950-02-20 1954-06-15 California Research Corp Alkyl orthosilicate and alkoxysiloxane base grease compositions
US2677661A (en) * 1950-02-21 1954-05-04 Standard Oil Dev Co Bentonite greases
US2654710A (en) * 1951-06-22 1953-10-06 California Research Corp Polysiloxane-aluminum soap greases
US2652364A (en) * 1951-12-29 1953-09-15 Shell Dev High-temperature grease compositions
US2642395A (en) * 1952-02-08 1953-06-16 Dow Corning Siloxane boundary lubricants
US2684944A (en) * 1952-06-02 1954-07-27 Standard Oil Co Lithium polyorgano siloxane polymer grease compositions
US2758981A (en) * 1952-10-29 1956-08-14 Exxon Research Engineering Co Corrosion preventive composition
US2826551A (en) * 1954-01-04 1958-03-11 Simoniz Co Nontangling shampoo
US2861950A (en) * 1955-02-28 1958-11-25 Theodore A Renshaw Method for grease manufacture utilizing fused metallic soaps
US3120184A (en) * 1960-04-22 1964-02-04 Universal Match Corp Pyrotechnical devices and methods of making the same
US3047497A (en) * 1960-08-15 1962-07-31 Gen Electric Greases thickened with metal salts of carboxyalkylpolysiloxanes
US3047499A (en) * 1960-08-15 1962-07-31 Gen Electric Grease compositions

Also Published As

Publication number Publication date
FR962224A (it) 1950-06-07
DE850047C (de) 1952-09-22
GB652754A (en) 1951-05-02

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