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US2864766A - Utilization of mixtures of organic and inorganic acids in the preparation of greases - Google Patents

Utilization of mixtures of organic and inorganic acids in the preparation of greases Download PDF

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Publication number
US2864766A
US2864766A US550176A US55017655A US2864766A US 2864766 A US2864766 A US 2864766A US 550176 A US550176 A US 550176A US 55017655 A US55017655 A US 55017655A US 2864766 A US2864766 A US 2864766A
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United States
Prior art keywords
acid
lubricating
grease
percent
molecular weight
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
US550176A
Inventor
Arnold J Morway
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.)
ExxonMobil Technology and Engineering Co
Original Assignee
Exxon Research and Engineering Co
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Filing date
Publication date
Application filed by Exxon Research and Engineering Co filed Critical Exxon Research and Engineering Co
Priority to US550176A priority Critical patent/US2864766A/en
Priority to DEE13277A priority patent/DE1052041B/en
Priority to FR1165143D priority patent/FR1165143A/en
Application granted granted Critical
Publication of US2864766A publication Critical patent/US2864766A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • 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
    • 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
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    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/08—Inorganic acids or salts thereof
    • C—CHEMISTRY; METALLURGY
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    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/08—Inorganic acids or salts thereof
    • C10M2201/081—Inorganic acids or salts thereof containing halogen
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    • C10M2201/082—Inorganic acids or salts thereof containing nitrogen
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    • C10M2201/084—Inorganic acids or salts thereof containing sulfur, selenium or tellurium
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    • C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
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    • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/04—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
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    • C10M2215/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
    • C10M2215/064—Di- and triaryl amines
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    • C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/042—Sulfate esters
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    • C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/044—Sulfonic acids, Derivatives thereof, e.g. neutral salts
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    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/06—Thio-acids; Thiocyanates; Derivatives thereof
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    • C10M2219/08—Thiols; Sulfides; Polysulfides; Mercaptals
    • C10M2219/082—Thiols; Sulfides; Polysulfides; Mercaptals containing sulfur atoms bound to acyclic or cycloaliphatic carbon atoms
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    • C10M2219/082—Thiols; Sulfides; Polysulfides; Mercaptals containing sulfur atoms bound to acyclic or cycloaliphatic carbon atoms
    • C10M2219/085—Thiols; Sulfides; Polysulfides; Mercaptals containing sulfur atoms bound to acyclic or cycloaliphatic carbon atoms containing carboxyl groups; Derivatives thereof
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    • C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
    • C10M2223/04—Phosphate esters
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    • C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
    • C10M2223/04—Phosphate esters
    • C10M2223/042—Metal salts thereof
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    • C10M2229/04—Siloxanes with specific structure
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    • C10M2229/041—Siloxanes with specific structure containing aliphatic substituents
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    • C10M2229/04—Siloxanes with specific structure
    • C10M2229/043—Siloxanes with specific structure containing carbon-to-carbon double bonds
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    • C10M2229/04—Siloxanes with specific structure
    • C10M2229/044—Siloxanes with specific structure containing silicon-to-hydrogen bonds
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    • 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
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    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/04—Groups 2 or 12
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    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/06—Groups 3 or 13
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    • 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 lubricating grease compositions, and more particularly to lubricating oil thickened to grease consistency with neutralized blends or mixtures of low molecular weight carboxylic acids and mineral acids and stabilized with a minor amount of an aluminum soap of a high molecular weight carboxylic acid.
  • this invention pertains to the stabilization of lubricating grease compositions containing as the thickening agent an alkaline earth metal neutralized blend of a low molecular weight carboxylic acid, e. g. acetic acid, with a strong inorganic acid, e. g. phosphoric acid, and an aluminum soap of a high molecular weight fatty acid, e. g. aluminum stearate.
  • a low molecular weight carboxylic acid e. g. acetic acid
  • a strong inorganic acid e. g. phosphoric acid
  • aluminum soap of a high molecular weight fatty acid e. g. aluminum stearate.
  • Suitable low molecular weight carboxylic acids include saturated and unsaturated aliphatic carboxylic acids having from about 1 to about 3 carbon atoms per molecule such as formic acid, acetic acid, propionic acid, etc.
  • Acetic acid is the preferred low molecular weight carboxylic acid of this invention and may be either glacial acetic acid or an aqueous solution thereof, the concentration of the acetic acid in the aqueous solution varying from about 60 to 99.9 wt. percent.
  • Substituted acetic acids having two carbon atoms per molecule such as chloro-acetic 'acid, glycolic acid, thioglycolic acid, glycine, etc.
  • the amount of low molecular weight carboxylic acid employed will be within the range of about 5 to 20 wt. percent, preferably about 10 to 15 wt. percent, based on the total lubricating composition.
  • the mineral acids which may be employed in this invention include phosphoric acid, nitric acid, sulphuric acid, hydrochloric acid and mixtures of any combination of these acids.
  • concentrations of the mineral acids may vary from about 5% to 100%.
  • the strong inorganic acids are utilized in amounts ranging from about 3 to 15 wt. percent, preferably about 5 to 10 wt. percent, based on the total lubricating composition.
  • the stabilizing agent of this invention is an aluminum soap of a high molecular weight carboxylic acid having from about 16 to 22 carbon atoms per molecule.
  • Aluminum stearate is preferred, though soaps of palmitic acid, arachidic acid, behenic acid, etc. may also be employed to stabilize the lubricating grease compositions of this invention. Only stabilizing proportions of the aluminum soap of from about 2 to 10 wt. percent, preferably about 3 to 6 wt. percent, based on the total lubricating composition, need be used.
  • Suitable metal bases for neutralizing the blends of low molecular weight carboxylic acids and mineralacids include the alkaline earth metals: calcium, barium, magnesium and strontium; and the alkali metals: sodium, potassium and lithium.
  • the alkaline earth metals are preferred, and calcium is especially preferred.
  • the grease-making process of this invention will utilize from about 10 to 20 wt. percent based on the total lubricating composition, of the metal hydroxide or carbonate. Mixtures of the above metals may also be employed, if desired.
  • the lubricating oils employed as the menstrua of the lubricating compositions of this invention may be either conventional grease-making mineral oils or synthetic lubricating oils.
  • the mineral and synthetic lubricating oils should have a viscosity within the range of about 50 to 2000 S. U. S. at 100 F. and about 30 to 200 S. U. S. at 210' R, an ASTM pour point of about +20 to F., a flash point of about 350 to 650 F., and a viscosity index of about 0 to 60, although lubricating oils having a viscosity index; of or higher can also be employed.
  • the preferred menstrum is a mineral lubricating oil.
  • the synthetic lubricating oils include esters of monobasic acids (e; g. an ester of C alcohol with C OX0 acid, an ester of C 0x0 alcohol with octanoic acid, etc.), esters of dibasic acids (e. g. di-Z-ethyl hexyl sebacate, dinonyl adipate, etc.), esters of glycols (e. g. C Oxo acid diester o-f tetraethylene glycol, etc), complex esters (e. g.
  • chlorotrifluoroethylene containing twelve recurring units of chlorotrifluoroethylene alkyl silicates (e. g. methyl polysiloxanes, ethyl polysiloxanes, methyl-phenyl polysiloxanes, etc.), sulfite esters (e. g. ester formed by reacting one mole of sulfur oxychloride with two moles of the methyl ether of ethylene glycol, etc.), carbonates (e. gather carbonateformed by reacting C Oxo alcohol .with ethyl carbonate to form a half ester and reacting this .half ester with tetraethylene glycol), mercaptals (e. g.
  • formals e. g. the formal formed by reacting C OX alcohol with formaldehyde
  • .polyglycol type synthetic oils e. g. the compounds formed by condensing butyl alcohol with fourteen units .of propylene. oxide, etc.
  • the lubricating compositions of the invention will con- :tain about 50. to 90 wt. percent, preferably about 60 to -80.wt..percent, of. the mineral .and/or synthetic lubricating oil and about 10 to 50 wt. percent, preferably about -20 to 40 .wt. percent of the reaction products of blends .ofithcabove acids with the metal base plus the aluminum .soap.
  • the lubricating grease compositions of this :invention may be prepared by coneutralization of a blend immediately.
  • the preferred method for preparing the lubricating compositions of the invention involves dispersing the .aluminum soa in the lubricating oil at a temperature of -from about 270 to 350 F. with stirring.
  • the resulting dispersion is cooled to room temperature, preferably by pan cooling.
  • the .cold aluminumsoap-lubricating oil dispersion is then charged to a grease kettle equipped with means for efficient stirring.
  • the metal hydroxide is .added with stirring to obtain a smooth uniform slurry.
  • the low molecular Weight carboxylic acid blended with t the mineral acid is then added to the grease kettle with stirring.
  • a solid grease forms almost immediately withoutthe application of external heat. Stirring is continued until the temperature subsides from about 180 to 210 F. to about 100 to 140 F.
  • the resulting grease composition may be finished by passage through a Morehouse .mill or Gaulin homogenizer at high rates of shear.
  • a portion of the lubricating oil is a saponifiable synthetic oil
  • lubricating grease additives may also be employed in the lubricating compositions of the present invention.
  • additives for example, include: oxida .tion inhibitors, such as phenyl alpha naphthylamine, cor
  • rosion inhibitors such as sorbitan monooleate, tackiness agents such as polyisobutene or high molecular weight polymerized acrylic esters, load-carrying compounds such as sulfurized and/or phosphorous and/or chlorine containing oil-soluble materials, and the like.
  • a lubricating grease composition according to this invention was prepared from the following constituents:
  • the aluminum stearate was dispersed in all of the mineral lubricating oil by heating to a temperature of about 300 F. with stirring.
  • the resulting dispersion was cooled to room temperature in pans. Just prior to drawing into the pans, the phenyl alpha naphthylamine was added to the dispersion.
  • the cooled dispersion was then charged to a grease kettle, and the lime added with mixing to obtain a smooth uniform slurry.
  • a blend of the acetic acid and the phosphoric acid was then charged to the grease kettle. Without heating the resulting grease batch, the temperature rose to about 190 F. Stirring was continued until the temperature subsided, and the grease was finished by being passed through a Gaulin homogenizer.
  • Lubrication lite (hours) (250, F. 1000+.
  • Lubri ation lile hours (250 F. 850. 10,000 R. P.
  • a lubricating composition comprising a major amount of a lubricating oil, and an alkaline earth metal neutralized blend of 5 to 20 wt. percent low molecular weight carboxylic acid having from about 1 to 3 carbon atoms per molecule and 3 to 15 wt. percent mineral acid, and 3 to 6 wt. percent aluminum soap, all of said weight percentages being based on the total weight of the lubricating composition.
  • a lubricating grease composition which consists essentially of dispersing an aluminum soap of a high molecular weight carboxylic acid having from about 16 to 22 carbon atoms per molecule in a lubricating oil by heating, cooling said dispersion to ambient temperature, adding an alkaline earth metal hydroxide to said cooled dispersion, then adding a blend of a low molecular weight carboxylic acid having from about 1 to 3 carbon atoms per molecule and a mineral acid to the resulting mixture to obtain said lubricating grease composition.

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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)

Description

UTILIZATION OF MIXTURES OF ORGANIC AND IfiiglggglgllC ACIDS IN THE PREPARATION OF Arnold J. Morway, Clark, N. J., assignor to Esso Research and Engineering Company, a corporation of Delaware No Drawing. Application November 30, 1955 Serial No. 550,176
9 Claims. (Cl. 25236) This invention relates to lubricating grease compositions, and more particularly to lubricating oil thickened to grease consistency with neutralized blends or mixtures of low molecular weight carboxylic acids and mineral acids and stabilized with a minor amount of an aluminum soap of a high molecular weight carboxylic acid.
In brief, this invention pertains to the stabilization of lubricating grease compositions containing as the thickening agent an alkaline earth metal neutralized blend of a low molecular weight carboxylic acid, e. g. acetic acid, with a strong inorganic acid, e. g. phosphoric acid, and an aluminum soap of a high molecular weight fatty acid, e. g. aluminum stearate.
When the metal salts of low molecular weight carboxylic acids are dispersed in lubricating oils, the reacid in lubricating grease compositions containing large amounts of metal soaps as the thickening agent has previously been suggested in the art. In U. S. Patent No. 2,513,680 to Schott and Armstrong, for example, less than about 2.0% by weight of calcium phosphate is employed to improve the skin hardening and storage stability properties of calcium base greases.
It has now been found that a large amount of a mineral acid in combination with a low molecular weight carboxylic acid can effectively thicken a lubricating oil to grease consistency provided that a minor amount of aluminum soap of a high molecular weight acid is employed in conjunction therewith. The aluminum soap appears to prevent the grease composition from separating oil during storage over long periods of time and to prevent the thickening agent from agglomerating and settling out of the lubricating composition.
It is not known what reactions the strong inorganic acid enters into during the grease preparation method of this invention. When nitric acid is employed, for example, the resulting grease composition had a distinctive red color, as hereinafter shown. However, for the purposes of this invention it is suificient to note that lubricating compositions encompassed therein are prepared by utilizing blends or mixtures of the low molecular weight carboxylic acids and mineral acids.
Suitable low molecular weight carboxylic acids include saturated and unsaturated aliphatic carboxylic acids having from about 1 to about 3 carbon atoms per molecule such as formic acid, acetic acid, propionic acid, etc. Acetic acid is the preferred low molecular weight carboxylic acid of this invention and may be either glacial acetic acid or an aqueous solution thereof, the concentration of the acetic acid in the aqueous solution varying from about 60 to 99.9 wt. percent. Substituted acetic acids having two carbon atoms per molecule such as chloro-acetic 'acid, glycolic acid, thioglycolic acid, glycine, etc. may also be used to modify the structure of lubricating compositions made in accordance with this invention. The amount of low molecular weight carboxylic acid employed will be within the range of about 5 to 20 wt. percent, preferably about 10 to 15 wt. percent, based on the total lubricating composition.
The mineral acids which may be employed in this invention include phosphoric acid, nitric acid, sulphuric acid, hydrochloric acid and mixtures of any combination of these acids. The concentrations of the mineral acids may vary from about 5% to 100%. The strong inorganic acids are utilized in amounts ranging from about 3 to 15 wt. percent, preferably about 5 to 10 wt. percent, based on the total lubricating composition.
The stabilizing agent of this invention is an aluminum soap of a high molecular weight carboxylic acid having from about 16 to 22 carbon atoms per molecule. Aluminum stearate is preferred, though soaps of palmitic acid, arachidic acid, behenic acid, etc. may also be employed to stabilize the lubricating grease compositions of this invention. Only stabilizing proportions of the aluminum soap of from about 2 to 10 wt. percent, preferably about 3 to 6 wt. percent, based on the total lubricating composition, need be used.
Suitable metal bases for neutralizing the blends of low molecular weight carboxylic acids and mineralacids include the alkaline earth metals: calcium, barium, magnesium and strontium; and the alkali metals: sodium, potassium and lithium. The alkaline earth metals are preferred, and calcium is especially preferred. Ordinarily, the grease-making process of this invention will utilize from about 10 to 20 wt. percent based on the total lubricating composition, of the metal hydroxide or carbonate. Mixtures of the above metals may also be employed, if desired.
The lubricating oils employed as the menstrua of the lubricating compositions of this invention may be either conventional grease-making mineral oils or synthetic lubricating oils. In general, the mineral and synthetic lubricating oils should have a viscosity within the range of about 50 to 2000 S. U. S. at 100 F. and about 30 to 200 S. U. S. at 210' R, an ASTM pour point of about +20 to F., a flash point of about 350 to 650 F., and a viscosity index of about 0 to 60, although lubricating oils having a viscosity index; of or higher can also be employed. When a strong acid like nitric or sulphuric is used in high concentrations according to the present invention, the preferred menstrum is a mineral lubricating oil.
The synthetic lubricating oils include esters of monobasic acids (e; g. an ester of C alcohol with C OX0 acid, an ester of C 0x0 alcohol with octanoic acid, etc.), esters of dibasic acids (e. g. di-Z-ethyl hexyl sebacate, dinonyl adipate, etc.), esters of glycols (e. g. C Oxo acid diester o-f tetraethylene glycol, etc), complex esters (e. g. the complex ester formed by reacting one mole of tetraethylene glycol with two moles of sesacic acid and two moles of Z-ethyI-hexanol, a complex ester formed by reacting one mole of azelaic acid, one mole of tetraethylene glycol, one mole of C Oxo alcohol and one mole of C Oxo acid), esters of phosphoric acid (e. g. the ester formed by contacting three moles of the mono-methyl ether of ethylene glycol with one mole of phosphorous oxychloride, etc.), halocarbon oils (e. g. the polymer of Patented Dec. 16, 1958 chlorotrifluoroethylene containing twelve recurring units of chlorotrifluoroethylene), alkyl silicates (e. g. methyl polysiloxanes, ethyl polysiloxanes, methyl-phenyl polysiloxanes, etc.), sulfite esters (e. g. ester formed by reacting one mole of sulfur oxychloride with two moles of the methyl ether of ethylene glycol, etc.), carbonates (e. gather carbonateformed by reacting C Oxo alcohol .with ethyl carbonate to form a half ester and reacting this .half ester with tetraethylene glycol), mercaptals (e. g. the mercaptal formed by reacting Z-ethyl hexyl mercap'tan with formaldehyde), formals (e. g. the formal formed by reacting C OX alcohol with formaldehyde), .polyglycol type synthetic oils (e. g. the compounds formed by condensing butyl alcohol with fourteen units .of propylene. oxide, etc.), or mixtures of the above in any proportions.
The lubricating compositions of the invention will con- :tain about 50. to 90 wt. percent, preferably about 60 to -80.wt..percent, of. the mineral .and/or synthetic lubricating oil and about 10 to 50 wt. percent, preferably about -20 to 40 .wt. percent of the reaction products of blends .ofithcabove acids with the metal base plus the aluminum .soap.
lngeneral, the lubricating grease compositions of this :invention may be prepared by coneutralization of a blend immediately.
The preferred method for preparing the lubricating compositions of the invention involves dispersing the .aluminum soa in the lubricating oil at a temperature of -from about 270 to 350 F. with stirring. The resulting dispersion is cooled to room temperature, preferably by pan cooling. The .cold aluminumsoap-lubricating oil dispersion is then charged to a grease kettle equipped with means for efficient stirring. The metal hydroxide is .added with stirring to obtain a smooth uniform slurry.
The low molecular Weight carboxylic acid blended with t the mineral acid is then added to the grease kettle with stirring. A solid grease forms almost immediately withoutthe application of external heat. Stirring is continued until the temperature subsides from about 180 to 210 F. to about 100 to 140 F. The resulting grease composition may be finished by passage through a Morehouse .mill or Gaulin homogenizer at high rates of shear.
Only a portion of the total lubricating oil required to prepare the compositions of this invention need be initially employed to disperse the aluminum soap and the blend of acids. The remainder of the lubricating oil can be conveniently added subsequent to the addition of the blend of low molecular weight carboxylic acids and mineral acids.
When a portion of the lubricating oil is a saponifiable synthetic oil, it is preferred to initially disperse the reactants in a mineral oil or the non-saponifiable synthetic or] portion of the lubricating oil, and to then add the .saponifiable synthetic oil to the grease batch after the latter has been cooled.
Conventional lubricating grease additives may also be employed in the lubricating compositions of the present invention. These additives, for example, include: oxida .tion inhibitors, such as phenyl alpha naphthylamine, cor
rosion inhibitors such as sorbitan monooleate, tackiness agents such as polyisobutene or high molecular weight polymerized acrylic esters, load-carrying compounds such as sulfurized and/or phosphorous and/or chlorine containing oil-soluble materials, and the like.
The invention will be more fully understood by reference to the following specific examples. illustrating various modifications of the invention.
. 4 EXAMPLE I A lubricating grease composition according to this invention was prepared from the following constituents:
Formulation: Percent weight Glacial acetic acid 14.0 Phosphoric acid conc.) 6.0 Hydrated lime 15.0 Aluminum stearate 3.2 Phenyl alpha naphthylamine 0.5 Mineral lubricating oil 55 SUS 210 F 61.3
Preparation The aluminum stearate was dispersed in all of the mineral lubricating oil by heating to a temperature of about 300 F. with stirring. The resulting dispersion was cooled to room temperature in pans. Just prior to drawing into the pans, the phenyl alpha naphthylamine was added to the dispersion. The cooled dispersion was then charged to a grease kettle, and the lime added with mixing to obtain a smooth uniform slurry. A blend of the acetic acid and the phosphoric acid was then charged to the grease kettle. Without heating the resulting grease batch, the temperature rose to about 190 F. Stirring was continued until the temperature subsided, and the grease was finished by being passed through a Gaulin homogenizer.
, Properties Excellent, smooth uniform grease.
Appearance Droooinz point, F... Penetration 77 F. mirth/10:
Unworked Worked on strokes 210.
Worked 70,000 strokes- 235. Water solu ility Nil.
-. Excellent.
After removal of water, crease becomes somewhat softer but does not lose structure.
Norma Hoffman oxidation test 335.
(hrs. to 5 n. s. 1. drop). Lubrication lite (hours) (250, F. 1000+.
Water renellency 11). Phase changes up to 400-F EXAMPLE II Formulation: Percent weight Glacial acetic acid 14.0 Nitric acid (70% cone.) ....1 -4 8.6 Hydrated lime 15.1 Aluminum stearate 3.1 Phenyl alpha naphthylamine 0.6 Mineral lubricating oil 55 SUS @210 F 58.6
Preparation Similar to thatdescribed in Example I, except that nitric acid was employed in place of the phosphoric acid.
Properties Appearance Excellent. smooth uniform red product.
Pen trations, 77 F., mmJlO:
Unworked 200.
Worked 60 St nkes..
Worked 70,000 strokes Semi-fluid Dro ping p int, F 400+. Water solubility (boilin wato No turbidity afte 10 minutes boiling. Phase changes up to 400 F. Grease softens after removal o water but does not lose structure. Semi {luld on cooling to room temperaure. Norma Hofimau oxidation test 250.
(hrs. to 5 p. s. i. drop). Lubri ation lile (hours) (250 F. 850. 10,000 R. P.
The above data shows that mineral acids other than phosphoric acid can be effectively employed to prepare lubricating grease compositions in combination with low molecular weight carboxylic acids. It will be further noted that when nitric acid is employed, the resulting grease composition had a red color indicating that this strong inorganic acid may have reacted in some manner with the lubricating oil base.
It will be further understood that the present invention is not necessarily limited to the specific materials and conditions of the foregoing examples. These materials and conditions may be varied within the limits indicated in the general portions of the specification.
What is claimed is:
l. A lubricating composition comprising a major amount of a lubricating oil, and an alkaline earth metal neutralized blend of 5 to 20 wt. percent low molecular weight carboxylic acid having from about 1 to 3 carbon atoms per molecule and 3 to 15 wt. percent mineral acid, and 3 to 6 wt. percent aluminum soap, all of said weight percentages being based on the total weight of the lubricating composition.
2. The lubricating composition of claim 1 wherein said lubricating oil is a mineral lubricating oil.
3. The lubricating composition of claim 1 wherein said alkaline earth metal is calcium.
4. The lubricating composition of claim 1 wherein said mineral acid is selected from the group consisting of phosphoric acid, nitric acid, hydrochloric acid, sulfuric acid, and mixtures thereof.
5. The lubricating composition of claim 1 wherein said aluminum soap is an aluminum soap of a high molecular weight carboxylic acid having from about 16 to 22 carbon atoms per molecule.
6. The method of preparing a lubricating grease composition which consists essentially of dispersing an aluminum soap of a high molecular weight carboxylic acid having from about 16 to 22 carbon atoms per molecule in a lubricating oil by heating, cooling said dispersion to ambient temperature, adding an alkaline earth metal hydroxide to said cooled dispersion, then adding a blend of a low molecular weight carboxylic acid having from about 1 to 3 carbon atoms per molecule and a mineral acid to the resulting mixture to obtain said lubricating grease composition.
7. The method of claim 6 wherein said aluminum soap is aluminum stearate.
8. The method of claim 6 wherein said low molecular weight carboxylic acid is acetic acid.
9. The method of claim 6 wherein said mineral acid is nitric acid.
References Cited in the file of this patent UNITED STATES PATENTS 2,417,429 McLennan Mar. 18, 1947

Claims (1)

1. A LUBRICATING COMPOSITION COMPRISING A MAJOR AMOUNT OF A LUBRICATING OIL, AND AN ALKALINE EARTH METAL NEUTRALIZED BLEND OF 5 TO 20 WT. PERCENT LOW MOLECULAR WEIGHT CARBOXYLIC ACID HAVING FROM ABOUT 1 TO 3 CARBON ATOMS PER MOLECULE AND 3 TO 15 WT. PERCENT MINERAL ACID, AND 3 TO 6 WT. PERCENT ALUMINUM SOAP, ALL OF SAID WEIGHT PERCENTAGES BEING BASED ON THE TOTAL WEIGHT OF THE LUBRICATING COMPOSITION.
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DEE13277A DE1052041B (en) 1955-11-30 1956-11-24 Grease and process for its manufacture
FR1165143D FR1165143A (en) 1955-11-30 1956-11-28 Use of mixtures of organic and mineral acids in the preparation of fats

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