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US2967151A - Utilization of phosphoric acid in the preparation of greases - Google Patents

Utilization of phosphoric acid in the preparation of greases Download PDF

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Publication number
US2967151A
US2967151A US550173A US55017355A US2967151A US 2967151 A US2967151 A US 2967151A US 550173 A US550173 A US 550173A US 55017355 A US55017355 A US 55017355A US 2967151 A US2967151 A US 2967151A
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Prior art keywords
molecular weight
acid
phosphoric acid
acids
low molecular
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US550173A
Inventor
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 US550173A priority Critical patent/US2967151A/en
Priority to GB35864/56A priority patent/GB793684A/en
Priority to DEE13282A priority patent/DE1040729B/en
Priority to FR1165150D priority patent/FR1165150A/en
Application granted granted Critical
Publication of US2967151A publication Critical patent/US2967151A/en
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    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • 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
    • C10M2215/065—Phenyl-Naphthyl amines
    • 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
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/26—Amines
    • 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
    • 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
    • C10M2219/04—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
    • 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
    • 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
    • C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
    • C10M2223/04—Phosphate esters
    • 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
    • C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • 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
    • 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
    • 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
    • C10M2229/041—Siloxanes with specific structure containing aliphatic substituents
    • 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
    • C10M2229/043—Siloxanes with specific structure containing carbon-to-carbon 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
    • 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
    • C10M2229/044—Siloxanes with specific structure containing silicon-to-hydrogen 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
    • 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
    • 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 high temperature lubricating greases thickened with neutralized products of a blend of low molecular weight carboxylic acids, high molecular weight carboxylic acids and phosphoric acid.
  • the lubricating grease compositions of the invention have outstanding extreme pressure characteristics in addition to other desirable grease characteristics.
  • this invention relates to the utilization of phosphoric acid directly in combination with a low molecular weight carboxylic acid having from about 1 to 3 carbon atoms per molecule and a high molecular weight carboxylic acid having from about 12 to 30 carbon atoms per molecule.
  • These blends of phosphoric acid and organic carboxylic acids are neutralized with metal hydroxides or carbonates to provide the grease thickening agents of this invention.
  • lubricating grease compositions can be prepared by utilizingfrom about 2.5 to wt. percent, preferably from about 2.5 to 6 wt. percent, of phosphoric acid in combination with about 10 to wt. percent of a low molecular weight carboxylic acid such as acetic acid and about 2 to 10 wt. percent of a high molecular weight carboxylic acid such as stearic acid.
  • the lubricating grease compositions of the invention are particularly characterized by high dropping points and outstanding load carrying properties. The greases exhibit these properties regardless of whether. they are prepared in either. the hydrous or anhydrous form.
  • stable lubricating grease compositions are prepared by the use of blends of the low molecular weight carboxylic acids, phosphoric acid and high molecular weight carboxylic acids, wherein the phosphoric acid contributes in some manner to the production of effective lubricating grease compositions.
  • the phosphoric acid may be utilized in concentrations ranging from about 5 to 100%.
  • Suitable low molecular weight carboxylic acids are the saturated and unsaturated aliphatic carboxylic acids having from about 1 to 3 carbon atoms per molecule. Examples of such acids include formic acid, acetic acid, propionic acid, etc. Acetic acid is preferred 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 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 grease compositions made in accordance with this invention. The amount of low molecular weight carboxylic acid employed will be within the range of about 10 to 15 wt. percent, preferably about 10 to 12 wt. percent, based on the total lubricating grease composition.
  • High molecular weight carboxylic acids containing from about 12 to 30, preferably about 18 to 22, carbon atoms per molecule are useful for the purposes of the present 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, palmitic, stearic, monoand poly-hydroxy stearic and arachidic acids as well as hydrogenated fish oil and tallow acids. Unsaturated fatty acids such as oleic, ricinoleic and similar acids may also be used. The amount of high molecular weight fatty acids employed in preparing the lubricating compositions of this invention will be from about 2 to 10 wt. percent, preferably about 2 to 5 wt. percent, based on the total lubricating grease composition.
  • the mol ratio of low to high molecular weightcarboxylic acids will range from about 10:1 to 30:1, preferably about 15:1 to 25:1, and the mol ratio of the average of the low molecular weight acids, i.e. the low molecular weight carboxylic acids and the phosphoric acid, to the high molecular weight carboxylic acids will be from 20:1 to 35:1, preferably about 25:1 to 30:1.
  • the metals suitable for neutralizing the above blend of acids are the alkaline earth metals: calcium, barium, magnesium and strontium.
  • the above metals are generally employed in the form of hydroxides or carbonates, and the process of this invention will utilize from about 8 to 15 wt. percent, based on the total lubricating grease composition, of the metal hydroxide or carbonate. Calcium hydroxide is preferred. Mixtures of the above metals may also be employed, if desired.
  • the lubricating oils employed as the mens-trua of the lubricant 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 220 S.U.S. at 210 F., 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 synthetic lubricating oils include esters of monobasic acids (e.-g.- an ester of C 'Oxo alcohol with C Oxo acid, an ester of C Oxo alcohol with octanoicacid, etc.), esters of dibasic acids (e.g. di-Z-ethyl hexyl sebacate, di-nonyl adipate, etc.), esters of glycols (e.g. C Oxo acid diester of tetraethylene glycol, etc.), complex esters (eg.
  • esters of phosphoric acid cg. 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
  • alkyl' silicates cg. methyl polysiloxanes, ethylpolysiloxanes, methylphenyl polysiloxanes, etc.
  • sulfite esters e.g..the ester. formed by reacting one mole of sulfur oxychloride with two moles of the methyl ether of ethylene glycol, etc.
  • carbonates e.g. the carbonate formed by. reacting C Oxo alcohol with ethyl carbonate to form a half esterand reacting this half ester with tetraethylene glycol
  • mercaptals' e.g. the mercaptal'forined by reacting Z-ethyl hexyl mercaptan with formaldehyde
  • formals e.g. .the
  • the lubricating grease compositions of the invention will contain from about 50 to 90 wt. percent, preferably about 65 to 85 wt. percent, of the mineral and/or synthetic lubricating oil and about 10 to 50 wt. percent, pref-- erably about 15 to wt. percent, of the reaction prodnets of blends or mixtures of the above acids with the metal base.
  • lubricating grease additives may alsobe employed in the lubricating grease compositions of the 1 present invention.
  • Such additives include: oxidation inhibitors such as phenyl alpha naphthylamine, corrosion inhibitors such as sorbitan monooleate, tackiness agents such as polyisobutene or high molecular weight polymerized acrylic esters, and the like.
  • the lubricating grease compositions of this invention may be prepared by coneutralizing the blend or mixture of phosphoric acid, the low molecular weight carboxylic acids and the high molecular weight carboxylic acids with the metal base, e.g. hydrated lime, and dispersing the products in the lubricatingoil. It is not essential that the water of reaction be removed. However, a somewhat greater stability can be achieved when the water of reaction is removed by carrying out the grease preparation at elevated temperatures.
  • the preferred method of preparing the-lubricating grease compositions of this invention involves mixing the metal base and the lubricating oil together at. room temperature to form an intimate slurry.
  • the high molecular weight carboxylic acid is added to the slurry with stirring.
  • a blend of the low molecular weight carboxylic acid and the phosphoric acid' is then added with continued mixing, and a solid grease forms almost instantaneously with the temperature rising to about. 180 to 210 reciprocal seconds.
  • the lubricating grease compositions of this 1 invention' may also be prepared by heating the grease batch to a temperature of about 400 to 550 following of shear within the range of about 100,000 to 500,000"
  • the stearic acid as a powder.
  • the phenyl alpha naphthylamine was added, and the stirring continued for about two-hours untilthe temperature subsided.
  • the grease was homogenized by being passed through a Morehouse mill.
  • the grease of Example II also showed the desired high temperature, stability and load carrying properties of the grease prepared in accordance with the method described in Example I, though the former was prepared at a much higher temperature to effect dehydration.
  • a lubricating grease composition comprising a major proportion of lubricating oil thickened with a grease thickening amount of an alkaline earth metal base neutralized mixture of high molecular weight monocarboxylic acids having about 12-30 carbon atoms per molecule, low molecular weight monocarboxylic acids having from about 1-3 carbon atoms per molecule, and phosphoric acid, the amount of said phosphoric acid being 2.5 to 10.0 wt. percent, wherein the mole ratio of low molecular weight acids to high molecular weight carboxylic acid is about 20:1 to 35:1 and wherein the mole ratio of said low molecular weight carboxylic acid to said high molecular weight carboxylic acid is about 10:1 to 30:1.
  • composition of claim 1 wherein said alkaline earth metal base is a calcium base.
  • composition of claim 1 wherein said lubricating oil is a mineral lubricating oil.
  • a lubricating grease composition comprising a major amount of mineral lubricating oil and about 10 to wt. percent of the alkaline earth metal salts of a C to C fatty acid, a C to C fatty acid and phosphoric acid, the amount of phosphoric acid being about 2.5 to 10.0 wt. percent, wherein the mole ratio of low molecular weight acids to high molecular weight carboxylic acid is about 20:1 to 35:1, and wherein the mole ratio of acetic acid to said C to C fatty acid is about 10:1 to 30:1.
  • the method of preparing a lubricating grease composition which comprises dispersing a metal base in a lubricating oil, adding to the resulting dispersion high molecular weight carboxylic acids having from about 12 to 30 carbon atoms per molecule, then adding a blend of low molecular weight carboxylic acids having about 1 to 3 carbon atoms per molecule and phosphoric acid wherein the mole ratio of low molecular weight carboxylic acid to high molecular weight carboxylic acid is about 10:1 to 30:1 and wherein the mole ratio of said low molecular weight carboxylic acid and said phosphoric acid to said high molecular weight carboxylic acid is about 20:1 to 35:1 and thereafter cooling the resulting grease mixture to obtain said lubricating grease composition, said metal base being present in suflicient amounts to neutralize said acids and the amount of said phosphoric acid being 2.5' to 10.0 wt. percent.

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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

United States Patent UTILIZATION OF PHOSPHORIC ACID IN THE PREPARATION OF GREASES Arnold J. Morway, Clark, N.J., assignor to Esso Research and Engineering Company, a corporation of Delaware No Drawing. Filed Nov. 30, 1955, Ser. No. 550,173
7 Claims. (Cl. 25240.7)
This invention relates to lubricating grease compositions, and more particularly to high temperature lubricating greases thickened with neutralized products of a blend of low molecular weight carboxylic acids, high molecular weight carboxylic acids and phosphoric acid. The lubricating grease compositions of the invention have outstanding extreme pressure characteristics in addition to other desirable grease characteristics.
In brief, this invention relates to the utilization of phosphoric acid directly in combination with a low molecular weight carboxylic acid having from about 1 to 3 carbon atoms per molecule and a high molecular weight carboxylic acid having from about 12 to 30 carbon atoms per molecule. These blends of phosphoric acid and organic carboxylic acids are neutralized with metal hydroxides or carbonates to provide the grease thickening agents of this invention.
The use of small amounts of a metal salt of phosphoric acid in lubricating grease compositions has been suggested in the prior art. In US. 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 thickened with a large amount of calcium soap. The use of more than about 2.0% by weight of phosphoric acid is taught to be definitely detrimental, and higher amounts to be positively destructive.
.It has now been found that excellent lubricating grease compositions can be prepared by utilizingfrom about 2.5 to wt. percent, preferably from about 2.5 to 6 wt. percent, of phosphoric acid in combination with about 10 to wt. percent of a low molecular weight carboxylic acid such as acetic acid and about 2 to 10 wt. percent of a high molecular weight carboxylic acid such as stearic acid. As previously stated, the lubricating grease compositions of the invention are particularly characterized by high dropping points and outstanding load carrying properties. The greases exhibit these properties regardless of whether. they are prepared in either. the hydrous or anhydrous form. j
It is notknown exactly whatfreactions the phosphoric acid enters into during the preparation of the greases of this invention. However, for the present purposes it is sufiicient to note that stable lubricating grease compositions are prepared by the use of blends of the low molecular weight carboxylic acids, phosphoric acid and high molecular weight carboxylic acids, wherein the phosphoric acid contributes in some manner to the production of effective lubricating grease compositions. The phosphoric acid may be utilized in concentrations ranging from about 5 to 100%.
Suitable low molecular weight carboxylic acids are the saturated and unsaturated aliphatic carboxylic acids having from about 1 to 3 carbon atoms per molecule. Examples of such acids include formic acid, acetic acid, propionic acid, etc. Acetic acid is preferred 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 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 grease compositions made in accordance with this invention. The amount of low molecular weight carboxylic acid employed will be within the range of about 10 to 15 wt. percent, preferably about 10 to 12 wt. percent, based on the total lubricating grease composition.
High molecular weight carboxylic acids containing from about 12 to 30, preferably about 18 to 22, carbon atoms per molecule are useful for the purposes of the present 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, palmitic, stearic, monoand poly-hydroxy stearic and arachidic acids as well as hydrogenated fish oil and tallow acids. Unsaturated fatty acids such as oleic, ricinoleic and similar acids may also be used. The amount of high molecular weight fatty acids employed in preparing the lubricating compositions of this invention will be from about 2 to 10 wt. percent, preferably about 2 to 5 wt. percent, based on the total lubricating grease composition.
In general, the mol ratio of low to high molecular weightcarboxylic acids will range from about 10:1 to 30:1, preferably about 15:1 to 25:1, and the mol ratio of the average of the low molecular weight acids, i.e. the low molecular weight carboxylic acids and the phosphoric acid, to the high molecular weight carboxylic acids will be from 20:1 to 35:1, preferably about 25:1 to 30:1.
The metals suitable for neutralizing the above blend of acids are the alkaline earth metals: calcium, barium, magnesium and strontium. The above metals are generally employed in the form of hydroxides or carbonates, and the process of this invention will utilize from about 8 to 15 wt. percent, based on the total lubricating grease composition, of the metal hydroxide or carbonate. Calcium hydroxide is preferred. Mixtures of the above metals may also be employed, if desired.
The lubricating oils employed as the mens-trua of the lubricant 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 220 S.U.S. at 210 F., 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 synthetic lubricating oils include esters of monobasic acids (e.-g.- an ester of C 'Oxo alcohol with C Oxo acid, an ester of C Oxo alcohol with octanoicacid, etc.), esters of dibasic acids (e.g. di-Z-ethyl hexyl sebacate, di-nonyl adipate, etc.), esters of glycols (e.g. C Oxo acid diester of tetraethylene glycol, etc.), complex esters (eg. the complex ester formed by reacting one mole of tetraethylene glycol with two moles of sebacic acid and two moles of 2-ethyl-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, etc.), esters of phosphoric acid (cg. 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 chlorotrifiuoroethylenecontaining twelve recurring units of chlorotrifluoroethylene),. alkyl' silicates (cg. methyl polysiloxanes, ethylpolysiloxanes, methylphenyl polysiloxanes, etc.), sulfite esters (e.g..the ester. formed by reacting one mole of sulfur oxychloride with two moles of the methyl ether of ethylene glycol, etc.), carbonates (e.g. the carbonate formed by. reacting C Oxo alcohol with ethyl carbonate to form a half esterand reacting this half ester with tetraethylene glycol),
mercaptals'(e.g. the mercaptal'forined by reacting Z-ethyl hexyl mercaptan with formaldehyde), formals (e.g. .the
formal formed by reacting C Oxo alcohol with'formaldehyde), polyglycol type synthetic oils (e.g. thecompounds formed by condensing butyl alcohol, with fourteen units of propylene oxide, etc.), or mixtures of the above in any proportions.
The lubricating grease compositions of the invention will contain from about 50 to 90 wt. percent, preferably about 65 to 85 wt. percent, of the mineral and/or synthetic lubricating oil and about 10 to 50 wt. percent, pref-- erably about 15 to wt. percent, of the reaction prodnets of blends or mixtures of the above acids with the metal base.
Conventional lubricating grease additives may alsobe employed in the lubricating grease compositions of the 1 present invention. Such additives, for example, include: oxidation inhibitors such as phenyl alpha naphthylamine, corrosion inhibitors such as sorbitan monooleate, tackiness agents such as polyisobutene or high molecular weight polymerized acrylic esters, and the like.
In general, the lubricating grease compositions of this invention may be prepared by coneutralizing the blend or mixture of phosphoric acid, the low molecular weight carboxylic acids and the high molecular weight carboxylic acids with the metal base, e.g. hydrated lime, and dispersing the products in the lubricatingoil. It is not essential that the water of reaction be removed. However, a somewhat greater stability can be achieved when the water of reaction is removed by carrying out the grease preparation at elevated temperatures.
The preferred method of preparing the-lubricating grease compositions of this invention involves mixing the metal base and the lubricating oil together at. room temperature to form an intimate slurry. The high molecular weight carboxylic acid is added to the slurry with stirring. A blend of the low molecular weight carboxylic acid and the phosphoric acid'is then added with continued mixing, and a solid grease forms almost instantaneously with the temperature rising to about. 180 to 210 reciprocal seconds.
If desired, the lubricating grease compositions of this 1 invention'may also be prepared by heating the grease batch to a temperature of about 400 to 550 following of shear within the range of about 100,000 to 500,000"
the addition of the blend of low molecular weight car-' boxylic acid and phosphoric acid.. The heated grease batch is then cooled to a temperature of about to F. with stirring and the conventional grease additives charged. This lubricating grease composition may also be finished by homogenization.
The invention will be more fully understood by reference to the following specific examples illustrating various modifications of the invention.
EXAMPLE I A lubricating grease composition according to this invention was prepared from the following constituents:
Formulation Percent Weight Glacial'acetic acid 12. Ste ric acid I 3. Phosphoric acid (85% cone.) 3. Hydrated li a 10. Phenyl alpha naphthylaminej'n' 0. Mineral libricating oil, 55 SUS @,210v F 70. M01 ratio of acetic acid'to stearic-acid 20: M01 ratio of low mol. wt. acids (i.e
phoric acid) to stcaric acid 22. 8:
Preparation The hydratedlime andthe mineral lubricating oil were mixed together at room temperature (about 70 F.) .to
form an intimate slurry. The stearic acid as a powder.
was added to the lime slurry A blend of the acetic and phosphoric acid. was thenadded, A solid grease formed.
immediately with the temperature rising to about F.-
The phenyl alpha naphthylamine was added, and the stirring continued for about two-hours untilthe temperature subsided. The grease was homogenized by being passed through a Morehouse mill.
The above data show that the lubricating grease.1com-..
positions encompassed by this invention have very'desirable high" temperature stability and extreme pressure characteristics.
EXAMPLE 1t Formulation Percent Weight Glacial acetic acid 12. 0 Stearic acid 3.0 Phosphoric acid (85% cone.) 3.0 Hvdratcd lim 11. 6 Phony] alpha naphthylaminm; 0.5 Mineral l'lbricating oil, 55 SUS 210 F 69.9 Mol ratio of accti: acid to stcaric acid..- 20:1 Mol ratio of low mol. wt. acids (in. acetic acid plus phosphoric acid) to stearic acid 22:8:1
Preparation Similar to that" described in Example I, except that following the'addition of the blend of acetic acid and phosphoric acid the grease mixture was heated ito a temperature'of about 500 F. The resulting 1greasejcomposition then cooled to, about200"F."withstirring, and
H HQUNEOOCO the phenyl alpha naphthylamine added. The grease was then Gaulin homogenized at 6500 p.s.i.
Properties Appearance Excellent, uniform product. Dropping point, F. 500+. Penetration, 77 F. mm./10':
Unworked 210. Worked 60 strokes 230. Worked 230,000 strokes 300 (118 F.). Cooled to 77 F. reworked 60 strokes 330. Phase change up to 450 F. None. E. P. properties, Timken test (50 lbs.
load) Pass, narrow scar. Norma Hoffman oxidation test (hrs.
to 5 psi. drop) 420. Lubrication life, hrs. (250 F.-
10,000 r.p.m.) 1200+.
1 N failure-test discontinued.
The grease of Example II also showed the desired high temperature, stability and load carrying properties of the grease prepared in accordance with the method described in Example I, though the former was prepared at a much higher temperature to effect dehydration.
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:
1. A lubricating grease composition comprising a major proportion of lubricating oil thickened with a grease thickening amount of an alkaline earth metal base neutralized mixture of high molecular weight monocarboxylic acids having about 12-30 carbon atoms per molecule, low molecular weight monocarboxylic acids having from about 1-3 carbon atoms per molecule, and phosphoric acid, the amount of said phosphoric acid being 2.5 to 10.0 wt. percent, wherein the mole ratio of low molecular weight acids to high molecular weight carboxylic acid is about 20:1 to 35:1 and wherein the mole ratio of said low molecular weight carboxylic acid to said high molecular weight carboxylic acid is about 10:1 to 30:1.
2. The composition of claim 1 wherein said alkaline earth metal base is a calcium base.
3. The composition of claim 1 wherein said lubricating oil is a mineral lubricating oil.
4. A lubricating grease composition comprising a major amount of mineral lubricating oil and about 10 to wt. percent of the alkaline earth metal salts of a C to C fatty acid, a C to C fatty acid and phosphoric acid, the amount of phosphoric acid being about 2.5 to 10.0 wt. percent, wherein the mole ratio of low molecular weight acids to high molecular weight carboxylic acid is about 20:1 to 35:1, and wherein the mole ratio of acetic acid to said C to C fatty acid is about 10:1 to 30:1.
5. A grease composition according to claim 4, wherein said alkaline earth metal is calcium and said C to C fatty acid is acetic acid.
6. The method of preparing a lubricating grease composition which comprises dispersing a metal base in a lubricating oil, adding to the resulting dispersion high molecular weight carboxylic acids having from about 12 to 30 carbon atoms per molecule, then adding a blend of low molecular weight carboxylic acids having about 1 to 3 carbon atoms per molecule and phosphoric acid wherein the mole ratio of low molecular weight carboxylic acid to high molecular weight carboxylic acid is about 10:1 to 30:1 and wherein the mole ratio of said low molecular weight carboxylic acid and said phosphoric acid to said high molecular weight carboxylic acid is about 20:1 to 35:1 and thereafter cooling the resulting grease mixture to obtain said lubricating grease composition, said metal base being present in suflicient amounts to neutralize said acids and the amount of said phosphoric acid being 2.5' to 10.0 wt. percent.
7. The method of claim 6 wherein said grease mixture is heated to a temperature of about 400 to 550 F. subsequent to the addition of the blend of low molecular weight carboxylic acid and phosphoric acid.
References Cited in the file of this patent UNITED STATES PATENTS 2,417,430 McLennan Mar. 18, 1947 2,417,431 McLennan Mar. 18, 1947 2,417,433 McLennan Mar. 18, 1947 2,513,680 Schott et a1. July 4, 1950 2,846,392 Morway et al. Aug. 5, 1958

Claims (1)

1. A LUBRICATING GREASE COMPOSITION COMPRISING A MAJOR PROPORTION OF LUBRICTING OIL THICKENED WITH A GREASE THICKNENING AMOUNT OF AN ALKALINE EARTH METAL BASE NEUTRALIZED MIXTURE OF HIGH MOLECULAR WEIGHT MONOCARBOXYLIC ACIDS HAVING ABOUT 12-30 CARBON ATOMS PER MOLECULE, LOW MOLECULAR WEIHT MONOCARBOXYLIC ACIDS HAVING FROM ABOUT 1-3 CARBON TOMS PER MOLECULE, AND PHOSPHORIC ACID, THE AMOUNT OF SAID PHOSPHORIC ACID BEING 2.5 TO 10.0 WT. PERCENT, WHEREIN THE MOLE RATIO OF LOW MOLECULAR WEIGHT ACIDS TO HIGH MOLECULAR WEIGHT CARBOXYLIC ACID IS ABOUT 20:1 TO 35:1 AND WHEREIN THE MOLE RATIO OF SAID LOW MOLECULAR WEIGHT CRBOXYLIC ACID TO SAID HIGH MOLECULR WEIGHT CARBOXYLIC ACID TO 10:1 TO 30:1.
US550173A 1955-11-30 1955-11-30 Utilization of phosphoric acid in the preparation of greases Expired - Lifetime US2967151A (en)

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US550173A US2967151A (en) 1955-11-30 1955-11-30 Utilization of phosphoric acid in the preparation of greases
GB35864/56A GB793684A (en) 1955-11-30 1956-11-23 Improved lubricating grease compositions
DEE13282A DE1040729B (en) 1955-11-30 1956-11-27 Grease and process for its manufacture
FR1165150D FR1165150A (en) 1955-11-30 1956-11-29 Lubricating grease

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US3196109A (en) * 1962-03-01 1965-07-20 Exxon Research Engineering Co Lubricating grease containing boron nitride
US3318807A (en) * 1963-05-13 1967-05-09 Texaco Inc Lubricating greases containing finely divided inorganic metal salts and method of preparation therefor
US3344065A (en) * 1965-01-25 1967-09-26 Molykote Produktions G M B H Extreme pressure lubricants
US3389085A (en) * 1964-03-31 1968-06-18 Exxon Research Engineering Co Lubricants containing mixed metal salts of mono- and polybasic acids
US4107058A (en) * 1977-08-19 1978-08-15 Exxon Research & Engineering Co. Pressure grease composition
EP0296362A2 (en) * 1987-05-22 1988-12-28 Amoco Corporation Lubricating grease, process for its preparation and its use
US5126062A (en) * 1991-01-15 1992-06-30 Nch Corporation Calcium sulfonate grease and method of manufacture
US6251840B1 (en) * 1995-09-12 2001-06-26 The Lubrizol Corporation Lubrication fluids for reduced air entrainment and improved gear protection
WO2012076025A1 (en) * 2010-12-06 2012-06-14 Aktiebolaget Skf Polymer thickened grease compositions and their use
US9273265B2 (en) 2011-10-31 2016-03-01 Nch Corporation Calcium carbonate based sulfonate grease compositions and method of manufacture
US9458406B2 (en) 2011-10-31 2016-10-04 Nch Corporation Calcium hydroxyapatite based sulfonate grease compositions and method of manufacture
US9976102B2 (en) 2011-10-31 2018-05-22 Nch Corporation Composition and method of manufacturing calcium sulfonate greases using alkali metal hydroxide and delayed addition of non-aqueous converting agents
US9976101B2 (en) 2011-10-31 2018-05-22 Nch Corporation Method of manufacturing calcium sulfonate greases using delayed addition of non-aqueous converting agents
US10087388B2 (en) 2016-05-18 2018-10-02 Nch Corporation Composition and method of manufacturing calcium sulfonate and calcium magnesium sulfonate greases using a delay after addition of facilitating acid
US10087387B2 (en) 2016-05-18 2018-10-02 Nch Corporation Composition and method of manufacturing calcium magnesium sulfonate greases
US10087391B2 (en) 2016-05-18 2018-10-02 Nch Corporation Composition and method of manufacturing calcium magnesium sulfonate greases without a conventional non-aqueous converting agent
US10392577B2 (en) 2016-05-18 2019-08-27 Nch Corporation Composition and method of manufacturing overbased sulfonate modified lithium carboxylate grease
US10519393B2 (en) 2016-05-18 2019-12-31 Nch Corporation Composition and method of manufacturing calcium magnesium sulfonate greases
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US12146114B2 (en) 2023-04-17 2024-11-19 Nch Corporation Composition and method of manufacturing and using extremely rheopectic sulfonate-based greases

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US2417433A (en) * 1945-04-23 1947-03-18 Union Oil Co Lubricating composition
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Publication number Priority date Publication date Assignee Title
US3196109A (en) * 1962-03-01 1965-07-20 Exxon Research Engineering Co Lubricating grease containing boron nitride
US3318807A (en) * 1963-05-13 1967-05-09 Texaco Inc Lubricating greases containing finely divided inorganic metal salts and method of preparation therefor
US3389085A (en) * 1964-03-31 1968-06-18 Exxon Research Engineering Co Lubricants containing mixed metal salts of mono- and polybasic acids
US3344065A (en) * 1965-01-25 1967-09-26 Molykote Produktions G M B H Extreme pressure lubricants
US4107058A (en) * 1977-08-19 1978-08-15 Exxon Research & Engineering Co. Pressure grease composition
EP0296362A2 (en) * 1987-05-22 1988-12-28 Amoco Corporation Lubricating grease, process for its preparation and its use
EP0296362A3 (en) * 1987-05-22 1989-02-08 Amoco Corporation Lubricating grease, process for its preparation and its use
US5126062A (en) * 1991-01-15 1992-06-30 Nch Corporation Calcium sulfonate grease and method of manufacture
US6251840B1 (en) * 1995-09-12 2001-06-26 The Lubrizol Corporation Lubrication fluids for reduced air entrainment and improved gear protection
WO2012076025A1 (en) * 2010-12-06 2012-06-14 Aktiebolaget Skf Polymer thickened grease compositions and their use
US20140011718A1 (en) * 2010-12-06 2014-01-09 Dick Meijer Polymer thickened grease compositions and their use
US9458406B2 (en) 2011-10-31 2016-10-04 Nch Corporation Calcium hydroxyapatite based sulfonate grease compositions and method of manufacture
US11072756B2 (en) 2011-10-31 2021-07-27 Nch Corporation Calcium hydroxyapatite based calcium sulfonate grease compositions and method of manufacture
US9976102B2 (en) 2011-10-31 2018-05-22 Nch Corporation Composition and method of manufacturing calcium sulfonate greases using alkali metal hydroxide and delayed addition of non-aqueous converting agents
US9976101B2 (en) 2011-10-31 2018-05-22 Nch Corporation Method of manufacturing calcium sulfonate greases using delayed addition of non-aqueous converting agents
US9273265B2 (en) 2011-10-31 2016-03-01 Nch Corporation Calcium carbonate based sulfonate grease compositions and method of manufacture
US10316266B2 (en) 2011-10-31 2019-06-11 Nch Corporation Calcium hydroxyapatite based calcium sulfonate grease compositions and method of manufacture
US10087391B2 (en) 2016-05-18 2018-10-02 Nch Corporation Composition and method of manufacturing calcium magnesium sulfonate greases without a conventional non-aqueous converting agent
US10087387B2 (en) 2016-05-18 2018-10-02 Nch Corporation Composition and method of manufacturing calcium magnesium sulfonate greases
US10392577B2 (en) 2016-05-18 2019-08-27 Nch Corporation Composition and method of manufacturing overbased sulfonate modified lithium carboxylate grease
US10519393B2 (en) 2016-05-18 2019-12-31 Nch Corporation Composition and method of manufacturing calcium magnesium sulfonate greases
US10087388B2 (en) 2016-05-18 2018-10-02 Nch Corporation Composition and method of manufacturing calcium sulfonate and calcium magnesium sulfonate greases using a delay after addition of facilitating acid
US11168277B2 (en) 2016-05-18 2021-11-09 Nch Corporation Composition and method of manufacturing calcium magnesium sulfonate greases
US12031100B2 (en) 2016-05-18 2024-07-09 Nch Corporation Composition and method of manufacturing calcium magnesium sulfonate greases
US11661563B2 (en) 2020-02-11 2023-05-30 Nch Corporation Composition and method of manufacturing and using extremely rheopectic sulfonate-based greases
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GB793684A (en) 1958-04-23
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