US3790479A - Lithium base lubricating grease method - Google Patents

Lithium base lubricating grease method Download PDF

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US3790479A
US3790479A US00100249A US3790479DA US3790479A US 3790479 A US3790479 A US 3790479A US 00100249 A US00100249 A US 00100249A US 3790479D A US3790479D A US 3790479DA US 3790479 A US3790479 A US 3790479A
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grease
temperature
oil
lubricating
lithium
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G Hommer
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Sunoco Inc
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Sun Oil Co
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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
    • C10M7/00—Solid or semi-solid compositions essentially based on lubricating components other than mineral lubricating oils or fatty oils and their use as lubricants; Use as lubricants of single solid or semi-solid substances
    • 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
    • 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
    • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • 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
    • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/102—Aliphatic fractions
    • 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
    • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/104—Aromatic fractions
    • 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
    • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/106—Naphthenic fractions
    • 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125—Carboxylix 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
    • 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/129—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of thirty or more carbon atoms
    • 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
    • C10M2215/02—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
    • 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
    • C10M2215/02—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
    • C10M2215/044—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms having cycloaliphatic groups
    • 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
    • C10M2215/02—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
    • 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
    • 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
    • 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
    • C10N2070/00—Specific manufacturing methods for lubricant compositions

Definitions

  • This invention relates to the preparation of a lubricating grease, the latter being a solid to semi-fluid product of a dispersion of a thickening agent in a liquid lubricant. Other ingredients imparting special properties can be included. More specifically, this invention relates to an improved low temperature method for preparing a lithium base lubricating grease.
  • the low temperature procedure for preparing a lithium base grease generally involves saponifying a sponifiable fatty material, e.g., commercial 12-hydroxystearic acid, with a saponifying agent, e.g., lithium hydroxide.
  • This saponification normally takes place in at least a portion of the lubricating oil, e.g., petroleum lubricating oil, contained in the grease at a temperature lower than the freezing point of the resulting soap-oil mixture.
  • the soap is the lithium-fatty material resulting from the saponification reaction. Thereafter the soap-oil mixture is heated to an elevated temperature which is below the melting point of the soap-oil mixture; during this heating, low boiling saponification by-products and added water evaporate.
  • the soapoil mixture After being heated to this elevated temperature, the soapoil mixture is allowed to cool. Furthermore, during the aforementioned heating and cooling, any additional lubricating oil or cut back oil required to provide a grease of desired grade is added to the saponified mixture.
  • the grease is milled during or after cooling; in other methods, the grease is sheared before cooling. Milling of the grease can be performed by a colloid mill, for example while shearing suitably can be performed by means of a valve properly located in the system and having suflicient pressure drop to obtain the proper consistency of the grease.
  • the present invention provides a low temperature procedure wherein neither shearing nor milling is required to obtain the desired grease properties.
  • the resulting grease despite the lack of shearing or milling, has excellent mechanical stability.
  • a lithium soap thickened grease having the desired properties and, in addition, excellent mechanical stability, is prepared without shearing and/or milling by the improvement defined hereinafter to the low temperature method of preparing said grease.
  • the low temperature method after the saponification mixture of lithium base saponifying agent and a saponifiable hydroxy fatty material is saponified in the presence of at least part of the lubricating oil contained in the finished grease and undesirable low boiling materials have evaporated, the mixture is further heated to an elevated temperature to obtain the desired grease properties; afterwards it is allowed to cool.
  • the balance of any lubricating oil or cut back oil required to provide a grease of the desired grade is added to the mixture.
  • the present improvement involves heating the mixture, during said heating step, to a maximum temperature within a specific narrow temperature range, herein referred to as the top temperature. This range is related to the aniline point of the lubricating oil in the composition being heated to the top temperature, and the relationship is defined in FIG. 11 which is explained under the Description section herein.
  • FIG. I is a graphic presentation of a typical temperature versus time relationship or temperature profile encountered when preparing a batch of lithium soap thickened grease in accordance with this invention. This temperature profile shows how the top temperature range used in this invention relates generally to the preparation of a lithium base grease. This figure is also used to assist in defining shearing and milling.
  • FIG. II relates the necessary top temperature range, referred to generally in FIG. 1, to the aniline point of the lubricating oil present in the composition being heated to within the top temperature range.
  • FIG. I The general method of preparing a lithium soap grease according to this invention can be described using the temperature-time profile shown in FIG. I.
  • Solid lithium hydroxide for example, is added at time-temperature 1 to a suitable container, e.g., a heatable kettle containing a stirring device, and then Water is added 1a; normally, both would be at ambient temperature.
  • a time-temperature point or line in FIG. I is referred to by just a number or a letter.
  • the solution is heated and agitated to insure that the lithium hydroxide dissolves. After the hydroxide dissolves, at least a portion of the lubricating oil to be ultimately incorporated into the grease is added to the kettle containing the aqueous solution 2.
  • the temperature of the mixture in the kettle can be held constant by adding the oil at a rate such that, coupled with the heat input to the kettle, the temperature will remain constant 3. After the constant temperature period 3, heating again increases the temperature 17. On the other hand, if the oil is at a higher temperature or sufficient heat is added to compensate for a lower temperature oil, then the temperature of the mixture continues to increase 4. After the addition of the lubricating oil, the saponifiable hydroxy fatty material, e.g., commercial 12-hydroxystearic acid, is added 7. During the addition of this acid, the temperature of the resulting mixture can be held constant 5 and increased afterword 18, or it can be continuously increased 6. Saponification occurs during time span 8.
  • the saponifiable hydroxy fatty material e.g., commercial 12-hydroxystearic acid
  • the temperature of the saponified mixture can be increased to drive off low boiling saponification by-products 19 and added water.
  • the temperature can be increased to some temperature 20 and maintained at that temperature until said low boiling materials are evaporated and after which the temperature is increased 21.
  • heating is continued until the temperature necessary to obtain the desired grease properties is reached 11.
  • This necessary temperature is the maximum temperature or the highest elevated temperature that the soap-oil composition experiences and which falls within the top temperature range 11.
  • This top temperature range 11 is a narrow range which lies between the melting point and the freezing point 12 of the soap-lubricating oil composition. As shown in FIG. 11 and explained hereinafter, this top temperature range is related to the aniline point of the lubricating oil contained in the soap-lubricating oil composition.
  • the composition can be cooled 13.
  • the composition can be cooled to a certain temperature and maintained at that temperature for a period and then the cooling continued 14.
  • the mixture can be partially cooled after reaching the top temperature range 11, but then reheated to a higher temperature, which is not above the freezing point 12, followed by further cooling 15.
  • the length of time 16 the soap-lubricating oil composition stays Within the top temperature range is not critical. Thus, heating of the kettle can stop as soon as the desired temperature is reached throughout the entire mixture and the length of time at the top temperature can be determined by the natural cooling of the equipment and materials in the kettle. Alternatively, the composition can be maintained at the desired temperature for an extended period.
  • any lubricating oil also referred to as cut back oil
  • any lubricating oil also referred to as cut back oil
  • the cut back oil is added after the evaporation since any oil added during this period can interfere with the evaporation of low boiling saponification by-products and added Water.
  • This cut back oil, or oils can have the same composition as the portion of the oil initially added to the aqueous solution or it can have some other composition or compositions. Also, this cut back oil is carefully added to and carefully stirred into the soap-oil composition after saponification.
  • the resulting grease does not require shearing or milling at any time during its manufacture to obtain the desired grease properties.
  • Shearing refers to subjecting the soap-lubricating oil composition or the mixture of said composition and any or all of the portion of the balance of any required oil to a strong force which slips or slides one part of the mixture relative to an adjacent part, prior to cooling, to obtain a finished lithium base lubricating grease which will afterwards change little in consistency while in use.
  • the invention described in US. Pat. 3,244,628, issued Apr. 5, 1966 to William R. Hencke et al. uses a partly closed valve with a pressure drop of about 10 to 200 pounds per square inch across the valve to obtain said shearing.
  • shearing would occur at any time to the left of the dashed line Z or at any temperature above the dashed line Y, both lines being shown in FIG. I. In other words, shearing would occur on any portion of the temperature-time profile line after saponiftcation except in 4 the area to the right of the dashed line Z and below the dashed line Y.
  • Milling refers to subjecting the cooled mixture of soaplubricating oil composition and the balance of any required lubricating oil to a force to obtain a finished lithium base lubricating grease which will afterwards change little in consistency while in use.
  • US. Pat. 3,242,082, issued Mar. 22, 1966 to Lloyd F. Badgett et al. mentions an apparatus that can be used for this purpose.
  • milling heretofore would occur any time and at any temperature within the area enclosed by dashed lines Z and Y.
  • Consistency refers to the flow characteristic of the grease under pressure.
  • the cone penetration test (ASTM Method D2l7-52T) is a measurement of this characteristic.
  • the aforementioned shearing and milling refers to the intentional application of substantial shear to the dispersion of thickening agent in the lubricating oil to obtain a finished product.
  • the dispersion may be subjected to the unintentional application of an insignificant amount of shear by mixing during saponification, heating, cooling and furthermore, during the transfer of the grease; e.g., pumping of the grease from the kettle to the product containers.
  • the dispersion prepared according to this invention can be subjected to low intensity shear for a very limited duration without modifying the grease structure or adversely altering the mechanical stability.
  • the lithium hydroxide is dissolved in hot water and then at least a portion of the lubricating oil to be ultimately used is added to the hot solution.
  • a satisfactory alternative method is first to place said portion of oil in the empty kettle and subsequently add hot lithium hydroxide solution previously prepared in another container.
  • FIG. II specifically defines the top temperature range shown generally in FIG. I.
  • FIG. II is a graph relating the aniline point of the lubricating oil component of the soaplubricating oil composition at the time the compositions temperature is within the top temperature range necessary to practice this invention.
  • the area enclosed by ABCD represents the operable top temperature range; the area enclosed by EFCD represents a more preferable top temperature range; the area enclosed by EFGH represents the most preferable top temperature range.
  • the operable top temperature range is 371 F. to 395 F.; a preferred top temperature range is 371 F. to 391 F.; the most preferable top temperature range is 382 F. to 391 F.
  • FIG. II are the equations for the lines shown thereon.
  • the omission of shearing or milling when using the top temperature range of present invention does not adversely change the mechanical stability. Even more surprisingly, the contrary occurs; i.e., the mechanical stability of the lithium base lubricating grease prepared by this invention is better than a grease prepared with shearing or milling.
  • Mechanical stability is defined herein as the numerical difference in penetration of the lithium base lubricating grease after rolling, i.e., Standard Method of Test For Roll Stability of Lubricating Grease, ASTM D1831-64, and after 60 strokes, i.e., Standard Method of Test For Cone Penetration of Lubricating Grease, ASTM D217-68. The smaller this numerical difference, everything else being equal, the more desirable the grease.
  • lithium base saponifying agent refers to lithium compounds which saponify fatty materials. Included within this definition are lithium hydroxide, lithium oxide and lithium carbonate. Preferably lithium hydroxide is used in the method defined herein.
  • the saponifying agent is generally added in aqueous mediums.
  • Oils which can be employed for forming the soap-oil composition and the lithium base lubricating grease include the oils normally referred to as lubricating oils.
  • Suitable lubricating oils synthetic or mineral, are those having Saybolat Universal viscosities of about 40-6000 seconds at 100 F.
  • Suitable petroleum lubricating oils can be naphthenic, paraflinic, aromatic, or asphaltic in type or blends of any of these. Preferably the oil is either naphthenic or parafiinic.
  • the aniline point of the petroleum lubricating oil as determined by Standard Test for Aniline Point and Mixed Aniline Point of Petroleum Products and Hydrocarbon Solvents, ASTM D611-64, is about 120 F.-360 F.
  • an oil which is substantially unreactive under the saponification conditions is preferably employed in the forming of the grease, petroleum lubricating oils being particularly suitable for this purpose.
  • Suitable saponifiable fatty materials which can be employed in the production of a lithium base lubricating grease include hydrogenated castor oil, hydrogenated triglycerides of ricinoleic acid, hydrogenated ricinoleic acid, hydroxystearic acids and, in particular 12-hydroxystearic acid, methyl or ethyl esters of hydroxystearic acid and, in particular, the methyl or ethyl ester of l2-hydroxystearic acid. It is preferred that the saponifiable fatty material contains at least 50 weight percent hydroxystearic acid and more preferably at least 75 weight percent 12-hydroxystearic acid.
  • l2-hydroxystearic acid can contain minor amounts of other saturated fatty acids such as arachidic and n-nonadecylic and unsaturated fatty acids such as palmitoleic, petroselinic, petroselaidic, elaidic, vaccenic and gadoleic.
  • the fatty material resulting from a hydrogenated castor oil from which glycerol has been removed also contains minor amounts of other fatty acids.
  • one commercial grade of such a material contains by weight: 86.5% of 12-hydroxystearic acid, 1% oleic acid, 2.5% ricinoleic acid, 2% palmitic acid and 8% stearic acid.
  • the saponifiable fatty materials include the methyl and ethyl esters of hydroxystearic acid and, in particular, the methyl ester of 12-hydroxystearic acid.
  • the rate of reaction between it and the lithium base saponifying agent, e.g., lithium hydroxide is slower than the rate of reaction between, e.g., just l2-hydroxystearic acid and lithium hydroxide.
  • the manufacturing time is greater when using esters than when using hydroxystearic acid.
  • the alcohol coproduct, e.g., methanol, formed during the saponification of the methyl ester is evaporated during the process and unless recovered, is lost.
  • the percentage of lithium soap in the finished grease product depends on the end use requirement. Thus, for example, some textile greases have a soap content as low as 0.25%, while some heavy industrial greases have a soap content as high as 30%.
  • the greases produced in accordance with this invention can contain various additives of the usual type such as corrosion inhibitors, oxidation inhibitors, extreme pressure agents and anti-wear agents. These additives can be added either before or during the cooling process. The additions are preferably performed while the temperature of the grease is between 300 F. and about F., suitably during the cooling step.
  • the desired properties or desired grade of grease refers to the physical arrangement of the component particles of a lubricating grease thickener, additive-if anyand the lubricating oil. It is the nature and stability of this arrangementwhich determines the appearance, texture and chemical and physical properties of the grease. Appearance refers to those characteristics of a grease which are observable by visual inspection only, e.g., bulk appearance, bloom, color and luster. Bulk appearance refers to visual appearance of the grease where the undisturbed surface is viewed in an opaque container. Bloom is the surface color, usually blue or green, of the grease when viewed by reflected daylight at an angle of about 45 from the surface. Color of a grease is the shade and the intensity shown when the grease is viewed under conditions to eliminate bloom. The intensity of light reflected by a grease, its sheen or brilliance refers to the luster of the grease. Texture is that property of the grease which is observed when a small separate portion of it is pressed together and then slowly drawn apart.
  • the first naphthenic oil added in two portions had the following properties: viscosities, SUS @100 F. of 514; SUS @210 F. of 52.4;
  • the third added naphthenic oil had the following properties: viscosities, SUS @100 F. of 5945; SUS @210 F. of 135; API gravity @60 F. of 17.3; pour point of +20 F.; aniline point of 185 F.
  • Table I lists, as an example, the numerous runs performed to obtain the data necessary to locate the top temperature range (shown in FIG. 11) for a soap-lubricating oil composition whose oil had an aniline point of 153 F. Other runs were performed using oils having a wide range of aniline points to obtain the data necessary to develop the relationships shown in FIG. ll.
  • Table I Also shown in Table I are the melting and freezing points of the soap-lubricating oil composition prepared with a lubricating oil having an aniline point of 153 F.
  • the melting point of said soap-oil composition was 392.S F., i.e., several degrees higher than the top temperature used in Runs 3-14, demonstrating that this invention relates to a low temperature method.
  • This melting point is also known as solution temperature, while the freezing point is also known as crystallization temperature. Tests for determining both melting and freezing points are described in US. Pat. 2,652,366, Robert C. Jones et a1., Sept. 15, 1953.
  • Runs 7, 8, 9, 10, 11, and 12 shown in Table 1 indicate that satisfactory greases were prepared, without milling or shearing, at the top temperatures shown.
  • the greases of Runs 7, 8, 9, 10 and 11 had excellent mechanical stability, i.e., the penetration differences between after rolling (ASTM 131831-64) and after 60 strokes (ASTM D217-68) were less than 62. The lower the latter value, the greater the mechanical stability.
  • Run 1 illustrates a melt temperature method of preparing, with milling, a satisfactory grease having a typical mechanical stability.
  • Run 2 compared to Run 1, indicates the need for milling in preparing a satisfactory grease at a melt temperature.
  • Runs 3, 4, 5, and 6 demonstrates that a temperature range exists between the melting point of the soap-oil composition and the top temperature necessary to practice this invention wherein, without milling, the resulting grease has an unsatisfactory structure.
  • the first paraffinic oil used to prepare the greases in Table II had the following properties: viscosities, SUS F. of 508; SUS @210 F. of 64.3; API gravity @60 F. of 30; pour point of 0 F.
  • the second oil used had these properties: SUS @100 F. of 2900; SUS @210 F. of 165; API gravity @60 F. of 27.2.
  • the resulting aniline point of the blended oils was 248 F.
  • Runs 19 and 20, 21 and 22, as reported in the accompanying Table III, demonstrates that milling the greases prepared within the top temperature range of this invention reduces the mechanical stability of the grease.
  • Runs 19-20 were made with a naphthenic oil; Runs 21-22 were made with a parafiinic oil.
  • lithium base lubricating greases containing 6-20 weight percent lithium soap, were prepared using a fatty material containing 30-90 weight percent triglycerides obtained from hydrogenated castor oil with the balance being commercial 12-hydroxystearic acid. The results were analogous to those reported for the runs in which the fatty material was just the commercial 12-hydroxy stearic acid. Thus greases having the desired structure were prepared using the aforementioned triglycerides. Use of other oils, i.e., synthetic and natural, will result in satisfactory greases.
  • the invention claimed is: 1.
  • a saponifiable hydroxy fatty material containing at least weight percent of 12-hydroxystearic acid is saponified with an aqueous lithium base saponifying agent selected from the class consisting of lithium hydroxide, lithium oxide and lithium carbonate, in the presence of at least a portion of the lubricating oil to be contained in the grease product, wherein the resulting saponified mixture is mixed by simple stirring only and is heated to an elevated temperature whereby low boiling saponification by-products and added water are evaporated and the oil and soap become transformed into a grease having high mechanical stability, the improvement which comprises the lubricating oil being a petroleum lubricating oil having a viscosity of 406000 SUS at F. and an aniline point of 360 F. and the top temperature reached during the heating step being within area EFGH of FIG. II, thereafter cooling the mixture and adding any additional oil needed to provide

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  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)
US00100249A 1970-12-21 1970-12-21 Lithium base lubricating grease method Expired - Lifetime US3790479A (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US9990670A 1970-12-21 1970-12-21
US9990570A 1970-12-21 1970-12-21
US10024970A 1970-12-21 1970-12-21

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US3790479A true US3790479A (en) 1974-02-05

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US00100249A Expired - Lifetime US3790479A (en) 1970-12-21 1970-12-21 Lithium base lubricating grease method

Country Status (8)

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US (1) US3790479A (xx)
BE (1) BE776932A (xx)
CA (1) CA965402A (xx)
DE (1) DE2163264A1 (xx)
FR (1) FR2118942B1 (xx)
GB (1) GB1343506A (xx)
IT (1) IT941228B (xx)
NL (1) NL7117601A (xx)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3998745A (en) * 1975-02-12 1976-12-21 Texaco Inc. Method for manufacturing traction motor gear lubricant
US5236607A (en) * 1991-01-15 1993-08-17 Shell Oil Company Preparation of lithium soap thickened greases
EP1327621A1 (en) * 2002-01-12 2003-07-16 Lithchem International Dry powder lithium carboxylates

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
PH18130A (en) * 1980-02-07 1985-03-22 Unilever Nv Process for the manufacture of soap

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3242084A (en) * 1963-05-22 1966-03-22 Texaco Inc Method of grease manufacture
US3242082A (en) * 1963-05-22 1966-03-22 Texaco Inc Method of grease manufacture
US3242086A (en) * 1963-05-22 1966-03-22 Texaco Inc Method of grease manufacture

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3998745A (en) * 1975-02-12 1976-12-21 Texaco Inc. Method for manufacturing traction motor gear lubricant
US5236607A (en) * 1991-01-15 1993-08-17 Shell Oil Company Preparation of lithium soap thickened greases
EP1327621A1 (en) * 2002-01-12 2003-07-16 Lithchem International Dry powder lithium carboxylates

Also Published As

Publication number Publication date
NL7117601A (xx) 1972-06-23
DE2163264A1 (de) 1972-07-13
FR2118942B1 (xx) 1976-02-13
CA965402A (en) 1975-04-01
BE776932A (fr) 1972-06-20
IT941228B (it) 1973-03-01
GB1343506A (en) 1974-01-10
FR2118942A1 (xx) 1972-08-04

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