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  • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
  • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
  • C10M169/06—Mixtures of thickeners and additives
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  • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
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  • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
  • C10M2201/08—Inorganic acids or salts thereof
  • C10M2201/082—Inorganic acids or salts thereof containing nitrogen
  • C10M2201/083—Inorganic acids or salts thereof containing nitrogen nitrites
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  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/10—Carboxylix acids; Neutral salts thereof
  • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
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  • C10M2207/10—Carboxylix acids; Neutral salts thereof
  • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
  • C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
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  • C10M2207/00—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
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  • C10M2207/10—Carboxylix acids; Neutral salts thereof
  • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
  • C10M2207/125—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
  • C10M2207/128—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 containing hydroxy groups; Ethers thereof
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  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/10—Carboxylix acids; Neutral salts thereof
  • 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
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  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
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  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/28—Esters
  • C10M2207/282—Esters of (cyclo)aliphatic oolycarboxylic acids
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  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
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  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
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  • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
  • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
  • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
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  • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
  • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
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  • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
  • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
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  • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
  • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
  • C10M2209/107—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of two or more specified different alkylene oxides covered by groups C10M2209/104 - C10M2209/106
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  • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
  • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
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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
  • C10M2215/04—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
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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
  • C10M2215/042—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms containing hydroxy groups; Alkoxylated derivatives thereof
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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
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  • 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
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  • C10M2215/26—Amines
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  • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
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  • C10M2219/06—Thio-acids; Thiocyanates; Derivatives thereof
  • C10M2219/062—Thio-acids; Thiocyanates; Derivatives thereof having carbon-to-sulfur double bonds
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Definitions

• Another object of this invention is to provide alkali metal soap-thickened greases which are substantially more recalcitrant to the attack by water than are comparable greases of the prior art.
• Typical alcohols, diols and polyols include methanol, n-butanol, n-octanol, ethylene glycol, propylene glycol, glycerol and sorbital, among others.
• the average molecular weights as measured by the ebullioscopic method or calculated from viscosity measurements or acetyl values are between about 300 to about 15,000.
• the favored copolymers usually contain from about 50 to 75 parts by weight of propoxy groups, and from about 25 to 50 parts by weight of ethoxy groups and have an average molecular weight of from about 1500 to about 10,000.
• One of the preferred copolymers is sold by Retzloif Chemical Company of Houston, Tex., as DPG-lS. It contains about 75 to parts by weight of propoxy groups and from about 25 to 10 parts by weight of ethoxy groups.
• novel copolymer additives are employed in an amount effective to substantially increase the resistance of the alkali metal soap-thickened grease to the attack by water. This amount will vary according to the additive employed, the degree of protection sought, the alkali metal soap contained in the grease, etc.
• lithium soaps are used to thicken a mineral oil base and the preferred copolymers are derived from alkoxylation of di-, tri-, or polyhydroxylated compounds, from about 0.1 part by weight to 5.0 parts by weight of copolymer per hundred parts by weight of the finished grease represents the extremes of the polymer content.
• a more useful range of about'0.l to 0.6 part by weight of copolymer produces greases which have good properties and consistently pass the water-resistance tests, and for this reason are preferred.
• Alcohols as used herein not only refer to aliphatic compounds containing at least one free-hydroxyl group but which as1 can be seen from supra also includes diols, trials and p0 yols. i 2 While the polymeric compositions noted above are not novel per se, their utilization in small quantities (i.e., from 0.1 to 5.0% by weight of the total grease composition) as additives in grease to effect a substantial increase in the re sisting of the greases to water is believed to be novel.
• alkoxylated adducts of alkylated phenols The second class of additives employed to provide improved water-resistance to alkali metal, particularly lithium, soap-thickened greases comprises alkylene oxide adducts of alkylated phenols.
• the favored alkylene oxides are ethylene oxide, propylene oxide and their mixtures.
• a favored group within the class are alkylated phenols wherein the alkyl group contains 5 to 15 carbon atoms, which have from 2 to 50 alkoxylate groups attached to the molecule.
• the preferred additives within this class are ethoxylated phenols whose alkyl groups contain 6 to 10 carbon atoms and an average of 5 to ethoxylate groups per molecule.
• Two of the preferred ethoxylated alkylated phenols are commercially available. One of these is a nonyl phenol ethoxylated with an average of 9.5 moles of ethylene oxide per mole of nonyl phenol.
• the second phenolic adduct which is preferred is supplied by the Retzloif Company of Houston, Tex., and is designated as DRE-203.
• the third class of additives which impart substantially improved water-resistance to greases refers to products formed by initially adding an alkylene oxide such as ethylene or propylene oxide to an alkylene diamine such as ethylene diamine (H NCH CH H N) to give the symmetrical tetrapropoxylated derivative followed by subsequent oxyethylation to a structure shown below:
• x an integer ranging from 6 to 16.
• the lubricating oils employed as the base fluids in this invention of prime interest are the natural (mineral) oils, or mixtures of one or more of these oils.
• the mineral oils which can be used are those of paraflinic, naphthenic, asphaltic or parafiinic-asphaltic type derived from crude oils by refining processes including distillation, cracking and/or polymerization. These oils will have a gravity (API) of about 10 to 35, a viscosity within the range of 100 to 2000 SUS at 100 F. and flash points within the range of about 275 F. to 650 F. Generally a viscosity of from about 700 to 1400 SUS at 100 F. is favored.
• the lubricating base oils preferred for the grease formulations are mineral oils of the paraflinic type having SUS viscosities at 210 F. in the range of about 75 to 95 and flash points in the range of about 450 F. to 600 F.
• the above oils are preferred as bases for greases because they consistently produce greases having the desired enhanced resistance to water.
• These adjuvants can be of diverse structure or origin and are typified by the following: extreme pressure (E.P.) agents such as the metallic naphthenates and sulfurized sperm oil, fillers such as the metal oxides, oxidation inhibitors including phenyl-beta-naphthylamine and the diphenyl amines, corrosion inhibitors including alkali metal nitrites, and stabilizers such as the fatty acid esters.
• E.P. extreme pressure
• these optional adjuvants are employed they are used in minor amounts, seldom totaling more than 10 percent by weight of the finished grease. More usually these adjuvants comprise from about 0.5 to 7.0 parts by weight per hundred parts by weight of finished grease. Ordinarily, these adjuvants are added at the expense of the oil base, most often during the cooling step that takes place during the finishing of greases.
• the soap-thickeners of prime interest in the formulation of the water-resistance greases of this invention include lithium soaps and, to a lesser extent, calcium and lithium soap mixtures.
• the additives are particularly use ful in lithium based greases because they require the addition of water-resistant additives for superior waterresistance and because they presently are of the greatest commercial importance.
• soaps formed in situ the alkali metal soaps being formed by saponifying at least one suitable saponifiable material with an alkaline form of the metal.
• saponifiable materials refers to fatty acids and hydroxysubstituted fatty acids, especially those containing from about 12 to 32 carbon atoms per molecule. Also included are glycerides or hydroxylated glycerides. Suitable saponifiable materials include the following illustrative materials: methyl-lZ-hydroxystearate, 12-hydroxystearic acid, stearic acid, hydrogenated castor oil, myristic acid and the like.
• the preferred saponifiable materials in the order of preference are the esters of 12-hydroxystearic acid, 12- hydroxystearic acid, and stearic acid and/or their mixtures.
• the saponifiable material comprises 30 to 50 parts by weight of methyl 12- hydroxystearate and 70-50 parts by weight of 12-hydroxystearic acid.
• the additive imparting water-resistance is added to a preformed alkali metal soap-thick ened grease such as is typified by a mineral oil based grease already containing a lithium soap of 12-hydroxystearic acid.
• the preformed grease containing some or none of the optional additives, such as extreme pressure additives is heated to about 200 to 400 F. to bring it to a fluid state.
• the preformed grease (as illustrated by lithium soapthickened grease) is continuously stirred.
• the grease is then cooled to about to 240 F., preferably from about 180 F. to 200 F.
• the additive imparting water-resistance is added along with any other compatible additives. The charge is held for about 30 minutes at this temperature range and then brought to the desired consistency by milling.
• a second favored procedure comprises forming the grease in situ.
• an aqueous solution of the alkaline lithium compound, the saponifiable (fatty) material, and part of the mineral oil is charge to a kettle equipped with heating, cooling and stirring means.
• the batch is heated to between about 180 and 225 F. and held at this range for about to 2 hours, then heated to between 250 F. and 350 F. with stirring to dehydrate the grease while slowly adding the remaining oil.
• the grease mixture is cooled to about 180 to 220 F. while stirring and at least one waterresistant additive, as well as optional additives, are added until a homogeneous mixture is obtained.
• a sample is taken for testing and milled to the desired consistency using a colloid mill.
• the lithium and mixed calcium-lithium soap-thickened greases having the following components in the proportions indicated are given below.
• EXAMPLE 1 Preparation of a lithium soap-thickened grease having enhance water-resistance
• a grease kettle equipped with heating, cooling and stirring means is charged with 5.5 parts by weight of a 9.5 percent by wt. aqueous solution of lithium hydroxide, 6.2 parts by weight'of the methyl ester of 12-hydroxystearic acid and 76.70 parts by weight of mineral oil base A.
• the batch is heated to F. with stirring, held at this temperature for 1 hour, then heated with continued stirring at 325 to dehydrate the grease.
• Mineral 011 base A has the following properties ARI gravity 18.1 Viscosity SUS at 100 F. 100 Viscosity SUS at 210 F. 210 Flash point (COC) F.-- 505 41.47 parts by weight of mineral oil base B is added to the stirred mixture at the rate of 0.5 part by weight per minute. When the oil addition is completed the stirred batch is cooled to 195 F. at the rate of 1 F.
• EXAMPLES 3-12 Effect of varying the concentration of the copolymer of Example 1
• the purpose of these examples is to determine the minimum eifective quantity of copolymer in lithium soapthickened, preformed grease. In all instances the copolymer was added to the stirred preformed grease at 190 F.-200 F.
• the concentrations studied varied from 0.1 part by weight to 1.0 part by weight. As the data of Table II indicate the minimum effective quantity is 0.10 part by weight with the upper limit being primary limited by economics.
• Mineral oil base B has the following properties:
• the copolymer has the following properties: Physical state at 77 F Liquid pH, 5% solution in 3: 1 H2O/IPA 6.8 Pounds per gallon at 77 F. 8.5 Flash point, F. (TOC) Viscosity, cps.
• EXAMPLE 14 Preparation of another water-resistant grease using alkoxylated adducts of alkylated phenols to impart water resistance
• a lithium soap-thickened grease was prepared using the process and mineral oils disclosed in Example 1.
• the product contained 2.0% by weight of the oxyethylene adduct of nonylphenol containing an average of 9.5 moles of ethylene oxide in the molecule.
• Table III show, a grease with good general pro erties and water-resistance is obtained.
• Example 13 Example 14
• Example 15 Water resistance additive, wt.
• EXAMPLE 16 Preparation of a preferred water resistant lithium-calcium thickened grease using the additive of Example 1
• the preformed grease process disclosed in Examples 3-12, 14 and 15 is employed but a difierent base grease is used.
• a mixture of lithium and calcium-l2-hydroxystearate soaps is used to thicken the oil base and 0.5 part by weight of the copolymer additive utilized in Example 1 is employed.
• the composition after formulation is shown below.
• novel additives of this invention are known as compositions of matter and have been employed as one of the major components of lubricating oils, insofar as is known they have not been used as additives in minor concentrations in lithium soap and/or lithiuml-calcium thickened lubricants.
• the polymeric alkoxylated polyol derivatives are advocated as lubricants in hydraulic fluids. When used for this purpose they have been used in much higher concentrations (col. 2 line 9) ranging from 1 to 30 percent.
• the inventive additives need be present in only minor proportions. Therefore, it was quite unexpected to find that for the purpose of this invention, the additive functioned well at much lower concentration levels. This discovery was empirically derived and could not have been predicted.
• the subject invention is relatively flexible insofar as several preparative processes can be employed, the mineral base oil employed and the ancillary additives are concerned.
• the metes and bounds of this invention are best ascertained by an examination of the claims which follow, read in conjunction with the preceding specification.
• a lithium soap or a lithium soap-calcium soap thickened mineral oil based grease having improved resistance to water comprising the following admixture of components in the following proportions:
• each 100 parts by weight of grease contains from about 0.5 to 7.0 parts by weight of grease adjuvants.
• alkaline forms of lithium and/or calcium metal compounds with a saponifiable material selected from fatty acids, hydroxy-substituted fatty acids, glycerides and hydroxylated glycerides, (c) from about 5.0 to 0.1 parts by weight of alkoxylated additives imparting water-resistance to said greases, said additives being selected from the group consisting of ethoxylated alkylated phenols and ethoxylated and propoxylated alkylene diamines.
• the soap is lithium 12-hydr0xystearate.

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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)

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Cited By (11)

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• 0
  • BE BE786090D patent/BE786090A/xx unknown
• 1971
  • 1971-07-12 US US00161993A patent/US3801506A/en not_active Expired - Lifetime
• 1972
  • 1972-06-15 DE DE2229065A patent/DE2229065A1/de active Pending
  • 1972-06-15 GB GB2798372A patent/GB1376835A/en not_active Expired
  • 1972-06-21 PH PH13647A patent/PH11908A/en unknown
  • 1972-06-23 AU AU43844/72A patent/AU456771B2/en not_active Expired
  • 1972-06-28 NL NL7208877A patent/NL7208877A/xx not_active Application Discontinuation
  • 1972-07-06 ES ES404606A patent/ES404606A1/es not_active Expired
  • 1972-07-06 CA CA146,540A patent/CA1000261A/en not_active Expired
  • 1972-07-10 IT IT26821/72A patent/IT962684B/it active
  • 1972-07-10 FR FR7224913A patent/FR2145563B3/fr not_active Expired
  • 1972-07-11 TR TR18719A patent/TR18719A/xx unknown
  • 1972-07-12 BR BR4588/72A patent/BR7204588D0/pt unknown

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