Classifications

• • 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
  • C10M115/00—Lubricating compositions characterised by the thickener being a non-macromolecular organic compound other than a carboxylic acid or salt thereof
  • C10M115/08—Lubricating compositions characterised by the thickener being a non-macromolecular organic compound other than a carboxylic acid or salt thereof containing nitrogen
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  • 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
  • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
  • C10M2201/10—Compounds containing silicon
  • C10M2201/102—Silicates
  • C10M2201/103—Clays; Mica; Zeolites
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  • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
  • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
  • C10M2201/10—Compounds containing silicon
  • C10M2201/105—Silica
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  • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
  • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
  • C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
  • C10M2205/026—Butene
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  • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
  • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
  • C10M2205/04—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing aromatic monomers, e.g. styrene
• • 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
  • C10M2207/40—Fatty vegetable or animal oils
• • 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
  • C10M2207/40—Fatty vegetable or animal oils
  • C10M2207/404—Fatty vegetable or animal oils obtained from genetically modified species
• • 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
  • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
  • C10M2209/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
  • C10M2209/08—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate type
  • C10M2209/084—Acrylate; Methacrylate
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  • 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
  • C10M2215/10—Amides of carbonic or haloformic acids
  • C10M2215/102—Ureas; Semicarbazides; Allophanates
• • 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
  • C10M2215/22—Heterocyclic nitrogen compounds
• • 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
  • C10M2215/22—Heterocyclic nitrogen compounds
  • C10M2215/221—Six-membered rings containing nitrogen and carbon only
• • 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
  • C10M2215/22—Heterocyclic nitrogen compounds
  • C10M2215/225—Heterocyclic nitrogen compounds the rings containing both nitrogen and oxygen
• • 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
  • C10M2215/22—Heterocyclic nitrogen compounds
  • C10M2215/225—Heterocyclic nitrogen compounds the rings containing both nitrogen and oxygen
  • C10M2215/226—Morpholines
• • 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
  • C10M2215/30—Heterocyclic compounds
• • 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
  • C10M2219/10—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring
• • 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
  • C10M2219/10—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring
  • C10M2219/102—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring containing sulfur and carbon only in the ring
• • 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
  • C10M2219/10—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring
  • C10M2219/104—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring containing sulfur and carbon with nitrogen or oxygen in the ring
• • 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
  • C10M2219/10—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring
  • C10M2219/104—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring containing sulfur and carbon with nitrogen or oxygen in the ring
  • C10M2219/106—Thiadiazoles
• • 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
  • C10M2223/045—Metal containing thio derivatives
• • 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

Definitions

• This invention relates to a diurea grease composition. More particularly, it relates to a diurea grease composition which undergoes little changes in consistency after use at higher temperatures for a prolonged period of time and small oil separtion at higher temperatures and which is also superior in various other properties.
• the lithium soap grease known as the "universal grease”
• the universal grease has a dropping point of the order of 200°C or thereabouts and cannot be used at higher temperatures above 150°C.
• urea greases such as diurea grease or tetraurea greases having modified terminal groups
• the tetraurea grease tends to be hardened or increased in consistency when exposed to higher temperatures for prolonged time period, while it may be disadvantageously hardened or softened depending on different shearing speeds given to the grease.
• the known diurea greases having only terminal alkyl groups have a low dropping point and undergoes considerable oil separation at higher temperatures so that they cannot be used for prolonged time at higher temperatures.
• the diurea greases having only aromatic hydrocarbon terminal groups are at most equivalent or even inferior to the diurea greases having the terminal alkyl groups with respect to the properties as the thickener.
• the present inventors have conducted researches towards overcoming the above mentioned drawbacks of the urea greases and have found that, while the diurea compound has highly desirable properties as the thickener, the terminal groups of the diurea compound plays an extremely important role.
• This diurea compound has been applied for patent in our Japanese Patent Publication No. 11156/1980.
• Ths diurea grease disclosed in the Japanese Patent Publication No. 11156/1980 has many excellent properties, such as
• a diurea grease composition comprising a base oil and 2 to 25 wt.%, based on the total weight of the composition, of a diurea compound as an essential ingredient, the diurea grease compound being produced by reacting a mixed system of two or more different diisocyanates represented by the formula (I) OCN-R-NCO (I) wherein R stands for a straight-chained or branched alkylene group, a straight-chained or branched alkenylene group, a cycloalkylene group or an aromatic group, with an amine compound selected from the group consisting of a primary amine represented by the formula (II) R1-NH2 (II) wherein R1 stands for a hydrocarbon residue having 6 to 20 carbon atoms, a secondary amine represented by the formula (III) wherein R2 and R3 may be the same or different and each stand for hydrocarbon residues having 6 to 20 carbon atoms, and mixtures thereof.
• R stands for a straight-chained or
• any oils commonly used as the lube base oil may be employed.
• mineral lube base oils mineral oils refined by a method consisting in a suitable combination of distillation under reduced pressure, solvent deasphalting, solvent extraction, hydrocracking, solvent dewaxing, hydrogenative dewaxing, washing by sulfuric acid, refining by terra abla or hydrofining.
• ⁇ -olefin oligomers such as normal paraffins, isoparaffins, polybutene, polyisobutyrene or 1-decene oligomers
• alkylbenzenes such as monoalkylbenzene, dialkylbenzene or polyalkylbenzene
• alkyl naphthalenes such as monoalkyl naphthalene, dialkyl naphthalene or polyalkyl naphthalene
• diesters such as di-2-ethylhexyl sebacate, dioctyl adipate, diisodecyl adipate, ditridecyl adipate or ditridecyl glutarate
• polyol esters such as trimethylolpropane caprylate, trimethylolpropane pelargonate, pentaerithritol-2-ethyl hexanoate or pentaerithr
• the diurea compound as the essential ingredient of the composition of the present invention may be obtained by reacting a mixed system of two or more different diisocyanates represented by the formula (I) OCN-R-NCO (I) wherein R stands for a straight-chained or branched alkylene group, a straight-chained or branched alkenylene group, a cycloalkylene group or an aromatic group, with an amine compound selected from the group consisting of a primary amine represented by the formula (II) R1-NH2 (II) wherein R1 stands for a hydrocarbon residue having 6 to 20 carbon atoms, a secondary amine represented by the formula (II) wherein R2 and R3 may be the same or different and each stand for hydrocarbon residues having 6 to 20 carbon atoms, and mixtures thereof.
• R stands for a straight-chained or branched alkylene group, a straight-chained or branched alkenylene group, a cycloalkylene group
• the number of carbon atoms in the group R in the isocyanate represented by the formula (I) may preferably be 6 to 20 and more preferably 6 to 15.
• the aforementioned mixed system of the diisocyanates preferably include mixtures of two or more compounds selected from the group consisting of, for example, diphenylmethane-4, 4′-diisocyanate, tolylene diisocyanate, hexamethylene diisocyanate, 2, 2, 4-trimethyl-hexamethylene diisocyanate, p-phenylene diisocyanate, 4, 4′-dicyclohexylmethane diisocyanate, 3, 3′-dimethyldiphenyl-4, 4′-diisocyanate, m-xylene diisocyanate, m-tetramethylxylene diisocyanate, p-tetramethylxylene diisocyanate, isophorone diisocyanate, 1, 5-naphthalene diisocyanate and trans-1,
• it may include a mixed system of diphenylmethane-4, 4′-diisocyanate and 4, 4′-dicyclohexylmethane diisocyanate, a mixed system of diphenylmethane-4, 4′-diisocyanate and 3, 3′-dimethyl­diphenyl-4, 4′-diisocyanate, a mixed system of diphenylmethane-4, 4′-diisocyanate and m-xylenedi­isocyanate, a mixed system of diphenylmethane-4, 4′-diisocyanate and tetramethylxylene diisocyanate, a mixed system of diphenylmethane-4, 4′-diisocyanate and a mixture of 2, 4-tolylene diisocyanate and 2, 6-tolylene diisocyanate, a mixed system of diphenylmethane-4, 4′-diisocyanate and isophorone diiso
• the mixing ratios of the above mentioned two or more different diisocyanates may be suitably selected in dependence upon the structures of the diisocyanates and the consistency of the greases to be produced.
• the mixing ratio may usually be 5 - 95 : 95 - 5, preferably 10 - 90 : 90 - 10, more preferably 20 - 80 : 80 - 20 and most preferably 30 - 70 : 70 - 30, in terms of the mol percent ratio.
• the mixing ratio less than the range of 5 - 95 : 95 - 5 is not desirable since problems are raised in changes in consistency after use or in oil separation so that the properties of the grese thickener are lowered.
• the mixing ratio is preferably 10 to 95 mol percent, prferably 20 to 80 mol percent and most preferably 30 to 70 mol percent of diphenylmethane-4, 4′-diisocyanate and 5 to 90 mol percent, preferably 20 to 80 mol percent and most preferably 30 to 70 mol percent of tolylene diisocyanate.
• the respective diisocyanates are preferably contained in amounts of not less than 5 mol percent and preferably not less than 10 mol percent.
• the amine compound reacted with the mixed diisocyanate system is a primary amine, a mixture of two or more primary amines, a secondary amine, or a mixture of two or more different secondary amines, represented by the above formulas (II) and (III), or mixtures thereof.
• R1, R2 and R3 may be the same or different groups and denote hydrocarbon residues with 6 to 20 caron atoms.
• hydrocarbon residues various groups such as alkyl, alkenyl, cycloalkyl or aromatic groups, may be employed.
• the alkyl groups may include those with straight or branched chains, such as hexyl, heptyl, octyl, nonyl, decyl, undecyl, dodecyl, tridecyl, tetradecyl, pentadecyl, hexadecyl, heptadecyl, octadecyl, nonadecyl or eicosyl groups.
• the alkenyl groups may include those with straight or branched chains, such as hexenyl, heptenyl, octenyl, nonenyl, decenyl, undecenyl, dodecenyl, tridecenyl, tetradecenyl, pentadecenyl, hexadecenyl, heptadecenyl, octadecenyl, nonadecenyl or eicosenyl groups.
• cyclohexyl group and the groups derived from the cyclohexyl group may preferably be employed.
• examples of the cyclohexyl group and its derivatives may include cyclohexyl, methyl cyclohexyl, dimethyl cyclohexyl, ethyl cyclohexyl, diethyl cyclohexyl, propyl cyclohexyl, isopropyl cyclohexyl, 1-methyl-3-propyl-­cyclohexyl, butyl cyclohexyl, amyl cyclohexyl, amylmethyl cyclohexyl, hexyl cyclohexyl, heptyl cyclohexyl, octyl cyclohexyl, nonyl cyclohexyl, decyl cyclohexyl, undecyl cyclohexyl,
• cyclohexyl group and C7 to C8 groups derived from the cyclohexyl group such as, for example, methyl cyclohexyl, dimethyl cyclohexyl or ethyl cyclohexyl groups.
• aromatic groups may include phenyl, toluyl, benzyl, ethyl phenyl, methyl benzyl, xylyl, propyl phenyl, cumenyl, ethyl benzyl, methyl phenetyl, butyl phenyl, propyl benzyl, ethyl phenetyl, pentyl phenetyl, butyl benzyl, propyl phenetyl, hexyl phenyl, pentyl benzyl, butyl phenetyl, heptyl phenyl, hexyl benzyl, pentyl phenetyl, octyl phenyl, heptyl benzyl, hexyl phenetyl, nonyl phenyl, octyl benzyl, heptyl phenety
• the most preferred amine compound to be reacted with the above mentioned diisocyanate mixed system is a primary amine represented by the formula (II) in which R1 denotes a cyclohexyl group, a C7 to C12 alkylcyclohexyl group, a C 6 to C20 alkyl group or a C6 to C20 alkenyl group, or a secondary amine represented by the formula (III) in which R2 and R3 each denote a cyclohexyl group or a C7 to C12 alkylcyclohexyl group.
• Most preferred is also an amine mixture in which the primary amine represented by the formula (II) is used and in which the ratio of the total number of cyclohexyl groups and/or the alkyl cyclohexyl groups to the number of the total amines given by the formula ⁇ (total number of the cyclohexyl groups and/or the alkylcyclohexyl groups)/(the total number of the groups selected from the group consisting of the cyclohexyl group, alkylcyclohexyl group, alkyl group and the alkenyl group bonded to the amine employed) ⁇ X 100 is 20 to 90 in terms of the mol percent.
• contents of the diurea compound containing both the cyclohexyl groups and/or alkylcyclohexyl groups and the alkyl groups and/or alkenyl groups in the produced diurea compound account for 10 mol percent or higher based on the total number of the produced diurea compounds.
• an amine mixture consisting of a primary amine of the formula (II) in which R1 is a cyclohexyl group, a C7 to C12 alkyl cyclohexyl group or a C6 to C20 alkyl group and a secondary amine of the formula (III) in which R2 and R3 each represent a cyclohexyl group or a C7 to C12 alkyl cyclohexyl group and in which the ratio of the contents of the secondary amine to the amount of total amine given by the formula ⁇ (number of amino groups in the secondary amine)/(number of the amino groups in the primary amine plus number of the amino groups in the secondary amine) ⁇ X 100 is 1 to 50 in terms of mol percent, or an amine mixture in which the total amount of the primary amine of the formula (II) in which R1 is a cyclohexyl group or an alkylcyclohexyl group bears a molar ratio of 1/4
• the diurea compound acting as the thickener, is produced by reacting the above mentioned mixed system of the diisocyanates with the above mentioned primary amine and/or secondary amine. This point is most crucial in the present invention.
• the effects of the present invention cannot be derived from the diurea grease obtained in any other methods, such as by separately reacting the above mentioned two or more diisocyanates with amines and subsequently mixing the produced two or more diurea compounds.
• volatile solvents such as benzene, toluene, xylene, hexane, naphtha, diisobutyl ether, carbon tetrachloride or petroleum ether, may be employed.
• Lube base oils may also be employed as suitable solvents.
• the preferred reaction temperature is 100 to 200°C. The reaction system need be mixed and agitated thoroughly to produce a uniform diurea grease.
• the thus produced diurea compound acting as the thickener, contains the diurea compounds in amounts corresponding to the mixing ratios of the diisocyanates. More specifically, if the mixed system consisting of 10 to 95 mol percent of diphenylmethane-4, 4′-diisocyanate and 5 to 95 mol percent of tolylene diisocyanate is employed, the thickener contains 10 to 95 mol percent of a diure compound represented by the formula and 5 to 90 mol percent of a diurea compound represented by the formula wherein X1, X2, X3 and X4 each stand for one of the groups R1-NH- or where R1, R2 and R3 have the same meaning as R1, R2 and R3 in the above formulas (II) and (III).
• the volatile solvent is used, the solvent is removed and a suitable amount of the lube base oil is added to give the grease.
• the reaction product may be used directly as the grease.
• the contents of the diurea compound acting as the thickener is 2 to 25 wt.% and preferably 3 to 20 wt.% based on the total weight of the composition.
• the contents of the diurea compound less than 2 wt.% are not desirable because the effects as the thickener are nill, whereas the contents in excess of 25 wt.% are also not desirable because the grease becomes too hard and cannot exhibit the lubricating effects sufficiently.
• the grease of the present invention may be admixed with suitable additives for further improving its properties.
• suitable additives include other thickeners, such as metal soaps, bentone or silica gel, extreme pressure agents, such as chlorine, sulphur or phosphorus extreme pressure agents or zinc dithiophosphate, oiliness agents such as fatty oils, animal or vegetable oils, viscosity index improvers, such as polymethacrylate, polybutene or polystyrene, anti-oxidants such as amine, phenol or sulpher anti-oxidants or zinc dithiophosphate, or metal inactivators, such as benzotriazole or thiadiazole.
• the dropping point was measured in accordance with the dropping point testing method in JIS K 2220 5.4.
• the oil separation was measured at 150°C for 200 hours in accordance with the oil separation testing method in JIS K 2220 5.7.
• the produced diurea compound was formed by 80 mol percent in total of diurea compounds represented by the formulas and 20 mol percent in total of diurea compounds represented by the formulas
• the contents in the composition of the thickener formed by the diurea compounds were 10 wt.%.
• the produced diurea compound was formed by 30 mol percent in total of the diurea compounds reprsented by the formulas and 70 mol percent in total of the diurea compounds represented by the formulas
• the contents in the composition of the thickener formed by the diurea compounds were 10 wt.%.
• the produced diurea compound was comprised of 50 mol percent in total of the diurea compounds represented by the formulas 50 mol percent in total of the diurea compounds represented by the formulas with the sum of the amounts of the compounds represented by the formulas (2) and (5) being 50 mol percent.
• the contents in the composition of the thickener formed by the diurea compounds were 10 wt.%.
• the substance was passed through a roll mill to produce a grease composition.
• the produced diurea compound was formed by 30 mol percent of a diurea compound represented by the formula and 70 mol percent of a diurea compound represented by the formula at a rate of 30 : 30 :40.
• the contents in the composition of the thickener formed by the diurea compounds were 10 wt.%.
• the performance appraisal tests similar to those of Example 1 were conducted on the produced diurea grease. The resulta are shown in Table 1.
• the resulting mixture was agitated thoroughly and passed through a roll mill to produce a grease composition.
• This diurea compounds were formed by 40 mol percent in total of diurea compounds represented by the formulas and 60 mol percent in total of diurea compounds represented by the formulas wherein the sum of the amounts of the compounds represented by the formulas (8) and (11) is 30 mol percent and the ratio of the contents of the methylcyclohexyl group and the octyl group is 70 : 30.
• the contents in the composition of the thickener formed by the diurea compounds were 10 wt.%.
• the produced diurea composition was formed by 60 mol percent of a diurea compound represented by the formula and 40 mol percent of a diurea compound represented by the formula wherein Y1, Y2, Y3 and Y4 each represent groups at the ratio of 40 : 30 : 30.
• the contents in the composition of the thickener formed by the diurea compounds were 10 wt.%.
• Diisocyanates A and B each shown in the following Table were charged into 900 g of a mineral oil having a viscosity at 100°C of 10.3 cSt and were heated to 60°C so as to be uniformly dissolved therein. To this solution was added cyclohexylamine in amounts respectively shown in the Table and agitated vigorously. Each of gel-like substances was produced immediately. After the temperature was raised to 120°C by sustaind agitation for 30 minutes, each substance was passed through a roll mill to produce a grease composition. The contents in the composition of the thickener formed by the diurea compounds were 10 wt.%, respectively.
• the contents of the diurea compound of the formula acting as the thickener were 10 wt.%.
• the contents of the diurea compound of the formula acting as the thickener were 10 wt.%.
• the diurea composition was formed by 50 mol percent of a diurea compound represented by the formula and 50 mol percent of a diurea compound represented by the formula
• the contents in the composition of the thickener formed by the diurea compounds were 10 wt.%.
• the diurea grease composition of the present invention has an improved shearing stability and a high dropping point while being subject to small oil separation and exhibiting superior thickening properties.
• the grease compositions of the Comparative Examples 1 to 5 are equivalent or inferior to the inventive grease composition in shearing stability and dropping point while being evidently inferior to the inventive grease in thickening properties and oil separation at higher temperatures.
• the grease composition of the present invention is superior in its various properties to the compositions of the Comparative Exmples 1 to 5.

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• Chemical Kinetics & Catalysis (AREA)
• General Chemical & Material Sciences (AREA)
• Oil, Petroleum & Natural Gas (AREA)
• Organic Chemistry (AREA)
• Lubricants (AREA)

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• 1990
  • 1990-06-15 JP JP2155338A patent/JP2777928B2/ja not_active Expired - Lifetime
  • 1990-07-06 DE DE90112952T patent/DE69005380T2/de not_active Expired - Fee Related
  • 1990-07-06 EP EP90112952A patent/EP0406894B1/de not_active Expired - Lifetime

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