Grease composition

Abstract

The invention provides a grease composition used for lubricating a mechanical part having a steel portion to be lubricated which performs a rolling motion and a rolling and sliding motion, containing a base oil, a thickener and an additive, wherein the additive includes at least one compound selected from the group consisting of polyethylene wax, oxidized polyethylene wax, polypropylene wax, montan wax and amide wax.

Claims

1. A grease composition for use in lubricating a mechanical part having a steel portion to be lubricated, the portion of which performs a rolling motion and a rolling and sliding motion, consisting of a base oil, a thickener and an additive, wherein the thickener is a diurea compound represented by formula (1): R1-NHCONHR2-NHCONHR3 (1) wherein R2 is a bivalent aromatic hydrocarbon group having 6 to 15 carbon atoms; and one of R1 or R3 represents a saturated alkyl group having 18 carbon atoms and the other represents a cyclohexyl group, the molar ratio of the cyclohexyl group to the alkyl group being 20:80 to 95:5, and wherein the additive consists of: at least one compound selected from the group consisting of polyethylene wax having a weight-average molecular weight of 18,000 to 20,000 and a dropping point of 100 to 150 C., and 0 to 20 mass % of other additives, with respect to the total mass of the grease composition, selected from the group consisting of: an antioxidant selected from the group consisting of phenyl a-naphthylamine, alkylphenyl a-naphthylamine, alkyldiphenylamine, 2,6-di-tert-butyl-p-cresol, pentaerythrityltetrakis[3-(3,5-di-t-butyl-4-hydroxyphenyl)propionate], and octadecyl-3-(3,5-di-t-butyl-4-hydroxyphenyl)propionate; an inorganic passivator; a rust preventive; a metallic corrosion inhibitor; an oiliness improver; a phosphorus-containing, sulfur-containing or organic metal-containing antiwear agent or extreme-pressure agent selected from the group consisting of tricresyl phosphate, tri-2-ethylhexylphosphate; dibenzyl disulfide, polysulfide; triphenylphosphorothionate; Mo, Sb or Bi salts of dialkyldithiophosphoric acid, Mo, Zn, Sb, Ni, Cu, or Bi salts of dialkyldithiocarbamic acid; ash-free dithiocarbamate, and ash-free dithiophosphate carbamate; and a solid lubricant selected from the group consisting of oxidized metal salts, metal salts of carbonate and molybdenum disulfide.

2. The grease composition of claim 1, wherein the at least one compound is contained in an amount of 0.1 to 10 mass % in the grease composition.

3. A mechanical part having a steel portion to be lubricated which performs a rolling motion and a rolling and sliding motion, wherein the grease composition of claim 1 is enclosed.

4. The grease composition of claim 1, wherein the base oil is selected from the group consisting of a mineral oil, a synthetic hydrocarbon oil, and an ester oil.

5. The grease composition of claim 1, wherein the base oil is a mixture of paraffinic mineral oil and naphthenic mineral oil, a synthetic hydrocarbon oil, or a mixture of a synthetic hydrocarbon oil and an ester oil.

6. The grease composition of claim 1, wherein the base oil has a kinematic viscosity at 40 C. of 10 to 200 mm2/s.

7. The grease composition of claim 1, wherein the base oil is contained in an amount of 50 to 95 mass % in the grease composition.

8. The grease composition of claim 1, wherein the thickener is contained in an amount of 3 to 30 mass % in the grease composition.

9. The grease composition of claim 1, wherein the rust preventive is contained in an amount of 0.1 to 10 mass %.

Description

DESCRIPTION OF EMBODIMENTS

(1) <Base Oil>

(2) The base oil that can be used in the invention is not particularly limited. Any base oils including mineral oils can be used. One kind of base oil may be used alone or two or more base oils may be used in combination.

(3) Examples of the mineral oils include paraffinic mineral oils, naphthenic mineral oils and mixtures thereof. In particular, the mixture of the paraffinic mineral oil and the naphthenic mineral oil is preferable.

(4) Examples of the synthetic oils include synthetic ester oils such as diesters and polyol esters, synthetic hydrocarbon oils such as poly -olefins and polybutene, synthetic ether oils such as alkyl diphenyl ethers and polypropylene glycols, silicone oils, fluorinated oils, and other kinds of synthetic oils. Of the above synthetic oils, it is preferable to use the synthetic hydrocarbon oil, the ester oil, the synthetic ether oil, and the mixture thereof. More preferably, the synthetic hydrocarbon oil, the ester oil and the mixture thereof may be used. Most preferably, the synthetic hydrocarbon oil and the mixture of the synthetic hydrocarbon oil and the ester oil may be used.

(5) As the base oil, the mineral oil, the synthetic hydrocarbon oil, and the ester oil are preferable. It is more preferable to use the mixture of paraffinic mineral oil and naphthenic mineral oil, the synthetic hydrocarbon oil, and the mixture of the synthetic hydrocarbon oil and the ester oil.

(6) The kinematic viscosity of the base oil used in the invention is not particularly limited, and may be determined if necessary. The kinematic viscosity at 40 C. may preferably be 10 to 200 mm.sup.2/s, more preferably 15 to 170 mm.sup.2/s, and most preferably 30 to 140 mm.sup.2/s.

(7) The content of the base oil may preferably be in the range of 50 to 95 mass %, and more preferably 60 to 90 mass %, in the grease composition of the invention.

(8) <Thickener>

(9) The thickener used in the grease composition of the invention is not particularly limited. Preferable examples of the thickener include soap type thickeners such as lithium soap, lithium complex soap and the like; urea type thickeners such as diurea and the like; inorganic thickeners such as organoclay, silica and the like; and organic thickeners such as polytetrafluoroethylene (PTFE) and the like. Particularly preferable is the urea type thickener.

(10) Of the urea type thickeners, a diurea compound represented by the following formula (1) is preferable:
R1-NHCONHR2-NHCONHR3(1)
wherein R2 is a bivalent aromatic hydrocarbon group having 6 to 15 carbon atoms; and R1 and R3, which may be the same or different from each other, each represent a saturated or unsaturated alkyl group having 6 to 30 carbon atoms, an aryl group having 6 or 7 carbon atoms, or cyclohexyl group.

(11) When one of R1 or R3 represents cyclohexyl group, the other may preferably be a saturated or unsaturated alkyl group having 6 to 30 carbon atoms. In this case, the molar ratio of the cyclohexyl group to the alkyl group may preferably be 20:80 to 95:5, and more preferably 30:70 to 90:10.

(12) R2 may represent tolylene diisocyanate or diphenylmethane diisocyanate, and the latter is preferable.

(13) R1 and R3, which may be the same or different from each other, each may preferably represent a saturated or unsaturated alkyl group having 8 to 20 carbon atoms, an aryl group having 6 or 7 carbon atoms, or cyclohexyl group. The saturated alkyl group having 8 or 18 carbon atoms, the aryl group having 7 carbon atoms, or cyclohexyl group is more preferable.

(14) A diurea compound where R2 represents tolylene diisocyanate or diphenylmethane diisocyanate in the formula (1) is preferable.

(15) A diurea compound where R2 represents diphenylmethane diisocyanate in the formula (1) is more preferable.

(16) A diurea compound where R2 represents diphenylmethane diisocyanate, and R1 and R3, which may be the same or different from each other, each represent a saturated or unsaturated alkyl group having 8 to 20 carbon atoms, an aryl group having 6 or 7 carbon atoms or cyclohexyl group in the formula (1) is further more preferable.

(17) A diurea compound where R2 represents diphenylmethane diisocyanate, and R1 and R3, which may be the same or different from each other, each represent a saturated alkyl group having 8 or 18 carbon atoms, an aryl group having 7 carbon atoms or cyclohexyl group in the formula (1) is particularly preferable.

(18) In particular, a diurea compound where R2 represents diphenylmethane diisocyanate, and R1 and R3 each represent a saturated alkyl group having 8 carbon atoms in the formula (1) is more preferable.

(19) In particular, a diurea compound where R2 represents diphenylmethane diisocyanate, and R1 and R3, which may be the same or different from each other, each represent a saturated alkyl group having 8 or 18 carbon atoms in the formula (1) is also more preferable. It is particularly preferred to use a mixture of a diurea compound where R1 and R3 each represent a saturated alkyl group having 8 carbon atoms, a diurea compound where R1 and R3 each represent a saturated alkyl group having 18 carbon atoms, and a diurea compound where one of R1 or R3 represents a saturated alkyl group having 8 carbon atoms and the other represents a saturated alkyl group having 18 carbon atoms. In this case, the molar ratio of the saturated alkyl group having 8 carbon atoms to the saturated alkyl group having 18 carbon atoms may preferably be 10:90 to 90:10, and more preferably 30:70 to 70:30.

(20) Also, a diurea compound where R2 represents diphenylmethane diisocyanate, and R1 and R3 each represent an aryl group having 7 carbon atoms in the formula (1) is more preferable.

(21) Further, a diurea compound where R2 represents diphenylmethane diisocyanate, and R1 and R3, which may be the same or different from each other, each represent a saturated alkyl group having 18 carbon atoms or cyclohexyl group in the formula (1) is particularly preferable. It is particularly preferred to use a mixture of a diurea compound where R1 and R3 each represent a saturated alkyl group having 18 carbon atoms, a diurea compound where R1 and R3 each represent cyclohexyl group, and a diurea compound where one of R1 or R3 represents a saturated alkyl group having 18 carbon atoms and the other represents cyclohexyl group. In this case, the molar ratio of the cyclohexyl group to the alkyl group may preferably be 20:80 to 95:5, and more preferably 30:70 to 90:10.

(22) The diurea compound of formula (1) is obtainable by reacting a predetermined diisocyanate with a predetermined monoamine, for example. Preferable specific examples of the diisocyanate include diphenylmethane-4,4-diisocyanate and tolylene diisocyanate. Examples of the monoamine include aliphatic amine compounds, aromatic amine compounds, alicyclic amine compounds and the mixtures thereof. Specific examples of the aliphatic amine compounds include octylamine, nonylamine, decylamine, undecylamine, dodecylamine, tridecylamine, tetradecylamine, pentadecylamine, hexadecylamine, heptadecylamine, octadecylamine, nonyldecylamine, eicodecylamine, oleylamine and the like. Specific examples of the aromatic amine compounds include aniline, p-toluidine, naphthylamine and the like. Specific examples of the alicyclic amine compounds include cyclohexylamine, dicyclohexylamine and the like.

(23) The content of the thickener in the grease composition of the invention varies depending upon the kind of thickener. The grease composition of the invention may preferably have a consistency of 200 to 400, and the content of the thickener is determined so as to obtain the above-mentioned consistency. The content of the thickener may generally be 3 to 30 mass %, and preferably in the range of 5 to 25 mass %, in the grease composition of the invention.

(24) <Additive>

(25) The additive used in the invention comprises at least one compound selected from the group consisting of polyethylene wax, oxidized polyethylene wax, polypropylene wax, montan wax, and amide wax.

(26) Addition of the above-mentioned additive makes it possible to form a thick oil film on the portion which is required to be lubricated although formation of the oil film is difficult, especially when the operating speed is within a low speed region. This can prevent the direct contact between metallic members, thereby reducing the friction torque and extending the anti-flaking life. It is presumed that the mechanism of making an oil film thick, especially at a low speed region, by the specific additive is that, at a low speed region, the equivalent viscosity of the grease becomes very high, the viscosity which is comparable to the first Newtonian viscosity, while the entraining speed is low, thereby forming a thick EHL film, as explained in the above-mentioned document (Dong, Komoriya. Endo and Kimura, Formation of EHL Film with Grease in Ball Bearings at Low Speeds, the JAST Tribologist 57-8 (2012) pp. 568-574).

(27) The polyethylene wax and the polypropylene wax may have a weight-average molecular weight of about 1,000 to about 20,000. There are the high-density type with a density of 0.96 or more, the medium-density type with a density ranging from 0.94 to 0.95 and the low-density type with a density of 0.93 or less. The high-density type is characterized by the high melting point, softening point and crystallinity, and high degree of hardness, while the low-density type has the low melting point and softening point and exhibits the soft properties. In consideration of the heat-resistance, the dropping point of the polyethylene wax and the polypropylene wax may preferably be 100 C. or more, and more preferably 120 C. or more. From the viewpoint of the solubility in the base oil, the dropping point may preferably be 150 C. or less, and the acid value may preferably be in the range of 0 to 10 mgKOH/g, and more preferably 0 to 5 mgKOH/g. When the acid value is within the above-mentioned range, oxidative deterioration of the resultant grease by acid components can be reduced.

(28) Specific examples of the commercially available polyethylene wax include Hi-WAX 200P, Hi-WAX 210P and Hi-WAX NL200 (made by Mitsui Chemicals, Inc.); and Licowax PE520, Licowax PE190 and Licowax PE130 (made by Clariant Japan K.K.). Specific examples of the commercially available polypropylene wax include Hi-WAX NP105 (made by Mitsui Chemicals, Inc.) and Ceridust 6050M (made by Clariant Japan K.K.) and the like.

(29) The oxidized polyethylene wax, which is obtained by subjecting the polyethylene wax to oxidation treatment and subjecting the high-density polyethylene resin to oxidation treatment may have a weight-average molecular weight of about 3,000 to about 12,000. In consideration of the heat-resistance, the dropping point of the oxidized polyethylene wax may preferably be 90 C. or more, and more preferably 100 C. or more. From the viewpoint of the solubility in the base oil, the dropping point may preferably be 125 C. or less. The acid value may preferably be 60 mgKOH/g or less, and more preferably 30 mgKOH/g or less. When the acid value is within the above-mentioned range, oxidative deterioration of the resultant grease by acid components can advantageously be reduced.

(30) Specific examples of the commercially available oxidized polyethylene wax include Hi-WAX 200MP, Hi-WAX 4051E and Hi-WAX 1105A (made by Mitsui Chemicals, Inc.); and Licowax PED522 (made by Clariant Japan K.K.) and the like.

(31) The montan wax, which belongs to the group of mineral wax comprises long-chain esters as the main component, free higher alcohols, resins, sulfur-containing compounds and the like. There are acid waxes having an acid value of 110 to 160 mgKOH/g; ester waxes having both non-polar portions and polar portions; partially saponified ester waxes containing a mixture of the esterified product of montanic acid and the saponified product of the above esterified product with calcium hydroxide saponified waxes of sodium salt and calcium salt of montanic acid; ethylene oxide added montan waxes and the like. In consideration of the heat-resistance, the dropping point of the montan wax may preferably be 75 C. or more, and more preferably 80 C. or more. From the viewpoint of the solubility in the base oil, the dropping point may preferably be 105 C. or less. The acid value may preferably be in the range of 0 to 160 mgKOH/g, and more preferably 0 to 40 mgKOH/g. When the acid value is within the above-mentioned range, oxidative deterioration of the resultant grease by acid components can advantageously be reduced.

(32) Specific examples of the commercially available montan wax include Licowax OP Flakes, Licowax S and Licolub WE40 (made by Clariant Japan K.K.) and the like.

(33) The amide wax, which has in the molecule thereof a long-chain alkyl group and an amide group with a large polarity. There are fatty acid amides and N-substituted fatty acid amides. Examples of the fatty acid amides include lauramide, oleamide, stearamide, erucamide and the like. In consideration of the heat-resistance, the dropping point of the amide wax may preferably be 70 C. or more, and more preferably 80 C. or more. From the viewpoint of the solubility in the base oil, the dropping point may preferably be 100 C. or less.

(34) Specific examples of the commercially available amide wax include Irmo slip CP powder, Irmo slip HT powder, Irmo slip E (made by Lion Aczo Co., Ltd.) and the like.

(35) The dropping point herein used is the value determined in accordance with DIN51801. The acid value and the saponification value are the values obtained in accordance with DIN53402 and DIN53401, respectively.

(36) As the essential additive as mentioned above, the polyethylene wax and the polypropylene wax are preferred, and the polyethylene wax is more preferred. In particular, the polyethylene wax with a weight-average molecular weight of 4,000 to 20,000 is desirable, and such a polyethylene wax may further preferably have an acid value of 5 mgKOH/g or less.

(37) The content of the above-mentioned essential additive may preferably be in the range of 0.1 to 10 mass %, more preferably 0.5 to 7 mass %, and most preferably 1 to 5 mass %, based on the total mass of the grease composition of the invention.

(38) <Other Additives>

(39) When necessary, the grease composition of the invention may further comprise any additives. Examples are as follows: an antioxidant including amine-based and phenol-based antioxidants (e.g., amine-based antioxidants such as phenyl -naphthylamine, alkylphenyl -naphthylamine, alkyldiphenylamine and the like; phenol-based antioxidants including hindered phenols, such as 2,6-di-tert-butyl-p-cresol, pentaerythrityl tetrakis[3-(3,5-di-t-butyl-4-hydroxyphenyl)propionate], octadecyl-3-(3,5-di-t-butyl-4-hydroxyphenyl)propionate and the like.

(40) An inorganic passivator such as sodium nitrite or the like.

(41) A rust preventive such as sulfonate type, succinic acid type, amine type and carboxylate type rust preventives (e.g., organic sulfonate rust preventives such as Ca, Ba, Zn and Na salts of organic sulfonic acid and the like; succinic acid type rust preventives such as alkenylsuccinic anhydride, alkenylsuccinate, half ester of alkenylsuccinic acid and the like; amine salts of fatty acids, dibasic acids, naphthenic acids, lanolin fatty acids, alkenylsuccinic acids and the like; and carboxylate type rust preventives such as Na. K and Zn salts of aliphatic dicarboxylic acids and naphthenic acids such as sebacic acid, undecanedioic acid, dodecanedioic acid, brassilic acid, tetradecanedioic acid and the like.

(42) A metallic corrosion inhibitor such as benzotriazole.

(43) An oiliness improver such as fatty acids, fatty acid esters, and phosphates.

(44) A phosphorus-containing, sulfur-containing or organic metal-containing antiwear agent or extreme-pressure agent (e.g., tricresyl phosphate, tri-2-ethylhexylphosphate; dibenzyl disulfide, a variety of polysulfides; triphenylphosphorothionate; Mo, Sb and Bi salts of dialkyldithiophosphoric acid, Mo, Zn, Sb, Ni, Cu and Bi salts of dialkyldithiocarbamic acid and the like; ash-free dithiocarbamate, ash-free dithiophosphate carbamate.

(45) A solid lubricant including oxidized metal salts, metal salts of carbonate and molybdenum disulfide (e.g., CaO, ZnO, MgO, CaCO.sub.3, ZnCO.sub.3, molybdenum disulfide, graphite, PTFE, MCA and the like). Such components may be generally used in an amount of about 0.1 to 20 mass %, preferably 0.5 to 10 mass %.

(46) <Worked Penetration>

(47) The worked penetration of the grease composition of the invention is adjusted according to the application, and may preferably be in the range of 200 to 400. Especially when used for the rolling bearing, the grease composition of the invention may preferably have a worked penetration of 200 to 350 because there is the risk of leakage of excessively soft grease composition. When used for the constant velocity joint, the grease composition of the invention may preferably have a worked penetration of 250 to 400. When used for the ball screws, the grease composition of the invention may preferably have a worked penetration of 250 to 400.

Examples

(48) <Preparation of Test Greases>

(49) Grease compositions of Examples and Comparative Examples were prepared using the thickeners, base oils and additives shown in the following Tables. Specifically, diphenylmethane diisocyanate was reacted with a predetermined amine in the base oil, and the resultant mixture was heated and then cooled, followed by kneading using a three-roll mill, thereby obtaining the grease compositions of Examples and Comparative Examples.

(50) The content of the thickener was adjusted so that the resultant grease composition might have a worked penetration of 300 (when determined in accordance with JIS K2220 7).

(51) The grease compositions thus prepared were evaluated according to the test methods shown below. The results are also shown in the following Tables.

(52) <Test Methods>

(53) Measurement of EHL Film Thickness

(54) The thickness of a grease film formed at the rolling contact portion was determined using a ultra-thin film thickness measuring instrument based on optical interference technique (EHL Ultra Thin Film Measurement System, made by PCS Instruments.) In the measurement, a steel ball with a diameter of 19.05 mm was brought into contact with a glass disc under rollingsliding contact conditions at 25 C. under a load of 20 N. With the speed of the ball (1 m/s) being gradually decreased, the film thickness was measured when the speed of the steel ball reached the predetermined value as shown below. The term film thickness herein used indicates the central oil film thickness. The specific test conditions are as follows.

(55) <Test Conditions>

(56) Load: 20 N

(57) Maximum contact pressure: 0.5 GPa

(58) Speed: 0.01 m/s

(59) Slide ratio: 5%

(60) Temperature: 25 C.

(61) Steel ball: with a diameter of 19.05 mm

(62) Glass disc: coated with silica and chromium

(63) <Decision Whether to Accept or Not>

(64) The central thickness of oil film: 100 nm or more: o (acceptable)

(65) less than 100 nm: x (unacceptable)

(66) Measurement of Traction Coefficient

(67) A two roll machine (TE54 Mini Traction friction tester, from Sanyo Trading Co., Ltd.) was used to determine the traction coefficient. The specific test conditions are as follows.

(68) <Test Conditions>

(69) Upper specimen: Steel ball with a diameter of 25 mm. Ra=0.01 m

(70) Lower specimen: Steel ring with a diameter of 50 mm, Ra=0.01 m

(71) Speed of upper specimen: 50 mm/s

(72) Speed of lower specimen: 47 mm/s

(73) Slide ratio: 5%

(74) Temperature: 25 C.

(75) Contact pressure: 1.5 GPa

(76) <Decision Whether to Accept or Not>

(77) The traction coefficient; less than 0.070: o (acceptable)

(78) 0.070 or more: x (unacceptable)

(79) Evaluation of Anti-Flaking Properties

(80) A rolling four-ball tester was used to evaluate the anti-flaking properties. Three steel balls with a diameter of 15 mm designed for bearings were disposed in a cylindrical container with a depth of 10.95 mm, having a bottom with an inner diameter of 36.0 mm and a top end with an inner diameter of 31.63 mm. To the steel balls, 20 g of each test grease composition was applied. Another steel ball (-in) for bearing was placed in contact with the three steel balls, and driven to rotate at the predetermined number of revolutions. The lower three steel balls then revolved as each rotating on its axis. The ball was driven to rotate continuously until the flaking took place on the steel ball surfaces. The flaking occurs at a point between two balls where the highest contact pressure is applied. The life was expressed as the total revolutions counted when the flaking took place.

(81) <Test Conditions>

(82) Steel balls for test: a -in steel ball for bearing (driving ball) and 15-mm-dia. steel balls for bearing (driven balls)

(83) Load for test: 400 kgf (Maximum contact pressure: 6.5 GPa)

(84) Rotational speed: 1500 rpm

(85) The number of repeated tests: five (average life: n=5)

(86) <Decision Whether to Accept or Not>

(87) The average life (total revolutions of the driving ball);

(88) 8010.sup.5 or more: o (acceptable) less than 8010.sup.5: x (unacceptable)

(89) Overall Evaluation

(90) The grease composition passed all the tests, i.e., the EHL film thickness test, the traction coefficient test and the rolling four-ball test: o (acceptable).

(91) The grease composition failed any one of the above tests: x (unacceptable)

(92) TABLE-US-00001 TABLE 1 Example 1 Example 2 Example 3 Example 4 Example 5 Thickener.sup.(*.sup.1) Aliphatic diurea A 10.0 (mass % in grease Aliphatic diurea B 12.0 composition) Aromatic diurea 21.0 Alicyclicaliphatic diurea C 10.0 Alicyclicaliphatic diurea D 10.0 Base oil.sup.(*.sup.2) Synthetic hydrocarbon oil E 100 100 100 100 100 (mass % of each Synthetic hydrocarbon oil F component based on total Mineral oil G mass of base oil) Mineral oil H Ester oil Phenyl ether oil Additives.sup.(*.sup.3) Polyethylene wax 5.0 5.0 5.0 5.0 5.0 (mass % in grease Oxidized polyethylene wax composition) Polypropylene wax Montan wax Amide wax Worked penetration 300 300 300 300 300 Central thickness of oil film (nm) 300 290 360 300 310 Decision whether to accept or not Traction coefficient 0.064 0.067 0.062 0.063 0.065 Decision whether to accept or not Average life (total revolutions of driving ball) 10.sup.5 131 130 137 140 123 Decision whether to accept or not Overall evaluation

(93) TABLE-US-00002 TABLE 2 Example Example 6 Example 7 Example 8 Example 9 10 Thickener.sup.(*.sup.1) Aliphatic diurea A 10.0 10.0 10.0 9.0 10.0 (mass % in grease Aliphatic diurea B composition) Aromatic diurea Alicyclicaliphatic diurea C Alicyclicaliphatic diurea D Base oil.sup.(*.sup.2) Synthetic hydrocarbon oil E (mass % of each Synthetic hydrocarbon oil F 100 component based on total Mineral oil G 100 mass of base oil) Mineral oil H 100 Ester oil 100 Phenyl ether oil 100 Additives.sup.(*.sup.3) Polyethylene wax 5.0 5.0 5.0 5.0 5.0 (mass % in grease Oxidized polyethylene wax composition) Polypropylene wax Montan wax Amide wax Worked penetration 300 300 300 300 300 Central thickness of oil film (nm) 300 260 270 260 280 Decision whether to accept or not Traction coefficient 0.064 0.068 0.065 0.067 0.067 Decision whether to accept or not Average life (total revolutions of driving ball) 10.sup.5 137 111 122 109 128 Decision whether to accept or not Overall evaluation

(94) TABLE-US-00003 TABLE 3 Example Example Example Example Example 11 12 13 14 15 Thickener.sup.(*.sup.1) Aliphatic diurea A (mass % in grease Aliphatic diurea B composition) Aromatic diurea Alicyclicaliphatic diurea C 10.0 10.0 10.0 10.0 10.0 Alicyclicaliphatic diurea D Base oil.sup.(*.sup.2) Synthetic hydrocarbon oil E 100 100 100 100 100 (mass % of each Synthetic hydrocarbon oil F component based on total Mineral oil G mass of base oil) Mineral oil H Ester oil Phenyl ether oil Additives.sup.(*.sup.3) Polyethylene wax 1.0 (mass % in grease Oxidized polyethylene wax 5.0 composition) Polypropylene wax 5.0 Montan wax 5.0 Amide wax 5.0 Worked penetration 300 300 300 300 300 Central thickness of oil film (nm) 210 250 220 200 350 Decision whether to accept or not Traction coefficient 0.068 0.068 0.068 0.069 0.062 Decision whether to accept or not Average life (total revolutions of driving ball) 10.sup.5 109 111 100 94 141 Decision whether to accept or not Overall evaluation

(95) TABLE-US-00004 TABLE 4 Example Example Example Example Example 16 17 18 19 20 Thickener.sup.(*.sup.1) Aliphatic diurea A (mass % in grease Aliphatic diurea B 12.0 composition) Aromatic diurea 21.0 Alicyclicaliphatic diurea C 9.0 10.5 9.5 Alicyclicaliphatic diurea D Base oil.sup.(*.sup.2) Synthetic hydrocarbon oil E 50 100 100 (mass % of each Synthetic hydrocarbon oil F 100 component based on total Mineral oil G 100 mass of base oil) Mineral oil H Ester oil 50 Phenyl ether oil Additives.sup.(*.sup.3) Polyethylene wax 5.0 5.0 3.0 0.2 9.0 (mass % in grease Oxidized polyethylene wax composition) Polypropylene wax Montan wax Amide wax Worked penetration 300 300 300 300 300 Central thickness of oil film (nm) 340 380 370 111 350 Decision whether to accept or not Traction coefficient 0.062 0.065 0.067 0.068 0.062 Decision whether to accept or not Average life (total revolutions of driving ball) 10.sup.5 140 145 135 86 140 Decision whether to accept or not Overall evaluation

(96) TABLE-US-00005 TABLE 5 Comp. Comp. Comp. Comp. Comp. Comp. Comp. Ex. 1 Ex. 2 Ex. 3 Ex. 4 Ex. 5 Ex. 6 Ex. 7 Thickener.sup.(*.sup.1) Aliphatic diurea A 11.0 10.0 10.0 (mass % in grease Aliphatic diurea B 13.0 composition) Aromatic diurea 22.5 Alicyclicaliphatic diurea C 11.0 Alicyclicaliphatic diurea D 11.0 Base oil.sup.(*.sup.2) Synthetic hydrocarbon oil E 100 100 100 100 100 100 100 (mass % of each Synthetic hydrocarbon oil F component based on Mineral oil G total mass of base oil) Mineral oil H Ester oil Phenyl ether oil Additives.sup.(*.sup.3) Polyethylene wax (mass % in grease Oxidized polyethylene wax composition) Polypropylene wax Montan wax Amide wax Ethylene vinyl acetate 5.0 copolymer wax Zinc oxide 5.0 Worked penetration 300 300 300 300 300 300 300 Central thickness of oil film (nm) 60 70 80 65 60 90 90 Decision whether to accept or not x x x x x x x Traction coefficient 0.080 0.081 0.085 0.078 0.080 0.082 0.084 Decision whether to accept or not x x x x x x x Average life (total revolutions of driving ball) 10.sup.5 40 47 56 47 45 82 95 Decision whether to accept or not x x x x x Overall evaluation x x x x x x x
(*1):
Aliphatic diurea A: A reaction product of two moles of octylamine with one mole of diphenylmethane diisocyanate.
Aliphatic diurea B: A reaction product of a mixture of one mole of octylamine and one mole of octadecylamine with one mole of diphenylmethane diisocyanate.
Aromatic diurea: A reaction product of two moles of para-toluidine with one mole of diphenylmethane diisocyanate.
Alicyclicaliphatic diurea C: A reaction product of a mixture of cyclohexylamine and octadecylamine with one mole of diphenylmethane diisocyanate, where the molar ratio of cyclohexylamine to octadecylamine is 7:1.
Alicyclicaliphatic diurea D: A reaction product of a mixture of cyclohexylamine and octadecylamine with one mole of diphenylmethane diisocyanate, where the molar ratio of cyclohexylamine to octadecylamine is 3:7.
(*2)
Synthetic hydrocarbon oil E: A synthetic hydrocarbon oil with a kinematic viscosity at 40 C. of 30.0 mm.sup.2/s.
Synthetic hydrocarbon oil F: A synthetic hydrocarbon oil with a kinematic viscosity at 40 C. of 63.3 mm.sup.2/s.
Mineral oil G: A mineral oil with a kinematic viscosity at 40 C. of 100 mm.sup.2/s.
Mineral oil H: A mineral oil with a kinematic viscosity at 40 C. of 135 mm.sup.2/s.
Ester oil: A pentaerythritol ester oil with a kinematic viscosity at 40 C. of 30.8 mm.sup.2/s.
Phenyl ether oil: A dialkyl diphenyl ether oil with a kinematic viscosity at 40 C. of 102 mm.sup.2 s.
(*3)

(97) Polyethylene Wax:

(98) having a dropping point of 135 C., an acid value of 0 mgKOH/g, and a weight-average molecular weight of 18.000.

(99) Oxidized Polyethylene Wax:

(100) having a dropping point of 101 C., an acid value of 25 mgKOH/g, and a weight-average molecular weight of 3100.

(101) Polypropylene Wax:

(102) having a dropping point of 145 C., an acid value of 0 mgKOH/g, and a weight-average molecular weight of 3800.

(103) Montan Wax:

(104) having a dropping point of 99 C., an acid value of 11 mgKOH/g, and a saponification value of 112 mgKOH/g.

(105) Amide Wax:

(106) stearamide having a dropping point of 100 C.

(107) Ethylene Vinyl Acetate Copolymer Wax:

(108) having a dropping point of 102 C., an acid value of 20 mgKOH/g, and a weight-average molecular weight of 10,000.