EP1160308A2 - Composition de graisse ayant des propriétés antifloculantes - Google Patents

Composition de graisse ayant des propriétés antifloculantes Download PDF

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Publication number
EP1160308A2
EP1160308A2 EP01304807A EP01304807A EP1160308A2 EP 1160308 A2 EP1160308 A2 EP 1160308A2 EP 01304807 A EP01304807 A EP 01304807A EP 01304807 A EP01304807 A EP 01304807A EP 1160308 A2 EP1160308 A2 EP 1160308A2
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EP
European Patent Office
Prior art keywords
group
carbon atoms
metal
stands
grease composition
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP01304807A
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German (de)
English (en)
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EP1160308A3 (fr
Inventor
Hirotugu Kinoshita
Kiyomi Sakamato
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Eneos Corp
Original Assignee
Nippon Mitsubishi Oil Corp
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Filing date
Publication date
Application filed by Nippon Mitsubishi Oil Corp filed Critical Nippon Mitsubishi Oil Corp
Publication of EP1160308A2 publication Critical patent/EP1160308A2/fr
Publication of EP1160308A3 publication Critical patent/EP1160308A3/fr
Withdrawn legal-status Critical Current

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    • C10M135/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing sulfur, selenium or tellurium
    • C10M135/12—Thio-acids; Thiocyanates; Derivatives thereof
    • C10M135/14—Thio-acids; Thiocyanates; Derivatives thereof having a carbon-to-sulfur double bond
    • C10M135/18—Thio-acids; Thiocyanates; Derivatives thereof having a carbon-to-sulfur double bond thiocarbamic type, e.g. containing the groups
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    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/02—Bearings

Definitions

  • the present invention relates to a grease composition. More particularly, the present invention relates to a grease composition for preventing flaking on a race way of a rolling bearing for electrical components and accessory devices for automotive vehicles, e.g., alternators, electromagnetic clutches for car air conditioners, idle pulleys and electric fan motors.
  • electrical components and accessory devices for automotive vehicles e.g., alternators, electromagnetic clutches for car air conditioners, idle pulleys and electric fan motors.
  • rolling bearings are used, and lubrication of the rolling bearings is achieved mainly by using a grease.
  • JP-A-1-259097, JP-A-3-28299 and JP-A-6-17079 propose grease compositions containing an alkyldiphenyl ether base oil and a urea type thickener.
  • JP-A-3-210394 reports a method for extending flaking life of the rolling bearing by addition of passivation agent.
  • sodium nitrite one of typical passivation agents, is added to a grease containing amine antioxidant for improving the life of the grease at high temperature, sodium nitrite reacts with amine antioxidant to produce N-nitrosoamine which is harmful to human beings.
  • the object of the present invention is to provide a grease composition which has long life even when used at a high temperature, is not harmful to humans and the environment, and can give an extended anti-flaking life to a rolling bearing.
  • a grease composition comprising a lubricant base oil and a metal dithiocarbamate represented by the formula (1): wherein R 1 to R 4 may be the same or different and each stands for a hydrocarbon group having 10 to 20 carbon atoms, and X stands for a metal or a metal-containing group.
  • the grease composition of the present invention contains a lubricant base oil and the specific metal dithiocarbamate represented by the aforementioned formula (1).
  • R 1 to R 4 may be the same or different and each stands for a hydrocarbon group having 10 to 20 carbon atoms. If the number of carbon atoms in these groups is 9 or less, anti-flaking effect at the early stage may be insufficient. The number of the carbon atoms is thus 10 or more, and may preferably be 12 or more. The number of carbon atoms is 20 or less in terms of availability.
  • hydrocarbon groups may include an alkyl group, an alkenyl group, an alkylcycloalkyl group (i.e., an alkyl-substituted cycloalkyl group), an aryl group, an alkylaryl group (i.e., an alkyl-substituted aryl group), and an arylalkyl group (i.e., an aryl-substituted alkyl group).
  • an alkyl group and an alkenyl group are particularly preferable for preventing flaking at early stage.
  • alkyl group may include a decyl group, an undecyl group, a dodecyl group, a tridecyl group, a tetradecyl group, a pentadecyl group, a hexadecyl group, a heptadecyl group, an octadecyl group, a nonadecyl group and an icosyl group, all of which may be straight or branched.
  • alkenyl group may include a decenyl group, an undecenyl group, a dodecenyl group, a tridecenyl group, a tetradecenyl group, a pentadecenyl group, a hexadecenyl group, a heptadecenyl group, an octadecenyl group such as oleyl group, a nonadecenyl group, and an icosenyl group, all of which may be straight or branched.
  • Examples of the alkylcycloalkyl group may include a cyclopentyl group with one or more alkyl substituents each having 1 to 15 carbon atoms (provided that the total number of carbon atoms of all of the alkyl substituents is 5 to 15), a cyclohexyl group with one or more alkyl substituents each having 1 to 14 carbon atoms (provided that the total number of carbon atoms of all of the alkyl substituents is 4 to 14), a cycloheptyl group with one or more alkyl substituents each having 1 to 13 carbon atoms (provided that the total number of carbon atoms of all of the alkyl substituents is 3 to 13).
  • Examples of the aryl group may include a naphthyl group.
  • alkylaryl group may include a phenyl group with one or more alkyl substituents each having 1 to 14 carbon atoms (provided that the total number of carbon atoms of all of the alkyl substituents is 4 to 14).
  • arylalkyl group may include an alkyl group having a phenyl substituent or an alkylaryl substituent.
  • X stands for a metal or a metal-containing group.
  • Examples of the metal may include Mo, Zn, Pb, Sb, Cu and Ni.
  • Zn, Cu and Ni are particularly preferable in terms of an ecological benefit.
  • Examples of the metal-containing group may include the group represented by the following formula (2)
  • Y stands for a metal, and each of Z 1 to Z 4 independently stand for a oxygen atom or a sulfur atom.
  • Y may be, for example, Mo, Zn, Pb, Sb, Cu and Ni, and usually Mo.
  • Examples of the metal dithiocarbamate represented by the formula (1) may include zinc didecyldithiocarbamate, zinc diundecyldithiocarbamate, zinc didodecyldithiocarbamate, zinc ditridecyldithiocarbamate, zinc ditetradecyldithicarbamate, zinc dipentadecyldithiocarbamate, zinc dihexadecyldithiocarbamate, zinc diheptadecyldithiocarbamate, zinc dioctadecyldithiocarbamate, zinc dinonadecyldithiocarbamate, zinc diicosyldithiocarbamate, copper didecyldithiocarbamate, copper diundecyldithiocarbamate, copper didodecyldithiocarbamate, copper ditridecyldithiocarbamate, copper ditetradecyld
  • metal dithiocarbamate represented by the formula (1) for use in the present invention those which are commercially available as a diluted form in a mineral oil or kerosene may be employed.
  • the lower limit of the content of the metal dithiocarbamate in the present grease composition may usually be 0.05 wt%, and preferably 0.25 wt%.
  • the upper limit thereof may usually be 10 wt%, and preferably 5 wt%. If the content is 0.05 wt% or more, sufficient anti-flaking effect may be obtained and shortening of flaking life may be prevented. If the content is more than 10 wt%, the adding amount may fail to measure up to the expected anti-flaking effect, thus not being preferable.
  • the lubricant base oil for use in the present invention may include mineral oil and/or synthetic oil.
  • the mineral oil may be those obtained by conventional method for producing lubricating oils in the field of petroleum refining.
  • the mineral oil may be prepared by distilling crude oil under atmospheric or reduced pressure to obtain lubricant fractions, and purifying the fractions by one or more treatments including solvent deasphalting, solvent extraction, hydrocracking, solvent dewaxing, contact dewaxing, hydrofining, washing with sulfuric acid, and clay purification.
  • the synthetic oil may be a poly- ⁇ -olefin such as polybutene, a 1-octene oligomer, or a 1-decene oligomer, or a hydride of such poly- ⁇ -olefin; a diester such as ditridecyl glutarate, di-2-ethylhexyl adipate, diisodecyl adipate, ditridecyl adipate, or di-3-ethylhexyl sebacate; a polyol ester such as trimethylolpropane caprylate, trimethylolpropane pelargonate, pentaerythritol-2-ethyl hexanoate, or pentaerythritol pelargonate; alkylnaphthalene; alkylbenzene, polyoxyalkylene glycol; polyphenyl ether; dialkyl diphenyl ether; silicone oil or mixtures thereof.
  • the kinematic viscosity of the base oil may usually be 10 to 500 mm 2 /s, and preferably 20 to 300 mm 2 /s at 40°C, but not limited thereto.
  • the grease composition of the present invention may usually contain thickener and other optional additives.
  • thickener may include soap thickeners such as a metal soap and a complex metal soap; bentone, silica gel, a urea compound, a urea-urethane compound, a urethane compound and mixtures thereof.
  • Examples of the soap thickener may include a sodium soap, a calcium soap, an aluminum soap, and a lithium soap.
  • Examples of the urea compound, urea-urethane compound and urethane compound may include a diurea compound, a triurea compound, a tetraurea compound, a polyurea compound (except for the diurea compound, triurea compound and tetraurea compound), a urea-urethane compound, a diurethane compound and mixtures thereof.
  • a diurea compound, urea-urethane compound, diurethane compound and mixtures thereof More preferable are the compound represented by the following formula (3): A-CONH-R 5 -NHCO-B
  • R 5 stands for a divalent hydrocarbon group.
  • a and B may be the same or different, and each stands for -NHR 6 , -NR 7 R 8 OR -OR 9 .
  • R 6 to R 9 may be the same or different and each stands for a hydrocarbon residue having 6 to 20 carbon atoms.
  • R 5 in formula (3) is preferably a divalent hydrocarbon group having 6 to 20, partucularly 6 to 15 carbon atoms .
  • the divalent hydrocarbon group may include a straight or branched alkylene group, a straight or branched alkenylene group, a cycloalkylene group, and an aromatic group.
  • R 5 may include ethylene group, 2,2-dimethyl-4-methylhexylene group and the group represented by the following formulae:
  • Examples of the hydrocarbon residue having 6 to 20 carbon atoms as R 6 to R 9 may include a straight or branched alkyl group, a straight or branched alkenyl group, a cycloalkyl group, an alkylcycloalkyl group, an aryl group, an alkylaryl group, or an arylalkyl group.
  • More Specific examples thereof may include straight or branched alkyl groups such as a hexyl group, a heptyl group, an octyl group, a nonyl group, a decyl group, an undecyl group, a dodecyl group, a tridecyl group, a tetradecyl group, a pentadecyl group, a hexadecyl group, a heptadecyl group, an octadecyl group, a nonadecyl group, or an eicosyl group; a straight or branched alkenyl group such as a hexenyl group, a heptenyl group, an octenyl group, a nonenyl group, a decenyl group, an undecenyl group, a dodecenyl group, a tridecenyl group, a te
  • the diurea compound, urea-urethane compound or diurethane compound may be produced by reacting a diisocyanate represented by the formular OCN-R 5 -NCO, with any of compounds represented by the formulae R 6 NH 2 , R 7 R 8 NH, R 9 OH or mixtures thereof, in a base oil at 10 to 200°C.
  • R 5 to R 9 are the same as R 5 to R 9 in the formula (3).
  • the content of the thickener in the present composition may usually be 2 wt% or more and preferably 3 wt% or more, and usually 30 wt% or less and preferably 25 wt% or less.
  • the grease composition of the present invention may optionally contain a solid lubricant, an extreme pressure agent, an antioxidant, a metal deactivator, an oilness agent, a rust inhibitor, and a viscosity index improver.
  • solid lubricant may include a graphite, fluorinated graphite, polytetrafluoroethylene, molybdenum disulfide, antimony sulfide, alkaline (earth) metal borate, magnesium oxide and zinc oxide.
  • Examples of the extreme pressure agent may include organic zinc compounds such as zinc dialkyldithiophosphate and zinc diaryldithiophosphate; organic molybdenum compounds such as molybdenum dialkyldithiophosphate and molybdenum diaryldithiophosphate; sulfur compounds such as polysulfide, and sulfurized oil and fat; and phosphates and phosphites.
  • antioxidants may include phenol compounds such as 2,6-di-t-butylphenol and 2,6-di-t-butyl-p-cresol; amine compounds such as dialkyldiphenylamine, phenyl- ⁇ -naphthylamine, p-alkylphenyl- ⁇ -naphthylamine; sulfur compounds; and phenothiazine compounds.
  • metal deactivator examples include benzotriazole, benzothiazole and sodium nitrate.
  • oilness agent may include amines such as laurylamine, myristylamine, palmitylamine, stearylamine and oleylamine; higher alcohols such as lauryl alcohol, myristyl alcohol, palmityl alcohol, stearyl alcohol and oleyl alcohol; higher fatty acids such as lauric acid, myristic acid, palmitic acid, stearic acid and oleic acid; higher fatty acid esters such as metyl laurate, methyl myristate, methyl palmitate, metyl stearate and methyl oleate; amides such as laurylamide, myristylamide, palmitylamide, stearylamide and oleylamide; and oil and fats.
  • amines such as laurylamine, myristylamine, palmitylamine, stearylamine and oleylamine
  • higher alcohols such as lauryl alcohol, myristyl alcohol, palmityl alcohol, stearyl alcohol and
  • rust inhibitor may include neutral or over-based metal sulfonates of petrol type or synthetic oil type such as a neutral or over-based calcium sulfonate, a neutral or over-based barium sulfonate, and a neutral or over-based zinc sulfonate; metal soaps; polyvalent alcohol partial esters such as sorbitan fatty acid ester; amines; phosphoric acid; and phosphates.
  • examples of the viscosity index improver may include a polymethacryalte, a polyisobutylene and a polystylene.
  • the objective grease composition may usually be produced by adding the metal dithiocarbamate to the base oil, stirring the mixture and optionally passing the mixture through a roll mill.
  • the present grease composition may be used for lubricating a rolling bearing, such as electrical components and accessory devices for automotive vehicles, e.g., alternators, electromagnetic clutches for car air conditioners, idle pulleys and electric fan motors.
  • the lubrication may be achieved by filling the rolling bearing with the present grease composition.
  • the present grease composition contains the specific metal dithiocarbamate, it can exhibit an excellent anti-flaking property in rolling bearings such as electrical components and accessory devices for automotive vehicles, e.g., alternators, electromagnetic clutches for car air conditioners, idle pulleys and electric fan motors, resulting in extension of the life of the rolling bearings.
  • rolling bearings such as electrical components and accessory devices for automotive vehicles, e.g., alternators, electromagnetic clutches for car air conditioners, idle pulleys and electric fan motors, resulting in extension of the life of the rolling bearings.
  • Diphenylmethane-4,4'-diisocyanate was dissolved under heat in base oil shown in Table 1. To this mixture were added the same base oil containing amines shown in Table 1 that had been dissolved therein under heat. The gel substance was obtained, to which the metal dithiocarbamate and other additives were further added. The mixture was stirred and then passed through a roll mill, to obtain grease compositions of Examples 1 and 2 and Comparative Examples 1 to 3.
  • a single-line deep groove ball bearing fitted with a contact rubber seal having an inner diameter of 12 mm, an outer diameter of 37 mm and a width of 12 mm was filled with 2.0 g of the grease and attached to an engine.
  • the rotation of the engine was quickly accelerated and decelerated from 1000 rpm to 6000 rpm and from 6000 rpm to 1000 rpm (rotation of outer ring of the bearing was from 1900 rpm to 11300 rpm, and from 11300 rpm to 1900 rpm), to continuously rotate the bearing at bearing load of 190 kgf.
  • the running life time was measured until occurrence of flaking in a bearing inner ring race way and fluctuation.
  • Example Comparative Example 1 2 1 2 3 Base oil (wt%) Dialkyldiphenyl ether ) 80.0 - 82.0 80.0 80.0 Pentaerythritol ester ) - 77.0 - - - Poly- ⁇ -olefin ) - - - - - Thickener (wt%) 13.0 17.0 13.0 13.0 13.0 Thickener (molar ratio) Diphenylmethane-4,4'-diisocyanate 5 5 1 1 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 Cyclo
  • the present grease composition can give a longer anti-flaking life than the grease composition of Comparative Example 1 that does not contain the metal dithiocarbamate and than the grease compositions of Comparative Examples 2 and 3 that contains metal dithiocarbamates which have hydrocarbon groups having less than 10 carbon atoms.

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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)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • Lubricants (AREA)
EP01304807A 2000-06-02 2001-05-31 Composition de graisse ayant des propriétés antifloculantes Withdrawn EP1160308A3 (fr)

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JP2000166152A JP4620219B2 (ja) 2000-06-02 2000-06-02 グリ−ス組成物

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EP1498472A3 (fr) * 2003-07-04 2005-02-23 Koyo Seiko Co., Ltd. Composition de graisse lubrifiante pour un palier à roulement
CN102031192A (zh) * 2010-12-30 2011-04-27 上海锦海特种润滑油厂 一种防锈洗涤两用润滑剂及其制备方法
EP2829597A4 (fr) * 2012-03-22 2015-03-18 Jtekt Corp Composition graisseuse et dispositif de roulement
EP2913385A4 (fr) * 2012-10-26 2016-05-25 Kyodo Yushi Composition de graissage
EP3694951B1 (fr) * 2017-10-13 2023-12-13 Merck Patent GmbH Matériau électroluminescent semiconducteur

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ES2431044T5 (es) * 2000-11-27 2022-05-27 Procter & Gamble Método de lavado de vajillas
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JP3537811B2 (ja) * 2002-03-29 2004-06-14 独立行政法人 科学技術振興機構 単層カーボンナノチューブの製造方法
JP4283491B2 (ja) * 2002-04-26 2009-06-24 新日本石油株式会社 グリース組成物
JP4883743B2 (ja) 2002-08-02 2012-02-22 Ｎｔｎ株式会社 グリース組成物および該グリース組成物封入軸受
JP4254225B2 (ja) * 2002-12-17 2009-04-15 日本精工株式会社 スタータ用一方向クラッチ装置
JP2005003197A (ja) * 2003-05-19 2005-01-06 Nsk Ltd 一方向クラッチ内蔵型回転伝達装置
WO2005083044A1 (fr) * 2004-02-27 2005-09-09 Kyodo Yushi Co., Ltd. Composition de graisse pour joint à vitesse constante et joint à vitesse constante
JP5258080B2 (ja) * 2007-05-30 2013-08-07 協同油脂株式会社 等速ジョイント用グリース組成物及びそれを封入した等速ジョイント
JP5188248B2 (ja) * 2008-04-11 2013-04-24 出光興産株式会社 グリース組成物およびそのグリース組成物を用いた直動装置
JP5330773B2 (ja) * 2008-07-07 2013-10-30 昭和シェル石油株式会社 樹脂潤滑用グリース組成物
JP5330774B2 (ja) * 2008-07-07 2013-10-30 昭和シェル石油株式会社 樹脂潤滑用グリース組成物
KR101652545B1 (ko) * 2008-09-30 2016-08-30 쉘 인터내셔날 리써취 마트샤피지 비.브이. 그리스 조성물
JP5214649B2 (ja) * 2010-02-26 2013-06-19 協同油脂株式会社 アンギュラ玉軸受を使用したハブユニット軸受用グリース組成物及びハブユニット軸受
JP2019026806A (ja) * 2017-08-03 2019-02-21 Ｊｘｔｇエネルギー株式会社 グリース組成物
CN108517246B (zh) * 2018-05-17 2021-09-03 北美防锈技术（上海）有限公司 一种具有协同作用的环保型防锈油
JP7751585B2 (ja) * 2020-08-12 2025-10-08 株式会社ジェイテクト グリース組成物および転がり軸受
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Publication number Priority date Publication date Assignee Title
EP1498472A3 (fr) * 2003-07-04 2005-02-23 Koyo Seiko Co., Ltd. Composition de graisse lubrifiante pour un palier à roulement
US7491683B2 (en) 2003-07-04 2009-02-17 Jtekt Corporation Grease composition for rolling bearing and rolling bearing using the same
CN102031192A (zh) * 2010-12-30 2011-04-27 上海锦海特种润滑油厂 一种防锈洗涤两用润滑剂及其制备方法
EP2829597A4 (fr) * 2012-03-22 2015-03-18 Jtekt Corp Composition graisseuse et dispositif de roulement
EP2913385A4 (fr) * 2012-10-26 2016-05-25 Kyodo Yushi Composition de graissage
US9719045B2 (en) 2012-10-26 2017-08-01 Kyodo Yushi Co., Ltd. Grease composition
EP3694951B1 (fr) * 2017-10-13 2023-12-13 Merck Patent GmbH Matériau électroluminescent semiconducteur

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JP2001342483A (ja) 2001-12-14
EP1160308A3 (fr) 2002-12-04
US20020013232A1 (en) 2002-01-31

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