EP2631284B1 - Grease composition - Google Patents

Grease composition Download PDF

Info

Publication number
EP2631284B1
EP2631284B1 EP11834414.2A EP11834414A EP2631284B1 EP 2631284 B1 EP2631284 B1 EP 2631284B1 EP 11834414 A EP11834414 A EP 11834414A EP 2631284 B1 EP2631284 B1 EP 2631284B1
Authority
EP
European Patent Office
Prior art keywords
grease composition
oil
base oil
group
synthetic oils
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.)
Active
Application number
EP11834414.2A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP2631284A1 (en
EP2631284A4 (en
Inventor
Yutaka Imai
Ryo Aida
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.)
Kyodo Yushi Co Ltd
Original Assignee
Kyodo Yushi Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Kyodo Yushi Co Ltd filed Critical Kyodo Yushi Co Ltd
Publication of EP2631284A1 publication Critical patent/EP2631284A1/en
Publication of EP2631284A4 publication Critical patent/EP2631284A4/en
Application granted granted Critical
Publication of EP2631284B1 publication Critical patent/EP2631284B1/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00Lubricating 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
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00Lubricating 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
    • C10M169/06Mixtures of thickeners and additives
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2203/00Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/1006Petroleum or coal fractions, e.g. tars, solvents, bitumen used as base material
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2203/00Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/102Aliphatic fractions
    • C10M2203/1025Aliphatic fractions used as base material
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/003Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions used as base material
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/028Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms
    • C10M2205/0285Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms used as base material
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/121Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
    • C10M2207/123Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms polycarboxylic
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125Carboxylix 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
    • C10M2207/127Carboxylix 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 polycarboxylic
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/287Partial esters
    • C10M2207/289Partial esters containing free hydroxy groups
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/10Amides of carbonic or haloformic acids
    • C10M2215/102Ureas; Semicarbazides; Allophanates
    • C10M2215/1026Ureas; Semicarbazides; Allophanates used as thickening material
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/044Sulfonic acids, Derivatives thereof, e.g. neutral salts
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2020/00Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01Physico-chemical properties
    • C10N2020/011Cloud point
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2020/00Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01Physico-chemical properties
    • C10N2020/02Viscosity; Viscosity index
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/02Pour-point; Viscosity index
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/12Inhibition of corrosion, e.g. anti-rust agents or anti-corrosives
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00Specified use or application for which the lubricating composition is intended
    • C10N2040/02Bearings
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00Specified use or application for which the lubricating composition is intended
    • C10N2040/14Electric or magnetic purposes
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00Specified use or application for which the lubricating composition is intended
    • C10N2040/40Generators or electric motors in oil or gas winning field
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10Semi-solids; greasy

Definitions

  • the present invention relates to a grease composition and its use for rolling bearings of the automotive electrical equipment and automotive auxiliaries.
  • diurea based greases For the rolling bearings of the automotive electrical equipment and automotive auxiliaries, diurea based greases have been widely used, especially from the viewpoint of the heat resistance. In the diurea based greases, aromatic diurea compounds are frequently used on the grounds of their durability under high temperatures.
  • the aromatic diurea compounds should be added in larger amounts than other diurea compounds to render the same hardness to a resultant grease composition.
  • the resistance to stirring of the resultant grease becomes too high to satisfy low torque performance.
  • JP 6-17079 A proposes a grease composition characterized by comprising a base oil which contains an ether type synthetic oil in an amount of more than 50 mass%; and at least one diurea compound represented by the following general formula as a gelling agent of one essential component: R 2 -NHCONH-R 3 wherein R 1 is a bivalent aromatic hydrocarbon group having 6 to 15 carbon atoms; and R 2 and R 3 , which may be the same or different represent cyclohexyl group, a cyclohexyl-derived group having 7 to 12 carbon atoms, or an alkyl group having 8 to 20 carbon atoms, with the content of cyclohexyl group or the derived groups thereof, as expressed by formula: [((the number of the cyclohexyl groups or the derived groups thereof) / (the number of the cyclohexyl groups or the derived groups thereof + the number of the al
  • the phenyl ether oil used as the base oil has a pour point of about -30°C, so that the low temperature properties are not so satisfactory. This will increase the torque at low temperatures.
  • JP 2008-239706 A proposes a grease composition characterized by comprising a base oil which contains an ester type synthetic oil; and a thickener represented by the following general formula as one essential component: R 1 -NHCONH-R 2 -NHCONH-R 3 wherein R 2 is a bivalent aromatic hydrocarbon group having 6 to 15 carbon atoms; and R 1 and R 3 , which may be the same or different represent cyclohexyl group or an alkyl group having 8 to 22 carbon atoms, with the content of cyclohexyl group, as expressed by formula: [((the number of the cyclohexyl groups) / (the number of the cyclohexyl groups + the number of the alkyl groups)) x 100] being 60 to 95%.
  • the ester type synthetic oil is subjected to hydrolysis when water penetrates from the outside and is mixed in, whereby the resultant acid component will unfavorably involve a risk of rust development.
  • EP-A-1 953 213 describes a grease composition for a constant velocity joint, said composition comprising the following components (a) to (g):
  • the synthetic ester oil (b) should be present in an amount of 5 to 40% by mass, based on the total mass of the composition.
  • An object of the invention is to provide a low torque grease composition having excellent rust preventing properties.
  • the low torque performance can be ensured under the circumstances of low temperature by using a low pour point synthetic hydrocarbon oil in an amount of 30 mass% or more of the base oil.
  • a low pour point synthetic hydrocarbon oil in an amount of 30 mass% or more of the base oil.
  • an aliphatic diurea is used alone or in combination with an alicyclic diurea to obtain a grease composition having a proper hardness even though the total amount of thickener is decreased.
  • the inventors of the invention have thus solved the above-mentioned problems by choosing and combining a particular base oil, a thickener and a rust inhibitor. Namely, the invention provides the following grease composition:
  • the grease composition of the invention can exhibit low torque performance within a wide temperature range, thereby improving fuel economy to contribute to reduction of CO 2 .
  • the grease composition of the invention also shows excellent rust preventing properties. Further, the resistance to evaporation of the grease composition according to the invention is also excellent.
  • the base oil used in the invention comprises a synthetic hydrocarbon oil and a highly purified mineral oil with a pour point of -35°C or less.
  • the ratio by mass of the synthetic hydrocarbon oil to the highly purified mineral oil with a pour point of -35°C or less is 100:0 to 30:70.
  • the content of the synthetic hydrocarbon oil in the base oil is 30 mass% or more, the low torque performance can be satisfied.
  • Examples of the synthetic hydrocarbon oil include poly- ⁇ -olefin, polybutene, ethylene- ⁇ -olefin oligomer and the like. Particularly, poly- ⁇ -olefin is preferred.
  • the highly purified mineral oil used in the invention is referred to as a mineral oil provided with a pour point lower than the pour points (about -5 to -20°C) of unpurified mineral oils by carrying out a dewaxing step to control the wax components from precipitating at low temperatures.
  • the highly purified mineral oil with a pour point of -35°C or less can be used without any adverse effect on the low torque performance at low temperatures and any problem in the resistance to evaporation.
  • the base oil may preferably have a kinematic viscosity at 40°C of 80 to 150 mm 2 /s, more preferably 85 to 140 mm 2 /s, and most preferably 90 to 130 mm 2 /s.
  • the kinematic viscosity at 40°C of the base oil exceeds 150 mm 2 /s, the grease viscosity becomes too high to satisfy the low torque performance.
  • the kinematic viscosity at 40°C of the base oil is less than 80 mm 2 /s, the resistance to evaporation will unfavorably be lowered although the requirement of low torque performance can be satisfied.
  • the synthetic hydrocarbon oil may comprise the one having a kinematic viscosity at 40°C of 300 mm 2 /s or more.
  • the kinematic viscosity of the base oil can be adjusted within a predetermined range, with the low torque performance at low temperatures being satisfied without impairing the resistance to evaporation.
  • the highly purified oil may comprise the one having a kinematic viscosity at 40°C of 80 to 130 mm 2 /s, more preferably 80 to 110 mm 2 /s.
  • the low torque performance can be satisfied, and at the same time, the resistance to evaporation can be improved.
  • the pour point of the synthetic hydrocarbon oil may preferably be -35°C or less. In this case, the low torque performance at low temperatures is satisfactory.
  • the grease composition optionally further comprises other base oil components that can be used in combination with the synthetic hydrocarbon oil
  • the other base oil components are selected from the group consisting of ether type synthetic oils such as alkyldiphenyl ethers, polyglycol type synthetic oils such as polypropylene glycol, silicone type synthetic oils, and fluorine type synthetic oils.
  • Ester type synthetic oils are not desirable because hydrolysis may be caused when water is mixed into the grease from the outside, as previously mentioned.
  • the ester type synthetic oils have pour points of as high as about -30°C, so that the torque will become high at low temperatures.
  • the polyglycol type synthetic oils, silicone type synthetic oils and fluorine type synthetic oils are poor in the lubricating properties and expensive.
  • Examples of the thickener commonly used in the grease compositions include metallic soaps containing lithium, sodium or the like, and non-soaps such as Benton, silica gel, diurea compounds, fluorine-containing thickeners such as polytetrafluoroethylene and the like.
  • the metallic soaps are not satisfactory in terms of the heat resistance, that is, the lubricating life of bearings at high temperatures; Benton and silica gel have poor water resistance; and the fluorine-containing thickeners are considerably expensive and lacking in versatility although the heat resistance is satisfactory.
  • the grease composition of the invention comprises a thickener represented by the above formula (1).
  • the content of alkyl groups in the above-mentioned formula (1) expressed as [(the number of moles of the alkyl groups) / (the number of moles of the alkyl groups + the number of moles of the cyclohexyl groups)] x 100 is 30 to 100%.
  • the content of alkyl groups is less than 30%, the amount of thickener will increase to unfavorably fail to achieve the low torque performance.
  • the amount of thickener (B) in the grease composition according to the invention may be preferably 10 to 20 mass%, and more preferably 12 to 17 mass%, from the viewpoint of low torque performance.
  • the grease composition of the invention comprises as the rust inhibitor an alkenylsuccinic anhydride.
  • the above-mentioned rust inhibitor can work to disperse water content even if water permeates into the grease from the outside.
  • the grease composition of the invention can further comprise an organic zink sulfonate.
  • the organic zinc sulfonate is a zinc salt of sulfonic acid having an organic lipophilic group.
  • the sulfonic acid includes petroleum sulfonic acids obtainable by sulfonation from an aromatic hydrocarbon moiety in the lubricating oil distillate or a petroleum fraction with a high boiling point, synthetic sulfonic acids such as dinonylnaphthalene sulfonic acid, heavy alkylbenzene sulfonic acid and the like.
  • an organic zinc sulfonate represented by the following formula (2) is preferable.
  • [R 4 - SO 3 ] 2 Zn (2) (wherein R 4 is an alkyl group, alkenyl group, alkylnaphthyl group, dialkylnaphthyl group, alkylphenyl group or a residue from the high-boiling petroleum fraction, and the above-mentioned alkyl or alkenyl group may be a straight-chain or branched group having 2 to 22 carbon atoms.)
  • zinc dioctyl naphthalenesulfonate zinc dinonyl naphthalene sulfonate, zinc didecyl naphthalenesulfonate, zinc petroleum sulfonate, zinc salt of highly basic alkylbenzenesulfonate and the like can be used.
  • zinc dinonyl naphthalenesulfonate is most preferable.
  • alkenylsuccinic anhydride alkenylsuccinic anhydrides having an alkenyl group with 6 to 18 carbon atoms can preferably be used.
  • the alkenylsuccinic anhydrides having an alkenyl group with 10 to 15 carbon atoms are preferable.
  • the amount of rust inhibitor (C) in the grease composition according to the invention may be preferably 0.1 to 3 mass%, and more preferably 0.5 to 2 mass% in order to ensure the rust preventing properties under the circumstances where salt water may permeate.
  • the grease composition of the invention may further comprise additives generally used in the conventional grease compositions.
  • the additives include an antioxidant such as amine-based and phenol-based antioxidants; an inorganic passivator such as sodium nitrite or the like; a rust inhibitor such as amine-based and carboxylate-based rust inhibitors; a metallic corrosion inhibitor such as benzotriazole or the like, an oiliness improver such as fatty acids, fatty acid esters, phosphates and the like; a phosphorus-containing, sulfur-containing or organic metal-containing antiwear agent or extreme-pressure agent; and a solid lubricant such as oxidized metal salts, molybdenum disulfide or the like.
  • an antioxidant such as amine-based and phenol-based antioxidants
  • an inorganic passivator such as sodium nitrite or the like
  • a rust inhibitor such as amine-based and carboxylate-based rust inhibitors
  • a metallic corrosion inhibitor such as benzotriazole or
  • the grease composition of the invention can be used for rolling bearings, in particular the rolling bearings for automotive electrical equipment and automotive auxiliaries such as the electromagnetic clutch for car air conditioners, center pulley, idler pulley, tension pulley, alternator, water pump and the like.
  • automotive auxiliaries such as the electromagnetic clutch for car air conditioners, center pulley, idler pulley, tension pulley, alternator, water pump and the like.
  • Example 6 is within the claimed invention.
  • the low torque performance was determined in accordance with a low temperature torque test defined by JIS K2220 18.
  • the rust preventing properties were evaluated in accordance with a rust prevention test for bearing in accordance with ASTM D1743-73 specifications.
  • the low torque performance and the rust preventing properties were both within the acceptable levels.
  • the low torque performance was unacceptable in Comparative Example 1 where the content of the synthetic hydrocarbon oil was 30 mass% or less.
  • the low torque performance was unacceptable in Comparative Examples 2 and 3 where the mineral oil not highly purified was contained.
  • the low torque performance was also unacceptable in Comparative Examples 4 and 5 where the content of alkyl groups was 30% or less.
  • the grease composition according to the invention found to be excellent in terms of both low torque performance and rust preventing properties.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)
EP11834414.2A 2010-10-20 2011-10-20 Grease composition Active EP2631284B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2010235372A JP5766425B2 (ja) 2010-10-20 2010-10-20 グリース組成物
PCT/JP2011/074109 WO2012053575A1 (ja) 2010-10-20 2011-10-20 グリース組成物

Publications (3)

Publication Number Publication Date
EP2631284A1 EP2631284A1 (en) 2013-08-28
EP2631284A4 EP2631284A4 (en) 2015-07-08
EP2631284B1 true EP2631284B1 (en) 2021-01-06

Family

ID=45975285

Family Applications (1)

Application Number Title Priority Date Filing Date
EP11834414.2A Active EP2631284B1 (en) 2010-10-20 2011-10-20 Grease composition

Country Status (5)

Country Link
EP (1) EP2631284B1 (zh)
JP (1) JP5766425B2 (zh)
KR (1) KR20130073977A (zh)
CN (1) CN103210070B (zh)
WO (1) WO2012053575A1 (zh)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5988376B2 (ja) * 2012-12-03 2016-09-07 協同油脂株式会社 鉄道車両の主電動機軸受用グリース組成物及び軸受
JP6268642B2 (ja) 2014-03-12 2018-01-31 協同油脂株式会社 グリース組成物及びグリース封入車輪用軸受
JP6845633B2 (ja) * 2016-08-04 2021-03-17 協同油脂株式会社 グリース組成物
CN107118137B (zh) * 2017-06-26 2021-10-29 锦州康泰润滑油添加剂股份有限公司 一种油品防锈剂重烷基苯磺酸锌及其制备方法
JP7280800B2 (ja) * 2019-10-16 2023-05-24 協同油脂株式会社 車載電装品の減速機部用グリース組成物
FR3129949B1 (fr) * 2021-12-06 2024-08-30 Totalenergies Marketing Services Graisses lubrifiantes conductrices.

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008050834A1 (fr) * 2006-10-26 2008-05-02 Kyodo Yushi Co., Ltd. Composition de graisse et arbre
EP1953213A1 (en) * 2005-11-22 2008-08-06 Kyodo Yushi Co., Ltd. Grease composition for constant velocity joint and constant velocity joint
JP2009299846A (ja) * 2008-06-16 2009-12-24 Nsk Ltd 鉄鋼圧延機用転がり軸受

Family Cites Families (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS617079A (ja) 1984-06-21 1986-01-13 Toyo Seikan Kaisha Ltd 溶接缶胴の製造方法
JP2979274B2 (ja) * 1992-06-29 1999-11-15 日本精工株式会社 高速ころがり軸受用グリース組成物
JP4102627B2 (ja) * 2002-09-13 2008-06-18 株式会社ジェイテクト 転がり軸受
JP4832724B2 (ja) * 2004-04-02 2011-12-07 Ntn株式会社 グリース組成物およびグリース封入軸受
JP2006300211A (ja) * 2005-04-20 2006-11-02 Ntn Corp 一方向クラッチ内蔵型回転伝達装置
JP2007106858A (ja) * 2005-10-13 2007-04-26 Nsk Ltd 掘削機用グリース組成物及び掘削機用転がり軸受
JP2008143979A (ja) * 2006-12-07 2008-06-26 Nsk Ltd グリース組成物及び転がり軸受
JP2008239706A (ja) * 2007-03-26 2008-10-09 Kyodo Yushi Co Ltd グリース組成物及び軸受
JP5467723B2 (ja) * 2008-01-23 2014-04-09 協同油脂株式会社 潤滑剤組成物及び機械部材
JP5467727B2 (ja) * 2008-02-22 2014-04-09 協同油脂株式会社 グリース組成物及び軸受
JP2010048389A (ja) * 2008-08-25 2010-03-04 Nsk Ltd 転がり軸受
JP5664890B2 (ja) * 2009-10-15 2015-02-04 協同油脂株式会社 風力発電機軸受用グリース組成物

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1953213A1 (en) * 2005-11-22 2008-08-06 Kyodo Yushi Co., Ltd. Grease composition for constant velocity joint and constant velocity joint
WO2008050834A1 (fr) * 2006-10-26 2008-05-02 Kyodo Yushi Co., Ltd. Composition de graisse et arbre
JP2009299846A (ja) * 2008-06-16 2009-12-24 Nsk Ltd 鉄鋼圧延機用転がり軸受

Also Published As

Publication number Publication date
CN103210070A (zh) 2013-07-17
EP2631284A1 (en) 2013-08-28
JP2012087221A (ja) 2012-05-10
CN103210070B (zh) 2015-04-08
KR20130073977A (ko) 2013-07-03
EP2631284A4 (en) 2015-07-08
JP5766425B2 (ja) 2015-08-19
WO2012053575A1 (ja) 2012-04-26

Similar Documents

Publication Publication Date Title
CA2777188C (en) Grease composition for bearing of wind power generator
EP1930400B1 (en) Lubricant composition
US9012386B2 (en) Grease composition for hub unit bearing employing an angular contact ball bearing and hub unit bearing
EP2687584B1 (en) Grease composition
EP2631284B1 (en) Grease composition
JP5707589B2 (ja) 潤滑剤組成物および潤滑液組成物
EP2264132B1 (en) Grease composition and bearings
EP2913385B1 (en) Grease composition
JP5738712B2 (ja) グリース組成物
JP3370829B2 (ja) 潤滑グリース組成物
WO2011102037A1 (ja) 無段変速機用潤滑油組成物
JP2001247888A (ja) グリース組成物
US20190177645A1 (en) Grease composition
RU2633350C1 (ru) Смазка пластичная антифрикционная высокотемпературная водостойкая
US11053451B2 (en) Lubricant composition for a speed reducer, and speed reducer
EP3178910B1 (en) Grease composition
JP4008992B2 (ja) 焼結含油軸受油組成物
JP2018203999A (ja) 転がり軸受用グリース組成物
JP4198391B2 (ja) 潤滑剤組成物
WO2024210159A1 (ja) 消費電力が低くかつ自己ロック性に優れるグリース組成物
JPH11343492A (ja) 潤滑剤組成物
US20170313953A1 (en) Compositions comprising an alternative to di-isotridecyl adipate
JP2016020481A (ja) グリース組成物

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 20130516

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

DAX Request for extension of the european patent (deleted)
RA4 Supplementary search report drawn up and despatched (corrected)

Effective date: 20150610

RIC1 Information provided on ipc code assigned before grant

Ipc: C10N 20/02 20060101ALI20150603BHEP

Ipc: C10M 169/00 20060101ALI20150603BHEP

Ipc: C10N 30/12 20060101ALI20150603BHEP

Ipc: C10N 20/00 20060101ALI20150603BHEP

Ipc: C10N 40/02 20060101ALI20150603BHEP

Ipc: C10N 10/04 20060101ALI20150603BHEP

Ipc: C10N 30/02 20060101ALI20150603BHEP

Ipc: C10M 169/06 20060101AFI20150603BHEP

Ipc: C10N 50/10 20060101ALI20150603BHEP

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: EXAMINATION IS IN PROGRESS

17Q First examination report despatched

Effective date: 20180221

REG Reference to a national code

Ref country code: DE

Ref legal event code: R079

Ref document number: 602011069909

Country of ref document: DE

Free format text: PREVIOUS MAIN CLASS: C10M0169000000

Ipc: C10M0169060000

GRAP Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOSNIGR1

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: GRANT OF PATENT IS INTENDED

RIC1 Information provided on ipc code assigned before grant

Ipc: C10M 169/06 20060101AFI20200622BHEP

Ipc: C10N 30/02 20060101ALI20200622BHEP

Ipc: C10N 40/00 20060101ALI20200622BHEP

Ipc: C10N 50/10 20060101ALI20200622BHEP

Ipc: C10N 20/00 20060101ALI20200622BHEP

Ipc: C10N 40/02 20060101ALI20200622BHEP

Ipc: C10N 20/02 20060101ALI20200622BHEP

Ipc: C10M 169/00 20060101ALI20200622BHEP

Ipc: C10N 30/12 20060101ALI20200622BHEP

Ipc: C10N 40/14 20060101ALI20200622BHEP

Ipc: C10N 30/06 20060101ALI20200622BHEP

Ipc: C10N 10/04 20060101ALI20200622BHEP

INTG Intention to grant announced

Effective date: 20200716

RIN1 Information on inventor provided before grant (corrected)

Inventor name: IMAI YUTAKA

Inventor name: AIDA RYO

GRAS Grant fee paid

Free format text: ORIGINAL CODE: EPIDOSNIGR3

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: THE PATENT HAS BEEN GRANTED

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

REG Reference to a national code

Ref country code: GB

Ref legal event code: FG4D

REG Reference to a national code

Ref country code: AT

Ref legal event code: REF

Ref document number: 1352374

Country of ref document: AT

Kind code of ref document: T

Effective date: 20210115

Ref country code: CH

Ref legal event code: EP

REG Reference to a national code

Ref country code: DE

Ref legal event code: R096

Ref document number: 602011069909

Country of ref document: DE

REG Reference to a national code

Ref country code: IE

Ref legal event code: FG4D

REG Reference to a national code

Ref country code: NL

Ref legal event code: MP

Effective date: 20210106

REG Reference to a national code

Ref country code: AT

Ref legal event code: MK05

Ref document number: 1352374

Country of ref document: AT

Kind code of ref document: T

Effective date: 20210106

REG Reference to a national code

Ref country code: LT

Ref legal event code: MG9D

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210407

Ref country code: HR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210106

Ref country code: FI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210106

Ref country code: LT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210106

Ref country code: PT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210506

Ref country code: NL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210106

Ref country code: NO

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210406

Ref country code: BG

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210406

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210106

Ref country code: LV

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210106

Ref country code: PL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210106

Ref country code: RS

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210106

Ref country code: AT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210106

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IS

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210506

REG Reference to a national code

Ref country code: DE

Ref legal event code: R097

Ref document number: 602011069909

Country of ref document: DE

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SM

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210106

Ref country code: CZ

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210106

Ref country code: EE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210106

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: RO

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210106

Ref country code: SK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210106

Ref country code: DK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210106

Ref country code: ES

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210106

26N No opposition filed

Effective date: 20211007

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: AL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210106

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210106

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210106

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IS

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210506

REG Reference to a national code

Ref country code: BE

Ref legal event code: MM

Effective date: 20211031

GBPC Gb: european patent ceased through non-payment of renewal fee

Effective date: 20211020

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MC

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210106

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LU

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20211020

Ref country code: GB

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20211020

Ref country code: BE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20211031

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LI

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20211031

Ref country code: CH

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20211031

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20211020

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: HU

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT; INVALID AB INITIO

Effective date: 20111020

Ref country code: CY

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210106

P01 Opt-out of the competence of the unified patent court (upc) registered

Effective date: 20230509

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 20230830

Year of fee payment: 13

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210106

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: TR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210106

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20210106

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 20240909

Year of fee payment: 14