EP0998544B1 - Grease composition for a constant velocity joint - Google Patents

Grease composition for a constant velocity joint Download PDF

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Publication number
EP0998544B1
EP0998544B1 EP98945164A EP98945164A EP0998544B1 EP 0998544 B1 EP0998544 B1 EP 0998544B1 EP 98945164 A EP98945164 A EP 98945164A EP 98945164 A EP98945164 A EP 98945164A EP 0998544 B1 EP0998544 B1 EP 0998544B1
Authority
EP
European Patent Office
Prior art keywords
grease
grease composition
urea
thiosulphate
constant velocity
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.)
Expired - Lifetime
Application number
EP98945164A
Other languages
German (de)
French (fr)
Other versions
EP0998544A1 (en
Inventor
Takahiro Ozaki
Tomoo Munakata
Tsutomu Yoshida
Ryuichi Masumori
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.)
Shell Internationale Research Maatschappij BV
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Shell Internationale Research Maatschappij BV
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/06—Mixtures of thickeners and additives
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M115/00—Lubricating compositions characterised by the thickener being a non-macromolecular organic compound other than a carboxylic acid or salt thereof
    • C10M115/08—Lubricating compositions characterised by the thickener being a non-macromolecular organic compound other than a carboxylic acid or salt thereof containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M119/00—Lubricating compositions characterised by the thickener being a macromolecular compound
    • C10M119/24—Lubricating compositions characterised by the thickener being a macromolecular compound containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/22—Compounds containing sulfur, selenium or tellurium
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • 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
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06—Metal compounds
    • C10M2201/065—Sulfides; Selenides; Tellurides
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06—Metal compounds
    • C10M2201/065—Sulfides; Selenides; Tellurides
    • C10M2201/066—Molybdenum sulfide
    • C—CHEMISTRY; METALLURGY
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/08—Inorganic acids or salts thereof
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
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    • C10M2201/081—Inorganic acids or salts thereof containing halogen
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/08—Inorganic acids or salts thereof
    • C10M2201/082—Inorganic acids or salts thereof containing nitrogen
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    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/08—Inorganic acids or salts thereof
    • C10M2201/084—Inorganic acids or salts thereof containing sulfur, selenium or tellurium
    • C—CHEMISTRY; METALLURGY
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    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/026—Butene
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    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/02—Hydroxy compounds
    • C10M2207/023—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings
    • C10M2207/026—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings with tertiary alkyl groups
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/006—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions used as thickening agents
    • C—CHEMISTRY; METALLURGY
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    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/026—Amines, e.g. polyalkylene polyamines; Quaternary amines used as thickening agents
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    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10M2215/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
    • C10M2215/064—Di- and triaryl amines
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    • C10M2215/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
    • C10M2215/064—Di- and triaryl amines
    • C10M2215/065—Phenyl-Naphthyl amines
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    • C10M2215/08—Amides
    • C10M2215/0813—Amides used as thickening agents
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    • C10M2215/10—Amides of carbonic or haloformic acids
    • C10M2215/1013—Amides of carbonic or haloformic acids used as thickening agents
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    • C10M2215/1026—Ureas; Semicarbazides; Allophanates used as thickening material
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    • C10M2215/12—Partial amides of polycarboxylic acids
    • C10M2215/121—Partial amides of polycarboxylic acids used as thickening agents
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
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    • C10M2215/22—Heterocyclic nitrogen compounds
    • C10M2215/2206—Heterocyclic nitrogen compounds used as thickening agents
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    • C10M2215/2275—Phthalocyanines used as thickening agents
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    • C10M2217/04—Macromolecular compounds from nitrogen-containing monomers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2217/044—Polyamides
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    • C10M2217/04—Macromolecular compounds from nitrogen-containing monomers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2217/045—Polyureas; Polyurethanes
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    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/04—Groups 2 or 12
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    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/12—Groups 6 or 16

Definitions

  • the present invention relates to the use of grease compositions in a constant velocity joint also referred to as CVJ.
  • Grease lubrication of CVJ's is extremely harsh since it is carried out under conditions of friction under high surface pressures where slipping and rolling over in reciprocating movement are intermixed.
  • the present invention relates to the use of a grease composition for lubricating a constant velocity joint having an extremely long-lived durability and to prevent the occurrence of abnormal wear and flaking.
  • CVJ's in automobiles are employed in front-wheel drive vehicles and four-wheel drive vehicles, as well as rear-wheel drive vehicles, and demand tends to increase. As automobiles achieve higher speeds, higher outputs and lighter weights, CVJ's become smaller, whilst sustaining higher torques and being applied at higher speeds. Therefore, the grease must meet increasing performance specifications.
  • CVJ's can be categorised as fixed joint or plunging joint depending on the mechanism. Conditions are extremely harsh for fixed joints since these are generally used for wheels and are employed at high angles and under high surface pressure.
  • CVJ greases contain lithium soap as thickener and additives such as sulphur/phosphorus-based extreme pressure agents and molybdenum disulphide. Recently, urea-based greases containing various extreme pressure agents have become more common. These have outstanding heat-resisting properties.
  • JP-A Japanese Laid-Open Patent Application
  • H 6-57284 (1994) discloses a grease composition for a constant velocity joint in which a urea grease contains, as essential constituents, (A) a molybdenum dialkyldithiocarbamide sulphide, (B) an extreme pressure additive comprising a specific zinc dithiophosphate compound, and (C) an epoxy-modified aliphatic acid ester or an epoxy-modified aliphatic acid glyceride.
  • compositions still suffer from flaking which stems from metal surface fatigue caused by roll-over slipping friction in complex reciprocating movements of tne inner and outer wheel channels and balls as well as cages and balls in a CVJ mechanism.
  • compositions for use in cutting and grinding operations.
  • the compositions contain a mixture of a metal thiosulfate and a metal phosphate to impart both extreme pressure and antiwear properties to a base lubricant.
  • US-A-3,505,223 describes a lubricating composition comprising a major amount of an organic liquid lubricating oil or grease and an extreme pressure reducing amount of a metal thiosulphate.
  • CVJ-producing manufacturers and grease-supplying manufacturers are trying to predict flaking in CVJ with the help of frictional wear tests such as the four-ball EP tests described in ASTM D2596.
  • durability in CVJ's is concerned appropriate greases cannot be selected using the test apparatuses mentioned above. This is thought to be due to the complexity of the lubrication conditions. Therefore, the performance in terms of the flaking life, state of wear and the like is evaluated using a bench test apparatus in which an actual CVJ is used.
  • the aim of the present invention is to provide a constant velocity joint grease composition whereby CVJ flaking can be prevented.
  • the present invention further relates to the use of a grease composition for lubricating a constant velocity joint, which grease composition comprises base oil and urea-based thickener, which composition further contains from 0.05 to 30% by weight of metal thiosulphate, based on weight of base oil and urea-based thickener.
  • the base oil used in the present embodiment can be a mineral oil or a synthetic oil such as an ester oil, ether oil or hydrocarbon oil, or an oil mixed from these.
  • the base oil is a mineral oil.
  • urea-based thickener Any urea-based thickener can be used.
  • urea-based thickeners include diurea, triurea and tetraurea.
  • various thickeners containing urea compounds such as urea-urethane compounds and urea-imido compounds.
  • the metal thiosulphate used in the present invention can contain any metal that is capable of forming a metal thiosulphate salt.
  • Typical examples are lithium, sodium, potassium, manganese, calcium, barium, strontium, titanium, zirconium, cadmium, zinc, nickel, cobalt, copper, iron, magnesium, lead, tin, silver, or a mixture of these.
  • a useful class of metal thiosulphate is represented by the following formula where R represents a hydrocarbon radical containing 1 to 30 carbon atoms, M is a metal capable of forming a metal thiosulphate salt and n is the valence of M.
  • R represents a hydrocarbon radical containing 1 to 30 carbon atoms
  • M is a metal capable of forming a metal thiosulphate salt
  • n is the valence of M.
  • Examples of this class of metal thiosulphates are sodium ethyl thiosulphate, potassium benzyl thiosulphate and barium isoamyl thiosulphate.
  • the compounds can be prepared by reacting an alkyl halide with sodium thiosulphate.
  • the metal thiosulphate used in the present invention is sodium thiosulphate.
  • the sodium thiosulphate is Na 2 S 2 O 3 (anhydrous), Na 2 S 2 O 3 .5H 2 O (pentahydrate) or a mixture of these.
  • the amount of sodium thiosulphate added is from 0.05 to 30 percent by weight, and preferably from 0.2 to 20 percent by weight based on weight of base oil and urea-based thickener, more preferably 0.2 to 10% by weight, more preferably 0.2 to 8% by weight, most preferably 0.5 to 6% by weight. If the amount is less than 0.05 percent by weight, the flaking-preventing effect is insufficient. If the amount is more than 30 percent by weight, there is no further increase in the effect.
  • composition of the present invention can further contain one or more known additives such as phenol-based and amine-based antioxidants, organic molybdenum compounds, molybdenum disulphide, sulphur-modified fats and oils, sulphur-modified olefins, zinc dithiophosphate, thiophosphate, phosphite, phosphate, and polysulphide, and other such extreme pressure/anti-wear agents, polybutenes, polymethacrylates and other such viscosity enhancers.
  • additives such as phenol-based and amine-based antioxidants, organic molybdenum compounds, molybdenum disulphide, sulphur-modified fats and oils, sulphur-modified olefins, zinc dithiophosphate, thiophosphate, phosphite, phosphate, and polysulphide, and other such extreme pressure/anti-wear agents, polybutenes, polymethacrylates and other such viscosity
  • Greases according to the invention and comparative examples were obtained using the formulations shown in Table 1 and Table 2 by adding the additives to a base grease and processing in a three-roll mill.
  • the compositions of the base greases are given below.
  • the base oil was purified mineral oil with a viscosity at 100°C of 15mm 2 /S.
  • a grease was obtained by reacting diphenylmethane-4,4'-diisocyanate (295.2 g) and octylamine (304.8g) in a base oil (5,400 g), and uniformly dispersing the resulting urea compound.
  • the urea compound content was 10 percent by weight.
  • a grease was obtained by reacting diphenylmethane-4,4'-diisocyanate (334.2 g), stearylamine (345.6 g) and ethylenediamine (40.2 g) in a base oil (5,280 g), and uniformly dispersing the resulting urea compound.
  • the urea compound content was 12 percent by weight.
  • a grease was obtained by dissolving lithium 12-hydroxystearate (540 g) in a base oil (5,460 g), and uniformly dispersing.
  • the lithium soap content was 9 percent by weight.
  • the resulting greases were subjected to durability testing on mounts using actual CVJ's, and the degree of flaking was checked.
  • fusion load (N) was determined using the four-ball EP test specified in ASTM D2596. The results are collated in Tables 1 to 4.
  • the grease composition for a constant velocity joint of the present invention has outstanding extreme pressure properties, and provides more effective flaking prevention properties than do conventional greases. This effect improves the durability of constant velocity joints.

Abstract

A grease composition for a constant velocity joint, characterised in that it contains from 0.05 to 30 percent by weight of sodium thiosulphate with respect to a base oil and urea-based thickener.

Description

  • The present invention relates to the use of grease compositions in a constant velocity joint also referred to as CVJ. Grease lubrication of CVJ's is extremely harsh since it is carried out under conditions of friction under high surface pressures where slipping and rolling over in reciprocating movement are intermixed. The present invention relates to the use of a grease composition for lubricating a constant velocity joint having an extremely long-lived durability and to prevent the occurrence of abnormal wear and flaking.
  • CVJ's in automobiles are employed in front-wheel drive vehicles and four-wheel drive vehicles, as well as rear-wheel drive vehicles, and demand tends to increase. As automobiles achieve higher speeds, higher outputs and lighter weights, CVJ's become smaller, whilst sustaining higher torques and being applied at higher speeds. Therefore, the grease must meet increasing performance specifications. CVJ's can be categorised as fixed joint or plunging joint depending on the mechanism. Conditions are extremely harsh for fixed joints since these are generally used for wheels and are employed at high angles and under high surface pressure.
  • Usually, CVJ greases contain lithium soap as thickener and additives such as sulphur/phosphorus-based extreme pressure agents and molybdenum disulphide. Recently, urea-based greases containing various extreme pressure agents have become more common. These have outstanding heat-resisting properties.
  • JP-A (Japanese Laid-Open Patent Application) H 6-57284 (1994) discloses a grease composition for a constant velocity joint in which a urea grease contains, as essential constituents, (A) a molybdenum dialkyldithiocarbamide sulphide, (B) an extreme pressure additive comprising a specific zinc dithiophosphate compound, and (C) an epoxy-modified aliphatic acid ester or an epoxy-modified aliphatic acid glyceride.
  • Further urea greases have been described in JP-B (Examined Japanese Patent Document) H 4-34590 (1992), JP-A H 6-57283 (1994), JP-A H 6-100878 (1994), JP-A H 7-197072 (1995) and JP-A H 8-41485 (1996), and US-A-4,840,740, US-A-5,160,645 and US-A-5,449,471. These documents teach to add an organic molybdenum compound to a base grease together with yet other additives (such as zinc dithiophosphate) to reduce frictional wear and, as a result, prevent flaking.
  • However, these compositions still suffer from flaking which stems from metal surface fatigue caused by roll-over slipping friction in complex reciprocating movements of tne inner and outer wheel channels and balls as well as cages and balls in a CVJ mechanism.
  • In US-A-4,923,625 grease compositions are described for use in cutting and grinding operations. The compositions contain a mixture of a metal thiosulfate and a metal phosphate to impart both extreme pressure and antiwear properties to a base lubricant.
  • US-A-3,505,223 describes a lubricating composition comprising a major amount of an organic liquid lubricating oil or grease and an extreme pressure reducing amount of a metal thiosulphate.
  • CVJ-producing manufacturers and grease-supplying manufacturers are trying to predict flaking in CVJ with the help of frictional wear tests such as the four-ball EP tests described in ASTM D2596. Where durability in CVJ's is concerned appropriate greases cannot be selected using the test apparatuses mentioned above.
    This is thought to be due to the complexity of the lubrication conditions. Therefore, the performance in terms of the flaking life, state of wear and the like is evaluated using a bench test apparatus in which an actual CVJ is used.
  • The fact that substances which exhibit outstanding results in general frictional wear tests do not necessarily prevent CVJ flaking or have long durability, makes it difficult to develop CVJ flaking prevention technology.
  • The aim of the present invention is to provide a constant velocity joint grease composition whereby CVJ flaking can be prevented.
  • The present invention further relates to the use of a grease composition for lubricating a constant velocity joint, which grease composition comprises base oil and urea-based thickener, which composition further contains from 0.05 to 30% by weight of metal thiosulphate, based on weight of base oil and urea-based thickener.
  • The base oil used in the present embodiment can be a mineral oil or a synthetic oil such as an ester oil, ether oil or hydrocarbon oil, or an oil mixed from these. Preferably, the base oil is a mineral oil.
  • Any urea-based thickener can be used. Examples of urea-based thickeners include diurea, triurea and tetraurea. Further, it is also possible to use various thickeners containing urea compounds such as urea-urethane compounds and urea-imido compounds.
  • The metal thiosulphate used in the present invention, can contain any metal that is capable of forming a metal thiosulphate salt. Typical examples are lithium, sodium, potassium, manganese, calcium, barium, strontium, titanium, zirconium, cadmium, zinc, nickel, cobalt, copper, iron, magnesium, lead, tin, silver, or a mixture of these.
  • A useful class of metal thiosulphate is represented by the following formula
    Figure 00050001
    where R represents a hydrocarbon radical containing 1 to 30 carbon atoms, M is a metal capable of forming a metal thiosulphate salt and n is the valence of M. Examples of this class of metal thiosulphates are sodium ethyl thiosulphate, potassium benzyl thiosulphate and barium isoamyl thiosulphate. The compounds can be prepared by reacting an alkyl halide with sodium thiosulphate.
  • Preferably, the metal thiosulphate used in the present invention is sodium thiosulphate. Most preferably, the sodium thiosulphate is Na2S2O3 (anhydrous), Na2S2O3.5H2O (pentahydrate) or a mixture of these. Further, it is possible to use commercial additives containing sodium thiosulphate, such as "Desilube 88," (trade mark) Desilube Technology, Inc. USA.
  • The amount of sodium thiosulphate added is from 0.05 to 30 percent by weight, and preferably from 0.2 to 20 percent by weight based on weight of base oil and urea-based thickener, more preferably 0.2 to 10% by weight, more preferably 0.2 to 8% by weight, most preferably 0.5 to 6% by weight. If the amount is less than 0.05 percent by weight, the flaking-preventing effect is insufficient. If the amount is more than 30 percent by weight, there is no further increase in the effect.
  • The composition of the present invention can further contain one or more known additives such as phenol-based and amine-based antioxidants, organic molybdenum compounds, molybdenum disulphide, sulphur-modified fats and oils, sulphur-modified olefins, zinc dithiophosphate, thiophosphate, phosphite, phosphate, and polysulphide, and other such extreme pressure/anti-wear agents, polybutenes, polymethacrylates and other such viscosity enhancers.
  • Greases according to the invention and comparative examples were obtained using the formulations shown in Table 1 and Table 2 by adding the additives to a base grease and processing in a three-roll mill. The compositions of the base greases are given below. The base oil was purified mineral oil with a viscosity at 100°C of 15mm2/S.
    • I. Diurea grease
  • A grease was obtained by reacting diphenylmethane-4,4'-diisocyanate (295.2 g) and octylamine (304.8g) in a base oil (5,400 g), and uniformly dispersing the resulting urea compound. The urea compound content was 10 percent by weight.
    • II. Tetraurea grease
  • A grease was obtained by reacting diphenylmethane-4,4'-diisocyanate (334.2 g), stearylamine (345.6 g) and ethylenediamine (40.2 g) in a base oil (5,280 g), and uniformly dispersing the resulting urea compound. The urea compound content was 12 percent by weight.
    • III. Lithium soap grease
  • A grease was obtained by dissolving lithium 12-hydroxystearate (540 g) in a base oil (5,460 g), and uniformly dispersing. The lithium soap content was 9 percent by weight.
  • The resulting greases were subjected to durability testing on mounts using actual CVJ's, and the degree of flaking was checked.
    • Test conditions
  • Rotational speed 1,400 rpm
    Load torque 294 N m
    Joint angle 6 deg
    Joint type Burfield joint
  • Further, the fusion load (N) was determined using the four-ball EP test specified in ASTM D2596. The results are collated in Tables 1 to 4.
  • It should be noted that, in the tables, *1 to 7 and ** are as follows.
    *1 "Desilube 88" (trade mark, made by Desilube Technology Inc.) is an inorganic additive containing sodium thiosulphate.
    *2 "Moliban A" (trade mark, made by the Vanderbilt company) is molybdenum dithiocarbamate.
    *3 "Sakura Lube 600" (trade mark, made by Asahi Denka) is molybdenum dithiocarbanate.
    *4 "Sakura Lube 300" (trade mark, made by Asahi Denka) is molybdenum dithiophosphate.
    *5 "Lubrizol 1395" (trade mark, made by the Lubrizol company) is zinc dithiophosphate.
    *6 "Anguramoru 33" (trade mark, made by the Lubrizol company) is a sulphur-modified olefin.
    *7 Iruga Lube TPPT" (trade mark, made by the Ciba-Geigy company) is triphenylphosphorothionate.
    **For the degree of flaking, the condition after 12,600,000 revolutions, and the condition after 25,200,000 revolutions of the CVJ was observed and evaluated as follows.
  • ⋄ No flaking
  • o Minor flaking
  • Δ Moderate flaking
  • x Extensive flaking
    Embodiment 1 2 3 4
    Composition wt% Base grease Diurea grease 97 95 97
    Tetraurea grease 95
    Additives Na2S2O3 (anhydrous) 3 5 5
    Na2S2O3.5H2O 3
    "Desilube 88"   *1
       Total 100 100 100 100
    Test results Four-ball EP test Fusion load (N) 6076 7840 7840 6076
    Degree of flaking ** By 12,600,000 revolutions ⋄ ⋄ ⋄ o
    By 25,200,000 revolutions o ⋄ ⋄ Δ
    Embodiment 5 6 7 8
    Composition wt% Base grease Diurea grease 97 99
    Tetraurea grease 97 97
    Additives Na2S2O3 (anhydrous)
    Na2S2O3.5H2O "Desilube 88"   *1 3
    3 3 1
       Total 100 100 100 100
    Test results Four-ball EP test Fusion load (N) 6076 >7840 7840 6076
    Degree of flaking ** By 12,600,000 revolutions o ⋄ ⋄ o
    By 25,200,000 revolutions Δ ⋄ ⋄ Δ
    Embodiment 1 2 3 4
    Composition wt% Base grease Diurea grease 93
    Tetraurea grease
    Lithium grease 97 97 97
    Additives Na2S2O3 (anhydrous) 3
    Na2S2O3 5H2O 3
    "Desilube 88"   *1 3
    "Moliban A" *2 3
    "Sakura Lube 600"   *3
    "Sakura Lube 300"   *4 2
    "Lubrizol 1395"   *5
    "Anguramoru 33"   *6 1
    "Icuga Lube TPPT"   *7
    Molybdenum disulphide
       Total 100 100 100 100
    Test results Four-ball EP Fusion load (N) test 6076 3920 6076 3087
    Degree of flaking ** By 12,600,000 revolutions x Δ Δ x
    By 25,200,000 revolutions - x Δ -
    Figure 00120001
  • As is clear from the results shown in Tables 1 to 4, the grease composition for a constant velocity joint of the present invention has outstanding extreme pressure properties, and provides more effective flaking prevention properties than do conventional greases. This effect improves the durability of constant velocity joints.

Claims (5)

  1. Use of a grease composition for lubricating a constant velocity joint, which grease composition comprises base oil, metal thiosulphate and thickener, characterised in that the thickener is a urea-based thickener and that the composition further contains from 0.05 to 30% by weight of metal thiosulphate, based on weight of base oil and urea-based thickener.
  2. Use of a grease composition according to claim 1, in which the grease composition contains from 0.2 to 20% by weight of metal thiosulphate.
  3. Use of a grease composition according to claim 1 or 2, in which the base oil is a mineral oil.
  4. Use of a grease composition according to any one of claims 1 to 3, in which grease composition the metal thiosulphate is sodium thiosulphate.
  5. Use of a grease composition according to any one of claims 1 to 4, in which grease composition the urea-based thickener is selected from diurea, triurea and tetraurea.
EP98945164A 1997-07-24 1998-07-23 Grease composition for a constant velocity joint Expired - Lifetime EP0998544B1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP21417197A JP3812995B2 (en) 1997-07-24 1997-07-24 Grease composition for constant velocity joints
JP21417197 1997-07-24
PCT/EP1998/004983 WO1999005240A1 (en) 1997-07-24 1998-07-23 Grease composition for a constant velocity joint

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EP0998544A1 EP0998544A1 (en) 2000-05-10
EP0998544B1 true EP0998544B1 (en) 2003-07-02

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JP4634585B2 (en) 2000-08-10 2011-02-16 昭和シェル石油株式会社 Grease composition with improved rust and wear resistance
US8153053B2 (en) 2002-11-21 2012-04-10 Diamet Corporation Method for forming compact from powder and sintered product
JP4769456B2 (en) 2004-12-27 2011-09-07 昭和シェル石油株式会社 Urea-based lubricating grease composition, rolling bearing and electric power steering device
JP5225354B2 (en) * 2010-10-18 2013-07-03 昭和シェル石油株式会社 Grease composition with improved rust and wear resistance

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US3505223A (en) * 1967-03-30 1970-04-07 Ethyl Corp Lubricant compositions
US4986923A (en) * 1989-06-27 1991-01-22 Amoco Corporation Front-wheel drive grease with synergistic sulfate and carbonate additive system
US4923625A (en) * 1989-09-28 1990-05-08 Desilube Technology, Inc. Lubricant compositions
US5354485A (en) * 1993-03-26 1994-10-11 The Lubrizol Corporation Lubricating compositions, greases, aqueous fluids containing organic ammonium thiosulfates

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KR100503108B1 (en) 2005-07-25
CN1260825A (en) 2000-07-19
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KR20010022118A (en) 2001-03-15

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