US20160075965A1 - Lubricant composition based on metal nanoparticles - Google Patents

Lubricant composition based on metal nanoparticles Download PDF

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US20160075965A1
US20160075965A1 US14/784,466 US201414784466A US2016075965A1 US 20160075965 A1 US20160075965 A1 US 20160075965A1 US 201414784466 A US201414784466 A US 201414784466A US 2016075965 A1 US2016075965 A1 US 2016075965A1
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lubricant composition
dispersant
metal nanoparticles
weight
composition according
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Alain Bouffet
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TotalEnergies Marketing Services SA
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Total Marketing Services SA
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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
    • C10M161/00—Lubricating compositions characterised by the additive being a mixture of a macromolecular compound and a non-macromolecular compound, each of these compounds being essential
    • 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
    • C10M141/00—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential
    • C10M141/06—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential at least one of them being an organic nitrogen-containing compound
    • 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
    • C10M171/00—Lubricating compositions characterised by purely physical criteria, e.g. containing as base-material, thickener or additive, ingredients which are characterised exclusively by their numerically specified physical properties, i.e. containing ingredients which are physically well-defined but for which the chemical nature is either unspecified or only very vaguely indicated
    • C10M171/06—Particles of special shape or size
    • 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
    • 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
    • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/102—Aliphatic fractions
    • C10M2203/1025—Aliphatic fractions used as base material
    • 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
    • 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
    • C10M2205/028—Organic 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
    • C—CHEMISTRY; METALLURGY
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/028—Organic 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
    • C10M2205/0285—Organic 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
    • 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
    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/04—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing aromatic monomers, e.g. styrene
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/02—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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28—Esters
    • C10M2207/2805—Esters used as base material
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    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28—Esters
    • C10M2207/283—Esters of polyhydroxy compounds
    • C10M2207/2835—Esters of polyhydroxy compounds used as base material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/08—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate type
    • C10M2209/084—Acrylate; Methacrylate
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • 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
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/28—Amides; Imides
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/04—Groups 2 or 12
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/06—Groups 3 or 13
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/08—Groups 4 or 14
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/10—Groups 5 or 15
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/12—Groups 6 or 16
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/14—Group 7
    • C—CHEMISTRY; METALLURGY
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    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/16—Groups 8, 9, or 10
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01—Physico-chemical properties
    • C10N2020/02—Viscosity; Viscosity index
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01—Physico-chemical properties
    • C10N2020/055—Particles related characteristics
    • C10N2020/06—Particles of special shape or size
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/04—Oil-bath; Gear-boxes; Automatic transmissions; Traction drives
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/04—Oil-bath; Gear-boxes; Automatic transmissions; Traction drives
    • C10N2040/044—Oil-bath; Gear-boxes; Automatic transmissions; Traction drives for manual transmissions
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/015—Dispersions of solid lubricants

Definitions

  • the present invention is applicable to the field of lubricants, and more particularly to the field of lubricants for motor vehicles, in particular to the field of lubricants for motor vehicle transmission components.
  • the invention relates to a lubricant composition comprising metal nanoparticles. More particularly, the invention relates to a lubricant composition comprising a dispersant with a high weight-average molecular weight and metal nanoparticles.
  • the lubricant composition according to the invention simultaneously has good stability and good anti-flaking properties.
  • the present invention also relates to a method for reducing the flaking of a mechanical part utilizing this lubricant composition.
  • the present invention also relates to a composition of the additive-concentrate type comprising a dispersant with a high weight-average molecular weight and metal nanoparticles.
  • Motor vehicle transmission components operate under a high load and high speeds.
  • the oils for these transmission components must therefore be particularly efficient at protecting parts against wear and fatigue, and in particular protect the gear teeth against the flaking phenomenon.
  • the phenomenon of wear corresponds to the abrasion and fretting of metal at the surface during friction between the moving parts.
  • the flaking phenomenon differs from the phenomenon of wear. It corresponds to a degradation of the parts due to fatigue and is produced after a long period of ageing, preceding visible deterioration. It is known that this phenomenon starts by the initiation of cracks at a certain depth under the surface, these cracks propagate, and when normal cracks are created at the surface, flakes suddenly break off. This phenomenon is prevented by reducing the contact stresses by means of an appropriate geometry of the parts, and by reducing friction, while avoiding adhesion. The lubricant is involved in this prevention process, mainly due to the physico-chemical reactivity of its additives.
  • the sulphur-, phosphorus-, phosphorus/sulphur-, or borate-containing anti-wear and extreme-pressure additives are known to give the transmission oils protection properties against flaking.
  • the other additives present in the lubricant can also have a positive or negative impact on the propagation of the cracks inside the parts and therefore on the flaking phenomenon.
  • the friction level is not adapted to the geometry of the parts, wear occurs on the cone-ring assembly.
  • the friction level can be adjusted by adding friction modifiers in these oils for gear boxes.
  • anti-wear, extreme-pressure additives and friction modifiers can co-exist, all having an action at the surface of the parts and potentially an effect on both the friction level and the flaking phenomenon.
  • lubricant compositions comprising friction modifier compounds of the organomolybdenum type with organophosphorus- and/or organosulphur- and/or organophosphorus/sulphur-containing anti-wear and extreme-pressure compounds, in particular in order to improve the anti-wear properties of these oils.
  • Other compounds have been described as possibly being useful in the lubrication of mechanical parts, in particular of the parts of an engine.
  • WO 2007/035626 describes a lubricant composition comprising metal nanoparticles, in particular based on lithium, potassium, sodium, copper, magnesium, calcium, barium or mixtures thereof.
  • Document US2011/0152142 A1 discloses a composition comprising at least one base oil, at least one dispersant and nanoparticles of metal hydroxides in the form of crystals. These compositions are used for lubricating combustion engines and for neutralizing the acids formed during combustion.
  • Document US2009/0203563 describes a method for manufacturing an ovebased or neutral detergent. This method utilizes a surfactant and an organic medium with a composition comprising at least one base oil, at least one dispersant and nanoparticles of metal hydroxides in the form of crystals.
  • Document EP 1 953 196 describes a dispersion of metal nanoparticles, in particular of metal oxides based on zinc, zirconium, cerium, titanium, aluminium, indium or tin in a organic solvent and in the presence of a polymeric dispersant of PIBSA (polyisobutenyl succinic anhydride) type.
  • PIBSA polyisobutenyl succinic anhydride
  • this document does not relate to the field of lubricant compositions and in particular discloses no lubricant composition comprising at least one base oil and metal nanoparticles.
  • the organic solvents mentioned in this document have no lubricant properties. Furthermore, they have a flash point of less than 100° C. which makes them incompatible with use in lubricant applications in which the implementation temperature is greater than or equal to 100° C.
  • no indication is given in this document of any anti-flaking properties of mechanical parts, in particular vis-à-vis the transmission components of a motor vehicle.
  • a lubricant composition in particular for motor vehicles, which is both stable and makes it possible to reduce, or even eliminate the flaking phenomenon, in particular in transmission components, and more particularly in gearboxes. It would also be desirable to have available a lubricant composition, in particular for motor vehicles having good anti-flaking properties while retaining satisfactory friction properties.
  • a subject of the invention is thus a lubricant composition
  • a lubricant composition comprising at least one base oil, at least one dispersant having a weight-average molecular weight greater than or equal to 2000 Daltons and metal nanoparticles in a content by weight ranging from 0.01 to 2% with respect to the total weight of the lubricant composition, said metal nanoparticles being concentric polyhedrons with a multilayer structure or in sheets.
  • the weight-average molecular weight of the dispersant is assessed according to the standard ASTM D5296.
  • the Applicant found that the presence of a dispersant having a weight-average molecular weight greater than or equal to 2000 Daltons in a lubricant composition comprising at least one base oil and metal nanoparticles makes it possible both to improve the stability of the lubricant composition, and to give said composition very good anti-flaking properties.
  • the present invention makes it possible to formulate lubricant compositions comprising a reduced content of metal nanoparticles and having, however, remarkable anti-flaking properties.
  • the risk of residual deposition of metal nanoparticles on mechanical parts, and more particularly on transmission components of motor vehicles is significantly reduced or even eliminated.
  • the lubricant compositions according to the invention have an improved storage stability as well as a viscosity that does not vary, or only very slightly.
  • the lubricant compositions according to the invention retain satisfactory friction properties.
  • the lubricant composition essentially consists of at least one base oil, at least one dispersant having a weight-average molecular weight greater than or equal to 2000 Daltons and at least a content by weight of metal nanoparticles ranging from 0.01 to 2% with respect to the total weight of the lubricant composition.
  • the invention also relates to a transmission oil comprising a lubricant composition as defined above.
  • the invention also relates to the use of a lubricant composition as defined above for the lubrication of gearboxes or axles, preferentially of the gearboxes of motor vehicles, advantageously for the lubrication of manual gearboxes.
  • the invention also relates to the use of a lubricant composition as defined above for reducing the flaking of a mechanical part, preferentially of a transmission component, more preferentially of a gearbox, even more preferentially of a manual gearbox.
  • the invention also relates to a process for reducing the flaking of a mechanical part, preferentially of a transmission component, advantageously of a gearbox or of an axle, comprising at least bringing the mechanical part into contact with a lubricant composition as defined above.
  • the invention also relates to a composition of the additive-concentrate type comprising at least one dispersant having a weight-average molecular weight greater than or equal to 2000 Daltons and tungsten disulphide nanoparticles.
  • FIG. 1 shows a closed-loop power circulation bench comprising a simulated gearbox ( 111 ), an electric motor ( 112 ), a torque meter ( 113 ), a torque producing device ( 114 ), a gearbox comprising the torque to be tested ( 115 ), a differential ( 116 ), a output shaft ( 117 ), an input shaft ( 118 ), a system for detecting the formation of flakes ( 119 ), fifth gear ( 120 ), reverse gear ( 121 ), fourth gear ( 122 ), third gear ( 123 ), second gear ( 124 ), first gear ( 125 ) and a drive belt ( 126 ).
  • FIG. 2 is a photograph of a gearbox housing after 600 h of testing on a closed-loop power circulation bench with a composition according to the invention.
  • FIG. 3 is a photograph of a gearbox housing after 400 h of testing on a closed-loop power circulation bench with a composition not according to the invention.
  • the lubricant composition according to the invention comprises metal nanoparticles in a content by weight ranging from 0.01 to 2% with respect to the total weight of the lubricant composition.
  • metal nanoparticles is meant in particular metal particles, generally solid, the average size of which is less than or equal to 600 nm.
  • the metal nanoparticles are constituted by at least 80% by mass of at least one metal, or by at least 80% by mass of at least one metal alloy or by at least 80% by mass of at least one metal, in particular transition metal, chalcogenide with respect to the total mass of the nanoparticle.
  • the metal nanoparticles are constituted by at least 90% by mass of at least one metal, or by at least 90% by mass of at least one metal alloy or by at least 90% by mass of at least one metal, in particular transition metal, chalcogenide with respect to the total mass of the nanoparticle.
  • the metal nanoparticles are constituted by at least 99% by mass of at least one metal, or by at least 99% by mass of at least one metal alloy or by at least 99% by mass of at least one metal, in particular transition metal, chalcogenide with respect to the total mass of the nanoparticle, the remaining 1% being constituted by impurities.
  • the metal of which the metal nanoparticle is constituted can be selected from the group formed by tungsten, molybdenum, zirconium, hafnium, platinum, rhenium, titanium, tantalum, niobium, zinc, cerium, aluminium, indium and tin.
  • the metal nanoparticles can have the form of spheres, lamellas, fibres, tubes, and fullerene-type structures.
  • M is selected from the group formed by tungsten, molybdenum, zirconium, hafnium, platinum, rhenium, titanium, tantalum and niobium. More preferably, M is selected from the group formed by molybdenum and tungsten. Even more preferably, M is tungsten.
  • X is selected from the group formed by oxygen, sulphur, selenium and tellurium.
  • X is selected from sulphur or tellurium. Even more preferably, X is sulphur.
  • the metal nanoparticles according to the invention are selected from the group formed by MoS 2 , MoSe 2 , MoTe 2 , WS 2 , WSe 2 , ZrS 2 , ZrSe 2 , HfS 2 , HfSe 2 , PtS 2 , ReS 2 , ReSe 2 , TiS 3 , ZrS 3 , ZrSe 3 , HfS 3 , HfSe 3 , TiS 2 , TaS 2 , TaSe 2 , NbS 2 , NbSe 2 and NbTe 2 .
  • the metal nanoparticles according to the invention are selected from the group formed by WS 2 , WSe 2 , MoS 2 and MoSe 2 , preferentially WS 2 and MoS 2 , preferentially WS 2 .
  • the nanoparticles according to the invention advantageously have a fullerene-type structure.
  • fullerene denotes a closed convex polyhedron nanostructure, composed of carbon atoms.
  • the fullerenes are similar to graphite, composed of sheets of linked hexagonal rings, but they contain pentagonal, and sometimes heptagonal rings, which prevent the structure from being flat.
  • fullerene-type structures were not limited to the carbon-containing materials, but was capable of being produced in all the nanoparticles of materials in the form of sheets, in particular in the case of the nanoparticles comprising chalcogens and transition metals.
  • These structures are analogous to that of the carbon fullerenes and are called inorganic fullerenes or fullerene-type structures (or “Inorganic Fullerene-like materials”, also denoted “IF”).
  • the fullerene-type structures are described in particular by Tenne, R., Margulis, L., Genut M. Hodes, G. Nature 1992, 360, 444.
  • the document EP 0580 019 describes in particular these structures and their synthesis process.
  • the metal nanoparticles are closed structures, of the spherical type, more or less perfect depending on the synthesis processes used.
  • the nanoparticles according to the invention are concentric polyhedrons with a multilayer or sheet structure. This is referred to as an “onion” or “nested polyhedron” structure.
  • concentric polyhedron having a multilayer or sheet structure is meant more particularly substantially spherical polyhedrons, the different layers of which constitute several spheres having the same centre.
  • the multilayer or sheet structure of the nanoparticles according to the invention can in particular be determined by transmission electron microscopy (TEM).
  • TEM transmission electron microscopy
  • the metal nanoparticles are multilayer metal nanoparticles comprising from 2 to 500 layers, preferably from 20 to 200 layers, advantageously from 20 to 100 layers.
  • the number of layers of the nanoparticles according to the invention can in particular be determined by transmission electron microscopy.
  • the average size of the metal nanoparticles according to the invention ranges from 5 to 600 nm, preferably from 20 to 400 nm, advantageously from 50 to 200 nm.
  • the size of the metal nanoparticles according to the invention can be determined using images obtained by transmission electron microscopy or by high resolution transmission electron microscopy. It is possible to determine the average size of the particles from measurement of the size of at least 50 solid particles visualized on transmission electron microscopy photographs.
  • the median value of the distribution histogram of the measured sizes of the solid particles is the average size of the solid particles used in the lubricant composition according to the invention.
  • the average diameter of the primary metal nanoparticles according to the invention ranges from 10 to 100 nm, preferably from 30 to 70 nm.
  • the average diameter of the nanoparticles according to the invention can in particular be determined by transmission electron microscopy.
  • the content by weight of metal nanoparticles ranges from 0.05 to 2%, preferably from 0.1 to 1%, advantageously from 0.1 to 0.5% with respect to the total weight of the lubricant composition.
  • NanoLub Gear Oil Concentrate marketed by the company Nanomaterials
  • the product NanoLub Gear Oil Concentrate marketed by the company Nanomaterials
  • the lubricant composition according to the invention comprises at least one dispersant having a weight-average molecular weight greater than or equal to 2000 Daltons.
  • the weight-average molecular weight of the dispersant is assessed according to the standard ASTM D5296.
  • dispersant within the meaning of the present invention, is meant more particularly any compound which ensures the maintenance in suspension of the metal nanoparticles.
  • the dispersant can be selected from the compounds comprising at least one succinimide group, the polyolefins, the olefin copolymers (OCP), the copolymers comprising at least one styrene unit, the polyacrylates or their derivatives.
  • OCP olefin copolymers
  • derivatives is meant any compound comprising at least one group or a polymer chain as defined above.
  • the dispersant according to the invention is selected from the compounds comprising at least one succinimide group.
  • the dispersant can be selected from the compounds comprising at least one substituted succinimide group or the compounds comprising at least two substituted succinimide groups, the succinimide groups being linked at their vertex bearing a nitrogen atom by a polyamine group.
  • substituted succinimide group within the meaning of the present invention, is meant a succinimide group at least one of the carbon-containing vertices of which is substituted with a hydrocarbon-containing group comprising from 8 to 400 carbon atoms.
  • the dispersant is selected from the polyisobutylene succinimide-polyamines
  • the dispersant is a substituted succinimide of formula (I) or a substituted succinimide of formula (II):
  • the dispersant is a substituted succinimide of formula (I) or a substituted succinimide of formula (II) in which R 2 represents a polyisobutylene group. Even more advantageously, the dispersant is a substituted succinimide of formula (II) in which R 2 represents a polyisobutylene group. Even more advantageously, the dispersant is a substituted succinimide of formula (II) in which:
  • the dispersant according to the invention has a weight-average molecular weight ranging from 2000 to 15000 Daltons, preferably ranging from 2500 to 10000 Daltons, advantageously from 3000 to 7000 Daltons.
  • the dispersant also has, moreover, a number-average molecular weight greater than or equal to 1000 Daltons, preferably ranging from 1000 to 5000 Daltons, more preferentially from 1800 to 3500 Daltons, advantageously from 1800 to 3000 Daltons.
  • the number-average molecular weight of the dispersant is assessed according to the standard ASTM D5296.
  • the content by weight of dispersant having a weight-average molecular weight greater than or equal to 2000 Daltons ranges from 0.1 to 10%, preferably from 0.1 to 5%, advantageously from 0.1 to 3% with respect to the total weight of the lubricant composition.
  • OLOA 13000 from the company Oronite may be mentioned.
  • the lubricant compositions according to the invention can contain any type of lubricant base, mineral, synthetic or natural, animal or vegetable suited to their use.
  • the base oil or oils used in the lubricant compositions according to the present invention can be oils of mineral or synthetic origin, of groups I to V according to the classes defined in the API classification (or their equivalents according to the ATIEL classification) as summarized below, alone or in a mixture.
  • base oil or oils used in the lubricant compositions according to the invention can be selected from the oils of synthetic origin of group VI according to the ATIEL classification.
  • the API classification is defined in American Petroleum Institute 1509 “Engine oil Licensing and Certification System” 17th edition, September 2012.
  • the mineral base oils according to the invention include any type of bases obtained by atmospheric and vacuum distillation of crude oil, followed by refining operations such as solvent extraction, deasphalting, solvent dewaxing, hydrotreatment, hydrocracking and hydroisomerization, hydrofinishing.
  • the base oils of the lubricant compositions according to the present invention can also be synthetic oils, such as the poly alpha olefins (PAO) or certain esters of carboxylic acids and alcohols, in particular polyol esters.
  • PAO poly alpha olefins
  • the poly alpha olefins used as base oils are for example obtained from monomers having from 4 to 32 carbon atoms (for example octene, decene), and have a viscosity at 100° C. comprised between 1.5 and 15 cSt measured according to the standard ASTM D445. Mixtures of synthetic and mineral oils can also be used.
  • the base oil has a flash point greater than or equal to 150° C., preferably greater than or equal to 170° C., even more preferentially greater than or equal to 190° C.
  • the base oil is selected from the group formed by the bases of group I, the bases of group II, the bases of group III, the bases of group IV, the bases of group V of the API classification (or their equivalents according to the ATIEL classification) and mixtures thereof.
  • the base oil can be selected from the bases of group VI of the ATI EL classification.
  • the base oil is selected from the group formed by the bases of group III, the bases of group IV, the bases of group V of the API classification and mixtures thereof. In a preferred embodiment of the invention, the base oil is a mixture of bases of group IV and group V of the API classification. In a preferred embodiment of the invention, the base oil is selected from the poly alpha olefins (PAO) and the esters, preferably the polyol esters or mixtures thereof. In a more preferred embodiment of the invention, the base oil is a mixture of at least one poly alpha olefin and at least one ester, preferably a polyol ester.
  • PAO poly alpha olefins
  • the base oil or the base oils can represent at least 50% by mass, with respect to the total mass of the lubricant composition, preferentially at least 60%, or also at least 70%. Typically, it (they) represent(s) between 75 and 99.89% by weight, with respect to the total weight of the lubricant compositions according to the invention.
  • the lubricant compositions according to the invention have a kinematic viscosity at 100° C. measured according to the standard ASTM D445 comprised between 4 and 41 cSt, according to the classification SAE J 306, preferably between 4.1 and 32.5 cSt.
  • the preferred grades are all the grades comprised between the grades SAE 75W and SAE 140, in particular the grades SAE 75W, SAE 75W-80 and SAE 75W-90.
  • the lubricant compositions according to the invention have a viscosity index (VI) greater than 95 (measured according to the standard ASTM 2270).
  • a subject of the invention is a transmission oil comprising a lubricant composition according to the invention. All of the characteristics and preferences presented for the lubricant composition also apply to the transmission oil according to the invention.
  • the lubricant compositions according to the invention can also contain any type of additives suitable for use in the formulations of transmission oils, for example one or more additives selected from the additional dispersants, polymeric viscosity index improvers, antioxidants, corrosion inhibitors, friction modifiers or anti-foaming agents, used alone or in mixtures, present in the usual contents required for the application.
  • the additional dispersants are selected from dispersants different from the dispersants having a weight-average molecular weight greater than or equal to 2000 Daltons. These additional dispersants can in particular ensure the maintenance in suspension and the removal of the insoluble solid contaminants constituted by the by-products of oxidation and combustion residues (soots) which are formed when a lubricant composition is in service.
  • the additional dispersants can be selected from the groups formed by the succinimides that are different from the compounds of formula (I) or (II) having a weight-average molecular weight greater than or equal to 2000 Daltons or the Mannich bases.
  • the lubricant composition according to the invention can also comprise at least one additional additive selected from the polymeric viscosity index improvers, the antioxidants and mixtures thereof.
  • the polymeric viscosity index improvers can be selected from polymers other than the dispersant according to the invention.
  • the polymeric viscosity index improvers can be selected from the group of the shear-stable polymers, preferably from the group constituted by the ethylene and alpha-olefin copolymers, in particular the ethylene/propylene copolymers.
  • the additional additive is a polymeric viscosity index improver selected from the ethylene and alpha-olefin copolymers.
  • the antioxidants can be selected from the amine-containing antioxidants, preferably the diphenylamines, in particular the dialkylphenylamines, such as the octadiphenylamines, phenyl-alpha-naphthyl amines, the phenolic antioxidants (dibutylhydroxytoluene BHT and derivatives) or sulphur-containing antioxidants (sulphurized phenates).
  • the additional additive is an antioxidant selected from the dialkyphenylamines, the phenolic antioxidants, used alone and mixtures thereof.
  • the friction modifiers can be compounds providing metallic elements that are different from the metal nanoparticles according to the invention, or an ash-free compound.
  • the compounds providing metallic elements the complexes of transition metals such as Mo, Sb, Sn, Fe, Cu, Zn, the ligands of which can be hydrocarbon-containing compounds containing oxygen, nitrogen, sulphur or phosphorus atoms, such as molybdenum dithiocarbamates or dithiophosphates may be mentioned.
  • the ash-free friction modifiers are of organic origin and can be selected from the monoesters of fatty acids and polyols, alkoxylated amines, alkoxylated fatty amines, amine phosphates, fatty alcohols, fatty epoxides, borated fatty epoxides, fatty amines or glycerol esters of fatty acid.
  • fatty is meant within the meaning of the present invention a hydrocarbon-containing group comprising from 8 to 24 carbon atoms.
  • the additional additive is a friction modifier selected from the molybdenum dithiocarbamates, amine phosphates and fatty alcohols, used alone or in a mixture.
  • the anti-corrosion additives can be selected from the phenol derivatives, in particular ethoxylated phenol derivatives and substituted with alkyl groups in the ortho position.
  • the corrosion inhibitors can be dimercaptothiadiazole derivatives.
  • the additional additive comprises a mixture of an anti-oxidant and a polymeric viscosity index improver selected from the group formed by the ethylene/alpha-olefin copolymers, in particular the ethylene/propylene copolymers.
  • the additional additive comprises a mixture of an amine-containing antioxidant, a phenolic antioxidant and a polymeric viscosity index improver selected from the ethylene and alpha-olefin copolymers.
  • the mass ratio (metal nanoparticles:dispersant) ranges from 1/50 to 10/1, preferably from 1/50 to 5/1, more preferentially from 1/30 to 5/1, advantageously from 1/10 to 5/1.
  • a subject of the invention is also a lubricant composition
  • a lubricant composition comprising:
  • a subject of the invention is also a lubricant composition
  • a lubricant composition comprising:
  • a subject of the invention is also a lubricant composition consisting essentially of:
  • a subject of the invention is also a lubricant composition essentially consisting of:
  • a subject of the invention is also a composition of the additive-concentrate type comprising:
  • the invention relates to a composition of the additive-concentrate type comprising:
  • the base oil is a base selected from the group formed by the bases of group III, the bases of group IV, the bases of group V of the API classification and mixtures thereof.
  • the base oil is a mixture of bases of group IV and group V of the API classification, preferably the base oil is selected from the poly alpha olefins (PAO) and the esters and a mixture thereof.
  • PAO poly alpha olefins
  • the base oil is a mixture of at least one poly alpha olefin and at least one ester, preferably a polyol ester.
  • the lubricant composition according to the invention can lubricate at least one mechanical part or mechanical component, in particular bearings, gears, universal joints, transmissions, the pistons/rings/liners system, camshafts, clutch, manual or automatic gearboxes, axles, rocker arms, housings etc.
  • the lubricant composition according to the invention can lubricate a mechanical part or a metal component of the transmission, clutch, manual or automatic gearboxes, preferably manual.
  • a subject of the invention is also a process for reducing the flaking of a mechanical part, preferentially of a transmission component, advantageously of a gearbox or an axle, comprising at least bringing the mechanical part into contact with a lubricant composition as defined above or obtained from the composition of the additive-concentrate type as defined above. All of the characteristics and preferences presented for the lubricant composition also apply to the process for reducing the flaking of a mechanical part according to the invention.
  • a subject of the invention is also the use of a lubricant composition according to the invention for the lubrication of gearboxes or axles, preferentially the gearboxes of motor vehicles.
  • the invention relates to the use of a lubricant composition according to the invention for the lubrication of manual gearboxes of motor vehicles. All of the characteristics and preferences presented for the lubricant composition also apply to the use for lubricating gearboxes according to the invention.
  • a subject of the invention is also the use of a lubricant composition according to the invention for reducing the flaking of a mechanical part, preferentially of a transmission component, more preferentially of a gearbox or an axle.
  • the invention relates to the use of a lubricant composition according to the invention for reducing the flaking of a manual gearbox. All of the characteristics and preferences presented for the lubricant composition also apply to the use for reducing the flaking according to the invention.
  • lubricant compositions according to the invention are assessed by monitoring, over time, the concentration of tungsten disulphide nanoparticles in the supernatant phase of the composition.
  • different lubricant compositions were prepared from the following compounds:
  • compositions L 1 to L 5 were prepared according to the procedure below:
  • the protocol for monitoring, over time, the concentration of tungsten disulphide nanoparticles in the supernatant phase for each of the compositions L 1 to L 5 is defined as follows:
  • the lubricant compositions according to the invention L 4 and L 5 comprising 0.2% by weight of tungsten disulphide nanoparticles and a dispersant having a weight-average molecular weight greater than or equal to 2000 Daltons, have an improved stability with respect to lubricant compositions comprising 0.2% by weight of tungsten disulphide nanoparticles and a dispersant having a weight-average molecular weight less than 2000 Daltons. It should be noted that this stability persists over time for the lubricant compositions according to the invention L 4 and L 5 , which is not at all the case for the other compositions L 1 , L 2 and L 3 .
  • the composition L 6 is a lubricant composition conventionally used for lubricating transmissions, and in particular motor vehicle gearboxes.
  • the kinematic viscosity at 100° C. of the compositions L 6 and L 7 was adjusted in order to be identical, in particular by the content of base oils 1, so as to be able to compare these two compositions.
  • the coefficient of friction of each composition was assessed by means of a Cameron Plint Friction laboratory test using a reciprocating tribometer of the Cameron-Plint TE-77 type.
  • the test bench is constituted by a cylinder-on-flat tribometer immersed in the lubricant composition to be tested.
  • the coefficient of friction is monitored throughout the test by measuring the tangential force over the normal force.
  • a cylinder (SKF 100C6) having a length of 10 mm and diameter of 7 mm is applied to the steel flat immersed in the lubricant composition to be tested, the temperature of the lubricant composition is set at each test.
  • a sinusoidal reciprocating movement is applied with a defined frequency. Each measurement is carried out over a period of 100 seconds during the test.
  • the average coefficient of friction at 60° C. was measured under different loads ranging from 300 MPa to 650 MPa and at different speeds ranging from 70 mm/s to 550 mm/s.
  • the average coefficient of friction at 100° C. was measured under different loads ranging from 300 MPa to 650 MPa and at different speeds ranging from 70 mm/s to 550 mm/s.
  • the average coefficient of friction under a load of 640 MPa was measured at different temperatures ranging from 60° C. to 140° C. and at different speeds ranging from 70 mm/s to 550 mm/s.
  • a lubricant composition according to the invention is assessed by implementing a test on a closed-loop power circulation bench.
  • the lubricant composition according to the invention L 8 and the composition L 9 not according to the invention, the compositions of which are described in Table V, were prepared; the percentages indicated correspond to percentages by mass.
  • the base oils 1 and 2, the polymers 1 and 2, the anti-foaming agent, dispersant and additive package 1 are identical to those described in Example 2.
  • the additive package 2 (Anglamol 2190 from the company Lubrizol) comprises a zinc dithiophosphate as friction modifier.
  • the closed-loop power circulation bench is represented in FIG. 1 .
  • a Renault JR5 gearbox is installed in a power recirculation loop and placed under load by means of a torsion system, the gearbox being engaged in 3rd gear.
  • the machine is put into operation using an electric motor in order to obtain a rotation speed of 3000 rpm under a torque of 148 N.m at the gearbox input.
  • the assessment criterion, and therefore the critical part to be assessed (because of the load supported), is the drive pinion of the output shaft.
  • the gearbox is inspected at regular intervals of approximately 150 h after dismantling and visual scoring.
  • the visual scoring is carried out using the “Chrysler” scoring system for monitoring the presence of flakes on the teeth of the drive pinion with, moreover, continuous vibration monitoring in order to detect the appearance of flaking in the gearbox during operation.
  • the “Chrysler” scoring system consists of noting the state of the teeth of the drive pinion after testing. Each tooth of the pinion is thus examined in order to monitor any presence of flaking(s) and a score is assigned to each flaking level.
  • the scoring system is defined as follows:
  • Vibration monitoring consists of placing an accelerometer close to the test piece and noting the intensity of the vibrations during operation. In the case of degradation of a part, the intensity of the vibrations increases. It is sufficient to set a threshold for stopping the device and verifying the appearance of flakes on the teeth.
  • the shaft bearings and the 3rd gear pinion are normally replaced every 150 h. The test is stopped when a flake of 12 mm 2 maximum is observed and/or when 80 mm 2 of flaked surface in total is observed and/or at 312 h when no flaking has appeared after this period.
  • composition according to the invention L 10 and the composition L 11 not according to the invention, the compositions of which are described in Table VI were prepared; the percentages indicated correspond to percentages by mass.
  • the base oils 1 and 2 are identical to those described in Example 2.
  • the test conditions are identical to those described in Example 3.
  • FIG. 2 shows that no excessive deposit ( 200 ) of tungsten disulphide nanoparticles was observed in the housing after testing with the composition according to the invention L 10 .
  • FIG. 3 shows an excessive deposit ( 300 ) of tungsten disulphide nanoparticles in the housing after testing with the composition L 11 , which can thus give rise to a risk of obstructing the lubricating holes of the bearings or also of the synchronizers.
  • the examples above show that the lubricant compositions according to the invention have both good stability over time and good anti-flaking properties, while retaining satisfactory friction reduction properties.

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BR112015026415A2 (pt) 2017-07-25
EP2986693A1 (fr) 2016-02-24
KR20160018490A (ko) 2016-02-17
BR112015026415B1 (pt) 2020-12-15
KR102154097B1 (ko) 2020-09-09
CN105247022B (zh) 2019-09-10
FR3004723B1 (fr) 2016-04-15
FR3004723A1 (fr) 2014-10-24
MX2015014698A (es) 2016-03-07
WO2014170485A1 (fr) 2014-10-23
JP2016515663A (ja) 2016-05-30
JP6440685B2 (ja) 2018-12-19
EP2986693B1 (fr) 2019-09-18
CN105247022A (zh) 2016-01-13
ES2753261T3 (es) 2020-04-07

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