EP3622042B1 - Schmierstoffzusammensetzung - Google Patents

Schmierstoffzusammensetzung Download PDF

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Publication number
EP3622042B1
EP3622042B1 EP18725407.3A EP18725407A EP3622042B1 EP 3622042 B1 EP3622042 B1 EP 3622042B1 EP 18725407 A EP18725407 A EP 18725407A EP 3622042 B1 EP3622042 B1 EP 3622042B1
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EP
European Patent Office
Prior art keywords
weight
lubricant composition
silasesquioxane
amount
composition according
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.)
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Application number
EP18725407.3A
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German (de)
English (en)
French (fr)
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EP3622042A1 (de
Inventor
Stefan Seemeyer
Stefan Grundei
Carla KRUTZSCH
Philipp ALTMANN
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.)
Klueber Lubrication Muenchen GmbH and Co KG
Original Assignee
Klueber Lubrication Muenchen SE and Co KG
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Application filed by Klueber Lubrication Muenchen SE and Co KG filed Critical Klueber Lubrication Muenchen SE and Co KG
Priority to EP23161458.7A priority Critical patent/EP4219668A1/de
Publication of EP3622042A1 publication Critical patent/EP3622042A1/de
Application granted granted Critical
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    • 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
    • C10M107/00Lubricating compositions characterised by the base-material being a macromolecular compound
    • C10M107/20Lubricating compositions characterised by the base-material being a macromolecular compound containing oxygen
    • C10M107/30Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M107/32Condensation polymers of aldehydes or ketones; Polyesters; Polyethers
    • C10M107/34Polyoxyalkylenes
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    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M139/00Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing atoms of elements not provided for in groups C10M127/00 - C10M137/00
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    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M101/00Lubricating compositions characterised by the base-material being a mineral or fatty oil
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    • C10M125/00Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/14Water
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    • C10M125/00Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/26Compounds containing silicon or boron, e.g. silica, sand
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    • C10M155/00Lubricating compositions characterised by the additive being a macromolecular compound containing atoms of elements not provided for in groups C10M143/00 - C10M153/00
    • C10M155/02Monomer containing silicon
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    • 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
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    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/10Compounds containing silicon
    • C10M2201/102Silicates
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    • C10M2201/105Silica
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    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/2805Esters used as base material
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    • C10M2209/00Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/102Polyesters
    • C10M2209/1023Polyesters used as base material
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    • C10M2209/00Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/1033Polyethers, i.e. containing di- or higher polyoxyalkylene groups used as base material
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    • C10M2209/10Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/107Polyethers, i.e. containing di- or higher polyoxyalkylene groups of two or more specified different alkylene oxides covered by groups C10M2209/104 - C10M2209/106
    • C10M2209/1075Polyethers, i.e. containing di- or higher polyoxyalkylene groups of two or more specified different alkylene oxides covered by groups C10M2209/104 - C10M2209/106 used as base material
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    • C10M2229/00Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
    • C10M2229/04Siloxanes with specific structure
    • C10M2229/041Siloxanes with specific structure containing aliphatic substituents
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    • C10M2229/04Siloxanes with specific structure
    • C10M2229/043Siloxanes with specific structure containing carbon-to-carbon double bonds
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    • C10M2229/04Siloxanes with specific structure
    • C10M2229/045Siloxanes with specific structure containing silicon-to-hydroxyl bonds
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    • C10M2229/04Siloxanes with specific structure
    • C10M2229/046Siloxanes with specific structure containing silicon-oxygen-carbon bonds
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    • C10M2229/00Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
    • C10M2229/04Siloxanes with specific structure
    • C10M2229/047Siloxanes with specific structure containing alkylene oxide groups
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    • C10M2229/048Siloxanes with specific structure containing carboxyl groups
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    • C10M2229/04Siloxanes with specific structure
    • C10M2229/05Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon
    • C10M2229/051Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon containing halogen
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    • C10M2229/00Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
    • C10M2229/04Siloxanes with specific structure
    • C10M2229/05Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon
    • C10M2229/052Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon containing nitrogen
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    • C10M2229/04Siloxanes with specific structure
    • C10M2229/05Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon
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    • C10M2229/04Siloxanes with specific structure
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    • C10N2020/00Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01Physico-chemical properties
    • C10N2020/055Particles related characteristics
    • C10N2020/06Particles of special shape or size
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    • C10N2020/00Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01Physico-chemical properties
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    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
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    • 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
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    • C10N2040/02Bearings
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    • C10N2040/04Oil-bath; Gear-boxes; Automatic transmissions; Traction drives

Definitions

  • the present invention relates to a lubricating composition for application to the surface of drive elements such as roller bearings, gears, plain bearings and chains.
  • the composition is suitable for preventing, reducing or avoiding signs of fatigue in the material of drive elements, such as micropitting, false brinelling and white etching cracks.
  • Another object of the present invention is the use of the lubricant composition for treating surfaces of drive elements and the further use of such drive elements.
  • One measure is to increase the thickness of the lubricating film.
  • Fatigue wear is caused by local overloading of the material due to periodic compressive stress.
  • the fatigue of the material becomes visible through gray spots (grey staining, surface fatigue, micro-pitting) or pits on the surface of the material.
  • gray spots grey staining, surface fatigue, micro-pitting
  • fine cracks appear in the metal lattice initially 20 to 40 ⁇ m below the surface, which lead to material breakouts.
  • the small microscopically visible break-outs on the tooth flank known as micropitting or gray spot formation can be recognized macroscopically as dull gray areas.
  • gray spots can usually be observed on tooth flanks in practically all speed ranges.
  • very flat pitting occurs as gray spots on the raceway in the area of the sliding contact.
  • White etching cracks can lead to fatigue damage that occurs much earlier than is to be expected for a drive element with given load parameters.
  • False brinelling is a form of damage that occurs in bearings that appear to be stationary. Micro-movements are introduced into the contact surfaces by vibrations (e.g. in machines, but also when transported by motor vehicles, rail vehicles or ships) or elastic deformations, which can lead to damage after just a few load changes. This can lead to unsteady running behavior and immediate or early component failure.
  • Various additives are also used to improve the viscosity properties in lubricants in order to avoid or at least minimize the above-mentioned damage in roller bearings, gears, gears and the like.
  • additives were investigated that can be used to reduce friction between the components or that have improved viscosity.
  • the EP 1 642 957 A1 relates to the use of MoS2 and molybdenum dithiocarbamate, which are used as additives in urea greases for cardan shafts.
  • the additives known from the prior art described above are not thermally stable as organic substances.
  • they can evaporate under the operating conditions or, as classic anti-wear additives, can react primarily with the metal surfaces, ie they react predominantly at the roughness points that are in contact, since the lightning temperatures that occur there provide sufficient energy for a chemical reaction with the metal friction layer is present. They can therefore counteract fatigue damage to a lesser extent at best.
  • Solid lubricants such as Molybdenum disulfide, on the other hand, due to its density, tends to settle out of oil formulations and can also be corrosive.
  • DE 102011103215 A1 describes the use of a composition containing surface-modified nanoparticles and a carrier material that is applied to the surfaces of drive elements to prevent or reduce fatigue damage. It is assumed that the mechanism of action of the nanoparticles is based on the fact that they accumulate on the surface of the drive elements and thereby smooth them out. The smoothing increases the contact surfaces and reduces the surface pressure.
  • JP 2006144827 A names compositions with silica nanoparticles to suppress WEC damage.
  • U.S. 7,217,683 B1 describes nanoscale polyhedral oligomeric silsesquioxanes (POSS) and polyhedral oligomeric silicates (POS) based chemicals as lubricants, mold release agents, and as additives to control viscosity, lubrication, wear, and thermal properties of lubricants.
  • the compositions described contain 5% by weight of POSS in a mineral turbine oil (L-7808).
  • the composition is suitable for preventing, reducing or avoiding signs of fatigue in the material of drive elements, such as micropitting, false brinelling and white etching cracks.
  • the positive influence of the lubricant composition is surprising, since silasesquioxane significantly smaller than those in the publications DE 102011103215 A1 and JP2006144827A are nanoparticles and it could therefore not be assumed that, analogously to these particles, they can bring about a reduction in the signs of fatigue by smoothing the surface.
  • the composition according to the invention can be mixed homogeneously with base oils of the most varied of polarities, since the polarity of the composition can be easily adjusted, for example, via the selection of the substituents of the silsesquioxane.
  • the polarity of the composition can be easily adjusted, for example, via the selection of the substituents of the silsesquioxane.
  • due to its production process sufficient saturation of the OH groups of the silasesquioxane can be guaranteed.
  • the use of silasesquioxane enables high storage stability and that there is no impairment of foaming behavior or filterability.
  • silsesquioxanes which are liquid at room temperature (20° C.) and/or have low melting points (preferably below 100° C., DIN EN ISO 11357-2 (edition: 2014-07)) can be used favorably can.
  • Silsesquioxanes are organosilicon compounds and form cage-like structures with Si-O-Si bonds and tetrahedral Si corners.
  • the silsesquioxane can have 6 to 12 Si corners in molecular form and/or be present as an oligomer and/or polymer.
  • Molecular silsesquioxanes are preferred according to the invention, more preferably molecular silsesquioxanes with 6 to 12, more preferably 7 to 10, in particular with 7 or 8 Si corners.
  • each Si center is bonded to three oxo groups, which in turn connect to other Si centers.
  • the Si centers are only partially bonded to three oxo groups bonded to other Si centers, and there are, preferably three, Si centers bonded to only two oxo groups bonded to other Si centers.
  • the third group herein is preferably a substituent, more preferably a hydroxy substituent.
  • the fourth group on the Si is also preferably a substituent, whereby a surface-modified silsesquioxane can be obtained, which is preferred according to the invention.
  • Suitable substituents are oxirane polymer (degree of polymerisation with 4 to 20 repeating units), each substituted or unsubstituted.
  • the silsesquioxane can have the same substituents or mixtures of different substituents.
  • Preferred substituents are polyethylene glycol, polypropylene glycol, polybutylene glycol and/or their copolymers (degree of polymerization 4 to 20, in particular 10 to 15 repeating units), each substituted or unsubstituted.
  • substituents are polyethylene glycol, polypropylene glycol and/or their copolymers (degree of polymerization 4 to 20, in particular 10 to 15 repeating units), each substituted or unsubstituted.
  • R can additionally have functional groups, in particular thio groups, phosphate groups, individually or in combination.
  • the optionally present thio or phosphate groups can also react with the metal surface to be protected.
  • the silsesquioxane can also be mixtures of structurally different silsesquioxanes.
  • silsesquioxanes can be synthesized by hydrolysis of organotrichlorosilanes (ideally: 8 RSiCl 3 ; + 12 H 2 O ⁇ [RSiO 3/2 ] 8 + 24 HCl).
  • organotrichlorosilanes ideally: 8 RSiCl 3 ; + 12 H 2 O ⁇ [RSiO 3/2 ] 8 + 24 HCl.
  • R substituent
  • the exterior of the cage can be further modified.
  • R H
  • the Si-H group can undergo hydrosilylation or oxidation to the silanol.
  • Bridged poly-silsesquioxanes are most readily prepared from clusters containing two or more trifunctional silyl groups attached to non-hydrolyzable silicon-carbon bonds.
  • Vinyl-substituted silsesquioxanes can be linked by alkene metathesis.
  • radicals R can be the same or different.
  • R is preferably, independently of one another, polyethylene glycol, polypropylene glycol, polybutylene glycol and/or their copolymers (degree of polymerization 4 to 20, in particular 10 to 15 repeating units), each substituted or unsubstituted.
  • R can additionally have functional groups, in particular thio groups, phosphate groups, individually or in combination.
  • the optionally present thio or phosphate groups can also react with the metal surface to be protected.
  • the lubricant composition can also contain mixtures of structurally different silasesquioxanes.
  • the silsesquioxane is present on nanoparticle carrier materials, preferably on oxidic nanoparticles, in particular on amorphous silicon dioxide nanoparticles.
  • nanoparticle carrier materials preferably on oxidic nanoparticles, in particular on amorphous silicon dioxide nanoparticles.
  • Such silasesquioxanes are available, for example, under the trade name POSS® Nanosilica Dispersion from Hybrid Plastics. Advantage here is the very good stabilization of the nanoparticles in different media and the combination of the two different particle sizes.
  • the silsesquioxane can be blended directly with the base oil of the lubricant or in the form of a masterbatch.
  • this advantageously contains a carrier material, preferably selected from the group consisting of mineral oils, synthetic hydrocarbons, including particularly preferably polyalphaolefins (PAO) and metallocene-catalyzed PAO (m-PAO), polyglycols, esters, perfluoropolyethers (PFPE ), silicone oils, native oils and derivatives of native oils, oils containing aromatics such as phenyl ethers, alkylated naphthalenes and mixtures of the carrier materials mentioned above.
  • PAO polyalphaolefins
  • m-PAO metallocene-catalyzed PAO
  • PFPE perfluoropolyethers
  • silicone oils native oils and derivatives of native oils
  • oils containing aromatics such as phenyl ethers, alkylated naphthalenes and mixtures
  • the base oil of the lubricant composition is selected from the group consisting of polyglycols.
  • suitable base oils are selected from the group consisting of silicone oils, PFPE, mineral oils, esters, synthetic hydrocarbons, including particularly preferably PAO, m-PAO, oils containing aromatics such as phenyl ethers, alkylated diphenyl ethers, alkylated naphthalenes, phenyl ethers, native oils and derivatives of native oils , and mixtures of the above base oils.
  • esters and/or synthetic hydrocarbons including particularly preferably polyalphaolefins (PAO) and metallocene-catalyzed PAO (m-PAO), are particularly preferably used as the base oil.
  • Particularly preferred esters are selected from an ester of an aliphatic or aromatic di-, tri- or tetracarboxylic acid (preferably C6 to C60) with one or a mixture of C7 to C22 alcohols, from an ester of trimethylolpropane, pentaerythritol or dipentaerythritol aliphatic C7 to C22 carboxylic acids, from C18 dimer acid esters with C7 bis C22 alcohols, from complex esters, as individual components or in any mixture.
  • PAO polyalphaolefins
  • m-PAO metallocene-catalyzed PAO
  • the lubricant composition can also contain other customary additives, e.g. aromatic amines, phenols, sulfates, etc.).
  • Preferred thickeners are lithium soaps, lithium complex soaps, ureas, calcium complex soaps, calcium sulfonate thickeners, bentonites, aluminum complex soaps.
  • Particularly preferred thickeners are lithium soaps, lithium complex soaps, aluminum complex soaps, bentonites and ureas.
  • the additives mentioned can be soluble additives, in particular as anti-corrosion agents, as agents for reducing friction, as agents for protection against metal influences and as UV stabilizers.
  • the lubricant composition has a viscosity of ISO VG 68-680, particularly preferably ISO VG 220-460.
  • the base oils preferably used are polyglycols on the one hand and mixtures of synthetic hydrocarbons on the other hand, including particularly preferably mixtures of PAO with m-PAO, mixtures of esters or compositions containing mixtures of synthetic hydrocarbons and esters as base oils. Medicinal white oils are also suitable.
  • the lubricant composition has an NLGI class of 0 to 3, preferably 1 or 2, according to DIN 51818.
  • the base oil preferably has a viscosity in the range from 50 to 460 mm 2 /sec on.
  • Base oils used with preference are PAO, m-PAO, esters and mixtures thereof.
  • Preferred thickeners are lithium soaps, lithium complex soaps and ureas.
  • the lubricant composition has an NLGI class of 1 to 3 according to DIN 51818.
  • Base oils that are preferably used are mineral oils, PAO, m-PAO, esters and mixtures thereof.
  • Preferred thickeners are lithium soaps, lithium complex soaps, calcium complex soaps and ureas.
  • the base oil preferably has a viscosity in the range of 30-300 mm 2 /sec, preferably in the range of 50-200 mm 2 /sec.
  • the lubricant composition contains the silsesquioxane in an amount from 0.01 to 40% by weight, preferably from 0.05 to 20% by weight, more preferably in an amount from 0.07 to 15% by weight and in particular from 0.1 to 10% by weight, based on the total weight of the lubricant composition. In a further preferred embodiment, the lubricant composition contains the silsesquioxane in an amount of 0.05 to 5% by weight.
  • the lubricating composition contains the base oil preferably in an amount of 99.99 to 50% by weight, more preferably 99 to 60% by weight and especially in an amount of 98 to 65% by weight based on the total weight of the lubricating composition.
  • polyglycol as base oil with PEGPOSS® Cage Mixture is particularly preferred.
  • composition according to the invention contains silsesquioxane in an amount of 0.01 to 40% by weight, more preferably 0.05 to 20% by weight, even more preferably in an amount of 0.07 to 15% by weight and in particular 0.1 up to 10% by weight;
  • Base oil in an amount of 99.99 to 50% by weight, more preferably in an amount of 99 to 50% by weight, still more preferably in an amount of 99 to 60% by weight, especially in an amount of 98 to 65% by weight.
  • Thickeners in an amount of 3 to 40% by weight, more preferably in an amount of 5 to 40% by weight and in particular in an amount of 7 to 25% by weight and solid lubricants in an amount of 0% to 30% by weight.
  • % more preferably in an amount of 0 to 20% by weight and additives in an amount of 0% to 15% by weight, even more preferably in an amount of 0 to 10% by weight and in particular in an amount of 2 to 10% by weight, based in each case on the total weight of the lubricant composition.
  • this lubricating composition can be considered a water-based lubricating composition.
  • the lubricant composition is present as a water-based gear oil formulation with which, when carrying out an FZG test according to DIN ISO 14635-3, the power level 12 with total wear on the wheel and pinion of ⁇ 150 mg is passed and preferably in the subsequent extended test of 50 hours at power level 10 no significant additional wear is generated.
  • Preferred base oils for the water-based lubricant composition are water-soluble polyalkylene glycols, optionally in combination with water-soluble carboxylic acid esters and/or water-soluble fatty alcohol ethoxylates.
  • water-soluble means that after mixing the base oils with water (stirring for 1 hour) in a concentration ratio of at least 5% by weight base oil in water at room temperature (25° C.), a transparent liquid is present.
  • carboxylic acid ester base oils for the water-based lubricant composition are selected from the group consisting of ethoxylated mono- or dicarboxylic acids with a chain length of C 4 - to C 40 - and degrees of ethoxylation of 2-15.
  • Preferred fatty alcohol ethoxylates consist of fatty alcohols with chain lengths of C6 to C22 and a degree of ethoxylation of more than 3.
  • the water-based lubricant composition contains 0.5 to 40% by weight lubricant thickener selected from the group consisting of metal soaps made from mono- and/or dicarboxylic acids, ureas, phyllosilicates, solid lubricants and aerosil.
  • the lubricant composition is present as a gear oil formulation with which, when carrying out an FZG micropitting test C/8.3/60 according to FVA information sheet 54/7 with injection lubrication, the profile deviation in step running is 7.5 ⁇ m and/or in continuous running 20 ⁇ m does not exceed.
  • the lubricant composition is characterized in that when a false brinell test is carried out using an SNR FEB 2 test device at room temperature, 8000 N load, pivot angle 3° and 24 Hz vibration frequency, a running time of at least 50 h is achieved and the Wear of the drive element is preferably below 100 mg, in particular below 20 mg.
  • the lubricant composition is characterized in that a mass loss of the drive element caused by vibrations is reduced by at least 50%, preferably by at least 90%, and/or the length of time until failure is at least doubled.
  • Another object of the present invention is the use of the lubricant composition according to the invention for treating surfaces of drive elements, preferably of roller bearings, gears, plain bearings and/or chains, in particular roller bearings and gears.
  • the lubricant composition according to the invention is also suitable for lubricating seals on rotating shafts.
  • roller bearings that are used as wheel bearings and/or in transmissions that are exposed to vibration.
  • the use in main bearings, blade bearings, adjustable bearings, generator bearings of wind turbines is also particularly advantageous.
  • the application in roller bearings that are used in electric motors of electrically powered vehicles is particularly advantageous.
  • the application in rolling bearings in clutches is particularly advantageous, especially in hybrid vehicles.
  • it is particularly advantageous to use it in joints in automotive applications such as constant velocity joints, azipod joints, tripod joints, chassis joints and/or ball joints, where material fatigue/fractures are also known to be a damage pattern.
  • the drive elements mentioned above are particularly susceptible to the damage mechanisms described at the beginning, so that the use of silsesquioxanes with their beneficial influence on them is particularly efficient.
  • Another object of the present invention is the use of drive elements, preferably roller bearings, gears, plain bearings and / or chains, the surfaces of which have been treated with the lubricant composition according to the invention, in systems and machines for the production and conveyance of food, in wind turbines, in automobiles, in Pulley bearings, in rail vehicles, in ships, in electric motors, generators, ancillary units, joints.
  • drive elements preferably roller bearings, gears, plain bearings and / or chains, the surfaces of which have been treated with the lubricant composition according to the invention
  • the wear behavior of lubricant compositions in roller bearings is determined with small oscillating rolling and sliding movements with a constant load.
  • the switch-off criterion for the SNR is the wear path. If the value for a bearing rises above 30 mm, the run is automatically ended or the specified running time is reached.
  • Bearing type FAG 51206 is used as a test bearing. The resulting wear is not determined via the wear path but by weighing the cleaned bearing rings before and after the test. The grooves of the bearing rings are completely filled with the lubricant composition to be tested, and excess grease is wiped off. Depending on the density, this results in a quantity of lubricant composition of approx. 1 g per bearing ring.
  • the test device consists of a closed gear housing with a viewing window. Two gears of the same size (external diameter 54 mm) are mounted centrally above vertical shafts, which are immersed in the test oil so that some of the gears are not covered by oil. The pair of gears is driven for 5 minutes at a speed of 1450 rpm. Air is mixed into the oil, so to speak. The change/increase in volume can be documented using a scale that is placed in the viewing window. Limit values of the standard are: after 1 min standstill after operation of the gear pair ⁇ 15% and after 5 min standstill ⁇ 10% total. Foam volumes must not be exceeded.
  • Viscosity measurement (DIN 51562) using a Stabinger viscometer SVM 3000 (Anton Paar).
  • air is foamed with a constant volume flow over an immersed sintered ball at room temperature, then at 94°C and then again at room temperature for 1 min. It is measured a) how much foam forms in ml and b) how long it takes for the foam to dissipate after the air inlet has ended. Specification is (a,b). Limit value: (max. 75 ml/10 min) for all 3 temperature sequences must not be exceeded. b is specified in the form x:y min. This means the foam has dissolved after x minutes and y seconds.
  • Achieved force level sum of the damage (width of all scores and seizures) on the active tooth flanks of the 16 pinion teeth is more than one tooth width or 20 mm.
  • a heatable oil reservoir (60°C) is filled with approx. 10L oil, with an adjustable pump (Vogel Fluidtec GmbH / flow sensor regulated) the oil is circulated (6L/min) through a filter with a precisely defined pore size (Mahle PI 2105 PS 3 ⁇ m/ Mahle PI 3105 PS 10 ⁇ m) pumped.
  • the pressure is measured by sensors in front of and behind the filter. The system switches off when the pressure difference here exceeds 2.2 bar. The duration of the test is up to 840 hours.
  • a lithium soap grease of NLGI class 2 with polyglycol base oil with approx. 46 mm 2 /sec viscosity at 40°C and an additive package (corrosion, oxidation stability, load carrying capacity, wear) was mixed with 5.85% PEGPOSS ® Cage Mixture and mixed with a speed mixer (company . Hauschild, Type DAC 700.1 FVZ) homogenized (example fat 1).
  • PEGPOSS ® Cage Mixture has a viscosity of approx. 80 mm 2 /sec at 40°C.
  • a comparison fat 1 was produced in which the fat was diluted with 5.85% of a polyglycol based on EO:PO approx.
  • Example Grease 1 PG Grease, Lithium Soap, PG Base Oil + Diluted with 5.85% PEGPOSS ® Cage Mixture Comparative Grease 1, PG Grease, Lithium Soap, PG Base Oil + Diluted with 5.85% PG Base Oil Wear Bearing 1 (mg) 21 95 Wear bearing 2 (mg) 0 216 test duration 50 h 19 h, 28 min (cancel)
  • Reference oil 2 Ester-based gear oil, ISO VG 100 additive package (corrosion, foam, oxidation stability, load carrying capacity, wear) Reference oil 2 + 1.3% Isooctyl POSS ® Cage Mixture (comparison) Kinematic viscosity 40°C [mm 2 /sec] 98 99.3 ASTM foam test rt 0 ml / 0 min 0 ml / 0:0 min 94°C 0 ml / 0 min 0 ml / 0:0 min rt 0 ml / 0 min 10 ml/ 0:03 min FZG gray spot test, C/8.3/60 Step test, change in weight (mg) after strength step 10 24 16 Step test, micropitting area (%) after power step 10/400 h 30 20 Step test, profile shape deviation ( ⁇ m) after power level 10/400 h 8.8 (fail) 7.3 (pass) Endurance test, change in weight (mg) according to strength level 10
  • Reference oil 3 Polyglycol gear oil, additive package (corrosion, oxidation stability, load carrying capacity, wear, foam) ISO VG 100 Reference Oil 3 + 5.8% PEGPOSS ® Cage Mixture Viscosity 40°C [mm 2 /sec] 101 102 ASTM foam test rt 10 ml / 0:15 min 0 ml / 0:0 min 94°C 20 ml / 0:15 min 10 ml / 0:0 min rt 20 ml / 0:25 min 10 ml/ 0.03 min Flender foam test Foam after 1 min standing time (%) 20 0 Foam after 5 min standing time (%) 19 4 FZG micropitting test, C/8.3/90°C splash lubrication Step test, change in weight (mg) after strength step 10 17 1 Step test, micropitting area (%) after power step 10 10 0 Step test, profile shape deviation ( ⁇ m) after power level 10 5 4.6 Endurance test, change in weight (mg) according to strength
  • Example 4 Filterability of oils containing silsesquioxane compared to oils containing SiO 2 nanoparticles
  • Reference oil 4 gear oil PAO/ester ISO VG 46 additive package (corrosion, oxidation stability, load carrying capacity, wear, foam) Reference oil 4 +1.3% IsooctylPOSS (comparison) ® Reference oil 4 + 0.5% SiO 2 nanoparticles, primary particles 10 nm, surface covered with phenyl and trimethylsilyl groups Viscosity 40°C [mm 2 /sec] 46.2 47 47.6 Flender foam test, before filtration test Foam after 1 min standing time (%) 2 2 2 Foam after 5 min standing time (%) 0 3 2 Filtration test 3 ⁇ m filter Pressure build-up/test duration ⁇ 2.2 bar/840 h ⁇ 2.2 bar/840 h > 2.2 bar/0h filterability passport passport failed Flender foam test, after filtration test 3 ⁇ m Foam after 1 min standing time (%) 4 5 not determined Foam after 5 min standing time (%) 5 5 not determined Filtration test 10 ⁇ m filter Pressure build-up/test duration not determined ⁇ 2.2 bar
  • Reference oil 4 can be filtered at 3 ⁇ m without any problems.
  • the addition of IsooctylPOSS ® Cage Mixture has no effect on the viscosity and the good filtration and foaming behavior.
  • SiO 2 nanoparticles which can also be used to reduce micropitting, high pressures are required for effective filtration.
  • the proportion of inorganic SiO x is approximately the same in the two oils with the additives containing silicon.
  • Reference oil 5 water-based gear oil based on polyglycol (approx. 39% by weight), additive package (approx. 21% by weight corrosion, load carrying capacity/wear, foam, biocide), water (approx. 40% by weight) Reference oil 5 + 1% by weight PEGPOSS ® Cage Mixture Viscosity 40°C ISO VG 460 ISO VG 460 FZG DIN ISO 14635-3-A/2.8/50 splash lubrication Achieved power level 12 12 Total wear after power level 11 188 mg 96 mg Total wear after power level 12 231 mg 145 mg Additional wear according to power level 10/50 h 63 mg 7 mg

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