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EP3372659B1 - High temperature lubricants - Google Patents

High temperature lubricants Download PDF

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Publication number
EP3372659B1
EP3372659B1 EP18000075.4A EP18000075A EP3372659B1 EP 3372659 B1 EP3372659 B1 EP 3372659B1 EP 18000075 A EP18000075 A EP 18000075A EP 3372659 B1 EP3372659 B1 EP 3372659B1
Authority
EP
European Patent Office
Prior art keywords
group
oil
temperature
acid esters
mixture
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
EP18000075.4A
Other languages
German (de)
French (fr)
Other versions
EP3372659A1 (en
Inventor
Karl EGERSDÖRFER
Thomas Kilthau
Stefan Grundei
Stefan Seemeyer
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
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Klueber Lubrication Muenchen SE and Co KG filed Critical Klueber Lubrication Muenchen SE and Co KG
Priority to SI201531644T priority Critical patent/SI3372659T1/en
Priority to PL18000075T priority patent/PL3372659T3/en
Publication of EP3372659A1 publication Critical patent/EP3372659A1/en
Application granted granted Critical
Publication of EP3372659B1 publication Critical patent/EP3372659B1/en
Active legal-status Critical Current
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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
    • 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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    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M111/00Lubrication compositions characterised by the base-material being a mixture of two or more compounds covered by more than one of the main groups C10M101/00 - C10M109/00, each of these compounds being essential
    • C10M111/04Lubrication compositions characterised by the base-material being a mixture of two or more compounds covered by more than one of the main groups C10M101/00 - C10M109/00, each of these compounds being essential at least one of them being a macromolecular organic compound
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    • C10M105/00Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
    • C10M105/02Well-defined hydrocarbons
    • C10M105/06Well-defined hydrocarbons aromatic
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    • C10M105/00Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
    • C10M105/08Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
    • C10M105/32Esters
    • C10M105/36Esters of polycarboxylic acids
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    • C10M107/00Lubricating compositions characterised by the base-material being a macromolecular compound
    • C10M107/02Hydrocarbon polymers; Hydrocarbon polymers modified by oxidation
    • C10M107/08Hydrocarbon polymers; Hydrocarbon polymers modified by oxidation containing butene
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    • C10M109/00Lubricating compositions characterised by the base-material being a compound of unknown or incompletely defined constitution
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    • C10M111/00Lubrication compositions characterised by the base-material being a mixture of two or more compounds covered by more than one of the main groups C10M101/00 - C10M109/00, each of these compounds being essential
    • C10M111/06Lubrication compositions characterised by the base-material being a mixture of two or more compounds covered by more than one of the main groups C10M101/00 - C10M109/00, each of these compounds being essential at least one of them being a compound of the type covered by group C10M109/00
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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
    • C10M169/04Mixtures of base-materials and additives
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    • C10M169/04Mixtures of base-materials and additives
    • C10M169/044Mixtures of base-materials and additives the additives being a mixture of non-macromolecular and macromolecular compounds
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    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06Metal compounds
    • C10M2201/062Oxides; Hydroxides; Carbonates or bicarbonates
    • C10M2201/0626Oxides; Hydroxides; Carbonates or bicarbonates used as thickening agents
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    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/10Compounds containing silicon
    • C10M2201/102Silicates
    • C10M2201/1026Silicates used as thickening agents
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    • C10M2201/102Silicates
    • C10M2201/103Clays; Mica; Zeolites
    • C10M2201/1036Clays; Mica; Zeolites used as thickening agents
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    • C10M2201/1056Silica used as thickening agents
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    • C10M2203/00Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/06Well-defined aromatic compounds
    • C10M2203/065Well-defined aromatic compounds used as base material
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    • C10M2205/00Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/026Butene
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    • C10M2205/00Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/026Butene
    • C10M2205/0265Butene used as base material
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    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/02Hydroxy compounds
    • C10M2207/023Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings
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    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/127Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids polycarboxylic
    • C10M2207/1276Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids polycarboxylic used as thickening agent
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    • C10M2207/125Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/128Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof
    • C10M2207/1285Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof used as thickening agents
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    • C10M2207/28Esters
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    • C10M2207/2855Esters of aromatic polycarboxylic acids used as base material
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    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/30Complex esters, i.e. compounds containing at leasst three esterified carboxyl groups and derived from the combination of at least three different types of the following five types of compounds: monohydroxyl compounds, polyhydroxy xompounds, monocarboxylic acids, polycarboxylic acids or hydroxy carboxylic acids
    • C10M2207/301Complex esters, i.e. compounds containing at leasst three esterified carboxyl groups and derived from the combination of at least three different types of the following five types of compounds: monohydroxyl compounds, polyhydroxy xompounds, monocarboxylic acids, polycarboxylic acids or hydroxy carboxylic acids used as base material
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    • C10M2213/06Perfluoro polymers
    • C10M2213/062Polytetrafluoroethylene [PTFE]
    • C10M2213/0626Polytetrafluoroethylene [PTFE] used as thickening agents
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    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant Compositions
    • C10M2215/10Amides of carbonic or haloformic acids
    • C10M2215/102Ureas; Semicarbazides; Allophanates
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    • C10M2215/14Containing carbon-to-nitrogen double bounds, e.g. guanidines, hydrazones, semicarbazones
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    • C10N2050/00Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10Semi-solids; greasy
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    • C10N2060/02Reduction, e.g. hydrogenation

Definitions

  • the invention relates to high-temperature lubricants, in particular greases based on an aromatic ester, such as a trimellitic acid ester and mixtures of different trimellitic acid esters and a fully hydrogenated or hydrogenated polyisobutylene or a mixture thereof, a thickener.
  • the invention also relates to the use of this high-temperature grease for continuous use temperatures of up to 250 ° C.
  • the lubricants have to fulfill a number of other tasks: They have to cool, reduce friction, wear and power transmission, protect against corrosion and at the same time have a sealing effect.
  • the high-temperature greases should be quiet.
  • lubricants are not suitable for high-temperature applications because they are destroyed at high temperatures, for example via oxidation and / or thermal decomposition reactions and polymerizations, and their lubricating properties are severely restricted.
  • the lubricant is split into low-molecular volatile components. Their evaporation leads to undesirable changes in viscosity, loss of oil and excessive vapor formation. This results in a loss of the lubricating effect.
  • the lubricants also lose their lubricating effect through polymerization due to the formation of insoluble polymerization products.
  • Synthetic esters are often used as base oils for high-temperature applications because they have very good oxidative, hydrolytic and thermal stability.
  • the lubricants In order to meet the diverse requirements of high-temperature applications, the lubricants must have, among other things, high stability, low coefficients of friction and high wear resistance. In order to be able to guarantee uniform lubrication even at high temperatures, a liquid lubricating film must remain between metal parts during the entire processing process. For this reason, the lubricant must only evaporate a little at the maximum processing temperature, form few residues and form as few cracking residues as possible.
  • lubricants ensure that a separating, load-transferring lubricating film is built up between parts sliding or rolling on each other. This ensures that the metallic surfaces do not touch each other and therefore no wear occurs.
  • the lubricants must therefore meet high requirements. These include extreme operating conditions such as very high or very low speeds, high temperatures caused by high speeds or external heating, very low temperatures, for example with bearings that work in a cold environment or that are used in the air and Space travel occur. Modern lubricants should also be able to be used under so-called clean room conditions in order to avoid room pollution from abrasion or consumption to avoid using lubricants.
  • Lubricants when using modern lubricants, it should be avoided that they evaporate and thus "clog", ie that they become solid after a short application and no longer show any lubricating effect. Special requirements are also placed on lubricants when they are used in such a way that the running surfaces of the bearings are not attacked by low friction, the bearing surfaces run quietly, and long running times are achieved without relubrication. Lubricants also have to withstand the effects of forces such as centrifugal force, gravity and vibrations.
  • the object of the present invention is to provide a high-temperature grease which meets the above-mentioned requirements.
  • the lubricating oil or grease should show a good lubricating effect at high temperature over a long period of time.
  • the cracking residues formed should not be laked up, but should be able to be dissolved again by fresh fat.
  • the high-temperature lubricant should have good hydrolytic stability, be corrosion- and wear-resistant, as well as good oxidation resistance and good low-temperature behavior adapted to the requirements. This is defined for lubricating oils by the pour point and for lubricating greases by the flow pressure at low temperatures.
  • the high-temperature grease should exhibit good noise behavior, have long running times and essentially cause no signs of wear on the devices.
  • the DE 10 2006 043 747 A1 discloses the use of trimelite ester base materials in conjunction with polyol ester compounds and a complex ester base material and an additive package for providing a high-temperature oil. On the basis of this composition, it is to be expected that the formulations based purely on esters tend to lye.
  • the EP 2 714 872 B1 discloses a high-temperature oil based on aromatic esters, such as trimellitic acid esters, pyromellitic acid esters, trimesic acid or mixtures thereof and hydrogenated polyisobutylene, which is provided without a solubilizer, so as to avoid evaporation losses in the Avoid application.
  • aromatic esters such as trimellitic acid esters, pyromellitic acid esters, trimesic acid or mixtures thereof and hydrogenated polyisobutylene, which is provided without a solubilizer, so as to avoid evaporation losses in the Avoid application.
  • the US 2006/0073989 A1 relates to a grease composition used at high temperatures and speeds in electrical parts of automobiles or auxiliary machines of engines and consists of an aromatic ester oil such as trimellitic ester oil or pyromellitic ester oil and a diurea thickener.
  • the high-temperature grease according to the invention shows high thermal stability combined with a long service life and good lubricating properties.
  • the high-temperature grease according to the invention comprises, as an ester compound, a trimellitic acid ester or a mixture of different trimellitic acid esters, the alcohol group of the ester being a linear or branched alkyl group having 8 to 16 carbon atoms.
  • the properties of the lubricant for example the viscosity, the viscosity-temperature behavior, the oxidation resistance and residue behavior can be adjusted.
  • the high temperature grease according to the invention can contain a second oil which comprises an alkyl aromatic.
  • An aromatic is preferably used.
  • an aromatic is understood to mean a monocyclic, bicyclic or tricyclic ring system with four to fifteen carbon atoms, the monocyclic ring system being aromatic or at least one of the rings in a bicyclic or tricyclic ring system being aromatic.
  • a bicyclic ring system which preferably has 10 carbon atoms, is preferably used.
  • the aromatic is preferably substituted by one or more aliphatic substituents.
  • the aromatic is particularly preferably substituted with one to four aliphatic substituents and in particular with two or three aliphatic substituents.
  • an alkyl group is a saturated aliphatic hydrocarbon group having 1 to 30, preferably 3 to 20, more preferably 4 to 17 and in particular 6 to 15 carbon atoms.
  • An alkyl group can be linear or branched and is optionally substituted with one or more of the above-mentioned substituents.
  • the high-temperature grease according to the invention further comprises a polyisobutylene.
  • the polyisobutylene can be used in hydrogenated or fully hydrogenated form, and a mixture of hydrogenated and fully hydrogenated polyisobutylene can also be used. Fully hydrogenated polyisobutylenes are preferably used.
  • the polyisobutylene is present in the composition in an amount of 6 to 45% by weight, preferably 10 to 45% by weight, in particular 15 to 45% by weight, are used.
  • the polyisobutylene has a number average molecular weight of 115 to 10,000 g / mol, preferably 160 to 5000 g / mol.
  • the high-temperature grease according to the invention also comprises from 0.1 to 10% by weight, additives, which are used individually or in combination and are selected from the group consisting of corrosion protection additives, antioxidants, wear protection additives, UV stabilizers, inorganic or organic solid lubricants.
  • the high-temperature grease according to the invention also comprises a thickening agent.
  • the thickener in the high-temperature grease of the lubricant composition according to the invention is either a reaction product of a diisocyanate, preferably 2,4-diisocyanatotoluene, 2,6-diisocyanatotoluene, 4,4'-diisocyanatodiphenylmethane, 2,4'-diisocyanatophenylmethane, 4,4'-diisocyanatodi- phenyl, 4,4'-diisocyanato-3-3'-dimethylphenyl, 4,4'-diisocyanato-3,3'-dimethylphenylmethane, which can be used individually or in combination, with an amine of the general formula R ' 2 -NR , or a diamine of the general formula R ' 2 -NR-NR' 2 , where R is an aryl, alky
  • additives for high-temperature greases have particularly good physical and chemical properties:
  • the addition of antioxidants can reduce or even prevent the oxidation of the oil or fat according to the invention, especially when it is used. In the event of oxidation, undesirable free radicals can arise and, as a result, more decomposition reactions of the high-temperature lubricant occur.
  • the high temperature fat is stabilized by adding antioxidants.
  • Antioxidants particularly suitable according to the invention are the following compounds: Styrenated diphenylamines, diaromatic amines, phenolic resins, thiophenolic resins, phosphites, butylated hydroxytoluene, butylated hydroxyanisole, phenyl-alphanaphthylamine, phenyl-beta-naphthylamine, octylated / butylated diphenylamine, dialpha-tocopherol, phenyl-phenyl-phenol, sulfur-propane, phenyl-tert-butyl-phenyl compounds , Phenolic compounds and mixtures of these components.
  • the high-temperature grease can also contain corrosion protection additives, metal deactivators or ion complexing agents. These include triazoles, imidazolines, N-methylglycine (sarcosine), benzotriazole derivatives, N, N-bis (2-ethylhexyl) -ar-methyl-1H-benzotriazole-1-methanamine; n-Methyl-N (1-oxo-9-octadecenyl) glycine, mixture of phosphoric acid and mono- and diisooctyl esters reacted with (C 11-14 ) -alkylamines, mixture of phosphoric acid and mono- and diisooctyl esters reacted with tert-alkylamine and primary (C 12-14 ) amines, dodecanoic acid, triphenyl phosphorothionate and amine phosphates.
  • metal deactivators or ion complexing agents include triazoles, imidazolines,
  • IRGAMET® 39 IRGACOR® DSS G, amine O; SARKOSYL® O (Ciba), COBRATEC® 122, CUVAN® 303, VANLUBE® 9123, CI-426, CI-426EP, CI-429 and CI-498.
  • anti-wear additives are amines, amine phosphates, phosphates, thiophosphates, phosphorothionates and mixtures of these components.
  • the commercially available anti-wear additives include IRGALUBE® TPPT, IRGALUBE® 232, IRGALUBE® 349, IRGALUBE® 211 and ADDITIN® RC3760 Liq 3960, FIRC-SHUN® FG 1505 and FG 1506, NA-LUBE® KR-015FG, LUBEBOND .®, FLUORBOND ® FG, SYNALOX® 40-D, ACHESON® FGA 1820 and ACHESON® FGA 1810.
  • the grease can contain solid lubricants such as PTFE, BN, pyrophosphate, Zn oxide, Mg oxide, pyrophosphates, thiosulfates, Mg carbonate, Ca carbonate, Ca stearate, Zn sulfide, Mo sulfide, W sulfide, Sn -Sulfide, graphite, graphene, nanotubes, SiO 2 modifications or a mixture thereof.
  • solid lubricants such as PTFE, BN, pyrophosphate, Zn oxide, Mg oxide, pyrophosphates, thiosulfates, Mg carbonate, Ca carbonate, Ca stearate, Zn sulfide, Mo sulfide, W sulfide, Sn -Sulfide, graphite, graphene, nanotubes, SiO 2 modifications or a mixture thereof.
  • the high-temperature grease according to the invention can contain, as a further base oil, an oil, preferably selected from the group consisting of mineral oil, aliphatic carboxylic acid and dicarboxylic acid esters, fatty acid triglycerides, pyromellitic acid esters, diphenyl ethers, phloroglucinic esters and / or poly-alpha-olefins, alpha-olefin copolymers.
  • an oil preferably selected from the group consisting of mineral oil, aliphatic carboxylic acid and dicarboxylic acid esters, fatty acid triglycerides, pyromellitic acid esters, diphenyl ethers, phloroglucinic esters and / or poly-alpha-olefins, alpha-olefin copolymers.
  • the high-temperature grease according to the invention due to its physical and chemical properties, is excellent for use in chains, roller and plain bearings, in vehicle technology, conveyor technology, mechanical engineering, office technology and in industrial systems and machines, but also in the Areas of household machines and consumer electronics. Due to its good temperature resistance, it can also be used at high operating temperatures of up to 260 ° C, preferably at temperatures of 150 to 250 ° C.
  • the invention also relates to a method for producing the above-described high-temperature grease, in which the base oils and the additives are mixed with one another.
  • Estolides or aliphatically substituted naphthalenes are placed in a stirred tank. At 100 ° C., the polyisobutylene and, if necessary, a further oil are added with stirring. Then the mixture is stirred for 1 hour to obtain a homogeneous mixture. The anti-wear agents and the antioxidant are added to the kettle at 60 ° C. while stirring. After approx. 1 hour, the finished oil can be filled into the containers provided.
  • the base oil is placed in a stirred tank. At 100 ° C., the polyisobutylene and, if necessary, a further oil and the thickener are added with stirring. The thickener results from an in situ reaction of the reactants used in the base oil. The mixture is then heated to 150 ° C. to 210 ° C., stirred for several hours and cooled again. In the cooling process at approx. 60 ° C, the necessary wear protection agents, antioxidants and corrosion protection agents are added. A homogeneous mixture of the fat is obtained by the final homogenization step using a roller, colloid mill or the Gaulin.
  • compositions of the high-temperature greases are shown in Table 6, Examples 3 and 6 relating to a composition according to the invention. ⁇ u> Table 6 ⁇ /u> Type Li complex Li complex Li complex Di-urea Di-urea Di-urea Example 3 Example 4 Example 5 Example 6 Example 7 Example 8 Trimellitic acid ester [wt.
  • Oil separation has a decisive influence on the lubricating effect of a grease. It must be ensured that, on the one hand, the oil separation is not too high and the oil runs out of the bearing and is therefore no longer available to the tribo-system and, on the other hand, no oil separation can be observed and the lubricating effect of the grease is lost.
  • the oil separation should ideally be between 0.5 and 8% by weight so that an optimal lubricating film can form in the bearing.
  • Table 8 shows that the running times due to the use of PIB in conjunction with various base oils have long running times and are therefore suitable for high application temperatures in continuous operation.
  • Example 3 The properties of the fat according to Example 3, in which fully hydrogenated PIB was used, was now compared with a fat (comparative example 3) that contained a PIB in which double bonds were still present, that is to say a not fully hydrogenated PIB.
  • the other composition of the fat according to comparative example 3 corresponded to that of example 3.

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Description

Die Erfindung betrifft Hochtemperaturschmierstoffe, insbesondere Fette auf Basis eines aromatischen Esters, wie eines Trimellitsäureesters und Mischungen verschiedener Trimellitsäureester und einem vollhydrierten oder hydrierten Polyisobutylen oder einer Mischung daraus, einem Verdickungsmittel. Die Erfindung betrifft ferner die Verwendung dieses Hochtemperaturfetts für Dauereinsatztemperaturen von bis zu 250°C.The invention relates to high-temperature lubricants, in particular greases based on an aromatic ester, such as a trimellitic acid ester and mixtures of different trimellitic acid esters and a fully hydrogenated or hydrogenated polyisobutylene or a mixture thereof, a thickener. The invention also relates to the use of this high-temperature grease for continuous use temperatures of up to 250 ° C.

Neben der Schmierwirkung müssen die Schmierstoffe noch eine Vielzahl weiterer Aufgaben erfüllen: Sie müssen kühlen, Reibung, Verschleiß und Kraftübertragung verringern, vor Korrosion schützen und gleichzeitig eine dichtende Wirkung aufweisen. Darüber hinaus sollten die Hochtemperaturfette geräuscharm sein.In addition to the lubricating effect, the lubricants have to fulfill a number of other tasks: They have to cool, reduce friction, wear and power transmission, protect against corrosion and at the same time have a sealing effect. In addition, the high-temperature greases should be quiet.

Herkömmliche Schmierstoffe sind für Hochtemperaturanwendungen nicht geeignet, da sie bei hohen Temperaturen beispielsweise über Oxidations- und/oder thermische Zersetzungsreaktionen und Polymerisationen zerstört werden und ihre schmierenden Eigenschaften stark eingeschränkt werden. Bei Zersetzungsreaktionen wird der Schmierstoff in niedermolekulare flüchtige Komponenten gespalten. Deren Verdampfen führt zu unerwünschten Viskositätsänderungen, Ölverlust und zur übermäßigen Dampfbildung. Hieraus resultiert ein Verlust der Schmierwirkung. Auch durch Polymerisation verlieren die Schmierstoffe ihre Schmierwirkung aufgrund der Bildung unlöslicher Polymerisationsprodukte.Conventional lubricants are not suitable for high-temperature applications because they are destroyed at high temperatures, for example via oxidation and / or thermal decomposition reactions and polymerizations, and their lubricating properties are severely restricted. During decomposition reactions, the lubricant is split into low-molecular volatile components. Their evaporation leads to undesirable changes in viscosity, loss of oil and excessive vapor formation. This results in a loss of the lubricating effect. The lubricants also lose their lubricating effect through polymerization due to the formation of insoluble polymerization products.

Das Entfernen dieser Verschmutzungen erhöht die Wartungsarbeiten und produziert chemische Abfallstoffe, die aufwendig entsorgt werden müssen. Aufgrund der vermehrten Reinigungs- und Wartungsarbeiten erhöhen sich die Ausfallzeiten. Insgesamt führt die Verwendung von ungeeigneten Schmierstoffen bei Hochtemperaturanwendungen zu höheren Kosten, da die Arbeitsgeräte verschmutzen und ein höherer Bedarf an Schmierstoffen besteht. Darüber hinaus sinkt die Produktqualität.Removing this contamination increases maintenance work and produces chemical waste that is laborious to dispose of. Due to the increased cleaning and maintenance work, the Downtime. Overall, the use of unsuitable lubricants in high-temperature applications leads to higher costs, since the tools become dirty and there is a higher demand for lubricants. In addition, the product quality decreases.

Als Basisöle für Hochtemperaturanwendungen werden oftmals synthetische Ester eingesetzt, da diese über eine sehr gute oxidative, hydrolytische und thermische Stabilität verfügen.Synthetic esters are often used as base oils for high-temperature applications because they have very good oxidative, hydrolytic and thermal stability.

Um den vielfältigen Anforderungen bei Hochtemperaturanwendungen gerecht zu werden, müssen die Schmierstoffe unter anderem eine hohe Stabilität, niedrige Reibungsbeiwerte und hohe Verschleißfestigkeiten aufweisen. Um eine gleichmäßige Schmierung auch bei hohen Temperaturen gewährleisten zu können, muss während des gesamten Verarbeitungsprozesses ein flüssiger Schmierfilm zwischen Metallteilen bestehen bleiben. Deshalb darf der Schmierstoff bei der maximalen Verarbeitungstemperatur nur wenig verdampfen, wenig Rückstände bilden und möglichst wenig Vercrackungsrückstände bilden.In order to meet the diverse requirements of high-temperature applications, the lubricants must have, among other things, high stability, low coefficients of friction and high wear resistance. In order to be able to guarantee uniform lubrication even at high temperatures, a liquid lubricating film must remain between metal parts during the entire processing process. For this reason, the lubricant must only evaporate a little at the maximum processing temperature, form few residues and form as few cracking residues as possible.

Hohe Temperaturen treten oftmals bei der Verwendung in Ketten, Wälz- und Gleitlagern, in der Fahrzeugtechnik, der Fördertechnik, dem Maschinenbau, der Bürotechnik sowie in industriellen Anlagen und Maschinen, aber auch in den Bereichen der Haushaltsmaschinen und der Unterhaltungselektronik.High temperatures often occur when used in chains, roller and plain bearings, in vehicle technology, conveyor technology, mechanical engineering, office technology and in industrial systems and machines, but also in the areas of household machines and entertainment electronics.

In Wälz- und Gleitlagern sorgen Schmierstoffe dafür, dass zwischen aufeinander gleitenden oder abrollenden Teilen ein trennender, lastübertragender Schmierfilm aufgebaut wird. Damit wird erreicht, dass die metallischen Oberflächen sich nicht berühren und somit auch kein Verschleiß auftritt. Die Schmierstoffe müssen deshalb hohen Anforderungen genügen. Dazu gehören extreme Betriebsbedingungen, wie sehr hohe oder sehr niedrige Drehzahlen, hohe Temperaturen, die durch hohe Drehzahlen oder durch Fremderwärmung bedingt sind, sehr tiefe Temperaturen, beispielsweise bei Lagern, die in kalter Umgebung arbeiten oder, die bei der Verwendung in der Luft- und Raumfahrt auftreten. Ebenso sollten die modernen Schmierstoffe unter sogenannten Reinraumbedingungen einsetzbar sein, um die Raumverschmutzung durch den Abrieb bzw. den Verbrauch an Schmierstoffen zu vermeiden. Außerdem sollte bei der Anwendung der modernen Schmierstoffe vermieden werden, dass sie verdampfen und damit "verlacken", d.h., dass sie nach kurzer Anwendung fest werden und keine Schmierwirkung mehr zeigen. An Schmierstoffe werden auch besondere Anforderungen bei der Anwendung dahingehend gestellt, dass die Laufflächen der Lager durch geringe Reibung nicht angegriffen werden, die Lagerflächen geräuscharm laufen, sowie langen Laufzeiten ohne Nachschmierung erreicht werden. Auch müssen Schmierstoffe Krafteinwirkungen, wie Fliehkraft, Schwerkraft und Schwingungen widerstehen.In roller and plain bearings, lubricants ensure that a separating, load-transferring lubricating film is built up between parts sliding or rolling on each other. This ensures that the metallic surfaces do not touch each other and therefore no wear occurs. The lubricants must therefore meet high requirements. These include extreme operating conditions such as very high or very low speeds, high temperatures caused by high speeds or external heating, very low temperatures, for example with bearings that work in a cold environment or that are used in the air and Space travel occur. Modern lubricants should also be able to be used under so-called clean room conditions in order to avoid room pollution from abrasion or consumption to avoid using lubricants. In addition, when using modern lubricants, it should be avoided that they evaporate and thus "clog", ie that they become solid after a short application and no longer show any lubricating effect. Special requirements are also placed on lubricants when they are used in such a way that the running surfaces of the bearings are not attacked by low friction, the bearing surfaces run quietly, and long running times are achieved without relubrication. Lubricants also have to withstand the effects of forces such as centrifugal force, gravity and vibrations.

Wichtige Kenngröße für eine lange Funktionsdauer eines fettgeschmierten Wälzlagers im Hochtemperaturbereich ist neben der oberen Gebrauchstemperatur das Geräuschverhalten des Schmierstoffes. Ein Schmierfett kann bei Umlaufteilnahme (Überrollung, Walkung) Schwingungen im Wälzlager anregen, die als "Schmierstoffgeräusche" in den Frequenzbändern Medium 300 bis 1.800 Hz und High 1.800 bis 10.000 Hz, gegenüber den Lagergeräuschen im Frequenzband Low bei 50 bis 300 Hz liegen. Das Schmierstoffgeräusch wird von den Geräuschspitzen überlagert, die bei der Überrollung von harten Partikeln durch die Wälzkörper in Form von Stoßimpulsen auf dem Lagerring entstehen. Die Bewertung des Geräuschverhaltens erfolgt nach der SKF-BeQuiet+ - MethodeDie Fettgeräuschklasse werden wie folgt eingeteilt:

  • GNX: etwas schlechter als GN1 (sehr schlechtes Geräuschverhalten)
  • GN1: >95% aller Peaks sind <=40 µm/s (schlechtes Geräuschverhalten)
  • GN2: >95% aller Peaks sind <=20 µm/s; > 98% aller Peaks sind <= 40 µm/s (mittleres Geräuschverhalten)
  • GN3: >95% aller Peaks sind <=10 µm/s; > 98% aller Peaks sind <= 20 µm/s; > 100% aller Peaks sind <= 40 µm/s (gutes Geräuschverhalten)
  • GN4: >95% aller Peaks sind <= 5 µm/s; > 98% aller Peaks sind <= 10 µm/s; > 100% aller Peaks sind <= 20 µm/s (sehr gutes Geräuschverhalten)
An important parameter for a long service life of a grease-lubricated roller bearing in the high temperature range is, in addition to the upper service temperature, the noise behavior of the lubricant. A lubricating grease can stimulate vibrations in the rolling bearing when it participates in circulation (rolling over, flexing), which are "lubricant noises" in the medium 300 to 1,800 Hz and high 1,800 to 10,000 Hz frequency bands, compared to the bearing noise in the low frequency band at 50 to 300 Hz. The lubricant noise is superimposed by the noise peaks that occur when hard particles roll over the rolling elements in the form of shock pulses on the bearing ring. The evaluation of the noise behavior is based on the SKF BeQuiet + method.
  • GNX: slightly worse than GN1 (very poor noise behavior)
  • GN1: > 95% of all peaks are <= 40 µm / s (poor noise behavior)
  • GN2: > 95% of all peaks are <= 20 µm / s; > 98% of all peaks are <= 40 µm / s (average noise behavior)
  • GN3: > 95% of all peaks are <= 10 µm / s; > 98% of all peaks are <= 20 µm / s; > 100% of all peaks are <= 40 µm / s (good noise behavior)
  • GN4: > 95% of all peaks are <= 5 µm / s; > 98% of all peaks are <= 10 µm / s; > 100% of all peaks are <= 20 µm / s (very good noise behavior)

Je besser das Geräuschverhalten eines Schmierfettes, desto geringer sind die durch den Schmierstoff erzwungenen Schwingungen des Lagers. Dies ist gleichbedeutend mit einer geringen Belastung des Lagers und führt zu einer längeren Funktionsdauer der Lagerung.The better the noise behavior of a lubricating grease, the lower the vibrations of the bearing caused by the lubricant. This is equivalent to a low load on the bearing and leads to a longer service life of storage.

Die Aufgabe der vorliegenden Erfindung besteht darin, ein Hochtemperaturfett bereitzustellen, das den oben genannten Anforderungen entspricht. Insbesondere soll das Schmieröl- bzw. fett bei hoher Temperatur über einen langen Zeitraum eine gute Schmierwirkung zeigen. Des weiteren sollen die gebildeten Vercrackungsrückstände nicht verlacken, sondern durch Frischfett wieder anlösbar sein. Ferner soll der Hochtemperaturschmierstoff eine gute hydrolytische Stabilität aufweisen, korrosions- und verschleißresistent sein, sowie eine gute Oxidationsbeständigkeit und ein an die Anforderung angepasstes gutes Tieftemperaturverhalten besitzen. Dies wir bei Schmierölen durch den Pourpoint und bei Schmierfetten durch den Fließdruck bei tiefen Temperaturen definiert. Außerdem soll das Hochtemperaturfett ein gutes Geräuschverhalten zeigen, lange Laufzeiten aufweisen und im wesentlichen keine Verschleißerscheinungen der Vorrichtungen bewirken.The object of the present invention is to provide a high-temperature grease which meets the above-mentioned requirements. In particular, the lubricating oil or grease should show a good lubricating effect at high temperature over a long period of time. Furthermore, the cracking residues formed should not be laked up, but should be able to be dissolved again by fresh fat. Furthermore, the high-temperature lubricant should have good hydrolytic stability, be corrosion- and wear-resistant, as well as good oxidation resistance and good low-temperature behavior adapted to the requirements. This is defined for lubricating oils by the pour point and for lubricating greases by the flow pressure at low temperatures. In addition, the high-temperature grease should exhibit good noise behavior, have long running times and essentially cause no signs of wear on the devices.

Es ist aus der EP 0 892 038 A1 bekannt Schmierfettzusammensetzungen bestehend aus einem oder mehreren Estern aromatischer Tri- oder Tetracarbonsäuren mit einem Alkohol und/oder einem oder mehrerer Ester von Trimethylolpropan, Pentaerytritol oder Dipentaerytritol mit aliphatischen Carbonsäuren, einem Verdickungsmittel auf Harnstoffbasis und Verschleißschutzmitteln. Eine Verwendung von Polymeren, insbesondere teil- oder vollhydrierte Polyisobutylene, ist nicht beschrieben.It's from the EP 0 892 038 A1 known lubricating grease compositions consisting of one or more esters of aromatic tri- or tetracarboxylic acids with an alcohol and / or one or more esters of trimethylolpropane, pentaerytritol or dipentaerytritol with aliphatic carboxylic acids, a urea-based thickener and anti-wear agents. The use of polymers, in particular partially or fully hydrogenated polyisobutylenes, is not described.

Die DE 10 2006 043 747 A1 offenbart die Verwendung von Trimelittatestergrundstoffen in Verbindung mit Polyolesterverbindungen und einem Komplexester-Grundstoff sowie einem Additivpaket zur Bereitstellung eines Hochtemperaturöls. Auf Grund dieser Zusammensetzung ist zu erwarten, dass die rein auf Ester aufgebauten Formulierungen zur Verlackung neigen.The DE 10 2006 043 747 A1 discloses the use of trimelite ester base materials in conjunction with polyol ester compounds and a complex ester base material and an additive package for providing a high-temperature oil. On the basis of this composition, it is to be expected that the formulations based purely on esters tend to lye.

Die EP 2 714 872 B1 offenbart eine Hochtemperaturöl auf der Basis von aromatischen Estern, wie beispielsweise Trimellitsäueester, Pyromellitsäureester, Trimesinsäure oder deren Mischungen und hydriertem Polyisobutylen, das ohne Lösungsvermittlers bereitgestellt wird, um so Verdampfungsverlusten bei der Anwendung zu vermeiden.The EP 2 714 872 B1 discloses a high-temperature oil based on aromatic esters, such as trimellitic acid esters, pyromellitic acid esters, trimesic acid or mixtures thereof and hydrogenated polyisobutylene, which is provided without a solubilizer, so as to avoid evaporation losses in the Avoid application.

Die US 2006/0073989 A1 betrifft eine Fettzusammensetzung, die bei hohen Temperaturen und Geschwindigkeiten in elektrischen Teilen von Kraftfahrzeugen oder Hilfsmaschinen von Motoren verwendet wird und besteht aus einem aromatischen Esteröl, wie beispielsweise Trimellitsäueesteröl oder Pyromellitsäureesteröl und einem Diharnstoffverdickungsmittel.The US 2006/0073989 A1 relates to a grease composition used at high temperatures and speeds in electrical parts of automobiles or auxiliary machines of engines and consists of an aromatic ester oil such as trimellitic ester oil or pyromellitic ester oil and a diurea thickener.

Diese Aufgabe wird erfindungsgemäß durch ein Hochtemperaturfett umfassend folgende Komponenten gelöst:

  1. a) 91,9 bis 25 Gew.-% mindestens eines Öls, ausgewählt aus der Gruppe bestehend aus Trimellitsäureestern, oder einem Gemisch aus verschiedenen Trimellitsäureestern, bei dem die Alkoholgruppe des Esters eine lineare oder verzweigte Alkylgruppe mit 8 bis 16 Kohlenstoffatomen ist,
  2. b) 6 bis 45 Gew.% eines Polymers, nämlich eines hydrierten oder vollhydrierten Polyisobutylen oder einer Mischung aus hydrierten oder vollhydrierten Polyisobutylen;
  3. c) 0,1 bis 10 Gew.-% Additive einzeln oder in Kombination, ausgewählt aus der Gruppe bestehend aus Korrosionsschutzadditiven, Antioxidantien, Verschleißschutzadditiven, UV-Stabilisatoren, anorganischen oder organischen Feststoffschmierstoffen und
  4. d) 2 bis 20 Gew.-% Verdickungsmittel.
According to the invention, this object is achieved by a high-temperature grease comprising the following components:
  1. a) 91.9 to 25% by weight of at least one oil selected from the group consisting of trimellitic acid esters, or a mixture of different trimellitic acid esters, in which the alcohol group of the ester is a linear or branched alkyl group with 8 to 16 carbon atoms,
  2. b) 6 to 45% by weight of a polymer, namely a hydrogenated or fully hydrogenated polyisobutylene or a mixture of hydrogenated or fully hydrogenated polyisobutylene;
  3. c) 0.1 to 10% by weight of additives, individually or in combination, selected from the group consisting of corrosion protection additives, antioxidants, wear protection additives, UV stabilizers, inorganic or organic solid lubricants and
  4. d) 2 to 20% by weight of thickener.

Überraschend wurde gefunden, dass sich das Hochtemperaturfett durch eine hervorragende Leistungsfähigkeit auszeichnen. So zeigt das erfindungsgemäße Hochtemperaturfett eine hohe thermische Stabilität kombiniert mit einer hohen Lebensdauer und guten Schmiereigenschaften.Surprisingly, it was found that the high-temperature grease is characterized by excellent performance. The high-temperature grease according to the invention shows high thermal stability combined with a long service life and good lubricating properties.

Das erfindungsgemäße Hochtemperaturfett umfasst als eine Esterverbindung einen Trimellitsäureester oder ein Gemisch aus verschiedenen Trimellitsäureestern, wobei die Alkoholgruppe des Esters eine lineare oder verzweigte Alkylgruppe mit 8 bis 16 Kohlenstoffatomen ist. Je nach Wahl des aromatischen Esters können die Eigenschaften des Schmierstoffs, beispielsweise die Viskosität, das Viskositäts-Temperatur-Verhalten, die Oxidationsbeständigkeit und Rückstandsverhalten angepasst werden.The high-temperature grease according to the invention comprises, as an ester compound, a trimellitic acid ester or a mixture of different trimellitic acid esters, the alcohol group of the ester being a linear or branched alkyl group having 8 to 16 carbon atoms. Depending on the choice of aromatic ester, the properties of the lubricant, for example the viscosity, the viscosity-temperature behavior, the oxidation resistance and residue behavior can be adjusted.

Das erfindungsgemäße Hochtemperaturfett kann ein zweites Öl enthalten, das einen Alkylaromaten umfasst. Bevorzugt wird ein Aromat eingesetzt. Unter einem Aromaten wird erfindungsgemäß ein monocyclisches, bicyclisches oder tricyclisches Ringsystem mit vier bis fünfzehn Kohlenstoffatomen verstanden, wobei das monocyclische Ringsystem aromatisch ist oder zumindest einer der Ringe in einem bi- oder tricylischen Ringsystem aromatisch ist. Bevorzugt wird ein bicyclisches Ringsystem, das vorzugsweise 10 Kohlenstoffatome aufweist, eingesetzt.The high temperature grease according to the invention can contain a second oil which comprises an alkyl aromatic. An aromatic is preferably used. According to the invention, an aromatic is understood to mean a monocyclic, bicyclic or tricyclic ring system with four to fifteen carbon atoms, the monocyclic ring system being aromatic or at least one of the rings in a bicyclic or tricyclic ring system being aromatic. A bicyclic ring system, which preferably has 10 carbon atoms, is preferably used.

Bevorzugt ist der Aromat mit einem oder mehreren aliphatischen Substituenten substituiert. Besonders bevorzugt ist der Aromat mit ein bis vier aliphatischen Substituenten und insbesondere mit zwei oder drei aliphatischen Substituenten substituiert.The aromatic is preferably substituted by one or more aliphatic substituents. The aromatic is particularly preferably substituted with one to four aliphatic substituents and in particular with two or three aliphatic substituents.

Eine Alkylgruppe ist erfindungsgemäß eine gesättigte aliphatische Kohlenwasserstoffgruppe mit 1 bis 30, vorzugsweise 3 bis 20, noch bevorzugter 4 bis 17 und insbesondere 6 bis 15 Kohlenstoffatomen. Eine Alkylgruppe kann linear oder verzweigt sein und ist wahlweise mit einem oder mehreren der oben genannten Substituenten substituiert.According to the invention, an alkyl group is a saturated aliphatic hydrocarbon group having 1 to 30, preferably 3 to 20, more preferably 4 to 17 and in particular 6 to 15 carbon atoms. An alkyl group can be linear or branched and is optionally substituted with one or more of the above-mentioned substituents.

Das erfindungsgemäße Hochtemperaturfett umfasst des weiteren ein Polyisobutylen. Durch geeignete Wahl des Polyisobutylens, insbesondere im Hinblick auf Hydrierungsgrad und Molekulargewicht, können die Eigenschaften des erfindungsgemäßen Fetts, beispielsweise deren kinematische Viskosität, in erwünschter Weise beeinflusst werden. Das Polyisobutylen kann in hydrierter oder vollhydrierter Form eingesetzt werden, ebenso kann eine Mischung aus hydriertem und vollhydriertem Polyisobutylen verwendet werden. Bevorzugt werden vollhydrierte Polyisobutylene eingesetzt. Das Polyisobutylen ist in einer Menge von 6 bis 45 Gew.-% in der Zusammensetzung vorhanden, bevorzugt werden 10 bis 45 Gew.-%, insbesondere 15 bis 45 Gew.-% eingesetzt.The high-temperature grease according to the invention further comprises a polyisobutylene. A suitable choice of polyisobutylene, in particular with regard to the degree of hydrogenation and molecular weight, can influence the properties of the fat according to the invention, for example its kinematic viscosity, in the desired manner. The polyisobutylene can be used in hydrogenated or fully hydrogenated form, and a mixture of hydrogenated and fully hydrogenated polyisobutylene can also be used. Fully hydrogenated polyisobutylenes are preferably used. The polyisobutylene is present in the composition in an amount of 6 to 45% by weight, preferably 10 to 45% by weight, in particular 15 to 45% by weight, are used.

Gemäß einer weiteren bevorzugten Ausführungsform weist das Polyisobutylen ein zahlenmittleres Molekulargewicht von 115 bis 10.000 g/mol, vorzugsweise von 160 bis 5000 g/mol auf.According to a further preferred embodiment, the polyisobutylene has a number average molecular weight of 115 to 10,000 g / mol, preferably 160 to 5000 g / mol.

Das erfindungsgemäße Hochtemperaturfett umfasst des weiteren von 0,1 bis 10 Gew.-%, Additive, die einzeln oder in Kombination eingesetzt werden und aus der Gruppe bestehend aus Korrosionsschutzadditiven, Antioxidantien, Verschleißschutzadditiven, UV-Stabilisatoren, anorganischen oder organischen Feststoffschmierstoffen, ausgewählt werden.The high-temperature grease according to the invention also comprises from 0.1 to 10% by weight, additives, which are used individually or in combination and are selected from the group consisting of corrosion protection additives, antioxidants, wear protection additives, UV stabilizers, inorganic or organic solid lubricants.

Das erfindungsgemäße Hochtemperaturfett umfasst außerdem ein Verdickungsmittel. Das Verdickungsmittel in dem erfindungsgemäßen Hochtemperaturfett der Schmierstoffzusammensetzung ist entweder ein Reaktionsprodukt aus einem Diisocyanat, vorzugsweise 2,4-Diisocyanatotoluol, 2,6-Diisocyanatotoluol, 4,4'-Diisocyanatodiphenylmethan, 2,4'-Diisocyanatophenylmethan, 4,4'-Diisocyanatodi-phenyl, 4,4'-Diisocyanato-3-3'-dimethylphenyl, 4,4'-Diisocyanato-3,3'-dimethylphenylmethan, die einzeln oder in Kombination verwendet werden können, mit einem Amin der allgemeinen Formel R'2-N-R, oder einem Diamin der allgemeinen Formel R'2-N-R-NR'2, wobei R ein Aryl-, Alkyl- oder Alkylenrest mit 2 bis 22 Kohlenstoffatomen ist und R' identisch oder verschieden ein Wasserstoff, ein Alkyl-, Alkylen- oder Arylrest ist, oder mit Gemischen aus Aminen und Diaminen
oder
wird aus gewählt aus Al-Komplexseifen, Metall-Einfachseifen der Elemente der ersten und zweiten Hauptgruppe des Perriodensystems, Metall-Komplexseifen der Elemente der ersten und zweiten Hauptgruppe des Periodensystems, Bentonite, Sulfonate, Silikate, Aerosil, Polyimide oder PTFE oder einer Mischung der vorgenannten Verdickungsmittel.
The high-temperature grease according to the invention also comprises a thickening agent. The thickener in the high-temperature grease of the lubricant composition according to the invention is either a reaction product of a diisocyanate, preferably 2,4-diisocyanatotoluene, 2,6-diisocyanatotoluene, 4,4'-diisocyanatodiphenylmethane, 2,4'-diisocyanatophenylmethane, 4,4'-diisocyanatodi- phenyl, 4,4'-diisocyanato-3-3'-dimethylphenyl, 4,4'-diisocyanato-3,3'-dimethylphenylmethane, which can be used individually or in combination, with an amine of the general formula R ' 2 -NR , or a diamine of the general formula R ' 2 -NR-NR' 2 , where R is an aryl, alkyl or alkylene radical having 2 to 22 carbon atoms and R ', identically or differently, is a hydrogen, an alkyl, alkylene or aryl radical is, or with mixtures of amines and diamines
or
is selected from Al complex soaps, metal single soaps of the elements of the first and second main group of the periodic table, metal complex soaps of the elements of the first and second main group of the periodic table, bentonites, sulfonates, silicates, Aerosil, polyimides or PTFE or a mixture of the above Thickener.

Als Additive für Hochtemperaturfette haben die nachfolgend genannten Additive besonders gute physikalische und chemische Eigenschaften:
Der Zusatz von Antioxidantien kann die Oxidation des erfindungsgemäßen Öls oder Fetts, insbesondere bei seinem Einsatz, verringern oder gar verhindern. Bei einer Oxidation können unerwünschte freie Radikale entstehen und infolgedessen vermehrt Zersetzungsreaktionen des Hochtemperaturschmierstoffes auftreten. Durch die Zugabe von Antioxidantien wird das Hochtemperaturfett stabilisiert.
As additives for high-temperature greases, the following additives have particularly good physical and chemical properties:
The addition of antioxidants can reduce or even prevent the oxidation of the oil or fat according to the invention, especially when it is used. In the event of oxidation, undesirable free radicals can arise and, as a result, more decomposition reactions of the high-temperature lubricant occur. The high temperature fat is stabilized by adding antioxidants.

Erfindungsgemäß besonders geeignete Antioxidantien sind die folgenden Verbindungen:
Styrolisierte Diphenylamine, diaromatische Amine, Phenolharze, Thiophenolharze, Phosphite, butyliertes Hydroxytoluol, butyliertes Hydroxyanisol, Phenyl-alphanaphthylamin, Phenyl-beta-naphthylamin, octyliertes/butyliertes Diphenylamin, dialpha-Tocopherol, di-tert.-butyl-Phenyl, Benzolpropansäure, schwefelhaltige Phenolverbindungen, Phenolverbindungen und Mischungen dieser Komponenten.
Antioxidants particularly suitable according to the invention are the following compounds:
Styrenated diphenylamines, diaromatic amines, phenolic resins, thiophenolic resins, phosphites, butylated hydroxytoluene, butylated hydroxyanisole, phenyl-alphanaphthylamine, phenyl-beta-naphthylamine, octylated / butylated diphenylamine, dialpha-tocopherol, phenyl-phenyl-phenol, sulfur-propane, phenyl-tert-butyl-phenyl compounds , Phenolic compounds and mixtures of these components.

Weiterhin kann das Hochtemperaturfett Korrosionsschutzadditive, Metalldesaktivatoren oder Ionen-Komplexbildner enthalten. Hierzu zählen Triazole, Imidazoline, N-Methylglycin (Sarcosin), Benzotriazolderivate, N,N-Bis(2-ethylhexyl)-ar-methyl-1 H-benzotriazol-1-methanamin; n-Methyl-N(1-oxo-9-octadecenyl)glycin, Gemisch aus Phosphorsäure und Mono-und Diisooctylester umgesetzt mit (C11-14)-Alkylaminen, Gemisch aus Phosphorsäure und Mono-und Diisooctylester umgesetzt mit tert.-Alkylamin und primären (C12-14)-Aminen, Dodekansäure, Triphenylphosphorthionat und Aminphosphate. Kommerziell erhältliche Additive sind die folgenden: IRGAMET® 39, IRGACOR® DSS G, Amin O; SARKOSYL® O (Ciba), COBRATEC® 122, CUVAN® 303, VANLUBE® 9123, CI-426, CI-426EP, CI-429 und CI-498.The high-temperature grease can also contain corrosion protection additives, metal deactivators or ion complexing agents. These include triazoles, imidazolines, N-methylglycine (sarcosine), benzotriazole derivatives, N, N-bis (2-ethylhexyl) -ar-methyl-1H-benzotriazole-1-methanamine; n-Methyl-N (1-oxo-9-octadecenyl) glycine, mixture of phosphoric acid and mono- and diisooctyl esters reacted with (C 11-14 ) -alkylamines, mixture of phosphoric acid and mono- and diisooctyl esters reacted with tert-alkylamine and primary (C 12-14 ) amines, dodecanoic acid, triphenyl phosphorothionate and amine phosphates. Commercially available additives are the following: IRGAMET® 39, IRGACOR® DSS G, amine O; SARKOSYL® O (Ciba), COBRATEC® 122, CUVAN® 303, VANLUBE® 9123, CI-426, CI-426EP, CI-429 and CI-498.

Weitere Verschleißschutzadditive sind Amine, Aminphosphate, Phosphate, Thiophosphate, Phosphorthionate und Mischungen dieser Komponenten. Zu den kommerziell erhältlichen Verschleißschutzadditiven gehören IRGALUBE® TPPT, IRGALUBE® 232, IRGALUBE® 349, IRGALUBE® 211 und ADDITIN® RC3760 Liq 3960, FIRC-SHUN® FG 1505 und FG 1506, NA-LUBE® KR-015FG, LUBEBOND®, FLUORO® FG, SYNALOX® 40-D, ACHESON® FGA 1820 und ACHESON® FGA 1810.Further anti-wear additives are amines, amine phosphates, phosphates, thiophosphates, phosphorothionates and mixtures of these components. The commercially available anti-wear additives include IRGALUBE® TPPT, IRGALUBE® 232, IRGALUBE® 349, IRGALUBE® 211 and ADDITIN® RC3760 Liq 3960, FIRC-SHUN® FG 1505 and FG 1506, NA-LUBE® KR-015FG, LUBEBOND .®, FLUORBOND ® FG, SYNALOX® 40-D, ACHESON® FGA 1820 and ACHESON® FGA 1810.

Des weiteren kann das Fett Festschmierstoffe wie PTFE, BN, Pyrophosphat, Zn-Oxid, Mg-Oxid, Pyrophosphate, Thiosulfate, Mg-Carbonat, Ca-Carbonat, Ca-Stearat, Zn-Sulfid, Mo-sulfid, W-sulfid, Sn-Sulfid, Graphite, Graphen, Nano-Tubes, SiO2-Modifikationen oder eine Mischung daraus enthalten.Furthermore, the grease can contain solid lubricants such as PTFE, BN, pyrophosphate, Zn oxide, Mg oxide, pyrophosphates, thiosulfates, Mg carbonate, Ca carbonate, Ca stearate, Zn sulfide, Mo sulfide, W sulfide, Sn -Sulfide, graphite, graphene, nanotubes, SiO 2 modifications or a mixture thereof.

Praktische Versuche haben gezeigt, dass das erfindungsgemäße Hochtemperaturfett bis zu einer Temperatur von 250°C keine oder zu vernachlässigende Zersetzungserscheinungen aufweist. Hierunter wird verstanden, dass sich weniger als 10% des Schmierstoffs zersetzen.Practical tests have shown that the high-temperature grease according to the invention shows no or negligible decomposition phenomena up to a temperature of 250 ° C. This means that less than 10% of the lubricant decomposes.

Das erfindungsgemäße Hochtemperaturfett kann als ein weiteres Grundöl ein Öl, vorzugsweise ausgewählt aus der Gruppe bestehend aus Mineralöl, aliphatischen Carbonsäure- und Dicarbonsäureestern, Fettsäuretriglyceriden, Pyromellitsäureester, Diphenylether, Phloroglucinester und/oder Poly-alpha-olefinen, alpha-Olefinen-Copolymere enthalten.The high-temperature grease according to the invention can contain, as a further base oil, an oil, preferably selected from the group consisting of mineral oil, aliphatic carboxylic acid and dicarboxylic acid esters, fatty acid triglycerides, pyromellitic acid esters, diphenyl ethers, phloroglucinic esters and / or poly-alpha-olefins, alpha-olefin copolymers.

Praktische Versuche haben gezeigt, dass das erfindungsgemäße Hochtemperaturfett aufgrund seiner physikalischen und chemischen Eigenschaften hervorragend bei der Verwendung in Ketten, Wälz- und Gleitlagern, in der Fahrzeugtechnik, der Fördertechnik, dem Maschinenbau, der Bürotechnik sowie in industriellen Anlagen und Maschinen, aber auch in den Bereichen der Haushaltsmaschinen und der Unterhaltungselektronik ist. Aufgrund seiner guten Temperaturbeständigkeit kann er auch bei hohen Einsatztemperaturen bis 260°C, vorzugsweise bei Temperaturen von 150 bis 250°C eingesetzt werden.Practical tests have shown that the high-temperature grease according to the invention, due to its physical and chemical properties, is excellent for use in chains, roller and plain bearings, in vehicle technology, conveyor technology, mechanical engineering, office technology and in industrial systems and machines, but also in the Areas of household machines and consumer electronics. Due to its good temperature resistance, it can also be used at high operating temperatures of up to 260 ° C, preferably at temperatures of 150 to 250 ° C.

Die Erfindung betrifft ferner ein Verfahren zur Herstellung des oben beschriebenen Hochtemperaturfetts, bei dem die Grundöle und die Additive miteinander vermischt werden.The invention also relates to a method for producing the above-described high-temperature grease, in which the base oils and the additives are mixed with one another.

Die Erfindung wird nun anhand der nachfolgenden Beispiele näher erläutert.The invention will now be explained in more detail with reference to the following examples.

Referenzbeispiele 1 bis 2Reference examples 1 to 2 Herstellung eines HochtemperaturölsProduction of a high temperature oil

Es werden Estolide oder aliphatisch substituierte Naphthaline in einem Rührkessel vorgelegt. Bei 100°C wird unter Rühren das Polyisobutylen und ggf. ein weiteres Öl hinzugegeben. Anschließend wird das Gemisch 1 h gerührt, um eine homogene Mischung zu erhalten. Die Verschleißschutzmittel und das Antioxidationsmittel werden bei 60°C unter Rühren in den Kessel zugegeben. Nach ca. 1 Stunde kann das fertige Öl in die vorgesehenen Gebinde abgefüllt werden.Estolides or aliphatically substituted naphthalenes are placed in a stirred tank. At 100 ° C., the polyisobutylene and, if necessary, a further oil are added with stirring. Then the mixture is stirred for 1 hour to obtain a homogeneous mixture. The anti-wear agents and the antioxidant are added to the kettle at 60 ° C. while stirring. After approx. 1 hour, the finished oil can be filled into the containers provided.

Zusammensetzung der Hochtemperaturöle:Composition of high temperature oils:

Tabelle 1Table 1 Beispiel 1example 1 Vergleichsbeispiel 1Comparative example 1 TrimellitatTrimellitate 0,00.0 63,063.0 Estolid 1Estolide 1 44,044.0 0,00.0 Estolid 2Estolide 2 19,019.0 0,00.0 hydriertes PIBhydrogenated PIB 30,430.4 30,430.4 aminisches Antioxidantamine antioxidant 2,02.0 2,02.0 phenolisches Antioxidantphenolic antioxidant 1,01.0 1,01.0 Verschleißschutz EP/WAWear protection EP / WA 3,53.5 3,53.5 KorrosionsschutzCorrosion protection 0,10.1 0,10.1 Anlösbarkeit derSolvability of the sehr gut (4)very good (4) sehr gut (4)very good (4) RückständeResidues Tabelle 2Table 2 Beispiel 2Example 2 Vergleichsbeispiel 2Comparative example 2 Trimellitat 1Trimellitate 1 00 76,076.0 alkyliertes Naphthalinalkylated naphthalene 76,076.0 0,00.0 hydriertes PIBhydrogenated PIB 20,020.0 20,020.0 aminisches Antioxidantamine antioxidant 4,04.0 4,04.0 Anlösbarkeit derSolvability of the sehr gut (4)very good (4) sehr gut (4)very good (4) RückständeResidues

Die Basisdaten der Ölbeispiele können aus Tabelle 3 entnommen werden. Tabelle 3 Rezeptur Beispiel 1 Vergleichsbeispiel 1 Beispiel 2 Vergleichsbeispiel 2 Eisenmann-Test [250°C, 72h] Anlösbarkeit 4 4 4 4 Basisdaten Flammpunkt (°C) > 250 > 250 > 250 > 250 kin. V40 280,0 270,0 300,0 140,5 kin. V100 29,00 25,0 25,00 16,13 VI 137 120,0 105 121 The basic data of the oil examples can be found in Table 3. <u> Table 3 </u> Recipe example 1 Comparative example 1 Example 2 Comparative example 2 Eisenmann test [250 ° C, 72h] Solvability 4th 4th 4th 4th Basic data Flash point (° C) > 250 > 250 > 250 > 250 kin. V40 280.0 270.0 300.0 140.5 kin. V100 29.00 25.0 25.00 16.13 VI 137 120.0 105 121

Des weiteren wurde das Reibverhalten der Öle im SRV in Anlehnung an DIN 51834-2 und der Verdampfungsverlust im dynamischen TGA gemessen. Die Ergebnisse werden in den Tabellen 4 und 5 gezeigt und sind graphisch in den Figuren 1 und 2 wiedergegeben. Tabelle 4 Beispiel 1 Vergleichsbeispiel 1 Beispiel 2 Vergleichsbeispiel 2 SRV TST (250 N) 50 - 120°C 0,116 0,112 0,156 0,091 120 - 140°C 0,111 0,127 0,155 0,091 140 - 160°C 0,105 0,141 0,158 0,128 160 - 180°C 0,1 0,145 0,163 0,139 180 - 200°C 0,095 0,143 0,171 0,165 200 - 210°C 0,08 0,137 0,177 0,194 210 - 220°C 0,086 0,132 0,175 0,206 220 - 230°C 0,085 0,129 0,179 0,208 230 - 240°C 0,087 0,126 0,185 0,208 240 - 250°C 0,091 0,121 0,189 0,206 250°C isotherm 0,093 0,118 0,186 0,201 Tabelle 5 Beispiel 1 Vergleichsbeispiel 1 Beispiel 2 Vergleichsbeispiel 2 TGA dynamisch 120°C 0,1 0,1 0,1 0,1 140°C 0,3 0,2 0,3 0,2 160°C 0,6 0,5 0,4 0,4 180°C 1 0,9 0,9 0,7 200°C 1,7 1,4 1,8 1,2 220°C 2,8 2,3 3,6 2,2 240°C 4,6 3,7 6,6 3,7 260°C 7,7 5,9 11,7 6,3 Furthermore, the friction behavior of the oils in the SRV was measured based on DIN 51834-2 and the evaporation loss in the dynamic TGA. The results are shown in Tables 4 and 5 and are graphed in FIG Figures 1 and 2 reproduced. <u> Table 4 </u> example 1 Comparative example 1 Example 2 Comparative example 2 SRV TST (250 N) 50 - 120 ° C 0.116 0.112 0.156 0.091 120-140 ° C 0.111 0.127 0.155 0.091 140-160 ° C 0.105 0.141 0.158 0.128 160-180 ° C 0.1 0.145 0.163 0.139 180-200 ° C 0.095 0.143 0.171 0.165 200-210 ° C 0.08 0.137 0.177 0.194 210-220 ° C 0.086 0.132 0.175 0.206 220-230 ° C 0.085 0.129 0.179 0.208 230-240 ° C 0.087 0.126 0.185 0.208 240-250 ° C 0.091 0.121 0.189 0.206 250 ° C isothermal 0.093 0.118 0.186 0,201 example 1 Comparative example 1 Example 2 Comparative example 2 TGA dynamic 120 ° C 0.1 0.1 0.1 0.1 140 ° C 0.3 0.2 0.3 0.2 160 ° C 0.6 0.5 0.4 0.4 180 ° C 1 0.9 0.9 0.7 200 ° C 1.7 1.4 1.8 1.2 220 ° C 2.8 2.3 3.6 2.2 240 ° C 4.6 3.7 6.6 3.7 260 ° C 7.7 5.9 11.7 6.3

Beispiele 3 und 6 sowie Referenzbeispiele 4,5, 7 und 8Examples 3 and 6 and Reference Examples 4, 5, 7 and 8 Herstellung eines erfindungsgemäßen HochtemperaturfettsProduction of a high temperature grease according to the invention

Das Grundöl wird in einem Rührkessel vorgelegt. Bei 100°C wird unter Rühren das Polyisobutylen und ggf. ein weiteres Öl und das Verdickungsmittel hinzugegeben. Das Verdickungsmittel entsteht durch eine in situ-Reaktion der eingesetzten Reaktanten im Grundöl. Anschließend wird das Gemisch auf 150°C bis 210°C erhitzt, mehrere Stunden gerührt und wieder abgekühlt. Im Abkühlprozeß bei ca. 60°C werden die notwendigen Verschleißschutzmittel, Antioxidationsmittel und Korrosionsschutzmittel hinzugegeben. Eine homogene Mischung des Fettes erhält man durch den abschließenden Homogenisierungsschritt über Walze, Kolloidmühle oder die Gaulin.The base oil is placed in a stirred tank. At 100 ° C., the polyisobutylene and, if necessary, a further oil and the thickener are added with stirring. The thickener results from an in situ reaction of the reactants used in the base oil. The mixture is then heated to 150 ° C. to 210 ° C., stirred for several hours and cooled again. In the cooling process at approx. 60 ° C, the necessary wear protection agents, antioxidants and corrosion protection agents are added. A homogeneous mixture of the fat is obtained by the final homogenization step using a roller, colloid mill or the Gaulin.

Die Zusammensetzungen der Hochtemperaturfette sind in Tabelle 6 gezeigt, wobei Beispiele 3 und 6 eine erfindungsgemäße Zusammensetzung betreffen. Tabelle 6 Typ Li-Komplex Li-Komplex Li-Komplex Di-Harnstoff Di-Harnstoff Di-Harnstoff Beispiel 3 Beispiel 4 Beispiel 5 Beispiel 6 Beispiel 7 Beispiel 8 Trimellitsäureester [Gew. %] 60 0 0 65,2 0 0 Estolid [Gew.%] 0 0 56 0 0 65,2 alkyliertes Naphtalin [Gew.%] 0 64 0 0 65,2 0 vollhydriertes Polyisobutylen [Gew.%] 26 25 25 25 25 25 Add itiv-Package [Gew.%] 4 1 4 1 1 1 Verdicker-Konzentration [Gew.%] 10 10 15,0 8,8 8,8 8,8 The compositions of the high-temperature greases are shown in Table 6, Examples 3 and 6 relating to a composition according to the invention. <u> Table 6 </u> Type Li complex Li complex Li complex Di-urea Di-urea Di-urea Example 3 Example 4 Example 5 Example 6 Example 7 Example 8 Trimellitic acid ester [wt. %] 60 0 0 65.2 0 0 Estolide [wt.%] 0 0 56 0 0 65.2 alkylated naphthalene [wt.%] 0 64 0 0 65.2 0 fully hydrogenated polyisobutylene [% by weight] 26th 25th 25th 25th 25th 25th Add itive package [wt.%] 4th 1 4th 1 1 1 Thickener concentration [wt.%] 10 10 15.0 8.8 8.8 8.8

Bei den in den Beispielen 3 bis 8 verwendeten Verdickungsmitteln handelt es sich um:

  • Beispiel 3: LiOH, 12-Hydroxystearinsäure, Azelainsäure,
  • Beispiel 4: LiOH, 12-Hydroxystearinsäure, Azelainsäure,
  • Beispiel 5: LiOH, 12-Hydroxystearinsäure, Azelainsäure,
  • Beispiel 6: Di-Harnstoff; Methylen-Di-phenyl-diisocyanat (MDI), Octylamin, Oleylamin
  • Beispiel 7: Di-Harnstoff; MDI, Octylamin, Oleylamin
  • Beispiel 8: Di-Harnstoff; MDI, Octylamin, Oleylamin
The thickeners used in Examples 3 to 8 are:
  • Example 3: LiOH, 12-hydroxystearic acid, azelaic acid,
  • Example 4: LiOH, 12-hydroxystearic acid, azelaic acid,
  • Example 5: LiOH, 12-hydroxystearic acid, azelaic acid,
  • Example 6: Di-urea; Methylene-diphenyl-diisocyanate (MDI), octylamine, oleylamine
  • Example 7: di-urea; MDI, octylamine, oleylamine
  • Example 8: di-urea; MDI, octylamine, oleylamine

Die allgemeinen Kenndaten der Fettmuster 3 bis 8 werden in Tabelle 7 gezeigt. Tabelle 7 Kenndaten Beispiel 3 Beispiel 4 Beispiel 5 Beispiel 6 Beispiel 7 Beispiel 8 Walpenentration nach 60 DT [DIN ISO 2137] 284 283 278 232 232 300 Walpenentration nach 100000 DT [DIN ISO 2137] 324 319 319 254 254 338 Tropfpunkt [C°] [DIN ISO 2176] >300 >300 >300 >300 280 292 Fließdruck -20°C; [mbar] [DIN 51805] >2000 275 284 575 525 <1400 Fließdruck -30°C; [mbar] [DIN 51805] >2000 425 675 <1400 <1400 <1400 Ölabsch 40°C/168h; [Gew.%] [DIN 51817] 3,80 3 1,70 1,2 0,10 5,60 Ölabsch 150°C/30h; [Gew.%] [FTMS 761 C] 7,4 7,5 2,50 0,20 0,30 5,00 Verdampfungsverlust 150°C/24°C [DIN 58397 Teil 1] 2 5,3 2,50 1,6 3,5 2,1 Wasserbeständigkeit statisch [DIN 51807] 1 2 1,00 0 1 1 The general characteristics of the fat samples 3 to 8 are shown in Table 7. <u> Table 7 </u> Characteristics Example 3 Example 4 Example 5 Example 6 Example 7 Example 8 Walpenentration according to 60 DT [DIN ISO 2137] 284 283 278 232 232 300 Walpenentration according to 100000 DT [DIN ISO 2137] 324 319 319 254 254 338 Drop point [C °] [DIN ISO 2176] > 300 > 300 > 300 > 300 280 292 Flow pressure -20 ° C; [mbar] [DIN 51805] > 2000 275 284 575 525 <1400 Flow pressure -30 ° C; [mbar] [DIN 51805] > 2000 425 675 <1400 <1400 <1400 Oil cut-off 40 ° C / 168h; [% By weight] [DIN 51817] 3.80 3 1.70 1.2 0.10 5.60 Oil cut-off 150 ° C / 30h; [% By weight] [FTMS 761 C] 7.4 7.5 2.50 0.20 0.30 5.00 Evaporation loss 150 ° C / 24 ° C [DIN 58397 part 1] 2 5.3 2.50 1.6 3.5 2.1 Static water resistance [DIN 51807] 1 2 1.00 0 1 1

Die Verdampfungsverluste der verschiedenen Fettmuster bei 150°C nach 30 h liegen zwischen 2% und 5%, was die sehr gute thermische Stabilität dieser Fettkonzepte unterstreicht.
Einen entscheidenden Einfluss auf die Schmierwirkung eines Fettes hat die Ölabscheidung. Dabei ist darauf zu achten, dass einerseits die Ölabscheidung nicht zu hoch ist und das Öl aus dem Lager läuft und somit dem Tribo-System nicht mehr zur Verfügung steht und anderseits keine Ölabscheidung zu beobachten ist und die Schmierwirkung des Fettes verloren geht. Die Ölabscheidung sollte idealerweise zwischen 0,5 und 8 Gew.-% liegen, damit sich ein optimaler Schmierfilm im Lager ausbilden kann.
The evaporation losses of the various fat samples at 150 ° C after 30 hours are between 2% and 5%, which underlines the very good thermal stability of these fat concepts.
Oil separation has a decisive influence on the lubricating effect of a grease. It must be ensured that, on the one hand, the oil separation is not too high and the oil runs out of the bearing and is therefore no longer available to the tribo-system and, on the other hand, no oil separation can be observed and the lubricating effect of the grease is lost. The oil separation should ideally be between 0.5 and 8% by weight so that an optimal lubricating film can form in the bearing.

Die Fette der Beispiele wurden einem FE 9 Wälzlagertest nach DIN 51 821 unterzogen, bei dem die Lebensdauer der untersuchten Fette ermittelt wird und die obere Gebrauchstemperatur von Schmierfetten in Wälzlagern bei mittleren Drehzahlen und mittleren axialen Belastungen bestimmt wird.
Die untersuchten Fette und die Ergebnisse der L10 und L50-Werte sind in Tabelle 8 gezeigt. Tabelle 8 Beispiel 3 Beispiel 4 Beispiel 5 Beispiel 6 Beispiel 7 Beispiel 8 FE 9 [180°C,6000 1/min,1500N] L 50 (h) 249 >100 207 146 >100 >100 L 10 (h) 169 >50 138 72 >50 >50
The greases in the examples were subjected to an FE 9 roller bearing test according to DIN 51 821, in which the service life of the greases examined is determined and the upper service temperature of lubricating greases in roller bearings at medium speeds and medium axial loads is determined.
The fats tested and the results of the L10 and L50 values are shown in Table 8. <u> Table 8 </u> Example 3 Example 4 Example 5 Example 6 Example 7 Example 8 FE 9 [180 ° C, 6000 rpm, 1500N] L 50 (h) 249 > 100 207 146 > 100 > 100 L 10 (h) 169 > 50 138 72 > 50 > 50

Die Tabelle 8 zeigt, dass die Laufzeiten durch die Verwendung von PIB in Verbindung mit verschiedenen Grundölen lange Laufzeiten aufweisen und somit für hohe Anwendungstemperaturen im Dauerbetrieb geeignet sind.Table 8 shows that the running times due to the use of PIB in conjunction with various base oils have long running times and are therefore suitable for high application temperatures in continuous operation.

Des weiteren wurde das Geräuschverhalten nach der Fette nach SKF Be Quiet + gemäß den Beispielen 3 bis 8 gemessen. Die Ergebnisse sind in Tabelle 9 angegeben. Tabelle 9 Beispiel 3 Beispiel 4 Beispiel 5 Beispiel 6 Beispiel 7 Beispiel 8 Geräuschprüfung [BeQuiet+ SKF] GN4 GN3 GN3 GN2 GN3 GN4 In addition, the noise behavior after the SKF Be Quiet + fats according to Examples 3 to 8 was measured. The results are given in Table 9. <u> Table 9 </u> Example 3 Example 4 Example 5 Example 6 Example 7 Example 8 Noise test [BeQuiet + SKF] GN4 GN3 GN3 GN2 GN3 GN4

Das Geräuschverhalten der verschiedenen Fettformulierungen wird durch die Verwendung des vollhydierten Polyisobutylens sehr positiv beeinflußt. Es können mit Ausnahme von Beispiel 6 gute bis sehr gute Geräuscheigenschaften erzielt werden.The use of fully hydrogenated polyisobutylene has a very positive effect on the noise behavior of the various fat formulations. With the exception of Example 6, good to very good noise properties can be achieved.

Die Eigenschaftes des Fetts gemäß Beispiel 3, bei dem vollhydriertes PIB verwendet wurde, wurde nun mit einem Fett (Vergleichsbeispiel 3) verglichen, dass ein PIB enthielt, bei dem noch Doppelbindungen vorhanden waren, also ein nicht vollhydriertes PIB.
Die sonstige Zusammensetzung des Fetts gemäß Vergleichsbeispiel 3 entsprach der des Beispiels 3. Tabelle 10 Beispiel 3 Vergleichsbeisp. 3 FE 9 [180°C,6000 1/min,1500N] L 50 (h) 249 126 L 10 (h) 169 72 Geräuschprüfung [BeQuiet+ SKF] GN4 GN1 Verdampfungsverlust [DIN ISO 58397] 170°C/24h 4,3 5,1 Verdampfungsverlust [DIN ISO 58397] 180°C/24h 6,9 7,4 Walpenentration nach 60 DT [DIN ISO 2137] 284 301 Walpenentration nach 100000 DT [DIN ISO 2137] 324 356 Korrosionswirkung von Schmierstoffen auf Kupfer [DIN ISO 51811] 150°C/24h 1a n.A. Ölabsch 150°C/30h; [Gew.%] [ASTM D 6184] 7,4 8,4 Ölabsch 150°C/30h; [Gew.%] [ASTM D 6184 17,9 14,7 Ölabsch 168°C/40h; [Gew.%] [DIN 51817] 3,8 6,5 Prüfung von Schmerfetten auf korrosionsverhindernde Eigenschaften [DIN 51801/ISO 11007] 0 n.A. Tropfpunkt [C°] [DIN ISO 2176] >300 295,0 Verdampfungsverlust 150°C/24°C [DIN 58397 Teil 1] 2 2,4 Wasserbeständigkeit statisch [DIN 51807] 90°C 0 n.A.
The properties of the fat according to Example 3, in which fully hydrogenated PIB was used, was now compared with a fat (comparative example 3) that contained a PIB in which double bonds were still present, that is to say a not fully hydrogenated PIB.
The other composition of the fat according to comparative example 3 corresponded to that of example 3. <u> Table 10 </u> Example 3 Comparative example 3 FE 9 [180 ° C, 6000 rpm, 1500N] L 50 (h) 249 126 L 10 (h) 169 72 Noise test [BeQuiet + SKF] GN4 GN1 Loss of evaporation [DIN ISO 58397] 170 ° C / 24h 4.3 5.1 Evaporation loss [DIN ISO 58397] 180 ° C / 24h 6.9 7.4 Walpenentration according to 60 DT [DIN ISO 2137] 284 301 Walpenentration according to 100000 DT [DIN ISO 2137] 324 356 Corrosion effect of lubricants on copper [DIN ISO 51811] 150 ° C / 24h 1a n / A Oil cut-off 150 ° C / 30h; [% By weight] [ASTM D 6184] 7.4 8.4 Oil cut-off 150 ° C / 30h; [% By weight] [ASTM D 6184 17.9 14.7 Oil cut-off 168 ° C / 40h; [% By weight] [DIN 51817] 3.8 6.5 Testing of fat greases for corrosion-preventing properties [DIN 51801 / ISO 11007] 0 n / A Drop point [C °] [DIN ISO 2176] > 300 295.0 Evaporation loss 150 ° C / 24 ° C [DIN 58397 part 1] 2 2.4 Static water resistance [DIN 51807] 90 ° C 0 n / A

Der Vergleich der Fette mit vollhydriertem PIB und nicht vollhydriertem PIB in Tabelle 10 zeigt, dass das Fett des Beispiels 3 eine verdoppelte Laufzeit bei der FE9 Prüfung zeigt, geringere Verdampfungsverluste und ein signifikant besseres Geräuschverhalten aufweist.

Figure imgb0001
The comparison of the fats with fully hydrogenated PIB and not fully hydrogenated PIB in Table 10 shows that the fat of Example 3 shows a doubled running time in the FE9 test, has lower evaporation losses and a significantly better noise behavior.
Figure imgb0001

Claims (4)

  1. A high-temperature grease, comprising
    a) 91.9 to 25 wt.-% of at least one oil, selected from trimellitic acid esters or a mixture of different trimellitic acid esters, in which the alcohol group of the ester is a linear or branched alkyl group with 8 to 16 carbon atoms;
    b) 6 to 45 wt.-% of a polymer, selected from the group consisting of a hydrogenated or fully hydrogenated polyisobutylene or a mixture of hydrogenated or fully hydrogenated polyisobutylene;
    c) 0.1 to 10 wt.-% of additives, alone or in combination, selected from the group consisting of corrosion-protection additives, antioxidants, wear-protection additives, UV stabilisers, inorganic or organic solid lubricants and
    d) 2 to 20 wt.-% of thickener.
  2. The high-temperature grease according to claim 1, in which the oil component comprises, as further oil, a compound selected from the group consisting of mineral oil, aliphatic carboxylic acid and dicarboxylic acid esters, fatty acid triglycerides, pyromellitic acid esters, diphenyl ether, phloroglucinol ester and/or polyalphaolefins, alpha olefin copolymers.
  3. The high-temperature grease according to claim 1, in which the thickener is selected from the group consisting of urea, aluminium complex soaps, metal simple soaps of the elements of the first and second main group of the periodic table, metal complex soaps of the elements of the first and second main group of the periodic table, bentonites, sulfonates, silicates, aerosil, polyimides, PTFE or a mixture of the aforementioned thickeners.
  4. A use of the high-temperature grease according to one of the preceding claims for lubricating rolling contact bearings and friction bearings in automotive engineering, materials handling technology, manufacturing systems engineering, office technology and in industrial installations and machines, but also in the fields of domestic machines, consumer electronics and for lubricating chains, chain rollers and belts of continuous presses.
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