EP4090723B1 - Lithium complex hybrid grease - Google Patents
Lithium complex hybrid grease Download PDFInfo
- Publication number
- EP4090723B1 EP4090723B1 EP21704440.3A EP21704440A EP4090723B1 EP 4090723 B1 EP4090723 B1 EP 4090723B1 EP 21704440 A EP21704440 A EP 21704440A EP 4090723 B1 EP4090723 B1 EP 4090723B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- weight
- lithium complex
- hydrogenated
- bearings
- ester
- 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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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims description 55
- 229910052744 lithium Inorganic materials 0.000 title claims description 55
- 239000004519 grease Substances 0.000 title claims description 48
- 239000000203 mixture Substances 0.000 claims description 80
- 239000010702 perfluoropolyether Substances 0.000 claims description 49
- 239000000314 lubricant Substances 0.000 claims description 47
- 239000003921 oil Substances 0.000 claims description 45
- 150000002148 esters Chemical class 0.000 claims description 43
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 26
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 26
- 239000000654 additive Substances 0.000 claims description 24
- 239000000344 soap Substances 0.000 claims description 22
- 239000002562 thickening agent Substances 0.000 claims description 18
- 238000004519 manufacturing process Methods 0.000 claims description 17
- -1 pyromellitic acid ester Chemical class 0.000 claims description 17
- 239000002253 acid Substances 0.000 claims description 15
- 125000004432 carbon atom Chemical group C* 0.000 claims description 14
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical class C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 claims description 14
- 150000002149 estolides Chemical class 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 14
- 238000005260 corrosion Methods 0.000 claims description 12
- 239000000539 dimer Substances 0.000 claims description 12
- 229920006007 hydrogenated polyisobutylene Polymers 0.000 claims description 12
- 230000007797 corrosion Effects 0.000 claims description 11
- CYIDZMCFTVVTJO-UHFFFAOYSA-N pyromellitic acid Chemical class OC(=O)C1=CC(C(O)=O)=C(C(O)=O)C=C1C(O)=O CYIDZMCFTVVTJO-UHFFFAOYSA-N 0.000 claims description 11
- 125000003545 alkoxy group Chemical group 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 8
- 125000000217 alkyl group Chemical group 0.000 claims description 7
- 150000007513 acids Chemical class 0.000 claims description 6
- 239000003963 antioxidant agent Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 235000011180 diphosphates Nutrition 0.000 claims description 4
- 230000001050 lubricating effect Effects 0.000 claims description 4
- 239000002480 mineral oil Substances 0.000 claims description 4
- 230000000737 periodic effect Effects 0.000 claims description 4
- 229920013639 polyalphaolefin Polymers 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 238000009749 continuous casting Methods 0.000 claims description 3
- 238000005461 lubrication Methods 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 229910002012 Aerosil® Inorganic materials 0.000 claims description 2
- 229920000089 Cyclic olefin copolymer Polymers 0.000 claims description 2
- 239000004642 Polyimide Substances 0.000 claims description 2
- 239000012963 UV stabilizer Substances 0.000 claims description 2
- 150000007933 aliphatic carboxylic acids Chemical class 0.000 claims description 2
- 150000004696 coordination complex Chemical class 0.000 claims description 2
- 150000001991 dicarboxylic acids Chemical class 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 229910021389 graphene Inorganic materials 0.000 claims description 2
- 235000010446 mineral oil Nutrition 0.000 claims description 2
- 238000012986 modification Methods 0.000 claims description 2
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- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 claims description 2
- 229920001721 polyimide Polymers 0.000 claims description 2
- 150000004760 silicates Chemical class 0.000 claims description 2
- 239000004711 α-olefin Substances 0.000 claims description 2
- 125000005590 trimellitic acid group Chemical class 0.000 claims 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical class C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims 1
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical class C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims 1
- JPYHHZQJCSQRJY-UHFFFAOYSA-N Phloroglucinol Natural products CCC=CCC=CCC=CCC=CCCCCC(=O)C1=C(O)C=C(O)C=C1O JPYHHZQJCSQRJY-UHFFFAOYSA-N 0.000 claims 1
- 239000000440 bentonite Substances 0.000 claims 1
- 229910000278 bentonite Inorganic materials 0.000 claims 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims 1
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- 229960001553 phloroglucinol Drugs 0.000 claims 1
- 239000000377 silicon dioxide Substances 0.000 claims 1
- 229910052682 stishovite Inorganic materials 0.000 claims 1
- 125000001273 sulfonato group Chemical group [O-]S(*)(=O)=O 0.000 claims 1
- DHCDFWKWKRSZHF-UHFFFAOYSA-L thiosulfate(2-) Chemical compound [O-]S([S-])(=O)=O DHCDFWKWKRSZHF-UHFFFAOYSA-L 0.000 claims 1
- 229910052905 tridymite Inorganic materials 0.000 claims 1
- 239000003925 fat Substances 0.000 description 69
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 32
- 238000001704 evaporation Methods 0.000 description 29
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- ARCGXLSVLAOJQL-UHFFFAOYSA-N anhydrous trimellitic acid Natural products OC(=O)C1=CC=C(C(O)=O)C(C(O)=O)=C1 ARCGXLSVLAOJQL-UHFFFAOYSA-N 0.000 description 10
- ULQISTXYYBZJSJ-UHFFFAOYSA-N 12-hydroxyoctadecanoic acid Chemical compound CCCCCCC(O)CCCCCCCCCCC(O)=O ULQISTXYYBZJSJ-UHFFFAOYSA-N 0.000 description 8
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- 238000012360 testing method Methods 0.000 description 8
- 229910019142 PO4 Inorganic materials 0.000 description 7
- 235000021317 phosphate Nutrition 0.000 description 7
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 6
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 6
- 229910052794 bromium Inorganic materials 0.000 description 6
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 6
- 230000000996 additive effect Effects 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 229940114072 12-hydroxystearic acid Drugs 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 4
- 150000001412 amines Chemical class 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000011065 in-situ storage Methods 0.000 description 4
- FSYKKLYZXJSNPZ-UHFFFAOYSA-N sarcosine Chemical compound C[NH2+]CC([O-])=O FSYKKLYZXJSNPZ-UHFFFAOYSA-N 0.000 description 4
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 4
- 239000003981 vehicle Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000005096 rolling process Methods 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 description 2
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- 108010077895 Sarcosine Proteins 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical class C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 description 2
- TVIDDXQYHWJXFK-UHFFFAOYSA-N dodecanedioic acid Chemical compound OC(=O)CCCCCCCCCCC(O)=O TVIDDXQYHWJXFK-UHFFFAOYSA-N 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 229910003002 lithium salt Inorganic materials 0.000 description 2
- 159000000002 lithium salts Chemical class 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 150000002989 phenols Chemical class 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 150000003852 triazoles Chemical class 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- SKDGWNHUETZZCS-UHFFFAOYSA-N 2,3-ditert-butylphenol Chemical compound CC(C)(C)C1=CC=CC(O)=C1C(C)(C)C SKDGWNHUETZZCS-UHFFFAOYSA-N 0.000 description 1
- DIOYAVUHUXAUPX-ZHACJKMWSA-N 2-[methyl-[(e)-octadec-9-enoyl]amino]acetic acid Chemical compound CCCCCCCC\C=C\CCCCCCCC(=O)N(C)CC(O)=O DIOYAVUHUXAUPX-ZHACJKMWSA-N 0.000 description 1
- DHTAIMJOUCYGOL-UHFFFAOYSA-N 2-ethyl-n-(2-ethylhexyl)-n-[(4-methylbenzotriazol-1-yl)methyl]hexan-1-amine Chemical compound C1=CC=C2N(CN(CC(CC)CCCC)CC(CC)CCCC)N=NC2=C1C DHTAIMJOUCYGOL-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- TVZRAEYQIKYCPH-UHFFFAOYSA-N 3-(trimethylsilyl)propane-1-sulfonic acid Chemical compound C[Si](C)(C)CCCS(O)(=O)=O TVZRAEYQIKYCPH-UHFFFAOYSA-N 0.000 description 1
- XMIIGOLPHOKFCH-UHFFFAOYSA-N 3-phenylpropionic acid Chemical compound OC(=O)CCC1=CC=CC=C1 XMIIGOLPHOKFCH-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- 239000004255 Butylated hydroxyanisole Substances 0.000 description 1
- 239000004322 Butylated hydroxytoluene Substances 0.000 description 1
- 102100039496 Choline transporter-like protein 4 Human genes 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 101000889282 Homo sapiens Choline transporter-like protein 4 Proteins 0.000 description 1
- 101000606535 Homo sapiens Receptor-type tyrosine-protein phosphatase epsilon Proteins 0.000 description 1
- BACYUWVYYTXETD-UHFFFAOYSA-N N-Lauroylsarcosine Chemical compound CCCCCCCCCCCC(=O)N(C)CC(O)=O BACYUWVYYTXETD-UHFFFAOYSA-N 0.000 description 1
- XQVWYOYUZDUNRW-UHFFFAOYSA-N N-Phenyl-1-naphthylamine Chemical compound C=1C=CC2=CC=CC=C2C=1NC1=CC=CC=C1 XQVWYOYUZDUNRW-UHFFFAOYSA-N 0.000 description 1
- KEQFTVQCIQJIQW-UHFFFAOYSA-N N-Phenyl-2-naphthylamine Chemical compound C=1C=C2C=CC=CC2=CC=1NC1=CC=CC=C1 KEQFTVQCIQJIQW-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
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- 102100039665 Receptor-type tyrosine-protein phosphatase epsilon Human genes 0.000 description 1
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/02—Mixtures of base-materials and thickeners
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
- C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
- C10M105/18—Ethers, e.g. epoxides
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
- C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
- C10M105/32—Esters
- C10M105/36—Esters of polycarboxylic acids
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- C10M107/08—Hydrocarbon polymers; Hydrocarbon polymers modified by oxidation containing butene
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- C10M2207/127—Carboxylix 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
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- C10M2207/1285—Carboxylix 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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- C10M2213/062—Polytetrafluoroethylene [PTFE]
- C10M2213/0623—Polytetrafluoroethylene [PTFE] used as base material
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- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
- C10N2020/01—Physico-chemical properties
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- C10N2030/08—Resistance to extreme temperature
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- C10N2040/00—Specified use or application for which the lubricating composition is intended
- C10N2040/04—Oil-bath; Gear-boxes; Automatic transmissions; Traction drives
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- C10N2040/00—Specified use or application for which the lubricating composition is intended
- C10N2040/30—Refrigerators lubricants or compressors lubricants
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- C10N2040/38—Conveyors or chain belts
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- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2050/00—Form in which the lubricant is applied to the material being lubricated
- C10N2050/10—Semi-solids; greasy
Definitions
- the present invention relates to the provision of a new lithium complex hybrid grease based on a lithium complex grease in combination with a PFPE grease, which can be used at high temperatures, does not varnish and shows a low tendency to hardening.
- the invention further relates to the use of the new lithium complex hybrid greases in components in the vehicle sector.
- Hybrid fats are mixtures that consist of at least two base oils that cannot be mixed with each other.
- Hybrid fats which contain urea or urea/PTFE mixtures as thickeners and ester/PFPE as immiscible base oil components, represent an important group of these fats. With these fats it is possible to create a temperature gap between approx. 180°C, as in fluorine-free greases can be achieved up to 270°C, which is possible with pure PTPE/PFPE greases. These products can also be adapted to specific requirements more easily than is possible with pure PFPE/PTFE greases.
- PFPE oils there are very few soluble additives known for PFPE oils, so that, for example, the corrosion protection properties of PFPE oils can only be improved to a limited extent.
- solid substances such as sodium nitrite or magnesium oxide are used as corrosion protection.
- the uniform distribution of a solid on the surface of a component is much more difficult to ensure than wetting the surface of a component with an oil that contains a dissolved corrosion protection additive. Therefore, the additives contained in the non-fluorine-containing liquid phase of a hybrid grease can have properties such as Provide better corrosion protection than is possible with pure PFPE/PTFE grease.
- the reduction in the content of PFPE oils in the hybrid grease and the lower density of the hybrid grease also result in significant cost advantages.
- ester/PFPE/PTFE/urea fats for example in the EP0902828 B1 are described or the ester/PTFE/urea fats, such as those described in US 6,063,743 described have the disadvantage that these greases tend to harden at high temperatures and have very low oil separations. In addition, they can sometimes be critical when used with certain elastomers, so that they cannot be used in a wide range, such as roller bearings, in corrugating plants. In addition, the fluorinated fats are very expensive, so that there is also a need for hybrid fats that can be produced inexpensively with the same or even better properties than the fluorinated fats.
- EP3372660 A1 describes high-temperature greases that contain an ester oil (estolide, trimellitic acid ester), a hydrogenated or fully hydrogenated polyisobutylene and a thickener.
- ester oil estolide, trimellitic acid ester
- polyisobutylene a hydrogenated or fully hydrogenated polyisobutylene
- Lithium complex greases have higher oil separation and a lower tendency to harden at high temperatures compared to ester/urea greases.
- the upper operating temperature is significantly lower than with urea hybrid greases, which is often associated with excessive oil separation or can be attributed to the use of base oils such as poly-alpha-olefins or mineral oils, which are less thermally stable.
- An object of the present invention was therefore to provide a lithium complex hybrid grease which overcomes the above-mentioned disadvantages and which has adequate oil separation and low hardening even at high temperatures.
- a method for lubricating or greasing components in particular in rolling bearings, plain bearings, transport and control chains in vehicle technology, is provided, which comprises applying the lubricant composition according to the invention.
- a method for lubricating or greasing roller bearings in continuous casting plants, transport roller bearings in continuous furnaces, open gear rings in rotary kilns, tube mills, drums and mixers, bearings in corrugated cardboard plants or film stretching plants, bearings in plants for the production and transport of foodstuffs is provided Applying the lubricant composition according to the invention includes.
- the lubricants according to the invention can contain additives and (H) solid lubricants as further components.
- Component (A) is contained in the lubricant composition according to the invention in an amount of 70 to 7% by weight, preferably 60 to 15% by weight.
- Component (A) is an ester or a mixture of esters, the ester being selected from the group consisting of trimellitic acid esters which have linear or branched alkyl groups as alkoxy groups which contain 6 to 18 carbon atoms, preferably 8 to 14 carbon atoms, where the Alkoxy groups can be the same or different, pyromellitic acid esters, preferably tetrakis (2-ethylhexyl) pyromellitate, hydrogenated or unhydrogenated dimer acid esters, preferably bis (2-ethylhexyl) dimerate, estolides.
- trimellitic acid esters which have linear or branched alkyl groups as alkoxy groups which contain 6 to 18 carbon atoms, preferably 8 to 14 carbon atoms, where the Alkoxy groups can be the same or different
- pyromellitic acid esters preferably tetrakis (2-ethylhexyl) pyromellitate
- Estolides are esters that contain oligomeric units made up of homopolymers of hydroxycarboxylic acids, for example 12-hydroxystearic acid, or unsaturated carboxylic acids, for example such as oleic acid. Suitable estolides are, for example, in the US 6,018,063 , US 6,316,649 , WO 2018/177588 A1 and the US 2013/0261325 A1 described.
- Component (B) is a polyisobutylene or polybutene and is present in the composition according to the invention in an amount of 0.5 to 20% by weight; 1.5 to 15% by weight is preferably used.
- Component (B) is a polymer, such as that in Synthetics, Mineral Oils And Bio Based Lubricants Chemistry And Technology, Second Edition, Editor Leslie R. Rudnik, authors M. Casserino, J. Corthouts, CRC Press 2013, Pages 273 - 300, (ISBN 978-1-4398-5537-9 ) is described.
- the properties of the fat according to the invention can be adjusted can be influenced in a desired way.
- the polyisobutylene can be used in non-hydrogenated, hydrogenated or fully hydrogenated form, and a mixture of non-hydrogenated, hydrogenated and fully hydrogenated polyisobutylene can also be used.
- Fully hydrogenated polyisobutylenes are preferably used. Due to the production process, the non-hydrogenated polyisobutylenes contain an unsaturated end group.
- Polyisobutylenes are polymers whose bromine number is at least 20% lower than unhydrogenated polyisobutylene of the same number-average molecular weight.
- the bromine number for a non-hydrogenated polyisobutylene with Mn of 1300 g/mol is 14 g bromine per 100 g polyisobutylene.
- the bromine number is fully hydrogenated polyisobutylene is less than 7 g bromine per 100 g polyisobutylene.
- the bromine number is determined according to ASTM D2170-09 (reaproved 2018).
- the polyisobutylene has a number-average molecular weight of 115 to 10,000 g/mol, preferably 500 to 5,000 g/mol.
- the number-average molecular weight is determined using gel permeation chromatography according to ISO 16014-1, edition 2019-05.
- Component (C) is contained in the lubricant composition according to the invention in an amount of 1 to 18% by weight, preferably 4 to 14% by weight.
- Component (C) is a lithium complex soap.
- Lithium complex soaps are understood to mean mixtures of lithium salts of monofunctional carboxylic acids, preferably carboxylic acids that contain 8 to 22 carbon atoms, particularly preferably carboxylic acids that contain 14 to 20 carbon atoms, particularly preferably 12-hydroxystearic acid and / or stearic acid with the lithium salts of higher-functional carboxylic acids, preferably dicarboxylic acids with 6 to 14 carbon atoms, particularly preferably azelaic acid, sebacic acid and dodecanedioic acid.
- Lithium complex soaps can additionally contain short-chain carboxylic acids such as acetic acid and lactic acid and / or phosphonic acids and / or boric acid as a further acid component.
- Component (D) is a perfluoropolyether (PFPE) according to the formula (I): R 1 -(O-CF 2 ) v -(OC 2 F 4 ) w -(O- C 3 F 6 ) x -(O- CFCF 3 ) y - (O- CF 2 CF(CF 3 )) z - OR 2 (I) where R 1 and R 2 are identical or different and are selected from -CF 3 , -C 2 F 5 , or -C 3 F 7 , v, w, x, y, z are integers from ⁇ 0 to 500.
- PFPE oils are sold, for example, under the brand names Aflunox ® , Krytox ® , Fomblin ® and Demnum ® .
- the PFPE oils are contained in amounts of 15 to 50% by weight in the lubricant composition according to the invention.
- the lithium complex hybrid grease according to the invention can comprise further thickeners (E) in addition to the lithium complex thickener.
- the further thickeners (E) are contained in the lubricant composition according to the invention in amounts of 1 to 30% by weight, preferably 3 to 20% by weight.
- the further thickeners (E) in the hybrid grease according to the invention are selected from the group consisting of Al complex soaps, metal simple soaps of the elements of the first and second main groups of the periodic table without lithium, metal complex soaps of the elements of the first and second main groups of the periodic table without lithium , bentonites, sulfonates, silicates, aerosil, polyimides or PTFE or a mixture of the aforementioned thickeners.
- a particularly preferred further thickener is PTFE.
- the preferred PTFE is as Micropowder is used, which is produced thermally or by irradiating high molecular weight PTFE to reduce the molecular weight.
- the hybrid greases according to the invention can contain further oils (F), which are contained in the lubricant composition according to the invention in amounts of 0 to 20% by weight, preferably 2 to 20% by weight.
- Component (F) is selected from the group consisting of mineral oil, alkylated benzenes, alkylated naphthalenes, aliphatic carboxylic acid and dicarboxylic acid esters, fatty acid triglycerides, alkylated diphenyl ethers, phloroglucin esters, estolides and/or poly-alpha-olefins, alpha-olefin copolymers, metallocene catalyzed poly-alfa-olefins.
- Preferred further oils are alkylated diphenyl ether oils.
- Alkylated diphenyl ether oils are sold, for example, by Moresco under the brand name Hilube® .
- the alkyl groups contain between 10 and 20 carbon atoms. On average, between one and three alkyl groups are bound to the diphenyl ether basic unit.
- the lubricant composition according to the invention further comprises from 0 to 10% by weight, preferably from 0.1 to 10% by weight, of additives (G), which are used individually or in combination.
- the component (G) will be selected from the group consisting of corrosion protection additives, antioxidants, wear protection additives, UV stabilizers. Both additives that are soluble in component (A) and additives that are soluble in the PFPE oils of component (D) or insoluble in both oil phases can be used.
- antioxidants are styrenated diphenylamines, diaromatic amines, phenolic resins, thiophenolic resins, phosphites, butylated hydroxytoluene, butylated hydroxyanisole, phenyl-alpha-naphthylamine, phenyl-beta-naphthylamine, octylated/butylated diphenylamine, di-alpha-tocopherol, di-tert-butyl-phenol or di-tert-butyl-4-methylphenol, benzenepropanoic acid, sulfur-containing phenolic compounds, phenolic compounds and mixtures of these components.
- Suitable anti-corrosion additives include triazoles, imidazolines, N-methylglycine (sarcosine), benzotriazole derivatives, N,N-bis(2-ethylhexyl)-ar-methyl-1 H-benzotriazole-1-methanamine; n-Methyl-N(1-oxo-9-octadecenyl)glycine, mixture of phosphoric acid and mono- and di-isooctyl esters reacted with (C 11-14 )-alkylamines, mixture of phosphoric acid and mono- and di-isooctyl esters reacted with tert-alkylamine and primary (C 12-14 ) amines, dodecanoic acid, triphenylphosphorothionate and amine phosphates.
- IRGAMET ® 39 IRGACOR ® DSS G, Amin O; SARKOSYL ® O (Ciba), COBRATEC ® 122, CUVAN ® 303, VANLUBE ® 9123, CI-426, CI-426EP, CI-429 and CI-498.
- wear protection additives are amines, amine phosphates, phosphates, thiophosphates, and mixtures of these components. Most of the compounds mentioned have organic groups.
- Commercially available anti-wear additives include IRGALUBE ® TPPT, URGALUBE ® 232, IRGALUBE ® 349, IRGALUBE ® 211 and ADDITIN ® RC3760 Liq 3960, FIRC-SHUN ® FG 1505 and FG 1506, NA-LUBE ® KR-015FG, LUBEBOND ® , F LUORO ® FG, SYNALOX ® 40-D, ACHESON ® FGA 1820 and ACHESON ® FGA 1810.
- PFPE derivatives can also be included as additives.
- Other suitable substances are, for example, WO01/72759A1 , WO 01/27916A1 , EP1070074B1 , EP1659165B1 and US2015011446A1 described.
- the lubricant compositions according to the invention can contain solid lubricants (H) which are selected from the group consisting of 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 solid lubricants (H) are contained in the lubricant composition according to the invention in amounts of 0 to 10% by weight, preferably 2 to 5% by weight.
- the lubricant composition according to the invention is used in the area of components, in particular in rolling bearings, plain bearings, transport and control chains in vehicle technology, in rail vehicles, conveyor technology, in film stretching systems, in corrugated cardboard systems, in roller bearings, fan bearings, bearings in traction motors, for the lubrication of bevel gear and Helical gears, springs, screws and compressors, pneumatic components, fittings, and machine components and in systems where occasional, unintentional contact with food occurs.
- the production of the lubricant composition according to the invention is not restricted and can be carried out using any suitable process.
- the production of the lubricant according to the invention can be carried out, for example, by producing a base oil mixture with components (A) and/or (B) and/or (F).
- the acids required for the lithium complex thickener (C) and an aqueous lithium hydroxide solution are melted into this base oil mixture, which is placed completely or only partially in a suitable reaction vessel containing heating, cooling and stirring devices admitted.
- the acids can be added and neutralized individually or the monocarboxylic acid is added and neutralized first and in a second step the higher functional carboxylic acid is added and neutralized.
- the brew is heated to 130°C to drive off water.
- the swelling of the thickener is carried out by thermal treatment at 150°C to 210°C.
- the thermally treated brew is then cooled, and part of the base oil mixture can also be used.
- the components (D), (E), (G), (H) and any components not used for the base oil mixture (A), (B) and (F) are added at a suitable temperature and pre-homogenized by stirring.
- Solid lubricant additives that are soluble in the base oil mixture are added, for example, at temperatures above their melting point.
- Liquid additives or non-melting additives/solid lubricants/thickener components are added at temperatures below 80°C.
- the lithium complex hybrid grease produced in this way can be homogenized using suitable equipment such as three-roll mills, colloid mills or Gaulin.
- the lubricant composition according to the invention is produced in one process.
- the addition of the PFPE oil (D) and the optional thickener component (E) can be omitted in the process described above, so that a lithium complex grease is formed.
- Components (D) and (E) can be combined to form a PFPE fat by stirring and homogenizing as described above.
- Lithium complex grease and PFPE grease can be combined in a second process step and the lubricant composition according to the invention can be produced therefrom while stirring and homogenizing.
- the production can also be carried out using continuous processes, whereby ready-made Li complex soap in powder form can also be used.
- Lithium complex soap grease (fat A) and a PFPE/PTFE grease (fat B) are produced separately and the two fats A and B are mixed in different ratios, stirred and homogenized by rolling.
- a lithium complex grease consisting of 77% of a mixture of an alkyl diphenyl ether (100 mm “/sec/40 ° C) and trimellitic acid ester as well as fully hydrogenated polyisobutylene (fully hydrogenated, Mn approx. 1300 g / mol) is used as a base oil, with a viscosity at 40 ° C of 220 mm 2 /sec, then 15% lithium complex from azelaic acid and 12-hydroxystearic acid, as well as 8% of an additive package consisting of amine antioxidants, phosphates, thiadiazoles, triazoles and amine phosphates are added. The full penetration is 270 1/10 mm (see Table 1)
- a PFPE/PTFE grease is used, containing 70% of a mixture of linear and branched PFPE, kinematic viscosity 200 mm 2 /sec at 40°C, 26% PTFE micropowder, average particle size d 50 (laser diffraction, DIN ISO 9277) approx. 5 ⁇ m, specific surface area (DIN ISO 9277) approx. 5 m 2 /g, and 4% disodium sebacate as a corrosion protection additive.
- the full penetration is 286 1/10 mm (see Table 1)
- a urea hybrid fat is produced consisting of 50% by weight of fat B and 50% by weight of a urea fat.
- the urea fat consists of a mixture of a trimellitic acid ester and a reaction product of octylamine and oleylamine with an MDI/TDI mixture as a urea thickener, as well as additives.
- the base oil viscosity is approx. 80 mm 2 /sec.
- the working penetration is 265 mm 2 /sec (see Table 2)
- a urea hybrid fat consisting of a complex ester, dimer acid based, V 40 apr. 400 mm"/sec at 40°C and branched PFPE oil with a kinematic viscosity of approx. 400 mm 2 /sec in a mass ratio of 2:1.
- the urea thickener is contained at 10% and is a reaction product of octylamine and oleylamine with a MDI/TDI mixture. In addition, it contains 8% by weight of PTFE powder (as in grease B) and 5% by weight of soluble additives (antioxidants, amine phosphates). The working penetration is 290 mm 2 /sec (see Table 2 )
- Table 1 shows the general characteristics of the lithium complex hybrid greases according to the invention of Examples B2-B4, Reference Examples B1 and B5 and Fats A and B, ⁇ b> ⁇ u>Table 1 ⁇ /u> ⁇ /b> Parameters/Grease fat (B) B1 B2 B3 B4 B5 fat (A) Work penetration 60 dT [1/10 mm] (DIN ISO 2137) 286 279 254 253 262 273 270 Delta work penetration after 100,000 dT 15 28 31 45 44 39 45 [1/10 mm] (DIN ISO 2137) Dropping point [°C] (DIN ISO 2176) >300 >300 >300 >300 >300 294 >300 Flow pressure [mbar] (-40°C) (DIN 51805) 200 375 575 850 875 875 925 Flow pressure [mbar] (-50°C) (DIN 51805) 325 575 1025 >1400 >1400 >1400 >1400 Shear viscosity, at 25°C, shear rate 300 1/
- Table 2 shows the data of comparative examples VG1 to 2.
- ⁇ b> ⁇ u>Table 2 ⁇ /u> ⁇ /b> Parameters/Grease VG1 VG2 Work penetration 60 dT [1/10 mm] (DIN ISO 2137) 262 290 Delta work penetration after 100,000 dT [1/10 mm] (DIN ISO 2137) 47 43 Dropping point [°C] (DIN ISO 2176) 285 285 Flow pressure [mbar] (-40°C) (DIN 51805) 725 625 Flow pressure [mbar] (-50°C) (DIN 51805) 1200 1375 Shear viscosity, at 25°C, shear rate 300 1/s (DIN 53019 -1, -3) 5913 11880 Evaporation loss, 22h/100°C [% by weight] (DIN 58397) 0.37 0.42 Oil separation, 24h/150°C [wt%], (ASTM D 6184) 0.42 0.11 Oil separation, 72h/150°C [
- the data also suggests that a desired oil separation behavior can be adjusted by choosing the amount of fats A and B.
- the lubricant compositions according to the invention were tested for their thermal stability and the results were compared, in particular, with those of the urea hybrid greases. For this purpose, studies were carried out regarding the evaporation and viscosity under temperature stress of 5 g of fat in a stainless steel bowl at 200 ° C. The results are shown in Tables 3 and 4.
- the evaporation loss is determined according to DIN standard 58397. Three evaporation loss dishes made of stainless steel are required for each fat sample. The geometry of the shells is described in the standard for determining evaporation loss (DIN 58397). At the beginning, the respective empty weight of the shells is determined. The three evaporation loss dishes are then filled with the fat sample. It is important to ensure that the grease is applied without any air bubbles. The surface is smoothed using a scraper and any excess fat that has found its way into the edge recess of the bowl is removed. The trays are then stored in a standard laboratory drying cabinet with convection with the flap closed at the appropriate test temperature (here 200°C).
- the shear viscosity is determined according to DIN standard 53019 part 1 and part 3.
- the fat samples are each transferred to three evaporation loss dishes made of stainless steel.
- the geometry of the shells is described in the standard for determining evaporation loss (DIN 58397).
- the trays are then stored in a standard laboratory drying cabinet with circulation at the appropriate test temperature (here 200°C). After the specified time period (48h, 96h, 144h and 168h), the bowls are removed from the drying cabinet and allowed to cool.
- the starting value for the shear viscosity is determined for each grease before thermal loading.
- Shear viscosity is measured using a device that is standardly used to determine the rheological parameters of lubricants (e.g. Rheometer MCR 302 from Anton Paar).
- a cone-plate system (DIN EN ISO 3219 and DIN 53019) is used, preferably with a measuring cone that has a diameter of 25 mm.
- the amount of fat sample required is based on typical amounts required for rheological measurements.
- the measuring time is 120 s, of which 60 s is the tempering or holding time.
- the measurements are taken at a constant shear rate of 300 1/s and a temperature of 25°C.
- the value, which can be read after 90 s, represents the shear viscosity for the respective fat sample.
- the average value is calculated from the three individual values determined and finally stated.
- VG2 shows a shear viscosity of 100,000 mPas after just 96 hours and is no longer lubricable. After 168 hours of testing, VG1 shows a shear viscosity that is twice as high as all compositions B1 to B5 according to the invention, see Table 4.
- the hardening behavior of the lubricants according to the invention at high temperatures is more favorable than that of urea hybrid greases.
- the oil separation behavior of the lubricants according to the invention can be adjusted by choosing a specific mixing ratio of the fats A (lithium complex fat) and B (PTFE/PFPE fat) and can therefore be adapted to different requirements.
- the lubricants according to the invention can be produced in various ways.
- a lithium complex fat (fat C) and a PFPE/PTFE fat (fat D) are produced separately and then mixed in a kettle in a ratio of 40 to 60% by weight with stirring.
- the resulting lithium complex hybrid grease B6 is then homogenized using a three-roll mill.
- the lithium complex grease is produced identically to grease C, but when it cools down, the components of grease D are also added, so that the lubricant composition according to the invention is produced in one operation.
- the lubricant composition B6 according to the invention is also finally rolled.
- a lithium complex fat consisting of 80% by weight of a mixture of an alkyl diphenyl ether (100 mm 2 /sec at 40 ° C) and a trimellitic acid ester and fully hydrogenated polyisobutylene (fully hydrogenated, Mn approx. 1300 g / mol) is produced as a base oil, whereby a viscosity at 40°C of 100 mm 2 /sec. 15% by weight of a lithium complex made from azelaic acid and 12-hydroxystearic acid, as well as 5% by weight of an additive package consisting of aminic antioxidants and phosphates are provided. The full penetration is 327 1/10 mm.
- the full penetration is 286 1/10 mm ⁇ b> ⁇ u>Table 7 ⁇ /u> ⁇ /b> Data from Example B6 according to the invention according to Example 2 Parameters / Grease Mixed in the kettle Cooked in situ Work penetration 60dT [1/10 mm] (DIN ISO 2137) 298 265 Dropping point [°C] (DIN ISO 2176) > 300 277 Delta work penetration to 100,000dT [1/10 mm] (DIN ISO 2137) 25 36 Flow pressure -40°C [mbar] (DIN 51805) 550 725 Flow pressure -50°C [mbar] (DIN 51805) 1025 1250 Shear viscosity, at 25°C, shear rate 300 1/s, [mPa*s] (DIN 53019-1, -3) 4392 5378 Evaporation loss, 24h/150°C [% by weight] (DIN 58397) 0.46 0.50 Oil separation, 30h/150°C [wt.-%] (ASTM D 6184) 0.44
- B6 according to production example 1 and production example 2, can be used as a lubricant with both production variants.
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Description
Die vorliegende Erfindung betrifft die Bereitstellung eines neuen Lithiumkomplexhybridfettes auf der Basis eines Lithiumkomplexfettes in Kombination mit einem PFPE-Fett, das bei hoher Temperatur eingesetzt werden kann, dabei nicht verlackt, und eine geringe Verhärtungstendenz zeigt. Des Weiteren betrifft die Erfindung die Verwendung der neuen Lithiumkomplexhybridfette in Bauteilen im Fahrzeugbereich.The present invention relates to the provision of a new lithium complex hybrid grease based on a lithium complex grease in combination with a PFPE grease, which can be used at high temperatures, does not varnish and shows a low tendency to hardening. The invention further relates to the use of the new lithium complex hybrid greases in components in the vehicle sector.
Hybridfette sind Mischungen, die mindestens aus zwei Basisölen bestehen, die nicht miteinander mischbar sind. So stellen Hybridfette, die als Verdicker Harnstoff oder Harnstoff/PTFE-Gemische und Ester/PFPE als nicht mischbare Grundölkomponenten enthalten, eine wichtige Gruppe dieser Fette dar. Mit diesen Fetten ist es möglich, eine Temperaturlücke zwischen ca. 180°C, wie sie bei fluorfreien Fetten erreicht werden, bis zu 270°C, die mit reinen PTPE/PFPE-Fetten möglich sind, zu schließen. Auch können diese Produkte an bestimmte Anforderungen leichter angepasst werden, als dies mit reinen PFPE/PTFE-Fetten möglich ist. Für PFPE Öle sind nämlich nur sehr wenige lösliche Additive bekannt, sodass beispielsweise die Korrosionsschutzeigenschaften von PFPE Ölen nur bedingt verbessert werden können. Bei PFPE/PTFE Fetten werden daher feste Stoffe wie Natriumnitrit oder Magnesiumoxid als Korrosionsschutz eingesetzt. Die gleichmäßige Verteilung eines Feststoffes auf der Oberfläche eines Bauteiles ist aber viel schwieriger zu gewährleisten als die Benetzung der Oberfläche eines Bauteiles mit einem Öl, das ein gelöstes Korrosionsschutzadditiv enthält. Daher können die in der nicht fluorhaltigen flüssigen Phase enthaltenen Additive eines Hybridfettes Eigenschaften wie Korrosionsschutz besser bewerkstelligen als es bei einem reinen PFPE/PTFE Fett möglich ist. Durch die Reduktion des Gehaltes an PFPE Ölen im Hybridfett und die geringere Dichte des Hybridfettes ergeben sich zudem signifikante Kostenvorteile. Die Ester/PFPE/PTFE/Harnstoff-Fette, die beispielsweise in der
Lithiumkomplexfette weisen eine höhere Ölabscheidung und eine geringere Verhärtungstendenz bei hohen Temperaturen verglichen mit Ester/Harnstoff-Fetten auf. Allerdings ist die obere Gebrauchstemperatur deutlich niedriger als bei Harnstoffhybridfetten, was oft mit einer zu hohen Ölabscheidung in Zusammenhang gebracht wird oder aber auf die Verwendung von Grundölen wie Poly-alpha-olefinen oder Mineralölen, die thermisch weniger beständig sind, zurückzuführen ist.Lithium complex greases have higher oil separation and a lower tendency to harden at high temperatures compared to ester/urea greases. However, the upper operating temperature is significantly lower than with urea hybrid greases, which is often associated with excessive oil separation or can be attributed to the use of base oils such as poly-alpha-olefins or mineral oils, which are less thermally stable.
Eine Aufgabe der vorliegenden Erfindung bestand daher darin, ein Lithiumkomplexhybridfett bereitzustellen, mit dem die vorstehend genannten Nachteile überwunden werden und das eine entsprechend ausreichende Ölabscheidung und eine geringe Verhärtung selbst bei hohen Temperaturen aufweist.An object of the present invention was therefore to provide a lithium complex hybrid grease which overcomes the above-mentioned disadvantages and which has adequate oil separation and low hardening even at high temperatures.
Diese Aufgabe konnte überraschenderweise dadurch gelöst werden, dass Lithiumkomplexfette, die Polyisobutylen und Ester enthalten mit PFPE-Ölen oder PFPE-Fetten, insbesondere PFPE/PTFE-Fetten kombiniert werden und so eine Hochtemperaturperformance erreicht werden kann, die an die Ester/Harnstoff/PFPE-Hybridfette heranreicht, aber nicht deren Nachteile aufweist. Überraschenderweise kann die Ölabscheidung durch Auswahl der Mengenanteile der beiden Fette so eingestellt werden, dass die Ölabscheidung niedriger als bei den beiden zur Mischung verwendeten Fetten liegt.This task could surprisingly be solved by combining lithium complex fats that contain polyisobutylene and esters with PFPE oils or PFPE fats, in particular PFPE/PTFE fats, and thus high-temperature performance can be achieved that is similar to the ester/urea/PFPE Hybrid fats come close, but do not have their disadvantages. Surprisingly, oil separation can be achieved by selecting the proportions of the two fats can be set so that the oil separation is lower than that of the two fats used for the mixture.
Des Weiteren wird ein Verfahren zur Schmierung oder zum Fetten von Bauteilen, insbesondere in Wälzlagern, Gleitlagern, Transport- und Steuerketten in der Fahrzeugtechnik bereitgestellt, dass das Auftragen der erfindungsgemäßen Schmiermittelzusammensetzung umfasst.Furthermore, a method for lubricating or greasing components, in particular in rolling bearings, plain bearings, transport and control chains in vehicle technology, is provided, which comprises applying the lubricant composition according to the invention.
Außerdem wird ein Verfahren zur Schmierung oder zum Fetten von Laufrollenlagern in Stranggießanlagen, Transportrollenlagern in Durchlauföfen, von offenen Zahnkränzen in Drehrohröfen, Rohrmühlen, Trommeln und Mischern, von Lagern in Wellpappanlagen oder Folienreckanlagen, Lagern zur Anlagen zur Herstellung und Transport von Lebensmitteln bereitgestellt, dass das Auftragen der erfindungsgemäßen Schmiermittelzusammensetzung umfasst.In addition, a method for lubricating or greasing roller bearings in continuous casting plants, transport roller bearings in continuous furnaces, open gear rings in rotary kilns, tube mills, drums and mixers, bearings in corrugated cardboard plants or film stretching plants, bearings in plants for the production and transport of foodstuffs is provided Applying the lubricant composition according to the invention includes.
Die erfindungsgemäße Schmierstoffzusammensetzung umfasst
- (A) einen Ester oder Mischung von Estern, die insbesondere ausgewählt werden aus der Gruppe bestehend aus Trimellithsäureestern, Pyromellithsäureestern, Dimersäureestern, Estoliden,
- (B) Polyisobutylenen,
- (C) Lithiumkomplexseifen und
- (D) PFPE-Öle.
- (A) an ester or mixture of esters, which are in particular selected from the group consisting of trimellitic acid esters, pyromellitic acid esters, dimer acid esters, estolides,
- (B) polyisobutylenes,
- (C) lithium complex soaps and
- (D) PFPE oils.
Eine bevorzugte erfindungsgemäße Schmierstoffzusammensetzung umfasst
- (A) einen Ester oder Mischung von Estern, die insbesondere ausgewählt werden aus der Gruppe bestehend aus Trimellithsäureestern, Pyromellithsäureestern, Dimersäureestern, Estoliden,
- (B) Polyisobutylenen,
- (C) Lithiumkomplexseifen,
- (D) PFPE-Öle und
- (E) ein weiteres Verdickungsmittel.
- (A) an ester or mixture of esters, which are in particular selected from the group consisting of trimellitic acid esters, pyromellitic acid esters, dimer acid esters, estolides,
- (B) polyisobutylenes,
- (C) lithium complex soaps,
- (D) PFPE oils and
- (E) another thickener.
Eine besonders bevorzugte erfindungsgemäße Schmierstoffzusammensetzung umfasst
- (A) einen Ester oder Mischung von Estern, die insbesondere ausgewählt werden aus der Gruppe bestehend aus Trimellithsäureestern, Pyromellithsäureestern, Dimersäureestern, Estoliden,
- (B) Polyisobutylenen,
- (C) Lithiumkomplexseifen,
- (D) PFPE-Öle und
- (E) PTFE als weiteres Verdickungsmittel.
- (A) an ester or mixture of esters, which are in particular selected from the group consisting of trimellitic acid esters, pyromellitic acid esters, dimer acid esters, estolides,
- (B) polyisobutylenes,
- (C) lithium complex soaps,
- (D) PFPE oils and
- (E) PTFE as an additional thickener.
Eine insbesonders bevorzugte erfindungsgemäße Schmierstoffzusammensetzung umfasst
- (A) einen Ester oder Mischung von Estern, die insbesondere ausgewählt werden aus der Gruppe bestehend aus Trimellithsäureestern, Pyromellithsäureestern, Dimersäureestern, Estoliden,
- (B) Polyisobutylenen,
- (C) Lithiumkomplexseifen,
- (D) PFPE-Öle und
- (F) ein weiteres Grundöl, wobei akylierte Diphenylether bevorzugt sind.
- (A) an ester or mixture of esters, which are in particular selected from the group consisting of trimellitic acid esters, pyromellitic acid esters, dimer acid esters, estolides,
- (B) polyisobutylenes,
- (C) lithium complex soaps,
- (D) PFPE oils and
- (F) another base oil, with akylated diphenyl ethers being preferred.
Eine weitere bevorzugte erfindungsgemäße Schmierstoffzusammensetzung umfasst
- (A) einen Ester oder Mischung von Estern, die insbesondere ausgewählt werden aus der Gruppe bestehend aus Trimellithsäureestern, Pyromellithsäureestern, Dimersäureestern, Estoliden,
- (B) Polyisobutylenen,
- (C) Lithiumkomplexseifen,
- (D) PFPE-Öle,
- (E) ein weiteres Verdickungsmittel und
- (F) alkylierte Diphenylether.
- (A) an ester or mixture of esters, which are in particular selected from the group consisting of trimellitic acid esters, pyromellitic acid esters, dimer acid esters, estolides,
- (B) polyisobutylenes,
- (C) lithium complex soaps,
- (D) PFPE oils,
- (E) another thickener and
- (F) alkylated diphenyl ethers.
Die erfindungsgemäßen Schmierstoffe können als weitere Komponente (G) Additive und (H) Festschmierstoffe enthalten.The lubricants according to the invention can contain additives and (H) solid lubricants as further components.
Die Komponente (A) ist in einer Menge von 70 bis 7 Gew.-%, bevorzugt 60 bis 15 Gew.-% in der erfindungsgemäßen Schmierstoffzusammensetzung enthalten.Component (A) is contained in the lubricant composition according to the invention in an amount of 70 to 7% by weight, preferably 60 to 15% by weight.
Die Komponente (A) ist ein Ester oder ein Gemisch von Estern, wobei der Ester ausgewählt wird aus der Gruppe bestehend aus Trimellithsäureestern, die als Alkoxygruppen lineare oder verzweigte Alkylgruppen aufweisen, die 6 bis 18 Kohlenstoffatome enthalten, bevorzugt 8 bis 14 Kohlenstoffatome, wobei die Alkoxygruppen gleich oder verschieden sein können, Pyromellithsäureestern, bevorzugt Tetrakis(2-ethylhexyl)pyromellitat, hydrierte oder unhydrierte Dimersäureester, bevorzugt Bis(2-ethylhexyl)dimerat, Estolide.Component (A) is an ester or a mixture of esters, the ester being selected from the group consisting of trimellitic acid esters which have linear or branched alkyl groups as alkoxy groups which contain 6 to 18 carbon atoms, preferably 8 to 14 carbon atoms, where the Alkoxy groups can be the same or different, pyromellitic acid esters, preferably tetrakis (2-ethylhexyl) pyromellitate, hydrogenated or unhydrogenated dimer acid esters, preferably bis (2-ethylhexyl) dimerate, estolides.
Unter Estoliden versteht man Ester, die oligomere Einheiten aufgebaut aus Homopolymeren von Hydroxycarbonsäuren, beispielsweise von 12-Hydroxystearinsäure oder ungesättigten Carbonsäuren, beispielsweise wie Ölsäure enthalten. Geeignete Estolide sind beispielsweise in der
Die Komponente (B) ist ein Polyisobutylen oder Polybuten und in einer Menge von 0,5 bis 20 Gew.-% in der erfindungsgemäßen Zusammensetzung vorhanden, bevorzugt werden 1,5 bis 15 Gew.-% eingesetzt.Component (B) is a polyisobutylene or polybutene and is present in the composition according to the invention in an amount of 0.5 to 20% by weight; 1.5 to 15% by weight is preferably used.
Bei Komponente (B) handelt es sich um ein Polymer, wie es beispielsweise in
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 nicht hydrierter" hydrierter oder vollhydrierter Form eingesetzt werden, ebenso kann eine Mischung aus nicht hydriertem, hydriertem und vollhydriertem Polyisobutylen verwendet werden. Bevorzugt werden vollhydrierte Polyisobutylene eingesetzt. Die nicht hydrierten Polyisobutylene enthalten herstellungsbedingt eine ungesättigte Endgruppe. Unter hydrierten bzw. teilhydrierten Polyisobutylenen werden solche Polymere verstanden, deren Bromzahl im Vergleich zum unhydrierten Polyisobutylen gleicher zahlengemittelten Molekularmasse um mindestens 20% geringer ist. So beträgt die Bromzahl für ein nicht hydriertes Polyisobutylen mit Mn von 1300 g/mol 14 g Brom pro 100 g Polyisobutylen. Die Bromzahl bei vollhydrierten Polyisobutylenen liegt unter 7 g Brom pro 100 g Polyisobutylen. Die Bromzahl wird gemäß ASTM D2170-09 (reaproved 2018) bestimmt.Through a suitable choice of polyisobutylene, particularly with regard to the degree of hydrogenation and molecular weight, the properties of the fat according to the invention, for example its kinematic viscosity, can be adjusted can be influenced in a desired way. The polyisobutylene can be used in non-hydrogenated, hydrogenated or fully hydrogenated form, and a mixture of non-hydrogenated, hydrogenated and fully hydrogenated polyisobutylene can also be used. Fully hydrogenated polyisobutylenes are preferably used. Due to the production process, the non-hydrogenated polyisobutylenes contain an unsaturated end group. Among hydrogenated or partially hydrogenated Polyisobutylenes are polymers whose bromine number is at least 20% lower than unhydrogenated polyisobutylene of the same number-average molecular weight. The bromine number for a non-hydrogenated polyisobutylene with Mn of 1300 g/mol is 14 g bromine per 100 g polyisobutylene. The bromine number is fully hydrogenated polyisobutylene is less than 7 g bromine per 100 g polyisobutylene. The bromine number is determined according to ASTM D2170-09 (reaproved 2018).
Gemäß einer weiteren bevorzugten Ausführungsform weist das Polyisobutylen ein zahlenmittleres Molekulargewicht von 115 bis 10000 g/mol, vorzugsweise von 500 bis 5000 g/mol auf. Das Zahlenmittlere Molekulargewicht wird nach ISO 16014-1, Ausgabe 2019-05 mittels Gelpermeationschromatographie bestimmt.According to a further preferred embodiment, the polyisobutylene has a number-average molecular weight of 115 to 10,000 g/mol, preferably 500 to 5,000 g/mol. The number-average molecular weight is determined using gel permeation chromatography according to ISO 16014-1, edition 2019-05.
Die Komponente (C) ist in einer Menge von 1 bis 18 Gew.-%, bevorzugt 4 bis 14 Gew.% in der erfindungsgemäßen Schmierstoffzusammensetzung enthalten.Component (C) is contained in the lubricant composition according to the invention in an amount of 1 to 18% by weight, preferably 4 to 14% by weight.
Bei der Komponente (C) handelt es sich um eine Lithiumkomplexseife. Unter Lithiumkomplexseifen versteht man Gemische von Lithiumsalzen aus monofunktionellen Carbonsäuren, bevorzugt Carbonsäuren die 8 bis 22 Kohlenstoffatome enthalten, insbesondere bevorzugt Carbonsäuren die 14 bis 20 Kohlenstoffatome enthalten, insbesondere bevorzugt 12-Hydroxystearinsäure und/oder Stearinsäure mit den Lithiumsalzen höherfunktionellen Carbonsäuren, bevorzugt Dicarbonsäuren mit 6 bis 14 Kohlenstoffatomen, insbesondere bevorzugt Azelainsäure, Sebacinsäure und Dodecandisäure. Lithiumkomplexseifen können zusätzlich kurzkettige Carbonsäuren wie Essigsäure und Milchsäure und/oder Phosphonsäuren und/oder Borsäure als weiter Säurekomponente enthalten.Component (C) is a lithium complex soap. Lithium complex soaps are understood to mean mixtures of lithium salts of monofunctional carboxylic acids, preferably carboxylic acids that contain 8 to 22 carbon atoms, particularly preferably carboxylic acids that contain 14 to 20 carbon atoms, particularly preferably 12-hydroxystearic acid and / or stearic acid with the lithium salts of higher-functional carboxylic acids, preferably dicarboxylic acids with 6 to 14 carbon atoms, particularly preferably azelaic acid, sebacic acid and dodecanedioic acid. Lithium complex soaps can additionally contain short-chain carboxylic acids such as acetic acid and lactic acid and / or phosphonic acids and / or boric acid as a further acid component.
Die Komponente (D) ist ein Perfluorpolyether (PFPE) gemäß der Formel (I):
R1-(O-CF2)v-(O-C2F4)w-(O- C3F6)x-(O- CFCF3)y- (O- CF2CF(CF3)) z -O-R2 (I)
wobei R1 und R2 identisch oder verschieden sind und ausgewählt werden aus -CF3, -C2F5, oder -C3F7 , v, w, x, y, z sind ganze Zahlen von ≥ 0 bis 500. PFPE-Öle werden beispielsweise unter dem Markennamen Aflunox®, Krytox®, Fomblin® und Demnum® vertrieben.Component (D) is a perfluoropolyether (PFPE) according to the formula (I):
R 1 -(O-CF 2 ) v -(OC 2 F 4 ) w -(O- C 3 F 6 ) x -(O- CFCF 3 ) y - (O- CF 2 CF(CF 3 )) z - OR 2 (I)
where R 1 and R 2 are identical or different and are selected from -CF 3 , -C 2 F 5 , or -C 3 F 7 , v, w, x, y, z are integers from ≥ 0 to 500. PFPE oils are sold, for example, under the brand names Aflunox ® , Krytox ® , Fomblin ® and Demnum ® .
Die PFPE Öle sind in Mengen von 15 bis 50 Gew.-% in der erfindungsgemäßen Schmierstoffzusammensetzung enthalten.The PFPE oils are contained in amounts of 15 to 50% by weight in the lubricant composition according to the invention.
Das erfindungsgemäße Lithiumkomplexhybridfett kann neben dem Lithiumkomplexverdicker weitere Verdickungsmittel (E) umfassen.The lithium complex hybrid grease according to the invention can comprise further thickeners (E) in addition to the lithium complex thickener.
Die weiteren Verdickungsmittel (E) sind in Mengen von 1 bis 30 Gew.-%, bevorzugt 3 bis 20 Gew.-% in der erfindungsgemäßen Schmierstoffzusammensetzung enthalten. Die weiteren Verdickungsmittel (E) in dem erfindungsgemäßen Hybridfett werden ausgewählt aus der Gruppe bestehend aus Al-Komplexseifen, Metall-Einfachseifen der Elemente der ersten und zweiten Hauptgruppe des Periodensystems ohne Lithium, Metall-Komplexseifen der Elemente der ersten und zweiten Hauptgruppe des Periodensystems ohne Lithium, Bentonite, Sulfonate, Silikate, Aerosil, Polyimide oder PTFE oder einer Mischung der vorgenannten Verdickungsmittel. Ein besonders bevorzugtes weiteres Verdickungsmittel ist PTFE. Das bevorzugte PTFE wird als Mikropulver eingesetzt, das thermisch oder durch Bestrahlen von hochmolekularem PTFE unter Abbau des Molekulargewichtes hergestellt wird.The further thickeners (E) are contained in the lubricant composition according to the invention in amounts of 1 to 30% by weight, preferably 3 to 20% by weight. The further thickeners (E) in the hybrid grease according to the invention are selected from the group consisting of Al complex soaps, metal simple soaps of the elements of the first and second main groups of the periodic table without lithium, metal complex soaps of the elements of the first and second main groups of the periodic table without lithium , bentonites, sulfonates, silicates, aerosil, polyimides or PTFE or a mixture of the aforementioned thickeners. A particularly preferred further thickener is PTFE. The preferred PTFE is as Micropowder is used, which is produced thermally or by irradiating high molecular weight PTFE to reduce the molecular weight.
Die erfindungsgemäßen Hybridfette können weitere Öle (F) enthalten, die in Mengen von 0 bis 20 Gew.-%, bevorzugt zu 2 bis 20 Gew.-% in der erfindungsgemäßen Schmierstoffzusammensetzung enthalten sind.The hybrid greases according to the invention can contain further oils (F), which are contained in the lubricant composition according to the invention in amounts of 0 to 20% by weight, preferably 2 to 20% by weight.
Die Komponente (F) wird ausgewählt aus der Gruppe bestehend aus Mineralöl, alkylierten Benzolen, alkylierte Naphthaline, aliphatischen Carbonsäure- und Dicarbonsäureestern, Fettsäuretriglyceriden, alkylierte Diphenylether, Phloroglucinester, Estolide und/oder Poly-alpha-olefinen, alpha-Olefin-Copolymere, Metallocen katalysierte Poly-alfa-olefine. Bevorzugte weitere Öle sind alkylierte Diphenyletheröle. Alkylierte Diphenyletheröle werden beispielsweise unter dem Markennamen Hilube® von der Fa. Moresco vertrieben. Die Alkylgruppen enthalten zwischen 10 und 20 Kohlenstoffatome. Im Mittel sind zwischen einer und drei Alkylgruppen an die Diphenylether-Grundeinheit gebunden.Component (F) is selected from the group consisting of mineral oil, alkylated benzenes, alkylated naphthalenes, aliphatic carboxylic acid and dicarboxylic acid esters, fatty acid triglycerides, alkylated diphenyl ethers, phloroglucin esters, estolides and/or poly-alpha-olefins, alpha-olefin copolymers, metallocene catalyzed poly-alfa-olefins. Preferred further oils are alkylated diphenyl ether oils. Alkylated diphenyl ether oils are sold, for example, by Moresco under the brand name Hilube® . The alkyl groups contain between 10 and 20 carbon atoms. On average, between one and three alkyl groups are bound to the diphenyl ether basic unit.
Das erfindungsgemäße Schmierstoffzusammensetzung umfasst des Weiteren von 0 bis 10 Gew.%, bevorzugt von 0,1 bis 10 Gew.-% Additive (G), die einzeln oder in Kombination eingesetzt werden.The lubricant composition according to the invention further comprises from 0 to 10% by weight, preferably from 0.1 to 10% by weight, of additives (G), which are used individually or in combination.
Die Komponente (G) wird ausgewählt aus der Gruppe bestehend aus Korrosionsschutzadditiven, Antioxidantien, Verschleißschutzadditiven, UV-Stabilisatoren, ausgewählt werden. Es können sowohl Additive verwendet werden, die in der Komponente (A) löslich als auch Additive, die in den PFPE-Ölen der Komponente (D) löslich oder aber auch in beiden Ölphasen unlöslich sind.The component (G) will be selected from the group consisting of corrosion protection additives, antioxidants, wear protection additives, UV stabilizers. Both additives that are soluble in component (A) and additives that are soluble in the PFPE oils of component (D) or insoluble in both oil phases can be used.
Beispiele für Antioxidantien sind styrolisierte Diphenylamine, diaromatische Amine, Phenolharze, Thiophenolharze, Phosphite, butyliertes Hydroxytoluol, butyliertes Hydroxyanisol, Phenyl-alpha-naphthylamin, Phenyl-beta-naphthylamin, octyliertes/butyliertes Diphenylamin, di-alpha-Tocopherol, di-tert.-butyl-Phenol oder ditert.butyl-4-methylphenol, Benzolpropansäure, schwefelhaltige Phenolverbindungen, Phenolverbindungen und Mischungen dieser Komponenten.Examples of antioxidants are styrenated diphenylamines, diaromatic amines, phenolic resins, thiophenolic resins, phosphites, butylated hydroxytoluene, butylated hydroxyanisole, phenyl-alpha-naphthylamine, phenyl-beta-naphthylamine, octylated/butylated diphenylamine, di-alpha-tocopherol, di-tert-butyl-phenol or di-tert-butyl-4-methylphenol, benzenepropanoic acid, sulfur-containing phenolic compounds, phenolic compounds and mixtures of these components.
Beispiele für geeignete Korrosionsschutzadditive, Metalldesaktivatoren oder lonen-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.Examples of suitable anti-corrosion additives, metal deactivators or ion complexing agents are included. These include triazoles, imidazolines, N-methylglycine (sarcosine), benzotriazole derivatives, N,N-bis(2-ethylhexyl)-ar-methyl-1 H-benzotriazole-1-methanamine; n-Methyl-N(1-oxo-9-octadecenyl)glycine, mixture of phosphoric acid and mono- and di-isooctyl esters reacted with (C 11-14 )-alkylamines, mixture of phosphoric acid and mono- and di-isooctyl esters reacted with tert-alkylamine and primary (C 12-14 ) amines, dodecanoic acid, triphenylphosphorothionate and amine phosphates. Commercially available additives are the following: IRGAMET ® 39, IRGACOR ® DSS G, Amin 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, und Mischungen dieser Komponenten. Meistens weisen die genannten Verbindungen organische Gruppen auf. Zu den kommerziell erhältlichen Verschleißschutzadditiven gehören IRGALUBE® TPPT, URGALUBE® 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.Other wear protection additives are amines, amine phosphates, phosphates, thiophosphates, and mixtures of these components. Most of the compounds mentioned have organic groups. Commercially available anti-wear additives include IRGALUBE ® TPPT, URGALUBE ® 232, IRGALUBE ® 349, IRGALUBE ® 211 and ADDITIN ® RC3760 Liq 3960, FIRC-SHUN ® FG 1505 and FG 1506, NA-LUBE ® KR-015FG, LUBEBOND ® , F LUORO ® FG, SYNALOX ® 40-D, ACHESON ® FGA 1820 and ACHESON ® FGA 1810.
Als Additive können auch PFPE-Derivate enthalten sein. Beispielsweise PFPE-Carbonsäuren, deren Metall- und Ammoniumsalze, deren Ester- und Amid-Derivate. Weitere geeignete Substanzen sind beispielsweise in
Des Weiteren können die erfindungsgemäßen Schmierstoffzusammensetzungen Festschmierstoffe (H) enthalten, die ausgewählt werden aus der Gruppe bestehend aus 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. Die Festschmierstoffe (H) sind in Mengen von 0 bis 10 Gew.-%, bevorzugt 2 bis 5 Gew.% in der erfindungsgemäßen Schmierstoffzusammensetzung enthalten.Furthermore, the lubricant compositions according to the invention can contain solid lubricants (H) which are selected from the group consisting of 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 solid lubricants (H) are contained in the lubricant composition according to the invention in amounts of 0 to 10% by weight, preferably 2 to 5% by weight.
Die erfindungsgemäße Schmierstoffzusammensetzung wird im Bereich von Bauteilen, insbesondere in Wälzlagern, Gleitlagern, Transport- und Steuerketten in der Fahrzeugtechnik, bei Schienenfahrzeugen, der Fördertechnik, bei Folienreckanlagen, bei Wellpappanlagen, von Laufrollenlagern, Lüfterlagern, Lagern von Traktionsmotoren, zur Schmierung von Kegelrad- und Stirnradgetrieben, Federn, Schrauben und Kompressoren, Pneumatikkomponenten, Armaturen, und von Maschinenbauteilen und in Anlagen, bei denen es zum gelegentlichen, unbeabsichtigten Kontakt mit Lebensmitteln kommt, eingesetzt.The lubricant composition according to the invention is used in the area of components, in particular in rolling bearings, plain bearings, transport and control chains in vehicle technology, in rail vehicles, conveyor technology, in film stretching systems, in corrugated cardboard systems, in roller bearings, fan bearings, bearings in traction motors, for the lubrication of bevel gear and Helical gears, springs, screws and compressors, pneumatic components, fittings, and machine components and in systems where occasional, unintentional contact with food occurs.
Die beigefügten Figuren zeigen die Vorteile der erfindungsgemäßen Lithiumhybridkomplexfette:
-
Fig. 1 zeigt die Walkpenetration 60dT, -
Fig. 2 zeigt die Ölabscheidung, d.h. den Verlust des Öls aus dem Schmierfett.
-
Fig. 1 shows the full penetration 60dT, -
Fig. 2 shows oil separation, ie the loss of oil from the grease.
Die Erfindung nun anhand der folgenden Beispiele näher erläutert.The invention is now explained in more detail using the following examples.
Die Herstellung der erfindungsgemäßen Schmierstoffzusammensetzung ist nicht eingeschränkt und kann nach allen geeigneten Verfahren durchgeführt werden.The production of the lubricant composition according to the invention is not restricted and can be carried out using any suitable process.
Die Herstellung der erfindungsgemäßen Schmierstoffherstellung kann beispielsweise so erfolgen, dass mit den Komponenten (A) und/oder (B) und/oder (F) ein Grundölgemisch hergestellt wird. In diesem Grundölgemisch, das komplett oder nur teilweise in einem geeigneten Reaktionsbehälter, der Heiz-, Kühl- und Rühreinrichtungen enthält, vorgelegt wird, werden die für den Lithiumkomplexverdicker (C) erforderlichen Säuren eingeschmolzen und eine wässrige Lithiumhydroxidlösung zugegeben. Dadurch bildet sich ein Sud, der die Lithiumseifen der Carbonsäuren enthält. Die Säuren können einzeln zugegeben und neutralisiert werden oder aber es wird erst die Monocarbonsäure zugegeben und neutralisiert und in einem zweiten Schritt die höherfunktionelle Carbonsäure zugegeben und neutralisiert. Der Sud wird auf 130°C erhitzt um Wasser auszutreiben. Die Quellung des Verdickers (Lithiumkomplexseife) wird durch thermische Behandlung bei 150°C bis 210°C durchgeführt. Der thermisch behandelte Sud wird dann abgekühlt, wobei auch ein Teil des Grundölgemisches verwendet werden kann. Die Komponenten (D), (E), (G), (H) und eventuell nicht für das Grundölgemisch verwendeten (A), (B) und (F) werden bei einer geeigneten Temperatur zugegeben und durch Rühren vorhomogenisiert.The production of the lubricant according to the invention can be carried out, for example, by producing a base oil mixture with components (A) and/or (B) and/or (F). The acids required for the lithium complex thickener (C) and an aqueous lithium hydroxide solution are melted into this base oil mixture, which is placed completely or only partially in a suitable reaction vessel containing heating, cooling and stirring devices admitted. This creates a brew that contains the lithium soaps of the carboxylic acids. The acids can be added and neutralized individually or the monocarboxylic acid is added and neutralized first and in a second step the higher functional carboxylic acid is added and neutralized. The brew is heated to 130°C to drive off water. The swelling of the thickener (lithium complex soap) is carried out by thermal treatment at 150°C to 210°C. The thermally treated brew is then cooled, and part of the base oil mixture can also be used. The components (D), (E), (G), (H) and any components not used for the base oil mixture (A), (B) and (F) are added at a suitable temperature and pre-homogenized by stirring.
Feste Schmierstoffadditive, die im Grundölgemisch löslich sind, werden beispielsweise bei Temperaturen oberhalb ihres Schmelzpunktes zugegeben. Flüssige Additive oder nicht schmelzende Additive/Festschmierstoffe/Verdickerkomponenten werden bei Temperaturen unter 80°C zugegeben. Das so hergestellte Lithiumkomplexhybridfett kann durch geeignete Geräte wie Dreiwalzwerke, Kolloidmühlen oder Gaulin homogenisiert werden.Solid lubricant additives that are soluble in the base oil mixture are added, for example, at temperatures above their melting point. Liquid additives or non-melting additives/solid lubricants/thickener components are added at temperatures below 80°C. The lithium complex hybrid grease produced in this way can be homogenized using suitable equipment such as three-roll mills, colloid mills or Gaulin.
in dem so beschriebenen Verfahren wird die erfindungsgemäße Schmierstoffzusammensetzung in einem Prozess hergestellt. Alternativ kann die Zugabe des PFPE-Öles (D) und der optionalen Verdickerkomponente (E) in dem oben beschriebenen Verfahren unterbleiben, so dass ein Lithiumkomplexfett entsteht. Die Komponenten (D) und (E) können durch Rühren, Homogenisieren wie oben beschrieben zu einem PFPE-Fett vereinigt werden. Lithiumkomplexfett und PFPE-Fett können in einem zweiten Verfahrensschritt vereinigt werden und daraus unter Rühren und Homogenisieren die erfindungsgemäße Schmierstoffzusammensetzung hergestellt werden.In the method described in this way, the lubricant composition according to the invention is produced in one process. Alternatively, the addition of the PFPE oil (D) and the optional thickener component (E) can be omitted in the process described above, so that a lithium complex grease is formed. Components (D) and (E) can be combined to form a PFPE fat by stirring and homogenizing as described above. Lithium complex grease and PFPE grease can be combined in a second process step and the lubricant composition according to the invention can be produced therefrom while stirring and homogenizing.
Die Herstellung kann auch mit kontinuierlichen Verfahren erfolgen, wobei auch Li-Komplex-Fertigseife in Pulverform verwendet werden kann.The production can also be carried out using continuous processes, whereby ready-made Li complex soap in powder form can also be used.
Herstellung mehrerer erfindungsgemäßer Schmierstoffzusammensetzungen, Vergleich mit den zur Herstellung verwendeten Lithiumkomplexfett bzw. PFPE/PTFE-Fett, Vergleich mit Harnstoff HybridfettenProduction of several lubricant compositions according to the invention, comparison with the lithium complex grease or PFPE/PTFE grease used for production, comparison with urea hybrid greases
Lithiumkomplexseifenfett (Fett A) und ein PFPE/PTFE-Fett (Fett B) werden separat hergestellt und die beiden Fette A und B in unterschiedlichen Verhältnissen vermischt, gerührt und durch Walzen homogenisiert.Lithium complex soap grease (fat A) and a PFPE/PTFE grease (fat B) are produced separately and the two fats A and B are mixed in different ratios, stirred and homogenized by rolling.
Es wird ein Lithiumkomplexfett bestehend aus 77 % einer Mischung eines Alkyldiphenylether (100 mm"/sec/40°C) und Trimellithsäureester sowie vollhydriertem Polyisobutylen (vollhydriert, Mn ca. 1300 g/mol) als Grundöl, wobei sich eine Viskosität bei 40°C von 220 mm2/sec ergibt, hergestellt, dann werden 15 % Lithiumkomplex aus Azelainsäure und 12-Hydroxystearinsäure, sowie 8 % eines Additivpackages bestehend aus aminischen Antioxidantien, Phosphaten, Thiadiazolen, Triazolen und Aminphosphaten zugegeben. Die Walkpenetration liegt bei 270 1/10 mm (siehe Tabelle 1)A lithium complex grease consisting of 77% of a mixture of an alkyl diphenyl ether (100 mm "/sec/40 ° C) and trimellitic acid ester as well as fully hydrogenated polyisobutylene (fully hydrogenated, Mn approx. 1300 g / mol) is used as a base oil, with a viscosity at 40 ° C of 220 mm 2 /sec, then 15% lithium complex from azelaic acid and 12-hydroxystearic acid, as well as 8% of an additive package consisting of amine antioxidants, phosphates, thiadiazoles, triazoles and amine phosphates are added. The full penetration is 270 1/10 mm (see Table 1)
Es wird ein PFPE/PTFE-Fett, enthaltend zu 70 % eine Mischung aus linearem und verzweigtem PFPE, kinematische Viskosität 200 mm2/sec bei 40°C, 26 % PTFE-Mikropulver, durchschnittliche Teilchengröße d 50 (Laserbeugung, DIN ISO 9277) ca. 5 µm, spezifische Oberfläche (DIN ISO 9277) ca. 5 m2/g, und 4 % Dinatriumsebacat als Korrosionschutzadditiv hergestellt. Die Walkpenetration liegt bei 286 1/10 mm (siehe Tabelle 1)A PFPE/PTFE grease is used, containing 70% of a mixture of linear and branched PFPE, kinematic viscosity 200 mm 2 /sec at 40°C, 26% PTFE micropowder, average particle size d 50 (laser diffraction, DIN ISO 9277) approx. 5 µm, specific surface area (DIN ISO 9277) approx. 5 m 2 /g, and 4% disodium sebacate as a corrosion protection additive. The full penetration is 286 1/10 mm (see Table 1)
Mischung aus Fett A und Fett B im Verhältnis 10 Gew.-% zu 90 Gew.-%.Mixture of fat A and fat B in a ratio of 10% by weight to 90% by weight.
Mischung aus Fett A und Fett B im Verhältnis 30 Gew.-% zu 70 Gew.-%.Mixture of fat A and fat B in a ratio of 30% by weight to 70% by weight.
Mischung aus Fett A und Fett B im Verhältnis 50 Gew.-% zu 50 Gew.-%.Mixture of fat A and fat B in a ratio of 50% by weight to 50% by weight.
Mischung aus Fett A und Fett B im Verhältnis 70 Gew.-% zu 30 Gew.-%.Mixture of fat A and fat B in a ratio of 70% by weight to 30% by weight.
Mischung aus Fett A und Fett B im Verhältnis 90 Gew.-% zu 10 Gew.-%.Mixture of fat A and fat B in a ratio of 90% by weight to 10% by weight.
Es wird ein Harnstoffhybridfett bestehend zu 50 Gew.-% aus Fett B und zu 50 Gew.% aus einem Harnstofffett hergestellt. Das Harnstofffett besteht aus einer Mischung eines Trimellitsäureesters und einem Reaktionsprodukt aus Octylamin und Oleylamin mit einem MDI/TDI-Gemisch als Harnstoffverdicker, sowie Additiven. Die Grundölviskosität liegt bei ca. 80 mm2/sec. Die Walkpenetration liegt bei 265 mm2/sec (siehe Tabelle 2)A urea hybrid fat is produced consisting of 50% by weight of fat B and 50% by weight of a urea fat. The urea fat consists of a mixture of a trimellitic acid ester and a reaction product of octylamine and oleylamine with an MDI/TDI mixture as a urea thickener, as well as additives. The base oil viscosity is approx. 80 mm 2 /sec. The working penetration is 265 mm 2 /sec (see Table 2)
Es wird ein Harnstoffhybridfett bestehend aus einem Komplexester, Dimersäure basiert, V 40 apr. 400 mm"/sec bei 40°C und verzweigtem PFPE-ÖI mit einer kinematischen Viskosität von ca. 400 mm2/sec im Massenverhältnis 2:1 hergestellt. Der Harnstoffverdicker ist zu 10 % enthalten und ist ein Reaktionsprodukt aus Octylamin und Oleylamin mit einem MDI/TDI-Gemisch. Darüber hinaus sind 8 Gew.% PTFE-Pulver (wie bei Fett B) und 5 Gew.-% lösliche Additive (Antioxidantien, Aminphosphate) enthalten. Die Walkpenetration liegt bei 290 mm2/sec (siehe Tabelle 2)A urea hybrid fat consisting of a complex ester, dimer acid based, V 40 apr. 400 mm"/sec at 40°C and branched PFPE oil with a kinematic viscosity of approx. 400 mm 2 /sec in a mass ratio of 2:1. The urea thickener is contained at 10% and is a reaction product of octylamine and oleylamine with a MDI/TDI mixture. In addition, it contains 8% by weight of PTFE powder (as in grease B) and 5% by weight of soluble additives (antioxidants, amine phosphates). The working penetration is 290 mm 2 /sec (see Table 2 )
Tabelle 1 zeigt die allgemeinen Kenndaten der erfindungsgemäßen Lithumkomplexhybridfette der Beispiele B2-B4, der Referenzbeispiele B1 und B5 und der Fette A und B,
Tabelle 2 zeigt die Daten der Vergleichsbeispiele VG1 bis 2.
Wie in
Wie in
Auch legen die Daten nahe, dass ein gewünschtes Ölabscheidungsverhalten durch Wahl der Menge an Fetten A und B eingestellt werden kann.The data also suggests that a desired oil separation behavior can be adjusted by choosing the amount of fats A and B.
Die erfindungsgemäßen Schmierstoffzusammensetzungen wurden auf ihre thermische Beständigkeit überprüft und die Ergebnisse vor allem mit denen der Harnstoff-Hybridfette verglichen. Dazu wurden Untersuchungen hinsichtlich der Verdampfung und Viskosität unter Temperaturbelastung von 5 g Fett Einwaage in einem Edelstahl-Schälchen bei 200°C durchgeführt. Die Ergebnisse sind in den Tabellen 3 und 4 gezeigt.The lubricant compositions according to the invention were tested for their thermal stability and the results were compared, in particular, with those of the urea hybrid greases. For this purpose, studies were carried out regarding the evaporation and viscosity under temperature stress of 5 g of fat in a stainless steel bowl at 200 ° C. The results are shown in Tables 3 and 4.
Der Verdampfungsverlust wird nach der DIN-Norm 58397 bestimmt. Für jede Fettprobe werden jeweils drei Verdampfungsverlustschalen aus nicht-rostendem Stahl benötigt. Die Geometrie der Schalen ist in der Norm zur Bestimmung des Verdampfungsverlustes (DIN 58397) beschrieben. Zu Beginn wird das jeweilige Leergewicht der Schalen ermittelt. Im Anschluss werden die drei Verdampfungsverlustschalen mit der Fettprobe gefüllt. Dabei ist darauf zu achten, das Fett luftblasenfrei aufzubringen. Mit einem Abstreifer wird die Oberfläche glattgestrichen und überschüssiges Fett, das in die Randvertiefung der Schale gelangt ist, wird entfernt. Die Schalen werden anschließend in einem gängigen Labor-Trockenschrank mit Konvektion bei geschlossener Klappe bei entsprechender Prüftemperatur (hier 200°C) eingelagert. Nach der jeweils vorgegebenen Zeitdauer (48h, 96h, 144h und 168h) entnimmt man die Schalen aus dem Trockenschrank und lässt diese erkalten. Anschließend werden die Schalen gewogen. Der Verdampfungsverlust wird aus der Differenz von Einwaage zu gemessenem Wert ermittelt. Aus den drei Einzelwerten wird ein Mittelwert bestimmt (VM) Zusammen mit dem Mittelwert der drei Einwaagen (AM) lässt sich der Verdampfungsverlust berechnen. V = (VM / AM)*100 [% ]. Nach dem Auswiegen werden die Schalen bis zum nächsten Zeitpunkt in den Trockenschrank gestellt. Dies wird solange wiederholt, bis 168h vergangen sind.
Die Scherviskosität wird nach der DIN-Norm 53019 Teil 1 und Teil 3 bestimmt. Die Fettproben werden in jeweils drei Verdampfungsverlustschalen aus nicht-rostendem Stahl überführt. Die Geometrie der Schalen ist in der Norm zur Bestimmung des Verdampfungsverlustes (DIN 58397) beschrieben. Die Schalen werden anschließend in einem gängigen Labor-Trockenschrank mit Umwälzung bei entsprechender Prüftemperatur (hier 200°C) eingelagert. Nach der jeweils vorgegebenen Zeitdauer (48h, 96h, 144h und 168h) entnimmt man die Schalen aus dem Trockenschrank und lässt diese erkalten. Der Startwert für die Scherviskosität wird von jedem Fett vor der thermischen Belastung bestimmt.The shear viscosity is determined according to DIN standard 53019 part 1 and part 3. The fat samples are each transferred to three evaporation loss dishes made of stainless steel. The geometry of the shells is described in the standard for determining evaporation loss (DIN 58397). The trays are then stored in a standard laboratory drying cabinet with circulation at the appropriate test temperature (here 200°C). After the specified time period (48h, 96h, 144h and 168h), the bowls are removed from the drying cabinet and allowed to cool. The starting value for the shear viscosity is determined for each grease before thermal loading.
Die Messung der Scherviskosität erfolgt mit einem Gerät, das standardmäßig zur Bestimmung rheologischer Parameter von Schmierstoffen verwendet wird (z.B. Rheometer MCR 302 von Anton Paar).Shear viscosity is measured using a device that is standardly used to determine the rheological parameters of lubricants (e.g. Rheometer MCR 302 from Anton Paar).
Eingesetzt wird dabei ein Kegel-Platte-System (DIN EN ISO 3219 und DIN 53019), bevorzugt mit einem Messkegel, der einen Durchmesser von 25 mm aufweist. Die benötigte Menge an Fettprobe orientiert sich an typischen Mengen, die für rheologische Messungen erforderlich sind. Die Messdauer beträgt 120 s, wovon 60 s Temperier- bzw. Haltezeit sind. Gemessen wird bei einer konstanten Scherrate von 300 1/s und einer Temperatur von 25°C. Der Wert, der nach 90 s abgelesen werden kann, stellt die Scherviskosität für die jeweilige Fettprobe dar. Aus den drei ermittelten Einzelwerten wird der Mittelwert gebildet und final angegeben.
Die Fette der Beispiele 1 bis 5 wurden nun mit den Fetten der Vergleichsbeispiele 1 und 2 und den beiden Einzelfetten (A) und (B) hinsichtlich ihrer thermischen Beständigkeit verglichen. Die Ergebnisse sind in den Tabellen 5 und 6 gezeigt.
Die obigen Ergebnisse zeigen, dass mit den erfindungsgemäßen Lithiumkomplexhybridfetten der Anstieg der Scherviskosität deutlich niedriger ausfällt als bei den Vergleichsprodukten VG1 und VG2. VG2 zeigt bereits nach 96 h eine Scherviskosität von 100.000 mPas und ist nicht mehr schmierfähig. VG1 zeigt nach 168 h Prüfzeit eine doppelt so hohe Scherviskosität als alle erfindungsgemäßen Zusammensetzungen B1 bis B5, siehe Tabelle 4.The above results show that with the lithium complex hybrid greases according to the invention, the increase in shear viscosity is significantly lower than with the comparison products VG1 and VG2. VG2 shows a shear viscosity of 100,000 mPas after just 96 hours and is no longer lubricable. After 168 hours of testing, VG1 shows a shear viscosity that is twice as high as all compositions B1 to B5 according to the invention, see Table 4.
Das PFPE/PTFE-Fett (Fett B) zeigt in dem Test erwartungsgemäß die geringsten Verdampfungsverluste. Überraschenderweise liegt die Scherviskosität der erfindungsgemäßen Beispiele B1, B2 und B4 nach 168 h Prüfzeit niedriger als bei Fett B und zeigt damit günstigeres Verhärtungsverhalten.As expected, the PFPE/PTFE grease (fat B) shows the lowest evaporation losses in the test. Surprisingly, the shear viscosity of examples B1, B2 and B4 according to the invention after 168 hours of testing is lower than that of grease B and thus shows more favorable hardening behavior.
Insgesamt zeigt sich, dass das Verhärtungsverhalten der erfindungsgemäßen Schmierstoffe bei hohen Temperaturen günstiger ist als bei Harnstoff-Hybridfetten. Überraschenderweise wurde sogar gefunden, dass bei manchen der erfindungsgemäßen Zusammensetzungen sogar eine geringere Verhärtung auftritt als bei einem PFPE/PTFE-Fett. Überraschenderweise wurde auch gefunden, dass das Ölabscheidungsverhalten der erfindungsgemäßen Schmierstoffe durch Wahl von bestimmten Mischungsverhältnisses der Fette A (Lithiumkomplexfett) und B (PTFE/PFPE-Fett) eingestellt und somit auf unterschiedliche Anforderungen angepasst werden kann.Overall, it can be seen that the hardening behavior of the lubricants according to the invention at high temperatures is more favorable than that of urea hybrid greases. Surprisingly, it was even found that with some of the compositions according to the invention even less hardening occurs than with a PFPE/PTFE grease. Surprisingly, it was also found that the oil separation behavior of the lubricants according to the invention can be adjusted by choosing a specific mixing ratio of the fats A (lithium complex fat) and B (PTFE/PFPE fat) and can therefore be adapted to different requirements.
Herstellung eines erfindungsgemäßen Schmierstoffes mit unterschiedlichen HerstellverfahrenProduction of a lubricant according to the invention using different production processes
Wie bereits beschrieben, können die erfindungsgemäßen Schmierstoffe auf verschiedene Weise hergestellt werden. Bei der Variante "im Kessel gemischt" werden ein Lithiumkomplexfett (Fett C) und ein PFPE/PTFE-Fett (Fett D) getrennt hergestellt und dann in einem Kessel im Verhältnis 40 zu 60 Gew.-% unter Rühren gemischt. Das so entstehende Lithiumkomplexhybridfett B6 wird mit einem Dreiwalzwerk abschließend homogenisiert.As already described, the lubricants according to the invention can be produced in various ways. In the "mixed in the kettle" variant, a lithium complex fat (fat C) and a PFPE/PTFE fat (fat D) are produced separately and then mixed in a kettle in a ratio of 40 to 60% by weight with stirring. The resulting lithium complex hybrid grease B6 is then homogenized using a three-roll mill.
Bei der "in situ" Herstellung wird das Lithiumkomplexfett identisch zum Fett C hergestellt, beim Abkühlen werden dann aber, abweichend auch die Bestandteile des Fettes D, zugegeben, sodass die erfindungsgemäße Schmierstoffzusammensetzung in einem Arbeitsgang hergestellt wird. Die erfindungsgemäße Schmierstoffzusammensetzung B6 wird ebenfalls abschließend gewalzt.During "in situ" production, the lithium complex grease is produced identically to grease C, but when it cools down, the components of grease D are also added, so that the lubricant composition according to the invention is produced in one operation. The lubricant composition B6 according to the invention is also finally rolled.
Es wird ein Lithiumkomplexfett bestehend aus 80 Gew.-%% einer Mischung eines Alkyldiphenylether (100 mm2/sec bei 40°C) und eines Trimellitsäureesters sowie vollhydriertem Polyisobutylen (vollhydriert, Mn ca. 1300 g/mol) als Grundöl hergestellt, wobei sich eine Viskosität bei 40°C von 100 mm2/sec ergibt. 15 Gew.-% eines Lithiumkomplexes aus Azelainsäure und 12-Hydroxystearinsäure, sowie 5 Gew.-% eines Additivpackages bestehend aus aminischen Antioxidantien, Phosphaten werden bereitgestellt. Die Walkpenetration liegt bei 327 1/10 mm.A lithium complex fat consisting of 80% by weight of a mixture of an alkyl diphenyl ether (100 mm 2 /sec at 40 ° C) and a trimellitic acid ester and fully hydrogenated polyisobutylene (fully hydrogenated, Mn approx. 1300 g / mol) is produced as a base oil, whereby a viscosity at 40°C of 100 mm 2 /sec. 15% by weight of a lithium complex made from azelaic acid and 12-hydroxystearic acid, as well as 5% by weight of an additive package consisting of aminic antioxidants and phosphates are provided. The full penetration is 327 1/10 mm.
Es wird ein PFPE/PTFE-Fett, enthaltend zu 65 Gew.-% eine Mischung aus linearem und verzweigtem PFPE, einer kinematischen Viskosität von 145 mm2/sec bei 40°C, 33 Gew.-% PTFE-Mikropulver, durchschnittliche Teilchengröße d 50 (Laserbeugung, DIN ISO 9277) ca. 5 µm, spezifische Oberfläche (DIN ISO 9277) ca. 5 m2/g, und 2 Gew.% Dinatriumsebacat als Korrosionschutzadditiv hergestellt. Die Walkpenetration liegt bei 286 1/10 mm
Beide Herstellungsvarianten liefern im Rahmen der Messgenauigkeit gleiche Werte.Both manufacturing variants deliver the same values in terms of measurement accuracy.
Aufgrund der vorliegenden Daten kann B6, nach Herstellungsbeispiel 1 und Herstellungsbeispiel 2, mit beiden Herstellvarianten als Schmierstoff eingesetzt werden.Based on the available data, B6, according to production example 1 and production example 2, can be used as a lubricant with both production variants.
Somit ist gezeigt, dass die erfindungsgemäßen Schmierstoffzusammensetzungen mit unterschiedlichen Verfahren hergestellt werden können.This shows that the lubricant compositions according to the invention can be produced using different processes.
Claims (14)
- Lithium complex hybrid grease, containing(A) 60 to 15 % by weight of an ester or of an ester mixture, selected from the group consisting of trimellitic acid esters, which as an alkoxy group comprise linear or branched alkyl groups, which contain 6 to 18 carbon atoms, preferably 8 to 14 carbon atoms, wherein the alkoxy groups can be the same or different, pyromellitic acid esters, hydrogenated or unhydrogenated dimer acids, estolides,(B) 0.5 to 20 % by weight of non-hydrogenated, hydrogenated, or fully hydrogenated polyisobutylene or mixtures thereof,(C) 1 to 18 % by weight of lithium complex soaps, and(D) 15 to 40 % by weight of perfluoropolyether (PFPE)
- Lithium complex hybrid grease according to claim 1, further comprising (E) 1 to 30 % of a further thickening agent.
- Lithium complex hybrid grease according to any one of the preceding claims, containing
(F) 0 to 20 % by weight, preferably 2 to 20 % by weight, of a further oil component. - Lithium complex hybrid grease according to any one of the preceding claims, containing
(G) 0 to 10 % by weight, preferably 0.1 to 10 % by weight, of additives. - Lithium complex hybrid grease according to any one of the preceding claims, containing
(H) 0 to 10 % by weight, preferably 2 to 5 % by weight, of solid lubricant. - Lithium complex hybrid grease according to any one of the preceding claims, characterized in that the pyromellitic acid ester of the component (A) is tetrakis(2-ethylhexyl) pyromellitate, and the dimer acid is bis(2-ethylhexyl) dimerate.
- Lithium complex hybrid grease according to claim 2, characterized in that the component (E) is selected from the group consisting of Al-complex soaps, metal simple soaps of the elements of the first and second main group of the periodic system without lithium, metal complex soaps of the elements of the first and second main group of the periodic system without lithium, bentonite, sulphonates, silicates, aerosil, polyimide, PTFE, or a mixture thereof.
- Lithium complex hybrid grease according to claim 3, characterized in that the component (F) is selected from the group consisting of mineral oil, alkylated benzols, alkylated naphthaline, aliphatic carboxylic acid and dicarboxylic acid esters, fatty acid glycerides, alkylated diphenyl ether, phloroglucinol ester, and/or poly-alpha olefins, alpha-olefin copolymers, metallocene catalyzed poly-alpha olefins.
- Lithium complex hybrid grease according to claim 4, characterized in that the component (G) is selected from the group consisting of corrosion protection additives, antioxidants, wear protection additives, UV-stabilizers.
- Lithium complex hybrid grease according to claim 5, characterized in that the component (H) is selected from the group consisting of BN, pyrophosphate, Zn-oxide, Mg-oxide, pyrophosphates, thiosulphate, Mg-carbonate, Ca-carbonate, Ca-stearate, Zn-sulphide, Mo-sulphide, W-sulphide, Sn-sulphide, graphites, graphene, nano-tubes, SiO2 modifications, or a mixture thereof.
- Use of a lithium complex hybrid grease according to any one of the preceding claims, for the lubrication of components, in particular in roller bearings, slide bearings, transport and control chains in automotive technology, on rail vehicles, in conveying technology, in film stretching systems, in corrugated cardboard systems, in bearings for run rollers, ventilator and fan bearings, bearings for traction motors, for lubricating bevel gears and spur gears, springs, screws and compressors, pneumatic components, armatures, and of machine components and in systems in which there is occasional unintentional contact with foodstuffs.
- Method for the lubrication or greasing of components, in particular in roller bearings, slide bearings, transport and control chains in automotive technology and on rail vehicles, the method comprising:
Application of a lubricant composition onto the surface of the component, the lubricant comprising:(A) 60-15 % by weight of an ester or an ester mixture, selected from the group consisting of trimellitic acid esters, which as an alkoxy group comprise linear or branched alkyl groups, which contain 6 to 18 carbon atoms, preferably 8 to 14 carbon atoms, wherein the alkoxy groups can be the same or different, pyromellitic acid esters, hydrogenated or unhydrogenated dimer acids, estolides(B) 0.5 to 20 % by weight of non-hydrogenated, hydrogenated, or fully hydrogenated polyisobutylene or mixtures thereof,(C) 1 to 18 % by weight of lithium complex soaps, and(D) 15 to 40 % by weight of perfluoropolyether (PFPE). - Method for lubricating or greasing bearings for run rollers in continuous casting plants, bearings for transport rollers in continuous furnaces, of open ring gears in rotary furnaces, pipe mills, drums and mixers, bearings in corrugated cardboard systems and film stretching systems, bearings in systems for the production and transport of foodstuffs, the method comprising:
Application of a lubricant composition onto the surface of the component, the lubricant comprising:(A) 60-15 % by weight of an ester or an ester mixture, selected from the group consisting of trimellitic acid esters, which as an alkoxy group comprise linear or branched alkyl groups, which contain 6 to 18 carbon atoms, preferably 8 to 14 carbon atoms, wherein the alkoxy groups can be the same or different, pyromellitic acid esters, hydrogenated or unhydrogenated dimer acids, estolides,(B) 0.5 to 20 % by weight of non-hydrogenated, hydrogenated, or fully(C) 1 to 18 % by weight of lithium complex soaps, and(D) 15 to 40 % by weight of perfluoropolyether (PFPE). - Method for the reduction of the hardening of lubricant greases at 200 °C and/or for the reduction of the oil deposition of lubricant greases on run rollers in continuous casting plants, bearings for transport rollers in continuous furnaces, of open ring gears in rotary furnaces, pipe mills, drums and mixers, bearings in corrugated cardboard systems and film stretching systems, bearings in systems for the production and transport of foodstuffs, the method comprising:
Application of a lubricant composition onto the surface of the component, the lubricant comprising:(A) 60-15 % by weight of an ester or an ester mixture, selected from the group consisting of trimellitic acid esters, which as an alkoxy group comprise linear or branched alkyl groups, which contain 6 to 18 carbon atoms, preferably 8 to 14 carbon atoms, wherein the alkoxy groups can be the same or different, pyromellitic acid esters, hydrogenated or unhydrogenated dimer acids, estolides(B) 0.5 to 20 % by weight of non-hydrogenated, hydrogenated, or fully hydrogenated polyisobutylene or mixtures thereof,(C) 1 to 18 % by weight of lithium complex soaps, and(D) 15 to 40 % by weight of perfluoropolyether (PFPE).
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102020112993.9A DE102020112993A1 (en) | 2020-05-13 | 2020-05-13 | Lithium complex hybrid grease |
| PCT/EP2021/052523 WO2021228442A1 (en) | 2020-05-13 | 2021-02-03 | Lithium complex hybrid grease |
Publications (2)
| Publication Number | Publication Date |
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| EP4090723A1 EP4090723A1 (en) | 2022-11-23 |
| EP4090723B1 true EP4090723B1 (en) | 2023-11-29 |
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| EP21704440.3A Active EP4090723B1 (en) | 2020-05-13 | 2021-02-03 | Lithium complex hybrid grease |
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| US (1) | US20230138681A1 (en) |
| EP (1) | EP4090723B1 (en) |
| CN (1) | CN115461434B (en) |
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| CN114150525B (en) * | 2021-11-26 | 2022-12-27 | 上海东升新材料有限公司 | Nano modified lubricant for papermaking |
| CN114574273B (en) * | 2022-03-18 | 2022-08-12 | 中国科学院兰州化学物理研究所 | Bearing roller bearing bush lubricating oil and preparation method and application thereof |
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| DE3918107A1 (en) | 1989-06-02 | 1990-12-06 | Klueber Lubrication | LUBRICATING GREASE COMPOSITION |
| DE19622906A1 (en) | 1996-06-07 | 1997-12-11 | Klueber Lubrication | Grease compositions |
| US6018063A (en) | 1998-11-13 | 2000-01-25 | The United States Of America As Represented By The Secretary Of Agriculture | Biodegradable oleic estolide ester base stocks and lubricants |
| US6184187B1 (en) | 1998-04-07 | 2001-02-06 | E. I. Dupont De Nemours And Company | Phosphorus compounds and their use as corrosion inhibitors for perfluoropolyethers |
| US6316649B1 (en) | 1998-11-13 | 2001-11-13 | The United States Of America As Represented By The Secretary Of Agriculture | Biodegradable oleic estolide ester having saturated fatty acid end group useful as lubricant base stock |
| WO2001027916A1 (en) | 1999-10-14 | 2001-04-19 | E.I. Du Pont De Nemours And Company | Phosphorous and fluorine containing compounds as magnetic media lubricants |
| US6541430B1 (en) | 2000-03-24 | 2003-04-01 | E. I. Du Pont De Nemours And Company | Fluorinated lubricant additives |
| JP5386803B2 (en) * | 2007-07-31 | 2014-01-15 | Ｎｏｋクリューバー株式会社 | Grease composition |
| ITMI20042238A1 (en) | 2004-11-19 | 2005-02-19 | Solvay Solexis Spa | COMPOUNDS FOR FLUOROPOLIRTEREI |
| US20110218128A1 (en) * | 2008-10-17 | 2011-09-08 | Nok Kluber Co., Ltd. | Lubricating grease composition and method for producing the same |
| US20150011446A1 (en) | 2012-02-17 | 2015-01-08 | Solvay Specialty Polymers Italy S.P.A. | (PER)FLUOROPOLYETHERS WITH bi- OR ter-PHENYL END GROUPS |
| US9018406B2 (en) | 2012-03-27 | 2015-04-28 | Biosynthetic Technologies, Llc | Dicarboxylate-capped estolide compounds and methods of making and using the same |
| US20150175931A1 (en) * | 2013-12-19 | 2015-06-25 | Hyundai Motor Company | Grease composition for engine bearing |
| DE102014018718A1 (en) * | 2014-12-17 | 2016-06-23 | Klüber Lubrication München Se & Co. Kg | High temperature lubricants |
| DE102014018719A1 (en) * | 2014-12-17 | 2016-06-23 | Klüber Lubrication München Se & Co. Kg | High temperature lubricant for the food industry |
| EP3385358B1 (en) * | 2015-12-04 | 2020-06-03 | NOK Klueber Co., Ltd. | Lubricant composition |
| DE102018002041A1 (en) | 2017-03-29 | 2018-10-04 | Klüber Lubrication München Se & Co. Kg | New ester compounds, process for their preparation and their use |
| JP6755905B2 (en) * | 2018-07-27 | 2020-09-16 | ミネベアミツミ株式会社 | Grease composition for resin lubrication and resin sliding member |
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2020
- 2020-05-13 DE DE102020112993.9A patent/DE102020112993A1/en active Pending
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2021
- 2021-02-03 EP EP21704440.3A patent/EP4090723B1/en active Active
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| EP4090723A1 (en) | 2022-11-23 |
| DE102020112993A1 (en) | 2021-11-18 |
| CN115461434A (en) | 2022-12-09 |
| US20230138681A1 (en) | 2023-05-04 |
| WO2021228442A1 (en) | 2021-11-18 |
| CN115461434B (en) | 2024-03-22 |
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