JP5429285B2 - Lubricating grease composition for reciprocating sliding and manufacturing method thereof - Google Patents
Lubricating grease composition for reciprocating sliding and manufacturing method thereof Download PDFInfo
- Publication number
- JP5429285B2 JP5429285B2 JP2011511173A JP2011511173A JP5429285B2 JP 5429285 B2 JP5429285 B2 JP 5429285B2 JP 2011511173 A JP2011511173 A JP 2011511173A JP 2011511173 A JP2011511173 A JP 2011511173A JP 5429285 B2 JP5429285 B2 JP 5429285B2
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- JP
- Japan
- Prior art keywords
- base oil
- fluorine
- weight
- lubricating grease
- reciprocating sliding
- 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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- 239000004519 grease Substances 0.000 title claims description 118
- 239000000203 mixture Substances 0.000 title claims description 43
- 230000001050 lubricating effect Effects 0.000 title claims description 34
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 239000011737 fluorine Substances 0.000 claims description 74
- 229910052731 fluorine Inorganic materials 0.000 claims description 74
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 71
- 239000002199 base oil Substances 0.000 claims description 71
- 239000000344 soap Substances 0.000 claims description 36
- 239000002131 composite material Substances 0.000 claims description 30
- 239000003921 oil Substances 0.000 claims description 30
- 229910052751 metal Inorganic materials 0.000 claims description 28
- 239000002184 metal Substances 0.000 claims description 28
- 239000002562 thickening agent Substances 0.000 claims description 24
- 239000000843 powder Substances 0.000 claims description 22
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 10
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 9
- 125000001931 aliphatic group Chemical group 0.000 claims description 9
- 229910052788 barium Inorganic materials 0.000 claims description 8
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 8
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 7
- 229910052744 lithium Inorganic materials 0.000 claims description 7
- 239000004215 Carbon black (E152) Substances 0.000 claims description 6
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 6
- 229930195733 hydrocarbon Natural products 0.000 claims description 6
- 150000002430 hydrocarbons Chemical class 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 6
- 229920005989 resin Polymers 0.000 claims description 6
- 229910000000 metal hydroxide Inorganic materials 0.000 claims description 3
- 150000004692 metal hydroxides Chemical class 0.000 claims description 3
- 150000002762 monocarboxylic acid derivatives Chemical class 0.000 claims 2
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 claims 1
- 229910001863 barium hydroxide Inorganic materials 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
- -1 trimellitic acid ester Chemical class 0.000 description 26
- 239000003963 antioxidant agent Substances 0.000 description 15
- 238000012360 testing method Methods 0.000 description 15
- 150000001412 amines Chemical class 0.000 description 12
- 238000002156 mixing Methods 0.000 description 12
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 12
- 239000004810 polytetrafluoroethylene Substances 0.000 description 12
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 12
- 230000003078 antioxidant effect Effects 0.000 description 10
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-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
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 description 8
- HCDGVLDPFQMKDK-UHFFFAOYSA-N hexafluoropropylene Chemical compound FC(F)=C(F)C(F)(F)F HCDGVLDPFQMKDK-UHFFFAOYSA-N 0.000 description 8
- 238000004898 kneading Methods 0.000 description 8
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 7
- 235000014113 dietary fatty acids Nutrition 0.000 description 6
- 238000001704 evaporation Methods 0.000 description 6
- 230000008020 evaporation Effects 0.000 description 6
- 239000000194 fatty acid Substances 0.000 description 6
- 229930195729 fatty acid Natural products 0.000 description 6
- 229920013639 polyalphaolefin Polymers 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 239000002480 mineral oil Substances 0.000 description 5
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- 239000000314 lubricant Substances 0.000 description 4
- 238000005461 lubrication Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- WLJVNTCWHIRURA-UHFFFAOYSA-N pimelic acid Chemical compound OC(=O)CCCCCC(O)=O WLJVNTCWHIRURA-UHFFFAOYSA-N 0.000 description 4
- 238000006116 polymerization reaction Methods 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- TYFQFVWCELRYAO-UHFFFAOYSA-N suberic acid Chemical compound OC(=O)CCCCCCC(O)=O TYFQFVWCELRYAO-UHFFFAOYSA-N 0.000 description 4
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- WXUAQHNMJWJLTG-UHFFFAOYSA-N 2-methylbutanedioic acid Chemical compound OC(=O)C(C)CC(O)=O WXUAQHNMJWJLTG-UHFFFAOYSA-N 0.000 description 2
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- WMRCTEPOPAZMMN-UHFFFAOYSA-N 2-undecylpropanedioic acid Chemical compound CCCCCCCCCCCC(C(O)=O)C(O)=O WMRCTEPOPAZMMN-UHFFFAOYSA-N 0.000 description 2
- OHGCZFNOIOXHIN-UHFFFAOYSA-N 9-(octylamino)-9-oxononanoic acid Chemical compound CCCCCCCCNC(=O)CCCCCCCC(O)=O OHGCZFNOIOXHIN-UHFFFAOYSA-N 0.000 description 2
- VVJKKWFAADXIJK-UHFFFAOYSA-N Allylamine Chemical compound NCC=C VVJKKWFAADXIJK-UHFFFAOYSA-N 0.000 description 2
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- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
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- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005536 corrosion prevention Methods 0.000 description 1
- KZZKOVLJUKWSKX-UHFFFAOYSA-N cyclobutanamine Chemical compound NC1CCC1 KZZKOVLJUKWSKX-UHFFFAOYSA-N 0.000 description 1
- NISGSNTVMOOSJQ-UHFFFAOYSA-N cyclopentanamine Chemical compound NC1CCCC1 NISGSNTVMOOSJQ-UHFFFAOYSA-N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
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- 150000001991 dicarboxylic acids Chemical class 0.000 description 1
- 229940043279 diisopropylamine Drugs 0.000 description 1
- WEHWNAOGRSTTBQ-UHFFFAOYSA-N dipropylamine Chemical compound CCCNCCC WEHWNAOGRSTTBQ-UHFFFAOYSA-N 0.000 description 1
- 150000002019 disulfides Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
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- 238000010894 electron beam technology Methods 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
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- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
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- ZQKXQUJXLSSJCH-UHFFFAOYSA-N melamine cyanurate Chemical compound NC1=NC(N)=NC(N)=N1.O=C1NC(=O)NC(=O)N1 ZQKXQUJXLSSJCH-UHFFFAOYSA-N 0.000 description 1
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
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- MJCJUDJQDGGKOX-UHFFFAOYSA-N n-dodecyldodecan-1-amine Chemical compound CCCCCCCCCCCCNCCCCCCCCCCCC MJCJUDJQDGGKOX-UHFFFAOYSA-N 0.000 description 1
- NQYKSVOHDVVDOR-UHFFFAOYSA-N n-hexadecylhexadecan-1-amine Chemical compound CCCCCCCCCCCCCCCCNCCCCCCCCCCCCCCCC NQYKSVOHDVVDOR-UHFFFAOYSA-N 0.000 description 1
- HKUFIYBZNQSHQS-UHFFFAOYSA-N n-octadecyloctadecan-1-amine Chemical compound CCCCCCCCCCCCCCCCCCNCCCCCCCCCCCCCCCCCC HKUFIYBZNQSHQS-UHFFFAOYSA-N 0.000 description 1
- DYUWTXWIYMHBQS-UHFFFAOYSA-N n-prop-2-enylprop-2-en-1-amine Chemical compound C=CCNCC=C DYUWTXWIYMHBQS-UHFFFAOYSA-N 0.000 description 1
- HSUGDXPUFCVGES-UHFFFAOYSA-N n-tetradecyltetradecan-1-amine Chemical compound CCCCCCCCCCCCCCNCCCCCCCCCCCCCC HSUGDXPUFCVGES-UHFFFAOYSA-N 0.000 description 1
- BNJOQKFENDDGSC-UHFFFAOYSA-N octadecanedioic acid Chemical compound OC(=O)CCCCCCCCCCCCCCCCC(O)=O BNJOQKFENDDGSC-UHFFFAOYSA-N 0.000 description 1
- 239000012860 organic pigment Substances 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- DPBLXKKOBLCELK-UHFFFAOYSA-N pentan-1-amine Chemical compound CCCCCN DPBLXKKOBLCELK-UHFFFAOYSA-N 0.000 description 1
- 125000005004 perfluoroethyl group Chemical group FC(F)(F)C(F)(F)* 0.000 description 1
- 125000005009 perfluoropropyl group Chemical group FC(C(C(F)(F)F)(F)F)(F)* 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000007539 photo-oxidation reaction Methods 0.000 description 1
- 229920001515 polyalkylene glycol Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920001083 polybutene Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
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- 229920001155 polypropylene Polymers 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- CYIDZMCFTVVTJO-UHFFFAOYSA-N pyromellityc acid Natural products OC(=O)C1=CC(C(O)=O)=C(C(O)=O)C=C1C(O)=O CYIDZMCFTVVTJO-UHFFFAOYSA-N 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 231100000241 scar Toxicity 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000010557 suspension polymerization reaction Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- VLLMWSRANPNYQX-UHFFFAOYSA-N thiadiazole Chemical compound C1=CSN=N1.C1=CSN=N1 VLLMWSRANPNYQX-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 1
- 125000006617 triphenylamine group Chemical class 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- 150000003672 ureas Chemical class 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
-
- 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
-
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
- C10M2205/028—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms
- C10M2205/0285—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms used as base material
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/04—Ethers; Acetals; Ortho-esters; Ortho-carbonates
- C10M2207/0406—Ethers; Acetals; Ortho-esters; Ortho-carbonates used as base material
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—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
- C10M2207/1256—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 used as thickening agent
-
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—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
- C10M2207/126—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 monocarboxylic
- C10M2207/1265—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 monocarboxylic used as thickening agent
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—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
- 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
- C10M2207/1276—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 used as thickening agent
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
- C10M2213/04—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions obtained from monomers containing carbon, hydrogen, halogen and oxygen
- C10M2213/043—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions obtained from monomers containing carbon, hydrogen, halogen and oxygen used as base material
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
- C10M2213/06—Perfluoro polymers
- C10M2213/062—Polytetrafluoroethylene [PTFE]
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
- C10M2213/06—Perfluoro polymers
- C10M2213/062—Polytetrafluoroethylene [PTFE]
- C10M2213/0626—Polytetrafluoroethylene [PTFE] used as thickening agents
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
- C10M2215/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
- C10M2215/064—Di- and triaryl amines
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
- C10M2229/04—Siloxanes with specific structure
- C10M2229/05—Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon
- C10M2229/051—Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon containing halogen
- C10M2229/0515—Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon containing halogen used as base material
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2010/00—Metal present as such or in compounds
- C10N2010/02—Groups 1 or 11
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- C10N2010/00—Metal present as such or in compounds
- C10N2010/04—Groups 2 or 12
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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
- C10N2020/02—Viscosity; Viscosity index
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- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/02—Pour-point; Viscosity index
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2040/00—Specified use or application for which the lubricating composition is intended
- C10N2040/14—Electric or magnetic purposes
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2050/00—Form in which the lubricant is applied to the material being lubricated
- C10N2050/10—Semi-solids; greasy
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Lubricants (AREA)
Description
本発明は、往復摺動用潤滑グリース組成物およびその製造法に関する。さらに詳しくは、互いに相溶性のない非フッ素系基油およびフッ素系基油よりなる基油混合物を用いた往復摺動用潤滑グリース組成物およびその製造法に関する。 The present invention relates to a lubricating grease composition for reciprocating sliding and a method for producing the same. More specifically, the present invention relates to a lubricating grease composition for reciprocating sliding using a base oil mixture composed of a non-fluorine base oil and a fluorine base oil that are not compatible with each other, and a method for producing the same.
往復摺動機構を有する代表的な産業用小型部品としては、マイクロスイッチや電磁駆動弁等がある。例えば、封入形マイクロスイッチは、アクチュエータ部位に加えられた外力が、内部のバネ機構に伝わり、可動接点を動かし、スイッチの開閉を行わせる部品である。アクチュエータに加えられた外力は、スイッチの開閉を行うためのプランジャの往復動に置き換えられる。その場合、プランジャと封入ケース部材との間の摺動は、可動範囲が数mmの往復動がくり返し行われる。 Typical industrial small parts having a reciprocating sliding mechanism include a micro switch and an electromagnetically driven valve. For example, an encapsulated microswitch is a component that causes an external force applied to an actuator part to be transmitted to an internal spring mechanism to move a movable contact and open / close the switch. The external force applied to the actuator is replaced with a reciprocating movement of the plunger for opening and closing the switch. In this case, the sliding between the plunger and the enclosing case member is repeatedly performed in a reciprocating manner with a movable range of several mm.
この種の用途には、従来鉱油系や合成炭化水素油〔PAO〕系のグリースが使用されてきたが、近年は例えば120〜150℃あるいはそれ以上の高温条件下において使用される封入形マイクロスイッチにおいては、グリースの耐久性が不足するという問題が発生している。 For this type of application, mineral oil and synthetic hydrocarbon oil [PAO] greases have been used in the past, but in recent years, encapsulated microswitches used under high temperature conditions of 120 to 150 ° C or higher, for example. However, there is a problem that the durability of the grease is insufficient.
高温耐久性という点では、従来からフッ素系のグリースが使用されており、高温耐久性のみならず、低温特性、酸化安定性、耐薬品性などが必要とされる苛酷な条件下で使用されている。フッ素系のグリースは、一般にパーフルオロポリエーテル油を基油として、テトラフルオロエチレンの単独重合体〔PTFE〕やテトラフルオロエチレンとヘキサフルオロプロペンとの共重合体〔HFP〕等を増稠剤として構成されている。しかしながら、これらのフッ素系グリースは、被潤滑材料である樹脂、ゴム、金属等とのなじみが悪いという欠点を有する。 In terms of high temperature durability, fluorine-based grease has been used in the past, and it is used under severe conditions that require not only high temperature durability but also low temperature characteristics, oxidation stability, and chemical resistance. Yes. Fluorine grease is generally composed of perfluoropolyether oil as base oil and tetrafluoroethylene homopolymer [PTFE] or copolymer of tetrafluoroethylene and hexafluoropropene [HFP] as a thickener. Has been. However, these fluorinated greases have the disadvantage that they are not compatible with resins, rubbers, metals, etc., which are materials to be lubricated.
転がり軸受に代表される転動装置等に使用される場合には、ボールと転送面との間に介在するグリースが潤滑に寄与するばかりではなく、摺動に寄与していない周囲部分に存在するグリースも、回転運動により軸受内を移動し、摺動部に供給されることで、後々潤滑に寄与することが可能であるから、この場合には問題がみられない。 When used in a rolling device such as a rolling bearing, the grease interposed between the ball and the transfer surface not only contributes to lubrication but also exists in the surrounding portion that does not contribute to sliding. Since the grease also moves in the bearing by the rotational motion and is supplied to the sliding portion, it can contribute to lubrication later, so that no problem is observed in this case.
これに対し、一定間隔のくり返し摺動となる往復動では、グリースが摺動部から掻き取られ易く、また一度摺動部から掻き取られたグリースは、再度摺動部に供給され難いため、特にフッ素系グリースにあっては潤滑に必要な油膜が形成されず、その結果摩耗が発生したり、摩擦係数が高くなったりして、耐久性が得られなくなるといった問題を発生させる。 On the other hand, in the reciprocating motion that repeats sliding at regular intervals, the grease is easily scraped from the sliding portion, and the grease once scraped from the sliding portion is difficult to be supplied to the sliding portion again. In particular, in the case of fluorine-based grease, an oil film necessary for lubrication is not formed, and as a result, wear occurs and the friction coefficient increases, resulting in a problem that durability cannot be obtained.
特許文献1には、特定の混合割合で用いられた水素添加鉱油および/または合成潤滑油、フルオロポリエーテルおよび増稠剤を含んでなるグリースが記載されており、エステル油、12-ヒドロキシステアリン酸、アゼライン酸および水酸化リチウムよりなるグリースに過フッ素化油およびPTFEを添加したグリースが、実施例4として示されているが、それの評価試験は固着温度、蒸発による重量損失、油分離性についてのみなされており、軸受高温寿命については評価されておらず、それの用途についての具体的記載はみられない。 Patent Document 1 describes a grease comprising a hydrogenated mineral oil and / or a synthetic lubricating oil, a fluoropolyether and a thickener used at a specific mixing ratio, and an ester oil, 12-hydroxystearic acid. A grease composed of azelaic acid and lithium hydroxide with a perfluorinated oil and PTFE added is shown as Example 4, and its evaluation tests are for fixing temperature, weight loss due to evaporation, and oil separability. The bearing high temperature life has not been evaluated, and no specific description of its use has been found.
電気接点等の摺動部に用いられるグリースについては、本出願人自身がいくつかの提案を行っている。 The applicant himself has made several proposals for grease used in sliding parts such as electrical contacts.
特許文献2には、パーフルオロポリエーテル油、合成潤滑油および増稠剤を含有する潤滑グリース組成物が記載されており、それの評価は低温トルク、回転寿命、摩耗痕径(シェル摩耗試験)について行われている。 Patent Document 2 describes a lubricating grease composition containing a perfluoropolyether oil, a synthetic lubricating oil, and a thickener, and the evaluation thereof is low temperature torque, rotational life, wear scar diameter (shell wear test). Has been done about.
特許文献3には、合成炭化水素油、エステル油またはエーテル系合成油よりなる基油に、フッ素化油およびリチウム系複合石けん増稠剤を含有する潤滑グリース組成物が記載されており、それの評価はピンオンディスク摩耗試験について行われている。 Patent Document 3 describes a lubricating grease composition containing a fluorinated oil and a lithium-based composite soap thickener in a base oil composed of a synthetic hydrocarbon oil, an ester oil or an ether-based synthetic oil. Evaluation is conducted on a pin-on-disk wear test.
特許文献4には、極圧性および耐摩耗性にすぐれた潤滑グリース組成物として、パーフルオロポリエーテル基油に増稠剤として脂肪酸金属塩とフッ素樹脂とが混合されたものとして構成されている。 Patent Document 4 is configured as a lubricating grease composition excellent in extreme pressure property and wear resistance in which a perfluoropolyether base oil is mixed with a fatty acid metal salt and a fluororesin as a thickener.
本発明の目的は、非フッ素系基油およびフッ素系基油よりなる基油混合物に増稠剤およびフッ素樹脂を含有させた往復摺動用潤滑グリース組成物であって、往復摺動用潤滑グリースにとって必要な特性を有するものを提供することにある。 An object of the present invention is a lubricating grease composition for reciprocating sliding in which a thickener and a fluororesin are contained in a base oil mixture composed of a non-fluorinated base oil and a fluorinated base oil. The object is to provide a product having special characteristics.
かかる本発明の目的は、非フッ素系基油に脂肪族ジカルボン酸とモノアミドモノカルボン酸との複合金属石けん増稠剤を含有させた、滴点が250℃以上の非フッ素系グリースおよび非フッ素系基油と相溶性のないフッ素系基油にフッ素樹脂粉末を含有させたフッ素系グリースの2種のグリース混合物よりなるマイクロスイッチまたは電磁駆動弁のアクチュエータ部位に用いられる往復摺動用潤滑グリース組成物によって達成される。 An object of the present invention is to provide a non-fluorine-based grease and a non-fluorine-based grease having a dropping point of 250 ° C. or higher, containing a composite metal soap thickener of an aliphatic dicarboxylic acid and a monoamide monocarboxylic acid in a non-fluorine base oil. According to the lubricating grease composition for reciprocating sliding used in the actuator part of a micro switch or electromagnetically driven valve consisting of two types of grease mixture of fluorine grease containing fluorine resin powder in fluorine base oil incompatible with base oil Achieved.
非フッ素系基油に複合金属石けん増稠剤を含有させた非フッ素系グリースおよびフッ素系基油にフッ素樹脂粉末を含有させたフッ素系グリースの2種のグリース混合物よりなり、非フッ素系基油に複合金属石けんを含有させた非フッ素系グリースとして、グリースとして成立する上限温度に相当する滴点が250℃以上であるものを用いることにより、蒸発損失および離油度が少なく、またSRV試験(往復動試験)での摩擦係数の変動幅が小さくかつその変動が少なく、安定している潤滑グリース組成物が得られる。 This non-fluorine base oil consists of a mixture of two types of grease: non-fluorine grease containing a composite metal soap thickener in a non-fluorine base oil and fluorine grease containing a fluororesin powder in a fluorine base oil. By using a non-fluorine grease containing composite metal soap in the base, a drop point corresponding to the upper limit temperature established as a grease is 250 ° C or higher, resulting in low evaporation loss and oil separation, and SRV test ( A stable lubricating grease composition is obtained in which the fluctuation range of the friction coefficient in the reciprocating motion test is small and the fluctuation is small.
このように、フッ素系グリースが摺動部に十分保持され難く、また供給され難いような条件下においても、互いに相溶性のない非フッ素系基油およびフッ素系基油よりなる基油混合物中に、金属複合石けん増稠剤およびフッ素樹脂粉末を含有せしめた潤滑グリース組成物を用い、かつ金属複合石けん含有非フッ素系基油(非フッ素系グリース)の滴点が一定温度以上のものを用いることにより、フッ素系グリースの耐熱耐久性を維持しながら、摺動部にグリースを保持し易く、かつ摩擦係数を改善し得るという効果を奏する。 In this way, even under conditions where the fluorinated grease is not sufficiently held and supplied to the sliding portion, the base oil mixture composed of the non-fluorinated base oil and the fluorinated base oil which are not compatible with each other is contained. Use a lubricating grease composition containing a metal composite soap thickener and fluororesin powder, and use a metal composite soap-containing non-fluorine base oil (non-fluorine grease) with a dropping point above a certain temperature. Thus, while maintaining the heat resistance and durability of the fluorinated grease, it is easy to hold the grease on the sliding portion, and the friction coefficient can be improved.
本発明で用いられる基油混合物である非フッ素系基油とフッ素系基油との間では、互いに相溶性のないものが用いられる。互いに相溶性のないということは、これら両者を単純に混合したとき均質な基油混合物を形成し得ないことを意味する。 A non-fluorine base oil and a fluorine base oil that are base oil mixtures used in the present invention are not compatible with each other. That they are not compatible with each other means that a homogeneous base oil mixture cannot be formed when they are simply mixed.
非フッ素系基油としては、例えばポリ-α-オレフィン、エチレン-α-オレフィンオリゴマー、ポリブテンまたはこれらの水素化物、アルキルベンゼン、アルキルナフタレン等の合成炭化水素油、ポリアルキレングリコール、ポリフェニルエーテル、アルキル置換ジフェニルエーテル等のエーテル系合成油、トリメリット酸エステル、ピロメリット酸エステル等の芳香族多価カルボン酸エステル、ネオペンチルグリコールエステル、トリメチロールプロパンエステル、ペンタエリスリトールエステル、ジペンタエリスリトールエステル等のポリオールエステル、さらに脂肪族二塩基酸エステル、リン酸エステル、亜リン酸エステル、炭酸エステル等のエステル系合成油、パラフィン系鉱油、ナフテン系鉱油またはこれらを精製した鉱油等の少くとも一種、好ましくは合成炭化水素油またはエーテル系合成油が用いられる。 Non-fluorinated base oils include, for example, poly-α-olefins, ethylene-α-olefin oligomers, polybutenes or their hydrides, synthetic hydrocarbon oils such as alkylbenzene and alkylnaphthalene, polyalkylene glycols, polyphenyl ethers, and alkyl-substituted Ether synthetic oils such as diphenyl ether, aromatic polyvalent carboxylic acid esters such as trimellitic acid ester and pyromellitic acid ester, polyol esters such as neopentyl glycol ester, trimethylolpropane ester, pentaerythritol ester, dipentaerythritol ester, Furthermore, at least a small amount of ester synthetic oils such as aliphatic dibasic acid esters, phosphoric acid esters, phosphite esters, and carbonic acid esters, paraffinic mineral oils, naphthenic mineral oils, or mineral oils obtained by refining them. One, preferably synthetic hydrocarbon oils or ether-based synthetic oil is used.
これらの非フッ素系基油は、40℃における動粘度(ASTM D445に対応するJIS K2283準拠)が約15〜350mm2/秒、好ましくは約20〜300mm2/秒のものが一般に用いられる。動粘度がこれ以下のものは高温耐久性が悪く、すなわち蒸発量が多くなり、一方これ以上の動粘度以上のものは、摺動時の隙間への浸透性が悪化し、グリース切れが生じ易くなる。These non-fluorinated base oils generally have a kinematic viscosity at 40 ° C. (based on JIS K2283 corresponding to ASTM D445) of about 15 to 350 mm 2 / sec, preferably about 20 to 300 mm 2 / sec. If the kinematic viscosity is lower than this, the durability at high temperature is poor, that is, the amount of evaporation is increased.On the other hand, if the kinematic viscosity is higher than this, the permeability to the gap during sliding deteriorates and the grease is likely to run out. Become.
フッ素系基油としては、非フッ素系基油の場合と同じ理由により、40℃における動粘度(JIS K2283準拠)が約15〜350mm2/秒、好ましくは約20〜300mm2/秒のものが一般に用いられ、より具体的には一般式
RfO(CF2O)x(C2F4O)y(C3F6O)zRf
で表わされるものが用いられる。具体的には、例えば下記一般式(1)〜(4)で表わされるようなものが用いられ、この他一般式(5)で表わされるようなものも用いられる。なお、Rfはパーフルオロメチル基、パーフルオロエチル基、パーフルオロプロピル基等の炭素数1〜5、好ましくは1〜3のパーフルオロ低級アルキル基である。
(1) RfO(CF2CF2O)m(CF2O)nRf
ここで、m+n=3〜200、m:n=10〜90:90〜10であり、またCF2CF2O基およびCF2O基は主鎖中にランダムに結合しているものであり、テトラフルオロエチレンの光酸化重合で生成した先駆体を完全にフッ素化することによって得られる。
(2) RfO〔CF(CF3)CF2O)〕m(CF2O)nRf
ここで、m+n=3〜200、m:n=10〜90:90〜10であり、またCF(CF3)CF2O基およびCF2O基は主鎖中にランダムに結合しているものであり、ヘキサフルオロプロピレンの光酸化重合で生成した先駆体を完全にフッ素化することによって得られる。
(3) RfO[CF(CF3)CF2O]p(CF2CF2O)q(CF2O)rRf
ここで、p+q+r=3〜200でqおよびrは0であり得、(q+r)/p=0〜2であり、またCF(CF3)CF2O基、CF2CF2O基およびCF2O基は主鎖中にランダムに結合しているものであり、ヘキサフルオロプロピレンおよびテトラフルオロエチレンの光酸化重合で生成した先駆体を完全にフッ素化することにより得られる。
(4) RfO[CF(CF3)CF2O]s(CF2CF2O)tRf
ここで、s+t=2〜200でtは0であり得、t/s=0〜2であり、またCF(CF3)CF2O基およびCF2CF2O基は主鎖中にランダムに結合しているものであり、ヘキサフルオロプロピレンおよびテトラフルオロエチレンの光酸化重合で生成した先駆体を完全にフッ素化することにより、あるいはフッ化セシウム触媒の存在下にヘキサフルオロプロピレンオキサイドまたはテトラフルオロエチレンオキサイドをアニオン重合させ、得られた末端-CF(CF3)COF基を有する酸フロライド化合物をフッ素ガスで処理することによって得られる。
(5) F(CF2CF2CF2O)2〜100C2F5
これは、フッ化セシウム触媒の存在下に2,2,3,3-テトラフルオロオキセタンをアニオン重合させ、得られた含フッ素ポリエーテル(CH2CF2CF2O)nを紫外線照射下に約160〜300℃でフッ素ガスで処理することによって得られる。Fluorine base oils have a kinematic viscosity (according to JIS K2283) at 40 ° C. of about 15 to 350 mm 2 / sec, preferably about 20 to 300 mm 2 / sec for the same reason as for non-fluorine base oils. Commonly used, more specifically the general formula
RfO (CF 2 O) x (C 2 F 4 O) y (C 3 F 6 O) z Rf
Is used. Specifically, for example, those represented by the following general formulas (1) to (4) are used, and those represented by the following general formula (5) are also used. Rf is a perfluoro lower alkyl group having 1 to 5, preferably 1 to 3, carbon atoms such as a perfluoromethyl group, a perfluoroethyl group, and a perfluoropropyl group.
(1) RfO (CF 2 CF 2 O) m (CF 2 O) n Rf
Here, m + n = 3 to 200, m: n = 10 to 90:90 to 10 and the CF 2 CF 2 O group and the CF 2 O group are randomly bonded in the main chain. Yes, it can be obtained by completely fluorinating the precursor produced by photo-oxidative polymerization of tetrafluoroethylene.
(2) RfO [CF (CF 3 ) CF 2 O)] m (CF 2 O) n Rf
Here, m + n = 3 to 200, m: n = 10 to 90:90 to 10 and the CF (CF 3 ) CF 2 O group and the CF 2 O group are randomly bonded in the main chain. It is obtained by completely fluorinating a precursor produced by photo-oxidative polymerization of hexafluoropropylene.
(3) RfO [CF (CF 3 ) CF 2 O] p (CF 2 CF 2 O) q (CF 2 O) r Rf
Where p + q + r = 3 to 200 and q and r can be 0, (q + r) / p = 0 to 2 and also a CF (CF 3 ) CF 2 O group, CF 2 CF The 2 O group and the CF 2 O group are randomly bonded in the main chain, and can be obtained by completely fluorinating a precursor formed by photo-oxidative polymerization of hexafluoropropylene and tetrafluoroethylene.
(4) RfO [CF (CF 3 ) CF 2 O] s (CF 2 CF 2 O) t Rf
Here, s + t = 2 to 200, t can be 0, t / s = 0 to 2, and CF (CF 3 ) CF 2 O group and CF 2 CF 2 O group are in the main chain Randomly bonded, by completely fluorinating the precursor produced by photo-oxidation polymerization of hexafluoropropylene and tetrafluoroethylene, or in the presence of a cesium fluoride catalyst, It is obtained by anionic polymerization of fluoroethylene oxide and treating the resulting acid fluoride compound having a terminal —CF (CF 3 ) COF group with fluorine gas.
(5) F (CF 2 CF 2 CF 2 O) 2 to 100 C 2 F 5
This is because 2,2,3,3-tetrafluorooxetane is anionically polymerized in the presence of a cesium fluoride catalyst, and the resulting fluorinated polyether (CH 2 CF 2 CF 2 O) n is subjected to about UV irradiation. It is obtained by treating with fluorine gas at 160 to 300 ° C.
これらの非フッ素系基油とフッ素系基油とは、一般に前者が1〜95重量%、好ましくは6〜89重量%に対し、後者が99〜5重量%、好ましくは94〜11重量%の割合で用いられる。非フッ素系基油の混合割合がこれよりも少ないと、耐荷重性は良くなるものの、耐摩耗性、耐熱性、せん断安定性など劣るようになり、一方これよりも多い混合割合では、耐摩耗性は良くなるもの、耐熱性、耐荷重性、せん断安定性などに劣るようになる。 These non-fluorinated base oils and fluorinated base oils are generally 1 to 95% by weight, preferably 6 to 89% by weight of the former, and 99 to 5% by weight, preferably 94 to 11% by weight of the latter. Used in proportions. If the mixing ratio of the non-fluorinated base oil is less than this, the load resistance is improved, but the wear resistance, heat resistance, shear stability, etc. are inferior. On the other hand, if the mixing ratio is higher than this, the wear resistance is decreased. However, it is inferior in heat resistance, load resistance and shear stability.
増稠剤としての複合金属石けんは、脂肪族ジカルボン酸とモノアミドモノカルボン酸との複合金属石けんとして形成される。複合金属石けんの形成は、後述の如く潤滑グリース組成物の調製時に行われる。 Composite metal soap as a thickener is formed as a complex metal soap of aliphatic dicarboxylic acid and monoamide monocarboxylic acid. The formation of the composite metal soap is performed at the time of preparing the lubricating grease composition as described later.
脂肪族ジカルボン酸としては、炭素数2〜20の飽和または不飽和のジカルボン酸が用いられる。飽和ジカルボン酸としては、例えばシュウ酸、マロン酸、コハク酸、メチルコハク酸、グルタル酸、アジピン酸、ピメリン酸、スベリン酸、アゼライン酸、セバシン酸、ノナメチレンジカルボン酸、デカメチレンジカルボン酸、ウンデカンジカルボン酸、ドデカンジカルボン酸、トリデカンジカルボン酸、テトラデカンジカルボン酸、ペンタデカンジカルボン酸、ヘキサデカンジカルボン酸、ヘプタデカンジカルボン酸、オクタデカンジカルボン酸等が挙げられ、好ましくはアジピン酸、ピメリン酸、スベリン酸、アゼライン酸、セバシン酸、ノナメチレンジカルボン酸、デカメチレンジカルボン酸、ウンデカンジカルボン酸、ドデカンジカルボン酸、トリデカンジカルボン酸、テトラデカンジカルボン酸、ペンタデカンジカルボン酸、ヘキサデカンジカルボン酸、ヘプタデカンジカルボン酸、オクタデカンジカルボン酸等が用いられる。また、不飽和ジカルボン酸としては、例えばマレイン酸、フマル酸、さらに2-メチレンコハク酸、2-エチレンコハク酸、2-メチレングルタル酸等のアルケニルコハク酸などが用いられる。これらの飽和または不飽和のジカルボン酸は、単独であるいは2種以上混合して用いられる。 As the aliphatic dicarboxylic acid, a saturated or unsaturated dicarboxylic acid having 2 to 20 carbon atoms is used. Examples of the saturated dicarboxylic acid include oxalic acid, malonic acid, succinic acid, methyl succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, sebacic acid, nonamethylene dicarboxylic acid, decamethylene dicarboxylic acid, undecane dicarboxylic acid , Dodecanedicarboxylic acid, tridecanedicarboxylic acid, tetradecanedicarboxylic acid, pentadecanedicarboxylic acid, hexadecanedicarboxylic acid, heptadecanedicarboxylic acid, octadecanedicarboxylic acid, etc., preferably adipic acid, pimelic acid, suberic acid, azelaic acid, sebacin Acid, nonamethylene dicarboxylic acid, decamethylene dicarboxylic acid, undecanedicarboxylic acid, dodecanedicarboxylic acid, tridecanedicarboxylic acid, tetradecanedicarboxylic acid, pentadecanedicarboxylic acid, hex Decanedicarboxylic acid, hepta-decane dicarboxylic acid, octadecane dicarboxylic acid, or the like is used. Examples of the unsaturated dicarboxylic acid include maleic acid, fumaric acid, alkenyl succinic acid such as 2-methylene succinic acid, 2-ethylene succinic acid, 2-methylene glutaric acid, and the like. These saturated or unsaturated dicarboxylic acids are used alone or in combination of two or more.
モノアミドモノカルボン酸は、上記ジカルボン酸のモノカルボキシル基がアミド化されたものであり、アミド化されるアミンとしては、例えばブチルアミン、アミルアミン、へキシルアミン、へプチルアミン、オクチルアミン、ノニルアミン、デシルアミン、ラウリルアミン、ミリスチルアミン、パルミチルアミン、ステアリルアミン、ベヘニルアミン等の脂肪族第1級アミン、ジプロピルアミン、ジイソプロピルアミン、ジブチルアミン、ジアミルアミン、ジラウリルアミン、モノメチルラウリルアミン、ジステアリルアミン、モノメチルステアリルアミン、ジミリスチルアミン、ジパルミチルアミン等の脂肪族第2級アミン、アリルアミン、ジアリルアミン、オレイルアミン、ジオレイルアミン等の脂肪族不飽和アミン、シクロプロピルアミン、シクロブチルアミン、シクロペンチルアミン、シクロヘキシルアミン等の脂環式アミン、アニリン、メチルアニリン、エチルアニリン、ベンジルアミン、ジベンジルアミン、ジフェニルアミン、α-ナフチルアミン等の芳香族アミンなどが挙げられ、好ましくはへキシルアミン、へプチルアミン、オクチルアミン、ノニルアミン、デシルアミン、ラウリルアミン、ミリスチルアミン、パルミチルアミン、ステアリルアミン、ベヘニルアミン、ジブチルアミン、ジアミルアミン、モノメチルラウリルアミン、モノメチルステアリルアミン、オレイルアミン等が用いられる。 The monoamide monocarboxylic acid is obtained by amidating the monocarboxyl group of the above dicarboxylic acid. Examples of amines to be amidated include butylamine, amylamine, hexylamine, heptylamine, octylamine, nonylamine, decylamine, laurylamine. Aliphatic primary amines such as myristylamine, palmitylamine, stearylamine, behenylamine, dipropylamine, diisopropylamine, dibutylamine, diamylamine, dilaurylamine, monomethyllaurylamine, distearylamine, monomethylstearylamine, Aliphatic secondary amines such as dimyristylamine and dipalmitylamine, aliphatic unsaturated amines such as allylamine, diallylamine, oleylamine and dioleylamine, cyclopropylamine Cycloaliphatic amines such as cyclohexane, cyclobutylamine, cyclopentylamine, and cyclohexylamine, and aromatic amines such as aniline, methylaniline, ethylaniline, benzylamine, dibenzylamine, diphenylamine, and α-naphthylamine. Xylamine, heptylamine, octylamine, nonylamine, decylamine, laurylamine, myristylamine, palmitylamine, stearylamine, behenylamine, dibutylamine, diamylamine, monomethyllaurylamine, monomethylstearylamine, oleylamine and the like are used.
これらの脂肪族ジカルボン酸とモノアミドモノカルボン酸とは、前者に対し後者が0.1〜10、好ましくは0.5〜5のモル比で用いられる。これ以外の混合割合で用いられると、滴点が低下するなどして好ましくない。これら両者は、水酸化物、酸化物等の形で用いられるリチウム、ナトリウム、カリウム、カルシウム、バリウム、マグネシウム、銅、鉄、コバルト、亜鉛、アルミニウム等の金属化合物によって複合金属石けんを形成させて用いられるが、好ましくは複合バリウム石けんまたは複合リチウム石けんとして用いられる。複合金属石けん調製に用いられる金属化合物は、けん化反応に必要な理論量に対しほぼ当量程度用いられる。 In these aliphatic dicarboxylic acids and monoamide monocarboxylic acids , the latter is used in a molar ratio of 0.1 to 10, preferably 0.5 to 5, with respect to the former. If it is used in a mixing ratio other than this, it is not preferable because the dropping point is lowered. Both of these are used by forming a composite metal soap with a metal compound such as lithium, sodium, potassium, calcium, barium, magnesium, copper, iron, cobalt, zinc, aluminum used in the form of hydroxide, oxide, etc. However, it is preferably used as composite barium soap or composite lithium soap. The metal compound used for the preparation of the composite metal soap is used in an amount equivalent to the theoretical amount necessary for the saponification reaction.
また、フッ素樹脂粉末としては、PTFE粉末、HFP粉末、パーフルオロアルキレン樹脂粉末等が用いられる。これらのフッ素樹脂粉末は、一般にその平均一次粒径が約500μm以下、好ましくは約0.1〜30μmのものが用いられる。 Further, as the fluororesin powder, PTFE powder, HFP powder, perfluoroalkylene resin powder and the like are used. These fluororesin powders generally have an average primary particle size of about 500 μm or less, preferably about 0.1 to 30 μm.
PTFE(ポリテトラフルオロエチレン)は、テトラフルオロエチレンの乳化重合、けん濁重合、溶液重合などの方法によってポリテトラフルオロエチレンを製造し、それを熱分解、電子線照射分解、物理的粉砕などの方法によって処理して数平均分子量Mnを約1000〜1000000程度としたものが用いられる。また、HFP粉末の場合には、テトラフルオロエチレンとヘキサフルオロプロペンとの共重合反応および低分子量化処理も、ポリテトラフルオロエチレンの場合と同様にして行われ、数平均分子量Mnを約1000〜600000程度としたものが用いられる。なお、分子量の制御は、共重合反応時に連鎖移動剤を用いても行うことができる。 PTFE (polytetrafluoroethylene) is a process that produces polytetrafluoroethylene by methods such as emulsion polymerization, suspension polymerization, and solution polymerization of tetrafluoroethylene, followed by thermal decomposition, electron beam irradiation decomposition, and physical grinding. The number average molecular weight Mn is about 1000 to 100,000. In the case of HFP powder, the copolymerization reaction of tetrafluoroethylene and hexafluoropropene and the molecular weight reduction treatment are also performed in the same manner as in the case of polytetrafluoroethylene, and the number average molecular weight Mn is about 1000 to 600,000. The grade is used. The molecular weight can also be controlled by using a chain transfer agent during the copolymerization reaction.
複合金属石けん増稠剤含有非フッ素系基油であるグリース(非フッ素系グリース)およびフッ素樹脂粉末含有フッ素系基油であるグリース(フッ素系グリース)の2種類のグリースを混合することによって、本発明の潤滑グリース組成物は調製される。 By mixing two types of grease, a grease that is a non-fluorine base oil containing composite metal soap thickener (non-fluorine grease) and a grease that is a fluorine base oil containing fluororesin powder (fluorine grease), The lubricating grease composition of the invention is prepared.
複合金属石けんの形成および潤滑グリース組成物の調製は、次の如くにして行われる。
(a-1) 加熱攪拌が可能な反応釜に、非フッ素系基油、脂肪族ジカルボン酸およびモノアミドモノカルボン酸を加え、攪拌可能な温度であり、反応を効率的に進めかつ基油の劣化を生じさせない温度である約80〜180℃に加熱して攪拌し、そこに金属水酸化物または金属酸化物を加えて複合金属石けんを非フッ素系基油中で形成させる。冷却後、そこにアミン系酸化防止剤等を所定量、例えば非フッ素系基油中約0.1〜5重量%を占めるような割合で配合し、3本ロールミルまたは高圧ホモジナイザで混練して、非フッ素系グリースを調製する。混練に先立って、最初に用いられた非フッ素系基油以外の他の非フッ素系基油を添加して用いることもできる。
(a-2) フッ素系基油とフッ素樹脂粉末とを混合釜中で混ぜ、その後3本ロールミルまたは高圧ホモジナイザを用いて混練し、フッ素系グリースを調製する。
(a-3) これら2種類のグリースを混合釜中で混ぜ、3本ロールミルまたは高圧ホモジナイザ、好ましくは3本ロールミルを用いて混練し、潤滑グリース組成物を調製する。なお、混練に用いられる3本ロールミルとしては、一般に油圧式のものが用いられる。
Formation of the composite metal soap and preparation of the lubricating grease composition are performed as follows.
(a-1) A non-fluorinated base oil, aliphatic dicarboxylic acid and monoamide monocarboxylic acid are added to a reaction kettle capable of being heated and stirred. The mixture is heated to about 80 to 180 ° C., which is a temperature that does not cause slag, and stirred, and a metal hydroxide or metal oxide is added thereto to form a composite metal soap in the non-fluorine base oil. After cooling, a predetermined amount of amine-based antioxidant, for example, is blended in a proportion that occupies about 0.1 to 5% by weight in the non-fluorinated base oil, and is kneaded with a three-roll mill or a high-pressure homogenizer. Prepare system grease. Prior to kneading, other non-fluorine base oils other than the first used non-fluorine base oil can be added and used.
(a-2) Fluorine base oil and fluororesin powder are mixed in a mixing kettle and then kneaded using a three-roll mill or a high-pressure homogenizer to prepare a fluorinated grease.
(a-3) These two types of grease are mixed in a mixing kettle and kneaded using a three-roll mill or a high-pressure homogenizer, preferably a three-roll mill, to prepare a lubricating grease composition. In addition, as a three-roll mill used for kneading, a hydraulic type is generally used.
(b) 上記の如くにして調製された非フッ素系グリースに、フッ素系基油およびフッ素樹脂を加え、混合釜中で混ぜた後、3本ロールミルまたは高圧ホモジナイザで混練しても、本発明の潤滑グリース組成物を調製することもできる。 (b) Fluorine base oil and fluorine resin are added to the non-fluorine grease prepared as described above, mixed in a mixing kettle, and then kneaded with a three-roll mill or a high-pressure homogenizer. Lubricating grease compositions can also be prepared.
この際、複合金属石けん増稠剤含有非フッ素系基油であるグリース(非フッ素系グリース)は、グリースとして成立する上限温度に相当する滴点が250℃以上のものが用いられる。滴点が250℃未満の非フッ素系グリースを用いると、120〜150℃あるいはそれ以上の温度での往復摺動用途への適用に際し、製品信頼性の低下が問題となる場合がある。なお、滴点は、ISO 2176に対応するJIS K2220.8に準拠して測定される。 At this time, a grease that is a non-fluorine base oil containing a composite metal soap thickener (non-fluorine grease) has a dropping point corresponding to an upper limit temperature that is established as a grease of 250 ° C. or higher. When a non-fluorine-based grease having a dropping point of less than 250 ° C. is used, there may be a problem that the product reliability is lowered when applied to a reciprocating sliding application at a temperature of 120 to 150 ° C. or higher. The dropping point is measured according to JIS K2220.8 corresponding to ISO 2176.
以上の必須各成分よりなる潤滑グリース組成物において、非フッ素系基油は1〜90重量%、好ましくは5〜80重量%の割合で、非フッ素系基油と前記の如き混合割合で用いられるフッ素系基油は5〜80重量%、好ましくは10〜80重量%の割合で、複合金属石けんは0.5〜30重量%、好ましくは1〜25重量%の割合で、またフッ素樹脂粉末は0.1〜20重量%、好ましくは1〜15重量%の割合でそれぞれ用いられる。 In the lubricating grease composition comprising the above essential components, the non-fluorine base oil is used in a proportion of 1 to 90% by weight, preferably 5 to 80% by weight, and in a mixing ratio as described above with the non-fluorine base oil. Fluorine base oil is 5 to 80% by weight, preferably 10 to 80% by weight, composite metal soap is 0.5 to 30% by weight, preferably 1 to 25% by weight, and fluororesin powder is 0.1 to Each is used in a proportion of 20% by weight, preferably 1 to 15% by weight.
このような割合での各成分の配合により、非フッ素系基油にあっては、フッ素系基油に相溶性のないあるいは乏しい増稠剤の添加を可能とし、それによって耐摩耗性の向上、摩擦係数の低減、防錆性や腐食防止効果の向上を図ることができ、フッ素系基油にあっては、耐熱性の向上を図ることができ、複合金属石けんにあっては、耐摩耗性の向上が図られ、またフッ素樹脂粉末にあっては、フッ素系基油と複合金属石けんとの相溶性の向上を図ることができる。 By blending each component at such a ratio, in the case of a non-fluorinated base oil, it is possible to add a thickener that is incompatible or poorly compatible with the fluorinated base oil, thereby improving wear resistance. The friction coefficient can be reduced and the rust prevention and corrosion prevention effects can be improved. In the case of fluorinated base oil, the heat resistance can be improved. In the case of composite metal soap, the wear resistance can be improved. In addition, in the case of the fluororesin powder, the compatibility between the fluorinated base oil and the composite metal soap can be improved.
潤滑グリース組成物中にはさらに、酸化防止剤、防錆剤、腐食防止剤、極圧剤、油性剤、固体潤滑剤などの従来潤滑剤に使用されている添加剤を必要に応じて配合することができる。酸化防止剤としては、例えば2,6-ジ第3ブチル-4-メチルフェノール、4,4′-メチレンビス(2,6-ジ第3ブチルフェノール)等のフェノール系の酸化防止剤、C4〜C20のアルキル基を有するアルキルジフェニルアミン、トリフェニルアミン、フェニル-α-ナフチルアミン、アルキル化フェニル-α-ナフチルアミン、フェノチアジン、アルキル化フェノチアジン等のアミン系の酸化防止剤、さらにはリン系酸化防止剤、イオウ系酸化防止剤などが挙げられる。Additives used in conventional lubricants such as antioxidants, rust inhibitors, corrosion inhibitors, extreme pressure agents, oiliness agents, solid lubricants, etc., are added to the lubricating grease composition as necessary. be able to. Examples of the antioxidant include phenol-based antioxidants such as 2,6-ditert-butyl-4-methylphenol and 4,4′-methylenebis (2,6-ditert-butylphenol), C 4 -C Amine-based antioxidants such as alkyldiphenylamines having 20 alkyl groups, triphenylamines, phenyl-α-naphthylamines, alkylated phenyl-α-naphthylamines, phenothiazines, alkylated phenothiazines, phosphorous antioxidants, sulfur And system antioxidants.
防錆剤としては、例えば脂肪酸、脂肪酸金属塩、脂肪酸アミン、アルキルスルホン酸金属塩、アルキルスルホン酸アミン塩、酸化パラフィン、ポリオキシエチレンアルキルエーテル等が挙げられ、また腐食防止剤としては、例えばベンゾトリアゾール、ベンゾイミダゾール、チアジアゾール等が挙げられる。 Examples of the rust preventive agent include fatty acids, fatty acid metal salts, fatty acid amines, alkyl sulfonic acid metal salts, alkyl sulfonic acid amine salts, oxidized paraffin, polyoxyethylene alkyl ether, and the like. Examples include triazole, benzimidazole, thiadiazole and the like.
極圧剤としては、例えばリン酸エステル、亜リン酸エステル、リン酸エステルアミン塩等のリン系化合物、スルフィド類、ジスルフィド類等のイオウ系化合物、ジアルキルジチオリン酸金属塩、ジアルキルジチオカルバミン酸金属塩等のイオウ系化合物金属塩、塩素化パラフィン、塩素化ジフェニル等の塩素系化合物などが挙げられる。 Examples of extreme pressure agents include phosphorous compounds such as phosphate esters, phosphite esters, phosphate ester amine salts, sulfur compounds such as sulfides and disulfides, dialkyldithiophosphate metal salts, and dialkyldithiocarbamic acid metal salts. And sulfur-based compound metal salts, chlorinated paraffin, chlorinated diphenyl and other chlorinated compounds.
油性剤としては、例えば脂肪酸またはそのエステル、高級アルコール、多価アルコールまたはそのエステル、脂肪族エステル、脂肪族アミン、脂肪酸モノグリセライド、モンタンワックス、アミド系ワックス等が挙げられる。また、他の固体潤滑剤としては、例えば二硫化モリブデン、グラファイト、窒化ホウ素、窒化シラン、メラミンシアヌレート等が挙げられる。これらの他の固体潤滑剤についても、その平均一次粒径は30μm以下、好ましくは0.1〜20μmのものが用いられる。 Examples of the oily agent include fatty acids or esters thereof, higher alcohols, polyhydric alcohols or esters thereof, aliphatic esters, aliphatic amines, fatty acid monoglycerides, montan waxes, and amide waxes. Examples of other solid lubricants include molybdenum disulfide, graphite, boron nitride, silane nitride, and melamine cyanurate. These other solid lubricants also have an average primary particle size of 30 μm or less, preferably 0.1 to 20 μm.
さらに、増稠剤として従来一般的に使用されている他の増稠剤、例えばシリカ、粘土、グラファイト、酸化亜鉛、ウレア化合物、ポリエチレン、ポリプロピレン、ポリアミド、有機顔料、金属石けん等を適宜添加して用いることもできる。 In addition, other thickeners conventionally used as thickeners, such as silica, clay, graphite, zinc oxide, urea compounds, polyethylene, polypropylene, polyamide, organic pigments, metal soaps, etc., may be added as appropriate. It can also be used.
次に、実施例について本発明を説明する。 Next, the present invention will be described with reference to examples.
参考例1
ポリ-α-オレフィン油(40℃粘度:30mm2/秒)中で、増稠剤として非フッ素系グリース中30重量%を占めるセバシン酸とセバシン酸モノステアリルアミドとのバリウム複合石けんを前記の如き方法(a-1)で合成し、これに2重量%のアミン系酸化防止剤(KING INDUSTRIES製品NA-LUBE AO-120;アルキルジフェニルアミン)を添加した後、3本ロールミルで2回混練して、グリースAを調製した。得られたグリースAの滴点は、283℃であった。Reference example 1
A barium composite soap of sebacic acid and sebacic acid monostearylamide occupying 30% by weight in a non-fluorinated grease as a thickener in a poly-α-olefin oil (40 ° C. viscosity: 30 mm 2 / sec) as described above After synthesizing by the method (a-1), 2% by weight of an amine-based antioxidant (KING INDUSTRIES product NA-LUBE AO-120; alkyldiphenylamine) was added thereto, and then kneaded twice with a three-roll mill. Grease A was prepared. The dropping point of the obtained grease A was 283 ° C.
参考例2
ポリ-α-オレフィン油(40℃粘度:30mm2/秒および400mm2/秒のものを1:1の重量比で混合したもの)中で、増稠剤として非フッ素系グリース中25重量%を占めるアゼライン酸とアゼライン酸モノオクチルアミドとのバリウム複合石けんを前記の如き方法(a-1)で合成し、これに2重量%のアミン系酸化防止剤(NA-LUBE AO-120)を添加した後、3本ロールミルで2回混練して、グリースBを調製した。得られたグリースBの滴点は、277℃であった。Reference example 2
25% by weight in non-fluorine grease as a thickener in poly-α-olefin oil (40 ° C viscosity: 30 mm 2 / s and 400 mm 2 / s mixed in a 1: 1 weight ratio) A barium complex soap of occupying azelaic acid and azelaic acid monooctylamide was synthesized by the method (a-1) as described above, and 2% by weight of an amine antioxidant (NA-LUBE AO-120) was added thereto. Thereafter, grease B was prepared by kneading twice with a three-roll mill. The dropping point of the obtained grease B was 277 ° C.
参考例3
アルキルナフタレン(40℃粘度:114mm2/秒)中で、増稠剤として非フッ素系グリース中25重量%を占めるアゼライン酸とアゼライン酸モノオクチルアミドとのバリウム複合石けんを前記の如き方法(a-1)で合成し、これに2重量%のアミン系酸化防止剤(NA-LUBE AO-120)を添加した後、3本ロールミルで2回混練して、グリースCを調製した。得られたグリースCの滴点は、273℃であった。Reference example 3
A barium composite soap of azelaic acid and azelaic acid monooctylamide, which occupies 25% by weight in a non-fluorine-based grease as a thickener in an alkylnaphthalene (40 ° C. viscosity: 114 mm 2 / sec) as described above (a- After synthesizing in 1), 2% by weight of an amine-based antioxidant (NA-LUBE AO-120) was added thereto, and then kneaded twice with a three-roll mill to prepare Grease C. The dropping point of the obtained grease C was 273 ° C.
参考例4
ジフェニルエーテル油(40℃粘度:100mm2/秒)中で、増稠剤として非フッ素系グリース中15重量%を占めるセバシン酸とセバシン酸モノステアリルアミドとのバリウム複合石けんを前記の如き方法(a-1)で合成し、これに2重量%のアミン系酸化防止剤(NA-LUBE AO-120)を添加した後、3本ロールミルで2回混練して、グリースDを調製した。得られたグリースDの滴点は、262℃であった。Reference example 4
A barium composite soap of sebacic acid and sebacic acid monostearylamide occupying 15% by weight in a non-fluorine-based grease as a thickener in diphenyl ether oil (40 ° C. viscosity: 100 mm 2 / sec) as described above (a- After synthesizing in 1), 2% by weight of an amine-based antioxidant (NA-LUBE AO-120) was added thereto, and then kneaded twice with a three-roll mill to prepare Grease D. The resulting grease D had a dropping point of 262 ° C.
参考例5
ジフェニルエーテル油(40℃粘度:100mm2/秒)中で、増稠剤として非フッ素系グリース中25重量%を占めるセバシン酸とセバシン酸モノステアリルアミドとのバリウム複合石けんを前記の如き方法(a-1)で合成し、これに2重量%のアミン系酸化防止剤(NA-LUBE AO-120)を添加した後、3本ロールミルで2回混練して、グリースEを調製した。得られたグリースEの滴点は、270℃であった。Reference Example 5
A barium composite soap of sebacic acid and sebacic acid monostearylamide, which occupies 25% by weight in a non-fluorine-based grease as a thickener in diphenyl ether oil (40 ° C viscosity: 100 mm 2 / sec) as described above (a- After synthesizing in 1), 2% by weight of an amine-based antioxidant (NA-LUBE AO-120) was added thereto, and then kneaded twice with a three-roll mill to prepare Grease E. The dropping point of the obtained grease E was 270 ° C.
参考例6
ポリ-α-オレフィン油(40℃粘度:46mm2/秒)中で、増稠剤中として非フッ素系グリース中20重量%を占めるアゼライン酸と12-ヒドロキシステアリン酸とのリチウム複合石けんを前記の如き方法(a-1)で合成し、これに2重量%のアミン系酸化防止剤(NA-LUBE AO-120)を添加した後、3本ロールミルで2回混練して、グリースFを調製した。得られたグリースFの滴点は、280℃であった。Reference Example 6
A lithium composite soap of azelaic acid and 12-hydroxystearic acid in poly-α-olefin oil (40 ° C. viscosity: 46 mm 2 / sec) and occupying 20% by weight in a non-fluorinated grease as a thickener The grease F was prepared by adding 2% by weight of an amine antioxidant (NA-LUBE AO-120) and then kneading twice with a three-roll mill. . The dropping point of the obtained grease F was 280 ° C.
参考例7
ジフェニルエーテル油(40℃粘度:100mm2/秒)中で、増稠剤として非フッ素系グリース中20重量%を占めるセバシン酸と12-ヒドロキシステアリン酸とのリチウム複合石けんを前記の如き方法(a-1)で合成し、これに2重量%のアミン系酸化防止剤(NA-LUBE AO-120)を添加した後、3本ロールミルで2回混練して、グリースGを調製した。得られたグリースGの滴点は、269℃であった。Reference Example 7
A lithium composite soap of sebacic acid and 12-hydroxystearic acid occupying 20% by weight in a non-fluorine-based grease as a thickener in diphenyl ether oil (40 ° C. viscosity: 100 mm 2 / sec) as described above (a- A grease G was prepared by adding 2% by weight of an amine antioxidant (NA-LUBE AO-120) and then kneading twice with a three-roll mill. The dropping point of the obtained grease G was 269 ° C.
参考例8
ポリ-α-オレフィン油(40℃粘度:30mm2/秒)中で、増稠剤中として非フッ素系グリース中10重量%を占める12-ヒドロキシステアリン酸のリチウム石けんを合成し、これに2重量%のアミン系酸化防止剤(NA-LUBE AO-120)を添加した後、3本ロールミルで2回混練して、グリースHを調製した。得られたグリースHの滴点は、182℃であった。Reference Example 8
In poly-α-olefin oil (40 ° C viscosity: 30 mm 2 / sec), a lithium soap of 12-hydroxystearic acid, which occupies 10% by weight of the non-fluorinated grease as a thickener, was synthesized, and 2 wt. % Amine-based antioxidant (NA-LUBE AO-120) was added and then kneaded twice with a three-roll mill to prepare Grease H. The dropping point of the obtained grease H was 182 ° C.
参考例9
分子構造RfO〔CF(CF3)CF2O〕mRfを有する基油(40℃粘度:230mm2/秒)に、フッ素系グリース中18重量%を占める量のPTFE粉末(平均粒子径0.3μm)を混合し、3本ロールミルで2回混練して、グリースIを調製した。得られたグリースIの滴点は、300℃以上であった。Reference Example 9
PTFE powder (average particle size 0.3 μm) in an amount of 18% by weight in a fluorine-based grease in a base oil (40 ° C. viscosity: 230 mm 2 / sec) having a molecular structure RfO [CF (CF 3 ) CF 2 O] m Rf ) And kneaded twice with a three-roll mill to prepare Grease I. The resulting grease I had a dropping point of 300 ° C. or higher.
参考例10
分子構造RfO(CF2CF2O)m(CF2O)nRfを有する基油(40℃粘度:85mm2/秒)に、フッ素系グリース中27重量%を占める量のPTFE粉末(平均粒子径0.3μm)を混合し、3本ロールミルで2回混練して、グリースIIを調製した。得られたグリースIIの滴点は、300℃以上であった。Reference Example 10
PTFE powder (average particle) in an amount of 27% by weight in a fluorine-based grease in a base oil (40 ° C viscosity: 85 mm 2 / sec) having a molecular structure RfO (CF 2 CF 2 O) m (CF 2 O) n Rf (Grease II) was prepared by kneading twice with a three-roll mill. The dropping point of the obtained grease II was 300 ° C. or higher.
参考例11
分子構造RfO(CF2CF2O)m(CF2O)nRfを有する基油(40℃粘度:85mm2/秒)に、フッ素系グリース中15重量%を占める量のPTFE粉末(平均粒子径0.3μm)を混合し、3本ロールミルで2回混練して、グリースIIIを調製した。得られたグリースIIIの滴点は、300℃以上であった。Reference Example 11
PTFE powder in the amount of 15% by weight in PTFE powder (average particle) in base oil (40 ° C viscosity: 85mm 2 / sec) with molecular structure RfO (CF 2 CF 2 O) m (CF 2 O) n Rf (Grease III) was prepared by kneading twice with a three-roll mill. The dropping point of the obtained grease III was 300 ° C. or higher.
参考例12
分子構造F(CF2CF2CF2O)2〜100C2F5を有する基油(40℃粘度:65mm2/秒)に、フッ素系グリース中31重量%を占める量のPTFE粉末(平均粒子径0.3μm)を混合し、3本ロールミルで2回混練して、グリースIVを調製した。得られたグリースIVの滴点は、300℃以上であった。Reference Example 12
PTFE powder (average) occupying 31% by weight in fluorine-based grease in base oil (40 ° C viscosity: 65mm 2 / sec) with molecular structure F (CF 2 CF 2 CF 2 O) 2-100 C 2 F 5 A particle size of 0.3 μm) was mixed and kneaded twice with a three-roll mill to prepare Grease IV. The dropping point of the obtained grease IV was 300 ° C. or higher.
実施例1〜6、比較例1〜7
上記各参考例で調製された非フッ素系グリースA〜Hおよびフッ素系グリースI〜IVの内の1種または2種を所定の重量比で混合し、混合釜中で十分に攪拌混合した後、3本ロールで2回混練し、潤滑グリース組成物を調製した。
Examples 1 6 and Comparative Examples 1-7
After mixing one or two of the non-fluorine-based greases A to H and fluorine-based greases I to IV prepared in each of the above reference examples at a predetermined weight ratio, the mixture is sufficiently stirred and mixed in a mixing kettle. A lubricating grease composition was prepared by kneading twice with three rolls.
調製された潤滑グリース組成物について、次の各項目の測定を行った。
蒸発損失(耐熱性):直径37mm、高さ5mmのアルミニウム製皿に、各試料
の比重に応じ、例えば比重1の場合0.3gに相当する
重量の試料を均一に塗布し、150℃の恒温槽中に24
時間静置した後恒温槽から取り出し、試料の蒸発損
失を算出
(この値が小さい程良い)
離油度(耐熱性):JIS K2220.11準拠
180℃、24時間後の離油度を測定
(この値が小さい程良い)
SRV試験(往復動試験):ASTM D5707準拠
試験片100CR6シリンダ/100CR6プレート
試験条件 温度:室温
荷重:50N
摺動幅:4mm
振動数:10Hz
試験時間:1時間
上記試験条件下で、試験後の摩擦係数、試験中
の摩擦係数の挙動を評価
摩擦係数の挙動については、試験開始10〜60分
間の間で摩擦係数の(最大値)−(最小値)=変動
幅とし、摩擦係数の変動が少なく、安定してい
る場合を○、摩擦係数の変動が大きく、安定し
ない場合を×と評価したThe prepared lubricating grease composition was measured for the following items.
Evaporation loss (heat resistance): Each sample on an aluminum dish with a diameter of 37 mm and a height of 5 mm
For example, when the specific gravity is 1, it corresponds to 0.3g.
Apply a sample of weight evenly and place it in a constant temperature bath at 150 ° C.
After standing for a period of time, remove from the thermostat and evaporate the sample.
Loss
(The smaller this value, the better)
Oil separation degree (heat resistance): JIS K2220.11 compliant
Measure oil separation after 24 hours at 180 ℃
(The smaller this value, the better)
SRV test (reciprocating test): ASTM D5707 compliant
Specimen 100CR6 cylinder / 100CR6 plate
Test conditions Temperature: Room temperature
Load: 50N
Sliding width: 4mm
Frequency: 10Hz
Test time: 1 hour
Under the above test conditions, the coefficient of friction after the test, during the test
Evaluation of friction coefficient behavior
Regarding the behavior of the coefficient of friction, the test starts 10-60 minutes
Friction coefficient (maximum value)-(minimum value) = fluctuation
Width, coefficient of friction is small and stable
○, the coefficient of friction is large and stable.
No case was rated as x
測定結果は、次の表1(実施例)および表2(比較例)に示される。
表1
実施例 1 2 3 4 5 6
〔非フッ素系グリース〕
A (重量%) 80 − − − − 30
B (重量%) − 50 − − − −
C (重量%) − − 60 − − −
D (重量%) − − − 50 − −
E (重量%) − − − − 10 −
F (重量%) − − − − − −
G (重量%) − − − − − −
H (重量%) − − − − − −
〔フッ素系グリース〕
I (重量%) 20 − − 50 − −
II (重量%) − 50 − − − −
III (重量%) − − − − 90 70
IV (重量%) − − 40 − − −
〔測定項目〕
蒸発損失 (重量%) 6.5 6.7 2.9 1.7 0.9 1.2
離油度 (重量%) 1.1 0.9 1.0 1.5 2.0 1.7
SRV試験
1時間後摩擦係数 0.179 0.171 0.163 0.175 0.177 0.171
変動幅 0.017 0.028 0.020 0.025 0.023 0.021
摩擦係数挙動 ○ ○ ○ ○ ○ ○
表2
比較例 1 2 3 4 5 6 7
〔非フッ素系グリース〕
A (重量%) − − 100 − − − −
B (重量%) − − − − − − −
C (重量%) − − − − − − −
D (重量%) − − − − − − −
E (重量%) − − − 3 − − −
F (重量%) 80 − − − − − −
G (重量%) − 70 − − − − −
H (重量%) − − − − 80 − −
〔フッ素系グリース〕
I (重量%) 20 − − − 20 100 −
II (重量%) − − − − − − 100
III (重量%) − − − 97 − − −
IV (重量%) − 30 − − − − −
〔測定項目〕
蒸発損失 (重量%) 3.2 1.9 14.0 0.6 13.9 1.8 0.4
離油度 (重量%) 3.0 2.7 2.4 4.5 5.2 5.5 5.0
SRV試験
1時間後摩擦係数 0.176 0.165 0.170 0.240 0.130 0.279 0.232
変動幅 0.019 0.017 0.015 0.155 0.025 0.076 0.204
摩擦係数挙動 ○ ○ ○ × ○ × ×
The measurement results are shown in the following Table 1 (Example) and Table 2 (Comparative Example).
Table 1
Example 1 2 3 4 5 6
[Non-fluorine grease]
A (wt%) 80 − − − − 30
B (wt%) − 50 − − − −
C (wt%) − − 60 − − −
D (wt%) − − − 50 − −
E (wt%) − − − − 10 −
F (wt%) − − − − − −
G (wt%) − − − − − −
H (wt%) − − − − − −
[Fluorine grease]
I (wt%) 20 − − 50 − −
II (wt%) − 50 − − − −
III (wt%) − − − − 90 70
IV (wt%) − − 40 − − −
〔Measurement item〕
Evaporation loss (wt%) 6.5 6.7 2.9 1.7 0.9 1.2
Oil separation (wt%) 1.1 0.9 1.0 1.5 2.0 1.7
SRV test
Friction coefficient after 1 hour 0.179 0.171 0.163 0.175 0.177 0.171
Fluctuation range 0.017 0.028 0.020 0.025 0.023 0.021
Coefficient of friction behavior ○ ○ ○ ○ ○ ○
Table 2
Comparative Example 1 2 3 4 5 6 7
[Non-fluorine grease]
A (wt%) − − 100 − − − −
B (wt%) − − − − − − −
C (wt%) − − − − − − −
D (wt%) − − − − − − −
E (wt%) − − − 3 − − −
F (wt%) 80 − − − − − −
G (wt%) − 70 − − − − −
H (wt%) − − − − 80 − −
[Fluorine grease]
I (wt%) 20 − − − 20 100 −
II (wt%) − − − − − − 100
III (wt%) − − − 97 − − −
IV (wt%) − 30 − − − − −
〔Measurement item〕
Evaporation loss (wt%) 3.2 1.9 14.0 0.6 13.9 1.8 0.4
Oil separation (wt%) 3.0 2.7 2.4 4.5 5.2 5.5 5.0
SRV test
Friction coefficient after 1 hour 0.176 0.165 0.170 0.240 0.130 0.279 0.232
Fluctuation range 0.019 0.017 0.015 0.155 0.025 0.076 0.204
Coefficient of friction behavior ○ ○ ○ × ○ × ×
本発明に係る潤滑グリース組成物は、往復摺動用潤滑グリースとして、例えば120〜150℃もしくはそれ以上の高温条件下で使用されるマイクロスイッチや電磁駆動弁等のアクチュエータ部位などに用いられる。この他に、往復摺動用潤滑グリースとして作用するガイドレール、スライドレール、ピストン、カム機構等の部位に好適に用いられる。 The lubricating grease composition according to the present invention is used as a reciprocating sliding lubricating grease, for example, in an actuator part such as a micro switch or an electromagnetically driven valve that is used under a high temperature condition of 120 to 150 ° C. or higher. In addition, it is suitably used for parts such as a guide rail, a slide rail, a piston, and a cam mechanism that act as lubrication grease for reciprocating sliding.
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