CN106433864B - 一种耐高温极压润滑脂及其制备方法 - Google Patents
一种耐高温极压润滑脂及其制备方法 Download PDFInfo
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- CN106433864B CN106433864B CN201610785208.8A CN201610785208A CN106433864B CN 106433864 B CN106433864 B CN 106433864B CN 201610785208 A CN201610785208 A CN 201610785208A CN 106433864 B CN106433864 B CN 106433864B
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- 239000004519 grease Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims abstract description 156
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 120
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000003921 oil Substances 0.000 claims abstract description 48
- 239000002199 base oil Substances 0.000 claims abstract description 37
- -1 alkyl diphenylamine Chemical compound 0.000 claims abstract description 29
- 229920000305 Nylon 6,10 Polymers 0.000 claims abstract description 25
- RAADJDWNEAXLBL-UHFFFAOYSA-N 1,2-di(nonyl)naphthalene Chemical compound C1=CC=CC2=C(CCCCCCCCC)C(CCCCCCCCC)=CC=C21 RAADJDWNEAXLBL-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052788 barium Inorganic materials 0.000 claims abstract description 21
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims abstract description 21
- DMBHHRLKUKUOEG-UHFFFAOYSA-N N-phenyl aniline Natural products C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 claims abstract description 20
- BIGYLAKFCGVRAN-UHFFFAOYSA-N 1,3,4-thiadiazolidine-2,5-dithione Chemical class S=C1NNC(=S)S1 BIGYLAKFCGVRAN-UHFFFAOYSA-N 0.000 claims abstract description 17
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002253 acid Substances 0.000 claims abstract description 17
- 239000011733 molybdenum Substances 0.000 claims abstract description 17
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 17
- 238000007127 saponification reaction Methods 0.000 claims abstract description 16
- 150000007524 organic acids Chemical class 0.000 claims abstract description 12
- ULQISTXYYBZJSJ-UHFFFAOYSA-N 12-hydroxyoctadecanoic acid Chemical compound CCCCCCC(O)CCCCCCCCCCC(O)=O ULQISTXYYBZJSJ-UHFFFAOYSA-N 0.000 claims description 37
- 238000010792 warming Methods 0.000 claims description 20
- 229940114072 12-hydroxystearic acid Drugs 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 13
- 150000002148 esters Chemical class 0.000 claims description 9
- 235000021355 Stearic acid Nutrition 0.000 claims description 5
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 5
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 5
- 239000008117 stearic acid Substances 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- 239000002480 mineral oil Substances 0.000 claims description 4
- 235000010446 mineral oil Nutrition 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000012188 paraffin wax Substances 0.000 claims description 3
- 229920005862 polyol Polymers 0.000 claims description 3
- 239000004305 biphenyl Substances 0.000 claims description 2
- 235000010290 biphenyl Nutrition 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000725 suspension Substances 0.000 claims 1
- 230000001050 lubricating effect Effects 0.000 abstract description 25
- 238000006243 chemical reaction Methods 0.000 abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 11
- 230000008901 benefit Effects 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 230000009970 fire resistant effect Effects 0.000 abstract description 2
- 238000007670 refining Methods 0.000 abstract 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 20
- 229910052744 lithium Inorganic materials 0.000 description 20
- 229940035422 diphenylamine Drugs 0.000 description 16
- 238000004519 manufacturing process Methods 0.000 description 14
- 230000008859 change Effects 0.000 description 11
- 229910052500 inorganic mineral Inorganic materials 0.000 description 10
- 239000011707 mineral Substances 0.000 description 10
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 238000001816 cooling Methods 0.000 description 7
- 238000007872 degassing Methods 0.000 description 7
- 238000001914 filtration Methods 0.000 description 7
- 239000000344 soap Substances 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 6
- 238000005461 lubrication Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 238000004939 coking Methods 0.000 description 5
- 239000000084 colloidal system Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000005272 metallurgy Methods 0.000 description 4
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 4
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 3
- 239000004327 boric acid Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- JVEOCWZEOQDIIK-UHFFFAOYSA-N formic acid;molybdenum Chemical compound [Mo].OC=O JVEOCWZEOQDIIK-UHFFFAOYSA-N 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical compound CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 229960004889 salicylic acid Drugs 0.000 description 2
- DCXXMTOCNZCJGO-UHFFFAOYSA-N tristearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCCCCCC DCXXMTOCNZCJGO-UHFFFAOYSA-N 0.000 description 2
- RSWGJHLUYNHPMX-UHFFFAOYSA-N 1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-octahydrophenanthrene-1-carboxylic acid Chemical compound C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- 229940114069 12-hydroxystearate Drugs 0.000 description 1
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- 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 1
- JFKGECWBYGQZME-UHFFFAOYSA-M OC(C(C=C1)=CC=C1C(O)=O)=O.[Li+].[OH-] Chemical compound OC(C(C=C1)=CC=C1C(O)=O)=O.[Li+].[OH-] JFKGECWBYGQZME-UHFFFAOYSA-M 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- BGXLJFQKNUKNKV-UHFFFAOYSA-N [S].C(CCCCCCCC)C1=C(C2=CC=CC=C2C=C1)CCCCCCCCC Chemical compound [S].C(CCCCCCCC)C1=C(C2=CC=CC=C2C=C1)CCCCCCCCC BGXLJFQKNUKNKV-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 1
- 229960002645 boric acid Drugs 0.000 description 1
- USOPFYZPGZGBEB-UHFFFAOYSA-N calcium lithium Chemical compound [Li].[Ca] USOPFYZPGZGBEB-UHFFFAOYSA-N 0.000 description 1
- QUAGBBNZTYHUEY-UHFFFAOYSA-N carbamic acid;molybdenum Chemical compound [Mo].NC(O)=O QUAGBBNZTYHUEY-UHFFFAOYSA-N 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000539 dimer Substances 0.000 description 1
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 description 1
- 150000002019 disulfides Chemical class 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- CDOWNLMZVKJRSC-UHFFFAOYSA-N hydroxyterephthalic acid Natural products OC(=O)C1=CC=C(C(O)=O)C(O)=C1 CDOWNLMZVKJRSC-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229940006116 lithium hydroxide Drugs 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium;hydroxide;hydrate Chemical compound [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 150000002751 molybdenum Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 230000001846 repelling effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 231100000241 scar Toxicity 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 230000009466 transformation Effects 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
- C10M169/04—Mixtures of base-materials and additives
- C10M169/044—Mixtures of base-materials and additives the additives being a mixture of non-macromolecular and macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
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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
- 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
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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
- C10M2207/128—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
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- 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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- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
- C10M2219/044—Sulfonic acids, Derivatives thereof, e.g. neutral salts
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- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/06—Thio-acids; Thiocyanates; Derivatives thereof
- C10M2219/062—Thio-acids; Thiocyanates; Derivatives thereof having carbon-to-sulfur double bonds
- C10M2219/066—Thiocarbamic type compounds
- C10M2219/068—Thiocarbamate metal salts
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2221/00—Organic macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2221/04—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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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
- C10N2030/06—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
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/08—Resistance to extreme temperature
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- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/10—Inhibition of oxidation, e.g. anti-oxidants
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Abstract
本发明公开了一种耐高温极压润滑脂及其制备方法,该润滑脂包括基础油、C12~C24的一元有机酸、二元酸、氢氧化锂油溶液、烷基二苯胺、二壬基萘磺酸钡、二烷基二硫代氨基甲酸钼及2,5‑二巯基‑1,3,4‑噻二唑二聚体;制法为将1/2~2/3的基础油、一元有机酸和癸二酸混匀升温,加入氢氧化锂油溶液,进行皂化反应;继续升温,加入对苯二甲酸,恒温皂化后,再升温进行高温炼制;加入剩余基础油,进行均化反应,随后加入烷基二苯胺、二壬基萘磺酸钡、二烷基二硫代氨基甲酸钼及2,5‑二巯基‑1,3,4‑噻二唑二聚体混匀,即可。优点为该润滑脂不仅耐高温抗氧化性强,不结焦,且极压抗磨性优越,遇水后仍具有较高的极压性能。
Description
技术领域
本发明属于润滑脂领域,尤其涉及一种耐高温极压润滑脂及其制备方法。
背景技术
复合锂基润滑脂是一款通用型高温润滑脂,被广泛地应用于矿山、冶金、轧钢、汽车、铁路、船舶等行业设备机械的润滑。其优点是滴点高,适用温度范围宽,优异的胶体安定性和抗剪切稳定性,具有较长的使用寿命,在一定意义上延长了设备维护保养寿命的周期。据统计,2009~2012年我国普通锂基润滑脂所占比例基本不变,约占70%,而复合锂基润滑脂呈逐年增长趋势,从2009年的14.14%提高至2012年的15.71%,这说明我国用脂水平有所提高。在北美,高滴点润滑脂以复合锂基润滑脂为主,所占比例为38.92%,高于锂基润滑脂(28.27%)。由此可见,随着设备及工业技术的发展,复合锂基脂润滑脂作为高滴点、长寿命润滑脂将越来越受到重视。
然而,现有的复合锂基润滑脂在某些苛刻条件下使用仍存在某些不足,如:(1)在长期高温,补脂周期较长的场合,复合锂基润滑脂氧化速度加快,颜色变深,且润滑脂出现碳化、结焦等现象;(2)在潮湿多水的环境下,容易乳化流失,防锈性能也差;(3)在重负荷潮湿的场合,极压性能会有所降低,不能满足多水重负荷设备的润滑需求。申请人通过对近年来国内外复合锂基润滑脂制备的专利汇总了解到,国内CN101200670,101481637A,101705141A以及国外WO 98/11180,GB2215346A等专利均报道了有关复合锂基润滑脂的生产方法,主要采用含C9~C10二元酸、硼酸或水杨酸的锂盐与12-羟基硬脂酸锂进行复合而制得。其中,使用癸二酸、12-羟基硬脂酸与氢氧化锂制作的二组分复合锂基润滑脂滴点较高,一般大于260℃,粘附性较好,但抗高温氧化和抗水性差;硼酸、12-羟基硬脂酸与氢氧化锂制作的二组分复合锂基润滑脂,滴点大于230℃,粘附性和抗水性差;水杨酸、12-羟基硬脂酸与氢氧化锂制作的二组分复合锂基润滑脂,滴点大于240℃,高温粘附性差;而使用癸二酸或水杨酸与12-羟基硬脂酸、硼酸及氢氧化锂制作的三组分复合锂基润滑脂,滴点大于260℃,粘附性好,并且具有较好的极压性能,但抗水性和抗高温结焦性能差。总而言之,上述的二组分及三组分复合锂基润滑脂,在滴点、粘附性、抗高温结焦及抗水性等方面分别存在一定的缺陷。
申请号为CN99107941.8的发明专利公开了采用12-羟基硬脂酸和对苯二甲酸制作了复合锂钙基润滑脂,但产品的制备过程是在高温高压密闭条件下进行,反应过程不易监控,产品批次质量难控制,且制备的产品胶体安定性和防腐蚀性差。尽管申请号为CN85108441的发明专利也公开了使用12-羟基硬脂酸、癸二酸和对苯二甲酸制作复合锂基润滑脂,但是制备产品的滴点只有260℃,且抗水性差,生产周期长。
目前复合锂基脂中的常用添加剂为硫化异丁烯、硼酸盐及ZDDP等,这些极性较强的添加剂易对皂纤维结构造成破坏,影响产品的胶体安定性和高温稳定性,或耐水性差导致遇水后极压性能急剧下降。
因此,开发耐高温性、极压性和抗水性等综合性能优异的复合锂基润滑脂对拓宽复合锂型高滴点润滑脂的应用及延长设备换脂周期都具有非常重要的意义。
发明内容
发明目的:本发明的第一目的是提供一种具有优异的耐高温抗结焦性、极压抗磨性、胶体安定性和抗水性的润滑脂;本发明的第二目的是提供该润滑脂的制备方法。
技术方案:本发明的耐高温极压润滑脂,按重量百分比计包括如下原料:基础油75~85%、C12~C24的一元有机酸5~15%、二元酸2~6%、氢氧化锂油溶液1~6%、烷基二苯胺0.2~0.5%、二壬基萘磺酸钡0.5%~3%、二烷基二硫代氨基甲酸钼1~4%及2,5-二巯基-1,3,4-噻二唑二聚体0.5~3%。
优选的,基础油75~80%、C12~C24的一元有机酸7~12%、二元酸3.5~6%、氢氧化锂油溶液3~5%、烷基二苯胺0.2~0.5%、二壬基萘磺酸钡1%~2.5%、二烷基二硫代氨基甲酸钼1~2%及2,5-二巯基-1,3,4-噻二唑二聚体1~2.5%。
进一步说,本发明采用的基础油可包括石蜡基矿物油、聚α烯烃油、酯类油、烷基二苯基醚中的至少一种。其中,石蜡基矿物油40℃运动粘度为90~500mm2/s,在此粘度范围内,能够形成稳定的皂纤维结构,并满足不同工况设备润滑需求;酯类油包括双酯和/或新戊基多元醇酯。
本发明采用的C12~C24的一元有机酸为12-羟基硬脂酸和/或硬脂酸;二元酸为癸二酸及对苯二甲酸,其中,该癸二酸与对苯二甲酸的摩尔比优选可为1:0.5~3,该摩尔比能够进一步提高润滑脂的耐高温及抗水性能。
本发明采用的氢氧化锂油溶液为含重量百分数20~50%氢氧化锂的油分散悬浮液,将氢氧化锂固体颗粒处理成20~50%氢氧化锂油溶液,替代传统的氢氧化水溶液,不仅提高了氢氧化锂与酸的接触面积,合理控制反应速率,缩短反应时间,提高反应转化效率及生产效率、工艺更可控、产品批次质量更稳定,便于大规模工业化生产;且在皂化复合时引入对苯二甲酸,该对苯二甲酸锂通过氢键作用在复合皂纤维中形成环状保护层,提高了产品的高温稠度稳定性和抗水性。
本发明采用特殊结构的2,5-二巯基-1,3,4-噻二唑二聚体与钼盐减磨剂的合理复配,不仅极压性能、抗磨性出色,PD高达6080N,磨斑直径小于0.45mm;而且高温或遇水后对润滑脂的稠度影响小,极压性能出色。
本发明制备耐高温极压润滑脂的方法包括如下步骤:
(1)按重量百分比将1/2~2/3的基础油、一元有机酸和癸二酸混匀升温至80~85℃,加入氢氧化锂油溶液,在90~100℃下皂化反应0.5~1h;
(2)继续升温至105~115℃,加入对苯二甲酸,恒温皂化1~1.5h后,再升温至210~220℃进行高温炼制5~10min;
(3)加入剩余基础油,在110~120℃、20~25MPa条件下均化1~2h;
(4)待上述温度降至90℃以下加入烷基二苯胺、二壬基萘磺酸钡、二烷基二硫代氨基甲酸钼及2,5-二巯基-1,3,4-噻二唑二聚体混匀,即可。
采用本发明的工艺参数,能够确保生产高性能、稳定的复合锂基润滑脂,且采用了先进的氢氧化锂油溶液,相比于单水氢氧化锂的生产工艺,缩短反应时间,提高生产效率。
有益效果:与现有技术相比,本发明的显著优点为:该润滑脂不仅具有优异的耐高温、抗氧化性,长时间高温稠度变化小、不结焦,且极压抗磨性出色,遇水后仍具有较高的极压性能,能够满足重载汽车轮毂、矿山、冶金等长时间高温或潮湿工况下重负荷设备的润滑需求;同时,在制备过程中将12-羟基硬脂酸及癸二酸优先与过量的氢氧化锂反应后再加入对苯二甲酸,使得12-羟基硬脂酸中的羟基全部用于复合,而不再有多余的游离羟基,避免了三种酸同时加入因竞争反应而导致皂化体系中存在剩余的游离羟基,在高温烘烤中出现氧化变黑、结焦等问题,与现有的复合锂基脂相比具有高温不硬化,稠度变化小,并且在180℃高温烘烤下不结焦,工艺简单、易于控制,生产周期短。
具体实施方式
下面结合实施例对本发明的技术方案作进一步说明。
实施例1
制备氢氧化锂油溶液:将市场上所购无水氢氧化锂用球磨机研磨成8μm的粉末,然后将微米级的氢氧化锂用高速分散机分散于基础油500SN中,所制成的氢氧化锂油溶液中氢氧化锂的含量为36.5%。
润滑脂原料组成:矿物基础油(150BS 1100kg及500SN 1300kg)、12-羟基硬脂酸225kg、癸二酸75kg、对苯二甲酸63kg、氢氧化锂油溶液100kg、烷基二苯胺10kg、二壬基萘磺酸钡37kg、二烷基二硫代氨基甲酸钼60kg和2,5-二巯基-1,3,4-噻二唑二聚体30kg。其中,癸二酸与对苯二甲酸的摩尔比为1:1,矿物基础油40℃运动粘度为90~500mm2/s。
制备步骤包括:取混合好的基础油1500kg、12-羟基硬脂酸、癸二酸依次加入到皂化反应釜,搅拌升温至82℃,加入氢氧化锂油溶液,在95℃下皂化反应45min,然后继续升温至110℃,加入对苯二甲酸,继续反应60min,最后升温至215℃,恒温5min后转入调和釜,加入上述混合好的基础油900kg降温,在115℃,22MPa的压力下均化1h,待物料温度降至85℃后,依次加入烷基二苯胺、二壬基萘磺酸钡、二烷基二硫代氨基甲酸钼和2,5-二巯基-1,3,4-噻二唑二聚体,循环过滤、脱气后即可制得本发明的润滑脂。
本实施例采用的原料除氢氧化锂油溶液外,其他原料均为市场所购常规原料。
实施例2
采用实施例1的方法制备氢氧化锂油溶液。
原料组成:矿物基础油(150BS 1238kg和PAO10 1100kg)、12-羟基硬脂酸243kg、癸二酸66kg、对苯二甲酸81kg、氢氧化锂油溶液107kg、烷基二苯胺15kg、二壬基萘磺酸钡60kg、二烷基二硫代氨基甲酸钼45kg和2,5-二巯基-1,3,4-噻二唑二聚体45kg。其中,癸二酸与对苯二甲酸的摩尔比为2:3,矿物基础油40℃运动粘度为90~500mm2/s。
制备步骤包括:取混合好的基础油1600kg、12-羟基硬脂酸、癸二酸依次加入到皂化反应釜,搅拌升温至85℃,加入氢氧化锂油溶液,在95℃下皂化反应60min,然后继续升温至115℃,加入对苯二甲酸,继续反应90min,最后升温至220℃,恒温5min后转入调和釜,加入上述混合好的基础油738kg降温,在120℃,20MPa的压力下均化1h,待物料温度降至90℃后,依次加入烷基二苯胺、二壬基萘磺酸钡、二烷基二硫代氨基甲酸钼和2,5-二巯基-1,3,4-噻二唑二聚体,循环过滤、脱气后即可制得本发明的润滑脂。
实施例3
采用实施例1的方法制备氢氧化锂油溶液。
原料组成:矿物基础油(150BS 1962kg和500SN 300kg)、12-羟基硬脂酸285kg、癸二酸57kg、对苯二甲酸108kg、氢氧化锂油溶液126kg、烷基二苯胺12kg、二壬基萘磺酸钡60kg、二烷基二硫代氨基甲酸钼30kg和2,5-二巯基-1,3,4-噻二唑二聚体60kg。其中,癸二酸与对苯二甲酸的摩尔比为2.2:5,矿物基础油40℃运动粘度为90~500mm2/s。
制备步骤包括:取混合好的基础油1800kg、12-羟基硬脂酸、癸二酸依次加入到皂化反应釜,搅拌升温至80℃,加入氢氧化锂油溶液,在100℃下皂化反应60min,然后继续升温至110℃,加入对苯二甲酸,继续反应60min,最后升温至220℃,恒温5min后转入调和釜,加入上述混合好的基础油462kg降温,在120℃,20MPa的压力下均化1h,待物料温度降至90℃后,依次加入烷基二苯胺、二壬基萘磺酸钡、二烷基二硫代氨基甲酸钼和2,5-二巯基-1,3,4-噻二唑二聚体,循环过滤、脱气后即可制得本发明的润滑脂。
对比例1
设计对比例,基本上与实施例1相同,不同之处在于原料中不加入对苯二甲酸,原料的组成具体为:矿物基础油(150BS1100kg和500SN1300kg)、12-羟基硬脂酸270kg、癸二酸90kg、氢氧化锂油溶液120kg、10kg烷基二苯胺、20kg二壬基萘磺酸钡、60kg二烷基二硫代氨基甲酸钼和30kg 2,5-二巯基-1,3,4-噻二唑二聚体。
制备步骤包括:取混合好的基础油2000kg、12-羟基硬脂酸、癸二酸依次加入到皂化反应釜,搅拌升温至82℃,加入氢氧化锂油溶液,在95℃下皂化反应120min,继续升温至215℃,恒温5min后转入调和釜,加入上述混合好的基础油500kg降温,在115℃,22MPa的压力下均化1h,待物料温度降至85℃后,依次加入烷基二苯胺、二壬基萘磺酸钡、二烷基二硫代氨基甲酸钼和2,5-二巯基-1,3,4-噻二唑二聚体,循环过滤、脱气后即可制得本发明的润滑脂。
对比例2
基本步骤与实施例1相同,不同之处在于,在制备润滑脂时,将对苯二甲酸与癸二酸同时加入,之后再加入氢氧化锂油溶液。具体为:取混合好的基础油1500kg、12-羟基硬脂酸、癸二酸、对苯二甲酸依次加入到皂化反应釜,搅拌升温至82℃,加入氢氧化锂油溶液,在95℃下皂化反应45min,然后继续升温至110℃,反应60min,最后升温至215℃,恒温5min后转入调和釜,加入上述混合好的基础油900kg降温,在115℃,22MPa的压力下均化1h,待物料温度降至85℃后,依次加入烷基二苯胺、二壬基萘磺酸钡、二烷基二硫代氨基甲酸钼和2,5-二巯基-1,3,4-噻二唑二聚体,循环过滤、脱气后即可制得本发明的润滑脂。
将实施例1-3和对比例1-2制备所得润滑脂进行的理化性能检测,获得的试验结果如表1所示。
表1实施例1-3及对比例1制备的润滑脂的理化性能检验数据
通过表1中的数据可以看出,本发明采用先进的氢氧化锂油溶液技术并在皂化复合时引入芳香酸--对苯二甲酸,不仅工艺简单,生产效率高,易于控制;制备的润滑剂具有优异的耐高温抗氧化性,长时间高温稠度变化小,不结焦;且极压抗磨性出色,遇水后仍具有较高的极压性能,可满足重载汽车轮毂、矿山、冶金等长时间高温或潮湿工况下重负荷设备的润滑需求。
实施例4
设计6组试验,基本步骤与实施例1相同,不同之处在于癸二酸与对苯二甲酸的摩尔比,具体为1:0.5、1:1、1:2及1:3,将该4组试验制备的润滑脂进行性能检测可知,其不仅具有优异的耐高温、抗氧化性,长时间高温稠度变化小、不结焦,且极压抗磨性出色,遇水后仍具有较高的极压性能。
实施例5
制备氢氧化锂油溶液:将市场上所购无水氢氧化锂用球磨机研磨成5μm的粉末,然后将微米级的氢氧化锂用高速分散机分散于基础油500SN中,所制成的氢氧化锂油溶液中氢氧化锂的含量为20%。
润滑脂原料组成:聚α烯烃油2250kg、硬脂酸450kg、癸二酸97.8kg、对苯二甲酸82.2kg、氢氧化锂油溶液30kg、烷基二苯胺15kg、二壬基萘磺酸钡15kg、二烷基二硫代氨基甲酸钼45kg和2,5-二巯基-1,3,4-噻二唑二聚体15kg。其中,癸二酸与对苯二甲酸的摩尔比为1:1,矿物基础油40℃运动粘度为90~500mm2/s。
制备步骤包括:取聚α烯烃油1125kg、硬脂酸、癸二酸依次加入到皂化反应釜,搅拌升温至80℃,加入氢氧化锂油溶液,在90℃下皂化反应0.5h,然后继续升温至105℃,加入对苯二甲酸,继续反应60min,最后升温至210℃,恒温5min后转入调和釜,加入剩余聚α烯烃油1125kg,降温,在110℃,20MPa的压力下均化1h,待物料温度降至80℃后,依次加入烷基二苯胺、二壬基萘磺酸钡、二烷基二硫代氨基甲酸钼和2,5-二巯基-1,3,4-噻二唑二聚体,循环过滤、脱气后即可制得本发明的润滑脂。
实施例6
制备氢氧化锂油溶液:将市场上所购无水氢氧化锂用球磨机研磨成10μm的粉末,然后将微米级的氢氧化锂用高速分散机分散于基础油500SN中,所制成的氢氧化锂油溶液中氢氧化锂的含量为50%。
润滑脂原料组成:双脂2550kg、一元有机酸150kg(其中,12-羟基硬脂酸75kg、硬脂酸75kg)、癸二酸32.6kg、对苯二甲酸27.4kg、氢氧化锂油溶液30kg、烷基二苯胺6kg、二壬基萘磺酸钡24kg、二烷基二硫代氨基甲酸钼60kg和2,5-二巯基-1,3,4-噻二唑二聚体60kg。其中,癸二酸与对苯二甲酸的摩尔比为1:1,矿物基础油40℃运动粘度为90~500mm2/s。
制备步骤包括:取双脂1700kg、一元有机酸、癸二酸依次加入到皂化反应釜,搅拌升温至85℃,加入氢氧化锂油溶液,在100℃下皂化反应1h,然后继续升温至115℃,加入对苯二甲酸,继续反应1.5h,最后升温至220℃,恒温10min后转入调和釜,加入剩余双脂850kg,降温,在120℃,25MPa的压力下均化2h,待物料温度降至75℃后,依次加入烷基二苯胺、二壬基萘磺酸钡、二烷基二硫代氨基甲酸钼和2,5-二巯基-1,3,4-噻二唑二聚体,循环过滤、脱气后即可制得本发明的润滑脂。
实施例7
基本步骤与实施例6相同,不同之处在于润滑脂原料组成,具体为:基础油(其中,双脂770kg、新戊基多元醇酯770kg、烷基二苯基醚770kg)2310kg、硬脂酸150kg、癸二酸32.6kg、对苯二甲酸27.4kg、氢氧化锂油溶液180kg、烷基二苯胺15kg、二壬基萘磺酸钡90kg、二烷基二硫代氨基甲酸钼120kg和2,5-二巯基-1,3,4-噻二唑二聚体75kg。其中,癸二酸与对苯二甲酸的摩尔比为1:1,矿物基础油40℃运动粘度为90~500mm2/s。
实施例8
设计3组试验,基本步骤与实施例1相同,不同之处在于原料的含量,具体如表2所示:
表2各组的原料含量
将实施例5-8制备的润滑脂进行性能检测可知,该润滑脂不仅具有优异的耐高温、抗氧化性,长时间高温稠度变化小、不结焦,且极压抗磨性出色,遇水后仍具有较高的极压性能,能够满足重载汽车轮毂、矿山、冶金等长时间高温或潮湿工况下重负荷设备的润滑需求。
Claims (8)
1.一种耐高温极压润滑脂,其特征在于按重量百分比计包括如下原料:基础油75~85%、C12~C24的一元有机酸5~15%、二元酸2~6%、氢氧化锂油溶液1~6%、烷基二苯胺0.2~0.5%、二壬基萘磺酸钡0.5%~3%、二烷基二硫代氨基甲酸钼1~4%及2,5-二巯基-1,3,4-噻二唑二聚体0.5~3%;所述二元酸为癸二酸及对苯二甲酸;其制备方法包括如下步骤:
(1)按重量百分比将1/2~2/3的基础油、一元有机酸和癸二酸混匀升温至80~85℃,加入氢氧化锂油溶液,在90~100℃下皂化反应0.5~1h;
(2)继续升温至105~115℃,加入对苯二甲酸,恒温皂化1~1.5h后,再升温至210~220℃进行高温炼制5~10min;
(3)加入剩余基础油,在110~120℃、20~25MPa条件下均化1~2h;
(4)待上述温度降至90℃以下加入烷基二苯胺、二壬基萘磺酸钡、二烷基二硫代氨基甲酸钼及2,5-二巯基-1,3,4-噻二唑二聚体混匀,即可。
2.根据权利要求1所述的耐高温极压润滑脂,其特征在于:所述基础油70~80%、C12~C24的一元有机酸7~12%、二元酸3.5~6%、氢氧化锂油溶液3~5%、烷基二苯胺0.2~0.5%、二壬基萘磺酸钡1%~2.5%、二烷基二硫代氨基甲酸钼1~2%及2,5-二巯基-1,3,4-噻二唑二聚体1~2.5%。
3.根据权利要求1或2所述的耐高温极压润滑脂,其特征在于:所述基础油包括石蜡基矿物油、聚α烯烃油、酯类油、烷基二苯基醚中的至少一种。
4.根据权利要求3所述的耐高温极压润滑脂,其特征在于:所述石蜡基矿物油40℃运动粘度为90~500mm2/s。
5.根据权利要求3所述的耐高温极压润滑脂,其特征在于:所述酯类油包括双酯和/或新戊基多元醇酯。
6.根据权利要求1或2所述的耐高温极压润滑脂,其特征在于:所述C12~C24的一元有机酸为12-羟基硬脂酸和/或硬脂酸。
7.根据权利要求1所述的耐高温极压润滑脂,其特征在于:所述癸二酸与对苯二甲酸的摩尔比为1:0.5~3。
8.根据权利要求1或2所述的耐高温极压润滑脂,其特征在于:所述氢氧化锂油溶液为含重量百分数20~50%氢氧化锂的油分散悬浮液。
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