CN106032477B - Lubricant composition and preparation method thereof - Google Patents
Lubricant composition and preparation method thereof Download PDFInfo
- Publication number
- CN106032477B CN106032477B CN201510105336.9A CN201510105336A CN106032477B CN 106032477 B CN106032477 B CN 106032477B CN 201510105336 A CN201510105336 A CN 201510105336A CN 106032477 B CN106032477 B CN 106032477B
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- Prior art keywords
- calcium
- newtonian
- weight
- content
- base oil
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- 239000000203 mixture Substances 0.000 title claims abstract description 98
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 239000000314 lubricant Substances 0.000 title description 55
- 230000001050 lubricating effect Effects 0.000 claims abstract description 134
- 239000002199 base oil Substances 0.000 claims abstract description 105
- 239000004519 grease Substances 0.000 claims abstract description 91
- 229920002396 Polyurea Polymers 0.000 claims abstract description 89
- ZCZLQYAECBEUBH-UHFFFAOYSA-L calcium;octadec-9-enoate Chemical compound [Ca+2].CCCCCCCCC=CCCCCCCCC([O-])=O.CCCCCCCCC=CCCCCCCCC([O-])=O ZCZLQYAECBEUBH-UHFFFAOYSA-L 0.000 claims abstract description 57
- 150000001875 compounds Chemical class 0.000 claims abstract description 55
- AVVIDTZRJBSXML-UHFFFAOYSA-L calcium;2-carboxyphenolate;dihydrate Chemical compound O.O.[Ca+2].OC1=CC=CC=C1C([O-])=O.OC1=CC=CC=C1C([O-])=O AVVIDTZRJBSXML-UHFFFAOYSA-L 0.000 claims abstract description 47
- NKFIBMOQAPEKNZ-UHFFFAOYSA-N 5-amino-1h-indole-2-carboxylic acid Chemical compound NC1=CC=C2NC(C(O)=O)=CC2=C1 NKFIBMOQAPEKNZ-UHFFFAOYSA-N 0.000 claims abstract description 45
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims abstract description 43
- 238000000034 method Methods 0.000 claims abstract description 38
- -1 urea compound Chemical class 0.000 claims abstract description 35
- 239000002562 thickening agent Substances 0.000 claims abstract description 19
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 17
- PFUVZUNNAOPQNQ-UHFFFAOYSA-N [Ca].[Ca].C1(=CC=CC=C1)O Chemical compound [Ca].[Ca].C1(=CC=CC=C1)O PFUVZUNNAOPQNQ-UHFFFAOYSA-N 0.000 claims abstract 4
- CPGKMLVTFNUAHL-UHFFFAOYSA-N [Ca].[Ca] Chemical compound [Ca].[Ca] CPGKMLVTFNUAHL-UHFFFAOYSA-N 0.000 claims abstract 2
- 239000011575 calcium Substances 0.000 claims description 198
- 229910052791 calcium Inorganic materials 0.000 claims description 198
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 195
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 78
- 238000003756 stirring Methods 0.000 claims description 67
- 238000006243 chemical reaction Methods 0.000 claims description 48
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims description 28
- 239000003795 chemical substances by application Substances 0.000 claims description 28
- 239000000463 material Substances 0.000 claims description 26
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 24
- 239000004327 boric acid Substances 0.000 claims description 24
- 239000003921 oil Substances 0.000 claims description 21
- 230000001131 transforming effect Effects 0.000 claims description 21
- 150000001412 amines Chemical class 0.000 claims description 17
- 125000005442 diisocyanate group Chemical group 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 15
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 15
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 14
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 150000004985 diamines Chemical class 0.000 claims description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 230000018044 dehydration Effects 0.000 claims description 12
- 238000006297 dehydration reaction Methods 0.000 claims description 12
- 239000000654 additive Substances 0.000 claims description 11
- 229910052799 carbon Inorganic materials 0.000 claims description 11
- 238000007872 degassing Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 150000004982 aromatic amines Chemical class 0.000 claims description 9
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 claims description 9
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 7
- 125000003118 aryl group Chemical group 0.000 claims description 6
- 125000000753 cycloalkyl group Chemical group 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 5
- 150000002191 fatty alcohols Chemical class 0.000 claims description 5
- 239000003208 petroleum Substances 0.000 claims description 5
- HNNQYHFROJDYHQ-UHFFFAOYSA-N 3-(4-ethylcyclohexyl)propanoic acid 3-(3-ethylcyclopentyl)propanoic acid Chemical compound CCC1CCC(CCC(O)=O)C1.CCC1CCC(CCC(O)=O)CC1 HNNQYHFROJDYHQ-UHFFFAOYSA-N 0.000 claims description 4
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 125000002529 biphenylenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3C12)* 0.000 claims description 4
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 4
- 229930195729 fatty acid Natural products 0.000 claims description 4
- 239000000194 fatty acid Substances 0.000 claims description 4
- 150000004665 fatty acids Chemical class 0.000 claims description 4
- 150000002192 fatty aldehydes Chemical class 0.000 claims description 4
- 125000000843 phenylene group Chemical group C1(=C(C=CC=C1)*)* 0.000 claims description 4
- 238000007670 refining Methods 0.000 claims description 4
- WBIQQQGBSDOWNP-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O WBIQQQGBSDOWNP-UHFFFAOYSA-N 0.000 claims description 3
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 claims description 3
- 229940060296 dodecylbenzenesulfonic acid Drugs 0.000 claims description 3
- 229910052736 halogen Chemical group 0.000 claims description 3
- 239000012948 isocyanate Substances 0.000 claims description 3
- GEYOCULIXLDCMW-UHFFFAOYSA-N 1,2-phenylenediamine Chemical compound NC1=CC=CC=C1N GEYOCULIXLDCMW-UHFFFAOYSA-N 0.000 claims description 2
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 claims description 2
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 claims description 2
- WCRKLZYTQVZTMM-UHFFFAOYSA-N 2-octadecylphenol Chemical compound CCCCCCCCCCCCCCCCCCC1=CC=CC=C1O WCRKLZYTQVZTMM-UHFFFAOYSA-N 0.000 claims description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 2
- PLZVEHJLHYMBBY-UHFFFAOYSA-N Tetradecylamine Chemical compound CCCCCCCCCCCCCCN PLZVEHJLHYMBBY-UHFFFAOYSA-N 0.000 claims description 2
- 150000004996 alkyl benzenes Chemical class 0.000 claims description 2
- 239000001569 carbon dioxide Substances 0.000 claims description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 2
- 150000002513 isocyanates Chemical class 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims description 2
- 125000002947 alkylene group Chemical group 0.000 claims 6
- 125000000732 arylene group Chemical group 0.000 claims 4
- 125000004432 carbon atom Chemical group C* 0.000 claims 3
- RZXMPPFPUUCRFN-UHFFFAOYSA-N p-toluidine Chemical compound CC1=CC=C(N)C=C1 RZXMPPFPUUCRFN-UHFFFAOYSA-N 0.000 claims 2
- RTTZISZSHSCFRH-UHFFFAOYSA-N 1,3-bis(isocyanatomethyl)benzene Chemical compound O=C=NCC1=CC=CC(CN=C=O)=C1 RTTZISZSHSCFRH-UHFFFAOYSA-N 0.000 claims 1
- PNPCRKVUWYDDST-UHFFFAOYSA-N 3-chloroaniline Chemical compound NC1=CC=CC(Cl)=C1 PNPCRKVUWYDDST-UHFFFAOYSA-N 0.000 claims 1
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims 1
- QSNSCYSYFYORTR-UHFFFAOYSA-N 4-chloroaniline Chemical compound NC1=CC=C(Cl)C=C1 QSNSCYSYFYORTR-UHFFFAOYSA-N 0.000 claims 1
- AFBPFSWMIHJQDM-UHFFFAOYSA-N N-methyl-N-phenylamine Natural products CNC1=CC=CC=C1 AFBPFSWMIHJQDM-UHFFFAOYSA-N 0.000 claims 1
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 claims 1
- KXBFLNPZHXDQLV-UHFFFAOYSA-N [cyclohexyl(diisocyanato)methyl]cyclohexane Chemical compound C1CCCCC1C(N=C=O)(N=C=O)C1CCCCC1 KXBFLNPZHXDQLV-UHFFFAOYSA-N 0.000 claims 1
- HFACYLZERDEVSX-UHFFFAOYSA-N benzidine Chemical compound C1=CC(N)=CC=C1C1=CC=C(N)C=C1 HFACYLZERDEVSX-UHFFFAOYSA-N 0.000 claims 1
- ZMRQTIAUOLVKOX-UHFFFAOYSA-L calcium;diphenoxide Chemical compound [Ca+2].[O-]C1=CC=CC=C1.[O-]C1=CC=CC=C1 ZMRQTIAUOLVKOX-UHFFFAOYSA-L 0.000 claims 1
- 125000004122 cyclic group Chemical group 0.000 claims 1
- 125000002993 cycloalkylene group Chemical group 0.000 claims 1
- PJMICNUGBHGMKQ-UHFFFAOYSA-N ethane-1,1,2-triamine Chemical compound NCC(N)N PJMICNUGBHGMKQ-UHFFFAOYSA-N 0.000 claims 1
- 150000002170 ethers Chemical class 0.000 claims 1
- 125000005843 halogen group Chemical group 0.000 claims 1
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims 1
- 238000000265 homogenisation Methods 0.000 claims 1
- AOHJOMMDDJHIJH-UHFFFAOYSA-N propylenediamine Chemical compound CC(N)CN AOHJOMMDDJHIJH-UHFFFAOYSA-N 0.000 claims 1
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims 1
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000004202 carbamide Substances 0.000 abstract description 2
- 229920000642 polymer Polymers 0.000 abstract 1
- 239000002585 base Substances 0.000 description 159
- 239000012530 fluid Substances 0.000 description 99
- 238000010792 warming Methods 0.000 description 28
- 239000002994 raw material Substances 0.000 description 27
- 235000019198 oils Nutrition 0.000 description 20
- 229940031826 phenolate Drugs 0.000 description 20
- 239000002253 acid Substances 0.000 description 15
- 238000007689 inspection Methods 0.000 description 15
- 238000001816 cooling Methods 0.000 description 12
- 208000005156 Dehydration Diseases 0.000 description 11
- 238000003860 storage Methods 0.000 description 11
- 229960001860 salicylate Drugs 0.000 description 9
- QIZUBPHXHVWGHD-UHFFFAOYSA-N 4-octadecylphenol Chemical compound CCCCCCCCCCCCCCCCCCC1=CC=C(O)C=C1 QIZUBPHXHVWGHD-UHFFFAOYSA-N 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 8
- 239000004615 ingredient Substances 0.000 description 8
- 238000005461 lubrication Methods 0.000 description 8
- 230000000996 additive effect Effects 0.000 description 7
- 125000001118 alkylidene group Chemical group 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 7
- 230000035515 penetration Effects 0.000 description 7
- 238000003786 synthesis reaction Methods 0.000 description 7
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 6
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 6
- 238000005299 abrasion Methods 0.000 description 6
- 239000003513 alkali Substances 0.000 description 6
- 239000000084 colloidal system Substances 0.000 description 6
- 229910052750 molybdenum Inorganic materials 0.000 description 6
- 239000011733 molybdenum Substances 0.000 description 6
- 125000000446 sulfanediyl group Chemical group *S* 0.000 description 6
- 150000007513 acids Chemical class 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 125000005609 naphthenate group Chemical group 0.000 description 4
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- 229910052725 zinc Inorganic materials 0.000 description 4
- 241000158728 Meliaceae Species 0.000 description 3
- 240000000203 Salix gracilistyla Species 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000003963 antioxidant agent Substances 0.000 description 3
- 230000003078 antioxidant effect Effects 0.000 description 3
- RXKJFZQQPQGTFL-UHFFFAOYSA-N dihydroxyacetone Chemical compound OCC(=O)CO RXKJFZQQPQGTFL-UHFFFAOYSA-N 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- KVXHGSVIPDOLBC-UHFFFAOYSA-N selanylidenetungsten Chemical class [Se].[W] KVXHGSVIPDOLBC-UHFFFAOYSA-N 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- FKTHNVSLHLHISI-UHFFFAOYSA-N 1,2-bis(isocyanatomethyl)benzene Chemical compound O=C=NCC1=CC=CC=C1CN=C=O FKTHNVSLHLHISI-UHFFFAOYSA-N 0.000 description 2
- WJUMWVJBOZKPPU-UHFFFAOYSA-N 2,3-bis(6-methylheptyl)-N-phenylaniline Chemical compound C(CCCCC(C)C)C=1C(=C(C=CC1)NC1=CC=CC=C1)CCCCCC(C)C WJUMWVJBOZKPPU-UHFFFAOYSA-N 0.000 description 2
- 241000219000 Populus Species 0.000 description 2
- 239000004990 Smectic liquid crystal Substances 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000013556 antirust agent Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- IOJUPLGTWVMSFF-UHFFFAOYSA-N benzothiazole Chemical compound C1=CC=C2SC=NC2=C1 IOJUPLGTWVMSFF-UHFFFAOYSA-N 0.000 description 2
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 125000006273 (C1-C3) alkyl group Chemical group 0.000 description 1
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- RYYWUUFWQRZTIU-UHFFFAOYSA-N Thiophosphoric acid Chemical compound OP(O)(S)=O RYYWUUFWQRZTIU-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
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- 150000001336 alkenes Chemical class 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 239000007866 anti-wear additive Substances 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 description 1
- 229940092714 benzenesulfonic acid Drugs 0.000 description 1
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 1
- 239000012964 benzotriazole Substances 0.000 description 1
- VBIGULIJWJPALH-UHFFFAOYSA-L calcium;2-carboxyphenolate Chemical group [Ca+2].OC1=CC=CC=C1C([O-])=O.OC1=CC=CC=C1C([O-])=O VBIGULIJWJPALH-UHFFFAOYSA-L 0.000 description 1
- JYUXOLTYMOTEFQ-UHFFFAOYSA-N calcium;2-hydroxybenzoic acid Chemical compound [Ca].OC(=O)C1=CC=CC=C1O JYUXOLTYMOTEFQ-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
- 235000013877 carbamide Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
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- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 150000001924 cycloalkanes Chemical class 0.000 description 1
- 239000010727 cylinder oil Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical group C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 150000004675 formic acid derivatives Chemical class 0.000 description 1
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 239000010705 motor oil Substances 0.000 description 1
- 150000005002 naphthylamines Chemical class 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003009 phosphonic acids Chemical class 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 238000012802 pre-warming Methods 0.000 description 1
- GGHDAUPFEBTORZ-UHFFFAOYSA-N propane-1,1-diamine Chemical compound CCC(N)N GGHDAUPFEBTORZ-UHFFFAOYSA-N 0.000 description 1
- 229910000338 selenium disulfide Inorganic materials 0.000 description 1
- JNMWHTHYDQTDQZ-UHFFFAOYSA-N selenium sulfide Chemical compound S=[Se]=S JNMWHTHYDQTDQZ-UHFFFAOYSA-N 0.000 description 1
- 229960005265 selenium sulfide Drugs 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- WSFQLUVWDKCYSW-UHFFFAOYSA-M sodium;2-hydroxy-3-morpholin-4-ylpropane-1-sulfonate Chemical compound [Na+].[O-]S(=O)(=O)CC(O)CN1CCOCC1 WSFQLUVWDKCYSW-UHFFFAOYSA-M 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- 125000004646 sulfenyl group Chemical group S(*)* 0.000 description 1
- 238000006277 sulfonation reaction Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- IKXFIBBKEARMLL-UHFFFAOYSA-N triphenoxy(sulfanylidene)-$l^{5}-phosphane Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=S)OC1=CC=CC=C1 IKXFIBBKEARMLL-UHFFFAOYSA-N 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Landscapes
- Lubricants (AREA)
Abstract
润滑脂组合物及其制备方法。本发明涉及润滑脂领域，公开了一种润滑脂组合物，所述润滑脂组合物含有基础油和稠化剂，所述稠化剂含有非牛顿体硫化烷基酚钙—磺酸钙和聚脲化合物，所述稠化剂还任选地含有非牛顿体环烷酸钙、非牛顿体水杨酸钙和非牛顿体油酸钙中的一种或多种，以润滑脂重量为基准，非牛顿体硫化烷基酚钙—磺酸钙的含量为10–70重量％；非牛顿体环烷酸钙的含量为0‑70重量％；非牛顿体水杨酸钙的含量为0‑70重量％；非牛顿体油酸钙的含量为0‑70重量％；聚脲化合物的含量为0.5–30重量％；基础油的含量为10–80重量％。还公开了润滑脂组合物的制备方法。本发明的润滑脂组合物具有优良的性能，制备工艺简单、环保，产品质量稳定。Grease compositions and methods of making the same. The invention relates to the field of lubricating grease, and discloses a lubricating grease composition. The lubricating grease composition contains a base oil and a thickening agent, and the thickening agent contains a non-Newtonian sulfurized alkyl phenol calcium-calcium sulfonate and a polymer A urea compound, the thickening agent further optionally containing one or more of non-Newtonian calcium naphthenate, non-Newtonian calcium salicylate and non-Newtonian calcium oleate, based on the weight of the grease, The content of non-Newtonian sulfurized alkylphenate calcium-calcium sulfonate is 10-70% by weight; the content of non-Newtonian calcium naphthenate is 0-70% by weight; the content of non-Newtonian calcium salicylate is 0-70% % by weight; the content of non-Newtonian calcium oleate is 0-70% by weight; the content of polyurea compound is 0.5-30% by weight; the content of base oil is 10-80% by weight. Methods of making the grease compositions are also disclosed. The lubricating grease composition of the invention has excellent performance, simple preparation process, environmental protection and stable product quality.
Description
Technical field
The present invention relates to a kind of lubricant compositions and preparation method thereof.
Background technique
SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER has preferable detergent-dispersant performance, good acid neutralization capacity and excellent diffusion
Property, it is used as the detersive of lubricating oil, is widely used in modulation medium and high classes I. C. engine oil, is particularly suitable for supercharged diesel engine
For oil to reduce the carbon deposit of top land and the additive of marine cylinder oil, technology development mainly makes its height alkalization, be exactly
Calcium carbonate, which is distributed in flux oil with the sulfurized alkylphenol calcium with surface-active, becomes a kind of colloidal dispersion system.High base number
Sulfurized alkylphenol calcium is that alkyl phenol is reacted with CaO, vulcanized, carbonated contour alkalization technology and obtain, and the correlation in relation to preparation is specially
Benefit has CN101423483 etc..
It is that raw material produces lubricating grease using calcium sulfonate with high base number, because it is with excellent antirust and anticorrosive property, from investment
Since market, the extensive concern of domestic and international lubricating grease industry is caused, however, although high base number composite calcium sulfonate base grease has
Very excellent antirust and anticorrosive property, but hardening is easy in storage process, and its raw materials for production calcium sulfonate with high base number is high
Price and complicated preparation process itself cause it not promoted rapidly, meanwhile, the requirement with people to environmental protection is got over
Come higher, necessary sulfonation process is also increasingly subject to the concern of people to the pollution of environment in calcium sulfonate with high base number production process.
It finds a kind of antirust and anticorrosive property is similar with high base number composite calcium sulfonate base grease but can reduce the lubrication of the above problem
Rouge becomes the big problem that people face at present.
Summary of the invention
The object of the present invention is to provide one kind to have good antirust and anticorrosive property, storage good security and its raw material system
Standby simple process, lubricating grease of environmental protection and preparation method thereof.
The present inventor has found that sulfurized alkylphenol calcium may hold at high temperature due to containing active sulfur under study for action
Elemental sulfur easily is precipitated and generates corrosion, therefore, when as detersive, the antirust and anticorrosive property of sulfurized alkylphenol calcium are far below
Sulfoacid calcium, but when sulfurized alkylphenol calcium is prepared lubricating grease as thickening agent, but it can get and sulfonate with high base number calcium-base grease
Quite even preferably antirust and anticorrosive property, and storage good security.
Therefore, to achieve the goals above, on the one hand, the present invention provides a kind of lubricant composition, the lubricating grease
Composition contains base oil and thickening agent, and the thickening agent contains non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium and polyureas chemical combination
Object, the thickening agent is also optionally containing in non-newtonian fluid calcium naphthenate, non-newtonian fluid calcium salicylate and non-newtonian fluid calcium oleate
It is one or more, on the basis of the weight of lubricant composition, non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium content is
10-70 weight %；The content of non-newtonian fluid calcium naphthenate is 0-70 weight %；The content of non-newtonian fluid calcium salicylate is 0-70 weight
Measure %；The content of non-newtonian fluid calcium oleate is 0-70 weight %；The content of polyurea compound is 0.5-30 weight %；Base oil
Content is 10-80 weight %.
Preferably, on the basis of the weight of lubricant composition, non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium content
For 20-65 weight %；The content of non-newtonian fluid calcium naphthenate is 0-50 weight %；The content of non-newtonian fluid calcium salicylate is 0-50
Weight %；The content of non-newtonian fluid calcium oleate is 0-50 weight %；The content of polyurea compound is 1-20 weight %；Base oil
Content is 20-70 weight %.
Second aspect, the present invention provides the preparation methods of lubricant composition as described above, this method comprises: by thick
Agent and part basis oil are uniformly mixed, and refine in 180-230 DEG C of constant temperature, surplus base oil is added, necessary additive is added,
Finished product is obtained, the thickening agent contains non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium and polyurea compound, and the thickening agent is also
Optionally contain one of non-newtonian fluid calcium naphthenate, non-newtonian fluid calcium salicylate and non-newtonian fluid calcium oleate or a variety of.
The third aspect, the present invention provides a kind of preparation methods of lubricant composition, this method comprises:
(1) will contain newton body sulfurized alkylphenol calcium, newton body and/or non-newtonian fluid sulfoacid calcium, or containing newton body and/
Or non-newtonian fluid sulfurized alkylphenol calcium, the high base number material of newton body sulfoacid calcium and the mixing of part basis oil, mixture is obtained,
The high base number material also optionally contains newton body and/or non-newtonian fluid calcium naphthenate, newton body and/or non-newtonian fluid bigcatkin willow
Sour calcium and one of newton body and/or non-newtonian fluid calcium oleate or a variety of；
(2) it optionally carries out the reaction of at least partly polyurea compound: part basis oil and monoamine is added, or is additionally added two
Amine is added diisocyanate and is reacted；
(3) transforming agent is added, heats up to material retrogradation, further heats up dehydration；
(4) reaction of remaining polyurea compound is carried out；
(5) 180-230 DEG C of constant temperature refinings are warming up to, surplus base oil is added, necessary additive is added, obtains finished product.
Preferably, in step (2), the reaction of at least partly polyurea compound is carried out.
Fourth aspect, the present invention provides the lubricant compositions as made from method as described above.
Lubricant composition of the invention with the antirust quite even more excellent with sulfoacid calcium base polyurea grease and is prevented
Corrosivity, and there is excellent storage stability, also have the viscous resistance better than sulfoacid calcium base polyurea grease, machinery stable
Property, water-resistance, colloid stability, abrasion resistance, extreme pressure anti-wear and bearing lubrication service life, and also there is excellent heat-resisting quantity
Etc. performances.The feed preparation process of lubricating grease of the invention is simple and environmentally-friendly, stable product quality.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The present invention provides a kind of lubricant composition, this lubricant composition uses calcium mahogany sulfonate and/or conjunction
At sulfoacid calcium, synthesis sulfurized alkylphenol calcium, optional petroleum naphthenic acid calcium and/or synthesis calcium naphthenate, optional synthesis bigcatkin willow
Sour calcium, optional natural calcium oleate and/or synthesis calcium oleate are raw material, the polyureas generated simultaneously containing isocyanates and amine reaction
Compound.
The present invention also provides the preparation methods of foregoing grease composition.
On the one hand, the present invention provides a kind of lubricant composition, lubricant composition contains base oil and thickening agent, thick
Agent contains non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium and polyurea compound, and thickening agent also optionally contains non-newtonian fluid ring
One of alkanoic acid calcium, non-newtonian fluid calcium salicylate and non-newtonian fluid calcium oleate are a variety of, are with the weight of lubricant composition
Benchmark, non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium content are 10-70 weight %；The content of non-newtonian fluid calcium naphthenate is
0-70 weight %；The content of non-newtonian fluid calcium salicylate is 0-70 weight %；The content of non-newtonian fluid calcium oleate is 0-70 weight
Measure %；The content of polyurea compound is 0.5-30 weight %；The content of base oil is 10-80 weight %.
Preferably, on the basis of the weight of lubricant composition, non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium content
For 20-65 weight %；The content of non-newtonian fluid calcium naphthenate is 0-50 weight %；The content of non-newtonian fluid calcium salicylate is 0-50
Weight %；The content of non-newtonian fluid calcium oleate is 0-50 weight %；The content of polyurea compound is 1-20 weight %；Base oil
Content is 20-70 weight %.
In the present invention, " optionally containing " refers to can be containing the component or without containing the component, that is, non-newtonian fluid
One of calcium naphthenate, non-newtonian fluid calcium salicylate and non-newtonian fluid calcium oleate or it is a variety of be optional component, profit of the invention
It may include the component in grease composition, can not also include the component.
Non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium, non-newtonian fluid calcium naphthenate, non-newtonian fluid calcium salicylate, non newtonian
Body calcium oleate or combinations thereof object is in infrared spectrum 873cm–1–886cm–1There is crystal form calcium carbonate characteristic absorption peak in place.Non-newtonian fluid
Sulfurized alkylphenol calcium-sulfoacid calcium is to convert to obtain by transforming agent by newton body sulfoacid calcium and newton body sulfurized alkylphenol calcium, non-
Newton body sulfurized alkylphenol calcium-sulfoacid calcium total base number is 250-450mgKOH/g, preferably 300-400mgKOH/g；Non- ox
The body calcium naphthenate that pauses is converted by newton body calcium naphthenate, and the total base number of non-newtonian fluid calcium naphthenate is 250-
450mgKOH/g, preferably 300-400mgKOH/g；Non-newtonian fluid calcium salicylate is converted by newton body calcium salicylate,
The total base number of non-newtonian fluid calcium salicylate is 250-450mgKOH/g, preferably 300-400mgKOH/g；Non-newtonian fluid calcium oleate
It is to be converted by newton body calcium oleate, the total base number of non-newtonian fluid calcium oleate is 250-450mgKOH/g, preferably 300-
400mgKOH/g.And newton body sulfoacid calcium, newton body sulfurized alkylphenol calcium, newton body calcium naphthenate, newton body calcium salicylate, ox
Contain unformed calcium carbonate in body calcium oleate, in infrared spectrum 860cm–1–865cm–1There is unformed calcium carbonate feature and inhales in place
Receive peak.Newton body sulfurized alkylphenol calcium is synthesis sulfurized alkylphenol calcium, total base number 250-450mgKOH/g, preferably 300-
400mgKOH/g；Newton body sulfoacid calcium is calcium mahogany sulfonate and/or calcium alkylbenzenesulfonate, total base number 250-450mgKOH/g,
Preferably 300-400mgKOH/g；Newton body calcium naphthenate is petroleum naphthenic acid calcium and/or synthesis calcium naphthenate, total base number are
250-450mgKOH/g, preferably 300-400mgKOH/g；Newton body calcium salicylate is salicylate calcium, and total base number is
250-450mgKOH/g, preferably 300-400mgKOH/g；Newton body calcium oleate be natural calcium oleate and/or synthesis calcium oleate,
Its total base number is 250-450mgKOH/g, preferably 300-400mgKOH/g.It is non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium, non-
The base number of newton body calcium naphthenate, non-newtonian fluid calcium salicylate and the mixing of non-newtonian fluid calcium oleate is the weight of the base number of each component
Weighted average.
In the present invention, polyurea compound can be polyurea compound commonly used in the art, for example, polyureas without particular/special requirement
The structural formula of compound can be
Wherein, n is preferably 0-3 integer.
Wherein, R1、R4It can be the same or different, can be alkyl, naphthenic base or aryl, the carbon of alkyl or cycloalkyl
Number can be 8-24, preferably 10-18, and aryl can be phenyl or substituted phenyl, preferably the alkyl of phenyl or C1-C3 or
The phenyl that halogen replaces.
Wherein, R2It can be alkylidene or arlydene, the carbon number of alkylidene can be 2-12, preferably 2-8, and arlydene can
To be phenylene or biphenylene.
Wherein, R3It can be arlydene, alkylidene or cycloalkylidene, the carbon number of arlydene, alkylidene or cycloalkylidene can
Think 6-30, preferably 6-20, R3More preferably WithIn
At least one.
In the present invention, single polyureas can be used, mixing polyureas also can be used, for example, polyurea compound can be two
At least one of polyurea compound, four polyurea compounds, six polyurea compounds and eight polyurea compounds.
Above-mentioned polyurea compound can be obtained using the thinkable various methods of those skilled in the art institute, such as can be by
The method preparation recorded according to CN103060069A, CN103060070A, CN103060068A, CN103060067A, US3243372
It obtains.
The lubricating base oil can be mineral oil, synthetic oil, vegetable oil or their mixture, 100 DEG C of dynamic viscosities
For 4-150mm2/ s, preferably 10-60mm2/s.Synthetic oil can be poly-a-olefin oil (PAO), Esters oil, alkyl-silicone oil, Fischer-Tropsch
Synthetic oil etc..
Various additives can also be contained in lubricant composition of the invention, such as antioxidant, extreme pressure anti-wear additives, antirust agent
Etc..Wherein, the preferred arylamine kind antioxidant of antioxidant, accounts for the 0.01-5% of lubricating grease total weight, preferably 0.1-2.5%, can be with
It is diphenylamines, phenyl-α-at least one of naphthylamines and di-iso-octyldiphenylamine, preferably di-iso-octyldiphenylamine.Extreme-pressure anti-wear
Agent accounts for the 0.5-12% of lubricating grease total weight, preferably 0.8-8%, can be two thio Acidic phosphates zinc, two thio dialkyl group
Carbamic acid molybdenum, two thio dialkyl amido lead formates, triphenylphosphorothionate, organic molybdenum complex compound, olefine sulfide, two sulphur
Change molybdenum, polytetrafluoroethylene (PTFE), thiophosphoric acid molybdenum, chlorinated paraffin, dibutyl dithiocaarbamate antimony, tungsten disulfide, selenium disulfide,
At least one of fluorographite, calcium carbonate and zinc oxide；Antirust agent accounts for the 0.01-4.5% of lubricating grease total weight, preferably 0.1-
2%, it can be in barium mahogany sulfonate, petroleum sodium sulfonate, benzothiazole, benzotriazole, zinc naphthenate and alkenyl succinic acid
It is at least one.
Second aspect, the present invention provides the preparation methods of lubricant composition as described above, this method comprises: by thick
Agent and part basis oil are uniformly mixed, and refine in 180-230 DEG C of constant temperature, surplus base oil is added, necessary additive is added,
Finished product is obtained, the thickening agent contains non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium and polyurea compound, and the thickening agent is also
Optionally contain one of non-newtonian fluid calcium naphthenate, non-newtonian fluid calcium salicylate and non-newtonian fluid calcium oleate or a variety of.
In the present invention, " optionally containing " is as previously mentioned, details are not described herein.
In the present invention, for non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium, non-newtonian fluid calcium naphthenate, non-newtonian fluid water
Poplar acid calcium, non-newtonian fluid calcium oleate, polyurea compound, base oil and additive are as described above, details are not described herein.
It will be understood by those skilled in the art that the sum of the amount of part basis oil and the amount of surplus base oil are used
Base oil total amount, in the present invention, the weight ratio of part basis oil and surplus base oil is preferably 1:0.1-5.
For non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium, non-newtonian fluid calcium naphthenate, non-newtonian fluid calcium salicylate, non-
Newton body calcium oleate or combinations thereof object, can by newton body sulfoacid calcium, newton body sulfurized alkylphenol calcium, newton body calcium naphthenate,
Non-newtonian fluid calcium salicylate, non-newtonian fluid calcium oleate or combinations thereof object pass through transforming agent respectively and convert to obtain, for example, by newton body
Sulfoacid calcium, newton body sulfurized alkylphenol calcium, optional newton body calcium naphthenate, optional newton body calcium salicylate, optional ox
Body calcium oleate and base oil Hybrid Heating are added required transforming agent and are reacted, all transforming agents add to 50-80 DEG C
Afterwards, 80-100 DEG C constant temperature 60-90 minutes, then heat to 110-130 DEG C of dehydrations.
In the present invention, " optional " refer to can there is the raw material or no raw material, for example, " optional newton body
Calcium naphthenate ", which refers to, can this raw material of newton body calcium naphthenate, can also not have this raw material of newton body calcium naphthenate.
The third aspect, the present invention provides a kind of preparation methods of lubricant composition, this method comprises:
(1) will contain newton body sulfurized alkylphenol calcium, newton body and/or non-newtonian fluid sulfoacid calcium, or containing newton body and/
Or non-newtonian fluid sulfurized alkylphenol calcium, the high base number material of newton body sulfoacid calcium and the mixing of part basis oil, mixture is obtained,
The high base number material also optionally contains newton body and/or non-newtonian fluid calcium naphthenate, newton body and/or non-newtonian fluid bigcatkin willow
Sour calcium and one of newton body and/or non-newtonian fluid calcium oleate or a variety of；
(2) it optionally carries out the reaction of at least partly polyurea compound: part basis oil and monoamine is added, or is additionally added two
Amine is added diisocyanate and is reacted；
(3) transforming agent is added, heats up to material retrogradation, further heats up dehydration；
(4) reaction of remaining polyurea compound is carried out；
(5) 180-230 DEG C of constant temperature refinings are warming up to, surplus base oil is added, necessary additive is added, obtains finished product.
" optionally containing " is as previously mentioned, details are not described herein.
In the present invention, newton body sulfurized alkylphenol calcium, non-newtonian fluid sulfurized alkylphenol calcium, newton body sulfoacid calcium, non newtonian
Body sulfoacid calcium, newton body calcium naphthenate, non-newtonian fluid calcium naphthenate, newton body calcium salicylate, non-newtonian fluid calcium salicylate, newton
Body calcium oleate, non-newtonian fluid calcium oleate, base oil are as previously mentioned, details are not described herein.
In step (1) of the present invention, " containing newton body sulfurized alkylphenol calcium, newton body and/or non-newtonian fluid sulfoacid calcium, or
High base number material containing newton body and/or non-newtonian fluid sulfurized alkylphenol calcium, newton body sulfoacid calcium " refers to high base number material
In sulfurized alkylphenol calcium and at least one of sulfoacid calcium be newton figure.
In step (1) of the present invention, for sulfoacid calcium and sulfurized alkylphenol calcium weight ratio without particular/special requirement, preferably 1:
0.25–4.For other optional high base number materials amount without particular/special requirement, can be according to actual needs using commonly used in the art
Amount, the total weight of high base number material and the weight ratio of part basis oil are preferably 1:0.1-3.
In step (2) of the present invention, " optionally carrying out the reaction of at least partly polyurea compound " includes three kinds of situations:
(i) without the reaction of polyurea compound, that is, do not have step (2), whole polyurea compounds is only carried out in step (4)
Reaction, is converted that is, transforming agent is first added in the method for the present invention, carries out the reaction of polyurea compound after conversion again；(ii)
The reaction of part polyurea compound is carried out, i.e., carries out the reaction of part polyurea compound in step (2), in step (4) again
The reaction of remaining polyurea compound is carried out, that is, the method for the present invention carries out the reaction of part polyurea compound before conversion,
Carry out the reaction of part polyurea compound again in post-conversion；(iii) reaction for carrying out whole polyurea compounds, i.e., in step (2)
The middle reaction for carrying out whole polyurea compounds, without step (4), that is, the method for the present invention first carries out polyurea compound
Reaction, then converted.
This field is generally transforming agent to be first added to be converted, then carry out polyurea compound when preparing lubricating grease
Reaction, when such as preparing sulfoacid calcium base polyurea grease.But the present inventor has found under study for action, according to above situation (ii)
Or (iii) carries out method of the invention, than carrying out method of the invention according to situation (i), i.e., first carries out all or part of poly-
Carbamide compound reaction, then converted, it can further improve the performance of lubricating grease obtained.This may be due to first carrying out
The reaction of polyurea compound can preferably vulcanize the non-newtonian fluid that the newton body sulfurized alkylphenol calcium of oily is converted into smectic
Alkyl phenol calcium.It is therefore preferred that carrying out the reaction of at least partly polyurea compound in step (2).
When carrying out step (2) and step (4), single polyureas can be prepared, mixing polyureas can also be prepared.Prepare polyureas
The method of compound can use those skilled in the art's commonly various methods without particular/special requirement, such as can be using as above
The method that described CN103060069A, CN103060070A, CN103060068A, CN103060067A, the US3243372 is recorded
Preparation.Preferably, in step (2) and step (4), after part basis oil, monoamine, optional diamines, diisocyanate is added,
100-120 DEG C constant temperature 10-30 minutes, wherein monoamine, optional diamines, diisocyanate the amount of substance meet following relationship:
Amount × 2 of amount+diamines substance of the amount of the substance of diisocyanate × 2=monoamine substance, or, diisocyanate is excessive,
Excessive amount≤10%.
The structure of the diisocyanate is OCN-R3- NCO, R3Can be carbon number is 6-30, preferably 6-20 arlydene,
Alkylidene or cycloalkylidene, preferably Deng.
For example, the diisocyanate can be toluene di-isocyanate(TDI) (TDI), methyl diphenylene diisocyanate (MDI), six it is sub- oneself
In group diisocyanate (HDI), dicyclohexyl methyl hydride diisocyanate (HMDI) and xylylene diisocyanate (XDI) etc.
At least one.
The monoamine can be fatty amine, aliphatic cyclic amine or arylamine, structural formula R1–NH2、R4–NH2, R therein1、R4It can be with
It is alkyl, naphthenic base or aryl, the carbon number of alkyl or cycloalkyl can be 8-24, preferably 10-18, and aryl can be phenyl or take
The phenyl that the phenyl in generation, preferably phenyl or C1-C3 alkyl or halogen replace.Preferred monoamine can be selected from aniline, chlorobenzene
The arylamine of amine, parachloroanilinum and/or para-totuidine, and/or selected from lauryl amine, tetradecy lamine, cetylamine, octadecylamine fatty amine.
The diamines can be fatty amine or arylamine, structural formula NH2–R2–NH2, wherein R2It can be alkylidene or Asia
Aryl, the carbon number of alkylidene can be 2-12, preferably 2-8, and arlydene can be phenylene or biphenylene.Preferred diamines can
Be selected from p-phenylenediamine, o-phenylenediamine, 4,4 '-benzidines aromatic amine and/or selected from ethylenediamine, propane diamine, 1,6-oneself
The straight-chain fatty amine of diamines.
In step (3) of the present invention, it is preferable that at 50-80 DEG C, required transforming agent is added in preferred constant temperature 10-30 minutes
It is reacted, is stirred 8-12 minutes after preferably adding every kind of transforming agent, after all transforming agents add, in 80-100 DEG C of constant temperature 60-
90 minutes, then heat to 110-130 DEG C of dehydrations.
Transforming agent be preferably selected from fatty alcohol, fatty acid, aliphatic ketone, fatty aldehyde, fatty amine, ether, calcium carbonate, boric acid, phosphonic acids,
In carbon dioxide, phenol, aromatic alcohol, aromatic amine, aphthenic acids, C8-C20 alkyl benzene sulphonate, C16-C24 alkyl phenol and water at least
It is a kind of；It is more preferably selected from the fatty alcohol of C1-C5, the fatty acid of C1-C5, the aliphatic ketone of C1-C5, the fatty aldehyde of C1-C5, C1-C5
Fatty amine, the ether of C1-C5, boric acid, the alkyl phosphonic acid of C1-C10, the di alkyl phosphonic acid of C2-C16, C6-C20 arylphosphonic acid,
The diaryl phosphonic acids of C12-C24, the aromatic alcohol of C7-C20, the aromatic amine of C7-C20, C8-C20 alkyl benzene sulphonate, C16-C22 alkane
At least one of base phenol and water；Still more preferably selected from dodecyl benzene sulfonic acid, aphthenic acids, octadecyl phenol, methanol, different
At least one of propyl alcohol, butanol, boric acid, acetic acid and water.The additional amount of transforming agent is preferably the 2-of high base number material total weight
30%, more preferably the 6-22% of high base number material total weight.
In the present invention, fatty alcohol includes straight chain, branch and cricoid fatty alcohol, fatty acid, aliphatic ketone, fatty aldehyde, fat
Amine is similarly.
In step (5) of the present invention, it is preferable that be warming up to 180-230 DEG C of constant temperature 5-30 minutes；Surplus base oil is added, to
Temperature is cooled to 100-120 DEG C, and necessary additive is added, stirring, circulating filtration, homogenizing, degassing.
In the present invention, in step (1) in base oil used and step (2) and step (4) base oil used total amount and step
Suddenly the weight ratio of base oil used is preferably 1:0.1-5:0.1-5 in (5).
Fourth aspect, the present invention also provides grease compositions made from the preparation method provided as third aspect present invention
Object.
Compared with the lubricant composition made from the preparation method provided as second aspect, preparation side that the third aspect provides
Lubricant composition made from method has better viscous resistance, mechanical stability, water-resistance, extreme pressure anti-wear and storage stable
Property.
Embodiment
The present invention is further illustrated for embodiment below, but is not intended to limit the present invention.
In the following Examples and Comparative Examples:
Non-newtonian fluid sulfenyl phenolate-sulfoacid calcium in lubricant composition obtained, non-newtonian fluid calcium naphthenate, non-ox
The total content of body calcium salicylate and non-newtonian fluid calcium oleate uses non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium % to indicate,
That is,
Non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium %=(overbased or calcium sulfonate with high base number raw material weight+superelevation
Base number or SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER raw material weight+overbased or overbased calcium alkyl-salicylate raw material weight+overbased or
High base number calcium salicylate raw material weight+overbased or high base number calcium oleate raw material weight+transforming agent total weight)/lubricating grease is total
Weight × 100%.Transforming agent is included in non-newtonian fluid sulfurized alkylphenol calcium-sulfoacid calcium content.
Overbased and SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER is prepared according to patent CN101423483.
Overbased and calcium sulfonate with high base number is prepared according to the method for patent CN101928239A.
Overbased and overbased calcium alkyl-salicylate raw material is purchased from Xinjiang Land Fine Petrochemical Co., Ltd.
Aphthenic acids is purchased from Jinzhou Tie Chen petrochemical industry Co., Ltd.
High base number calcium salicylate is prepared according to the method for patent CN1345921.
(NLGI Spokeman, 2009,73 (2): 1-17) prepared by method according to document for high base number calcium oleate.
Embodiment 1
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: overbased sulfoacid calcium (total base number 400mgKOH/g, 24kg)；Overbased sulfurized alkylphenol calcium
(total base number 400mgKOH/g, 6kg)；(100 DEG C of kinematic viscosity are 31mm to HVI150BS lubricating base oil2/ s, 30kg)；4-ten
Eight alkylphenols (2.8kg)；Acetic acid (0.56kg)；Boric acid (2.32kg)；Octadecylamine (1.5kg)；MDI(0.7kg)；HVI500SN
(100 DEG C of kinematic viscosity are 11mm to lubricating base oil2/ s, 18kg).
It in a volume is 160L and with 24kg total base number is added in heating, stirring, circulation, cooling normal-pressure reaction kettle
For the overbased sulfoacid calcium of 400mgKOH/g, 6kg total base number be 400mgKOH/g overbased sulfurized alkylphenol calcium and
The HVI150BS lubricating base oil of 30kg, stirring, is warming up to 120 DEG C, the HVI500SN lubricating base oil and 1.5kg of 2kg is added
Octadecylamine stirs 4 minutes, is added with stirring the 0.7kg MDI dissolved with 2kg HVI500SN lubricating base oil, stirs 4 minutes,
The molar ratio of added MDI and octadecylamine be 1:2,120 DEG C constant temperature 20 minutes；50 DEG C are cooled to, constant temperature 10 minutes, is added
4-octadecylphenol of 2.8kg, temperature are controlled at 50 DEG C, are stirred 10 minutes；The acetic acid that 2.8kg concentration is 20 weight % is added
Aqueous solution stirs 10 minutes；The boric acid aqueous solution that 16.24kg concentration is 14.3 weight % is added, stirs 10 minutes, is warming up to 80
DEG C, constant temperature 90 minutes, material retrogradation；It is warming up to 130 DEG C under stirring, is kept for 30 minutes, dehydration；Finally it is warming up to 200 DEG C of constant temperature
10 minutes.Then, 160 DEG C are cooled to, remaining HVI500SN lubricating base oil is added；110 DEG C are cooled to temperature, is circulated throughout
Filter, homogenizing, degassing obtain finished product.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate
41.5 weight % of calcium-sulfoacid calcium；2.6 weight % of polyureas；55.9 weight % of lubricating base oil.
Embodiment 2
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: overbased sulfoacid calcium (total base number 400mgKOH/g, 24kg)；SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER
(total base number 320mgKOH/g, 6kg)；(100 DEG C of kinematic viscosity are 31mm to HVI150BS lubricating base oil2/ s, 10kg)；4-ten
Eight alkylphenols (2.2kg)；N-butanol (0.6kg)；Acetic acid (0.56kg)；Boric acid (2.32kg)；Lauryl amine (1.31kg)；MDI
(0.89kg)；(100 DEG C of kinematic viscosity are 11mm to HVI500SN lubricating base oil2/ s, 38kg).
It in a volume is 160L and with 24kg total base number is added in heating, stirring, circulation, cooling normal-pressure reaction kettle
For the overbased sulfoacid calcium of 400mgKOH/g, 6kg total base number be 320mgKOH/g overbased sulfurized alkylphenol calcium and
The HVI150BS lubricating base oil of 10kg, stirring, be warming up to 100 DEG C, be added 1kg HVI500SN lubricating base oil and
0.131kg lauryl amine stirs 8 minutes, is added with stirring the 0.0895kg MDI dissolved with 1kg HVI500SN lubricating base oil,
Stirring 8 minutes, the molar ratio of added MDI and lauryl amine are 1:2,100 DEG C constant temperature 10 minutes；80 DEG C are cooled to, constant temperature 10 divides
Clock, is added 4-octadecylphenol of 2.8kg and 0.6kg n-butanol, and temperature is controlled at 80 DEG C or so, stirred 10 minutes；It is added
2.8kg concentration is the aqueous acetic acid of 20 weight %, is stirred 10 minutes；The boric acid that 16.24kg concentration is 14.3 weight % is added
Aqueous solution stirs 10 minutes, is warming up to 90 DEG C, and constant temperature 60 minutes, material retrogradation；It is warming up to 110 DEG C under stirring, is kept for 60 points
Clock, dehydration；The HVI500SN lubricating base oil and 1.179kg lauryl amine of 1kg is added, stirs 8 minutes, is added with stirring with 1kg
The 0.801kg MDI of HVI500SN lubricating base oil dissolution, is stirred 8 minutes, and the molar ratio of added MDI and lauryl amine is 1:2,
110 DEG C constant temperature 10 minutes；Finally being warming up to 230 DEG C, constant temperature for 5 minutes.Then, remaining HVI500SN lubricating base oil is added；To
Temperature is cooled to 120 DEG C, and circulating filtration, homogenizing, degassing obtain finished product.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate
41.5 weight % of calcium-sulfoacid calcium；2.6 weight % of polyureas；55.9 weight % of lubricating base oil.
Embodiment 3
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: calcium sulfonate with high base number (total base number 320mgKOH/g, 6kg)；Overbased sulfurized alkylphenol calcium is (total
Base number is 400mgKOH/g, 24kg)；(100 DEG C of kinematic viscosity are 31mm to HVI150BS lubricating base oil2/ s, 25kg)；4-ten eight
Alkylphenol (2.8kg)；Acetic acid (0.56kg)；Boric acid (2.32kg)；Octadecylamine (1.66kg)；TDI(0.54kg)；HVI500SN
(100 DEG C of kinematic viscosity are 11mm to lubricating base oil2/ s, 23kg).
It in a volume is 160L and with 6kg total base number is added in heating, stirring, circulation, cooling normal-pressure reaction kettle
The overbased sulfurized alkylphenol calcium and 25kg that calcium sulfonate with high base number, 24kg total base number for 320mgKOH/g are 400mgKOH/g
HVI150BS lubricating base oil, stirring, be warming up to 110 DEG C, the HVI500SN lubricating base oil and 1.66kg 18 of 2kg be added
Amine stirs 6 minutes, is added with stirring the 0.54kg TDI dissolved with 2kg HVI500SN lubricating base oil, stirs 6 minutes, institute
The molar ratio of the TDI and octadecylamine that add be 1:2,110 DEG C constant temperature 15 minutes；65 DEG C are cooled to, constant temperature 10 minutes, 2.8kg is added
4-octadecylphenols, temperature are controlled at 65 DEG C, are stirred 10 minutes；The aqueous acetic acid that 2.8kg concentration is 20 weight % is added,
Stirring 10 minutes；The boric acid aqueous solution that 16.24kg concentration is 14.3 weight % is added, stirs 10 minutes, is warming up to 100 DEG C, perseverance
Temperature 70 minutes, material retrogradation；It is warming up to 120 DEG C under stirring, is kept for 45 minutes, dehydration；180 DEG C of constant temperature 20 are finally warming up to divide
Clock.Then, 160 DEG C are cooled to, remaining HVI500SN lubricating base oil is added；100 DEG C are cooled to temperature, circulating filtration,
Homogenizing, degassing obtain finished product.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate
39.6 weight % of calcium-sulfoacid calcium；2.6 weight % of polyureas；57.8 weight % of lubricating base oil.
Embodiment 4
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: calcium sulfonate with high base number (total base number 320mgKOH/g, 14kg)；SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER is (total
Base number is 320mgKOH/g, 6kg)；Naphthenate with superhigh base number calcium (total base number 400mgKOH/g, 10kg)；HVI150BS lubrication
(100 DEG C of kinematic viscosity are 31mm to base oil2/ s, 15kg)；4-octadecylphenols (2.8kg)；Acetic acid (0.56kg)；Boric acid
(2.32kg)；Octadecylamine (1.5kg)；MDI(0.7kg)；(100 DEG C of kinematic viscosity are 11mm to HVI500SN lubricating base oil2/ s,
7kg)；It is right, right '-di-iso-octyldiphenylamine (0.4kg).
Lubricant composition is prepared according to the method for embodiment 1, unlike, sulfoacid calcium is using total base number
The calcium sulfonate with high base number of 320mgKOH/g, the high base number sulfenyl phenolate that sulfurized alkylphenol calcium is 320mgKOH/g using total base number
Calcium, and increase the naphthenate with superhigh base number calcium that total base number is 400kgKOH/g；And 110 DEG C are cooled to temperature, is added
Pair of 0.4kg, right '-di-iso-octyldiphenylamine stir 10 minutes, and then circulating filtration, homogenizing, degassing obtain finished product；Each ingredient
Dosage it is as above.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate
59.2 weight % of calcium-sulfoacid calcium；3.6 weight % of polyureas；36.5 weight % of lubricating base oil；It is right, right '-di-iso-octyldiphenylamine
0.7 weight %.
Embodiment 5
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: overbased sulfoacid calcium (total base number 400mgKOH/g, 10kg)；Overbased sulfurized alkylphenol calcium
(total base number 400mgKOH/g, 10kg)；Overbased calcium salicylate (total base number 400mgKOH/g, 10kg)；HVI150BS
(100 DEG C of kinematic viscosity are 31mm to lubricating base oil2/ s, 25kg)；4-octadecylphenols (2.8kg)；Acetic acid (0.56kg)；Boron
Sour (2.32kg)；Octadecylamine (4.5kg)；MDI(2.1kg)；(100 DEG C of kinematic viscosity are 11mm to HVI500SN lubricating base oil2/
S, 18kg).
Lubricant composition is prepared according to the method for embodiment 1, unlike, high base number material increases overbased water
Poplar acid calcium, the dosage of each ingredient are as above.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate
41.8 weight % of calcium-sulfoacid calcium；7.8 weight % of polyureas；50.4 weight % of lubricating base oil.
Embodiment 6
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: overbased sulfoacid calcium (total base number 400mgKOH/g, 6kg)；SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER is (total
Base number is 320mgKOH/g, 20kg)；Overbased calcium oleate (total base number 400mgKOH/g, 4kg)；Poly- α-the alkene of full synthetic oil
(100 DEG C of kinematic viscosity are 41mm to hydrocarbon ils PAO 402/ s, 25kg)；4-octadecylphenols (2.8kg)；Acetic acid (0.56kg)；Boron
Sour (2.32kg)；Octadecylamine (1.5kg)；MDI(0.7kg)；(100 DEG C of kinematic viscosity are the poly- α of full synthetic oil-alkene oil PAO 10
11mm2/ s, 23kg)；Two thio dibutylphosphoric acid zinc (2kg), dibutyl dithiocaarbamate molybdenum (1kg), tungsten disulfide
(2kg), two tungsten selenides (2kg) are right, right '-di-iso-octyldiphenylamine (0.2kg).
Lubricant composition is prepared according to the method for embodiment 1, unlike, sulfurized alkylphenol calcium is using total base number
The SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER of 320mgKOH/g, and increase the overbased calcium oleate that total base number is 400kgKOH/g；Make
HVI150BS and HVI500SN are replaced respectively with the poly- α of full synthetic oil-alkene oil PAO 40 and PAO10；And it is cooled to temperature
110 DEG C, the two thio dibutylphosphoric acid zinc of 2kg are added, stirs 10 minutes, the dibutyl dithiocaarbamate molybdenum of 1kg is added,
The tungsten disulfide of 2kg is added in stirring 10 minutes, stirs 10 minutes, and two tungsten selenides of 2kg are added, and stirs 10 minutes, is added
Pair of 0.2kg, right '-di-iso-octyldiphenylamine stir 10 minutes, and then circulating filtration, homogenizing, degassing obtain finished product；Each ingredient
Dosage it is as above.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate
38.3 weight % of calcium-sulfoacid calcium；2.4 weight % of polyureas；51.6 weight % of lubricating base oil；Two thio dibutylphosphoric acid zinc 2.2
Weight %；1.1 weight % of dibutyl dithiocaarbamate molybdenum；2.1 weight % of tungsten disulfide；Two tungsten selenides, 2.1 weight %；
It is right, right ' 0.2 weight % of-di-iso-octyldiphenylamine.
Embodiment 7
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: calcium sulfonate with high base number (total base number 320mgKOH/g, 6kg)；Overbased sulfurized alkylphenol calcium is (total
Base number is 400mgKOH/g, 12kg)；Overbased calcium alkyl-salicylate (total base number 300mgKOH/g, 6kg)；High base number calcium salicylate
(total base number 300mgKOH/g, 6kg)；(100 DEG C of kinematic viscosity are 31mm to HVI150BS lubricating base oil2/ s, 25kg)；4-ten
Eight alkylphenols (2.8kg)；Acetic acid (0.56kg)；Boric acid (2.32kg)；Octadecylamine (1.5kg)；MDI(0.7kg)；HVI500SN
(100 DEG C of kinematic viscosity are 11mm to lubricating base oil2/ s, 23kg).
Lubricant composition is prepared according to the method for embodiment 1, unlike, sulfoacid calcium is using total base number
The calcium sulfonate with high base number of 320mgKOH/g, while increasing overbased calcium alkyl-salicylate and high base number calcium salicylate；The use of each ingredient
Amount is as above.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate
41.5 weight % of calcium-sulfoacid calcium；2.6 weight % of polyureas；55.9 weight % of lubricating base oil.
Embodiment 8
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: calcium sulfonate with high base number (total base number 320mgKOH/g, 6kg)；SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER (total alkali
Value is 320mgKOH/g, 12kg)；High base number calcium salicylate (total base number 360mgKOH/g, 6kg)；High base number calcium oleate (total alkali
Value is 400mgKOH/g, 6kg)；(100 DEG C of kinematic viscosity are 31mm to HVI150BS lubricating base oil2/ s, 25kg)；4-octadecanes
Base phenol (2.8kg)；Acetic acid (0.56kg)；Boric acid (2.32kg)；Octadecylamine (1.5kg)；MDI(0.7kg)；HVI500SN lubrication
(100 DEG C of kinematic viscosity are 11mm to base oil2/ s, 23kg).
Lubricant composition is prepared according to the method for embodiment 1, unlike, sulfoacid calcium is using total base number
The calcium sulfonate with high base number of 320mgKOH/g, the high base number sulfenyl phenolate that sulfurized alkylphenol calcium is 320mgKOH/g using total base number
Calcium, while increasing high base number calcium salicylate and high base number calcium oleate；The dosage of each ingredient is as above.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate
41.5 weight % of calcium-sulfoacid calcium；2.6 weight % of polyureas；55.9 weight % of lubricating base oil.
Embodiment 9
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: overbased sulfoacid calcium (total base number 400mgKOH/g, 10kg)；Overbased sulfurized alkylphenol calcium
(total base number 400mgKOH/g, 10kg)；Overbased calcium alkyl-salicylate (total base number 360mgKOH/g, 5kg)；High base number calcium oleate
(total base number 320mgKOH/g, 5kg)；(100 DEG C of kinematic viscosity are 31mm to HVI150BS lubricating base oil2/ s, 25kg)；4-ten
Eight alkylphenols (2.8kg)；Acetic acid (0.56kg)；Boric acid (2.32kg)；Octadecylamine (0.94kg)；Para-totuidine (0.38kg)；
MDI(0.88kg)；(100 DEG C of kinematic viscosity are 11mm to HVI500SN lubricating base oil2/ s, 23kg).
Lubricant composition is prepared according to the method for embodiment 1, unlike, increase overbased calcium alkyl-salicylate and high-alkali
It is worth calcium oleate, meanwhile, after octadecylamine is added, it is additionally added para-totuidine, then adds MDI；The dosage of each ingredient is as above.It examines
It the results are shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate
41.5 weight % of calcium-sulfoacid calcium；2.6 weight % of polyureas；55.9 weight % of lubricating base oil.
Embodiment 10
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: calcium sulfonate with high base number (total base number 320mgKOH/g, 5kg)；SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER (total alkali
Value is 320mgKOH/g, 12kg)；Naphthenate with superhigh base number calcium (total base number 400mgKOH/g, 3kg)；Overbased salicylic acid
Calcium (total base number 400mgKOH/g, 5kg)；Overbased calcium oleate (total base number 400mgKOH/g, 5kg)；HVI150BS profit
(100 DEG C of kinematic viscosity are 31mm to sliding base oil2/ s, 25kg)；4-octadecylphenols (1.6kg)；(total acid number is aphthenic acids
180mgKOH/g, 1.2kg)；Acetic acid (0.56kg)；Boric acid (2.32kg)；Octadecylamine (0.84kg)；Lauryl amine (0.58kg)；MDI
(0.78kg)；(100 DEG C of kinematic viscosity are 11mm to HVI500SN lubricating base oil2/ s, 23kg).
Lubricant composition is prepared according to the method for embodiment 1, unlike, sulfoacid calcium is using total base number
The calcium sulfonate with high base number of 320mgKOH/g, the high base number sulfenyl phenolate that sulfurized alkylphenol calcium is 320mgKOH/g using total base number
Calcium, and increase naphthenate with superhigh base number calcium, calcium salicylate and calcium oleate；After 4-octadecylphenols are added, it is additionally added cycloalkanes
Then acid adds acetic acid and boric acid；After octadecylamine is added, it is additionally added lauryl amine, then adds MDI；The dosage of each ingredient
As above.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate
41.5 weight % of calcium-sulfoacid calcium；2.6 weight % of polyureas；55.9 weight % of lubricating base oil.
Embodiment 11
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: calcium sulfonate with high base number (total base number 360mgKOH/g, 5kg)；SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER (total alkali
Value is 360mgKOH/g, 12kg)；Overbased calcium alkyl-salicylate (total base number 300mgKOH/g, 3kg)；High base number calcium salicylate is (total
Base number is 300mgKOH/g, 5kg)；High base number calcium oleate (total base number 300mgKOH/g, 5kg)；HVI150BS lubricating base oil
(100 DEG C of kinematic viscosity are 31mm2/ s, 25kg)；4-octadecylphenols (2.8kg)；N-butanol (1kg)；Acetic acid (0.56kg)；
Boric acid (2.32kg)；Octadecylamine (1.5kg)；MDI(0.7kg)；(100 DEG C of kinematic viscosity are HVI500SN lubricating base oil
11mm2/ s, 23kg).
Lubricant composition is prepared according to the method for embodiment 1, unlike, sulfoacid calcium is using total base number
The calcium sulfonate with high base number of 360mgKOH/g, the high base number sulfenyl phenolate that sulfurized alkylphenol calcium is 360mgKOH/g using total base number
Calcium, while increasing overbased calcium alkyl-salicylate, calcium salicylate and calcium oleate；Transforming agent increases n-butanol, is being added 4-ten eight
It is added after alkylphenol；The dosage of each ingredient is as above.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate
41.5 weight % of calcium-sulfoacid calcium；2.6 weight % of polyureas；55.9 weight % of lubricating base oil.
Embodiment 12
The present embodiment is for illustrating lubricant composition prepared by the present invention.
The preparation of non-newtonian fluid calcium sulfonate with high base number: in a volume being 30L and with heating, stirring, circulation, cooling
100 DEG C of kinematic viscosity of calcium sulfonate with high base number and 5kg that 15kg total base number is 350mgKOH/g are added in normal-pressure reaction kettle is
31mm2The HVI150BS lubricating base oil of/s, stirring, heats to 80 DEG C, constant temperature 10 minutes；2.5kg dodecyl is added
Benzene sulfonic acid, temperature are controlled at 80 DEG C or so, are stirred 10 minutes；The acetic acid and 4 times of acetic acid weight of aqueous solution of 0.5kg is added, stirs
It mixes 10 minutes；85 DEG C are warming up to, constant temperature 90 minutes, it is spare to obtain non-newtonian fluid sulfoacid calcium at smectic for material retrogradation.
It in volume is 160L and with above-mentioned prepare is added in heating, stirring, circulation, cooling normal-pressure reaction kettle A
The overbased sulfurized alkylphenol calcium and 25kg that non-newtonian fluid calcium sulfonate with high base number, 7kg total base number are 400mgKOH/g
(100 DEG C of kinematic viscosity are 31mm to HVI150BS lubricating base oil2/ s, similarly hereinafter), it stirs evenly.
In volume for 10L and with heating, the HVI500SN for stirring, recycling, 5kg being added in the normal-pressure reaction kettle B of cooling
(100 DEG C of kinematic viscosity are 11mm to lubricating base oil2/ s, similarly hereinafter) and 1kg MDI rapidly pre-warming is to 90 DEG C, is quickly added with stirring
0.12kg ethylenediamine stirs 4 minutes, 1.08kg octadecylamine is added and stirs 4 minutes, and added MDI, ethylenediamine and octadecylamine rub
You than be 2:1:2,120 DEG C constant temperature 20 minutes, obtain polyureas I.
It in volume is 20L and with 10kg100 DEG C of movement is added in heating, stirring, circulation, cooling normal-pressure reaction kettle C
Viscosity is 11mm2The HVI500SN lubricating base oil and 1.29kg MDI of/s is preheating to 90 DEG C, is quickly added with stirring 0.84kg
Octadecylamine and 0.19kg ethylenediamine, added MDI, octadecylamine, ethylenediamine molar ratio be 3.3:2:2,120 DEG C of constant temperature 20 divide
Clock obtains polyureas II.
Gained polyureas I and polyureas II are all squeezed into reaction kettle A, stirred evenly, at 60 DEG C, constant temperature 10 minutes, is added
Enter 4-octadecylphenol of 3kg, temperature is controlled at 60 DEG C, stirred 10 minutes；It is water-soluble that the 12.5kg butanol that concentration is 20% is added
Liquid stirs 10 minutes；87 DEG C constant temperature 70 minutes, material retrogradation；It is warming up to 130 DEG C under stirring, is kept for 30 minutes, dehydration.Most
After be warming up to 200 DEG C constant temperature for 5 minutes.Then, 150 DEG C are cooled to, the HVI500SN lubricating base oil of 8kg is added；To temperature
110 DEG C are cooled to, circulating filtration, homogenizing, degassing obtain finished product.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate
40.4 weight % of calcium-sulfoacid calcium；5.0 weight % of polyureas；54.6 weight % of lubricating base oil.
Embodiment 13
The present embodiment is for illustrating lubricant composition prepared by the present invention.
It in a volume is 160L and with 6kg total base number is added in heating, stirring, circulation, cooling normal-pressure reaction kettle
Overbased sulfurized alkylphenol calcium, the 6kg for being 420mgKOH/g for the overbased sulfoacid calcium of 400mgKOH/g, 6kg total base number
High base number calcium salicylate that overbased calcium alkyl-salicylate that total base number is 320mgKOH/g, 6kg total base number are 360mgKOH/g, 6kg
Total base number is the overbased calcium oleate of 400mgKOH/g and the HVI150BS lubricating base oil of 10kg, is stirred evenly.
In volume for 20L and with heating, the HVI500SN for stirring, recycling, 10kg being added in the normal-pressure reaction kettle of cooling
Lubricating base oil and 1.17kg MDI are preheating to 80 DEG C, be quickly added with stirring 0.84kg octadecylamine, 0.19kg ethylenediamine it is mixed
Close object, added MDI, monoamine, diamines molar ratio be 3:2:2,120 DEG C constant temperature 20 minutes, obtain polyureas.
Gained polyureas is all squeezed into a upper kettle, is stirred evenly, at 50 DEG C, constant temperature 10 minutes；1kg 12 is added
4-octadecylphenol of alkyl benzene sulphonate and 1kg, temperature are controlled at 50 DEG C, are stirred 10 minutes；1kg methanol is added, stirs 10 points
Clock；The aqueous acetic acid that 2kg concentration is 20 weight % is added, stirs 10 minutes；83 DEG C constant temperature 80 minutes, material retrogradation；It stirs
It mixes down and is warming up to 120 DEG C, kept for 45 minutes, dehydration.Finally being warming up to 200 DEG C, constant temperature for 5 minutes.Then, it is added 8kg's
HVI500SN lubricating base oil；110 DEG C are cooled to temperature, circulating filtration, homogenizing, degassing obtain finished product.Inspection result is shown in Table
1。
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate
52.5 weight % of calcium-sulfoacid calcium；3.5 weight % of polyureas；44.0 weight % of lubricating base oil.
Embodiment 14
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: overbased sulfoacid calcium (total base number 400mgKOH/g, 24kg)；Overbased sulfurized alkylphenol calcium
(total base number 400mgKOH/g, 6kg)；(100 DEG C of kinematic viscosity are 31mm to HVI150BS lubricating base oil2/ s, 30kg)；4-ten
Eight alkylphenols (2.8kg)；Acetic acid (0.56kg)；Boric acid (2.32kg)；Octadecylamine (1.5kg)；MDI(0.7kg)；HVI500SN
(100 DEG C of kinematic viscosity are 11mm to lubricating base oil2/ s, 18kg).
It in a volume is 160L and with 24kg total base number is added in heating, stirring, circulation, cooling normal-pressure reaction kettle
For the overbased sulfoacid calcium of 400mgKOH/g, 6kg total base number be 400mgKOH/g overbased sulfurized alkylphenol calcium and
The HVI150BS lubricating base oil of 30kg, stirring, heats to 50 DEG C, constant temperature 10 minutes；4-octadecyl of 2.8kg is added
Phenol, temperature are controlled at 50 DEG C, are stirred 10 minutes；The aqueous acetic acid that 2.8kg concentration is 20 weight % is added, stirs 10 points
Clock；The boric acid aqueous solution that 16.24kg concentration is 14.3 weight % is added, stirs 10 minutes, is warming up to 80 DEG C, constant temperature 90 minutes,
Material retrogradation；It is warming up to 130 DEG C under stirring, is kept for 30 minutes, dehydration.
It in another volume is 10L and with being added 2kg's in heating, stirring, circulation, cooling normal-pressure reaction kettle
HVI500SN lubricating base oil and 1.5kg octadecylamine are warming up to 120 DEG C, stir 4 minutes, are added with stirring with 2kg
The 0.7kg MDI of HVI500SN lubricating base oil dissolution, is stirred 4 minutes, and the molar ratio of added MDI and octadecylamine is 1:2,
120 DEG C constant temperature 20 minutes, obtain polyureas.
Gained polyureas is all squeezed into a upper kettle, is stirred evenly, is finally warming up to 200 DEG C of constant temperature 10 minutes.Then,
160 DEG C are cooled to, remaining HVI500SN lubricating base oil is added；110 DEG C are cooled to temperature, circulating filtration, homogenizing, degassing
Obtain finished product.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate
41.5 weight % of calcium-sulfoacid calcium；2.6 weight % of polyureas；55.9 weight % of lubricating base oil.
The two polyureas molecular structural formulas contained in component are as follows:
Embodiment 15
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Raw material components: overbased sulfoacid calcium (total base number 400mgKOH/g, 24kg)；Overbased sulfurized alkylphenol calcium
(total base number 400mgKOH/g, 6kg)；(100 DEG C of kinematic viscosity are 31mm to HVI150BS lubricating base oil2/ s, 30kg)；4-ten
Eight alkylphenols (2.8kg)；Acetic acid (0.56kg)；Boric acid (2.32kg)；Octadecylamine (1.5kg)；MDI(0.7kg)；HVI500SN
(100 DEG C of kinematic viscosity are 11mm to lubricating base oil2/ s, 18kg).
It in a volume is 160L and with 24kg total base number is added in heating, stirring, circulation, cooling normal-pressure reaction kettle
For the overbased sulfoacid calcium of 400mgKOH/g, 6kg total base number be 400mgKOH/g overbased sulfurized alkylphenol calcium and
The HVI150BS lubricating base oil of 30kg, stirring are warming up to 50 DEG C, constant temperature 10 minutes, 4-octadecylphenol of 2.8kg are added,
Temperature is controlled at 50 DEG C, is stirred 10 minutes；The aqueous acetic acid that 2.8kg concentration is 20 weight % is added, stirs 10 minutes；It is added
16.24kg concentration is the boric acid aqueous solution of 14.3 weight %, is stirred 10 minutes, is warming up to 80 DEG C, constant temperature 90 minutes, material became
It is thick；It is warming up to 130 DEG C under stirring, is kept for 30 minutes, dehydration；The HVI500SN lubricating base oil and 1.5kg 18 of 2kg is added
Amine stirs 4 minutes, is added with stirring the 0.7kg MDI dissolved with 2kg HVI500SN lubricating base oil, stirs 4 minutes, added
MDI and octadecylamine molar ratio be 1:2,120 DEG C constant temperature 20 minutes.Finally it is warming up to 200 DEG C of constant temperature 10 minutes.Then, cold
But to 160 DEG C, remaining HVI500SN lubricating base oil is added；110 DEG C are cooled to temperature, circulating filtration, deaerates at homogenizing
To finished product.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate
41.5 weight % of calcium-sulfoacid calcium；2.6 weight % of polyureas；55.9 weight % of lubricating base oil.
Embodiment 16
The present embodiment is for illustrating lubricant composition prepared by the present invention.
Lubricant composition is prepared according to the method for embodiment 1, unlike, 4-octadecylphenols are replaced with into fourth
Ketone, replaces with ethylene glycol monobutyl ether for aqueous acetic acid, and boric acid aqueous solution is replaced with octadecylamine.Inspection result is shown in Table 1.
In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfenyl phenolate
41.5 weight % of calcium-sulfoacid calcium；2.6 weight % of polyureas；55.9 weight % of lubricating base oil.
Comparative example 1
Lubricant composition is prepared according to the method for embodiment 1, unlike, overbased sulfurized alkylphenol calcium total alkali
Value is replaced by the overbased sulfoacid calcium of 400mgKOH/g, and obtained each performance data of lubricating grease finished product is shown in Table 1.
In the lubricating grease that this comparative example obtains, on the basis of lubricating grease weight, composition are as follows: 41.5 weight of non-newtonian fluid sulfoacid calcium
Measure %；2.6 weight % of polyureas；55.9 weight % of lubricating base oil.
Each lubricating grease properties of sample data of table 1
Each indication test method: dropping point: GB/T 3498；Work cone penetration and extension work cone penetration: GB/T 269；It is rotten
Erosion: GB/T 7326；Anticorrosive property: GB/T 5018；Water drenches number of dropouts: SH/T 0109；Salt spray test: SH/T 0081；Water resistant
It is spraying: SH/T0643；Stencil oil-dividing: SH/T 0324；Surface hardened layer value: 0370 appendix A of SH/T；Coefficient of friction: SH/T
0721；Tetra-ball machine test: SH/T 0202；The bearing lubrication service life: ASTM D 3336.
Each lubricating grease properties of sample data of 1 (Continued) of table
Each indication test method: dropping point: GB/T 3498；Work cone penetration and extension work cone penetration: GB/T 269；It is rotten
Erosion: GB/T 7326；Anticorrosive property: GB/T 5018；Water drenches number of dropouts: SH/T 0109；Salt spray test: SH/T 0081；Water resistant
It is spraying: SH/T0643；Stencil oil-dividing: SH/T 0324；Surface hardened layer value: 0370 appendix A of SH/T；Coefficient of friction: SH/T
0721；Tetra-ball machine test: SH/T 0202；The bearing lubrication service life: ASTM D 3336.
It will be understood by those skilled in the art that work cone penetration is smaller, grease thickening performance is better；Extend work
The difference for making cone penetration and the cone penetration that works is smaller, and the mechanical stability of lubricating grease can be better；Water leaching number of dropouts is smaller, lubricating grease
Water-resistance it is better；Salt spray test higher grade, and the antirust and anticorrosive property of lubricating grease are better；Water resistant is worth smaller, lubrication by spraying
The adhesiveness and water-resistance of rouge are better；Stencil oil-dividing value is smaller, and the colloid stability of lubricating grease is better；Surface hardened layer value it is absolute
It is worth smaller, the storage stability of lubricating grease is better；Coefficient of friction is smaller, and the abrasion resistance of lubricating grease is better；PB, PD value are bigger,
The extreme pressure anti-wear of lubricating grease is better.
Embodiment 1 and comparative example 1 are compared to antirust and anticorrosion as can be seen that lubricant composition of the invention
Property, storage stability be substantially better than sulfoacid calcium base polyurea grease.Moreover, lubricant composition of the invention, which has, is better than sulfonic acid
Viscous resistance, mechanical stability, water-resistance, colloid stability, abrasion resistance, extreme pressure anti-wear and the bearing of calcium base polyurea grease
Lubricating life.Moreover, lubricant composition of the invention also has excellent heat-resisting quantity.
Embodiment 1 and embodiment 14 are compared the lubricant composition as can be seen that being prepared in situ, had better
Viscous resistance, mechanical stability, water-resistance, extreme pressure anti-wear and storage stability；By embodiment 1 and embodiment 14, embodiment 15
It is compared as can be seen that first carrying out the reaction of polyurea compound, then converted, lubricant composition obtained has more preferable
Viscous resistance, mechanical stability, water-resistance, colloid stability, storage stability, abrasion resistance, extreme pressure anti-wear and bearing profit
The sliding service life；Embodiment 1 and embodiment 16 are compared as can be seen that transforming agent is selected from dodecyl benzene sulfonic acid, aphthenic acids, ten
At least one of eight alkyl phenols, methanol, isopropanol, butanol, boric acid, acetic acid and water, lubricant composition obtained have more
Good viscous resistance, mechanical stability, water-resistance, colloid stability, storage stability, abrasion resistance, extreme pressure anti-wear and bearing
Lubricating life.
Lubricant composition of the invention with the antirust quite even more excellent with sulfoacid calcium base polyurea grease and is prevented
Corrosivity, and there is excellent storage stability, also have the viscous resistance better than sulfoacid calcium base polyurea grease, machinery stable
Property, water-resistance, colloid stability, abrasion resistance, extreme pressure anti-wear and bearing lubrication service life, and also there is excellent heat-resisting quantity
Etc. performances.The feed preparation process of lubricating grease of the invention is simple and environmentally-friendly, stable product quality.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention to it is various can
No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (23)
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Citations (4)
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|---|---|---|---|---|
| US4181619A (en) * | 1978-10-30 | 1980-01-01 | Mobil Oil Corporation | Antiwear composition |
| WO2002012418A3 (en) * | 2000-08-10 | 2002-04-25 | Shell Int Research | Grease composition with improved rust prevention and abrasion resistance properties |
| CN101117604A (en) * | 2006-07-31 | 2008-02-06 | 中国石油化工股份有限公司 | grease composition |
| CN101550095A (en) * | 2009-05-26 | 2009-10-07 | 辽宁渤大化工有限公司 | Method for preparing overbased synthesized heavy alkyl benzene calcium sulfonate |
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2015
- 2015-03-11 CN CN201510105336.9A patent/CN106032477B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4181619A (en) * | 1978-10-30 | 1980-01-01 | Mobil Oil Corporation | Antiwear composition |
| WO2002012418A3 (en) * | 2000-08-10 | 2002-04-25 | Shell Int Research | Grease composition with improved rust prevention and abrasion resistance properties |
| CN101117604A (en) * | 2006-07-31 | 2008-02-06 | 中国石油化工股份有限公司 | grease composition |
| CN101550095A (en) * | 2009-05-26 | 2009-10-07 | 辽宁渤大化工有限公司 | Method for preparing overbased synthesized heavy alkyl benzene calcium sulfonate |
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