CN1852969B - 协同有机硼酸酯组合物及含有该组合物的润滑剂组合物 - Google Patents
协同有机硼酸酯组合物及含有该组合物的润滑剂组合物 Download PDFInfo
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- CN1852969B CN1852969B CN2003801008068A CN200380100806A CN1852969B CN 1852969 B CN1852969 B CN 1852969B CN 2003801008068 A CN2003801008068 A CN 2003801008068A CN 200380100806 A CN200380100806 A CN 200380100806A CN 1852969 B CN1852969 B CN 1852969B
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- composition
- component
- boric acid
- ratio
- ester
- Prior art date
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- Expired - Lifetime
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- 239000000203 mixture Substances 0.000 title claims abstract description 186
- 230000001050 lubricating effect Effects 0.000 title description 5
- 230000002195 synergetic effect Effects 0.000 title description 3
- -1 organo borate ester Chemical class 0.000 claims abstract description 121
- 150000002148 esters Chemical class 0.000 claims abstract description 57
- 239000000654 additive Substances 0.000 claims abstract description 46
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 26
- 239000011733 molybdenum Substances 0.000 claims abstract description 25
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 21
- DKVNPHBNOWQYFE-UHFFFAOYSA-N carbamodithioic acid Chemical compound NC(S)=S DKVNPHBNOWQYFE-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000012990 dithiocarbamate Substances 0.000 claims abstract description 19
- 239000010685 fatty oil Substances 0.000 claims abstract description 15
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims abstract description 11
- PTISTKLWEJDJID-UHFFFAOYSA-N sulfanylidenemolybdenum Chemical compound [Mo]=S PTISTKLWEJDJID-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004327 boric acid Substances 0.000 claims description 64
- 229910052796 boron Inorganic materials 0.000 claims description 33
- 229910052799 carbon Inorganic materials 0.000 claims description 33
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 32
- 125000004432 carbon atom Chemical group C* 0.000 claims description 31
- 239000005864 Sulphur Substances 0.000 claims description 30
- 229910052739 hydrogen Inorganic materials 0.000 claims description 21
- 239000001257 hydrogen Substances 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 15
- NAGJZTKCGNOGPW-UHFFFAOYSA-K dioxido-sulfanylidene-sulfido-$l^{5}-phosphane Chemical compound [O-]P([O-])([S-])=S NAGJZTKCGNOGPW-UHFFFAOYSA-K 0.000 claims description 13
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 12
- 125000001931 aliphatic group Chemical group 0.000 claims description 10
- 150000004867 thiadiazoles Chemical class 0.000 claims description 9
- 125000001118 alkylidene group Chemical group 0.000 claims description 5
- 239000003879 lubricant additive Substances 0.000 claims description 5
- 150000002431 hydrogen Chemical class 0.000 claims description 4
- 125000002298 terpene group Chemical group 0.000 claims description 4
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 3
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical group OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 2
- 150000004869 1,3,4-thiadiazoles Chemical class 0.000 claims 1
- MBBWTVUFIXOUBE-UHFFFAOYSA-L zinc;dicarbamodithioate Chemical compound [Zn+2].NC([S-])=S.NC([S-])=S MBBWTVUFIXOUBE-UHFFFAOYSA-L 0.000 claims 1
- 239000000314 lubricant Substances 0.000 abstract description 39
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 34
- 150000001875 compounds Chemical class 0.000 abstract description 30
- 239000011574 phosphorus Substances 0.000 abstract description 30
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 26
- 230000000996 additive effect Effects 0.000 abstract description 20
- 239000005078 molybdenum compound Substances 0.000 abstract description 8
- 150000002752 molybdenum compounds Chemical class 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 55
- 125000000217 alkyl group Chemical group 0.000 description 42
- 239000002253 acid Substances 0.000 description 33
- 239000003795 chemical substances by application Substances 0.000 description 29
- 150000001721 carbon Chemical group 0.000 description 27
- 239000003921 oil Substances 0.000 description 27
- 235000019198 oils Nutrition 0.000 description 27
- 150000003839 salts Chemical group 0.000 description 25
- 150000001412 amines Chemical class 0.000 description 24
- 239000003112 inhibitor Substances 0.000 description 19
- 239000000047 product Substances 0.000 description 18
- 230000003647 oxidation Effects 0.000 description 17
- 238000007254 oxidation reaction Methods 0.000 description 17
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 16
- 239000006185 dispersion Substances 0.000 description 16
- 238000002360 preparation method Methods 0.000 description 14
- 229910052751 metal Inorganic materials 0.000 description 13
- 239000002184 metal Substances 0.000 description 13
- 238000000034 method Methods 0.000 description 13
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 12
- 229910019142 PO4 Inorganic materials 0.000 description 11
- 238000005885 boration reaction Methods 0.000 description 11
- 239000003153 chemical reaction reagent Substances 0.000 description 11
- 235000021317 phosphate Nutrition 0.000 description 11
- 229920000768 polyamine Polymers 0.000 description 11
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 10
- 239000010452 phosphate Substances 0.000 description 10
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 9
- 239000002270 dispersing agent Substances 0.000 description 9
- 150000002632 lipids Chemical class 0.000 description 9
- 239000003607 modifier Substances 0.000 description 9
- 238000000746 purification Methods 0.000 description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 8
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 8
- 239000002199 base oil Substances 0.000 description 8
- 239000007795 chemical reaction product Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 230000000994 depressogenic effect Effects 0.000 description 6
- 235000014113 dietary fatty acids Nutrition 0.000 description 6
- 239000000194 fatty acid Substances 0.000 description 6
- 229930195729 fatty acid Natural products 0.000 description 6
- 150000002894 organic compounds Chemical class 0.000 description 6
- 150000002989 phenols Chemical class 0.000 description 6
- 229910052717 sulfur Inorganic materials 0.000 description 6
- 238000005299 abrasion Methods 0.000 description 5
- 125000003118 aryl group Chemical group 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- KZNICNPSHKQLFF-UHFFFAOYSA-N succinimide Chemical compound O=C1CCC(=O)N1 KZNICNPSHKQLFF-UHFFFAOYSA-N 0.000 description 5
- WMYJOZQKDZZHAC-UHFFFAOYSA-H trizinc;dioxido-sulfanylidene-sulfido-$l^{5}-phosphane Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([S-])=S.[O-]P([O-])([S-])=S WMYJOZQKDZZHAC-UHFFFAOYSA-H 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000011701 zinc Substances 0.000 description 5
- 229910052725 zinc Inorganic materials 0.000 description 5
- 229910000831 Steel Inorganic materials 0.000 description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 4
- 150000008431 aliphatic amides Chemical class 0.000 description 4
- 150000005690 diesters Chemical class 0.000 description 4
- 150000004665 fatty acids Chemical class 0.000 description 4
- 239000006260 foam Substances 0.000 description 4
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 4
- 239000010687 lubricating oil Substances 0.000 description 4
- 239000010705 motor oil Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 4
- 230000003449 preventive effect Effects 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 239000004034 viscosity adjusting agent Substances 0.000 description 4
- 150000003751 zinc Chemical class 0.000 description 4
- KGRVJHAUYBGFFP-UHFFFAOYSA-N 2,2'-Methylenebis(4-methyl-6-tert-butylphenol) Chemical compound CC(C)(C)C1=CC(C)=CC(CC=2C(=C(C=C(C)C=2)C(C)(C)C)O)=C1O KGRVJHAUYBGFFP-UHFFFAOYSA-N 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 150000001336 alkenes Chemical class 0.000 description 3
- 239000003963 antioxidant agent Substances 0.000 description 3
- 230000003078 antioxidant effect Effects 0.000 description 3
- 235000006708 antioxidants Nutrition 0.000 description 3
- 150000001491 aromatic compounds Chemical class 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 150000001639 boron compounds Chemical class 0.000 description 3
- 150000001733 carboxylic acid esters Chemical class 0.000 description 3
- NAGJZTKCGNOGPW-UHFFFAOYSA-N dithiophosphoric acid Chemical compound OP(O)(S)=S NAGJZTKCGNOGPW-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229960002317 succinimide Drugs 0.000 description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 3
- 125000006705 (C5-C7) cycloalkyl group Chemical group 0.000 description 2
- 0 *C(N1CCOB(O*)OCC1)=O Chemical compound *C(N1CCOB(O*)OCC1)=O 0.000 description 2
- PFEFOYRSMXVNEL-UHFFFAOYSA-N 2,4,6-tritert-butylphenol Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 PFEFOYRSMXVNEL-UHFFFAOYSA-N 0.000 description 2
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- 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 2
- OWYWGLHRNBIFJP-UHFFFAOYSA-N Ipazine Chemical compound CCN(CC)C1=NC(Cl)=NC(NC(C)C)=N1 OWYWGLHRNBIFJP-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- KEQFTVQCIQJIQW-UHFFFAOYSA-N N-Phenyl-2-naphthylamine Chemical compound C=1C=C2C=CC=CC2=CC=1NC1=CC=CC=C1 KEQFTVQCIQJIQW-UHFFFAOYSA-N 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- GNVMUORYQLCPJZ-UHFFFAOYSA-M Thiocarbamate Chemical compound NC([S-])=O GNVMUORYQLCPJZ-UHFFFAOYSA-M 0.000 description 2
- RYYWUUFWQRZTIU-UHFFFAOYSA-N Thiophosphoric acid Chemical compound OP(O)(S)=O RYYWUUFWQRZTIU-UHFFFAOYSA-N 0.000 description 2
- 150000008065 acid anhydrides Chemical class 0.000 description 2
- 150000001299 aldehydes Chemical class 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 150000001342 alkaline earth metals Chemical class 0.000 description 2
- 150000003973 alkyl amines Chemical class 0.000 description 2
- 230000002152 alkylating effect Effects 0.000 description 2
- 150000001408 amides Chemical class 0.000 description 2
- 239000002518 antifoaming agent Substances 0.000 description 2
- 150000004982 aromatic amines Chemical class 0.000 description 2
- 125000003710 aryl alkyl group Chemical group 0.000 description 2
- 229910052728 basic metal Inorganic materials 0.000 description 2
- 150000003818 basic metals Chemical class 0.000 description 2
- 235000010354 butylated hydroxytoluene Nutrition 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
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- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- PXJJSXABGXMUSU-UHFFFAOYSA-N disulfur dichloride Chemical compound ClSSCl PXJJSXABGXMUSU-UHFFFAOYSA-N 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- FKRCODPIKNYEAC-UHFFFAOYSA-N ethyl propionate Chemical compound CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 description 2
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- 125000005908 glyceryl ester group Chemical group 0.000 description 2
- 238000009775 high-speed stirring Methods 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 238000006703 hydration reaction Methods 0.000 description 2
- 125000001183 hydrocarbyl group Chemical group 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000002480 mineral oil Substances 0.000 description 2
- 235000010446 mineral oil Nutrition 0.000 description 2
- KHYKFSXXGRUKRE-UHFFFAOYSA-J molybdenum(4+) tetracarbamodithioate Chemical compound C(N)([S-])=S.[Mo+4].C(N)([S-])=S.C(N)([S-])=S.C(N)([S-])=S KHYKFSXXGRUKRE-UHFFFAOYSA-J 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 150000002903 organophosphorus compounds Chemical class 0.000 description 2
- 150000002931 p-cresols Chemical class 0.000 description 2
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N pentanoic acid group Chemical group C(CCCC)(=O)O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-M phenolate Chemical compound [O-]C1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-M 0.000 description 2
- 229940031826 phenolate Drugs 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 2
- 229920001281 polyalkylene Polymers 0.000 description 2
- 229920000098 polyolefin Polymers 0.000 description 2
- 150000003141 primary amines Chemical class 0.000 description 2
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- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000001384 succinic acid Substances 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 230000006209 tert-butylation Effects 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
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- 229910000165 zinc phosphate Inorganic materials 0.000 description 2
- CFQZKFWQLAHGSL-FNTYJUCDSA-N (3e,5e,7e,9e,11e,13e,15e,17e)-18-[(3e,5e,7e,9e,11e,13e,15e,17e)-18-[(3e,5e,7e,9e,11e,13e,15e)-octadeca-3,5,7,9,11,13,15,17-octaenoyl]oxyoctadeca-3,5,7,9,11,13,15,17-octaenoyl]oxyoctadeca-3,5,7,9,11,13,15,17-octaenoic acid Chemical compound OC(=O)C\C=C\C=C\C=C\C=C\C=C\C=C\C=C\C=C\OC(=O)C\C=C\C=C\C=C\C=C\C=C\C=C\C=C\C=C\OC(=O)C\C=C\C=C\C=C\C=C\C=C\C=C\C=C\C=C CFQZKFWQLAHGSL-FNTYJUCDSA-N 0.000 description 1
- YJTKZCDBKVTVBY-UHFFFAOYSA-N 1,3-Diphenylbenzene Chemical group C1=CC=CC=C1C1=CC=CC(C=2C=CC=CC=2)=C1 YJTKZCDBKVTVBY-UHFFFAOYSA-N 0.000 description 1
- LDVVTQMJQSCDMK-UHFFFAOYSA-N 1,3-dihydroxypropan-2-yl formate Chemical compound OCC(CO)OC=O LDVVTQMJQSCDMK-UHFFFAOYSA-N 0.000 description 1
- YSQZSPCQDXHJDJ-UHFFFAOYSA-N 1-(pentyldisulfanyl)pentane Chemical compound CCCCCSSCCCCC YSQZSPCQDXHJDJ-UHFFFAOYSA-N 0.000 description 1
- NSOAQRMLVFRWIT-UHFFFAOYSA-N 1-ethenoxydecane Chemical class CCCCCCCCCCOC=C NSOAQRMLVFRWIT-UHFFFAOYSA-N 0.000 description 1
- OPLCSTZDXXUYDU-UHFFFAOYSA-N 2,4-dimethyl-6-tert-butylphenol Chemical compound CC1=CC(C)=C(O)C(C(C)(C)C)=C1 OPLCSTZDXXUYDU-UHFFFAOYSA-N 0.000 description 1
- DKCPKDPYUFEZCP-UHFFFAOYSA-N 2,6-di-tert-butylphenol Chemical compound CC(C)(C)C1=CC=CC(C(C)(C)C)=C1O DKCPKDPYUFEZCP-UHFFFAOYSA-N 0.000 description 1
- BXXRINAXUZZBNJ-UHFFFAOYSA-N 2-methyl-6-(2-phenylethenyl)phenol Chemical compound CC1=CC=CC(C=CC=2C=CC=CC=2)=C1O BXXRINAXUZZBNJ-UHFFFAOYSA-N 0.000 description 1
- WJQOZHYUIDYNHM-UHFFFAOYSA-N 2-tert-Butylphenol Chemical compound CC(C)(C)C1=CC=CC=C1O WJQOZHYUIDYNHM-UHFFFAOYSA-N 0.000 description 1
- BKZXZGWHTRCFPX-UHFFFAOYSA-N 2-tert-butyl-6-methylphenol Chemical compound CC1=CC=CC(C(C)(C)C)=C1O BKZXZGWHTRCFPX-UHFFFAOYSA-N 0.000 description 1
- MDWVSAYEQPLWMX-UHFFFAOYSA-N 4,4'-Methylenebis(2,6-di-tert-butylphenol) Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 MDWVSAYEQPLWMX-UHFFFAOYSA-N 0.000 description 1
- VHYFNPMBLIVWCW-UHFFFAOYSA-N 4-Dimethylaminopyridine Chemical compound CN(C)C1=CC=NC=C1 VHYFNPMBLIVWCW-UHFFFAOYSA-N 0.000 description 1
- DSIUZBLIPJBAMZ-UHFFFAOYSA-N 8-methyl-octadecanoic acid Chemical compound CCCCCCCCCCC(C)CCCCCCC(O)=O DSIUZBLIPJBAMZ-UHFFFAOYSA-N 0.000 description 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- 235000017060 Arachis glabrata Nutrition 0.000 description 1
- 244000105624 Arachis hypogaea Species 0.000 description 1
- 235000010777 Arachis hypogaea Nutrition 0.000 description 1
- 235000018262 Arachis monticola Nutrition 0.000 description 1
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- KXDHJXZQYSOELW-UHFFFAOYSA-N Carbamic acid Chemical compound NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 1
- 102100039496 Choline transporter-like protein 4 Human genes 0.000 description 1
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
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Abstract
为润滑剂组合物提供抗磨特性的添加剂，该添加剂基于(1)有机硼酸酯组合物与(2)一种或多种含硫或含磷化合物或非-硫钼化合物的组合。所述含硫或含磷化合物为二硫代氨基甲酸盐、双二硫代氨基甲酸酯、1，3，4-噻二唑、二硫代磷酸盐、二硫代磷酸酯，而所述钼化合物可通过下列材料的反应来制备：(a)约1.0mol具有12个或更多碳原子的脂肪油，(b)约1.0mol到约2.5mol的二乙醇胺和(c)钼源。
Description
说明书
技术背景
本发明涉及提供抗磨和抗刮伤特性的低磷含量的润滑剂组合物。本发明的另一方面在于降低了润滑剂组合物中硫和/或磷的量，或将磷从其中完全去除，以提供不希望含有高含量的硫和/或磷的润滑剂。
近年来润滑剂技术的发展趋势(特别是对于客车发动机润滑油)是降低润滑油中来自称为二烷基二硫代磷酸锌(ZDDP)的抗磨添加剂的磷水平。目前发动机润滑油中磷水平设定在0.10％P，而研究者正致力于将此水平降低至0.08％或0.05％P，并最终将磷全部消除。问题在于以合理的成本保持在润滑油中有充分的抗磨保护。人们关心发动机润滑油中的磷对催化式排气净化器的毒性作用。同样地，研究者致力于全面降低发动机润滑油中存在的硫，既是出于环境的考虑又是由于硫的腐蚀作用。由于目前普遍使用含硫化合物作为抗磨添加剂，因此非常需要降低获得有效抗磨保护时所需的此类化合物的量。
已知在美国专利第4,389,322号中公开了某些具有抗磨特性和其它所需润滑性能的硼酸酯组合物，本文将其引入作为参考。
美国专利第5,641,731号和公开号为2003/0119682号的美国专利申请教导了包括如下组分的7-组分润滑剂添加剂：油溶性钼添加剂、二硫代磷酸锌、无水PTFE(聚四氟乙烯)、聚-α-烯烃、二酯、粘度指数改进剂和硼酸酯组合物。测试了作为特定钼组分的无-硫855有机钼氨配合物，并指出二硫代氨基甲酸钼也是可能的添加剂。所述参考文献涉及意图同时提高多种性能的综合配方，抗磨保护只是其中之一。尽管该专利权人报道了在抗磨性能方面的改进，但二硫代磷酸锌的用量在很高的水平。因此，含有包括二硫代磷酸锌在内的化合物的分散剂抑制剂具有约占1％质量比的磷组分。依照所述参考文献教导，分散剂抑制剂的加入量在约11％体积比(约12.3％质量比)的水平，则润滑剂中的磷水平约为0.1％质量比。因此，如此高的磷水平致使此配方不适于新的GF-4要求。
我们意外地发现有机硼酸酯组合物与某些有机硫、有机磷和非-硫钼化合物结合时产生协同抗磨作用，其结果是使用较少量的这些化合物就可保持或增强其在润滑剂性能水平中的功效。将少量的具有低硼含量的硼酸酯组合物与这些添加剂结合使用能够大幅提高已知抗磨添加剂的性能。与硼酸酯组合物结合显示协同作用的添加剂包括诸如二烷基二硫代磷酸锌(ZDDP)的二硫代磷酸盐、诸如二硫代氨基甲酸钼和无灰二硫代氨基甲酸盐的二硫代氨基甲酸盐、噻二唑和诸如润滑剂添加剂的非-硫钼氨化物配合物。我们意外地发现当在润滑剂中使用组合的添加剂时在金属表面形成坚韧的膜，且此类膜使上面列举的不同类型的抗磨化合物的性能增强。
对于二硫代磷酸盐化合物，其优点在于在保持必要的性能的同时可大大降低磷的含量(至远低于0.05％质量比)。此外，鉴于新的GF-4规范将限定允许的硫含量，其优点还在于能够降低在抗磨添加剂中总的硫使用量。本申请人发现的两组分体系的组合物以较少量的硫化合物(及在使用二硫代磷酸盐(酯)的情况下以较少量的磷)提供优良的性能，从而使润滑剂整体含有较少的硫(和/或磷)。至于诸如钼氨化物配合物
添加剂的非-硫钼化合物，由于将较少量的添加剂与有机硼酸酯组合物结合使用，可降低抗磨保护的成本。
发明内容
本发明提供了协同抗磨组合物，包括：
(1)有机硼酸酯组合物；及
(2)有机硫或有机磷化合物、无-硫-钼化合物或其混合物，选自：
(i)如式(I)所示的1，3，4-噻二唑化合物：
其中，R和R1独立地选自氢和C8-12硫代烷基或氢、C1-22烷基基团、萜残基及如下式所示的马来酸残基：
及R2和R3表示C1-22烷基和C5-7环烷基，R或R1以及R2和R3两者之一可为氢；
(ii)如式(II)所示的双二硫代氨基甲酸酯：
其中R4、R5、R6和R7为具有1到13个碳原子的脂肪烃基，并且R8为具有1到8个碳原子的亚烷基；
(iii)如式(III)所示的二硫代氨基甲酸盐：
其中R9和R10表示具有1到8个碳原子的烷基，M表示元素周期表中第IIA、IIIA、VA、VIA、IB、IIB、VIB、VIII族的金属及由下式的胺形成的盐部分：
R11、R12和R13独立地选自氢和具有1到18个碳原子的脂肪族基团，而n为M的价态；
或如示(IV)所示：
X＝S或O
其中R4、R5、R6和R7为具有1到13个碳原子的脂肪烃基基团；
(iv)如式(V)所示的二硫代磷酸盐：
其中X1和X2独立地选自S和O，R14和R15表示氢和具有1到22个碳原子的烷基，M代表元素周期表中第IIA、IIIA、VA、VIA、IB、IIB、VIB、VIII族的金属，及由下式的胺形成的盐部分：
R16、R17和R18独立地选自氢和具有1到18个碳原子的脂肪族基团，且n为M的价态；及
(v)如示(VI)所示的二硫代磷酸酯：
其中R19、R20、R21和R22可以相同或不同，且选自具有1到8个碳原子的烷基基团；
(iv)非-硫钼添加剂(non-sulfur molybdenum additive)，其通过美国专利第4,889,647号(本文将其引入作为参考)所述的缩合方法将脂肪油、二乙醇胺和含钼原料顺序反应来制备，认为其含有以下成分：
其中R’为脂肪油残基。在一个实施方案中，所述的非-硫钼添加剂可通过用下列物质进行反应来制备：(a)约1.0mol具有12个或更多碳原子的脂肪油，(b)约1.0mol到2.5mol的二乙醇胺和(c)钼源。
本发明的另一个实施方案涉及具有增强的润滑特性的润滑剂组合物，其包含作为主要成分的润滑粘度的油和约0.1％到约10.0％质量比(基于该润滑剂组合物总重量)的包括(1)有机硼酸酯组合物和(2)式I、II、III、IV、V、VI、VII的有机化合物或其混合物。此润滑剂组合物的一个实施方案包括约0.5％到约3.0％质量比(基于该润滑剂总质量)的包括(1)有机硼酸酯组合物和(2)式I、II、III、IV、V、VI、VII的有机化合物或其混合物。
附图的简要说明
图1所示为通过ASTM D5707评价的非-硫钼氨配合物与有机硼酸酯组合物的摩擦降低结果。
图2所示为通过ASTM D5707评价的噻二唑与有机硼酸酯组合物的摩擦降低结果。
图3所示为通过ASTM D5707评价的二硫代磷酸锌与有机硼酸酯组合物的摩擦降低结果。
发明的详细说明
本发明的有机硼酸酯组合物包括用硼酸处理的和未用硼酸处理的化合物。研究者认为硼酸酯组合物中硼酸处理的和未用硼酸处理的化合物在所述协同组合物中同样起到重要的作用。优选的硼酸酯组合物是通过将约1mol脂肪油与约1.0到2.5mol二乙醇胺反应，随后与硼酸反应得到的含约0.1％到3％质量比的硼的反应产物。研究者认为该反应产物可以包括以下两种主要组分中的一种或两种，当该反应朝充分水合的方向进行时，其它所列出的组分也是可能的组分：
和/或
其中R1＝H或CxHy，其中x＝1-60，而y＝3-121
其中Y表示脂肪油残基。优选的脂肪油为含有至少12个碳原子且可含有22个碳原子或更多的高级脂肪酸甘油酯。此类酯为公知的植物或动物油。特别适用的植物油为源自椰子、谷类、棉籽、亚麻子、花生、大豆和向日葵籽的油。类似地，可以使用诸如牛油的动物脂肪油。
硼的来源是硼酸或可提供硼并能与脂肪油和二乙醇胺的反应中间产物反应形成硼酸酯组合物的物质。
尽管上文特别描述了上述有机硼酸酯组合物，可以理解，其它有机硼酸酯组合物(如本文引入作为参考的公开号为2003/0119682的美国专利申请中所述的)也具有与本发明效果类似的功能。此外，诸如硼酸钾的硼酸盐分散体也是适用的。
如下文详细描述的，本发明的润滑剂添加剂包括与诸如上述组分(i)到(vi)的含硫化合物或非-硫钼化合物结合的有机硼酸酯化合物。
上述这些无硼化合物已知具有某些润滑特性，如在各种润滑介质中的抗氧化、抗磨和抗腐蚀特性。然而，有时单独的硫化合物不能为许多工业上的多种重要应用和机动车润滑剂提供充分的抗磨保护。
此外，在某些情况下，高浓度的硫化合物可能对润滑剂的整体性能产生负面影响。例如，所谓的硫供体可能在某些受防护的表面或催化式排气净化器上产生大量的不需要的硫化合物。
对于所述的非-硫钼化合物(vi)，希望提高其已经很优良的抗磨特性和摩擦降低特性。
当与硼酸酯组合物以某种比例结合时，上述硫化合物和非-硫钼化合物意外地产生协同抗磨作用。该硼酸酯协同作用表现出更高的抗磨特性。
此外，本领域所属技术人员可以理解，用于实现本发明目的的上述两种协同抗磨组分的完全配方的组合物可包括一种或多种如下物质：
(1)经硼酸处理的和/或未经硼酸处理的分散剂，(2)抗氧剂，(3)密封件膨胀(seal swell)组合物，(4)摩擦改进剂，(5)极压/抗磨剂，(6)粘度调节剂，(7)倾点降低剂，(8)清净剂，(9)抗泡沫剂(antifoamants)。
1.经硼酸处理的和/或未经硼酸处理的分散剂。可向最终的流体组合物中加入包括接近无油基底的10％质量比的量的未经硼酸处理的无灰分散剂。下文列举的许多类型的无灰分散剂是本领域所公知的。也可包括经硼酸处理的无灰分散剂。
(a)“羧基分散剂”是含有至少约34个碳原子优选至少约54个碳原子的羧基酰化试剂(酸、酸酐、酯等)与含氮化合物(如胺)、含羟基的有机化合物(例如包括单羟基和多羟基醇的脂肪族化合物，或包括酚和萘酚的芳香族化合物)和/或碱性无机材料反应的产物。此类反应产物包括羧基酰化试剂的酰亚胺、酰胺及酯类反应产物。此类材料的例子包括琥珀酰亚胺分散剂和羧酸酯分散剂。
所述羧基酰化试剂包括烷基琥珀酸和烷基琥珀酸酐，其中所述烷基基团为polybutyl部分、脂肪酸、异脂肪酸(如8-甲基-十八酸)、二聚酸、加和二羧酸(不饱和脂肪酸与不饱和羧基试剂的加和(4+2和2+2)产物)、三聚酸、加和三羧酸(如 和
)和烃基取代的羧基酰化试剂(源自烯烃和/或多聚烯烃)。在一个实施方案中，所述羧基酰化试剂为脂肪酸。脂肪酸通常包括约8至约30个碳，或约12至约24个碳。在美国专利第2,444,328、3,219,666和4,234,435号中教导了羧基酰化试剂，本文将其引入作为参考。
所述胺可以是单胺或多元胺。所述单胺通常具有至少一个含有1到约24个碳原子的烃基基团，具有1到约12个碳原子。单胺的例子包括脂肪胺(C8-30)、一级醚胺(
胺)、三级脂肪族基伯胺(“Primene”)、羟基胺(一级、二级或三级烷醇胺)、醚N-(羟基烃基)胺和羟基烃基胺(“Ethomees”和“Propomeens”)。所述多元胺包括烷氧基化的二胺(Ethoduomeens)、脂肪二胺(“Duomeens”)、亚烷基多元胺(亚乙基多元胺)、含羟基的多元胺、聚氧化亚烷基多元胺(Jeffamines)、缩合多元胺(在至少一种羟基化合物与至少一种含有至少一个伯氨基或仲氨基基团的多元胺反应物之间进行的缩合反应)，和杂环多元胺。有用的胺包括在美国专利第4,234,435号和第5,230,714号中公开的胺，本文将其引入作为参考。
这些“羧基分散剂”的例子如英国专利第1,306,529号和许多美国专利包括：第3,219,666；3,316,177；3,340,281；3,351,552；3,381,022；3,433,744；3,444,170；3,467,668；3,501,405；3,542,680；3,576,743；3,632,511；4,234,435号和Re 26,433中所述，本文将其引入作为参考。
(b)“胺分散剂”为相对高分子量的脂肪族卤化物或脂环族卤化物与胺(优选为聚亚烷基多元胺)反应的产物。其例子在以下美国专利中公开：美国专利第3,275,554；3,438,757；3,454,555和3,565,804号，本文将其引入作为参考。
(c)“Mannich分散剂”为烷基部分含有至少约30个碳原子的烷基酚与醛(特别是甲醛)和胺(特别是聚亚烷基多元胺)反应的产物。所述物质在以下美国专利中进行了说明性的描述：美国专利第3,036,003；3,236,770；3,414,347；3,448,047；3,461,172；3,539,633；3,586,629；3,591,598；3,634,515；3,725,480；3,726,882和3,980,569号，本文将其引入作为参考。
(d)处理后的分散剂是通过将羧基分散剂、胺分散剂或Mannich分散剂与诸如尿素、硫脲、二硫化碳、醛、酮、羧酸、烃基取代的琥珀酸酐、腈、环氧化物、硼化合物、磷化合物等等的试剂反应获得的。示例性的此类物质在以下美国专利中进行了描述：美国专利第3,200,107；3,282,955；3.367,943；3,513,093；3,639,242；3,649,659；3,442,808；3,455,832；3,579,450；3,600,372；3,702,757；和3,708,422号，本文将其引入作为参考。
(e)聚合物分散剂为诸如甲基丙烯酸癸酯、乙烯基癸基醚的高分子量的烯烃的油溶性单体与具有极性取代基的单体(例如丙烯酸氨基烷基酯或丙烯酰胺和聚-氧乙烯基取代的丙烯酸酯)的互聚物。聚合物分散剂的例子在以下美国专利中进行了描述：美国专利第3,329,658；3,449,250；3,519,656；3,666,730；3,687,849和3,702,300号，本文将其引入作为参考。
硼酸化的分散剂在美国专利第3,087,936和3,254,025号中进行了描述，本文将其引入作为参考。
能够作为分散剂添加剂的物质还包括在美国专利第5,198,133和4,857,214号中公开的物质，本文将其引入作为参考。这些专利中的所述分散剂与如下反应产物进行比较：烯基琥珀酰亚胺或琥珀酰亚胺无灰分散剂与含磷酯，或与无机含磷酸或酸酐以及硼化合物的反应产物。
2.抗氧剂。多数油质组合物优选包括常规量的一种或多种抗氧剂以防止组合物在空气中(特别是高温下)过早降解。典型的抗氧剂包括位阻酚性抗氧剂、二级芳香胺抗氧剂、硫化的酚抗氧剂、油溶性铜化合物、含磷抗氧剂、有机硫化物、二硫化物和多硫化物等等。
示例性的空间位阻酚性抗氧剂包括诸如2，6-二叔丁基酚、4-甲基-2，6-二叔丁基酚、2，4，6-三叔丁基酚、2-叔丁基酚、2，6-二异丙基酚、2-甲基-6-叔丁基酚、2，4-二甲基-6-叔丁基酚、4-(N，N-二甲基氨基甲基)-2，8-二叔丁基酚、4-甲基-2，6-二叔丁基酚、2-甲基-6-苯乙烯基酚、2，6-二苯乙烯基-4-壬基酚的邻位烷基化的酚类化合物及其类似物或同系物。两种或多种此类单环酚类化合物的混合物也是适用的。
其它本发明组合物优选使用的酚类抗氧剂为亚甲基桥联的烷基酚，其可单独使用或相互结合使用，或与空间位阻的非桥联酚类化合物结合使用。示例性的亚甲基桥联的化合物包括4，4’-亚甲基双(6-叔丁基-邻-甲酚)、4，4’-亚甲基双(2-叔戊基-邻-甲酚)、2，2’-亚甲基双(4-甲基-6-叔丁基酚)、4，4’-亚甲基双(2，6-二叔丁基酚)及类似的化合物。特别优选为诸如美国专利第3,211,652中(本文将其全文引入作为参考)所述的亚甲基桥联的烷基酚的混合物。
本发明组合物中也使用胺抗氧剂，特别是油溶性芳香仲胺。尽管一元芳香仲胺是优选的，多元芳香仲胺也可适用。示例性的一元芳香仲胺包括二苯胺、含有一个或两个烷基取代基且每个烷基具有最多约16个碳原子的烷基二苯胺、苯基-t-萘胺、苯基-β-萘胺、包括一个或两个烷基或芳烷基基团且每个基团具有最多约16个碳原子的烷基或芳烷基取代的苯基-β-萘基胺、包括一个或两个烷基或芳烷基基团且每个基团具有最多约16个碳原子的烷基或芳烷基取代的苯基-p-萘基胺及类似的化合物。
一类优选的芳香胺抗氧剂为烷基化的二苯胺，其具有如下通式：
R23-(C6H4)-NH-(C6H4)-R24
其中R23为具有8到12个碳原子(更优选8或9个碳原子)的烷基基团(优选为支链烷基)，且R24为氢原子、烷基芳基或含8到12个碳原子(更优选8或9个碳原子)的烷基基团(优选为支链烷基)。优选的化合物可以通过商业渠道获得，如Crompton Corporation制造的
438L、640和680。其它可通过商业渠道获得的芳香胺抗氧剂包括R.T.VanderbiltCompany，Inc.销售的
SL、DND、NA、81、961和2005。本发明组合物优选包括的其它适用类型的抗氧剂是由一种或多种液态的部分硫化的酚化合物构成，所述部分硫化的酚化合物例如通过将一氯化硫与酚的液体混合物(该酚混合物的至少约50％质量比由一种或多种具有反应活性的位阻酚构成)反应制备得到的液体产物，其中反应物比例为每摩尔具有反应活性的位阻酚对应约0.3到约0.7克原子的一氯化硫。用于制备此类液体产物组合物的典型的酚混合物包括含有约75％质量比的2，6-二叔丁基酚、约10％质量比的2-二叔丁基酚、约13％质量比的2，4，6-三叔丁基酚和约2％质量比的2，4-二叔丁基酚的混合物。该反应为放热反应，因此优选保持在约15℃到约70℃范围，更优选在约40℃到约60℃之间。
也可以使用不同抗氧剂的混合物。一种适合的混合物由以下物质的组合物构成：(i)至少三种不同的空间位阻的叔丁基化单羟基酚的油溶性混合物，其在25℃为液态，(ii)至少三种不同的空间位阻的叔丁基化亚甲基桥联的多元酚的油溶性混合物，及(iii)至少一种双(4-烷基苯基)胺，其中所述烷基基团为含有8到12个碳原子的支链烷基基团，其中(i)、(ii)和(iii)的质量比例为每份质量的组分(iii)对应3.5到5.0份的组分(i)和0.9到1.2份的组分(ii)。以上论述的抗氧剂如美国专利第5,328,619号中所述，本文将其引入作为参考。
其它适用的优选抗氧剂如美国专利第4,031,023号中所公开的，本文将其引入作为参考。所参考的第4,031,023号专利所述的抗氧剂如下面修订的通式所示：
其中R25为烃基或含有最多约30个碳原子并具有a+e化合价的取代烃基；R26和R27独立地选自氢和含最多约20个碳原子的以烃基为基础的基团；b和c独立地选自从2到5；d为从0到5；a为从0到4及e为从1到5，同时满足a+e为1到6，其具有增强的抗氧化降解和抗磨特性。所述组合物中优选包括的抗氧剂的量为约0.1-5％质量比。
3.密封件膨胀组合物。具有保持密封件弹性的组合物也是本领域所公知的。优选的密封件膨胀组合物为异癸基四氢噻吩砜。所述封闭件膨胀剂优选以约0.1-3％质量比混入所述组合物中。在美国专利第4,029,587号中公开了取代的3-烷氧基四氢噻吩砜，本文将其引入作为参考。
4.摩擦调节剂。摩擦调节剂也是本领域所属技术人员所公知的。在美国专利第4,792,410号中包括了适用的摩擦调节剂的列表，本文将其引入作为参考。美国专利第5,110,488号中公开了脂肪酸的金属盐(特别是锌盐)，本文将其引入作为上述公开的参考。所述摩擦调节剂列表包括脂肪亚磷酸盐、脂肪酸酰胺、脂肪族环氧化物、经硼酸处理的脂肪族环氧化物、脂肪胺、甘油酯、经硼酸处理的甘油酯、烷氧基化的脂肪胺、经硼酸处理的烷氧基化的脂肪胺、脂肪酸的金属盐、硫化烯烃、脂肪族咪唑啉及其混合物。
优选的摩擦调节剂是经硼酸处理的脂肪族环氧化物，如上所述根据其硼含量将其加入。摩擦调节剂优选在组合物中具有0.1-10％质量比，且可以是单一的摩擦调节剂或两种或多种的混合物。
摩擦调节剂还包括脂肪酸金属盐。优选的阳离子为锌、镁、钙和钠以及任何其它可使用的碱金属或碱土金属。可通过使每当量胺包含过量的阳离子使所述盐过碱化(overbased)。其后用二氧化碳处理该过量的阳离子从而形成碳酸盐。所述金属盐是通过将适合的盐与酸反应形成盐来制备的，当适当时，向上述反应混合物中加入二氧化碳以使任何超过成盐所需量的阳离子形成碳酸盐。优选的摩擦调节剂为油酸锌。
5.抗磨/极压剂。以下为已知可提供抗磨和/或极压特性的可供选择的添加剂。某些此类添加剂(包括下列的5(i)和5(iv))因为可与硼酸酯结合产生协同作用因而也构成本发明的一部分。如实验数据所示，所要求保护的组合物具有的性能远超过单独使用此类添加剂所获得的性能。然而，本领域所属技术人员可选择利用一种或多种此类添加剂与所要求保护的组合物一起使用。
(i)以下结构式所示的二烷基二硫代磷酸酯琥珀酸酯
其中R19、R20、R21和R22独立地选自具有3到8个碳原子的烷基基团(以VANLUBE 7611M名称，从R.T.Vanderbilt Co.，Inc.通过商业渠道获得)，
(ii)下式所示的二硫代磷酸酯羧酸酯
其中，R28和R29为具有3到8个碳原子的烷基，及R30为具有2到8个碳原子的烷基(可以Irgalube 63名称从Ciba Geigy Corp.公司通过商业渠道获得)，及
(iii)下式所示的三苯基硫代磷酸酯
其中f＝1-2，m＝2-3，R31为具有1到20个碳原子的烷基，R32、R33和R34独立地选自氢或烷基基团(可以TPPT名称从Ciba Geigy Corp.通过商业渠道获得)；
(iv)亚甲基双(二烷基二硫代氨基甲酸酯)其中所述烷基基团含有4到8个碳原子(可以VANLUBE 7723名称从R.T.Vanderbilt Co.，Inc.通过商业渠道获得)。
(v)含磷酸。所述润滑剂组合物还优选包括至少一种含磷酸、含磷酸盐、含磷酸酯或其衍生物(包括含硫类似物)，优选含量为0.002-1.0％质量比。所述含磷酸、含磷酸盐、含磷酸酯或其衍生物包括选自含磷酸酯或其盐、亚磷酸盐、含磷酰胺、含磷羧酸或羧酸酯、含磷醚或其混合物的化合物。
在一个实施方案中，所述含磷酸、含磷酸酯或其衍生物可以是含磷酸、含磷酸酯、含磷酸盐或其衍生物。所述含磷酸包括磷酸、膦酸、次膦酸，以及硫代磷酸(包括二硫代磷酸和一硫代磷酸、硫代次膦酸和硫代膦酸)。
(vi)另一类对于本发明有用的化合物为羧酸酯的二硫代磷酸酯。优选为具有2到8个碳原子的烷基酯，例如3-[[双(1-甲基乙氧基)硫膦基]硫]丙酸乙基酯。
(vii)优选的磷化合物是如下式所示的二烷基磷酸一烷基伯胺盐
其中R35、R36和R37独立地为氢或烷基(烃基)基团。在美国专利第5,354,484号中描述了此类化合物，本文将其引入作为参考。85％的磷酸是加入所述完整配方的ATF包(package)的优选化合物，且优选以基于ATF质量的0.01-0.3％质量比的水平加入。磷酸烷基酯的协同胺盐是通过已知方法制备的，例如美国专利第4,130,494号所述的方法，本文将其引入作为参考。将适合的磷酸单酯或二酯或其混合物用胺中和。当使用单酯时，需要2摩尔的胺，而二酯需要1摩尔的胺。在任何情况下，可通过控制反应的中性点(即总酸量与总碱量基本相等)来控制所需胺的量。可选择地，可将诸如氨或亚乙基二胺的中和试剂加入上述反应中。
优选的磷酸酯为脂肪族酯，其中包括2-乙基己基、n-辛基和己基的单酯或二酯。所述胺可选自伯胺或仲胺。特别优选为具有10到24个碳原子的叔-烷基胺。这些胺是可通过商业渠道获得的，例如由Rohm and Haas Co.制造的
81R。
加入润滑剂组合物中的锌盐的优选量为0.1-5％质量比以提供抗磨保护。该锌盐优选以二硫代磷酸或二硫代氨基甲酸的锌盐加入。优选的化合物为二异辛基二硫代磷酸锌和二苄基二硫代磷酸锌和戊基二硫代氨基甲酸。润滑剂组合物中还可以与所述锌盐相似的量加入用来提供抗磨/极压性能的氢亚磷酸二丁酯(DBPH)和一硫代磷酸三苯酯，以及通过二丁基胺-二硫化碳和丙烯酸甲酯反应形成的硫代氨基甲酸酯。所述的硫代氨基甲酸酯在美国专利第4,758,362号中有描述，而所述的含磷金属盐在美国专利第4,466,894号中有描述，两项专利在本文中引入作为参考。
也可使用锑盐或铅盐作为极压剂。优选的盐为二硫代氨基甲酸的盐，如二戊基二硫代氨基甲酸锑。
6.粘度调节剂。粘度调节剂(VM)和分散剂粘度调节剂(DVM)是公知的。VM和DVM的例子为聚异丁烯酸酯、聚丙烯酸酯、聚烯烃、苯乙烯-马来酸酯共聚物，以及类似的聚合物包括均聚物、共聚物和接枝共聚物。
商业上可获得的VM、DVM及其化学型在下表中列出。DVM在其数字后标有(D)。
粘度调节剂的近期综述见美国专利第5,157,088、5,256,752和5,395,539号，本文将其引入作为本发明相关公开内容的参考。VM和/或DVM优选以接近10％质量比的水平加入所述完整配方的组合物中。
7.倾点降低剂。此组分特别有利于提高润滑油的低温质量。优选的倾点降低剂为烷基萘。在美国专利第4,880,553和4,753,745号中描述了倾点降低剂，本文将其引入作为参考。PPD通常用于润滑剂组合物以降低在低温和低剪切速率下测量的粘度。所述倾点降低剂优选的使用范围在0.1-5％质量比。用于评价润滑液体的低温低剪切速率流变学的测试的例子包括ASTM D97(倾点)，ASTM D2983(布氏粘度(Brookfieldviscosity))，D4684(小型旋转粘度计(Mini-rotary Viscometer))和D5133(布氏扫描仪(Scanning Brookfield))。
商业上可获得的倾点降低剂及其化学型的例子为：
8.清净剂。在许多情况下润滑剂组合物还优选包括清净剂。本发明所使用的清净剂优选为有机酸的金属盐。所述清净剂的有机酸部分优选为磺酸盐、羧酸盐、苯酚盐、水杨酸盐。所述清净剂的金属部分优选为碱金属或碱土金属。优选的金属为钠、钙、钾和镁。所述清净剂优选为过碱性的，即金属的量超过形成中性金属盐所需的化学计量。
优选的过碱性有机盐为具有充分亲脂性的由有机原料形成的磺酸盐。有机磺酸盐在润滑剂和清净剂领域是公知的。所述磺酸盐化合物优选平均含有约10到约40个碳原子，更优选含有约12到约36个碳原子，最优选含有约14到约32个碳原子。类似地，所述的苯酚盐、oxylates(草酸盐)和羧酸盐优选具有充分亲脂性。
尽管本发明允许碳原子既可以是芳香结构，也可以是链烷烃结构，但更优选使用烷基化的芳香结构。尽管可以采用以萘为基础的物质，但优选的芳香部分为苯部分。
因此最优选的组分为过碱性的单磺化的烷基化苯，且优选为单烷基化的苯。优选地，烷基苯部分从釜底原料(still bottom source)获得，且为单烷基化的或二烷基化的。在本发明中，研究者认为单烷基化的芳香化合物在整体性能上高于二烷基化的芳香化合物。
在本发明中优选利用单烷基化的芳香化合物(苯)的混合物来获得单烷基化的盐(苯磺酸盐)。在所述混合物中，所述组合物的主要部分含有丙烯聚合物作为烷基基团的来源，其有助于盐的溶解性。使用单官能团(如单磺酸盐)物质可避免分子间的交联从而减少盐从润滑剂中沉淀。
所述盐优选为“过碱性”的。过碱性指盐中金属的量超过中和阴离子所需的化学计量值。由过碱性带来的过量金属具有中和润滑剂中可能产生的酸的作用。第二个优点是过碱性的盐增加摩擦的动力学系数。优选地，所述过量的金属在等当量基础上与中和所述酸所需量的比例最高约30∶1，优选为5∶1到18∶1。
所述组合物中所用的过碱性盐的量优选为无油成分的约0.1％到约10％质量比。所述过碱性盐通常在50％的油中(基于无油成分TBN范围为10-600)配制。在美国专利第5,403,501和4,792,410号中公开了经硼酸处理的和未经硼酸处理的清净剂，其在本文中引入作为本发明相关公开内容的参考。
9.抗泡沫剂。如硅氧烷或氟硅氧烷组合物的抗泡沫剂是本领域所公知的。这类抗泡沫试剂可从Dow Corning Chemical Corporation和UnionCarbide Corporation获得。优选的氟硅氧烷抗泡沫产品为Dow FS-1265。优选的硅氧烷抗泡沫产品为Dow Corning DC-200和Union CarbideUC-L45。其它可单独或以混合物形式包含在所述组合物中的抗泡沫试剂为从Nitro，West Virginia的Monsanto Polymer Products Co.以PC-1244名称获得的产品。此外还可包括从Farmington Hills，Michigan的OSISpecialties，Inc.获得的硅氧烷聚醚共聚物抗泡沫剂。此类物质中的一种以SILWET-L-7220名称出售。本发明组合物中所包含的抗泡沫产品的量优选为活性成分的百万分之5-80(基于无油成分)。
可以用已知方法将所述协同组合物加入任何润滑介质中。所述组合物可增强天然及合成的油类或脂类配方的润滑剂的抗磨和极压特性。
用作润滑剂载体的基础油为用于机动车和工业应用的常用天然和合成油类(API基础库存目录I，II，III，IV，V组)，除其它外例如透平油、液压油、齿轮油、曲轴箱用油和柴油。天然基础油包括矿物油、石油、石蜡油和符合生态学的植物油。典型的合成油类包括诸如硅酸酯和季戊四醇酯的酯类油、氢化矿物油、硅氧烷和硅烷。
本发明的添加剂组合物包括(a)有机硼酸酯组合物和(b)选自含硫有机化合物、含磷有机化合物和无-硫有机钼化合物的化合物。所述组分(a)和(b)可以约1∶15到约15∶1的比例存在。
本发明的组合物可以能够产生预期抗磨特性的有效量加入润滑剂中。约0.1％到10.0％的量对于多数应用是足够的。优选的范围为占总润滑剂组合物的约0.5％到约3.0％质量比，最优选范围为约0.7％到约1.5％质量比。
依据润滑剂的使用目的，所述润滑用组合物可包括其它常规添加剂。所述脂类配方可包括各种增稠剂，除其它外例如硅酸盐矿物、金属皂(metal soaps)和有机聚合物。
提供以下实施例是为了对本发明进行说明，而不是以任何方式限定本发明。除非另有说明，所有百分比和等分数都基于质量比。
实验数据
实施例1A
OCD-289经硼酸处理的二醇混合物
通过将(C8-18脂肪酸残基)二乙醇酰胺(75％)和(C8-18脂肪酸残基)甘油单酯(22％)的混合物部分硼酸化，使硼酸化的水平达到1％。该硼酸化水平可赋予发动机润滑油的溶解性。实施例1的配方是下面表1和表2的测试的基础。
制备：
1.向500ml单颈烧瓶中加入14.3g硼酸和247.5g OD-896。OD-896是脂肪油与二乙醇胺反应的产物，其可从R.T.Vanderbilt Company，Inc获得。
2.室温下将上述烧瓶置于真空蒸发装置上，中速旋转直到硼酸均匀地分布于OD-896之中。
3.对上述烧瓶抽真空除去混合物中含有的空气。
4.将上述混合物逐渐加热至65℃保持1小时以初步除水。
5.将上述混合物继续加热至95℃保持4小时以除去残余的水。
6.将上述产物在80℃条件下过滤，然后包装。
实施例1B
OCD-289(纯的，1％硼)的制备
丁醇方法
制备：
1.向500ml三颈烧瓶中加入5.78g硼酸、100.0g OD-896NT和40.0g丁醇。
2.开动搅拌装置以适当的高速搅拌直到硼酸均匀地分散于OD-896NT/丁醇溶液中。
3.将混合物逐渐加热至95℃保持3小时以初步除水。
4.将混合物继续加热至130℃的回流温度，保持3小时以除去残余的水。
5.升温至150℃，并对烧瓶抽真空2小时以除去残余的丁醇。
6.将上述产物在110℃条件下过滤，其后进行包装。
实施例1C
OCD 289的制备
1.向2升三颈圆底烧瓶中加入1103.0g OD 896和71.05g硼酸。OD-289是脂肪油与二乙醇胺反应的产物，其可从R.T.VanderbiltCompany，Inc获得。
2.在上述烧瓶上安装Dean Stark Trap、冷凝器、温度计和机械搅拌。
3.将整个装置置于约50mm Hg气压下，加热至130℃。
4.在130℃，用5-7小时的时间收集水。
5.将上述反应体系冷却至约80℃，并在搅拌下加入123.5g napthenic(环烷)基础油，然后经热过滤获得黄色液体。
实施例2A
10％油含量的OCD-289
可以用napthenic基础油代替10％的所述二醇原料(过量的)并如实施例1中硼酸化至1％的水平，以此来改进硼酸化产物的倾点。
制备：
A.向500ml单颈烧瓶中加入17.2g硼酸、267.0g OD-896和30.0gNapthenic基础油。
B.室温下将上述烧瓶置于真空蒸发装置上，中速旋转直到硼酸均匀地分布于OD-896和Uninap油之中。
C.对上述烧瓶抽真空除去混合物中含有的空气。
D.将上述混合物逐渐加热至65℃保持1小时以初步除水。
E.将上述混合物继续加热至95℃保持4小时以除去残余的水。
F.将上述产物在80℃条件下过滤，然后包装。
实施例2B
OCD-289(含10％油，1％B)的制备
丁醇方法
制备：
A.向500ml三颈烧瓶中加入5.78g硼酸、90.0g OD-896NT、10.0gNapthenic基础油和40g丁醇。
B.开动搅拌装置以适当的高速搅拌直到硼酸均匀地分散于OD-896NT/丁醇溶液中。
C.将所述混合物逐渐加热至95℃保持3小时以初步除去水。
D.将所述混合物继续加热至130℃保持3小时以除去残余的水。
E.升温至150℃，并对所述体系抽真空2小时以除去残余的丁醇。
F.将上述产物在110℃条件下过滤，其后包装。
实施例1B和2B的方法制备出与实施例1A和2A相同的化合物，但是由于所述反应更易于完成，因此产物的储存稳定性得到提高。同样地，实施例1C与1A和1B类似，但为优选方案。尽管表1-4中的某些测试源自制备硼酸化的酯的A、B或C方法，但无论其生产方法如何其在润滑剂中的表现相同。实施例1B和2B的方法基本遵照美国专利第4,389,322号的教导，本文将其引入作为参考。
上述实施例基于所述硼酸化的酯中硼含量为1％。研究者认为含有最高3％的硼含量是有利的，且理论上硼的最高含量能够达到约3.68％。尽管目前的实施例都基于硼含量为1％，但是可以理解，当硼酸化的酯中硼含量最高为3％或更高时可获得相当的或更好的性能。从经济和粘度方面考虑，组合物的硼含量通常优选为约0.8-1.2％，特别优选硼含量为约1％。
认为由上述方法制备的有机硼酸酯组合物包括以下两种反应产物。如果所述反应朝充分水合方向进行，则认为还可能存在以下其它反应产物中的部分或全部。
和/或
其中R1＝H或CxHy，其中x＝1-60，而y＝3-121
实验室测试中用标准Falex装置来模拟机动车发动机的气阀机构(valve train)磨损。将V-block(V形块)和pin(销钉)在矿物油精中用超声清洁器洗涤，用丙酮漂洗，风干并称重。将测试样品(60g)置于油杯中。开动发动机，将负载臂置于棘轮上。当达到参考负载227kg时，将棘轮释放并将所述负载保持3.5小时不变。其后，将所述发动机关闭。将所述V-block和pin洗涤、干燥并称重。记录所失去的重量(磨损的测量值)并在下文中列出。在测试条件下，由于产生过度磨损和高转矩(即不能保持所述负载)，任何运行达60分钟的测试被认为是FAIL。对FAIL测试，其质量损失无关紧要，因此没有显示。
表A显示了在基础油中仅含硼酸化的二醇(硼酸化的酯)样品OCD-289的测试结果。结果显示，失败(或至少是不一致的结果)在硼酸化二醇水平等于或低于0.7％质量比时出现。只有在等于或高于0.7％质量比的水平时才获得一致的较好的结果。因此，我们意外发现，当与某些添加剂化合物结合时用较低水平的硼酸化二醇即可达到很好的抗磨水平。表B清楚地显示，当与例如二硫代磷酸盐(
1395)、二硫代磷酸酯(7611M)、二硫代氨基甲酸盐(822)和双二硫代氨基甲酸酯(
7723)的添加剂化合物结合时，0.35％的低水平的硼酸化二醇即可提供良好的抗磨保护。这些及其它添加剂的更详细数据列于以下表1-4中。这些数据显示，所述协同组合物的抗磨保护作用远超单独使用所述组合物中任一组分的情况。
如以下本发明的各种实施方案中所描述，结合上下文可以得出重要的结论，即只有在较高质量百分比含量时，硼酸酯组合物在抗磨测试条件下才能实现期望的效果，即OCD-289显示出相对好的抗磨特性(见表1的测试1)。降低OCD-289的量会引起抗磨性能的急剧下降(见表1的测试10)。所获得的意外结果的一个方面是通过加入本发明所述的添加剂组分，能够将硼酸酯含量降低至与较差抗磨性能对应的较低水平，而仍能达到良好的抗磨效果。
在第一实施方案中，本发明涉及含有与如式(I)所示的1，3，4-噻二唑化合物结合的有机硼酸酯组合物的添加剂组合物：
其中，R和R1独立地选自氢和C8-12硫代烷基或氢、C1-22烷基基团、萜残基及下式所示的马来酸残基：
及R2和R3表示C1-22烷基和C5-7环烷基，R或R1以及R2和R3两者之一可为氢。
式I所示的1，3，4-噻二唑可通过在美国专利第4,761,842号和第4,880,437号中公开的方法来制备，上述专利在本文中引入作为参考。萜残基优选源自蒎烯和莱烯。
R和R1表示的烷基基团优选含有1到22个碳原子，且可以是支链或直链的。特别优选的化合物为两个烷基总共含有至少22个碳原子的化合物。式I的基团R2和R3表示含1-22个碳原子的支链或直链烷基基团以及诸如环己基、环戊基和环庚基的环脂肪族基团。
具体测试的噻二唑化合物是丁二酸((4，5-二氢-5-硫代-1，3，4-噻二唑-2-基)硫-双(2-乙基己基)酯，其可以
名称从R.T.VanderbiltCompany，Inc.获得。结果在下面表2中列出。可以明显地看出，尽管单独的噻二唑化合物(测试12)不能提供充分的抗磨保护，但是当与有机硼酸酯组合物结合使用时会获得优良的结果。
图2显示了进一步的
871测试。在SRV机器上测试本发明的添加剂组合物(在下文中将详细描述)。结果显示当OCD-289与871一起使用时，在长达2小时的测试过程中油膜强度未被损坏。尽管单独使用
871的结果失败，但OCD-289和
871以各种比例的混合物产生显著的改进。因此，由诸如
871的噻二唑获得的油膜强度可以通过以适当的硼酸酯：噻二唑比例与有机硼酸酯组合物结合而大大增强。在一个硼酸酯组合物与噻二唑结合的实施方案中，所述硼酸酯组合物∶噻二唑比例为约1∶3到约15∶1。在另一个硼酸酯组合物与噻二唑结合的实施方案中，所述硼酸酯组合物∶噻二唑比例为约3∶7到约9∶1。
本发明第二方案涉及含有与式(II)的双二硫代氨基甲酸酯化合物结合的有机硼酸酯组合物的添加剂组合物：
其中，R4、R5、R6、和R7为具有1到13个碳原子的脂肪族烃基，并且R8为具有1到8个碳原子的亚烷基。
所述的式(II)的双二硫代氨基甲酸酯为美国专利第4,648,985号描述的已知化合物，本文将其引入作为参考。所述化合物以R4-R7基团为特征，其可以是相同的或不同的具有1-13个碳原子的烃基基团。优选为具有1-8个碳原子的支链或直链烷基基团。R8基团为含有1-8个碳原子的诸如支链或直链亚烷基脂肪族基团。特别优选为亚甲基双(二丁基二硫代氨基甲酸酯)，其可通过商业途径以
7723商标从R.T.VanderbiltCompany，Inc.获得。
测试了所述的双二硫代氨基甲酸酯
7723，结果在表4中列出。可以明显看出，尽管单独使用双二硫代氨基甲酸酯不能提供充分的抗磨保护(测试29)，但当与所述有机硼酸酯组合物(记为OCD-289)结合使用时获得了优良的结果。在硼酸酯组合物结合双二硫代氨基甲酸酯的一个实施方案中，硼酸酯组合物∶双二硫代氨基甲酸酯的比例为约1∶6到约15∶1。在另一个硼酸酯组合物结合双二硫代氨基甲酸酯的实施方案中，硼酸酯组合物∶双二硫代氨基甲酸酯的比例为约1∶4到约9∶1。
本发明的第三实施方案涉及含有与式(III)所示的二硫代氨基甲酸盐结合的有机硼酸酯组合物的添加剂组合物：
其中，R9和R10表示具有1到8个碳原子的烷基基团，M表示周期表中第IIA、IIIA、VA、VIA、IB、IIB、VIB、VIII族的金属和由下式的胺形成的盐部分：
R11、R12和R13独立地选自氢和具有1到18个碳原子的脂肪族基团，且n为M的价态；
或式(IV)：
X＝S或O
其中R4、R5、R6和R7为具有1到13个碳原子的脂肪族烃基基团，而R8为具有1到8个碳原子的亚烷基基团。
式III所示的二硫代氨基甲酸盐为已知化合物。在美国专利第2,492,314号中公开了一种制备方法，其在本文中引入作为参考。式III中的R4和R5基团表示具有1到8个碳原子的支链或直链烷基基团。特别优选为锑和锌的二硫代氨基甲酸盐。
本发明中特别的二硫代氨基甲酸盐测试化合物(见表3)为二烷基二硫代氨基甲酸钼(822，可从R.T.Vanderbilt Company，Inc.获得)和二戊基二硫代氨基甲酸锌(
AZ(50％活化)，可从R.T.Vanderbilt Company，Inc.获得)。可以明显看出，尽管单独使用二硫代氨基甲酸盐不能提供充分的抗磨保护，但当与有机硼酸酯组合物结合使用时获得了优良的结果。在硼酸酯组合物结合二硫代氨基甲酸盐的一个实施方案中，硼酸酯组合物∶二硫代氨基甲酸盐的比例为约1∶15到约15∶1。在另一个硼酸酯组合物结合二硫代氨基甲酸盐的实施方案中，硼酸酯组合物∶二硫代氨基甲酸盐的比例为约1∶9到约9∶1。在另一个硼酸酯组合物结合二硫代氨基甲酸盐的实施方案中，硼酸酯组合物∶二硫代氨基甲酸盐的比例为约2∶1到约1∶1。
本发明的第四实施方案涉及含有与式(V)所示的二硫代磷酸盐结合的有机硼酸酯组合物的添加剂组合物：
其中，X1和X2独立地选自S和O，R14和R15表示氢和具有1到22个碳原子的烷基基团，M表示周期表中第IIA、IIIA、VA、VIA、IB、IIB、VIB、VIII族的金属和由下式的胺形成的盐部分：
R16、R17和R18独立地选自氢和具有1到18个碳原子的脂肪族基团，且n为M的价态。
式(V)所示的二硫代磷酸盐为已知的，可通过商业获得的物质。美国专利第4,215,067号中教导了一种制备方法，本文将其引入作为参考。R14和R15基团表示具有1-22个碳原子的支链或直链烷基基团，且可以衍生自脂肪酸。特别优选为二硫代磷酸锌。式III和式IV的金属离子可选自下列周期表中的族：IIA、IIIA、VA、VIA、IB、IIB、VIB和VIII。所述化合物的胺盐也是本发明有用的协同剂。除其它外，示例性的盐包括那些由烷基胺和混合的烷基胺制备的盐。特别有用的为脂肪酸胺。
测试的二硫代磷酸盐是伯烷基二硫代磷酸锌(
1395从Lubrizol Corporation获得)，结果列于表1中。尽管众所周知当具有足够高的磷水平时二硫代磷酸盐可提供抗磨保护，但是工业上普遍避免如此高的水平。因此，人们对以较低的磷水平获得抗磨保护具有兴趣。可以看出，当二硫代磷酸盐低于基础油的1％质量比时，尽管含磷水平很低(低于0.080％甚至低至0.009％P)，本组合物仍是有效的。图3涉及与图1和图2所示类似的SRV检测，某些不同参数的如图3本身所示。同样可以清楚看出硼酸酯和ZDDP组合物显示优良的结果，而单独使用ZDDP的硼酸酯在此重要的测试中失败。在硼酸酯组合物结合二硫代磷酸盐的一个实施方案中，硼酸酯组合物∶二硫代磷酸盐的比例为约1∶15到约15∶1。在另一个硼酸酯组合物结合二硫代磷酸盐的实施方案中，硼酸酯组合物∶二硫代磷酸盐的比例为约1∶9到约9∶1。
本发明的第五实施方案涉及含有与式(VI)所示的二硫代磷酸酯结合的有机硼酸酯组合物的添加剂组合物。式(VI)：
其中R19、R20、R21和R22可以相同或不同且选自具有1到8个碳原子的烷基基团。
式(VI)所示的二硫代磷酸酯为已知化合物。美国专利第3,567,638号公开了制备方法之一。式(VI)中的R19、R20、R21和R22基团可以相同或不同且可选自直链或支链的烷基基团。优选含有1到8个碳原子的基团。测试的二硫代磷酸酯是二烷基二硫代磷酸酯(
7611M从R.T.Vanderbilt Company，Inc.获得)，结果列于表4中。尽管众所周知当具有足够高的磷水平时二硫代磷酸酯可提供抗磨保护，但是工业上普遍避免如此高的水平。因此，人们对以较低的磷水平获得抗磨保护具有兴趣。同样可以看出，当二硫代磷酸酯含量低于基础油的1％质量比时，尽管含磷水平很低(低于0.050％甚至低至0.006％P)，本组合物仍是有效的。在硼酸酯组合物结合二硫代磷酸酯的一个实施方案中，硼酸酯组合物∶二硫代磷酸酯的比例为约1∶15到约15∶1。在另一个硼酸酯组合物结合二硫代磷酸酯的实施方案中，硼酸酯组合物∶二硫代磷酸酯的比例为约1∶9到约9∶1。
本发明的第六实施方案涉及含有与非-硫钼添加剂结合的有机硼酸酯组合物的添加剂组合物。特别优选为无-硫和无磷的有机酰胺配合物，其可根据美国专利第4,889,647号所述的缩合方法通过将脂肪油、二乙醇胺和钼源依次反应而制备，获得钼含量最高达12％质量比的产物，本文将其引入作为下式的参考：
和/或 (VII)
其中，R’为脂肪油残基。
将与有机硼酸酯组合物结合进行了测试，结果列于表3。公知855具有优良的抗磨特性。然而，意外地发现当与硼酸酯组合物结合时，该特性得到进一步增强。比较测试20和测试21可以看出，降低855量引起抗磨性能的下降。比较测试21和测试22可以看出，与单独使用
855时的量相同，而与结合使用硼酸酯组合物比较，其使抗磨性能几乎提高了2倍。
图1和图2的测试参数
测试温度，80℃
测试试验性操作负载，N50(30秒)
测试负载，N200
测试频率，Hz 50
测试冲程，mm 1.00
测试时间，分钟 50
测试球材料 52100钢，60±2Rc强度
0.025±0.005μm Ra表面抛光
10-mm直径
测试盘材料 52100钢，60±2Rc强度
0.45-0.65μm Rz抛光的表面
24-mm直径、7.85mm
所述“失败”点是指在该点上摩擦系数增至单独使用油时的摩擦系数。从图1可以看出，与单独使用任一组分(分别为测试2和测试3)相比，测试4和测试6分别对应于以质量比1∶1和3∶1结合的OCD-289和855)显示出良好的摩擦降低性能。
在硼酸酯组合物结合非-硫钼添加剂的一个实施方案中，硼酸酯组合物∶非-硫钼添加剂的比例为约1∶15到约15∶1。在另一个硼酸酯组合物结合非-硫钼添加剂的实施方案中，硼酸酯组合物∶非-硫钼添加剂的比例为约1∶9到约9∶1。在另一个硼酸酯组合物结合非-硫钼添加剂的实施方案中，硼酸酯组合物∶非-硫钼添加剂的比例为约1∶1到约3∶1。
表A：测试中OCD-289的性能
测试：Falex Pin&Vee Block(Falex销钉&V型块)
测试条件：500lbs.，60分钟
基础：Napthenic油
| 处理率 | 测试时间 | 质量损失，mg | |
| (质量百分比) | 分钟 | ||
| 0.5 | 57(失败) | FAIL | |
| 0.6 | 60 | 39 | |
| 0.6 | 60 | 28 | |
| 0.7 | 5(失败) | FAIL | |
| 0.7 | 6(失败) | FAIL | |
| 0.8 | 60 | 30 | |
| 0.9 | 60 | 27 | |
| 1.0 | 60 | 23* |
*21次测试的平均值。范围8.7-60.8mg
表B：含其它添加剂的OCD-289的性能
测试：Falex Pin&Vee Block
测试条件：500 lbs.，60分钟
基础：99.3％Napthenic油+0.35％OCD-289+0.35％其它添加剂
| 其它添加剂 | 测试时间 | 质量损失，mg | |
| 分钟 | |||
| LZ1395 | 60 | 1.8 | |
| LZ1395 | 60 | 18 | |
| MOLYVAN 822 | 60 | 39 | |
| MOLYVAN 822 | 60 | 31 | |
| VANLUBE 7723 | 60 | 43.6 | |
| VANLUBE 7723 | 60 | 59.2 | |
| VANLUBE 7611M | 60 | 25.5 | |
| VANLUBE 7611M | 60 | 30.5 |
表1：含其它添加剂的OCD-289的Falex Pin&Vee Block性能
基础：Napthenic油
质量百分比
| 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 11 | |
| OCD-289 | 1.0 | 0.5 | 0.9 | 0.1 | 0.5 | ||||||
| LZ 1395(ZDDP) | 1.06 | 1.5 | 2.0 | 5.0 | 0.5 | 0.1 | 0.9 | 0.5 | |||
| OD-896B | 1.0 | ||||||||||
| ％磷 | 0 | 0.10 | 0 | 0.14 | 0.19 | 0.47 | .047 | .009 | 0.08 | 0 | .047 |
| Falex Pin&Vee Block(500lb 60分钟) | |||||||||||
| 持续时间，分钟s＝秒 | 60 | 7s(5s) | 19s(15s) | 13s | 15s | 47 | 60 | 60 | 60 | 40 | 2s |
| FAIL | FAIL | FAIL | FAIL | FAIL | FAIL | FAIL | |||||
| 质量损失，mg | 23.0* | 2.8 | 7.5 | 23.3 |
()＝重复测试；*21次测试的平均值(范围8.7-60.8mg)
表2
质量百分比
| 12 | 13 | 14 | 15 | 16 | 17 | |
| OCD-289 | 0.5 | 0.9 | 0.1 | 0.2 | 0.3 | |
| Vanlube 871 | 1.0 | 0.5 | 0.1 | 0.9 | 0.8 | 0.7 |
| ％磷 | 0 | 0 | 0 | 0 | 0 | 0 |
| Falex Pin&VeeBlock(500lb 60分钟) | ||||||
| 持续时间，分钟s＝秒 | 48s | 60 | 60 | 25s | 1 | 60 |
| FAIL | FAIL | FAIL | ||||
| 质量损失，mg | 3.9 | 3.2 | 7.2 |
s＝秒
运行低于60分钟的测试具有过度磨损或高转矩。不能保持负载。
表3
质量百分比
| 18 | 19 | 20 | 21 | 22 | 23 | 24 | 25 | 26 | 27 | 28 | |
| OCD-289 | 0.5 | 0.5 | 0.9 | 0.1 | 0.5 | 0.5 | |||||
| Molyvan 822 | 0.5 | 0.25 | |||||||||
| Molyvan 855 | 1.0 | 0.5 | 0.5 | 0.1 | 0.9 | ||||||
| Vanlube AZ | 1.0 | 0.5 | |||||||||
| 环烷酸钼(6％Mo) | 1.0 | 0.5 | |||||||||
| ％磷 | 0 | 0 | 0 | 0 | 0 | 0 | 0 | 0 | 0 | 0 | 0 |
| Falex Pin&VeeBlock(500lb 60分钟) | |||||||||||
| 持续时间，分钟s＝秒 | 16s | 60 | 60 | 60 | 60 | 60 | 60 | 3.5 | 60 | 5s | 7 |
| FAIL | FAIL | FAIL | FAIL | ||||||||
| 质量损失，mg | 3.9 | 24.4 | 31.1 | 16.1 | 22.2 | 25.4 | 12.8 |
表4
质量百分比
| 1 | 29 | 30 | 31 | 32 | 33 | 34 | 35 | 36 | 37 | |
| OCD-289 | 1.0 | 0.5 | 0.9 | 0.1 | 0.2 | 0.5 | 0.9 | 0.1 | ||
| Vanlube 7723 | 1.0 | 0.5 | 0.1 | 0.9 | 0.8 | |||||
| Vanlube 7611M | 1.0 | 0.5 | 0.1 | 0.9 | ||||||
| ％磷 | 0 | 0 | 0 | 0 | 0 | 0 | 0.06 | 0.03 | 0.006 | 0.05 |
| Falex Pin&VeeBlock(500lb 60分钟) | ||||||||||
| 持续时间，分钟 | 60 | 31 | 60 | 60 | 4 | 60 | 23 | 60 | 60 | 60 |
| FAIL | FAIL | FAIL | ||||||||
| 质量损失，mg | 23.0* | 25.0 | 17.8 | 63.3 | 9.6 | 13.2 | 23.3 |
*21次测试的平均值(范围8.7-60.8mg)
运行低于60分钟的测试具有过度磨损或高转矩，(不能保持负载)记为“FAIL”。
本发明的另一实施方案涉及具有改善的润滑性能并含有作为主要成分的润滑粘度的油及占润滑剂组合物总质量的约0.1％到约10.0％质量比的组合物，其包括(1)有机硼酸酯组合物及(2)式I、II、III、IV、V、VI、VII所示的有机化合物或其混合物。此润滑剂组合物的一个实施方案包括约0.5％到约3.0％质量比(基于所述润滑剂组合物的总质量)的含有(1)有机硼酸酯组合物和(2)式I、II、III、IV、V、VI、VII所示的有机化合物或其混合物的组合物。
Claims (12)
1.用作润滑剂添加剂的抗磨组合物，包括：
(1)有机硼酸酯组合物，其通过1mol脂肪油与1.0-2.5mol二乙醇胺反应，随后与硼酸进行反应而制得，其中所述有机硼酸酯组合物的硼含量为0.8％至1.2％重量比；以及
(2)一种或多种组分选自：
(i)式(II)所示的双二硫代氨基甲酸酯化合物：
其中R4、R5、R6和R7为具有1到13个碳原子的脂肪烃基基团，并且R8为具有1到8个碳原子的亚烷基，其中有机硼酸酯与双二硫代氨基甲酸酯之比为1∶4至9∶1；
(ii)二硫代氨基甲酸盐化合物，其包括二烷基二硫代氨基甲酸钼或二(C1-C8烷基)二硫代氨基甲酸锌，其中有机硼酸酯与二硫代氨基甲酸盐之比为1∶15至15∶1；
(iii)二硫代磷酸盐化合物，其包括伯烷基二硫代磷酸锌，其中有机硼酸酯与二硫代磷酸盐之比为1∶15至15∶1；及
(iv)二硫代磷酸酯化合物，其包括二烷基二硫代磷酸酯，其中有机硼酸酯与二硫代磷酸酯之比为1∶15至15∶1。
2.如权利要求1所述的组合物，其中组分(2)含有(ii)的二硫代氨基甲酸盐。
3.如权利要求2所述的组合物，其中组分(1)与组分(2)之比为2∶1到1∶1。
4.如权利要求1所述的组合物，其中组分(2)含有(i)的双二硫代氨基甲酸酯。
5.如权利要求4所述的组合物，其中组分(1)与组分(2)比为1∶4到9∶1。
6.如权利要求1所述的组合物，其中组分(2)含有(iii)的二硫代磷酸盐。
7.如权利要求1所述的组合物，其中组分(2)含有(iv)的二硫代磷酸酯。
8.用作润滑剂添加剂的抗磨组合物，包括：
(1)有机硼酸酯组合物，其通过1mol脂肪油与1.0-2.5mol二乙醇胺反应，随后与硼酸进行反应而制得，其中所述有机硼酸酯组合物的硼含量为0.8％至1.2％重量比；以及
(2)一种或多种组分选自：
(i)式(I)所示的1，3，4-噻二唑化合物：
其中，R和R1独立地选自氢和C8-12硫代烷基或氢、C1-22烷基基团、萜残基及如下式所示的马来酸残基：
且R2和R3代表C1-22烷基和C5-7环烷基基团，R或R1为氢且R2和R3两者之一为氢，其中有机硼酸酯与1，3，4-噻二唑之比为3∶7至9∶1，及
(ii)非-硫钼添加剂，其通过用下列物质进行反应来制备：(a)1.0mol具有12个或更多碳原子的脂肪油，(b)1.0mol到2.5mol的二乙醇胺和(c)钼源，其中有机硼酸酯与非-硫钼添加剂之比为1∶9至9∶1。
9.如权利要求8所述的组合物，其中组分(2)含有(ii)的非-硫钼添加剂。
10.如权利要求9所述的组合物，其中组分(1)与组分(2)之比为1∶1到3∶1。
11.如权利要求8所述的组合物，其中组分(2)含有(i)的噻二唑。
12.如权利要求11所述的组合物，其中组分(1)与组分(2)之比为3∶7到9∶1。
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| EP2460870B1 (en) | 2013-12-04 |
| EP2436753A1 (en) | 2012-04-04 |
| BR0315029A (pt) | 2005-08-16 |
| JP4296153B2 (ja) | 2009-07-15 |
| EP2366762B1 (en) | 2013-05-22 |
| EP2436753B1 (en) | 2014-08-13 |
| US7598211B2 (en) | 2009-10-06 |
| BR0315029B1 (pt) | 2014-03-11 |
| JP2006502287A (ja) | 2006-01-19 |
| EP2302023A3 (en) | 2011-04-13 |
| MXPA05002664A (es) | 2005-09-08 |
| EP2302023B1 (en) | 2013-04-17 |
| EP1573839A2 (en) | 2005-09-14 |
| EP2302023A2 (en) | 2011-03-30 |
| CN1852969A (zh) | 2006-10-25 |
| ATE548437T1 (de) | 2012-03-15 |
| US20080261838A1 (en) | 2008-10-23 |
| US7897549B2 (en) | 2011-03-01 |
| WO2004033605A2 (en) | 2004-04-22 |
| WO2004033605A3 (en) | 2005-09-22 |
| EP2460870A1 (en) | 2012-06-06 |
| EP1573839A4 (en) | 2010-03-24 |
| EP1573839B1 (en) | 2012-03-07 |
| CA2495199C (en) | 2010-11-02 |
| US20040138073A1 (en) | 2004-07-15 |
| AU2003282730A1 (en) | 2004-05-04 |
| AU2003282730A8 (en) | 2004-05-04 |
| CA2495199A1 (en) | 2004-04-22 |
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