CN103695137B - A kind of Composite calcium naphthenate base lubricating grease and preparation method thereof - Google Patents
A kind of Composite calcium naphthenate base lubricating grease and preparation method thereof Download PDFInfo
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- CN103695137B CN103695137B CN201210365823.5A CN201210365823A CN103695137B CN 103695137 B CN103695137 B CN 103695137B CN 201210365823 A CN201210365823 A CN 201210365823A CN 103695137 B CN103695137 B CN 103695137B
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- acid
- calcium
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- 230000001050 lubricating effect Effects 0.000 title claims abstract description 90
- 239000004519 grease Substances 0.000 title claims abstract description 74
- 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 title claims abstract description 53
- 239000002131 composite material Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000011575 calcium Substances 0.000 claims abstract description 61
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 48
- 239000002199 base oil Substances 0.000 claims abstract description 24
- 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 abstract description 23
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 21
- 229930195729 fatty acid Natural products 0.000 claims abstract description 21
- 239000000194 fatty acid Substances 0.000 claims abstract description 21
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 20
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000012530 fluid Substances 0.000 claims abstract description 18
- 150000004665 fatty acids Chemical class 0.000 claims abstract description 17
- 159000000007 calcium salts Chemical class 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 5
- 239000003208 petroleum Substances 0.000 claims abstract description 5
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 78
- 239000002253 acid Substances 0.000 claims description 67
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 27
- 235000011054 acetic acid Nutrition 0.000 claims description 26
- -1 hydroxy fatty acid Chemical class 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 23
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 16
- 150000003384 small molecules Chemical class 0.000 claims description 14
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 13
- 239000011707 mineral Substances 0.000 claims description 13
- 230000001131 transforming effect Effects 0.000 claims description 13
- 239000003921 oil Substances 0.000 claims description 12
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims description 12
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 11
- 239000004327 boric acid Substances 0.000 claims description 11
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- 125000003118 aryl group Chemical group 0.000 claims description 9
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 9
- HSSYVKMJJLDTKZ-UHFFFAOYSA-N 3-phenylphthalic acid Chemical compound OC(=O)C1=CC=CC(C=2C=CC=CC=2)=C1C(O)=O HSSYVKMJJLDTKZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000000654 additive Substances 0.000 claims description 7
- 230000000996 additive effect Effects 0.000 claims description 7
- 125000000217 alkyl group Chemical group 0.000 claims description 7
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 7
- 239000000920 calcium hydroxide Substances 0.000 claims description 7
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 7
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 7
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 claims description 6
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 6
- 230000018044 dehydration Effects 0.000 claims description 6
- 238000006297 dehydration reaction Methods 0.000 claims description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 6
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims description 6
- 239000004571 lime Substances 0.000 claims description 6
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 5
- 235000021355 Stearic acid Nutrition 0.000 claims description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000002329 infrared spectrum Methods 0.000 claims description 5
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 5
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 5
- 239000008117 stearic acid Substances 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 150000002632 lipids Chemical class 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000001384 succinic acid Substances 0.000 claims description 4
- 239000000725 suspension Substances 0.000 claims description 4
- 125000006527 (C1-C5) alkyl group Chemical group 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 239000005639 Lauric acid Substances 0.000 claims description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 3
- 125000000304 alkynyl group Chemical group 0.000 claims description 3
- 150000004982 aromatic amines Chemical class 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 3
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 3
- HCPOCMMGKBZWSJ-UHFFFAOYSA-N ethyl 3-hydrazinyl-3-oxopropanoate Chemical compound CCOC(=O)CC(=O)NN HCPOCMMGKBZWSJ-UHFFFAOYSA-N 0.000 claims description 3
- 125000001475 halogen functional group Chemical group 0.000 claims description 3
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 235000019260 propionic acid Nutrition 0.000 claims description 3
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 3
- 125000005480 straight-chain fatty acid group Chemical group 0.000 claims description 3
- 125000002769 thiazolinyl group Chemical group 0.000 claims description 3
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 claims description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 2
- 150000008431 aliphatic amides Chemical class 0.000 claims description 2
- 235000011089 carbon dioxide Nutrition 0.000 claims description 2
- RXKJFZQQPQGTFL-UHFFFAOYSA-N dihydroxyacetone Chemical compound OCC(=O)CO RXKJFZQQPQGTFL-UHFFFAOYSA-N 0.000 claims description 2
- 150000002191 fatty alcohols Chemical group 0.000 claims description 2
- 150000003009 phosphonic acids Chemical class 0.000 claims description 2
- 238000007670 refining Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 10
- 239000000084 colloidal system Substances 0.000 abstract description 3
- 150000003839 salts Chemical class 0.000 abstract description 2
- 239000007921 spray Substances 0.000 abstract description 2
- 229960001860 salicylate Drugs 0.000 description 12
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 12
- 125000005609 naphthenate group Chemical group 0.000 description 10
- ASLMJVVWFAQOQS-UHFFFAOYSA-N calcium;terephthalic acid Chemical compound [Ca].OC(=O)C1=CC=C(C(O)=O)C=C1 ASLMJVVWFAQOQS-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 125000004119 disulfanediyl group Chemical group *SS* 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 3
- 239000012964 benzotriazole Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000003112 inhibitor Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- VIDTVPHHDGRGAF-UHFFFAOYSA-N selenium sulfide Chemical compound [Se]=S VIDTVPHHDGRGAF-UHFFFAOYSA-N 0.000 description 3
- 229960005265 selenium sulfide Drugs 0.000 description 3
- 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
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- IOJUPLGTWVMSFF-UHFFFAOYSA-N benzothiazole Chemical compound C1=CC=C2SC=NC2=C1 IOJUPLGTWVMSFF-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 239000010687 lubricating oil Substances 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- AIDLAEPHWROGFI-UHFFFAOYSA-N 2-methylbenzene-1,3-dicarboxylic acid Chemical compound CC1=C(C(O)=O)C=CC=C1C(O)=O AIDLAEPHWROGFI-UHFFFAOYSA-N 0.000 description 1
- NEQFBGHQPUXOFH-UHFFFAOYSA-N 4-(4-carboxyphenyl)benzoic acid Chemical compound C1=CC(C(=O)O)=CC=C1C1=CC=C(C(O)=O)C=C1 NEQFBGHQPUXOFH-UHFFFAOYSA-N 0.000 description 1
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 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
- 241000158728 Meliaceae Species 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- RYYWUUFWQRZTIU-UHFFFAOYSA-N Thiophosphoric acid Chemical compound OP(O)(S)=O RYYWUUFWQRZTIU-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- WDAORDHNLAOPIT-UHFFFAOYSA-N [Ca].C1(=CC=C(C=C1)C(=O)O)C1=CC=C(C=C1)C(=O)O Chemical compound [Ca].C1(=CC=C(C=C1)C(=O)O)C1=CC=C(C=C1)C(=O)O WDAORDHNLAOPIT-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 125000003368 amide group Chemical group 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
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- JXLHNMVSKXFWAO-UHFFFAOYSA-N azane;7-fluoro-2,1,3-benzoxadiazole-4-sulfonic acid Chemical compound N.OS(=O)(=O)C1=CC=C(F)C2=NON=C12 JXLHNMVSKXFWAO-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
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000001246 colloidal dispersion Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000004821 distillation Methods 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
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N pentanoic acid group Chemical group C(CCCC)(=O)O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000376 reactant Substances 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
- 238000006277 sulfonation reaction Methods 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 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
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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- Lubricants (AREA)
Abstract
The invention provides a kind of Composite calcium naphthenate base lubricating grease and preparation method thereof.With lubricating grease weight for benchmark, this lubricating grease comprises following component: 1) non-newtonian fluid calcium naphthenate 10%-70%; 2) the calcium salt 1%-10% of higher fatty acid; 3) the calcium salt 1%-15% of aromatic acid; 4) lubricating base oil 10%-80%.Described lubricating grease have employed petroleum naphthenic acid calcium or synthesis calcium naphthenate is raw material, simultaneously containing composite calcium viscosifying agent.This lubricating grease has fabulous water resistant sprayability and water resistant drenches leachability, also has the performances such as excellent adhesivity, extreme pressure anti-wear, colloid stability, high dropping point, heat-resistant quality, non-corrosibility, resistance to salt(spray)fog simultaneously.
Description
Technical field
The present invention relates to lubricant, is specifically a kind of high base number Composite calcium naphthenate base lubricating grease and preparation method thereof.
Background technology
Overbased calcium alkyl-salicylate has good detergent-dispersant performance, good acid neutralization capacity and excellent diffustivity, the purification agent of lubricating oil can be used as, be widely used in the additive of internal combustion (IC) engine lubricating oil, its technical development mainly makes its high alkalization, exactly calcium carbonate is distributed in thinning oil becomes a kind of colloidal dispersion system with having surface-active naphthenic acid calcium.Mostly overbased calcium alkyl-salicylate is the acidic components extracted from the distillate that crude distillation obtains, warp and Ca (OH)
2reaction, the contour alkalization technology of carbonating and obtain, about the Patents prepared has CN 1465560 etc.
Utilize the lubricating grease that calcium sulfonate with high base number is raw material production, because it has excellent high temperature performance, mechanical stability, colloid stability, oxidation stability, water resisting property, non-corrosibility and antirust resistance to abrasion, since putting goods on the market, cause the extensive concern of domestic and international lubricating grease industry, but, although high base number composite calcium sulfonate base grease has very excellent over-all properties, but the high price of its raw materials for production calcium sulfonate with high base number and complicated preparation technology itself cause it not promoted rapidly, simultaneously, along with the requirement of people to environment protection is more and more higher, in calcium sulfonate with high base number production process must through sulfonation process the pollution of environment also received day by day to the concern of people.Find a kind of performance and the similar but large problem lubricating grease of the problems referred to above can being avoided to become people face at present of high base number composite calcium sulfonate.
Summary of the invention
The invention provides a kind of Composite calcium naphthenate base lubricating grease, it is raw material that this lubricating grease have employed overbased calcium alkyl-salicylate, simultaneously containing composite calcium viscosifying agent.
The present invention also provides above-mentioned preparation of greases method.
Calcium naphthenate base grease provided by the invention, with lubricating grease weight for benchmark, comprises following component:
1) non-newtonian fluid calcium naphthenate 10%-70%, preferred 20%-60%, most preferably 30%-55%;
2) the calcium salt 1%-10% of higher fatty acid, preferred 2%-6%, most preferably 2.2%-4.2%;
3) the calcium salt 1%-18% of aromatic acid, preferred 2%-15%, most preferably 3%-12%;
4) lubricating base oil 10%-80%, preferred 20%-70%, most preferably 30%-60%.
Described non-newtonian fluid calcium naphthenate is at infrared spectrum 873cm
-1-886cm
-1there is crystal form calcium carbonate charateristic avsorption band in place, total basicnumber is 250mgKOH/g-450mgKOH/g, preferred 300mgKOH/g-400mgKOH/g.Described non-newtonian fluid calcium naphthenate is obtained by transforming agent conversion by newton's body calcium naphthenate.And containing unformed calcium carbonate in newton's body calcium naphthenate, 860cm in infrared spectrum
-1-865cm
-1there is charateristic avsorption band in place.Described newton's body calcium naphthenate is petroleum naphthenic acid calcium or synthesis calcium naphthenate, its structure is as shown in (I) formula, and its total basicnumber is 250mgKOH/g-450mgKOH/g, preferred 300mgKOH/g-400mgKOH/g, after changing into non-newtonian fluid calcium naphthenate, its base number is constant.
Wherein, R is the alkyl chain of C3-C20, (CH
2)
nin also may comprise 1-4 five-ring or six-ring, n=7-36; M can up to 45.
Said higher fatty acid is carbon number is 8-20, the straight chain fatty acid of preferred 10-16 or hydroxy fatty acid, such as, one or more mixtures in lauric acid, palmitinic acid, stearic acid, 12-oxystearic acid, eicosyl carboxylic acid, preferred 12-oxystearic acid.
Said aromatic acid is the carboxylic acid having at least 1 carboxyl to be directly connected with aromatic ring, and other substituting group can be the alkyl or aryl etc. of hydrogen, alkyl, thiazolinyl, alkynyl, aryl, halo or perhalogeno, and molecular weight is less than or equal to 550.The preferred binary aromatic acid of described aromatic acid, such as, can be selected from one or more in phthalic acid that unsubstituted or C1-C5 alkyl replaces, m-phthalic acid, terephthalic acid, biphenyl dicarboxylic acid, santowax dioctyl phthalate.Preferred phthalic acid, m-phthalic acid, terephthalic acid, biphenyl dicarboxylic acid, and one or more in methyl substituted biphenyl dicarboxylic acid, santowax dioctyl phthalate etc.
The calcium salt of small molecules mineral acid and/or small molecules lipid acid can also be contained in lubricating grease of the present invention.The molecular weight of said small molecules mineral acid or small molecules lipid acid is less than or equal to 150.Wherein, small molecules mineral acid can be selected from the mixture of one or more in boric acid, phosphoric acid, sulfuric acid etc., preferred boric acid and/or phosphoric acid; Small molecules lipid acid can be selected from the mixture of one or more in acetic acid, oxalic acid, propionic acid, propanedioic acid, butyric acid, succinic acid etc., preferred acetic acid.
Described lubricant base can be mineral oil, synthetic oil, vegetables oil or their mixture, and 100 ° of C kinematic viscosities are 4mm
2/ s-60mm
2/ s, preferred 10mm
2/ s-30mm
2/ s.Synthetic oil can be poly & Alpha ,-olefin oil (PAO), Esters oil, alkyl-silicone oil, F-T synthesis wet goods.
Can also various additive be contained in lubricating grease of the present invention, as oxidation inhibitor, anti-wear agent, rust-preventive agent etc.Wherein the preferred arylamine kind antioxidant of oxidation inhibitor, accounts for the 0.1%-5% of lubricating grease gross weight, preferred 0.2%-1%, can be pentanoic, phenyl-a-naphthylamine, di-iso-octyldiphenylamine or their mixture, preferred di-iso-octyldiphenylamine.Anti-wear agent can be dithio Acidic phosphates zinc, dithio dialkyl amido formic acid molybdenum, dithio dialkyl amido lead formiate, triphenylphosphorothionate, organic molybdenum complex compound, olefine sulfide, molybdenumdisulphide, tetrafluoroethylene, thiophosphoric acid molybdenum, clorafin, dibutyl dithiocaarbamate antimony, tungsten disulfide, Selenium Sulfide, fluorographite, calcium carbonate and zinc oxide; Rust-preventive agent can be barium mahogany sulfonate, petroleum sodium sulfonate, benzothiazole, benzotriazole, zinc naphthenate and alkenyl succinic acid.
Described Composite calcium naphthenate base preparation of greases method, comprising:
(1) newton's body calcium naphthenate, part basis oil and transforming agent are mixed, heat, make material retrogradation;
(2) add lime or calcium hydroxide, add higher fatty acid and aromatic acid respectively, heat up dehydration;
(3) be warmed up to 200 ° of C-220 ° of C constant temperature refinings, cooling, adds surplus base oil, adds necessary additive, obtains finished product.
Specifically, in step (1), by newton's body calcium naphthenate, part basis oil Hybrid Heating to 50 ° of C-90 ° of C, preferred constant temperature 10 minutes-30 minutes, add required transforming agent successively to react, preferably add rear stirring about 10 minutes at every turn, react fully, preferably 60 ° of C-100 ° of C constant temperature 0.5 hour-3 hours, make material retrogradation.
Described newton's body calcium naphthenate is petroleum naphthenic acid calcium or synthesis calcium naphthenate, its total basicnumber 250mgKOH/g-450mgKOH/g, preferred 300mgKOH/g-400mgKOH/g.
Described transforming agent is selected from fatty alcohol, lipid acid, aliphatic ketone, alkanoic, aliphatic amide, cycloalkanes amine, cycloalkanol, the ether of C1-C5, and one or more in boric acid, calcium carbonate, phosphonic acids, carbonic acid gas, phenol, aromatic alcohol, aromatic amine, C8-C20 alkyl benzene sulphonate (ABS), C16-C62 naphthenic acid, water etc., one or more in preferred Witco 1298 Soft Acid, methyl alcohol, Virahol, butanols, C20-C40 naphthenic acid, acetic acid and water.The add-on of transforming agent is the 2%-30% of newton's body calcium naphthenate weight, preferred 6%-22%.
In step (2), the suspension liquid of lime or calcium hydroxide is added at 85 ° of C-100 ° of C, add higher fatty acid at 85 ° of C-100 ° of C, stir 5 minutes-20 minutes, add aromatic acid, necessary small molecules mineral acid and/or small molecules lipid acid can also be added, stir 5 minutes-20 minutes, be warmed up to 105 ° of C-120 ° of C, preferably keep 30 minutes-60 minutes, dehydration, cools to 90 ° of C-105 ° of C; Its Fatty Acids and aromatic acid addition sequence can exchange.
Said higher fatty acid is carbon number is 8-20, the straight chain fatty acid of preferred 10-16 or hydroxy fatty acid, such as, one or more mixtures in lauric acid, palmitinic acid, stearic acid, 12-oxystearic acid, eicosyl carboxylic acid, preferred 12-oxystearic acid.
Said aromatic acid is the carboxylic acid having at least 1 carboxyl to be directly connected with aromatic ring, and other substituting group can be the alkyl or aryl etc. of hydrogen, alkyl, thiazolinyl, alkynyl, aryl, halo or perhalogeno, and molecular weight is less than or equal to 550.The preferred binary aromatic acid of described aromatic acid, such as, can be selected from one or more in phthalic acid that unsubstituted or C1-C5 alkyl replaces, m-phthalic acid, terephthalic acid, biphenyl dicarboxylic acid, santowax dioctyl phthalate.Preferred phthalic acid, m-phthalic acid, terephthalic acid, biphenyl dicarboxylic acid, and one or more in methyl substituted biphenyl dicarboxylic acid, santowax dioctyl phthalate etc.
The molecular weight of said small molecules mineral acid or small molecules lipid acid is less than or equal to 150.Wherein, small molecules mineral acid can be selected from the mixture of one or more in boric acid, phosphoric acid, sulfuric acid etc., preferred boric acid and/or phosphoric acid; Small molecules lipid acid can be selected from the mixture of one or more in acetic acid, oxalic acid, propionic acid, propanedioic acid, butyric acid, succinic acid etc., preferred acetic acid.
The H of higher fatty acid and aromatic acid and small molecules mineral acid and/or small molecules lipid acid
+total amount of substance and the OH contained by calcium hydroxide
-total amount of substance is equal, and the amount of calcium hydroxide also can excessive 1%-10%.
In step (3), the product of step (2) is heated up, preferably at 100 ° C-120 ° C constant temperature 10-20 minute, be finally warmed up to 200 ° of C-220 ° of C constant temperature 5 minutes-10 minutes; Be cooled to 150 ° of C-160 ° of C, add surplus lubricating base oil, treat that temperature is cooled to 100 ° of C-120 ° of C, add necessary additive, stir, circulating filtration, homogenizing, degassedly obtain finished product.
Lubricating grease of the present invention has good extreme pressure anti-wear and overlength lubricating life, meanwhile, also has the performances such as excellent adhesivity, water resisting property, colloid stability, high dropping point, heat-resistant quality, non-corrosibility, resistance to salt(spray)fog.This product preparation process is simple, constant product quality.
Accompanying drawing explanation
Fig. 1 is the infrared spectrum of lubricating grease and the infrared spectrum of overbased calcium alkyl-salicylate raw material of embodiment 1 preparation.As can be seen from the figure, at 873cm
-1-886cm
-1there is crystal form calcium carbonate charateristic avsorption band in place.In raw material, the absorption peak of unformed calcium carbonate is 863cm
-1, after one-tenth fat, its absorption peak is 874cm
-1.
Embodiment
In embodiment, the method for calculation of each component concentration are as follows:
Non-newtonian fluid calcium naphthenate %=(overbased or overbased calcium alkyl-salicylate raw materials quality+transforming agent total mass)/lubricating grease total mass; Transforming agent naphthenic acid, acetic acid, Witco 1298 Soft Acid, methyl alcohol, butanols etc. all count in the content of non-newtonian fluid calcium naphthenate.
The content of the calcium salt of higher fatty acid and the calcium salt of small molecules mineral acid or lipid acid, the gauge generating calcium salt according to added higher fatty acid and small molecules mineral acid or lipid acid and calcium hydroxide complete reaction is calculated.
In embodiment, overbased and overbased calcium alkyl-salicylate raw material, also can according to the disclosed method preparation of CN101885677A (a kind of preparation method of highly basic calcium naphthenate) purchased from Xinjiang Land Fine Petrochemical Co., Ltd.
In comparative example, calcium sulfonate with high base number raw material is purchased from Jinzhou Huifa Tianhe Chemical Co., Ltd..
Embodiment 1
Feed composition: naphthenate with superhigh base number calcium (total basicnumber is 400mgKOH/g, 30kg); 150BS (30kg); Naphthenic acid (total acid value is 120mgKOH/g, acid content 70%, 2.8kg); Acetic acid (0.56kg); Ca (OH)
2(1.8kg); 12-oxystearic acid (2kg); Terephthalic acid (3.5kg); 500SN (17kg).
A volume be 110L and with heating, stir, circulation, cooling normal-pressure reaction kettle in add naphthenate with superhigh base number calcium that 30kg total basicnumber is 400mgKOH/g and 30kg 100 ° of C kinematic viscosity are 31mm
2the HVI150BS lubricating base oil of/s, stirs, heats to 50 ° of C, constant temperature 10 minutes; Add 2.8kg naphthenic acid, temperature controls at 50 ° of about C, stirs 10 minutes; Add the acetic acid of 0.56kg and the aqueous solution of acetic acid weight 4 times, stir 10 minutes; Be warmed up to 60 ° of C, constant temperature 90 minutes, material retrogradation; Add 1.8kgCa (OH)
2and with 4 times of water-reducible suspension liquids, stir 10 minutes; Add 2kg12-oxystearic acid, stir 10 minutes; Add 3.5kg terephthalic acid, stir, be warmed up to 110 ° of C under stirring, keep 60 minutes, dehydration; 120 ° of C constant temperature 20 minutes, is warmed up to 200 ° of C constant temperature 5 minutes.Then, be cooled to 160 ° of C, the 100 ° of C kinematic viscosity adding 17kg are 11mm
2the HVI500SN lubricating base oil of/s; Treat that temperature is cooled to 110 ° of C, add and account for lubricating grease weight 0.2kg couple, after right '-di-iso-octyldiphenylamine stirs 10 minutes, circulating filtration, homogenizing, degassedly obtain finished product.Assay is in table 1.
In the lubricating grease that the present embodiment obtains, with lubricating grease weight for benchmark, consist of: non-newtonian fluid calcium naphthenate 38.4%; Lubricating base oil 54.2%; 12-oxystearic acid calcium 2.4%; Terephthalic acid calcium 5.0%.
Embodiment 2
Feed composition: naphthenate with superhigh base number calcium (total basicnumber is 420mgKOH/g, 30kg); 150BS (30kg); Naphthenic acid (2.8kg); Acetic acid (0.56kg); Ca (OH)
2(1.8kg); 12-oxystearic acid (2kg); Phthalic acid (3.5kg); 500SN (18kg).
Prepare overbased Composite calcium naphthenate base lubricating grease by the method for example 1, unlike the use of the total basicnumber of naphthenate with superhigh base number calcium be 420mgKOH/g, each performance data of lubricating grease finished product obtained is in table 1.
Embodiment 3
Feed composition: naphthenate with superhigh base number calcium (total basicnumber is 400mgKOH/g, 30kg); 150BS (20kg); Butanols (2.8kg); Acetic acid (0.56kg); Ca (OH)
2(1.8kg); Stearic acid (1.9kg); M-phthalic acid (3.5kg); 500SN (28kg).
Overbased Composite calcium naphthenate base lubricating grease is prepared by the method for example 1, naphthenic acid, 12-oxystearic acid, terephthalic acid is replaced unlike the use of butanols, stearic acid, m-phthalic acid, the amount of base oil also changes to some extent, and each performance data of lubricating grease finished product obtained is in table 1.
Embodiment 4
Feed composition: naphthenate with superhigh base number calcium (total basicnumber is 400mgKOH/g, 39kg); 150BS (20kg); Witco 1298 Soft Acid (2.8kg); Acetic acid (0.56kg); Ca (OH)
2(1.8kg); 12-oxystearic acid (2kg); Terephthalic acid (3.5kg); 500SN (28kg); Right, right '-di-iso-octyldiphenylamine (0.2kg).
Prepare overbased Composite calcium naphthenate base lubricating grease by the method for example 1, replace naphthenic acid unlike with Witco 1298 Soft Acid, the amount of base oil also changes to some extent, and each performance data of lubricating grease finished product obtained is in table 1.
In the lubricating grease that the present embodiment obtains, with lubricating grease weight for benchmark, consist of: non-newtonian fluid calcium naphthenate 39.6%; Lubricating base oil 54.2%; 12-oxystearic acid calcium 2.0%; Terephthalic acid calcium 4.0%; Right, right '-di-iso-octyldiphenylamine 0.2%.
Embodiment 5
Feed composition: naphthenate with superhigh base number calcium (total basicnumber is 400mgKOH/g, 30kg); 150BS (15kg); Naphthenic acid (2.8kg); Acetic acid (0.56kg); Ca (OH)
2(1.8kg); 12-oxystearic acid (2kg); Terephthalic acid (3.5kg); 500SN (7kg).
Prepare overbased Composite calcium naphthenate base lubricating grease by the method for example 1, the amount unlike base oil changes to some extent, thus makes each material rate that larger change occur, and each performance data of lubricating grease finished product obtained is in table 1.
In the lubricating grease that the present embodiment obtains, with lubricating grease weight for benchmark, consist of: non-newtonian fluid calcium naphthenate 54.0%; Lubricating base oil 35.6%; 12-oxystearic acid calcium 3.4%; Terephthalic acid calcium 7.0%.
Embodiment 6
Feed composition: naphthenate with superhigh base number calcium (total basicnumber is 400mgKOH/g, 30kg); 150BS (30kg); Witco 1298 Soft Acid (2.8kg); Acetic acid (0.56kg); Ca (OH)
2(1.8kg); 12-oxystearic acid (2kg); Terephthalic acid (3.5kg); 500SN (17kg).
Prepare overbased Composite calcium naphthenate base lubricating grease by the method for example 1, replace naphthenic acid unlike the use of Witco 1298 Soft Acid and use full synthetic oil poly & Alpha ,-olefin oil PAO 10 (100 ° of C kinematic viscosity are 11mm
2/ s) and PAO 40 (100 ° of C kinematic viscosity are 41mm
2/ s) replace 500SN and 150BS respectively, each performance data of lubricating grease finished product obtained is in table 1.
Embodiment 7
Feed composition: overbased calcium alkyl-salicylate (total basicnumber is 320mgKOH/g, 30kg); 150BS (30kg); Naphthenic acid (2.8kg); Acetic acid (0.56kg); Ca (OH)
2(1.8kg); 12-oxystearic acid (2kg); 2-methyl isophthalic acid, 4-phthalic acid (3.8kg); 500SN (16.7kg).
Prepare high base number Composite calcium naphthenate base lubricating grease by the method for example 1, unlike the use of the total basicnumber of overbased calcium alkyl-salicylate be 320mgKOH/g, each performance data of lubricating grease finished product obtained is in table 1.
Embodiment 8
Feed composition: overbased calcium alkyl-salicylate (total basicnumber is 360mgKOH/g, 30kg); 150BS (30kg); Naphthenic acid (2.8kg); Acetic acid (0.56kg); Ca (OH)
2(1.8kg); 12-oxystearic acid (2kg); 4,4'-biphenyl dicarboxylic acid (5.1kg); 500SN (20kg); Right, right '-di-iso-octyldiphenylamine (0.2kg); Dithio dialkyl amido formic acid molybdenum (4kg); Selenium Sulfide (4kg); Benzotriazole (0.4kg).
Prepare high base number Composite calcium naphthenate base lubricating grease by the method for example 1, unlike the use of the total basicnumber of overbased calcium alkyl-salicylate be 360mgKOH/g, and add certain additive, each performance data of lubricating grease finished product obtained is in table 1.
In the lubricating grease that the present embodiment obtains, with lubricating grease weight for benchmark, consist of: non-newtonian fluid calcium naphthenate 33.4%; Lubricating base oil 50.0%; 12-oxystearic acid calcium 2.1%; 4,4'-biphenyl dicarboxylic acid calcium 5.9%; Right, right '-di-iso-octyldiphenylamine 0.2%; Dithio dialkyl amido formic acid molybdenum 4.0%; Selenium Sulfide 4.0%; Benzotriazole 0.4%.
Embodiment 9
Feed composition: naphthenate with superhigh base number calcium (total basicnumber is 400mgKOH/g, 30kg); 150BS (15kg); Naphthenic acid (2.8kg); Acetic acid (0.56kg); Ca (OH)
2(1.8kg); 12-oxystearic acid (2kg); Terephthalic acid (3.5kg); 500SN (32kg).
Prepare overbased Composite calcium naphthenate base lubricating grease by the method for example 1, unlike not containing oxidation inhibitor pair, right '-di-iso-octyldiphenylamine, the amount of base oil also changes to some extent, and each performance data of lubricating grease finished product obtained is in table 1.
In the lubricating grease that the present embodiment obtains, with lubricating grease weight for benchmark, consist of: non-newtonian fluid calcium naphthenate 38.4%; Lubricating base oil 54.2%; 12-oxystearic acid calcium 2.4%; Terephthalic acid calcium 5.0%.
Embodiment 10
Feed composition: overbased calcium alkyl-salicylate (total basicnumber is 360mgKOH/g, 30kg); 150BS (30kg); Witco 1298 Soft Acid (2.8kg); Acetic acid (0.56kg); Ca (OH)
2(3.3kg); 12-oxystearic acid (2kg); Boric acid (2.32kg); Terephthalic acid (3.5kg); 500SN (15kg); Right, right '-di-iso-octyldiphenylamine (0.2kg).
A volume be 110L and with heating, stir, circulation, cooling normal-pressure reaction kettle in add naphthenate with superhigh base number calcium that 30kg total basicnumber is 360mgKOH/g and 30kg 100 ° of C kinematic viscosity are 31mm
2the HVI150BS lubricating base oil of/s, stirs, heats to 50 ° of C, constant temperature 10 minutes; Add 2.8kg naphthenic acid, temperature controls at 50 ° of about C, stirs 10 minutes; Add the acetic acid of 0.56kg and the aqueous solution of acetic acid weight 4 times, stir 10 minutes; Be warmed up to 60 ° of C, constant temperature 90 minutes, material retrogradation; Add 3.3kgCa (OH)
2and with 4 times of water-reducible suspension liquids, stir 10 minutes; Add 2kg12-oxystearic acid, stir 10 minutes; Add 2.32kg boric acid, stir 10 minutes; Add 3.5kg terephthalic acid, stir, be warmed up to 110 ° of C under stirring, keep 60 minutes, dehydration; 120 ° of C constant temperature 20 minutes, is warmed up to 200 ° of C constant temperature 5 minutes.Then, be cooled to 160 ° of C, the 100 ° of C kinematic viscosity adding 15kg are 11mm
2the HVI500SN lubricating base oil of/s; Treat that temperature is cooled to 110 ° of C, add and account for lubricating grease weight 0.2kg couple, after right '-di-iso-octyldiphenylamine stirs 10 minutes, circulating filtration, homogenizing, degassedly obtain finished product.Assay is in table 1.
In the lubricating grease that the present embodiment obtains, with lubricating grease weight for benchmark, consist of: non-newtonian fluid calcium naphthenate 38.2%; Lubricating base oil 51.5%; 12-oxystearic acid calcium 2.5%; Lime borate 2.7%; Terephthalic acid calcium 4.9%; Right, right '-di-iso-octyldiphenylamine (0.2kg) 0.2%.
Embodiment 11
Feed composition: overbased calcium alkyl-salicylate (total basicnumber is 360mgKOH/g, 30kg); 150BS (30kg); Naphthenic acid (2.8kg); Acetic acid (0.56kg); Ca (OH)
2(3kg); 12-oxystearic acid (2kg); Terephthalic acid (3.5kg); Acetic acid (2kg); 500SN (14kg); Right, right '-di-iso-octyldiphenylamine (0.2kg).
Prepare high base number Composite calcium naphthenate base lubricating grease by the method for example 10, change acetic acid into unlike boric acid, each performance data of lubricating grease finished product obtained is in table 1.
In the lubricating grease that the present embodiment obtains, with lubricating grease weight for benchmark, consist of: non-newtonian fluid calcium naphthenate 38.5%; Lubricating base oil 50.8%; 12-oxystearic acid calcium 2.4%; Terephthalic acid calcium 5.0%; Lime acetate 3.1%; Right, right '-di-iso-octyldiphenylamine 0.2%.
Comparative example
Feed composition: calcium sulfonate with high base number (320mgKOH/g, 30kg); 150BS (20kg); Witco 1298 Soft Acid (2.8kg); Acetic acid (0.56kg); Ca (OH)
2(1.8kg); 12-oxystearic acid (2kg); Boric acid (2.32kg); 500SN (28kg); Right, right '-di-iso-octyldiphenylamine (0.2kg).
Prepare high base number composite calcium sulfonate base grease by the method for example 1, replace unlike newton's body calcium naphthenate calcium sulfonate with high base number in reactant, each performance data of lubricating grease finished product obtained is in table 1.
In the lubricating grease that this example obtains, with lubricating grease weight for benchmark, consist of: non-newtonian fluid calcium sulphonate 38.5%; Lubricating base oil 55.4%; 12-oxystearic acid calcium 2.4%; Lime borate 3.7%.
Table 1 each lubricating grease properties of sample data
Continued
As seen from Table 1, adopt high base number naphthenic acid to be better than as the performance of the lubricating grease prepared by raw material the lubricating grease adopted prepared by calcium sulfonate with high base number, especially in water resisting property and adhesion, have unique advantage especially, this is the result expected useless.
Claims (16)
1. a Composite calcium naphthenate base lubricating grease, with lubricating grease weight for benchmark, comprising:
1) non-newtonian fluid calcium naphthenate 10%-70%; 2) the calcium salt 1%-10% of higher fatty acid; 3) the calcium salt 1%-15% of aromatic acid; 4) lubricating base oil 10%-80%.
2. according to lubricating grease according to claim 1, wherein with lubricating grease weight for benchmark, comprise following component:
1) non-newtonian fluid calcium naphthenate 20%-60%; 2) the calcium salt 2%-6% of higher fatty acid; 3) the calcium salt 2%-10% of aromatic acid; 4) lubricating base oil 20%-70%.
3., according to lubricating grease according to claim 1, described non-newtonian fluid calcium naphthenate is at infrared spectrum 873cm
-1-886cm
-1there is crystal form calcium carbonate charateristic avsorption band in place, its total basicnumber is 250mgKOH/g-450mgKOH/g.
4. according to lubricating grease according to claim 1, straight chain fatty acid or the hydroxy fatty acid of said higher fatty acid to be carbon number be 8-20.
5., according to lubricating grease according to claim 1, said higher fatty acid is selected from one or more mixtures in lauric acid, palmitinic acid, stearic acid, 12-oxystearic acid, eicosyl carboxylic acid.
6., according to lubricating grease according to claim 1, described aromatic acid is the carboxylic acid having at least 1 carboxyl to be directly connected with aromatic ring, and other substituting group can be the alkyl or aryl of hydrogen, alkyl, thiazolinyl, alkynyl, aryl, halo or perhalogeno, and molecular weight is less than 550.
7., according to lubricating grease according to claim 1, described aromatic acid is selected from one or more in phthalic acid that unsubstituted or C1-C5 alkyl replaces, m-phthalic acid, terephthalic acid, biphenyl dicarboxylic acid, santowax dioctyl phthalate.
8., according to lubricating grease according to claim 1, wherein also contain the calcium salt of small molecules mineral acid and/or small molecules lipid acid, described small molecules mineral acid and/or small molecules fatty acid molecule amount are less than or equal to 150.
9. according to lubricating grease according to claim 1, said small molecules mineral acid is selected from the mixture of one or more in boric acid, phosphoric acid, sulfuric acid, and said small molecules lipid acid is selected from the mixture of one or more in acetic acid, oxalic acid, propionic acid, propanedioic acid, butyric acid, succinic acid.
10. one of claim 1 ~ 9 described Composite calcium naphthenate base preparation of greases method, comprising:
(1) newton's body calcium naphthenate, part basis oil and transforming agent are mixed, heat, make material retrogradation;
(2) add lime or calcium hydroxide, add higher fatty acid and aromatic acid respectively, cooling after the dehydration that heats up;
(3) be warmed up to 200 ° of C-220 ° of C constant temperature refinings, cooling, adds surplus base oil, adds necessary additive, obtains finished product.
11. according to preparation method according to claim 10, in step (1), by newton's body calcium naphthenate, part basis oil Hybrid Heating to 50 ° of C-90 ° of C, constant temperature 10 minutes-30 minutes, add required transforming agent successively to react, add rear stirring about 10 minutes at every turn, react fully, 60 ° of C-100 ° of C constant temperature 0.5 hour-3 hours, make material retrogradation.
12. according to preparation method according to claim 10, in step (2), add the suspension liquid of lime or calcium hydroxide at 85 ° of C-100 ° of C, add higher fatty acid at 85 ° of C-100 ° of C, stir 5 minutes-20 minutes, add small molecules mineral acid and/or the small molecules lipid acid of aromatic acid and necessity, stir 5 minutes-20 minutes, be warmed up to 105 ° of C-120 ° of C, dehydration, cool to 90 ° of C-105 ° of C, the order of its Fatty Acids and small molecules acid can exchange.
13. according to preparation method according to claim 10, in step (3), heats up to the product of step (3), 100 ° of C-120 ° of C constant temperature 10 minutes-20 minutes, is finally warmed up to 200 ° of C-220 ° of C constant temperature 5 minutes-10 minutes; Be cooled to 150 ° of C-160 ° of C, add surplus lubricating base oil, treat that temperature is cooled to 100 ° of C-120 ° of C, add necessary additive, stir, circulating filtration, homogenizing, degassed.
14. according to preparation method according to claim 10, and described newton's body calcium naphthenate is petroleum naphthenic acid calcium or synthesis calcium naphthenate, and its total basicnumber is 250mgKOH/g-450mgKOH/g.
15. according to preparation method according to claim 10, said transforming agent is selected from fatty alcohol, lipid acid, aliphatic ketone, alkanoic, aliphatic amide, cycloalkanes amine, cycloalkanol, the ether of C1-C5, and boric acid, calcium carbonate, phosphonic acids, carbonic acid gas, phenol, aromatic alcohol, aromatic amine, C8-C20 alkyl benzene sulphonate (ABS), C16-C62 naphthenic acid, one or more in water, the add-on of transforming agent is the 2%-30% of newton's body calcium naphthenate weight.
16. according to preparation method according to claim 10, said transforming agent is selected from one or more in Witco 1298 Soft Acid, methyl alcohol, Virahol, butanols, C20-C40 naphthenic acid, acetic acid and water, and the add-on of transforming agent is the 6%-22% of newton's body calcium naphthenate weight.
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