CN100404655C - Composite lithium base lubricant and its preparing method - Google Patents
Composite lithium base lubricant and its preparing method Download PDFInfo
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- CN100404655C CN100404655C CNB2003101134895A CN200310113489A CN100404655C CN 100404655 C CN100404655 C CN 100404655C CN B2003101134895 A CNB2003101134895 A CN B2003101134895A CN 200310113489 A CN200310113489 A CN 200310113489A CN 100404655 C CN100404655 C CN 100404655C
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- Prior art keywords
- acid
- grease
- base oil
- lipid
- weight
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 6
- 239000000314 lubricant Substances 0.000 title description 3
- 239000002131 composite material Substances 0.000 title 1
- 239000002253 acid Substances 0.000 claims abstract description 49
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims abstract description 42
- 239000004519 grease Substances 0.000 claims abstract description 41
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 30
- 239000011575 calcium Substances 0.000 claims abstract description 30
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 29
- 230000001050 lubricating effect Effects 0.000 claims abstract description 20
- 239000002199 base oil Substances 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- -1 C24 fatty acids Chemical class 0.000 claims abstract description 13
- 150000001875 compounds Chemical class 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 238000007127 saponification reaction Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910021532 Calcite Inorganic materials 0.000 claims abstract description 11
- 230000001131 transforming effect Effects 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 8
- 239000000344 soap Substances 0.000 claims abstract description 8
- 239000013078 crystal Substances 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims abstract description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 19
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- 150000002632 lipids Chemical class 0.000 claims description 14
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims description 12
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 10
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 230000018044 dehydration Effects 0.000 claims description 8
- 238000006297 dehydration reaction Methods 0.000 claims description 8
- BKIMMITUMNQMOS-UHFFFAOYSA-N nonane Chemical compound CCCCCCCCC BKIMMITUMNQMOS-UHFFFAOYSA-N 0.000 claims description 8
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 7
- 150000007520 diprotic acids Chemical class 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000005639 Lauric acid Substances 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 6
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 6
- 239000004327 boric acid Substances 0.000 claims description 6
- JFCQEDHGNNZCLN-UHFFFAOYSA-N glutaric acid Chemical compound OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 claims description 6
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims description 6
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims description 6
- WLJVNTCWHIRURA-UHFFFAOYSA-N pimelic acid Chemical compound OC(=O)CCCCCC(O)=O WLJVNTCWHIRURA-UHFFFAOYSA-N 0.000 claims description 6
- TYFQFVWCELRYAO-UHFFFAOYSA-N suberic acid Chemical compound OC(=O)CCCCCCC(O)=O TYFQFVWCELRYAO-UHFFFAOYSA-N 0.000 claims description 6
- 235000011054 acetic acid Nutrition 0.000 claims description 5
- 235000012204 lemonade/lime carbonate Nutrition 0.000 claims description 5
- 235000019260 propionic acid Nutrition 0.000 claims description 5
- 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 5
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 4
- HNNQYHFROJDYHQ-UHFFFAOYSA-N 3-(4-ethylcyclohexyl)propanoic acid 3-(3-ethylcyclopentyl)propanoic acid Chemical compound CCC1CCC(CCC(O)=O)C1.CCC1CCC(CCC(O)=O)CC1 HNNQYHFROJDYHQ-UHFFFAOYSA-N 0.000 claims description 4
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 claims description 4
- 235000021355 Stearic acid Nutrition 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 claims description 4
- 239000008117 stearic acid Substances 0.000 claims description 4
- SXNBVULTHKFMNO-UHFFFAOYSA-N 2,2-dihydroxyoctadecanoic acid Chemical class CCCCCCCCCCCCCCCCC(O)(O)C(O)=O SXNBVULTHKFMNO-UHFFFAOYSA-N 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 3
- CUBCNYWQJHBXIY-UHFFFAOYSA-N benzoic acid;2-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=CC=C1.OC(=O)C1=CC=CC=C1O CUBCNYWQJHBXIY-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 235000011089 carbon dioxide Nutrition 0.000 claims description 3
- RXKJFZQQPQGTFL-UHFFFAOYSA-N dihydroxyacetone Chemical compound OCC(=O)CO RXKJFZQQPQGTFL-UHFFFAOYSA-N 0.000 claims description 3
- 125000006527 (C1-C5) alkyl group Chemical group 0.000 claims description 2
- JYDYHSHPBDZRPU-UHFFFAOYSA-N 3-methylcyclohexan-1-amine Chemical compound CC1CCCC(N)C1 JYDYHSHPBDZRPU-UHFFFAOYSA-N 0.000 claims description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 claims description 2
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 claims description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 2
- 150000003973 alkyl amines Chemical class 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 150000004982 aromatic amines Chemical class 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 150000003009 phosphonic acids Chemical class 0.000 claims description 2
- 125000000373 fatty alcohol group Chemical group 0.000 claims 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 abstract description 14
- 239000003921 oil Substances 0.000 abstract description 14
- 229910000019 calcium carbonate Inorganic materials 0.000 abstract description 7
- 150000007513 acids Chemical class 0.000 abstract description 6
- 239000000654 additive Substances 0.000 abstract description 5
- 239000000084 colloidal system Substances 0.000 abstract description 4
- 230000002349 favourable effect Effects 0.000 abstract description 3
- 239000002562 thickening agent Substances 0.000 abstract description 3
- 235000014113 dietary fatty acids Nutrition 0.000 abstract description 2
- 229930195729 fatty acid Natural products 0.000 abstract description 2
- 239000000194 fatty acid Substances 0.000 abstract description 2
- 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 abstract 2
- 239000003925 fat Substances 0.000 abstract 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 abstract 1
- 238000010521 absorption reaction Methods 0.000 description 7
- 238000003756 stirring Methods 0.000 description 6
- 238000010792 warming Methods 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 230000009466 transformation Effects 0.000 description 5
- 230000000996 additive effect Effects 0.000 description 4
- 150000002148 esters Chemical class 0.000 description 4
- 229910003002 lithium salt Inorganic materials 0.000 description 4
- FYHXNYLLNIKZMR-UHFFFAOYSA-N calcium;carbonic acid Chemical compound [Ca].OC(O)=O FYHXNYLLNIKZMR-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 150000002191 fatty alcohols Chemical class 0.000 description 2
- 159000000002 lithium salts Chemical class 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 241000158728 Meliaceae Species 0.000 description 1
- 229920002396 Polyurea Polymers 0.000 description 1
- 150000004996 alkyl benzenes Chemical class 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000002288 cocrystallisation Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- SMBQBQBNOXIFSF-UHFFFAOYSA-N dilithium Chemical class [Li][Li] SMBQBQBNOXIFSF-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- VLHZUYUOEGBBJB-UHFFFAOYSA-N hydroxy stearic acid Natural products OCCCCCCCCCCCCCCCCCC(O)=O VLHZUYUOEGBBJB-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000005956 quaternization reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- RIUWBIIVUYSTCN-UHFFFAOYSA-N trilithium borate Chemical class [Li+].[Li+].[Li+].[O-]B([O-])[O-] RIUWBIIVUYSTCN-UHFFFAOYSA-N 0.000 description 1
Abstract
The present invention relates to compound lithium grease which comprises 20 to 60% of calcium sulphonate with high alkalinity, 3 to 15% of thickening agent and lubricating basic oil as the rest, wherein calcium carbonate is solid particles existing in the forms of calcite crystals and dispersed colloids, and the thickening agent is composed of compound lithium soap. The grease has the preparation method that newtonian calcium sulphonate with high alkalinity, transforming agents and base oil are mixed and heated until the materials are thickened, the materials, together with a lithium hydroxide solution, carry out a saponification reaction after C12 to C24 fatty acids and auxiliary acids are added, and the mixed solution is cooled into fats after the processes of temperature rise and dewatering. Under the condition of no other additives, the compound lithium grease of the present invention has favorable mechanical stability, colloid stability, water resistance, rust protection and high temperature service property.
Description
Technical field
The present invention relates to lubricant, exactly is complex lithium grease and preparation method thereof.
Background technology
Lubricating grease is a kind of lubricant that mechanical means is often used when lubricated, occupies very consequence in industrial production is used.Compositing lithio ester came out in 1962, and developing into has become the very important lubricating grease of a class now, and the annual production proportion is ascendant trend year by year.The viscosifying agent of complex lithium grease is formed by polymer fatty acid lithium soap and low molecular acid lithium salts cocrystallization, but, the use properties of basis fat often can not satisfy actual needs, so have lot of documents, patent discussion other compound of interpolation or various additive to improve the use properties of complex lithium grease.
The complex lithium grease that Chinese patent CN1055384A mentions is by 12 oxystearic acid lithium soaps, the complex thickener of diprotic acid lithium salts and boric acid lithium salts, naphthenic acid lithium salts and other have the additive of property to be formed, and has the favorable mechanical stability, water resisting property and high-temperature stability.
The viscosifying agent of the complex lithium grease that U.S. Pat 4897210 is introduced is made up of the lithium salts of 12 oxystearic acids and the dilithium salt of terephthalic acid, can improve dropping point.But the lubricating grease of two patents preparation need add additive, and its use properties still remains to be improved.
High alkaline calcium sulfonate is widely used in the internal combustion (IC) engine lubricating oil as purification agent.High alkaline calcium sulfonate is by mahogany acid or alkyl benzene sulphonate (ABS) and calcium hydroxide neutralization, and carries out carbonating and high quaternization makes.Eighties of last century the seventies has the people that high alkaline calcium sulfonate is transformed in lubricating base oil and lubricating grease is made in multiviscosisty, and unformed carbonic acid calcium wherein is converted into the calcite crystal habit and exists and with colloidal form dispersive lime carbonate solid particulate.Later have the performance of many pieces of patent p-sulfonic acid calcium grease to improve again, for example, CN1414076A discloses a kind of with polyureas and calcium sulphonate compound lubricating grease, but does not find as yet complex lithium grease and high alkaline calcium sulfonate are moistened the report of compound use.
Summary of the invention
The purpose of this invention is to provide a kind of complex lithium grease that contains high alkaline calcium sulfonate, this complex lithium grease has good mechanical stability, colloid stability, anti-water, antirust and high temperature use properties.
Another object of the present invention provides above-mentioned preparing complex lithium grease.
Complex lithium grease provided by the invention comprises following component (by weight):
A) high alkaline calcium sulfonate 20-60%, lime carbonate wherein exist and with colloidal form dispersed solids particle with the calcite crystal habit;
B) the viscosifying agent 3-15% of compound lithium soap composition;
C) base oil, surplus.
The base number of said high alkaline calcium sulfonate is generally 260-360mgKOH/g.Commercially available high alkaline calcium sulfonate belongs to Newtonian fuid, contains unformed carbonic acid calcium in the product, at 862cm
-1The infrared signature absorption peak that unformed lime carbonate is arranged; Under the effect of transforming agent, unformed carbonic acid calcium wherein is converted into the calcite crystal habit and exists and with colloidal form dispersive lime carbonate solid particulate, at 881-886cm
-1The infrared signature absorption peak of calcite type calcium carbonate is arranged, and at this moment, high alkaline calcium sulfonate changes non-Newtonian fluid into by Newtonian fuid.The content of high alkaline calcium sulfonate in lubricating grease is 20-60%, preferred 30-50%.
Said compound lithium soap is by a kind of C
12-C
24Lipid acid and at least a auxiliary acid and lithium hydroxide aqueous solution saponification form.C wherein
12-C
24The preferred lauric acid of lipid acid, ten dihydroxystearic acids, stearic acid, said auxiliary acid is to be selected from C
1-C
22In lipid acid, boric acid, phosphoric acid, aromatic acid, naphthenic acid and diprotic acid or the polyprotonic acid one or more.Wherein, C
1-C
22The preferred acetate of lipid acid, propionic acid, n-caprylic acid, lauric acid, the preferred phthalic acid of aromatic acid, terephthalic acid, Whitfield's ointment etc., the preferred pentanedioic acid of diprotic acid, hexanodioic acid, pimelic acid, suberic acid, nonane diacid, sebacic acid etc.
The content of compound lithium soap in lubricating grease is 3-15%, preferred 5-12%.
The used base oil of the present invention can be Dormant oils, synthetic oil or their mixture, and 100 ℃ of kinematic viscosity are 6-33mm
2/ s, preferred 14-20mm
2/ s.
Preparing complex lithium grease provided by the invention comprises: newton's height alkaline sulfoacid calcium is converted into the non-newtonian fluid high alkaline calcium sulfonate, adds C
12-C
24Lipid acid and at least a auxiliary acid and lithium hydroxide aqueous solution carry out saponification reaction, and the dehydration that heats up is cooled to fat.
Specifically, preparing complex lithium grease provided by the invention may further comprise the steps:
1) transform: newton's height alkaline sulfoacid calcium, transforming agent and base oil are mixed, stir, and heat temperature raising is to 70-100 ℃, and preferred 80-95 ℃, the maintenance certain hour was generally 0.5-1.5 hour, until the material retrogradation.With the Fourier transformation infrared spectrometer test, at 881-886cm
-1The absorption peak that calcite type calcium carbonate is arranged.
Newton's height alkaline sulfoacid calcium is converted into the non-newtonian fluid high alkaline calcium sulfonate, can carry out according to the prior art disclosed method, transforming agent wherein can be that carbon number is the Fatty Alcohol(C12-C14 and C12-C18) of C1-C5, lipid acid, aliphatic ketone, the method of opening is carried out, transforming agent wherein can be that carbon number is the Fatty Alcohol(C12-C14 and C12-C18) of C1-C5, lipid acid, aliphatic ketone, alkanoic, low molecule ether, alkylamine, and water, boric acid, alkyl or aryl phosphoric acid, phosphonic acids, carbonic acid gas, phenol, cycloalkanol, aromatic alcohol, the cycloalkanes amine that the C1-C5 alkyl replaces, aromatic amine etc., also can be the mixture of above-mentioned two or more compound, preferable formic acid, acetic acid, propionic acid, methyl alcohol, ethanol, Virahol, n-propyl alcohol, ethylene glycol monomethyl ether, phenol, acetaldehyde, ketone, methylamine, ethamine, propylamine, the 3-methyl cyclohexylamine, the mixture of two or more in the compound such as aniline and water.
The consumption of transforming agent is the 5-60% of newton's height alkaline sulfoacid calcium weight, preferred 10-45%, more preferably 10-30%.
The consumption of base oil is the 20-80% of grease base oil gross weight in the conversion reaction, preferred 30-55%.
2) add base oil, a kind of C in product saponification: 1)
12-C
24Lipid acid and at least a auxiliary acid, the aqueous solution that slowly adds lithium hydroxide in 90-100 ℃ of scope carries out saponification reaction.
Said C
12-C
24The preferred lauric acid of lipid acid, ten dihydroxystearic acids, stearic acid.
Said auxiliary acid is to be selected from C
1-C
22In lipid acid, boric acid, phosphoric acid, aromatic acid, naphthenic acid and diprotic acid or the polyprotonic acid one or more.Wherein, C
1-C
22The preferred acetate of lipid acid, propionic acid, n-caprylic acid, lauric acid, the preferred phthalic acid of aromatic acid, terephthalic acid, Whitfield's ointment etc., the preferred pentanedioic acid of diprotic acid, hexanodioic acid, pimelic acid, suberic acid, nonane diacid, sebacic acid etc.
C
12-C
24The ratio of lipid acid and auxiliary acid (weight) is 1: 0.1-1: 1, preferably 1: 0.2-1: 0.8.
Acid and lithium hydroxide carry out the equivalent reaction, and lithium hydroxide also can be suitably excessive.
The consumption of base oil is the 5-40% of grease base oil gross weight in the saponification reaction, preferred 15-25%.
3) product heating one-tenth fat: with 2) up to dehydration fully, is warming up to 190-220 ℃, adds base oil and cools off, and circulation is stirred and added base oil adjustment denseness down.
Complex lithium grease provided by the invention promptly has favorable mechanical stability, colloid stability, anti-water, rust-preventing characteristic and high temperature use properties under the situation that does not add other additive.
Embodiment
Embodiment 1
With the 400g base number is that the high alkaline calcium sulfonate of 280mgKOH/g joins in the 500SN Dormant oils of 200g, is heated to 80-95 ℃, adds 38.5g water and 5.4g acetic acid, treats the material retrogradation, with the Fourier transformation infrared spectrometer test, at 881-886cm
-1There is the absorption peak of calcite type calcium carbonate at the place, the 500SN Dormant oils that adds 150g, 12 oxystearic acids and the 12.5g sebacic acid that add 37.5g, in the time of 90-100 ℃, slowly drip the aqueous solution of 10.8g lithium hydroxide, after the saponification dehydration, be warming up to 200 ℃, the 500SN Dormant oils that adds 160g, stir, be chilled to room temperature, grind evenly.The physical and chemical performance analysis of the lubricating grease of doing the results are shown in Table 1.
Embodiment 2
With the 300g base number is that the high alkaline calcium sulfonate of 300mgKOH/g joins in the 500SN Dormant oils of 180g, is heated to 80-95 ℃, adds 40g water and 6g ethanol, treats the material retrogradation, with the Fourier transformation infrared spectrometer test, at 881-886cm
1There is the absorption peak of calcite type calcium carbonate at the place, the 750ZN Dormant oils that adds 150g, the stearic acid and the 27.2g hexanodioic acid that add 54.4g, in the time of 90-100 ℃, slowly drip the aqueous solution of 20.9g lithium hydroxide, after the saponification dehydration, be warming up to 210 ℃, the 150BS Dormant oils that adds 200g, stir, be chilled to room temperature, grind evenly.The physical and chemical performance analysis of the lubricating grease of doing the results are shown in Table 1.
Embodiment 3
With the 280g base number is that the high alkaline calcium sulfonate of 280mgKOH/g joins in the poly-a-olefin oil of 200g, be heated to 80-95 ℃, add 50g water, 11.2g acetic acid and 14.3g ethylene glycol monomethyl ether, treat the material retrogradation, with the Fourier transformation infrared spectrometer test, at 881-886cm
-1There is the absorption peak of calcite type calcium carbonate at the place, the poly-a-olefin oil that adds 90g, 12 oxystearic acids and the 20.6g nonane diacid that add 42.6g, in the time of 90-100 ℃, slowly drip the aqueous solution of 21.8g lithium hydroxide, after the saponification dehydration, be warming up to 200 ℃, the 500SN Dormant oils that adds 200g, stir, be chilled to room temperature, grind evenly.The physical and chemical performance analysis of the lubricating grease of doing the results are shown in Table 1.
Embodiment 4
With the 380g base number is that the high alkaline calcium sulfonate of 290mgKOH/g joins in the 500DN Dormant oils of 250g, is heated to 80-95 ℃, adds 4.3g acetic acid and 12.9g ethylene glycol monomethyl ether, at the uniform velocity logical carbonic acid gas, treat the material retrogradation, with the Fourier transformation infrared spectrometer test, at 881-886cm
-1There is the absorption peak of calcite type calcium carbonate at the place, the 500DN that adds 95g, 12 oxystearic acids and the 14.3g terephthalic acid that add 43g, in the time of 90-100 ℃, slowly drip the aqueous solution of 10.8g lithium hydroxide, after the saponification dehydration, be warming up to 200 ℃, the 500DN that adds 165g, stir, be chilled to room temperature, grind evenly.The physical and chemical performance analysis of the lubricating grease of doing the results are shown in Table 1.
Comparative Examples 1
This Comparative Examples is the preparation of the common compositing lithio ester of prior art.
In the 500SN Dormant oils still that 12 oxystearic acids and the 18.3g sebacic acid of 60.2g joined 300g, be heated to 80-95 ℃, slowly drip the aqueous solution of 18.1g lithium hydroxide, after the saponification dehydration, add the 500SN of 200g, be warming up to 200 ℃, the 500SN that adds 300g, stir, be chilled to room temperature, grind evenly.The physical and chemical performance analysis of the lubricating grease of doing the results are shown in Table 1.
As can be seen from Table 1, the salient features of compositing lithio ester provided by the invention all is better than the performance according to the common compositing lithio ester of prior art for preparing.
The physicochemical property check data of each embodiment lubricating grease of table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative Examples 1 | Test method | |
| The Drawing cone in-degree, 0.1mm | 310 | 300 | 298 | 289 | 295 | GB/T269 |
| Prolong Drawing cone in-degree (100,000 times), 0.1mm | 323 | 315 | 315 | 305 | 326 | GB/T269 |
| Dropping point, ℃ | 297 | 305 | 320 | 311 | 284 | GB/T3498 |
| Corrosion (the T2 copper sheet, 100 ℃, 24h) | Qualified | Qualified | Qualified | Qualified | Qualified | GB/T7326 second method |
| Stencil oil-dividing (100 ℃, 24h), % | 0.91 | 1.1 | 1.5 | 0.86 | 2.54 | SH/T0324 |
| Water pouring number of dropouts (38 ℃, 1h), % | 0.96 | 0.65 | 0.78 | 1.24 | 16.44 | SH/T0109 |
Claims (12)
1. complex lithium grease by weight, comprises following component:
A) high alkaline calcium sulfonate 20-60%, lime carbonate wherein exist and with colloidal form dispersed solids particle with the calcite crystal habit;
B) the viscosifying agent 3-15% of compound lithium soap composition;
C) base oil, surplus.
2. according to the described lubricating grease of claim 1, it is characterized in that the base number of said high alkaline calcium sulfonate is 260-360mgKOH/g.
3. according to the described lubricating grease of claim 1, it is characterized in that the weight content of high alkaline calcium sulfonate in lubricating grease is 30-50%.
4. according to the described lubricating grease of claim 1, it is characterized in that the weight content of compound lithium soap in lubricating grease is 5-12%.
5. the described preparation of greases method of claim 1 comprises: newton's height alkaline sulfoacid calcium, transforming agent and base oil are mixed, are heated to 70-100 ℃ and carry out conversion reaction, until the material retrogradation, add C
12-C
24Lipid acid and auxiliary acid and lithium hydroxide aqueous solution carry out saponification reaction at 90-100 ℃, dehydration heats up, be cooled to fat, wherein transforming agent is that carbon number is Fatty Alcohol(C12-C14 and C12-C18), lipid acid, aliphatic ketone, alkanoic, ether, the alkylamine of C1-C5, the perhaps cycloalkanes amine, the aromatic amine that replace of water, boric acid, alkyl or aryl phosphoric acid, phosphonic acids, carbonic acid gas, phenol, cycloalkanol, aromatic alcohol, C1-C5 alkyl, or the mixture of above-mentioned two or more compound, auxiliary acid is selected from C
1-C
22In lipid acid, boric acid, phosphoric acid, aromatic acid, naphthenic acid and diprotic acid or the polyprotonic acid one or more, the consumption of transforming agent is the 5-60% of newton's height alkaline sulfoacid calcium weight, the consumption of base oil is the 20-80% of grease base oil gross weight in the conversion reaction, C
12-C
24The part by weight of lipid acid and auxiliary acid is 1: 0.1-1: 1, and acid and lithium hydroxide equivalent or lithium hydroxide are excessive.
6. according to the described preparation method of claim 5, it is characterized in that said transforming agent is two or more the mixture in formic acid, acetic acid, propionic acid, methyl alcohol, ethanol, Virahol, n-propyl alcohol, ethylene glycol monomethyl ether, phenol, acetaldehyde, ketone, methylamine, ethamine, propylamine, 3-methyl cyclohexylamine, aniline and the water.
7. according to the described preparation method of claim 5, it is characterized in that the consumption of base oil is the 30-55% of grease base oil gross weight in the conversion reaction.
8. according to the described preparation method of claim 5, it is characterized in that the consumption of transforming agent is the 10-45% of newton's height alkaline sulfoacid calcium weight.
9. according to the said preparation method of claim 5, it is characterized in that C
12-C
24Lipid acid is selected from lauric acid, ten dihydroxystearic acids, stearic acid.
10. according to the said preparation method of claim 5, it is characterized in that auxiliary acid is selected from C
1-C
22In lipid acid, boric acid, phosphoric acid, aromatic acid, naphthenic acid and diprotic acid or the polyprotonic acid one or more.
11., it is characterized in that C according to the said preparation method of claim 13
1-C
22Lipid acid is selected from acetate, propionic acid, n-caprylic acid, lauric acid; Aromatic acid is selected from phthalic acid, terephthalic acid, Whitfield's ointment; Diprotic acid is selected from pentanedioic acid, hexanodioic acid, pimelic acid, suberic acid, nonane diacid, sebacic acid.
12., it is characterized in that C according to the described preparation method of claim 5
12-C
24The ratio of lipid acid and auxiliary acid is 1: 0.2-1: 0.8.
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| CN101153239B (en) * | 2007-08-27 | 2010-12-01 | 无锡市高润杰化学有限公司 | Method for producing compound sulphonic acid albany grease |
| US11473032B2 (en) | 2010-02-02 | 2022-10-18 | Fuchs Petrolub Se | Constant velocity joint having a boot |
| DE102010006745A1 (en) * | 2010-02-02 | 2011-08-04 | Fuchs Petrolub AG, 68169 | Greases containing lignosulfonate, their preparation and use |
| CN101824357A (en) * | 2010-05-27 | 2010-09-08 | 李墨菊 | High-performance complex calcium sulfonate grease and preparation method thereof |
| CN102433205A (en) * | 2011-10-27 | 2012-05-02 | 无锡惠源高级润滑油有限公司 | Lithium calcium lubricating grease and preparation method thereof |
| CN102433206B (en) * | 2011-10-27 | 2014-08-20 | 无锡惠源高级润滑油有限公司 | Composite lithium-calcium lubricating grease and preparation method thereof |
| CN102766500B (en) * | 2012-07-10 | 2014-01-15 | 华北电力大学 | High-base-number compound-sulfonic lithium/calcium composite lubricating grease and preparation method thereof |
| CN102977979B (en) * | 2012-12-17 | 2014-07-09 | 江苏龙蟠科技股份有限公司 | Composite lithium-calcium base lubricating grease and preparation method thereof |
| CN104194873B (en) * | 2014-07-23 | 2016-08-24 | 中国石油化工股份有限公司 | Power shovel gear lubrication oil/fat composition and preparation method |
| CN104327906A (en) * | 2014-10-25 | 2015-02-04 | 中国石油化工股份有限公司 | Composition of compound calcium sulfonate-based lubricating grease for improving high-temperature performance and preparation method thereof |
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| CN109054965B (en) * | 2018-07-12 | 2021-06-15 | 福建优立盛油脂有限公司 | Low-noise composite lithium-based grease |
| CN108949328B (en) * | 2018-09-05 | 2020-03-10 | 西南交通大学 | Composite calcium sulfonate lubricating grease and preparation method thereof |
| CN111500343B (en) * | 2020-04-21 | 2022-04-29 | 无锡中石油润滑脂有限责任公司 | Composite calcium sulfonate type railway wheel-rail lubricating grease and preparation method thereof |
| CN113046149B (en) * | 2021-03-22 | 2022-09-06 | 华东交通大学 | Lubricating grease containing composite additive and preparation method thereof |
| CN115678633B (en) * | 2022-09-09 | 2023-07-18 | 中国科学院兰州化学物理研究所 | Composite lithium prefabricated thickener and preparation method thereof, lubricating grease composition and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85108441A (en) * | 1985-11-22 | 1987-06-03 | 中国石油化工总公司一坪化工厂 | Composition of compound lithium soap grease and preparation method thereof |
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2003
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85108441A (en) * | 1985-11-22 | 1987-06-03 | 中国石油化工总公司一坪化工厂 | Composition of compound lithium soap grease and preparation method thereof |
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