CN101921650A - Complex lithium grease and preparation method thereof - Google Patents

Complex lithium grease and preparation method thereof Download PDF

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CN101921650A
CN101921650A CN2010102448315A CN201010244831A CN101921650A CN 101921650 A CN101921650 A CN 101921650A CN 2010102448315 A CN2010102448315 A CN 2010102448315A CN 201010244831 A CN201010244831 A CN 201010244831A CN 101921650 A CN101921650 A CN 101921650A
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lithium
grease
base oil
complex
acid lithium
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CN101921650B (en
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陈新国
刘洪涛
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China National Offshore Oil Corp CNOOC
CNOOC Research Institute of Refining and Petrochemicals Beijing Co Ltd
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China National Offshore Oil Corp CNOOC
CNOOC Oil and Gas Development and Utilization Corp
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Abstract

The invention provides complex lithium grease and a preparation method thereof. The complex lithium grease comprises grease base oil, complex lithium thickening agents and surfactants with mass part ratio of (290-1450):(50.4-251.3):(2-10), wherein the grease base oil is at least one of vacuum second line base oil, vacuum third line base oil and vacuum fourth line base oil; the complex lithium thickening agents are formed by C12-C24 fatty acid lithium and auxiliary acid lithium with mass part ratio of (34-70):(16.4-81.3); and the auxiliary acid lithium is any two of C1-C22 fatty acid lithium, lithium borate, lithium phosphate, aromatic acid lithium, lithium naphthenate, dicarboxylic acid lithium and polybasic acid lithium. The invention also provides the preparation method of the complex lithium grease. The surfactants are added to the complex lithium grease to have synergistic effect with soap molecules of the complex lithium grease and further improve the arrangement of the soap molecules and the capability of curing the base oil, thus increasing the dropping point of the grease.

Description

A kind of complex lithium grease and preparation method thereof
Technical field
The present invention relates to refining of petroleum and chemical engineering industry field, be specifically related to a kind of complex lithium grease and preparation method thereof.
Background technology
Complex lithium grease has received increasing concern owing to have higher dropping point with good high-temperature behavior, and its research starts from the sixties in 20th century, and first compound lithium base fat prod of the U.S. passed through test in place in 1962.Compositing lithio ester obtains to develop rapidly since the seventies, contain diprotic acid, boric acid, salicylic compositing lithio ester and be called as " a new generation " lithium saponify, at U.S.'s compositing lithio ester as industrial multiple-effect fat, automobile multiple-effect fat, alkaline-friction bearing fat and widespread use.China is since the Study of Compound Lithium Grease work seventies in 20th century, and successfully in industrial application, has been a kind of very important lubricating grease till now, and proportion rises year by year.But, adopt the complex lithium grease of different base oils preparation can not practical requirement, therefore, people prepare complex lithium grease at dissimilar base oils and have carried out number of research projects.
U.S. Pat P3681242,3929651 and 3711407 has reported the composition and the preparation method of complex lithium grease, adopt 12-hydroxy lithium stearate and diprotic acid or boric acid, salicylic lithium salts two components to be composited, the viscosifying agent of U.S. Pat P4897210 is made up of the lithium salts of 12-oxystearic acid and the dilithium salt of terephthalic acid.
CN89109442.3 has reported a kind of complex lithium grease of high temperature resistant, anti-heavy loading.Its viscosifying agent is the compound soap of 12-oxystearic acid lithium soap, Whitfield's ointment lithium salts and boric acid lithium salts three components.Base oil can be selected Dormant oils, synthetic hydrocarbon oil, ester class oil, silicone oil or its mixing oil.Additive is one group and contains dialkyl group curing carboxylamine metal-salt, compound extreme-pressure anti-friction additives such as nitrogen heterocyclic ring amine salt and tackifier.The dropping point of this lubricating grease is more than 260 ℃, and integrated abrasion value is greater than 588.4N (60kgf), has good high temperature resistant, extreme-pressure anti-wear and adhesion property, can satisfy in-20~200 ℃ of temperature ranges and heavy load conditions under the power lubrication requirement.
Adopt two components or the three component complex lithium greases of prior art preparation, its dropping point generally is lower than 330 ℃, has limited the application of complex lithium grease.
Summary of the invention
The purpose of this invention is to provide higher complex lithium grease of a kind of dropping point and preparation method thereof.
Complex lithium grease of the present invention, comprise grease base oil, compound lithium base viscosifying agent and tensio-active agent, the ratio of quality and the number of copies of described grease base oil, compound lithium base viscosifying agent and tensio-active agent is: (290-1450): (50.4-251.3): (2-10); Described grease base oil is the second line of distillation base oil, subtracts three-way base oil and subtract in the four line base oils at least a; Described compound lithium base viscosifying agent is by C 12-C 24The complex thickener that fatty acid lithium and auxiliary acid lithium are formed, described C 12-C 24The ratio of quality and the number of copies of fatty acid lithium and auxiliary acid lithium is: (34-70): (16.4-81.3); Described auxiliary acid lithium is C 1-C 22In fatty acid lithium, lithium tetraborate, Trilithium phosphate, aromatic acid lithium, naphthenic acid lithium, diprotic acid lithium and the polyprotonic acid lithium any two.
Above-mentioned grease base oil is that cycloalkyl second line of distillation base oil, cycloalkyl subtract three-way base oil and cycloalkyl subtracts in the four line base oils at least a.
Kinematic viscosity during 100 ℃ of above-mentioned grease base oils is 5-40mm 2/ s, preferred 8-26mm 2/ s.
Above-mentioned C 12-C 24Fatty acid lithium can be 12-hydroxy lithium stearate or lithium stearate.
Above-mentioned C 12-C 24The ratio of quality and the number of copies of fatty acid lithium and auxiliary acid lithium specifically can be: (34-46.7): (16.4-22.4) or (46.7-70): (22.4-81.3).
Above-mentioned C 1-C 22Fatty acid lithium can be lithium acetate, propionic acid lithium, n-caprylic acid lithium or lithium laurate.
Above-mentioned aromatic acid lithium can be phthalic acid lithium or lithium salicylate; Above-mentioned diprotic acid lithium can be pentanedioic acid lithium, lithium adipate, pimelic acid lithium, suberic acid lithium, nonane diacid lithium or sebacic acid lithium.
Above-mentioned tensio-active agent can be Dodecyl trimethyl ammonium chloride, palmityl trimethyl ammonium chloride, octadecyl trimethyl ammonium chloride, two octyl alkyl dimethyl ammonium chlorides, two ten alkyl-dimethyl ammonium chlorides, two dodecyl dimethyl ammonium chlorides, two tetradecyl alkyl dimethyl ammonium chlorides, Varisoft 432PPG, distearyl dimethyl ammonium chloride, benzyl tripropyl ammonium chloride, Trimethyllaurylammonium bromide, cetyl trimethylammonium bromide, the octadecyl trimethylammonium bromide, two octyl dimethyl brometo de amonios, two nonyl dimethyl brometo de amonios, two ten alkyl dimethyl brometo de amonios, didodecyldimethylammbromide bromide, two tetradecyl dimethyl brometo de amonios, double hexadecyl dimethyl brometo de amonio, two octadecyl dimethyl brometo de amonios, benzyltrimethylammonium bromide, at least a in benzyl triethyl ammonium bromide and the benzyl tripropyl brometo de amonio.
Complex lithium grease of the present invention specifically can be following 1) and 2) in the lubricating grease any:
1) be made up of grease base oil, compound lithium base viscosifying agent and tensio-active agent, the ratio of quality and the number of copies of described grease base oil, compound lithium base viscosifying agent and tensio-active agent is: (290-1450): (50.4-251.3): (2-10);
2) be made up of grease base oil, compound lithium base viscosifying agent, tensio-active agent and additive, the ratio of quality and the number of copies of described grease base oil, compound lithium base viscosifying agent, tensio-active agent and additive is: (290-1450): (50.4-251.3): (2-10): (5.8-29); Described additive is oxidation inhibitor, anti-corrosion additive, rust-preventive agent and overstocked anti-wear agent.
Above-mentioned 1) in the lubricating grease, the ratio of quality and the number of copies of described grease base oil, compound lithium base viscosifying agent and tensio-active agent specifically can be: (290-400): (50.4-69.1): (2-8) or (400-1450): (69.1-251.3): (8-10).
Above-mentioned 2) in the lubricating grease, the ratio of quality and the number of copies of described grease base oil, compound lithium base viscosifying agent, tensio-active agent and additive specifically can be: (290-400): (50.4-69.1): (2-8): (5.8-22.2) or (400-1450): (69.1-251.3): (22.2-29).
Above-mentioned oxidation inhibitor can be pentanoic or N-phenyl alpha-naphthylamine; Above-mentioned anti-corrosion additive and rust-preventive agent can be benzotriazole or barium mahogany sulfonate; Above-mentioned extreme pressure anti-wear additives can be dialkyl dithiocarbamate.
Complex lithium grease of the present invention is to prepare according to the method that may further comprise the steps:
1) with the C of (33.2-166) mass parts 12-C 24The tensio-active agent of the auxiliary acid of lipid acid, (14.6-73) mass parts, (2-10) mass parts and the aqueous solution that contains (12-60) mass parts lithium hydroxide add in the grease base oil of (130-650) mass parts and carry out saponification reaction;
2) treat that saponification reaction fully after, dewater behind the grease base oil of heat temperature raising to 140 ℃-150 ℃ of adding (80-400) mass parts, be warming up to then 220 ℃-230 ℃ refine after, the grease base oil that adds (80-400) mass parts cools off, and grinds evenly promptly to get the described complex lithium grease of being made up of grease base oil, compound lithium base viscosifying agent and tensio-active agent;
3) in step 2) the basis on add the additive of (5.8-29) mass parts, grind and evenly promptly get the complex lithium grease of forming by grease base oil, compound lithium base viscosifying agent, tensio-active agent and additive.
Among the above-mentioned preparation method, the described saponified temperature of step 1) is 100 ℃-110 ℃.
Add tensio-active agent in the preparation process of complex lithium grease of the present invention, the tensio-active agent of adding and soap molecule form synergy, and then improve the arrangement mode of soap molecule and the ability of solidifying base oil, thereby improve the dropping point of lubricating grease.
Description of drawings
Fig. 1 is the infrared spectrum of the lubricating grease of embodiment 1 preparation.
Fig. 2 is the stereoscan photograph of the lubricating grease of embodiment 1 preparation.
Fig. 3 is the infrared spectrum of the lubricating grease of Comparative Examples 1 preparation.
Fig. 4 is the stereoscan photograph of the lubricating grease of Comparative Examples 1 preparation.
By the contrast of Fig. 2 and Fig. 4 as can be seen, the soap molecule that embodiment 1 obtains has fine and close more structure, just because of the improvement of soap molecular structure, the dropping point of complex lithium grease is greatly improved.
Embodiment
Employed experimental technique is ordinary method if no special instructions among the following embodiment.
Used material, reagent etc. if no special instructions, all can obtain from commercial channels among the following embodiment.
Kinematic viscosity when used cycloalkyl second line of distillation base oil, the cycloalkyl of the present invention subtracts three-way base oil and cycloalkyl and subtract 100 ℃ of four line base oils is respectively 8.01mm 2/ s, 19.98mm 2/ s and 24.56mm 2/ s all sends out the company that utilizes available from CNOOC's air to open.
The preparation of Comparative Examples 1, the complex lithium grease formed by second line of distillation base oil, compound lithium base viscosifying agent and additive
(100 ℃ the time, kinematic viscosity is 8.01mm to adopt cycloalkyl second line of distillation base oil 2/ s) as grease base oil.12-oxystearic acid, 11.2g sebacic acid, 3.4g boric acid, the 130g cycloalkyl second line of distillation base oil of getting 33.2g drop in the reactor, fully stir and slowly intensification, rise to 100-110 ℃ of 10% aqueous solution that contains 12g one hydronium(ion) oxidation lithium that adds heating, constant temperature saponification 2 hours, suitable make up water in the saponification process.Being warming up to 140-150 ℃ after saponification finishes dewaters compound.Dehydration back fully slowly adds the base oil dilution of 80g cycloalkyl second line of distillation and continues to heat up, rise to 220-230 ℃ gradually and carry out the high temperature refining, fully stirred 10 minutes, add the cooling of 80g cycloalkyl second line of distillation base oil, temperature is reduced to and is added additive below 120 ℃: pentanoic 0.5g, barium mahogany sulfonate 0.8g, benzotriazole 0.5g, dialkyldithiocarbamacompositions antimony 4g, grinding evenly promptly gets by cycloalkyl second line of distillation base oil, the compound lithium base viscosifying agent is (by the 12-hydroxy lithium stearate, sebacic acid lithium and lithium tetraborate are formed) and the complex lithium grease of additive composition.Its characteristic parameter such as table 1.
The preparation of embodiment 1, the complex lithium grease formed by second line of distillation base oil, compound lithium base viscosifying agent, tensio-active agent and additive
(100 ℃ the time, kinematic viscosity is 8.01mm to adopt cycloalkyl second line of distillation base oil 2/ s) as grease base oil.12-oxystearic acid, 11.2g sebacic acid, 3.4g boric acid, 130g cycloalkyl second line of distillation base oil and the 2g cetyl trimethylammonium bromide of getting 33.2g drop in the reactor, fully stir and slowly intensification, rise to 100 ℃ of 10% aqueous solution that contain 12g one hydronium(ion) oxidation lithium that add heating, constant temperature saponification 2 hours, suitable make up water in the saponification process.Being warming up to 140 ℃ after saponification finishes dewaters compound.Dehydration back fully slowly adds the base oil dilution of 80g cycloalkyl second line of distillation and continues to heat up, rise to 220 ℃ gradually and carry out the high temperature refining, fully stirred 10 minutes, add the cooling of 80g cycloalkyl second line of distillation base oil, temperature is reduced to and is added additive below 120 ℃: pentanoic 0.5g, barium mahogany sulfonate 0.8g, benzotriazole 0.5g, dialkyldithiocarbamacompositions antimony 4g, grind and evenly promptly get by cycloalkyl second line of distillation base oil, the compound lithium base viscosifying agent is (by the 12-hydroxy lithium stearate, sebacic acid lithium and lithium tetraborate are formed), the complex lithium grease that cetyl trimethylammonium bromide and additive are formed, wherein, cycloalkyl second line of distillation base oil, the compound lithium base viscosifying agent is (by the 12-hydroxy lithium stearate, sebacic acid lithium and lithium tetraborate are formed), the ratio of quality and the number of copies of cetyl trimethylammonium bromide and additive is: 290: 50.4: 2: 5.8, and its characteristic parameter such as table 1.
The preparation of embodiment 2, the complex lithium grease formed by second line of distillation base oil, compound lithium base viscosifying agent, tensio-active agent and additive
Present embodiment is the amplification test to embodiment 1.(100 ℃ the time, kinematic viscosity is 8.01mm to get the 12-oxystearic acid, 56g sebacic acid, 17g boric acid, 650g cycloalkyl second line of distillation base oil of 166g 2/ s) and in the 10g cetyl trimethylammonium bromide input reactor drop in the reactor, fully stir and slowly intensification, rise to 102 ℃ of 10% aqueous solution that contain 60g one hydronium(ion) oxidation lithium that heated, constant temperature saponification 2 hours, suitable make up water in the saponification process.Being warming up to 142 ℃ after saponification finishes dewaters compound.Dehydration back fully slowly adds the base oil dilution of 400g cycloalkyl second line of distillation and continues to heat up, rise to 222 ℃ gradually and carry out the high temperature refining, fully stirred 10 minutes, add the cooling of 400g cycloalkyl second line of distillation base oil, temperature is reduced to and is added additive below 120 ℃: pentanoic 2.5g, barium mahogany sulfonate 4g, benzotriazole 2.5g, dialkyldithiocarbamacompositions antimony 20g, grind and evenly promptly get by cycloalkyl second line of distillation base oil, the compound lithium base viscosifying agent is (by the 12-hydroxy lithium stearate, sebacic acid lithium and lithium tetraborate are formed), the complex lithium grease that cetyl trimethylammonium bromide and additive are formed, wherein, cycloalkyl second line of distillation base oil, the compound lithium base viscosifying agent is (by the 12-hydroxy lithium stearate, sebacic acid lithium and lithium tetraborate are formed), the ratio of quality and the number of copies of cetyl trimethylammonium bromide and additive is: 1450: 251: 10: 29, and its characteristic parameter such as table 1.
Embodiment 3, by the preparation that subtracts the complex lithium grease that three-way base oil, compound lithium base viscosifying agent, tensio-active agent and additive form
(100 ℃ the time, kinematic viscosity is 19.98mm to adopt cycloalkyl to subtract three-way base oil 2/ s) as grease base oil.12-oxystearic acid, 11.2g sebacic acid, 3.4g boric acid, the 130g cycloalkyl of getting 33.2g subtract in three-way base oil and the 2g cetyl trimethylammonium bromide input reactor, fully stir and slowly intensification, rise to 104 ℃ of 10% aqueous solution that contain 12g one hydronium(ion) oxidation lithium that add heating, constant temperature saponification 2 hours, suitable make up water in the saponification process.Being warming up to 144 ℃ after saponification finishes dewaters compound.The dehydration slow 80g of adding in back cycloalkyl fully subtracts three-way base oil dilution and continues to heat up, rise to 224 ℃ gradually and carry out the high temperature refining, fully stirred 10 minutes, add the 80g cycloalkyl and subtract three-way base oil cooling, temperature is reduced to and is added additive below 120 ℃: pentanoic 0.5g, barium mahogany sulfonate 0.8g, benzotriazole 0.5g, dialkyldithiocarbamacompositions antimony 4g, grind evenly promptly to get and subtract three-way base oil by cycloalkyl, the compound lithium base viscosifying agent is (by the 12-hydroxy lithium stearate, sebacic acid lithium and lithium tetraborate are formed), the complex lithium grease that cetyl trimethylammonium bromide and additive are formed, wherein, cycloalkyl subtracts three-way base oil, the compound lithium base viscosifying agent is (by the 12-hydroxy lithium stearate, sebacic acid lithium and lithium tetraborate are formed), the ratio of quality and the number of copies of cetyl trimethylammonium bromide and additive is: 290: 50.4: 2: 5.8, and its characteristic parameter such as table 1.
Embodiment 4, by the second line of distillation base oil, subtract the lubricated preparation of compound lithium base that four line base oils, compound lithium base viscosifying agent, tensio-active agent and additive form
12-oxystearic acid, 56g sebacic acid, 17g boric acid, the 650g cycloalkyl of getting 166g subtracts four line base oils, and (100 ℃ the time, kinematic viscosity is 19.98mm 2/ s) and in the 10g cetyl trimethylammonium bromide input reactor drop in the reactor, fully stir and slowly intensification, rise to 108 ℃ of 10% aqueous solution that contain 60g one hydronium(ion) oxidation lithium that heated, constant temperature saponification 2 hours, suitable make up water in the saponification process.Being warming up to 146 ℃ after saponification finishes dewaters compound.Dehydration fully back slowly adds 400g cycloalkyl second line of distillation base oil (100 ℃ the time, kinematic viscosity is 19.98mm 2/ s) dilution and continuation intensification, rise to 226 ℃ gradually and carry out the high temperature refining, fully stirred 10 minutes, adding 400g cycloalkyl second line of distillation base oil and cycloalkyl subtract the mixing oil cooling of four line base oils, temperature is reduced to and is added additive below 120 ℃: pentanoic 2.5g, barium mahogany sulfonate 4g, benzotriazole 2.5g, dialkyldithiocarbamacompositions antimony 20g, grind and evenly promptly get by cycloalkyl second line of distillation base oil, cycloalkyl subtracts four line base oils, the compound lithium base viscosifying agent is (by the 12-hydroxy lithium stearate, sebacic acid lithium and lithium tetraborate are formed), the complex lithium grease fat that cetyl trimethylammonium bromide and additive are formed, wherein, cycloalkyl second line of distillation base oil and cycloalkyl subtract the mixing oil of four line base oils, the compound lithium base viscosifying agent is (by the 12-hydroxy lithium stearate, sebacic acid lithium and lithium tetraborate are formed), the ratio of quality and the number of copies of cetyl trimethylammonium bromide and additive is: 1450: 251.3: 10: 29, and its characteristic parameter such as table 1.
Embodiment 5, by the second line of distillation base oil, subtract the preparation of the complex lithium grease that three-way base oil, compound lithium base viscosifying agent, tensio-active agent and additive form
(100 ℃ the time, kinematic viscosity is 24.56mm to adopt cycloalkyl second line of distillation base oil 2/ s) and subtract three-way base oil (100 ℃ the time, kinematic viscosity is 24.56mm 2/ s) mixing oil is as grease base oil.Get 200g cycloalkyl second line of distillation base oil and 200g cycloalkyl and subtract the mixing oil of three-way base oil as grease base oil.The two tetradecyl dimethyl brometo de amonios of 12-oxystearic acid, 15.4g sebacic acid, 4.7g boric acid, the above-mentioned mixing oil of 180g and 8g of getting 45.8g drop in the reactor, fully stir and slowly intensification, rise to 110 ℃ of 10% aqueous solution that contain 16.5g one hydronium(ion) oxidation lithium that heated, constant temperature saponification 2 hours, suitable make up water in the saponification process.Being warming up to 150 ℃ after saponification finishes dewaters compound.Dehydration back fully slowly adds the above-mentioned mixing oil dilution of 110g and continues to heat up, rise to 230 ℃ gradually and carry out the high temperature refining, fully stirred 10 minutes, add the above-mentioned mixing oil cooling of 110g, temperature is reduced to and is added additive below 120 ℃: pentanoic 2g, barium mahogany sulfonate 3g, benzotriazole 2.2g, dialkyldithiocarbamacompositions antimony 15g, grind and evenly promptly get by cycloalkyl second line of distillation base oil, cycloalkyl subtracts three-way base oil, the compound lithium base viscosifying agent is by the 12-hydroxy lithium stearate, sebacic acid lithium and lithium tetraborate are formed), the complex lithium grease that two tetradecyl dimethyl brometo de amonios and additive are formed, wherein, cycloalkyl second line of distillation base oil and cycloalkyl subtract the mixing oil of three-way base oil, the compound lithium base viscosifying agent is by the 12-hydroxy lithium stearate, sebacic acid lithium and lithium tetraborate are formed), the ratio of quality and the number of copies of two tetradecyl dimethyl brometo de amonios and additive is: 400: 69.1: 8: 22.2, and its characteristic parameter such as table 1.
Embodiment 6, by the second line of distillation base oil, subtract three-way base oil, subtract the preparation of the complex lithium grease that four line base oils, compound lithium base viscosifying agent, tensio-active agent and additive form
This example adopts cycloalkyl second line of distillation base oil, and (100 ℃ the time, kinematic viscosity is 8.01mm 2/ s), (100 ℃ the time, kinematic viscosity is 8.01mm to subtract three-way base oil 2/ s) and subtract four line base oils (100 ℃ the time, kinematic viscosity is 8.01mm 2/ s) mixing oil is as grease base oil.Getting 200g cycloalkyl second line of distillation oil, 100g cycloalkyl subtracts three-way base oil and 100g cycloalkyl and subtracts four line base oils and mix as grease base oil.Except the base oil difference, the compositing formula of lubricating grease is identical with embodiment 5 with the preparation method.
The detection data of the complex lithium grease product of table 1 embodiment 1-6 and Comparative Examples
Data as can be known in the contrast table 1, tensio-active agent among the present invention has improved the dropping point of complex lithium grease, and can also add additives such as oxidation inhibitor, anti-corrosion additive, rust-preventive agent or overstocked anti-wear agent as required, can improve the performance of the aspects such as oxidation stability, Corrosion Protection, mechanical stability, colloid stability and anti-attrition of lubricating grease, thereby enlarge the range of application of complex lithium grease.

Claims (10)

1. complex lithium grease, comprise grease base oil, compound lithium base viscosifying agent and tensio-active agent, the ratio of quality and the number of copies of described grease base oil, compound lithium base viscosifying agent and tensio-active agent is: (290-1450): (50.4-251.3): (2-10); Described grease base oil is the second line of distillation base oil, subtracts three-way base oil and subtract in the four line base oils at least a; Described compound lithium base viscosifying agent is by C 12-C 24The complex thickener that fatty acid lithium and auxiliary acid lithium are formed; C 12-C 24The ratio of quality and the number of copies of fatty acid lithium and auxiliary acid lithium is: (34-70): (16.4-81.3); Described auxiliary acid lithium is C 1-C 22In fatty acid lithium, lithium tetraborate, Trilithium phosphate, aromatic acid lithium, naphthenic acid lithium, diprotic acid lithium and the polyprotonic acid lithium any two.
2. complex lithium grease according to claim 1 is characterized in that: described grease base oil is that cycloalkyl second line of distillation base oil, cycloalkyl subtract three-way base oil and cycloalkyl subtracts in the four line base oils at least a; Kinematic viscosity during 100 ℃ of described grease base oils is 5mm 2/ s-40mm 2/ s, preferred 8mm 2/ s-26mm 2/ s.
3. complex lithium grease according to claim 1 and 2 is characterized in that: described C 12-C 24Fatty acid lithium is 12-hydroxy lithium stearate or lithium stearate.
4. according to claim 1,2 or 3 described complex lithium greases, it is characterized in that: described C 1-C 22Fatty acid lithium is lithium acetate, propionic acid lithium, n-caprylic acid lithium or lithium laurate; Described aromatic acid lithium is phthalic acid lithium or lithium salicylate; Described diprotic acid lithium is pentanedioic acid lithium, lithium adipate, pimelic acid lithium, suberic acid lithium, nonane diacid lithium or sebacic acid lithium.
5. according to each described complex lithium grease among the claim 1-4, it is characterized in that: described tensio-active agent is a Dodecyl trimethyl ammonium chloride, palmityl trimethyl ammonium chloride, octadecyl trimethyl ammonium chloride, two octyl alkyl dimethyl ammonium chlorides, two ten alkyl-dimethyl ammonium chlorides, two dodecyl dimethyl ammonium chlorides, two tetradecyl alkyl dimethyl ammonium chlorides, Varisoft 432PPG, distearyl dimethyl ammonium chloride, benzyl tripropyl ammonium chloride, Trimethyllaurylammonium bromide, cetyl trimethylammonium bromide, the octadecyl trimethylammonium bromide, two octyl dimethyl brometo de amonios, two nonyl dimethyl brometo de amonios, two ten alkyl dimethyl brometo de amonios, didodecyldimethylammbromide bromide, two tetradecyl dimethyl brometo de amonios, double hexadecyl dimethyl brometo de amonio, two octadecyl dimethyl brometo de amonios, benzyltrimethylammonium bromide, at least a in benzyl triethyl ammonium bromide and the benzyl tripropyl brometo de amonio.
6. according to each described complex lithium grease among the claim 1-4, it is characterized in that: described complex lithium grease is following 1) and 2) in the lubricating grease any:
1) be made up of grease base oil, compound lithium base viscosifying agent and tensio-active agent, the ratio of quality and the number of copies of described grease base oil, compound lithium base viscosifying agent and tensio-active agent is: (290-1450): (50.4-251.3): (2-10);
2) be made up of grease base oil, compound lithium base viscosifying agent, tensio-active agent and additive, the ratio of quality and the number of copies of described grease base oil, compound lithium base viscosifying agent, tensio-active agent and additive is: (290-1450): (50.4-251.3): (2-10): (5.8-29); Described additive is oxidation inhibitor, anti-corrosion additive, rust-preventive agent and overstocked anti-wear agent.
7. complex lithium grease according to claim 6 is characterized in that: described oxidation inhibitor is pentanoic or N-phenyl alpha-naphthylamine; Described anti-corrosion additive and rust-preventive agent are benzotriazole or barium mahogany sulfonate; Described extreme pressure anti-wear additives is a dialkyl dithiocarbamate.
8. according to arbitrary described complex lithium grease among the claim 1-7, it is characterized in that: described complex lithium grease is according to claim 9 or 10 described method preparations.
9. each described preparing complex lithium grease among the claim 1-8 may further comprise the steps:
1) with the C of (33.2-166) mass parts 12-C 24The tensio-active agent of the auxiliary acid of lipid acid, (14.6-73) mass parts, (2-10) mass parts and the aqueous solution that contains (12-60) mass parts lithium hydroxide add in the grease base oil of (130-650) mass parts and carry out saponification reaction;
2) treat that saponification reaction fully after, dewater behind the grease base oil of heat temperature raising to 140 ℃-150 ℃ of adding (80-400) mass parts, be warming up to then 220 ℃-230 ℃ refine after, the grease base oil that adds (80-400) mass parts cools off, and grinds evenly promptly to get the described complex lithium grease of being made up of grease base oil, compound lithium base viscosifying agent and tensio-active agent;
3) in step 2) the basis on add the additive of (5.8-29) mass parts, grind and evenly promptly get the complex lithium grease of forming by grease base oil, compound lithium base viscosifying agent, tensio-active agent and additive.
10. method according to claim 9 is characterized in that: described step 1) saponified temperature is 100 ℃-110 ℃.
CN2010102448315A 2010-08-04 2010-08-04 Complex lithium grease and preparation method thereof Active CN101921650B (en)

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Cited By (8)

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CN104194873A (en) * 2014-07-23 2014-12-10 中国石油化工股份有限公司 Lubricating grease composition for gears of electric shovel and preparation method thereof
CN105419906A (en) * 2013-12-30 2016-03-23 北京雅士科莱恩石油化工有限公司 Complex lithium grease
CN107090324A (en) * 2017-04-28 2017-08-25 杭州高烯科技有限公司 A kind of complex lithium grease containing spitball shape graphene microballoon and preparation method thereof
CN108102770A (en) * 2017-12-04 2018-06-01 薛银福 A kind of wear-resisting type lubricating grease
CN108531263A (en) * 2018-06-08 2018-09-14 深圳市优宝新材料科技有限公司 Lithium base grease and preparation method thereof
CN111979029A (en) * 2020-09-09 2020-11-24 中国科学院兰州化学物理研究所 Composite lithium-based thickening agent, lubricating grease prepared from composite lithium-based thickening agent and preparation method of lubricating grease
CN112759613A (en) * 2019-10-21 2021-05-07 中国石油化工股份有限公司 Biodegradable composite lithium-based lubricating grease composition and preparation method thereof
US11225414B2 (en) 2017-04-28 2022-01-18 Hangzhou Gaoxi Technology Co., Ltd. Paper ball-like graphene microsphere, composite material thereof, and preparation method therefor

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105419906A (en) * 2013-12-30 2016-03-23 北京雅士科莱恩石油化工有限公司 Complex lithium grease
CN105419906B (en) * 2013-12-30 2018-07-27 北京雅士科莱恩石油化工有限公司 A kind of complex lithium grease
CN104194873A (en) * 2014-07-23 2014-12-10 中国石油化工股份有限公司 Lubricating grease composition for gears of electric shovel and preparation method thereof
CN107090324A (en) * 2017-04-28 2017-08-25 杭州高烯科技有限公司 A kind of complex lithium grease containing spitball shape graphene microballoon and preparation method thereof
US11225414B2 (en) 2017-04-28 2022-01-18 Hangzhou Gaoxi Technology Co., Ltd. Paper ball-like graphene microsphere, composite material thereof, and preparation method therefor
CN108102770A (en) * 2017-12-04 2018-06-01 薛银福 A kind of wear-resisting type lubricating grease
CN108531263A (en) * 2018-06-08 2018-09-14 深圳市优宝新材料科技有限公司 Lithium base grease and preparation method thereof
CN112759613A (en) * 2019-10-21 2021-05-07 中国石油化工股份有限公司 Biodegradable composite lithium-based lubricating grease composition and preparation method thereof
CN112759613B (en) * 2019-10-21 2023-03-31 中国石油化工股份有限公司 Biodegradable composite lithium-based lubricating grease composition and preparation method thereof
CN111979029A (en) * 2020-09-09 2020-11-24 中国科学院兰州化学物理研究所 Composite lithium-based thickening agent, lubricating grease prepared from composite lithium-based thickening agent and preparation method of lubricating grease

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