CN102618359B - Silicon-based lubricating grease composition for electrical contact, and preparation method thereof - Google Patents

Silicon-based lubricating grease composition for electrical contact, and preparation method thereof Download PDF

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CN102618359B
CN102618359B CN201210031345.4A CN201210031345A CN102618359B CN 102618359 B CN102618359 B CN 102618359B CN 201210031345 A CN201210031345 A CN 201210031345A CN 102618359 B CN102618359 B CN 102618359B
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silica
grease composition
silicon
temperature
base oil
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CN102618359A (en
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曾晖
纪红兵
陈哲
梁伟灿
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Sun Yat Sen University
National Sun Yat Sen University
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National Sun Yat Sen University
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Abstract

The present invention discloses a silicon-based lubricating grease composition for electrical contact, and a preparation method thereof. The silicon-based lubricating grease composition comprises, by weight, 70-85% of a silicon-based base oil, 12-27% of a thickening agent, and 0.1-3% of an additive. The silicon-based lubricating grease composition of the present invention adopts the silicone oil with excellent high temperature property and excellent low temperature property as the silicon-based base oil, and is added with a solid conductive agent, such that the product has good colloidal stability, mechanical stability and good high temperature performance, and can be used for contact lubrication of electronic products. The composition of the present invention is prepared through the one-step synthesis method, and has advantages of simple process, low energy consumption and the like.

Description

A kind of silica-based grease composition for electric contact and preparation method thereof
Technical field
The present invention relates to electronic product and manufacture field, specifically a kind of silica-based grease composition for electric contact and preparation method thereof.
Background technology
Lubricating grease is the important component part of industrial lubricants, it be a kind of by viscosifying agent and base oil, formed there is plastic solid to semi-solid lubricant, for meeting harsh application conditions, often add various functional additives and improve its performance and be widely used in iron and steel, automobile, aerospace and war industry.Silica-based lubricating grease is a class high-performance grease product of being made as viscosifying agent by the compound lithium soap of 12-oxystearic acid and diprotic acid, because it has very high dropping point, good mechanical stability, bearing wastage is few, outstanding water-resistant antirust and oxidation stability, be able to have wide application in industries such as Iron And Steel Industry, automotive industrys.
Along with the unprecedented progress of information industry, people increase day by day for the demand of electronic product.In electronic product use procedure, if electrical contact near time there is no electrical contact lubricating grease, electric arc will directly puncture medium, form electrical discharge arc, cause arc erosion and the oxidation of contact, affect the work-ing life of electrical pickoff.Use electrical pickoff lubricating grease to there is anti-oxidant, etch-proof effect, can effectively ensure that the operating mode electrically contacting is good.
CN1295119A discloses a kind of for electric contact point lubricating fat, with compound lithium base metallic soap multiviscosisty lipid base oil, becomes fat, has added oxidation inhibitor, rust-preventive agent and organic conductive agent, and the dropping point of product all, below 200 ℃, is not suitable for the application conditions under high temperature.
The disclosed lubricating grease of US5282986, with compound lithium base metallic soap multiviscosisty synthetic hydrocarbon oil, has added the inorganicss such as zinc oxide as conductive agent, but resistivity is not controlled.
CN1715377A discloses a kind of lubricating grease for wheels of airplanes, adopt complex lithium, calcium soap to come multiviscosisty poly-a-olefin oil to become fat with ethyl silicon oil, product is mainly used in the lubricated of wide temperature range airplane wheel bearing, wherein add the amount of Graphite Powder 99 to reach 2%-20%, object improves withstand load and wear resistance.
In the research of silica-based lubricating grease, all do not make full use of the feature of synthetic oil and additive above, product cannot meet the electric contact use that adapts to high temperature and low temperature requirement.
Summary of the invention
The object of the invention is for above-mentioned problem, adopt the silicone oil that possesses outstanding high temperature performance, and property
A kind of composition of silica-based lubricating grease is prepared in the inorganic conductive agent that matter is stable.
To achieve these goals, the present invention adopts following technical scheme:
For a silica-based grease composition for electric contact point lubricating, by the material of following weight percentage, formed: silica-based base oil 70%-85%, viscosifying agent 12%-27%, additive 0.1%-3%.
In above-mentioned silica-based grease composition, described silica-based base oil is preferably a kind of in ethyl silicon oil, methyl-silicone oil, polymethylphenyl siloxane fluid.
In above-mentioned silica-based grease composition, described viscosifying agent is the mixture of 12-oxystearic acid lithium salts and sebacic acid lithium salts, and described 12-oxystearic acid lithium salts mass percent is 50%-90%, and the mass percent of sebacic acid lithium salts is 10%-50%.
In above-mentioned silica-based grease composition, described additive is the mixture of a kind of, two kinds or three kinds in antioxidant, conductive agent, pigment.
In above-mentioned silica-based grease composition, described antioxidant is a kind of in pentanoic, di-iso-octyldiphenylamine or the mixture of the two.
In above-mentioned silica-based grease composition, described conductive agent is a kind of in graphite and zinc oxide or both mixtures.
In above-mentioned silica-based grease composition, described pigment is Sudan III or naphthol green or oily molten orange.
The preparation method of the above-mentioned silica-based grease composition for electric contact point lubricating, comprises the steps:
(1) 12-oxystearic acid, sebacic acid, silica-based base oil are added in the middle of reactor, heated and stirred adds the hot strong solution of lithium hydroxide to carry out saponification after dissolving;
(2) heat up and dewater, carry out afterwards high temperature puffing;
(3) keep certain temperature to stir after adding additive, system naturally cools to room temperature and obtains product.
In above-mentioned preparation method, step (1) saponification temperature is 80 ℃-120 ℃; The described dehydration temperaturre of step (2) is 130 ℃-180 ℃, and swelling temperature is 190 ℃-230 ℃; The described temperature of step (3) is 170 ℃-200 ℃.
Silica-based lubricating grease of the present invention, take a series of silicone oil as silica-based lubricating grease, makes full use of that silicone oil high temperature performance is good, the feature of excellent in oxidation resistance; Adopt compound lithium base metal soap base to carry out single stage method multiviscosisty, method is simply saved production energy consumption; Product possesses good colloid stability and mechanical stability, contain antioxidant and possess the performance of at high temperature working, and by making adding of conductive additive silica-based grease composition possess adjustable resistivity, can be extensively in electronic product different electric contacts use.
Embodiment
Below in conjunction with embodiment, the present invention is described further, but protection scope of the present invention is not limited to the scope that embodiment represents.
Comparative example 1:
6 grams of 12-oxystearic acids and 2 grams of sebacic acid are added in the middle of 40 grams of ethyl silicon oils, heated and stirred at 110 ℃, after dissolving, two kinds of lipid acid add the hot strong solution of lithium hydroxide to carry out saponification, then will be warming up to 140 ℃ dewaters, after having dewatered, at 210 ℃, carry out expanded, keep subsequently stirring, system naturally cools to room temperature and obtains product.
Comparative example 2:
6 grams of 12-oxystearic acids and 2 grams of sebacic acid are added in the middle of 40 grams of methyl-silicone oils, heated and stirred at 110 ℃, after dissolving, two kinds of lipid acid add the hot strong solution of lithium hydroxide to carry out saponification, then will be warming up to 140 ℃ dewaters, after having dewatered, at 210 ℃, carry out expanded, keep subsequently stirring, system naturally cools to room temperature and obtains product.
Comparative example 3:
6 grams of 12-oxystearic acids and 2 grams of sebacic acid are added in the middle of 40 grams of polymethylphenyl siloxane fluids, heated and stirred at 110 ℃, after dissolving, two kinds of lipid acid add the hot strong solution of lithium hydroxide to carry out saponification, then will be warming up to 140 ℃ dewaters, after having dewatered, at 210 ℃, carry out expanded, keep subsequently stirring, system naturally cools to room temperature and obtains product.
Embodiment 1:
6 grams of 12-oxystearic acids and 2 grams of sebacic acid are added in the middle of 40 grams of ethyl silicon oils, heated and stirred at 110 ℃, after dissolving, two kinds of lipid acid add the hot strong solution of lithium hydroxide to carry out saponification, then will be warming up to 140 ℃ dewaters, after having dewatered, at 210 ℃, carry out expanded, after expanded end, the base oil that is dissolved with 0.5 gram of pentanoic, 0.2 gram of Sudan III and 0.0025 gram of zinc oxide added and keep stirring, system naturally cools to room temperature and obtains product.
Embodiment 2:
6 grams of 12-oxystearic acids and 2 grams of sebacic acid are added in the middle of 40 grams of ethyl silicon oils, heated and stirred at 110 ℃, after dissolving, two kinds of lipid acid add the hot strong solution of lithium hydroxide to carry out saponification, then will be warming up to 140 ℃ dewaters, after having dewatered, at 210 ℃, carry out expanded, after expanded end, the base oil that is dissolved with 0.5 gram of pentanoic, 0.2 gram of Sudan III and 0.0025 gram of graphite added and keep stirring, system naturally cools to room temperature and obtains product.
Embodiment 3:
6 grams of 12-oxystearic acids and 2 grams of sebacic acid are added in the middle of 40 grams of ethyl silicon oils, heated and stirred at 110 ℃, after dissolving, two kinds of lipid acid add the hot strong solution of lithium hydroxide to carry out saponification, then will be warming up to 140 ℃ dewaters, after having dewatered, at 210 ℃, carry out expanded, after expanded end, the base oil that is dissolved with 0.5 gram of pentanoic, 0.2 gram of Sudan III, 0.0012 gram of graphite and 0.0013 gram of zinc oxide added and keep stirring, system naturally cools to room temperature and obtains product.
Embodiment 4:
By in 28 grams of 12-oxystearic acids and 294 grams of ethyl silicon oils, heating is stirred, add containing lithium hydroxide hot solution, system temperature is risen to 150 ℃, then system temperature is reduced within the scope of 105 ℃ and adds 11.5 grams of sebacic acid, add lithium hydroxide hot solution, system temperature is risen to 150 ℃, expanded at 200 ℃ subsequently, finally stop heating and keep stirring after system temperature is cooled to room temperature, to obtain product.
The product performance contrast of each embodiment is as shown in table 1.
Table 1
Project Comparative example 1 Comparative example 2 Comparative example 3 Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4
Outward appearance The smooth even ointment of white The smooth even ointment of white The smooth even ointment of white The smooth even ointment of white The smooth even ointment of black The smooth even ointment of grey The smooth even ointment of white
Cone penetration/0.1mm 270 332 333 311 305 308 228
Dropping point/℃ 295 270 277 >300 298 >300 >300
Stencil oil-dividing/% 0.7 0.9 1.4 0.8 1.0 0.9 0.5
Moisture/% Trace Trace Trace Trace Trace Trace Trace

Claims (1)

1. for a silica-based grease composition for electric contact, it is characterized in that being formed by the material of following weight percentage: silica-based base oil 70%-85%, viscosifying agent 12%-27%, additive 0.1%-3%;
Silica-based base oil is ethyl silicon oil;
Described viscosifying agent is the mixture of 12-oxystearic acid lithium salts and sebacic acid lithium salts, and described 12-oxystearic acid lithium salts mass percent is 50%-90%, and the mass percent of sebacic acid lithium salts is 10%-50%;
Described additive is the mixture of three kinds in antioxidant, conductive agent, pigment;
The described silica-based grease composition for electric contact prepares by the following method:
(1) 12-oxystearic acid, sebacic acid, silica-based base oil are added in the middle of reactor, heated and stirred adds the hot strong solution of lithium hydroxide to carry out saponification after dissolving;
(2) heat up and dewater, carry out afterwards high temperature puffing;
(3) keep certain temperature to stir after adding additive, system naturally cools to room temperature and obtains product;
Step (1) saponification temperature is 80 ℃-120 ℃; The described dehydration temperaturre of step (2) is 130 ℃-180 ℃, and swelling temperature is 190 ℃-230 ℃; The described temperature of step (3) is 170 ℃-200 ℃;
Described antioxidant is a kind of in pentanoic, di-iso-octyldiphenylamine or the mixture of the two;
Described conductive agent is a kind of in graphite and zinc oxide or both mixtures;
Described pigment is Sudan III or naphthol green or oily molten orange.
CN201210031345.4A 2012-02-13 2012-02-13 Silicon-based lubricating grease composition for electrical contact, and preparation method thereof Active CN102618359B (en)

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CN105482872B (en) * 2015-07-17 2018-12-18 路伯润滑油(苏州)有限公司 Rotary connector lubricating grease and preparation method thereof
CN108165351B (en) * 2017-12-22 2020-11-17 武汉博达特种润滑技术有限公司 High-low temperature instrument oil composition and preparation method thereof

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CN101481637A (en) * 2008-01-09 2009-07-15 中国石油化工股份有限公司 Process for preparing composite lithium base grease

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CN1100130C (en) * 1999-11-04 2003-01-29 中国石油化工集团公司 Lubricant grease for electric contact
CN1307293C (en) * 2000-11-29 2007-03-28 日本精工株式会社 Conductive grease and rolling apparatus packed with the same
JP4242610B2 (en) * 2002-07-09 2009-03-25 協同油脂株式会社 Water-soluble lubricant composition
JP2010195958A (en) * 2009-02-26 2010-09-09 Alps Electric Co Ltd Lubricating composition for use in electric contact

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Publication number Priority date Publication date Assignee Title
CN101481637A (en) * 2008-01-09 2009-07-15 中国石油化工股份有限公司 Process for preparing composite lithium base grease

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