CN112940828A - Composition for forming heat-conducting lubricant - Google Patents
Composition for forming heat-conducting lubricant Download PDFInfo
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- CN112940828A CN112940828A CN202110151300.XA CN202110151300A CN112940828A CN 112940828 A CN112940828 A CN 112940828A CN 202110151300 A CN202110151300 A CN 202110151300A CN 112940828 A CN112940828 A CN 112940828A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/08—Inorganic acids or salts thereof
- C10M2201/082—Inorganic acids or salts thereof containing nitrogen
- C10M2201/083—Inorganic acids or salts thereof containing nitrogen nitrites
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
- C10M2207/126—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/28—Esters
- C10M2207/281—Esters of (cyclo)aliphatic monocarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2227/00—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
- C10M2227/04—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions having a silicon-to-carbon bond, e.g. organo-silanes
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
- C10M2229/04—Siloxanes with specific structure
- C10M2229/041—Siloxanes with specific structure containing aliphatic substituents
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Abstract
The invention provides a composition for forming a heat-conducting lubricant, which comprises the following components in parts by weight: 100 parts of dimethyl silicone oil; 200-400 parts of alumina; 10-50 parts of zinc oxide; 5-45 parts of a lubricant; 1-10 parts of an anti-settling agent; 0.1-10 parts of inorganic salt; 0.1-10 parts of a heat stabilizer; 0.01-5 parts of a silane coupling agent; wherein the lubricant comprises one or more of zinc stearate, calcium stearate, paraffinic oil, naphthenic oil, and silicone; the anti-settling agent comprises one or more of ethyl acetate, butyl acetate, xylene, n-hexane and butanol; the inorganic salt is selected from one or more of nitrite and sulfite. According to the invention, by optimizing the formula, the provided composition can be used for conveniently preparing the heat-conducting lubricant, and the formed heat-conducting lubricant has excellent heat-conducting property and lubricating property.
Description
Technical Field
The invention relates to the technical field of lubricants, in particular to a composition for forming a heat-conducting lubricant.
Background
The temperature rise and temperature distribution of the high-speed rolling bearing directly affect the working performance and service life of the bearing system. The improvement of antifriction bearing rotational speed can lead to bearing friction themogenesis to increase, if the heat can not in time distribute effectively, can cause the inside high temperature of bearing, and then leads to bearing inner part surface burn even veneer, sting and abandonment too early.
Therefore, there is a need to develop a multifunctional heat-conducting silicone grease mixture which has both lubricating function and heat-conducting function, and the application of the heat-conducting grease in the bearing structure not only can slow down the aging and heat-conducting problems of the bearing structure, but also can avoid the corrosion problem brought by the traditional lubricating oil.
CN 110257139 a discloses a method for preparing a heat-resistant, high-temperature-resistant and durable lubricant, comprising the following steps: weighing raw materials according to a given ratio, carrying out addition melting copolymerization on 1-cyanobenzocyclobutene and a terephthaloyl chloride monomer to form a prepolymer, cooling the prepolymer, adding an active diluent, carrying out heat preservation, cooling, adding a solution in which a catalyst is dissolved, uniformly mixing, and carrying out vacuum evaporation to remove a solvent in which the catalyst is dissolved 1, 3-butanediol dimethacrylate, dioxacene ester, glycidyl methacrylate, butyl glycidyl ether and dimethylamino methyl phenol, cooling the diluted prepolymer to room temperature, adding a catalyst solution in which a catalyst is dissolved in a catalyst solvent, wherein the catalyst is selected from 2-methylimidazole, 2-ethyl-4-methylimidazole, aluminum acetylacetonate, zinc acetylacetonate and manganese acetylacetonate; the solvent of the catalyst is selected from acetone, butanone and tetrahydrofuran, and the solvent for dissolving the catalyst is removed by vacuum evaporation at the temperature of 30-50 ℃ to obtain the benzocyclobutene amide lubricating grease; adding dimethylchlorosilane and dicyclopentadiene into another reaction kettle, heating, stirring, introducing nitrogen, adding a butyl lithium solution at 135-140 ℃, keeping the temperature for 30-60 min, keeping the temperature for 10-20 min, adding dimethylamine, stirring, reacting for 10-20 min, adding isopropylmagnesium bromide and ferrous chloride, and stirring, reacting for 10-20 min to obtain a borosilicate ferrocene prepolymer; adding the borosilicate ferrocene prepolymer prepared in the step two into butanediol, continuously stirring, adding alkaline water to adjust the pH value to 2.0-10.0, and reacting for 1-2 hours at 130-145 ℃ to obtain a modified borosilicate ferrocene prepolymer; fourthly, introducing the modified borosilicate ferrocene performed polymer, benzocyclobutene amide lubricating grease, pentaerythritol stearate, poly adamantane-1, 3-diformyl m-phenylenediamine, aluminum oxide, polyphenyl ether and a clean dispersing agent into a ball mill, mixing and ball-milling for 2-3 h, introducing an antioxidant into a mixer, heating at 80-90 ℃, stirring and reacting for 20-30 min at a stirring speed of 200-400 r/min, then adding ammonia water, cooling to the normal temperature, and stirring and reacting for 1-2 h to obtain a mixture A; adding zinc dialkyl dithiophosphate, dimethylamino dinitrogen selenated indene and tungsten oxide into the mixture A, guiding the mixture A into a stirrer, mixing the mixture A and the tungsten oxide for 15-25 min under magnetic stirring, and filtering to remove precipitates to obtain a mixture B; and adding zinc dialkyl dithiophosphate, sodium allylsulfonate and isooctyl glycidyl ether into the mixture B, stirring and reacting for 2-3 hours at the temperature of 65-75 ℃ and the pressure of 2-4 MPa, then heating to 95-100 ℃, and uniformly stirring to obtain a finished product. The heat-conducting lubricant prepared by the method meets the requirements in terms of functions, but is not suitable for large-area popularization at least because the preparation process is complicated and the economic benefit is poor.
Disclosure of Invention
In view of the problems in the prior art, an object of the present invention is to provide a composition for forming a heat-conducting lubricant, which can be used to conveniently prepare the heat-conducting lubricant by optimizing the formulation, and the formed heat-conducting lubricant has both excellent heat-conducting property and lubricating property.
The second purpose of the invention is to provide a preparation method of the heat-conducting lubricant corresponding to the first purpose.
It is a further object of the present invention to provide a thermally conductive lubricant that corresponds to the above object.
In order to achieve one of the purposes, the technical scheme adopted by the invention is as follows:
a composition for forming a heat-conducting lubricant comprises the following components in parts by weight:
wherein the lubricant comprises one or more of zinc stearate, calcium stearate, paraffinic oil, naphthenic oil, and silicone; the anti-settling agent comprises one or more of ethyl acetate, butyl acetate, xylene, n-hexane and butanol; the inorganic salt is selected from one or more of nitrite and sulfite.
In some preferred embodiments of the present invention, the composition or the raw material thereof comprises the following components in parts by weight:
in some preferred embodiments of the present invention, the dynamic viscosity of the dimethylsilicone fluid is 100 to 15000mPa · S.
In some preferred embodiments of the present invention, the dimethylsilicone fluid has a dynamic viscosity of 1000 to 10000mPa · S.
In some preferred embodiments of the present invention, the dimethylsilicone fluid has a dynamic viscosity of 1000mPa · S to 5000mPa · S.
According to the present invention, dimethylsilicone fluids having kinematic viscosities within the above-mentioned ranges may be used in the present invention. The dynamic viscosity of the dimethylsilicone fluid may be, for example, 100 mPaS, 500 mPaS, 1000 mPaS, 1500 mPaS, 2000 mPaS, 2500 mPaS, 3000 mPaS, 3500 mPaS, 4000 mPaS, 4500 mPaS, 5000 mPaS, 5500 mPaS, 6000 mPaS, 6500 mPaS, 7000 mPaS, 7500 mPaS, 8000 mPaS, 8500 mPaS, 9000 mPaS, 9500 mPaS, 10000 mPaS, 11000 mPaS, 12000 mPaS, 13000 mPaS, 14000 mPaS, 15000 mPaS and any value therebetween.
In some preferred embodiments of the invention, the alumina has a particle size of 0.1 to 10 μm, preferably 0.1 to 5 μm.
According to the present invention, the particle size of the alumina may be any value within the above-specified range, for example, but not limited to, 0.1 μm, 0.5 μm, 1.0 μm, 1.5 μm, 2.0 μm, 2.5 μm, 3.0 μm, 3.5 μm, 4.0 μm, 4.5 μm, 5.0 μm, 5.5 μm, 6.0 μm, 6.5 μm, 7.0 μm, 7.5 μm, 8.0 μm, 8.5 μm, 9.0 μm, 9.5 μm, 10.0 μm and any value therebetween.
In some preferred embodiments of the invention, the zinc oxide has a particle size of 0.1 to 5 μm, preferably 0.5 to 3 μm.
According to the present invention, the particle size of the zinc oxide may be any value within the above-specified range, for example, but not limited to, 0.1 μm, 0.5 μm, 1.0 μm, 1.5 μm, 2.0 μm, 2.5 μm, 3.0 μm, 3.5 μm, 4.0 μm, 4.5 μm, 5.0 μm, and any value therebetween.
In some preferred embodiments of the present invention, the thermal stabilizer comprises one or more of a calcium zinc thermal stabilizer, a barium zinc stabilizer, and a barium cadmium stabilizer.
In some preferred embodiments of the invention, the silane coupling agent comprises one or more of KH550, KH560, KH570, preferably KH 550.
According to the invention, the sulphite may be sodium sulphite and magnesium sulphite.
According to the invention, the nitrite may be sodium nitrite or zinc nitrite.
In order to achieve the second purpose, the invention adopts the following technical scheme:
the preparation method of the heat-conducting lubricant takes the composition as a raw material and comprises the following steps:
s1, modifying the heat-conducting filler comprising the aluminum oxide and the zinc oxide by using the silane coupling agent to prepare a modified heat-conducting filler;
s2, mixing, curing and ball-milling the modified heat-conducting filler and the dimethyl silicone oil to obtain a silicone grease mixture;
and S3, mixing and ball-milling the silicone grease mixture, the zinc stearate, the ethyl acetate, the inorganic salt and the heat stabilizer to prepare the heat-conducting lubricant.
In some preferred embodiments of the present invention, in step S1, the step of modifying treatment includes:
1) dissolving the silane coupling agent in a solvent, preferably absolute ethanol;
2) mixing the heat-conducting filler with the product prepared in the step 1);
3) adjusting the pH value of the product prepared in the step 2) to 9-11, and then carrying out water bath treatment on the product; and
optionally, 4) subjecting the product obtained in step 3) to ultrasonic treatment;
preferably, in step 3), the conditions of the water bath treatment include: the temperature is 35-65 ℃; the time is 1-5 h; and/or in step 4), the ultrasonic treatment conditions comprise: the frequency is 30 kHz-120 kHz; the time is 1min to 30 min.
In some preferred embodiments of the present invention, in step S2, the conditions of ripening include: the temperature is 80-150 ℃; the time is 1min to 30 min; and/or the conditions of said ball milling comprise: the rotating speed is 100 r/min-1000 r/min; the time is 1min to 60 min.
In some preferred embodiments of the present invention, in step S3, the ball milling conditions include: the rotating speed is 100 r/min-1000 r/min; the time is 1min to 60 min.
In order to achieve the third purpose, the technical scheme adopted by the invention is as follows:
a heat-conducting lubricant which takes the composition as a raw material or is prepared according to the preparation method.
According to the invention, the heat-conducting lubricant can be used as a heat-conducting lubricant for a rolling bearing.
The invention has the advantages that at least the following aspects are achieved:
firstly, when the heat-conducting lubricant formed by the composition provided by the invention is applied to a rolling bearing, for example, the heat-conducting lubricant plays a lubricating role of lubricating grease on one hand, and plays a heat-conducting role through high filling of the heat-conducting filler on the other hand, so that heat generated by operation is effectively taken away, the damage and the abrasion of the bearing on a device body are reduced, and the service life of the bearing is prolonged.
Secondly, the heat-conducting lubricant provided by the invention is prepared in a ball-milling mode, and compared with the traditional stirring mode, the heat-conducting particles in the heat-conducting lubricant can be uniformly distributed, so that the heat transfer coefficient is improved; the heat-conducting lubricant can reduce the corrosivity to bearing materials and avoid the corrosive damage of the traditional lubricant to the bearing.
Thirdly, the novel heat-conducting lubricant with high viscosity and high heat conductivity can be designed and prepared, so that the problems of low viscosity, quick volatilization of grease, decomposition of grease and the like caused by high-speed operation of the traditional lubricant can be solved, the heat-conducting lubricant can be uniformly coated between the roller shaft and the roller, and the heat-conducting lubricant can fully form a grease outline along with the high-speed and low-speed rotation between the roller shaft and the roller.
Drawings
FIG. 1 is a process flow diagram of example 1 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to examples, but the scope of the present invention is not limited to the following description.
The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available from commercial sources.
In the following embodiments, unless otherwise specified:
dimethicone was purchased from wacke, germany, WACKER AK1000, with a kinematic viscosity of 1000mPa · S;
the grade of the silane coupling agent is KH 550;
the particle size of the alumina is 0.1-5 μm;
the particle size of the zinc oxide is 0.5-3 μm;
zinc stearate was purchased from weng shi chemistry and analytically pure;
ethyl acetate was purchased from weng shi chemical and analytically pure;
the inorganic salt is sodium nitrite, purchased from Dache chemical reagent factory in Tianjin;
the calcium-zinc heat stabilizer is purchased from Guangdong Weilinnan New materials science and technology GmbH, and has the brand number of WINNERWWP-Z08.
In the following embodiments, unless otherwise specified:
the thermal conductivity is tested in accordance with the standard ASTM-D547.
The rolling friction coefficient was tested with reference to the standard GB/T12583.
Example 1
The raw materials and the mixture ratio adopted in the embodiment are as follows:
100 parts by weight of simethicone; 1.65 parts by weight of a silane coupling agent KH 550; 300 parts of alumina; 30 parts of zinc oxide; 20 parts by weight of zinc stearate; ethyl acetate, 5 parts by weight; 3 parts of inorganic salt; 2 parts of calcium-zinc heat stabilizer.
The process flow diagram of the embodiment is shown in fig. 1, and the preparation method is as follows:
1) modifying the dried heat-conducting filler powder (namely aluminum oxide and zinc oxide) by using a silane coupling agent KH550, wherein the addition amount is 0.5 percent of the weight of the heat-conducting filler powder, specifically, firstly adding the silane coupling agent KH550 into absolute ethyl alcohol accounting for 25 percent of the weight of the heat-conducting filler powder, continuously stirring, adding the heat-conducting filler powder after the silane coupling agent KH550 is dissolved, and continuously stirring. Adjusting the pH value of the prepared mixture to 10, placing the mixture in a water bath at 50 ℃, continuously stirring for 3h, and finally performing ultrasonic dispersion for 15min under the condition of 60 kHz.
2) Filtering the heat-conducting filler powder, drying the modified heat-conducting filler obtained by filtering in a vacuum drying oven at 200 ℃ until the weight of the heat-conducting filler powder is constant, and taking out for later use;
3) mixing the modified heat-conducting filler powder with 100 parts of dimethyl silicone oil for 3 times, uniformly stirring, and then putting into a 120 ℃ oven for curing for 10 min;
4) placing the cured mixture obtained in the step 3) into a ball mill for ball milling and mixing, wherein the set rotating speed is 300r/min, and the stirring time is 30 min;
5) adding zinc stearate, ethyl acetate, inorganic salt and a calcium-zinc heat stabilizer into the mixture prepared in the step 4) in a set amount; setting the speed of the ball mill to be 350r/min and the ball milling time to be 30min, and obtaining the composite material which is fine, smooth and uniform and has no visible particles, namely the uniformly mixed multifunctional heat-conducting lubricant.
Tests show that the heat conductivity coefficient of the prepared multifunctional heat-conducting lubricant can reach 0.98W/m.K; the rolling friction coefficient of the heat-conductive lubricant was 0.05%.
Example 2
The raw materials and the mixture ratio adopted in the embodiment are as follows:
100 parts by weight of simethicone; 1.8 parts by weight of a silane coupling agent KH 550; 320 parts of alumina; 32 parts by weight of zinc oxide; 21 parts by weight of zinc stearate; ethyl acetate, 5.5 parts by weight; 3.5 parts by weight of inorganic salt; 2.5 parts of calcium-zinc heat stabilizer.
The preparation method adopted in this example is the same as that of example 1.
The test of the prepared heat-conducting lubricant shows that the heat-conducting performance of the heat-conducting lubricant can reach 0.98W/m.K; the rolling friction coefficient of the heat-conductive lubricant was 0.06%.
Example 3
The raw materials and the mixture ratio adopted in the embodiment are as follows:
100 parts by weight of simethicone; 1.5 parts by weight of a silane coupling agent KH 550; 280 parts by weight of alumina; 28 parts by weight of zinc oxide; 19 parts by weight of zinc stearate; ethyl acetate, 4.5 parts by weight; 2.5 parts by weight of inorganic salt; 1.5 parts of calcium-zinc heat stabilizer.
The preparation method adopted in this example is the same as that of example 1.
The test of the prepared heat-conducting lubricant shows that the heat-conducting performance of the heat-conducting lubricant can reach 0.96W/m.K; the rolling friction coefficient of the heat-conductive lubricant was 0.08%.
Example 4
The raw materials and the mixture ratio adopted in the embodiment are as follows:
100 parts by weight of simethicone; 1.65 parts by weight of a silane coupling agent KH 550; 300 parts of alumina; 30 parts of zinc oxide; 20 parts by weight of zinc stearate; ethyl acetate, 5 parts by weight; 3 parts of inorganic salt; 2 parts of calcium-zinc heat stabilizer.
The preparation method adopted in the embodiment is as follows:
1) modifying the dried heat-conducting filler powder (namely aluminum oxide and zinc oxide) by using a silane coupling agent KH550, wherein the addition amount is 0.5 percent of the weight of the heat-conducting filler powder, specifically, firstly adding the silane coupling agent KH550 into absolute ethyl alcohol accounting for 25 percent of the weight of the heat-conducting filler powder, continuously stirring, adding the heat-conducting filler powder after the silane coupling agent KH550 is dissolved, and continuously stirring. Adjusting the pH value of the prepared mixture to 10, placing the mixture in a water bath at 50 ℃, continuously stirring for 3h, and finally performing ultrasonic dispersion for 15 min.
2) Filtering the heat-conducting filler powder, drying the modified heat-conducting filler obtained by filtering in a vacuum drying oven at 200 ℃ until the weight of the heat-conducting filler powder is constant, and taking out for later use;
3) mixing the modified heat-conducting filler powder with 100 parts of dimethyl silicone oil for 3 times, uniformly stirring, and then putting into a 120 ℃ oven for curing for 10 min;
4) uniformly mixing the aged mixture obtained in the step 3) with zinc stearate, ethyl acetate, inorganic salt and a calcium-zinc heat stabilizer in a set amount to obtain the multifunctional heat-conducting lubricant.
The uniformity of the prepared heat-conducting lubricant material is poor, and the heat-conducting lubricant is tested, and the result shows that the heat-conducting property of the heat-conducting lubricant is only 0.45W/m.K; the rolling friction coefficient of the heat conductive lubricant was 0.2%.
Example 5
The raw materials and the mixture ratio adopted in the embodiment are as follows:
100 parts by weight of simethicone; 0.1 part by weight of silane coupling agent KH 550; 200 parts of alumina; 10 parts of zinc oxide; 10 parts by weight of zinc stearate; 1 part by weight of ethyl acetate; 1 part by weight of inorganic salt; 1 part of calcium-zinc heat stabilizer.
The test of the prepared heat-conducting lubricant shows that the heat-conducting performance of the heat-conducting lubricant is deteriorated, and the heat-conducting coefficient is only 0.35W/m.K; the rolling friction coefficient of the heat conductive lubricant was 0.15%.
Example 6
The raw materials and the mixture ratio adopted in the embodiment are as follows:
100 parts by weight of simethicone; 0.05 part by weight of silane coupling agent KH 550; 400 parts by weight of alumina; 50 parts by weight of zinc oxide; 30 parts by weight of zinc stearate; ethyl acetate, 7 parts by weight; 5 parts by weight of inorganic salt; 5 parts of calcium-zinc heat stabilizer.
The test of the prepared heat-conducting lubricant shows that the heat-conducting performance of the heat-conducting lubricant is poor, the heat-conducting lubricant is sticky and cannot be uniformly coated, and the heat-conducting coefficient is only 0.35W/m.K; the rolling friction coefficient of the heat conductive lubricant was 0.35%.
Example 7
The only difference from example 1 is that paraffin oil was used instead of zinc stearate to prepare a heat conductive lubricant. The results show that the performance of the prepared thermally conductive lubricant is comparable to that of example 1.
Example 8
The only difference from example 1 is that silicone was used instead of zinc stearate to prepare a thermally conductive lubricant. The results show that the performance of the prepared thermally conductive lubricant is comparable to that of example 1.
Example 9
The only difference from example 1 is that xylene was used instead of ethyl acetate to make a thermally conductive lubricant. The results show that the performance of the prepared thermally conductive lubricant is comparable to that of example 1.
Example 10
The only difference from example 1 is that n-hexane was used instead of ethyl acetate to prepare a thermally conductive lubricant. The results show that the performance of the prepared thermally conductive lubricant is comparable to that of example 1.
Example 11
The only difference from example 1 is that butanol was used instead of ethyl acetate to prepare a thermally conductive lubricant. The results show that the performance of the prepared thermally conductive lubricant is comparable to that of example 1.
Example 12
The only difference from example 1 is that sodium sulfite was used instead of the inorganic salt to prepare the thermally conductive lubricant. The results show that the performance of the prepared thermally conductive lubricant is comparable to that of example 1.
Comparative example 1
The raw materials and the mixture ratio adopted in the comparative example are as follows:
100 parts by weight of simethicone; 1.65 parts by weight of a silane coupling agent KH 550; 330 parts of alumina; 20 parts by weight of zinc stearate; ethyl acetate, 5 parts by weight; 3 parts of inorganic salt; 2 parts of calcium-zinc heat stabilizer.
This comparative example was prepared in the same manner as in example 1. The test of the prepared heat-conducting lubricant shows that the uniformity of the material is slightly poor, and the heat-conducting property of the heat-conducting lubricant is 0.6W/m.K; the rolling friction coefficient of the heat conductive lubricant was 0.12%.
Comparative example 2
The raw materials and the mixture ratio adopted in the comparative example are as follows:
100 parts by weight of simethicone; 1.65 parts by weight of a silane coupling agent KH 550; 330 parts by weight of zinc oxide; 20 parts by weight of zinc stearate; ethyl acetate, 5 parts by weight; 3 parts of inorganic salt; 2 parts of calcium-zinc heat stabilizer.
This comparative example was prepared in the same manner as in example 1. The test of the prepared heat-conducting lubricant shows that the surface uniformity of the heat-conducting lubricant is better, but the heat-conducting property of the heat-conducting lubricant is poorer and is only 0.3W/m.K; the rolling friction coefficient of the heat-conductive lubricant was 0.08%.
Comparative example 3
The raw materials and the mixture ratio adopted in the embodiment are as follows:
100 parts by weight of simethicone; 1.65 parts by weight of a silane coupling agent KH 550; 300 parts of alumina; 30 parts of zinc oxide; ethyl acetate, 5 parts by weight; 3 parts of inorganic salt; 2 parts of calcium-zinc heat stabilizer.
This comparative example was prepared in the same manner as in example 1. The prepared heat-conducting lubricant is tested, and the result shows that the heat-conducting performance of the heat-conducting lubricant is 0.95W/m.K; the lubricating property is poor, and the rolling friction coefficient of the heat-conducting lubricant is 0.4%.
Comparative example 4
The raw materials and the mixture ratio adopted in the embodiment are as follows:
100 parts by weight of simethicone; 1.65 parts by weight of a silane coupling agent KH 550; 300 parts of alumina; 30 parts of zinc oxide; 20 parts by weight of zinc stearate; 3 parts of inorganic salt; 2 parts of calcium-zinc heat stabilizer.
This comparative example was prepared in the same manner as in example 1. The prepared heat-conducting lubricant is tested, and the result shows that the heat-conducting lubricant generates a deposition phenomenon after being placed for 72 hours, the heat conductivity is 0.85W/m.K when the deposition phenomenon does not occur in the early stage, and the heat conductivity is only 0.4W/m.K after the deposition is generated; the rolling friction coefficient of the heat conductive lubricant was 0.28%.
Comparative example 5
The raw materials and the mixture ratio adopted in the embodiment are as follows:
100 parts by weight of simethicone; 1.65 parts by weight of a silane coupling agent KH 550; 300 parts of alumina; 30 parts of zinc oxide; 20 parts by weight of zinc stearate; ethyl acetate, 5 parts by weight; 3 parts of inorganic salt; 2 parts of calcium-zinc heat stabilizer.
This comparative example was prepared in the same manner as in example 1. The prepared heat-conducting lubricant is tested, and the result shows that the metal surface generates corrosion phenomenon after the heat-conducting lubricant is smeared on the metal surface for 720 hours, and the heat-conducting property of the heat-conducting lubricant is 0.95W/m.K; the lubricating property is good, the rolling friction coefficient of the heat-conducting lubricant is 0.06%, but the heat-conducting lubricant is easy to corrode a base material.
Comparative example 6
The raw materials and the mixture ratio adopted in the comparative example are as follows:
100 parts by weight of simethicone; 300 parts of alumina; 30 parts of zinc oxide; 20 parts by weight of zinc stearate; ethyl acetate, 5 parts by weight; 3 parts of inorganic salt; 2 parts of calcium-zinc heat stabilizer.
The preparation method adopted by the comparative example is as follows:
1) mixing heat-conducting filler powder (namely aluminum oxide and zinc oxide) with 100 parts of dimethyl silicone oil for 3 times, uniformly stirring, and putting into a 120 ℃ oven for curing for 10 min;
2) placing the cured mixture obtained in the step 1) into a ball mill for ball milling and mixing, wherein the set rotating speed is 300r/min, and the stirring time is 30 min;
3) adding zinc stearate, ethyl acetate, inorganic salt and a calcium-zinc heat stabilizer into the mixture prepared in the step 2) in a set amount; setting the speed of the ball mill to be 350r/min and the ball milling time to be 30min, and obtaining the composite material which is fine, smooth and uniform and has no visible particles, namely the uniformly mixed multifunctional heat-conducting lubricant.
The prepared heat-conducting lubricant is tested, and the result shows that the materials are not fully mixed, the particle phenomenon occurs, and the heat conductivity of the heat-conducting lubricant is only 0.15W/m.K; the lubricating property is poor, and the rolling friction coefficient of the heat-conducting lubricant is 0.5%.
It should be noted that the above-mentioned embodiments are only for explaining the present invention, and do not constitute any limitation to the present invention. The present invention has been described with reference to exemplary embodiments, but the words which have been used herein are words of description and illustration, rather than words of limitation. The invention can be modified, as prescribed, within the scope of the claims and without departing from the scope and spirit of the invention. Although the invention has been described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, but rather extends to all other methods and applications having the same functionality.
Claims (11)
1. A composition for forming a heat-conducting lubricant comprises the following components in parts by weight:
wherein the lubricant comprises one or more of zinc stearate, calcium stearate, paraffinic oil, naphthenic oil, and silicone; the anti-settling agent comprises one or more of ethyl acetate, butyl acetate, xylene, n-hexane and butanol; the inorganic salt is selected from one or more of nitrite and sulfite.
2. The composition according to claim 1, wherein the dimethicone has a dynamic viscosity of 100 to 15000mPa S.
3. Composition according to claim 1 or 2, characterized in that the particle size of the alumina is between 0.1 and 10 μm, preferably between 0.1 and 5 μm.
4. A composition according to any of claims 1 to 3, characterized in that the zinc oxide has a particle size of 0.1 to 5 μm, preferably 0.5 to 3 μm.
5. The composition of any one of claims 1-4, wherein the thermal stabilizer comprises one or more of a calcium zinc thermal stabilizer, a barium zinc stabilizer, and a barium cadmium stabilizer.
6. Composition according to any one of claims 1 to 5, characterized in that the silane coupling agent comprises one or more of KH550, KH560, KH570, preferably KH 550.
7. A method for preparing a thermally conductive lubricant starting from a composition according to any one of claims 1 to 6 and comprising the steps of:
s1, modifying the heat-conducting filler comprising the aluminum oxide and the zinc oxide by using the silane coupling agent to prepare a modified heat-conducting filler;
s2, mixing, curing and ball-milling the modified heat-conducting filler and the dimethyl silicone oil to obtain a silicone grease mixture;
and S3, mixing and ball-milling the silicone grease mixture, the zinc stearate, the ethyl acetate, the inorganic salt and the heat stabilizer to prepare the heat-conducting lubricant.
8. The production method according to claim 7, wherein in step S1, the step of modification treatment includes:
1) dissolving the silane coupling agent in a solvent, preferably absolute ethanol;
2) mixing the heat-conducting filler with the product prepared in the step 1);
3) adjusting the pH value of the product prepared in the step 2) to 9-11, and then carrying out water bath treatment on the product; and
optionally, 4) subjecting the product obtained in step 3) to ultrasonic treatment;
preferably, in step 3), the conditions of the water bath treatment include: the temperature is 35-65 ℃; the time is 1-5 h; and/or in step 4), the ultrasonic treatment conditions comprise: the frequency is 30 kHz-120 kHz; the time is 1min to 30 min.
9. The method according to claim 7 or 8, wherein in step S2, the conditions for aging include: the temperature is 80-150 ℃; the time is 1min to 30 min; and/or the conditions of said ball milling comprise: the rotating speed is 100 r/min-1000 r/min; the time is 1min to 60 min.
10. The method according to any one of claims 7 to 9, wherein in step S3, the ball milling conditions include: the rotating speed is 100 r/min-1000 r/min; the time is 1min to 60 min.
11. A thermally conductive lubricant prepared from the composition of any one of claims 1 to 6 or the preparation method of any one of claims 7 to 10.
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