CN106928722B - Silicone grease composition and preparation method thereof - Google Patents
Silicone grease composition and preparation method thereof Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/10—Liquid materials
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
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Abstract
The invention relates to the field of silicone grease, and discloses a silicone grease composition and a preparation method thereof, wherein the silicone grease composition comprises, by weight, 80-120 parts of silicone oil, 10-40 parts of modified phenyl silicone resin, 500-1500 parts of filler and 2-15 parts of coupling agent, wherein the modified phenyl silicone resin is prepared by semi-interpenetrating hybridization of phenyl silicone resin and α omega-dihydroxy polydimethylsiloxane under the action of alkali glue, and the silicone grease prepared by the invention can not become dry, hard and crack at 250 ℃, can keep a paste shape and can be used for a long time, has an oil separation degree of less than 0.1%, and can meet the requirements of products with high requirements on heat dissipation standards.
Description
Technical Field
The invention relates to the field of silicone grease, in particular to a silicone grease composition and a preparation method thereof.
Background
With the continuous progress of science and technology, the development of the industries such as electronics and electricity tends to be more intensive and miniaturized. Electronic devices can release a large amount of heat during operation, and if the heat cannot be conducted out in time, local high temperature is easily caused, so that the service life of the device is reduced. In general, silicone grease, which is a heat conductive material for electronic devices, is required to be used at 200 ℃ or higher for a long period of time while maintaining the original state of the grease, to have good chemical stability, to be nontoxic and odorless, and to be non-corrosive to a base material. However, with the development of electronic devices, the demand for silicone grease has also increased, and it is of practical significance to develop a silicone grease which remains as a grease when used at 250 ℃ for a long period of time and has a low oil separation degree.
Disclosure of Invention
The invention aims to provide a silicone grease composition.
In order to achieve the purpose, the invention adopts the following technical scheme:
the silicone grease composition comprises, by weight, 100 parts of silicone oil, 10-40 parts of modified phenyl silicone resin, 500-1500 parts of filler and 2-15 parts of coupling agent, wherein the modified phenyl silicone resin is prepared by half interpenetrating hybridization of phenyl silicone resin and α, omega-dihydroxy polydimethylsiloxane under the action of alkali glue.
Preferably, the silicone oil is 100 parts by weight, and the modified phenyl silicone resin is 30 parts by weight.
Preferably, 20-40 parts by weight of ethyl orthosilicate, 1-5 parts by weight of diphenyldimethoxysilane and 5-15 parts by weight of hexamethyldisiloxane are subjected to hydrolytic condensation under an acidic condition to obtain phenyl silicone resin, 10-60 parts by weight of phenyl silicone resin is added into a solvent to be dissolved, 100-200 parts by weight of α, omega-dihydroxy polydimethylsiloxane and 1-10 parts by weight of alkali gum are added, the reaction is carried out for 1-5 hours at 90-110 ℃, the temperature is raised to 140 ℃, the reaction is carried out for 20 minutes, and the solvent is evaporated under reduced pressure to obtain the alkali gum, wherein the alkali gum is prepared by the following method that 100 parts by weight of methyl cyclosiloxane is subjected to dehydration treatment for 30-40 minutes at 70-80 ℃, then 0.5-3 parts by weight of alkali is added, the temperature is raised to 120-130 ℃, and the reaction is carried out for 30-50 minutes under vacuum to obtain the methyl cyclosiloxane.
Preferably, the viscosity of the silicone oil is 350 to 1000 cps.
Preferably, the silicone oil is one or a mixture of more than two of dimethyl silicone oil, hydroxyl silicone oil, vinyl silicone oil, methyl phenyl silicone oil, chlorohydrocarbon modified silicone oil, fluorochlorohydrocarbon modified silicone oil and long-chain alkyl silicone oil.
Preferably, the particle size of the filler is 1-100 μm. Wherein, the shape of the filler can be granular, flaky, spherical and fibrous.
Preferably, the filler is one or a mixture of two or more of a metal, a metal oxide and a nonmetal.
Preferably, the metal is one or a mixture of more than two of silver, copper and aluminum; the metal oxide is one or a mixture of more than two of aluminum oxide, magnesium oxide and zinc oxide; the nonmetal is one or a mixture of more than two of aluminum nitride, silicon carbide and graphite.
Preferably, the coupling agent is one or a mixture of more than two of gamma-aminopropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane, propyltrimethoxysilane and vinyltrimethoxysilane.
The invention also aims to disclose a preparation method of the silicone grease composition, which comprises the following steps:
s1, mixing the silicone oil and the modified phenyl silicone resin according to the parts by weight at room temperature;
s2: adding a coupling agent to the mixture obtained in step S1 with stirring;
s3: adding a filler into the mixture prepared in the step S2, heating to 80-100 ℃, and stirring for 1h at constant temperature under reduced pressure;
s4: and (4) continuously heating the mixture prepared in the step (S3) to 115-130 ℃, stirring for 0.5-3 h, cooling and discharging.
In a semi-interpenetrating hybrid system, only one polymer is crosslinked, while the other polymer is still linear or branched, which can be generally divided into two types, one is that polymer I exists in the form of network and polymer II is linear; the other is that polymer I is linear and polymer II is in the form of a network.
The silicone grease composition mixes the silicone oil and the modified phenyl silicone resin to be used as the base oil, has the advantages of high temperature resistance and low oil separation, has better application property and thermal conductivity on the basis of keeping other excellent physical properties, can not become dry, hard and crack at 250 ℃, can keep pasty and can be used for a long time, the oil separation degree is less than 0.1 percent, and the requirements of special products can be met.
Detailed Description
In the embodiment of the invention, the methyl cyclosiloxane mixture is purchased from Hesheng Si Co., Zhejiang and is of industrial grade; gamma-aminopropyltriethoxysilane was purchased from japan shin-Etsu corporation under the model number KBM-903; gamma-glycidoxypropyltrimethoxysilane was purchased from Nippon Beacon corporation and designated KBM-403; gamma- (methacryloyloxy) propyltrimethoxysilane was purchased from japan shin-Etsu corporation under the model number KBM-503; propyltrimethoxysilane was purchased from Hubei Jusheng science and technology Co., Ltd; vinyl trimethoxy silane was purchased from Union, USA under the type A-171.
The present invention will be further described with reference to the following examples.
Example 1: preparation of alkali gels example 1
And (3) dehydrating 100g of methyl cyclosiloxane mixture at 70 ℃ for 40min, adding 0.5g of tetramethylammonium hydroxide, heating to 130 ℃ and reacting at-0.1 MPa for 50min to obtain the alkali glue.
Example 2: preparation of alkali Gum example 2
And (3) dehydrating 100g of methyl cyclosiloxane mixture at 80 ℃ for 30min, adding 3g of tetramethyl ammonium hydroxide, heating to 120 ℃, and reacting at-0.1 MPa for 30min to obtain the alkali glue.
Example 3: phenyl silicone resin preparation example 1
The preparation method comprises the steps of mixing 20g of ethyl orthosilicate, 1g of diphenyldimethoxysilane and 5g of hexamethyldisiloxane, slowly dropwise adding a mixed solution of ethanol, concentrated hydrochloric acid and deionized water in a volume ratio of 15:1:25, stirring for 50min at 45 ℃ after dropwise adding, heating to 70 ℃, reacting for 3-4 h under stirring, neutralizing reaction liquid after reaction, and extracting, washing with water, drying and distilling under reduced pressure to obtain the phenyl silicone resin.
Example 4: phenyl silicone resin preparation example 2
The preparation method comprises the steps of mixing and stirring 40g of ethyl orthosilicate, 5g of diphenyl dimethoxysilane and 15g of hexamethyldisiloxane, slowly dropwise adding a mixed solution of ethanol, concentrated hydrochloric acid and deionized water in a volume ratio of 15:1:25, stirring for 10min at 80 ℃ after dropwise adding, heating to 85 ℃, reacting for 3-4 h under stirring, neutralizing reaction liquid after reaction, and extracting, washing with water, drying and distilling under reduced pressure to obtain the phenyl silicone resin.
Example 5: preparation of modified phenyl Silicone resin example 1
Taking 10g of the phenyl silicone resin prepared in example 3, adding a solvent to completely dissolve the phenyl silicone resin, adding 100g of α, omega-dihydroxy polydimethylsiloxane and 1g of the alkali glue prepared in example 1 under rapid stirring, reacting for 5h at 90 ℃, continuously heating to 140 ℃, reacting for 20min, and evaporating the solvent under reduced pressure to obtain the modified phenyl silicone resin.
Example 6: preparation of modified phenyl Silicone resin example 2
60g of the phenyl silicone resin prepared in example 4 is taken, added with a solvent to be completely dissolved, added with 200g of α, omega-dihydroxy polydimethylsiloxane and 10g of the alkali glue prepared in example 2 under rapid stirring, reacted for 1h at 110 ℃, continuously heated to 150 ℃, reacted for 20min, and decompressed to remove the solvent, thus obtaining the modified phenyl silicone resin.
Example 7: preparation example 1 of Silicone grease composition
80g of methyl phenyl silicone oil with the viscosity of 350cps and 10g of the modified phenyl silicone resin prepared in the example 5 are stirred for 5min at room temperature under the revolution speed of 30r/min and the dispersion speed of 50 r/min; adding 2g of vinyl trimethoxy silane, and stirring for 5min at room temperature at a revolution speed of 20r/min and a dispersion speed of 50 r/min; then adding 350g of silicon carbide and 400g of flaky magnesium oxide, heating to 100 ℃, vacuumizing to-0.1 MPa, and stirring for 1h at constant pressure and constant temperature at a revolution speed of 30r/min and a dispersion speed of 50 r/min; heating to 130 ℃, vacuumizing and stirring for 0.5 h; and discharging after cooling.
Example 8: preparation example 2 of Silicone grease composition
120g of hydroxyl silicone oil with the viscosity of 350cps and 40g of the modified phenyl silicone resin prepared in the embodiment 6 are stirred for 20min at room temperature under the revolving speed of 10r/min and the dispersing speed of 30 r/min; adding 15g of propyl trimethoxy silane, and stirring at room temperature at a revolution speed of 10r/min and a dispersion speed of 30r/min for 15 min; adding 300g of copper powder and 200g of graphite, heating to 80 ℃, vacuumizing to-0.085 MPa, and stirring for 1h at constant pressure and constant temperature at a revolution speed of 10r/min and a dispersion speed of 30 r/min; heating to 115 ℃, vacuumizing and stirring for 3 hours; and discharging after cooling.
Example 9: preparation example 3 of Silicone grease composition
As a preferred example, 100g of the dimethylsilicone fluid having a viscosity of 350cps and 30g of the modified phenylsilicone resin obtained in example 5 were stirred at room temperature at a revolution speed of 15r/min and a dispersion speed of 40r/min for 10 min; adding 2g of gamma-glycidoxypropyltrimethoxysilane, and stirring at room temperature at revolution speed of 10r/min and dispersion speed of 30r/min for 5 min; then adding 600g of zinc oxide and 500g of spherical alumina, heating to 80 ℃, vacuumizing to-0.085 MPa, and stirring for 1h at constant pressure and constant temperature at a revolution speed of 20r/min and a dispersion speed of 40 r/min; heating to 115 ℃, vacuumizing and stirring for 3 hours; and discharging after cooling.
Example 10: preparation example 4 of Silicone grease composition
As a preferred example, 100g of hydroxy silicone oil with a viscosity of 350cps and 30g of the modified phenyl silicone resin obtained in example 6 were stirred at room temperature for 10min at a revolution speed of 15r/min and a dispersion speed of 40 r/min; adding 2g of gamma-glycidoxypropyltrimethoxysilane, and stirring at room temperature at a revolution speed of 10r/min and a dispersion speed of 30r/min for 5 min; then adding 600g of zinc oxide and 500g of spherical alumina, heating to 80 ℃, vacuumizing to-0.085 MPa, and stirring for 1h at constant pressure and constant temperature at a revolution speed of 20r/min and a dispersion speed of 40 r/min; heating to 115 ℃, vacuumizing and stirring for 3 hours; and discharging after cooling.
Example 11: silicone grease composition preparation comparative example 1
Stirring 100g of dimethyl silicone oil with the viscosity of 350cps and 30g of hydroxyl silicone oil with the viscosity of 1000cps for 10min at room temperature at the revolution speed of 15r/min and the dispersion speed of 40 r/min; adding 2g of gamma-glycidoxypropyltrimethoxysilane, and stirring at room temperature at a revolution speed of 10r/min and a dispersion speed of 30r/min for 5 min; adding 600g of granular zinc oxide and 500g of flaky alumina, heating to 80 ℃, vacuumizing to-0.085 MPa, stirring for 1h at constant pressure and constant temperature at a revolution speed of 20/min and a dispersion speed of 40 r/min; heating to 115 ℃, vacuumizing and stirring for 3 hours; and discharging after cooling.
Example 12: preparation of Silicone grease composition comparative example 2
Stirring 100g of dimethyl silicone oil with the viscosity of 350cps and 30g of chlorocarbon modified silicone oil with the viscosity of 1000cps for 10min at room temperature at the revolution speed of 15r/min and the dispersion speed of 40 r/min; adding 2g of gamma-glycidoxypropyltrimethoxysilane, and stirring at room temperature at a revolution speed of 10r/min and a dispersion speed of 30r/min for 5 min; adding 600g of zinc oxide and 500g of spherical alumina, heating to 80 ℃, vacuumizing to-0.085 MPa, stirring for 1h at constant pressure and constant temperature at a revolution speed of 20/min and a dispersion speed of 40 r/min; heating to 130 ℃, vacuumizing and stirring for 0.5 h; and discharging after cooling.
Example 13: preparation of Silicone grease composition comparative example 3
Stirring 100g of hydroxyl silicone oil with the viscosity of 350cps and 30g of dimethyl silicone oil with the viscosity of 1000cps for 10min at room temperature at the revolution speed of 15r/min and the dispersion speed of 40 r/min; adding 2g of gamma-glycidoxypropyltrimethoxysilane, and stirring at room temperature at a revolution speed of 10r/min and a dispersion speed of 30r/min for 5 min; adding 600g of zinc oxide and 500g of spherical alumina, heating to 80 ℃, vacuumizing to-0.085 MPa, stirring for 1h at constant pressure and constant temperature at a revolution speed of 20/min and a dispersion speed of 40 r/min; heating to 115 ℃, vacuumizing and stirring for 3 hours; and discharging after cooling.
Example 14: effects of the embodiment
The silicone grease compositions prepared in examples 9 to 13 were subjected to performance tests, and the results are as follows. It can be concluded that the silicone grease composition of the present invention with the modified phenyl silicone resin still presents a paste shape after being placed at 250 ℃ for 14 days, does not become dry, hard and cracked, has a freeness of less than 0.1%, and can be applied to products with high requirements for heat dissipation.
| Condition | Example 9 | Example 10 | Example 11 | Example 12 | Example 13 |
| 250℃×14d | Paste form | Paste form | Becomes dry and hard | Becomes dry and hard | Becomes dry and hard |
| Oil degree of separation/%) | 0.02 | 0.08 | 0.24 | 0.19 | 0.31 |
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be encompassed by the present invention.
Claims (8)
1. The silicone grease composition is characterized by comprising the following components, by weight, 100 parts of silicone oil, 30 parts of modified phenyl silicone resin, 500-1100 parts of filler and 2-15 parts of coupling agent, wherein the modified phenyl silicone resin is prepared by semi-interpenetrating hybridization of phenyl silicone resin and α, omega-dihydroxy polydimethylsiloxane under the action of alkali glue, and is prepared by the following method:
the preparation method comprises the steps of carrying out hydrolytic condensation on 20-40 parts by weight of ethyl orthosilicate, 1-5 parts by weight of diphenyldimethoxysilane and 5-15 parts by weight of hexamethyldisiloxane under an acidic condition to obtain phenyl silicone resin, adding 10-60 parts by weight of phenyl silicone resin into a solvent to dissolve the phenyl silicone resin, adding 100-200 parts by weight of α, omega-dihydroxy polydimethylsiloxane and 1-10 parts by weight of alkali glue to react for 1-5 hours at 90-110 ℃, then heating to 140-150 ℃, reacting for 20min, and evaporating the solvent under reduced pressure to obtain the phenyl silicone resin.
2. The silicone grease composition according to claim 1, wherein: the viscosity of the silicone oil is 350-1000 cps.
3. The silicone grease composition according to claim 1, wherein: the silicone oil is one or a mixture of more than two of dimethyl silicone oil, hydroxyl silicone oil, vinyl silicone oil, methyl phenyl silicone oil, chlorohydrocarbon modified silicone oil, fluorochlorohydrocarbon modified silicone oil and long-chain alkyl silicone oil.
4. The silicone grease composition according to claim 1, wherein: the particle size of the filler is 1-100 mu m.
5. The silicone grease composition according to claim 4, wherein: the filler is one or a mixture of more than two of metal, metal oxide and nonmetal.
6. The silicone grease composition according to claim 5, wherein: the metal is one or a mixture of more than two of silver, copper and aluminum; the metal oxide is one or a mixture of more than two of aluminum oxide, magnesium oxide and zinc oxide; the nonmetal is one or a mixture of more than two of aluminum nitride, silicon carbide and graphite.
7. The silicone grease composition according to claim 1, wherein: the coupling agent is one or a mixture of more than two of gamma-aminopropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane, propyltrimethoxysilane and vinyl trimethoxysilane.
8. The method for preparing a silicone grease composition according to claim 1, characterized by comprising the steps of:
s1, mixing the silicone oil with the modified phenyl silicone resin at room temperature;
s2: adding a coupling agent to the mixture obtained in step S1 with stirring;
s3: adding a filler into the mixture prepared in the step S2, heating to 80-100 ℃, and stirring for 1h at constant temperature under reduced pressure;
s4: and (4) continuously heating the mixture prepared in the step (S3) to 115-130 ℃, stirring for 0.5-3 h, cooling and discharging.
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| CN103289414A (en) * | 2012-02-29 | 2013-09-11 | 中化蓝天集团有限公司 | Heat-resistant and flame-retardant room-temperature vulcanized silicone rubber composition |
| CN104788961A (en) * | 2015-05-20 | 2015-07-22 | 龚灿锋 | LED encapsulating material |
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| US8772407B2 (en) * | 2007-09-17 | 2014-07-08 | Ppg Industries Ohio, Inc. | One component polysiloxane coating compositions and related coated substrates |
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| CN103289414A (en) * | 2012-02-29 | 2013-09-11 | 中化蓝天集团有限公司 | Heat-resistant and flame-retardant room-temperature vulcanized silicone rubber composition |
| CN104788961A (en) * | 2015-05-20 | 2015-07-22 | 龚灿锋 | LED encapsulating material |
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| Title |
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| 聚二甲基硅氧烷/苯基MDQ硅树脂弹性体的制备与性能;黄计锋; 葛建芳 等;《化工新型材料》;20150915;第77-79页 * |
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