CN115433461B - Heat-conducting silicone grease with low oil separation rate and long storage life and preparation method thereof - Google Patents
Heat-conducting silicone grease with low oil separation rate and long storage life and preparation method thereof Download PDFInfo
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- CN115433461B CN115433461B CN202211120189.9A CN202211120189A CN115433461B CN 115433461 B CN115433461 B CN 115433461B CN 202211120189 A CN202211120189 A CN 202211120189A CN 115433461 B CN115433461 B CN 115433461B
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- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 60
- 239000004519 grease Substances 0.000 title claims abstract description 59
- 238000003860 storage Methods 0.000 title claims abstract description 33
- 238000000926 separation method Methods 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000000945 filler Substances 0.000 claims abstract description 56
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 29
- 229920002545 silicone oil Polymers 0.000 claims abstract description 11
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- AMTWCFIAVKBGOD-UHFFFAOYSA-N dioxosilane;methoxy-dimethyl-trimethylsilyloxysilane Chemical compound O=[Si]=O.CO[Si](C)(C)O[Si](C)(C)C AMTWCFIAVKBGOD-UHFFFAOYSA-N 0.000 claims description 20
- 229940083037 simethicone Drugs 0.000 claims description 20
- 238000004381 surface treatment Methods 0.000 claims description 14
- 239000011231 conductive filler Substances 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 10
- 238000004898 kneading Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- ZYAASQNKCWTPKI-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propan-1-amine Chemical compound CO[Si](C)(OC)CCCN ZYAASQNKCWTPKI-UHFFFAOYSA-N 0.000 claims description 7
- MQWFLKHKWJMCEN-UHFFFAOYSA-N n'-[3-[dimethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical compound CO[Si](C)(OC)CCCNCCN MQWFLKHKWJMCEN-UHFFFAOYSA-N 0.000 claims description 7
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 5
- CZWLNMOIEMTDJY-UHFFFAOYSA-N hexyl(trimethoxy)silane Chemical compound CCCCCC[Si](OC)(OC)OC CZWLNMOIEMTDJY-UHFFFAOYSA-N 0.000 claims description 5
- 150000004757 linear silanes Chemical group 0.000 claims description 5
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 claims description 5
- 238000004821 distillation Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- VRINOTYEGADLMW-UHFFFAOYSA-N heptyl(trimethoxy)silane Chemical compound CCCCCCC[Si](OC)(OC)OC VRINOTYEGADLMW-UHFFFAOYSA-N 0.000 claims description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 3
- JEPXSTGVAHHRBD-UHFFFAOYSA-N trimethoxy(nonyl)silane Chemical compound CCCCCCCCC[Si](OC)(OC)OC JEPXSTGVAHHRBD-UHFFFAOYSA-N 0.000 claims description 3
- NMEPHPOFYLLFTK-UHFFFAOYSA-N trimethoxy(octyl)silane Chemical compound CCCCCCCC[Si](OC)(OC)OC NMEPHPOFYLLFTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims 1
- HILHCDFHSDUYNX-UHFFFAOYSA-N trimethoxy(pentyl)silane Chemical compound CCCCC[Si](OC)(OC)OC HILHCDFHSDUYNX-UHFFFAOYSA-N 0.000 claims 1
- 239000003973 paint Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 12
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000004020 conductor Substances 0.000 description 4
- 238000007790 scraping Methods 0.000 description 4
- 238000009413 insulation Methods 0.000 description 3
- KRJRKEPWQOASJN-UHFFFAOYSA-N aniline;trimethoxy(methyl)silane Chemical compound NC1=CC=CC=C1.CO[Si](C)(OC)OC KRJRKEPWQOASJN-UHFFFAOYSA-N 0.000 description 2
- 239000002612 dispersion medium Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000012756 surface treatment agent Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- MEWFSXFFGFDHGV-UHFFFAOYSA-N cyclohexyl(trimethoxy)silane Chemical group CO[Si](OC)(OC)C1CCCCC1 MEWFSXFFGFDHGV-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 1
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/16—Solid spheres
- C08K7/18—Solid spheres inorganic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- 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
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
Abstract
The invention discloses a heat-conducting silicone grease with low oil separation rate and long storage life and a preparation method thereof. The heat-conducting silicone grease with low oil separation rate and long storage period comprises the following raw materials: 100 parts of dimethyl silicone oil, 800-1200 parts of heat conducting filler, 0.3-0.8 part of surface treating agent and 0.1-0.2 part of accelerator. The invention also provides a preparation method of the heat-conducting silicone grease, which has the advantages of low oil-off rate, long storage period, low viscosity and good insulativity, can ensure that the working life of electronic products is longer, more stable and reliable in application, is easy to paint, and can be normally used at the position with dense electrodes.
Description
Technical Field
The invention relates to heat-conducting silicone grease, in particular to heat-conducting silicone grease with low oil release rate and long storage life, and belongs to the technical field of heat-conducting materials.
Background
The heat-conducting silicone grease is a product widely applied, and is mainly coated on high-power electronic components, so that the heat is conducted away in time, and the temperature is prevented from rising greatly. The reliability is reduced by 10% when the temperature of the electronic components is increased by 2 ℃, so the stability of the heat conduction silicone grease is particularly important.
The traditional heat conduction silicone grease has a storage period of about 4-8 months, and after the storage period is exceeded, the heat conduction filler in the heat conduction silicone grease can be separated due to the gravity of the heat conduction filler and the problems of poor interface compatibility with silicone oil and the like, so that the phenomena of oil seepage and the like occur, other elements of a circuit board are polluted, and particularly, when the heat conduction silicone grease is used on an upright surface, even oil dripping occurs. Meanwhile, the heat conduction performance and stability of the heat conduction silicone grease are obviously reduced after oil powder is separated, so that the temperature rise of the electronic element is obvious, and the electronic element is unstable in work and even fails. The shelf life of the thermally conductive silicone grease is therefore important for the stability of the electronic component.
The heat conduction silicone grease disclosed in the specification of CN201610935441.X mainly selects silicone oil with the viscosity of 50-1500 mPas, adds a certain amount of oil-inhibiting additive, and matches with proper heat conduction filler to enable the heat conductivity to reach 2.3W/m.k, and reduces the oil separation rate to 0.65%.
The heat conduction silicone grease disclosed in CN201711395858.2 is prepared by adding a proper amount of vinyl silane into 500-1000 parts of dimethylbenzene to perform surface treatment on a heat conduction filler, wherein the oil separation degree of the heat conduction silicone grease is 0.19%, and the heat conduction coefficient is 2.6W/mK, but a large amount of dimethylbenzene solvent is used in the production process, so that the heat conduction silicone grease does not meet the current increasingly strict environmental protection requirements and trends.
The heat-conducting silicone grease disclosed in CN201910804383.0 uses copper powder as a main heat-conducting material, and has high heat conductivity and low oil separation rate of 0.48-0.54%, but cannot be used in the field with insulation requirements.
In the heat-conducting silicone grease disclosed in CN202110817413.9, a layer of aniline methyl trimethoxy silane is wrapped on the surface of the heat-conducting filler, so that the stability of powder in resin is improved, and the storage life of the silicone grease is prolonged, but the viscosity of the finished silicone grease is relatively high due to relatively large molecular steric hindrance of the aniline methyl trimethoxy silane, and the viscosity of the finished silicone grease is as high as 500000 mPa.s or even 800000 mPa.s, and the coating and scraping properties are relatively poor.
Therefore, the manufacture of the heat-conducting silicone grease with low oil release rate, long storage period, easy coating and scraping (low viscosity) and high insulativity is an urgent need for industry development.
Disclosure of Invention
In view of the above, the present invention aims to overcome the defects of the prior art and provide a heat-conducting silicone grease with low oil release rate, long storage period, easy coating and scraping and high insulation property. The heat-conducting silicone grease can effectively solve the problems of high oil release rate, short storage period and the like of the traditional heat-conducting silicone grease, greatly improves the working stability of electronic components and prolongs the working life.
In order to achieve the above purpose, the invention adopts the following technical scheme: the heat-conducting silicone grease with low oil release rate and long storage period is provided, and the raw material composition of the heat-conducting silicone grease with low oil release rate and long storage period comprises: 100 parts of dimethyl silicone oil, 800-1200 parts of heat conducting filler, 0.3-0.8 part of surface treating agent and 0.1-0.2 part of accelerator.
Specifically, the heat-conducting silicone grease with low oil separation rate and long storage life comprises the following raw materials: 100 parts of dimethyl silicone oil, 800-1200 parts of heat conducting filler, 0.5-0.8 part of surface treating agent and 0.1-0.2 part of accelerator.
Specifically, the viscosity of the adopted simethicone is 5000cPs-20000cPs.
Specifically, the heat conductive filler used is spherical alumina.
Specifically, the particle diameter D50 of the heat conductive filler is 1-5 μm.
Specifically, the adopted surface treating agent is a linear silane coupling agent and comprises at least one of n-amyl trimethoxy silane, n-hexyl trimethoxy silane, n-heptyl trimethoxy silane, n-octyl trimethoxy silane, n-nonyl trimethoxy silane and n-sunflower trimethoxy silane.
Specifically, the accelerator is amino dialkoxysilane, and contains at least one of N- (beta-aminoethyl) -gamma-aminopropyl methyl dimethoxy silane and gamma-aminopropyl methyl dimethoxy silane.
In order to achieve the technical aim, the invention also provides a preparation method of the heat-conducting silicone grease with low oil separation rate and long storage life, which comprises the following steps:
mixing a heat conducting filler, a surface treating agent and an accelerator, and carrying out surface treatment on the heat conducting filler;
and (3) mixing and kneading the simethicone and the heat-conducting filler subjected to surface treatment for 1-2 h, heating to 110-120 ℃, keeping the vacuum degree between-0.08 and-0.09 MPa, vacuumizing and kneading for 3-6 h, and cooling to room temperature to obtain the heat-conducting silicone grease with low oil separation rate and long storage period.
Specifically, the method for surface treatment of the heat conductive filler comprises the following steps:
adding ethanol and a surface treating agent into the heat-conducting filler, and stirring and dispersing for 1h;
slowly dripping an accelerator, and stirring and refluxing for 2-4 hours at 60-70 ℃;
cooling to room temperature, and performing reduced pressure distillation;
baking the distilled heat conducting filler for 2-4 hours at 120-140 ℃; cooling to room temperature to obtain the heat conducting filler subjected to surface treatment.
Specifically, the mixing mass ratio of the heat conduction filler to the ethanol is 100-120:70-90; preferably 100:80.
The heat-conducting silicone grease with low oil separation rate and long storage period is prepared by taking high-viscosity dimethyl silicone oil as a matrix, adding spherical alumina with small particle size as a heat-conducting material, and carrying out high-temperature mixing. Meanwhile, the heat conducting material is subjected to surface modification by taking ethanol as a dispersion medium and adding a linear silane coupling agent, so that the compatibility of the heat conducting filler and the dimethyl silicone oil is effectively improved, the viscosity after mixing can be obviously reduced, and the coating and scraping performance is greatly improved.
The heat-conducting silicone grease has the advantages of low oil release rate, long storage period, low viscosity and good insulativity, can ensure that the working life of electronic products is longer, more stable and reliable in application, is easy to paint, and can be normally used at the position where the electrodes are dense. Only ethanol is used as a dispersion medium in the treatment process of the heat conducting filler, and the heat conducting filler can be recycled, thereby meeting the current environmental protection requirement.
Detailed Description
The heat-conducting silicone grease with low oil separation rate and long storage period comprises the following raw materials: 100 parts of dimethyl silicone oil, 800-1200 parts of heat conducting filler, 0.3-0.8 part of surface treating agent and 0.1-0.2 part of accelerator.
In one embodiment of the invention, the viscosity of the dimethyl silicone oil is 5000cPs-20000cPs. For example, the viscosity of the simethicone is 5000cPs, 6000cPs, 7000cPs, 8000cPs, 9000cPs, 15000cPs, 18000cPs.
In one embodiment of the present invention, the thermally conductive filler used is spherical alumina.
In one embodiment of the invention, the thermally conductive filler is used with a particle size D50 of 1 to 5. Mu.m. For example, the particle diameter D50 of the heat conductive filler is 2 μm, 3 μm, 4 μm.
In one embodiment of the present invention, the surface treating agent is a linear silane coupling agent, and the surface treating agent comprises at least one of n-amyl trimethoxy silane, n-hexyl trimethoxy silane, n-heptyl trimethoxy silane, n-octyl trimethoxy silane, n-nonyl trimethoxy silane and n-sunflower trimethoxy silane. For example, the surface treating agent is n-amyl trimethoxy silane, n-hexyl trimethoxy silane or n-sunflower-base trimethoxy silane.
In one embodiment of the present invention, the accelerator is amino dialkoxysilane comprising at least one of N- (beta-aminoethyl) -gamma-aminopropyl methyldimethoxy silane and gamma-aminopropyl methyldimethoxy silane. For example, the accelerator used is N- (beta-aminoethyl) -gamma-aminopropyl methyldimethoxy silane or gamma-aminopropyl methyldimethoxy silane.
The preparation method of the heat-conducting silicone grease with low oil separation rate and long storage life comprises the following steps:
mixing a heat conducting filler, a surface treating agent and an accelerator, and carrying out surface treatment on the heat conducting filler;
and mixing and kneading the simethicone and the heat-conducting filler subjected to surface treatment for 1-2 h (such as 1h or 2 h), heating to 110-120 ℃ (such as 110 ℃, 115 ℃ or 120 ℃), maintaining the vacuum degree between-0.08 and-0.09 MPa (such as-0.08 MPa, -0.088MPa, -0.09 MPa), vacuumizing and kneading for 3-6 h (such as 3h, 4h, 5h or 6 h), and cooling to room temperature to obtain the heat-conducting silicone grease with low oil separation rate and long storage life.
Specifically, the method for surface treatment of the heat conductive filler comprises the following steps:
adding ethanol and a surface treating agent into the heat-conducting filler, and stirring and dispersing for 1h; specifically, the mixing mass ratio of the heat conduction filler to the ethanol is 100-120:70-90; for example, it may be 100-90, 100:85, 100:80.
Slowly dripping the accelerator, and stirring and refluxing for 2-4 h (such as 2h, 3h or 4 h) at 60-70 ℃ (such as 60 ℃, 65 ℃ or 70 ℃);
cooling to room temperature, and performing reduced pressure distillation;
baking the distilled heat conducting filler for 2-4 h (such as 2h, 3h or 4 h) at 120-140 ℃ (such as 120 ℃, 130 ℃ or 140 ℃); cooling to room temperature to obtain the heat conducting filler subjected to surface treatment.
The following detailed description of the preferred embodiments of the present invention will be provided in connection with.
Example 1
The embodiment provides a heat-conducting silicone grease with low oil separation rate and long storage life, which comprises the following components in parts by weight: 100 parts of simethicone, 800 parts of heat conducting filler, 0.5 part of surface treating agent and 0.1 part of accelerator.
In the embodiment, the viscosity of the simethicone is 20000cPs, the heat conducting filler is alumina, the particle diameter D50 of the heat conducting filler is 1 mu m, the surface treating agent is n-amyl trimethoxy silane, and the accelerator is gamma-aminopropyl methyl dimethoxy silane.
The preparation method of the heat-conducting silicone grease with low oil separation rate and long storage life comprises the following steps:
adding 80 parts of ethanol and a surface treating agent into 100 parts of heat conducting filler, and stirring and dispersing for 1h; dripping an accelerator, and stirring and refluxing for 2-4 hours at 60-70 ℃; cooling to room temperature, and performing reduced pressure distillation by using a rotary evaporator; placing the distilled heat conducting filler into a baking oven at 120-140 ℃ for baking for 2-4 hours; and cooling to room temperature to obtain the heat conducting filler with the finished surface treatment.
The preparation method of the heat-conducting silicone grease comprises the following steps: adding the simethicone and the heat-conducting filler into a kneader, mixing and kneading for 1-2 h, heating to 110-120 ℃, keeping the vacuum degree at-0.08 to-0.09 MPa, vacuumizing and kneading for 3-6 h, and cooling to room temperature to obtain the heat-conducting silicone grease.
Example 2
The embodiment provides a heat-conducting silicone grease with low oil separation rate and long storage life, which comprises the following components in parts by weight: 100 parts of simethicone, 800 parts of heat conducting filler, 0.5 part of surface treating agent and 0.1 part of accelerator.
In the embodiment, the viscosity of the simethicone is 20000cPs, the heat conducting filler is spherical alumina, the particle diameter D50 of the heat conducting filler is 5 mu m, the surface treating agent is n-amyl trimethoxy silane, and the accelerator is gamma-aminopropyl methyl dimethoxy silane.
Example 3
The embodiment provides a heat-conducting silicone grease with low oil separation rate and long storage life, which comprises the following components in parts by weight: 100 parts of simethicone, 1200 parts of heat conducting filler, 0.5 part of surface treating agent and 0.1 part of accelerator.
In the embodiment, the viscosity of the simethicone is 20000cPs, the heat conducting filler is spherical alumina, the particle diameter D50 of the heat conducting filler is 5 mu m, the surface treating agent is n-amyl trimethoxy silane, and the accelerator is gamma-aminopropyl methyl dimethoxy silane.
Example 4
The embodiment provides a heat-conducting silicone grease with low oil separation rate and long storage life, which comprises the following components in parts by weight: 100 parts of simethicone, 1200 parts of heat conducting filler, 0.8 part of surface treating agent and 0.2 part of accelerator.
In the embodiment, the viscosity of the simethicone is 20000cPs, the heat conducting filler is spherical alumina, the particle diameter D50 of the heat conducting filler is 5 mu m, the surface treating agent is N-amyl trimethoxy silane, and the accelerator is N- (beta-aminoethyl) -gamma-aminopropyl methyl dimethoxy silane.
Example 5
The embodiment provides a heat-conducting silicone grease with low oil separation rate and long storage life, which comprises the following components in parts by weight: 100 parts of simethicone, 1200 parts of heat conducting filler, 0.5 part of surface treating agent and 0.2 part of accelerator.
In the embodiment, the viscosity of the simethicone is 20000cPs, the heat conducting filler is spherical alumina, the particle diameter D50 of the heat conducting filler is 5 mu m, the surface treating agent is N-sunflower-base trimethoxysilane, and the accelerator is N- (beta-aminoethyl) -gamma-aminopropyl methyldimethoxy silane.
Example 6
The embodiment provides a heat-conducting silicone grease with low oil separation rate and long storage life, which comprises the following components in parts by weight: 100 parts of simethicone, 1200 parts of heat conducting filler, 0.5 part of surface treating agent and 0.2 part of accelerator.
In the embodiment, the viscosity of the simethicone is 5000cPs, the heat conducting filler is spherical alumina, the particle size D50 of the heat conducting filler is 2 mu m, the surface treating agent is N-hexyl trimethoxysilane, and the accelerator is N- (beta-aminoethyl) -gamma-aminopropyl methyldimethoxy silane.
Comparative example 1
The only difference between this example and example 1 is that the viscosity of the simethicone was 500cPs.
Comparative example 2
The only difference between this comparative example and example 1 is that the particle diameter D50 of the heat conductive filler is 20 μm.
Comparative example 3
The only difference between this comparative example and example 1 is that the surface treatment agent is cyclohexyltrimethoxysilane.
Comparative example 4
The only difference between this comparative example and example 1 is that the surface treatment agent was 2 parts.
Comparative example 5
The only difference between this comparative example and example 1 is that the accelerator is gamma- (2, 3-glycidoxy) propyltrimethoxysilane.
Comparative example 6
The only difference between this comparative example and example 1 is that the accelerator was 1 part.
The heat conductive silicone greases obtained in examples 1 to 6 and comparative examples 1 to 6 were tested for heat conductivity according to ASTM-D5470, oil separation according to HG/T2502-1993, viscosity according to ASTM D2196-1999, volume resistivity according to GB/T1410-2006. The performance indexes are shown in table 1.
TABLE 1
As can be seen from Table 1, the heat-conducting silicone grease of the present invention has the advantages of low oil release rate, long storage life, low viscosity and high insulation.
The above embodiments are provided to illustrate the technical concept and features of the present invention and are intended to enable those skilled in the art to understand the content of the present invention and implement the same, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made in accordance with the spirit of the present invention should be construed to be included in the scope of the present invention.
Claims (9)
1. The heat conduction silicone grease with low oil release rate and long storage period comprises the following raw materials: 100 parts of dimethyl silicone oil, 800-1200 parts of heat conducting filler, 0.3-0.8 part of surface treating agent and 0.1-0.2 part of accelerator;
the preparation method of the heat-conducting silicone grease with low oil separation rate and long storage period comprises the following steps:
surface treatment is carried out on the heat conducting filler;
the method for carrying out surface treatment on the heat-conducting filler comprises the following steps:
adding ethanol and a surface treating agent into the heat-conducting filler, and stirring and dispersing for 1h;
slowly dripping an accelerator, and stirring and refluxing for 2-4 hours at the temperature of 60-70 ℃;
cooling to room temperature, and performing reduced pressure distillation;
drying the distilled heat conducting filler at 120-140 ℃ for 2-4 hours; cooling to room temperature to obtain the heat-conducting filler subjected to surface treatment; the surface treating agent is a linear silane coupling agent;
and mixing and kneading the simethicone and the heat-conducting filler subjected to surface treatment for 1-2 hours, heating to 110-120 ℃, maintaining the vacuum degree at-0.08 to-0.09 MPa, vacuumizing and kneading for 3-6 hours, and cooling to room temperature to obtain the heat-conducting silicone grease with low oil separation rate and long storage life.
2. The long shelf life heat conductive silicone grease of claim 1, wherein the raw material composition of the long shelf life heat conductive silicone grease comprises: 100 parts of dimethyl silicone oil, 800-1200 parts of heat conducting filler, 0.5-0.8 part of surface treating agent and 0.1-0.2 part of accelerator.
3. The heat conductive silicone grease having a low oil release rate and a long shelf life according to claim 1 or 2, wherein the viscosity of the simethicone is 5000cPs to 20000cPs.
4. The heat conductive silicone grease having a low oil release rate and a long pot life according to claim 1 or 2, wherein the heat conductive filler is spherical alumina.
5. The heat conductive silicone grease with low oil release rate and long shelf life according to claim 1, 2 or 4, wherein the particle diameter D50 of the heat conductive filler is 1-5 μm.
6. The low oil-release rate long shelf life heat conductive silicone grease according to claim 1 or 2, wherein the linear silane coupling agent comprises at least one of n-pentyltrimethoxysilane, n-hexyltrimethoxysilane, n-heptyltrimethoxysilane, n-octyltrimethoxysilane, n-nonyltrimethoxysilane, and n-sunflower-based trimethoxysilane.
7. The heat conductive silicone grease with low oil separation rate and long pot life according to claim 1 or 2, wherein the accelerator is amino dialkoxysilane comprising at least one of N- (β -aminoethyl) - γ -aminopropyl methyl dimethoxy silane and γ -aminopropyl methyl dimethoxy silane.
8. The long shelf life heat conductive silicone grease with low oil release rate according to claim 1, wherein the mixing mass ratio of the heat conductive filler to ethanol is 100-120:70-90.
9. The long shelf life heat conductive silicone grease with low oil release rate according to claim 8, wherein the mixing mass ratio of the heat conductive filler to ethanol is 100:80.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211120189.9A CN115433461B (en) | 2022-09-15 | 2022-09-15 | Heat-conducting silicone grease with low oil separation rate and long storage life and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211120189.9A CN115433461B (en) | 2022-09-15 | 2022-09-15 | Heat-conducting silicone grease with low oil separation rate and long storage life and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115433461A CN115433461A (en) | 2022-12-06 |
| CN115433461B true CN115433461B (en) | 2023-11-24 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924924A (en) * | 2012-11-13 | 2013-02-13 | 东莞兆舜有机硅新材料科技有限公司 | Paste heat-conductive silicone grease and preparation method thereof |
| CN104231634A (en) * | 2014-10-17 | 2014-12-24 | 深圳市宝力科技有限公司 | Efficiently-insulated heat-conducting silicone grease and preparation method for same |
| CN108003625A (en) * | 2017-12-21 | 2018-05-08 | 深圳市东成电子有限公司 | Low hypotonic oily heat-conducting silicone grease filler of volatilization and preparation method thereof |
| CN114410113A (en) * | 2021-11-08 | 2022-04-29 | 佛山金戈新材料股份有限公司 | Flowing type fine heat-conducting silicone grease and preparation method thereof |
| WO2022126383A1 (en) * | 2020-12-15 | 2022-06-23 | 万华化学集团股份有限公司 | Asymmetric silicone oil, preparation method therefor, and application thereof |
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| CN103221520A (en) * | 2010-11-18 | 2013-07-24 | 电气化学工业株式会社 | High durability thermally conductive composite and low pump-out grease |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924924A (en) * | 2012-11-13 | 2013-02-13 | 东莞兆舜有机硅新材料科技有限公司 | Paste heat-conductive silicone grease and preparation method thereof |
| CN104231634A (en) * | 2014-10-17 | 2014-12-24 | 深圳市宝力科技有限公司 | Efficiently-insulated heat-conducting silicone grease and preparation method for same |
| CN108003625A (en) * | 2017-12-21 | 2018-05-08 | 深圳市东成电子有限公司 | Low hypotonic oily heat-conducting silicone grease filler of volatilization and preparation method thereof |
| WO2022126383A1 (en) * | 2020-12-15 | 2022-06-23 | 万华化学集团股份有限公司 | Asymmetric silicone oil, preparation method therefor, and application thereof |
| CN114410113A (en) * | 2021-11-08 | 2022-04-29 | 佛山金戈新材料股份有限公司 | Flowing type fine heat-conducting silicone grease and preparation method thereof |
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