CN118931185A - High-heat-conductivity high-elasticity heat-conducting silica gel and preparation method and application thereof - Google Patents
High-heat-conductivity high-elasticity heat-conducting silica gel and preparation method and application thereof Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 239000000741 silica gel Substances 0.000 title claims abstract description 84
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 84
- 238000002360 preparation method Methods 0.000 title abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 37
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 35
- 239000010439 graphite Substances 0.000 claims abstract description 35
- 229920001971 elastomer Polymers 0.000 claims abstract description 31
- 239000000178 monomer Substances 0.000 claims abstract description 31
- 239000005060 rubber Substances 0.000 claims abstract description 31
- 150000004756 silanes Chemical class 0.000 claims abstract description 29
- 125000005395 methacrylic acid group Chemical group 0.000 claims abstract description 27
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 23
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 23
- ROPXFXOUUANXRR-YPKPFQOOSA-N bis(2-ethylhexyl) (z)-but-2-enedioate Chemical compound CCCCC(CC)COC(=O)\C=C/C(=O)OCC(CC)CCCC ROPXFXOUUANXRR-YPKPFQOOSA-N 0.000 claims abstract description 23
- 239000001257 hydrogen Substances 0.000 claims abstract description 23
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 23
- 229910000077 silane Inorganic materials 0.000 claims abstract description 23
- 239000000945 filler Substances 0.000 claims abstract description 15
- 150000001875 compounds Chemical class 0.000 claims abstract description 13
- 239000003999 initiator Substances 0.000 claims abstract description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 6
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 6
- -1 2-carbonyl-tetrahydrofuran-3-hydroxy-methacrylate Chemical compound 0.000 claims description 38
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 23
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 23
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 12
- FZSHSWCZYDDOCK-UHFFFAOYSA-N 2-methylprop-2-enoic acid;oxolane Chemical compound C1CCOC1.CC(=C)C(O)=O FZSHSWCZYDDOCK-UHFFFAOYSA-N 0.000 claims description 10
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 claims description 10
- JCMFXEIQKSSNTG-UHFFFAOYSA-N 3-[[3-(2-methylprop-2-enoyloxy)propyl-bis(trimethylsilyloxy)silyl]oxy-bis(trimethylsilyloxy)silyl]propyl 2-methylprop-2-enoate Chemical group CC(=C)C(=O)OCCC[Si](O[Si](C)(C)C)(O[Si](C)(C)C)O[Si](O[Si](C)(C)C)(O[Si](C)(C)C)CCCOC(=O)C(C)=C JCMFXEIQKSSNTG-UHFFFAOYSA-N 0.000 claims description 9
- QYJHBNLRANFWHO-UHFFFAOYSA-N [ethenyl-[(ethenyl-methyl-phenylsilyl)amino]-methylsilyl]benzene Chemical compound C=1C=CC=CC=1[Si](C)(C=C)N[Si](C)(C=C)C1=CC=CC=C1 QYJHBNLRANFWHO-UHFFFAOYSA-N 0.000 claims description 9
- 125000002768 hydroxyalkyl group Chemical group 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- NYMPGSQKHIOWIO-UHFFFAOYSA-N hydroxy(diphenyl)silicon Chemical compound C=1C=CC=CC=1[Si](O)C1=CC=CC=C1 NYMPGSQKHIOWIO-UHFFFAOYSA-N 0.000 claims description 4
- 125000004122 cyclic group Chemical group 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 238000004132 cross linking Methods 0.000 abstract description 9
- 238000006116 polymerization reaction Methods 0.000 abstract description 7
- 230000000052 comparative effect Effects 0.000 description 40
- 238000012360 testing method Methods 0.000 description 11
- 230000000694 effects Effects 0.000 description 9
- 229920002379 silicone rubber Polymers 0.000 description 8
- 229910052782 aluminium Inorganic materials 0.000 description 7
- 238000004073 vulcanization Methods 0.000 description 7
- 230000002195 synergetic effect Effects 0.000 description 6
- 238000013329 compounding Methods 0.000 description 5
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 229910052582 BN Inorganic materials 0.000 description 3
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 3
- 230000003139 buffering effect Effects 0.000 description 3
- 230000017525 heat dissipation Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000003607 modifier Substances 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 229920001296 polysiloxane Polymers 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000004945 silicone rubber Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- 239000002390 adhesive tape Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000010074 rubber mixing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
Abstract
The application relates to a high-heat-conductivity high-elasticity heat-conductivity silica gel, and a preparation method and application thereof. The material is prepared from the following raw materials in percentage by weight: 20-50% of raw rubber, 1-3% of platinum vulcanizing agent, 3-17% of filler and 40-76% of modified heat conducting filler; the modified heat conducting filler is prepared from expanded graphite, aluminum powder, hydrogen-containing silane, methacrylic monomers, unsaturated silane, bis (2-ethylhexyl) maleate and an initiator. After self-polymerization is carried out on the methacrylic monomer, the self-polymerization is further carried out on the methacrylic monomer and unsaturated silane, hydrogen-containing silane and bis (2-ethylhexyl) maleate, and the prepared compound can further improve the compatibility of aluminum powder and expanded graphite in raw rubber and can further carry out a crosslinking reaction on the aluminum powder and the expanded graphite and the raw rubber, so that the obtained heat-conducting silica gel has better heat-conducting property and elasticity.
Description
Technical Field
The application relates to the field of heat-conducting silica gel, in particular to a high-heat-conducting and high-elasticity heat-conducting silica gel, and a preparation method and application thereof.
Background
The heat-conducting silica gel is widely applied to the fields of electronics, electrical appliances, automobiles and the like, such as the bottom of a radiator or a frame, a high-speed hard disk drive, an automobile engine control device, semiconductor automatic test equipment and the like, improves the heat dissipation performance, prolongs the service life, or plays a role in buffering, and reduces the collision and damage among parts.
In general, metal oxide, graphene and hexagonal boron nitride are added into the heat-conducting silica gel to improve the heat conduction performance of the heat-conducting silica gel, but with the increase of the heat-conducting filler, the elasticity of the heat-conducting silica gel is obviously reduced, so that the buffer effect of the heat-conducting silica gel is reduced, and further research is needed for the heat-conducting silica gel.
Disclosure of Invention
In order to solve the technical problems, the application provides a high-heat-conductivity high-elasticity heat-conductivity silica gel, and a preparation method and application thereof.
In a first aspect, the application provides a high-heat-conductivity high-elasticity heat-conductivity silica gel, which is prepared from the following raw materials in percentage by weight:
Raw rubber 20-50%
Platinum vulcanizing agent 1-3%
3-17% Of filling material
40-76% Of modified heat conducting filler;
The modified heat conducting filler is prepared from expanded graphite, aluminum powder, hydrogen-containing silane, methacrylic monomers, unsaturated silane, bis (2-ethylhexyl) maleate and an initiator.
In the technical scheme, the expanded graphite is of a porous worm-shaped structure, has softness and compression rebound resilience which are not available in natural graphite, and has good heat conduction performance; the aluminum powder has higher heat conduction performance, and when the aluminum powder is compounded with the expanded graphite, the heat conduction silica gel has better heat conduction performance and elasticity. The methacrylic monomer can form a macromolecular polymer through self-polymerization, and after unsaturated silane, hydrogen-containing silane and bis (2-ethylhexyl) maleate are blended with the macromolecular polymer, the formed compound can modify the surfaces of expanded graphite and aluminum powder so as to improve the compatibility of the expanded graphite, the aluminum powder and raw rubber, and meanwhile, the compound can further carry out crosslinking reaction with the raw rubber to form a crosslinked reticular structure, so that the prepared heat-conducting silica gel has better elasticity and heat-conducting property. When the heat radiator is used, the heat radiator has better buffering function and reduces damage to the heat radiator.
The unsaturated silane, the hydrogen-containing silane and the bis (2-ethylhexyl) maleate can be used as a cross-linking agent to promote the cross-linking of the heat-conducting silicone grease to form a network structure and interact with the methacrylic monomer, so that the compatibility of the expanded graphite and the aluminum powder in the heat-conducting silica gel is improved. Bis (2-ethylhexyl) maleate also serves to increase flexibility and wear resistance, so that the thermally conductive silicone has better adhesion, flexibility, elasticity and thermal conductivity.
In conclusion, after the self-polymerization of the methacrylic monomer, the self-polymerization is further compounded with unsaturated silane, hydrogen-containing silane and bis (2-ethylhexyl) maleate, and the prepared compound can further improve the compatibility of aluminum powder and expanded graphite in raw rubber and can further carry out a crosslinking reaction with the raw rubber, so that the heat-conducting silica gel has better heat-conducting property, elasticity and adhesiveness. The silicon rubber has better elasticity in the use process, reduces the effect of collision between parts, has better heat dissipation effect, is easy to adhere to the surfaces of metal and plastic, reduces the possibility of falling off, and provides installation stability.
Preferably, the weight ratio of the expanded graphite, the aluminum powder, the hydrosilane, the methacrylic monomer, the unsaturated silane, the bis (2-ethylhexyl) maleate and the initiator is (2.0-3.5): (0.3-0.5): (1-3): (0.25-0.13): (0.15-0.28): (0.0898-0.3995): (0.0002-0.0005).
When the expanded graphite, the aluminum powder, the hydrosilane, the methacrylic monomer, the unsaturated silane, the bis (2-ethylhexyl) maleate and the initiator are compounded according to the dosage ratio, the better synergistic effect is achieved, and the heat-conducting silica gel has better elasticity, heat-conducting property and adhesiveness.
Preferably, the expanded graphite has a particle size of 200-325 mesh.
The expanded graphite is obtained by expanding nano-scale expandable graphite by 125-200 times, and is obtained by sieving through a 200-325 mesh sieve, and has better heat conducting property and softness under the particle size, so that when the compound is prepared by compounding hydrogen-containing silane, methacrylic monomer, unsaturated silane and bis (2-ethylhexyl) maleate, the surface modification is carried out on the expanded graphite and aluminum powder, the dispersibility and the compatibility of the compound are improved, and the surface modifier is further subjected to crosslinking reaction with raw rubber, so that the prepared heat conducting silica gel has better elasticity, heat conducting property and adhesion effect.
Preferably, the methacrylic monomer is one or more of trimethylolpropane triacrylate, tetrahydrofuran methacrylate and 2-carbonyl-tetrahydrofuran-3-hydroxy-methacrylate.
Trimethylolpropane triacrylate, tetrahydrofuran methacrylate and 2-carbonyl-tetrahydrofuran-3-hydroxy-methacrylate can be self-polymerized and can react with silicon hydroxyl in the silicon rubber, so that the flexibility, elasticity and adhesiveness of the silicon rubber are improved, and unsaturated silane, hydrosilane and bis (2-ethylhexyl) maleate are matched, so that the obtained modified heat conducting filler is easy to disperse in the silicon rubber, and further cross-linking reaction is carried out with the silicon rubber, so that the prepared heat conducting silica gel has better wear resistance, flexibility, adhesiveness, elasticity and heat conducting property.
When trimethylolpropane triacrylate, tetrahydrofuran methacrylate and 2-carbonyl-tetrahydrofuran-3-hydroxy-methacrylate are adopted for compounding, a better synergistic effect is achieved, and further the heat conduction silica gel has better heat conduction performance, adhesiveness and elasticity.
Preferably, the unsaturated silane is 1, 3-bis (3-methacryloxypropyl) tetrakis (trimethylsiloxy) disiloxane and/or 1, 3-divinyl-1, 3-diphenyl-1, 3-dimethyl disilazane.
1, 3-Bis (3-methacryloxypropyl) tetra (trimethylsiloxy) disiloxane or 1, 3-divinyl-1, 3-diphenyl-1, 3-dimethyl disilazane can be used as a cross-linking agent, so that the performance of the heat conducting silica gel is improved, and meanwhile, the heat conducting silica gel has a better dispersing effect on inorganic matters, and further, hydrogen-containing silane, methacrylic monomers and bis (2-ethylhexyl) maleate are matched, so that the prepared modified heat conducting filler can have better compatibility, and can be subjected to further cross-linking reaction with silicone rubber, so that expanded graphite, aluminum powder and a silicone rubber raw material system are tightly combined, and further, the heat conducting silica gel has better heat conducting performance, elasticity, flexibility, adhesiveness and the like.
When the 1, 3-bis (3-methacryloxypropyl) tetra (trimethylsiloxy) disiloxane or 1, 3-divinyl-1, 3-diphenyl-1, 3-dimethyl disilazane plays a better synergistic effect, the heat-conducting silica gel has better heat-conducting property, elasticity and adhesiveness.
Preferably, the hydrogen-containing silane is hydroxyalkyl double-end-capped polydimethylsiloxane and/or double-end-methacryloxypropyl polydimethylsiloxane.
The hydroxyalkyl double-end-capped polydimethylsiloxane and/or double-end-methacryloxypropyl polydimethylsiloxane can be further crosslinked with raw rubber, and can also be compounded with the hydroxyalkyl double-end-capped polydimethylsiloxane and double-end-methacryloxypropyl polydimethylsiloxane when the hydroxyalkyl double-end-capped polydimethylsiloxane and the double-end-methacryloxypropyl polydimethylsiloxane are adopted, so that a synergistic effect is achieved, and the performance of the heat-conducting silica gel is further provided.
Preferably, the raw rubber is one or more of alpha, omega dihydroxy polydimethyl diphenyl siloxane, vinyl end-capped dimethyl methyl vinyl and cyclic dimethyl polysiloxane.
The alpha, omega dihydroxy polydimethyl diphenyl siloxane, vinyl end-capped dimethyl methyl vinyl and cyclic dimethyl polysiloxane have better flexibility, elasticity and adhesiveness, and further cross-link reaction with hydrogen-containing silane, methacrylic monomers, unsaturated silane and bis (2-ethylhexyl) maleate, and the heat conduction silica gel prepared by the method is matched with expanded graphene and aluminum powder, so that the heat conduction silica gel has better heat conduction performance and elasticity.
In a second aspect, a method for preparing a high-thermal-conductivity high-elasticity thermal-conductivity silica gel is prepared by the following steps:
Weighing and mixing methacrylic monomers and an initiator according to parts by weight, heating and reacting for 2-3 hours, adding hydrogen-containing silane, unsaturated silane and bis (2-ethylhexyl) maleate, uniformly mixing, and adding expanded graphite, and uniformly mixing to obtain the modified heat-conducting filler;
Weighing raw rubber, filling materials and modified heat conducting filler according to parts by weight, uniformly mixing, heating for polycondensation to obtain rubber compound, and then adding a platinum vulcanizing agent and the rubber compound for uniform mixing to obtain the heat conducting silica gel.
The process is simple to operate, and the prepared heat-conducting silica gel has better elasticity and heat-conducting property. The rebound rate of the heat-conducting silica gel obtained by the application is 30-36%, and the heat conductivity coefficient is 4.3-7.1. When applied to an adhesive aluminum plate, the peel force was 33-40.8g/inch after vulcanization.
In the third aspect, the application of the high-heat-conductivity high-elasticity heat-conductivity silica gel is that the high-heat-conductivity high-elasticity heat-conductivity silica gel is rolled into the heat-conductivity silica gel piece, adhered to the surface of the carrier, vulcanized, and the heat-conductivity silica gel piece is stably adhered to the surface of the carrier.
According to the technical scheme, the heat-conducting silica gel is rolled into the heat-conducting silica gel piece, so that the heat-conducting silica gel piece is conveniently attached to the surface of the carrier, and after vulcanization, the heat-conducting silica gel piece is crosslinked and stably attached to the surface of the carrier.
At present, after the heat-conducting silica gel is required to be formed into a sheet through vulcanization in the application process, the sheet is attached to a heat dissipating device through double faced adhesive tape, adhesive and the like, the process is required to be used for auxiliary bonding, is complex, is difficult to control in the operation process, and is easy to cause the phenomenon of misalignment. The application convenience of the heat conduction silica gel is reduced.
The high-heat-conductivity high-elasticity heat-conducting silica gel is not vulcanized in the production process, but is vulcanized after being adhered to a carrier in the application process, and is also stably adhered to the carrier after being solidified. The auxiliary adhesion process of other materials is saved, the process is simplified, and the convenience of the application process is improved.
For example, the heat-conducting silica gel can be used for auxiliary parts of electronic products, such as a support frame, a bracket, a radiator and the like of a computer, a tablet, a mobile phone, and the like, and is used for the contact positions of the computer, the mobile phone and the tablet, so as to play a role in buffering and assisting in radiating.
In summary, the application has the following beneficial effects:
After self-polymerization is carried out on the methacrylic monomer, the self-polymerization is further carried out on the methacrylic monomer and unsaturated silane, hydrogen-containing silane and bis (2-ethylhexyl) maleate, and the prepared compound can further improve the compatibility of aluminum powder and expanded graphite in raw rubber and can further carry out a crosslinking reaction on the aluminum powder and the expanded graphite and the raw rubber, so that the obtained heat-conducting silica gel has better heat-conducting property, elasticity and adhesiveness. The silicon rubber has better elasticity in the use process, reduces the effect of collision between parts, has better heat dissipation effect, is easy to adhere to the surfaces of metal and plastic, reduces the possibility of falling off, and provides installation stability.
Detailed Description
The present application will be described in further detail with reference to examples.
Introduction of a part of raw materials;
table 1 part of raw material introduction table
Examples
Example 1
The preparation method of the high-heat-conductivity high-elasticity heat-conductivity silica gel comprises the following steps:
Weighing 0.25kg of methacrylic monomer and 0.0005kg of initiator according to parts by weight, putting into a stirring device, mixing for 10min at the rotating speed of 50r/min, heating to 65 ℃ for reaction for 2h, adding 0.3kg of hydrogen-containing silane, 0.15kg of unsaturated silane and 0.3995kg of bis (2-ethylhexyl) maleate, continuously stirring for 10min to fully mix uniformly, obtaining a surface modifier, adding 3.5kg of expanded graphite and 3.0kg of graphite into the surface modifier, stirring for 30min at the rotating speed of 30r/min, and fully mixing uniformly to obtain a modified heat conducting filler;
Weighing 2.0kg of raw rubber, 0.3kg of filling material and 7.6kg of modified heat-conducting filling material according to parts by weight, putting into a kneader, heating to 150 ℃ at 5 ℃/min, reacting for 1h, discharging, and cooling to 40 ℃ to obtain mixed rubber; and (3) mixing all the mixed rubber by a double-roller rubber mixing machine, and adding 0.1kg of platinum vulcanizing agent and all the mixed rubber to uniformly mix to obtain the heat-conducting silica gel.
The particle size of the expanded graphite is 325 meshes, and the methacrylic monomer is tetrahydrofuran methacrylate; the unsaturated silane is 1, 3-bis (3-methacryloxypropyl) tetra (trimethylsiloxy) disiloxane; the raw rubber is alpha, omega dihydroxy polydimethyl diphenyl siloxane; the hydrosilane is a hydroxyalkyl double-end-capped polydimethylsiloxane.
Examples 2 to 5
Examples 2-5 differ from example 1 in that: the amounts of the raw materials are specifically shown in Table 2;
TABLE 2 raw material amounts (kg) for examples 1 to 5
Example 4
Example 4 differs from example 2 in that: the particle size of the expanded graphite is 300 meshes.
Example 5
Example 5 differs from example 2 in that: the particle size of the expanded graphite is 200 meshes.
Example 6
Example 6 differs from example 2 in that: the methacrylate monomer consists of trimethylolpropane triacrylate and tetrahydrofuran methacrylate in the weight ratio of 1:0.8.
Example 7
Example 7 differs from example 2 in that: the methacrylate monomer consists of trimethylolpropane triacrylate and 2-carbonyl-tetrahydrofuran-3-hydroxy-methacrylate in a weight ratio of 1:0.8.
Example 8
Example 8 differs from example 2 in that: the methacrylate monomer consists of trimethylolpropane triacrylate, tetrahydrofuran methacrylate and 2-carbonyl-tetrahydrofuran-3-hydroxy-methacrylate in the weight ratio of 1:0.4: 0.4.
Example 9
Example 9 differs from example 2 in that: the methacrylate monomer consists of trimethylolpropane triacrylate, tetrahydrofuran methacrylate and 2-carbonyl-tetrahydrofuran-3-hydroxy-methacrylate in the weight ratio of 5:5:8.
Example 10
Example 10 differs from example 8 in that: the unsaturated silane is 1, 3-divinyl-1, 3-diphenyl-1, 3-dimethyl disilazane.
Example 11
Example 11 differs from example 8 in that: the unsaturated silane consists of 1, 3-bis (3-methacryloxypropyl) tetra (trimethylsiloxy) disiloxane and 1, 3-divinyl-1, 3-diphenyl-1, 3-dimethyl disilazane in a weight ratio of 1:1.
Example 12
Example 12 differs from example 8 in that: the unsaturated silane is prepared from 1, 3-bis (3-methacryloxypropyl) tetra (trimethylsiloxy) disiloxane and 1, 3-divinyl-1, 3-diphenyl-1, 3-dimethyl disilazane in a weight ratio of 1: 1.2.
Example 13
Example 13 differs from example 8 in that: the unsaturated silane consists of 1, 3-bis (3-methacryloxypropyl) tetra (trimethylsiloxy) disiloxane and 1, 3-divinyl-1, 3-diphenyl-1, 3-dimethyl disilazane in a weight ratio of 0.5:1.7.
Example 14
Example 14 differs from example 12 in that: the hydrogen-containing silane is double-end methacryloxypropyl polydimethylsiloxane.
Example 15
Example 15 differs from example 12 in that: the hydrogen-containing silane consists of hydroxyalkyl double-end-capped polydimethylsiloxane and double-end methacryloxypropyl polydimethylsiloxane in a weight ratio of 1:1.
Example 16
Example 16 differs from example 12 in that: the hydrogen-containing silane consists of hydroxyalkyl double-end-capped polydimethylsiloxane and double-end methacryloxypropyl polydimethylsiloxane in a weight ratio of 1:2.8.
Example 17
Example 17 differs from example 12 in that: the hydrogen-containing silane comprises hydroxyalkyl double-end-capped polydimethylsiloxane and double-end methacryloxypropyl polydimethylsiloxane in a weight ratio of 0.8: 3.
Comparative example
Comparative example 1
Comparative example 1 differs from example 1 in that: the methacrylic monomer is replaced by unsaturated silane in equal amount.
Comparative example 2
Comparative example 2 is different from example 1 in that: the unsaturated silane is replaced by methacrylic monomer in equal amount.
Comparative example 3
Comparative example 3 is different from example 1 in that: bis (2-ethylhexyl) maleate is replaced equally with a hydrogen-containing silane.
Comparative example 4
Comparative example 4 differs from example 1 in that: the aluminum powder was replaced with hexagonal boron nitride having a particle size of 325 mesh in equal amounts.
Comparative example 5
Comparative example 5 is different from example 1 in that: the methacrylic monomer, unsaturated silane, bis (2-ethylhexyl) maleate and initiator are replaced by hydrogen-containing silane in equal amounts.
Comparative example 6
Comparative example 6 differs from example 1 in that: the expanded graphite is replaced with aluminum powder in equal amount.
Comparative example 7
Comparative example 7 differs from example 1 in that: the aluminum powder is replaced by the expanded graphite in equal quantity.
Application example
Application example 1
The application of the high-heat-conductivity high-elasticity heat-conductivity silica gel is characterized in that the high-heat-conductivity high-elasticity heat-conductivity silica gel obtained in the embodiment 1 is rolled by a calender, a heat-conductivity silica gel piece with the thickness of 1.5mm, the width of 2cm and the length of 10cm is formed by die cutting by a die cutting machine, the heat-conductivity silica gel piece is adhered to the surface of an aluminum plate, and then the heat-conductivity silica gel piece on the aluminum plate is vulcanized for 5min at the temperature of 150 ℃ to enable the heat-conductivity silica gel piece to be stably adhered to the surface of the aluminum plate, so that an experimental sample is obtained.
Application examples 2 to 24
Application examples 2 to 24 differ from example 1 in that: the sources of the high-heat-conductivity and high-elasticity heat-conductivity silica gel are different, and are shown in table 3:
TABLE 3 sources of highly thermally conductive and highly elastic thermally conductive silica gels
Comparative examples of application
Comparative example 1 was used
The application comparative example 1 is different from the application example 1 in that: different application procedures
The heat-conducting silica gel obtained in example 1 is subjected to compression and extension to form a sheet, then is vulcanized for 5min at 150 ℃ and is subjected to demoulding to obtain a heat-conducting silica gel piece with the thickness of 1.5mm, the width of 2cm and the length of 10cm, and the heat-conducting silica gel piece is adhered to the surface of an aluminum plate through double-sided adhesive, so that the heat-conducting silica gel piece is stably adhered to the surface of the aluminum plate, and an experimental sample is obtained.
Performance test
The thermally conductive silica gels obtained in examples 1 to 17 and comparative examples 1 to 5 were subjected to the following test.
Test method/test method test one: placing the heat-conducting silica gel obtained in examples 1-17 and comparative examples 1-5 into a mold, vulcanizing for 5min at 150 ℃, and removing the film to obtain test samples of various types;
the test samples were then subjected to the following performance tests:
rebound rate: the test was performed with reference to GB/T1681-2009, the thickness of the test specimen being 5mm.
Thermal conductivity coefficient: the test sample was 3mm thick, as measured by reference to ASTM D5470.
The above experimental data are shown in table 4;
TABLE 4 Experimental data for examples 1-17 and comparative examples 1-5
| Experimental item | Rebound Rate (%) | Coefficient of thermal conductivity |
| Example 1 | 30.1 | 5.8 |
| Example 2 | 31.2 | 5.1 |
| Example 3 | 32.3 | 4.3 |
| Example 4 | 31.9 | 5.5 |
| Example 5 | 31.5 | 5.4 |
| Example 6 | 32.8 | 5.7 |
| Example 7 | 32.3 | 5.8 |
| Example 8 | 33.1 | 6.1 |
| Example 9 | 32.9 | 6.1 |
| Example 10 | 32.8 | 5.7 |
| Example 11 | 34.5 | 6.5 |
| Example 12 | 34.8 | 6.8 |
| Example 13 | 34.3 | 6.9 |
| Example 14 | 35.2 | 6.7 |
| Example 15 | 36.7 | 7.0 |
| Example 16 | 36.9 | 7.1 |
| Example 17 | 36.4 | 7.0 |
| Comparative example 1 | 25.8 | 4.5 |
| Comparative example 2 | 23.6 | 4.3 |
| Comparative example 3 | 26.8 | 4.8 |
| Comparative example 4 | 16.8 | 3.9 |
| Comparative example 5 | 21.6 | 4.1 |
| Comparative example 6 | 20.7 | 7.5 |
| Comparative example 7 | 29.6 | 2.3 |
By combining the examples 1 and the comparative examples 1 to 7 and combining the table 4, it can be seen that the rebound rates of the comparative examples 1 to 7 are all lower than 30%, the rebound rate of the example 1 is above 30%, and the thermal conductivity coefficients of the comparative examples 1 to 5 and the comparative example 7 are all below 5, which indicates that the compound obtained by compounding the methacrylic monomer, the unsaturated silane, the bis (2-ethylhexyl) maleate and the initiator has better compatibility to the expanded graphite and the aluminum powder, promotes the mixture with a raw rubber system, and further cross-links with the raw rubber, so that the heat-conducting silica gel has better elasticity and heat-conducting property after vulcanization. The aluminum powder is only added in the comparative example 6, but the elasticity is obviously reduced although the better heat conduction effect is achieved, and the hexagonal boron nitride is adopted to replace the aluminum powder in the comparative example 5, so that the heat conduction performance and the elasticity are both reduced, and the effect of better synergism is achieved by adopting the combination of the expanded graphite and the aluminum powder, so that the elasticity and the heat conduction performance of the vulcanized heat conduction silica gel are better.
As can be seen from the comparison of example 2 and example 8 and the combination of table 4, the rebound rate of example 8 is 3% higher than that of example 2, and the thermal conductivity is also higher than that of example 2, which indicates that the use of trimethylolpropane triacrylate, tetrahydrofuran methacrylate, and 2-carbonyl-tetrahydrofuran-3-hydroxy-methacrylate for compounding has synergistic effect, so that the thermal conductive silica gel has better elasticity and thermal conductivity after vulcanization.
Comparing example 8 with example 12 and combining Table 4, it can be seen that the rebound rate and thermal conductivity of example 8 are lower than that of example 12, indicating that the thermal conductive silica gel has better elasticity and thermal conductivity by compounding 1, 3-bis (3-methacryloxypropyl) tetra (trimethylsiloxy) disiloxane and 1, 3-divinyl-1, 3-diphenyl-1, 3-dimethyl disilazane.
Comparing example 12 with example 16 and combining table 4, it can be seen that the rebound rate and thermal conductivity of example 12 are lower than that of example 16, which indicates that the use of the hydroxyalkyl-terminated polydimethylsiloxane and the double-end methacryloxypropyl polydimethylsiloxane in combination has synergistic effect, so that the thermal conductive silica gel has better elasticity and thermal conductivity.
Test II
(1) The experimental samples obtained in application examples 1 to 24 and comparative example 1 were left for 7 days in an environment having a humidity of 80% and a temperature of 120℃and then observed for the occurrence of a falling phenomenon, and the experimental results were recorded.
(2) The test samples obtained in application examples 1 to 24 and application comparative example 1 were examined with reference to JIS Z0237 (300 mm/min,180 ℃) to obtain the peel force of the heat conductive silicone members of the test samples obtained in application examples 1 to 24 and application comparative example 1.
The above specific data are shown in table 5;
Table 5 application examples 1-24 and application comparative example 1
As can be seen by combining example 1, application comparative example 1 and application examples 18-24 with Table 5, the peeling phenomenon does not occur in both example 1 and application comparative example 1, the peeling force is above 30g/inch, and the peeling force is below 30g/inch, which shows that the compound prepared by adopting the application and adopting the methacrylic monomer, unsaturated silane, bis (2-ethylhexyl) maleate and initiator has better compatibility to the expanded graphite and aluminum powder, promotes the mixture of the expanded graphite and aluminum powder with a raw rubber system, and further carries out crosslinking reaction with the raw rubber, so that the heat-conducting silica gel has better elasticity, heat-conducting property and adhesiveness after vulcanization.
In addition, the application method of the heat-conducting silica gel can be described, the adhesive material can be introduced, the operation is simple, the heat-conducting silica gel can be stably adhered to an aluminum plate after vulcanization, the possibility of falling off is reduced, and if the application method of the heat-conducting silica gel is used for carriers such as plastics, rubber, metal and the like with the melting temperature of more than 150 ℃.
The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.
Claims (10)
1. The high-heat-conductivity high-elasticity heat-conductivity silica gel is characterized by being prepared from the following raw materials in percentage by weight:
raw rubber 20-50%
Platinum vulcanizing agent 1-3%
3-17% Of filling material
40-76% Of modified heat conducting filler;
The modified heat conducting filler is prepared from expanded graphite, aluminum powder, hydrogen-containing silane, methacrylic monomers, unsaturated silane, bis (2-ethylhexyl) maleate and an initiator.
2. The high thermal conductivity and high elasticity thermal conductive silica gel according to claim 1, wherein: the weight ratio of the expanded graphite, aluminum powder, hydrogen-containing silane, methacrylic monomer, unsaturated silane, bis (2-ethylhexyl) maleate and initiator is (2.0-3.5): (0.3-0.5): (1-3): (0.25-0.13): (0.15-0.28): (0.0898-0.3995): (0.0002-0.0005).
3. The high thermal conductivity and high elasticity thermal conductive silica gel according to claim 1, wherein: the particle size of the expanded graphite is 200-325 meshes.
4. The high thermal conductivity and high elasticity thermal conductive silica gel according to claim 1, wherein: the methacrylic monomer is one or more of trimethylolpropane triacrylate, tetrahydrofuran methacrylate and 2-carbonyl-tetrahydrofuran-3-hydroxy-methacrylate.
5. The high thermal conductivity and high elasticity thermal conductive silica gel according to claim 4, wherein: the weight ratio of the trimethylolpropane triacrylate to the tetrahydrofuran methacrylate to the 2-carbonyl-tetrahydrofuran-3-hydroxy-methacrylate is 1: (0.4-1): (0.4-1.6).
6. The high thermal conductivity and high elasticity thermal conductive silica gel according to claim 1, wherein: the unsaturated silane is 1, 3-bis (3-methacryloxypropyl) tetra (trimethylsiloxy) disiloxane and/or 1, 3-divinyl-1, 3-diphenyl-1, 3-dimethyl disilazane.
7. The high thermal conductivity and high elasticity thermal conductive silica gel according to claim 1, wherein: the hydrogen-containing silane is hydroxyalkyl double-end-capped polydimethylsiloxane and/or double-end methacryloxypropyl polydimethylsiloxane.
8. The high thermal conductivity and high elasticity thermal conductive silica gel according to claim 1, wherein: the raw rubber is one or more of alpha, omega dihydroxy polydimethyl diphenyl siloxane, vinyl-terminated dimethyl methyl vinyl and cyclic dimethyl polysiloxane.
9. A method for preparing the high-heat-conductivity and high-elasticity heat-conductivity silica gel according to any one of claims 1 to 8, wherein the silica gel is prepared by the following method:
Weighing and mixing methacrylic monomers and an initiator according to parts by weight, heating and reacting for 2-3 hours, adding hydrogen-containing silane, unsaturated silane and bis (2-ethylhexyl) maleate, uniformly mixing, and adding expanded graphite and aluminum powder, and uniformly mixing to obtain a modified heat-conducting filler;
And (3) weighing raw rubber, filling materials and modified heat conducting filler according to parts by weight, uniformly mixing, reacting to obtain a rubber compound, and then adding a platinum vulcanizing agent and the rubber compound to uniformly mix to obtain the heat conducting silica gel.
10. The application of the high-heat-conductivity high-elasticity heat-conductivity silica gel, which is characterized in that the high-heat-conductivity high-elasticity heat-conductivity silica gel is rolled into a heat-conductivity silica gel piece, is adhered to the surface of a carrier, and is vulcanized, so that the heat-conductivity silica gel piece is stably adhered to the surface of the carrier.
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| Publication Number | Publication Date |
|---|---|
| CN118931185A true CN118931185A (en) | 2024-11-12 |
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