CN109777345A - One kind can the thermally conductive Silica hydrogel of self-healing dual composition addition type and preparation method thereof - Google Patents
One kind can the thermally conductive Silica hydrogel of self-healing dual composition addition type and preparation method thereof Download PDFInfo
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- CN109777345A CN109777345A CN201811646827.4A CN201811646827A CN109777345A CN 109777345 A CN109777345 A CN 109777345A CN 201811646827 A CN201811646827 A CN 201811646827A CN 109777345 A CN109777345 A CN 109777345A
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- 238000002360 preparation method Methods 0.000 title abstract description 11
- 239000000203 mixture Substances 0.000 title abstract 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title abstract 4
- 230000009977 dual effect Effects 0.000 title abstract 3
- 239000000017 hydrogel Substances 0.000 title abstract 2
- 239000000377 silicon dioxide Substances 0.000 title abstract 2
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 69
- 239000002994 raw material Substances 0.000 claims abstract description 46
- -1 polysiloxane Polymers 0.000 claims abstract description 44
- 239000003054 catalyst Substances 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 15
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 14
- 239000003112 inhibitor Substances 0.000 claims abstract description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000001257 hydrogen Substances 0.000 claims abstract description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 7
- 239000000945 filler Substances 0.000 claims description 31
- 229910020447 SiO2/2 Inorganic materials 0.000 claims description 24
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 24
- 239000002245 particle Substances 0.000 claims description 23
- 229910020388 SiO1/2 Inorganic materials 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 13
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 12
- 229910052593 corundum Inorganic materials 0.000 claims description 12
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 9
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 6
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 claims description 5
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 claims description 4
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 4
- CEBKHWWANWSNTI-UHFFFAOYSA-N 2-methylbut-3-yn-2-ol Chemical compound CC(C)(O)C#C CEBKHWWANWSNTI-UHFFFAOYSA-N 0.000 claims description 3
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 abstract description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052710 silicon Inorganic materials 0.000 abstract description 2
- 239000010703 silicon Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 2
- 239000000499 gel Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 6
- 238000001879 gelation Methods 0.000 description 5
- 239000002904 solvent Substances 0.000 description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229920002379 silicone rubber Polymers 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 230000001678 irradiating effect Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- ZDWQSEWVPQWLFV-UHFFFAOYSA-N C(CC)[Si](OC)(OC)OC.[O] Chemical compound C(CC)[Si](OC)(OC)OC.[O] ZDWQSEWVPQWLFV-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
One kind can the thermally conductive Silica hydrogel of self-healing dual composition addition type and preparation method thereof, including component A and component B；Wherein, the composition of raw materials of the component A includes 30~50 parts of vinyl terminated polysiloxane for meeting general formula (1)；First heat filling 5-15；0.1~5 part of catalyst；The composition of raw materials of the component B includes more vinyl polysiloxane 15-25 parts for meeting general formula (2)；Meet hydrogen polysiloxanes 5-25 parts of the end side of general formula (3)；Second 5-15 parts of heat filling；5-15 parts of silane coupling agent；0.1-1.0 parts of inhibitor；The mass ratio of the component A and component B is 1:0.8-1.2.One kind produced by the present invention can the thermally conductive process for preparing silicon gel of self-healing dual composition addition type it is simple, can be used double planetary mixer use after mixing, raw material is easy to get, and facilitates industrialized production.
Description
Technical Field
The invention relates to a self-healing double-component addition type heat-conducting silicone gel and a preparation method thereof, belonging to the technical field of adhesive materials.
Background
Along with the development of science and technology, electronic components, electric appliance power circuit modules and large-scale integrated circuits with high reliability increasingly attract attention of people. And the heat effect of each component in the use process easily causes the reliability reduction, thereby reducing the service life of the component. Aiming at the traditional heat-conducting silicon rubber, because the cross-linking density is high, on one hand, the interface thermal resistance is generated because the contact between a heat source interface and a heat dissipation interface is incomplete in the using process; on the other hand, when the device is impacted by external force, the loss is easy to generate due to high internal stress.
The invention patent with publication number CN106496468B discloses a preparation method of a silicon elastomer with self-healing and shape memory properties, which comprises the following steps:
(1) polymethylvinylsiloxane grafting reaction: respectively and uniformly mixing 50 parts by mass of polymethylvinylsiloxane and 9-26 parts by mass of amino-containing terminal mercapto micromolecules in a good solvent, adding 0.5-1.5 parts by mass of photoinitiator, uniformly mixing, and irradiating under an ultraviolet lamp for 10min-3h to obtain a grafted amino product; the polymethylvinylsiloxane is polymethylvinylsiloxane with the vinyl content of 15-50%;
uniformly mixing 50 parts by mass of polymethylvinylsiloxane and 12-36 parts by mass of carboxyl-containing sulfydryl micromolecules in a good solvent, adding 0.5-1.5 parts by mass of photoinitiator, uniformly mixing, and irradiating under an ultraviolet lamp for 10min-3h to obtain a product grafted with carboxyl;
(2) and (3) crosslinking reaction: and (2) mixing and dissolving the grafted amino and grafted carboxyl products obtained in the step (1) in a good solvent according to a ratio of 1:1, adding 2-30 parts by mass of a cross-linking agent and 0.5-1.5 parts by mass of a photoinitiator, stirring at room temperature, uniformly mixing, fully volatilizing the solvent under the condition of no light and room temperature, and then illuminating under an ultraviolet lamp for 1-30min to obtain the silicon-containing elastomer.
Disclosure of Invention
The invention aims to provide a self-healing double-component addition type heat-conducting silicone gel and a preparation method thereof.
In order to achieve the above objects and other related objects, the present invention provides the following technical solutions: a self-healing two-component addition type heat-conducting silicone gel comprises a component A and a component B; wherein,
the raw material formula of the component A comprises the following raw materials in parts by weight:
30-50 parts of vinyl-terminated polysiloxane corresponding to the general formula (1);
5-15 parts of a first heat-conducting filler;
0.1-5 parts of a catalyst;
(CH3)2(CH2＝CH)SiO1/2[(CH3)2SiO2/2]n(1)；
in the general formula (1), n is 100-;
the raw material formula of the component B comprises the following raw materials in parts by weight:
(CH3)2(CH2＝CH)SiO1/2[(CH3)2SiO2/2]z[CH3(CH2＝CH)SiO2/2]m(2)；
in the general formula (2), z is 80-100, and m is 50-80;
R(CH3)2SiO1/2[(CH3)2SiO2/2]x[CH3RSiO2/2]y(3)；
in the general formula (3), R is H, x-30 and y is 10-30;
the mass ratio of the component A to the component B is 1: 0.8-1.2.
The preferable technical scheme is as follows: the viscosity of the vinyl-terminated polysiloxane according to formula (1) ranges from 300 and 1000 centipoise.
The preferable technical scheme is as follows: the first heat-conducting filler is Al2O3The particles have a median particle diameter of 18-30 μm and a specific surface area of 0.3-0.5m2/g。
The preferable technical scheme is as follows: the catalyst is a platinum metal complex, and the mass concentration of platinum metal in the platinum metal complex is 3000-5000 ppm; the dosage of the platinum metal is 2-20ppm of the total mixing amount of the raw material formula.
The preferable technical scheme is as follows: the viscosity of the polyvinyl polysiloxane according to the general formula (2) is in the range of 250-350 centipoises.
The preferable technical scheme is as follows: the viscosity of the terminal hydrogenpolysiloxane according to the general formula (3) ranges from 50 to 250 centipoises.
The preferable technical scheme is as follows: the second heat-conducting filler is Al2O3The particles have a median particle diameter of 32-45 μm and a specific surface area of 0.2-0.4m2/g。
The preferable technical scheme is as follows: the silane coupling agent is at least one of gamma-glycidoxypropyltrimethoxysilane, 2- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, vinyltrimethoxysilane and vinyltriethoxysilane.
The preferable technical scheme is as follows: the inhibitor is at least one of 3-methyl-1-butyn-3-ol, 1-ethynyl cyclohexanol and tetravinylcyclotetrasiloxane.
In order to achieve the above objects and other related objects, the present invention provides the following technical solutions: a method for preparing self-healing double-component addition type heat-conducting silicone gel is characterized by comprising the following steps: adding vinyl-terminated polysiloxane according to a general formula (1) and a catalyst into a double-planet stirrer according to a raw material formula of the component A, then adding a first heat-conducting filler in batches, uniformly stirring, and defoaming in vacuum for later use; adding the polyvinyl polysiloxane according to the general formula (2), the end-side hydrogen polysiloxane according to the general formula (3), the silane coupling agent and the inhibitor into a double-planet stirrer according to the raw material formula of the component A, then adding the second heat-conducting filler in batches, uniformly stirring, and defoaming in vacuum for later use; when in use, the component A and the component B are mixed according to the mass ratio of 1: 0.8-1.2.
Due to the application of the technical scheme, compared with the prior art, the invention has the advantages that:
1. the self-healing two-component addition type heat-conducting silicone gel prepared by the invention has the advantages of no by-product in the vulcanization process of common addition type silicone rubber, good heat resistance, weather resistance, oil resistance, electric insulation property and the like. Meanwhile, due to the addition of the heat-conducting filler, the material is endowed with heat conductivity, and the heat conductivity can reach 1.0W/(m.K); the material has low elasticity modulus and low internal stress due to the flexibility of the material due to low crosslinking density, and can be filled on uneven surfaces to reduce interface thermal resistance; on the other hand, when the material is torn by external force, the material can be self-healed after being contacted for 5min, thereby providing good damping and shock absorption effects for electronic components and prolonging the service life of the electronic components.
2. The self-healing double-component addition type heat-conducting silicone gel prepared by the invention is simple in preparation method, can be uniformly mixed by using a double-planet stirrer and then is used, raw materials are easy to obtain, and the industrial production is facilitated.
Detailed Description
The following description of the embodiments of the present invention is provided for illustrative purposes, and other advantages and effects of the present invention will be apparent to those skilled in the art from the present disclosure.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise.
In describing the preferred embodiments, specific terminology may be employed for the sake of clarity; however, it is not intended that the disclosure herein be limited to the specific terminology so selected; and it is to be understood that each specific element includes all equivalent techniques that perform the same function, operate in a similar manner, and achieve a similar result.
Example 1: self-healing two-component addition type heat-conducting silicone gel and preparation method thereof
A self-healing two-component addition type heat-conducting silicone gel comprises a component A and a component B; wherein,
the raw material formula of the component A comprises the following raw materials in parts by weight:
40 parts of vinyl-terminated polysiloxane corresponding to general formula (1);
10 parts of first heat-conducting filler;
2.5 parts of a catalyst;
(CH3)2(CH2＝CH)SiO1/2[(CH3)2SiO2/2]n(1)；
in the general formula (1), n is 260;
the raw material formula of the component B comprises the following raw materials in parts by weight:
(CH3)2(CH2＝CH)SiO1/2[(CH3)2SiO2/2]z[CH3(CH2＝CH)SiO2/2]m(2)；
in the general formula (2), z is 90, m is 65;
R(CH3)2SiO1/2[(CH3)2SiO2/2]x[CH3RSiO2/2]y(3)；
in the general formula (3), R is H, x-40, and y is 20;
the mass ratio of the component A to the component B is 1: 1.
the preferred embodiment is: the vinyl-terminated polysiloxane according to formula (1) has a viscosity in the range of 600 centipoise.
The preferred embodiment is: the first mentionedOne heat-conducting filler is Al2O3Particles with a median particle size of 26 microns and a specific surface area of 0.4m2/g。
The preferred embodiment is: the catalyst is a platinum metal complex, and the mass concentration of platinum metal in the platinum metal complex is 4000 ppm; the dosage of the platinum metal is 10ppm of the total mixing amount of the raw material formula.
The preferred embodiment is: the polyvinyl polysiloxane according to formula (2) has a viscosity in the range of 300 centipoise.
The preferred embodiment is: the viscosity of the terminal hydrogenpolysiloxane according to formula (3) ranges from 150 centipoise.
The preferred embodiment is: the second heat-conducting filler is Al2O3Particles with a median particle size of 40 microns and a specific surface area of 0.3m2/g。
The preferred embodiment is: the silane coupling agent is gamma-glycidol ether oxygen propyl trimethoxy silane.
The preferred embodiment is: the inhibitor is 3-methyl-1-butyne-3-ol.
The method for preparing the self-healing two-component addition type heat-conducting silicone gel comprises the steps of adding vinyl-terminated polysiloxane and a catalyst which accord with a general formula (1) into a double-planet stirrer according to a raw material formula of a component A, then adding a first heat-conducting filler in batches, uniformly stirring, and defoaming in vacuum for later use; adding the polyvinyl polysiloxane according to the general formula (2), the end-side hydrogen polysiloxane according to the general formula (3), the silane coupling agent and the inhibitor into a double-planet stirrer according to the raw material formula of the component A, then adding the second heat-conducting filler in batches, uniformly stirring, and defoaming in vacuum for later use; when in use, the component A and the component B are mixed according to the mass ratio of 1:1 and mixing.
Example 2: self-healing two-component addition type heat-conducting silicone gel and preparation method thereof
A self-healing two-component addition type heat-conducting silicone gel comprises a component A and a component B; wherein,
the raw material formula of the component A comprises the following raw materials in parts by weight:
30 parts of vinyl-terminated polysiloxane corresponding to general formula (1);
5 parts of a first heat-conducting filler;
0.1 part of catalyst;
(CH3)2(CH2＝CH)SiO1/2[(CH3)2SiO2/2]n(1)；
in the general formula (1), n is 100;
the raw material formula of the component B comprises the following raw materials in parts by weight:
(CH3)2(CH2＝CH)SiO1/2[(CH3)2SiO2/2]z[CH3(CH2＝CH)SiO2/2]m(2)；
in the general formula (2), z is 80, m is 50;
R(CH3)2SiO1/2[(CH3)2SiO2/2]x[CH3RSiO2/2]y(3)；
in the general formula (3), R is H, x-30, and y is 10;
the mass ratio of the component A to the component B is 1: 0.8.
the preferred embodiment is: the vinyl-terminated polysiloxane according to formula (1) has a viscosity in the range of 300 centipoise.
The preferred embodiment is: the first heat-conducting filler is Al2O3The median particle diameter of the granules is 18 microns, and the specific surface area of the granules is 0.3m2/g。
The preferred embodiment is: the catalyst is a platinum metal complex, and the mass concentration of platinum metal in the platinum metal complex is 3000 ppm; the dosage of the platinum metal is 2ppm of the total mixing amount of the raw material formula.
The preferred embodiment is: the polyvinyl polysiloxane according to formula (2) has a viscosity in the range of 250 centipoise.
The preferred embodiment is: the terminal hydrogenpolysiloxane according to the general formula (3) has a viscosity ranging from 50 centipoise.
The preferred embodiment is: the second heat-conducting filler is Al2O3Particles with a median particle size of 32 microns and a specific surface area of 0.2m2/g。
The preferred embodiment is: the silane coupling agent is 2- (3, 4-epoxy cyclohexyl) ethyl trimethoxy silane and gamma-methacryloxypropyl trimethoxy silane, and the weight ratio of the silane coupling agent to the gamma-methacryloxypropyl trimethoxy silane is 1:1 in a mass ratio.
The preferred embodiment is: the inhibitor is 1-ethynylcyclohexanol and tetravinylcyclotetrasiloxane in a ratio of 1:1 in a mass ratio.
The method for preparing the self-healing two-component addition type heat-conducting silicone gel comprises the steps of adding vinyl-terminated polysiloxane and a catalyst which accord with a general formula (1) into a double-planet stirrer according to a raw material formula of a component A, then adding a first heat-conducting filler in batches, uniformly stirring, and defoaming in vacuum for later use; adding the polyvinyl polysiloxane according to the general formula (2), the end-side hydrogen polysiloxane according to the general formula (3), the silane coupling agent and the inhibitor into a double-planet stirrer according to the raw material formula of the component A, then adding the second heat-conducting filler in batches, uniformly stirring, and defoaming in vacuum for later use; when in use, the component A and the component B are mixed according to the mass ratio of 1: 0.8 mixing.
Example 3: self-healing two-component addition type heat-conducting silicone gel and preparation method thereof
A self-healing two-component addition type heat-conducting silicone gel comprises a component A and a component B; wherein,
the raw material formula of the component A comprises the following raw materials in parts by weight:
50 parts of vinyl-terminated polysiloxane corresponding to general formula (1);
15 parts of first heat-conducting filler;
5 parts of a catalyst;
(CH3)2(CH2＝CH)SiO1/2[(CH3)2SiO2/2]n(1)；
in the general formula (1), n is 400;
the raw material formula of the component B comprises the following raw materials in parts by weight:
(CH3)2(CH2＝CH)SiO1/2[(CH3)2SiO2/2]z[CH3(CH2＝CH)SiO2/2]m(2)；
in the general formula (2), z is 100, m is 80;
R(CH3)2SiO1/2[(CH3)2SiO2/2]x[CH3RSiO2/2]y(3)；
in the general formula (3), R is H, x-50, and y is 30;
the mass ratio of the component A to the component B is 1: 1.2.
the preferred embodiment is: the vinyl-terminated polysiloxane according to formula (1) has a viscosity in the range of 1000 centipoise.
The preferred embodiment is: the first heat-conducting filler is Al2O3Particles with a median particle size of 30 microns and a specific surface area of 0.5m2/g。
The preferred embodiment is: the catalyst is a platinum metal complex, and the mass concentration of platinum metal in the platinum metal complex is 5000 ppm; the dosage of the platinum metal is 20ppm of the total mixing amount of the raw material formula.
The preferred embodiment is: the polyvinyl polysiloxane according to formula (2) has a viscosity in the range of 350 cps.
The preferred embodiment is: the viscosity of the terminal hydrogenpolysiloxane according to formula (3) ranges from 250 centipoise.
The preferred embodiment is: the second heat-conducting filler is Al2O3Particles with a median particle size of 45 microns and a specific surface area of 0.4m2/g。
The preferred embodiment is: the silane coupling agent is gamma-glycidoxypropyltrimethoxysilane, 2- (3, 4-epoxy cyclohexyl) ethyltrimethoxysilane or gamma-methacryloxypropyltrimethoxysilane, and the weight ratio of the gamma-glycidoxypropyltrimethoxysilane to the monomer is 1: 1: 2 in mass ratio.
The preferred embodiment is: the inhibitor is 1-ethynylcyclohexanol.
The method for preparing the self-healing two-component addition type heat-conducting silicone gel comprises the steps of adding vinyl-terminated polysiloxane and a catalyst which accord with a general formula (1) into a double-planet stirrer according to a raw material formula of a component A, then adding a first heat-conducting filler in batches, uniformly stirring, and defoaming in vacuum for later use; adding the polyvinyl polysiloxane according to the general formula (2), the end-side hydrogen polysiloxane according to the general formula (3), the silane coupling agent and the inhibitor into a double-planet stirrer according to the raw material formula of the component A, then adding the second heat-conducting filler in batches, uniformly stirring, and defoaming in vacuum for later use; when in use, the component A and the component B are mixed according to the mass ratio of 1: 1.2 mixing.
Example 4: self-healing two-component addition type heat-conducting silicone gel and preparation method thereof
A self-healing two-component addition type heat-conducting silicone gel comprises a component A and a component B; wherein,
the raw material formula of the component A comprises the following raw materials in parts by weight:
47 parts of vinyl-terminated polysiloxane corresponding to general formula (1);
7 parts of a first heat-conducting filler;
2.3 parts of a catalyst;
(CH3)2(CH2＝CH)SiO1/2[(CH3)2SiO2/2]n(1)；
in the general formula (1), n is 100-;
the raw material formula of the component B comprises the following raw materials in parts by weight:
(CH3)2(CH2＝CH)SiO1/2[(CH3)2SiO2/2]z[CH3(CH2＝CH)SiO2/2]m(2)；
in the general formula (2), z is 92, m is 55;
R(CH3)2SiO1/2[(CH3)2SiO2/2]x[CH3RSiO2/2]y(3)；
in the general formula (3), R is H, x-34, and y is 20;
the mass ratio of the component A to the component B is 1: 1.1.
the preferred embodiment is: the vinyl-terminated polysiloxane according to formula (1) has a viscosity in the range of 700 centipoise.
The preferred embodiment is: the first heat-conducting filler is Al2O3Particles with a median particle size of 20 microns and a specific surface area of 0.35m2/g。
The preferred embodiment is: the catalyst is a platinum metal complex, and the mass concentration of platinum metal in the platinum metal complex is 3500 ppm; the dosage of the platinum metal is 5ppm of the total mixing amount of the raw material formula.
The preferred embodiment is: the polyvinyl polysiloxane according to formula (2) has a viscosity in the range of 270 cps.
The preferred embodiment is: the viscosity of the terminal hydrogenpolysiloxane according to formula (3) ranges from 250 centipoise.
The preferred embodiment is: the second heat-conducting filler is Al2O3Particles with a median particle size of 35 microns and a specific surface area of 0.4m2/g。
The preferred embodiment is: the silane coupling agent is gamma-methacryloxypropyltrimethoxysilane.
The preferred embodiment is: the inhibitor is 1-ethynylcyclohexanol.
The method for preparing the self-healing two-component addition type heat-conducting silicone gel comprises the steps of adding vinyl-terminated polysiloxane and a catalyst which accord with a general formula (1) into a double-planet stirrer according to a raw material formula of a component A, then adding a first heat-conducting filler in batches, uniformly stirring, and defoaming in vacuum for later use; adding the polyvinyl polysiloxane according to the general formula (2), the end-side hydrogen polysiloxane according to the general formula (3), the silane coupling agent and the inhibitor into a double-planet stirrer according to the raw material formula of the component A, then adding the second heat-conducting filler in batches, uniformly stirring, and defoaming in vacuum for later use; when in use, the component A and the component B are mixed according to the mass ratio of 1: 1.1 mixing.
The foregoing is illustrative of the preferred embodiment of the present invention and is not to be construed as limiting thereof in any way, and any modifications or variations thereof that fall within the spirit of the invention are intended to be included within the scope thereof.
Claims (10)
1. A self-healing double-component addition type heat-conducting silicone gel is characterized in that: the self-healing two-component addition type heat-conducting silicone gel comprises a component A and a component B; wherein,
the raw material formula of the component A comprises the following raw materials in parts by weight:
30-50 parts of vinyl-terminated polysiloxane corresponding to the general formula (1);
5-15 parts of a first heat-conducting filler;
0.1-5 parts of a catalyst;
(CH3)2(CH2＝CH)SiO1/2[(CH3)2SiO2/2]n(1)；
in the general formula (1), n is 100-;
the raw material formula of the component B comprises the following raw materials in parts by weight:
(CH3)2(CH2＝CH)SiO1/2[(CH3)2SiO2/2]z[CH3(CH2＝CH)SiO2/2]m(2)；
in the general formula (2), z is 80-100, and m is 50-80;
R(CH3)2SiO1/2[(CH3)2SiO2/2]x[CH3RSiO2/2]y(3)；
in the general formula (3), R is H, x-30 and y is 10-30;
the mass ratio of the component A to the component B is 1: 0.8-1.2.
2. A self-healing two-component addition type heat-conductive silicone gel according to claim 1, characterized in that: the viscosity of the vinyl-terminated polysiloxane according to formula (1) ranges from 300 and 1000 centipoise.
3. A self-healing two-component addition type heat-conductive silicone gel according to claim 1, characterized in that: the first heat-conducting filler is Al2O3The particles have a median particle diameter of 18-30 μm and a specific surface area of 0.3-0.5m2/g。
4. A self-healing two-component addition type heat-conductive silicone gel according to claim 1, characterized in that: the catalyst is a platinum metal complex, and the mass concentration of platinum metal in the platinum metal complex is 3000-5000 ppm; the dosage of the platinum metal is 2-20ppm of the total mixing amount of the raw material formula.
5. A self-healing two-component addition type heat-conductive silicone gel according to claim 1, characterized in that: the viscosity of the polyvinyl polysiloxane according to the general formula (2) is in the range of 250-350 centipoises.
6. A self-healing two-component addition type heat-conductive silicone gel according to claim 1, characterized in that: the viscosity of the terminal hydrogenpolysiloxane according to the general formula (3) ranges from 50 to 250 centipoises.
7. A self-healing two-component addition type heat-conductive silicone gel according to claim 1, characterized in that: the second heat-conducting filler is Al2O3The particles have a median particle diameter of 32-45 μm and a specific surface area of 0.2-0.4m2/g。
8. A self-healing two-component addition type heat-conductive silicone gel according to claim 1, characterized in that: the silane coupling agent is at least one of gamma-glycidoxypropyltrimethoxysilane, 2- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, vinyltrimethoxysilane and vinyltriethoxysilane.
9. A self-healing two-component addition type heat-conductive silicone gel according to claim 1, characterized in that: the inhibitor is at least one of 3-methyl-1-butyn-3-ol, 1-ethynyl cyclohexanol and tetravinylcyclotetrasiloxane.
10. A method of preparing the self-healing two-component addition type thermally conductive silicone gel according to any one of claims 1 to 9, characterized in that: adding vinyl-terminated polysiloxane according to a general formula (1) and a catalyst into a double-planet stirrer according to a raw material formula of the component A, then adding a first heat-conducting filler in batches, uniformly stirring, and defoaming in vacuum for later use; adding the polyvinyl polysiloxane according to the general formula (2), the end-side hydrogen polysiloxane according to the general formula (3), the silane coupling agent and the inhibitor into a double-planet stirrer according to the raw material formula of the component A, then adding the second heat-conducting filler in batches, uniformly stirring, and defoaming in vacuum for later use; when in use, the component A and the component B are mixed according to the mass ratio of 1: 0.8-1.2.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112521754A (en) * | 2020-10-30 | 2021-03-19 | 广东工业大学 | MXene nanosheet compounded heat-conducting gel with thermal self-repairing performance and preparation method thereof |
| CN112724927A (en) * | 2020-12-25 | 2021-04-30 | 浙江中特化工有限公司 | UV curing silicone gel for lead sealing |
| WO2021164241A1 (en) * | 2020-02-17 | 2021-08-26 | 苏州桐力光电股份有限公司 | Organosilicon porous breathable disinfection and sterilization nano-filtration material for masks and preparation method therefor |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1176181A2 (en) * | 2000-07-20 | 2002-01-30 | Dow Corning Corporation | Silicone composition and electrically conductive silicone adhesive formed therefrom |
| CN104403626A (en) * | 2014-11-28 | 2015-03-11 | 广州市白云化工实业有限公司 | High-anti-poisoning one-component pouring sealant for LED driving power supply and preparation method of high-anti-poisoning one-component pouring sealant |
| CN106833510A (en) * | 2017-01-11 | 2017-06-13 | 宁波聚力新材料科技有限公司 | New energy high heat conduction low-gravity organic silicon potting adhesive |
-
2018
- 2018-12-30 CN CN201811646827.4A patent/CN109777345B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1176181A2 (en) * | 2000-07-20 | 2002-01-30 | Dow Corning Corporation | Silicone composition and electrically conductive silicone adhesive formed therefrom |
| CN104403626A (en) * | 2014-11-28 | 2015-03-11 | 广州市白云化工实业有限公司 | High-anti-poisoning one-component pouring sealant for LED driving power supply and preparation method of high-anti-poisoning one-component pouring sealant |
| CN106833510A (en) * | 2017-01-11 | 2017-06-13 | 宁波聚力新材料科技有限公司 | New energy high heat conduction low-gravity organic silicon potting adhesive |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021164241A1 (en) * | 2020-02-17 | 2021-08-26 | 苏州桐力光电股份有限公司 | Organosilicon porous breathable disinfection and sterilization nano-filtration material for masks and preparation method therefor |
| CN112521754A (en) * | 2020-10-30 | 2021-03-19 | 广东工业大学 | MXene nanosheet compounded heat-conducting gel with thermal self-repairing performance and preparation method thereof |
| CN112724927A (en) * | 2020-12-25 | 2021-04-30 | 浙江中特化工有限公司 | UV curing silicone gel for lead sealing |
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