CN109777345B - Self-healing two-component addition type heat-conducting silicone gel and preparation method thereof - Google Patents
Self-healing two-component addition type heat-conducting silicone gel and preparation method thereof Download PDFInfo
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Abstract
A self-healing double-component addition type heat-conducting silicone gel and a preparation method thereof, which comprises a component A and a component B; wherein the raw material formula of the component A comprises 30-50 parts of vinyl terminated polysiloxane which accords with a general formula (1); 5-15 parts of first heat-conducting filler; 0.1-5 parts of a catalyst; the raw material formula of the component B comprises 15-25 parts of polyvinyl polysiloxane corresponding to a general formula (2); 5-25 parts of terminal hydrogenpolysiloxane according to general formula (3); 5-15 parts of a second heat-conducting filler; 5-15 parts of a silane coupling agent; 0.1-1.0 part of inhibitor; the mass ratio of the component A to the component B is 1: 0.8-1.2. 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.
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 content of the first and second substances,
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 content of the first and second substances,
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 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 content of the first and second substances,
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 above-mentionedThe 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 content of the first and second substances,
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 content of the first and second substances,
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 (6)
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 content of the first and second substances,
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 = 100-;
the raw material formula of the component B comprises the following raw materials in parts by weight:
15-25 parts of polyvinyl polysiloxane corresponding to general formula (2);
5-25 parts of terminal hydrogenpolysiloxane according to general formula (3);
5-15 parts of a second heat-conducting filler;
5-15 parts of a silane coupling agent;
0.1-1.0 part of inhibitor;
(CH3)2(CH2=CH)SiO1/2[(CH3)2SiO2/2]z[CH3(CH2=CH)SiO2/2]m (2);
in the general formula (2), z =80-100, m = 50-80;
R(CH3)2SiO1/2[(CH3)2SiO2/2]x[CH3RSiO2/2]y (3);
in the general formula (3), R = H, x =30-50, y = 10-30;
the mass ratio of the component A to the component B is 1: 0.8-1.2;
the viscosity of the vinyl-terminated polysiloxane according to the general formula (1) is in the range of 300-1000 centipoises;
the viscosity range of the polyvinyl polysiloxane according to the general formula (2) is 250-350 centipoises;
the viscosity of the terminal hydrogenpolysiloxane according to the general formula (3) ranges from 50 to 250 centipoises;
the inhibitor is at least one of 3-methyl-1-butyne-3-alcohol and tetravinylcyclotetrasiloxane.
2. 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。
3. 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.
4. 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。
5. 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.
6. A method of preparing the self-healing two-component addition type heat conductive silicone gel according to any one of claims 1 to 5, 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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