1. The organic silicon heat-conducting pouring sealant is characterized by being prepared from the following raw materials in parts by weight:

10-25 parts of vinyl-terminated silicone oil;

60-95 parts of heat-conducting filler;

1-3 parts of a silane coupling agent;

8-16 parts of hydrogen-containing silicone oil;

0.1-0.5 part of platinum catalyst;

0.00005-0.001 part of ethyne cyclohexanol.

2. The silicone heat-conducting pouring sealant as claimed in claim 1, wherein: the vinyl-terminated silicone oil contains 0.1-1% of vinyl.

3. The silicone heat-conducting pouring sealant as claimed in claim 1, wherein: the thermally conductive filler includes one or more of spherical alumina, silicon carbide, and aluminum hydroxide.

4. The silicone heat-conducting pouring sealant as claimed in claim 3, wherein: the heat-conducting filler comprises spherical alumina, silicon carbide and aluminum hydroxide, and the mixing ratio of the spherical alumina, the silicon carbide and the aluminum hydroxide in parts by weight is (45-60): (5-15): (10-20).

5. The silicone heat-conducting pouring sealant as claimed in claim 3 or 4, wherein: the spherical alumina comprises spherical alumina A and spherical alumina B, the mesh number of the spherical alumina A is 200-800 meshes, and the mesh number of the spherical alumina B is 2000-5000 meshes; the mixing ratio of the spherical alumina A to the spherical alumina B in parts by weight is (30-40): (15-20).

6. The silicone heat-conducting pouring sealant according to claim 4 or 5, characterized in that: the mesh number of the silicon carbide is 300-2000 meshes; the mesh number of the aluminum hydroxide is 1000-3000 meshes.

7. The silicone heat-conducting pouring sealant as claimed in claim 1, wherein: the silane coupling agent is methyl trimethoxy silane.

8. The silicone heat-conducting pouring sealant as claimed in claim 1, wherein: the hydrogen-containing silicone oil comprises terminal hydrogen-containing silicone oil and side hydrogen-containing silicone oil, and the weight part mixing ratio of the terminal hydrogen-containing silicone oil to the side hydrogen-containing silicone oil is (5-10): (3-6).

9. The silicone heat-conducting pouring sealant as claimed in claim 8, wherein: the hydrogen content of the hydrogen-terminated silicone oil is 0.05-0.2%; the hydrogen content of the lateral hydrogen-containing silicone oil is 0.1-0.5%.

10. A method for preparing the silicone heat-conducting pouring sealant as claimed in any one of claims 1 to 9, characterized in that the method comprises the following preparation steps:

s1, mixing the vinyl-terminated silicone oil, the heat-conducting filler and the silane coupling agent, placing the mixture in an environment with the temperature of 160 ℃ below zero and 0.1-0.09 MPa, and stirring and mixing the mixture for 3-5 hours to obtain a mixture;

s2, stirring and cooling the mixture to 40-60 ℃, dividing the mixture into a material A and a material B, adding a platinum catalyst into the material A, stirring and mixing the materials, sieving the mixture with a 100-mesh sieve for subpackage, adding hydrogen-containing silicone oil and acetylene cyclohexanol into the material B, stirring and mixing the mixture, sieving the mixture with a 100-mesh sieve for subpackage.

Background

The electronic packaging adhesive is used for bonding, sealing, encapsulating and coating protection of electronic components, the electronic pouring adhesive is in a liquid state before being solidified and has fluidity, and the viscosity of the adhesive liquid is different according to the material, the performance and the production process of the electronic pouring adhesive product. The application value of the pouring sealant can be realized only after the pouring sealant is completely cured.

The electronic packaging glue has many kinds, and the most common main types of electronic packaging glue are epoxy resin packaging glue, silicone resin packaging glue and polyurethane packaging glue. The organic silicon resin packaging adhesive can be added with some functional fillers to endow the organic silicon resin packaging adhesive with performances in the aspects of electric conduction, heat conduction, magnetic conduction and the like, and meanwhile, the flowability and the mechanical strength of the packaging adhesive can be influenced after the fillers are added.

Organosilicon heat conduction pouring sealant in the market mainly adds a large amount of heat conduction filler and realizes, however because the addition of a large amount of heat conduction filler, has influenced the mobility of heat conduction glue, and the defoaming nature is poor, has the bubble in the solidification glue piece, has greatly reduced the heat conductivility of heat conduction glue on the contrary, but does not add a large amount of heat conduction filler, and the heat conductivility of heat conduction glue can receive the influence equally, has caused a situation of contradiction. In addition, because a large amount of heat-conducting fillers are added, the glue solution is very easy to settle in the storage process, and the hardness of the solidified glue solution is high and is fragile, so that the original elasticity is lost.

Disclosure of Invention

In order to obtain the heat-conducting pouring sealant which is low in viscosity, good in fluidity, high in heat conductivity coefficient and good in elasticity and toughness after glue solution is solidified and formed, the application provides the organic silicon heat-conducting pouring sealant and the preparation method thereof.

In a first aspect, the application provides an organosilicon heat-conducting pouring sealant, which adopts the following technical scheme:

the organic silicon heat-conducting pouring sealant is prepared by polymerizing the following raw materials in parts by weight:

by adopting the technical scheme, the end vinyl silicone oil is used as the matrix composition of the pouring sealant, the heat-conducting filler is added into the end vinyl silicone oil, the heat-conducting filler is connected to form a heat-conducting network, so that heat transfer is performed, the silane coupling agent modifies the surface of the heat-conducting filler, so that the heat-conducting filler is changed from hydrophilicity to lipophilicity, the heat-conducting filler is dispersed in the end vinyl silicone oil more uniformly and has lower viscosity, the rubber material has better fluidity, and the phenomenon of sedimentation of the rubber material is reduced; after the hydrogen-containing silicone oil is added, the hardness and the tensile capability of the pouring sealant after curing molding can be improved, so that the pouring sealant does not become brittle while having certain hardness; after the platinum catalyst and the ethyne cyclohexanol are added, the curing performance of the pouring sealant can be improved.

Preferably, the vinyl-terminated silicone oil has a vinyl content of 0.1-1%.

Preferably, the thermally conductive filler comprises one or more of spherical alumina, silicon carbide and aluminum hydroxide.

Preferably, the heat conducting filler comprises spherical alumina, silicon carbide and aluminum hydroxide, and the mixing ratio of the spherical alumina, the silicon carbide and the aluminum hydroxide in parts by weight is (45-60): (5-15): (10-20).

Preferably, the spherical alumina comprises spherical alumina A and spherical alumina B, the mesh number of the spherical alumina A is 200-800 meshes, and the mesh number of the spherical alumina B is 2000-5000 meshes; the mixing ratio of the spherical alumina A to the spherical alumina B in parts by weight is (30-40): (15-20).

Preferably, the mesh number of the silicon carbide is 300-2000 meshes; the mesh number of the aluminum hydroxide is 1000-3000 meshes.

Preferably, the silane coupling agent is methyltrimethoxysilane.

Preferably, the hydrogen-containing silicone oil comprises terminal hydrogen-containing silicone oil and side hydrogen-containing silicone oil, and the mixing ratio of the terminal hydrogen-containing silicone oil to the side hydrogen-containing silicone oil in parts by weight is (5-10): (3-6).

Preferably, the hydrogen content of the hydrogen-terminated silicone oil is 0.05-0.2%; the hydrogen content of the lateral hydrogen-containing silicone oil is 0.1-0.5%.

In a second aspect, the application provides a preparation method of an organosilicon heat-conducting pouring sealant, which adopts the following technical scheme:

a preparation method of an organic silicon heat conduction pouring sealant comprises the following preparation steps:

s1, mixing the vinyl-terminated silicone oil, the heat-conducting filler and the silane coupling agent, placing the mixture in an environment with the temperature of 160 ℃ below zero and 0.1-0.09 MPa, and stirring and mixing the mixture for 3-5 hours to obtain a mixture;

s2, stirring and cooling the mixture to 40-60 ℃, dividing the mixture into a material A and a material B, adding a platinum catalyst into the material A, stirring and mixing the materials, sieving the mixture with a 100-mesh sieve for subpackage, adding hydrogen-containing silicone oil and acetylene cyclohexanol into the material B, stirring and mixing the mixture, sieving the mixture with a 100-mesh sieve for subpackage.

In summary, the present application has the following beneficial effects:

1. the pouring sealant is prepared by polymerizing the following raw materials in parts by weight: 10-25 parts of vinyl-terminated silicone oil; 60-95 parts of heat-conducting filler; 1-3 parts of a silane coupling agent; 8-16 parts of hydrogen-containing silicone oil; 0.1-0.5 part of platinum catalyst; 0.00005-0.001 part of ethyne cyclohexanol; the vinyl-terminated silicone oil is used as a matrix composition of the pouring sealant, the heat-conducting filler is added into the vinyl-terminated silicone oil, the heat-conducting filler is connected to form a heat-conducting network, so that heat transfer is performed, the silane coupling agent modifies the surface of the heat-conducting filler, the heat-conducting filler is changed from hydrophilicity to lipophilicity, the heat-conducting filler is dispersed in the vinyl-terminated silicone oil more uniformly and has lower viscosity, the rubber material has better fluidity, and the phenomenon that the rubber material is settled is reduced; after the hydrogen-containing silicone oil is added, the hardness and the tensile capability of the pouring sealant after curing molding can be improved, so that the pouring sealant does not become brittle while having certain hardness; after the platinum catalyst and the ethyne cyclohexanol are added, the curing performance of the pouring sealant can be improved.

Detailed Description

The present application is described in further detail below with reference to examples 1-30.

Examples

Examples 1 to 5

The weight parts of the components of the silicone heat-conducting pouring sealant in examples 1-5 are shown in table 1.

TABLE 1 weight parts of the components of the organosilicon thermal conductive pouring sealant in examples 1-5

In examples 1 to 5, the vinyl group content in the terminal vinyl silicone oil was 0.1 to 1%; the mesh number of the spherical alumina A is 200-300 meshes, and the mesh number of the spherical alumina B is 2000-2500 meshes; the mesh number of the silicon carbide is 300-500 meshes; the mesh number of the aluminum hydroxide is 1000-2000 meshes; the silane coupling agent is methyl trimethoxy silane; the hydrogen content of the terminal hydrogen-containing silicone oil is 0.05-0.2%, and the hydrogen content of the side hydrogen-containing silicone oil is 0.1-0.5%; the platinum catalyst was a platinum (0) -divinyltetramethyldisiloxane complex having a platinum content of 5000 ppm.

The preparation method of the organic silicon heat-conducting pouring sealant in the embodiments 1 to 5 comprises the following steps:

s1, mixing the vinyl-terminated silicone oil, the spherical alumina A, the spherical alumina B, the silicon carbide, the aluminum hydroxide and the silane coupling agent, placing the mixture in an environment with the vacuum degree of-0.1 to-0.09 MPa and the temperature of 150 ℃, and stirring and mixing for 4 hours to obtain a mixture;

and S2, introducing cooling water, stirring and cooling the mixture to 50 ℃, evenly dividing the mixture into a material A and a material B, adding a platinum catalyst into the material A, stirring and mixing the materials, subpackaging the mixture by a 100-mesh screen, adding hydrogen-containing silicone oil at the end, hydrogen-containing silicone oil at the side and ethynl cyclohexanol into the material B, stirring and mixing the mixture, and subpackaging the mixture by a 100-mesh screen.

Examples 6 to 10

The weight parts of the components of the silicone heat-conducting pouring sealant in the embodiments 6-10 are shown in table 2.

TABLE 2 weight parts of the components of the organosilicon thermal conductive pouring sealant in examples 6-10

As used in examples 6 to 10, the vinyl-terminated silicone oil had a vinyl group content of 0.1 to 1%; the mesh number of the spherical alumina A is 700-; the mesh number of the silicon carbide is 1500-; the mesh number of the aluminum hydroxide is 2500-; the silane coupling agent is methyl trimethoxy silane; the hydrogen content of the terminal hydrogen-containing silicone oil is 0.05-0.2%, and the hydrogen content of the side hydrogen-containing silicone oil is 0.1-0.5%; the platinum catalyst was a platinum (0) -divinyltetramethyldisiloxane complex having a platinum content of 5000 ppm.

The preparation method of the organic silicon heat-conducting pouring sealant in the embodiment 6 comprises the following steps:

s1, mixing the vinyl-terminated silicone oil, the spherical alumina A, the silicon carbide, the aluminum hydroxide and the silane coupling agent, placing the mixture in an environment with a vacuum degree of-0.1 to-0.09 MPa and a temperature of 160 ℃, and stirring and mixing for 4 hours to obtain a mixture;

and S2, introducing cooling water, stirring and cooling the mixture to 50 ℃, evenly dividing the mixture into a material A and a material B, adding a platinum catalyst into the material A, stirring and mixing the materials, subpackaging the mixture by a 100-mesh screen, adding hydrogen-containing silicone oil at the end, hydrogen-containing silicone oil at the side and ethynl cyclohexanol into the material B, stirring and mixing the mixture, and subpackaging the mixture by a 100-mesh screen.

The preparation method of the organic silicon heat-conducting pouring sealant in the embodiment 7 comprises the following steps:

s1, mixing the vinyl-terminated silicone oil, the spherical alumina B, the silicon carbide, the aluminum hydroxide and the silane coupling agent, placing the mixture in an environment with the vacuum degree of below 0.09MPa and the temperature of 150-;

and S2, introducing cooling water, stirring and cooling the mixture to 50 ℃, evenly dividing the mixture into a material A and a material B, adding a platinum catalyst into the material A, stirring and mixing the materials, subpackaging the mixture by a 100-mesh screen, adding hydrogen-containing silicone oil at the end, hydrogen-containing silicone oil at the side and ethynl cyclohexanol into the material B, stirring and mixing the mixture, and subpackaging the mixture by a 100-mesh screen.

The preparation method of the organic silicon heat-conducting pouring sealant in the embodiment 8 comprises the following steps:

s1, mixing the vinyl-terminated silicone oil, the spherical alumina B and the silane coupling agent, placing the mixture in an environment with the vacuum degree of-0.1 to-0.09 MPa and the temperature of 155 ℃, and stirring and mixing for 4 hours to obtain a mixture;

and S2, introducing cooling water, stirring and cooling the mixture to 50 ℃, evenly dividing the mixture into a material A and a material B, adding a platinum catalyst into the material A, stirring and mixing the materials, subpackaging the mixture by a 100-mesh screen, adding hydrogen-containing silicone oil at the end, hydrogen-containing silicone oil at the side and ethynl cyclohexanol into the material B, stirring and mixing the mixture, and subpackaging the mixture by a 100-mesh screen.

Embodiment 9 a method for preparing an organosilicon thermal conductive potting adhesive, comprising the steps of:

s1, mixing the vinyl-terminated silicone oil, the spherical alumina A and the silane coupling agent, placing the mixture in an environment with the vacuum degree of 0.09MPa and the temperature of 150 ℃, and stirring and mixing for 4 hours to obtain a mixture;

and S2, introducing cooling water, stirring and cooling the mixture to 50 ℃, evenly dividing the mixture into a material A and a material B, adding a platinum catalyst into the material A, stirring and mixing the materials, subpackaging the mixture by a 100-mesh screen, adding hydrogen-containing silicone oil at the end, hydrogen-containing silicone oil at the side and ethynl cyclohexanol into the material B, stirring and mixing the mixture, and subpackaging the mixture by a 100-mesh screen.

The preparation method of the organic silicon heat-conducting pouring sealant in embodiment 10 includes the following steps:

s1, mixing the vinyl-terminated silicone oil, the spherical alumina A, the spherical alumina B and the silane coupling agent, placing the mixture in an environment with the vacuum degree of below 0.09MPa and the temperature of 150-160 ℃, and stirring and mixing for 4 hours to obtain a mixture;

and S2, introducing cooling water, stirring and cooling the mixture to 50 ℃, evenly dividing the mixture into a material A and a material B, adding a platinum catalyst into the material A, stirring and mixing the materials, subpackaging the mixture by a 100-mesh screen, adding hydrogen-containing silicone oil at the end, hydrogen-containing silicone oil at the side and ethynl cyclohexanol into the material B, stirring and mixing the mixture, and subpackaging the mixture by a 100-mesh screen.

Examples 11 to 15

The weight parts of the components of the silicone heat-conducting potting adhesive in examples 11-15 are shown in table 3.

TABLE 3 weight parts of the components of the organosilicon thermal conductive pouring sealant in examples 11-15

As used in examples 11 to 15, the vinyl-terminated silicone oil had a vinyl group content of 0.1 to 1%; the mesh number of the spherical alumina A is 500-600 meshes, and the mesh number of the spherical alumina B is 3000-4000 meshes; the mesh number of the silicon carbide is 1500-; the mesh number of the aluminum hydroxide is 2000-2500 meshes; the silane coupling agent is methyl trimethoxy silane; the hydrogen content of the terminal hydrogen-containing silicone oil is 0.05-0.2%, and the hydrogen content of the side hydrogen-containing silicone oil is 0.1-0.5%; the platinum catalyst was a platinum (0) -divinyltetramethyldisiloxane complex having a platinum content of 5000 ppm.

The preparation method of the organic silicon heat-conducting pouring sealant in embodiment 11 includes the following steps:

s1, mixing the vinyl-terminated silicone oil, the silicon carbide and the silane coupling agent, placing the mixture in an environment with the vacuum degree of-0.1 to-0.09 MPa and the temperature of 160 ℃, and stirring and mixing for 4 hours to obtain a mixture;

and S2, introducing cooling water, stirring and cooling the mixture to 50 ℃, evenly dividing the mixture into a material A and a material B, adding a platinum catalyst into the material A, stirring and mixing the materials, subpackaging the mixture by a 100-mesh screen, adding hydrogen-containing silicone oil at the end, hydrogen-containing silicone oil at the side and ethynl cyclohexanol into the material B, stirring and mixing the mixture, and subpackaging the mixture by a 100-mesh screen.

The preparation method of the organic silicon heat-conducting pouring sealant in embodiment 12 includes the following steps:

s1, mixing the vinyl-terminated silicone oil, the aluminum hydroxide and the silane coupling agent, placing the mixture in an environment with the vacuum degree of-0.1 to-0.09 MPa and the temperature of 160 ℃, and stirring and mixing for 4 hours to obtain a mixture;

and S2, introducing cooling water, stirring and cooling the mixture to 50 ℃, evenly dividing the mixture into a material A and a material B, adding a platinum catalyst into the material A, stirring and mixing the materials, subpackaging the mixture by a 100-mesh screen, adding hydrogen-containing silicone oil at the end, hydrogen-containing silicone oil at the side and ethynl cyclohexanol into the material B, stirring and mixing the mixture, and subpackaging the mixture by a 100-mesh screen.

The preparation method of the organic silicon heat-conducting pouring sealant in embodiment 13 includes the following steps:

s1, mixing the vinyl-terminated silicone oil, the spherical alumina A, the silicon carbide and the silane coupling agent, placing the mixture in an environment with the vacuum degree of-0.1 to-0.09 MPa and the temperature of 150 ℃, and stirring and mixing for 4 hours to obtain a mixture;

and S2, introducing cooling water, stirring and cooling the mixture to 50 ℃, evenly dividing the mixture into a material A and a material B, adding a platinum catalyst into the material A, stirring and mixing the materials, subpackaging the mixture by a 100-mesh screen, adding hydrogen-containing silicone oil at the end, hydrogen-containing silicone oil at the side and ethynl cyclohexanol into the material B, stirring and mixing the mixture, and subpackaging the mixture by a 100-mesh screen.

The preparation method of the organic silicon heat-conducting pouring sealant in embodiment 14 includes the following steps:

s1, mixing the vinyl-terminated silicone oil, the spherical alumina A, the spherical alumina B, the silicon carbide and the silane coupling agent, placing the mixture in an environment with the vacuum degree of-0.1 to-0.09 MPa and the temperature of 155 ℃, and stirring and mixing for 4 hours to obtain a mixture;

and S2, introducing cooling water, stirring and cooling the mixture to 50 ℃, evenly dividing the mixture into a material A and a material B, adding a platinum catalyst into the material A, stirring and mixing the materials, subpackaging the mixture by a 100-mesh screen, adding hydrogen-containing silicone oil at the end, hydrogen-containing silicone oil at the side and ethynl cyclohexanol into the material B, stirring and mixing the mixture, and subpackaging the mixture by a 100-mesh screen.

The preparation method of the organic silicon heat-conducting pouring sealant in embodiment 15 includes the following steps:

s1, mixing the vinyl-terminated silicone oil, the spherical alumina A, the aluminum hydroxide and the silane coupling agent, placing the mixture in an environment with the vacuum degree of-0.1 to-0.09 MPa and the temperature of 150 ℃, and stirring and mixing for 4 hours to obtain a mixture;

and S2, introducing cooling water, stirring and cooling the mixture to 50 ℃, evenly dividing the mixture into a material A and a material B, adding a platinum catalyst into the material A, stirring and mixing the materials, subpackaging the mixture by a 100-mesh screen, adding hydrogen-containing silicone oil at the end, hydrogen-containing silicone oil at the side and ethynl cyclohexanol into the material B, stirring and mixing the mixture, and subpackaging the mixture by a 100-mesh screen.

Examples 16 to 20

The weight parts of the components of the silicone heat-conducting potting adhesive in examples 16 to 20 are shown in table 4.

TABLE 4 weight parts of the components of the organosilicon thermal conductive pouring sealant in examples 16-20

As used in examples 16 to 20, the vinyl-terminated silicone oil had a vinyl group content of 0.1 to 1%; the mesh number of the spherical alumina A is 500-600 meshes, and the mesh number of the spherical alumina B is 2500-3000 meshes; the mesh number of the silicon carbide is 1500-; the mesh number of the aluminum hydroxide is 2500-; the silane coupling agent is methyl trimethoxy silane; the hydrogen content of the terminal hydrogen-containing silicone oil is 0.05-0.2%, and the hydrogen content of the side hydrogen-containing silicone oil is 0.1-0.5%; the platinum catalyst was a platinum (0) -divinyltetramethyldisiloxane complex having a platinum content of 5000 ppm.

The preparation method of the organic silicon heat-conducting pouring sealant in embodiment 16 includes the following steps:

s1, mixing the vinyl-terminated silicone oil, the spherical alumina A, the spherical alumina B, the aluminum hydroxide and the silane coupling agent, placing the mixture in an environment with the vacuum degree of-0.1 to-0.09 MPa and the temperature of 156 ℃, and stirring and mixing for 4 hours to obtain a mixture;

and S2, introducing cooling water, stirring and cooling the mixture to 50 ℃, evenly dividing the mixture into a material A and a material B, adding a platinum catalyst into the material A, stirring and mixing the materials, subpackaging the mixture by a 100-mesh screen, adding hydrogen-containing silicone oil at the end, hydrogen-containing silicone oil at the side and ethynl cyclohexanol into the material B, stirring and mixing the mixture, and subpackaging the mixture by a 100-mesh screen.

The preparation method of the organic silicon heat-conducting pouring sealant in embodiment 17 comprises the following steps:

s1, mixing the vinyl-terminated silicone oil, the silicon carbide, the aluminum hydroxide and the silane coupling agent, placing the mixture in an environment with the vacuum degree of-0.1 to-0.09 MPa and the temperature of 150 ℃, and stirring and mixing for 4 hours to obtain a mixture;

and S2, introducing cooling water, stirring and cooling the mixture to 50 ℃, evenly dividing the mixture into a material A and a material B, adding a platinum catalyst into the material A, stirring and mixing the materials, subpackaging the mixture by a 100-mesh screen, adding hydrogen-containing silicone oil at the end, hydrogen-containing silicone oil at the side and ethynl cyclohexanol into the material B, stirring and mixing the mixture, and subpackaging the mixture by a 100-mesh screen.

The preparation method of the organic silicon heat-conducting pouring sealant in embodiment 18 includes the following steps:

s1, mixing the vinyl-terminated silicone oil, the spherical alumina A, the silicon carbide, the aluminum hydroxide and the silane coupling agent, placing the mixture in an environment with the vacuum degree of-0.1 to-0.09 MPa and the temperature of 150 ℃, and stirring and mixing for 4 hours to obtain a mixture;

and S2, introducing cooling water, stirring and cooling the mixture to 50 ℃, evenly dividing the mixture into a material A and a material B, adding a platinum catalyst into the material A, stirring and mixing the materials, subpackaging the mixture by a 100-mesh screen, adding hydrogen-containing silicone oil at the end, hydrogen-containing silicone oil at the side and ethynl cyclohexanol into the material B, stirring and mixing the mixture, and subpackaging the mixture by a 100-mesh screen.

The preparation method of the organic silicon heat-conducting pouring sealant in embodiment 19 includes the following steps:

s1, mixing the vinyl-terminated silicone oil, the spherical alumina B, the silicon carbide, the aluminum hydroxide and the silane coupling agent, placing the mixture in an environment with a vacuum degree of-0.1 to-0.09 MPa and a temperature of 156 ℃, and stirring and mixing for 4 hours to obtain a mixture;

and S2, introducing cooling water, stirring and cooling the mixture to 50 ℃, evenly dividing the mixture into a material A and a material B, adding a platinum catalyst into the material A, stirring and mixing the materials, subpackaging the mixture by a 100-mesh screen, adding hydrogen-containing silicone oil at the end, hydrogen-containing silicone oil at the side and ethynl cyclohexanol into the material B, stirring and mixing the mixture, and subpackaging the mixture by a 100-mesh screen.

The preparation method of the organic silicon heat-conducting pouring sealant in embodiment 20 includes the following steps:

s1, mixing the vinyl-terminated silicone oil, the spherical alumina B, the silicon carbide and the silane coupling agent, placing the mixture in an environment with the vacuum degree of-0.1 to-0.09 MPa and the temperature of 150 ℃, and stirring and mixing for 4 hours to obtain a mixture;

and S2, introducing cooling water, stirring and cooling the mixture to 50 ℃, evenly dividing the mixture into a material A and a material B, adding a platinum catalyst into the material A, stirring and mixing the materials, subpackaging the mixture by a 100-mesh screen, adding hydrogen-containing silicone oil at the end, hydrogen-containing silicone oil at the side and ethynl cyclohexanol into the material B, stirring and mixing the mixture, and subpackaging the mixture by a 100-mesh screen.

Examples 21 to 25

The weight parts of the components of the silicone heat-conducting potting adhesive in examples 21-25 are shown in table 5.

TABLE 5 weight parts of the components of the organosilicon thermal conductive pouring sealant in examples 21-25

As used in examples 21 to 25, the vinyl-terminated silicone oil had a vinyl group content of 0.1 to 1%; the mesh number of the spherical alumina A is 400-500 meshes, and the mesh number of the spherical alumina B is 2700-3500 meshes; the mesh number of the silicon carbide is 1200-1700 meshes; the mesh number of the aluminum hydroxide is 2300-2800 meshes; the silane coupling agent is methyl trimethoxy silane; the hydrogen content of the terminal hydrogen-containing silicone oil is 0.05-0.2%, and the hydrogen content of the side hydrogen-containing silicone oil is 0.1-0.5%; the platinum catalyst was a platinum (0) -divinyltetramethyldisiloxane complex having a platinum content of 5000 ppm.

The preparation method of the organic silicon heat-conducting pouring sealant in the embodiments 21 to 25 includes the following steps:

s1, mixing the vinyl-terminated silicone oil, the spherical alumina A, the spherical alumina B, the silicon carbide, the aluminum hydroxide and the silane coupling agent, placing the mixture in an environment with the vacuum degree of-0.1 to-0.09 MPa and the temperature of 150 ℃, and stirring and mixing for 4 hours to obtain a mixture;

and S2, introducing cooling water, stirring and cooling the mixture to 50 ℃, evenly dividing the mixture into a material A and a material B, adding a platinum catalyst into the material A, stirring and mixing the materials, subpackaging the mixture by a 100-mesh screen, adding hydrogen-containing silicone oil at the end, hydrogen-containing silicone oil at the side and ethynl cyclohexanol into the material B, stirring and mixing the mixture, and subpackaging the mixture by a 100-mesh screen.

Examples 26 to 30

The weight parts of the components of the silicone heat-conducting potting adhesive in examples 26 to 30 are shown in table 6.

TABLE 6 weight parts of the components of the organosilicon thermal conductive pouring sealant in examples 26-30

As used in examples 26 to 30, the vinyl-terminated silicone oil had a vinyl group content of 0.1 to 1%; the mesh number of the spherical alumina A is 300-600 meshes, and the mesh number of the spherical alumina B is 4500-5000 meshes; the mesh number of the silicon carbide is 1300-2000 meshes; the mesh number of the aluminum hydroxide is 1900-2300 meshes; the silane coupling agent is methyl trimethoxy silane; the hydrogen content of the terminal hydrogen-containing silicone oil is 0.05-0.2%, and the hydrogen content of the side hydrogen-containing silicone oil is 0.1-0.5%; the platinum catalyst was a platinum (0) -divinyltetramethyldisiloxane complex having a platinum content of 5000 ppm.

The preparation method of the organic silicon heat-conducting pouring sealant in embodiment 26 includes the following steps:

s1, mixing the vinyl-terminated silicone oil, the spherical alumina A, the spherical alumina B, the silicon carbide, the aluminum hydroxide and the silane coupling agent, placing the mixture in an environment with the vacuum degree of-0.1 to-0.09 MPa and the temperature of 150 ℃, and stirring and mixing for 4 hours to obtain a mixture;

and S2, introducing cooling water, stirring and cooling the mixture to 50 ℃, evenly dividing the mixture into a material A and a material B, adding a platinum catalyst into the material A, stirring and mixing the materials, subpackaging the mixture by using a 100-mesh screen, adding hydrogen-containing silicone oil and acetylene cyclohexanol into the material B, stirring and mixing the mixture, and subpackaging the mixture by using a 100-mesh screen.

The preparation method of the organic silicon heat-conducting pouring sealant in embodiment 27 includes the following steps:

s1, mixing the vinyl-terminated silicone oil, the spherical alumina A, the spherical alumina B, the silicon carbide, the aluminum hydroxide and the silane coupling agent, placing the mixture in an environment with the vacuum degree of-0.1 to-0.09 MPa and the temperature of 160 ℃, and stirring and mixing for 4 hours to obtain a mixture;

and S2, introducing cooling water, stirring and cooling the mixture to 50 ℃, evenly dividing the mixture into a material A and a material B, adding a platinum catalyst into the material A, stirring and mixing the materials, subpackaging the mixture by using a 100-mesh screen, adding lateral hydrogen-containing silicone oil and acetylene cyclohexanol into the material B, stirring and mixing the mixture, and subpackaging the mixture by using a 100-mesh screen.

The preparation method of the organic silicon heat-conducting pouring sealant in the embodiments 28 to 30 includes the following steps:

s1, mixing the vinyl-terminated silicone oil, the spherical alumina A, the spherical alumina B, the silicon carbide, the aluminum hydroxide and the silane coupling agent, placing the mixture in an environment with the vacuum degree of-0.1 to-0.09 MPa and the temperature of 160 ℃, and stirring and mixing for 4 hours to obtain a mixture;

and S2, introducing cooling water, stirring and cooling the mixture to 50 ℃, evenly dividing the mixture into a material A and a material B, adding a platinum catalyst into the material A, stirring and mixing the materials, subpackaging the mixture by a 100-mesh screen, adding hydrogen-containing silicone oil at the end, hydrogen-containing silicone oil at the side and ethynl cyclohexanol into the material B, stirring and mixing the mixture, and subpackaging the mixture by a 100-mesh screen.

Performance test

The detection method comprises the following steps: observing the appearances of the material A and the material B by using a visual inspection method;

the viscosities of the A and B materials at 25 ℃ are respectively detected by using the standard in GB/T10247-2008;

materials a and B1 were tested using the standard in HG/T2728-2012: 1 density after mixing and curing;

and (3) detecting the material A and the material B by using the standard in GB/T531-2008: 1 hardness after hybrid curing (Shore-A);

the standard in GB/T528-2009 was used to test feed A and feed B1: 1 tensile strength (MPa) and elongation at break (%) after mixing and curing;

and (3) detecting the material A and the material B by using the standard in GB/T529-2008: 1 tear strength after hybrid curing (KN/m);

materials A and B were tested using the standard in GB/T10297-2015 for 1: 1 thermal conductivity (W/mk) after mixed curing;

the appearance and viscosity detection data of the organic heat-conducting pouring sealant in the embodiments 1 to 30 are shown in table 7; the data of the density, hardness, tensile strength, elongation at break, tear strength and thermal conductivity of the organic thermal conductive potting adhesive of examples 1-30 are shown in Table 8.

TABLE 7 appearance and viscosity measurements of Silicone thermal conductivity pouring sealants in examples 1-30

TABLE 8 Silicone Heat conducting pouring sealant for examples 1-30

Density, hardness, tensile strength, elongation at break, tear strength and thermal conductivity measurements

As can be seen from the combination of examples 1 to 5, examples 6 and 18, and table 7, in examples 1 to 5, the heat conductive filler contains spherical alumina B, that is, spherical alumina with small particle size, which can be filled between the rubber compounds, so that the filling property of the rubber compounds is increased, that is, the viscosity is relatively reduced, but still in the standard range, and in examples 6 and 18, the gaps between the components of the rubber compounds are relatively large without adding spherical alumina B, so that good adhesion is difficult to obtain, so that the viscosity of the rubber compounds is relatively increased, but still in the standard range, and in examples 1 to 6 and 18, the appearance of the rubber compounds is not substantially affected; as can be seen from table 8, in examples 1 to 5, after the spherical alumina B is added, the density of the pouring sealant after mixing and curing is higher than that in example 6, which is substantially because the spherical alumina B is filled between the pores of the sizing material, the mass of the pouring sealant per unit volume is improved, and the density of the pouring sealant after curing is improved, so that the hardness of the pouring sealant after curing is also improved, and simultaneously, the tensile strength of the pouring sealant after curing is higher than that in examples 6 and 18, which is because the hardness of the pouring sealant itself is improved, and the deformation capability of the pouring sealant is substantially deteriorated, but the tensile strength is still within the standard range; after curing, the elongation at break and tear strength of the pouring sealant of examples 1-5 are reduced compared with those of examples 6 and 18, which are inevitably more "brittle" due to the hardness of the pouring sealant of examples 1-5, but still within the standard range; in the embodiments 1 to 5, the spherical alumina B is added to the heat conductive filler, and the spherical alumina B is filled in the pores of the rubber material, so that in the cured potting adhesive, the heat conductive filler can be uniformly distributed in the potting adhesive, thereby completing the heat conduction, and further improving the heat conductivity coefficient of the potting adhesive in the embodiments 1 to 5.

Combining examples 1-5 with examples 6-7 and examples 18-19, and combining table 7, it can be seen that in examples 1-5, spherical alumina a is added to the heat conductive filler, i.e. spherical alumina with large particle size is included, and the filling ability of spherical alumina a to the compound is relatively poor compared to spherical alumina B, in examples 7 and 19, the heat conductive filler does not include spherical alumina, resulting in an increase in the viscosity of the compound, and combining examples 6-7 and examples 18-19, it can be seen that the addition of spherical alumina a in examples 6 and 18, the addition of spherical alumina B in examples 7 and 19, the addition of spherical alumina B in examples 6 and 18, the addition of spherical alumina B in examples 7 and 19, the viscosity of the compound in examples 6 and 18 is relatively lower, and the viscosity of the compound in examples 7 and 19 is relatively higher; and the appearance of the compound of examples 1-5 and 6-7, examples 18-19 was not substantially changed; combining examples 6-7 and 18-19, it can be seen that the addition of spherical alumina B alone in examples 7 and 19 affects the hardness and tensile strength of the cured potting compound, but the thermal conductivity of the potting compounds in examples 6-7 and 18-19 is significantly lower than that of the potting compounds in examples 1-5.

With reference to examples 1 to 5 and 8, and with reference to tables 7 and 8, it can be seen that the heat conductive filler in example 8 is filled with spherical alumina a only, and the filling property of the sizing material is insufficient, so that the viscosity of the sizing material is significantly improved, that is, the spherical alumina a is difficult to be filled in the sizing material completely, and further, in the cured potting adhesive, the spherical alumina a is difficult to form a heat conductive network, that is, as can be seen from table 8, the heat conductive performance of the potting adhesive in example 8 after curing is greatly reduced; and the properties of the potting adhesive in example 8, such as density, hardness, tensile strength and the like, are obviously reduced compared with those of the potting adhesives in examples 1-5.

With reference to examples 1 to 5, examples 8 to 9, and tables 7 and 8, it can be seen that the heat conductive filler in example 9 was heat conductive filled with only spherical alumina B, and the filling property of the compound was inferior to that in examples 1 to 5, but better than that in example 8, so that the viscosity of the compound in example 9 was slightly inferior to that of the compound in example 8, but still within the standard range; since the particle size of the spherical alumina B is smaller than that of the spherical alumina a, the hardness and tensile strength of the potting adhesive after curing in example 9 are slightly reduced compared with those in example 8, but the elongation at break and the tear strength are slightly increased, and the thermal conductivity coefficient of the potting adhesive in examples 8-9 is significantly reduced compared with that of the potting adhesive in examples 1-5, which is still caused by only adding a single thermal conductive filler, and it can be seen from combining examples 8-9 that the thermal conductivity of the spherical alumina B is slightly improved compared with that of the spherical alumina a.

In combination with examples 8-10 and table 8, it can be seen that the heat conductive filler in example 10 is compounded by using spherical alumina a and spherical alumina B, the hardness, density and tensile strength of the cured potting adhesive in example 10 are all improved compared with those in examples 8-9, the elongation at break and the tear strength are all reduced, and the heat conductive performance of the potting adhesive in example 10 is improved compared with those in examples 8-9, because the spherical alumina a and the spherical alumina B are dispersed in the potting adhesive, and the spherical alumina B is filled in the pores of the spherical alumina a to form a dense and interconnected heat conductive network.

In combination with examples 1 to 5 and examples 11 to 12, and in combination with table 8, it can be seen that the heat conductive filler in example 11 was heat-conductive-filled with only silicon carbide, and the heat conductive filler in example 12 was heat-conductive-filled with only aluminum hydroxide, and the heat conductive properties of examples 11 to 12 were significantly reduced as compared with examples 1 to 5.

By combining example 11 and example 13, and combining table 8, it can be seen that the thermal conductive filler in example 13 is compounded by using spherical alumina a and silicon carbide, so that the thermal conductivity of the potting adhesive in example 13 is slightly higher than that in example 11, i.e. the thermal conductivity is slightly better.

By combining example 11 and example 20, and combining table 8, it can be seen that the thermal conductive filler in example 20 is compounded by using spherical alumina B and silicon carbide, so that the thermal conductivity of the potting adhesive in example 20 is slightly higher than that in example 11, i.e. the thermal conductivity is slightly better.

Combining example 13 and example 20, and combining table 8, it can be seen that the thermal conductivity of the potting compound in example 20 and example 13 is different, but not obvious.

By combining example 13 and example 14, and combining table 8, it can be seen that the thermal conductive filler in example 14 is compounded by using spherical alumina a, spherical alumina B and silicon carbide, so that the thermal conductivity of the potting adhesive in example 14 is slightly higher than that of example 13, i.e. the thermal conductivity is slightly better.

By combining example 12 and example 15, and combining table 8, it can be seen that the thermal conductive filler in example 15 is compounded by using spherical alumina a and aluminum hydroxide, so that the thermal conductivity of the potting adhesive in example 15 is slightly higher than that of example 12, i.e., the thermal conductivity is slightly better.

By combining the example 15 and the example 16 and combining the table 8, it can be seen that the thermal conductive filler in the example 16 is compounded by using the spherical alumina a, the spherical alumina B and the aluminum hydroxide, so that the thermal conductivity of the potting adhesive in the example 16 is slightly higher than that in the example 15, that is, the thermal conductivity is slightly better.

By combining example 11, example 12, and example 17, and by combining table 8, it can be seen that the heat conductive filler in example 17 is a combination of silicon carbide and aluminum hydroxide, so that the heat conductivity of the potting adhesive in example 17 is higher than that of examples 11 and 12, i.e., the heat conductivity is better.

By combining examples 1 to 5 with examples 14 and 16 and combining table 8, it can be seen that the thermal conductive fillers in examples 1 to 5 are compounded by using spherical alumina a, spherical alumina B, silicon carbide and aluminum hydroxide, so that the thermal conductivity of the potting adhesive in examples 1 to 5 is higher than that of the potting adhesive in examples 14 and 16, i.e., the thermal conductive property is better.

Combining examples 1-5 and examples 21-25, and combining table 8, it can be seen that when spherical alumina a: spherical alumina B: silicon carbide: aluminum hydroxide is added in a compounding way according to the proportion of (30-40): (15-20): (5-15): (10-20), the thermal conductivity of the potting adhesive is in the optimal range.

By combining examples 1-5 and examples 26-27 and combining table 8, it can be seen that in example 26, only terminal hydrogen-containing silicone oil is added to material B, and in example 27, only side hydrogen-containing silicone oil is added to material B, both of which significantly reduce the hardness and tensile strength of the cured potting adhesive, but greatly improve the elongation at break and tear strength, and affect the thermal conductivity of the potting adhesive.

The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.