CN112341821A - Solid silicon resin compound and preparation method and application thereof - Google Patents

Solid silicon resin compound and preparation method and application thereof Download PDF

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CN112341821A
CN112341821A CN201910722991.7A CN201910722991A CN112341821A CN 112341821 A CN112341821 A CN 112341821A CN 201910722991 A CN201910722991 A CN 201910722991A CN 112341821 A CN112341821 A CN 112341821A
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filler
solid
solid silicone
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CN112341821B (en
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王锐
张琛
刘志莹
李海亮
王善学
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Beijing Kehua Advanced Material Technology Co ltd
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2237Oxides; Hydroxides of metals of titanium
    • C08K2003/2241Titanium dioxide
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets
    • C08L2203/206Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend

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Abstract

The invention relates to the field of application of LED support packaging materials, in particular to a solid silicone resin compound and a preparation method and application thereof. The solid silicone resin compound comprises 10-25 wt% of vinyl-containing polysiloxane, 2-15 wt% of high-reflectivity filler, 25-45 wt% of high-thermal-conductivity filler, 25-45 wt% of solid filler, 0.01-2 wt% of initiator, 0.01-3 wt% of release agent, 0.001-1 wt% of stress modifier and 0.1-2 wt% of adhesion promoter. The solid silicone resin compound has the characteristics of high heat conduction, high reflectivity, high strength, good storage property and the like.

Description

Solid silicon resin compound and preparation method and application thereof
Technical Field
The invention relates to the field of application of LED support packaging materials, in particular to a solid silicone resin compound and a preparation method and application thereof.
Background
The LED support packaging material mainly comprises thermoplastic polyamide (PPA) resin, thermoplastic polyester resin (PCT), thermosetting epoxy resin (EMC) and thermosetting silicone resin (SMC). With the continuation of the use time and the increase of the use temperature, PPA and PCT can be seriously degraded to cause the problems of peeling, falling off, reduction of mechanical strength, yellowing and the like; compared with PPA and PCT resins, EMC resin can effectively avoid the problem of degradation, but the yellowing resistance under long-time high-temperature conditions is still poor; the SMC resin has excellent high temperature resistance and yellowing resistance, can meet the application requirement that the power of a single LED lamp bead is more than or equal to 3W, is favored by more and more LED packaging manufacturers, and invests a large amount of manpower and material resources to develop the LED bracket based on the SMC material.
At present, the development direction of SMC resin materials is mainly based on a hydrosilylation mechanism, Karstedt catalyst is adopted as a catalytic system, and the method has the defects of easy poisoning, short storage period, low glass transition temperature, low high-temperature strength, easy warping and the like of the catalyst.
Disclosure of Invention
The invention aims to overcome the defects of easy degradation, easy yellowing, poor strength, poor storage property and the like of the existing LED support packaging material, and provides a solid silicone resin compound and a preparation method and application thereof.
In order to achieve the above object, according to one aspect of the present invention, there is provided a solid silicone composite, wherein the solid silicone composite comprises 10 to 25 wt% of a vinyl group-containing polysiloxane, 2 to 15 wt% of a high-reflectance filler, 25 to 45 wt% of a high-thermal-conductivity filler, 25 to 45 wt% of a solid filler, 0.01 to 2 wt% of an initiator, 0.01 to 3 wt% of a mold release agent, 0.001 to 1 wt% of a stress modifier, and 0.1 to 2 wt% of an adhesion promoter.
Preferably, the vinyl-containing polysiloxane is composed of CH2=CHSiO3/2Unit, CH2=CHCH3CH3SiO1/2Unit, C6H6SiO3/2Unit, CH3SiO3/2Unit (C)6H6)2SiO2/2Unit, (CH)3)2SiO2/2Unit and C6H6CH3SiO2/2Copolymers composed of all or part of the units.
Preferably, the vinyl group-containing polysiloxane contains a structural unit provided by vinyltrimethoxysilane and/or a structural unit provided by tetramethyldivinyldisiloxane and at least one selected from the group consisting of a structural unit provided by phenyltrimethoxysilane, a structural unit provided by methyltrimethoxysilane, a structural unit provided by diphenyldimethoxysilane, a structural unit provided by dimethyldimethoxysilane and a structural unit provided by methylphenyldimethoxysilane.
Preferably, the vinyl group-containing polysiloxane is solid at room temperature.
Preferably, the high-reflectivity filler is selected from one or more of titanium dioxide, barium sulfate, antimony oxide, zinc sulfide, and zinc oxide.
Preferably, the high thermal conductive filler is selected from one or more of alumina, silicon carbide, silicon nitride, boron nitride, aluminum nitride, graphene, and carbon nanotubes.
Preferably, the solid filler is selected from one or more of silica powder, magnesium hydroxide, aluminum hydroxide, calcium carbonate and fumed silica.
Preferably, the initiator is selected from one or more of cyclohexanone peroxide, dibenzoyl peroxide, t-butyl hydroperoxide, azobisisobutyronitrile and azobisisoheptonitrile.
Preferably, the release agent is selected from one or more of carnauba wax, polyethylene wax, oxidized polyethylene wax, Fischer-Tropsch wax, polypropylene wax, and fatty acid wax.
Preferably, the stress modifier is selected from one or more of polyether modified silicone oil, silicone modified epoxy resin, liquid carboxyl terminated nitrile rubber and triblock copolymer containing silicone component.
Preferably, the adhesion promoter is an organosilicon compound containing an epoxy group; further preferably, the adhesion promoter has at least one of the structures represented by formula (1) and formula (2);
Figure BDA0002157896070000031
in a second aspect, the present invention provides a method for preparing the solid silicone composite, comprising the steps of:
(1) mixing polysiloxane containing vinyl, high-reflection filler, high-thermal-conductivity filler, solid filler, initiator, release agent, stress modifier and adhesion promoter, and then dispersing for multiple times;
(2) and (2) mixing the mixture dispersed in the step (1) on an open mill.
The third aspect of the invention provides the application of the solid silicone compound as an LED bracket packaging material.
The solid silicone resin compound is prepared by adopting solid vinyl silicone resin as a basic raw material, using a free radical initiator and introducing heat-resistant and high-reflectivity fillers based on a free radical polymerization mechanism, and has the characteristics of high heat conductivity, high reflectivity, high strength, good storability and the like.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a solid silicone resin compound, wherein the solid silicone resin compound comprises 10-25 wt% of vinyl-containing polysiloxane, 2-15 wt% of high-reflectivity filler, 25-45 wt% of high-thermal-conductivity filler, 25-45 wt% of solid filler, 0.01-2 wt% of initiator, 0.01-3 wt% of release agent, 0.001-1 wt% of stress modifier and 0.1-2 wt% of adhesion promoter.
Preferably, the solid silicone resin composite contains 11-20 wt% of vinyl-containing polysiloxane, 3-14 wt% of high-reflectivity filler, 30-44 wt% of high-thermal-conductivity filler, 30-42 wt% of solid filler, 0.1-1 wt% of initiator, 0.02-2 wt% of release agent, 0.005-0.6 wt% of stress modifier and 0.15-1 wt% of adhesion promoter.
Further preferably, the solid silicone resin composite contains 12 to 18 wt% of vinyl-containing polysiloxane, 4 to 13 wt% of high-reflectance filler, 35 to 42 wt% of high-thermal-conductivity filler, 35 to 40 wt% of solid filler, 0..2 to 0.5 wt% of initiator, 0.05 to 1 wt% of release agent, 0.05 to 0.4 wt% of stress modifier, and 0.2 to 0.8 wt% of adhesion promoter.
Preferably, the vinyl-containing polysiloxane contains CH2=CHSiO3/2Unit, CH2=CHCH3CH3SiO1/2Unit, C6H6SiO3/2Unit, CH3SiO3/2Unit, (C)6H6)2SiO2/2Unit, (CH)3)2SiO2/2Unit and C6H6CH3SiO2/2At least one of the units.
Further preferably, the vinyl group-containing polysiloxane contains a structural unit provided by vinyltrimethoxysilane and/or a structural unit provided by tetramethyldivinyldisiloxane and at least one selected from the group consisting of a structural unit provided by phenyltrimethoxysilane, a structural unit provided by methyltrimethoxysilane, a structural unit provided by diphenyldimethoxysilane, a structural unit provided by dimethyldimethoxysilane and a structural unit provided by methylphenyldimethoxysilane.
Still further preferably, the vinyl-containing polysiloxane is a copolymer composed of a structural unit provided by phenyltrimethoxysilane, a structural unit provided by methyltrimethoxysilane and a structural unit provided by vinyltrimethoxysilane (for example, the molar ratio of the three is 5-7:1-3:1), or the vinyl-containing polysiloxane is a copolymer composed of a structural unit provided by phenyltrimethoxysilane, a structural unit provided by methyltrimethoxysilane, a structural unit provided by dimethyldimethoxysilane and a structural unit provided by vinyltrimethoxysilane (for example, the molar ratio of the four is 1-4:1-3:1-2: 1).
Preferably, the vinyl group-containing polysiloxane is solid at room temperature.
In the present invention, the high-reflectance filler means a filler having a reflectance of between 95% and 100%.
In the method of the present invention, the high-reflectivity filler may be one or more of titanium dioxide, barium sulfate, antimony oxide, zinc sulfide, and zinc oxide, preferably at least one of titanium dioxide, barium sulfate, and antimony oxide, and more preferably titanium dioxide. In the most preferred embodiment, the high reflectance filler is selected from the group consisting of rutile titanium dioxide, and more preferably has an average particle size of 0.5 to 1 μm.
In the present invention, the high thermal conductive filler means a thermal conductive filler having a thermal conductivity of 10W/mK or more (for example, 10 to 350W/mK).
In the present invention, the high thermal conductive filler may be one or more of alumina, silicon carbide, silicon nitride, boron nitride, aluminum nitride, graphene, and carbon nanotubes, preferably at least one of alumina, boron nitride, and aluminum nitride, and more preferably boron nitride.
Preferably, in a particular embodiment, the alumina is spherical in shape.
In the present invention, the solid filler may be one or more of silica powder, magnesium hydroxide, aluminum hydroxide, calcium carbonate and fumed silica, preferably at least one of silica powder and fumed silica, more preferably silica powder.
In the present invention, the initiator may be one or more of cyclohexanone peroxide, dibenzoyl peroxide, t-butyl hydroperoxide, azobisisobutyronitrile and azobisisoheptonitrile, preferably at least one of cyclohexanone peroxide and azobisisobutyronitrile.
In the present invention, the release agent may be one or more of carnauba wax, polyethylene wax, oxidized polyethylene wax, fischer-tropsch wax, polypropylene wax, and fatty acid wax, and preferably at least one of polypropylene wax and fatty acid wax.
In the invention, the stress modifier can be one or more of polyether modified organic silicon oil, organic silicon modified epoxy resin, liquid carboxyl-terminated butadiene-acrylonitrile rubber and triblock copolymer containing organic silicon components, and preferably polyether modified organic silicon oil.
In the present invention, the adhesion promoter may be an organic silicon compound containing an epoxy group; preferably, the adhesion promoter has at least one of the structures represented by formula (1) and formula (2);
Figure BDA0002157896070000061
in a second aspect, the present invention provides a method for preparing the solid silicone composite, comprising the steps of:
(1) mixing polysiloxane containing vinyl, high-reflection filler, high-thermal-conductivity filler, solid filler, initiator, release agent, stress modifier and adhesion promoter, and then dispersing for multiple times;
(2) and (2) mixing the mixture dispersed in the step (1) on an open mill.
In the method of the present invention, the vinyl-containing polysiloxane is prepared in a manner conventional in the art, and specifically, in a preferred embodiment, is prepared according to the following steps: uniformly mixing phenyl trimethoxy silane, methyl trimethoxy silane, vinyl trimethoxy silane and xylene, and then dropwise adding an HCl solution; then raising the reaction temperature to 70 ℃ for reaction for 4h, raising the reaction temperature to 90 ℃ for fractionation, evaporating the generated by-product, and stopping fractionation when the temperature of a distillation head reaches 80 ℃; after supplementing xylene and NaOH, raising the reaction temperature to 110 ℃ for fractional distillation, distilling off the generated by-products, and stopping fractional distillation when the temperature of a distillation head reaches 100 ℃. Washing the product with water, separating to remove low-boiling-point substances, and obtaining the polysiloxane containing vinyl.
The third aspect of the invention provides the application of the solid silicone compound as an LED bracket packaging material.
The present invention will be described in detail by way of examples, but the scope of the present invention is not limited thereto.
In the following examples, the rutile type titanium dioxide was obtained from Shanghai Hughai titanium white chemical Co., Ltd, and had an average particle size of 0.8 μm;
spherical alumina was purchased from Jiangsu alli New materials GmbH, No. NA 1450;
the silicon dioxide powder is purchased from Jiangsu alli Rui New Material Co., Ltd, and is of a mark DQ 1200;
azobisisobutyronitrile, benzoyl peroxide and tert-butyl hydroperoxide are all available from Shanghai Michelin Biotech, Inc.;
the polyether modified silicone oil is purchased from Dow Corning company under the trade name SF 8421;
polyethylene wax was purchased from clariant corporation under the designation PE 520;
spherical aluminum nitride was purchased from Dalian Miao materials science and technology Limited, under the designation SFS.
Example 1
a) Preparation of vinyl-containing polysiloxane V1:
0.6mol of phenyltrimethoxysilane, 0.2mol of methyltrimethoxysilane, 0.1mol of vinyltrimethoxysilane and 2mol of xylene are put into a three-neck flask and stirred uniformly, then 0.05L of 1 percent HCl solution is dripped at 0 ℃, and the dripping is finished within 2 hours; then the reaction temperature is raised to 70 ℃ and reacted for 4h at the temperature; the reaction temperature is increased to 90 ℃ for fractional distillation, the generated by-product is distilled out, and when the temperature of the distillation head reaches 80 ℃, the fractional distillation is stopped. After 1mol of xylene and 0.001mol of NaOH are added, the reaction temperature is raised to 110 ℃ for fractional distillation, the generated by-product is distilled out, and when the temperature of the distillation head reaches 100 ℃, the fractional distillation is stopped. Washing the product with water, separating and removing low-boiling-point substances to obtain the vinyl-containing polysiloxane V1.
b) Preparation of solid silicone composite a 1:
the method comprises the following steps: 80g of the V1 resin, 30g of rutile titanium dioxide, 190g of spherical alumina, 190g of silicon dioxide powder, 1.6g of azodiisobutyronitrile and 1g of polyether modified silicone oil are accurately weighed, 2g of the adhesion promoter shown in the formula (I) and 0.5g of polyethylene wax are added. Mixing the materials in a ball mill, pre-dispersing for 30 minutes, transferring the materials to an open mill with the roller temperature of 90 ℃, mixing and grinding for 5 minutes, taking down and naturally cooling to obtain a solid silicon resin compound A1, bagging, and storing at 0-5 ℃ for later use.
Figure BDA0002157896070000081
Example 2
a) Preparation of vinyl-containing polysiloxane V2:
0.5mol of phenyltrimethoxysilane, 0.3mol of methyltrimethoxysilane, 0.15mol of vinyltrimethoxysilane, 0.15mol of dimethyldimethoxysilane and 2mol of xylene are put into a three-neck flask and stirred uniformly, and then 0.1L of 1 percent HCl solution is dripped at the temperature of 0 ℃, and the dripping is finished within 2 hours; then the reaction temperature is raised to 70 ℃ and reacted for 4h at the temperature; the reaction temperature is increased to 90 ℃ for fractional distillation, the generated by-product is distilled out, and when the temperature of the distillation head reaches 80 ℃, the fractional distillation is stopped. After 1mol of xylene and 0.001mol of NaOH are added, the reaction temperature is raised to 110 ℃ for fractional distillation, the generated by-product is distilled out, and when the temperature of the distillation head reaches 100 ℃, the fractional distillation is stopped. Washing the product with water, separating and removing low-boiling-point substances to obtain the vinyl-containing polysiloxane V2.
b) Preparation of solid silicone resin compound:
the method comprises the following steps: 80g of the V2 resin, 30g of rutile titanium dioxide, 210g of spherical alumina, 200g of silicon dioxide powder, 1.6g of benzoyl peroxide and 1g of polyether modified silicone oil are accurately weighed, 2g of an adhesion promoter shown in the formula (II) and 0.5g of polyethylene wax are added. Mixing the materials in a ball mill, pre-dispersing for 30 minutes, transferring the materials to an open mill with the roller temperature of 90 ℃, mixing and grinding for 5 minutes, taking down and naturally cooling to obtain a solid silicon resin compound A2, bagging, and storing at 0-5 ℃ for later use.
Example 3
a) Preparation of vinyl-containing polysiloxane V3:
0.25mol of phenyltrimethoxysilane, 0.5mol of methyltrimethoxysilane, 0.25mol of vinyltrimethoxysilane, 0.25mol of dimethyldimethoxysilane and 2mol of xylene are put into a three-neck flask and stirred uniformly, and then 0.15L of 1 percent HCl solution is dripped at 0 ℃, and the dripping is finished within 2 hours; then the reaction temperature is raised to 70 ℃ and reacted for 4h at the temperature; the reaction temperature is increased to 90 ℃ for fractional distillation, the generated by-product is distilled out, and when the temperature of the distillation head reaches 80 ℃, the fractional distillation is stopped. After 1mol of xylene and 0.001mol of NaOH are added, the reaction temperature is raised to 110 ℃ for fractional distillation, the generated by-product is distilled out, and when the temperature of the distillation head reaches 100 ℃, the fractional distillation is stopped. Washing the product with water, separating and removing low-boiling-point substances to obtain the vinyl-containing polysiloxane V3.
b) Preparation of solid silicone resin compound:
the method comprises the following steps: 80g of the V3 resin, 30g of rutile titanium dioxide, 210g of spherical aluminum nitride, 200g of silicon dioxide powder, 1.6g of tert-butyl hydroperoxide and 1g of polyether modified silicone oil are accurately weighed, 2g of the adhesion promoter shown in the formula (I) and 0.5g of polyethylene wax are added. Pre-dispersing the materials in a ball mill for 30 minutes, then transferring the materials to an open mill with the roller temperature of 90 ℃, mixing and grinding the materials for 5 minutes, taking down the materials and naturally cooling the materials to obtain a solid silicone resin compound A3, bagging the solid silicone resin compound A3, and storing the solid silicone resin compound A3 at the temperature of 0-5 ℃ for later use.
Example 4
A solid silicone resin composite was prepared according to the method of example 1, except that the spherical alumina was replaced with spherical aluminum nitride of the same weight, thereby obtaining a solid silicone resin composite A4.
Example 5
A solid silicone resin composite was prepared according to the method of example 2, except that the spherical alumina was replaced with spherical aluminum nitride of the same weight, thereby preparing a solid silicone resin composite A5.
Example 6
A solid silicone resin composite was prepared according to the method of example 3, except that the weight of the rutile type titanium dioxide was changed from 30g to 60g, thereby obtaining a solid silicone resin composite A6.
Comparative example 1
A white epoxy molding compound, available from Hitachi chemical Co., Ltd., under the trade name CEL-W-7005, was D1.
Comparative example 2
A solid silicone resin composite was prepared according to the method of example 1, except that the amount of V1 resin was changed to 40g, thereby obtaining a solid silicone resin composite D2.
Test example
The solid silicone resin composites A1-A6 and D1-D2 prepared in the examples and comparative examples were tested for their respective properties as follows.
(1) Glass transition temperature the test was carried out using a thermomechanical analyzer (TMA).
(2) Gel time: heating an electric heating plate to 175 +/-1 ℃, placing 2-3 g of sample on an iron plate, continuously stirring by using a small needle, and testing the time for the sample to change from fluid to colloid.
(3) Fluidity: a20 g sample was taken and measured by means of a spiral flow metal mold with a resin transfer injection molding machine at an injection pressure of 70kgf/cm2 and a mold temperature of 175. + -. 1 ℃.
(4) Coefficient of thermal conductivity: the method is carried out according to the GB/T10294 standard by adopting a steady-state method.
(5) Initial reflectance measurement: transferring and injecting the prepared solid silicone resin into a specific mould by using a mould press under the process conditions of mould temperature of 175 ℃ and curing time of 240s, and curing and forming the solid silicone resin into a sheet with the thickness of 1 mm; after curing the sheet at 150 ℃ for 4 hours, the reflectance at a wavelength of 550nm was measured using an integrating sphere spectrophotometer V770;
(6) reflectance after aging: the sheet in test example (5) was subjected to reflow soldering at 265 ℃ for 3 times (260 ℃ C. or more for 10 seconds), and the reflectance at a wavelength of 550nm was again measured.
The test results are shown in Table 1.
TABLE 1
Figure BDA0002157896070000111
As can be seen from the results in table 1, the thermal conductivity, initial reflectance, and reflectance after aging of the examples of the present invention are all significantly higher than those of the comparative examples, resulting in better results.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.

Claims (10)

1. A solid silicone resin composite comprising 10 to 25 wt% of a vinyl group-containing polysiloxane, 2 to 15 wt% of a high-reflectance filler, 25 to 45 wt% of a high-thermal-conductive filler, 25 to 45 wt% of a solid filler, 0.01 to 2 wt% of an initiator, 0.01 to 3 wt% of a mold release agent, 0.001 to 1 wt% of a stress modifier, and 0.1 to 2 wt% of an adhesion promoter.
2. The solid silicone composite of claim 1, wherein said vinyl-containing polysiloxane comprises CH2=CHSiO3/2Unit, CH2=CHCH3CH3SiO1/2Unit, C6H6SiO3/2Unit, CH3SiO3/2Unit (C)6H6)2SiO2/2Unit, (CH)3)2SiO2/2Unit and C6H6CH3SiO2/2At least one of the units;
preferably, the vinyl group-containing polysiloxane contains a structural unit provided by vinyltrimethoxysilane and/or a structural unit provided by tetramethyldivinyldisiloxane and at least one selected from the group consisting of a structural unit provided by phenyltrimethoxysilane, a structural unit provided by methyltrimethoxysilane, a structural unit provided by diphenyldimethoxysilane, a structural unit provided by dimethyldimethoxysilane and a structural unit provided by methylphenyldimethoxysilane;
preferably, the vinyl group-containing polysiloxane is solid at room temperature.
3. The solid silicone composite of claim 1, wherein the high reflectance filler is selected from one or more of titanium dioxide, barium sulfate, antimony oxide, zinc sulfide, and zinc oxide;
the high-thermal-conductivity filler is selected from one or more of alumina, silicon carbide, silicon nitride, boron nitride, aluminum nitride, graphene and carbon nanotubes.
4. The solid silicone composite according to claim 1, wherein the solid filler is selected from one or more of silica powder, magnesium hydroxide, aluminum hydroxide, calcium carbonate and fumed silica.
5. The solid silicone composite of claim 1, wherein said initiator is selected from one or more of cyclohexanone peroxide, dibenzoyl peroxide, t-butyl hydroperoxide, azobisisobutyronitrile, and azobisisoheptonitrile.
6. The solid silicone composite of claim 1, wherein the release agent is selected from one or more of carnauba wax, polyethylene wax, oxidized polyethylene wax, Fischer-Tropsch wax, polypropylene wax, and fatty acid wax.
7. The solid silicone composite according to claim 1, wherein the stress modifier is selected from one or more of polyether modified silicone oils, silicone modified epoxy resins, liquid carboxyl terminated nitrile rubbers and triblock copolymers containing silicone components.
8. The solid silicone composite according to any one of claim 1, wherein the adhesion promoter is an organosilicon compound containing epoxy groups;
preferably, the adhesion promoter has at least one of the structures represented by formula (1) and formula (2);
Figure FDA0002157896060000021
9. a method of preparing a solid silicone composite according to any one of claims 1 to 8, comprising the steps of:
(1) mixing polysiloxane containing vinyl, high-reflection filler, high-thermal-conductivity filler, solid filler, initiator, release agent, stress modifier and adhesion promoter, and then dispersing for multiple times;
(2) and (2) mixing the mixture dispersed in the step (1) on an open mill.
10. Use of the solid silicone composite according to any one of claims 1 to 8 or prepared according to the method of claim 9 as LED-rack encapsulating material.
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