CN109627473B - Preparation process of enhanced organic silicon composite sheet with surface tack removal function - Google Patents
Preparation process of enhanced organic silicon composite sheet with surface tack removal function Download PDFInfo
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- C08J2383/00—Characterised by the use 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; Derivatives of such polymers
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- C08J2483/00—Characterised by the use 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; Derivatives of such polymers
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Abstract
The invention discloses a preparation process of a reinforced organic silicon composite sheet with a surface subjected to viscosity removal, which comprises the following steps: mixing the components of the silicone rubber composition a, calendering and curing to obtain a silica gel layer matrix, mixing the components of the silicone rubber composition b, calendering and curing to obtain a high-hardness tack-free silica gel layer, directly compounding the high-hardness tack-free silica gel layer with the silica gel layer matrix, or compounding the silicone rubber composition b on the silica gel layer matrix, heating and cooling to obtain the reinforced silicone composite sheet with the tack-free surface. According to the invention, the silicon gel layer matrix and the high-hardness viscosity-removed silicon gel layer are compounded through a hydrosilylation reaction, so that the product has a firm and reliable joint surface, low hardness, extremely low surface viscosity, high surface hardness and strength, scratch resistance and friction resistance, meets the requirements on the mechanical property and reliability of an interface material in practical application, is beneficial to improving the comprehensive performance, and has a simple preparation process and a wide application prospect.
Description
Technical Field
The invention relates to the technical field of organic silicon materials, in particular to a preparation process of an enhanced organic silicon composite sheet with a surface subjected to viscidity removal.
Background
The organic silicon composite sheet is used as a main heat conduction material variety of an organic silicon heat conduction interface material, is applied between a heating part and a radiating part of electrical equipment, plays the functions of heat conduction, shock absorption, sealing and insulation, has the excellent characteristics of high and low temperature resistance, electrical insulation, oxidation resistance stability, weather resistance, flame retardancy, corrosion resistance and the like, and is widely applied to the fields of electronic wear, power supplies and communication. The organosilicon composite sheet material of low rigidity is very soft and has good interface adherence, and the general surface has special natural viscidity simultaneously, because its two sides have the similar viscidity of size simultaneously for the compound sheet material of large-scale robot is difficult for separating with the robot hand at automatic dress in-process organosilicon, easily produces the error when the large scale robot pastes the dress, and the difficult removal adjustment after pasting the dress, has leaded to the assembly efficiency low, and its surface is soft fragile, makes its surface appear dirty and mar easily. In the prior art, the overall hardness of the silica gel layer matrix is generally improved, or a layer of insulating sheet or double-sided adhesive is adhered to the surface of the silica gel layer matrix to change the viscosity difference of the surface of the organic silicon composite sheet.
Disclosure of Invention
In order to overcome the technical problem, the invention discloses a preparation process of a reinforced organic silicon composite sheet with a surface subjected to tack removal.
The technical scheme adopted by the invention for realizing the purpose is as follows:
a preparation process of a reinforced organic silicon composite sheet with a surface being tack-free comprises the following steps:
step 1, mixing the components of the silicone rubber composition a, and then calendering and curing to obtain a silicone rubber layer matrix;
step 2, mixing the components of the silicone rubber composition b, and then calendaring and curing to obtain a high-hardness viscosity-removed silicone rubber layer;
and 3, directly compounding the high-hardness de-adhesion silica gel layer and the silica gel layer matrix, or compounding the silicone rubber composition b on the silica gel layer matrix, heating, and cooling to obtain the enhanced organic silicon composite sheet with the de-adhesion surface.
The process for preparing the enhanced silicone composite sheet with the tack-removed surface, wherein in the steps 1 and 2, the curing conditions are as follows: the temperature is 40-150 ℃, and the reaction time is 10-30 min.
The preparation process of the reinforced silicone composite sheet with the tack removed surface, wherein in step 3, the heating conditions are as follows: the temperature is 60-100 ℃, and the reaction time is 10-30 min.
The preparation process of the reinforced silicone composite sheet with the surface being tack-free is characterized in that in step 3, the compounding step comprises: when the viscosity of the silicone rubber composition b is high, namely the viscosity of the silicone rubber composition b is greater than 100000mPa · s, diluting the silicone rubber composition b with a solvent to obtain a treatment composition, compounding the treatment composition on the surface to be bonded of the silica gel layer matrix, drying to remove the solvent, and heating and curing to obtain the enhanced organic silicon composite sheet with the surface removed with viscosity, wherein the high-hardness removed with viscosity silica gel layer is firmly bonded with the silica gel layer matrix and has a thin and uniform thickness, preferably, the enhanced organic silicon composite sheet with the surface removed with viscosity has a thickness of 0-0.3 mm.
The preparation process of the enhanced organosilicon composite sheet with the tack-free surface comprises the following steps of dissolving the organic silicon composite sheet in a solvent, wherein the solvent is one or more of low-molecular-weight methyl silicone oil, toluene, isopropanol, carbon tetrachloride and ethyl acetate.
The preparation process of the reinforced silicone composite sheet with the surface being tack-free is characterized in that the reinforced silicone composite sheet is compounded in any one of coating, molding, rolling and casting.
In the preparation process of the enhanced silicone composite sheet with the de-sticky surface, the joint surface of the silica gel layer matrix and the high-hardness de-sticky silica gel layer contains a treating agent, and the treating agent is hydrogen-containing organopolysiloxane.
The preparation process of the enhanced organosilicon composite sheet with the tack-free surface comprises the following steps of (1) preparing a hydrogen-containing organopolysiloxane, wherein the hydrogen content of the hydrogen-containing organopolysiloxane is 0.01-1% by mass, the viscosity at 25 ℃ is 10-500 mPa · s, the hydrogen-containing organopolysiloxane is an organopolysiloxane containing two or more silicon-bonded hydrogen groups, the positions of the silicon-bonded hydrogen groups can be on a side chain, a molecular terminal or both the molecular terminal and the side chain, and preferably the positions of the silicon-bonded hydrogen groups are on the molecular terminal or both the molecular terminal and the side chain and contain at least two silicon-bonded hydrogen groups.
Preferably, the hydrogen-containing organopolysiloxane is one or more of trimethylsiloxy-terminated polymethylhydrosiloxane, trimethylsiloxy-terminated copolymer of methylhydrogensiloxane and dimethylsiloxane, dimethylhydrosiloxy-terminated copolymer of methylhydrogensiloxane and methylphenylsiloxane, dimethylhydrosiloxy-terminated copolymer of methylhydrogensiloxane and dimethylsiloxane, dimethylhydrosiloxy-terminated polydimethylsiloxane, trimethylsiloxy-terminated copolymer of methylhydrogensiloxane and methylphenylsiloxane, trimethylsiloxy-terminated copolymer of methylhydrogensiloxane and methyl (3, 3, 3-trifluoropropyl) siloxane, cyclic methylhydrogensiloxane or tetra (dimethylhydrosiloxy) silane.
In the preparation process of the reinforced silicone composite sheet with the tack removed surface, in step 1, the silicone rubber composition a consists of the following components in parts by weight:
preferably, the silicone rubber composition a consists of the following components in parts by weight:
according to the preparation process of the enhanced organosilicon composite sheet with the surface being tack-free, the Shore 00 hardness value of the silica gel layer matrix is 5-60, and the Shore 00 hardness of the silica gel layer matrix is tested according to the standard ASTM D2240.
In the silicone rubber composition a, the ratio of the molar weight of the hydrogen groups in the crosslinking agent to the molar weight of the vinyl groups in the vinyl-containing organopolysiloxane is 0.2 to 0.8: 1.
in the above process for preparing the reinforced silicone composite sheet with the tack-free surface, in step 2, the silicone rubber composition b comprises the following components in parts by weight:
preferably, the silicone rubber composition b consists of the following components in parts by weight:
in the above-described process for producing a surface-detackified reinforced silicone composite sheet, in the silicone rubber composition b, the ratio of the molar amount of hydrogen groups in the hydrogen group-containing silicone polysiloxane to the molar amount of vinyl groups in the vinyl group-containing silicone polysiloxane is greater than 1: 1.
in the silicone rubber composition b, the hydrogen content of the hydrogen-containing silicone polysiloxane is 0.01-0.3% by mass, and the viscosity at 25 ℃ is 10-1000 mPa · s.
The preparation process of the enhanced silicone composite sheet with the surface being tack-free is characterized in that the hardness value of the high-hardness tack-free silica gel layer ranges from shore 0061 to shore a 50, and the shore 00 hardness and shore a of the high-hardness tack-free silica gel layer are tested according to the standard ASTM D2240.
In the preparation process of the enhanced organic silicon composite sheet with the tack removed from the surface, the vinyl-containing organic polysiloxane is an organic polysiloxane of which the molecule contains two or more vinyl groups connected with silicon, the positions of the vinyl groups can be side groups or are positioned on the molecular terminal and the side chains at the same time, preferably, the vinyl-containing organic polysiloxane has the vinyl content of 0.03-5% by mass and the viscosity at 25 ℃ of 50-50000 mPas.
In the preparation process of the reinforced silicone composite sheet with the tack removed on the surface, the organopolysiloxane containing vinyl groups is one or more of α, omega-divinyl polydimethylsiloxane, methylphenyl vinyl siloxane terminated polydimethylsiloxane, dimethyl vinyl siloxane terminated polymethylphenylsiloxane and a copolymer of dimethyl vinyl siloxane terminated methylphenylsiloxane and dimethylsiloxane.
In the preparation process of the enhanced organosilicon composite sheet with the tack-free surface, the crosslinking agent is hydrogen-containing organopolysiloxane, the molecule of the organopolysiloxane has at least three silicon-hydrogen bonds, and the positions of the silicon-hydrogen bonds can be side groups or can be positioned on the molecular terminal and the side chain simultaneously, and are preferably positioned on the side chain. The crosslinking agent has a hydrogen content of 0.01 to 0.3% by mass and a viscosity of 10 to 1000 mPas, more preferably 30 to 300 mPas, at 25 ℃.
In the preparation process of the enhanced silicone composite sheet with the tack removed on the surface, the crosslinking agent is one or more of trimethylsiloxy terminated polymethylhydrosiloxane, trimethylsiloxy terminated copolymer of methylhydrosiloxane and dimethylsiloxane, dimethylhydrosiloxy terminated copolymer of methylhydrosiloxane and methylphenylsiloxane, and dimethylhydrosiloxy terminated copolymer of methylhydrosiloxane and dimethylsiloxane.
The preparation process of the reinforced silicone composite sheet with the tack removed surface includes that the filler includes a heat conductive filler, an extender filler, and a pigment filler, the type of the filler is determined according to specific needs, more preferably, the filler includes the heat conductive filler, the heat conductive filler is one or more of magnesium oxide, aluminum oxide, iron oxide, calcium oxide, titanium oxide, silicon dioxide, aluminum nitride, boron nitride, and silicon nitride, and the particle size of the heat conductive filler is not particularly limited.
In the preparation process of the enhanced organosilicon composite sheet with the surface being tack-free, the platinum catalyst is one or more of platinum micro powder, platinum black, chloroplatinic acid, platinum tetrachloride, platinum complex of olefin, platinum complex of carbonyl or thermoplastic organic resin powder containing the platinum group catalyst, and preferably platinum catalyst or chloroplatinic acid.
It is to be noted that the viscosity at 25 ℃ is the dynamic viscosity value of the material at 25 ℃.
The invention has the beneficial effects that: according to the invention, the silicon gel layer matrix and the high-hardness de-adhesive silicon gel layer are compounded through a hydrosilylation reaction, the joint surface of the product is firm and reliable, the hardness is lower, the surface viscosity is extremely low, the surface hardness and the strength are high, the scratch resistance and the friction resistance are realized, the requirements on the mechanical property and the reliability of the interface material in practical application are met, the improvement on the comprehensive performance is facilitated, the preparation process is simple, and the application prospect is wide.
Detailed Description
The preparation process of the enhanced silicone composite sheet with the tack-free surface provided by the embodiment comprises the following steps:
step 1, mixing the components of the silicone rubber composition a, and then calendering and curing to obtain a silicone rubber layer matrix;
step 2, mixing the components of the silicone rubber composition b, and then calendaring and curing to obtain a high-hardness de-adhesion silicone rubber layer;
and 3, directly compounding the high-hardness de-adhesion silica gel layer and the silica gel layer matrix, or compounding the silicone rubber composition b on the silica gel layer matrix, heating, and cooling to obtain the enhanced silicone composite sheet with the de-adhesion surface.
The process for preparing the enhanced silicone composite sheet with the tack-removed surface, wherein in the steps 1 and 2, the curing conditions are as follows: the temperature is 40-150 ℃, and the reaction time is 10-30 min.
The preparation process of the reinforced silicone composite sheet with the tack removed surface, wherein in step 3, the heating conditions are as follows: the temperature is 60-100 ℃, and the reaction time is 10-30 min.
The preparation process of the reinforced silicone composite sheet with the surface being tack-free is characterized in that in step 3, the compounding step comprises: when the viscosity of the silicone rubber composition b is high, namely the viscosity of the silicone rubber composition b is greater than 100000mPa · s, diluting the silicone rubber composition b with a solvent to obtain a treatment composition, compounding the treatment composition on the surface to be bonded of the silica gel layer matrix, drying to remove the solvent, and heating and curing to obtain the enhanced organic silicon composite sheet with the surface removed with viscosity, wherein the high-hardness removed with viscosity silica gel layer is firmly bonded with the silica gel layer matrix and has a thin and uniform thickness, preferably, the enhanced organic silicon composite sheet with the surface removed with viscosity has a thickness of 0-0.3 mm.
The preparation process of the enhanced organosilicon composite sheet with the tack-free surface comprises the following steps of dissolving the organic silicon composite sheet in a solvent, wherein the solvent is one or more of low-molecular-weight methyl silicone oil, toluene, isopropanol, carbon tetrachloride and ethyl acetate.
The preparation process of the reinforced silicone composite sheet with the surface being tack-free is characterized in that the reinforced silicone composite sheet is compounded in any one of coating, molding, rolling and casting.
In the preparation process of the enhanced silicone composite sheet with the de-sticky surface, the joint surface of the silica gel layer matrix and the high-hardness de-sticky silica gel layer contains a treating agent, and the treating agent is hydrogen-containing organopolysiloxane.
The preparation process of the enhanced organosilicon composite sheet with the tack-free surface comprises the following steps of (1) preparing a hydrogen-containing organopolysiloxane, wherein the hydrogen content of the hydrogen-containing organopolysiloxane is 0.01-1% by mass, the viscosity at 25 ℃ is 10-500 mPa · s, the hydrogen-containing organopolysiloxane is an organopolysiloxane containing two or more silicon-bonded hydrogen groups, the positions of the silicon-bonded hydrogen groups can be on a side chain, a molecular terminal or both the molecular terminal and the side chain, and preferably the positions of the silicon-bonded hydrogen groups are on the molecular terminal or both the molecular terminal and the side chain and contain at least two silicon-bonded hydrogen groups.
Preferably, the hydrogen-containing organopolysiloxane is one or more of trimethylsiloxy-terminated polymethylhydrosiloxane, trimethylsiloxy-terminated copolymer of methylhydrogensiloxane and dimethylsiloxane, dimethylhydrosiloxy-terminated copolymer of methylhydrogensiloxane and methylphenylsiloxane, dimethylhydrosiloxy-terminated copolymer of methylhydrogensiloxane and dimethylsiloxane, dimethylhydrosiloxy-terminated polydimethylsiloxane, trimethylsiloxy-terminated copolymer of methylhydrogensiloxane and methylphenylsiloxane, trimethylsiloxy-terminated copolymer of methylhydrogensiloxane and methyl (3, 3, 3-trifluoropropyl) siloxane, cyclic methylhydrogensiloxane or tetra (dimethylhydrosiloxy) silane.
In the preparation process of the reinforced silicone composite sheet with the tack removed surface, in step 1, the silicone rubber composition a consists of the following components in parts by weight:
preferably, the silicone rubber composition a consists of the following components in parts by weight:
according to the preparation process of the enhanced organosilicon composite sheet with the surface being tack-free, the Shore 00 hardness value of the silica gel layer matrix is 5-60, and the Shore 00 hardness of the silica gel layer matrix is tested according to the standard ASTM D2240.
In the silicone rubber composition a, the ratio of the molar weight of the hydrogen groups in the crosslinking agent to the molar weight of the vinyl groups in the vinyl-containing organopolysiloxane is 0.2 to 0.8: 1.
in the above process for preparing the reinforced silicone composite sheet with the tack-free surface, in step 2, the silicone rubber composition b comprises the following components in parts by weight:
preferably, the silicone rubber composition b consists of the following components in parts by weight:
in the above-described process for producing a surface-detackified reinforced silicone composite sheet, in the silicone rubber composition b, the ratio of the molar amount of hydrogen groups in the hydrogen group-containing silicone polysiloxane to the molar amount of vinyl groups in the vinyl group-containing silicone polysiloxane is greater than 1: 1.
in the silicone rubber composition b, the hydrogen content of the hydrogen-containing silicone polysiloxane is 0.01-0.3% by mass, and the viscosity at 25 ℃ is 10-1000 mPa · s.
The preparation process of the enhanced silicone composite sheet with the surface being tack-free is characterized in that the hardness value of the high-hardness tack-free silica gel layer ranges from shore 0061 to shore a 50, and the shore 00 hardness and shore a of the high-hardness tack-free silica gel layer are tested according to the standard ASTM D2240.
In the preparation process of the enhanced organic silicon composite sheet with the tack removed from the surface, the vinyl-containing organic polysiloxane is an organic polysiloxane of which the molecule contains two or more vinyl groups connected with silicon, the positions of the vinyl groups can be side groups or are positioned on the molecular terminal and the side chains at the same time, preferably, the vinyl-containing organic polysiloxane has the vinyl content of 0.03-5% by mass and the viscosity at 25 ℃ of 50-50000 mPas.
In the preparation process of the reinforced silicone composite sheet with the tack removed on the surface, the organopolysiloxane containing vinyl groups is one or more of α, omega-divinyl polydimethylsiloxane, methylphenyl vinyl siloxane terminated polydimethylsiloxane, dimethyl vinyl siloxane terminated polymethylphenylsiloxane and a copolymer of dimethyl vinyl siloxane terminated methylphenylsiloxane and dimethylsiloxane.
In the preparation process of the enhanced organosilicon composite sheet with the tack-free surface, the crosslinking agent is hydrogen-containing organopolysiloxane, the molecule of the organopolysiloxane has at least three silicon-hydrogen bonds, and the positions of the silicon-hydrogen bonds can be side groups or can be positioned on the molecular terminal and the side chain simultaneously, and are preferably positioned on the side chain. The crosslinking agent has a hydrogen content of 0.01 to 0.3% by mass and a viscosity of 10 to 1000 mPas, more preferably 30 to 300 mPas, at 25 ℃.
In the preparation process of the enhanced silicone composite sheet with the tack removed on the surface, the crosslinking agent is one or more of trimethylsiloxy terminated polymethylhydrosiloxane, trimethylsiloxy terminated copolymer of methylhydrosiloxane and dimethylsiloxane, dimethylhydrosiloxy terminated copolymer of methylhydrosiloxane and methylphenylsiloxane, and dimethylhydrosiloxy terminated copolymer of methylhydrosiloxane and dimethylsiloxane.
The preparation process of the reinforced silicone composite sheet with the tack removed surface includes that the filler includes a heat conductive filler, an extender filler, and a pigment filler, the type of the filler is determined according to specific needs, more preferably, the filler includes the heat conductive filler, the heat conductive filler is one or more of magnesium oxide, aluminum oxide, iron oxide, calcium oxide, titanium oxide, silicon dioxide, aluminum nitride, boron nitride, and silicon nitride, and the particle size of the heat conductive filler is not particularly limited.
In the preparation process of the enhanced organosilicon composite sheet with the surface being tack-free, the platinum catalyst is one or more of platinum micro powder, platinum black, chloroplatinic acid, platinum tetrachloride, platinum complex of olefin, platinum complex of carbonyl or thermoplastic organic resin powder containing the platinum group catalyst, and preferably platinum catalyst or chloroplatinic acid.
It is to be noted that the viscosity at 25 ℃ is the dynamic viscosity value of the material at 25 ℃.
Specific examples of the process for preparing a reinforced silicone composite sheet with a tack-free surface according to the present invention are given below.
The amounts of the substances in the silica gel layer matrix and the high-hardness detackified silica gel layer used for preparing the enhanced silicone composite sheet with the surface detackified in examples 1 to 3 and the amount of the substance in the silicone rubber composition of the silica gel layer used for preparing the comparative sheet in comparative example 1 are shown in table 1, and the unit is mass fraction.
TABLE 1
Example 1
In this embodiment, in the silicone rubber composition a, the vinyl-containing organopolysiloxane is α, omega-divinyl polydimethylsiloxane, the viscosity is 100mPa · s at 25 ℃, the mass percentage content of vinyl is 2.0%, the heat-conducting filler is alumina with an average particle size of 30 μm, the crosslinking agent is methyl hydrogen-containing silicone oil, the viscosity is 100mPa · s at 25 ℃, the hydrogen content is 0.2% by mass, and the platinum catalyst is a platinum catalyst.
In the silicone rubber composition b, the vinyl-containing organopolysiloxane is α, omega-divinyl polydimethylsiloxane, the viscosity is 300mPa & s at 25 ℃, the mass percentage of vinyl is 2%, the heat-conducting filler is alumina with the average particle size of 20 mu m, the hydrogen-containing organopolysiloxane is methyl hydrogen-containing silicone oil, the viscosity is 400mPa & s at 25 ℃, the hydrogen content is 0.08% by mass, and the platinum catalyst is a platinum catalyst.
The preparation process of the enhanced organic silicon composite sheet with the surface removed with stickiness comprises the following steps:
A. fully and uniformly mixing the components contained in the silicone rubber composition a, then rolling and forming, curing at 80 ℃ for 20min, and cooling to room temperature to obtain a silica gel layer matrix;
B. and C, rolling a layer of uniform mixture of the silicon rubber composition b with the thickness of 0.2mm on the surface to be compounded of the silica gel layer matrix in the step A, heating to 50 ℃, and baking for 30min to obtain the reinforced silicone composite sheet with the surface tack free, wherein the thickness of the reinforced silicone composite sheet is 1.0mm, the Shore 00 hardness of the silica gel layer matrix is 58, and the Shore A hardness of the high-hardness tack free silica gel layer is 40.
Example 2
In this embodiment, in the silicone rubber composition a, the vinyl-containing organopolysiloxane is α, omega-divinyl polydimethylsiloxane, the viscosity is 40000mPa · s at 25 ℃, the mass percentage of vinyl is 0.2%, the heat-conducting filler is aluminum nitride with an average particle size of 20 μm, the crosslinking agent is methyl hydrogen-containing silicone oil, the viscosity is 1000mPa · s at 25 ℃, the hydrogen content is 0.03% by mass, and the platinum catalyst is a platinum catalyst.
In the silicone rubber composition b, the vinyl-containing organopolysiloxane is α, omega-divinyl polydimethylsiloxane, the viscosity is 300mPa & s at 25 ℃, the mass percentage of vinyl is 1%, the heat-conducting filler is aluminum nitride with the average particle size of 5 mu m, the hydrogen-containing organopolysiloxane is methyl hydrogen-containing silicone oil, the viscosity is 700mPa & s at 25 ℃, the hydrogen content is 0.06% by mass, and the platinum catalyst is platinum catalyst and 100 parts of toluene are added for dilution and uniform mixing.
The preparation process of the enhanced organic silicon composite sheet with the surface removed with stickiness comprises the following steps:
A. fully and uniformly mixing the components contained in the silicone rubber composition a, then rolling and forming, curing at 70 ℃ for 30min, and cooling to room temperature to obtain a silica gel layer matrix;
B. and D, blade-coating a layer of uniform mixture of the silicon rubber composition b with the thickness of 0.1mm on the surface to be compounded of the silica gel layer matrix in the step A by using a comma scraper, heating to 80 ℃, and baking for 10min to obtain the enhanced organic silicon composite sheet with the surface tack free, wherein the thickness of the enhanced organic silicon composite sheet is 1.0mm, the Shore 00 hardness of the silica gel layer matrix is 35, and the Shore A hardness of the high-hardness tack free silica gel layer is 10.
Example 3
In the embodiment, in the silicone rubber composition a, the vinyl-containing organopolysiloxane is α, omega-divinyl polydimethylsiloxane, the viscosity is 4000mPa · s at 25 ℃, the mass percentage of the vinyl is 0.5%, the heat-conducting filler is obtained by mixing alumina with the average particle size of 3 μm and alumina with the average particle size of 50 μm according to the mass ratio of 2: 3, the crosslinking agent is methyl hydrogen-containing silicone oil, the viscosity is 300mPa · s at 25 ℃, the hydrogen content is 0.07% by mass, and the platinum catalyst is a platinum catalyst.
In the silicone rubber composition b, the hydrogen-containing organosilicone polysiloxane is methyl hydrogen-containing silicone oil, the viscosity at 25 ℃ is 70mPa & s, the hydrogen content is 0.5% by mass fraction, and the platinum catalyst is a platinum catalyst.
The preparation process of the enhanced organic silicon composite sheet with the surface removed with stickiness comprises the following steps:
A. fully and uniformly mixing the components contained in the silicone rubber composition a, then rolling and forming, curing at 90 ℃ for 10min, and cooling to room temperature to obtain a silica gel layer matrix;
B. and B, rolling a layer of uniform mixture of the silicon rubber composition b with the thickness of 0.02mm on the surface to be compounded of the silica gel layer matrix in the step A, heating to 90 ℃, and baking for 5min to obtain the reinforced silicone composite sheet with the surface tack free, wherein the thickness of the reinforced silicone composite sheet is 1.0mm, the Shore 00 hardness of the silica gel layer matrix is 45, and the Shore 00 hardness of the high-hardness tack free silica gel layer is 75.
Example 4
In this embodiment, the silica gel layer substrate is TP120-H45-T10 from Auchuan science and technology Limited in Shenzhen, with a thickness of 1.0mm and a Shore 00 hardness of 45.
In the silicone rubber composition b, the hydrogen-containing organosilicone polysiloxane is methyl hydrogen-containing silicone oil, the viscosity at 25 ℃ is 70mPa & s, the hydrogen content is 0.5% by mass fraction, and the platinum catalyst is a platinum catalyst.
The preparation process of the enhanced organic silicon composite sheet with the surface removed with stickiness comprises the following steps:
and rolling a layer of uniform mixture of the silicone rubber composition b with the thickness of 0.02mm on the surface to be compounded of the silica gel layer matrix, heating to 90 ℃, and baking for 5min to obtain the enhanced silicone composite sheet with the surface tack free, wherein the thickness of the enhanced silicone composite sheet is 1.0mm, the Shore 00 hardness of the silica gel layer matrix is 45, and the Shore 00 hardness of the high-hardness tack free silica gel layer is 75.
Comparative examples
In the embodiment, in the silicone rubber composition a, the vinyl-containing organopolysiloxane is α, omega-divinyl polydimethylsiloxane, the viscosity is 4000mPa · s at 25 ℃, the mass percentage of the vinyl is 0.5%, the heat-conducting filler is obtained by mixing alumina with the average particle size of 3 μm and alumina with the average particle size of 50 μm according to the mass ratio of 2: 3, the crosslinking agent is methyl hydrogen-containing silicone oil, the viscosity is 300mPa · s at 25 ℃, the hydrogen content is 0.07% by mass, and the platinum catalyst is a platinum catalyst.
The preparation process of the comparative sheet was: mixing the components contained in the silicone rubber composition a, then rolling and molding, curing at 90 ℃ for 15min, and cooling to room temperature to obtain the silica gel layer contrast sheet, wherein the thickness of the silica gel layer matrix is 1.0mm, and the Shore 00 hardness is 45.
Test examples
The performance tests of the organic silicon composite sheets prepared in the embodiments 1 to 4 and the comparative example include a heat conduction coefficient and a heat resistance, and a tensile strength of the sheet, and the peel strength test method includes: the test is carried out according to GB/T2792-.
TABLE 2 sheet Property data
The data in table 2 show that the enhanced organosilicon composite sheet with the tack-free surface is obtained by compounding the silica gel layer matrix and the high-hardness tack-free silica gel layer, and the silica gel layer matrix and the high-hardness tack-free silica gel layer in the enhanced organosilicon composite sheet are combined through hydrosilylation, so that the enhanced organosilicon composite sheet is firm and reliable in combination surface, low in hardness, extremely low in surface tack, high in surface hardness and strength, resistant to scratch and friction, capable of meeting the requirements on mechanical properties and reliability of interface materials in practical application, beneficial to improvement of comprehensive properties, simple in preparation process and wide in application prospect.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner. Those skilled in the art can make many possible variations and modifications to the invention using the above disclosed technical means and teachings, or can modify equivalent embodiments with equivalent variations, without departing from the scope of the invention. Therefore, all equivalent changes made according to the shape, structure and principle of the present invention should be covered in the protection scope of the present invention without departing from the content of the technical scheme of the present invention.
Claims (7)
1. The preparation process of the organic silicon composite sheet is characterized by comprising the following steps of:
step 1, mixing the components of the silicone rubber composition a, and then calendering and curing to obtain a silicone rubber layer matrix;
step 2, rolling the silicon rubber composition b onto the silica gel layer substrate, heating, and cooling to obtain the organic silicon composite sheet;
the silicone rubber composition a comprises the following components in parts by weight:
the silicone rubber composition b comprises the following components in parts by weight:
the hydrogen content of the hydrogen-containing organosilicon polysiloxane is 0.01-0.3% by mass, and the viscosity at 25 ℃ is 10-1000 mPa & s; the vinyl-containing organopolysiloxane contains 0.03-5% by mass of vinyl and has a viscosity of 50-50000 mPas at 25 ℃; the crosslinking agent has a hydrogen content of 0.01-0.3% by mass and a viscosity of 10-1000 mPas at 25 ℃.
2. The process for producing the silicone composite sheet according to claim 1, characterized in that in step 1, the curing conditions are: the temperature is 40-150 ℃, and the reaction time is 10-30 min.
3. The process for producing the silicone composite sheet according to claim 1, characterized in that in step 2, the heating conditions are: the temperature is 60-100 ℃, and the reaction time is 10-30 min.
4. The process for preparing the silicone composite sheet according to claim 1, characterized in that in step 2, the step of calendering: when the viscosity of the silicone rubber composition b is higher, diluting the silicone rubber composition b with a solvent to obtain a treatment composition, compounding the treatment composition on the surface to be bonded of the silica gel layer matrix, drying to remove the solvent, and heating and curing to obtain the organic silicon composite sheet.
5. The process for preparing the silicone composite sheet according to claim 4, wherein the solvent is one or more of low molecular weight methyl silicone oil, toluene, isopropanol, carbon tetrachloride and ethyl acetate.
6. The process for producing the silicone composite sheet according to claim 1, characterized in that in the silicone rubber composition a, the ratio of the molar amount of hydrogen groups in the crosslinking agent to the molar amount of vinyl groups in the vinyl group-containing organopolysiloxane is 0.2 to 0.8: 1.
7. the process for producing the silicone composite sheet according to claim 1, characterized in that the ratio of the molar amount of hydrogen groups in the hydrogen group-containing silicone polysiloxane to the molar amount of vinyl groups in the vinyl group-containing silicone in the silicone rubber composition b is greater than 1: 1.
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