Disclosure of Invention
The present invention is directed to solving, at least in part, one of the technical problems in the related art. Therefore, the invention mainly aims to provide a silicone rubber self-adhesive tape and a preparation method thereof, and aims to solve the problems that the existing silicone rubber self-adhesive tape is short in storage life, poor in comprehensive performance and incapable of meeting the use requirements of the existing power equipment.
The purpose of the invention is realized by the following technical scheme:
the silicone rubber self-adhesive tape comprises the following raw materials in percentage by weight: 45-75 parts of base material, 3-10 parts of boron modified MQ silicon resin, 5-15 parts of alumina, 5-10 parts of hydrophobic white carbon black, 3-6 parts of nano montmorillonite, 5-15 parts of composite flame retardant, 3-5 parts of dibenzoyl peroxide, 2-5 parts of ethynyl cyclohexanol, 1-3 parts of vinyl silane-platinum complex and 1-2 parts of iron oxide red, wherein the base material comprises 35-55 parts of vinyl terminated methyl vinyl silicone rubber raw rubber with the mole fraction of vinyl chain segments of 0.03-0.05%, 5-10 parts of vinyl silicone oil with the mole fraction of hydroxyl terminated vinyl chain segments of 0.45-1.2% and the viscosity of 500-5000 mPa.s, and 5-10 parts of hydrogen-containing silicone oil with the hydrogen content of 0.5-0.12wt% and the viscosity of 100-500 mPa.s.
Preferably, wherein the boron modified MQ silicone resin is prepared by: adding 250g of xylene solution of methyl MQ silicon resin into a reactor, wherein the content of the methyl MQ silicon resin in the xylene solution of the methyl MQ silicon resin is 60wt%, then adding 42.5g of phenyl boric acid methanol solution with the content of 50wt% while stirring, heating to 70-90 ℃, reacting for 4-8 hours, and cooling to obtain the boric acid modified methyl MQ silicon resin.
Preferably, the nano montmorillonite is dioctadecyl intercalation modified montmorillonite.
Preferably, the alumina is spherical alumina, the spherical alumina comprises alumina with the particle size of 50-70 μm, alumina with the particle size of 15-30 μm and alumina with the particle size of 3-5 μm, and the mass ratio of the alumina with the particle size of 50-70 μm to the alumina with the particle size of 15-30 μm to the alumina with the particle size of 3-5 μm is (4-6): (3-5): (1-3).
Preferably, the specific surface area of the hydrophobic white carbon black is 250-380m 2 /g。
Preferably, the composite flame retardant comprises a phosphorus-fluorine-containing flame retardant and magnesium hydroxide, and the mass ratio of the phosphorus-fluorine-containing flame retardant to the magnesium hydroxide is (1-2): (3-5).
Preferably, wherein the phosphorus and fluorine containing flame retardant is prepared by the steps of: adding 3, 5-bis (trifluoromethyl) aniline, DOPO, paraformaldehyde and tetrahydrofuran into a reaction vessel, wherein the mass ratio of the 3, 5-bis (trifluoromethyl) aniline to the DOPO to the paraformaldehyde to the tetrahydrofuran is 1:6:10:56, carrying out reflux reaction for 8-72h at 40-120 ℃, cooling and standing to precipitate a solid, and separating the precipitated solid, namely the phosphorus-fluorine-containing flame retardant.
Preferably, wherein the vinylsilane-platinum complex is the reaction product of vinyltriethoxysilane and chloroplatinic acid at a concentration of 8000-20000ppm.
The preparation method of the silicone rubber self-adhesive tape comprises the following steps:
1) Preparing an alumina filler according to the formula requirement;
2) Adding the base material with the formula amount into a stirring kettle, uniformly stirring at the rotating speed of 40-60rpm, then sequentially adding the hydrophobic white carbon black, the nano montmorillonite, the composite flame retardant, the boron modified MQ silicon resin, the alumina and the iron oxide red in the step 1), adjusting the rotating speed to 50-120rpm, heating to 80-120 ℃, starting vacuum to remove bubbles and micromolecule substances, and maintaining at the rotating speed of 50-120rpm for 1.5-2 hours to uniformly mix the materials in the stirring kettle;
3) After the material obtained in the step 2) is cooled to room temperature, firstly adding the ethynyl cyclohexanol with the formula amount, uniformly stirring at the rotating speed of 40-80rpm, then sequentially adding the dibenzoyl peroxide and the vinyl silane-platinum complex with the formula amount, uniformly mixing at the rotating speed of 40-80rpm, and vacuumizing until bubbles in the material are completely pumped out to obtain a mixed rubber material;
4) Placing the mixed rubber material obtained in the step 3) on a calender for calendering, curing and molding, and then cutting to obtain the silicone rubber self-adhesive tape.
Preferably, step 4) further comprises the steps of firstly paving a base material on a conveying belt of a calender, then uniformly adding the mixed rubber obtained in step 3) to the starting end of the paved base material, and starting the calender to calender, cure and form.
Compared with the prior art, the invention has at least the following advantages:
1) According to the silicone rubber self-adhesive tape provided by the invention, basic physical properties can be ensured in a vulcanization process by adding hydrophobic white carbon black into raw vinyl silicone rubber containing low vinyl chain unit mole fraction; then, the vinyl silicone oil with specific vinyl chain link mole fraction and low viscosity and the hydrogen-containing silicone oil with specific hydrogen content and low viscosity are added into raw vinyl silicone rubber, so that the effective mixing of the rest heat-conducting filler, flame-retardant filler, reinforcing filler and the like into the base material can be effectively ensured, and further the comprehensive properties of the silicone rubber self-adhesive tape, such as flame retardance, heat conduction, insulation, mechanical strength and the like, can be ensured to meet the use requirements; the boron modified MQ silicon resin can be uniformly added in the production process due to the addition of the low-viscosity vinyl silicone oil and the hydrogen-containing silicone oil, and is uniformly mixed with the rest materials, so that the mechanical strength of the silicon rubber self-adhesive tape is effectively improved, the silicon rubber tape has better self-adhesiveness, the phenomenon that a tackifier (the boron modified MQ silicon resin) is not easy to separate out in the use process is effectively avoided or slowed down, the phenomena of moisture absorption and viscosity reduction are prevented, and the storage life of the silicon rubber self-adhesive tape is greatly prolonged.
2) The utility model provides a silicon rubber self-adhesion type sticky tape, through adopting different viscosity vinylsiloxane and hydrogen-containing silicone oil as the base stock, pack different particle diameters, the heat conduction filler of different shapes, including reasonable gradation, and pack compound fire retardant, its all the other components synergy with silicon rubber self-adhesion type sticky tape, mechanical strength has been guaranteed, on the insulating properties's basis, make its fire behaviour and heat conductivility accord with the operation requirement again, satisfy the demand of current power equipment to the silicon rubber self-adhesion type sticky tape that has excellent comprehensive properties.
Detailed Description
The present invention will be further described with reference to the following examples, which are illustrative only and not intended to be limiting, and the scope of the present invention is not limited thereby.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or upper and lower limit of preferred values, it is understood that any range by combining any pair of range upper limits or preferred values with any range lower limits or preferred values is expressly disclosed without regard to whether or not such range is expressly disclosed. Unless otherwise indicated, numerical range values set forth herein are intended to include the endpoints of the range, and all integers and fractions within the range.
All percentages, parts, ratios, etc. herein are by weight unless otherwise indicated.
The materials, methods, and examples herein are illustrative and, unless otherwise specified, are not to be construed as limiting, and non-illustrated materials may be obtained commercially.
The silicone rubber self-adhesive tape comprises the following raw materials in percentage by weight: 45-75 parts of base material, 3-10 parts of boron modified MQ silicon resin, 5-15 parts of alumina, 5-10 parts of hydrophobic white carbon black, 3-6 parts of nano montmorillonite, 5-15 parts of composite flame retardant, 3-5 parts of dibenzoyl peroxide, 2-5 parts of ethynyl cyclohexanol, 1-3 parts of vinyl silane-platinum complex and 1-2 parts of iron oxide red, wherein the base material comprises 35-55 parts of vinyl terminated methyl vinyl silicone rubber crude rubber with the mole fraction of vinyl chain links of 0.03-0.05%, 5-10 parts of vinyl silicone oil with the mole fraction of hydroxyl terminated vinyl chain links of 0.45-1.2%, the viscosity of 500-5000 mPa.s, 0.5-0.12wt% of hydrogen content and 5-10 parts of hydrogen-containing silicone oil with the viscosity of 100-500 mPa.s.
The silicone rubber self-adhesive tape provided by the invention contains 2-5 parts by weight of ethynylcyclohexanol, the ethynylcyclohexanol is diluted to 0.1wt% by adopting viscosity of 1000mPa & s and then used, and the ethynylcyclohexanol is diluted by adopting vinyl silicone oil, so that the storage stability of the ethynylcyclohexanol is improved, the ethynylcyclohexanol is conveniently and rapidly and uniformly dispersed in a base material system, and the ethynylcyclohexanol is mainly used as a hydrosilylation reaction inhibitor; the source of the inhibitor is not particularly limited in the present invention, and any inhibitor known to those skilled in the art may be used.
The silicone rubber self-adhesive tape provided by the invention contains 3-10 parts by weight of boron modified MQ silicone resin, and the boron modified MQ silicone resin is prepared by the following steps: adding 250g of xylene solution of methyl MQ silicon resin into a reactor, wherein the content of the methyl MQ silicon resin in the xylene solution of the methyl MQ silicon resin is 60wt%, then adding 42.5g of 50wt% of phenyl boric acid methanol solution under stirring, heating to 70-90 ℃, reacting for 4-8 hours, and cooling to obtain the boric acid modified methyl MQ silicon resin.
The silicone rubber self-adhesive tape provided by the invention contains 5-15 parts of alumina by weight, wherein the alumina is spherical alumina, the spherical alumina comprises alumina with the particle size of 50-70 mu m, alumina with the particle size of 15-30 mu m and alumina with the particle size of 3-5 mu m, and the mass ratio of the alumina with the particle size of 50-70 mu m to the alumina with the particle size of 15-30 mu m to the alumina with the particle size of 3-5 mu m is (4-6): (3-5): (1-3).
The silicone rubber self-adhesive tape provided by the invention contains 3-6 parts of nano montmorillonite in parts by weight, wherein the nano montmorillonite is dioctadecyl intercalation modified montmorillonite, and the nano montmorillonite is mainly used for compounding with the existing polymer to manufacture nano plastics, nano rubber, nano fibers, nano paint, nano adhesive and the like. The strength, heat resistance, modulus, gas barrier property, wear resistance, flame retardant property and the like of the polymer material can be greatly improved by adding a small amount (3-5 wt%), and particularly, the heat resistance and the barrier property can be improved by times. The nano montmorillonite modified by the dioctadecyl intercalation used in the application can greatly improve the properties of the silicone rubber tape such as strength, elongation and the like, and can also improve the properties of the silicone rubber tape in the aspects of hardness, flame retardance and gas barrier;
the silicone rubber self-adhesive tape provided by the invention contains 5-15 parts of composite flame retardant by weight, wherein the composite flame retardant comprises a phosphorus-fluorine-containing flame retardant and magnesium hydroxide, and the mass ratio of the phosphorus-fluorine-containing flame retardant to the magnesium hydroxide is (1-2): (3-5), further defined as: wherein the phosphorus and fluorine-containing flame retardant is prepared by the following steps: adding 3, 5-bis (trifluoromethyl) aniline, DOPO, paraformaldehyde and tetrahydrofuran into a reaction vessel, wherein the mass ratio of the 3, 5-bis (trifluoromethyl) aniline to the DOPO to the paraformaldehyde to the tetrahydrofuran is 1:6:10:56, carrying out reflux reaction for 8-72h at 40-120 ℃, cooling and standing to precipitate solids, and separating the precipitated solids, namely the phosphorus-fluorine-containing flame retardant.
The silicone rubber self-adhesive tape provided by the invention contains 1-3 parts of vinyl silane-platinum complex by weight, wherein the vinyl silane-platinum complex is a reaction product of vinyl triethoxysilane and chloroplatinic acid, and the concentration is 8000-20000ppm, and more preferably 12000-16000ppm.
A preparation method of a silicone rubber self-adhesive tape comprises the following steps:
1) Preparing an alumina filler according to the formula requirement;
2) Adding the base material with the formula amount into a stirring kettle, uniformly stirring at the rotating speed of 40-60rpm, then sequentially adding the hydrophobic white carbon black, the nano montmorillonite, the composite flame retardant, the boron modified MQ silicon resin, the alumina and the iron oxide red in the step 1), adjusting the rotating speed to 50-120rpm, heating to 80-120 ℃, starting vacuum to remove bubbles and micromolecule substances, and maintaining at the rotating speed of 50-120rpm for 1.5-2 hours to uniformly mix the materials in the stirring kettle;
3) After the material obtained in the step 2) is cooled to room temperature, firstly adding the ethynyl cyclohexanol with the formula amount, uniformly stirring at the rotating speed of 40-80rpm, then sequentially adding the dibenzoyl peroxide and the vinyl silane-platinum complex with the formula amount, uniformly mixing at the rotating speed of 40-80rpm, and vacuumizing until bubbles in the material are completely pumped out to obtain a mixed rubber material;
4) Placing the mixed rubber material obtained in the step 3) on a calender for calendering, curing and molding, and then cutting to obtain the silicon rubber self-adhesive tape; further defined, the step 4) also comprises the steps of firstly paving a base material on a conveying belt of a calender, then uniformly adding the mixed rubber material obtained in the step 3) to the starting end of the paved base material, and starting the calender to perform calendering, curing and molding.
Example 1
1) Pre-preparation of various raw materials:
preparation of alumina filler:
mixing 60-micron alumina, 25-micron alumina and 5-micron alumina in a mass ratio of 4:5:1, uniformly mixing in a stirrer to obtain the alumina filler in the application, and packaging for later use;
preparing a composite flame retardant:
the mass ratio of the phosphorus-fluorine-containing flame retardant to the magnesium hydroxide is 1:3, uniformly mixing in a stirrer to obtain the composite flame retardant in the application, and packaging for later use;
2) Sequentially adding 35 parts of vinyl-terminated methyl vinyl silicone rubber raw rubber with a vinyl chain link mole fraction of 0.03%, 10 parts of hydroxyl-terminated vinyl silicone oil with a vinyl chain link mole fraction of 1.2% and a viscosity of 1000mPa & s, and 8 parts of hydrogen-containing silicone oil with a hydrogen content of 0.8wt% and a viscosity of 250mPa & s into a stirring kettle, uniformly stirring at a rotating speed of 40-60rpm, sequentially adding 6 parts of hydrophobic white carbon black, 4 parts of nano montmorillonite, 6 parts of composite flame retardant, 5 parts of boron-modified MQ silicone resin, 15 parts of alumina and 1 part of iron oxide red in the step 1), adjusting the rotating speed to 120rpm, heating to 80-120 ℃, starting vacuum to remove bubbles and small molecular substances, maintaining at the rotating speed of 120rpm for 1.5-2 hours, and uniformly mixing the materials in the stirring kettle;
3) After the material obtained in the step 2) is cooled to room temperature, firstly adding 4 parts of ethynyl cyclohexanol, stirring uniformly at the rotating speed of 60rpm, then sequentially adding 3 parts of dibenzoyl peroxide and 3 parts of vinyl silane-platinum complex, mixing uniformly at the rotating speed of 60rpm, and vacuumizing until air bubbles in the material are completely pumped out to obtain a mixed sizing material;
4) Adjusting the distance between a press roll and a transmission belt in a calender to be the thickness required by the silicon rubber self-adhesive tape, in the embodiment, adjusting the distance to be 2 +/-0.2 mm, adjusting the transmission speed of the transmission belt to be 20m/min, meanwhile, paving a base material on the surface of the paved PE film, then guiding the mixed rubber material obtained in the step 3) into the pre-paved base material, vulcanizing and molding at the temperature of 130-150 ℃ and the vulcanization time of 35-45s, and cutting the size at the discharge end of the calender according to actual requirements to obtain the silicon rubber self-adhesive tape.
Wherein the specific surface area of the hydrophobic white carbon black is 380m 2 The vinylsilane-platinum complex concentration was 10000 ppm/g.
The performance of the silicone rubber self-adhesive tape obtained in example 1 was tested, and the results are shown in table one.
Example 2
1) Pre-preparation of various raw materials:
preparation of alumina filler:
mixing 50 μm of alumina, 15 μm of alumina and 3 μm of alumina in a mass ratio of 5:3:1, uniformly mixing in a stirrer to obtain the alumina filler in the application, and packaging for later use;
preparing a composite flame retardant:
the mass ratio of the phosphorus-fluorine-containing flame retardant to the magnesium hydroxide is 1:4, uniformly mixing in a stirrer to obtain the composite flame retardant in the application, and packaging for later use;
2) Sequentially adding 40 parts of vinyl-terminated methyl vinyl silicone rubber raw rubber with the vinyl chain link mole fraction of 0.03%, 8 parts of hydroxyl-terminated vinyl silicone oil with the vinyl chain link mole fraction of 0.8% and the viscosity of 1000mPa & s and 6 parts of hydrogen-containing silicone oil with the hydrogen content of 0.6wt% and the viscosity of 250mPa & s into a stirring kettle, uniformly stirring at the rotating speed of 40-60rpm, sequentially adding 8 parts of hydrophobic white carbon black, 3 parts of nano montmorillonite, 12 parts of composite flame retardant, 6 parts of boron-modified MQ silicone resin, 8 parts of alumina and 1 part of iron oxide red in the step 1), adjusting the rotating speed to 100rpm, heating to 80-120 ℃, starting vacuum to remove bubbles and small molecular substances, and maintaining at the rotating speed of 100rpm for 1.5-2 hours to uniformly mix the materials in the stirring kettle;
3) After the material obtained in the step 2) is cooled to room temperature, firstly adding 3 parts of ethynyl cyclohexanol, stirring uniformly at the rotating speed of 60rpm, then sequentially adding 3 parts of dibenzoyl peroxide and 2 parts of vinyl silane-platinum complex, mixing uniformly at the rotating speed of 60rpm, and vacuumizing until air bubbles in the material are completely pumped out to obtain a mixed rubber material;
4) Adjusting the distance between a press roll and a transmission belt in a calender to be the thickness required by the silicon rubber self-adhesive tape, in the embodiment, adjusting the distance to be 2 +/-0.2 mm, adjusting the transmission speed of the transmission belt to be 20m/min, meanwhile, paving a base material on the surface of the paved PE film, then guiding the mixed rubber material obtained in the step 3) into the pre-paved base material, vulcanizing and molding at the temperature of 130-150 ℃ and the vulcanization time of 35-45s, and cutting the size at the discharge end of the calender according to actual requirements to obtain the silicon rubber self-adhesive tape.
Wherein the specific surface area of the hydrophobic white carbon black is 250m 2 The concentration of vinylsilane-platinum complex per gram was 12000ppm.
The properties of the silicone rubber self-adhesive tape obtained in example 2 were tested, and the results are shown in table one.
Example 3
1) Pre-preparation of various raw materials:
preparation of alumina filler:
mixing 55-micron alumina, 20-micron alumina and 4-micron alumina in a mass ratio of 6:3:1, uniformly mixing in a stirrer to obtain the alumina filler in the application, and packaging for later use;
preparing a composite flame retardant:
the mass ratio of the phosphorus-fluorine-containing flame retardant to the magnesium hydroxide is 2:3, uniformly mixing in a stirrer to obtain the composite flame retardant in the application, and packaging for later use;
2) Sequentially adding 45 parts of vinyl-terminated methyl vinyl silicone rubber raw rubber with the vinyl chain link mole fraction of 0.05 percent, 7 parts of hydroxyl-terminated vinyl silicone oil with the vinyl chain link mole fraction of 0.8 percent and the viscosity of 1000mPa & s and 6 parts of hydrogen-containing silicone oil with the hydrogen content of 0.5wt percent and the viscosity of 350mPa & s into a stirring kettle, uniformly stirring at the rotating speed of 40-60rpm, sequentially adding 6 parts of hydrophobic white carbon black, 5 parts of nano montmorillonite, 8 parts of composite flame retardant, 6 parts of boron-modified MQ silicone resin, 9 parts of alumina and 1 part of iron oxide red in the step 1), adjusting the rotating speed to 80rpm, heating to 80-120 ℃, starting vacuum to remove bubbles and small molecular substances, and maintaining at the rotating speed of 80rpm for 1.5-2 hours to uniformly mix the materials in the stirring kettle;
3) After the material obtained in the step 2) is cooled to room temperature, firstly adding 3 parts of ethynyl cyclohexanol, stirring uniformly at the rotating speed of 60rpm, then sequentially adding 3 parts of dibenzoyl peroxide and 1 part of vinyl silane-platinum complex, mixing uniformly at the rotating speed of 60rpm, and vacuumizing until bubbles in the material are completely pumped out to obtain a mixed rubber material;
4) Adjusting the distance between a press roll and a transmission belt in a calender to be the thickness required by the silicon rubber self-adhesive tape, in the embodiment, adjusting the distance to be 2 +/-0.2 mm, adjusting the transmission speed of the transmission belt to be 20m/min, meanwhile, paving a base material on the surface of the paved PE film, then guiding the mixed rubber material obtained in the step 3) into the pre-paved base material, vulcanizing and molding at the temperature of 130-150 ℃ and the vulcanization time of 35-45s, and cutting the size at the discharge end of the calender according to actual requirements to obtain the silicon rubber self-adhesive tape.
Wherein the specific surface area of the hydrophobic white carbon black is 250m 2 The concentration of the vinylsilane-platinum complex was 12000ppm per gram.
The properties of the silicone rubber self-adhesive tape obtained in example 3 were tested, and the results are shown in table one.
Example 4
1) Pre-preparation of various raw materials:
preparation of alumina filler:
mixing 70 μm of alumina, 15 μm of alumina and 5 μm of alumina in a mass ratio of 5:3:1, uniformly mixing in a stirrer to obtain the alumina filler in the application, and packaging for later use;
preparing a composite flame retardant:
the mass ratio of the phosphorus-fluorine-containing flame retardant to the magnesium hydroxide is 2:5, uniformly mixing in a stirrer to obtain the composite flame retardant, and packaging for later use;
2) Sequentially adding 50 parts of vinyl-terminated methyl vinyl silicone rubber raw rubber with the vinyl chain link mole fraction of 0.03%, 6 parts of hydroxyl-terminated vinyl silicone oil with the vinyl chain link mole fraction of 1.2% and the viscosity of 500mPa & s and 8 parts of hydrogen-containing silicone oil with the hydrogen content of 0.35wt% and the viscosity of 350mPa & s into a stirring kettle, uniformly stirring at the rotating speed of 40-60rpm, sequentially adding 7 parts of hydrophobic white carbon black, 3 parts of nano-montmorillonite, 6 parts of composite flame retardant, 5 parts of boron-modified MQ silicone resin, 6 parts of alumina and 1 part of iron oxide red in the step 1), adjusting the rotating speed to 100rpm, heating to 80-120 ℃, starting vacuum to remove bubbles and small molecular substances, and maintaining at the rotating speed of 100rpm for 1.5-2 hours to uniformly mix the materials in the stirring kettle;
3) After the material obtained in the step 2) is cooled to room temperature, firstly adding 2 parts of ethynyl cyclohexanol, stirring uniformly at the rotating speed of 60rpm, then sequentially adding 4 parts of dibenzoyl peroxide and 2 parts of vinyl silane-platinum complex, mixing uniformly at the rotating speed of 60rpm, and vacuumizing until air bubbles in the material are completely pumped out to obtain a mixed rubber material;
4) Adjusting the distance between a press roll and a transmission belt in a calender to be the thickness (generally 0.5-3.0 mm) required by the silicon rubber self-adhesive tape, adjusting the distance to be 2 +/-0.2 mm in the embodiment, adjusting the transmission speed of the transmission belt to be 20m/min, laying a base material on the surface of the laid PE film, then introducing the mixed rubber material obtained in the step 3) onto the pre-laid base material, vulcanizing and forming under the conditions that the temperature is 130-150 ℃ and the vulcanization time is 35-45s, and cutting the self-adhesive tape at the discharge end of the calender according to the actual required size to obtain the silicon rubber self-adhesive tape.
Wherein the specific surface area of the hydrophobic white carbon black is 300m 2 The concentration of the vinylsilane-platinum complex was 15000ppm.
The performance of the silicone rubber self-adhesive tape obtained in example 4 was tested, and the results are shown in table one.
Example 5
1) Pre-preparation of various raw materials:
preparation of alumina filler:
mixing 60 mu m of alumina, 25 mu m of alumina and 3 mu m of alumina according to the mass ratio of 6:3:2, uniformly mixing in a stirrer to obtain the alumina filler in the application, and packaging for later use;
preparing a composite flame retardant:
the mass ratio of the phosphorus-fluorine-containing flame retardant to the magnesium hydroxide is 2:5, uniformly mixing in a stirrer to obtain the composite flame retardant, and packaging for later use;
2) Sequentially adding 55 parts of vinyl-terminated methyl vinyl silicone rubber raw rubber with the vinyl chain link mole fraction of 0.05 percent, 5 parts of hydroxyl-terminated vinyl silicone oil with the vinyl chain link mole fraction of 0.8 percent and the viscosity of 1000mPa & s and 5 parts of hydrogen-containing silicone oil with the hydrogen content of 0.4wt percent and the viscosity of 450mPa & s into a stirring kettle, uniformly stirring at the rotating speed of 40-60rpm, then sequentially adding 5 parts of hydrophobic white carbon black, 3 parts of nano montmorillonite, 5 parts of composite flame retardant, 8 parts of boron-modified MQ silicone resin, 5 parts of alumina and 1 part of iron oxide red in the step 1), adjusting the rotating speed to 120rpm, heating to 80-120 ℃, starting vacuum to remove bubbles and small molecular substances, and maintaining at the rotating speed of 120rpm for 1.5-2 hours to uniformly mix the materials in the stirring kettle;
3) After the material obtained in the step 2) is cooled to room temperature, firstly adding 2 parts of ethynyl cyclohexanol, stirring uniformly at the rotating speed of 80rpm, then sequentially adding 5 parts of dibenzoyl peroxide and 1 part of vinyl silane-platinum complex, mixing uniformly at the rotating speed of 80rpm, and vacuumizing until air bubbles in the material are completely pumped out to obtain a mixed rubber material;
4) Adjusting the distance between a press roll and a transmission belt in a calender to be the thickness (generally 0.5-3.0 mm) required by the silicone rubber self-adhesive tape, adjusting the distance to be 2 +/-0.2 mm in the embodiment, adjusting the transmission speed of the transmission belt to be 20m/min, laying a base material on the surface of the laid PE film, then introducing the mixed rubber obtained in the step 3) onto the pre-laid base material, vulcanizing and forming under the conditions that the temperature is 130-150 ℃ and the vulcanizing time is 35-45s, and cutting the size at the discharge end of the calender according to the actual self-adhesive requirement to obtain the silicone rubber self-adhesive tape.
Wherein the nano montmorillonite is dioctadecyl intercalation modified montmorillonite; the specific surface area of the hydrophobic white carbon black is 380m 2 The vinyl silane-platinum complex is a reaction product of vinyl triethoxysilane and chloroplatinic acid, and has a concentration of 10000ppm.
The performance of the silicone rubber self-adhesive tape obtained in example 5 was tested, and the results are shown in table one.
Comparative group 1
In this comparison group, the corresponding self-adhesive silica gel with the patent number of 201610252719.3 is selected, and alumina, hydrophobic silica, nano-montmorillonite, composite flame retardant, dibenzoyl peroxide, ethynyl cyclohexanol, vinyl silane-platinum complex with the same proportion in the filling example are found to be incapable of coating the filler substance well in the implementation process, so that the filler substance cannot enter the vulcanization stage, namely, the corresponding performance test cannot be carried out.
Comparative example 1
The components, the proportion, the preparation method and the like of the comparative example 1 are the same as those of the example 3, except that only the magnesium hydroxide in the composite flame retardant is added, and the phosphorus-containing fluorine flame retardant is not added.
The properties of the silicone rubber self-adhesive tape obtained in this comparative example 1 were tested, and the results are shown in table one.
Comparative example 2
The components, the ratio, the preparation method and the like of the comparative example 2 are the same as those of the example 3, except that only the phosphorus-containing fluorine flame retardant in the composite flame retardant is added, and the magnesium hydroxide is not added.
The properties of the silicone rubber self-adhesive tape obtained in this comparative example 2 were tested, and the results are shown in table one.
Comparative example 3
The components, the proportion, the preparation method and the like of the comparative example 3 are the same as those of the example 3, except that the nano montmorillonite is not added.
The properties of the silicone rubber self-adhesive tape obtained in this comparative example 3 were tested, and the results are shown in table one.
Comparative example 4
The components, the proportion and the preparation method of the comparative example 4 are the same as those of the example 3, except that the specific surface area of the hydrophobic white carbon black added only is 150-200m 2 /g。
The properties of the silicone rubber self-adhesive tape obtained in this comparative example 4 were tested, and the results are shown in table one.
Comparative example 5
The components, the mixture ratio, the preparation method and the like of the comparative example 5 are the same as those of the example 3, except that the particle size of the alumina added is only 55 μm, and incomplete coating occurs during the filling process, so that the vulcanization operation cannot be carried out.
Comparative example 6
Comparative example 6 has the same composition, formulation and preparation method as example 3, except that only alumina of 55 μm and alumina of 20 μm were mixed.
The properties of the silicone rubber self-adhesive tape obtained in this comparative example 6 were tested, and the results are shown in table one.
Comparative example 7
Comparative example 7 was prepared by the same method as example 3 except that alumina of 55 μm and alumina of 4 μm were mixed.
The properties of the silicone rubber self-adhesive tape obtained in this comparative example 7 were tested, and the results are shown in table one.
Comparative example 8
Comparative example 8 has the same composition, ratio and preparation method as example 3, except that only 20 μm alumina and 4 μm alumina were added.
The properties of the silicone rubber self-adhesive tape obtained in this comparative example 8 were tested, and the results are shown in table one.
Comparative example 9
The composition, formulation, and preparation method of comparative example 9 were the same as those of example 3 except that the hydrogen-containing silicone oil and the vinylsilane-platinum complex were not added and the hydrogen-containing silicone oil was used in an amount substituted with a vinyl silicone oil having a hydroxyl group-terminated vinyl moiety mole fraction of 0.8% and a viscosity of 1000mPa · s.
The properties of the silicone rubber self-adhesive type adhesive tape obtained in this comparative example 9 were tested, and the results are shown in table one.
The properties of the silicone rubber self-adhesive tapes obtained in examples 1 to 5, comparative group 1 and comparative examples 1 to 9 of the present invention were measured, and are specifically shown in table one:
TABLE 1 Performance test results of the silicone rubber self-adhesive type adhesive tape obtained in the example of the present invention
As can be seen from the table I, the silicone rubber self-adhesive tape provided by the invention adopts the silicone as the main material, has better thermal conductivity, insulativity and flame retardance besides the excellent properties of the silicone, and good mechanical strength and self-adhesive strength, and the other indexes also meet the use requirements of the power industry, wherein the volume resistivity is not less than 1 multiplied by 10 14 Omega.cm (GB 31838.2-2019), dielectric constant not more than 3.5 (GB/T1409-2006), and water absorption not more than 0.35% (GB/T1409-2006)1034-2008), the thermal aging performance is unchanged after 136 ℃ and 168 hours (GB/T2951.12), the low-temperature toughness is-55 +/-2 ℃,4 hours of passing (UL 224), the power frequency withstand voltage is 42kV withstand voltage for 1min (GB/T1408-2016), the lightning impulse is 75KV, and is not broken down (DL/T1059-2007) for +/-15 times (the distance is 70 mm), and the metal corrosivity is grade A (GB/T14834-2009); in addition, this silicon rubber self-adhesion type sticky tape convenient to use, each layer of sticky tape of single book all has special isolation lining to protect, remove the lining during the use can directly partly take the winding contact surface, the spiral partly take the winding can, it is half suitable to overlap when tensile sticky tape winding, twine the last circle natural light tensile overlap joint, make this silicon rubber self-adhesion type sticky tape and electrical equipment closely laminate, not only can derive the heat that electrical equipment produced in the operation process effectively, the human casualties accident that causes is arranged to dirty sudden strain of a muscle, condensation flashover, toy short circuit and naked mother in the transformer substation has also been stopped effectively.
The above description is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are also within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.