Self-adhesive and preparation method and application thereof
阅读说明：本技术 一种自粘胶及其制备方法和应用 (Self-adhesive and preparation method and application thereof ) 是由 岑海波 莫远强 姜金燕 王雅苓 于 2021-08-02 设计创作，主要内容包括：本发明提供一种自粘胶及其制备方法和应用,所述自粘胶的制备原料包括乙烯基生胶、硅橡胶、羟基硅油、硼酸、白炭黑、复合阻燃剂和硫化剂的组合；通过在制备原料中添加特定份数的硅橡胶和硼酸,使二者发生反应,提高了所述自粘胶的自粘性能；进一步添加特定份数的白炭黑和复合阻燃剂,使得所述自粘胶兼具优异的机械性能和阻燃性能；且所述自粘胶的制备工艺简单,适合批量化工业生产,具有重要的研究价值。(The invention provides a self-adhesive and a preparation method and application thereof, wherein the preparation raw materials of the self-adhesive comprise raw vinyl rubber, silicon rubber, hydroxyl silicone oil, boric acid, white carbon black, a composite flame retardant and a vulcanizing agent; the silicon rubber and the boric acid in specific parts are added into the preparation raw materials to react with each other, so that the self-adhesive property of the self-adhesive is improved; further adding a specific part of white carbon black and a composite flame retardant, so that the self-adhesive has excellent mechanical property and flame retardant property; and the preparation process of the self-adhesive is simple, is suitable for batch industrial production, and has important research value.)
1. The self-adhesive is characterized by comprising the following raw materials in parts by weight:
2. the self-adhesive glue according to claim 1, characterized in that the molecular weight of the raw vinyl glue is 300000-600000 Da.
3. The self-adhesive according to claim 1 or 2, characterized in that the white carbon black comprises fumed silica;
preferably, the particle size of the white carbon black is 7000-9000 meshes.
4. The self-adhesive according to any one of claims 1 to 3, wherein the vulcanizing agent comprises any one or a combination of at least two of 2, 4-dichloroperoxybenzoyl, 2, 5-dimethyl-2, 5-bis (t-butylperoxy) hexane or dicumyl peroxide.
5. The self-adhesive according to any one of claims 1 to 4, wherein the silicone rubber comprises 107 silicone rubber;
preferably, the viscosity of the silicone rubber is 30000-1000000 cst;
preferably, the molecular weight of the silicone rubber is 90000-200000 Da;
preferably, the viscosity of the hydroxyl silicone oil is 20-40 cst;
preferably, the hydroxyl content of the hydroxyl silicone oil is 8-9%;
preferably, the polymerization degree of the hydroxyl silicone oil is 100-200.
6. The self-adhesive according to any one of claims 1 to 5, wherein the composite flame retardant comprises a combination of a brominated flame retardant and antimony trioxide;
preferably, the mass ratio of the antimony trioxide to the brominated flame retardant is 1 (1-4);
preferably, the brominated flame retardant comprises any one of decabromodiphenylethane, decabromodiphenyl ether or tetrahexabisphenol A or a combination of at least two of the same.
7. A process for the preparation of the self-adhesive according to any one of claims 1 to 6, comprising the following steps:
(1) mixing vinyl raw rubber and white carbon black to obtain mixed base rubber;
(2) mixing the mixed base rubber obtained in the step (1), silicon rubber, hydroxyl silicone oil, boric acid and a composite flame retardant, and reacting to obtain mixed rubber;
(3) and (3) vulcanizing the mixing rubber obtained in the step (2) and a vulcanizing agent to obtain the self-adhesive rubber.
8. The method of claim 7, wherein the temperature of the mixing of step (1) is less than 80 ℃;
preferably, the mixing time in the step (1) is 1-3 h;
preferably, the temperature of the mixing in the step (2) is room temperature;
preferably, the mixing time in the step (2) is 1-3 h;
preferably, the reaction in the step (2) is carried out under the conditions of temperature rise and vacuum pumping;
preferably, the method of raising temperature and evacuating comprises: heating the system to 170-180 ℃, and vacuumizing to-0.05 to-0.07 Mpa; keeping for 0.5-1.5 h; stopping vacuumizing, and keeping for 1-2 h to finish the temperature rise and the vacuumizing;
preferably, the temperature of the vulcanization in the step (3) is 120-130 ℃;
preferably, the vulcanizing time in the step (3) is 10-20 min.
9. The method according to claim 7 or 8, characterized in that it comprises the steps of:
(1) mixing vinyl raw rubber and white carbon black for 1-3 hours at the temperature of less than 80 ℃ to obtain mixed base rubber;
(2) mixing the mixed base rubber obtained in the step (1), silicon rubber, hydroxyl silicone oil, boric acid and a flame retardant for 1-3 hours at room temperature, and reacting under the conditions of temperature rise and vacuum pumping to obtain mixed rubber; the method for heating and vacuumizing comprises the following steps: heating the system to 170-180 ℃, and vacuumizing to-0.05 to-0.07 Mpa; keeping for 0.5-1.5 h; stopping vacuumizing, and keeping for 1-2 h to finish the temperature rise and the vacuumizing;
(3) and (3) vulcanizing the mixing glue obtained in the step (2) and a vulcanizing agent at 120-130 ℃ for 10-20 min to obtain the self-adhesive glue.
10. Use of the self-adhesive glue according to any one of claims 1 to 6 in batteries.
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a self-adhesive and a preparation method and application thereof.
Background
At present, the common self-adhesive insulating tapes mainly comprise two types, one type is a high-voltage insulating rubber tape formed by laminating two rubber sheets, and the high-voltage insulating rubber tape comprises an elastic insulating layer and an adhesive layer; the other is self-adhesive rubber tape prepared by taking butyl rubber as a main material; however, both types of tapes are susceptible to hardening and losing their tackiness in a long-term high-temperature environment. At present, pure silicon rubber insulating cement has excellent high-temperature resistance and is widely applied to coils of high-voltage motors and power systems.
CN102965048A discloses a reinforced silicon rubber self-adhesive insulating tape, which takes cotton fiber cloth as a base material, and the upper surface and the lower surface of the base material are respectively coated with an adhesive layer; the adhesive layer comprises the following materials in parts by weight: 30-60 parts of silicon rubber, 10-25 parts of fumed silica, 0-5 parts of silicone oil softener, 5-20 parts of silicon boron tackifier, 0.2-0.5 part of colorant and 0.5-5 parts of vulcanizing agent. The tensile strength of the reinforced silicon rubber self-adhesive insulating tape obtained by the invention is more than or equal to 5PMa, the tensile strength is more than or equal to 3MPa, and the reinforced silicon rubber self-adhesive insulating tape improves the safe operation capability, the anti-cracking capability, the anti-fouling capability and the wear-resisting capability of a cable in the insulating sealing lapping process of various cable joints of 35kV and below, is more compact in lapping, has better sealing and waterproof effects, and is safe and reliable to use within the temperature range of-40-260 ℃. However, since the adhesive is produced by using the solid silicone rubber, the adhesive is solid, and when the adhesive is coated on the upper surface and the lower surface of the cotton fiber cloth, the coating is difficult, the production process is complicated, the self-adhesion is poor and unstable, and the storage time of the adhesive tape is short.
CN103421465A discloses a silicone rubber for an organic silicon self-adhesive tape and a synthesis process thereof, wherein the silicone rubber is mainly prepared from the following raw materials in percentage by mass: 8-33% of methyl vinyl MQ silicon resin; 14-40% of methyl vinyl silicone rubber; 11-34% of hydroxyl silicone rubber; 20-55% of white carbon black; adding the raw materials into a kneader according to the formula amount, and uniformly stirring at normal temperature to obtain the silicone rubber for the organic silicon self-adhesive tape. The silicone rubber for the organic silicon self-adhesive tape is synthesized by reasonable selection of raw materials and proportions. The raw materials are synergistic, so that the obtained silicon rubber product has better high and low temperature resistance, weather resistance, insulativity and excellent moisture-proof and waterproof performances, and the comprehensive performance of the silicon rubber product is superior to that of the silicon rubber of the existing organic silicon self-adhesive tape. However, the self-adhesive prepared by the method is difficult to be discharged when the self-adhesive is milled on an open mill; after the silicone rubber is molded and vulcanized, the self-adhesive tape is easy to fall off after being constructed for a period of time due to low bonding force and poor self-adhesion among the silicone resins.
CN101921550A discloses a silicon rubber self-adhesive tape, which is prepared from methyl vinyl silicon rubber, gas phase white carbon black, tackifier, vinyl silicone oil and iron oxide red by mixing the above raw materials, and placing the mixture in a 60Co gamma ray irradiation field for radiation vulcanization. The silicon rubber self-adhesive tape not only meets the urgent need of special engine manufacturing, but also can be independently used as an insulation protection product under high-temperature and high-pressure environment, is applied to electrical insulation protection of large motors, special machinery and the like, can meet the strong insulation sealing prevention requirement under special high-temperature and high-pressure severe environment in the industries of ships, mines, oil gas, chemical industry, steel and the like, but has poor flame retardance and cannot meet the application in certain specific occasions.
Therefore, the development of a self-adhesive with excellent self-adhesion, flame retardancy and mechanical properties is a technical problem to be solved urgently in the field.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a self-adhesive and a preparation method and application thereof, the preparation raw materials of the self-adhesive comprise a combination of raw vinyl rubber, silicon rubber, hydroxyl silicone oil, boric acid, white carbon black, a composite flame retardant and a vulcanizing agent, and the self-adhesive obtained after vulcanization has excellent self-adhesiveness, flame retardance and mechanical properties through mutual matching of the components, meets the performance requirements of various occasions on self-adhesive products, and has important research significance.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a self-adhesive, which comprises the following raw materials in parts by weight:
the vinyl gum stock may be 21, 22, 23, 24, 25, 26, 27, 28, or 29 parts by weight, and specific points therebetween, not to be construed as exhaustive, and for brevity, the invention is not intended to include specific points within the indicated ranges.
The silicone rubber may be 2.1 parts by weight, 2.2 parts by weight, 2.3 parts by weight, 2.4 parts by weight, 2.5 parts by weight, 2.6 parts by weight, 2.7 parts by weight, 2.8 parts by weight, or 2.9 parts by weight, and specific values therebetween, not to limit the disclosure and for the sake of brevity, the invention is not exhaustive of the specific values included in the ranges.
The hydroxyl silicone oil can be 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, or 1.9 parts by weight, and the specific values therebetween are not intended to be exhaustive for the sake of brevity and clarity.
The boric acid may be 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8 or 1.9 parts by weight, and specific values therebetween, not to be construed as limiting the disclosure and for the sake of brevity, the invention is not intended to be exhaustive of the specific values included in the ranges set forth.
The white carbon black may be 21 parts by weight, 22 parts by weight, 23 parts by weight, 24 parts by weight, 25 parts by weight, 26 parts by weight, 27 parts by weight, 28 parts by weight or 29 parts by weight, and specific values therebetween are not exhaustive for the purpose of brevity and clarity.
The composite flame retardant may be 21 parts by weight, 22 parts by weight, 23 parts by weight, 24 parts by weight, 25 parts by weight, 26 parts by weight, 27 parts by weight, 28 parts by weight, or 29 parts by weight, and specific points therebetween, which are not exhaustive and included in the range for brevity.
The vulcanizing agent may be 3.2 parts by weight, 3.4 parts by weight, 3.6 parts by weight, 3.8 parts by weight, 4 parts by weight, 4.2 parts by weight, 4.4 parts by weight, 4.6 parts by weight, or 4.8 parts by weight, and specific values therebetween, not to limit the disclosure and for the sake of brevity, the invention is not exhaustive of the specific values included in the ranges.
The raw materials for preparing the self-adhesive provided by the invention comprise raw vinyl rubber, silicon rubber, hydroxyl silicone oil, boric acid, white carbon black, a composite flame retardant and a vulcanizing agent; the silicon rubber and the boric acid in specific parts are added into the preparation raw materials to react with each other, so that the self-adhesive property of the self-adhesive is improved; and white carbon black and a composite flame retardant in a specific part are further added, so that the self-adhesive has excellent mechanical property and flame retardant property.
Preferably, the molecular weight of the vinyl green rubber is 3 × 105～6×105Da, e.g. 3.3X 105Da、3.6×105Da、3.9×105Da、4.3×105Da、4.6×105Da、4.9×105Da、5.3×105Da、5.6×105Da or 5.9X 105Da, and the specific values between the above points, are not meant to be exhaustive of the invention for the sake of brevity and clarity.
As a preferred embodiment of the present invention, vinyl raw rubber having a molecular weight of 3X 10 is selected5～6×105While Da, the self-adhesive with excellent comprehensive performance can be obtained, on one hand, if the molecular weight of the vinyl crude rubber is too low, the strength of the vulcanized silica gel is too low to use; on the other hand, if the molecular weight of the vinyl raw rubber is too high and a certain amount of filler is added to mix, the processability of the silica gel is deteriorated.
Preferably, the white carbon black comprises fumed silica.
Preferably, the fumed silica has a particle size of 7000 to 9000 meshes, such as 72000 meshes, 7400 meshes, 7600 meshes, 7800 meshes, 8000 meshes, 8200 meshes, 8400 meshes, 8600 meshes or 8800 meshes, and specific values between the above values are limited to space and for brevity, and the invention is not exhaustive.
As a preferred technical scheme of the invention, when the particle size of the fumed silica is 7000-9000 meshes, the prepared self-adhesive has the most excellent comprehensive performance, on one hand, if the particle size of the added fumed silica is smaller, the prepared self-adhesive product has a higher price, and is not beneficial to product popularization; on the other hand, if the particle size of the fumed silica added is larger, the strength of the silica gel is too poor, and the use strength of the product cannot be achieved.
Preferably, the vulcanizing agent comprises any one of 2, 4-dichloroperoxybenzoyl, 2, 5-dimethyl-2, 5-bis (t-butylperoxy) hexane or dicumyl peroxide or a combination of at least two of the two.
Preferably, the silicone rubber comprises 107 silicone rubber.
Preferably, the viscosity of the silicone rubber is 3 × 104～1×106cst, e.g. 5X 104cst、1×105cst、2×105cst、3×105cst、4×105cst、5×105cst、6×105cst、7×105cst、8×105cst or 9X 105cst, and specific point values between the above point values, are limited by space and for the sake of brevity and the present invention is not intended to be exhaustive of the specific point values included in the scope.
Preferably, the molecular weight of the silicone rubber is 9 × 104～20×104Da, e.g. 10X 104Da、11×104Da、12×104Da、13×104Da、14×104Da、15×104Da、16×104Da、17×104Da、18×104Da or 19X 104Da, and the specific values between the above points, are not meant to be exhaustive of the invention for the sake of brevity and clarity.
Preferably, the viscosity of the hydroxyl silicone oil is 20-40 cst, such as 22cst, 24cst, 26cst, 28cst, 30cst, 32cst, 34cst, 36cst or 38cst, and the specific values therebetween are limited by space and for the sake of brevity, and the invention is not exhaustive.
Preferably, the hydroxyl silicone oil has a hydroxyl content of 8 to 9%, such as 8.1%, 8.2%, 8.3%, 8.4%, 8.5%, 8.6%, 8.7%, 8.8% or 8.9%, and the specific values therebetween are not exhaustive, and for brevity and clarity, the specific values included in the ranges are not limited to the space.
Preferably, the degree of polymerization of the hydroxy silicone oil is 100 to 200, such as 110, 120, 130, 140, 150, 160, 170, 180 or 190, and the specific values therebetween are limited for brevity and clarity, and the invention is not intended to be exhaustive of the specific values included in the scope.
Preferably, the composite flame retardant comprises a combination of a brominated flame retardant and antimony trioxide.
Preferably, the mass ratio of the antimony trioxide to the bromine-based flame retardant is 1 (1-4), such as 1:1.3, 1:1.6, 1:1.9, 1:2.3, 1:2.6, 1:2.9, 1:3.3, 1:3.6 or 1: 3.9.
As a preferred technical scheme, when the mass ratio of the antimony trioxide to the brominated flame retardant added in the raw materials for preparing the self-adhesive provided by the invention is 1 (1-4), the finally obtained self-adhesive can have excellent flame retardant property; on the one hand, if the amount of antimony trioxide used therein is too large or too small, a decrease in flame retardancy may result.
Preferably, the brominated flame retardant comprises any one of decabromodiphenylethane, decabromodiphenyl ether or tetrahexabisphenol A or a combination of at least two of the same.
In a second aspect, the present invention provides a method for preparing the self-adhesive according to the first aspect, the method comprises the following steps:
(1) mixing vinyl raw rubber and white carbon black to obtain mixed base rubber;
(2) mixing the mixed base rubber obtained in the step (1), silicon rubber, hydroxyl silicone oil, boric acid and a composite flame retardant, and reacting to obtain mixed rubber;
(3) and (3) vulcanizing the mixing rubber obtained in the step (2) and a vulcanizing agent to obtain the self-adhesive rubber.
Preferably, the temperature of the mixing of step (1) is less than 80 ℃, e.g., 70 ℃, 60 ℃, 50 ℃, 40 ℃, 30 ℃, 20 ℃, 10 ℃ or 5 ℃, and the specific values therebetween, are not exhaustive for the invention and for brevity.
Preferably, the mixing time in step (1) is 1 to 3 hours, such as 1.2 hours, 1.4 hours, 1.6 hours, 1.8 hours, 2 hours, 2.2 hours, 2.4 hours, 2.6 hours or 2.8 hours, and the specific values therebetween are not exhaustive, and the invention is not limited to the specific values included in the range for brevity and conciseness.
Preferably, the temperature of the mixing in step (2) is room temperature.
Preferably, the mixing time in step (2) is 1 to 3 hours, such as 1.2 hours, 1.4 hours, 1.6 hours, 1.8 hours, 2 hours, 2.2 hours, 2.4 hours, 2.6 hours or 2.8 hours, and the specific values therebetween are not exhaustive, and the invention is not limited to the specific values included in the range for brevity and conciseness.
Preferably, the reaction in step (2) is carried out under the conditions of temperature rise and vacuum pumping.
Preferably, the method of raising temperature and evacuating comprises: heating the system to 170-180 deg.C (such as 171 deg.C, 172 deg.C, 173 deg.C, 174 deg.C, 175 deg.C, 176 deg.C, 177 deg.C, 178 deg.C or 179 deg.C), and vacuumizing to-0.05-0.07 Mpa (such as-0.052 Mpa, -0.054Mpa, -0.056Mpa, -0.058Mpa, -0.06Mpa, -0.062Mpa, -0.064Mpa, -0.066Mpa or-0.068 Mpa); keeping for 0.5-1.5 h (such as 0.6h, 0.7h, 0.8h, 0.9h, 1h, 1.1h, 1.2h, 1.3h or 1.4 h); and stopping vacuumizing, and keeping for 1-2 h (for example, 1.1h, 1.2h, 1.3h, 1.4h, 1.5h, 1.6h, 1.7h, 1.8h or 1.9 h) to finish the temperature rising and vacuumizing.
Preferably, the temperature of the vulcanization in the step (3) is 120-130 ℃, for example 121 ℃, 122 ℃, 123 ℃, 124 ℃, 125 ℃, 126 ℃, 127 ℃, 128 ℃ or 129 ℃, and the specific values therebetween are limited by space and for the sake of brevity, and the invention is not exhaustive of the specific values included in the range.
Preferably, the vulcanizing time of the step (3) is 10-20 min, such as 11min, 12min, 13min, 14min, 15min, 16min, 17min, 18min or 19min, and the specific values therebetween are limited by space and for the sake of brevity, and the invention is not exhaustive.
As a preferred technical scheme, the preparation method comprises the following steps:
(1) mixing vinyl raw rubber and white carbon black for 1-3 hours at the temperature of less than 80 ℃ to obtain mixed base rubber;
(2) mixing the mixed base rubber obtained in the step (1), silicon rubber, hydroxyl silicone oil, boric acid and a flame retardant for 1-3 hours at room temperature, and reacting under the conditions of temperature rise and vacuum pumping to obtain mixed rubber; the method for heating and vacuumizing comprises the following steps: heating the system to 170-180 ℃, and vacuumizing to-0.05 to-0.07 Mpa; keeping for 0.5-1.5 h; stopping vacuumizing, and keeping for 1-2 h to finish the temperature rise and the vacuumizing;
(3) and (3) vulcanizing the mixing glue obtained in the step (2) and a vulcanizing agent at 120-130 ℃ for 10-20 min to obtain the self-adhesive glue.
In a third aspect, the use of a self-adhesive according to the first aspect in a battery.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the self-adhesive provided by the invention, the combination of vinyl crude rubber, silicon rubber, hydroxyl silicone oil, boric acid, white carbon black, a composite flame retardant and a vulcanizing agent in a specific part is added into the preparation raw materials, so that the finally prepared self-adhesive has excellent mechanical property, self-adhesiveness and flame retardant property. Specifically, the silicon rubber and the boric acid in specific parts are added into the preparation raw materials to react with each other, so that the self-adhesive property of the self-adhesive is improved; the white carbon black and the composite flame retardant are further added in specific parts, so that the self-adhesive has excellent mechanical properties and flame retardance, and the preparation process of the self-adhesive is simple, suitable for batch industrial production and has important research value.
(2) Specifically, the self-adhesive performance of the self-adhesive glue obtained by the invention is 4.7-6.3N/cm; the flame retardant property can reach V0-V1 level; the tensile strength is 5.1-9.0 MPa; the elongation at break is 510-730%; the dielectric strength is 28-29 kV/mm; the high-temperature insulation resistance is 3.0 multiplied by 105 to 4.6 multiplied by 105; and no burn-through phenomenon occurs.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The self-adhesive comprises the following raw materials in parts by weight:
wherein the average molecular weight of the vinyl raw rubber is 500000Da and is derived from (Hesheng silicon industry, 110 type); the mesh number of the fumed silica is 80000 meshes; 107 silicone rubber has a viscosity of 500000cst and a molecular weight of 150000 Da; the viscosity of the hydroxyl silicone oil is 40mm2(ii)/s, from (Jiangsu Hokkendo chemical);
the preparation method of the self-adhesive provided by the embodiment comprises the following steps:
(1) mixing vinyl raw rubber and gas-phase white carbon black for 2 hours at the temperature of 25 ℃ to obtain mixed base rubber;
(2) mixing the mixed base rubber obtained in the step (1), 107 silicon rubber, hydroxyl silicone oil, boric acid, antimony trioxide and decabromodiphenylethane at room temperature for 2 hours, and reacting under the conditions of temperature rise and vacuum pumping to obtain mixed rubber; the method for heating and vacuumizing comprises the following steps: heating the system to 175 ℃, vacuumizing to-0.06 Mpa, and keeping for 0.75 h; stopping vacuumizing, keeping for 1.5h, and finishing the temperature rising and vacuumizing;
(3) and (3) vulcanizing the mixed glue obtained in the step (2) and 2, 4-dichloro benzoyl peroxide at 125 ℃ for 15min to obtain the self-adhesive glue.
Example 2
The self-adhesive comprises the following raw materials in parts by weight:
wherein the average molecular weight of the vinyl raw rubber is 300000Da and is sourced from (Hesheng silicon industry, 110 type); the mesh number of the fumed silica is 70000 meshes; 107 silicone rubber has a viscosity of 300000cst and a molecular weight of 90000 Da; the viscosity of the hydroxyl silicone oil is 40mm2(ii)/s, from (Jiangsu Hokkendo chemical);
the preparation method of the self-adhesive provided by the embodiment comprises the following steps:
(1) mixing vinyl raw rubber and gas-phase white carbon black for 1h at the temperature of 70 ℃ to obtain mixed base rubber;
(2) mixing the mixed base rubber obtained in the step (1), 107 silicon rubber, hydroxyl silicone oil, boric acid, antimony trioxide and decabromodiphenyl ether at room temperature for 1h, and reacting under the conditions of temperature rise and vacuum pumping to obtain mixed rubber; the method for heating and vacuumizing comprises the following steps: heating the system to 170 ℃, vacuumizing to-0.07 Mpa, and keeping for 1.5 h; stopping vacuumizing, keeping for 2 hours, and finishing the heating and vacuumizing;
(3) and (3) vulcanizing the mixing glue obtained in the step (2) and 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane at 120 ℃ for 20min to obtain the self-adhesive glue.
Example 3
The self-adhesive comprises the following raw materials in parts by weight:
wherein the average molecular weight of the vinyl raw rubber is 600000Da and is sourced from (Hesheng silicon industry, 110 type); the mesh number of the fumed silica is 90000 meshes; 107 silicone rubber has a viscosity of 1000000cst and a molecular weight of 200000 Da; the viscosity of the hydroxyl silicone oil is 40mm2(ii)/s, from (Jiangsu Hokkendo chemical);
the preparation method of the self-adhesive provided by the embodiment comprises the following steps:
(1) mixing vinyl raw rubber and gas-phase white carbon black for 3 hours at the temperature of 15 ℃ to obtain mixed base rubber;
(2) mixing the mixed base rubber obtained in the step (1), 107 silicon rubber, hydroxyl silicone oil, boric acid, antimony trioxide and tetrahexabisphenol A at room temperature for 3 hours, and reacting under the conditions of temperature rise and vacuum pumping to obtain mixed rubber; the method for heating and vacuumizing comprises the following steps: heating the system to 180 ℃, and vacuumizing to-0.05 Mpa; keeping for 0.5 h; stopping vacuumizing, keeping for 0.5h, and finishing the temperature rising and vacuumizing;
(3) and (3) vulcanizing the mixing glue obtained in the step (2) and dicumyl peroxide at 130 ℃ for 10min to obtain the self-adhesive glue.
Example 4
A self-adhesive which differs from the adhesive of example 1 only in that antimony trioxide is added in an amount of 12.5 parts by weight, decabromodiphenylethane is added in an amount of 12.5 parts by weight, and the other components, amounts and preparation methods are the same as those of example 1.
Example 5
A self-adhesive which differs from the adhesive of example 1 only in that the amount of antimony trioxide added is 5 parts by weight, the amount of decabromodiphenylethane added is 20 parts by weight, and the other components, the amounts and the preparation method are the same as those of example 1.
Example 6
A self-adhesive which differs from the adhesive of example 1 only in that the amount of antimony trioxide added is 15 parts by weight, the amount of decabromodiphenylethane added is 10 parts by weight, and the other components, the amounts and the preparation method are the same as those of example 1.
Example 7
A self-adhesive which differs from example 1 only in that antimony trioxide is added in an amount of 2.5 parts by weight, decabromodiphenylethane is added in an amount of 22.5 parts by weight, and the other components, amounts and preparation methods are the same as in example 1.
Example 8
A self-adhesive glue differs from example 1 only in that instead of a vinyl gum with a molecular weight of 500000Da, a vinyl gum with a molecular weight of 200000Da (Hoseiko) is used, the other components, amounts and preparation method being the same as in example 1.
Example 9
A self-adhesive glue which differs from example 1 only in that instead of a vinyl gum with a molecular weight of 500000Da a vinyl gum with a molecular weight of 700000Da (hesheng silicon) is used, the other components, amounts and preparation method being the same as in example 1.
Comparative example 1
A self-adhesive which differs from the adhesive of example 1 only in that the amount of antimony trioxide added is 25 parts by weight, decabromodiphenylethane is not added, and the other components, the amounts and the preparation method are the same as those of example 1.
Comparative example 2
A self-adhesive which differs from example 1 only in that decabromodiphenylethane is added in an amount of 25 parts by weight, antimony trioxide is not added, and the other components, the amounts and the preparation method are the same as in example 1.
Comparative example 3
A self-adhesive, which is different from the adhesive of example 1 only in that fumed silica is not added, and other components, the using amount and the preparation method are the same as those of example 1.
And (3) performance testing:
(1) self-adhesive performance: testing according to ASTM D2148 test standard;
(2) flame retardant property: testing according to UL94-V0 test standard;
(3) tensile strength and elongation at break: testing according to ASTM D3759;
(4) dielectric strength: testing according to IEC 60243 test standard;
(5) high-temperature insulation resistance: testing according to IEC 60245 test standard;
(6) high temperature resistance: and (3) applying test flame to the center of the test piece at the flame temperature of 1000 +/-200 ℃, carrying out a high-temperature resistance test for 5min, and observing whether the test piece is burnt through/melted.
The self-adhesive glues provided in examples 1 to 9 and comparative examples 1 to 3 were tested according to the test method described above, and the results are shown in table 1:
TABLE 1
As can be seen from the data in table 1: the self-adhesive provided by the invention has excellent comprehensive performance; specifically, the self-adhesive obtained in the embodiments 1 to 9 has a self-adhesive property of 4.7 to 6.3N/cm; the flame retardant property can reach V0-V1 level; the tensile strength is 5.1-9.0 MPa; the elongation at break is 510-730%; the dielectric strength is 28-29 kV/mm; high temperature insulation resistance of 3.0 × 105～4.6×105(ii) a And no burn-through phenomenon occurs.
Comparing the example 1 with the comparative examples 1-2, it can be found that the flame retardant property of the self-adhesive is reduced by adopting a single flame retardant, and a burn-through phenomenon occurs; comparing example 1 with comparative example 3, it can be seen that the tensile strength, self-adhesive property and dielectric strength of the self-adhesive obtained without adding fumed silica are all reduced.
Further comparing example 1 with examples 4-7, it can be found that the self-adhesive obtained by using the antimony trioxide and the decabromodiphenylethane in the composite flame retardant in a preferred range, which is not limited in the application, can not burn through, but the flame retardant performance is reduced to some extent; further comparing examples 1 and 8 to 9, it was found that the tensile strength and self-adhesive properties of the self-adhesive obtained using the vinyl raw rubber having a relatively low molecular weight were reduced, while the self-adhesive obtained using the vinyl raw rubber having a relatively high molecular weight was difficult to process although excellent in properties.
The applicant states that the present invention is illustrated by the above examples of a self-adhesive and a method for its preparation and use, but the present invention is not limited to the above examples, i.e. it does not mean that the present invention must be implemented by means of the above examples. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
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