CN114231247A - Room-temperature-curing two-component addition-type self-adhesive high-temperature-resistant silica gel and preparation method thereof - Google Patents
Room-temperature-curing two-component addition-type self-adhesive high-temperature-resistant silica gel and preparation method thereof Download PDFInfo
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on 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; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
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Abstract
The invention provides room-temperature curing double-component addition type self-adhesive high-temperature-resistant silica gel which consists of an agent A and an agent B, wherein the mass ratio of the agent A to the agent B is 1: 1; the agent A comprises the following components in parts by weight: 0-30 parts of base rubber, 15-65 parts of vinyl silicone oil, 35-75 parts of filler, 0-10 parts of iron oxide red, 0-5 parts of heat-resistant agent, 0.05-5 parts of platinum catalyst and 1-8 parts of tackifier; the agent B comprises the following components in parts by weight: 0-30 parts of base rubber, 15-65 parts of vinyl silicone oil, 35-75 parts of filler, 0-5 parts of heat-resistant agent, 0.1-15 parts of cross-linking agent, 1-8 parts of tackifier and 0-5 parts of inhibitor; the preparation method of the tackifier comprises the following steps: (1) synthesizing a tackifier main agent; (2) synthesizing the tackifier by the tackifier main agent. The two-component addition type silica gel can be deeply cured at room temperature and effectively bonded with a metal base material, has the characteristic of high temperature resistance, and can stably work at 200-350 ℃ for a long time.
Description
Technical Field
The invention belongs to the technical field of adhesives, and relates to room-temperature-curing double-component addition-type self-adhesive high-temperature-resistant silica gel.
Background
The addition type liquid silica gel is an organic silicon product with the advantages of rapid development, high grade, large technical content of the product and high added value in recent years, and has the characteristics of high heating and vulcanizing speed, high production efficiency, low comprehensive cost and the like. The method is often applied to packaging electronic components, electrical equipment, fabrics, medical materials and the like. However, it also has the disadvantages of poor adhesion to various types of substrates and slow adhesion speed in the normal state, which is particularly prominent in room temperature curing addition type silicone gels. Aiming at the defect of poor bonding performance, methods such as treating a base material by using a base coat or adding a performance tackifier into a rubber material are adopted to solve the problem.
At present, related reports of adding a tackifier into room temperature curing addition type silica gel are provided, for example, in patent CN201811165355, "an addition type room temperature bonding two-component pouring sealant and a preparation method thereof," a pouring sealant is disclosed, the component a of the pouring sealant comprises vinyl silicone oil, aluminum oxide, silicon micropowder and a platinum catalyst, the component B of the pouring sealant comprises vinyl silicone oil, aluminum oxide, silicon micropowder, hydrogen-containing silicone oil, an inhibitor and a tackifier, wherein the tackifier is siloxane oligomer containing silicon hydride and acryloxy groups, and the two-component pouring sealant improves the bonding strength of the pouring sealant to stainless steel, aluminum and other base materials at room temperature by adding the novel tackifier and compounding the components, and solves the problems of large odor, low efficiency, solvent volatilization and the like of the traditional addition type pouring sealant using a base coat. However, the tackifier has the following disadvantages: (1) the platinum catalyst is added during synthesis, and cannot be separated and removed after the reaction is finished, redundant active hydrogen has the risk of self-polymerization dehydrogenation under the action of the platinum catalyst, and certain negative effects are caused on the storage stability of the tackifier and the pouring sealant, such as abnormal fluctuation of viscosity after long-term storage, gelation of the tackifier, hardening of glue and the like; (2) the hydrosilylation reaction activity of methacryloxypropyl in 3-methacryloxypropyl trimethoxy silane is poor, the grafting rate of the methacryloxypropyl with tetramethylcyclotetrasiloxane is not high or the methacryloxypropyl with tetramethylcyclotetrasiloxane is caused to remain in a tackifier, the grafting rate is easy to generate self polymerization or isomerization under the conditions of heating, illumination and the like, and finally the problems of slow curing or deep curing failure, unstable adhesion property or accidental failure of pouring sealant, poor adhesion at low temperature (the room temperature is lower than 20 ℃) and the like are caused.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides room-temperature-cured two-component addition type self-adhesive high-temperature-resistant silica gel which can be deeply cured at room temperature and effectively adhered to a metal substrate, has the characteristic of high temperature resistance and can stably work at 200-350 ℃ for a long time.
The technical scheme adopted for realizing the above purpose of the invention is as follows:
the room-temperature curing double-component addition type self-adhesive high-temperature-resistant silica gel is characterized in that: the agent A consists of an agent A and an agent B, wherein the mass ratio of the agent A to the agent B is 1: 1; the agent A comprises the following components in parts by weight: 5-30 parts of base rubber, 15-65 parts of vinyl silicone oil, 35-75 parts of filler, 1.5-10 parts of iron oxide red, 1-5 parts of heat-resistant agent, 0.05-5 parts of platinum catalyst and 1-8 parts of tackifier; the agent B comprises the following components in parts by weight: 1-30 parts of base rubber, 15-65 parts of vinyl silicone oil, 35-75 parts of filler, 1-5 parts of heat-resistant agent, 0.1-15 parts of cross-linking agent, 1-8 parts of tackifier and 0.1-5 parts of inhibitor;
the preparation method of the tackifier comprises the following steps: (1) after nitrogen is introduced into a flask, adding 10-200 parts of hydroxyl silicone oil and 0.1-20 parts of alcohol compound into the flask, uniformly stirring, adding 0.1-20 parts of organic titanium compound, fully stirring and dissolving, dropwise adding 0.5-200 parts of silane coupling agent, reacting at 30-120 ℃ for 0.5-8 h while keeping the temperature, distilling at 30-150 ℃ under reduced pressure for 1-8 h, cooling and filtering to obtain a tackifier main agent; (2) introducing nitrogen into a flask, adding 5-100 parts of tackifier main agent into the flask, adding 5-100 parts of organic titanium compound and 5-100 parts of silane coupling agent, uniformly stirring, filtering, and directly using or using after heat preservation at 50-150 ℃ for 1-7 h, cooling and filtering, wherein the obtained product is colorless to orange red transparent viscous liquid, and discharging to obtain the tackifier.
The tackifier preparation method comprises the following components in the step (1) in parts by weight: 90-120 parts of hydroxyl silicone oil, 1-5 parts of alcohol compound, 0.1-1 part of organic titanium compound and 15-30 parts of silane coupling agent; the components and the weight ratio in the step (2) are as follows: 90-100 parts of tackifier main agent, 35-45 parts of organic titanium compound and 5-15 parts of silane coupling agent.
The general structural formula of the hydroxyl silicone oil is as follows:
wherein a is more than 0, and b is more than or equal to 0; the hydroxyl silicone oil is one or a mixture of more than two according to the general formula, and the viscosity of the hydroxyl silicone oil is 5-5000 cSt.
The silane coupling agent is one or a mixture of more than two of ethyl orthosilicate, methyl orthosilicate, methyltriethoxysilane, methyltrimethoxysilane, dimethyldiethoxysilane, dimethyldimethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, methylphenyldimethoxysilane and diphenyldimethoxysilane.
The alcohol compound is one or a mixture of more than two of alcohol compounds containing no more than 6 carbon atoms; the organic titanium compound is one or a mixture of more than two of isopropyl titanate, n-butyl titanate and titanate chelate.
The base adhesive is a product formed by kneading fumed silica and vinyl silicone oil according to a mass ratio of (2-3.5): (6.5-8) at 120-180 ℃ and (0.09-0.1) MPa for 2-6 h and defoaming, and a silane coupling agent or silazane is added in the kneading process for end-capping treatment, wherein the viscosity of the vinyl silicone oil is 100-20000 mPa s, and the specific surface area of the fumed silica is 150-380.
The filler is one or a mixture of more than two of 200-3000-mesh silicon micropowder, nano calcium carbonate, zinc oxide, aluminum hydroxide, fumed silica and diatomite.
The cross-linking agent is low-hydrogen silicone oil with hydrogen content wt being 0.1-1.2%; the inhibitor is an alkynol inhibitor or a modified alkynol inhibitor.
The platinum catalyst is a Karster catalyst, and the concentration of the platinum catalyst is 1000-5000 ppm; the heat-resistant agent is one or a mixture of more than two of vapor-phase titanium dioxide, rhodium metal oxide, zinc oxide, chromium oxide, an antioxidant, a yellow-resistant agent and a diluent.
The invention also provides a preparation method of the room-temperature curing two-component addition type self-adhesive high-temperature-resistant silica gel, which comprises the following steps: (1) putting the base rubber and the vinyl silicone oil into a power mixer, uniformly mixing, then sequentially adding the filler, the iron oxide red and the heat-resistant agent, heating to 80-200 ℃, mixing for 1-5 h under a vacuum condition, cooling to room temperature, sequentially adding the platinum catalyst and the tackifier, uniformly mixing, defoaming and discharging to obtain an agent A;
(2) and (2) putting the base rubber and the vinyl silicone oil into a power mixer, uniformly mixing, then sequentially putting the filler and the heat-resistant agent, heating to 80-200 ℃, mixing for 1-5 h under a vacuum condition, cooling to room temperature, sequentially putting the cross-linking agent, the tackifier and the inhibitor, uniformly mixing, defoaming, and discharging to obtain the B agent.
Compared with the prior art, the invention has the following advantages: (1) the tackifier in the room-temperature-curing two-component addition-type self-adhesive high-temperature-resistant silica gel is a self-made tackifier, contains glycidyl ether oxypropyl, vinyl, alkoxy and methacryloxypropyl groups, and is suitable for adhering various base materials, such as carbon steel, stainless steel, aluminum alloy, polyamide (such as PA66), glass fiber, PCB, polycarbonate and the like. The tackifier is synthesized by a two-step method, a tackifying main agent is synthesized firstly, and the structural general formula of the tackifying main agent is as follows:
wherein a is more than 0, b is more than or equal to 0, and c + d is 2;
the tackifying main agent has good stability, is convenient to produce and stock, and can be independently stored for a long time; when glue preparation is needed, adding an organic titanium compound and a silane coupling agent into the tackifying main agent to synthesize a tackifier for later use; on one hand, when the self-made tackifier is bonded with the base material, the titanium element generates an inducing effect on the tackifier main agent, so that the effect of assisting adhesion and reducing the bonding activation temperature can be achieved; on the other hand, the introduction of the silane coupling agent is beneficial to improving the polarity difference between the tackifier and the base material, and can play a role in improving the wetting degree between the tackifier and the base material, so that the bonding effect is further improved. Therefore, the addition type silica gel product reasonably prepared by the self-made tackifier can be cured in a lower temperature environment (room temperature) and can form a good bonding effect with various base materials.
The tackifier is synthesized by a two-step method, so that excessive organic titanium compounds can be prevented from being added at one time, adverse effects of overhigh crosslinking degree, gelation and the like of products caused by rapid reaction of hydroxyl silicone oil, alcohol compounds and silane coupling agents in a short time under the catalytic action of the organic titanium compounds can be avoided, and the stable and appropriate synthetic reaction and stable products of the tackifier can be ensured. In addition, the tackifier provided by the invention has a structure similar to a dendritic structure and contains a silicon hydroxyl group. Therefore, hydrogen bond action is formed among tackifier molecules and between the tackifier molecules and other materials (silicone oil, base glue, silicon micropowder and the like), so that the thixotropy of the glue is improved, the storage stability of the glue is improved, and the problem of filler settlement and hardening in the long-term glue storage process is solved.
(2) The room temperature curing two-component addition type self-adhesive high-temperature-resistant silica gel provided by the invention can be deeply cured at room temperature, can form effective adhesion with metal base materials and the like without high-temperature curing, is suitable for glue-pouring sealing protection of medium and large metal pieces, such as potting of a wind power generator rotor, potting of a high-temperature high-efficiency filter and the like, and has the characteristics of convenience in use and good applicability.
(3) The room temperature curing two-component addition type self-adhesive high-temperature-resistant silica gel provided by the invention is reinforced by adding the base adhesive, so that the silica gel has excellent mechanical properties (tensile strength, elongation at break, tearing strength and the like), and the base adhesive has low cost and low application cost; in addition, base glue is added into the agent A and the agent B, so that the data of the agent A/B in the aspects of viscosity, specific gravity and the like are kept basically consistent, and glue production is conveniently carried out by using semi-automatic or full-automatic pneumatic glue dispensing equipment.
(4) According to the invention, various fillers and additives, such as iron oxide red, silicon micropowder, fumed silica, a heat-resistant agent and the like, are reasonably matched according to a certain proportion, so that the product has the characteristic of high temperature resistance, the dispersibility of the fillers is improved by adding the heat-resistant agent, the fillers are uniformly dispersed, the heat resistance is further improved, and the product can stably work at 200-350 ℃ for a long time.
Drawings
FIG. 1 is a diagram showing the state of a sample block in example 1 after aging test at 250 ℃ for 300 hours;
FIG. 2 is a diagram showing the state of the sample block in example 2 after aging test at 350 ℃ for 300 hours;
FIG. 3 is a diagram showing the state of the sample block in comparative example 1 after aging test at 350 ℃ for 300 hours;
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention is further described in detail with reference to the following examples.
The base adhesive in the room-temperature curing two-component addition type self-adhesive high-temperature-resistant silica gel provided in the embodiment is a product obtained by kneading fumed silica with a specific surface area of 200 and vinyl silicone oil with a viscosity of 5000mPa · s at 165 ℃ and under-0.095 MPa for 5 hours and defoaming, wherein the mixing mass ratio of the fumed silica to the vinyl silicone oil is 3.5: 6.5.
Tackifiers X-1 and X-2 were used in the following examples and were prepared by the following methods, respectively:
preparation of tackifier X-1: (1) after nitrogen is introduced into a flask, 500g of hydroxy silicone oil with the viscosity of 35cSt and the hydroxyl content of 7.5 wt% and 7.5g of ethylene glycol are added into a 1000mL four-neck flask, 2g of isopropyl titanate are added after uniform stirring and fully stirred until the hydroxy silicone oil and the 7.5g of ethylene glycol are completely dissolved, 20.82g of vinyl trimethoxy silane and 33.21g of a mixture of gamma-glycidyl ether oxypropyl trimethoxy silane and 34.90g of gamma-methacryloxypropyl trimethoxy silane are added dropwise, the dropwise adding speed is 180 drops/minute, the dropwise adding is finished within about 30 minutes, the temperature is raised to 85 ℃, after 2.5 hours of heat preservation reaction, the mixture is distilled under reduced pressure at-0.095 MPa and 90 ℃ for 4 hours, the temperature is lowered, and then filtered to obtain 550.29g of light yellow transparent viscous liquid, namely the tackifier main agent-1, and the tackifier is sealed and stored for later use. (2) After nitrogen is introduced into a flask, 100g of tackifier main agent-1 is added into a 500mL three-neck flask, 50g of a mixture of n-butyl titanate and methyltrimethoxysilane (mass ratio is 4:1) is dropwise added at a dropping speed of 120 drops/min for about 25 min, the dropwise addition is finished, the temperature is kept at 85 ℃ for 2h, 148.5g of light yellow transparent viscous liquid is obtained, namely the target product tackifier X-1, and the light yellow transparent viscous liquid is sealed and stored for later use.
Preparation of tackifier X-2: (1) after nitrogen is introduced into a flask, 500g of hydroxy vinyl silicone oil with the viscosity of 31cSt, the hydroxyl content wt being 6.0 percent and the vinyl content wt being 6.0 percent, 4g of isopropanol and 2g of ethylene glycol are added into a 1000mL four-neck flask, 1.5g of n-butyl titanate is added after uniform stirring, the mixture is fully stirred until the mixture is completely dissolved, the temperature is increased to 80 ℃, 52.11g of gamma-glycidyl ether oxypropyl trimethoxy silane and 56.0g of gamma-methacryloxypropyl trimethoxy silane are added dropwise at the dropping speed of 180 drops/minute, the dropping is completed within about 45 minutes, after the reaction is carried out at the temperature of 85 ℃ for 3 hours, the mixture is distilled under reduced pressure for 5 hours at the pressure of-0.095 MPa and the temperature of 90 ℃, and is filtered after the temperature is reduced to obtain 568.40g of light yellow transparent viscous liquid, namely a tackifier main agent-2, and the tackifier main agent is sealed and stored for later use. (2) After nitrogen is introduced into a flask, 100g of tackifier main agent-2 is added into a 500mL three-neck flask, 50g of a mixture of titanate chelate and ethyl orthosilicate (mass ratio is 5:1) is dropwise added, the dropwise adding speed is 120 drops/min, the dropwise adding is finished within about 25 min, after the temperature preservation reaction at 85 ℃ is carried out for 2h, the distillation is carried out under reduced pressure at-0.095 MPa and 85 ℃ for 1h, 133g of orange-red transparent viscous liquid is obtained, namely the target product tackifier X-2, and the orange-red transparent viscous liquid is sealed and stored for later use in dark place.
Example 1:
the preparation method comprises the following steps of: (1) putting the base rubber and the vinyl silicone oil into a power mixer, uniformly mixing, then sequentially adding the filler, the iron oxide red and the heat-resistant agent, heating to 80-200 ℃, mixing for 1-5 h under a vacuum condition, cooling to room temperature, sequentially adding the platinum catalyst and the tackifier, uniformly mixing, defoaming and discharging to obtain an agent A; (2) and (2) putting the base rubber and the vinyl silicone oil into a power mixer, uniformly mixing, then sequentially putting the filler and the heat-resistant agent, heating to 80-200 ℃, mixing for 1-5 h under a vacuum condition, cooling to room temperature, sequentially putting the cross-linking agent, the tackifier and the inhibitor, uniformly mixing, defoaming, and discharging to obtain the B agent.
After the preparation of the agent A and the agent B, the viscosity of the agent A is 5500cP, the specific gravity is 1.55, the viscosity of the agent B is 5552cP, the specific gravity is 1.558, glue preparation is carried out according to the mass ratio of the agent A to the agent B of 1:1, the mixing viscosity is 5490cP, the specific gravity is 1.556, and the glue preparation operation time of the agent A and the agent B is 4h (25 ℃). A sample block was prepared, which had a hardness of 58A, a tensile strength of 2.2MPa, an elongation of 96% and a tear strength of 11.5 KN/m. The adhesion strength between the silica gel and the substrate was tested according to GB/T13936-. The sample piece is subjected to an aging test at 250 ℃, and after 300 hours, the sample piece has no degumming, no bulge, no cracking and no obvious change in color, and as shown in figure 1, the hardness climbing is small (60A), the tensile strength is 1.7MPa, the elongation is 78%, and the tear strength is 9.2 KN/m. The agent A and the agent B are stored in a closed condition at room temperature for 12 months, the appearance properties of the agent A and the agent B are not obviously changed, and the phenomenon of thickening or hardening is avoided.
Example 2:
the preparation method comprises the following steps of: (1) putting the base rubber and the vinyl silicone oil into a power mixer, uniformly mixing, then sequentially adding the filler, the iron oxide red and the heat-resistant agent, heating to 80-200 ℃, mixing for 1-5 h under a vacuum condition, cooling to room temperature, sequentially adding the platinum catalyst and the tackifier, uniformly mixing, defoaming and discharging to obtain an agent A; (2) and (2) putting the base rubber and the vinyl silicone oil into a power mixer, uniformly mixing, then sequentially putting the filler and the heat-resistant agent, heating to 80-200 ℃, mixing for 1-5 h under a vacuum condition, cooling to room temperature, sequentially putting the cross-linking agent, the tackifier and the inhibitor, uniformly mixing, defoaming, and discharging to obtain the B agent.
After the preparation of the agent A and the agent B, the viscosity of the agent A is 9750cP, the specific gravity is 1.581, the viscosity of the agent B is 9800cP, the specific gravity is 1.579, the glue is prepared according to the mass ratio of the agent A to the agent B of 1:1, the mixing viscosity is 9810cP, and the specific gravity is 1.580. The glue preparation operation time of the agent A and the agent B is 2h (25 ℃). A sample block was prepared, which had a hardness of 65A, a tensile strength of 2.0MPa, an elongation of 60% and a tear strength of 10 KN/m. The adhesion strength between the silica gel and the substrate was tested according to GB/T13936-. The sample piece is subjected to an aging test at 350 ℃, and after 300 hours, the sample piece has no degumming, no bulge and no cracking, the color is changed from brick red to date red, and as shown in figure 2, the hardness climbing is small (72A), the tensile strength is 1.4MPa, the elongation is 52 percent, and the tear strength is 8.1 KN/m. The agent A and the agent B are stored in a closed condition at room temperature for 12 months, the appearance properties of the agent A and the agent B are not obviously changed, and the phenomenon of thickening or hardening is avoided.
Comparative example 1:
the preparation method comprises the following steps of: (1) putting the base rubber and the vinyl silicone oil into a power mixer, uniformly mixing, then sequentially adding the filler, the iron oxide red and the heat-resistant agent, heating to 80-200 ℃, mixing for 1-5 h under a vacuum condition, cooling to room temperature, sequentially adding the platinum catalyst and the tackifier main agent, uniformly mixing and defoaming, and discharging to obtain an agent A; (2) and (2) putting the base rubber and the vinyl silicone oil into a power mixer, uniformly mixing, then sequentially putting the filler and the heat-resistant agent, heating to 80-200 ℃, mixing for 1-5 h under a vacuum condition, cooling to room temperature, sequentially putting the cross-linking agent, the tackifier main agent and the inhibitor, uniformly mixing and defoaming, and discharging to obtain the B agent.
After the agent A and the agent B were prepared, the viscosity of the agent A was measured to be 9430cP, the specific gravity was measured to be 1.579, the viscosity of the agent B was measured to be 9620cP, the specific gravity was measured to be 1.578, and the mixing was carried out at a mass ratio of the agent A to the agent B of 1:1, the mixing viscosity was measured to be 9520cP, and the specific gravity was measured to be 1.578. The glue preparation operation time of the agent A and the agent B is 1.5h (25 ℃). A sample block was prepared, which had a hardness of 62A, a tensile strength of 1.9MPa, an elongation of 62% and a tear strength of 10.3 KN/m. The adhesive strength between the silica gel and the substrate was tested according to GB/T13936-. The aging test is carried out at 350 ℃, a sample piece solidified at 80 ℃ is adopted, the color is changed from brick red to date red after 300h, and large-area degumming appears at the same time, as shown in figure 3. The glue sample is stored for 12 months in a closed condition at room temperature, the appearance properties of the agent A and the agent B are not obviously changed, and the phenomenon of thickening or hardening is avoided.
Compared with the embodiment 2, the adhesion strength of the glue is obviously attenuated or even fails by simply adopting the tackifier main agent-2 to replace the tackifier X-2. The adhesive strength can be kept at a certain level during medium-temperature curing, but the strength is far lower than that when the tackifier X-2 is used, and obvious peeling occurs to different substrates during low-temperature curing. In addition, large-area degumming occurs to the sample pieces after the high-temperature aging test. Therefore, compared with the tackifier main agent-2, the tackifier X-2 has better low-temperature bonding activity, bonding strength and high-temperature aging stability.
Claims (10)
1. The room-temperature curing double-component addition type self-adhesive high-temperature-resistant silica gel is characterized in that: the agent A consists of an agent A and an agent B, wherein the mass ratio of the agent A to the agent B is 1: 1; the agent A comprises the following components in parts by weight: 5-30 parts of base rubber, 15-65 parts of vinyl silicone oil, 35-75 parts of filler, 1.5-10 parts of iron oxide red, 1-5 parts of heat-resistant agent, 0.05-5 parts of platinum catalyst and 1-8 parts of tackifier; the agent B comprises the following components in parts by weight: 1-30 parts of base rubber, 15-65 parts of vinyl silicone oil, 35-75 parts of filler, 1-5 parts of heat-resistant agent, 0.1-15 parts of cross-linking agent, 1-8 parts of tackifier and 0.1-5 parts of inhibitor;
the preparation method of the tackifier comprises the following steps: (1) after nitrogen is introduced into a flask, adding 10-200 parts of hydroxyl silicone oil and 0.1-20 parts of alcohol compound into the flask, uniformly stirring, adding 0.1-20 parts of organic titanium compound, fully stirring and dissolving, dropwise adding 0.5-200 parts of silane coupling agent, reacting at 30-120 ℃ for 0.5-8 h while keeping the temperature, distilling at 30-150 ℃ under reduced pressure for 1-8 h, cooling and filtering to obtain a tackifier main agent; (2) introducing nitrogen into a flask, adding 5-100 parts of tackifier main agent into the flask, adding 5-100 parts of organic titanium compound and 5-100 parts of silane coupling agent, uniformly stirring, filtering, and directly using or using after heat preservation at 50-150 ℃ for 1-7 h, cooling and filtering, wherein the obtained product is colorless to orange red transparent viscous liquid, and discharging to obtain the tackifier.
2. The room temperature curing two-component addition-type self-adhesive high temperature resistant silica gel as claimed in claim 1, wherein: the tackifier preparation method comprises the following components in the step (1) in parts by weight: 90-120 parts of hydroxyl silicone oil, 1-5 parts of alcohol compound, 0.1-1 part of organic titanium compound and 15-30 parts of silane coupling agent; the components and the weight ratio in the step (2) are as follows: 90-100 parts of tackifier main agent, 35-45 parts of organic titanium compound and 5-15 parts of silane coupling agent.
3. The room temperature curing two-component addition-type self-adhesive high temperature resistant silica gel as claimed in claim 1, wherein: the general structural formula of the hydroxyl silicone oil is as follows:
wherein a is more than 0, and b is more than or equal to 0; the hydroxyl silicone oil is one or a mixture of more than two according to the general formula, and the viscosity of the hydroxyl silicone oil is 5-5000 cSt.
4. The room temperature curing two-component addition-type self-adhesive high temperature resistant silica gel as claimed in claim 1, wherein: the silane coupling agent is one or a mixture of more than two of ethyl orthosilicate, methyl orthosilicate, methyltriethoxysilane, methyltrimethoxysilane, dimethyldiethoxysilane, dimethyldimethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, methylphenyldimethoxysilane and diphenyldimethoxysilane.
5. The room temperature curing two-component addition-type self-adhesive high temperature resistant silica gel as claimed in claim 1, wherein: the alcohol compound is one or a mixture of more than two of alcohol compounds containing no more than 6 carbon atoms; the organic titanium compound is one or a mixture of more than two of isopropyl titanate, n-butyl titanate and titanate chelate.
6. The room temperature curing two-component addition-type self-adhesive high temperature resistant silica gel as claimed in claim 1, wherein: the base adhesive is a product formed by kneading fumed silica and vinyl silicone oil according to a mass ratio of (2-3.5): (6.5-8) at 120-180 ℃ and (0.09-0.1) MPa for 2-6 h and defoaming, and a silane coupling agent or silazane is added in the kneading process for end-capping treatment, wherein the viscosity of the vinyl silicone oil is 100-20000 mPa s, and the specific surface area of the fumed silica is 150-380.
7. The room temperature curing two-component addition-type self-adhesive high temperature resistant silica gel as claimed in claim 1, wherein: the filler is one or a mixture of more than two of 200-3000-mesh silicon micropowder, nano calcium carbonate, zinc oxide, aluminum hydroxide, fumed silica and diatomite.
8. The room temperature curing two-component addition-type self-adhesive high temperature resistant silica gel as claimed in claim 1, wherein: the cross-linking agent is low-hydrogen silicone oil with hydrogen content wt being 0.1-1.2%; the inhibitor is an alkynol inhibitor or a modified alkynol inhibitor.
9. The room temperature curing two-component addition-type self-adhesive high temperature resistant silica gel as claimed in claim 1, wherein: the platinum catalyst is a Karster catalyst, and the concentration of the platinum catalyst is 1000-5000 ppm; the heat-resistant agent is one or a mixture of more than two of vapor-phase titanium dioxide, rhodium metal oxide, zinc oxide, chromium oxide, an antioxidant, a yellow-resistant agent and a diluent.
10. The preparation method of the room-temperature curing two-component addition type self-adhesive high-temperature-resistant silica gel as claimed in claim 1 is characterized by comprising the following steps: (1) putting the base rubber and the vinyl silicone oil into a power mixer, uniformly mixing, then sequentially adding the filler, the iron oxide red and the heat-resistant agent, heating to 80-200 ℃, mixing for 1-5 h under a vacuum condition, cooling to room temperature, sequentially adding the platinum catalyst and the tackifier, uniformly mixing, defoaming and discharging to obtain an agent A;
(2) and (2) putting the base rubber and the vinyl silicone oil into a power mixer, uniformly mixing, then sequentially putting the filler and the heat-resistant agent, heating to 80-200 ℃, mixing for 1-5 h under a vacuum condition, cooling to room temperature, sequentially putting the cross-linking agent, the tackifier and the inhibitor, uniformly mixing, defoaming, and discharging to obtain the B agent.
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Effective date of registration: 20230525 Address after: 518107, Zone A, 2nd Floor, Building A57, Xinwei Fourth Industrial Zone, Jiangshi Community, Gongming Office, Guangming New District, Shenzhen City, Guangdong Province Patentee after: Shenzhen Double bond Organic Silicon Technology Co.,Ltd. Address before: 432400 China Canada chemical industry park, Yingcheng City, Xiaogan City, Hubei Province Patentee before: HUBEI DOUBLE-BOND FINE CHEMICAL Co.,Ltd. |