UV / moisture dual-curing high-strength neutral dealcoholized RTV silicone rubber and preparation method thereof

Through UV/moisture dual curing technology and modified optical resin raw materials, the problem of insufficient curing effect and strength of RTV silicone rubber is solved, and the preparation of silicone rubber with high strength, weather resistance and environmental protection is achieved. It is suitable for glass curtain walls and other applications. Improves building safety and service life.

CN119193097AActive Publication Date: 2024-12-27SHENZHEN KANGLIBANG TECH
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Patent Information

Application Number
CN202411393016.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-10-08
Publication Date
2024-12-27
Estimated Expiration
2044-10-08

AI Technical Summary

Technical Problem

The curing effect and strength of existing RTV silicone rubbers are insufficient, resulting in a shortening of service life. The glass glue on the market contains irritating gases that are harmful to the human body and affect building safety.

Method used

UV/moisture dual curing high-intensity neutral dealcoholization RTV silicone rubber is used, and the modified photoresin and photoinitiator are used to cure moisture under UV light irradiation, using methacrylic acid, tetrabutyl ammonium bromide, and glycidol. Raw materials such as etheroxypropyl trimethoxysilane and hydroquinol promote rapid, deep curing and high-strength bonding of silicone rubber.

Benefits of technology

It improves the curing efficiency and depth of silicone rubber, enhances its tensile strength and weather resistance, extends its service life, reduces the release of irritating gases, and improves the safety and environmental protection of bonding effects to glass curtain walls and other adhesives.

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Abstract

The invention relates to the technical field of novel polymer organic silicon materials, and particularly discloses UV / moisture dual-curing high-strength neutral dealcoholization type RTV silicone rubber and a preparation method of the UV / moisture dual-curing high-strength neutral dealcoholization type RTV silicone rubber. The UV / moisture dual-curing high-strength neutral dealcoholized RTV silicone rubber is prepared from the following raw materials in parts by weight: 90 to 110 parts of terminated 107 silicone rubber, 10 to 20 parts of filler, 6 to 10 parts of cross-linking agent, 1 to 3 parts of coupling agent, 0.2 to 0.4 part of catalyst, 10 to 20 parts of modified light resin and 0.2 to 0.4 part of photoinitiator, the modified light resin is prepared from the following raw materials: glycidyl ether oxypropyl trimethoxy silane, methacrylic acid, hydroquinone and tetrabutylammonium bromide; according to the UV / moisture dual-curing high-strength neutral dealcoholization type RTV silicone rubber, the modified photoresin and the photoinitiator are utilized, and a moisture mixed curing mode is combined, so that the UV / moisture dual-curing high-strength neutral dealcoholization type RTV silicone rubber has relatively good curing efficiency and relatively high tensile strength and weather resistance.
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Description

Technical Field

[0001] The present application relates to the technical field of new polymer organic silicon materials, and in particular to a UV / moisture dual-curing high-strength neutral dealcoholization RTV silicone rubber and a preparation method thereof. Background Art

[0002] Alcohol-type room temperature vulcanized silicone rubber is an adhesive product that cures by releasing alcohol small molecules through contact with moisture. The substances released during curing are harmless small molecule alcohol substances, which have good weather resistance, fast volatilization and no corrosion. They are widely used in furniture decoration, construction industry and electronic products. Because glass curtain wall buildings are exposed to the air for a long time and are corroded by sunlight, rain and other factors, the glass glue sold in the market is mainly composed of dealcoholized, deoximized, and deacidified silicone glues, which contain volatile butanone, acetic acid and other strong irritating gases that are harmful to the human body. In order to save production costs, some manufacturers use white oil as the main body, which leads to oil seepage, debonding and debonding in the later stage, which seriously affects the safety of the building.

[0003] UV light-curing silicone materials have good mechanical and thermal stability. They are used in the construction field and have great advantages in improving strength and resistance to yellowing and mildew. However, there are currently problems such as insufficient deep curing, which leads to insufficient hardness and strength of the prepared silicone rubber, shortening the service life of the silicone rubber. Summary of the invention

[0004] In order to improve the curing effect and insufficient strength of existing RTV silicone rubber, the present application provides a UV / moisture dual-curing high-strength neutral dealcoholization type RTV silicone rubber and a preparation method thereof.

[0005] In the first aspect, the present application provides a UV / moisture dual-curing high-strength neutral dealcoholization RTV silicone rubber, which adopts the following technical solution: A UV / moisture dual-curing high-strength neutral dealcoholization RTV silicone rubber comprises the following raw materials in parts by weight: 90-110 parts of end-capped 107 silicone rubber, 10-20 parts of filler, 6-10 parts of crosslinking agent, 1-3 parts of coupling agent, 0.2-0.4 parts of catalyst, 10-20 parts of modified photoresin, and 0.2-0.4 parts of photoinitiator; the modified photoresin raw materials include glycidyloxypropyltrimethoxysilane, methacrylic acid, hydroquinone and tetrabutylammonium bromide.

[0006] By adopting the above technical scheme, methacrylic acid is used in the modified photoresin raw material to improve the photocuring efficiency of silicone rubber, so that silicone rubber can be quickly cured under UV light. At the same time, tetrabutylammonium bromide can act as a photoinitiator. The modification can further promote the UV curing process and improve the curing speed and depth of silicone rubber. Glycidyloxypropyltrimethoxysilane can use the epoxy group to react with the hydroxyl group on the surface of the substrate to generate a chemical bond, and the silane group forms a covalent bond with the silicone rubber, thereby promoting the prepared silicone rubber to adhere firmly to the surface of the substrate. Hydroquinone can improve the oxidation resistance and weather resistance of silicone rubber, thereby improving the durability of silicone rubber.

[0007] By using modified photoresin and photoinitiator, the prepared silicone rubber is cured under natural light or ultraviolet light in combination with moisture mixed curing, so that the prepared silicone rubber has better curing efficiency and higher tensile strength and weather resistance.

[0008] Fillers are used to enhance the strength and toughness of RTV silicone rubber. End-capped 107 silicone rubber molecules are linked by cross-linking agents to cure the end-capped 107 silicone rubber colloid. Adding catalysts can improve the curing efficiency of silicone rubber and enhance the curing effect of silicone rubber. The active groups generated by the hydrolysis of coupling agents are firmly adhered to the substrate, thereby improving the bonding strength of silicone rubber.

[0009] Preferably, the mass ratio of glycidyloxypropyltrimethoxysilane, methacrylic acid, hydroquinone and tetrabutylammonium bromide is: (0.8-1.2): 1: (0.01-0.03): (0.0001-0.0003).

[0010] Preferably, the cross-linking agent raw material includes methyl orthosilicate, a buffer and potassium hydroxide, and the mass ratio of the methyl orthosilicate, the buffer and potassium hydroxide is 1: (1.5-2.5): (0.0001-0.0003).

[0011] By adopting the above technical solution, potassium hydroxide is used as a catalyst to promote the condensation of methyl orthosilicate to form oligomers, which are connected with the end-capped 107 silicone rubber, thereby improving the curing efficiency of the silicone rubber and enhancing the strength and bonding performance of the silicone rubber.

[0012] Preferably, the preparation method of the cross-linking agent comprises the following specific steps: mixing methyl orthosilicate and a buffer, heating to 95-105° C., adding potassium hydroxide, reacting and condensing to obtain the cross-linking agent.

[0013] Preferably, the coupling agent raw materials include boron trichloride-ethanol solution, dichloromethane, Grignard reagent, trimethylsilanol and triphenylphosphine, and the mass ratio of the boron trichloride-ethanol solution, dichloromethane, Grignard reagent, trimethylsilanol and triphenylphosphine is 1:(0.8-1.2):(0.8-1.2):(2.5-3.5):(0.0001-0.0003).

[0014] Preferably, the boron trichloride-ethanol solution can promote the crosslinking reaction of the silicone rubber system and enhance the mechanical strength and weather resistance of the silicone rubber. The Grignard reagent is an organic magnesium compound that can react with the silane group in the silicone rubber to form a more stable chemical bond, enhance the crosslinking density of the silicone rubber, and improve the strength and hardness of the silicone rubber. Triphenylphosphine can be used as a catalyst to improve the curing efficiency of the silicone rubber.

[0015] Preferably, the method for preparing the coupling agent comprises the following specific steps: under the protection of nitrogen, mixing boron trichloride-ethanol solution, dichloromethane and Grignard reagent for reaction, standing for stratification, heating and filtering the supernatant to obtain borane, and then mixing borane with trimethylsilane and triphenylphosphine to obtain the coupling agent.

[0016] By adopting the above technical scheme, boron trichloride-ethanol solution, dichloromethane and Grignard reagent can carry out cross-coupling reaction of halogenated hydrocarbons, and the generated borane can form a coupling agent through condensation reaction with trimethylsilanol under the catalysis of triphenylphosphine. The obtained neutral coupling agent has borate groups, has better adhesion to glass, marble, wood and the like than traditional coupling agents, and is not easy to turn white and has good colloid transmittance.

[0017] Preferably, the end-capping 107 silicone rubber has a viscosity of 3000-20000 cps.

[0018] By adopting the above technical solution, the end-capped 107 silicone rubber at this viscosity has good extrusion and thixotropy, which is convenient for extrusion during gluing.

[0019] Preferably, the filler is fumed hydrophobic silica, and the surface area of ​​the fumed hydrophobic silica is ≥150m 2 / g, the catalyst is a chelated tin catalyst, and the photoinitiator is a ketone photoinitiator.

[0020] By adopting the above technical solution and using gas phase hydrophobic white carbon black, it is possible to reduce the condensation of water in the air into agglomerates after contacting the white carbon black during storage and transportation. At the same time, the surface area of ​​the gas phase hydrophobic white carbon black is not less than 150m 2 / g, it can promote the prepared silicone rubber to have higher strength. Ketone photoinitiators have higher initiation efficiency and better thermal stability, thereby improving the curing efficiency of silicone rubber. At the same time, ketone photoinitiators have no yellowing phenomenon and have better storage stability. Compared with other thiol photoinitiators, they have less irritating odor. Chelated tin catalysts have low tin content and high catalytic reaction activity, which can promote the prepared silicone rubber to have higher curing efficiency and strength.

[0021] In a second aspect, the present application provides a method for preparing a UV / moisture dual-curing high-strength neutral dealcoholization RTV silicone rubber, using the following technical solution: A method for preparing a UV / moisture dual-curing high-strength neutral dealcoholization RTV silicone rubber comprises the following specific steps: Under the protection of nitrogen, glycidyloxypropyltrimethoxysilane and methacrylic acid are mixed and heated for reaction, hydroquinone is added for reaction, and then tetrabutylammonium bromide is added for reaction to obtain a modified photoresist; The end-capped 107 silicone rubber is mixed with the modified photoresin and filler, and stirred evenly under a vacuum degree of -0.1-0.1MPa. Then a crosslinking agent, a coupling agent, a catalyst, and a photoinitiator are added and mixed, and stirred evenly to obtain a UV / moisture dual-curing high-strength neutral dealcoholization RTV silicone rubber.

[0022] By adopting the above technical scheme, by using modified photoresin to introduce photoinitiator, synergistically enhancing with other components, the silicone rubber is promoted to have higher curing efficiency, tensile strength and weather resistance.

[0023] In summary, this application has the following beneficial effects: 1. Since the present application adopts modified photoresin and photoinitiator, the prepared silicone rubber is cured under natural light or ultraviolet light in combination with moisture mixed curing to improve the curing efficiency of silicone rubber. Methacrylic acid and tetrabutylammonium bromide are used in the modified photoresin raw materials for synergistic enhancement, and the photoinitiator is introduced into the photoresin to further improve the curing efficiency and curing depth of silicone rubber. At the same time, the use of glycidyloxypropyltrimethoxysilane and hydroquinone in the modified photoresin raw materials can improve the strength and weather resistance of silicone rubber.

[0024] 2. In this application, oligomers formed by condensation of methyl orthosilicate, buffer and potassium hydroxide are used as crosslinking agents, which are connected with end-capped 107 silicone rubber to improve the curing efficiency of silicone rubber and enhance the strength and bonding performance of silicone rubber. A neutral coupling agent generated by the reaction of boron trichloride-ethanol solution, dichloromethane, Grignard reagent, trimethylsilanol and triphenylphosphine can enhance the crosslinking density of silicone rubber and improve the strength, hardness and weather resistance of silicone rubber. DETAILED DESCRIPTION

[0025] The present application is further described in detail below with reference to the embodiments.

[0026] All raw materials in the examples are commercially available. Example

[0027] Example 1 This embodiment provides a UV / moisture dual-curing high-strength neutral dealcoholization RTV silicone rubber, including the following raw materials by weight: 100 kg of end-capped 107 silicone rubber, 15 kg of filler, 8 kg of cross-linking agent, 2 kg of coupling agent, 0.3 kg of catalyst, 15 kg of modified photoresin, and 0.3 kg of photoinitiator. The filler is fumed hydrophobic silica, and the surface area of ​​the fumed hydrophobic silica is 150-300 m 2 / g, the catalyst is chelated tin catalyst C-103, the photoinitiator is ketone photoinitiator 1173, and the viscosity of the end-capped 107 silicone rubber is 10000cps.

[0028] The modified photoresin raw materials include glycidyloxypropyl trimethoxysilane, methacrylic acid, hydroquinone and tetrabutylammonium bromide, and the mass ratio of glycidyloxypropyl trimethoxysilane, methacrylic acid, hydroquinone and tetrabutylammonium bromide is 1:1:0.2:0.0002; the amount of methacrylic acid used is 100kg.

[0029] The cross-linking agent raw materials include methyl orthosilicate, a buffer and potassium hydroxide, wherein the buffer is ethanol, and the mass ratio of methyl orthosilicate, the buffer and potassium hydroxide is 1:2:0.0002; wherein the amount of methyl orthosilicate used is 100 kg.

[0030] The coupling agent raw materials include boron trichloride-ethanol solution, dichloromethane, Grignard reagent, trimethylsilanol and triphenylphosphine, and the mass ratio of boron trichloride-ethanol solution, dichloromethane, Grignard reagent, trimethylsilanol and triphenylphosphine is 1:1:1:3:0.0002; the amount of boron trichloride-ethanol solution used is 100kg.

[0031] A method for preparing a UV / moisture dual-curing high-strength neutral dealcoholization RTV silicone rubber comprises the following specific steps: S1: heating glycidyloxypropyltrimethoxysilane to 100°C, introducing nitrogen for protection, adding methacrylic acid, then adding hydroquinone, stirring at a speed of 300 rpm for 30 minutes, adding tetrabutylammonium bromide, mixing and reacting for 60 minutes, and then cooling to obtain a modified photoresist.

[0032] S2: Methyl orthosilicate and ethanol buffer are mixed, the temperature is raised to 100° C., potassium hydroxide is added, and the mixture is reacted at a rotation speed of 300 rpm for 120 min. Then, ethanol and small molecular products are recovered by filtration to obtain a cross-linking agent.

[0033] S3: Mix a 20% by mass boron trichloride-ethanol solution, dichloromethane and a Grignard reagent, introduce nitrogen for protection, react at a speed of 300 rpm for 60 minutes, let stand for stratification, remove the lower turbid liquid, take the supernatant, heat it to 100°C, filter and recover ethanol to obtain borane, and mix borane with trimethylsilanol and triphenylphosphine to obtain a coupling agent.

[0034] S4: The end-capped 107 silicone rubber, modified photoresin and filler are mixed, and stirred evenly at 1000 rpm under a vacuum degree of 0.1 MPa, and then a crosslinking agent, a coupling agent, a catalyst and a photoinitiator are added and mixed, and stirred for 50 minutes to obtain a UV / moisture dual-curing high-strength neutral dealcoholization RTV silicone rubber.

[0035] Example 2 The difference between Example 2 and Example 1 is that the amount of blocked 107 silicone rubber used in the UV / moisture dual-curing high-strength neutral dealcoholization type RTV silicone rubber raw material is 90 kg, the amount of filler used is 20 kg, the amount of cross-linking agent used is 10 kg, the amount of coupling agent used is 1 kg, the amount of catalyst used is 0.2 kg, the amount of modified photoresin used is 20 kg, and the amount of photoinitiator used is 0.2 kg.

[0036] Example 3 The difference between Example 3 and Example 1 is that the amount of blocked 107 silicone rubber used in the UV / moisture dual-curing high-strength neutral dealcoholization type RTV silicone rubber raw material is 110 kg, the amount of filler used is 10 kg, the amount of cross-linking agent used is 6 kg, the amount of coupling agent used is 3 kg, the amount of catalyst used is 0.4 kg, the amount of modified photoresin used is 10 kg, and the amount of photoinitiator used is 0.4 kg.

[0037] Example 4 The difference between Example 4 and Example 1 is that the mass ratio of glycidyloxypropyltrimethoxysilane, methacrylic acid, hydroquinone and tetrabutylammonium bromide in the modified photoresin raw material is 0.8:1:0.01:0.0001.

[0038] Example 5 The difference between Example 5 and Example 1 is that the mass ratio of glycidyloxypropyltrimethoxysilane, methacrylic acid, hydroquinone and tetrabutylammonium bromide in the modified photoresin raw material is 1.2:1:0.03:0.0003.

[0039] Example 6 The difference between Example 6 and Example 1 is that the mass ratio of methyl orthosilicate, buffer and potassium hydroxide in the cross-linking agent raw material is 1:1.5:0.0001.

[0040] Example 7 The difference between Example 7 and Example 1 is that the mass ratio of methyl orthosilicate, buffer and potassium hydroxide in the cross-linking agent raw material is 1:2.5:0.0003.

[0041] Example 8 The difference between Example 8 and Example 1 is that the mass ratio of boron trichloride-ethanol solution, dichloromethane, Grignard reagent, trimethylsilanol and triphenylphosphine in the coupling agent raw material is 1:0.8:0.8:2.5:0.0001.

[0042] Example 9 The difference between Example 9 and Example 1 is that the mass ratio of boron trichloride-ethanol solution, dichloromethane, Grignard reagent, trimethylsilanol and triphenylphosphine in the coupling agent raw material is 1:1.2:1.2:3.5:0.0003.

[0043] Example 10 The difference between Example 10 and Example 1 is that an equal amount of methyltriethoxysilane is used instead of the crosslinking agent in the UV / moisture dual-curing high-strength neutral dealcoholization type RTV silicone rubber raw material.

[0044] A method for preparing a UV / moisture dual-curing high-strength neutral dealcoholization RTV silicone rubber comprises the following specific steps: S1: heating glycidyloxypropyltrimethoxysilane to 100°C, introducing nitrogen for protection, adding methacrylic acid, then adding hydroquinone, stirring at a speed of 300 rpm for 30 minutes, adding tetrabutylammonium bromide, mixing and reacting for 60 minutes, and then cooling to obtain a modified photoresist.

[0045] S2: Mix 20% by mass boron trichloride-ethanol solution, dichloromethane and Grignard reagent, introduce nitrogen for protection, react at 300 rpm for 60 min, let stand for stratification, remove the lower turbid liquid, take the supernatant, heat it to 100°C, filter and recover ethanol to obtain borane, and mix borane with trimethylsilanol and triphenylphosphine to obtain a coupling agent.

[0046] S3: The end-capped 107 silicone rubber, modified photoresin and filler are mixed, and stirred evenly at 1000 rpm under a vacuum degree of 0.1 MPa, and then methyltriethoxysilane, coupling agent, catalyst and photoinitiator are added and mixed, and stirred for 50 minutes to obtain UV / moisture dual-curing high-strength neutral dealcoholization RTV silicone rubber.

[0047] Embodiment 11 The difference between Example 11 and Example 1 is that an equal amount of aminopropyltrimethoxysilane is used instead of a coupling agent in the UV / moisture dual-curing high-strength neutral dealcoholization type RTV silicone rubber raw material.

[0048] A method for preparing a UV / moisture dual-curing high-strength neutral dealcoholization RTV silicone rubber comprises the following specific steps: S1: heating glycidyloxypropyltrimethoxysilane to 100°C, introducing nitrogen for protection, adding methacrylic acid, then adding hydroquinone, stirring at a speed of 300 rpm for 30 minutes, adding tetrabutylammonium bromide, mixing and reacting for 60 minutes, and then cooling to obtain a modified photoresist.

[0049] S2: Methyl orthosilicate and ethanol buffer are mixed, the temperature is raised to 100° C., potassium hydroxide is added, and the mixture is reacted at a rotation speed of 300 rpm for 120 min. Then, ethanol and small molecular products are recovered by filtration to obtain a cross-linking agent.

[0050] S3: The end-capped 107 silicone rubber, modified photoresin and filler are mixed, and stirred evenly at 1000 rpm under a vacuum degree of 0.1 MPa, and then a crosslinking agent, aminopropyltrimethoxysilane, a catalyst and a photoinitiator are added and mixed, and stirred for 50 minutes to obtain a UV / moisture dual-curing high-strength neutral dealcoholization RTV silicone rubber.

[0051] Example 12 The difference between Example 12 and Example 1 is that the viscosity of the end-capped 107 silicone rubber in the UV / moisture dual-curing high-strength neutral dealcoholization type RTV silicone rubber raw material is 1000 cps.

[0052] Comparative Example Comparative Example 1 The difference between Comparative Example 1 and Example 1 is that no modified photoresin is used in the UV / moisture dual-curing high-strength neutral dealcoholization type RTV silicone rubber raw material.

[0053] A method for preparing UV / moisture dual-curing high-strength neutral dealcoholization RTV silicone rubber comprises the following specific steps: S1: mixing methyl orthosilicate and ethanol buffer, heating to 100° C., adding potassium hydroxide, reacting at a rotation speed of 300 rpm for 120 min, and then filtering and recovering ethanol and small molecule products to obtain a crosslinking agent.

[0054] S2: Mix 20% by mass boron trichloride-ethanol solution, dichloromethane and Grignard reagent, introduce nitrogen for protection, react at 300 rpm for 60 min, let stand for stratification, remove the lower turbid liquid, take the supernatant, heat it to 100°C, filter and recover ethanol to obtain borane, and mix borane with trimethylsilanol and triphenylphosphine to obtain a coupling agent.

[0055] S3: The end-capped 107 silicone rubber and filler are mixed, and stirred evenly at 1000 rpm under a vacuum degree of 0.1 MPa, and then a crosslinking agent, a coupling agent, a catalyst, and a photoinitiator are added and mixed, and stirred for 50 minutes to obtain a UV / moisture dual-curing high-strength neutral dealcoholization RTV silicone rubber.

[0056] Comparative Example 2 The difference between Comparative Example 2 and Example 1 is that the amount of modified photoresin used in the UV / moisture dual-curing high-strength neutral dealcoholization type RTV silicone rubber raw material is 5 kg.

[0057] Comparative Example 3 The difference between Comparative Example 3 and Example 1 is that the amount of modified photoresin used in the UV / moisture dual-curing high-strength neutral dealcoholization type RTV silicone rubber raw material is 30 kg.

[0058] Comparative Example 4 The difference between Comparative Example 4 and Example 1 is that the amount of the crosslinking agent used in the UV / moisture dual-curing high-strength neutral dealcoholization type RTV silicone rubber raw material is 4 kg.

[0059] Comparative Example 5 The difference between Comparative Example 5 and Example 1 is that the amount of the crosslinking agent used in the UV / moisture dual-curing high-strength neutral dealcoholization type RTV silicone rubber raw material is 12 kg.

[0060] Comparative Example 6 The difference between Comparative Example 6 and Example 1 is that the amount of coupling agent used in the UV / moisture dual-curing high-strength neutral dealcoholization type RTV silicone rubber raw material is 5 kg.

[0061] Comparative Example 7 The difference between Comparative Example 7 and Example 1 is that no catalyst, photoinitiator, coupling agent, or modified photoresin is used in the UV / moisture dual-curing high-strength neutral dealcoholization RTV silicone rubber raw material, and an equal amount of methyltriacetoxysilane is used instead of a cross-linking agent.

[0062] A method for preparing silicone rubber comprises the following specific steps: The end-capped 107 silicone rubber and filler were mixed, stirred evenly at 1000 rpm under a vacuum degree of 0.1 MPa, and then methyl triacetoxy silane was added and mixed, and stirred for 50 minutes to obtain silicone rubber.

[0063] Comparative Example 8 The difference between Comparative Example 8 and Example 1 is that no photoinitiator, coupling agent, crosslinking agent or modified photoresin is used in the UV / moisture dual-curing high-strength neutral dealcoholization type RTV silicone rubber raw material.

[0064] A method for preparing silicone rubber comprises the following specific steps: The end-capped 107 silicone rubber and filler were mixed, stirred evenly at 1000 rpm under a vacuum degree of 0.1 MPa, and then a chelated tin catalyst was added and mixed, and stirred for 50 minutes to obtain silicone rubber.

[0065] Comparative Example 9 The difference between Comparative Example 9 and Example 1 is that no photoinitiator or modified photoresin is used in the UV / moisture dual-curing high-strength neutral dealcoholization type RTV silicone rubber raw material, an equal amount of methyl tributylidene oxime is used instead of the cross-linking agent, and an equal amount of aminopropyl triethoxysilane is used instead of the coupling agent.

[0066] A method for preparing silicone rubber comprises the following specific steps: The end-capped 107 silicone rubber and filler were mixed, and stirred evenly at 1000 rpm under a vacuum degree of 0.1 MPa, and then methyl tributylidene oxime, aminopropyl triethoxysilane, and chelated tin catalyst were added, mixed, and stirred for 50 minutes to obtain silicone rubber.

[0067] Comparative Example 10 The difference between Comparative Example 10 and Example 1 is that no photoinitiator or modified photoresin is used in the UV / moisture dual-curing high-strength neutral dealcoholization RTV silicone rubber raw material, an equal amount of methyltriethoxysilane is used instead of the cross-linking agent, and an equal amount of aminopropyltrimethoxysilane is used instead of the coupling agent.

[0068] A method for preparing silicone rubber comprises the following specific steps: The end-capped 107 silicone rubber and filler were mixed, and stirred evenly at 1000 rpm under a vacuum degree of 0.1 MPa. Methyltriethoxysilane, aminopropyltrimethoxysilane and chelated tin catalyst were then added, mixed, and stirred for 50 minutes to obtain silicone rubber.

[0069] Performance testing According to the UV / moisture dual-curing high-strength neutral dealcoholization RTV silicone rubber provided in Examples 1-12 and Comparative Examples 1-10 of the present application, the following performance tests were performed, and the specific test results are shown in Table 1.

[0070] Testing method: Surface drying time: The test shall be carried out in accordance with GB / T13477.5-2002 "Test methods for building sealing materials Part 5: Determination of surface drying time".

[0071] Tensile and tear strength: Tested in accordance with GB / T528-2009 "Determination of tensile stress-strain properties of vulcanized rubber or thermoplastic rubber".

[0072] Glass bonding: The bonding area is 2x2cm, and the adhesion is tested in accordance with GB / T16776-2005 "Silicone structural sealant for construction".

[0073] Voc- Volatile Organic Compounds- Test: Tested in accordance with GB / T38507-2020.

[0074] Full curing time: The time required for full curing based on the 2cm colloid thickness.

[0075] Yellowing / mildew: Place the colloid at 85℃ x 85 humidity for one month and observe whether it turns yellow or moldy.

[0076] Table 1: Performance test results data table It can be seen from the performance test results that the RTV silicone rubber prepared in this application has high strength and toughness, while maintaining good curing rate, weather resistance and yellowing resistance. At the same time, it has a strong bonding effect on glass curtain walls, etc., and has good effects in resisting typhoons, sunlight ultraviolet aging, etc., and is healthy and environmentally friendly to the environment and human body.

[0077] This specific embodiment is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make modifications to the present embodiment without any creative contribution as needed, but such modifications are protected by the patent law as long as they are within the scope of the claims of the present application.

Claims

1. A UV / moisture dual-curing high-strength neutral dealcoholization RTV silicone rubber, characterized in that: The invention comprises the following raw materials in parts by weight: 90-110 parts of end-capped 107 silicone rubber, 10-20 parts of filler, 6-10 parts of crosslinking agent, 1-3 parts of coupling agent, 0.2-0.4 parts of catalyst, 10-20 parts of modified photoresin and 0.2-0.4 parts of photoinitiator; the raw materials of the modified photoresin comprise glycidyloxypropyltrimethoxysilane, methacrylic acid, hydroquinone and tetrabutylammonium bromide.

2. The UV / moisture dual-curing high-strength neutral dealcoholization type RTV silicone rubber according to claim 1, characterized in that: The mass ratio of the glycidyloxypropyltrimethoxysilane, methacrylic acid, hydroquinone and tetrabutylammonium bromide is: (0.8-1.2): 1: (0.01-0.03): (0.0001-0.0003).

3. The UV / moisture dual-curing high-strength neutral dealcoholization type RTV silicone rubber according to claim 1, characterized in that: The cross-linking agent raw materials include methyl orthosilicate, a buffer and potassium hydroxide, and the mass ratio of the methyl orthosilicate, the buffer and potassium hydroxide is 1: (1.5-2.5): (0.0001-0.0003).

4. The UV / moisture dual-curing high-strength neutral dealcoholization type RTV silicone rubber according to claim 3, characterized in that: The preparation method of the cross-linking agent comprises the following specific steps: mixing methyl orthosilicate and a buffer, heating to 95-105° C., adding potassium hydroxide, reacting and condensing to obtain the cross-linking agent.

5. The UV / moisture dual-curing high-strength neutral dealcoholization type RTV silicone rubber according to claim 1, characterized in that: The coupling agent raw materials include boron trichloride-ethanol solution, dichloromethane, Grignard reagent, trimethylsilanol and triphenylphosphine, and the mass ratio of the boron trichloride-ethanol solution, dichloromethane, Grignard reagent, trimethylsilanol and triphenylphosphine is 1: (0.8-1.2): (0.8-1.2): (2.5-3.5): (0.0001-0.0003).

6. The UV / moisture dual-curing high-strength neutral dealcoholization type RTV silicone rubber according to claim 5, characterized in that: The preparation method of the coupling agent comprises the following specific steps: under the protection of nitrogen, boron trichloride-ethanol solution, dichloromethane and Grignard reagent are mixed for reaction, after standing for stratification, the supernatant is heated and filtered to obtain borane, and then the borane is mixed with trimethylsilane and triphenylphosphine to obtain the coupling agent.

7. The UV / moisture dual-curing high-strength neutral dealcoholization type RTV silicone rubber according to claim 1, characterized in that: The end-capping 107 silicone rubber has a viscosity of 3000-20000 cps.

8. The UV / moisture dual-curing high-strength neutral dealcoholization type RTV silicone rubber according to claim 1, characterized in that: The filler is fumed hydrophobic white carbon black, and the surface area of ​​the fumed hydrophobic white carbon black is ≥150m 2 / g, the catalyst is a chelated tin catalyst, and the photoinitiator is a ketone photoinitiator.

9. A method for preparing the UV / moisture dual-curing high-strength neutral dealcoholization type RTV silicone rubber according to any one of claims 1 to 8, characterized in that: The specific steps include: Under the protection of nitrogen, glycidyloxypropyltrimethoxysilane and methacrylic acid are mixed and heated for reaction, hydroquinone is added for reaction, and then tetrabutylammonium bromide is added for reaction to obtain a modified photoresist; The end-capped 107 silicone rubber is mixed with the modified photoresin and filler, and stirred evenly under a vacuum degree of -0.1-0.1MPa. Then a crosslinking agent, a coupling agent, a catalyst, and a photoinitiator are added and mixed, and stirred evenly to obtain a UV / moisture dual-curing high-strength neutral dealcoholization RTV silicone rubber.

Citation Information

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