A UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber and its preparation method

Through the use of UV/moisture dual curing technology and the use of modified photoresin, combined with fillers and other crosslinking agents, the problem of insufficient curing of RTV silicone rubber is solved, and silicone rubber products with high strength, weather resistance and long life are achieved.

CN119193097BActive Publication Date: 2025-05-27SHENZHEN KANGLIBANG TECH

Patent Information

Application Number
CN202411393016.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-10-08
Publication Date
2025-05-27
Estimated Expiration
2044-10-08

AI Technical Summary

Technical Problem

The existing RTV silicone rubber has insufficient deep curing during the curing process, resulting in insufficient hardness and strength and shortening service life.

Method used

UV/moisture dual curing technology is adopted to promote the hybrid curing of silicon rubber in combination with moisture under UV light irradiation, thereby improving curing efficiency and depth. At the same time, components such as fillers, crosslinkers, coupling agents and catalysts are used to enhance the strength and bonding properties of the silicone rubber.

Benefits of technology

It significantly improves the curing efficiency and depth of silicone rubber, enhances its tensile strength and weather resistance, extends its service life, and improves the stability of bonding effects to glass curtain walls and other aspects.

✦ Generated by Eureka AI based on patent content.

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Abstract

This application relates to the technical field of new polymer silicone materials, and specifically discloses a UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber and a preparation method thereof; a UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber, comprising 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 cross-linking agent, 1-3 parts of coupling agent, 0.2-0.4 parts of catalyst, 10-20 parts of modified light resin, 0.2-0.4 parts of photoinitiator; the raw materials of the modified light resin include glycidyl ether oxypropyltrimethoxysilane, methacrylic acid, hydroquinone and tetrabutylammonium bromide; the UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber of this application utilizes the modified light resin and photoinitiator, combined with the moisture hybrid curing method, has good curing efficiency, and has both high tensile strength and weather resistance.
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Description

Technical Field

[0001] This application relates to the technical field of new polymer silicone materials, and particularly to a UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber and a preparation method thereof. Background Art

[0002] Alcohol-type room temperature vulcanized room temperature silicone rubber is an adhesive product that cures by releasing small alcohol molecules upon contact with moisture. The substance released during its curing is a small molecule alcohol, which is a harmless substance. It has the advantages of good weather resistance, fast volatilization, and no corrosion, and is widely used in furniture decoration, construction industry, and electronic products. For glass curtain wall buildings, due to being exposed to the air for a long time and being eroded by sunlight, rainwater, etc., the glass glues currently on the market are mainly composed of alcohol-free, oxime-free, and acid-free silicone adhesives, etc., which contain volatile and strongly irritating gases such as methyl ethyl ketone and acetic acid that are harmful to the human body. In order to save production costs, some manufacturers use white oil as the main body, resulting in problems such as oil leakage, glue peeling, etc. in the later stage, seriously affecting the safety of the building.

[0003] UV ultraviolet light-cured silicone materials have good mechanical properties and thermal stability. When applied in the construction field, they have great advantages in improving strength, yellowing resistance, and mildew resistance. However, there are currently situations such as insufficient deep curing, which in turn leads to insufficient hardness and strength of the prepared silicone rubber and shortens the service life of the silicone rubber. Summary of the Invention

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

[0005] In the first aspect, this application provides a UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber, adopting the following technical solution:

[0006] A UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber, comprising the following raw materials in parts by weight: 90 - 110 parts of endblocked 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 light resin, 0.2 - 0.4 parts of photoinitiator; the raw materials of the modified light resin include glycidoxypropyltrimethoxysilane, methacrylic acid, hydroquinone, and tetrabutylammonium bromide.

[0007] By adopting the above technical solution, methacrylic acid is used in the modified photo-resin raw material to improve the photocuring efficiency of silicone rubber, enabling the silicone rubber to cure rapidly under UV light irradiation. At the same time, tetrabutylammonium bromide can act as a photoinitiator, and the modification can further promote the UV curing process, improving the curing speed and depth of the silicone rubber. Glycidoxypropyltrimethoxysilane can react with the hydroxyl groups on the substrate surface through epoxy groups to form chemical bonds, and the silyl groups form covalent bonds with the silicone rubber, thereby promoting the firmly adhesion of the prepared silicone rubber to the substrate surface. Hydroquinone can improve the antioxidant and weather resistance of the silicone rubber, and thus enhance the durability of the silicone rubber.

[0008] Using the modified photo-resin and photoinitiator, the prepared silicone rubber is promoted to cure under natural light or UV lamp irradiation, combined with the way of moisture-mixed curing, enabling the prepared silicone rubber to have good curing efficiency, and at the same time having relatively high tensile strength and weather resistance.

[0009] The strength and toughness of RTV silicone rubber are enhanced by using fillers. The capped 107 silicone rubber molecules are linked by a crosslinking agent to solidify the capped 107 silicone rubber colloid. Adding a catalyst can improve the curing efficiency of the silicone rubber and enhance the curing effect. By hydrolysis of the coupling agent, the generated active groups adhere firmly to the substrate, thereby improving the bonding strength of the silicone rubber.

[0010] Preferably, the mass ratio of glycidoxypropyltrimethoxysilane, methacrylic acid, hydroquinone and tetrabutylammonium bromide is: (0.8 - 1.2) : 1 : (0.01 - 0.03) : (0.0001 - 0.0003).

[0011] Preferably, the crosslinking agent raw materials include methyl orthosilicate, buffer and potassium hydroxide, and the mass ratio of methyl orthosilicate, buffer and potassium hydroxide is 1 : (1.5 - 2.5) : (0.0001 - 0.0003).

[0012] By adopting the above technical solution, potassium hydroxide as a catalyst can promote the condensation of methyl orthosilicate to form oligomers, which are connected to the capped 107 silicone rubber, improving the curing efficiency of the silicone rubber and enhancing the strength and bonding performance of the silicone rubber.

[0013] Preferably, the preparation method of the crosslinking agent includes the following specific steps: Mix methyl orthosilicate and buffer, heat up to 95 - 105 °C, add potassium hydroxide, and react and condense to obtain the crosslinking agent.

[0014] Preferably, 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:(0.8 - 1.2):(0.8 - 1.2):(2.5 - 3.5):(0.0001 - 0.0003).

[0015] Preferably, the boron trichloride-ethanol solution can promote the crosslinking reaction of the silicone rubber system, enhancing the mechanical strength and weather resistance of the silicone rubber. The Grignard reagent is an organomagnesium compound that can react with the silicon alkyl groups in the silicone rubber to form more stable chemical bonds, enhancing the crosslinking density of the silicone rubber and improving the strength and hardness of the silicone rubber. Triphenylphosphine can act as a catalyst to improve the curing efficiency of the silicone rubber.

[0016] Preferably, the preparation method of the coupling agent includes the following specific steps: Under the protection of nitrogen, the boron trichloride-ethanol solution, dichloromethane and Grignard reagent are mixed and reacted, and after standing for layering, the supernatant is taken and heated and filtered to obtain borane. Then, the borane is mixed and reacted with trimethylsilane and triphenylphosphine to obtain the coupling agent.

[0017] By adopting the above technical solution, the boron trichloride-ethanol solution, dichloromethane and Grignard reagent can carry out cross-coupling reaction of halogenated hydrocarbons, and the generated borane can condense and react with trimethylsilanol under the catalytic action of triphenylphosphine to form a coupling agent. The obtained neutral coupling agent has borate radicals, and has better adhesiveness to glass, marble, wood, etc. compared with traditional coupling agents, and is not easy to turn white, and the obtained colloid has good light transmittance.

[0018] Preferably, the viscosity of the end-capped 107 silicone rubber is 3000 - 20000 cps.

[0019] By adopting the above technical solution, the end-capped 107 silicone rubber at this viscosity has good extrudability and thixotropy, which is convenient for extrusion and use during caulking.

[0020] Preferably, the filler is fumed hydrophobic silica, the surface area of the fumed hydrophobic silica ≥ 150m 2 / g, the catalyst is a chelating tin catalyst, and the photoinitiator is a ketone photoinitiator.

[0021] By adopting the above technical solution, using fumed hydrophobic silica can reduce the condensation and caking after the moisture in the air contacts with the silica during storage and transportation. At the same time, the surface area of the fumed hydrophobic silica is not less than 150m 2In the case of / g, it can promote the preparation of silicone rubber with high strength. Ketone photoinitiators have high initiation efficiency and good thermal stability, thereby improving the curing efficiency of silicone rubber. At the same time, ketone photoinitiators have no yellowing phenomenon and have good storage stability. Compared with other thiol photoinitiators, they have less pungent odor. The chelating tin catalyst has a low tin content and high catalytic reaction activity, and can promote the preparation of silicone rubber with high curing efficiency and strength.

[0022] In a second aspect, the present application provides a method for preparing a UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber, adopting the following technical solution:

[0023] A method for preparing a UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber includes the following specific steps:

[0024] Under the protection of nitrogen, glycidyl ether oxypropyltrimethoxysilane and methacrylic acid are mixed and heated for reaction, hydroquinone is added for reaction, and then tetrabutylammonium bromide is added for mixing reaction to obtain a modified photo resin;

[0025] The blocked 107 silicone rubber is mixed with the modified photo resin and filler, stirred evenly under a vacuum of -0.1 - 0.1 MPa, and then a crosslinking agent, a coupling agent, a catalyst, and a photoinitiator are added and mixed evenly to obtain a UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber.

[0026] By adopting the above technical solution, by using the modified photo resin to introduce a photoinitiator, synergistically enhancing with other components, it promotes the silicone rubber to have high curing efficiency, tensile strength, and weather resistance.

[0027] In summary, the present application has the following beneficial effects:

[0028] 1. Since the present application uses a modified photo resin and a photoinitiator, it promotes the silicone rubber prepared to be cured by a combined method of moisture mixing under natural light or ultraviolet lamp irradiation, improving the curing efficiency of the silicone rubber. In the modified photo resin raw material, methacrylic acid and tetrabutylammonium bromide are used synergistically to introduce the photoinitiator into the photo resin, further improving the curing efficiency and curing depth of the silicone rubber. At the same time, in the modified photo resin raw material, glycidyl ether oxypropyltrimethoxysilane and hydroquinone can improve the strength and weather resistance of the silicone rubber.

[0029] 2. In this application, methyl orthosilicate, a buffer, and potassium hydroxide are condensed to form an oligomer as a crosslinking agent, which is connected to the blocked 107 silicone rubber, improving the curing efficiency of the silicone rubber and enhancing the strength and adhesion performance of the silicone rubber. A neutral coupling agent generated by reacting boron trichloride-ethanol solution, dichloromethane, Grignard reagent, trimethylsilanol, and triphenylphosphine can enhance the crosslinking density of the silicone rubber, improving the strength, hardness, and weather resistance of the silicone rubber. Detailed Embodiments

[0030] The following further elaborates on this application in conjunction with embodiments.

[0031] All raw materials in the embodiments can be obtained commercially.

[0032] Embodiments

[0033] Embodiment 1

[0034] This embodiment provides a UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber, which includes the following raw materials in parts by weight: 100 kg of blocked 107 silicone rubber, 15 kg of filler, 8 kg of crosslinking agent, 2 kg of coupling agent, 0.3 kg of catalyst, 15 kg of modified photo resin, 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 chelating tin catalyst C-103, the photoinitiator is ketone photoinitiator 1173, and the viscosity of the blocked 107 silicone rubber is 10,000 cps.

[0035] Among them, the raw materials of the modified photo resin include glycidoxypropyltrimethoxysilane, methacrylic acid, hydroquinone, and tetrabutylammonium bromide, and the mass ratio of glycidoxypropyltrimethoxysilane, methacrylic acid, hydroquinone, and tetrabutylammonium bromide is 1:1:0.2:0.0002; the usage amount of methacrylic acid is 100 kg.

[0036] The raw materials of the crosslinking agent include methyl orthosilicate, a buffer, and potassium hydroxide. The buffer is ethanol, and the mass ratio of methyl orthosilicate, the buffer, and potassium hydroxide is 1:2:0.0002; the usage amount of methyl orthosilicate is 100 kg.

[0037] The raw materials of the coupling agent 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 usage amount of boron trichloride-ethanol solution is 100 kg.

[0038] A preparation method of a UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber includes the following specific steps: S1: Heat glycidoxypropyltrimethoxysilane to 100 °C, introduce nitrogen for protection, add methacrylic acid, then add hydroquinone, stir at a speed of 300 rpm for 30 min, add tetrabutylammonium bromide and mix for reaction for 60 min, and then cool down to obtain a modified photo-resin.

[0039] S2: Mix methyl orthosilicate and an ethanol buffer, heat to 100 °C, add potassium hydroxide, react at a speed of 300 rpm for 120 min, then filter to recover ethanol and small molecule products to obtain a crosslinking agent.

[0040] S3: Mix a boron trichloride-ethanol solution with a mass fraction of 20%, dichloromethane, and a Grignard reagent, introduce nitrogen for protection, react at a speed of 300 rpm for 60 min, let it stand for layering, remove the lower turbid liquid, take the supernatant, heat to 100 °C and filter to recover ethanol to obtain borane, and mix borane with trimethylsilanol and triphenylphosphine for reaction to obtain a coupling agent.

[0041] S4: Mix endblocked 107 silicone rubber, the modified photo-resin, and a filler, stir evenly at a vacuum degree of 0.1 MPa and a speed of 1000 rpm, then add the crosslinking agent, the coupling agent, the catalyst, and the photoinitiator and mix, stir for 50 min to obtain a UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber.

[0042] Example 2

[0043] The difference between Example 2 and Example 1 is that in the raw materials of the UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber, the usage amount of endblocked 107 silicone rubber is 90 kg, the usage amount of the filler is 20 kg, the usage amount of the crosslinking agent is 10 kg, the usage amount of the coupling agent is 1 kg, the usage amount of the catalyst is 0.2 kg, the usage amount of the modified photo-resin is 20 kg, and the usage amount of the photoinitiator is 0.2 kg.

[0044] Example 3

[0045] The difference between Example 3 and Example 1 is that in the raw materials of the UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber, the usage amount of endblocked 107 silicone rubber is 110 kg, the usage amount of the filler is 10 kg, the usage amount of the crosslinking agent is 6 kg, the usage amount of the coupling agent is 3 kg, the usage amount of the catalyst is 0.4 kg, the usage amount of the modified photo-resin is 10 kg, and the usage amount of the photoinitiator is 0.4 kg.

[0046] Example 4

[0047] Example 4 is different from Example 1 in that the mass ratio of glycidoxypropyltrimethoxysilane, methacrylic acid, hydroquinone and tetrabutylammonium bromide in the modified optical resin raw material is 0.8:1:0.01:0.0001.

[0048] Example 5

[0049] Example 5 is different from Example 1 in that the mass ratio of glycidoxypropyltrimethoxysilane, methacrylic acid, hydroquinone and tetrabutylammonium bromide in the modified optical resin raw material is 1.2:1:0.03:0.0003.

[0050] Example 6

[0051] Example 6 is different from Example 1 in that the mass ratio of methyl orthosilicate, buffer and potassium hydroxide in the crosslinking agent raw material is 1:1.5:0.0001.

[0052] Example 7

[0053] Example 7 is different from Example 1 in that the mass ratio of methyl orthosilicate, buffer and potassium hydroxide in the crosslinking agent raw material is 1:2.5:0.0003.

[0054] Example 8

[0055] Example 8 is different from Example 1 in 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.

[0056] Example 9

[0057] Example 9 is different from Example 1 in 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.

[0058] Example 10

[0059] Example 10 is different from Example 1 in that an equal amount of methyltriethoxysilane is used to replace the crosslinking agent in the UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber raw material.

[0060] A preparation method of a UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber includes the following specific steps: S1: Heat glycidoxypropyltrimethoxysilane to 100°C, introduce nitrogen for protection, add methacrylic acid, then add hydroquinone, stir at a speed of 300 rpm for 30 min, add tetrabutylammonium bromide and mix and react for 60 min, and then cool down to obtain a modified optical resin.

[0061] S2: Mix the boron trichloride-ethanol solution with a mass fraction of 20%, dichloromethane, and Grignard reagent, introduce nitrogen for protection, react at a rotation speed of 300 rpm for 60 min, let it stand for layering, remove the lower turbid liquid, heat the supernatant to 100 °C and filter to recover ethanol to obtain borane, and mix and react borane with trimethylsilanol and triphenylphosphine to obtain a coupling agent.

[0062] S3: Mix the blocked 107 silicone rubber, modified photo-resin, and filler, stir evenly at a vacuum degree of 0.1 MPa and a rotation speed of 1000 rpm, then add methyltriethoxysilane, coupling agent, catalyst, and photoinitiator and mix, stir for 50 min to obtain a UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber.

[0063] Example 11

[0064] The difference between Example 11 and Example 1 is that an equal amount of aminopropyltrimethoxysilane is used instead of the coupling agent in the raw materials of the UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber.

[0065] A preparation method of a UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber includes the following specific steps: S1: Heat glycidyletheroxypropyltrimethoxysilane to 100 °C, introduce nitrogen for protection, add methacrylic acid, then add hydroquinone, stir at a rotation speed of 300 rpm for 30 min, add tetrabutylammonium bromide and mix and react for 60 min, and then cool down to obtain a modified photo-resin.

[0066] S2: Mix methyl orthosilicate and ethanol buffer, heat to 100 °C, add potassium hydroxide, react at a rotation speed of 300 rpm for 120 min, then filter to recover ethanol and small molecule products to obtain a crosslinking agent.

[0067] S3: Mix the blocked 107 silicone rubber, modified photo-resin, and filler, stir evenly at a vacuum degree of 0.1 MPa and a rotation speed of 1000 rpm, then add the crosslinking agent, aminopropyltrimethoxysilane, catalyst, and photoinitiator and mix, stir for 50 min to obtain a UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber.

[0068] Example 12

[0069] The difference between Example 12 and Example 1 is that the viscosity of the blocked 107 silicone rubber in the raw materials of the UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber is 1000 cps.

[0070] Comparative example

[0071] Comparative example 1

[0072] The difference between Comparative Example 1 and Example 1 is that a modified photo-resin is not used in the raw materials of the UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber.

[0073] A preparation method of a UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber comprises the following specific steps: S1: Mix methyl orthosilicate and an ethanol buffer, heat up to 100 °C, add potassium hydroxide, react at a rotation speed of 300 rpm for 120 min, and then perform suction filtration to recover ethanol and small-molecule products to obtain a crosslinking agent.

[0074] S2: Mix a boron trichloride-ethanol solution with a mass fraction of 20%, dichloromethane, and a Grignard reagent, protect with nitrogen gas, react at a rotation speed of 300 rpm for 60 min, let it stand for layering, remove the lower turbid liquid, take the supernatant, heat it to 100 °C, perform suction filtration to recover ethanol, obtain borane, and mix and react borane with trimethylsilanol and triphenylphosphine to obtain a coupling agent.

[0075] S3: Mix endblocked 107 silicone rubber and a filler, stir evenly at a vacuum degree of 0.1 MPa and a rotation speed of 1000 rpm, then add a crosslinking agent, a coupling agent, a catalyst, and a photoinitiator and mix, and stir for 50 min to obtain a UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber.

[0076] Comparative Example 2

[0077] The difference between Comparative Example 2 and Example 1 is that the usage amount of the modified photo-resin in the raw materials of the UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber is 5 kg.

[0078] Comparative Example 3

[0079] The difference between Comparative Example 3 and Example 1 is that the usage amount of the modified photo-resin in the raw materials of the UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber is 30 kg.

[0080] Comparative Example 4

[0081] The difference between Comparative Example 4 and Example 1 is that the usage amount of the crosslinking agent in the raw materials of the UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber is 4 kg.

[0082] Comparative Example 5

[0083] The difference between Comparative Example 5 and Example 1 is that the usage amount of the crosslinking agent in the raw materials of the UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber is 12 kg.

[0084] Comparative Example 6

[0085] 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 alcohol-free RTV silicone rubber raw material is 5 kg.

[0086] Comparative Example 7

[0087] The difference between Comparative Example 7 and Example 1 is that no catalyst, photoinitiator, coupling agent, or modified photo-resin is used in the UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber raw material, and an equal amount of methyltriacetoxysilane is used instead of the cross-linking agent.

[0088] A method for preparing silicone rubber includes the following specific steps:

[0089] Mix the blocked 107 silicone rubber and the filler, stir evenly at 1000 rpm under a vacuum of 0.1 MPa, then add methyltriacetoxysilane and mix, and stir for 50 min to obtain silicone rubber.

[0090] Comparative Example 8

[0091] The difference between Comparative Example 8 and Example 1 is that no photoinitiator, coupling agent, cross-linking agent, or modified photo-resin is used in the UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber raw material.

[0092] A method for preparing silicone rubber includes the following specific steps:

[0093] Mix the blocked 107 silicone rubber and the filler, stir evenly at 1000 rpm under a vacuum of 0.1 MPa, then add the chelating tin catalyst and mix, and stir for 50 min to obtain silicone rubber.

[0094] Comparative Example 9

[0095] The difference between Comparative Example 9 and Example 1 is that no photoinitiator or modified photo-resin is used in the UV / moisture dual-curing high-strength neutral alcohol-free RTV silicone rubber raw material, an equal amount of methyl tributanone oxime alkane is used instead of the cross-linking agent, and an equal amount of aminopropyltriethoxysilane is used instead of the coupling agent.

[0096] A method for preparing silicone rubber includes the following specific steps:

[0097] Mix the blocked 107 silicone rubber and the filler, stir evenly at 1000 rpm under a vacuum of 0.1 MPa, then add methyl tributanone oxime alkane, aminopropyltriethoxysilane, and the chelating tin catalyst and mix, and stir for 50 min to obtain silicone rubber.

[0098] Comparative Example 10

[0099] The difference between Comparative Example 10 and Example 1 lies in that in the raw material of the UV / moisture dual-cured high-strength neutral alcohol-free RTV silicone rubber, photoinitiators and modified photo-resins are not used, an equal amount of methyltriethoxysilane is used to replace the cross-linking agent, and an equal amount of aminopropyltrimethoxysilane is used to replace the coupling agent.

[0100] A method for preparing silicone rubber includes the following specific steps:

[0101] Mix the blocked 107 silicone rubber and the filler, and under a vacuum of 0.1 MPa, stir evenly at 1000 rpm, then add methyltriethoxysilane, aminopropyltrimethoxysilane, and chelating tin catalyst and mix, and stir for 50 min to obtain silicone rubber.

[0102] Performance detection test

[0103] For the UV / moisture dual-cured high-strength neutral alcohol-free RTV silicone rubber provided by Examples 1-12 and Comparative Examples 1-10 of the present application, the following performance detections are carried out, and the specific detection results are shown in Table 1.

[0104] Detection method: Surface drying time: Test according to GB / T13477.5-2002 "Test Methods for Building Sealants - Part 5: Determination of Surface Drying Time".

[0105] Tensile and tear strength: Test according to GB / T528-2009 "Determination of Tensile Stress-Strain Properties of Vulcanized Rubber or Thermoplastic Rubber".

[0106] Glass bonding: The bonding area is 2x2 cm, and the bonding property is tested according to GB / T16776-2005 "Silicone Structural Sealant for Building".

[0107] Voc-Volatile Organic Compounds - Test: Test according to GB / T38507-2020.

[0108] Full cure time: The time required for complete cure according to the thickness of 2 cm of the colloid.

[0109] Yellowing / mildewing situation: Place it at 85°C and 85% humidity for one month, and observe whether the colloid turns yellow and mildews.

[0110] Table 1: Data table of performance detection results

[0111]

[0112] It can be seen from the performance detection results that the RTV silicone rubber prepared in the present application has high strength and toughness, and at the same time also maintains good curing rate, weather resistance and yellowing resistance. At the same time, the bonding effect on glass curtain walls is firm, and it has good effects in aspects such as anti-typhoon and sunlight ultraviolet aging, and is healthy and environmentally friendly to the environment and human body.

[0113] This specific embodiment is only an interpretation of the present application and does not limit the present application. After reading this specification, those skilled in the art can make modifications to this embodiment that do not contribute creatively as needed, but as long as it is within the scope of the claims of the present application, it is protected by the patent law.

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 photoresist, and 0.2-0.4 parts of photoinitiator; the modified photoresin raw materials include glycidyloxypropyltrimethoxysilane, methacrylic acid, hydroquinone and tetrabutylammonium bromide; the crosslinking agent raw materials include methyl orthosilicate, buffer and potassium hydroxide; the methyl orthosilicate, The mass ratio of the buffer and potassium hydroxide is 1: (1.5-2.5): (0.0001-0.0003); 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).

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 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.

4. The UV / moisture dual-curing high-strength neutral dealcoholization type RTV silicone rubber according to claim 1, 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.

5. 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.

6. 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.

7. A method for preparing the UV / moisture dual-curing high-strength neutral dealcoholization RTV silicone rubber according to any one of claims 1 to 6, 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

Patent Citations

  • Ultraviolet-moisture dual-cured modified organosilicon adhesive and preparation method therefor

    CN105505302A

  • Oil-resistant, high-temperature-resistant and low-volatile organic silica gel

    CN111875970A

  • Bi-component fast-curing neutral dealcoholization type RTV (Room Temperature Vulcanization) silicone rubber and preparation method thereof

    CN117327398A

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