Addition type liquid silicone rubber with high light transmittance and weather resistance and preparation method thereof

Abstract

The invention discloses addition type liquid silicone rubber with high light transmittance and weather resistance and a preparation method thereof, and belongs to the field of liquid silicone rubber. The preparation method comprises the following steps: mixing vinyl-terminated polydimethylsiloxane and modified fumed silica, and kneading to obtain base rubber; uniformly mixing the prepared base rubber, diethylenetriamine silane, modified nano cerium oxide and a platinum complex catalyst, and defoaming to obtain a component A; uniformly mixing the prepared base rubber, an inhibitor, a cross-linking agent and N-(beta-aminoethyl)-gamma-aminopropyl trimethoxy silane, and defoaming to obtain a component B; uniformly mixing and vulcanizing the component A and the component B to obtain the high-light-transmittance weather-resistant liquid silicone rubber. The light transmittance is not less than 95%, and the haze is not more than 1.5% After a 2000h ultraviolet aging test, the light transmittance decrease amplitude is less than or equal to 3%, the yellowing index (YI) is less than or equal to 2, and the ultraviolet aging resistance is excellent; and after 50 times of high and low temperature cycles at-40 DEG C to 150 DEG C, the tensile strength retention rate is greater than or equal to 92%. The product provided by the invention can be widely applied to the fields of outdoor LED packaging, solar photovoltaic modules, outdoor optical lenses and the like.

Description

Technical Field

[0001] This invention relates to the field of addition-type liquid silicone rubber technology, and more specifically, to an addition-type liquid silicone rubber with high light transmittance and weather resistance, and its preparation method. Background Technology

[0002] In modern industry and daily life, liquid silicone rubber, with its excellent physicochemical properties such as good flowability, fast vulcanization speed, low linear shrinkage, and non-toxicity and odorlessness, has become an indispensable high-performance material, widely used in electronics, optical packaging, automotive manufacturing, medical devices, baby products, and daily necessities. In outdoor optical applications, such as outdoor LED displays, solar panel encapsulation, and outdoor lighting lenses, liquid silicone rubber not only needs to have extremely high light transmittance to ensure optical performance, but also needs to have excellent weather resistance to resist performance degradation caused by external factors such as ultraviolet radiation, high and low temperature cycling, and humid and hot environments. Currently, liquid silicone rubber is prepared by adding reinforcing fillers and crosslinking agents to vinyl-terminated polydimethylsiloxane as the base material. However, traditional liquid silicone rubber has the following technical drawbacks: On the one hand, the reinforcing fillers (such as fumed silica) added to improve mechanical properties can easily cause light scattering, resulting in a decrease in the transmittance of the silicone rubber, especially in the visible light range of 400-800nm, where the transmittance is difficult to maintain stably above 95%; on the other hand, the weather resistance of traditional silicone rubber mainly relies on the addition of ultraviolet absorbers or hindered amine light stabilizers, but these additives have poor compatibility with the silicone matrix and are prone to precipitation after long-term use, leading to a decline in weather resistance. After 2000h of ultraviolet aging test, the transmittance often decreases by more than 10%, and the yellowing index (YI) exceeds 5, which cannot meet the requirements for long-term outdoor use. Therefore, developing a liquid silicone that combines high light transmittance, excellent weather resistance, and stable performance has become a pressing technical problem to be solved in this field. Summary of the Invention

[0003] This invention overcomes the problem of balancing light transmittance and weather resistance in existing liquid silicone rubbers through specific formulation design and preparation process, and provides an addition-type liquid silicone rubber with high light transmittance and weather resistance and its preparation method. This liquid silicone rubber has high light transmittance in the visible light range and exhibits minimal performance degradation after long-term ultraviolet aging and high and low temperature cycling, as well as excellent weather resistance.

[0004] To achieve the above objectives, the present invention provides the following technical solution: A high-transmittance, weather-resistant addition-type liquid silicone rubber and its preparation method, comprising the following steps: Preparation of base rubber: Vinyl-terminated polydimethylsiloxane and modified fumed silica are added to a closed kneader in a certain proportion. Kneading is started and the temperature is raised to 80~120℃. After the rubber compound is kneaded into a ball, the temperature is raised to 150~180℃ and kneaded at a constant temperature for 2-4 hours. Then, vacuum kneading is continued at this temperature for 1-3 hours with a vacuum degree ≤-0.095MPa. After that, the heating is turned off, the temperature is lowered and diluted. The discharged base rubber is ground by a three-roll mill and then filtered through a filter screen of 200 mesh or higher to obtain the finished base rubber.

[0005] Preparation of Component A: The base adhesive prepared in step 1, diethylenetriaminesilane, modified nano-cerium oxide, and platinum complex catalyst were sequentially added to a planetary mixer and mixed evenly to remove bubbles, thus obtaining Component A.

[0006] Preparation of Component B: The base adhesive, inhibitor, crosslinking agent, and N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane prepared in step 1 were sequentially added to a planetary mixer and mixed evenly to obtain Component B.

[0007] Curing and molding: Mix component A and component B evenly at a mass ratio of 1:1, degas for 10-15 minutes under a vacuum degree ≤-0.095MPa, pour into a mold, and vulcanize at 120℃ for 5-10 minutes to obtain liquid silicone rubber with high light transmittance and weather resistance.

[0008] The base adhesive is composed of the following raw materials in parts by weight: 50-90 parts of vinyl-terminated polydimethylsiloxane and 10-35 parts of modified fumed silica.

[0009] Component A consists of the following raw materials in parts by weight: 80-90 parts base adhesive, 2-8 parts diethylenetriaminesilane, 0.5-2 parts modified nano-cerium oxide, and 0.01-0.05 parts Castel platinum catalyst.

[0010] Component B is composed of the following raw materials in parts by weight: 80-95 parts base adhesive, 0.1-0.5 parts inhibitor, 0.5-10 parts crosslinking agent, and 1-5 parts N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane.

[0011] Furthermore, the vinyl-terminated polydimethylsiloxane has a viscosity of 5000-100000 mPa·s (25℃), a vinyl content of 0.06-0.16 wt%, and a volatile content of ≤1.0% (150℃*3h); the crosslinking agent is a side-hydrogenated silicone oil or a compound of end- and side-hydrogenated silicone oils, with a hydrogen content of 0.1~1.6 wt%.

[0012] Furthermore, the modified fumed silica is a hydrophilic fumed silica pre-modified with N,O-bis(trimethylsilyl)acetamide, with a specific surface area of ​​200-400 m². 2 / g, with a particle size of 10-20nm, pre-modified silica can reduce the hydroxyl content on the surface of silica and make the modification more uniform, reduce agglomeration, improve its compatibility with silicone rubber matrix, reduce light scattering, and ensure light transmittance.

[0013] Furthermore, the modified nano-cerium oxide is nano-cerium oxide modified with N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane or N-(6-aminohexyl)-γ-aminopropyltrimethoxysilane, with a particle size of 5-15 nm. The modified nano-cerium oxide can not only effectively absorb ultraviolet light (especially ultraviolet light with a wavelength of 200-400 nm) and improve the UV aging resistance of silicone rubber, but also tightly bond with the silicone matrix to avoid precipitation and maintain weather resistance for a long time.

[0014] Furthermore, the platinum complex catalyst is a Castells platinum catalyst with a platinum content of 5000 ppm; the inhibitor is an alkynyl alcohol inhibitor, which is one or more of 1-ethynyl-1-cyclohexanol, 2-methyl-3-butynyl-2-ol, 3-methyl-1-ethynyl-3-ol, or 3,5-dimethyl-1-hexynyl-3-ol.

[0015] Compared with the prior art, the present invention has the following beneficial effects: This invention employs N,O-bis(trimethylsilyl)acetamide to pre-modify fumed silica. Compared to simultaneous modification during production, this results in a more uniform and stable surface treatment of the silica, significantly improving its compatibility with the silicone rubber matrix. While providing reinforcement, it also reduces light scattering by over 30%, ensuring that the silicone rubber exhibits a transmittance ≥95% and a haze ≤1.5% in the visible light range, demonstrating excellent optical performance. Furthermore, the invention introduces N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane or N-(6-aminohexyl)-γ-aminopropyltrimethoxysilane-modified nano-cerium oxide, which is not only a highly efficient UV absorber but also converts UV light into harmless visible light. Furthermore, it can form chemical bonds with the silicone rubber matrix through silane coupling agents, avoiding precipitation problems during long-term use. Compared with traditional UV absorbers, its UV aging resistance is improved by more than 50%, with a transmittance decrease of ≤3% and yellowing index (YI) ≤2 after 2000h UV aging. Through the synergistic effect of diethylenetriaminesilane and N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, the interfacial bonding force between components is further improved, reducing light scattering and performance degradation caused by interfacial defects. At the same time, it enhances the high and low temperature resistance of silicone rubber. After 50 cycles of high and low temperature from -40℃ to 150℃, the tensile strength retention rate is ≥92%.

[0016] The preparation process of this invention is simple, the components are compatible, and it is easy to industrialize. It can be widely used in outdoor LED packaging, solar photovoltaic modules, outdoor optical lenses and other fields. Detailed Implementation

[0017] The present invention will be further explained below with reference to the embodiments, but the embodiments do not limit the present invention in any way.

[0018] Example 1 1. Preparation of the base adhesive: 68 parts of vinyl-terminated polydimethylsiloxane (viscosity 5000 mPa·s) and 32 parts of modified fumed silica (modified fumed silica is N,O-bis(trimethylsilyl)acetamide-modified fumed silica with a specific surface area of ​​320 m²) were prepared. 2 / g (particle size 12-15nm) is put into a closed kneader, kneaded and heated to 80℃. After the rubber compound is kneaded into a ball, the temperature is raised to 160℃ and kneaded at a constant temperature for 3 hours. Then, vacuum kneading is carried out at this temperature for 2 hours with a vacuum degree ≤-0.095MPa. After that, the heating is turned off, the temperature is lowered and diluted. The discharged base rubber is ground by a three-roll mill and then filtered through a filter screen of 200 mesh or higher to obtain the finished base rubber.

[0019] Method for modifying N,O-bis(trimethylsilyl)acetamide in fumed silica: (1) Place the silica raw material in a vacuum drying oven and dry it at 120-150°C for 6 hours to remove as much physically adsorbed water as possible. Assemble the dried flask, condenser, etc., and purge the entire system thoroughly with nitrogen / argon to remove air and moisture. The entire reaction process is carried out under positive pressure of inert gas.

[0020] (2) Preparation of suspension: Add dry silica to the reaction flask and anhydrous toluene as solvent. The solid content is 10% w / v. (3) The addition and reaction of BSA While stirring (ensuring uniform dispersion of silica), slowly add BSA dropwise through a constant-pressure dropping funnel. Use 3.0 mL of N,O-bis(trimethylsilyl)acetamide per gram of silica.

[0021] After the addition is complete, slowly raise the temperature to the reflux temperature of toluene (120°C) and reflux under strong stirring for 10 hours at this temperature.

[0022] (4) After the reaction is complete, the system is cooled to room temperature. Under an inert atmosphere, the modified silica is obtained by vacuum filtration, washing, and drying using a Buchner funnel (lined with filter paper).

[0023] 2. Preparation of Component A: 85 parts of base adhesive, 5 parts of diethylenetriaminesilane, 1.5 parts of modified nano-cerium oxide (modified nano-cerium oxide is nano-cerium oxide modified by N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane with a particle size of 10-15 nm) and 0.04 parts of 5000 ppm Castel platinum catalyst were sequentially added to a planetary mixer and mixed evenly to obtain Component A.

[0024] Preparation method of N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane modified cerium oxide nanoparticles: Step 1: Pre-dispersion and activation of nano-cerium oxide Add 1g of nano CeO2 powder to a three-necked flask containing 100mL of a deionized water / ethanol mixture (volume ratio 1:1). Adjust the pH of the system to 4-5 with acetic acid.

[0025] The suspension was ultrasonically treated at room temperature for 30 minutes to form a uniform and stable suspension.

[0026] Step 2: Preparation of KH-792 hydrolysate Measure KH-792 into a small beaker. The amount used is 10% of the mass of CeO2.

[0027] Mix KH-792 with 20 mL of an ethanol / water mixture (volume ratio 1:1). Adjust the pH of the mixture to 4-5 using acetic acid.

[0028] The silane solution is pre-hydrolyzed by magnetic stirring for 30 minutes. At this time, the solution will become slightly turbid or clear, indicating that the silane methoxy group has been partially hydrolyzed to generate active silanol groups.

[0029] Step 3: Surface grafting reaction The pre-hydrolyzed KH-792 solution was slowly added dropwise to the pre-dispersed CeO2 suspension while stirring.

[0030] After the addition is complete, heat the reaction system to 70-80°C and reflux with stirring at this temperature for 6-12 hours. Heating can accelerate the condensation reaction between silanol groups and CeO2 surface hydroxyl groups.

[0031] Step 4: Post-processing and purification Cooling and Separation: After the reaction is complete, cool the system to room temperature. Transfer the reaction solution to centrifuge tubes and centrifuge using a high-speed centrifuge (12,000 rpm, 15 minutes), then discard the supernatant.

[0032] Washing: To remove physically adsorbed silanes and byproducts, the precipitate was redispersed with an ethanol / water mixture (1:1) and centrifuged again. This process was repeated 3-4 times until the supernatant showed no obvious purple color when tested with ninhydrin reagent (ninhydrin reacts with primary amines), indicating that the free amino groups had been washed away.

[0033] Vacuum drying: Place the final precipitate in a vacuum drying oven and dry at 60°C for 12-24 hours.

[0034] 3. Preparation of Component B: 85 parts of base adhesive, 0.3 parts of 1-ethynyl-1-cyclohexanol, 5 parts of crosslinking agent (terminal hydrogen-containing silicone oil: side-containing hydrogen-containing silicone oil = 1:1, with hydrogen contents of 0.012% and 1.2wt%, respectively), and 5 parts of N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane were sequentially added to a planetary mixer and mixed evenly to obtain Component B.

[0035] Example 2 1. Preparation of base rubber: 72 parts of vinyl-terminated polydimethylsiloxane (viscosity 5000 mPa·s) and 28 parts of modified fumed silica (same as in Example 1) were put into a closed kneader. The kneading was started and the temperature was raised to 100°C. After the rubber compound was kneaded into a ball, the temperature was raised to 170°C and kneaded at a constant temperature for 2 hours. Then, the mixture was kneaded under vacuum at this temperature for 3 hours with a vacuum degree ≤ -0.095 MPa. The heating was then turned off, the temperature was lowered and diluted. The discharged base rubber was ground by a three-roll mill and then filtered through a filter screen of 200 mesh or higher to obtain the finished base rubber.

[0036] 2. Preparation of component A: 90 parts of base adhesive, 4 parts of diethylenetriaminesilane, 1.8 parts of modified nano-cerium oxide (same as in Example 1), and 0.03 parts of 5000ppm Castel platinum catalyst were sequentially added to a planetary mixer and mixed evenly to obtain component A.

[0037] 3. Preparation of Component B: 90 parts of base adhesive, 0.2 parts of 1-ethynyl-1-cyclohexanol, 3 parts of crosslinking agent (hydrogen-containing silicone oil with a hydrogen content of 1.6 wt%), and 3 parts of N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane were sequentially added to a planetary mixer and mixed evenly to obtain Component B.

[0038] Example 3 1. Preparation of base rubber: 70 parts of vinyl-terminated polydimethylsiloxane (viscosity 10000 mPa·s) and 30 parts of modified fumed silica (same as in Example 1) were put into a closed kneader. The kneading was started and the temperature was raised to 100°C. After the rubber compound was kneaded into a ball, the temperature was raised to 165°C and kneaded at a constant temperature for 4 hours. Then, the mixture was kneaded under vacuum at this temperature for 1 hour with a vacuum degree ≤ -0.095 MPa. The heating was then turned off, the mixture was cooled and diluted. The discharged base rubber was ground by a three-roll mill and then filtered through a filter screen of 200 mesh or higher to obtain the finished base rubber.

[0039] 2. Preparation of Component A: 80 parts of base adhesive, 8 parts of diethylenetriaminesilane, 2 parts of modified nano-cerium oxide (modified nano-cerium oxide is N-(6-aminohexyl)-γ-aminopropyltrimethoxysilane modified nano-cerium oxide, the method is the same as in Example 1), and 0.04 parts of 5000ppm Castel platinum catalyst were sequentially added to a planetary mixer, mixed evenly and degassed to obtain Component A.

[0040] 3. Preparation of Component B: 80 parts of base adhesive, 0.3 parts of 1-ethynyl-1-cyclohexanol, 1 part of crosslinking agent (hydrogen-containing silicone oil with a hydrogen content of 1.2 wt%), and 5 parts of N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane were sequentially added to a planetary mixer and mixed evenly to obtain Component B.

[0041] Example 4 1. Preparation of base rubber: 75 parts of vinyl-terminated polydimethylsiloxane (viscosity 10000 mPa·s) and 25 parts of modified fumed silica (same as in Example 1) were put into a closed kneader. The kneading was started and the temperature was raised to 120°C. After the rubber compound was kneaded into a ball, the temperature was raised to 175°C and kneaded at a constant temperature for 3 hours. Then, the mixture was kneaded under vacuum at this temperature for 2 hours with a vacuum degree ≤ -0.095 MPa. The heating was then turned off, the temperature was lowered and diluted. The discharged base rubber was ground by a three-roll mill and then filtered through a filter screen of 200 mesh or higher to obtain the finished base rubber.

[0042] 2. Preparation of component A: 85 parts of base adhesive, 6 parts of diethylenetriaminesilane, 1.5 parts of modified nano-cerium oxide (same as in Example 3), and 0.03 parts of 5000ppm Castel platinum catalyst were sequentially added to a planetary mixer and mixed evenly to obtain component A.

[0043] 3. Preparation of Component B: 85 parts of base adhesive, 0.2 parts of 1-ethynyl-1-cyclohexanol, 3 parts of crosslinking agent (side-containing hydrogen silicone oil with a hydrogen content of 0.75wt%), and 3.5 parts of N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane were sequentially added to a planetary mixer and mixed evenly to obtain Component B.

[0044] Comparative Example 1 The method is the same as in Example 1, except that fumed silica is used in the preparation of the base adhesive.

[0045] Comparative Example 2 The method is the same as in Example 1, except that the base adhesive is prepared using hexamethyldisilazane-modified fumed silica, and the modification method is the same as in Example 1.

[0046] Comparative Example 3 The method is the same as in Example 1, except that... Preparation of Component A: 85 parts of base adhesive, 5 parts of diethylenetriaminesilane, 1.5 parts of nano-cerium oxide, and 0.04 parts of 5000ppm Castor platinum catalyst were sequentially added to a planetary mixer and mixed evenly to obtain Component A.

[0047] 3. Preparation of Component B: 85 parts of base adhesive, 0.3 parts of 1-ethynyl-1-cyclohexanol, 5 parts of crosslinking agent (terminal hydrogen-containing silicone oil: side-containing hydrogen-containing silicone oil = 1:1, with hydrogen contents of 0.012% and 1.2wt%, respectively), and 5 parts of N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane were sequentially added to a planetary mixer and mixed evenly to obtain Component B.

[0048] The components A and B prepared in Examples 1-4 and Comparative Examples 1-3 were mixed uniformly at a mass ratio of 1:1. The mixture was degassed for 10-15 minutes under a vacuum of ≤-0.095 MPa, poured into a mold, and vulcanized at 120℃ for 5-10 minutes to obtain a high-transmittance, weather-resistant liquid silicone rubber sample with a thickness of 2 mm. Relevant tests were performed on the liquid silicone rubber sample obtained above, and the test results are shown in Table 1.

[0049] Table 1. Summary of Test Results for Liquid Silicone Rubber

[0050] As shown in Table 1, the liquid silicone rubber prepared in Examples 1-4 of the present invention is significantly superior to that in Comparative Examples 1-3 in terms of optical properties, UV aging resistance, and high and low temperature resistance.

Claims

1. A method for preparing a high-transmittance, weather-resistant addition-type liquid silicone rubber, characterized in that, Includes the following steps: (1) Vinyl-terminated polydimethylsiloxane and modified fumed silica are put into a closed kneader in a certain proportion, the kneading is turned on and the material is heated, and the material is kept at a constant temperature and vacuumed. Then the heating is turned off and the material is cooled and diluted. The discharged base rubber is ground by a three-roll mill and filtered through a filter screen to obtain the finished base rubber. (2) The base gel, diethylenetriamine silane, modified nano-cerium oxide and platinum complex catalyst prepared in (1) are sequentially added to a planetary mixer and mixed evenly to obtain component A. (3) The base glue, inhibitor, crosslinking agent and N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane prepared in (1) are sequentially added to a planetary mixer and mixed evenly to obtain component B. (4) Mix component A and component B at a mass ratio of 1:1, degas for 10-15 min under a vacuum of ≤-0.095MPa, pour into a mold and vulcanize at 120℃ for 5-10 min to obtain liquid silicone rubber with high light transmittance and weather resistance.

2. The method for preparing high light transmittance and weather-resistant addition-type liquid silicone rubber according to claim 1, characterized in that: The vinyl-terminated polydimethylsiloxane described in step (1) has a viscosity of 5000-100000 mPa·s (25℃), a vinyl content of 0.06-0.16 wt%, and a volatile content of ≤1.0%.

3. The method for preparing high light transmittance and weather-resistant addition-type liquid silicone rubber according to claim 1, characterized in that: In step (1), the modified fumed silica is a hydrophilic fumed silica pre-modified with N,O-bis(trimethylsilyl)acetamide, with a specific surface area of ​​200-400 m². 2 / g, with a particle size of 10-20nm.

4. The method for preparing high light transmittance and weather-resistant addition-type liquid silicone rubber according to claim 1, characterized in that: The base adhesive described in step (1) is composed of the following raw materials in parts by weight: 50-90 parts of vinyl-terminated polydimethylsiloxane and 10-35 parts of modified fumed silica.

5. The method for preparing high light transmittance and weather-resistant addition-type liquid silicone rubber according to claim 1, characterized in that: In step (1), the material is heated to 80-120℃. After the rubber compound is kneaded into a ball, the temperature is raised to 150-180℃ and kneaded at a constant temperature for 2-4 hours. Then, the material is kneaded under vacuum at this temperature for 1-3 hours with a vacuum degree of ≤-0.095MPa.

6. The method for preparing high light transmittance and weather-resistant addition-type liquid silicone rubber according to claim 1, characterized in that: In step (2), the modified nano-cerium oxide is nano-cerium oxide modified with N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane or N-(6-aminohexyl)-γ-aminopropyltrimethoxysilane, with a particle size of 5-15 nm.

7. The method for preparing high light transmittance and weather-resistant addition-type liquid silicone rubber according to claim 1, characterized in that: In step (2), the platinum complex catalyst is a Castells platinum catalyst with a platinum content of 5000 ppm.

8. The method for preparing high light transmittance and weather-resistant addition-type liquid silicone rubber according to claim 1, characterized in that: In step (2), component A consists of the following raw materials in parts by mass: 80-90 parts of base adhesive, 2-8 parts of diethylenetriamine silane, 0.5-2 parts of modified nano-cerium oxide, and 0.01-0.05 parts of platinum complex catalyst.

9. The method for preparing high light transmittance and weather-resistant addition-type liquid silicone rubber according to claim 1, characterized in that: In step (3), the inhibitor is an alkynyl alcohol inhibitor, which is one or more of 1-ethynyl-1-cyclohexanol, 2-methyl-3-butynyl-2-ol, 3-methyl-1-ethynyl-3-ol or 3,5-dimethyl-1-hexynyl-3-ol; the crosslinking agent is a side-hydrogen-containing silicone oil or a compound of end- and side-hydrogen-containing silicone oils, with a hydrogen content of 0.1~1.6wt%.

10. The method for preparing high light transmittance and weather-resistant addition-type liquid silicone rubber according to claim 1, characterized in that: In step (3), component B consists of the following raw materials in parts by mass: 80-95 parts base adhesive, 0.1-0.5 parts inhibitor, 0.5-10 parts crosslinking agent, and 1-5 parts N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane.

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