Peroxide type primer for adhesion of addition type liquid silica gel to molded silica gel and preparation method of peroxide type primer
By using peroxide primer to promote the cross-linking reaction between silane coupling agent and molded silica gel, the problem of insufficient bonding strength on the surface of molded silica gel is solved, and efficient and reliable bonding effect is achieved, and is suitable for a variety of rigorous application scenarios.
Patent Information
- Application Number
- CN202411951701.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-27
- Publication Date
- 2025-04-11
AI Technical Summary
Traditional bonding methods are difficult to form a firm and long-lasting bonding interface on the surface of molded silicone, resulting in insufficient bonding strength and degumming problems, especially in strict application scenarios such as medical devices and electronic packaging.
A peroxide-type primer is used to cross-link with molded silica gel through a silane coupling agent or oligomer with reactive epoxy groups, double bonds and other groups under the action of peroxide to form a firm bonding interface.
The bonding strength between the addition-molded liquid silicone and the molded silicone is effectively improved, so that it is bonded firmly and does not fall off. The preparation method is simple, low-cost and easy to be produced in industrial use.
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Abstract
Description
Technical Field
[0001] The present application relates to the technical field of silicone adhesives, and in particular to a peroxide-type primer for addition-type liquid silicone adhesives and a preparation method thereof. Background Art
[0002] With the continuous development of science and technology, silicone materials have been widely used in modern industry and high-end manufacturing due to their excellent properties, such as excellent chemical stability, high and low temperature resistance, good elasticity and biocompatibility. However, in the actual production and product development process, there are often bonding needs between silicone parts, such as the construction of multi-layer silicone structures, composite bonding of silicone and surfaces of different materials, etc.; traditional bonding methods have many challenges for molded silicone: on the one hand, molded silicone has strong chemical inertness and low surface energy, and ordinary adhesives are difficult to form a strong and lasting bonding interface on its surface, which is prone to problems such as insufficient bonding strength and debonding; on the other hand, in some special application scenarios, such as medical devices and electronic packaging, there are extremely strict requirements for bonding reliability, aging resistance and non-toxic and environmental protection, which are difficult to meet with conventional bonding technology. With the continuous improvement of the demand for integrated and high-performance silicone products in various industries, the development of an efficient, reliable, and primer that is compatible with addition-type liquid silicone and molded silicone has become a key issue that needs to be solved urgently to promote the innovative application and industrial development of silicone materials in a wider range of fields. Summary of the invention
[0003] In view of the deficiencies in the prior art, the present application provides a peroxide-type primer for bonding addition-type liquid silicone to molded silicone and a preparation method thereof. The primer can effectively improve the bonding strength between addition-type liquid silicone and molded silicone, making them firmly bonded and not falling off.
[0004] The primer of the addition type liquid silicone adhesive forming silicone disclosed in the present application is a silane coupling agent or oligomer having reactive epoxy groups, double bonds and the like, which undergoes a cross-linking reaction with the forming silicone under the action of peroxide to make the bonding firm and prevent debonding. The preparation method is simple, the cost is low, and it is easy to industrialize.
[0005] In the first aspect, the present application provides a peroxide-type primer for addition-type liquid silicone adhesive forming silicone, using the following technical solution: A peroxide-type primer for addition-type liquid silicone adhesive forming silicone, the primer comprising the following raw materials in parts by mass: Film former 0.3-5 parts; 0.1-15 parts of the first silane coupling agent;
[0006] Preferably, the tackifier comprises the following raw materials in parts by weight:
[0007] Preferably, the second silane coupling agent includes at least one of vinyltriethoxysilane, vinyltrimethoxysilane, vinylmethyldimethoxysilane, vinylmethyldiethoxysilane, hexamethyldisiloxane, tetramethyldivinyldisiloxane, vinyldimethylmethoxysilane, vinyldimethylethoxysilane, γ-glycidyloxypropyltrimethoxysilane, γ-glycidyloxypropylmethyldimethoxysilane, γ-glycidyloxypropylmethyldiethoxysilane, γ-(methacryloyloxy)propyltrimethoxysilane, γ-(methacryloyloxy)propylmethyldimethoxysilane, octyltrimethoxysilane, and phenyltriethoxysilane.
[0008] Preferably, the preparation method of the tackifier comprises the following steps: mixing the second silane coupling agent, deionized water and concentrated hydrochloric acid, reacting at 60-80°C for 6-8 hours, cooling to 45-55°C after the reaction, adding sodium bicarbonate and reacting for 2-4 hours, and distilling under reduced pressure at 60-80°C after the reaction, removing low-boiling substances, and filtering to obtain the tackifier.
[0009] Preferably, the film former includes at least one of epoxy resin, acrylic resin, polyester resin or polyalkoxy oligomer.
[0010] More preferably, the film-forming agent is bisphenol F epoxy resin NPEF-170.
[0011] Preferably, the first silane coupling agent includes at least one of vinyltriethoxysilane, vinyltrimethoxysilane, vinylmethyldimethoxysilane, vinylmethyldiethoxysilane, hexamethyldisiloxane, tetramethyldivinyldisiloxane, vinyldimethylmethoxysilane, vinyldimethylethoxysilane, γ-glycidyloxypropyltrimethoxysilane, γ-glycidyloxypropylmethyldimethoxysilane, γ-glycidyloxypropylmethyldiethoxysilane, γ-(methacryloyloxy)propyltrimethoxysilane, γ-(methacryloyloxy)propylmethyldimethoxysilane, octyltrimethoxysilane, and phenyltriethoxysilane.
[0012] Preferably, the crosslinking agent includes at least one of tetraethyl silicate, ethyl titanate, n-butyl titanate, isopropyl titanate, tris(3-trimethoxysilylpropyl)isocyanurate, triallyl isocyanurate, bis(triethoxysilyl)ethane, and bis(trimethoxysilylethyl)benzene.
[0013] Preferably, the organic solvent includes at least one of toluene, xylene, ethanol, isopropanol, cyclohexanol, n-heptane, white spirit, cyclohexane, ethylene glycol methyl ether, propylene glycol methyl ether, ethyl acetate, butyl acetate, and solvent oil.
[0014] Preferably, the catalyst comprises at least one of dicumyl peroxide, benzoyl peroxide, and 2,4-dichlorobenzoyl peroxide.
[0015] The present application discloses a peroxide-type primer for bonding addition-type liquid silicone to molded silicone. Since molded silicone rubber generally has a highly saturated structure and low surface activity, it is difficult to bond. The present application adopts organic peroxides, because organic peroxides are generally stable at room temperature, but can quickly decompose to produce free radicals at higher temperatures. The peroxide free radicals can capture the hydrogen on the methyl group of the molded silicone rubber to form macromolecular free radicals, and then the macromolecular free radicals are combined with the primer vinyl, epoxy, hydrogen, hydroxyl, etc. to form cross-linking bonds; and a combination of multiple solvents is used to make it have good wettability and strong bonding.
[0016] The primer of the addition type liquid silicone adhesive forming silicone disclosed in the present application is a silane coupling agent or oligomer having reactive epoxy groups, double bonds and the like, which undergoes a cross-linking reaction with the forming silicone under the action of peroxide to make the bonding firm and prevent debonding. The preparation method is simple, the cost is low, and it is easy to industrialize.
[0017] In a second aspect, the present application provides a method for preparing a peroxide-type primer for addition-type liquid silicone adhesive-type silicone, using the following technical solution: A method for preparing a peroxide-type primer for addition-type liquid silicone adhesive-type silicone, the steps of the preparation method are as follows: Weigh each raw material according to the formula; After the film-forming agent, the first silane coupling agent, the tackifier, the cross-linking agent and the organic solvent are mixed, a catalyst is added, mixed and filtered to obtain a primer.
[0018] In summary, the present application includes at least one of the following beneficial technical effects: 1. The present application discloses a peroxide-type primer for bonding addition-type liquid silicone to molded silicone and a preparation method thereof. The primer prepared in the present application can effectively improve the bonding strength between addition-type liquid silicone and molded silicone, making the bonding firm and non-falling off; 2. The preparation method of the primer disclosed in the present application is simple, low-cost, and easy to industrialize; 3. The primer prepared in this application is easy to use. It only needs to be evenly coated on the surface of the molded silicone to achieve a firm bond between the addition-type liquid silicone and the molded silicone; 4. The primer prepared in the present application is cured by peroxide and is easy to cross-link with the molded silica gel. DETAILED DESCRIPTION
[0019] The technical solution of the present application is further illustrated by specific embodiments below. The specific embodiments do not limit the protection scope of the present application; some non-essential modifications and adjustments made by others based on the concept of the present application still fall within the protection scope of the present application.
[0020] The raw materials involved in this application are all commercially available products, among which bisphenol F epoxy resin NPEF-170 is purchased from Shanghai Kaiyin Chemical Co., Ltd.
[0021] The present application is further described in detail below in conjunction with embodiments and comparative examples.
[0022] Embodiment 1: A method for preparing a peroxide-type primer for addition-type liquid silicone adhesive-type silicone, the steps are as follows: (1) Preparation of tackifier: 118.12g of silane coupling agent KH-560 (γ-glycidyloxypropyltrimethoxysilane), 74.12g of vinyltrimethoxysilane, 94.2g of tetramethyldivinyldisiloxane, 28g of deionized water and 0.3g of concentrated hydrochloric acid were added into a 500ml four-necked flask, and reacted at 70°C for 6 hours. After the reaction was completed, the temperature was lowered to 50°C, 0.5g of sodium bicarbonate was added and the reaction was continued for 3 hours. After the reaction was completed, low boiling materials were removed by reduced pressure distillation at 80°C, and then filtered to obtain thickener A1.
[0023] (2) Preparation of primer: Take 0.5g of bisphenol F epoxy resin NPEF-170, 1g of tackifier A1, 20g of xylene, 10g of butyl acetate, 10g of solvent oil, 15g of propylene glycol methyl ether, 1g of n-butyl titanate, 5g of octyltrimethoxysilane, 0.5g of triallyl isocyanurate, and 0.2g of phenyltriethoxysilane, mix well, add 0.5g of 2,4-dichlorobenzoyl peroxide, stir evenly at room temperature, filter, and obtain a primer.
[0024] Embodiment 2: A method for preparing a peroxide-type primer for addition-type liquid silicone adhesive-type silicone, the steps are as follows: (1) Preparation of tackifier: 128.17g of silane coupling agent KH-570 (γ-(methacryloyloxy)propyltrimethoxysilane), 74.12g of vinyltrimethoxysilane, 94.2g of tetramethyldivinyldisiloxane, 29.6g of deionized water and 0.3g of concentrated hydrochloric acid were added into a 500ml four-necked flask, and reacted at 70°C for 6 hours. After the reaction was completed, the temperature was lowered to 50°C, 0.5g of sodium bicarbonate was added and the reaction was continued for 3 hours. After the reaction was completed, low boiling materials were removed by reduced pressure distillation at 80°C, and then the thickener A2 was obtained by filtration.
[0025] (2) Preparation of primer: Take 0.5g of bisphenol F epoxy resin NPEF-170, 1g of tackifier A2, 20g of xylene, 20g of butyl acetate, 10g of solvent oil, 5g of ethylene glycol methyl ether, 1g of n-butyl titanate, 5g of octyltrimethoxysilane, and 0.5g of triallyl isocyanurate, mix well, add 0.5g of 2,4-dichlorobenzoyl peroxide, stir evenly at room temperature, filter, and obtain a primer.
[0026] Embodiment 3: A method for preparing a peroxide-type primer for addition-type liquid silicone adhesive-type silicone, the steps are as follows: (1) Preparation of tackifier: 234.4g of γ-(methacryloyloxy)propylmethyldimethoxysilane, 37.68g of tetramethyldivinyldisiloxane, 21.6g of deionized water and 0.3g of concentrated hydrochloric acid were added into a 500ml four-necked flask, and reacted at 70°C for 6 hours. After the reaction was completed, the temperature was lowered to 50°C, 0.5g of sodium bicarbonate was added and the reaction was continued for 3 hours. After the reaction was completed, low boiling materials were removed by reduced pressure distillation at 80°C, and then the thickener A3 was obtained by filtration.
[0027] (2) Preparation of primer: Take 0.5g of bisphenol F epoxy resin NPEF-170, 1g of tackifier A3, 20g of xylene, 10g of butyl acetate, 10g of solvent oil, 10g of propylene glycol methyl ether, 1g of n-butyl titanate, 0.5g of triallyl isocyanurate, and 0.1g of phenyltriethoxysilane, mix well, add 0.5g of 2,4-dichlorobenzoyl peroxide, stir evenly at room temperature, filter, and obtain a primer.
[0028] Embodiment 4: A method for preparing a peroxide-type primer for addition-type liquid silicone adhesive-type silicone, the steps are as follows: (1) Preparation of tackifier: 70.9 g of silane coupling agent KH560 (γ-glycidyloxypropyltrimethoxysilane), 74.5 g of γ-(methacryloyloxy)propyltrimethoxysilane, 26 g of vinyldimethylethoxysilane, 17.1 g of deionized water and 0.2 g of concentrated hydrochloric acid were added into a 500 ml four-necked flask, and reacted at 70°C for 6 hours. After the reaction was completed, the temperature was lowered to 50°C, 0.3 g of sodium bicarbonate was added and the reaction was continued for 3 hours. After the reaction was completed, low boiling materials were removed by reduced pressure distillation at 80°C, and then filtered to obtain thickener A4.
[0029] (2) Preparation of primer: Take 0.3g of bisphenol F epoxy resin NPEF-170, 1g of tackifier A4, 30g of xylene, 10g of solvent oil, 15g of propylene glycol methyl ether, 1g of n-butyl titanate, 0.5g of triallyl isocyanurate, and 0.1g of phenyltriethoxysilane, mix well, add 0.5g of 2,4-dichlorobenzoyl peroxide, stir evenly at room temperature, filter, and obtain a primer.
[0030] Embodiment 5: A method for preparing a peroxide-type primer for addition-type liquid silicone adhesive-type silicone, the steps are as follows: (1) Preparation of tackifier: 110g of γ-glycidyloxypropylmethyldimethoxysilane, 116g of γ-(methacryloyloxy)propylmethyldimethoxysilane, 38g of vinyldimethylethoxysilane, 46.8g of deionized water and 0.3g of concentrated hydrochloric acid were added into a 500ml four-necked flask, and reacted at 70°C for 6 hours. After the reaction was completed, the temperature was lowered to 50°C, 0.5g of sodium bicarbonate was added, and the reaction was continued for 3 hours. After the reaction was completed, low boiling materials were removed by reduced pressure distillation at 80°C, and then filtered to obtain thickener A5.
[0031] (2) Preparation of primer Take 0.5g of bisphenol F epoxy resin NPEF-170, 1g of tackifier A5, 20g of xylene, 10g of butyl acetate, 10g of isopropanol, 15g of propylene glycol methyl ether, 1g of n-butyl titanate, 0.5g of triallyl isocyanurate, and 0.2g of phenyltriethoxysilane, mix well, add 0.5g of 2,4-dichlorobenzoyl peroxide, stir evenly at room temperature, filter, and obtain a primer.
[0032] Embodiment 6: A method for preparing a peroxide-type primer for addition-type liquid silicone adhesive-type silicone, the steps are as follows: (1) Preparation of tackifier: 47.2g of γ-glycidyloxypropyltrimethoxysilane, 38g of vinyltriethoxysilane, 49.6g of γ-(methacryloyloxy)propylmethyldimethoxysilane, 37.2g of tetramethyldivinyldisiloxane, 7.2g of deionized water and 0.18g of concentrated hydrochloric acid were added into a 500ml four-necked flask, and reacted at 70°C for 6 hours. After the reaction was completed, the temperature was lowered to 50°C, 0.3g of sodium bicarbonate was added and the reaction was continued for 3 hours. After the reaction was completed, low boiling materials were removed by reduced pressure distillation at 80°C and filtered to obtain thickener A6.
[0033] (2) Preparation of primer: Take 0.3g of bisphenol F epoxy resin NPEF-170, 1g of tackifier A6, 20g of xylene, 10g of butyl acetate, 10g of n-heptane, 15g of propylene glycol methyl ether, 1g of n-butyl titanate, 0.5g of triallyl isocyanurate, and 0.2g of phenyltriethoxysilane, mix well, add 0.5g of 2,4-dichlorobenzoyl peroxide, stir evenly at room temperature, filter, and obtain a primer.
[0034] Embodiment 7: A method for preparing a peroxide-type primer for addition-type liquid silicone adhesive-type silicone, the steps are as follows: (1) Preparation of tackifier: 49g of γ-glycidyloxypropyltrimethoxysilane, 32g of vinyltriethoxysilane, 37g of γ-(methacryloyloxy)propylmethyldimethoxysilane, 42g of tetramethyldivinyldisiloxane, 5g of deionized water and 0.1g of concentrated hydrochloric acid were added into a 500ml four-necked flask, and reacted at 70°C for 6 hours. After the reaction was completed, the temperature was lowered to 50°C, 0.1g of sodium bicarbonate was added and the reaction was continued for 3 hours. After the reaction was completed, low boiling materials were removed by reduced pressure distillation at 80°C and filtered to obtain thickener A7.
[0035] (2) Preparation of primer: Take 5g of bisphenol F epoxy resin NPEF-170, 5g of tackifier A7, 30g of xylene, 20g of butyl acetate, 15g of solvent oil, 15g of propylene glycol methyl ether, 1g of n-butyl titanate, 1g of triallyl isocyanurate, and 15g of phenyltriethoxysilane, mix well, add 1g of 2,4-dichlorobenzoyl peroxide, stir evenly at room temperature, filter, and obtain a primer.
[0036] Embodiment 8: A method for preparing a peroxide-type primer for addition-type liquid silicone adhesive-type silicone, the steps are as follows: (1) Preparation of tackifier: 118g of silane coupling agent KH-570 (γ-(methacryloyloxy)propyltrimethoxysilane), 95g of vinyltrimethoxysilane, 97g of tetramethyldivinyldisiloxane, 50g of deionized water and 0.5g of concentrated hydrochloric acid were added into a 500ml four-necked flask, and reacted at 70°C for 6 hours. After the reaction was completed, the temperature was lowered to 50°C, 0.8g of sodium bicarbonate was added and the reaction was continued for 3 hours. After the reaction was completed, low boiling materials were removed by reduced pressure distillation at 80°C, and then the thickener A8 was obtained by filtration.
[0037] (2) Preparation of primer: Take 3g of bisphenol F epoxy resin NPEF-170, 0.5g of tackifier A8, 20g of xylene, 20g of butyl acetate, 10g of solvent oil, 5g of ethylene glycol methyl ether, 0.1g of n-butyl titanate, 10g of octyltrimethoxysilane, and 0.1g of triallyl isocyanurate, mix well, add 0.1g of 2,4-dichlorobenzoyl peroxide, stir well at room temperature, filter, and obtain a primer.
[0038] Comparative Example 1: A method for preparing a primer, the preparation steps are as follows: Take 0.6g of bisphenol F epoxy resin NPEF-170, 1g of vinyl triethoxysilane, 1.5g of n-butyl titanate, 0.5g of tetraethyl silicate, 0.6g of chloroplatinic acid, 15g of xylene, 20g of ethyl acetate, and 15g of isopropanol, and mix them evenly to obtain a primer.
[0039] Comparative Example 2: A method for preparing a primer, the preparation steps are as follows: Take 1g of bisphenol F epoxy resin NPEF-170, 1g of γ-glycidyloxypropyltrimethoxysilane, 2g of n-butyl titanate, 0.5g of tetraethyl silicate, 0.5g of chloroplatinic acid, 15g of xylene, 25g of solvent oil, and 20g of ethylene glycol methyl ether, and mix them evenly to obtain a primer.
[0040] Comparative Example 3: A method for preparing a primer, the preparation steps are as follows: Take 0.5g of bisphenol F epoxy resin NPEF-170, 1.3g of octyltrimethoxysilane, 1.5g of n-butyl titanate, 0.5g of tetraethyl silicate, 0.5g of chloroplatinic acid, 20g of xylene, 20g of ethyl acetate, and 10g of solvent oil, mix well to obtain a primer.
[0041] Comparative Example 4: A method for preparing a primer, the preparation steps are as follows: Take 0.8g of bisphenol F epoxy resin NPEF-170, 3g of γ-(methacryloyloxy)propyltrimethoxysilane, 2g of n-butyl titanate, 0.5g of tetraethyl silicate, 0.8g of chloroplatinic acid, 20g of xylene, 20g of ethyl acetate, 10g of n-heptane, and 15g of propylene glycol methyl ether, and mix them evenly to obtain a primer.
[0042] Comparative Example 5: The difference from Example 1 is that no tackifier is added. The specific preparation steps are as follows: A method for preparing a primer, the preparation steps are as follows: Take 0.5g of bisphenol F epoxy resin NPEF-170, 20g of xylene, 10g of butyl acetate, 10g of solvent oil, 15g of propylene glycol methyl ether, 1g of n-butyl titanate, 5g of octyltrimethoxysilane, 0.5g of triallyl isocyanurate, and 0.2g of phenyltriethoxysilane, mix well, add 0.5g of 2,4-dichlorobenzoyl peroxide, stir evenly at room temperature, filter, and obtain a primer.
[0043] Comparative Example 6: The difference from Example 2 is that no tackifier is added. The specific preparation steps are as follows: A method for preparing a primer, the preparation steps are as follows: Take 0.5g of bisphenol F epoxy resin NPEF-170, 20g of xylene, 20g of butyl acetate, 10g of solvent oil, 5g of ethylene glycol methyl ether, 1g of n-butyl titanate, 5g of octyltrimethoxysilane, and 0.5g of triallyl isocyanurate, mix well, add 0.5g of 2,4-dichlorobenzoyl peroxide, stir evenly at room temperature, filter, and obtain a primer.
[0044] Comparative Example 7: The difference from Example 6 is that no tackifier is added. The specific preparation steps are as follows: A method for preparing a primer, the preparation steps are as follows: Take 0.3g of bisphenol F epoxy resin NPEF-170, 20g of xylene, 10g of butyl acetate, 10g of n-heptane, 15g of propylene glycol methyl ether, 1g of n-butyl titanate, 0.5g of triallyl isocyanurate, and 0.2g of phenyltriethoxysilane, mix well, add 0.5g of 2,4-dichlorobenzoyl peroxide, stir well at room temperature, filter, and obtain a primer.
[0045] Blank test: Without using a primer, the addition type liquid silicone rubber is directly bonded to the molding silicone rubber.
[0046] Performance Test: 1. Adhesive performance test: Clean the molded silica gel with ethanol, apply the primer obtained above to the cleaned silica gel surface, put it into the oven and bake it at 130℃-140℃ for 10-15 minutes, then take it out. Apply the base material coated with the primer with the degassed liquid silica gel, then put it into the oven and bake it for 10-30 minutes, and finally judge the bonding strength between the molded silica gel and the liquid glue.
[0047] The bonding strength results of the performance test are judged as follows: 100% of the colloid cohesion failure is recorded as V, 80% or more of the colloid cohesion failure is recorded as IV, 60% or more of the colloid cohesion failure is recorded as III, 40% or more of the colloid cohesion failure is recorded as II, 20% or more of the colloid cohesion failure is recorded as I, and debonding is recorded as 0.
[0048] The test results of the bonding and forming silica gel of each embodiment, comparative example and blank control example are shown in the following table: Table 1 Test results of bonding silicone From the above test results, it can be seen that Examples 1, 2, and 6 of the present application have a good bonding effect on the molded silicone substrate (molded silicone prepared by the laboratory), and cohesive failure is caused by pulling; Examples 3, 4, 5, 7, and 8 have a small amount of debonding on the edges, and the bonding effect is relatively good.
[0049] In comparative examples 1-4, after the molded silica gel is treated with a primer product obtained by directly mixing a film-forming agent with a variety of coupling agents, cross-linking agents and other materials, the bonding effect is poor.
[0050] Combining Example 1 and Comparative Example 5, it can be seen that the bonding performance of Example 1 is better than that of Comparative Example 5, which means that when no tackifier is added, the bonding effect of the prepared primer is poor.
[0051] Combining Example 2 and Comparative Example 6, it can be seen that the bonding performance of Example 2 is better than that of Comparative Example 6, which means that when no tackifier is added, the bonding effect of the prepared primer is poor.
[0052] Combining Example 6 and Comparative Example 7, it can be seen that the bonding performance of Example 6 is better than that of Comparative Example 7, which means that when no tackifier is added, the bonding effect of the prepared primer is poor.
[0053] It can be seen that the primer of the present application can effectively improve the bonding strength between the addition-type liquid silicone and the molded silicone, the bonding is firm, and the rubber is cohesively destroyed.
[0054] 2. Shear strength performance test: The shear strength performance of the primers prepared in the above examples and comparative examples was tested. The testing method was based on "ASTM D1002-10 Standard Test Method for Shear Strength Properties of Metal-to-Metal Adhesives Using Tensile Loads". The test results are shown in the following table: Table 2 Shear strength performance test results It can be seen from Table 2 that the primer prepared by the method of the present application can effectively improve the bonding effect of the primer.
[0055] In comparative examples 1-4, after the molded silica gel is treated with a primer product obtained by directly mixing a film-forming agent with a variety of coupling agents, cross-linking agents and other materials, the bonding effect is poor.
[0056] Combining Example 1 and Comparative Example 5, it can be seen that the shear strength of Example 1 is better than that of Comparative Example 5, which means that when no tackifier is added, the bonding effect of the prepared primer is poor.
[0057] Combining Example 2 and Comparative Example 6, it can be seen that the shear strength of Example 2 is better than that of Comparative Example 6, which means that when no tackifier is added, the bonding effect of the prepared primer is poor.
[0058] Combining Example 6 and Comparative Example 7, it can be seen that the shear strength of Example 6 is better than that of Comparative Example 7, which means that when no tackifier is added, the bonding effect of the prepared primer is poor.
[0059] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the protection scope of the present invention.
Claims
1. A peroxide-type primer for addition-type liquid silicone adhesive-type silicone, characterized in that: The primer comprises the following raw materials in parts by weight: Film-forming agent 0.3-5 parts; 0.1-15 parts of the first silane coupling agent; 0.5-5 parts of tackifier; Cross-linking agent 0.2-2 parts; 50-80 parts of organic solvent; Catalyst 0.1-1 part.
2. A peroxide-based primer for addition-type liquid silicone adhesive-type silicone according to claim 1, characterized in that: The tackifier comprises the following raw materials in parts by weight: 160-310 parts of the second silane coupling agent; 5-50 parts of deionized water; 0.1-0.5 parts of concentrated hydrochloric acid; Sodium bicarbonate 0.1-0.
8.
3. A peroxide-based primer for addition-type liquid silicone adhesive-type silicone according to claim 2, characterized in that: The second silane coupling agent includes at least one of vinyl triethoxysilane, vinyl trimethoxysilane, vinyl methyl dimethoxysilane, vinyl methyl diethoxysilane, hexamethyl disiloxane, tetramethyl divinyl disiloxane, vinyl dimethyl methoxy silane, vinyl dimethyl ethoxy silane, γ-glycidyl ether oxypropyl trimethoxy silane, γ-glycidyl ether oxypropyl methyl dimethoxy silane, γ-glycidyl ether oxypropyl methyl diethoxy silane, γ-(methacryloxy) propyl trimethoxy silane, γ-(methacryloxy) propyl methyl dimethoxy silane, octyl trimethoxy silane, and phenyl triethoxy silane.
4. A peroxide-type primer for addition-type liquid silicone adhesive-type silicone according to claim 2, characterized in that: The preparation method of the tackifier comprises the following steps: mixing a second silane coupling agent, deionized water and concentrated hydrochloric acid, reacting at 60-80°C for 6-8 hours, cooling to 45-55°C, adding sodium bicarbonate and reacting for 2-4 hours, performing reduced pressure distillation at 60-80°C, removing low boiling substances, filtering and obtaining the tackifier.
5. The peroxide-based primer for addition-type liquid silicone adhesive-type silicone according to claim 1, characterized in that: The film former includes at least one of epoxy resin, acrylic resin, polyester resin or polyalkoxy oligomer.
6. A peroxide-based primer for addition-type liquid silicone adhesive-type silicone according to claim 1, characterized in that: The first silane coupling agent includes at least one of vinyl triethoxysilane, vinyl trimethoxysilane, vinyl methyl dimethoxysilane, vinyl methyl diethoxysilane, hexamethyldisiloxane, tetramethyl divinyl disiloxane, vinyl dimethyl methoxysilane, vinyl dimethyl ethoxysilane, γ-glycidyloxypropyl trimethoxysilane, γ-glycidyloxypropyl methyl dimethoxysilane, γ-glycidyloxypropyl methyl diethoxysilane, γ-(methacryloxy)propyl trimethoxysilane, γ-(methacryloxy)propyl methyl dimethoxysilane, octyl trimethoxysilane, and phenyl triethoxysilane.
7. A peroxide-based primer for addition-type liquid silicone adhesive-type silicone according to claim 1, characterized in that: The crosslinking agent includes at least one of tetraethyl silicate, ethyl titanate, n-butyl titanate, isopropyl titanate, tris(3-trimethoxysilylpropyl)isocyanurate, triallyl isocyanurate, bis(triethoxysilyl)ethane, and bis(trimethoxysilylethyl)benzene.
8. The peroxide-based primer for addition-type liquid silicone adhesive-type silicone according to claim 1, characterized in that: The organic solvent includes at least one of toluene, xylene, ethanol, isopropanol, cyclohexanol, n-heptane, white spirit, cyclohexane, ethylene glycol methyl ether, propylene glycol methyl ether, ethyl acetate, butyl acetate, and solvent oil.
9. The peroxide-based primer for addition-type liquid silicone adhesive-type silicone according to claim 1, characterized in that: The catalyst includes at least one of dicumyl peroxide, benzoyl peroxide, and 2,4-dichlorobenzoyl peroxide.
10. A method for preparing a peroxide-type primer for addition-type liquid silicone adhesive-type silicone according to any one of claims 1 to 9, characterized in that: The steps of the preparation method are as follows: Weigh each raw material according to the formula; After the film-forming agent, the first silane coupling agent, the tackifier, the cross-linking agent and the organic solvent are mixed, a catalyst is added, mixed and filtered to obtain a primer.