Bonding anti-yellowing silicone gel, its preparation method, tackifier used therein and its preparation method

Through the preparation method of dendritic structure tackifier, the problems of insufficient adhesion, aging resistance and yellowing resistance of traditional silicon gels are solved, and high adhesion and yellowing resistance of silicone gels are achieved, which are suitable for precision electronic components.

CN116751366BActive Publication Date: 2025-07-25TANGSHAN SANYOU SILICON IND
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Patent Information

Application Number
CN202310913768.7
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-07-25
Publication Date
2025-07-25
Estimated Expiration
2043-07-25

AI Technical Summary

Technical Problem

Traditional silicone gel products have shortcomings in adhesion, aging resistance and yellowing resistance, and cannot meet the potting requirements of precision electronic components.

Method used

A dendritic structured tackifier is used to prepare a bonded anti-yellowing silicone gel through addition reactions under a series of catalytic conditions. The tackifier is compatible with the silicone gel and provides multiple reactive groups to improve adhesion and anti-aging properties.

Benefits of technology

The prepared silicone gel has good fluidity, adhesion, anti-aging and yellowing properties, and does not affect the refractive index and electrical properties of the silicone gel.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention relates to the technical field of silicone gels, and in particular to a tackifier for a bonding type anti-yellowing silicone gel, a preparation method thereof, a bonding type anti-yellowing silicone gel containing the tackifier, and a preparation method thereof. The tackifier for the bonding type anti-yellowing silicone gel has a dendritic structure, has good compatibility with the prepared silicone gel, does not affect the refractive index and electrical properties of the silicone gel, and the silicone gel prepared by using the tackifier has good fluidity, adhesiveness, anti-aging property and anti-yellowing property.
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Description

Technical Field

[0001] The present invention relates to the technical field of silicone gels, and particularly to a tackifier for a bonding type anti-yellowing silicone gel, a preparation method thereof, a bonding type anti-yellowing silicone gel containing the tackifier, and a preparation method thereof. Background Art

[0002] Silicone gel refers to a silicone rubber product with a hardness of zero, which is mainly used for some precision electronic components with a hardness requirement of zero to reduce the damage to electronic components during deformation. Traditional silicone gel products have poor adhesion to substrates, are prone to aging and yellowing after long-term use, and cannot meet the potting requirements for precision electronic components. Patent CN110305486B discloses a silicone gel and a preparation method thereof. This patent uses the traditional hydrosilylation method to prepare silicone gel, and its anti-yellowing and adhesion properties are poor; Patent CN102516775A discloses a highly adhesive silicone gel for potting precision electronic components. This patent uses additives containing epoxy groups, alkoxy groups, MQ resin, etc. as tackifiers. Although it has adhesiveness, its anti-aging property is poor; Patent CN110408031A discloses an active branched carbosilane with multi-terminal functional groups and a preparation method thereof. The compound prepared by this method does not have adhesiveness. Summary of the Invention

[0003] In order to solve the above technical problems, the present invention provides a tackifier for a bonding type anti-yellowing silicone gel, a preparation method thereof, a bonding type anti-yellowing silicone gel containing the tackifier, and a preparation method thereof. The tackifier has good compatibility with the silicone gel and significantly improves the adhesiveness, anti-aging property and anti-yellowing property of the silicone gel.

[0004] To achieve the above technical objectives, the present invention adopts the following solutions:

[0005] In the first aspect, the present invention provides a tackifier for a bonding type anti-yellowing silicone gel, and its structural formula is:

[0006]

[0007] Wherein the structural formula of R1 is:

[0008]

[0009] The structural formula of R2 is:

[0010]

[0011] Or

[0012]

[0013] The preparation method of the above-mentioned tackifier includes the following steps:

[0014] S1. Hydrolyze phenylalkoxysilane under acidic conditions, and then carry out a condensation reaction with tetramethylhydroxyvinylsiloxane or vinylhydroxysiloxane under alkaline conditions. After the reaction is completed, carry out vacuum distillation to obtain product a;

[0015] S2. Carry out an addition reaction between a and tetramethyldihydrodisiloxane under catalytic conditions to obtain product b;

[0016] S3. Carry out an addition reaction between b and tetravinylsilane or tetramethylhydroxyvinylsiloxane under catalytic conditions to obtain product c;

[0017] S4. Carry out an addition reaction between c and tetramethyldihydrodisiloxane under catalytic conditions to obtain product d;

[0018] S5. React d with epoxyalkoxysilane under catalytic conditions. After the reaction is completed, carry out vacuum distillation to obtain the target product e;

[0019] S6. React e with tetramethyldihydrodisiloxane under catalytic conditions. After the reaction is completed, carry out vacuum distillation to obtain the target product f;

[0020] S7. React f with divinylalkoxysilane under catalytic conditions. After the reaction is completed, carry out vacuum distillation to obtain a tackifier for a bonding-type anti-yellowing silicone gel.

[0021] Further, in step S1, the molar ratio of phenylalkoxysilane to tetramethylhydroxyvinylsiloxane or vinylhydroxysiloxane is 1:3. The phenylalkoxysilane is phenyltrimethoxysilane or phenyltriethoxysilane. The hydrolysis reaction temperature is 60 ± 5°C. The acid added is hydrochloric acid or sulfuric acid, and the addition amount is 5% of the total mass of the raw materials. The hydrolysis reaction time is 1 hour. After the reaction is completed, wash with water to neutrality at 40 ± 2°C.

[0022] Further, in step S1, the condensation reaction temperature is 50 ± 5°C, the reaction time is 1 hour, the base added is sodium hydroxide or potassium hydroxide, and after the reaction, neutralize with phosphoric acid.

[0023] Further, in steps S2 - S4, the catalyst is a platinum catalyst, the reaction temperature is 60 - 70°C, and the reaction time is 1 - 2 hours; in steps S5 - S7, the catalyst is dodecylbenzenesulfonic acid, the reaction temperature is 80 - 90°C, and the reaction time is 2 - 3 hours.

[0024] Further, in step S5, the epoxyalkoxysilane is one of (epoxypropoxy)propyltrimethoxysilane, (epoxypropoxy)propyltriethoxysilane, (epoxypropoxy)propyldimethoxysilane, or (epoxypropoxy)propyldiethoxysilane;

[0025] In step S7, the divinylalkoxysilane is divinyldimethylsilane or divinyldiethylsilane.

[0026] In a second aspect, the present invention also provides an adhesive anti-yellowing silicone gel, which is formed by mixing component A and component B, and the mass ratio of component A to component B is 1:1;

[0027] Component A includes the following components by weight: 10-20 parts of vinyl-terminated phenylsiloxane, 5-20 parts of terminal hydrogen-containing siloxane, 10-20 parts of side hydrogen-containing siloxane, and 0-0.01 part of inhibitor;

[0028] Component B includes the following components by weight: 50-80 parts of vinyl-terminated phenylsiloxane, 5-10 parts of the tackifier as described above, and 0.0001-0.03 part of platinum catalyst.

[0029] Furthermore, the vinyl content of the vinyl-terminated phenylsiloxane is 0.27-0.53 wt%, the phenyl content is 5-10 wt%, and the viscosity is 500-1000 mPa·s;

[0030] The hydrogen content of the terminal hydrogen-containing siloxane is 0.09-0.20 wt%, and the viscosity is 20-30 mPa·s;

[0031] The hydrogen content of the side hydrogen-containing siloxane is 0.025-0.06 wt%, and the viscosity is 40-50 mPa·s.

[0032] Furthermore, the inhibitor is vinylsiloxane and / or alkynol, and the platinum catalyst is a complex of platinum.

[0033] The preparation method of the above-mentioned adhesive anti-yellowing silicone gel includes the following steps:

[0034] Prepare component A: Mix vinyl-terminated phenylsiloxane, terminal hydrogen-containing siloxane and side hydrogen-containing siloxane in proportion, add an inhibitor, and stir evenly to obtain component A;

[0035] Prepare component B: Mix vinyl-terminated phenylsiloxane and the tackifier as described above evenly in proportion, add a platinum catalyst, and obtain component B;

[0036] Mix component A and component B evenly in equal mass to obtain the adhesive anti-yellowing silicone gel.

[0037] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0038] The present invention provides a tackifier for a bonding type anti-yellowing silicone gel, a preparation method thereof, a bonding type anti-yellowing silicone gel containing the tackifier, and a preparation method thereof. The tackifier for the bonding type anti-yellowing silicone gel has a dendritic structure, can provide a plurality of reactive groups, has good compatibility during the preparation of the silicone gel, does not affect the refractive index and electrical properties of the silicone gel, and the silicone gel prepared by using the tackifier has good fluidity, adhesiveness, anti-aging property, and anti-yellowing property. Detailed Embodiments

[0039] To fully understand the purpose, features, and effects of the present invention, the present invention will be described in detail through the following specific embodiments, but the present invention is not limited thereto.

[0040] Example 1

[0041] A preparation method of a tackifier for a bonding type anti-yellowing silicone gel is provided.

[0042] S1. Mix 10 g of phenyltrimethoxysilane with 20 g of isopropanol evenly, add 60 g of deionized water to the above mixture, and the concentrated hydrochloric acid is 5% of the total mass. Heat up to 60 °C and carry out a hydrolysis reaction for 1 h. Let the reacted solution stand, separate the acid water, add deionized water, and wash to neutral at 40 °C. Add 27 g of tetramethylhydroxyvinylsiloxane to the above solution, add a sodium hydroxide solution (concentration: 50%) accounting for 5% of the raw material mass, carry out a condensation reaction at 50 °C for 1 hour. After the reaction ends, add phosphoric acid for neutralization, and carry out vacuum distillation to obtain product a;

[0043] S2. Add 21 g of tetramethyldihydrodisiloxane to a, and add 10 ppm of a platinum catalyst at 60 °C and react for 1 hour to obtain product b;

[0044] S3. Add 21 g of tetraethylsilane to b, and add 10 ppm of a platinum catalyst at 60 °C and react for 1 hour to obtain product c;

[0045] S4. Add 61 g of tetramethyldihydrodisiloxane to c, and add 10 ppm of a platinum catalyst at 60 °C and react for 1 hour to obtain product d;

[0046] S5. Add 107 g of (glycidoxy)propyltrimethoxysilane to d, then add 5% of dodecylbenzenesulfonic acid and react at 80 °C for 2 h. After the reaction ends, carry out vacuum distillation to obtain product e;

[0047] S6. Add 30 g of tetramethyldihydrodisiloxane to e, add 5% of dodecylbenzenesulfonic acid and react at 80 °C for 2 h. After the reaction ends, carry out vacuum distillation to obtain product f;

[0048] S7. Add 169 g of divinyldimethoxysiloxane to f, add 5% dodecylbenzenesulfonic acid, react at 80 °C for 2 h, and after the reaction, perform vacuum distillation to obtain a tackifier for a bonding type anti-yellowing organogel.

[0049] Example 2

[0050] Provide a preparation method for a tackifier for a bonding type anti-yellowing silicone gel.

[0051] S1. Mix 10 g of phenyltriethoxysilane and 20 g of isopropanol evenly, add 60 g of deionized water to the above mixture, and the concentrated hydrochloric acid is 5% of the total mass. Heat to 60 °C and carry out a hydrolysis reaction for 1 h. Let the reaction solution stand, separate out the acid water, add deionized water, and wash to neutral at 40 °C. Add 22 g of tetramethylhydroxyvinylsiloxane to the above solution, add a sodium hydroxide solution (concentration 50%) of 5% of the raw material mass, carry out a condensation reaction at 50 °C for 1 hour. After the reaction, add phosphoric acid for neutralization and perform vacuum distillation to obtain product a;

[0052] S2. Add 16.7 g of tetramethyldihydrodisiloxane to a, add 10 ppm of a platinum catalyst at 60 °C, and react for 1 h to obtain product b;

[0053] S3. Add 17 g of tetravinylsilane to b, add 10 ppm of a platinum catalyst at 60 °C, and react for 1 h to obtain product c;

[0054] S4. Add 50 g of tetramethyldihydrodisiloxane to c, add 10 ppm of a platinum catalyst at 60 °C, and react for 1 h to obtain product d;

[0055] S5. Add 105 g of (glycidoxy)propyltriethoxysilane to d, then add 5% dodecylbenzenesulfonic acid and react at 80 °C for 2 h. After the reaction, perform vacuum distillation to obtain product e;

[0056] S6. Add 25 g of tetramethyldihydrodisiloxane to e, add 5% dodecylbenzenesulfonic acid and react at 80 °C for 2 h. After the reaction, perform vacuum distillation to obtain product f;

[0057] S7. Add 140 g of divinyldiethoxysiloxane to f, add 5% dodecylbenzenesulfonic acid and react at 80 °C for 2 h. After the reaction, perform vacuum distillation to obtain a tackifier for a bonding type anti-yellowing organogel.

[0058] Example 3

[0059] Provide a preparation method for a tackifier for a bonding type anti-yellowing silicone gel.

[0060] S1. Mix 10 g of phenyltriethoxysilane evenly with 20 g of isopropanol. Add 60 g of deionized water to the above mixture, and the concentrated hydrochloric acid is 5% of the total mass. Heat up to 60 °C and carry out a hydrolysis reaction for 1 h. Let the reacted solution stand, separate out the acid water, add deionized water, and wash it to neutral at 40 °C. Add 15 g of vinylhydroxysiloxane to the above solution, add a sodium hydroxide solution (concentration 50%) of 5% of the raw material mass, carry out a condensation reaction at 50 °C for 1 hour. After the reaction is completed, add phosphoric acid for neutralization and carry out vacuum distillation to obtain product a;

[0061] S2. Add 16.7 g of tetramethyldihydrodisiloxane to a, and under the condition of 60 °C, add 10 ppm of platinum catalyst and react for 1 hour to obtain product b;

[0062] S3. Add 22 g of tetramethylhydroxyvinylsiloxane to b, and under the condition of 60 °C, add 10 ppm of platinum catalyst and react for 1 hour to obtain product c;

[0063] S4. Add 50 g of tetramethyldihydrodisiloxane to c, under the condition of 60 °C, add 10 ppm of platinum catalyst and react for 1 hour to obtain product d;

[0064] S5. Add 90 g of (glycidoxy)propyl diethoxysilane to d, then add 5% of dodecylbenzenesulfonic acid and react at 80 °C for 2 h. After the reaction is completed, carry out vacuum distillation to obtain product e;

[0065] S6. Add 25 g of tetramethyldihydrodisiloxane to e, add 5% of dodecylbenzenesulfonic acid and react at 80 °C for 2 h. After the reaction is completed, carry out vacuum distillation to obtain product f;

[0066] S7. Add 102 g of divinyldimethoxysilane to f, add 5% of dodecylbenzenesulfonic acid and react at 80 °C for 2 h. After the reaction is completed, carry out vacuum distillation to obtain a tackifier for a bonding type anti-yellowing organogel.

[0067] Example 4

[0068] Provide a preparation method for a tackifier for a bonding type anti-yellowing silicone gel.

[0069] S1. Mix 10 g of phenyltriethoxysilane evenly with 20 g of isopropanol. Add 60 g of deionized water to the above mixture, and the concentrated hydrochloric acid is 5% of the total mass. Heat up to 60 °C and carry out a hydrolysis reaction for 1 h. Let the reacted solution stand, separate out the acid water, add deionized water, and wash it to neutral at 40 °C. Add 15 g of vinylhydroxysiloxane to the above solution, add a sodium hydroxide solution (concentration 50%) of 5% of the raw material mass, carry out a condensation reaction at 50 °C for 1 hour. After the reaction is completed, add phosphoric acid for neutralization and carry out vacuum distillation to obtain product a;

[0070] S2. Add 16.7 g of tetramethyldihydrodisiloxane to a, and at 60 °C, add 10 ppm of platinum catalyst and react for 1 hour to obtain product b;

[0071] S3. Add 22 g of tetramethylhydroxyvinylsiloxane to b, and at 60 °C, add 10 ppm of platinum catalyst and react for 1 hour to obtain product c;

[0072] S4. Add 50 g of tetramethyldihydrodisiloxane to c, and at 60 °C, add 10 ppm of platinum catalyst and react for 1 hour to obtain product d;

[0073] S5. Add 85 g of (glycidoxy)propyl dimethoxysilane to d, then add 5% dodecylbenzenesulfonic acid and react at 80 °C for 2 h. After the reaction, carry out vacuum distillation to obtain product e;

[0074] S6. Add 25 g of tetramethyldihydrodisiloxane to e, add 5% dodecylbenzenesulfonic acid and react at 80 °C for 2 h. After the reaction, carry out vacuum distillation to obtain product f;

[0075] S7. Add 110 g of divinyldimethoxysilane to f, add 5% dodecylbenzenesulfonic acid and react at 80 °C for 2 h. After the reaction, carry out vacuum distillation to obtain a tackifier for a bonding type anti-yellowing organogel.

[0076] Example 5

[0077] Provide a bonding type anti-yellowing silicone gel and its preparation method.

[0078] Preparation of Component A: Mix vinyl-terminated phenylsiloxane (vinyl content 0.27 wt%, viscosity 1000 mPa·s), hydrogen-terminated siloxane (hydrogen content 0.15 wt%, viscosity 20 mPa·s), and side hydrogen-containing siloxane (hydrogen content 0.03 wt%, viscosity 40 mPa·s) evenly in a mass ratio of 10:5:10, add 20 ppm of inhibitor, and stir evenly to obtain Component A;

[0079] Preparation of Component B: Mix vinyl-terminated phenylsiloxane (vinyl content 0.27 wt%, viscosity 500 mPa·s) and the tackifier prepared in Example 1 evenly in a mass ratio of 50:5, add 15 ppm of catalyst to obtain Component B;

[0080] Mix Component A and Component B evenly in equal mass to prepare a bonding type anti-yellowing silicone gel.

[0081] Example 6

[0082] Provide a bonding type anti-yellowing silicone gel and its preparation method.

[0083] Preparation of Component A: Mix vinyl-terminated phenyl siloxane (vinyl content 0.30 wt%, viscosity 900 mPa·s), terminal hydrogen-containing siloxane (hydrogen content 0.15 wt%, viscosity 25 mPa·s), and side hydrogen-containing siloxane (hydrogen content 0.05 wt%, viscosity 45 mPa·s) evenly according to a mass ratio of 15:10:15, add 20 ppm of inhibitor, and stir evenly to obtain Component A;

[0084] Preparation of Component B: Mix vinyl-terminated phenyl siloxane (vinyl content 0.30 wt%, viscosity 900 mPa·s) and the tackifier prepared in Example 2 evenly according to a mass ratio of 60:8, add 15 ppm of catalyst to obtain Component B;

[0085] Mix Component A and Component B evenly in equal mass to prepare a bonding type anti-yellowing silicone gel.

[0086] Example 7

[0087] Provide a bonding type anti-yellowing silicone gel and its preparation method.

[0088] Preparation of Component A: Mix vinyl-terminated phenyl siloxane (vinyl content 0.38 wt%, viscosity 700 mPa·s), terminal hydrogen-containing siloxane (hydrogen content 0.15 wt%, viscosity 30 mPa·s), and side hydrogen-containing siloxane (hydrogen content 0.05 wt%, viscosity 50 mPa·s) evenly according to a mass ratio of 15:10:15, add 20 ppm of inhibitor, and stir evenly to obtain Component A;

[0089] Preparation of Component B: Mix vinyl-terminated phenyl siloxane (vinyl content 0.42 wt%, viscosity 500 mPa·s) and the tackifier prepared in Example 3 evenly according to a mass ratio of 60:8, add 15 ppm of catalyst to obtain Component B.

[0090] Mix Component A and Component B evenly in equal mass to prepare a bonding type anti-yellowing silicone gel.

[0091] Example 8

[0092] Provide a bonding type anti-yellowing silicone gel and its preparation method.

[0093] Preparation of Component A: Vinyl-terminated phenyl siloxane (vinyl content 0.42 wt%, viscosity 500 mPa·s), hydrogen-terminated siloxane (hydrogen content 0.15 wt%, viscosity 30 mPa·s), and side hydrogen-containing siloxane (hydrogen content 0.05 wt%, viscosity 50 mPa·s) were mixed evenly in a mass ratio of 15:10:15. 20 ppm of inhibitor was added and stirred evenly to obtain Component A.

[0094] Preparation of Component B: Vinyl-terminated phenyl siloxane (vinyl content 0.42 wt%, viscosity 500 mPa·s) and the tackifier prepared in Example 4 were mixed evenly in a mass ratio of 60:8. 15 ppm of catalyst was added to obtain Component B.

[0095] Component A and Component B were mixed evenly in equal mass to prepare a bonding type anti-yellowing silicone gel.

[0096] Example 9

[0097] Provide a bonding type anti-yellowing silicone gel and its preparation method.

[0098] Preparation of Component A: Vinyl-terminated phenyl siloxane (vinyl content 0.30 wt%, viscosity 900 mPa·s), hydrogen-terminated siloxane (hydrogen content 0.15 wt%, viscosity 25 mPa·s), and side hydrogen-containing siloxane (hydrogen content 0.05 wt%, viscosity 45 mPa·s) were mixed evenly in a mass ratio of 15:10:15. 20 ppm of inhibitor was added and stirred evenly to obtain Component A.

[0099] Preparation of Component B: Vinyl-terminated phenyl siloxane (vinyl content 0.30 wt%, viscosity 900 mPa·s) and the tackifier prepared in Example 2 were mixed evenly in a mass ratio of 60:10. 15 ppm of catalyst was added to obtain Component B.

[0100] Component A and Component B were mixed evenly in equal mass to prepare a bonding type anti-yellowing silicone gel.

[0101] Example 10

[0102] Provide a bonding type anti-yellowing silicone gel and its preparation method.

[0103] Preparation of Component A: Vinyl-terminated phenyl siloxane (vinyl content 0.30 wt%, viscosity 900 mPa·s), hydrogen-terminated siloxane (hydrogen content 0.15 wt%, viscosity 25 mPa·s), and side hydrogen-containing siloxane (hydrogen content 0.05 wt%, viscosity 45 mPa·s) were mixed evenly in a mass ratio of 15:10:15. 20 ppm of inhibitor was added and stirred evenly to obtain Component A.

[0104] Preparation of Component B: Vinyl-terminated phenyl siloxane (vinyl content 0.30 wt%, viscosity 900 mPa·s) and the tackifier prepared in Example 2 were mixed evenly at a mass ratio of 60:11, and 15 ppm of catalyst was added to obtain Component B;

[0105] The Component A and Component B were mixed evenly in equal mass to prepare a bonding type anti-yellowing silicone gel.

[0106] Example 11

[0107] Provide a bonding type anti-yellowing silicone gel and its preparation method.

[0108] Preparation of Component A: Vinyl-terminated phenyl siloxane (vinyl content 0.30 wt%, viscosity 900 mPa·s), hydrogen-terminated siloxane (hydrogen content 0.15 wt%, viscosity 25 mPa·s), and side hydrogen-containing siloxane (hydrogen content 0.05 wt%, viscosity 45 mPa·s) were mixed evenly at a mass ratio of 15:10:15, 20 ppm of inhibitor was added, and stirred evenly to obtain Component A;

[0109] Preparation of Component B: Vinyl-terminated phenyl siloxane (vinyl content 0.30 wt%, viscosity 900 mPa·s) and the tackifier prepared in Example 2 were mixed evenly at a mass ratio of 60:4, and 15 ppm of catalyst was added to obtain Component B;

[0110] The Component A and Component B were mixed evenly in equal mass to prepare a bonding type anti-yellowing silicone gel.

[0111] Comparative Example 1

[0112] Provide a bonding type anti-yellowing silicone gel and its preparation method.

[0113] Preparation of Component A: Vinyl-terminated phenyl siloxane (vinyl content 0.30 wt%, viscosity 900 mPa·s), hydrogen-terminated siloxane (hydrogen content 0.15 wt%, viscosity 25 mPa·s), and side hydrogen-containing siloxane (hydrogen content 0.05 wt%, viscosity 45 mPa·s) were mixed evenly at a mass ratio of 15:10:15, 20 ppm of inhibitor was added, and stirred evenly to obtain Component A;

[0114] Preparation of Component B: Vinyl-terminated phenyl siloxane (vinyl content 0.30 wt%, viscosity 900 mPa·s) and MQ resin were mixed evenly at a mass ratio of 60:8, and 15 ppm of catalyst was added to obtain Component B;

[0115] The Component A and Component B were mixed evenly in equal mass to prepare a bonding type anti-yellowing silicone gel.

[0116] Comparative Example 2

[0117] The selected silicone gel is a commercially available silicone gel (silicone gel prepared by Hebei Hongtu Rubber and Plastic Products).

[0118] Comparative Example 3

[0119] The selected silicone gel is a commercially available silicone gel (Saimosi New Materials).

[0120] The silicone gels of Examples 5 to 11 and Comparative Examples 1 to 3 were cured at room temperature, and their performance was tested. The test results are shown in Table 1.

[0121] Table 1 Performance Test Results of Silicone Gels in Examples 5 to 11 and Comparative Examples 1 to 3

[0122]

[0123] As can be seen from Table 1, the refractive index and anti-yellowing property of the silicone gels in Examples 5 to 11 are better than those in Comparative Examples 1 to 3, indicating that the silicone gels prepared by the tackifier of the present invention have good refractive index and anti-yellowing properties. When the addition amount of the tackifier is 5 to 10 parts, the silicone gel does not turn yellow after being irradiated with ultraviolet light, and the anti-yellowing property is excellent. By comparing the shear strength, it can be seen that the shear strength of Examples 5 to 11 is higher than that of Comparative Examples 1 to 3, indicating that the adhesiveness of Examples 5 to 11 is better than that of Comparative Examples 1 to 3.

[0124] Finally, it should be noted that the above are only the preferred embodiments of the present invention. Of course, those skilled in the art can make changes and modifications to the present invention. If these modifications and variations fall within the scope of the claims of the present invention and its equivalent technologies, they should be considered as the protection scope of the present invention.

Claims

1. A tackifier for a bonding type anti-yellowing silicone gel, characterized in that, Its structural formula is: Among them, the structural formula of R1 is: The structural formula of R2 is:

2. A method for preparing a tackifier as described in claim 1, characterized in that, It includes the following steps: S1. Hydrolyze phenylalkoxysilane under acidic conditions, and then carry out a condensation reaction with tetramethylhydroxyvinylsiloxane or vinylhydroxysiloxane under alkaline conditions. After the reaction is completed, carry out vacuum distillation to obtain product a; S2. Carry out an addition reaction between a and tetramethyldihydrodisiloxane under catalytic conditions to obtain product b; S3. Carry out an addition reaction between b and tetravinylsilane or tetramethylhydroxyvinylsiloxane under catalytic conditions to obtain product c; S4. Carry out an addition reaction between c and tetramethyldihydrodisiloxane under catalytic conditions to obtain product d; S5. Carry out a reaction between d and epoxyalkoxysiloxane under catalytic conditions. After the reaction is completed, carry out vacuum distillation to obtain the target product e; S6. Carry out a reaction between e and tetramethyldihydrodisiloxane under catalytic conditions. After the reaction is completed, carry out vacuum distillation to obtain the target product f; S7. Carry out a reaction between f and divinyldialkoxysilane under catalytic conditions. After the reaction is completed, carry out vacuum distillation to obtain a tackifier for a bonding type anti-yellowing silicone gel.

3. The preparation method of the tackifier according to claim 2, wherein, In step S1, the molar ratio of phenylalkoxysilane to tetramethylhydroxyvinylsiloxane or vinylhydroxysiloxane is 1:

3. The phenylalkoxysilane is phenyltrimethoxysilane or phenyltriethoxysilane. The hydrolysis reaction temperature is 60±5°C. The acid added is hydrochloric acid or sulfuric acid, and the acid addition amount is 5% of the total mass of the raw materials. The hydrolysis reaction time is 1 hour. After the reaction is completed, wash with water to neutrality at 40±2°C.

4. The preparation method of the tackifier according to claim 2, characterized in that, In step S1, the condensation reaction temperature is 50±5°C, the reaction time is 1 hour, the base added is sodium hydroxide or potassium hydroxide, and after the reaction, it is neutralized with phosphoric acid.

5. The preparation method of the tackifier according to claim 2, characterized in that, The catalyst used in steps S2 to S4 is a platinum catalyst, the reaction temperature is 60 to 70°C, and the reaction time is 1 to 2 hours; the catalyst in steps S5 to S7 is dodecylbenzenesulfonic acid, the reaction temperature is 80 to 90°C, and the reaction time is 2 to 3 hours.

6. The preparation method of the tackifier according to claim 2, wherein In step S5, the epoxyalkoxysilane is one of (glycidoxy)propyltrimethoxysilane, (glycidoxy)propyltriethoxysilane, (glycidoxy)propyldimethoxysilane or (glycidoxy)propyldiethoxysilane; In step S7, the divinyldialkoxysilane is divinyldimethylsilane or divinyldiethylsilane.

7. A bonded anti-yellowing silicone gel, characterized in that, It is composed of component A and component B, and the mass ratio of component A to component B is 1:1; Component A includes the following components by weight: 10 to 20 parts of vinyl-terminated phenylsiloxane, 5 to 20 parts of hydrogen-terminated siloxane, 10 to 20 parts of side hydrogen-containing siloxane, and 0 to 0.01 part of inhibitor; Component B includes the following components by weight: 50 to 80 parts of vinyl-terminated phenylsiloxane, 5 to 10 parts of the tackifier as described in claim 1, and 0.0001 to 0.03 part of platinum catalyst.

8. The adhesive anti-yellowing silicone gel according to claim 7, characterized in that, The vinyl content of the vinyl-terminated phenylsiloxane is 0.27 to 0.53 wt%, the phenyl content is 5 to 10 wt%, and the viscosity is 500 to 1000 mPa·s; The hydrogen content of the terminal hydrogen-containing siloxane is 0.09 - 0.20 wt%, and the viscosity is 20 - 30 mPa·s; The hydrogen content of the side hydrogen-containing siloxane is 0.025 - 0.06 wt%, and the viscosity is 40 - 50 mPa·s.

9. The adhesive anti-yellowing silicone gel according to claim 7, wherein The inhibitor is vinyl siloxane and / or alkynol, and the platinum catalyst is a complex of platinum.

10. A method for preparing the adhesive anti-yellowing silicone gel as described in claim 7, characterized in that, It includes the following steps: Prepare Component A: The vinyl-terminated phenyl siloxane, terminal hydrogen-containing siloxane and side hydrogen-containing siloxane are mixed in proportion, and an inhibitor is added and stirred evenly to obtain Component A; Prepare Component B: The vinyl-terminated phenyl siloxane and the tackifier as described in Claim 1 are mixed evenly in proportion, and a platinum catalyst is added to obtain Component B; Mix Component A and Component B in equal mass and stir evenly to obtain the adhesive anti-yellowing silicone gel.

Citation Information

Patent Citations

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