Modified MQ resin, and preparation method and application thereof

Abstract

The invention provides a modified MQ resin, and a preparation method and an application thereof. The modified MQ resin comprises a compound with a structure represented by formula I; and in the formula I, MA is selected from a functional group containing a beta-dicarbonyl group, MH is selected from dimethyl siloxane, M is selected from trimethyl siloxane, m is selected from 0.02 to 0.3, n is selected from 0.05 to 0.8, a is selected from 0.4 to 1.4, and m + n + a is greater than 0.6 and less than 1.6. The modified MQ resin provided by the invention has very good cohesiveness and good mechanicalstrength, so that the modified MQ resin provided by the invention is a cohesive reinforced modified MQ resin, the manufacturing process of the packaging adhesive can be simplified, and the productioncost of the packaging adhesive is reduced.

Description

technical field

[0001] The invention belongs to the technical field of silicone rubber and relates to a modified MQ resin and its preparation method and application, in particular to a modified MQ resin with bonding and reinforcing properties and its preparation method and application. Background technique

[0002] High-brightness light-emitting diode (Light Emitting Diode, LED) is a new type of lighting source. It consumes only 1 / 10 of the power of traditional light sources. It does not use mercury that seriously pollutes the environment. It is small in size, low in driving voltage and long in life. Become the new focus of the global lighting industry. At present, some thermoplastic resins such as polymethyl methacrylate, polycarbonate, optical nylon and thermosetting epoxy resin are mostly used for LED packaging. With the improvement of LED brightness and power, these materials are prone to discoloration due to poor heat resistance, resulting in light decay, which serious...

Examples

Embodiment 1

[0059] A modified MQ resin, the preparation method is as follows:

[0060] (1) Synthesis of hydrogen-containing MQ silicone resin

[0061] Add 240g of methyl MQ silicone resin (M / Q=0.9, Si-OH=1.8wt%), 1,1,3,3-tetramethyldi 11.3g of siloxane and 160g of n-hexane were stirred and heated to 45°C under nitrogen protection in a flask, 1.2g of trifluoromethanesulfonic acid and 0.15g of distilled water were added thereto, and the reaction was stirred at about 70°C for 6h. Then, cool to 50° C., add dimethylformamide to precipitate the catalyst, and then stir the reaction mixture at 50° C. for 1 h. Cool to room temperature, add 10 g of sodium bicarbonate for neutralization, filter, and concentrate under reduced pressure to a solid content of 70% (309 g, the mass fraction of Si-H groups in chemical analysis is 0.10%).

[0062] (2) Preparation of modified MQ resin

[0063] Add 12.8 g of allyl acetoacetate and 0.27 g of platinum catalyst into a four-necked flask equipped with a stirrer...

Embodiment 2

[0065] A modified MQ resin, the preparation method is as follows:

[0066] (1) Synthesis of hydrogen-containing MQ silicone resin

[0067] Add 240 g of methyl MQ silicone resin (M / Q=1.0, Si-OH=2wt%), 1,1,3,3-tetramethyldisilazol into a four-necked flask equipped with a stirrer, condenser and thermometer 20.9g of oxane and 160g of n-hexane were stirred and heated to 46°C under nitrogen protection in a flask, 1.2g of trifluoromethanesulfonic acid and 0.20g of distilled water were added thereto, and the reaction was stirred at about 70°C for 6h. Then, cool to 50° C., add dimethylformamide to precipitate the catalyst, and then stir the reaction mixture at 50° C. for 1 h. Cool to room temperature, add 10 g of sodium bicarbonate for neutralization, filter, and concentrate under reduced pressure to a solid content of 70% (341 g, the mass fraction of Si-H groups by chemical analysis is 0.11%).

[0068] (2) Preparation of modified MQ resin

[0069] Add 14.2 g of allyl acetoacetate a...

Embodiment 3

[0071] A modified MQ resin, the preparation method is as follows:

[0072] (1) Synthesis of hydrogen-containing MQ silicone resin

[0073] Add 240 g of methyl MQ silicone resin (M / Q=0.6, Si-OH=3wt%), 1,1,3,3-tetramethyldisilazol into a four-necked flask equipped with a stirrer, condenser, and thermometer 31.2g of oxane and 160g of n-hexane were stirred and heated to 46°C under nitrogen protection in a flask, 1.5g of trifluoromethanesulfonic acid and 0.30g of distilled water were added thereto, and the reaction was stirred at about 70°C for 6h. Then, cool to 50° C., add dimethylformamide to precipitate the catalyst, and then stir the reaction mixture at 50° C. for 1 h. Cool to room temperature, add 10 g of sodium bicarbonate to neutralize, filter, and concentrate under reduced pressure to a solid content of 70% (348 g, the mass fraction of Si-H groups in chemical analysis is 0.15%).

[0074] (2) Preparation of modified MQ resin

[0075] Add 9.4 g of allyl acetoacetate and 0....

technical field

[0001] The invention belongs to the technical field of silicone rubber and relates to a modified MQ resin and its preparation method and application, in particular to a modified MQ resin with bonding and reinforcing properties and its preparation method and application. Background technique

[0002] High-brightness light-emitting diode (Light Emitting Diode, LED) is a new type of lighting source. It consumes only 1 / 10 of the power of traditional light sources. It does not use mercury that seriously pollutes the environment. It is small in size, low in driving voltage and long in life. Become the new focus of the global lighting industry. At present, some thermoplastic resins such as polymethyl methacrylate, polycarbonate, optical nylon and thermosetting epoxy resin are mostly used for LED packaging. With the improvement of LED brightness and power, these materials are prone to discoloration due to poor heat resistance, resulting in light decay, which serious...

Examples

Embodiment 1

[0059] A modified MQ resin, the preparation method is as follows:

[0060] (1) Synthesis of hydrogen-containing MQ silicone resin

[0061] Add 240g of methyl MQ silicone resin (M / Q=0.9, Si-OH=1.8wt%), 1,1,3,3-tetramethyldi 11.3g of siloxane and 160g of n-hexane were stirred and heated to 45°C under nitrogen protection in a flask, 1.2g of trifluoromethanesulfonic acid and 0.15g of distilled water were added thereto, and the reaction was stirred at about 70°C for 6h. Then, cool to 50° C., add dimethylformamide to precipitate the catalyst, and then stir the reaction mixture at 50° C. for 1 h. Cool to room temperature, add 10 g of sodium bicarbonate for neutralization, filter, and concentrate under reduced pressure to a solid content of 70% (309 g, the mass fraction of Si-H groups in chemical analysis is 0.10%).

[0062] (2) Preparation of modified MQ resin

[0063] Add 12.8 g of allyl acetoacetate and 0.27 g of platinum catalyst into a four-necked flask equipped with a stirrer...

Embodiment 2

[0065] A modified MQ resin, the preparation method is as follows:

[0066] (1) Synthesis of hydrogen-containing MQ silicone resin

[0067] Add 240 g of methyl MQ silicone resin (M / Q=1.0, Si-OH=2wt%), 1,1,3,3-tetramethyldisilazol into a four-necked flask equipped with a stirrer, condenser and thermometer 20.9g of oxane and 160g of n-hexane were stirred and heated to 46°C under nitrogen protection in a flask, 1.2g of trifluoromethanesulfonic acid and 0.20g of distilled water were added thereto, and the reaction was stirred at about 70°C for 6h. Then, cool to 50° C., add dimethylformamide to precipitate the catalyst, and then stir the reaction mixture at 50° C. for 1 h. Cool to room temperature, add 10 g of sodium bicarbonate for neutralization, filter, and concentrate under reduced pressure to a solid content of 70% (341 g, the mass fraction of Si-H groups by chemical analysis is 0.11%).

[0068] (2) Preparation of modified MQ resin

[0069] Add 14.2 g of allyl acetoacetate a...

Embodiment 3

[0071] A modified MQ resin, the preparation method is as follows:

[0072] (1) Synthesis of hydrogen-containing MQ silicone resin

[0073] Add 240 g of methyl MQ silicone resin (M / Q=0.6, Si-OH=3wt%), 1,1,3,3-tetramethyldisilazol into a four-necked flask equipped with a stirrer, condenser, and thermometer 31.2g of oxane and 160g of n-hexane were stirred and heated to 46°C under nitrogen protection in a flask, 1.5g of trifluoromethanesulfonic acid and 0.30g of distilled water were added thereto, and the reaction was stirred at about 70°C for 6h. Then, cool to 50° C., add dimethylformamide to precipitate the catalyst, and then stir the reaction mixture at 50° C. for 1 h. Cool to room temperature, add 10 g of sodium bicarbonate to neutralize, filter, and concentrate under reduced pressure to a solid content of 70% (348 g, the mass fraction of Si-H groups in chemical analysis is 0.15%).

[0074] (2) Preparation of modified MQ resin

[0075] Add 9.4 g of allyl acetoacetate and 0....

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