Preparation method of high-temperature-resistant silicon resin containing phenylethynyl group
A technology of phenylethynyl and phenyltriethoxysilane, which is applied in the field of high-temperature-resistant silicone resin preparation, can solve the problems of low thermal stability of active groups and unsatisfactory temperature resistance of silicone resin, and achieve high-temperature resistance. Improved temperature resistance, simple and easy operation, and the effect of expanding the scope of application
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Embodiment 1
[0021] Example 1, add 240 g of water to the four-necked bottle, add hydrochloric acid to adjust the pH to 1, and place the four-necked bottle in an ice-water bath to cool to about 5°C. Mix 132g of phenylethynyltriethoxysilane, 37.1g of dimethyldiethoxysilane, and 170mL of toluene, and place them in a dropping funnel. Stirring was started, and the mixture was added dropwise to the four-necked bottle. After the dropwise addition, the ice-water bath was removed, heated to 80° C. with an electric heating mantle and maintained for 1 hour. After the reaction was completed, the reaction solution was poured into a separatory funnel and allowed to stand for stratification, the acidic water layer was removed, the organic layer was washed with distilled water until neutral, and dried by adding anhydrous calcium chloride. After drying, the organic solvent was evaporated under the reduced pressure of 0.05MPa, and then the polycondensation reaction was carried out at 0.01MPa and 120°C for ...
Embodiment 2
[0023] Example 2, add 360 g of water into the four-necked bottle, add sulfuric acid to adjust the pH to 0, and control the reaction temperature at about 50°C. Mix 58.6g of methylphenylethynyldiethoxysilane, 89.2g of methyltriethoxysilane, 450mL of toluene and 35mL of ether, and put them in the dropping funnel. Stirring was started, and the mixture was added dropwise to the four-necked bottle. After the dropwise addition was complete, the temperature was raised to 50°C and maintained for 3 hours. After the reaction was completed, the reaction solution was poured into a separatory funnel and allowed to stand for stratification, the acidic water layer was removed, the organic layer was washed with distilled water until neutral, and dried by adding anhydrous calcium chloride. After drying, the organic solvent was evaporated under the reduced pressure of 0.05MPa, and then the polycondensation reaction was carried out under the condition of 0.01MPa and 100°C for 60 minutes to obtai...
Embodiment 3
[0025] Example 3, add 170 g of water into the four-neck bottle, add acetic acid to adjust the pH to 2, and control the reaction temperature at about 25°C. Mix 88.2g of phenylethynyltriethoxysilane, 21.6g of methylphenylethynyldichlorosilane, 45.4g of diphenyldiethoxysilane, 235mL of toluene and 5mL of diethyl ether, and put them in the dropping funnel. Stirring was started, and the mixture was added dropwise to the four-necked bottle. After the dropwise addition was completed, the mixture was heated to 70° C. with an electric heating mantle and maintained for 2 hours. After the reaction was completed, the reaction solution was poured into a separatory funnel and allowed to stand for stratification, the acidic water layer was removed, the organic layer was washed with distilled water until neutral, and dried by adding anhydrous calcium chloride. After drying, the organic solvent was distilled off under a reduced pressure of 0.05 MPa, and then the polycondensation reaction was ...
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