Preparation method for high-temperature-resistant silicon resin
A technology of high temperature resistance and resin, which is applied in the field of preparation of high temperature resistant silicone resin, can solve the problems of poor temperature resistance, complex reaction, and many raw materials, and achieve the effect of less environmental pollution
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Embodiment 1
[0019] 640g potassium acetate and 1700ml toluene were added to a four-neck flask, and the temperature was raised to reflux to remove water. Mix 424g of phenyltrichlorosilane and methyltrichlorosilane at a molar ratio of 3:1, and slowly add them dropwise into a four-neck flask. Control the reaction temperature at about 40°C. After the addition is complete, continue to stir for 2hr and add 209g methanol. In a four-necked flask, control the reaction temperature at 50°C. After the addition is complete, continue stirring for 1hr, heat up to 70°C and reflux for 2hr, recover the fraction below 78°C, distill out 484ml, add tap water to wash to pH=7, heat up and low pressure Distill toluene. 210 g of solid methyl phenyl silicone resin was obtained, the solid content was 99.5%, and the gel time was 28 minutes and 30 seconds.
Embodiment 2
[0021] 588g of sodium acetate and 1700ml of toluene were added to a four-necked flask, and the temperature was raised to reflux to remove water. Mix 426g of phenyltrichlorosilane, methyltrichlorosilane, and dimethyldichlorosilane with a molar ratio of 3:1:1, and slowly add them dropwise into a four-neck flask. Control the reaction temperature at about 42°C. Add dropwise After the completion, continue to stir for 2hr, add 215g of methanol to the four-necked flask, control the reaction temperature at 60℃, after the addition is complete, continue to stir for 1hr, heat up to 68℃, reflux for 2hr, recover the fraction below 80℃, distill out 496ml, add Wash with tap water to pH=7, and distill toluene at elevated temperature and low pressure. 200 g of solid methyl phenyl silicone resin was obtained, the solid content was 99.8%, and the gel time was 18 minutes and 47 seconds.
Embodiment 3
[0023] 671g of acetic anhydride and 1700ml of toluene were added to a four-necked flask and heated to reflux to remove water. Mix 575g of diphenyldichlorosilane and methyltrichlorosilane at a molar ratio of 3:2, and slowly add them dropwise into a four-neck flask. Control the reaction temperature at about 45°C. After the addition is complete, continue to stir for 2hr and add 215g Put methanol into a four-necked flask, control the reaction temperature at 60°C, after the addition, continue to stir for 1hr, heat up to 71°C and reflux for 2hr, recover the fraction below 80°C, distill 476ml, add tap water to wash to pH=7, warm up Toluene is distilled at low pressure. 215 g of solid methyl phenyl silicone resin was obtained, the solid content was 99.2%, and the gel time was 30 minutes and 15 seconds.
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