Addition type organic silicon resin as well as preparation method and application thereof
An addition type, silicone technology, applied in the direction of coating, can solve the problems of inability to meet the volatile content, difficult to control, equipment corrosion and so on
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Embodiment 1
[0051] Fill 33mol (594g) of water into a 5000ml glass bottle equipped with a stirrer, heating, condenser distillation and dropping funnel, and heat to 60°C. Under stirring, drop 2mol (480g) PhSi(OEt) through the dropping funnel 3 、1mol(134g)MeHSi(OEt) 2 , 1mol (160g) MeViSi (OEt) 2 , 0.5mol (54.3g) Me 3 SiCl mixture, the dropping time is 25min. Raise the temperature to 80°C and react for 8h. After the reaction was completed, it was cooled to room temperature, and 900 g of ethyl acetate was added. Stir, let stand, and divide the acid water. The organic layer was washed 500 mL×3 times until neutral, and ethyl acetate was distilled off. The temperature was raised to 150° C., and the vacuum pressure was maintained at 50 hPa for 3 hours to obtain 500 g of silane hydrolyzate.
[0052] Add 500 g of ethyl acetate and 25 g of trimethylchlorosilane to the above silane hydrolyzate, raise the temperature to 60° C., and react for 4 hours. Add 45g of absolute ethanol and continue th...
Embodiment 2
[0062] Put 208mol (3744g) of water in a 10000ml glass bottle equipped with a stirrer, heating, condenser distillation and dropping funnel and heat it to 30°C. Under stirring, drop 6mol (1188g) PhSi(OMe) through the dropping funnel 3 、3mol(402g)MeHSi(OEt) 2 , 1mol (132g) MeViSi (OMe) 2 , 2.0mol (217g) Me 3 SiCl mixture, the dropping time is 30min. Raise the temperature to 60°C and react for 3h. After the reaction was completed, it was cooled to room temperature, and 1000 g of dichloromethane was added. Stir, let stand, and divide the acid water. The organic layer was washed 1000 mL×3 times with water until neutral, and dichloromethane was distilled off. The temperature was raised to 50° C., and the vacuum pressure was maintained at 80 hPa for 4 hours to obtain 1200 g of silane hydrolyzate.
[0063] Add 700 g of dichloromethane and 15 g of trimethylchlorosilane to the above 1200 g of silane hydrolyzate, raise the temperature to 30° C., and react for 8 hours. Add 10g of a...
Embodiment 3
[0073] Fill 65mol (1170g) of water into a 5000ml glass bottle equipped with a stirrer, heating, condenser distillation and dropping funnel, and heat to 45°C. Under stirring, drop 3.0mol (720g) PhSi(OEt) through the dropping funnel 3 , 1.5mol (201g) MeHSi (OEt) 2 , 1mol (160g) MeViSi (OEt) 2 , 1.5mol (162.8g) Me 3 SiCl mixture, the dropwise addition time is 20min. Raise the temperature to 70°C and react for 5h. After the reaction is completed, cool to room temperature, and add 1500 g of petroleum ether (boiling range 60-90). Stir, let stand, and divide the acid water. The organic layer was washed 500 mL×3 times with water until neutral, and the petroleum ether was distilled off. The temperature was raised to 80° C., and the vacuum pressure was maintained at 30 hPa for 2 hours to obtain 780 g of silane hydrolyzate.
[0074] Add 700g of petroleum ether (boiling range 60-90) and 25g of trimethylchlorosilane to the above 780g of silane hydrolyzate, raise the temperature to 6...
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