Flame retardant tri-(tribromophenoxy) halogen propoxy silane compound and preparation method thereof
A technology of halopropoxysilane and tribromophenoxy, which is applied in the field of flame retardant trihalopropoxysilane compound and its preparation, can solve the problems of application limitation and high price of silicon-based flame retardants, and achieve production cost Low, overcome the effect of volatile reaction and high flame retardant efficiency
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[0032] Example 1 In a 500ml four-necked flask equipped with a stirrer, a thermometer, a dropping funnel, a high-efficiency reflux condenser, and a hydrogen chloride absorption device connected in series with a drying tube at the top of the condenser, the air in the flask was replaced with nitrogen , Add 180ml dioxane and 16.99g (0.1mol) silicon tetrachloride, while stirring, cool with an ice water bath to reduce the temperature of the reaction system to 0℃, add 9.45g dropwise to the organic solution of silicon tetrachloride (0.1mol) 2-Chloro-1-propanol, the temperature of the dripping process is controlled below 5℃, after dripping, the temperature is raised to 30℃ for 1h, and the reaction is kept for 1h. After the hydrogen chloride is released, add 99.24g (0.3mol) Tribromophenol, heat up to 90℃, heat preservation reaction for 7h, after the hydrogen chloride is discharged, cool down to below 40℃, install an extremely retractable soft sealing sleeve on the upper mouth of the conde...
Example Embodiment
[0033] Example 2 In a 500ml four-necked flask equipped with a stirrer, a thermometer, a dropping funnel, a high-efficiency reflux condenser and a hydrogen chloride absorption device connected in series with a drying tube at the top of the condenser, the air in the flask was replaced with nitrogen , Add 180ml of acetonitrile and 16.99g (0.1mol) of silicon tetrachloride, cool with an ice water bath while stirring, reduce the temperature of the reaction system to 0℃, and add 9.45g (0.1mol) to the organic solution of silicon tetrachloride. ) 1-Chloro-2-propanol, the temperature of the dripping process is controlled below 5℃, after dripping, the temperature is raised to 30℃ for 1h, and the reaction is kept for 1h. After the hydrogen chloride is released, add 99.24g (0.3mol) of tribromophenol After the hydrogen chloride is released, the temperature is lowered to below 40°C, and propylene oxide is added dropwise to remove the trace acid in the reaction solution. The end point is when t...
Example Embodiment
[0034] Example 3 In a 500ml four-necked flask equipped with a stirrer, a thermometer, a dropping funnel, a high-efficiency reflux condenser, and a hydrogen chloride absorption device connected in series with a drying tube at the top of the condenser, the air in the flask was replaced with nitrogen , Add 180ml tetrachloroethane and 16.99g (0.1mol) silicon tetrachloride, while stirring, cool with an ice water bath to reduce the temperature of the reaction system to 0℃, add 9.45g dropwise to the organic solution of silicon tetrachloride (0.1mol) 3-chloro-1-propanol, the temperature of the dropping process is controlled below 5°C, after dropping, the temperature is raised to 30°C for 1 hour, and the reaction is kept for 1 hour. After the hydrogen chloride is released, add 99.24g (0.3mol) Tribromophenol, heat up to 100℃, keep the temperature for 6h, after the hydrogen chloride is released, cool to below 40℃, add propylene oxide dropwise to remove the trace acid in the reaction soluti...
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