A flame retardant tris(tribromophenoxy)dichloropropoxysilane compound and its preparation method
A technology of dichloropropoxysilane and tribromophenoxy, which is applied in the field of flame retardant tridichloropropoxysilane compound and its preparation, can solve the problems such as difficulty in finding substitutes, and achieve easy purification and separation, phase Good capacity and simple operation
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Embodiment 1
[0032] Example 1 In the 500ml four-necked flask equipped with agitator, thermometer, dropping funnel and high-efficiency reflux condenser and a hydrogen chloride absorbing device connected in series with a drying tube at the top of the condenser, replace the air in the bottle with nitrogen , add 180ml of diethylene glycol dimethyl ether and 16.99g (0.1mol) of silicon tetrachloride, under stirring, cool with an ice-water bath, reduce the temperature of the reaction system to 0 ° C, drop into the organic solution of silicon tetrachloride Add 12.90g (0.1mol) of 2,3-dichloro-1-propanol, and control the temperature below 8°C during the dropwise addition process. After the dropwise addition, raise the temperature to 35°C for 1 hour, and keep the temperature for 1 hour. After the hydrogen chloride is released, add 99.24g (0.3mol) tribromophenol, heat up to 110°C, keep warm for 7 hours, after the hydrogen chloride is released, cool down to below 40°C, install an extremely stretchable s...
Embodiment 2
[0033]Example 2 In a 500ml four-necked flask equipped with a stirrer, a thermometer, a dropping funnel and a high-efficiency reflux condenser and a hydrogen chloride absorbing device connected in series with a drying tube at the top of the condenser, replace the air in the bottle with nitrogen , add 180ml of ethylene glycol dimethyl ether and 16.99g (0.1mol) of silicon tetrachloride, under stirring, cool with an ice-water bath, reduce the temperature of the reaction system to 0°C, and add dropwise to the organic solution of silicon tetrachloride 12.90g (0.1mol) 2,3-dichloro-1-propanol, the dropwise addition process controls the temperature below 8°C, after the drop is completed, the temperature is raised to 35°C for 1h, and the temperature is kept for 1h. After the hydrogen chloride is released, add 99.24 g (0.3mol) of tribromophenol, heat up to 80°C, keep warm for 9 hours, after the hydrogen chloride is released, cool down to below 40°C, install an extremely stretchable soft s...
Embodiment 3
[0034] Example 3 In a 500ml four-neck flask equipped with a stirrer, a thermometer, a dropping funnel and a high-efficiency reflux condenser and a hydrogen chloride absorbing device connected in series with a drying tube at the top of the condenser, replace the air in the bottle with nitrogen , add 180ml of dioxane and 16.99g (0.1mol) of silicon tetrachloride, under stirring, cool with an ice-water bath, reduce the temperature of the reaction system to 0°C, and drop 12.90g of silicon tetrachloride into the organic solution (0.1mol) 2,3-dichloro-1-propanol, the temperature of the dropwise addition process is controlled below 8°C, after the drop is completed, the temperature is raised to 35°C in 1h, and the heat preservation reaction is carried out for 1h. After the hydrogen chloride is released, add 99.24g ( 0.3mol) tribromophenol, heat up to 90°C, keep warm for 8 hours, after the hydrogen chloride is released, cool down to below 40°C, install an extremely stretchable soft seali...
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