Fire retardant 2[3(3-bromine propoxy) silicon acyloxy] ethane compound and preparation method thereof
A technology of bromopropoxy and silyloxy, which is applied in the field of flame retardant bis[trisilyloxy]ethane compound and its preparation, can solve the problem that the material has little influence on mechanical processing properties, high flame retardant efficiency, and is difficult to Find alternatives and other issues to achieve the effect of high synergistic flame retardant efficiency, good plasticity and large molecular weight
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Embodiment 1
[0025] Example 1 In a 250ml four-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, and a drying tube on the condenser, replace the air in the bottle with nitrogen, add 60ml of dichloroethane and 17g (11.47ml, 0.1mol) of silicon tetrachloride, under stirring, cooled with a cold water bath, so that the temperature of the reaction system was lowered below 25°C, 13.9g (8.88ml, 0.1mol) of 3-bromopropanol was added dropwise, and The process controls the reaction temperature not to be higher than 30°C. After dripping, raise the temperature to 45°C and keep it warm for 2 hours; after the HCl gas is released, drop 3.1g (2.78ml, 0.05mol) of ethylene glycol into the four-necked flask , control the reaction temperature not higher than 50°C with the dropping speed, raise the temperature to 55°C after dropping, and react for 10h; ) 3-bromopropanol, the reaction temperature is controlled by the dropping rate not higher than 55°C, after the drop, the te...
Embodiment 2
[0026] Example 2 In a 250ml four-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, and a drying tube on the condenser, replace the air in the bottle with nitrogen, add 60ml carbon tetrachloride and 17g (11.47ml, 0.1mol) of silicon tetrachloride, under stirring, cooled with a cold water bath to lower the temperature of the reaction system below 25 ° C, dropwise added 13.9g (8.88ml, 0.1mol) 3-bromopropanol, dropwise added The process controls the reaction temperature not to be higher than 30°C. After dripping, raise the temperature to 45°C and keep it warm for 2 hours; after the HCl gas is released, drop 3.1g (2.78ml, 0.05mol) of ethylene glycol into the four-necked flask , control the reaction temperature not higher than 50°C with the dropping speed, raise the temperature to 65°C after dropping, and react for 8h; ) 3-bromopropanol, the reaction temperature is controlled by the dropping rate not higher than 55°C, after the drop, the temper...
Embodiment 3
[0027]Example 3 In a 250ml four-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, and a drying tube on the upper mouth of the condenser, replace the air in the bottle with nitrogen, add 60ml of dioxane and 17g (11.47ml, 0.1mol) of silicon tetrachloride, under stirring, cooled with a cold water bath, so that the temperature of the reaction system was lowered below 25°C, 13.9g (8.88ml, 0.1mol) of 3-bromopropanol was added dropwise, and The process controls the reaction temperature not to be higher than 30°C. After dripping, raise the temperature to 45°C and keep it warm for 2 hours; after the HCl gas is released, drop 3.1g (2.78ml, 0.05mol) of ethylene glycol into the four-necked flask , control the reaction temperature not higher than 50°C with the dropping speed, raise the temperature to 70°C after dropping, and react for 7h; ) 3-bromopropanol, the reaction temperature is controlled by the rate of addition not to be higher than 55°C, aft...
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