Method for preparing flame retardant bis[tri(chloroethoxy)silicon-acyloxy]ethane
A technology of chloroethoxy and silyloxy, which is applied in the direction of silicon organic compounds, can solve problems such as threats to people's life and property safety, fires, etc., and achieve the effects of overcoming volatile reactions, low production costs, and high flame retardant efficiency
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Embodiment 1
[0029] 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) silicon tetrachloride, under stirring, cool with a cold water bath to reduce the temperature of the reaction system to below 20°C, add 8.051g (6.71ml, 0.1mol) chloroethanol dropwise, and control the reaction during the dropwise addition The temperature is not higher than 30°C. After the drop, the temperature is raised to 35°C, and the temperature is kept for 1 hour; after the HCl gas is released, 3.1g (2.78ml, 0.05mol) of ethylene glycol is dropped into the four-necked flask, and the drop rate is Control the reaction temperature not to be higher than 45°C, raise the temperature to 50°C after dripping, and react for 8 hours; after the HCl gas is released, cool the system down to below 40°C, add 16.50g (13.74ml, 0.205mol) of ch...
Embodiment 2
[0030]Example 2 In a 250ml four-necked flask equipped with an agitator, 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) silicon tetrachloride, under stirring, cool with a cold water bath to reduce the temperature of the reaction system to below 20°C, add 8.051g (6.71ml, 0.1mol) chloroethanol dropwise, and control the reaction during the dropwise addition The temperature is not higher than 30°C. After dropping, raise the temperature to 35°C and keep it warm for 1 hour; after the HCl gas is released, drop 3.1g (2.78ml, 0.05mol) of ethylene glycol into the four-necked flask to Acceleration controls the reaction temperature not to be higher than 45°C. After the drop is completed, the temperature is raised to 65°C and reacted for 5 hours; after the HCl gas is released, the temperature of the system is lowered to below 40°C, and 16.90...
Embodiment 3
[0031] 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 acetonitrile and 17g (11.47ml , 0.1mol) silicon tetrachloride, under stirring, cool with a cold water bath to reduce the temperature of the reaction system to below 20°C, add 8.051g (6.71ml, 0.1mol) of chloroethanol dropwise, and control the reaction temperature during the dropwise addition process. At 30°C, after dropping, raise the temperature to 35°C, and keep it warm for 1 hour; after the HCl gas is released, drop 3.1g (2.78ml, 0.05mol) of ethylene glycol into the four-necked flask, and control the reaction with the dropping rate The temperature is not higher than 45°C. After the dripping, the temperature is raised to 60°C, and the reaction is 6h; after the HCl gas is released, the temperature of the system is lowered to below 40°C, and 17.71g...
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