A novel macromolecular sulfur-containing organic phosphine flame retardant compound and preparation method thereof
A compound and organic phosphine technology, which is applied in the field of polyphenylthiophosphonic acid ethylene glycol ester and its preparation, can solve problems such as safety threats, and achieve the effects of good compatibility, large molecular weight, and difficult migration
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Embodiment 1
[0025] Example 1 In a 150ml three-neck flask equipped with a stirrer, a thermometer, and a reflux condenser, add 0.35mol (21.72g) of ethylene glycol, 0.2g of anhydrous zinc chloride, and raise the temperature to 45°C under nitrogen protection to start dripping Add 0.35mol (73.87g) of phenyl phosphonothioate dichloride, dropwise the addition in 2 hours, control the reaction temperature at 120°C, react at normal pressure for 3 hours, and then react for 7 hours under reduced pressure through the hydrogen chloride absorption device, and then transfer the reaction product to a 250ml three-port Add 100ml of N,N-dimethylformamide to the flask, heat to 100°C and keep stirring for 1 hour, cool to 25°C to completely precipitate the solid product, filter, wash with methanol, and dry to obtain white powdery solid polyphenylsulfide Ethylene glycol phosphonate. Its yield is 76%, its melting point is 175°C, and its decomposition temperature is 288°C.
Embodiment 2
[0026] Example 2 In a 150ml three-necked flask equipped with a stirrer, a thermometer, and a reflux condenser, add 0.35mol (21.72g) of ethylene glycol and 0.2g of anhydrous aluminum chloride, and raise the temperature to 45°C under nitrogen protection to start dripping Add 0.35mol (73.87g) of phenyl phosphonothioate dichloride, drop it in 2 hours, control the reaction temperature at 120°C, react at normal pressure for 4 hours, and then react for 6 hours under reduced pressure through the hydrogen chloride absorption device, and then transfer the reaction product to a 250ml three-port Add 100ml of N,N-dimethylformamide to the flask, heat to 100°C and keep stirring for 1 hour, cool to 25°C to completely precipitate the solid product, filter, wash with methanol, and dry to obtain white powdery solid polyphenylsulfide Ethylene glycol phosphonate. Its yield is 71%, its melting point is 175°C, and its decomposition temperature is 288°C.
Embodiment 3
[0027] Example 3 In a 150ml three-necked flask equipped with a stirrer, a thermometer, and a reflux condenser, add 0.35mol (21.72g) of ethylene glycol, 0.2g of anhydrous calcium chloride, and raise the temperature to 45°C under nitrogen protection to start dripping Add 0.35mol (73.87g) of phenylphosphonothioate dichloride, dropwise the addition in 2 hours, control the reaction temperature at 120°C, react at normal pressure for 5 hours, then pass the hydrogen chloride absorbing device to react under reduced pressure for 5 hours, and then transfer the reaction product to a 250ml three-port Add 100ml of N,N-dimethylformamide to the flask, heat to 100°C and keep stirring for 1 hour, cool to 25°C to completely precipitate the solid product, filter, wash with methanol, and dry to obtain white powdery solid polyphenylsulfide Ethylene glycol phosphonate. Its yield is 70%, its melting point is 175°C, and its decomposition temperature is 288°C.
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