A kind of reactive phosphorus-containing flame retardant and its preparation method and application
A flame retardant and reactive technology, applied in the field of flame retardants, can solve the problems of complex synthesis methods and cumbersome process flow of flame retardants, and achieve excellent durability, wide application range, and good fire prevention effect
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Embodiment 1
[0040] First, under the protection of nitrogen, add 0.2mol phosphorus oxychloride to 150mL tetrahydrofuran at 0~-5°C and mix well, then add 0.6mol triethylamine at this temperature, and then slowly add 50mL tetrahydrofuran dropwise within 2h After the dissolved 0.2mol hydroxyethyl acrylate is added dropwise, the reaction is continued at this temperature for 6 hours to obtain a solution of a monosubstituted phosphorus-containing intermediate (III) containing a double bond structure. Add 0.2 mol of triethylamine to the intermediate (Ⅲ) solution obtained in the above step at room temperature, then slowly add 0.2 mol of 4,4-diaminodiphenyl ether dissolved in 60 mL of tetrahydrofuran dropwise within 2 hours, after the dropwise addition is completed Raise the temperature of the solution to 100°C and react for 8 hours. After the reaction, the liquid is removed by suction filtration, and the obtained yellow solid is washed with deionized water for 3 to 4 times. After drying, the reacti...
Embodiment 2
[0042] First, under the protection of nitrogen, add 0.22mol phosphorus oxychloride to 150mL acetonitrile at 0~-10℃ and mix well, then add 0.66mol pyridine at this temperature, then slowly add 50mL acetonitrile dropwise within 1.5h to dissolve 0.2mol of hydroxyethyl acrylate, after the dropwise addition, the reaction was continued at this temperature for 7 hours to obtain a solution of a single-substituted phosphorus-containing intermediate (Ⅲ) containing a double bond structure. Add 0.2 mol of pyridine to the intermediate (Ⅲ) solution obtained in the above step at room temperature, then slowly add 0.2 mol of 4,4-diaminodiphenylmethane dissolved in 60 mL of acetonitrile dropwise within 2 hours, and dissolve the solution after the dropwise addition The temperature is raised to 90°C for 7 hours. After the reaction, the liquid is removed by suction filtration, and the obtained yellow solid is washed with deionized water for 3 to 4 times. After drying, the reactive phosphorus-contai...
Embodiment 3
[0044] First, under the protection of nitrogen, add 0.2mol phosphorus oxychloride to 150mL tetrahydrofuran at 0~-5°C and mix well, then add 0.7mol triethylamine at this temperature, and then slowly add 50mL tetrahydrofuran dropwise within 2h After the dissolved 0.2mol hydroxyethyl acrylate is added dropwise, the reaction is continued at this temperature for 6 hours to obtain a solution of a monosubstituted phosphorus-containing intermediate (III) containing a double bond structure. Add 0.2 mol of triethylamine to the intermediate (Ⅲ) solution obtained in the above steps at room temperature, then slowly add 0.2 mol of 4,4-diaminodiphenyl ether dissolved in 60 mL of tetrahydrofuran dropwise within 2 hours, The temperature of the solution is raised to 85°C and reacted for 8 hours. After the reaction, the liquid is removed by suction filtration, and the obtained yellow solid is washed with deionized water for 3 to 4 times. After drying, the reactive phosphorus-containing flame reta...
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