Application and preparation method of hexa(4-methoxyphenylethylamino) cyclotriphosphazene flame retardant
A technology of methoxyphenethylamine and methoxyphenethylamine, which is applied in the field of novel nitrogen and phosphorus-based additive flame retardants, and can solve problems such as being difficult to decompose.
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Embodiment 1
[0027] Take a dry 500ml three-necked bottle, replace it with nitrogen three times, add 12.3g of potassium carbonate to it, stir and add 100ml of THF, slowly add 50ml of THF solution containing 27g of p-methoxyphenylethylamine dropwise, and heat up after the dropwise addition To 45°C, add dropwise 10g of hexachlorocyclotriphosphazene in 50ml THF solution at 40-50°C, heat up to 68°C after the dropwise addition, and monitor the end point of the reaction by thin-layer chromatography. Concentrate under low pressure to obtain a viscous yellow solid, which is washed with water, ethanol, and n-hexane in turn, and finally crystallized in n-hexane to obtain 3.04 g of a yellow solid, with a yield of 61.29%.
Embodiment 2
[0029] Take a dry 500ml three-necked bottle, replace it with nitrogen three times, add 12.3g of potassium carbonate to it, stir and add 100ml of THF, slowly add 50ml of THF solution containing 27g of p-methoxyphenylethylamine dropwise, and heat up after the dropwise addition To 45°C, add dropwise 10g of hexachlorocyclotriphosphazene in 50ml THF solution at 40-50°C, heat up to 68°C after the dropwise addition, and monitor the end point of the reaction by thin-layer chromatography. Concentrate under low pressure to obtain a viscous yellow solid, which is washed with water, ethanol, and n-hexane in turn, and finally column chromatography gives 2.31 g of a yellow solid with a yield of 46.57%.
Embodiment 3
[0031] Take a dry 500ml three-necked bottle, replace it with nitrogen three times, add 7.14g of sodium hydroxide to it, stir and add 50ml of MCB, after stirring evenly, slowly add 100ml of 30.45g of p-methoxyphenethylamine MCB solution, warm up to 45°C after the dropwise addition, add dropwise 50ml MCB solution of 10g hexachlorocyclotriphosphazene at 40-50°C, raise the temperature to 100°C after the dropwise addition, monitor the end point of the reaction by thin-layer chromatography, after the end of the reaction , filtered with suction, and the filtrate was concentrated under vacuum to obtain a viscous yellow solid, which was washed with water, ethanol, and n-hexane in turn, and finally crystallized in n-hexane to obtain 1.97 g of a yellow solid, with a yield of 39.72%.
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