离子液体[Bmim]BF4催化合成环状膦酸酯Antiblaze

TTHE SYNTHESIS OF CYCLIC PHOSPHONATE ESTER FLAME RETARDANT Antiblaze CATALYZED BY IONIC LIQUID [Bmim]BF4

摘要:

该文制备了离子液体[Bmim]BF4，对其催化乙基双环亚磷酸酯与甲基膦酸二甲酯进行聚合反应合成环状膦酸酯做了考察。配合正交实验确定了最佳合成路线。结果显示，乙基双环亚磷酸酯与甲基膦酸二甲酯的摩尔比为 1：1.6，催化剂用量为反应物总量的0.4%，反应温度为185℃，反应时间为16h，产率达98%。热重分析显示500℃时残炭率为 7.37% ,具有良好的成炭作用。

Abstract:

The condensation of ethyl bicyclic phosphite (1-ethyl-4-phospha-3,5,8-trioxabicyclo-[2,2,2]-octane) and dimethyl methylphosphonate has been investigated using self-made ionic liquid [Bmim]BF4 as catalyst under solvent-free conditions. The effects of process parameters, such as molar ratio, reaction temperature and catalyst on the yield were studied respectively from the orthogonal experiment.The suitable synthesis conditions as follows: the molar ratio of ethyl bicyclic phosphite and dimethyl methylphosphonate is 1:1.6,reaction temperature is 185℃,reaction time is 16h,catalyst dosage is 0.4% of the amount of all. The cyclic phosphonate ester was obtained in this condition with the yield 98%. TG test under pure nitrogen showed it had high residual char rate at 500℃.