离子液体[Bmim]BF_4催化合成环状膦酸酯Antiblaze  

Synthesis of Cyclic Phosphonate Ester Flame Retardant Catalyzed by Ionic Liquid[Bmim]BF_4

作　　者：董春梅[1] 孙才英[1] 展召顺[1] 王红[1] 

机构地区：[1]东北林业大学理学院黑龙江省高校阻燃新材料重点实验室,黑龙江哈尔滨150040

出　　处：《精细化工》2011年第6期581-584,共4页Fine Chemicals

摘　　要：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进行了考察。正交实验确定了最佳合成路线。结果表明,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质量的0.4%,反应温度185℃,反应时间16 h,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。An ionic liquidBF4 was prepared and was subsequently used to catalyze the polymerization of ethyl bicyclic phosphite（1-ethyl-4-phospha-3,5,8-trioxabicyclo——octane） and dimethyl methylphosphonate under solvent-free conditions.The effect of process parameters,such as molar ratio,reaction temperature and catalyst on the yield was studied by method of the orthogonal experiment.The optimal synthesis conditions were as follows：the molar ratio of ethyl bicyclic phosphite to dimethyl methylphosphonate is 1∶ 1.6,the reaction temperature is 185 ℃,the reaction time is 16 h,the catalyst dosage is 0.4% of the whole reaction amount.The yield of cyclic phosphonate ester obtained under such conditions reached 98%.TG test in pure nitrogen environment shows that it had a high residual char rate of 7.37% at 500 ℃.

关 键 词：环状膦酸酯 阻燃剂 离子液体[Bmim]BF4 纺织染整助剂 

分 类 号：TQ314.2[化学工程—高聚物工业] O631[理学—高分子化学]