环状磷酸酯阻燃剂Antiblaze的合成

Synthesis of Fire Retardant Cyclic Phosphonate Ester

用三羟甲基丙烷、亚磷酸三甲酯、磷酸三甲酯为原料合成了环状磷酸酯阻燃剂Antiblaze．用正交法讨论了物质的量之比、反应温度、反应时间、催化剂种类和用量对反应的影响，确定了反应的最佳条件：三乙胺为催化剂，用量为三羟甲基丙烷质量的2％，n（亚磷酸三甲酯）：n（三羟甲基丙烷）：n（磷酸三甲酯）=1．10：1：1．07；第一步反应温度为80～85℃，反应时间5h；第二步反应温度180～185℃，反应时间16h；产品收率90．6％．采用红外证实了产品的结构．热重分析表明其具有较高的残炭率．

Cyclic phosphonate ester Antiblaze was synthesized by trimethylolpropane, trimethyl phosphite and trimethyl phosphate. The effects of process parameters, such as molar ratio, reaction temperature, reaction time and catalyst on the yield were studied respectively from the orthogonal experiment. The suitable synthesis conditions were defined as follows ： triethylamine is the sutible catalyst, its dosage is 2.0% of the amount of all; the molar ratio of trimethylolpropane,trimethyl phosphite and trimethyl phosphate is 1.10： 1： 1.07; in the first step, the reaction temperature is 80 - 85℃, and the reaction time is 5 hours; in the second step, the reaction temperature is 180 - 185℃, and the reaction time is 16 hours. On the above conditions, the synthesis productivity is 90. 6%. The structure of the product was corfirmed by IR. TG test showed it had high residual char rate.