甲基亚磷酸二乙酯和丙烯酸甲酯在微反应器中加成反应研究

Addition Reaction of Methyl Diethoxyphosphine and Methyl Acrylate in a Microreactor

考查了反应温度、反应压力、物料摩尔比、溶剂用量、停留时间对反应的影响并优化。结果表明:在优化工艺条件(温度120℃、压力1 MPa、n(丙烯酸甲酯)∶n(甲基亚磷酸二乙酯)=1.05∶1,n(甲醇)∶n(甲基亚磷酸二乙酯)=6∶1,反应物料停留时间为110 s时,原料甲基亚磷酸二乙酯转化率达99.5%以上,产物3-(甲基甲氧基膦酰基)丙酸甲酯的选择性达96%以上。相比于间歇反应釜,微反应器大大缩短了反应时间,提高了生产效率。

Reaction temperature, reaction pressure, molar ratio of materials, amount of solvent and residence time on the reaction were investigated and optimized. Under optimized process conditions (temperature 120℃, pressure 1 MPa, molar ratio of methyl acrylate and methyl diethoxyphosphine 1.05∶1, molar ratio of methanol and methyl diethoxyphosphine 6∶1, material stay time 110 s), the conversion rate of methyl diethoxyphosphine is more than 99.5% and the selectivity of 3 -(methyl methoxyphosphono)methyl propionate is up to 96%. The microreactor can greatly shorten the reaction time and improve the production efficiency compared with the batch reactor.