缚酸法丙二烯膦酰氯合成及工艺过程研究  

Synthesis and process research of allene phosphoryl chloride by acid binding method

作　　者：桑国龙 郭瓦力[1] 符丽[1] 韩俊涛[1] 

机构地区：[1]沈阳化工大学化学工程学院,辽宁沈阳110142

出　　处：《化学工程师》2015年第1期5-9,13,共6页Chemical Engineer

基　　金：沈阳市科技计划项目(1091036-4-00);沈阳市科技计划项目(F12-188-9-00)

摘　　要：为解决丙二烯膦酰氯生产中环境污染严重,产品收率低等问题,在以三氯化磷、丙炔醇为原料,甲苯为溶剂的条件下,引入缚酸剂三乙胺吸收反应过程中产生的HCl气体,实现了丙二烯膦酰氯的低耗高效绿色制备。通过单因素实验考察了缚酸剂用量、溶媒比、原料比、反应温度、滴料时间对产率的影响,通过响应面法进行实验设计及实验,利用Design-Expert7.0.0软件优化工艺条件,并经验证性实验获得了适宜的工艺条件:原料比3.7,缚酸投料比1.2,溶媒比0.2,反应温度50℃,滴料时间1h,保温温度70℃,保温时间2h,在该工艺条件下丙二烯二氯化磷收率可达61.51%。A cost effective preparation method for allene phosphoryl chloride was studied with phosphorus trichloride and propiolic alcohol as material, methylbenzene as solvent, and triethylamine as acid binding agent to absorb HC1 for solving the environmental pollution and low yield problems. The effect of amount of allene phos- phoryl chloride, solvent ratio, feed composition, reaction temperature and adding time on yield were investigated. The experiment was designed by RSM; the conditions were optimized by Design-Expert 7.0.0. The best conditions were feed composition 3.7, allene phosphoryl chloride ratio 1.2, solvent ratio 0.2, reaction temperature 50℃, adding time lh, holding temperature 70℃, holding time 2h. The yield of allene phosphoryl chloride was 61.51%.

关 键 词：三氯化磷 三乙胺 丙二烯膦酰氯、丙二烯二氯化磷 缚酸剂 

分 类 号：O621.3[理学—有机化学]