摘要
目的研究新型杀虫剂杀线威的合成方法.方法制取杀线威有两种不同方法,即非溶剂法和溶剂法,前者采用水为反应介质,后者采用丙酮为反应介质,从产品制造成本,产品纯度,操作环境的安全性以及生产设备投资等方面进行比较,确定可行的合成方法.结果通过比较和讨论,确定非溶剂水相合成法是较好的工艺方法.按料比n（杀线威肟）∶n（异氰酸甲酯）=1∶1.2,控制温度30 ℃左右滴加异氰酸甲酯,反应液经结晶、过滤、干燥得杀线威原药,w（杀线威）≥99%（HPLC）,以杀线威肟计收率≥95%,m.p.98～101 ℃.结论水相法合成杀线威不需催化剂和溶剂,产品制造成本低,纯度高,反应结束异氰酸甲酯无残留,出料环境好,操作方便,设备投资少。
Objective： To study synthesis of the new type pesticide Oxamyl. Methods： The two methods of non-solvent process and solvent process were adopted to prepare oxamyl. Oxamyl was prepared in water in the first one and in acetone in the second. By the comparisons of productive cost, production purity, operation safety and equipment cost, a proper proceeds for preparation oxamyl was adopted. Results： The non-solvent process was better. The materials ratio was n（oxamyl oxime） ： n（methyl isocyanate） = 1 ： 1.2. Methyl isoeyanate was slowly added dropwise to oxamyl oxime in water at about 30 ℃ . After being crystallized, filtered and dried, oxamyl could be obtained with purity≥99% （HPLC）, m. p. 98--101℃ , yield≥95 % （base on oxamyl oxime）. Conclusion： The non-solvent process of the preparation for oxamyl is suitable for mass production due to its low production cost, high purity, no methyl isocyante remains, easy operation and lower equipment cost.
出处
《泰山医学院学报》
CAS
2006年第1期31-32,共2页
Journal of Taishan Medical College
