O,O-二甲基-S-(N-甲基氨基甲酰甲基)硫代磷酸酯清洁合成新工艺研究  

Study on the new clean synthesis process of O,O-dimethyl S-methylcarbamoylmethyl phosphorothioate

作　　者：霍二福 程伟琴[1] 冯明 王延花 师传兴 王柏楠 王宏力 HUO Er-fu;CHENG Wei-qin;FENG Ming;WANG Yan-hua;SHI Chuan-xing;WANG Bo-nan;WANG Hong-li(Henan Chemical Iudustry Research Institute Limited Company,Zhengzhou 450052,China;Quality Inspection and Analytical Test Research Center,Henan Academy of Sciences,Zhengzhou 450008,China)

机构地区：[1]河南省化工研究所有限责任公司,河南郑州450052 [2]河南省科学院质量检验与分析测试研究中心,河南郑州450008

出　　处：《化学研究与应用》2021年第12期2449-2456,共8页Chemical Research and Application

基　　金：河南省科学院重大科研项目聚焦项目(210108004)资助;河南省科学院基本科研费项目(210608028)资助。

摘　　要：针对氧乐果[O,O-二甲基-S-(N-甲基氨基甲酰甲基)硫代磷酸酯]传统工艺存在的污染严重、能耗高,收率低、纯度低,含水量高等问题,以氯乙酰氯、亚磷酸二甲酯为起始原料,首次采用无水、均相反应体系-结晶分离清洁生产工艺制备氧乐果,提高了产品收率和纯度,实现了副产氯化钠全部回收;采用低温反应、低温萃取、低温干燥的方法合成2-氯-N-甲基乙酰胺;制备2-氯-N-甲基乙酰胺和氧乐果的反应母液可以循环使用7次以上,反应废液减少85%;通过新合成工艺得到的氧乐果的产品纯度高,比传统工艺(三氯化磷后胺解法)制备的产品纯度(86%)提高近10个百分点,产品含水量小于0.05%,解决了产品因含水量高而分解等问题。新合成工艺具有工艺简单、绿色环保、反应条件温和等优点。In order to solve the problems of omethoate[O,O-dimethyl S-(N-methylcarbamoylmethyl)phosphorothioate]in traditional process, such as serious pollution, high energy consumption, low yield, low purity and high water content, omethoate was prepared from chloroacetyl chloride and dimethyl phosphite by anhydrous homogeneous reaction system and crystallization separation clean production process for the first time, which improved the yield and purity of the product.All by-product sodium chloride was recycled.2-Chlorine-N-methyl acetamide was synthesized by low-temperature reaction, low-temperature extraction and low-temperature drying.The mother fluid of 2-chloro-N-methylacetamide and omethoate could be recycled for more than 7 times, and the reactive waste liquid could be reduced by 85%.The purity of omethoate obtained by the new synthesis process was high, which was nearly 10%higher than that of omethoate(86%)prepared by the traditional process.The water content of omethoate was less than 0.05%,which solved the problem of decomposition of omethoate due to its high water content.The new synthesis process had the advantages of simple process, environmental protection and mild reaction conditions.

关 键 词：O O-二甲基-S-(N-甲基氨基甲酰甲基)硫代磷酸酯 新工艺 结晶 分离 优化 

分 类 号：O623.7[理学—有机化学]