氧气氧化法合成草甘膦的工艺研究  

Process research in glyphosate synthesis by oxidizing of oxygen

作　　者：来虎钦[1] 刘风强[1] 蔡鹏[1] 丁成荣[1] 周瑛[1] 

机构地区：[1]浙江工业大学化学工程与材料学院,浙江杭州310032

出　　处：《浙江工业大学学报》2011年第2期151-153,共3页Journal of Zhejiang University of Technology

摘　　要：以双甘膦为原料,氧气为氧化剂,高活性钯炭为催化剂氧化合成草甘膦,并对反应工艺参数进行了优化:在双甘膦与催化剂的质量比为1∶0.01,反应温度为95℃,反应压力为0.25 MPa条件下,保温3 h后停止通氧;然后通入保护气,加热、加压反应一段时间后得到草甘膦,且损耗在溶液中的大部分钯离子得到还原,反应收率为94.6%,纯度为95.6%,产品用IR1,HNMR进行表征,母液回收循环利用,催化剂连续使用次数达到30次.Glyphosate was synthesized by oxidation of PMIDA（N-phosphonomethyliminodiacet-ic acid） using oxygen in the presence of Pd catalyst on activated carbon.The conditions of the reactions were optimized and selected as following： the weight ratio of PMIDA and catalyst was 1∶0.01,the reaction temperature was 95 ℃,the reaction pressure was 0.25 MPa and the reaction time was 3 hours;Then,the supply of oxygen was cut off and protective gas was pressurized in to the reactor.Aimed compound was obtained and most of the palladium lost in solution was reduced.Finally,the yield of glyphosate was 94.6%,as well as its purity was 95.6%,The structure of aimed compound was confirmed by IR and HNMR.The mother liquid was recycled for re-used.The catalyst was reused for more than 30 consecutive times.

关 键 词：双甘膦 草甘膦 贵金属 氧化 

分 类 号：TQ457.29[化学工程—农药化工]