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作 者:魏义兰 张旭 王宇 李华轩 WEI Yilan;ZHANG Xu;WANG Yu;LI Huaxuan(College of Chemical Engineering,Hunan Chemical Vocational Technology College,Zhuzhou 412000 China;Xiangtan Sewage Treatment Co.,Ltd.,Xiangtan 411100,China;Hunan Bide Biochemical Technology Co.,Ltd.,Yueyang 414306,China)
机构地区:[1]湖南化工职业技术学院化学工程学院,湖南株洲412000 [2]湘潭市污水处理有限责任公司,湖南湘潭411100 [3]湖南比德生化科技股份有限公司,湖南岳阳414306
出 处:《河南化工》2023年第9期24-26,32,共4页Henan Chemical Industry
基 金:湖南省教育厅科学研究项目(19C0643)。
摘 要:以2-氯-5-氯甲基噻唑与3-甲基-4-硝基亚胺基四氢-1,3,5-噁二嗪为原料,通过双分子亲核取代反应得到噻虫嗪,产品采用HPLC、IR、^(1)H-NMR等手段进行了分析与表征。通过改进生产工艺,优选工艺条件为:DMF作溶剂,K_(2)CO_(3)作缚酸剂,n(3-甲基-4-硝基亚胺四氢-1,3,5-噁二嗪)∶n(2-氯-5氯甲基噻唑)∶n(K_(2)CO_(3))为1.1∶1.0∶1.2,反应温度35℃,甲醇作重结晶溶剂,噻虫嗪产品的外标含量高于98%,收率达80%。该工艺路线有效地降低了废水排放量,产品收率高,适用于工业化生产。Using 2-chloro-5-chloromethylthiazole and 3-methyl-4-nitroimino-dihydro-1,3,5-oxadiazine as materials,thiamethoxam is synthesized by bimolecular nucleophilic substitution reaction.The product is analyzed and characterized by HPLC,IR and^(1)H-NMR.By improving the production process,the optimized process conditions are as follows,DMF as solvent,K_(2)CO_(3)as acid binding agent,the molar ratio of raw materials 3-methyl-4-nitroimine tetrahydro-1,3,5-oxadiazine,2-chloro-5-chloromethylthiazole and K_(2)CO_(3)is 1.1∶1.0∶1.2,the reaction temperature is 35℃,methanol as recrystallization solvent.The external standard content of thiamethoxam product is more than 98%and the yield is 80%.The process route can effectively reduce the discharge of wastewater,and the product yield is high,which is suitable for industrial production.
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