N-甲基-1-(甲硫基)-2-硝基乙烯胺的环保合成工艺  

Environmental Synthesis Process of N-Methyl-1-(methylthio)-2-nitroethenamine

作　　者：薛子桥 田克情[2] 王娇[1] 杨田[1] 张萍[1] XUE Zi-qiao;TIAN Ke-qing;WANG Jiao;YANG Tian;ZHANG Ping(National Demonstration Center for Experimental Chemistry Education, College of Chemistry and Material Science, Hebei Normal University, Shijiazhuang 050024, China;School of Environment and Chemical Engineering, Hebei Chemical and Pharmaceutical College, Shijiazhuang 050026, China)

机构地区：[1]河北师范大学化学与材料科学学院化学国家级实验教学示范中心,河北石家庄050024 [2]河北化工医药职业技术学院化学与环境工程系,河北石家庄050026

出　　处：《化学试剂》2018年第4期400-402,共3页Chemical Reagents

基　　金：河北省自然科学基金资助项目(B2017205100);河北师范大学应用基金资助项目(130388)

摘　　要：硝基甲烷和二硫化碳作用生成硫醇钾盐,再经胺化和甲基化反应是工业生产标题化合物主要采用的方法。该工艺产生的废气、废液无法处理,使整个生产受限。对该工艺进行了优化和改进,确定了甲基化反应的另一产物为硫酸单甲酯钾盐,研究了溶剂的回收使用、废气废液的处理等工艺条件,优化后的工艺成本降低、环保,适合工业化生产。3步反应的总收率为42%,外标含量为98.8%。The main method of industrial production of N-methyl-1-（ methylthio）-2-nitroethenamine is the formation of potassium thiolate through nitromethane and carbon disulfide followed the amination and methylation reactions.The waste gas and liquid produced by the process cannot be processed,so the whole production is limited.In this work,the process is optimized and improved,another product of the methylation reaction is determined to be potassium monomethyl sulfate,the recovery of solvent and the treatment of waste gas and liquid are also investigated. The optimized process is lower cost,environmental and suitable for industrial production.The total yield is 42% by 3 steps reaction,and the external standard content is 98. 8%.

关 键 词：N-甲基-1-(甲硫基)-2-硝基乙烯胺 硫酸单甲酯钾盐 废气废液处理 

分 类 号：O622.3[理学—有机化学]