N-PMI的合成新方法及中试放大研究  

Novel Synthetic Method of N-PMI

作　　者：李进京[1] 吴义班 张召来 李林博 刘玉肖 姬金岭 魏洪福 张杰[1] Li Jinjing;Wu Yiban;Zhang Zhaolai;Li Linbo;Liu Yuxiao;Ji Jinling;Wei Hongfu;Zhang Jie(School of Pharmacy,Jiamusi University,Jiamusi 154007,China;Jiaxing Shicheng Technology Co.,Ltd.,Jiaxing 314001,China)

机构地区：[1]佳木斯大学药学院,黑龙江佳木斯154007 [2]嘉兴市世诚科技有限公司,浙江嘉兴314001

出　　处：《山东化工》2020年第15期27-28,共2页Shandong Chemical Industry

基　　金：黑龙江省省属本科高校基本科研业务费优秀创新团队建设项目(2018-KYYWF-0914);黑龙江省属高校基本科研业务费项目(2018-KYYWF-0946);大学生创新创业项目(202010222024,202010222027)。

摘　　要：以马来酸酐为原料、苯胺磺酸盐为催化剂、苯和DMF为混合溶剂,应用“一锅法”合成N-苯基马来酰亚胺。研究了原料配料比、溶剂用量、回流脱水时间、对甲苯磺酸成盐次数等因素对产品收率的影响。本文首次采用对甲苯磺酸与苯胺成盐的分离方法,极大了降低了酸性废水的排放。单因素实验得到N-苯基马来酰亚胺最佳合成工艺:1 g苯胺磺酸盐,8.8 mL苯,0.5 mL DMF,n苯胺磺酸盐∶n马来酸酐=1.00∶1.10,回流脱水时间为4 h,N-苯基马来酰亚胺平均产率为88%,纯度为93%。其中苯胺磺酸盐循环使用次数至少达3次。Using maleic anhydride as raw material,aniline sulfonate as catalyst,benzene and DMF as mixed solvent,N-phenylmaleimide was synthesized by"one-pot method".The effects of raw material ratio,solvent dosage,reflux dehydration time,and number of p-toluenesulfonic acid formation on product yield were studied.Innovatively,the separation method of p-toluenesulfonic acid and aniline is used to greatly reduce the discharge of acidic wastewater.Single factor experiment to obtain the best process of N-phenylmaleimide synthesis:1g aniline sulfonate,8.8mL benzene,0.5mL DMF,naniline sulfonate∶nmaleic anhydride=1.00∶1.10,reflux dehydration time is 4h.The average yield of the N-phenylmaleimide is 88% and the purity is 93%.Among them,the aniline sulfonate is recycled at least 3 times.

关 键 词：N-苯基马来酰亚胺 苯胺磺酸盐 一锅法 

分 类 号：TQ320.4[化学工程—合成树脂塑料工业]