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.
作者
李进京
吴义班
张召来
李林博
刘玉肖
姬金岭
魏洪福
张杰
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)
出处
《山东化工》
CAS
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)。
