N,N′-4,4′-二苯甲烷双马来酰亚胺的催化合成  

Catalytic synthesis of N, N′-(4, 4′-diphenylmethane) bismaleimide

作　　者：曹娜[1] 袁海涛[1] 符玉华[1] 贺军辉[1] 

机构地区：[1]中国科学院理化技术研究所

出　　处：《北京化工大学学报（自然科学版）》2007年第6期594-598,603,共6页Journal of Beijing University of Chemical Technology(Natural Science Edition)

摘　　要：由顺丁烯二酸酐和4,4′-二氨基二苯基甲烷两步法合成N,N′-4,4′-二苯甲烷双马来酰亚胺,以甲苯和N,N′-二甲基甲酰胺(DMF)为溶剂,用水沉析、旋转蒸发两种方式处理产品,并且对比了催化剂对甲苯磺酸和干氢催化树脂的催化效果。还讨论了反应温度、DMF等因素的影响。结果表明:树脂的催化效果优于对甲苯磺酸的催化效果,并且树脂可以反复使用。第一步酰胺化在室温下反应,第二步在树脂催化作用下,溶剂和水共沸不断蒸出生成的水,而且加入DMF可使环化反应在均相状态下进行。由核磁共振谱图分析合成的产品,其纯度高。产品熔点在155～159℃之间,最高收率达92.18%。The synthesis of N, N′-（4, 4′-diphenylmethane） bismaleimide has been carried out by a two-step reaction of maleic anhydride and 4, 4′-diaminodiphenylmethane. Toluene and dimethylforrnamide （DMF） were used as solvent, and the product was isolated by precipitation with water or by rotary evaporation. A dry acid resin was found to be superior to p-toluenesulfonate as a catalyst for the second step and furthermore the resin could be used repeatedly. The effects of varying reaction temperature and amount of added DMF were also investigated. The optimum conditions were found to involve carrying out the initial acyl-amination reaction at room temperature, with the second step being catalyzed by the resin with water being removed by co-evaporation with the solvent and sufficient DMF being added to produce a single homogeneous phase. The high purity of the product was confirmed by XH-NMR spectroscopy and its melting point （ 155 - 159℃ ）. The maximum observed yield was 92.18 %.

关 键 词：顺丁烯二酸酐 4 4′-二氨基二苯基甲烷 N N′-4 4′-二苯甲烷双马来酰亚胺 干氢催化树脂 

分 类 号：TQ323.7[化学工程—合成树脂塑料工业]