N-苯基马来酰亚胺的合成与表征

摘要

以顺丁烯二酸酐和苯胺为原料,研究在催化剂作用下合成N-苯基马采酰亚胺(N-PMI)的新工艺,在N-苯基马来酰胺酸合成时采用乙酸已酯作溶剂,在N-PMI合成时采用乙二胺四乙酸(ED-TA)钠盐作为催化剂、醋酐作为脱水剂、丙酮作为溶剂,考察了原料配比、催化剂的选择及用量、反应温度与反应时间等因素对反应结果的影响,合成N-PMI的最佳工艺条件为:顺酐与苯胺质量比为1.06:1.00,催化剂用量为0.35 g/g中间体,反应温度为55℃,反应时间为4h.在最佳工艺下产品收率可达92％以上,产品纯度可达99％(质量分数)以上,并通过气相色谱检测了产品纯度,通过红外光谱对产品结构进行了表征.%The novel technology of the synthesis of N-phenylmaleimide under catalyst was studied by using maleic anhydride and aniline as starting materials. In the investigation,ethyl acetate was selected as solvent when the N-phenylmaleamic acid was synthesized. In addition,during the process of the synthesis of N-phenylmaleimide,edetate disodium,acetic anhydride and acetone were used as catalyst , dehydration reagent and solvent, respectively. The ratio of starting materials, the selection and dosage of catalysts,reaction temperature as well as the rection time were investigated in order to understand their influences on the results. The optimized technological condition was that the mass ratio of maleic anhydride and aniline was 1. 06 : 1, catalyst dosage was 0. 35 (g/g intermediates) ,the reaction temperature was 55 ℃ and the reaction time was 4 hours. Under such conditions, the yield and the purity were 92% and 99%, respectively. Besides, the purity was detected by GCand the structure of product was identified by IR.