ZSM-5分子筛催化苯基羟胺制对氨基苯酚性能考察

Preparation of p-Aminophenol from Phenyl-Hydroxylamine Catalyzed by ZSM-5 Zeolites

李文强 陈子璇 丁晓光 安会勇 于芳

Li Wenqiang Chen Zixuan Ding Xiaoguang An Huiyong Yu Fang

(1.辽宁石油化工大学 化学化工与环境学部，辽宁 抚顺 113001；2.辽宁石油化工大学 计算机与通信工程学院，辽宁 抚顺 113001)

(1. College of Chemistry, Chemical Engineering and Environmental Engineering, Liaoning Shihua University， Fushun Liaoning 113001, China;  2. School of Computer and Engineering, Liaoning Shihua University， Fushun Liaoning 113001, China)

关键词: ZSM-5分子筛, 固体酸催化剂, 苯基羟胺, Bambenger重排, 对氨基苯酚

Na-ZSM-5 was prepared by in-situ hydrothermal process. H-ZSM-5 (n(Si)/n(Al)=40) molecular sieves were prepared by ion exchange. p-Aminophenol was prepared by Bamberger rearrangement catalyzed by the molecular sieves using phenyl-hydroxylamine as raw material. XRD, FT-IR, N2 adsorption-desorption, SEM and Py-FTIR techniques were used to study the topological structure, micropore pore size and acidity of Na-ZSM-5 and H-ZSM-5 molecular sieves. The results showed that the prepared molecular sieves had MFI microporous structures with well crystallinity. Py-FTIR technique showed that Na-ZSM-5 had almost no B acid. H-ZSM-5(40) molecular sieve had weaker B acid and L acid. Catalysis performance showed that phenyl-hydroxylamine conversion was low in the presence of ZSM-5 with weaker acidity as catalyst. However, because of its moderate pore size, p-aminophenol selectivity and yield reached as high as 72.48% and 58.75%, respectively. The optimal conditions of p-aminophenol preparation from phenyl-hydroxylamine Bamberger rearrangement were as follows: mass ratio 1∶3 of phenyl-hydroxylamine to H-ZSM-5(40) molecular sieve, optimal reaction temperature of 353 K, optimal reaction time of 2 h, and water as solvent. Phenyl-hydroxylamine conversion and p-aminophenol selectivity were as high as 86.35% and 78.33%, respectively.

国家自然科学基金项目(No.21402078)

10.3969/j.issn.1006-396X.2018.02.004