二氧化硅负载磷钼钒酸铯选择性催化硝化苯酚为邻硝基苯酚

doi:10.3724/SP.J.1095.2014.30463

摘要/Abstract

摘要： 采用溶胶-凝胶法制备了二氧化硅负载磷钼钒酸铯催化剂，利用XRD、红外、SEM以及物理吸附等技术手段对催化剂进行了表征分析，并以稀硝酸（30%）为硝化剂，考察了该催化剂对苯酚硝化反应的催化性能，系统研究了反应时间、催化剂用量、硝酸与苯酚用量以及催化剂重复利用等对催化反应的影响。结果表明，制备的负载磷钼钒酸铯催化剂具有典型的Keggin结构，在温和的苯酚硝化反应条件下，表现出优良的催化活性和高的邻硝基苯酚选择性，在实验优化条件下，邻硝基苯酚收率达到88%，催化剂回收方便可多次重复使用。负载磷钼钒酸铯催化苯酚硝化反应结合水蒸汽蒸馏提供了一种简单可行的制备邻硝基苯酚的方法。

关键词: 苯酚, 硝化, 催化, 邻硝基苯酚

Abstract: A series of silica supported cesium salts of molybdovanadophosphoric acid catalysts with different loadings was prepared by sol-gel technology. Their properties were verified by XRD, IR spectra, SEM and physical adsorption technology. The catalytic activity of these catalysts was evaluated for the liquid phase nitration of phenol with dilute nitric acid under mild conditions. The effects of various parameters on the nitration were tested, which included reaction time, catalyst loading and reactants ratio. The results indicate that the catalyst prepared has the Keggin type structure and these particles are well dispersed on the surface of silica. The catalysts exhibit strong activity and high selectivity toward the o-nitration of phenol with a yield of 88% under appropriate conditions. Moreover, the supported catalysts can be recovered simply and reused several times. After the nitration, the o-nitrophenol obtained can be extracted via steam distillation.

Key words: phenol, nitration, catalysis, o-nitrophenol

中图分类号:

O643.3

刘丽君, 慈英倩, 王齐聊, 龚树文, 崔庆新. 二氧化硅负载磷钼钒酸铯选择性催化硝化苯酚为邻硝基苯酚[J]. 应用化学, DOI: 10.3724/SP.J.1095.2014.30463.

LIU Lijun, CI Yingqian, WANG Qiliao, GONG Shuwen*, CUI Qingxin. Selective Catalytic Nitration of Phenol to o-Nitrophenol by Silica Supported Cesium Salts of Molybdovanadophosphoric Acid[J]. Chinese Journal of Applied Chemistry, DOI: 10.3724/SP.J.1095.2014.30463.

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