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有机化学
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有机化学 ›› 2004, Vol. 24 ›› Issue (7): 778-782. 上一篇    下一篇

研究论文

高氯酸锂促进的固体酸催化酯化反应

王丽琼, 聂进*, 李小永, 张正波, 尹飞   

  1. 华中科技大学化学系 武汉 430074
  • 收稿日期:2003-06-23 修回日期:2004-01-07 接受日期:2004-02-09 发布日期:2022-09-20
  • 通讯作者: *E-mail: niejin@mail.hust.edu.cn

Enhancement Effect of Lithium Perchlorate on the Esterification Catalyzed by Yb(NTf2)3-Resin Catalyst

WANG, Li-Qiong, NIE, Jin*, LI, Xiao-Yong, ZHANG, Zheng-Bo, YIN, Fei   

  1. Department of Chemistry, Huazhong University of Technology and Science, Wuhan430074
  • Received:2003-06-23 Revised:2004-01-07 Accepted:2004-02-09 Published:2022-09-20

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将二(三氟甲基磺酰)亚胺镱(III) [Yb(NTf2)3]负载于NKC-9树脂上得到一种催化活性更高的酯化固体酸催化剂,发现高氯酸锂能够显著加速固体酸催化剂酯化反应速度,在不分水,相对于苯甲酸负载树脂用量30 wt%, Yb(NTf2)3用量0.8 mol%, LiClO4用量58 mol%, n(苯甲酸)∶n(乙醇)=1∶7的条件下,2 h内即可使苯甲酸与乙醇的直接酯化反应进行完全.同时研究了负载量、温度、高氯酸锂用量对苯甲酸酯化反应的影响.

关键词: Yb(NTf2)3, 高氯酸锂, 固体酸催化剂, 树脂, 酯化反应

A novel solid acid catalyst was prepared by supporting Yb(NTf2)3 on NKC-9 resin and the new catalyst showed higher catalytic activity inesterification reactions compared with that of Yb(NTf2)3 as homogenous catalyst. When lithium perchlorate was added together with this solid acid catalyst, the esterification of benzoic acid with alcohols was significantly accelerated. The effects of reaction time, temperature, Yb(NTf2)3 loadings and LiClO4 dosage upon esterification were also investigated. Under the optimum conditions: supported resin 30 wt%, Yb(NTf2)3 0.8 mol%, LiClO4 58 mol%, acid∶alcohol (molar ratio)=1∶7 and reflux for 2 h, the yield of ethyl benzoate was over 99%. A tentative study of the LiClO4 acceleration effect was made through comparison of different catalysts.

Key words: Yb(NTf2)3, lithium perchlorate, solid acid, resin, esterification