应用化学

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硅胶负载H6PMo9V3O40催化合成5-硝基水杨醛

吴锦明,汤艳峰,沈爱宝*   

  1. (南通大学化学化工学院 南通 226019)
  • 收稿日期:2011-06-20 修回日期:2011-08-23 出版日期:2012-05-10 发布日期:2012-05-10
  • 通讯作者: 沈爱宝,副教授; Tel:0513-85012853; Fax:0513-85012853; E-mail:ajie@ntu.edu.cn; 研究方向:功能有机分子的合成、分析
  • 基金资助:
    国家自然科学基金(21006054)南通市科技计划(K2010021)南通大学自然科学基金(10Z013)资助项目

Synthesis of 5-Nitrosalicylaldehyde Catalyzed by H6PMo9V3O40 Supported on Silica Gel

WU Jinming, TANG Yanfeng, SHEN Aibao*   

  1. (School of Chemistry and Chemical Engineering,Nantong University,Nantong 226019)
  • Received:2011-06-20 Revised:2011-08-23 Published:2012-05-10 Online:2012-05-10
  • Contact: shen aibao

摘要: 采用硅胶负载Keggin型H6PMo9V3O40催化水杨醛与硝酸反应合成5-硝基水杨醛,考察了催化剂负载量、反应时间、反应温度、催化剂用量、硝酸用量和溶剂对反应的影响及催化剂的重复使用性能。 实验结果表明,m(水杨醛)∶m(质量分数65%硝酸)∶m(负载量20%H6PMo9V3O40/SiO2)=2.44∶3.00∶3.00,用石油醚作为溶剂,45 ℃反应2.5 h,水杨醛的转化率为98%,5-硝基水杨醛的选择性为96.8%。 催化剂回收容易,重复使用5次后,活性基本不变。

关键词: 硝基水杨醛, 硅胶负载H6PMo9V3O40, 硝化反应, 水杨醛

Abstract: 5-Nitrosalicylaldehyde was synthesized by the nitration of salicylaldehyde with nitric acid over H6PMo9V3O40 supported on silica gel. The effects of parameters were investigated, such as H6PMo9V3O40 loading, reaction time, temperature, solvent, and so on. Under the optimal conditions:m(salicylaldehyde)∶m(65%HNO3)∶m(20%H6PMo9V3O40/SiO2)=2.44∶3.00∶3.00, in petroleum ether at 45 ℃ for 2.5 h, the conversion of salicylaldehyde was 98%, the selectivity of 5-nitrosalicylaldehyde was up to 96.8%. The catalyst could be recovered easily and reused for five times without noticeable drop in activity.

Key words: nitrosalicylaldehyde, H6PMo9V3O40 supported on silica gel, nitration, salicylaldehyde

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