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硅胶负载H6PMo9V3O40催化合成5-硝基水杨醛
引用本文:吴锦明,汤艳峰,沈爱宝.硅胶负载H6PMo9V3O40催化合成5-硝基水杨醛[J].应用化学,2012,29(5):545-550.
作者姓名:吴锦明  汤艳峰  沈爱宝
作者单位:(南通大学化学化工学院 南通 226019)
基金项目: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
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  
收稿时间:2011-06-20

Synthesis of 5-Nitrosalicylaldehyde Catalyzed by H6PMo9V3O40 Supported on Silica Gel
WU Jinming , TANG Yanfeng , SHEN Aibao.Synthesis of 5-Nitrosalicylaldehyde Catalyzed by H6PMo9V3O40 Supported on Silica Gel[J].Chinese Journal of Applied Chemistry,2012,29(5):545-550.
Authors:WU Jinming  TANG Yanfeng  SHEN Aibao
Institution:(School of Chemistry and Chemical Engineering,Nantong University,Nantong 226019)
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.
Keywords:nitrosalicylaldehyde  H6PMo9V3O40 supported on silica gel  nitration  salicylaldehyde
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