硅胶负载H_6PMo_9V_3O_(40)催化合成5-硝基水杨醛  

Synthesis of 5-Nitrosalicylaldehyde Catalyzed by H_6PMo_9V_3O_(40) Supported on Silica Gel

作　　者：吴锦明[1] 汤艳峰[1] 沈爱宝[1] 

机构地区：[1]南通大学化学化工学院,南通226019

出　　处：《应用化学》2012年第5期545-550,共6页Chinese Journal of Applied Chemistry

基　　金：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。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.

关 键 词：硝基水杨醛 硅胶负载H6PMo9V3O40 硝化反应 水杨醛 

分 类 号：O625.6[理学—有机化学] O643.3[理学—化学]