介孔分子筛的制备及催化合成2-三氟甲氧基-5-硝基苯胺  

Preparation of MCM-41-SO_3H and Catalytic Synthesis of 2-Trifluoromethoxy-5-nitroaniline

作　　者：奚立民[1] 陈晓芳[1] 

机构地区：[1]台州职业技术学院生物与化学工程系,浙江台州318000

出　　处：《化学世界》2009年第3期163-166,173,共5页Chemical World

基　　金：浙江省科技计划重大项目(2006C11026)

摘　　要：采用直接合成法制备出由MCM-41介孔分子筛负载SO3H的催化剂,测定了催化剂表面的酸中心组成,并考察了不同工艺条件下邻三氟甲氧基苯胺区域选择性硝化的催化性能。用硫酸钡重量法、TEM和N2吸附-脱附表征了MCM-41-SO3H的结构。结果表明,MCM-41-SO3H保持了MCM-41的介孔结构,BET表面积高达560 m2/g,表面含有质子酸中心;得到最佳的工艺条件:m(邻三氟甲氧基苯胺)/m(催化剂)=32,n(硝酸)/n(邻三氟甲氧基苯胺)=3.0,反应温度65°C,反应时间3 h,邻三氟甲氧基苯胺转化率为93.5%,2-三氟甲氧基-5-硝基苯胺含量达到84.2%。催化剂焙烧温度290°C,催化剂重复使用6次仍保持较高活性。Catalyst of sulfonie acid group supported on mesoporous MCM-41 was prepared by directsynthesis method. The acid sites on catalyst surface were tested. The catalytic performance for o-trifluoromethoxyaniline regioselective nitration was investigated under various conditions. The structure of MCM-41-SO3 H was characterized by the gravimetry of BaSO4, TEM and N2 adsorption/desorption. The results showed that the mesoporous structure of MCM-41 was maintained in the MCM-41-SO3 H system. The catalyst had a high BET surface area of 560 m^2/g, and there were abundant Bronsted acid sites on the catalyst surface. The optimum reaction conditions were 65 ℃, 3 h, m （o-trifluoromethoxyaniline）/m （catalyst） =32 and n （nitric acid）/n （o-trifluoromethoxyaniline）= 3. 0. The conversion of o- trifluoromethoxyaniline reached 93.5 % and the percentage of 2-trifluoromethoxy-5-nitroaniline reached 84. 2%. When calcined at 290 ℃, the catalyst still kept highly active after being reused six times.

关 键 词：MCM-41分子筛 磺酸 2-三氟甲氧基-5-硝基苯胺 区域选择性硝化 催化 

分 类 号：O643[理学—物理化学]