溶剂热合成氮化铁及其催化氯代硝基苯加氢反应的研究

Solvothermal synthesis of Fe_xN catalysts and catalytic hydrogenation of chloronitrobenzene

采用溶剂热法制备了氮化铁催化剂,并用于邻氯硝基苯加氢合成氯代苯胺反应,考察了合成温度、原料配比以及合成时间等制备条件对其催化性能的影响.通过XRD、TG-DTG、BET等方法对催化剂的结构和性质进行表征.结果表明:在合成温度400℃、m(NaN_3)∶m(FeCl_2)=4∶1以及反应时间为30h的条件下制备的氮化铁催化剂,在邻氯硝基苯加氢反应中,邻氯代硝基苯转化率为58.41%,邻氯苯胺选择性为100%.所制备的氮化铁催化剂具有较好的热稳定性;除了有介孔结构外,还有大孔结构的颗粒.提高合成温度,有利于提高所制备的氮化铁催化剂的结晶度和纯度.

A series of FexN catalysts were prepared by the solvent thermal method.The physicochemical properties of the catalysts were characterized by X-ray diffraction（XRD）,thermal gravimetric analysis（TG-DTG）,pupil analysis（BET）.The results shows that the chloronitrobenzene conversion was 58.41%,and the selectivity reached 100% when the reaction temperature was set at 400 ℃,NaN_3∶FeCl_2 was 4∶1and reaction time was 30 h.These catalysts have good thermal stability.In addition to the mesoporous structure,there are large pore structure of particles.The crystallinity and purity of FexN catalyst were improved with increasing the synthesis temperature.