Abstract:

Al-MCM-41 mesoporous molecular sieves were prepared by the azeotropic distillation and ultrasonic dispersive technology using sodium silicate as silica source ，aluminum sulfate as aluminum source and cetyltrimethyl ammonium bromide as structure-directing agent. By using Al-MCM-41 as support，nickel nitrate and diammonium hydrogen phosphate as raw materials，a series of supported Ni₂P catalysts on Al-MCM-41 was prepared via the method of temperature-programmed reduction under ultrasonic oscillation. The catalysts were characterized by FTIR，BET，XRD and SEM. Hydrodesulfurization of thiophene catalyzed by Ni₂P/Al-MCM-41 was carried out in a high pressure autoclave reactor. The experimental results showed that Al-MCM-41 prepared by ultrasonic dispersive technology had a much higher specific surface area，larger pore volume and pore diameter than that prepared by conventional mechanical mixing. The Al-MCM-41 prepared by azeotropic distillation with ultrasonic dispersive technology was also better than that using only ultrasonic dispersive technology. The Ni₂P/Al-MCM-41 catalysts，hydrodesulfurization conversion of thiophene nearly reached 100% at the reaction time 5 h，reaction temperature 548 K，and reaction pressure 3.5 MPa.

摘要：

以硅酸钠为硅源、硫酸铝为铝源、十六烷基三甲基溴化铵（CTAB）作模板剂，采用共沸蒸馏与超声波分散技术相结合的方法制备了介孔分子筛Al-MCM-41。以Al-MCM-41为载体、硝酸镍和磷酸氢二氨为原料，采用超声波振荡、程序升温还原法制备了Ni₂P/Al-MCM-41催化剂，并对Al-MCM-41和Ni₂P/Al-MCM-41进行了傅里叶变换红外光谱、比表面积测定、X射线衍射、扫描电镜表征。考察了Ni₂P/Al-MCM-41催化剂对噻吩加氢脱硫的催化性能。结果表明：采用超声波制得的Al-MCM-41其比表面积、孔容和孔径明显高于常规搅拌制得的Al-MCM-41，共沸蒸馏制得的Al-MCM-41其比表面积、孔容和孔径高于未共沸蒸馏的Al-MCM-41；在反应时间为5 h、548 K、3.5 MPa条件下，Ni₂P/Al-MCM-41催化剂对噻吩加氢脱硫的转化率接近100%。