磷化镍催化剂的制备及表征

Preparation and characterization of Nickel phosphide catalyst

采用溶胶-凝胶法制备钛铝复合氧化物载体,并用饱和浸渍法制备磷化镍催化剂氧化态前驱体,在小型连续流动固定床反应器中采用原位还原技术用氢气制备出磷化镍催化剂,并用X射线衍射(XRD)、红外和氮气吸附(BET)等表征方法对载体及催化剂进行表征.复合载体的BET结果表明,采用溶胶-凝胶法制备的钛铝复合载体,比表面积较大,孔体积和平均孔径适中,孔结构最为理想.XRD结果表明,复合载体负载磷化镍后,表面结构、孔结构和晶型均发生较大变化,比表面积和孔径、孔容都有很大程度的降低,证明活性组分在催化剂表面得到了很好的分散.

The carrier of titanium aluminum composite oxide was prepared by sol-gel method,and the oxidation state precursor of nickel phosphide catalyst was prepared by saturated impregnation method.Nnickel phosphide catalyst was prepared in a small fixed bed flow reactor using hydrogen by situ reduction technology.X ray diffraction （XRD）,infrared and nitrogen adsorption （BET） methods were used to characterize the carrier and catalyst.BET results show that the composite carrier prepared by sol-gel method has ideal pore structure with large specific surface area,moderate pore volume and average pore size.XRD results show that surface structure,pore structure and crystal are changed after composite carrier supports nickel phosphide; the specific surface area and pore size,pore volume reduces greatly,which proves that the active components of the catalyst surface are well dispersed.