尿素反应法制备介孔Ni-Mo复合氧化物

Synthesis of Mesoporous Ni-Mo Mixed Oxides with Urea Method

采用尿素反应法合成出具有介孔结构的Ni-Mo复合氧化物。用XRD、低温氮气吸附-脱附表征、HRTEM、TG-DTA、FTIR等分析手段对所合成的Ni-Mo复合氧化物及其前躯体进行了表征,并确定了制备Ni-Mo复合氧化物适宜的焙烧温度。以2%二苯并噻吩(DBT)溶液为模型化合物,在固定床连续高压微反装置上考察了介孔Ni-Mo复合氧化物作为催化剂的加氢脱硫(HDS)性能。尿素反应法合成的Ni-Mo复合氧化物具有较高的比表面积,达到124m2·g-1,适宜的孔容0.22mL·g-1,和理想的孔径分布,平均孔径为5.8nm。HDS活性评价表明,这种催化剂具有较高的脱硫率和加氢活性,在反应温度为280℃时脱硫率可达100%,远高于对比催化剂Ni-Mo/Al2O3。

Mesoporous Ni-Mo mixed oxide was synthesized using urea method. The Ni-Mo mixed oxide and precursor were characterized by X-ray powder diffraction analysis （XRD）, low temperature nitrogen adsorptiondesorption, HRTEM, TG-DTA, FTIR techniques, and the optimum calcination temperature of Ni-Mo mixed oxide precursors was detemined. The mesoporous Ni-Mo catalyst was prepared with the Ni-Mo mixed oxides and its activity of hydrodesulfurization（HDS） was also evaluated in a continuous flow micro-reactor using dibenzothiophene（DBT） as a model compound. The Ni-Mo mixed oxide has higher specific area of 124 m2· g^-1 proper pore volume of 0.22 mL· g^-1, and ideal average pore size of 5.8 nm. The evaluation results show that the catalyst has excellent performance for hydrodesulfurization, when the reaction temperature is 280 ℃, the desulfurization rate is 100%, which is much higher than the conventional catalyst Ni-Mo/Al2O3.