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
作者单位
邵长丽 中国石油大学(华东)化学化工学院重质油加工国家重点实验室CNPC催化重点实验室,青岛 266555
开滦精煤股份有限公司唐山 063018 
殷长龙 中国石油大学(华东)化学化工学院重质油加工国家重点实验室CNPC催化重点实验室,青岛 266555 
张俊萍 中国石油大学(华东)化学化工学院重质油加工国家重点实验室CNPC催化重点实验室,青岛 266555 
陈世安 抚顺石油化工公司催化剂厂抚顺 113008 
刘晨光 中国石油大学(华东)化学化工学院重质油加工国家重点实验室CNPC催化重点实验室,青岛 266555 
摘要: 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124 m2·g-1,适宜的孔容0.22 mL·g-1,和理想的孔径分布,平均孔径为5.8 nm。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
关键词: 尿素  Ni-Mo复合氧化物  加氢脱硫  二苯并噻吩
基金项目: 
Abstract: 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 adsorption-desorption, 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.
Keywords: urea  Ni-Mo mixed oxides  hydrodesulfurization  Dibenzothiophene
 
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邵长丽,殷长龙,张俊萍,陈世安,刘晨光.尿素反应法制备介孔Ni-Mo复合氧化物[J].无机化学学报,2008,24(11):1782-1788.
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