Ni/Mo/N间隙型催化剂具有高的加氢活性及良好耐硫性,可应用于煤液化油加氢精制高性能喷气燃料.N原子由于只占据晶格间隙位置,在进入Ni/Mo过程中会因不占据晶格中的特定晶位,容易从金属晶格溢出导致无法形成稳定的Ni/Mo/N间隙型催化剂.为此,本文利用前驱体晶型控制的方式来实现Ni/Mo/N催化剂合成.采用络合物分解一步法,考察了不同结晶过程和老化时间对合成的Ni/Mo/N催化剂用于苯加氢反应活性影响,并采用X射线衍射、X射线光电子能谱和透射电镜-能量色散X射线光谱对催化剂结构组成进行表征.XRD分析结果显示,钼酸铵[(NH4)6Mo7O24·4H2O]、乙酸镍[Ni(CH3COO)2·4H2O]和六亚甲基四胺(HMT)添加顺序、结晶过程和老化时间直接影响催化剂组成,并决定Ni/Mo/N晶相的形成.结晶过程慢速搅拌速度和短老化时间有利于合成含Ni2Mo3N,Mo2C和Ni晶相的高活性Ni/Mo/N间隙型催化剂,使苯加氢制环己烷模型反应苯的最大转化率达93％,环己烷选择性为100％.含0.01 wt％噻吩的存在使苯转化率由72％降至50％,XPS分析结果表明,催化剂表面形成的MoS2是催化剂活性降低的重要因素.
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