CIESC Journal ›› 2004, Vol. 55 ›› Issue (1): 37-41.

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EFFECTS OF PREPARATION CONDITIONS ONNi/SiO2 CATALYST ACTIVITYIN m-DINITROBENZENE HYDROGENATION

LIU Yingxin;CHEN Jixiang;ZHANG Jiyan   

  • Online:2004-01-25 Published:2004-01-25

Ni/SiO2催化剂的制备条件对催化间二硝基苯加氢反应性能的影响

刘迎新;陈吉祥;张继炎   

  1. 天津大学化工学院催化科学与工程系,天津300072

Abstract: The effects of calcination temperature and reduction temperature on the silica supported nickel catalyst, which were prepared by impregnation of silica with nickel nitrate solution, were investigated in the liquid-phase hydrogenation of m-dinitrobenzene to m-phenylenediamine. The nature of the catalysts was discussed based on the characterization results of nitrogen adsorption-desorption (BET), X-ray diffraction (XRD), transmission electron microscopy (TEM) and temperature-programmed reduction (TPR). With increasing calcination temperature, the surface area of the catalyst decreased progressively, but the interaction between NiO and SiO2 became stronger. At the same time, the crystallite of nickel increased with the increase of calcination temperature. The optimal calcination temperature was 773 K, at which highly dispersed nickel species could be present. The reduction temperature also affected the properties of the catalyst. At a lower temperature, the catalyst could not be reduced completely, while an improperly high temperature would cause sintering of the catalyst. The catalyst reduced at 723 K showed higher catalytic activity and selectivity.

Key words:

Ni/SiO2催化剂, 催化加氢, 间二硝基苯, 间苯二胺

摘要: 将Ni/SiO2催化剂应用于间二硝基苯加氢反应中,考察了该催化剂制备过程中焙烧温度和还原温度对其催化性能的影响,并通过BET、XRD、TEM、TPR等方法对催化剂进行了表征.结果表明,在实验研究范围内,随着焙烧温度的提高,Ni/SiO2催化剂比表面积降低,NiO与载体SiO2之间的相互作用逐渐增强,催化剂的还原温度明显提高,活性组分Ni的晶粒度增大,焙烧温度为773 K时催化剂具有最佳的催化反应性能,此时活性组分Ni以高分散状态存在.催化剂的还原温度对Ni/SiO2催化剂的结构和催化性能影响显著,当还原温度较低时,活性组分还原不完全,催化剂活性较低;而还原温度太高会使活性组分烧结,导致催化剂活性明显降低;还原温度为723 K时催化剂表现出最佳的活性和选择性.

关键词:

Ni/SiO2催化剂, 催化加氢, 间二硝基苯, 间苯二胺