化工进展 ›› 2015, Vol. 34 ›› Issue (07): 1882-1886.DOI: 10.16085/j.issn.1000-6613.2015.07.012

• 工业催化 • 上一篇    下一篇

制备条件对Ni2P/TiO2-Al2O3催化剂加氢脱硫性能的影响

苑丹丹1, 张永江1, 李锋1, 宋华1,2   

  1. 1 东北石油大学化学化工学院, 黑龙江 大庆 163318;
    2 东北石油大学石油与天然气化工省重点实验室, 黑龙江 大庆 163318
  • 收稿日期:2014-12-09 修回日期:2015-02-02 出版日期:2015-07-05 发布日期:2015-07-05
  • 通讯作者: 宋华,教授,主要从事催化剂方面的研究。E-mail:songhua2004@sina.com。
  • 作者简介:苑丹丹(1978—),女,博士研究生,研究方向为工业催化和绿色化学。E-mail:yuandandan111@163.com。
  • 基金资助:
    国家自然科学基金(21276048)、黑龙江省自然基金(ZD201201)及黑龙江省教育厅项目(12541080)。

Effect of preparation conditions on hydrodesulfurization performance of the Ni2P/TiO2-Al2O3 catalyst

YUAN Dandan1, ZAHNG Yongjiang1, LI Feng1, SONG Hua1,2   

  1. 1 College of Chemistry & Chemical Engineering, Northeast Petroleum University, Daqing 163318, Heilongjiang, China;
    2 Provincial Key Laboratory of Oil & Gas Chemical Technology, Northeast Petroleum University, Daqing 163318, Heilongjiang, China
  • Received:2014-12-09 Revised:2015-02-02 Online:2015-07-05 Published:2015-07-05

摘要: 采用溶胶-凝胶法制备了TiO2-Al2O3复合载体, 以柠檬酸为络合剂, 浸渍法制备了负载型Ni2P/TiO2-Al2O3催化剂前体, 程序升温H2还原法制备了Ni2P/TiO2-Al2O3催化剂, 并用 X 射线衍射(XRD)、N2吸附比表面积(BET)测定技术对催化剂的结构和性质进行了表征, 考察了浸渍方法、Ni/P摩尔比、Ni2P负载量对其进行的二苯并噻吩(DBT)加氢脱硫(HDS)性能的影响。结果表明, 当Ni/P比低于1:1时, 能得到单一的Ni2P物相;当Ni/P比为2:1时, 开始出现Ni3P物相。采用Ni/P比为1:1、Ni2P负载量为30%、采用共浸渍方法制备的Ni2P/TiO2-Al2O3催化剂具有最好的活性, 在360℃、3.0MPa、氢油比500 (体积比)、液时体积空速2.0h-1的条件下反应4h时, 二苯并噻吩转化率为99.5%。

关键词: 磷化二镍, 加氢脱硫, 柠檬酸, 络合剂, 催化剂, 制备

Abstract: The TiO2-Al2O3 complex support was prepared by the sol-gel method. A nickel phosphide catalyst, Ni2P/TiO2-Al2O3 with citric acid (CA) as chelating agent, was prepared by impregnation method using citric acid (CA) as complexing agent. The catalysts were characterized by X-ray diffraction (XRD) and N2-adsorption specific surface area measurements (BET). The catalytic performance of Ni2P/TiO2-Al2O3 was investigated by hydrodesulfurization (HDS) of dibenzothiophene (DBT). The effects of different, immersion sequences, Ni/P molar ratios and Ni2P loadings on catalytic activity were studied. The results showed that, when the Ni/P molar ratio was less than 1:1, the single Ni2P phase can be obtained. However, Ni3P phase can be observed with the Ni/P molar ratio of 2:1. The Ni2P/TiO2-Al2O3 prepared by co-impregnation method with Ni/P molar ratio of 1:1, a loading of 30% exhibits the optimized catalytic performance. When reaction temperature was 360℃, pressure was 3.0MPa, and hydrogen/oil ratio was 500, and liquid hourly space velocity was 2.0h-1, the conversion of dibenzothiophene HDS was 99.5%.

Key words: nickel phosphide, hydrodesulfurization, citric acid, chelating agent, catalyst, preparation

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