催化学报 ›› 2006, Vol. 27 ›› Issue (12): 1127-1132.

• 研究论文 • 上一篇    下一篇

由非晶态Ni-P低温制备Ni2P催化剂及其对二苯并噻吩加氢脱硫的催化性能

宋立民,李伟,张明慧,陶克毅   

  1. 南开大学化学学院材料化学系新催化材料科学研究所, 天津 300071
  • 收稿日期:2006-12-25 出版日期:2006-12-25 发布日期:2006-12-25

Preparation of Ni2P Catalyst from Amorphous Ni-P at Low Temperature and Its Catalytic Performance for Dibenzothiophene Hydrodesulfurization

SONG Limin, LI Wei*, ZHANG Minghui, TAO Keyi   

  1. SONG Limin, LI Wei*, ZHANG Minghui, TAO Keyi
  • Received:2006-12-25 Online:2006-12-25 Published:2006-12-25

摘要: 以非晶态Ni-P合金为前驱体,在低温下通过PH3处理制备了Ni2P/SiO2-Al2O3催化剂,并用X射线衍射(XRD)、 透射电镜(TEM)、 电感耦合等离子体发射光谱、 N2吸附和X射线光电子能谱(XPS)进行了表征,以二苯并噻吩为探针,在小型连续流动固定床反应器上考察了催化剂的加氢脱硫性能. XRD结果表明,在200~300 ℃范围内前驱体都可以完全转化为Ni2P, 随着磷化温度的升高,晶体结构变得越来越完整. TEM观察发现, Ni-P粒子和Ni2P粒子的平均尺寸都在40~50 nm, 并且都能够高分散在SiO2-Al2O3载体上. XPS结果表明,不论是非负载还是SiO2-Al2O3负载的Ni2P, 表层主要为Ni2P和钝化层Ni3(PO4)2. Ni2P/SiO2-Al2O3催化剂在实验范围内表现出很好的二苯并噻吩加氢脱硫性能.

关键词: 非晶态合金, 磷化镍, 二苯并噻吩, 加氢脱硫

Abstract: Ni2P/SiO2-Al2O3 catalysts were successfully prepared by treating amorphous Ni-P alloys with phosphine at low temperature. The as-prepared catalysts were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), inductively coupled plasma atomic emission spectroscopy, N2 adsorption, and X-ray photoelectron spectroscopy (XPS). The XRD data showed that the amorphous Ni-P/SiO2-Al2O3 precursors could be completely transformed to crystalline Ni2P/SiO2-Al2O3 at 200-300 ℃. The crystalline structure of Ni2P became more prominent with increasing phosphatization temperature. The results of TEM indicated that Ni-P and Ni2P particles were both 40-50 nm in diameter and were well dispersed on the supports. The XPS results suggested that the main components were Ni2P and Ni3(PO4)2 on the surface of both Ni2P and Ni2P/SiO2-Al2O3. The Ni2P/SiO2-Al2O3 catalysts showed good activity for dibenzothiophene hydrodesulfurizationunder the experimental conditions.

Key words: amorphous alloy, nickel phosphide, dibenzothiophene, hydrodesulfurization