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作 者:宋立民[1] 李伟[1] 张明慧[1] 陶克毅[1]
机构地区:[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
出 处:《催化学报》2006年第12期1127-1132,共6页
基 金:国家自然科学基金(20403009);教育部科学技术研究重点项目(105045)资助.
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40~50nm,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.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.
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