In Situ XRD, XAS, and Magnetic Susceptibility Study of the Reduction of Ammonium Nickel Phosphate NiNH4PO4•H2O into Nickel Phosphide

被引:52
作者
Berhault, Gilles [1 ]
Afanasiev, Pavel [1 ]
Loboue, Hermione [1 ]
Geantet, Christophe [1 ]
Cseri, Tivadar [2 ]
Pichon, Christophe [2 ]
Guillot-Deudon, Catherine [3 ]
Lafond, Alain [3 ]
机构
[1] Univ Lyon 1, CNRS, Inst Rech Catalyse & Environm Lyon, F-69626 Villeurbanne, France
[2] IFP Lyon, F-69390 Vernaison, France
[3] Univ Nantes, Inst Mat Jean Rouxel, CNRS, F-44322 Nantes 3, France
关键词
THIOPHENE HYDRODESULFURIZATION; HYDROTREATING ACTIVITY; CATALYSTS; NI2P; DIFFRACTION; NI2P/SIO2; SPECTRA; FTIR;
D O I
10.1021/ic802074k
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
The reduction of the ammonium nickel phosphate NiNH4PO4 center dot H2O precursor into nickel phosphide (Ni2P), a highly active phase in hydrotreating catalysis, was studied using a combination of magnetic susceptibility and in situ X-ray diffraction and X-ray absorption spectroscopy (XAS) techniques. The transformation of NiNH4PO4 center dot H2O into Ni2P could be divided into three distinguishable zones: (1) from room temperature to 250 degrees C, the NiNH4PO4 center dot H2O structure was essentially retained; (2) from 300 to 500 degrees C, only an amorphous phase was observed; (3) above 500 degrees C, a crystallization process occurred with the formation of Ni2P. An in situ XAS study and magnetic susceptibility measurements clearly revealed for the first time that the amorphous region corresponds to the nickel pyrophosphate phase alpha-Ni2P2O7. The phosphate reduction into phosphide did not start before 550 degrees C and led to the selective formation of Ni2P at 650 degrees C,
引用
收藏
页码:2985 / 2992
页数:8
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