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- Author or Editor: F. Delannay x
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Abstract
A57Co doped unsupported CoMo sulfide catalyst with atomic composition ratio r=Co/(Co+Mo)=0.3 was prepared by the homogeneous sulfide precipitation method and exposed to a series of reduction-sulfidation treatments. The treated samples were analyzed by Mössbauer emission spectroscopy using very long accumulation times. Computer decomposition of the spectra revealed the presence of five different cobalt species which were identified as Co9S8, CoS1+x, and three species related to the Co–Mo–S structure. Reduction of the sample under atmospheric pressure of H2 at (and above) 573 K causes an increase of the amount of Co9S8 at the expense of all other species. These results afford a new insight into the stability of the Co–Mo–S structure and of the sulfur rich CoS1+x phase under hydrotreating conditions.
Precursors of unsupported NiMo and FeMo sulfide hydrodesulfurization catalysts with concentration ratiosr=Ni(Fe)/(Ni(Fe) + Mo) ranging from 0.1 to 0.3 were prepared by three methods: homogeneous sulfide precipitation (HSP), inverse HSP and coprecipitation. Differential thermal analysis was used to study the decomposition under argon, and the reduction/sulfidation under 15% H2S—H2 of the precursors and the subsequent oxidation under air of the samples obtained after these reactions. The reactivity of the solids varies as a function of the preparation method, the nature of the promoter and the concentration ratio. The degree of sulfidation of the precursor and the presence of either NH4NO3 or NH2Cl formed from group VIII metal salts and (NH4)2S may affect the thermal behaviour of samples during DTA.
