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Synthesis of catalysts based on nitrides and carbides of Nb and Mo for thiophene hydrodesulfurization

Abstract:

Niobium and molybdenum nitride- and carbide-based catalysts were synthesized from the precursor compounds: ammonium and niobium oxalate, molybdenum heptamolybdate and molybdenum trioxide. Nitrides were prepared by ammonolysis under a NH3 atmosphere with a flow of 100 ml/min, heating at 3 °C/min up to final temperatures in the 700-800 °C range. For the carbides synthesis two methods were employed: The first treating the Nb or Mo nitrides previously synthesized under flow of 100 ml/min of 20% CH 4/balance H2 up to a final temperature of 700 or 800 °C, at a rate of 3 °C/min. The second method consisted of a carbothermal treatment of mechanical mixtures of the Nb or Mo precursor compounds with activated carbon, in a molar ratio 1:3, under a 100 ml/min flow of H2 and heating at a rate of 3 °C/min up to 700-800 °C The solid products were characterized by X-ray diffraction (XRD), BET specific surface areas (SSA), X-ray photoelectron spectroscopy (XPS) and finally were catalytically evaluated in the hydrodesulfurization (HDS) of thiophene at atmospheric pressure and 350 °C From XRD and XPS results it is concluded that, under the employed experimental conditions, Nb and Mo nitrides and carbides could be synthesized with the exception of the mechanical mixture of activated carbon and the niobium precursor; SSA values were in the range 10 - 35 m2/g for nitrides and carbides prepared by direct nitriding and carbiding, and a strong influence of activated carbon residua in the areas of samples obtained by carboreduction of mechanical mixtures was evident. It was also observed that the higher the SSA, the higher the catalytic activity. Among all the synthesized solids, the molybdenum nitrides and carbides proved to be the more active catalysts in HDS.