Catalysis Letters

, Volume 134, Issue 1–2, pp 138–146 | Cite as

Unsupported Ni/Mo(W)S2 Catalysts from Hexamethylenediammonium Thiometallates Precursors: In Situ Activation During the HDS of DBT

  • J. A. Lumbreras
  • R. Huirache-Acuña
  • E. M. Rivera-Muñoz
  • G. Berhault
  • G. Alonso-Núñez
Article

Abstract

Unsupported Ni/MoS2 and Ni/WS2 HDS catalysts were prepared by in situ activation of hexamethylenediammonium thiometallates promoted with Ni. The method involved an aqueous solution reaction of ammonium thiomolybdate (ATM) or ammonium thiotungstate (ATT) with Ni(NO3)2·6H2O and hexamethylenediamine. Ni-promoted precursors were then in situ activated during the hydrodesulfurization (HDS) of dibenzothiophene (DBT) producing Ni/MoS2 and Ni/WS2 catalysts. Solids were analyzed after the in situ activation by scanning electron microscopy, transmission electron microscopy, X-ray diffraction, and for textural properties by using the BET and BJH methods. Catalysts with relatively high surface area and type IV N2 adsorption–desorption isotherms were obtained. The use of the hexamethylenediammonium precursor led to a significant nickel promotion of MoS2 and WS2 catalysts. For Ni/MoS2, the use of this carbon-containing precursor was found to be more beneficial for the final HDS catalytic activity than using the classical ammonium tetrathiomolybdate (ATM) without carbon. For Ni/WS2, compared to tetraalkylammonium thiosalts, the lower amount of carbon in excess formed during the decomposition of the hexamethylenediammonium precursor coupled with a lower crystallization rate of WS2 favors a correct nickel accommodation on the WS2 edges.

Keywords

Hexamethylenediammonium thiometallates In situ activation Ni-promotion Hydrodesulfurization 

Notes

Acknowledgments

The authors appreciate the valuable technical assistance of C. Ornelas, W. Antúnez, F. Paraguay-Delgado and E. Torres and DGAPA-UNAM IN102509-3 by financial support. R. Huirache-Acuña thanks the postdoctoral fellowship support to Universidad Nacional Autónoma de México (UNAM) and Project DGAPA-UNAM PAPIIT NI113806-3.

Supplementary material

10562_2009_209_MOESM1_ESM.doc (450 kb)
(DOC 450 kb)

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Copyright information

© Springer Science+Business Media, LLC 2009

Authors and Affiliations

  • J. A. Lumbreras
    • 1
  • R. Huirache-Acuña
    • 2
  • E. M. Rivera-Muñoz
    • 2
  • G. Berhault
    • 3
  • G. Alonso-Núñez
    • 4
  1. 1.Universidad del Istmo Campus TehuantepecSanto Domingo TehuantepecMexico
  2. 2.Centro de Física Aplicada y Tecnología AvanzadaUniversidad Nacional Autónoma de MéxicoQuerétaroMexico
  3. 3.Institut de Recherches sur la Catalyse et l’Environnement de Lyon, IRCELYONUMR5256 CNRS—Université de LyonVilleurbanneFrance
  4. 4.Centro de Nanociencias y NanotecnologíaUniversidad Nacional Autónoma de MéxicoEnsenadaMexico

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