Probing the Active Sites of MoS2 Based Hydrotreating Catalysts Using Modulation Excitation Spectroscopy

Gaur, Abhijeet; Hartmann Dabros, Trine Marie; Høj, Martin; Boubnov, Alexey; Prüssmann, Tim; Jelic, Jelena; Studt, Felix; Jensen, Anker Degn; Grunwaldt, Jan -Dierk

doi:10.1021/acscatal.8b04778

Probing the Active Sites of MoS₂ Based Hydrotreating Catalysts Using Modulation Excitation Spectroscopy

Journal Article · Thu Jan 31 04:00:00 EST 2019 · ACS Catalysis

DOI:https://doi.org/10.1021/acscatal.8b04778· OSTI ID:1505429

^[1]; Hartmann Dabros, Trine Marie ^[2]; ^[3]; Boubnov, Alexey ^[4]; ^[1]; Jelic, Jelena ^[1]; Studt, Felix ^[1]; ^[3]; ^[1]

Karlsruhe Institute of Technology (KIT), Karlsruhe (Germany)
Technical Univ. of Denmark (DTU), Lyngby (Denmark); Haldor Topsoes Alle1, Lyngby (Denmark)
Technical Univ. of Denmark (DTU), Lyngby (Denmark)
Karlsruhe Institute of Technology (KIT), Karlsruhe (Germany); SLAC National Accelerator Lab., Menlo Park, CA (United States)

The reactive surface sites of MoS₂ hydrotreating catalysts (unpromoted as well as Co- and Ni-promoted) supported on MgAl₂O₄ spinel were investigated with respect to the substitution of sulfur by oxygen using in situ XAS coupled with modulation excitation spectroscopy (MES). Specifically, MES experiments were carried out by periodically cycling between a H₂O and H₂S containing hydrogen gas mixture at 400 °C. Due to the low fraction of S–O exchange, conventional XANES and EXAFS data hardly showed any changes when these catalysts were exposed to increasing ratios of H₂O to H₂S in an H₂ atmosphere. XANES and EXAFS data extracted at the Mo K-edge by MES analysis showed that for approximately 1% of the Mo atoms, sulfur atoms are replaced by oxygen atoms when exposed to H₂O, causing partial oxidation of these active sites. The reaction is reversible and Mo returns to its initial sulfide phase when H₂O is removed and H₂S is supplied in the feed. In the case of Co- and Ni-promoted catalysts, the magnitude of S–O exchange was found to be reduced, indicating the beneficial effect of promotion. MES at the Ni K-edge showed that Ni was oxidized during H₂O exposure, which in turn delayed the Mo oxidation in the Ni-promoted catalyst. The structures of these catalysts under S–O exchange were modeled using density functional theory (DFT) calculations, showing that the edge atoms are affected strongly. For all three catalysts, OH substitution is more favorable, while O substitution could be possible at high H₂O pressure for unpromoted MoS₂. Mo K-edge XANES spectra calculated using these simulated structures support the results obtained from the MES experiments. In conclusion, the presented approach using MES in combination with XAS and supported by DFT can be extended in general to catalysts under operando conditions and is thus a useful tool for determination of the active site on an atomic-scale.

View Accepted Manuscript (DOE)

Research Organization:: SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States)

Sponsoring Organization:: USDOE

Grant/Contract Number:: AC02-76SF00515

OSTI ID:: 1505429

Journal Information:: ACS Catalysis, Journal Name: ACS Catalysis Journal Issue: 3 Vol. 9; ISSN 2155-5435

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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Hydrodeoxygenation (HDO) of Aliphatic Oxygenates and Phenol over NiMo/MgAl2O4: Reactivity, Inhibition, and Catalyst Reactivation Dabros, Trine Marie Hartmann; Andersen, Mads Lysgaard; Lindahl, Simon Brædder Catalysts, Vol. 9, Issue 6 https://doi.org/10.3390/catal9060521	journal	June 2019
The Influence of Active Phase Loading on the Hydrodeoxygenation (HDO) of Ethylene Glycol over Promoted MoS$_{2}$/MgAl$_{2}$O$_{4}$ Catalysts Dabros, T. M. H.; Kramer, H.; Høj, M. Karlsruhe https://doi.org/10.5445/ir/1000095136	text	January 2019
Hydrodeoxygenation (HDO) of aliphatic oxygenates and phenol over NiMo/MgAl$_{2}$O$_{4}$: Reactivity, inhibition, and catalyst reactivation Dabros, T. M. H.; Andersen, M. L.; Lindahl, S. B. Karlsruhe https://doi.org/10.5445/ir/1000097265	text	January 2019

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37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
Ni/Co-promoted MoS2
S−O exchange
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hydrotreating
modulation excitation spectroscopy
phase sensitive detection