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Elucidation of the Reaction Mechanism for High-Temperature Water Gas Shift over an Industrial-Type Copper–Chromium–Iron Oxide Catalyst

  • Felipe Polo-Garzon
    Felipe Polo-Garzon
    Chemical Sciences Division and Center for Nanophase Materials Sciences, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831, United States
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    Orcidhttp://orcid.org/0000-0002-6507-6183
  • , 
  • Victor Fung
    Victor Fung
    Chemical Sciences Division and Center for Nanophase Materials Sciences, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831, United States
    Department of Chemistry, University of California, Riverside, California 92521, United States
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    Orcidhttp://orcid.org/0000-0002-3347-6983
  • , 
  • Luan Nguyen
    Luan Nguyen
    Departments of Chemical Engineering and Chemistry, The University of Kansas, Lawrence, Kansas 66047, United States
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  • , 
  • Yu Tang
    Yu Tang
    Departments of Chemical Engineering and Chemistry, The University of Kansas, Lawrence, Kansas 66047, United States
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    Orcidhttp://orcid.org/0000-0001-9435-9310
  • , 
  • Franklin Tao
    Franklin Tao
    Departments of Chemical Engineering and Chemistry, The University of Kansas, Lawrence, Kansas 66047, United States
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    Orcidhttp://orcid.org/0000-0002-4916-6509
  • , 
  • Yongqiang Cheng
    Yongqiang Cheng
    Neutron Scattering Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831, United States
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    Orcidhttp://orcid.org/0000-0002-3263-4812
  • , 
  • Luke L. Daemen
    Luke L. Daemen
    Neutron Scattering Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831, United States
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  • , 
  • Anibal J. Ramirez-Cuesta
    Anibal J. Ramirez-Cuesta
    Neutron Scattering Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831, United States
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  • , 
  • Guo Shiou Foo
    Guo Shiou Foo
    Chemical Sciences Division and Center for Nanophase Materials Sciences, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831, United States
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  • Minghui Zhu
    Minghui Zhu
    Operando Molecular Spectroscopy & Catalysis Laboratory, Department of Chemical and Biomolecular Engineering, Lehigh University, Bethlehem, Pennsylvania 18015, United States
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    Orcidhttp://orcid.org/0000-0003-1593-9320
  • , 
  • Israel E. Wachs
    Israel E. Wachs
    Operando Molecular Spectroscopy & Catalysis Laboratory, Department of Chemical and Biomolecular Engineering, Lehigh University, Bethlehem, Pennsylvania 18015, United States
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    Orcidhttp://orcid.org/0000-0001-5282-128X
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  • De-en Jiang
    De-en Jiang
    Department of Chemistry, University of California, Riverside, California 92521, United States
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    Orcidhttp://orcid.org/0000-0001-5167-0731
  • , and 
  • Zili Wu*
    Zili Wu
    Chemical Sciences Division and Center for Nanophase Materials Sciences, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831, United States
    *[email protected]
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    Orcidhttp://orcid.org/0000-0002-4468-3240
Cite this: J. Am. Chem. Soc. 2019, 141, 19, 7990–7999
Publication Date (Web):April 25, 2019
https://doi.org/10.1021/jacs.9b03516
Copyright © 2019 American Chemical Society
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    Abstract

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    The water gas shift (WGS) reaction is of paramount importance for the chemical industry, as it constitutes, coupled with methane reforming, the main industrial route to produce hydrogen. Copper–chromium–iron oxide-based catalysts have been widely used for the high-temperature WGS reaction industrially. The WGS reaction mechanism by the CuCrFeOx catalyst has been debated for years, mainly between a “redox” mechanism involving the participation of atomic oxygen from the catalyst and an “associative” mechanism proceeding via a surface formate-like intermediate. In the present work, advanced in situ characterization techniques (infrared spectroscopy, temperature-programmed surface reaction (TPSR), near-ambient pressure XPS (NAP-XPS), and inelastic neutron scattering (INS)) were applied to determine the nature of the catalyst surface and identify surface intermediate species under WGS reaction conditions. The surface of the CuCrFeOx catalyst is found to be dynamic and becomes partially reduced under WGS reaction conditions, forming metallic Cu nanoparticles on Fe3O4. Neither in situ IR not INS spectroscopy detect the presence of surface formate species during WGS. TPSR experiments demonstrate that the evolution of CO2 and H2 from the CO/H2O reactants follows different kinetics than the evolution of CO2 and H2 from HCOOH decomposition (molecule mimicking the associative mechanism). Steady-state isotopic transient kinetic analysis (SSITKA) (CO + H216O → CO + H218O) exhibited significant 16O/18O scrambling, characteristic of a redox mechanism. Computed activation energies for elementary steps for the redox and associative mechanism by density functional theory (DFT) simulations indicate that the redox mechanism is favored over the associative mechanism. The combined spectroscopic, computational, and kinetic evidence in the present study finally resolves the WGS reaction mechanism on the industrial-type high-temperature CuCrFeOx catalyst that is shown to proceed via the redox mechanism.

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    • SSITKA-reactor scheme, NAP-XPS for RWGS, INS spectra for formic acid, simulated vibrational modes of formic acid, DFT calculations, and SSITKA (PDF)

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