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Influence of framework Al density in chabazite zeolites on copper ion mobility and reactivity during NOx selective catalytic reduction with NH3

Nature Catalysis volume 6, pages 276–285 (2023)Cite this article

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Abstract

Cu zeolites catalyse low-temperature (<523 K) selective catalytic reduction (SCR) of nitrogen oxides (NOx) via a redox cycle involving dynamic interconversion between NH3-solvated mononuclear CuI and binuclear CuII complexes. CuI oxidation requires the pairing of two mobilized CuI(NH3)2 complexes to form binuclear intermediates, implying that CuI oxidation kinetics should depend on framework Al density, given that Cu ions are ionically tethered to anionic charges at Al sites in zeolite lattices. Here we combine statistical simulations, steady-state kinetics and operando X-ray absorption spectroscopy to interrogate Cu–chabazite (Cu–CHA) zeolites of varying framework Al density (0.2–1.7 Al centres per cha cage). Increasing the Al density leads to systematic increases in both the fraction of CuI ions that are SCR active (that is, O2 oxidizable) and CuI oxidation rate constants (per Cu), revealing insights into how anionic Al centres in zeolite frameworks regulate the mobility of ionically tethered Cu cations and their dynamic reactivity during low-temperature NOx SCR.

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Fig. 1: Schematics of the pairing of CuI cations ionically tethered to framework Al.
Fig. 2: SCR rates (per Cu site) as a function of O2 pressure.
Fig. 3: Steady-state CuI fractions measured by operando XAS.
Fig. 4: CuI oxidation kinetics and transient XAS (473 K) on Cu–CHA materials of varying composition.
Fig. 5: Statistically predicted fractions of pairable Cu sites versus Cu and Al density as a function of the number of remote cha cages separating Cu site pairs.
Fig. 6: CuII reduction kinetics and transient XAS (473 K) on Cu–CHA materials of varying composition.

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Data availability

Experimental raw data underlying all of the results and conclusions of this work are available upon request to the corresponding author. Initial and final configurations for the calculations can be found at https://doi.org/10.5281/zenodo.7604048.

Code availability

Simulation codes used in this work have been uploaded to a Zenodo repository at https://doi.org/10.5281/zenodo.7604048.

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Acknowledgements

We acknowledge financial support provided by the National Science Foundation Designing Materials to Revolutionize and Engineer our Future programme under award number 1922173-CBET (received by R.G. and W.F.S.). S.H.K. acknowledges funding via the Henson Postdoctoral Fellowship from the Charles D. Davidson School of Chemical Engineering at Purdue University. Use of the Advanced Photon Source is supported by the US Department of Energy Office of Science and Office of Basic Energy Sciences under contract number DE-AC02-06CH11357. Materials Research Collaborative Access Team operations and beamline 10-ID are supported by the Department of Energy and Materials Research Collaborative Access Team member institutions. We thank C. Paolucci (Virginia) for helpful technical discussions. We thank SACHEM for providing the organic structure-directing agent used to synthesize SSZ-13. We thank J. Harwood (Purdue Interdepartmental NMR Facility) for assistance with collecting NMR spectra.

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  1. Charles D. Davidson School of Chemical Engineering, Purdue University, West Lafayette, IN, USA

    Siddarth H. Krishna, Casey B. Jones, David P. Dean, Jeffrey T. Miller & Rajamani Gounder

  2. Department of Chemical and Biomolecular Engineering, University of Notre Dame, Notre Dame, IN, USA

    Anshuman Goswami & William F. Schneider

  3. Department of Chemistry and Biochemistry, University of Notre Dame, Notre Dame, IN, USA

    Yujia Wang

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Contributions

S.H.K., C.B.J. and R.G. acquired and analysed the kinetic data in this work. S.H.K., C.B.J., D.P.D., J.T.M. and R.G. acquired and analysed the spectroscopic data in this work. A.G., Y.W. and W.F.S. acquired and analysed the computational data in this work. S.H.K. and R.G. led the writing of the manuscript. All authors assisted in writing and revision of the manuscript.

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Correspondence to Rajamani Gounder.

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Krishna, S.H., Goswami, A., Wang, Y. et al. Influence of framework Al density in chabazite zeolites on copper ion mobility and reactivity during NOx selective catalytic reduction with NH3. Nat Catal 6, 276–285 (2023). https://doi.org/10.1038/s41929-023-00932-5

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