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Quantifying Kinetically Relevant Species on Zr-SiO2 Materials for MPV Reduction.

Emily Chase1, Justin Notestein2

  • 1Department of Chemical and Biological Engineering, Northwestern University, 2145 Sheridan Rd, Evanston, IL, 60208, USA.

Chemphyschem : a European Journal of Chemical Physics and Physical Chemistry
|October 4, 2024
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Summary

Phosphonic acid titration quantifies zirconium (Zr) species on Zr-SiO2 catalysts for cyclohexanone hydrogenation. This method distinguishes between well-dispersed and supported ZrOx, improving catalyst characterization and regeneration understanding.

Keywords:
Heterogeneous catalysisSupported catalystsSurface chemistry

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Area of Science:

  • Heterogeneous catalysis
  • Materials science
  • Surface chemistry

Background:

  • Supported metal catalysts like Zr-SiO2 present challenges in distinguishing active site properties from environmental influences.
  • Accurate characterization of active sites is crucial for understanding and optimizing catalytic performance.

Purpose of the Study:

  • To quantitatively describe kinetically relevant zirconium (Zr) species on Zr-SiO2 catalysts using in-situ titration.
  • To elucidate the role of different Zr species in the Meerwein-Ponndorf-Verley (MPV) reduction of cyclohexanone.

Main Methods:

  • In-situ titration of Lewis acid sites with phosphonic acid to quantify Zr species.
  • Meerwein-Ponndorf-Verley (MPV) reduction of cyclohexanone using Zr-SiO2 catalysts.
  • Comparison of phosphonic acid titration with UV-vis spectroscopy for Zr dispersion analysis.

Main Results:

  • Catalytic activity for MPV reduction correlates with both titratable (well-dispersed Zr) and non-titratable (supported ZrOx) Zr species.
  • The fraction of well-dispersed Zr depends on surface grafting density, not the Zr precursor.
  • Phosphonic acid titration provides a more relevant and quantitative measure of Zr dispersion than UV-vis.

Conclusions:

  • Phosphonic acid titration is an effective method for quantitatively characterizing Zr dispersion and active sites on Zr-SiO2 catalysts.
  • This technique can monitor changes in the catalyst material during regeneration, offering insights into catalyst stability and reusability.