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Catalytic reactor for operando spatially resolved structure-activity profiling using high-energy X-ray diffraction.

Birte Wollak1, Diego Espinoza1, Ann Christin Dippel2

  • 1Institute of Chemical Reaction Engineering (CRT), Hamburg University of Technology (TUHH), Eißendorfer Straße 38, 21073 Hamburg, Germany.

Journal of Synchrotron Radiation
|April 12, 2023
PubMed
Summary
This summary is machine-generated.

This study introduces an automated reactor for operando measurements, combining temperature, gas analysis, and X-ray diffraction (XRD) for heterogeneous catalysis. This enables detailed structure-activity profiling of catalysts under reaction conditions.

Keywords:
catalytic reactorsheterogeneous catalysisoperando profile measurementsstructure–activity relationships

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Area of Science:

  • Heterogeneous catalysis
  • Materials science
  • Chemical engineering

Background:

  • Operando measurements are crucial for understanding catalyst structure-activity relationships under reaction conditions.
  • Spatiially resolved studies using synchrotron light sources are advancing, but often lack integrated gas analysis.
  • Current methods typically analyze gas composition only at the reactor outlet, limiting in-situ understanding.

Purpose of the Study:

  • To develop and demonstrate a fully automated, integrated catalytic profile reactor setup.
  • To combine operando temperature, gas composition, and high-energy X-ray diffraction (XRD) measurements.
  • To enable spatially resolved structure-activity profiling for enhanced catalyst optimization.

Main Methods:

  • Utilized a profile reactor methodology, previously established for X-ray absorption spectroscopy, and extended it for operando XRD.
  • Integrated temperature and gas composition analysis with high-energy X-ray diffraction (XRD) measurements.
  • Employed the oxidative dehydrogenation of ethane (C2H6) to ethylene (C2H4) over MoO3/γ-Al2O3 as a model catalytic system.

Main Results:

  • Successfully demonstrated combined operando measurements of temperature, gas composition, and XRD profiles.
  • The integrated system allows for detailed, spatially resolved analysis of catalyst behavior during reactions.
  • The test reaction of C2H6 to C2H4 over MoO3/γ-Al2O3 provided valuable structure-activity data.

Conclusions:

  • The developed profile reactor is a versatile and accessible tool for combined operando structure-activity profiling.
  • This approach enables the use of multiple synchrotron-based characterization methods for catalyst research.
  • Facilitates time- and resource-efficient, knowledge-based optimization of diverse catalytic systems.