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A large fixed bed reactor for MRI operando experiments at elevated temperature and pressure.

Harm Ridder1, Christoph Sinn1, Georg R Pesch1

  • 1Chemical Process Engineering (CVT), Faculty of Production Engineering (FB 4), University of Bremen, Leobener Straße 6, 28359 Bremen, Germany.

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Summary

Researchers developed a new NMR-compatible reactor for studying gas-phase reactions under high temperature and pressure. This reactor enables operando monitoring of reactions like CO2 methanation, overcoming previous limitations.

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Area of Science:

  • Chemical Engineering
  • Spectroscopy
  • Materials Science

Background:

  • In situ nuclear magnetic resonance (NMR) can monitor gas-phase reactions in opaque media.
  • Existing NMR methods face challenges with temperature and pressure constraints for heterogeneous catalysis.
  • Monitoring catalytic reactions under realistic conditions is crucial for process optimization.

Purpose of the Study:

  • To design and test an NMR-compatible reactor for high-temperature and high-pressure applications.
  • To enable operando studies of heterogeneously catalyzed gas-phase reactions using NMR.
  • To overcome limitations of current NMR techniques in studying challenging chemical environments.

Main Methods:

  • Designed and manufactured a novel NMR-compatible reactor capable of withstanding extreme conditions.
  • Conducted rigorous temperature and pressure tests to validate reactor performance.
  • Utilized a 3D magnetic resonance spectroscopic imaging sequence for operando measurements.

Main Results:

  • The reactor successfully withstood pressures up to 28 bars at room temperature and temperatures exceeding 400°C.
  • Minimal magnetic shielding was observed, ensuring high-quality NMR data acquisition.
  • Successfully demonstrated applicability by performing operando measurements of the CO2 methanation reaction.

Conclusions:

  • The developed NMR-compatible reactor effectively enables in situ monitoring of gas-phase reactions under demanding conditions.
  • This advancement opens new possibilities for studying heterogeneously catalyzed reactions operando.
  • The reactor's design is adaptable for various chemical reactions and other challenging NMR investigations.