A novel laboratory setup for combined operando X-ray diffraction and Raman spectroscopy of catalytic solids with online product analysis by gas chromatography has been developed. The setup can be used with a laboratory-based X-ray source, which results in important advantages in terms of time-on-stream that can be measured, compared to synchrotron-based experiments as it makes it possible to run long-term deactivation experiments for days or even weeks. The data quality was much improved by the use of a relatively high-energy MoKa radiation instead of the more conventional CuKa radiation. We have applied the instrument to study the long-term deactivation of Co/TiO2 Fischer–Tropsch synthesis catalysts. No sign of Co sintering or bulk oxidation<br/>was found during the experiments. However, part of the metallic Co was converted into cobalt carbide at elevated pressures. Furthermore, graphitic-like coke species are clearly formed under Fischer-Tropsch Synthesis conditions.

Combined operando x-ray diffraction/Raman spectroscopy of catalytic solids in the laboratory: The Fischer–Tropsch synthesis catalyst showcase

253rd National Meeting (2017)

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