| Summary: | This study describes the phenomena involved during the regeneration of an aged industrial hydrodesulfurization catalyst (CoMoP/Al<sub>2</sub>O<sub>3</sub>) using a non-thermal plasma at a low temperature (200 °C). The changes occurring during regeneration were studied by characterizing spent, partially, and fully regenerated catalysts by XRD, Raman, TEM spectroscopy, and the coke deposited on the catalyst surface by Laser desorption/ionization time-of-flight mass spectrometry (LDI TOF/MS). The coke is a mixture of several polycyclic molecules, the heaviest with a coronene backbone, containing up to seven sulfur atoms. This kinetic study shows that the oxidation rate depends on the nature of the coke. Hence, explaining the formation of VOCs from heavy polycyclic carbon molecules without complete oxidation to CO<sub>2</sub>. However, XRD and Raman spectroscopies evidence CoMoO<sub>4</sub> formation after a long treatment time, indicating hot spots during the regeneration.
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