The hydrodeoxygenation (HDO) of the cyclic five-membered ester γ-valerolactone (GVL) was studied on a Ni2P/MCM-41 catalyst. The activation of the passivated catalyst in H2 was followed by in situ near-edge X-ray absorption spectroscopy (NEXAFS) which indicated reduction of the catalyst after 3 h at 550 °C. In situ infrared measurements under reactive H2 and inert N2 showed the presence of adsorbed GVL and pentanoic acid (PA) as the most abundant surface intermediates. The results supported a previous reaction network that showed that ring-opening of GVL to produce pentanoic acid was the rate-determining step. This was confirmed by transient infrared measurements which showed that the number of CH2 groups in the adsorbed species increased under H2 flow, consistent with PA formation but not an alkoxide. The results provide understanding of the key steps in the reaction mechanism.
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