The catalytic activity of nickel and cobalt phosphides, with a metal loading of 5 wt.%, supported on silica was investigated in the hydrodeoxygenation reaction (HDO) of dibenzofuran (DBF) as a model oxygenated compound at different contact times, H2 pressures and H2/DBF molar ratios. The aim of the study was to understand the mechanism of the reaction and to study the impact of H2 pressure and H2/DBF molar ratio on the reaction. The catalysts were characterized by N2 adsorption–desorption isotherm measurement at −196 °C, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), CO chemisorption, NH3 Temperature-Programmed Desorption (NH3-TPD), IR spectroscopy and H2 Temperature-Programmed Desorption (H2-TPD). The prepared catalysts were tested in the HDO reaction of DBF in a continuous-flow fixed-bed stainless steel catalytic reactor at pressures ranging from 1–30 bar at 275 °C. The results obtained indicate that the Ni2P catalyst is more active than the CoP catalyst, converting more than 90% of DBF at the highest contact time into oxygen-free products. The activity of both catalysts increases with increased contact time. At low contact times, the intermediates tetrahydrodibenzofuran (THDBF) and hexahydrodibenzofuran (HHDBF) are observed as products, while an increment in the contact time led to the transformation of THDBF and HHDBF into O-free compounds, mainly bicyclohexane (BCH), indicating that the HDO of DBF follows the path: DBF → HHDBF → THDBF → 2-CHP → BCH. Further, both Ni2P and CoP catalysts are active at medium pressures with HDO degrees similar to those obtained at 30 bar. Ni2P is less affected by the changes in H2/DBF ratio than CoP and the catalysts are more active at high H2/DBF molar ratios
In
this work, La6–x
MoO12−δ (0 ≤ x ≤ 0.8) materials are investigated
as a new family of ceramic proton conductors. Different polymorphic
phases with rhombohedral and cubic structure are obtained, depending
on the cooling rate applied during the synthesis process. The materials
have been thoroughly characterized by different techniques, including
X-ray powder diffraction, transmission electron microscopy, and X-ray
photospectroscopy in order to fully understand the structural features
of the samples. Thermogravimetric analysis and impedance spectroscopy
in dry/wet gases (N2, O2, and 5% H2–Ar) confirmed the existence of proton conductivity at low
temperature. Under a reducing atmosphere, the materials are mixed
ionic-electronic conductors. The sample prepared at the fastest cooling
rate exhibits cubic structure and higher n-type electronic conductivity
compared to those prepared at a slower cooling rate with rhombohedral
structure.
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