Synthesis of Nickel Phosphide Nanorods as Catalyst for the Hydrotreating of Methyl Oleate

Abstract

Arrays of nickel phosphide nanorods were successfully synthesized by nanocasting using mesostructured silica SBA-15 as a hard template (HT-Ni₂P). After temperature-programmed reduction of the phosphate precursor infiltrated within the pore walls of SBA-15, the unsupported material was obtained by removing the silica matrix with diluted HF. The pore channel of the SBA-15 template stabilizes the Ni₂P particles, preventing sintering after the high reduction temperature and shaping their elongated morphology. Moreover, HT-Ni₂P catalyst shows an improvement in the textural properties with a significantly higher surface area than the reference sample synthesized in the absence of template. X-ray diffraction revealed that the only crystalline phase present in this material was Ni₂P. On the other hand, transmission electron microscopy shows that the catalyst is mainly constituted by agglomerates of nanorods. Through EDX microanalysis the efficient removal of silicon was confirmed. Under hydrotreating conditions, nanorods of Ni₂P show a fourfold enhancement in the conversion of methyl oleate with respect to conventional Ni₂P synthesized in absence of hard template. Nevertheless, when these data are normalized to surface area, the specific activity of HT-Ni₂P nanorods is significantly lower than that of the conventionally prepared sample. Differences in selectivity were also observed as Ni₂P nanorods favored the decarboxylation reaction leading to a higher yield of n-heptadecane.