In this paper, bulk and MCM-41-supported Ni2P catalysts were synthesized by the one-step direct reduction of metal phosphate precursors. The role of cations and anions in the synthesis of Ni2P was studied. Catalytic properties for the hydrodeoxygenation (HDO) of methyl palmitate were first investigated in a continuous-flow fixed-bed microreactor. The resulting catalysts were characterized using XRD, TEM, BET, XPS, and carbon monoxide chemisorption. Results indicated that Ni2P can be synthesized at 600 degrees C from its phosphate precursors with a mole ratio of Ni/P = 211. Based on the analytical result of GC-MS, we propose a possible HDO reaction mechanism for the HDO of methyl palmitate on MCM-41-supported nickel phosphide catalysts. (C) 2015 Elsevier B.V. All rights reserved.