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This paper presents a simple technique for preparation of alumina supported nickel phosphide by the thermal treatment of beehmite and nickel hypophosphite in a flowing N2 at relatively low temperau- re (473 K). The resulting catalysts were characterized by X-ray diffraction (XBD) and transmission electron mieroscopy(TEM), indicating that Ni2P nanopaxticles may be well-dispersed in the alumina supported Ni2P catalysts with modest Ni2P loading. Therefore, this method provides a new effective route for the preparation of alumina supported Ni2P catalysts.