Abstract: This paper introduces a simple and mild route to prepare Ni₂P catalysts. Ni₂P/MCM-41 catalysts were successfully prepared using MCM-41 as the support. The catalysts were characterized by H₂ temperature program reduction (H₂-TPR), X-ray diffraction (XRD), N₂-adsorption specific surface area measurements (BET), and X-ray photoelectron spectroscopy (XPS) analysis. The effects of initial Ni/P molar ratio on hydrodesulfurization (HDS) performance of catalysts and catalyst stability were studied with a lab-scale continuous flow type fixed-bed reactor systemusing a feed containing 1% dibenzothiophene (DBT) in decahydronaphthalene. The results indicated that a pure Ni₂P phase was obtained when the initial Ni/P molar ratios were 1/2 and 1/3. The catalyst prepared with initial Ni/P mol ratios of 1/2 exhibited the highest activity. At a reaction temperature of 340 ℃, a pressure of 3.0 MPa, a H₂/oil volume ratio of 500, and a weight hourly space velocity (WHSV) of 2.0 h^-1, the HDS conversion was close to 100%.