Abstract: The Ni₂P/MCM-41 catalysts was prepared at low reduction temperature by temperature programmed reduction. The catalyst was characterized by H₂-TPR, TG-DTG, XRD, BET, and XPS. The effects of reduction temperature on formation of the active Ni₂P phase and HDS performance of the catalysts were studied. The results showed that a pure Ni₂P phase can be obtained with samples reduced at low reduction temperature range of 210~390 ℃. The catalyst obtained at reduction temperature of 390 ℃ exhibited the highest HDS activity. At a reaction temperature of 340 ℃, pressure of 3.0 MPa, H₂/oil volume ratio of 500, and weight hourly space velocity (WHSV) of 2.0 h^-1, the DBT HDS conversion reached to 99.0%.