The one-step synthesis of methyl isobutyl ketone from acetone (MIBK) and H2 in liquid phase was studied over Ni-zirconia catalyst prepared by precipitation. The performances of Ni/ZrO2 catalysts were evaluated by the conversion of acetone and the selectivity of MIBK. The effect of different preparation conditions such as aging temperature, calcination temperature, nickel content and reduction temperature was investigated. The results showed that high acetone conversions of up to 33% and MIBK selectivities of up to 85% were recorded at a nickel content of 13.0 wt % and the reduction temperature of 400°C.