A novel binary promoter NiCoMo layered molybdate was synthesized as potential hydrodesulfurization (HDS) catalyst precursor by chemical precipitation from a solution containing nickel nitrate, cobalt nitrate and ammonium heptamolybdate. NiMo and CoMo layered molybdates were also prepared for comparison by the same method. The NiCoMo, NiMo and CoMo layered molybdates were characterized by means of N-2 physisorption, XRD, FT-IR, TG-DSC-MS, SEM and HRTEM, and catalytic properties were evaluated in the continuous HDS of dibenzothiophene (DBT) and straight-run gas oil. The characterization results indicated the three precursors were endowed with the same structure of ammonium nickel molybdate, and catalytic results showed that the NiCoMo catalyst exhibited higher HDS activity towards DBT and straight-run gas oil, which might be more attractive for industrial applications.