The catalyst molybdenum dibutyl dithiocarbamate was synthesized by one-pot method.The optimum ratio of experimental raw materials and technological parameters were studied, and the structure was characterized by FTIR, ¹H NMR and elemental analysis.The result showed that the best synthetic conditions were that molybdenum trioxide∶sodium sulfide∶sulfuric acid∶sodium dibutyl dithiocarbamate were 1∶1.4∶1.6∶1,the reaction temperature was 110℃ and reaction time was 4 h.