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Cobaltosic oxide has been used as catalysts in dehydrogenation for tail chlorine due to the advantages of low price and security. The Co3O4/ZSM-5 was synthesized by the volume impregnation method. The catalytic dehydrogenation performance of Co3O4/ZSM-5 was investigated, the catalytic reaction of hydrogen with oxygen and chlorine was carried out in a fixed-bed, and the mixed reactant gases were prepared according to the composition and content of tail chlorine in industry: Cl2(65%-80%), N2(6-16%), O2(8%-10%) and H2(1.5%-4%). The catalytic efficiency and stability of Co3O4/ZSM-5 in dehydrogenation for tail chlorine were better than that of Co3O4. After the calcination on 300°C, the Co3O4/ZSM-5 with 1 %wt. Co3O4 shown excellent catalytic performance at 50°C, and the average conversion of hydrogen can reach up to 99.59%.