Preparation　methods　are　essential　for　the　synthesis　of　materials　with　diverse　structures,　which　may　lead　to　the　different　physicochemical　properties.　The　activities　of　catalysts　for　volatile　organic　compounds　(VOCs)　combustion　can　be　improved　by　optimizing　the　preparation　methods.　In　this　paper,　a　novel　ammonium　bicarbonate　pyrolysis　method　is　successfully　applied　to　prepare　Co3O4　catalyst　(Co3O4-A),　which　is　not　only　facile　in　preparation,　but　also　superior　to　the　Co3O4　catalysts　prepared　by　the　hydrothermal,　sol-gel,　MOFs　pyrolysis　and　carbonate　pyrolysis　method　in　the　performance　of　chlorobenzene　catalytic　oxidation　with　90%　conversion　and　mineralization　temperature　at　310　and　325　degrees　C,　respectively　(1000　ppm　CB,　Air,　WHSV　=60,000　mL.g(-1).　h(-1)).　Furthermore,　Co3O4-A　catalyst　can　maintain　high　catalytic　activity　for　a　long　time,　and　has　high　tolerance　to　water　vapor,　which　indicates　Co3O4-A　catalyst　has　a　good　potential　application　value　in　catalytic　combustion　of　chlorobenzene.