By adopting hydrothermal method with cobalt chloride as cobalt source, terephthalic acid as ligand and ketjenblack 600 as conductive carbon carrier, Co3O4-C/KB was obtained by calcinating CoMOF precursor in an inert atmosphere. The dosage effects of cobalt chloride and terephthalic acid on catalytic performance were systematically studied. As the result suggested, the oxygen reduction catalytic performance of Co3O4-C/KB was greatly changed with different usages of cobalt chloride and terephthalic acid. When the amounts of cobalt chloride and terephthalic acid were 3 mmol and 2 mmol respectively, the catalytic performance was the best.