The invention discloses a preparation method of a dual-functional electrocatalyst with a hollow polyhedral nano-cage microstructure doped with carbon material loading alloy, belonging to the field ofzinc Air Battery Catalyst Technology. The technical scheme of the invention mainly comprises the following steps of: adding an alcohol solution of cobalt nitrate and 2-Polyhedral ZIF- 67 precursor Wassynthesized by the reaction of methimidazole with ethanol at room temperature., and then that ZIF-67 precursor and that nickel source are heat and refluxed in an alcohol solvent to obtain hollow polyhedral nanocage product, and the obtained product is solvothermally react with the magnesium source and the boron source to obtain the target product. The catalyst of the invention introduces nickel and magnesium, so that the synergistic action between different components enhances the catalytic activity of the composite material, and the introduction of heteroatom boron effectively optimizes theelectronic structure of the material and improves the electrocatalytic performance. The catalyst of the invention and the preparation method thereof are prepared from zinc. The catalyst for air battery has a wide application prospect.