The invention discloses a preparation method and application of a cyanuro metal-organic framework/Ni composite material based on catalyst electrolytic water oxygen evolution and belongs to the technical field of nanometer catalysis, nanometer materials and metal-organic frameworks. The preparation method comprises the following main steps: blending a cobalt nitrate aqueous solution and a cyanuricacid suspension, coating blended liquid on an activated nickel mesh, heating to 300-400 DEG C in an air atmosphere and successfully preparing a hybrid material of which a triazinyl metal-organic framework nanometer crystal is loaded on the activated nickel mesh. The material is low in raw material cost, simple in preparation process and low in reaction energy consumption and has industrial application prospect. A catalyst has efficient electrolytic water oxygen evolution activity and electrochemical stability.