The invention belongs to the technical field of material preparation, in particular to a preparation method of a super-hydrophobic/oleophylic Ni-Cu composite coating mesh film for oil and water separation. The preparation method is characterized in that by using an electrochemical deposition process, a Ni-Cu composite coating in a micro nano coarse structure is formed on the surface of a substrate of a metal mesh, then surface modification is carried out on the Ni-Cu composite coating by using low surface energy material modification liquid, finally the Ni-Cu composite coating mesh film having a super-hydrophobic/oleophylic function is prepared on the surface of the metal mesh. Oil can infiltrate and penetrate the surface of the Ni-Cu composite coating rapidly, and water is intercepted to be left on the surface of the Ni-Cu composite coating, so that the oil and water separation is realized. The preparation method of the super-hydrophobic/oleophylic Ni-Cu composite coating mesh film has the advantages that a technology is simple and feasible, the Ni-Cu composite coating is stable in structure and the oil and water separation efficiency is high. The preparation method can be widely applied to separation of oil and water mixtures.