The invention belongs to the field of electro-catalysis, and relates to a monatomic metal-molybdenum sulfide nano-composite as well as a preparation method and an application thereof. The preparation method comprises the following specific steps: modifying the surface of a glassy carbon electrode with a molybdenum sulfide suspension, carrying out underpotential deposition in an inert gas saturated copper sulfate precursor solution, and then transferring into an inert gas saturated potassium chloroplatinite solution to carry out chemical replacement, thereby obtaining the monatomic platinum-molybdenum sulfide nanocomposite. In addition, the invention provides other metal monatomic (palladium, lead, tin and bismuth)-molybdenum sulfide nano-composites prepared by adopting the preparation method. In addition, compared with a commercial platinum/carbon catalyst, the monatomic platinum-molybdenum sulfide nano-composite is higher in hydrogen precipitation catalysis reaction activity, and the preparation method disclosed by the invention is normal in temperature and pressure, controllable in operation, simple and easy to implement, and can be widely applied to various heterogeneous catalysis reactions.