The invention discloses a method for preparing a molybdenum trioxide material with an orthorhombic phase single crystal nano belt structure. The method comprises the following steps: preparing molybdenum acid sol from ammonium heptamolybdate acidified by nitric acid; adding a template agent cetyltrimethylammonium bromide; and carrying out hydrothermal reaction, filtering, washing and drying so as to obtain the orthorhombic phase single crystal nano belt. In the method for preparing the molybdenum trioxide material with the orthorhombic phase single crystal nano belt structure, the ammonium heptamolybdate and the nitric acid are used as raw materials, the cetyltrimethylammonium bromide is used as the template agent, the acidification procedure is simple, process is easy to control, the reaction temperature is low, and the width and thickness of the product are small; the nano belt is of a single crystal structure and has good topography; and the preparation process is short in process flow period, the yield is high, the preparation equipment is simple and the cost is low. By using the method, the molybdenum trioxide material with the orthorhombic phase single crystal nano belt structure, which has width of 50-100nm, length of 1-10 mu m and thickness of 30-60nm, is obtained, and the powder grain size of the molybdenum trioxide nano belt is even.