The invention discloses a preparation method of a titanium, aluminum, niobium, zirconium and molybdenum alloy, and belongs to the technical field of preparation of titanium alloys. The method comprises the following steps: weighing Ti, Al, Nb, Zr and Mo metal powder according to certain proportions, mixing the metal powder, performing intermittent dry type ball grinding through a ball grinder to obtain mixed powder, putting the obtained mixed powder into a graphite mold, prepressing the mixed powder, placing the graphite mold into a discharge plasma sintering furnace, applying axial pressure of 10 to 50 MPa for sintering under the condition that the vacuum degree is 2 to 8 Pa, heating the mixed powder in a multi-stage heating mode to 1,000 to 1,150 DEG C, preserving the heat for 3 to 8 min, cooling the mixture to room temperature, and demolding the mixture, thus obtaining the titanium, aluminum, niobium, zirconium and molybdenum alloy material. The titanium, aluminum, niobium, zirconium and molybdenum alloy prepared by the method disclosed by the invention has the advantages of uniform component, high compactness, high intensity, high plasticity and the like; and in addition, the method is easy to operate, short in time, energy-saving and environmentally friendly and has a good popularization value.