The invention relates to a pretreatment method of zircon powder. The pretreatment method comprises: performing heating and pressurizing treatments on zircon powder, wherein the temperature of the heating treatment is 350-400 DEG C, and the pressure of the pressurizing treatment is 0.4-0.6MPa; then performing acid cleaning on the zircon powder after the heating and pressurizing treatments until the zircon powder is neutral; and performing drying at first and then performing grinding on the zircon powder after acid cleaning to obtain zircon powder after pretreatment. The invention also relates to a preparation method of a vanadium-zirconium blue material. The pretreatment method of the zircon powder, provided by the invention, can significantly reduce reaction impurities and significantly improve the reactivity of the zircon powder; and the preparation method of the vanadium-zirconium blue material, provided by the invention, has the advantages of improving the productive rate and being simple and easy to control.