The invention discloses a defluorination material for a zinc sulfate solution in the zinc smelting process and a preparing method. The defluorination material is mainly prepared from oxide containing aluminum elements, rare earth elements, iron elements and magnesium elements. The preparing method includes the steps that aluminum hydroxide powder is placed into iron-magnesium salt mixed liquid, the mixture is stirred, alkaline is added to adjust pH, and the obtained mixture stands and is subjected to suction filtration; the obtained sample is added into a rare earth salt solution, the mixture is stirred again, alkaline is added to adjust pH, and the obtained mixture is subjected to suction filtration and dried; finally, the obtained product is placed into a high-temperature resistance furnace and roasted under the ventilation condition, and the defluorination material is obtained. The preparing method is simple, and the product is stable in nature, has high selective adsorbability and high adsorbing capacity for high-concentration fluorinion in the zinc sulfate solution and can be recycled with a simple method. When the material is applied to removing the high-concentration fluorinion in the zinc sulfate solution, the concentration of F in the solution can be effectively and rapidly reduced, the enterprise cost can be reduced, and environment pollution can be reduced. The material is suitable for large-scale industrial application.