Abstract: A solid acid catalyst SO₄^2-/ZrO₂ was prepared by coprecipitation-impregnation method. The effects of five different calcination temperatures on catalyst activity were investigated. The structure and physicochemical properties of the catalyst were analyzed by XRD, BET, TEM and FT-IR. The solid acid SZ-550 calcined at 550 ℃ for 3 h showed good catalytic performance. When it was used to catalyze the dehydration of fructose to prepare 5-HMF, the optimal reaction conditions were as follows: the reaction temperature of 120 ℃, the reaction time of 90 min, and the amount of catalyst of 30 mg with dimethyl sulfoxide(DMSO) as the reaction solvent. Under these conditions, the conversion rate of fructose was 99.91%, and the yield of 5-HMF was 76.01%. XRD results showed that the solid acid SO₄^2-/ZrO₂ had obvious tetragonal ZrO₂ structure, which was one of the reasons for its high catalytic activity.