Solid acid Zr(SO4)2/TiO2 catalyst has highly catalytic activity, and has non-corrosiveness to equipment. It is separated from production expediently. As the above advantages, the influence of Zr(SO4)2 loading amount, calcination temperature, and calcination time on the solid acid Zr(SO4)2/TiO2 catalyst preparation process is discussed. The experimental condition is optimized by orthogonal test, the result indicate that Zr(SO4)2 load is 65%, calcination temperature is 430°C, and calcination time is 2.5 h. Solid acid catalyst Zr(SO4)2/TiO2 is analyzed and characterized by FT-IR, XRD and SEM. The results will provide the experimental condition for enlarging experimental study.