Abstract: The nanometer solid superacid SO42-/ZrO2 was used as catalyst for acetylating of terpineol. By orthogonal tests, the optimum technology condition was obtained. The optimum temperature and time were (50℃) and 5 h, respectively, catalyst quantity was 3%, the ratio between acetic anhydride and terpineol was (1.3:1.) Under this condition, the conversion ratio of terpineol was 100%, the total ester was 92.79%, the content of lemonene with carene as main byproducts was 5.27% among products. The activity and selectivity of the nanometer solid superacid SO42-/ZrO2 were higher than those of ordinary solid superacid SO42-/ZrO2. The nanometer solid superacid SO42-/ZrO2 could be repeatedly used for 5 times.