A kind of nanosized sulfated zirconia was prepared by a hydrothermal method, and full characterized by XRD, TEM, BET, TGA, and FTIR. Its catalytic activity was evaluated in the esterification reactions, including the testing of the catalytic reusability and the optimization of reaction conditions. The obtained catalyst was revealed to be highly efficient solid catalyst for the esterification of acetic acid with n-butanol, presenting the advantages of high conversion and selectivity, easy recovery, and steady reusability.