A new spinel-style S 2 O 8 2À /ZnAl 2 O 4 solid acid catalyst was prepared by sol-gel method. The catalytic performance was evaluated by the esterification of n-butyl acetate. The structure, morphology and acidity of the samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Field emission scanning electron microscopy (FE-SEM), N 2 physisorption, X-ray photoelectron spectroscopy (XPS) and NH 3 temperature programmed desorption (NH 3 -TPD). The results showed that the catalytic performances were significantly affected by the calcination temperature. S 2 O 8 2À /ZnAl 2 O 4 -600 exhibited the highest catalytic activity of 91.7% under the optimum reaction conditions. The characterization showed that the mesoporous structure S 2 O 8 2À /ZnAl 2 O 4 -600 maintained the well crystallinity of spinel as well as the spinel-style carrier in the sulfidation and recycling. a From Debye-Scherrer equation using the width (at half maximum) of [3 1 1] line. b The synthesis condition: calcination temperature was 600 C; the concentration of (NH 4 ) 2 S 2 O 8 solution was 1.50 mol L À1 .This journal is