Sisal fiber, an agricultural resource abundantly available in china, has been used as raw material to prepare activated carbon with high surface area and huge pore volume by chemical activation with zinc chloride. The orthogonal test was designed to investigate the influence of zinc chloride concentration, impregnation ratio, activation temperature and activation time on preparation of activated carbon. Scanning electron micrograph, Thermo-gravimetric, N 2 -adsorption isotherm, mathematical models such as t-plot, H-K equation, D-R equation and BJH methods were used to characterize the properties of the prepared carbons and the activation mechanism was discussed. The results showed that ZnCl 2 changed the pyrolysis process of sisal fiber. Characteristics of activated carbon are: BET surface area was 1628 m 2 /g, total pore volume was 1.316 m 3 /g and ratio of mesopore volume to total pore volume up to 94.3%. These results suggest that sisal fiber is an attractive source to prepare mesoporous high-capacity activated carbon by chemical activation with zinc chloride.