Walnut peel as raw material, zinc chloride was used as activating agent for preparation walnut peel activated carbon in the muffle furnace in this experiment, using orthogonal design. Yield, the specific surface area and iodine number of walnut peel activated carbon were determined at all designed experimental conditions and the optimum technological condition of preparation was obtained. By analysis of aperture, infrared spectra and the content of acidic group in surface with Boehm, walnut peel activated carbon of prepared at the optimum condition was characterized. The results showed the optimum technological parameters of preparation: activation temperature (600 ℃), activation time (1h), the concentration of zinc chloride (50%), the particle size( 60 mesh). The specific surface area of walnut peel activated carbon obtained at optimum condition was mounting to 1 258.05 m2·g-1 , the ratio of medium porous 32.18%. Therefore, walnut peel can be used in the preparation of the high-quality activated carbon of large surface area. Agricultural wastes, as walnut peel, not only were implemented recycle, but also didn’t make any pollution. Meanwhile, a cheap adsorbent was provided and it was of great significance to open a new source of activated carbon.