Abstract: The adsorption and regeneration of toluene by different kinds of activated carbon were studied, and the effects of temperature and physical structure of activated carbon were analyzed. The results of scanning electron microscope(SEM), measurement of specific surface area and pore volume, and toluene adsorption and desorption(toluene-TPD)revealed that the coconut shell activated carbon and tar activated carbon had better adsorption capacity and strength than other activated carbons, caused by the large micropore volume. The adsorption properties of toluene showed that the adsorption and diffusion of toluene in micropores require an activation temperature. The coconut shell activated carbon had the best adsorption performance, and after 10 repeated regeneration experiments, the saturation adsorption capacity could still reach 90% or more.