The purpose of this work is to study the adsorption and desorption characteristics of acetone vapor and toluene vapor from adsorption tower in the VOCs recovery device. The six kinds of activated carbon with different pore structures were used and the adsorption and desorption characteristics were compared according to pore structure, desorption temperature, and adsorption method, respectively. Adsorption capacity of acetone vapor and toluene vapor by batch method was higher than that by dynamic method. Especially, activated carbon with medium-sized or large pores had more difference in adsorption capacity according to adsorption methods as a result of gradually condensation of vapors on relatively mesopore and large pores. Activated carbons with relatively large pores and relatively small saturated adsorption capacity had excellent desorption ability.