Abstract: Activated carbon fibers were prepared from general purpose pitch-based carbon fibers with different steam dosage and activation time by cobalt catalytic activation. Dynamic adsorption of toluene on the resultant activated carbon fibers as well as the regeneration properties were studied. The prepared activated carbon fibers are very promising material for toluene adsorption and the adsorption capacity depends on the specific surface area, the pore size and distribution. Saturated adsorption capacity of toluene on the activated carbon fibers reaches 1250mg/g and remains 900mg/g after 20 regeneration cycles of adsorption-desorption.