The cellulose acetate (CA) membrane prepared via electrospun was innovatively utilized as fiber-adsorbent for the separation of aqueous triclson (TCS). It was found that the presence of the room temperature ionic liquid (RTIL) in the precursor amplified electric force toward the CA-solution, thereby benefiting the formation of CA fibers. The as-spun CA fibers exhibit excellent adsorptive performance toward TCS, with fast adsorption kinetics, and the maximum adsorption capacity achieved to 797.7 mg g(-1), which established much better performance in contrast to conventional adsorbents. We proposed that the adsorption of TCS onto CA fibers was primarily facilitated by the hydrogen bonding between the abundant carbonyl, hydroxyl groups of CA surface, and the hydrogen atoms of phenol functional groups in TCS molecular.