Activated carbon fibers (ACFs) were treated by electroless plating of CuO to improve their removal performance for volatile organic compounds (VOCs). The properties of these samples(CuO@ACFs) were evaluated by X-ray photoelectron spectroscopy (XPS), BET and N2O chemisorption to determine the area and dispersion of metallic CuO. The removal efficiency for benzene was investigated by gas chromatography (GC). The breakthrough time of CuO@ACFs increased by approximately 120% compared to that of untreated ACFs at benzene of 100 ppm. CuO@ACFs removed 100% of the benzene in 20 h, indicating this material can be used as a removal technology for VOCs.