Abstract: Activated carbon fibers (ACFs) have high adsorption capacities and can be used in the treatment of benzene, while electrospun nanofibers are expected to be used as a filtration material. In this work, two hybrids of electrospun nanofibers and ACF cloth were prepared by electrospinning polyvinyl alcohol and polyacrylonitrile nanofibers into a phenolic resin-based ACF cloth. The filtration performance of the two hybrids was evaluated. Results indicate that there is a positive correlation between the filtration efficiency and the amount of electrospun nanofibers in the hybrid. The filtration efficiency increases with increasing air velocity, which is attributed to a piezoelectric effect introduced by the electrospun nanofibers. The hybrids have a good adsorption capacity for benzene, which suggests that the materials are promising for treating air pollution.