Based on the composite fibers made from polyvinylchloride (PVC) and polystyrene (PS), the composite fibers obtained were further crosslinked and sulphonated with 50% oleum to produce the acidic cation ion exchange fibers. The optimal technology of the fibers obtained were discussed, the structures of the fibers thus obtained were investigated by using Fourier transform infrared (FTIR) spec trophotometry, thermogravimetry analysis (TG), differential thermogravimetry analysis (DTG), and scaning electron microscope (SEM) etc. Their properties were measured using chemical titration, filament mightiness instrument, etc. The absorption kinetics and the main factors affecting absorption capacity on aniline were studied, and their regenerating properties were probed. The results indicated that the cation exchange fibers with better mechanical property and higher exchange capability were obtained. The fibers had bigger hydrophilicity, better ability of acid, and alkali corrosion resistance, so they had better practical application value. This type of ion exchange fibers had faster absorption property and better working stability to aniline and could be used repeatedly, so they were applied for treatment of waste water containing aniline with a promising prospect. (C) 2010 Wiley Periodicals, Inc. J Appl Polym Sci 117: 1914-1923, 2010