A new type of cation-exchange nanocomposite membrane was prepared via in-situ formation of FeOOH nanoparticles in a blend containing sulfonated poly (2,6-dimethyl-1,4-phenylene oxide) and sulfonated polyvinylchloride by a simple one-step chemical method. Prepared nanocomposite membranes were characterized using Fourier transform infrared spectroscopy, scanning electron microscopy and X-ray diffraction. The SEM images showed uniform dispersion of FeOOH nanoparticles throughout the polymeric matrices. The effect of additive loading on physicochemical and electrochemical properties of prepared cation-exchange nanocomposite membranes was studied. Various characterizations showed that the incorporation of different amounts of FeOOH nanoparticles into the basic membrane structure had a significant influence on the membrane performance and could improve the electrochemical properties.