To prepare good polymeric materials for the preparation of the polyion complex membranes useful for water-alcohol separation, polycations were synthesized by the quaternization polymerization of 1,3-di(4-pyridyl)propane with dibromoalkanes or with 1,8-bis(p-toluenesulfonyl)octane. The polycations were characterized by FTIR spectroscopy, viscometery, DSC, and X-ray diffractometry. The polycations were in molecular weight ranges good enough to be used as membrane materials. The polycations were very hygroscopic and easily soluble in highly polar solvents such as water and these properties might be good for the membrane materials. The thermal properties and X-ray diffraction patterns of these polycations suggested that the polycations were semicrystalline and difficult to form crystals by melt crystallization.