A new material of cotton fiber/Al(2)O(3)/SiPy(+)Cl(-), COTALPy, was prepared containing on its surface the polymer silsesquioxane 3-n-propylpyridinium chloride strongly adhered. This new composite based on long fibers of natural cotton is chemically stable and had its adsorption properties studied. The COTALPy presented a maximum ionic exchange capacity of 0.85 mmol g(-1) by potentiometric titulation. The adsorption isotherms of CuCl(2), ZnCl(2), CdCl(2), NiCl(2), and FeCl(2) in ethanol solutions were determined for each metal. The adsorption process was studied and data compared with the Langmuir model. The maximum adsorption capacities (in mmol g(-1)) were: CuCl(2) = 0.20, ZnCl(2) = 0.18, CdCl(2=) 0.35, NiCl(2) = 0.22, and FeCl(2) = 0.68. Real samples of fuel ethanol were eluted through a column containing the COTALPy, and it presented high-practical potential for removal of metallic ions. (C) 2011 Wiley Periodicals, Inc. J Appl Polym Sci 121: 1214-1219, 2011