Mixed hydroxy-Al-Fe pillared montmorillonites with large basal spacing were successfully prepared through cation-exchanging of Na +- montmorillonite with mixed hydroxy-Al and hydroxy-Fe pillaring solutions made from hydrolysis of corresponding metal salts, followed by calcination to convert hydroxy-Al and hydroxy-Fe into intercalated polycations. According to XRD analysis, the basal spacing d（001） of pillared products dramatically enlarged from 12.7 *! in the Na-montmorillonite to 81 *! in the hydroxy-Fe -montmorillonite and 77.5 *! in mixed hydroxy-Al-Fe-montmorillonite. The N2 BET surface areas of the pillared montmorillonites also greatly increased to more than 200 m 2/g as compared to about 27 m 2/g for the Na-montmorillonite. IR analysis of hydroxy-Fe, and mixed hydroxy-Al-Fe pillared montmorillonites revealed a new absorption vibration at 1384 cm -1 wavelength. XRF elemental analysis data also showed a high content of Fe2O3 in the hydroxy-Fe pillared montmorillonite.
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