Abstract--Beidellite was synthesized hydrothermally from a noncrystalline gel at 320~ and 130 bar pressure. The beidellitic character of the product was verified by infrared spectroscopy on the NH4 § exchanged form. Intercalation was achieved with hydroxy-aluminum solutions having different OH/A1 molar ratios. The solutions were investigated by several methods, including 27A1 nuclear magnetic resonance. Essentially, two Al species were detected: monomeric A1 and a polymerized form containing A1 in four-fold coordination. This latter species was found to be selectively fixed in the interlamellar region, which resulted in a stable spacing of 18 ,~ at 110~ and 16.2 ~ at 700~ The pillared beidellites had specific surface areas of > 300 m2/g, mainly due to micropores. Both Br6nsted and Lewis acid sites were evidenced by infrared spectroscopy using pyridine as a probe molecule.