Abstract: A stable porous system consisting of montmorillonite cross-linked by Al-hydroxide oligomers was synthesized by reacting at room temperature an aqueous solution of such oligomers with a unit-layer dispersion of montmorillonite. The resulting cross-linked montmorillonite (Al-CLM) is a nonswelling material, showing basal spacings of 14.4 to 18.8 Å after air drying and between 14.2 to 18.0 Å after treatment at 110°C. The basal spacing is found to depend on the age and OH/Al ratio of the Al-hydroxide solution, as well as on the relative amounts of the two reactants. A specific surface area of 160 m2/g and a diffraction pattern with a dominant basal spacing of 17.5 Å is obtained by using Al-hydroxide with OH/Al = 1.85, aged for at least 5 days, and by applying an Al/montmorillonite ratio greater than 1.5 in the cross-linking process. The basal spacing of Al-CLM remains essentially unchanged after heating at 220°C, while the specific surface area is not affected by heat treatment up to 480°C.
Two possible configurations of Al-hydroxide oligomers, homogeneously distributed between parallel montmorillonite unit-layers, were considered in order to account for the basal spacing of 17.5–18.8 Å, viz. (a) stacking of two oligomeric ring units in parallel orientation relative to the clay lamellae and (b) perpendicular orientation of individual oligomeric units.