Aluminium pillared clays (PILCs) from three different starting materials namely two Portuguese clays from Benavila (Alentejo) and Porto Santo (Madeira archipelago) and a Wyoming SPV-200 clay were obtained. A characterisation of the textural and some surface chemistry properties of the starting materials and PILCs was made using the adsorption of different probe molecules (water, ethylene glycol, nitrogen, n-hexane, cyclohexane, triethylamine) and also by other routine techniques. The adsorption of probe molecules was also employed to characterise the microporosity of the obtained PILCs. The effect of freeze-drying on PILCs texture was also discussed and related with the size of the clay particles.