Smectite-type clays from the state of Pará, Brazil, were characterized by XRD, 27Al MAS NMR, FTIR and textural analysis by nitrogen adsorpition-desorption isotherms. In the production of pillared clays, the Al13 ion (keggin's ion) was used. This ion was obtained by the reaction of AlCl36H2O/NaOH solutions with OH/Al=2 molar ratio and with Al/clay ratios of 5, 10, 15, 20, 25 meq/g of clay, intercalated at 25 ºC during 3 h and calcined at 450 ºC (adequate temperature for calcination). The results showed that the pillarization process increased the basal spaces of the natural clay from 14.02 to 18.84 Å and the surface area from 44.30 to 198.03 m2/g (Al/g of clay = 25 meq/g of clay, pH=4). Materials prepared with different Al/g clay ratio showed the maximum Al incorporation for Al/g of clay = 25 meq/g of clay. The thermal stability of the natural clay was improved by the pillaring procedure.
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