By the sol-gel method, there have been prepared different phosphate-phosphonates of zirconium-titanium with formula Zr(0.)7(5)Ti(0.25)(HPO4)(2-x)(C6H5PO3)(x,) X varies from 0.65 to 1.8. The intercalation of hydrolysed derivatives from aminopropyltriethoxysilane, NH2(CH2)(3)Si(OC2H5)(3), into these compounds gives rise, after heating at 773 K, to the formation of silica pillars between the layers, with basal spacing approximately 14.5 Angstrom, surface area up to 149 m(2)/g and high acidity (1.1-1.6 mmol NH3 g(-1) between 373-673 K).