By means of sol-gel synthesis with silicon and aluminium alkoxides, Triton X-114, and hydrothermal stabilization at various times and temperatures, were obtained aluminosilicates which have a porous structure (MSA) and are thermally stable and partially ordered. The as-synthesized MSA samples were subjected to hydrothermal treatment (HT) from 6 to 96 hours at 150 °C and at 110 to 175 °C for 6 hours to determine the effect of time and temperature on the structure of the final aluminosilicate. All the materials obtained are mesoporous, showing changes in their structural properties: surface area, pore diameter, and mesopore area and volume in direct relation to temperature and HT time