A novel porous silica matrix has been prepared from Pyrex glass, using hydrothermal treatment under saturated‐steam condition. This process makes it possible to obtain, in one step, a silica support formed of a homogeneously distributed and interconnected macropore microstructure. The new matrix contains silanol groups that can be used in reactions of surface modification to provide a hybrid material and a selective macrofiltration membrane, and also it can improve chemical inertness. The porous matrix is noncrystalline as obtained and, after thermal treatment at temperatures higher than 950°C, exhibits an X‐ray pattern characteristic of α‐cristobalite and low volume contraction. The present samples were characterized by scanning electron microscopy, mercury intrusion porosimetry, nitrogen adsorption‐desorption isotherms, infrared spectroscopy, X‐ray powder diffractometry, atomic absorption, and high‐resolution solid‐state nuclear magnetic resonance. The results present a new way of producing a macroporous silica matrix.

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