Résumé
Abstract Despite previous explorations of reaction conditions (temperature, time, solvent), the construction mechanism of mesoporous titania‐bisphosphonate hybrids remains under‐researched. This study provides a further understanding of the construction mechanism of these materials by investigating the formation of key chemical bonds Ti─OAc (acetoxylation), Ti─O─Ti (TiO 2 formation), and Ti─O─P (bisphosphonate cross‐linking). It is found that the competitive reactions between Ti─O─Ti and Ti─O─P significantly influence the specific surface areas, average pore sizes, crystallite sizes, and the degree of condensation. In addition, the Ac 2 O/Ti molar ratio plays a crucial role in determining the texture and composition of the resulting hybrids. This study will guide the synthesis strategy and regulate the texture and composition of these new mesoporous nonsiliceous materials with great application potential.