Phosphorylation of Pluronic‐Filled Silica Mesostructure as a Circular Route for Surfactant Removal and Recycling

Abstract Expanding the pore size of mesostructured silica above 2 nm has constituted a breakthrough in materials science. Unfortunately, the lack of recyclability of the costly used surfactant impedes large‐scale implementation of these precisely calibrated nanoreactors. Unlike the commonly used template‐destructive, energy‐intensive protocols, we herein report that gentle treatment of the as‐prepared silica‐surfactant composite with phosphoryl chloride allows for performing two goals in a single action. Concomitant to surface phosphorylation, the released hydrochloric acid disturbs the hydrogen‐bonding of the Pluronic to the silica network, triggering, as a consequence, its easy escape from the mesostructure. The presence of the Pluronic limits oligomerization of the phosphorus reagent inside of the mesostructure, thereby providing better site isolation for acid and cooperative acid‐base functionalities compared to the phosphorylation undertaken through two‐step implying conventional Soxhlet extraction and post‐grafting, as substantiated by gas adsorption and catalytic tests. Besides, this nondestructive approach offers additional assets for template recovery and further recycling.