Wormhole Mesoporous Silica Framework with Enhanced Thiol Loading for Improved Hg²⁺ Sequestration

Thiol‐functionalized mesoporous silica and materials potentially dedicated to diverse applications of composite materials, metal colloids, and metal catalysts, etc. Here, we developed a new synthesis route for 3‐methacryloxypropyl trimethoxy silane (MPTMS) functionalized mesoporous silica (KIT‐6), achieving a 71.5 % enhancement in thiol functionalization on KIT‐6 surfaces. Characterization using XRD, TEM, BET, FTIR, Raman, 29 Si NMR, XPS, and ICP‐OES revealed structural and morphological features. XRD, TEM, and BET confirmed the three‐dimensional structural stabilization of mesoporous silica with ~4 nm pore diameter and a surface area of 1451 m 2 g −1 . FTIR, Raman, and 29 Si NMR studies established the mechanism of thiol functionalization, the formation of a new wormhole chain structural framework (WCSF), and stabilization through hydrogen bonding within the mesopores. The 29 Si NMR spectra showed characteristic peaks (T 3 , T 2 , Q 4 , Q 3 ) indicating self‐condensed functionalized thiols with siloxane networks. XPS analysis validated enhanced thiol functionalization, indicating a structurally homogeneous WCSF suitable for mercury adsorption. ICP‐OES measured a mercury adsorption capacity of 3199.6 mg g −1 for KIT‐6, with an Hg 2+ /S ratio of 1.8, corroborated by molecular structure and mechanism analysis. This innovative thiol functionalization approach enhances the efficacy of applications such as extracting Hg 2+ from contaminated sources.