Liquid‐Mediated Treatment for Silanol Defects Healing and Sn Coordination Optimization in Sn‐Beta for Improved Catalytic Activity

Abstract The use of Sn‐beta zeolite as a heterogeneous catalyst for biomass conversion has garnered substantial attention over recent decades. This study investigates the effects of postsynthetic liquid‐mediated treatments on Sn‐beta zeolites, emphasizing the healing of silanol defects and optimization of Sn coordination to enhance catalytic performance. The treatments successfully reduced silanol concentrations, resulting in increased hydrophobicity, as confirmed by 29 Si MAS NMR and water vapor adsorption measurements. Further characterization using UV–vis spectroscopy and dynamic nuclear polarization (DNP)‐enhanced 119 Sn NMR spectroscopy demonstrated effective framework rearrangement and optimization of Sn coordination. Consequently, the treated samples exhibited significantly improved catalytic activity, with the top‐performing sample achieving a glucose conversion of 66% and a fructose selectivity of 71%, leading to a fructose yield of 47%. This study highlights framework rearrangement and silicate species migration as effective strategies for tailoring metal‐containing zeolite catalysts.