Mesoporous silica materials with an extremely high content of organic sulfonic groups and their comparable activities with that of concentrated sulfuric acid in catalytic esterification |
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Authors: | Feng Ye-Fei Yang Xiao-Yu Di Yan Du Yun-Chen Zhang Yong-Lai Xiao Feng-Shou |
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Institution: | College of Chemistry & State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, Jilin University, Changchun 130023, China. |
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Abstract: | Mesoporous silica materials (HS-JLU-20) with an extremely high content of mercaptopropyl groups have been successfully synthesized using fluorocarbon-hydrocarbon surfactant mixtures through a simple co-condensation approach of tetraethyl orthosilicate (TEOS) and (3-mercaptopropyl)trimethoxysilane (MPTS), which are characterized by X-ray diffraction (XRD), nitrogen adsorption and desorption isotherms, transmission electron microscopy (TEM), CHNS elemental analysis, thermogravimetry analysis (TGA), and (29)Si NMR spectroscopy. The results show that HS-JLU-20 samples with molar ratios of MPTS/(MPTS + TEOS) at 0.5-0.8 in the starting synthetic gels still show their mesostructures, while HS-SBA-15 with the molar ratio of MPTS/(MPTS + TEOS) at 0.50 completely loses its mesostructure in the absence of fluorocarbon surfactant. Possibly, fluorocarbon surfactant containing N(+) species with a positive charge could effectively interact with negatively charged mercapto groups in the synthesis of HS-JLU-20 materials, resulting in the formation of mesoporous silicas with good cross-linking of silica condensation even at an extremely high content of organic mercapto groups. More interestingly, after the treatment with hydrogen peroxide, HSO(3)-JLU-20 materials with an extremely high content of organic sulfonic groups exhibit comparable activity with liquid concentrated sulfuric acid in catalytic esterification of cyclohexanol with acetic acid. |
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