Synthesis of acid-base bifunctional mesoporous materials by oxidation and thermolysis |
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| Authors: | Xiaofang Yu Shujie Wu Jingqi Guan Qiubin Kan |
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| Affiliation: | a College of Chemistry, Jilin University, Jiefang Road 2519, Changchun 130023, PR China
b State Key Laboratory of Inoranic Synthesis and Preparative Chemistryg, College of Chemistry, Jilin University, Changchun 130012, PR China |
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| Abstract: | A novel and efficient method has been developed for the synthesis of acid-base bifunctional catalyst SO3H-MCM-41-NH2. This method was achieved by co-condensation of tetraethylorthosilicate (TEOS), 3-mercaptopropyltrimethoxysilane (MPTMS) and (3-triethoxysilylpropyl) carbamicacid-1-methylcyclohexylester (3TAME) in the presence of cetyltrimethylammonium bromide (CTAB), followed by oxidation and then thermolysis to generate acidic site and basic site. X-ray diffraction (XRD) and transmission electron micrographs (TEM) show that the resultant materials keep mesoporous structure. Thermogravimetric analysis (TGA), X-ray photoelectron spectra (XPS), back titration, solid-state 13C CP/MAS NMR and solid-state 29Si MAS NMR confirm that the organosiloxanes were condensed as a part of the silica framework. The bifunctional sample (SO3H-MCM-41-NH2) containing amine and sulfonic acids exhibits excellent acid-basic properties, which make it possess high activity in aldol condensation reaction between acetone and various aldehydes. |
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| Keywords: | A. Structural materials B. Chemical synthesis C. X-ray diffraction D. Catalytic properties |
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