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《Chinese Journal of Catalysis》 2006-11
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Preparation of Solid Acid SO~(2-)_4/SiO_2-TiO_2 and Its Catalytic Activity for Esterification

ZHANG Qi~ 1,2 , CHANG Jie~1, WANG Tiejun~ 1* , XU Ying~1(1 Guangzhou Institute of Energy Conversion, The Chinese Academy of Sciences, Guangzhou 510640, Guangdong, China; 2 Department of Thermal Science and Energy Engineering, University of Science and Technology of China, Hefei 230027, Anhui, China)  
Solid acid catalysts SO~ 2- _4/SiO_2-TiO_2 with different SiO_2/TiO_2 ratios and calcined at different temperatures were prepared by mechanical mixing and impregnation methods. The catalysts were used for esterification of ethanol and acetic acid. SO~ 2- _4/40%SiO_2-TiO_2 prepared by mechanical mixing and calcination at 400 ℃ exhibited the highest activity, and the acetic acid conversion was nearly 100% in partial reflux rectifying esterification and up to 84% in total reflux esterification, which was close to the chemical equilibrium composition. X-ray diffraction patterns indicated that SiO_2 inhibited the excessive formation of titanium oxide sulfate. The combination of tetragonal crystal anatase TiO_2, orthorhombic crystal titanium oxide sulfate, and cubic crystal titanium with high surface area SiO_2 ensured the high activity of the catalysts. Infrared spectra showed that the addition of SiO_2 helped the formation of Ti-O-Si linkage which enhanced the strong bonding of SO~ 2- _4 with the catalyst surface. The sulfate species bonded were in bidentately chelating and covalent sulfate structures. Thermogravimetric-differential scanning calorimetry proved that SO~ 2- _4 was hardly removed with the addition of SiO_2 and the temperature for transformation of anatase to rutile was lowered.
【Fund】: 国家自然科学基金(50476090);; 广东省自然科学基金(04000378)资助项目.
【CateGory Index】: O643.36
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