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《Journal of Chemical Engineering of Chinese Universities》 2009-03
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Synthesis and Characteristic of Catalytic Epoxidation of W,Mo-containing Hydrotalcite-like Materials

ZHOU Chun-hui1 , XIE Hua-li1, Du Ze-xue2, Fan Yong-xian1, GE Zhong-hua1, LI Xiao-nian1, (1. College of Chemical Engineering and Materials Science, Zhejiang University of Technology, Hangzhou 310032, China; 2. SINOPEC Research Institute of Petroleum Processing, Beijing 100083, China)  
Tungsten (W), molybdenum (Mo)-intercalated hydrotalcite-like materials (HTL) were synthesized by ionic exchange reaction with Mg/Al HTL precursors, during which the interlayer of the used precursors were enlarged by large organic molecules of p-toluenesulfonate. The M/Al (M=W, Mo) molar ratio of the prepared W, Mo-intercalated HTL (W, Mo-HTL) are 7:6, 7:20 and 7:60, respectively, and they were characterized by IR, UV-Vis, PXRD, SEM, TGA and XPS, respectively. In the IR spectra of the synthesized W, Mo-HTL, the absorbance of p-toluenesulfonate appears and the absorbance intensities of p-toluenesulfonate decrease with the increase of the M/Al ratio in W, Mo-HTL, these indicate that the intercalation of Mo and W into the interlayer of HTL occurs. The UV-Vis analyses show that the diverse coordination state exists in the prepared Mo-HTL, while the prepared W-HTL has diverse coordination only when the W/Al ratio in it is high. The XRD patterns and SEM micrographs show that the synthesized W, Mo-HTL materials have layered structure and morphology, and their gallery heights increase with the increase of M/Al ratio in the prepared W, Mo-HTL. The catalytic performance of the prepared W, Mo-HTL was studied through the epoxidation reaction with the allyl chloride as substrate, H2O2 (30%) as oxidant and acetonitrile as solvent. The experimental epoxidations of allyl chloride were conducted at 50℃ and for 2 h, and the W, Mo-HTL used as catalyst are active to some extent for the epoxidation reaction. The highest selectivity of epichlorohydrine is 85.2% and 77.3% over the W-HTL and Mo-HTL, respectively; and the conversion of H2O2 are in the range of 41.2% to 94.3%. The lower H2O2 conversion efficiency may impute to the existent of the diverse coordination state of Mo or W in the W, Mo-HTL which leads to the catalytic decomposition of H2O2.
【Fund】: 国家自然科学基金(20773110 20541002);; 浙江省自然科学基金(Y405064 Y405064 Y407200 Y405025);; 中石化公司科技项目(X504034)
【CateGory Index】: O643.3
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