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One-pot synthesis of 1-acetylpyrene over supported phosphotungstic heteropoly acid catalysts

Journal 2012 · IF 0.829 · 108(2): 531-544 · 发表于 2012 年 12 月 8 日
作者: He Min-Qiang,Pan Ai-Xia,Xie Ji-Min,Jiang De-Li,Yuan Xin-Hua,Chen Min
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摘要

Phosphotungstic heteropoly acid (PW) supported on various oxides (SiO 2 , TiO 2 , K-10 montmorillonite and γ-Al 2 O 3 ) were synthesized and used as catalysts for Friedel–Crafts acylation of pyrene with acetic anhydride to 1-acetylpyrene for the first time. The as-prepared catalysts were characterized by specific surface area measurement, X-ray diffraction, infrared spectroscopy, and temperature programmed desorption of ammonia. SiO 2 -supported phosphotungstic heteropoly acid (PW/SiO 2 , 40 wt%) was found to be the most active catalyst in the acylation giving 91.8 % yield and 100 % selectivity for 1-acetylpyrene at reaction temperature of 60 °C under ambient pressure. The effect of PW Loading, PW/SiO 2 amount, molar ratio of reactants, reaction temperature and reaction time on the catalytic acylation reaction were studied in detail to optimize the process parameters. The reusability of the PW/SiO 2 catalyst was appraised, and the possible pathway for the production of the Friedel–Crafts acylation of pyrene with acetic anhydride catalyzed by phosphotungstic heteropoly acid was also discussed briefly.