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

机译:负载型磷钨杂多酸催化剂上一锅法合成1-乙酰基ne

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摘要

Phosphotungstic heteropoly acid (PW) supported on various oxides (SiO2, TiO2, K-10 montmorillonite and γ-Al2O3) 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. SiO2-supported phosphotungstic heteropoly acid (PW/SiO2, 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/SiO2 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/SiO2 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.
机译:合成了负载在各种氧化物(SiO2,TiO2,K-10蒙脱土和γ-Al2O3)上的磷钨杂多酸(PW),并将其首次用作Fried与乙酸酐的Friedel-Crafts酰化为1-乙酰基re的催化剂。所制备的催化剂的特征在于比表面积测量,X射线衍射,红外光谱和程序升温的氨解吸。发现SiO 2负载的磷钨杂多酸(PW / SiO 2,40 wt%)是酰化反应中最活泼的催化剂,在环境温度为60°C的反应温度下,对1-乙酰基%的产率为91.8%,选择性为100%。详细研究了PW负载量,PW / SiO2量,反应物摩尔比,反应温度和反应时间对催化酰化反应的影响,以优化工艺参数。评估了PW / SiO2催化剂的可重复使用性,并简要讨论了磷钨杂多酸催化pyr与乙酸酐的Fried弗里德-克拉夫茨酰化反应的可能途径。

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