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作 者:翟庆辉 王学敏[1] 龚树文[1] 卢静[1] 崔庆新[1]
出 处:《化学研究与应用》2015年第11期1671-1676,共6页Chemical Research and Application
基 金:国家自然科学基金项目(21101086)资助;聊城大学大学生科技文化创新基金项目(SF2013080)资助
摘 要:采用乙醚反萃取方法合成了Dawson结构磷钼钒酸H8P2Mo16V2O62,进而与碳酸铯反应得到Dawson结构磷钼钒酸铯催化剂CsnH8-nP2Mo16V2O62(n=1-5),利用X射线粉末衍射(XRD)、红外(FTIR)以及SEM等对催化剂进行分析,并以H2O2为氧化剂,评价其在苯液相氧化直接羟基化合成苯酚反应中的催化性能,系统的研究了反应时间、催化剂用量、H2O2用量、反应溶剂等反应条件对催化反应的影响。结果表明,合成Cs3H5P2Mo16V2O62在催化反应中表现出优良的催化活性,优化条件下,苯酚收率达到31.0%;催化剂回收方便,可多次重复使用,在反应过程中,催化剂的Dawson结构没有明显变化。Heteropoly acid H8P2Mo16V2O62 with Dawson structure was prepared by ether anti-extraction method and then the cesium salts CsnH8-nP2Mo16V2O62( n= 1-5) were prepared. These cesium salts ware characterized by IR,XRD and SEM methods. The catalytic activity of these catalysts was evaluated in the hydroxylation of benzene to phenol with H2O2 as oxidant. The effects of various parameters on hydroxylation were also tested,which included reaction time,catalyst amount,reaction temperature,different solvents and reactants ratio. Results indicated that the prepared cesium salt,Cs3H5P2Mo16V2O62 presented best catalytic activity,and the yield of phenol could reach 31. 0% at optimal reaction conditions. Cs3H5P2Mo16V2O62 also had excellent stability in the hydroxylation of benzene,and the Dawson-type structure still retained after reused several times.
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