化学研究与应用
化學研究與應用
화학연구여응용
Chemical Research and Application
2015年
11期
1671-1676
,共6页
翟庆辉%王学敏%龚树文%卢静%崔庆新
翟慶輝%王學敏%龔樹文%盧靜%崔慶新
적경휘%왕학민%공수문%로정%최경신
杂多酸%铯盐%苯%羟基化%苯酚
雜多痠%銫鹽%苯%羥基化%苯酚
잡다산%색염%분%간기화%분분
heteropoly acid%cesium salt%benzene%hydroxylation%phenol
采用乙醚反萃取方法合成了Dawson结构磷钼钒酸H8 P2 Mo16 V2 O62,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H2 O2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、H2 O2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Cs3 H5 P2 Mo16 V2 O62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。
採用乙醚反萃取方法閤成瞭Dawson結構燐鉬釩痠H8 P2 Mo16 V2 O62,進而與碳痠銫反應得到Dawson結構燐鉬釩痠銫催化劑CsnH8-nP2Mo16V2O62(n=1-5),利用X射線粉末衍射(XRD)、紅外(FTIR)以及SEM等對催化劑進行分析,併以H2 O2為氧化劑,評價其在苯液相氧化直接羥基化閤成苯酚反應中的催化性能,繫統的研究瞭反應時間、催化劑用量、H2 O2用量、反應溶劑等反應條件對催化反應的影響。結果錶明,閤成Cs3 H5 P2 Mo16 V2 O62在催化反應中錶現齣優良的催化活性,優化條件下,苯酚收率達到31.0%;催化劑迴收方便,可多次重複使用,在反應過程中,催化劑的Dawson結構沒有明顯變化。
채용을미반췌취방법합성료Dawson결구린목범산H8 P2 Mo16 V2 O62,진이여탄산색반응득도Dawson결구린목범산색최화제CsnH8-nP2Mo16V2O62(n=1-5),이용X사선분말연사(XRD)、홍외(FTIR)이급SEM등대최화제진행분석,병이H2 O2위양화제,평개기재분액상양화직접간기화합성분분반응중적최화성능,계통적연구료반응시간、최화제용량、H2 O2용량、반응용제등반응조건대최화반응적영향。결과표명,합성Cs3 H5 P2 Mo16 V2 O62재최화반응중표현출우량적최화활성,우화조건하,분분수솔체도31.0%;최화제회수방편,가다차중복사용,재반응과정중,최화제적Dawson결구몰유명현변화。
Heteropoly acid H8 P2 Mo16 V2 O62 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 cata-lytic activity of these catalysts was evaluated in the hydroxylation of benzene to phenol with H2 O2 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, Cs3 H5 P2 Mo16 V2 O62 presented best catalytic activity, and the yield of phenol could reach 31. 0%at optimal reaction conditions. Cs3 H5 P2 Mo16 V2 O62 also had excellent stability in the hydroxyl-ation of benzene,and the Dawson-type structure still retained after reused several times.