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机构地区:[1]湖南师范大学化学化工学院,湖南长沙410081 [2]湖南大学化学化工学院,湖南长沙410082
出 处:《应用化工》2009年第4期477-482,共6页Applied Chemical Industry
基 金:国家自然科学基金资助项目(20673103)
摘 要:研究了在硫酸溶液中以Mn(Ⅱ)/Mn(Ⅲ)作为媒质,铅为阴极和阳极,在无隔膜电解槽中间接电化学氧化茴香脑合成茴香醛,讨论了电解反应条件对电解产率的影响。结果表明,以5.5 mol/L H2SO4+0.15 mol/LMn(Ⅱ)为电解液,控制电流密度为50 mA/cm2,电解温度为40℃,阴、阳极面积比为1∶6,电解2 h时,得到的Mn(Ⅲ)电解产率高达95.6%;以乙醚为溶剂,在50℃恒温搅拌且回流冷凝的条件下,用Mn(Ⅲ)氧化稍超过理论量的茴香脑,合成的茴香醛产率高达80.7%。Indirect electrochemical oxidation of anethole to anisaldehyde was investigated in non-membrane electrolytic cell using Mn( Ⅱ )/Mn( Ⅲ ) as redox mediator, and pure lead as cathode and anode in sulphuric acid solution. The effects of electrolysis conditions on the yield of Mn( Ⅲ ) was particularly discussed. The result showed that using 5.5 moi/L sulfuric acid and 0.15 moL/L Mn( Ⅱ ) solution as the electrolyte with the current density at 50 mA/cm^2, temperature at 40 ℃ and control the ratio of area of cathode to anode as 1 : 6, electrolysis for 2 h, the electrolytic yield of Mn (Ⅲ ) reached 95.6%. Using Mn( Ⅲ ) to oxidate anethole with quantity a little over than in theory, aether as solvent,whisk, circulate and condensate with constant temperature at 50 ℃, the yield of anisaldehyde reached 80.7%.
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