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化工学报  2014 

准毛细间隙反应器中直接电氧化合成茴香醛二甲基缩醛

DOI: 10.3969/j.issn.0438-1157.2014.06.033, PP. 2193-2201

Keywords: 准毛细间隙反应器,茴香醚,茴香醛二甲基缩醛,电化学,氧化,电解质,工艺条件

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Abstract:

以准毛细间隙反应器为电化学合成装置,采用恒电流电解技术考察了阳极材料、支持电解质、电流密度等工艺参数对茴香醚直接电氧化合成茴香醛二甲基缩醛的影响。结果表明,收率从高到低采用的阳极材料依次为:石墨>钛基铱钽>钛基钌铱>钛基铂;支持电解质依次为:对甲基苯磺酸钠>苯磺酸钠>氟化钾>甲醇钠>高氯酸钠>间硝基苯磺酸钠;在电流密度1~9A·dm-2范围内,反应选择性随着电流密度的增大而减小;添加适量的2,6-二甲基吡啶能抑制茴香醛二甲基缩醛的氧化从而提高反应选择性。在优化条件下,茴香醛二甲基缩醛的收率和电流效率分别达到75%和47%。

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