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以Ti为基底电极,在PdCl2溶液中电沉积制备了Pd/Ti电极,采用SEM和XPS进行表征.采用循环伏安法研究了Cu,Ag,Ti和Pd/Ti电极对间氯苯甲酸(3-CBA)的电还原特性,与Cu,Ag和Ti电极相比,Pd/Ti电极对3-CBA有较好的电化学还原活性.同时采用电化学原位红外反射光谱对3-CBA在Pd/Ti电极上的电还原反应机理进行了系统分析,结果表明3-CBA在Pd/Ti电极上的电化学脱氯反应是一个脱氯加氢过程,3-CBA首先得到一个电子形成阴离子自由基中间体,随后释放一个氯离子,产生苯甲酸盐的自由基,最后该自由基得到一个电子并夺取一个氢质子,在电极表面脱去氯得到最终产物苯甲酸.
Pd / Ti electrodes were electrodeposited with Ti as substrate electrode in PdCl2 solution and characterized by SEM and XPS. Cyclic voltammetry was used to study the effect of Cu, Ag, Ti and Pd / -CBA), compared with Cu, Ag and Ti electrodes, Pd / Ti electrode has better electrochemical reduction activity for 3-CBA. At the same time, electrochemical in situ IR reflectance spectra of 3-CBA in Pd / Ti electrode was studied systematically. The results showed that the electrochemical dechlorination reaction of 3-CBA on Pd / Ti electrode was a dechlorination hydrogenation process. The 3-CBA first got an electron-forming anion radical The intermediate then releases a chloride ion to produce a benzoate free radical. Eventually the radical gets an electron and takes a hydrogen proton off the surface of the electrode to give the final benzoic acid.