采用金属Cu,Zn,Ni为“牺牲”阳极,在无隔膜电解槽和含配体水杨醛缩甘氨酸Schiff碱、2-氨基吡啶的甲醇溶液中首次电解合成了Cu(Ⅱ),Zn(Ⅱ),Ni(Ⅱ)配合物.利用元素分析、质谱、核磁、红外光谱、紫外光谱、热分析对配体和配合物进行了表征,确定了配合物的化学组成为ML.L.′nH2O[L=C9H7NO3,(M=Cu(Ⅱ),L′=CH3OH,n=0;M=Zn(Ⅱ)、Ni(Ⅱ),L′=2-氨基吡啶n=1)].电合成Zn(Ⅱ)、Ni(Ⅱ)配合物的电化学效率Ef接近0.5 mol.F-1,电极反应为2电子反应,电合成Cu(Ⅱ)配合物的电化学效率Ef接近1.0 mol.F-1,电极反应为1电子反应,Schiff碱配体均以三齿进行配位.Cu(Ⅱ)配合物中Cu(Ⅱ)(L)L′/Cu(I)(L)L′电对的可逆半波电位Er1/2为-1.225 V(vs SCE).
The electrosynthesis processes have been carried out by anodic dissolution metals(Cu,Zn,Ni) in methanol solutions of salicylidene glycine and 2-aminopyridine in not-membrane electrolytic cell. The complexes are characterized by FTIR, elemental analysis, UV-Visible spectra and so on . The Complex formula is M(L) L'. nH2O, where L=glycine Schiff base, M=Cu(Ⅱ),( M=Cu(Ⅱ),L'=CH3OH, n=0;M=Zn(Ⅱ).Ni(Ⅱ), L'=2-aminopyridine n=1) have been determined. The Schiff base Ligand is tricoordinate. The electrochemical efficiency Ef is near 0.5 mol · F^-1 [for Zn( Ⅱ ) 、Ni( Ⅱ ) complexes] and 1.0 mol · F^-1 [for Cu( Ⅱ ) complexes]. And electrochemical behavior of metal(copper) electrode in electrolyte solution is examined and in the Cu( Ⅱ ) complex ,El/2 of Cu( Ⅱ ) (L) L'/ Cu(I) (L) L'couple was -1. 225 V (vs SCE).