采用Cu,Zn,Ni为“牺牲”阳极,在无隔膜电解槽和含配体水杨醛缩L-异亮氨基酸Schiff碱的乙腈溶液中电解合成了Cu(Ⅱ),Zn(Ⅱ)和Ni(Ⅱ)配合物.利用元素分析、红外光谱、紫外光谱、热分析等手段对配合物的结构进行了表征,测定了Cu(Ⅱ)配合物的电化学性质.结果表明,配合物的化学组成为ML·nH2O(L=C13H15NO3,M=Cu(Ⅱ),Zn(Ⅱ),Ni(Ⅱ),n=1,1,2),配合物具有相似的空间结构,配体均以三齿进行配位;电合成配合物的电化学效率Ef接近0.5mol/F[Zn(Ⅱ),Ni(Ⅱ)]和1.0mol/F[Cu(Ⅱ)],Cu(Ⅱ)配合物中Cu(Ⅱ)L/Cu(Ⅰ)L电对的可逆半波电位Er1/2为-0.79V.
The direct electrosynthesis of Cu( Ⅱ ), Zn( Ⅱ ) and Ni( Ⅱ ) complexes of salicylideneamino acid was accomplished by electrochemical dissolution of sacrificial metallic anodes in an acetonitrile solution of the ligand salicylideneamino acid in not-membrane electrolytic cell. The complexes were characterized by FTIR, elemental analysis, UV-Vis spectra and thermal analysis. And the electrochemical property of Cu ( Ⅱ ) complex was examined. The complex formula is ML · nH2 O, where L = L-isoleucine Schiff base, M = Cu ( Ⅱ ), Zn( Ⅱ ), Ni( Ⅱ ), n = 1,1,2. The complexes have a similar spatial structure and the ligand was tricoordinate. The electrochemical efficiency Ef is near 0. 5 mol/F[ for Zn( Ⅱ ), Ni( Ⅱ ) complexes] and 1.0 mol/F [for Cu( Ⅱ ) complex]. In the Cu( Ⅱ ) complex, E1/2 ^r of Cu( Ⅱ )L/Cu( Ⅰ )L couple was -0.79 V(vs. SCE).