The direct electrochemical synthesis of metal alkoxides [Ti（OEt）4, Ti（OPr-i）4, Ti（OBu）4, Ti（OEt）2（acac）, Cu（OEt）2, Cu（OBu）2, Mg（OEt）2 and Ni（OEt）2] were studied by anode dissolution of metals in abso...The direct electrochemical synthesis of metal alkoxides [Ti（OEt）4, Ti（OPr-i）4, Ti（OBu）4, Ti（OEt）2（acac）, Cu（OEt）2, Cu（OBu）2, Mg（OEt）2 and Ni（OEt）2] were studied by anode dissolution of metals in absolute ethanol in the presence of a conductive additives. The anodic behaviour of Ti electrode in ethanol was investigated by using cyclic voltammetry（CV）. These metal alkoxides were characterized by FTIR spectra. The results show that direct electrochemical synthesis of metal alkoxides have a high current efficiency and electrolysis yield. These alkoxides have a high purity and can be directly used as the precursor of nanosize oxides prepared by sol-gel procedure. The anodic behaviour of Ti electrode in alcohol is markedly the feature of the pitting corrosion. The passivation of Ti anode would occur in the presence of trace water.展开更多
经过三步反应合成了红色晶体,双六甲基二硅胺基二甲基硅基环戊二烯基稀土二价镱配合物[η5-C5H4S iM e2N(S iM e3)2]2Yb(Ⅱ).2THF,X射线衍射结果表明,[η5-C5H4S iM e2N(S iM e3)2]2Yb(Ⅱ).2THF属于单斜晶系,空间群为P21/c,a=1.646 87(1...经过三步反应合成了红色晶体,双六甲基二硅胺基二甲基硅基环戊二烯基稀土二价镱配合物[η5-C5H4S iM e2N(S iM e3)2]2Yb(Ⅱ).2THF,X射线衍射结果表明,[η5-C5H4S iM e2N(S iM e3)2]2Yb(Ⅱ).2THF属于单斜晶系,空间群为P21/c,a=1.646 87(12)nm,b=0.907 70(6)nm,c=3.049 4(3)nm,β=93.642(4),°V=4.549 3(6)nm3,Z=2,C34H72N2O2S i6Yb,Mr=1 905.41,Dc=1.288 g/cm3,F(000)=1 840.00,μ(MoKα)=22.42 cm-1(λ=0.071 070 nm)。收集独立衍射点7 814个,将其中I>3.00σ(1)的用于结构解析,用全矩阵最小二乘法校正,得最终偏离因子R=0.039,Rw=0.050。8配位的中心镱原子与2个四氢呋喃的氧及2个环戊二烯基配位形成扭曲的四面体结构。展开更多
文摘The direct electrochemical synthesis of metal alkoxides [Ti（OEt）4, Ti（OPr-i）4, Ti（OBu）4, Ti（OEt）2（acac）, Cu（OEt）2, Cu（OBu）2, Mg（OEt）2 and Ni（OEt）2] were studied by anode dissolution of metals in absolute ethanol in the presence of a conductive additives. The anodic behaviour of Ti electrode in ethanol was investigated by using cyclic voltammetry（CV）. These metal alkoxides were characterized by FTIR spectra. The results show that direct electrochemical synthesis of metal alkoxides have a high current efficiency and electrolysis yield. These alkoxides have a high purity and can be directly used as the precursor of nanosize oxides prepared by sol-gel procedure. The anodic behaviour of Ti electrode in alcohol is markedly the feature of the pitting corrosion. The passivation of Ti anode would occur in the presence of trace water.
