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本文用控制阴极电位电解还原方法,制得了以Si为杂原子的Keggin结构二电子、四电子杂多蓝K_2H_4[SiMo_2~ⅤMo_(10)~ⅥO_(40)]·12H_20(Ⅰ)和K_3H_5[SiMo_4~ⅤMo_8~ⅥO_(40)]·12H_2O(Ⅱ).通过IR,UV,极谱,XPS,ESR及单晶X射线衍射对所合成的杂多蓝进行了表征,确定了被还原的Mo(V)位置位于不同的边共用三金属簇内,测定结果表明,Keggin结构杂多阴离子还原后,八面体结构有轻微畸变,畸变程度随还原程度增大而增大。
In this paper, the Keggin structure two-electron and four-electron heteropoly blue K_2H_4 [SiMo_2 ~ ⅤMo_ (10) ~ ⅥO_ (40)] · 12H_20 (Ⅰ) and K_3H_5 [SiMo_4 ~ (V) Mo_8 ~ VO_ (40)] · 12H_2O (Ⅱ). The synthesized heteropoly blue was characterized by IR, UV, polarography, XPS, ESR and single crystal X-ray diffraction. ) Were located in different trimeric metal clusters. The results showed that the octahedral structure was slightly distorted after the Keggin structure heteropolyanions were reduced, and the degree of distortion increased with the degree of reduction.