Fe^(Ⅱ)修饰的沙漏型磷钼酸盐的合成、表征与电化学性能研究

Synthesis,Characterization and Electrochemical Properties of Fe^(Ⅱ) Modified Hourglass Phosphomolybdate

以Fe(NO_(3))_(3)·9H_(2)O、H_(3)PO_(4)、Na_(2)MoO_(4)·2H_(2)O、3-氨甲基吡啶为原料,利用水热合成法成功合成了一例Fe^(Ⅱ)修饰的沙漏型磷钼酸基配合物1(分子式为(C_(6)H_(10)N_(2))_(6){Fe[Mo_(6)O_(12)(OH)_(3)(PO_(4))_(2)(H_(2)PO_(4))_(2)]_(2)}·3.5H_(2)O),并对配合物1进行了单晶X-射线衍射、红外光谱(FT-IR)、粉末X射线衍射(PXRD)和热重(TG)等分析,以证明其结构和组成,同时进行了结构分析。结果表明,配合物1呈一个三维超分子框架,是通过N(6)—H(6B)···O(15)、N(6)—H(6A)···O(8)、N(2)—H(2C)···O(23)、N(2)—H(2B)···O(19)和N(1)—H(1A)···O(30)等五种氢键,将{Fe[P_(4)Mo_(6)^(V)O_(31)]_(2)}^(22-)(记为{Fe(P_(4)Mo_(6))_(2)})和质子化的3-氨甲基吡啶连接而形成的。此外,利用配合物1修饰的碳糊电极(1-CPE)对盐酸呋喃它酮进行了电化学检测。结果表明,1-CPE具有良好的稳定性以及对盐酸呋喃它酮的高选择性。

Using Fe(NO_(3))_(3)·9H_(2)O,H_(3)PO_(4),Na_(2)MoO_(4)·2H_(2)O,3-aminomethylpyridine as raw materials,a complex 1 based on the hourglass phosphomolybdate modified with FeⅡ was successfully synthesized by hydrothermal synthesis method.The molecular formula is(C_(6)H_(10)N_(2))_(6){Fe[Mo_(6)O_(12)(OH)_(3)(PO_(4))_(2)(H_(2)PO_(4))_(2)]_(2)}·3.5H_(2)O.The single crystal X-ray diffraction infrared spectroscopy(FT-IR) powder X-ray diffraction(PXRD) and thermogravimetric analysis(TGA) were used to prove its structure and composition which was analyzed at the same time The results show that complex 1 has a three-dimensional supramolecular framework,which connected {Fe[P_(4)Mo_(6)~VO_(31)]_(2)}^(22-)(denoted as {Fe(P_(4)Mo_(6))_(2)}) and protonated 3-aminomethylpyridine by five hydrogen bond interactions of N(6)—H(6B) ···O(15),N(6)—H(6A)···O(8),N(2) —H(2C)···O(23),N(2) —H(2B) ···O(19) and N(1) —H(1A) ···O(30).Besides,the electrochemical detection of furaltadone hydrochloride was further studied by using complex modified carbon paste electrode(1-CPE).The experimental results show that 1-CPE has good stability and high selectivity for furaltadone hydrochloride.