还原型磷钼酸盐构筑的多酸基超分子化合物的合成及电催化性能研究  

Synthesis and Electrocatalytic Performance of a Polyoxometalate-Based Supramolecular Compound Constructed with Reduced Phosphomolybdate

作　　者：刘晓慧[1] 李慧[1] 徐娜[1] LIU Xiaohui;LI Hui;XU Na(Professional Technology Innovation Center of Liaoning Province for Conversion Materials of Solar Cell,College of Chemistry and Materials Engineering,Bohai University,Jinzhou 121013,China)

机构地区：[1]渤海大学化学与材料工程学院,辽宁省全谱太阳能电池转光材料专业技术创新中心,锦州121013

出　　处：《人工晶体学报》2023年第11期2034-2040,共7页Journal of Synthetic Crystals

基　　金：辽宁省博士启动基金(2021-BS-255);渤海大学校级项目(0522xn032,0521bs011)。

摘　　要：以钼酸钠、硝酸铁、磷酸和三亚乙基四胺为原料,采用水热合成法成功制备了一种还原型磷钼酸盐与FeⅡ构筑的超分子化合物,其化学式为[C_(8)H_(24)N_(4)]_(1.5)[C_(6)H_(22)N_(4)]_(1.5){Fe[Mo_(6)O_(12)(OH)_(3)(PO_(4))_(3)(HPO_(4))]_(2)}·5H_(2)O(1),并通过单晶X射线衍射、粉末X射线衍射(PXRD)和红外光谱(FT-IR)对其结构进行了表征。结果表明,该化合物是由{Fe[P_(4)Mo V_(6)O_(31)]_(2)}^(22-)(记为{Fe(P_(4)Mo_(6))_(2)})、质子化的三亚乙基四胺和质子化的N,N′-二(氨乙基)-哌嗪通过氢键相互作用连接形成的三维超分子结构。电催化性能的研究表明,化合物1对铬离子(CrⅥ)、铁离子(FeⅢ)、溴酸钾(KBrO_(3))和抗坏血酸(AA)具有良好的电化学传感性能和低检测限(LOD)。A supramolecular compound composed of reduced phosphopolybdate and Fe II was synthesized by hydrothermal method with sodium molybdate,ferric nitrate,phosphoric acid and triethylenetetramine as raw materials.The chemical formula of the compound is[C_(8)H_(24)N_(4)]_(1.5)[C_(6)H_(22)N_(4)]_(1.5){Fe[Mo_(6)O_(12)(OH)_(3)(PO_(4))_(3)(HPO_(4))]_(2)}·5H_(2)O(1).Single crystal X-ray diffraction,powder X-ray diffraction(PXRD)and infrared spectroscopy(FT-IR)characterizations show that compound 1 is composed of{Fe[P_(4)Mo V_(6)O_(31)]_(2)}^(22-)(denoted by{Fe(P_(4)Mo_(6))_(2)}),protomated triethyltetramine and protomated N,N′-bis(aminoethyl)-piperazine in a three-dimensional supramolecular structure through hydrogen bond interactions.The results of electrocatalytic performance measurement show that compound 1 has good electrochemical sensing performance and low limit of detection(LOD)for chromium ion(CrⅥ),iron ion(FeⅢ),potassium bromate(KBrO_(3))and ascorbic acid(AA).

关 键 词：还原型磷钼酸盐 超分子结构 电催化性能 水热合成法 晶体结构 

分 类 号：O641[理学—物理化学]