2,6-二甲基-3,5-二(吡唑-3-基)吡啶构筑的新型八钼酸盐的合成及其电化学性质

Synthesis and Electrochemical Properties of A Novel Octamolybdate Based on 2,6-Dimethyl-3,5-bis (pyrazol-3-yl) pyridine

利用六水合硫酸锌(ZnSO4·6H2 O)、七钼酸铵[(NH4)6 Mo7O24·4H 2O]和2,6-二甲基-3,5-二(吡唑-3-基)吡啶(H2L)为原料,通过水热反应,合成了一个新型的八钼酸盐[Zn(H3L)2(H4Mo8O28),1)],其结构和性能经IR、元素分析,X-射线单晶衍射和TGA表征。结果表明:1(CCDC:1860339)属三斜晶系,P-1空间群,晶胞参数a=9.421(5),b=10.737(5),c=11.826(5),α=100.340(5)°,β=97.939(5)°,γ=100.053(5)°,V=1140.9(4)3,Z=1,R 1=0.0292,wR 2=0.0769。在1的结构中,锌离子被质子化的有机配体H 3 L+连接形成一维链结构,同多钼酸簇{Mo8O28}将相邻的一维链连接起来形成二维层结构。电化学分析结果表明:1对亚硝酸根离子还原具有较好的催化作用,当亚硝酸根离子浓度为5 mmol·L-1时,催化效率为61%。

A new octamolybdate, Zn(H3L)2(H4Mo8O28)(H3L=2,6-dimethyl-3,5-bis(pyrazol-3-yl) pyridine)(1, CCDC: 1860339), was synthesized under hydrothermal conditions by using ZnSO4· 6 H2O,(NH4)6Mo7O24· 4 H2O and 2,6-dimethyl-3,5-bis(pyrazol-3-yl) pyridine as starting materials. The structure and properties were characterized by IR, elemental analysis, single crystal X-ray diffraction analysis and TGA. The results showed that 1 belonged to triclinic system, space group P-1 with a=9.421(5)A, b=10.737(5)A, c=11.826(5)A, α=100.340(5)°, β=97.939(5)°, γ=100.053(5)°, V=1 140.9(4) A3, Z=1, R1=0.029 2, wR2=0.076 9. It consists of 1 D chains based on Zn2+ and protonated H3L+, which are further connected into a 2 D layer by {Mo8O28} clusters. In addition, the electrochemical properties of 1 display better electrocatalytic activity toward the reduction of nitrite.The electrocatalytic efficiency towards 5 mmol·L-1 NO2^-1 was calculated to be 61%.