铅基配位聚合物的制备及其对硝基苯的荧光检测  

Preparation of Lead-based Coordination Polymers and Fluorescence Detection of Nitrobenzene

作　　者：王策 WANG Ce(College of Chemistry and Material,Weinan Normal University,Weinan,Shaanxi 714099,China)

机构地区：[1]渭南师范学院化学与材料学院,陕西渭南714099

出　　处：《中国无机分析化学》2024年第12期1624-1631,共8页Chinese Journal of Inorganic Analytical Chemistry

基　　金：陕西省高校科协青年人才托举计划项目(20210608);陕西省教育厅科研计划项目(22JK0373);渭南师范学院人才项目(2021RC24)。

摘　　要：为寻找检测水溶液中硝基苯类化合物的高效检测方法,选取三羧酸配体1,3,5-均苯三甲酸(H3btc)合成两例新型三维柱链型配位化合物[Pb_(3)(btc)_(2) H_(2) O]·4EtOH(1^(#))和[Pb(gac)(H_(2) O)]·H_(2) O(2^(#))。通过X-射线单晶衍射仪、红外光谱仪对该化合物表征,并对其热稳定性及荧光性质进行研究。结果表明,化合物1#结晶在单斜晶系P-1空间群。晶胞参数为a=0.703(2)nm、b=1.173(4)nm、c=2.275(7)nm。晶体的每个不对称单元包括两个btc 3-配体阴离子,三个Pb^(2+)以及一个配位H_(2) O分子;整个金属-有机框架呈电中性。与自由配体H 3 btc的固态荧光相比,该化合物的发射峰出现了较大的红移(红移60 nm),这可能是由于涉及s轨道和p轨道的金属中心跃迁以及配体与Pb(II)离子的配位相互作用所致。此外,测试了化合物1#对硝基苯的荧光传感,浓度在2.0×10^(-5)~2.0×10^(-4) mol/L时,检出限为9.3×10^(-6) mol/L。结果证明化合物1#可对水体中的硝基苯具有良好的荧光检测作用。In order to find an efficient method for detecting nitrobenzene compounds in aqueous solution,the three-dimensional coordination compound[Pb_(3)(btc)2 H_(2) O]·4EtOH(1#)and[Pb(gac)(H_(2) O)]·H_(2) O(2^(#))was constructed under solvethermal conditions.The compound was characterized by X-ray single crystal diffractometer and infrared spectrometer,and its thermal stability and fluorescence properties were studied.The parameters of compound 1#crystallized in monocline P-1 space group cell were a=0.703(2)nm,b=1.173(4)nm and c=2.275(7)nm.Each asymmetric unit of the compound consisted of three Pb^(2+)ions,two btc 3-ligand anions,and a coordination H_(2)O molecule.The fluorescence properties of the compound were further studied.Compared with the emission spectrum of the free ligand,the emission peak showed a large red shift,and the strongest fluorescence peak was 60 nm compared with that of H 3 btc.This might be due to metal-center transitions involving s and p orbitals and coordination interactions between ligands and Pb(Ⅱ)ions.In addition,the fluorescence sensing of nitrobenzene of compound 1#was tested.When the concentration range was 2.0×10^(-5)~2.0×10^(-4) mol/L,the detection limit was 9.3×10^(-6) mol/L.The results showed that compound 1#had good fluorescence detection effect on nitrobenzene in water.

关 键 词：金属有机框架 水热合成法 热稳定性 荧光检测 

分 类 号：O482.31[理学—固体物理]