双色烯二酮及其金属配合物的合成与表征

发布时间：2018-04-26 15:12

本文选题：双色烯二酮 + 金属配合物　；参考：《天津理工大学》2014年硕士论文

【摘要】：配位化合物在自然界中普遍存在，自从1704年柏林的Diesbach偶然得到普鲁士蓝KCN·Fe(CN)2·Fe(CN)3以来，配位化学的理论和实验研究都取得了迅速发展。通过多种配位形式得到的各种金属配合物不仅结构新颖，还兼有催化、电导、光学、磁学以及生命科学等潜在的应用价值。本课题组具有知识产权的4H,4'H-2,2'-双色烯-4,4'-二酮（简称为BCDO）有良好的荧光性能及ESR信号，是一种荧光-磁性双功能的有机分子化合物。本论文首次以具有荧光性能的分子自由基BCDO为配体，与3d自旋载体过渡金属离子反应，合成了新型的未见报道的BCDO-M配合物，具体研究内容如下：（1）以苯酐和丁二酸为原料，合成了即BCDO（化合物1），并利用IR，1HNMR，HRMS对其结构进行表征，结构正确；（2）首次以分子自由基化合物1为配体，按不同的原料配比与自旋载体3d过渡金属盐（Fe3+、Co2+、Ni2+）反应，采用经典溶液法和水热法合成了6种新型的金属配合物2a～2f。利用IR，1HNMR，HRMS等对配合物的结构进行了表征，依此推测出BCDO-M配合物2a～2f的结构，并对合成方法进行了筛选确认；（3）对所合成的BCDO-M配合物2a～2f进行了UV-Vis吸收光谱和荧光光谱测定，发现其皆具有良好的荧光性能，是一类新型的具有荧光的金属配合物；（4）针对所合成配合物的荧光性能，以2b为为探针，采用荧光法对阳离子表面活性剂双十八烷基二甲基氯化铵（D1821）的临界胶束浓度（CMC）进行了测定，，测定结果0.1mmol·L-1与文献报道值一致，说明配合物2b可作为一种新型荧光探针，方法简便、可行。
[Abstract]:Coordination compounds are ubiquitous in nature. Since the birth of Prussian Blue KCN Fe(CN)2 Fe(CN)3 from Diesbach in Berlin in 1704, the theoretical and experimental studies of coordination chemistry have developed rapidly. All kinds of metal complexes obtained by various coordination forms are novel in structure and have potential applications in catalysis, conductance, optics, magnetism and life sciences. Our group has good fluorescence properties and ESR signal, which is a kind of organic compound with dual functions of fluorescence and magnetism. In this thesis, a novel unreported BCDO-M complex was synthesized by the reaction of the fluorescent free radical BCDO with 3D spin carrier transition metal ions for the first time. The specific research contents are as follows. BCDO (compound 1) was synthesized from phthalic anhydride and succinic acid, and its structure was characterized by IR 1H N MRMS. (2) for the first time, six new metal complexes 2aa2f were synthesized by classical solution method and hydrothermal method, using molecular free radical compound 1 as ligand, and reaction with spin carrier 3d transition metal salt Fe _ 3H _ 3CO _ 2H _ 2 / Ni _ 2 at different raw material ratios for the first time. The structure of the complex was characterized by IR 1H NMR-HRMS, and the structure of BCDO-M complex 2a~2f was deduced, and the synthetic method was screened and confirmed. The synthesized BCDO-M complex 2a~2f was characterized by UV-Vis absorption spectra and fluorescence spectra. It was found that 2a~2f has good fluorescence properties and is a new kind of metal complexes with fluorescence. The critical micelle concentration of cationic surfactant dioctadecyl dimethylammonium chloride (D1821) was determined by fluorescence method with 2b as probe. The results of 0.1mmol L-1 were in agreement with those reported in the literature. The results show that the complex 2b can be used as a new fluorescent probe, and the method is simple and feasible.
【学位授予单位】：天津理工大学
【学位级别】：硕士
【学位授予年份】：2014
【分类号】：O641.4

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