发光巯基配合物的制备及其在金属离子检测中的应用
发布时间：2018-07-25 18:10
【摘要】：荧光材料因其自身所具有的特殊发光性能,多年来一直被科研工作者们所关注与研究。同时荧光材料在荧光分子探针、生物成像、光电响应、发光二极管(LED)和太阳能电池等多个领域都有着广泛的应用。本文在调研了大量的国内外之前发表工作的基础上,采用了燃烧法、溶剂热法和搅拌法这三种方法合成了三组不同的荧光材料,研究探讨了它们的性质及其应用。主要内容包括以下三个方面:(1)荧光碳纳米颗粒(Au-C NPs)的合成及其对Fe3+和Hg2+的检测采用直接燃烧的方式处理氯金酸(HAuCl4)和谷胱甘肽(GSH)的混合物,制备出了具有荧光性质的碳纳米颗粒(Au-CNPs)。通过使用X-射线衍射仪(XRD),X-射线光电子能谱仪(XPS),透射电子显微镜(TEM)和红外光谱仪(IR)等手段对碳纳米颗粒进行了物相、形貌等表征。测试结果表明了 Au被包裹在碳颗粒的里层,整个颗粒的表面被大量的有机基团修饰。探究Au-CNPs对金属离子的响应性质,一共选择了 13种待检测的金属离子,测试结果发现Au-CNPs对Fe3+和Hg2+这两种离子都能够特殊识别。当Fe3+的浓度在1.0*10-5到2.0*10-3 M和Hg2+的浓度在5.0*10-5到3.0*10-2M的范围时,Au-CNPs的荧光强度分别与两种离子浓度都具有很好的线性相关性。除此之外,我们也探究了在实际水样中Au-CNPs对Fe3+和Hg2+的响应情况,结果表明了 Au-C NPs在实际水样中对两种离子也能很好的响应,实际水样环境并不会影响Au-CNPs对离子的检测。(2)荧光石墨烯量子点(GQDs)的合成及其对Fe3+的检测基于此前的研究,用谷胱甘肽(GSH)作为碳源,乙二醇作为溶剂,利用溶剂热法制备出能够发荧光的石墨烯量子点。通过AgN03来调节石墨烯量子点表面修饰的基团种类,当没有加入AgNO3时,所制备的石墨烯量子点(SN-GQDs)表面有羟基(-OH),羧基(-COOH),氨基(-NH2)和巯基(-SH)等基团修饰。当在反应体系中加入了 AgNO3时,因AgNO3可以与GSH中的-SH结合从而形成了 Ag2S,即-SH从石墨烯量子点表面脱落,所制备出的石墨烯量子点(N-GQDs)表面就没有该基团修饰。随后用XRD、TEM、原子力显微镜(AFM)、XPS和IR等手段对量子点进行了物相、形貌、元素等表征。同时也研究了两种量子点对金属离子的检测。同样挑选了 13种待检测的金属离子,测试结果发现SN-GQDs对Hg2+具有特殊地离子响应性质。而N-GQDs则能对Fe3+快速离子响应,并且在5.0*10-5到2.0*10-3M这一范围内,Fe3+浓度与N-GQDs的相对荧光强度呈现出很好的线性关系。(3)三基色荧光材料调制白光的制备探索通过处理两种含有巯基的有机物2-巯基苯并噻唑和2-巯基吡啶,分别与AgN03按一定的比例混合后溶解在乙酸乙酯溶剂中,快速搅拌,离心洗涤后烘干即可得到荧光粉末。将制备出的能发出红色荧光和黄绿色荧光的聚集诱导荧光材料与之前合成的蓝色荧光量子点,通过调配这三基色的荧光材料的比例,得到了可以发出白光的荧光材料。
[Abstract]:Fluorescent materials have been paid attention to by researchers for many years because of their special luminescent properties. At the same time, fluorescent materials have been widely used in many fields, such as fluorescent molecular probes, biological imaging, photoresponse, light-emitting diode (LED) and solar cells. In this paper, three different groups of fluorescent materials have been synthesized by combustion, solvothermal and agitation methods, and their properties and applications have been discussed based on the investigation of a large number of previous work published at home and abroad. The main contents include the following three aspects: (1) the synthesis of fluorescent carbon nanoparticles (Au-C NPs) and the direct combustion of Fe3 and Hg2 were carried out to prepare fluorescent carbon nanoparticles (Au-CNPs) from the mixture of HAuCl4 and glutathione (GSH). The phase and morphology of carbon nanoparticles were characterized by means of X-ray diffractometer (XRD) and X-ray photoelectron spectroscopy (XPS),) transmission electron microscope (TEM) and infrared spectrometer (IR). The results show that au is encapsulated in the inner layer of carbon particles, and the surface of the particles is modified by a large number of organic groups. In order to investigate the response of Au-CNPs to metal ions, 13 kinds of metal ions were selected. The results show that Au-CNPs can recognize both Fe3 and Hg2 ions. The fluorescence intensity of Au-CNPs is linearly correlated with the concentration of both ions when the concentration of Fe3 is 1.0 ~ (-5) ~ 2.0 ~ (-1) ~ (-3) M and the concentration of Hg2 is in the range of 5.0 ~ (-5) ~ 3.0 ~ (-2) M. In addition, we also investigated the response of Au-CNPs to Fe3 and Hg2 in real water samples. The results show that Au-C NPs can also respond well to two kinds of ions in real water samples. (2) Synthesis of fluorescent graphene quantum dot (GQDs) and its detection of Fe3 based on previous studies, glutathione (GSH) was used as carbon source and ethylene glycol as solvent. Graphene quantum dots were prepared by solvothermal method. The types of groups modified on the surface of graphene quantum dots were regulated by AgN03. When AgNO3 was not added, the surface of graphene quantum dots (SN-GQDs) was modified with hydroxyl group (-OH), carboxyl group (-COOH), amino group (-NH2) and mercapto group (-SH). When AgNO3 was added to the reaction system, the Ag _ 2S was formed because AgNO3 could bind to the -SH in GSH, that is, the surface of graphene quantum dots (N-GQDs) was not modified by Ag _ 2S when -SH was removed from the surface of graphene quantum dots. Then the phase, morphology and elements of the QDs were characterized by XRD-Tem, atomic force microscope (AFM) (AFM) and IR. The detection of metal ions by two quantum dots is also studied. Thirteen kinds of metal ions were also selected. It was found that SN-GQDs has a special earth ion response to Hg2. N-GQDs, on the other hand, can respond to the fast ions of Fe3. There is a good linear relationship between the concentration of Fe _ 3 and the relative fluorescence intensity of N-GQDs in the range of 5.0 ~ 2.0 ~ 10 ~ (-3) M. (3) the preparation of white light modulated by tricolor fluorescent materials and the treatment of two organic compounds containing mercapto group 2-mercaptobenzothiothiothioate Azoles and 2-mercaptopyridine, The fluorescent powder was obtained by mixing with AgN03 in a certain proportion and then dissolving in ethyl acetate solvent, stirring quickly, drying after centrifugation and washing. The aggregation induced fluorescence material which can emit red fluorescence and yellow green fluorescence was mixed with the blue fluorescence quantum dot, and the white fluorescent material was obtained by the proportion of the three primary color fluorescent materials.
【学位授予单位】：安徽大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O657.3
本文编号：2144619
[Abstract]:Fluorescent materials have been paid attention to by researchers for many years because of their special luminescent properties. At the same time, fluorescent materials have been widely used in many fields, such as fluorescent molecular probes, biological imaging, photoresponse, light-emitting diode (LED) and solar cells. In this paper, three different groups of fluorescent materials have been synthesized by combustion, solvothermal and agitation methods, and their properties and applications have been discussed based on the investigation of a large number of previous work published at home and abroad. The main contents include the following three aspects: (1) the synthesis of fluorescent carbon nanoparticles (Au-C NPs) and the direct combustion of Fe3 and Hg2 were carried out to prepare fluorescent carbon nanoparticles (Au-CNPs) from the mixture of HAuCl4 and glutathione (GSH). The phase and morphology of carbon nanoparticles were characterized by means of X-ray diffractometer (XRD) and X-ray photoelectron spectroscopy (XPS),) transmission electron microscope (TEM) and infrared spectrometer (IR). The results show that au is encapsulated in the inner layer of carbon particles, and the surface of the particles is modified by a large number of organic groups. In order to investigate the response of Au-CNPs to metal ions, 13 kinds of metal ions were selected. The results show that Au-CNPs can recognize both Fe3 and Hg2 ions. The fluorescence intensity of Au-CNPs is linearly correlated with the concentration of both ions when the concentration of Fe3 is 1.0 ~ (-5) ~ 2.0 ~ (-1) ~ (-3) M and the concentration of Hg2 is in the range of 5.0 ~ (-5) ~ 3.0 ~ (-2) M. In addition, we also investigated the response of Au-CNPs to Fe3 and Hg2 in real water samples. The results show that Au-C NPs can also respond well to two kinds of ions in real water samples. (2) Synthesis of fluorescent graphene quantum dot (GQDs) and its detection of Fe3 based on previous studies, glutathione (GSH) was used as carbon source and ethylene glycol as solvent. Graphene quantum dots were prepared by solvothermal method. The types of groups modified on the surface of graphene quantum dots were regulated by AgN03. When AgNO3 was not added, the surface of graphene quantum dots (SN-GQDs) was modified with hydroxyl group (-OH), carboxyl group (-COOH), amino group (-NH2) and mercapto group (-SH). When AgNO3 was added to the reaction system, the Ag _ 2S was formed because AgNO3 could bind to the -SH in GSH, that is, the surface of graphene quantum dots (N-GQDs) was not modified by Ag _ 2S when -SH was removed from the surface of graphene quantum dots. Then the phase, morphology and elements of the QDs were characterized by XRD-Tem, atomic force microscope (AFM) (AFM) and IR. The detection of metal ions by two quantum dots is also studied. Thirteen kinds of metal ions were also selected. It was found that SN-GQDs has a special earth ion response to Hg2. N-GQDs, on the other hand, can respond to the fast ions of Fe3. There is a good linear relationship between the concentration of Fe _ 3 and the relative fluorescence intensity of N-GQDs in the range of 5.0 ~ 2.0 ~ 10 ~ (-3) M. (3) the preparation of white light modulated by tricolor fluorescent materials and the treatment of two organic compounds containing mercapto group 2-mercaptobenzothiothiothioate Azoles and 2-mercaptopyridine, The fluorescent powder was obtained by mixing with AgN03 in a certain proportion and then dissolving in ethyl acetate solvent, stirring quickly, drying after centrifugation and washing. The aggregation induced fluorescence material which can emit red fluorescence and yellow green fluorescence was mixed with the blue fluorescence quantum dot, and the white fluorescent material was obtained by the proportion of the three primary color fluorescent materials.
【学位授予单位】：安徽大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O657.3
【参考文献】
相关期刊论文 前1条
1 王艳忠,黄素萍;新型荧光材料的应用及其发展趋势[J];化工新型材料;2000年11期
，本文编号：2144619
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