壳聚糖复合碳纳米管修饰电极的制备及其在电分析化学中的应用
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摘要
碳纳米管(CNT)独特的一维分子结构和奇特的物理、化学特性，成为世界范围内的研究热点之一。相对于其它领域，CNT在分析化学中的应用研究起步相对较晚。本论文对这种新型的纳米材料进行壳聚糖功能化，研究了它在分子的电催化、分离方面的应用。本工作对于进一步开拓纳米材料的应用基础研究具有较大的意义。
本论文的工作分为两大部分：
一、碳纳米管的羧基化及壳聚糖功能化。
1．以浓硝酸和浓硫酸的混合物作为氧化剂对多壁碳纳米管(MWNT)的氧化程度进行了研究。结果表明，同等强度的酸对不同制备方法获得的MWNT的氧化程度和截短程度不同。针对实验中使用的MWNT，系统的研究了酸强度和氧化时间对于MWNT的羧基化程度的影响。一般超声3～5 h，采用不同强度的酸可以获得不同氧化程度的羧基化MWNT。
2．对壳聚糖功能化MWNT的分散性进行了研究，发现功能化后的MWNT水溶液能长时间保持均匀的悬浮状态。通过红外光谱、扫描电镜及电化学方法对壳聚糖功能化的碳纳米管进行了表征。研究了它们之间的相互作用及机理。
二、构置了壳聚糖复合碳纳米管修饰电极，并研究了其在电分析化学领域的应用。
壳聚糖复合碳纳米管修饰层内壳聚糖与碳纳米管相互缠绕，形成了多孔的界面结构，即发挥了碳纳米管的独特性能又体现了壳聚糖的吸附、络合性能。重点研究了对生物分子多巴胺的识别和选择性灵敏测定；对无机离子：碘离子、铅离子、亚锡离子的电催化测定。
Studies on carbon nanotubes (CNT) become a hot topic in the world due to the uniqueone-dimensional tubular structure and subtle physical and chemical properties of CNT.Compared with other area, the application of CNT in analytical chemistry has beenstudied recently. In the present dissertation, the electro catalysis and separation ability ofCTs/CNT modified electrodes were studied firstly by using CNT and CTs as materials ofelectrode. This work may be of great signification for applying nano-material further. Themain achievements obtained in this research include:
1. Carboxyl and chitosan (CTS) functionalized of multi-wall carbon nanotubes(MWNT)
(1) The MWNTs was oxidized with mixture of concentrated sulfuric acid and nitric acid.It was showed that the degree of oxidation and truncation was different even using thesame acids as oxidant. The difference was mainly caused by the preparation methods ofMWNT. According to the properties of the MWNT used in this study, the relationbetween the degree of carboxyl and oxidation time or acids strength was systematicallystudied. Usually the MWNT Was ultrasonic in different acids for 3 to 5 hours, and theproper oxidized carboxyl MWNT can be obtained.
(2) The dispersancy of CTs functionalized MWNT was studied, and found that the watersolution of it could be keep symmetrical suspend state for a several days. The CTsfunctionalized MWNT was characterized by FT-IR, SEM and electrochemistry. The effectand mechanism of them was also studied.
2. A new kind of CTs/CNT modified electrode was constructed and it's applications inelectrical analytical chemistry were investigated.
A lacunaris interface was formed in which CTs and CNT were intertwisted. And theunique performance of CNT and adsorption, complexation effect of CTs were combined.The modified electrode applied to the sensitive and selective determination DA from AAand electrocatalytic determination of I~-, Pb~(2+), Sn~(2+).
本论文的工作分为两大部分：
一、碳纳米管的羧基化及壳聚糖功能化。
1．以浓硝酸和浓硫酸的混合物作为氧化剂对多壁碳纳米管(MWNT)的氧化程度进行了研究。结果表明，同等强度的酸对不同制备方法获得的MWNT的氧化程度和截短程度不同。针对实验中使用的MWNT，系统的研究了酸强度和氧化时间对于MWNT的羧基化程度的影响。一般超声3～5 h，采用不同强度的酸可以获得不同氧化程度的羧基化MWNT。
2．对壳聚糖功能化MWNT的分散性进行了研究，发现功能化后的MWNT水溶液能长时间保持均匀的悬浮状态。通过红外光谱、扫描电镜及电化学方法对壳聚糖功能化的碳纳米管进行了表征。研究了它们之间的相互作用及机理。
二、构置了壳聚糖复合碳纳米管修饰电极，并研究了其在电分析化学领域的应用。
壳聚糖复合碳纳米管修饰层内壳聚糖与碳纳米管相互缠绕，形成了多孔的界面结构，即发挥了碳纳米管的独特性能又体现了壳聚糖的吸附、络合性能。重点研究了对生物分子多巴胺的识别和选择性灵敏测定；对无机离子：碘离子、铅离子、亚锡离子的电催化测定。
Studies on carbon nanotubes (CNT) become a hot topic in the world due to the uniqueone-dimensional tubular structure and subtle physical and chemical properties of CNT.Compared with other area, the application of CNT in analytical chemistry has beenstudied recently. In the present dissertation, the electro catalysis and separation ability ofCTs/CNT modified electrodes were studied firstly by using CNT and CTs as materials ofelectrode. This work may be of great signification for applying nano-material further. Themain achievements obtained in this research include:
1. Carboxyl and chitosan (CTS) functionalized of multi-wall carbon nanotubes(MWNT)
(1) The MWNTs was oxidized with mixture of concentrated sulfuric acid and nitric acid.It was showed that the degree of oxidation and truncation was different even using thesame acids as oxidant. The difference was mainly caused by the preparation methods ofMWNT. According to the properties of the MWNT used in this study, the relationbetween the degree of carboxyl and oxidation time or acids strength was systematicallystudied. Usually the MWNT Was ultrasonic in different acids for 3 to 5 hours, and theproper oxidized carboxyl MWNT can be obtained.
(2) The dispersancy of CTs functionalized MWNT was studied, and found that the watersolution of it could be keep symmetrical suspend state for a several days. The CTsfunctionalized MWNT was characterized by FT-IR, SEM and electrochemistry. The effectand mechanism of them was also studied.
2. A new kind of CTs/CNT modified electrode was constructed and it's applications inelectrical analytical chemistry were investigated.
A lacunaris interface was formed in which CTs and CNT were intertwisted. And theunique performance of CNT and adsorption, complexation effect of CTs were combined.The modified electrode applied to the sensitive and selective determination DA from AAand electrocatalytic determination of I~-, Pb~(2+), Sn~(2+).
引文
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