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摘要: 以聚碳酸酯膜为硬模板，表面活性剂P123为软模板，结合微波法和萃取脱模法制备出SBA-15型有机/无机复合介孔膜。通过扫描电子显微镜方法进行表征。实验结果表明：通过该方法，在聚碳酸酯膜的亚微米（200 nm）孔道中组装长度为9μm、直径为200nm的一文棒状介孔材料及其阵列，且该一文棒状介孔材料具有有序的751方介孔结构，介孔孔径为6.0 nm。以偏苯三甲酸酐与尿素和CoC12反应，再水解合成了2,9,16,23-四羧基钴酞菁化合物，利用吸附酞菁的复合介孔膜制备成有机/无机复合介孔膜化学修饰电极。研究发现：在PH=6的磷酸缓冲溶液中，该电极上的2,9,16,23-四羧基钴酞菁表现出很好的直接电化学行为，其循环伏安（CV）曲线上显示出明显的还原峰，还原峰的峰电位为-0.5V（vs. Ag/AgCl）。扫速实验结果表明：氧化峰和还原峰的峰电位不随扫描的变化而改变，且峰电流与扫速的一次方成正比。上述实验结果表明：2,9,16,23-四羧基钴酞菁在该化学修饰电极上的电化学反应过程是一个表面控制的快速电子转移过程。
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另外，本工作还进一步考察了该化学修饰电极对氧的电催化还原作用。实验结果表明：该化学修饰电极对氧具有很好的电催化还原能力，并具有良好的重现性和稳定性，因此，该化学修饰电极可用于氧的分析和检测。
关键词: 微波法；固相法；有机/无机复合介孔膜；2,9,16,23-四羧基钴酞菁；直接电化学；电催化4847
Study of Electrochemical Sensor Organic/inorganic Hybrid Mesoporous Membrane
Abstract: In this work, SBA-15 organic/inorganic hybrid mesoporous membrane was synthesized by employing the microwave-assisted method combined with solvent-extraction, as well as by using polycarbonate filtration membrane（PC）as the hard template and P123 as the soft template. Scanning electron microscopy (SEM) were used to characterize the morphology and structures of as-prepared membrane. The experimental result shows that one-dimensional silica rods and their arrays with 9μm in length and 200nm in diameter formed inside the channels of polycarbonate membrane. Those rods are mesoporous silica rods with hexagonal mesoporous structure and the mesopore size is 6.0nm. 2,9,16,23- Tetracarboxylic cobalt phthalocyanines were prepared by the reaction of trimellitic anhydride with urea and CoCl2•6H2O. Then, the direct electrochemistry of Phthalocynaines immobilized on organic/inorganic hybrid mesoporous membrane modified on a glassy carbon electrode（GCE）was studied. The CV results illuminate that Phthalocynaines existed on such a chemically modified electrode (CME) displayed irreversible reduction-behavior with reduction peak at the potential of -0.5V (vs. Ag/AgCl). The scan rate experiment shows that the potential of oxidation peak and reduction peak does not change with the scan rate. And the relationship of peak current and scan rate is completely proportional. All of above results indicate that the electrochemical reaction of 2,9,16,23- Tetracarboxylic cobalt phthalocyanine on such a chemically modified electrode is a surface-controlled process with a fast electron transfer.
Furthermore, it was found that there are well-defined electrocatalytic responses to the reduction of oxygen for such a CME, which can be used to develop a novel electrochemical-sensor for oxygen. The results demonstrate that the electrocatalytic response of such a CME presents good reproducibility and stability. Thus, such a chemically modified electrode can be applied into the analysis of oxygen peroxide.
KeyWords: microwave-assisted method; Solid-phase method; Organic/inorganic hybrid mesoporous membrane; 2,9,16,23-Tetracarboxylic cobalt phthalocyanine; Direct electrochemistry; Electrocatalysis
目录
1 绪论 5
1.1 酞菁化合物的结构特点及应用 5