二硫化钼纳米复合物的制备及其对水中亚硝酸盐的电催化性能研究

发布时间：2018-01-14 12:39

本文关键词：二硫化钼纳米复合物的制备及其对水中亚硝酸盐的电催化性能研究　出处：《扬州大学》2017年硕士论文　论文类型：学位论文

【摘要】：亚硝酸根是氮循环的中间产物之一,广泛存在于与生命过程密切相关的土壤、天然水和食品中。由食物链进入人体的亚硝酸根不仅能够与血色素结合或氧化低铁血红蛋白生成高铁血红蛋白,造成人体缺氧中毒,而且能够与胃液中不同的胺类反应产生致癌的亚硝胺类,进而引起消化系统器官的癌变。此外,空气中各种含氮污染物也常转化为亚硝酸根。因此,简便、快速定量分析亚硝酸根具有重要的意义。目前,检测废水中亚硝酸根的方法主要有N-(1-萘基)-胺光法、紫外分光光度法、示波极谱法、离子色谱法和电催化法。其中,电催化法具有准确、简便、成本低等特点。本论文针对亚硝酸根离子快速准确的检测问题,了解了亚硝酸盐的污染危害、处理方法及检测方法;通过材料复合,制备出Fe304-MoS2、TOSC-MoS2和PANI-MoS2三种新型纳米复合物,对亚硝酸根具有优良的电催化效果,并可以对亚硝酸根在不同线性浓度范围内进行线性检测。这种方法简单又准确,具有很强的现实意义。本文的主要结论如下:(1)本论文制备了 Fe3O4-MoS2、TOSC(被TEMPO氧化的纤维素)-MoS2和聚苯胺(PANI)-MoS2三种纳米复合物,并对三种材料分别表征。Fe3O4-MoS2的HRTEM和FT-IR结果显示Fe304纳米球在MoS2纳米片上均匀分布,已经复合成功;XPS表明存在三种形式的氧,包括晶格氧,羟基基团和S-OH。TOSC-MoS2的SEM和TEM图像显示TOSC是一个碳纳米管结构,MoS2分布在TOSC基片的边缘;FT-IR和XRD结果显示两者已经成功复合。PANI-MoS2的FT-IR和XRD结果显示两者已经成功复合。(2)通过水热法合成了新型Fe3O4-MoS2纳米复合材料。Fe3O4-MoS2材料的修饰玻碳电极(GCE)与Fe304和MoS2修饰玻碳电极比有最好的电化学活性。安培响应曲线的结果表明Fe3O4-MoS2修饰玻碳电极可以在1.0-2630μM的线性范围内检测亚硝酸根的浓度,检出限为0.5μM。(3)通过水热法合成了新型TOSC-MoS2纳米复合材料。TOSC-MoS2修饰玻碳电极是一个简单的、无酶的电化学传感器。循环伏安法结果显示TOSC-MoS2对于亚硝酸根的氧化有很好的电催化活性。安培响应曲线的结果表明TOSC-MoS2修饰玻碳电极可以在6.0-3140和3140-4200μM的线性范围内检测亚硝酸根的浓度,检出限为2.0μM。这个传感器有很好的抗干扰特性。(4)通过水热法和原位聚合法合成了新型PANI-MoS2新型纳米复合材料。循环伏安法结果显示相比MoS2和PANI以及其他的PANI-MoS2修饰玻碳电极,PANI-0.1 gMoS2修饰玻碳电极在0.1MPBS溶液中具有更好的电化学活性。循环伏安法的结果同样表明在pH=5的PBS溶液中,PANI-0.1gMoS2可以氧化亚硝酸根。安培响应曲线的结果表明PANI-0.1gMoS2修饰玻碳电极可以在4.0-4834μM的线性范围内检测亚硝酸根的浓度,检出限为1.5μM。
[Abstract]:Nitrite is one of the intermediate products of nitrogen cycle and widely exists in soil which is closely related to life process. Natural water and food. The nitrite that enters the human body from the food chain can not only combine with hemoglobin or oxidize low iron hemoglobin to produce methemoglobin, resulting in anoxic poisoning of human body. And different amines in gastric juice can produce carcinogenic nitrosamines, which can lead to carcinogenesis of digestive organs. In addition, various nitrogen pollutants in the air are often converted to nitrite. Therefore, it is simple and convenient. The rapid quantitative analysis of nitrite is of great significance. At present, the main methods for the detection of nitrite in wastewater are N-N 1-naphthyl carbamine-amine method, ultraviolet spectrophotometry and oscillographic polarography. Ion chromatography and electrocatalysis. Among them, electrocatalysis has the characteristics of accuracy, simplicity, low cost and so on. In this paper, the pollution hazards of nitrite have been understood in view of the rapid and accurate detection of nitrite ion. Treatment method and detection method; Fe304-MoS2TOSC-MoS2 and PANI-MoS2 nanocomposites were prepared by composite materials, which have excellent electrocatalytic effect on nitrite. The method is simple and accurate for the linear detection of nitrite in different linear concentration range. The main conclusions of this paper are as follows: 1) Fe3O4-MoS2 has been prepared in this paper. Tosc (cellulose / MoS _ 2 and Polyaniline / PANI- MoS _ 2 nanocomposites) were oxidized by TEMPO. The results of HRTEM and FT-IR of Fe _ 3O _ 4-MoS _ 2 show that the Fe304 nanospheres are uniformly distributed on MoS2 nanoparticles and have been recombined successfully. XPS shows that there are three forms of oxygen, including lattice oxygen, hydroxyl group and S-OH.TOSC-MoS2 SEM and TEM images show that TOSC is a carbon nanotube structure. MoS2 was distributed on the edge of TOSC substrate. FT-IR and XRD results show that both have been successfully combined. PANI-MoS2 FT-IR and XRD results show that both have been successfully combined. A novel Fe3O4-MoS2 nanocomposite, Fe _ 3O _ 4-MoS _ 2 modified glassy carbon electrode, was synthesized by hydrothermal method. Compared with Fe304 and MoS2 modified glassy carbon electrode, the electrochemical activity of Fe3O4-MoS2 modified glassy carbon electrode was the best. The results of amperometric response curve showed that Fe3O4-MoS2 modified glassy carbon electrode could be used in the range of 1.0-2630 渭 M. The concentration of nitrite was detected in the range of sex. The detection limit is 0.5 渭 M. ~ (3)) A novel TOSC-MoS2 nanocomposite. TOSC-MoS _ 2 modified glassy carbon electrode was synthesized by hydrothermal method. Enzymatic electrochemical sensors. Cyclic voltammetry showed that TOSC-MoS2 had good electrocatalytic activity for nitrite oxidation. Amperometric response curve showed that TOSC-MoS2 modified glass. The concentration of nitrite can be detected by carbon electrode in the linear range of 6.0-3140 and 3140-4200 渭 M. The detection limit is 2.0 渭 M. this sensor has good anti-jamming characteristics. Novel PANI-MoS2 nanocomposites were synthesized by hydrothermal method and in situ polymerization. Cyclic voltammetry showed that compared with MoS2, PANI and other PANI-MoS2 modification, the results of cyclic voltammetry showed. Glassy carbon electrode. PANI-0.1 gMoS2 modified glassy carbon electrode has better electrochemical activity in 0.1 MPBS solution. Cyclic voltammetry also shows that the electrode is in PBS solution of pH=5. PANI-0.1gMoS2 can oxidize nitrite. The results of amperometric response curve show that the linear range of PANI-0.1gMoS2 modified glassy carbon electrode is 4.0-4834 渭 M. The concentration of nitrite was detected. The detection limit was 1.5 渭 M.
【学位授予单位】：扬州大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：X832;O657.1;TB33

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