本文關(guān)鍵詞：二硫化鉬納米復(fù)合物的制備及其對(duì)水中亞硝酸鹽的電催化性能研究　出處：《揚(yáng)州大學(xué)》2017年碩士論文　論文類(lèi)型：學(xué)位論文

  更多相關(guān)文章： 亞硝酸根 電催化 二硫化鉬 四氧化三鐵 纖維素 聚苯胺

【摘要】：亞硝酸根是氮循環(huán)的中間產(chǎn)物之一,廣泛存在于與生命過(guò)程密切相關(guān)的土壤、天然水和食品中。由食物鏈進(jìn)入人體的亞硝酸根不僅能夠與血色素結(jié)合或氧化低鐵血紅蛋白生成高鐵血紅蛋白,造成人體缺氧中毒,而且能夠與胃液中不同的胺類(lèi)反應(yīng)產(chǎn)生致癌的亞硝胺類(lèi),進(jìn)而引起消化系統(tǒng)器官的癌變。此外,空氣中各種含氮污染物也常轉(zhuǎn)化為亞硝酸根。因此,簡(jiǎn)便、快速定量分析亞硝酸根具有重要的意義。目前,檢測(cè)廢水中亞硝酸根的方法主要有N-(1-萘基)-胺光法、紫外分光光度法、示波極譜法、離子色譜法和電催化法。其中,電催化法具有準(zhǔn)確、簡(jiǎn)便、成本低等特點(diǎn)。本論文針對(duì)亞硝酸根離子快速準(zhǔn)確的檢測(cè)問(wèn)題,了解了亞硝酸鹽的污染危害、處理方法及檢測(cè)方法;通過(guò)材料復(fù)合,制備出Fe304-MoS2、TOSC-MoS2和PANI-MoS2三種新型納米復(fù)合物,對(duì)亞硝酸根具有優(yōu)良的電催化效果,并可以對(duì)亞硝酸根在不同線(xiàn)性濃度范圍內(nèi)進(jìn)行線(xiàn)性檢測(cè)。這種方法簡(jiǎn)單又準(zhǔn)確,具有很強(qiáng)的現(xiàn)實(shí)意義。本文的主要結(jié)論如下:(1)本論文制備了 Fe3O4-MoS2、TOSC(被TEMPO氧化的纖維素)-MoS2和聚苯胺(PANI)-MoS2三種納米復(fù)合物,并對(duì)三種材料分別表征。Fe3O4-MoS2的HRTEM和FT-IR結(jié)果顯示Fe304納米球在MoS2納米片上均勻分布,已經(jīng)復(fù)合成功;XPS表明存在三種形式的氧,包括晶格氧,羥基基團(tuán)和S-OH。TOSC-MoS2的SEM和TEM圖像顯示TOSC是一個(gè)碳納米管結(jié)構(gòu),MoS2分布在TOSC基片的邊緣;FT-IR和XRD結(jié)果顯示兩者已經(jīng)成功復(fù)合。PANI-MoS2的FT-IR和XRD結(jié)果顯示兩者已經(jīng)成功復(fù)合。(2)通過(guò)水熱法合成了新型Fe3O4-MoS2納米復(fù)合材料。Fe3O4-MoS2材料的修飾玻碳電極(GCE)與Fe304和MoS2修飾玻碳電極比有最好的電化學(xué)活性。安培響應(yīng)曲線(xiàn)的結(jié)果表明Fe3O4-MoS2修飾玻碳電極可以在1.0-2630μM的線(xiàn)性范圍內(nèi)檢測(cè)亞硝酸根的濃度,檢出限為0.5μM。(3)通過(guò)水熱法合成了新型TOSC-MoS2納米復(fù)合材料。TOSC-MoS2修飾玻碳電極是一個(gè)簡(jiǎn)單的、無(wú)酶的電化學(xué)傳感器。循環(huán)伏安法結(jié)果顯示TOSC-MoS2對(duì)于亞硝酸根的氧化有很好的電催化活性。安培響應(yīng)曲線(xiàn)的結(jié)果表明TOSC-MoS2修飾玻碳電極可以在6.0-3140和3140-4200μM的線(xiàn)性范圍內(nèi)檢測(cè)亞硝酸根的濃度,檢出限為2.0μM。這個(gè)傳感器有很好的抗干擾特性。(4)通過(guò)水熱法和原位聚合法合成了新型PANI-MoS2新型納米復(fù)合材料。循環(huán)伏安法結(jié)果顯示相比MoS2和PANI以及其他的PANI-MoS2修飾玻碳電極,PANI-0.1 gMoS2修飾玻碳電極在0.1MPBS溶液中具有更好的電化學(xué)活性。循環(huán)伏安法的結(jié)果同樣表明在pH=5的PBS溶液中,PANI-0.1gMoS2可以氧化亞硝酸根。安培響應(yīng)曲線(xiàn)的結(jié)果表明PANI-0.1gMoS2修飾玻碳電極可以在4.0-4834μM的線(xiàn)性范圍內(nèi)檢測(cè)亞硝酸根的濃度,檢出限為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.
【學(xué)位授予單位】：揚(yáng)州大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類(lèi)號(hào)】：X832;O657.1;TB33

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