本文選題：微波輔助法 + 氧化石墨　； 參考：《吉林大學(xué)》2015年碩士論文

【摘要】：近年來，石墨烯及石墨烯基復(fù)合材料成為研究的熱點。研究的內(nèi)容主要是合成方法的改進(jìn)和石墨烯基復(fù)合材料應(yīng)用的拓展。在合成方法上，利用氧化石墨合成石墨烯是成本最低的一種方法，適合大批量生產(chǎn)。因此，氧化石墨合成方法的改進(jìn)也成為時下研究的重點。 本文對氧化石墨的快速合成方法進(jìn)行了探索，之后利用合成的氧化石墨制備了磁性還原氧化石墨烯并將其應(yīng)用于水樣中三嗪類除草劑的富集，結(jié)合高效液相色譜-串聯(lián)質(zhì)譜法對其進(jìn)行了檢測，實現(xiàn)了環(huán)境水樣中三嗪類污染物的快速萃取、富集、分離和檢測。具體的研究內(nèi)容分為以下三個方面： 1改進(jìn)了氧化石墨的合成方法，對比改進(jìn)的Hummers法，不但減少了硫酸的用量，而且不使用亞硝酸鈉，避免了氮氧化物有毒氣體的釋放。利用微波加熱法，將反應(yīng)時間從12h縮短至30s，獲得了氧化程度較高的氧化石墨。該方法具有操作簡單，合成效率高的特點。另外，為了改進(jìn)常壓微波輔助法在合成過程中有酸霧釋放，反應(yīng)條件不易控制等缺點，利用高壓微波法合成了氧化石墨。在70℃的反應(yīng)溫度下制備了氧化石墨，反應(yīng)過程比常壓微波輔助法更加溫和。對這兩種方法合成的氧化石墨進(jìn)行了表征，結(jié)果表明產(chǎn)物的氧化程度較好。 2用溶劑熱還原法成功地合成了磁性還原氧化石墨烯（magnetic reducedgraphene oxide，M-RGO），并對其做了詳細(xì)的表征。表征結(jié)果表明磁性粒子主要由Fe3O4組成，具有很好的磁性（飽和磁化強(qiáng)度70emu g-1）。通過掃描電鏡圖可以看出磁性還原氧化石墨烯具有很好的形貌，F(xiàn)e3O4粒子呈球形，粒徑為500nm左右，均勻的分布在石墨烯片層上。這種石墨烯基復(fù)合材料對三嗪類除草劑有強(qiáng)烈的吸附作用，在水質(zhì)凈化和水質(zhì)分析上有很好的應(yīng)用前景。 3建立了用磁性還原氧化石墨烯作為吸附劑結(jié)合高效液相色譜-串聯(lián)質(zhì)譜法檢測水中三嗪類除草劑的分析方法。磁性還原氧化石墨烯對含苯環(huán)的小分子有很好的吸附作用，同時磁性粒子對還原氧化石墨烯的修飾能使其快速從復(fù)雜體系中分離。用磁性還原氧化石墨烯做吸附劑富集水中三嗪類除草劑，富集倍數(shù)可達(dá)500倍。優(yōu)化了萃取條件，吸附劑的量為70mg，吸附時間10min，上樣pH為7，洗脫溶劑為丙酮，洗脫體積為4mL，在最佳萃取條件下，采用高效液相色譜-串聯(lián)質(zhì)譜法進(jìn)行分析，方法的檢出限為0.16-0.52ng L-1，回收率在72-96%之間。運(yùn)用該方法成功地檢測了長春市內(nèi)三個環(huán)境水樣中的三嗪類除草劑，，結(jié)果令人滿意。
[Abstract]:In recent years, graphene and graphene matrix composites have become the focus of research. The main contents of the research are the improvement of synthesis method and the application of graphene-based composites. The synthesis of graphene from graphite oxide is the lowest cost and suitable for mass production. Therefore, the improvement of graphite oxide synthesis method has also become the focus of current research. In this paper, the rapid synthesis method of graphite oxide was explored, and then the magnetic reductive graphene oxide was prepared by using the synthesized graphite oxide and applied to the enrichment of triazine herbicides in water samples. High performance liquid chromatography-tandem mass spectrometry (HPLC-MS) was used to detect the triazines in environmental water. The rapid extraction, enrichment, separation and detection of triazines in environmental water samples were achieved. The specific research contents are as follows: 1 the synthesis method of graphite oxide has been improved. Compared with the improved Hummers method, not only the amount of sulfuric acid is reduced, but also sodium nitrite is not used. The release of noxious nitrogen oxide gas is avoided. Graphite oxide with high oxidation degree was obtained by microwave heating and the reaction time was shortened from 12 h to 30 s. This method has the characteristics of simple operation and high synthesis efficiency. In addition, graphite oxide was synthesized by high pressure microwave method in order to improve the acid mist release in the synthesis process, and the reaction conditions were not easy to control. Graphite oxide was prepared at 70 鈩

本文編號：2107740