本文關(guān)鍵詞：石墨烯復(fù)合材料的制備及萃取性能研究　出處：《河南工業(yè)大學(xué)》2015年碩士論文　論文類型：學(xué)位論文

  更多相關(guān)文章： 石墨烯 聚合離子液體 磁性石墨烯 萃取性能 高效液相色譜

【摘要】：石墨烯(Graphene,G)具有比表面積大、疏水性、熱穩(wěn)定性和化學(xué)穩(wěn)定性等性質(zhì),而且它含有豐富的π電子體系,有望成為良好的吸附劑材料廣泛應(yīng)用于分離分析領(lǐng)域。但是,G的層與層間距小,范德華力和π-π相互作用力較強(qiáng),極易發(fā)生團(tuán)聚現(xiàn)象,這使其在水中或者有機(jī)溶劑中的分散性差。對(duì)G進(jìn)行功能化能賦予它更新更好的特點(diǎn),使它的應(yīng)用范圍進(jìn)一步擴(kuò)大。本文制備了G復(fù)合材料,探討它對(duì)環(huán)境中有機(jī)污染物的萃取性能及應(yīng)用。利用1-乙烯基-3-己基咪唑溴鹽與氧化石墨烯之間的靜電吸引力將其附著于氧化石墨烯表面,然后經(jīng)聚合、還原制備了聚合離子液體-G復(fù)合材料(Poly(VHIm+Br-)-G),利用掃描電子顯微鏡、傅里葉變換紅外光譜和紫外光譜等對(duì)Poly(VHIm+Br-)-G復(fù)合材料進(jìn)行了表征。首次將Poly(VHIm+Br-)-G復(fù)合材料用于SPE的吸附劑,結(jié)合HPLC,研究了該新型吸附劑對(duì)環(huán)境水樣中4種有機(jī)磷農(nóng)藥(OPPs)的萃取性能。對(duì)影響SPE效率的參數(shù)(吸附劑量、上樣體積、上樣流速、洗脫劑和洗脫劑體積)進(jìn)行了優(yōu)化。在優(yōu)化條件下,殺螟松、對(duì)硫磷、倍硫磷和辛硫磷在5-200μg L-1有良好的線性關(guān)系,相關(guān)系數(shù)(r2)為0.9908-0.9995。將建立的方法應(yīng)用于環(huán)境水樣中OPPs的測(cè)定,加標(biāo)回收率在80.0%-110.0%之間,RSD(n=3)小于4.5%。結(jié)果表明,與G相比,Poly(VHIm+Br-)-G復(fù)合材料作為SPE吸附劑,能降低萃取過程中的團(tuán)聚現(xiàn)象,對(duì)目標(biāo)分析物的萃取效能更高;建立的方法Poly(VHIm+Br-)-G-SPE-HPLC-UV適用于實(shí)際水樣中OPPs殘留的測(cè)定。利用氧化石墨烯與硫酸亞鐵之間的氧化還原性以及在堿性條件下Fe2+和Fe3+可以共沉淀形成Fe3O4,自組裝G與Fe3O4形成三維磁性石墨烯復(fù)合材料(3D-G-Fe3O4),利用傅利葉變換紅外光譜、透射電子顯微鏡、熱重分析和比表面積及孔徑分析等對(duì)其進(jìn)行結(jié)構(gòu)表征。將3D-G-Fe3O4復(fù)合材料用作MSPE的吸附劑,結(jié)合HPLC,研究其對(duì)水樣中PAHs的萃取性能。對(duì)影響MSPE效率的參數(shù)(吸附劑量、樣品體積、吸附時(shí)間、解析劑、解吸劑量及時(shí)間和鹽濃度)進(jìn)行了優(yōu)化。在優(yōu)化的條件下,萘在0.1-40.0μg L-1、聯(lián)苯在0.05-20.0μg L-1、菲在0.6-100.0μg L-1、蒽在0.2-100.0μg L-1有良好的線性關(guān)系,相關(guān)系數(shù)(r2)為0.9994-0.9997。將建立的方法應(yīng)用于環(huán)境水樣中PAHs的測(cè)定,加標(biāo)回收率在84.2%-107.0%之間,RSD(n=3)小于5.8%。與其它測(cè)定PAHs的方法比較,該方法測(cè)定環(huán)境水樣中的PAHs有好的重復(fù)性和寬的線性范圍,吸附劑用量少,減少了成本,且萃取時(shí)間短,加快了分析速率。建立的方法3D-G-Fe3O4-MSPE-HPLC-UV適用于檢測(cè)水樣中的PAHs殘留。為了進(jìn)一步探討3D-G-Fe3O4對(duì)不同種類分析物的吸附效能以及吸附機(jī)理,將3D-G-Fe3O4用作吸附劑材料,以3種多環(huán)芳烴(萘、菲和熒蒽)、3種氨基甲酸酯類(甲萘威、仲丁威和異丙威)和3種酚類(對(duì)硝基苯酚、甲萘酚和雙酚A)為目標(biāo)分析物,研究了其在3D-G-Fe3O4上的吸附等溫線和動(dòng)力學(xué)行為。結(jié)果表明,分析物結(jié)構(gòu)不同,與3D-G-Fe3O4上活性位點(diǎn)的相互作用不同,導(dǎo)致不同的吸附行為。3D-G-Fe3O4對(duì)甲萘威、對(duì)硝基苯酚、甲萘酚和雙酚A的吸附符合Langmuir吸附模型,而對(duì)萘、菲、熒蒽、仲丁威和異丙威的吸附符合Freundlich吸附模型。所有目標(biāo)分析物的吸附過程均遵循二級(jí)吸附動(dòng)力學(xué)模型。
[Abstract]:Shi Moxi (Graphene, G) with a large surface area, hydrophobicity, thermal stability and chemical stability and other properties, and it contains rich pi electron system, is expected to be widely used in the separation and analysis of good adsorbent material. However, the G layer and the layer spacing is small, van Edward and PI pi interaction the force is strong, easy to agglomerate phenomenon, which makes it in water or organic solvent in dispersion. The G function can give it the better, to further expand the scope of its application. The G composite material was prepared in this paper, it discusses on the extraction performance of organic pollutants in the environment and application by the electrostatic attraction between 1- vinyl -3- hexyl imidazolium bromide and graphene oxide will be attached to the surface of graphene oxide, then prepared by polymerization, reduction of ionic liquid polymer -G composites (Poly (VHIm+Br-) -G), by using scanning electric The electron microscope, Fourier transform infrared spectroscopy and UV spectra of Poly (VHIm+Br-) -G composites were characterized for the first time. Poly (VHIm+Br-) -G composite adsorbent for SPE, combined with HPLC, the research of the new adsorbent of 4 organophosphorus pesticides in environmental water samples (OPPs) extraction performance. The parameters affecting the efficiency of SPE (adsorption dosage, sample volume, sample flow rate, eluent and elution volume) were optimized. Under the optimized conditions, fenitrothion, parathion, fenthion and phoxim had a good linear relationship in the range of 5-200 g L-1, the correlation coefficient (R2) method for the determination of 0.9908-0.9995. the application to OPPs in environmental water samples, the recoveries were 80.0%-110.0%, RSD (n=3) is less than 4.5%.. The results showed that compared with G, Poly (VHIm+Br-) -G composite material as SPE adsorbent can reduce the agglomeration of the extraction process of target analyte The extraction efficiency is high; the Poly method (VHIm+Br- -G-SPE-HPLC-UV) was applied to the determination of OPPs residues in real water samples. The oxidation between graphene oxide and ferrous sulfate reduction and Fe2+ under alkaline conditions and Fe3+ can form Fe3O4 co precipitation, and the formation of Fe3O4 self assembled G 3D magnetic graphene composites (3D-G-Fe3O4) and by using Fourier transform infrared spectroscopy, transmission electron microscopy, thermogravimetric analysis and specific surface area and pore size distribution and characterized. The 3D-G-Fe3O4 composites used as adsorbent, MSPE combined with HPLC, the research of PAHs in water extraction performance. The parameters influencing the efficiency of the MSPE (the adsorption dose. The sample volume, time of adsorption, desorption agent, desorption time and dose and salt concentration) were optimized. Under the optimized conditions, the 0.1-40.0 g L-1 of naphthalene, biphenyl in 0.05-20.0 g L-1 0.6-100.0 g L-1, phenanthrene, anthracene There is a good linear relationship in the range of 0.2-100.0 g L-1, the correlation coefficient (R2) method for the determination of the 0.9994-0.9997. will be built based on PAHs in environmental water samples, the recoveries were 84.2%-107.0%, RSD (n=3) is less than 5.8%. and the other PAHs determination method, the determination method of PAHs is good repeatability and wide linear range, adsorbent dosage, lower cost, and shorter extraction time, speed up the rate of analysis. The 3D-G-Fe3O4-MSPE-HPLC-UV method is suitable for the detection of residues in water samples by PAHs. In order to further explore the effectiveness of different types of 3D-G-Fe3O4 on the adsorption of the analyte and the adsorption mechanism of 3D-G-Fe3O4, will be used as an adsorbent material to 3 kinds of PAHs (naphthalene, phenanthrene and fluoranthene), 3 carbamates (carbaryl, fenobucarb, Isoprocarb) and 3 kinds of phenols (p-nitrophenol, 1-naphthol and bisphenol A) as the target analyte was studied The 3D-G-Fe3O4 in the adsorption isotherm and kinetics analysis. The results show that the structure is different, different interactions with the 3D-G-Fe3O4 active site, resulting in different adsorption behavior of.3D-G-Fe3O4 for carbaryl, p-nitrophenol, phenol and bisphenol A adsorption accords with Langmuir adsorption model and of naphthalene, phenanthrene, fluoranthene, adsorption fenobucarb and Isoprocarb with Freundlich adsorption model. The adsorption process of all the objectives were to follow two adsorption kinetic model.

【學(xué)位授予單位】：河南工業(yè)大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：TQ127.11;TB33

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相關(guān)期刊論文 前1條

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本文編號(hào)：1375295