本文選題：EDTA-Fe插層水滑石 + 偶氮胭脂紅B�。� 參考：《湘潭大學》2016年碩士論文

【摘要】：為了解決目前異相光-Fenton反應(yīng)體系中反應(yīng)pH值較低,以及傳統(tǒng)單因素實驗方法存在的耗時長、成本高且過程復(fù)雜的問題,本論文制備了負載有含鐵絡(luò)合物的異相光-Fenton反應(yīng)催化劑,并運用響應(yīng)曲面法(RSM)對偶氮胭脂紅B的異相光-Fenton降解過程進行了研究,還針對反應(yīng)體系中可能存在的活性物種進行了檢測,推測其反應(yīng)機理。取得了以下一些研究成果：(1)通過離子交換法成功制備了EDTA-Fe插層水滑石(EDTA-Fe-LDH)異相光-Fenton催化材料。X射線衍射分析(XRD)、傅立葉變換紅外光譜(FTIR)等結(jié)果表明[FeEDTA]-順利插入鋅鋁水滑石(ZnAl-LDH)的層間；經(jīng)紫外可見漫反射(UV-Vis)圖譜分析表明EDTA-Fe-LDH對整個紫外光區(qū)域都具有明顯的吸收性能；氮吸附-脫附等溫線、掃描電鏡(SEM)則顯示經(jīng)離子交換法制備的EDTA-Fe-LDH相較于ZnAl-LDH具有更大的比表面積和孔體積。而通過對偶氮胭脂紅B的光-Fenton降解實驗得出EDTA-Fe-LDH在紫外光輻射下具有較高的催化活性和穩(wěn)定性。(2)采用Box-Behnken設(shè)計(BBD)對異相光-Fenton反應(yīng)體系的實驗條件進行優(yōu)化,結(jié)果顯示當pH值為6.54、偶氮胭脂紅B的濃度為100 mg/L、過氧化氫的濃度為11.5 mM時具有最佳的反應(yīng)效果,在此條件下偶氮胭脂紅B的實際脫色率和TOC去除率分別為97.27%和90.36%,與BBD設(shè)計的預(yù)測結(jié)果相符。(3)通過實驗證實在異相光-Fenton反應(yīng)體系中有三種活性物質(zhì)產(chǎn)生：羥基自由基(·OH)、超氧自由基(·O2-)和單線態(tài)氧(1O2),并對其產(chǎn)生機理繪制了相應(yīng)的示意圖。此外,還通過UV-Vis掃描圖譜及GC-MS等表征手段對偶氮胭脂紅B的降解途徑進行了分析,發(fā)現(xiàn)偶氮胭脂紅B分子首先分解為如1-亞硝基-2,4-二甲氨基苯等的具有苯環(huán)結(jié)構(gòu)的中間產(chǎn)物,接著隨著反應(yīng)的不斷進行,這些中間產(chǎn)物的苯環(huán)結(jié)構(gòu)被打開,生成了丁酸等小分子物質(zhì),最后徹底礦化為C02和H20。
[Abstract]:In order to solve the problems of low pH value in the heterogeneous photo-Fenton reaction system and the problems of long time consuming, high cost and complicated process in the traditional single-factor experimental method, a heterogeneous light-Fenton reaction catalyst loaded with iron complex was prepared in this paper. The heterogeneous photo-Fenton degradation process of azo carmine B was studied by using response surface method (RSM). The possible active species in the reaction system were detected and the reaction mechanism was speculated. The following research results have been obtained: (1) EDTA-Fe intercalated hydrotalcite EDTA-Fe-LDH has been successfully prepared by ion exchange method. The results of X-ray diffraction analysis and Fourier transform infrared spectroscopy (FTIR) show that [FeEDTA]-successfully inserted into the interlayer of zinc aluminum hydrotalcite ZnAl-LDH; The UV-Vis-UV spectra showed that EDTA-Fe-LDH had obvious absorptivity to the whole ultraviolet region, and nitrogen adsorption-desorption isotherm, the absorption isotherm of nitrogen adsorption and desorption isotherm, Scanning electron microscopy (SEM) showed that EDTA-Fe-LDH prepared by ion exchange method had larger specific surface area and pore volume than ZnAl-LDH. However, the photo-Fenton degradation experiment of azocarmine B showed that EDTA-Fe-LDH had high catalytic activity and stability under ultraviolet radiation. The Box-Behnken design was used to optimize the experimental conditions of heterogeneous light-Fenton reaction system. The results showed that when pH was 6.54, the concentration of azo carmine B was 100 mg / L, and the concentration of hydrogen peroxide was 11.5 mm, the optimum reaction effect was obtained. Under these conditions, the actual decolorization rate and TOC removal rate of azo carmine B were 97.27% and 90.36%, respectively, which were consistent with the predicted results of BBD design. Base (OHH), superoxide free radical (O _ 2-O _ 2) and singlet oxygen ~ (1) O _ (2) O _ (2), and the corresponding schematic diagram of its production mechanism is given. In addition, the degradation pathway of azocarmine B was analyzed by means of UV-Vis scanning spectrum and GC-MS characterization. It was found that azo carmine B molecules were first decomposed into intermediate products with benzene ring structure, such as 1-nitroso -2o 4- dimethylaminobenzene, etc. As the reaction proceeded, the benzene ring structure of these intermediates was opened to form small molecules, such as butyric acid, which were mineralized to CO2 and H20.
【學位授予單位】：湘潭大學
【學位級別】：碩士
【學位授予年份】：2016
【分類號】：X788

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