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研究生： 魏豪正
Wei, Hao-Cheng
論文名稱： 草酸於異相光催化系統降解偶氮染料之研究
Study on the heterogeneous photocatalytic system by using oxalic acid for the degradation of azo dye Reactive Black 5
指導教授： 陳志勇
Chen, Chih-Yung
學位類別： 碩士
Master
系所名稱： 工學院 - 化學工程學系
Department of Chemical Engineering
論文出版年： 2006
畢業學年度： 94
語文別： 中文
論文頁數： 139
中文關鍵詞： 異相催化 、吸附 、鐵氧化物 、偶氮染料
外文關鍵詞： Iron oxide, heterogeneous catalysis, azo dye, adsorption
相關次數： 點閱：114  下載：1 
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    • 摘要
    本研究主要分兩大部份，第一部份結合光源、鐵氧化物B1觸媒與草酸處理反應性偶氮染料Reactive Black 5，稱為異相Photo-Fenton法。此法利用草酸於開光及有氧系統會氧化成氫氧自由基之特性來降解偶氮染料。研究內容包括：背景實驗、pH值、草酸加藥量之探討、溶鐵量研究。並針對系統差異做TOC分析，進行有氧、無氧狀態之影響探討與觸媒重複利用之研究等。
    實驗結果顯示染料降解反應的最適操作條件是pH值為5、草酸加藥量為30 mg/L，處理結果顯示染料脫色程度與礦化指標分別達90 %與40 %左右，此外，研究顯示溶液在曝空氣的有氧狀態下比曝氮氣的無氧狀態有更快的降解染料速率，最後依此結果來推測出反應機制。
    第二部份進行B1觸媒吸附草酸之動力研究，由染料降解實驗中發現B1觸媒和草酸能有效錯合，會進行染料與草酸彼此之間的競爭吸附，影響異相Photo-Fenton法處理效果，主要探討吸附動力之模式，操作變因包括：背景電解質、pH值、溫度、B1觸媒量。
    動力實驗結果顯示最佳操作條件為pH控制於5，觸媒量為20 g/L且背景電解質不會影響反應結果，此時觸媒吸附草酸系統符合二階動力吸附模式。

    Abstract
    This study is composed of two parts. The first was the application of heterogeneous photo-catalysis system by introducing into light source, B1 catalyst, and oxalic acid to degrade the azo dye Reactive Black 5(RB5), which is known as the Photo-Fenton method. The oxalic acid was able to produce hydrogen radical by itself in the light system and thereby degrade RB5. The contents of this part include：background experiment, pH effect, the dosage of oxalic acid, the effect of soluble iron, etc. In light of the characteristics of this system, some tests as TOC analysis, the experiment with air or nitrogen and recycle catalyst were also done.
    From the first part, it indicated that the optimal situation takes place when the pH value was 5 and the dosage of oxalic acid was at 30 mg/L. As a result, about 90 % de-colorization was measured and 40 % mineralization was eliminated at pH 5 in the presence of 10 g/L B1, 30 mg/L oxalic acid, and a light under 15W UVA. Besides, it had faster degradable rate in the system with air than it did in the nitrogen system. According to these results, we could infer the mechanism as to how those were reacted to each other.
    In the second part of this study, the experiment of adsorption was discussed. It was found that oxalic acid was easily adsorbed by the surface of B1 catalyst. Therefore, some experiments were done in search of the balance between dynamics and thermodynamics. Due to the fact that the dyestuff and oxalic acid will complete for adsorption, the effect of the Photo-Fenton method were greatly influenced. In this part, the effect of electrolyte, pH value, temperature, the dosage of B1 catalyst and dynamic models are important parameters.
    Our research shows that the best operational condition was set at pH 5 when the dosage of catalyst was at 20 g/L and the electrolyte could not interfere with the result. The system confirms the Pseudo-Second order model.

    目錄 中文摘要.....................................................................Ⅰ 英文摘要.....................................................................Ⅱ 致 謝.....................................................................Ⅲ 目 錄.....................................................................Ⅴ 表目錄.....................................................................Ⅸ 圖目錄.....................................................................Ⅹ 符號表...................................................................ⅩⅣ 第一章 緒論...................................................................1 第二章 文獻回顧...............................................................4 2-1 染料性質與應用........................................................4 2-1-1 染料之簡介.....................................................4 2-1-2 偶氮染料.......................................................4 2-1-3 染料基本結構...................................................5 2-1-4 染料使用與污染現況.............................................6 2-2 染整廢水之處理技術....................................................8 2-2-1 物理法.........................................................8 2-2-2 化學法.........................................................9 2-2-3 生物處理法....................................................10 2-2-4 利用高級氧化技術來處理含偶氮染料之廢水........................11 2-3 草酸於紫外光催化下自生雙氧水.........................................24 第三章 實驗方法與儀器設備....................................................29 3-1 實驗架構.............................................................30 3-1-1 異相光催化反應處理偶氮染料(Reactive Black5)...................30 3-1-2 不同擔體吸附草酸之研究........................................31 3-2 吸附材料基本性質鑑定.................................................32 3-2-1 表面型態觀察..................................................32 3-2-2 表面元素分析..................................................32 3-2-3 比表面積與孔徑分佈............................................33 3-2-4 化學結構分析..................................................33 3-2-5 晶相分析......................................................33 3-2-6 覆膜總鐵量分析................................................34 3-2-7 真密度與孔隙率量測............................................35 3-3 反應性偶氮染料(Reactive Black 5)降解實驗.............................36 3-3-1 實驗藥品......................................................36 3-3-2 實驗設備......................................................36 3-3-3 實驗裝置......................................................37 3-3-4 實驗步驟......................................................37 3-4 草酸吸附實驗.........................................................39 3-4-1 實驗藥品......................................................39 3-4-2 實驗設備......................................................39 3-4-3 實驗裝置......................................................40 3-4-4 恆溫吸附動力實驗..............................................40 3-5 分析方法.............................................................42 3-5-1 偶氮染料分析方法..............................................42 3-5-2 鐵分析方法....................................................43 3-5-3 草酸分析方法..................................................45 第四章 實驗結果與討論........................................................47 4-1 吸附材料基本性質與篩選...............................................48 4-1-1 物理性質分析..................................................48 4-1-2 表面型態與元素分析............................................49 4-1-3 吸附材料篩選..................................................61 4-2 Photo-Fenton法降解反應性偶氮染料之探討...............................66 4-2-1 光源..........................................................66 4-2-2 試藥UV分析....................................................67 4-2-3 背景實驗......................................................69 4-2-4 pH值..........................................................75 4-2-5 草酸加藥量....................................................77 4-2-6 溶鐵量及系統差異性............................................79 4-2-7 IC、TOC分析...................................................82 4-2-8 無氧狀態之探討................................................85 4-2-9 觸媒重複利用之研究............................................92 4-2-10反應機制探討..................................................94 4-3 鐵氧化物吸附草酸之探討..............................................102 4-3-1 背景實驗.....................................................102 4-3-2 背景電解質之影響.............................................104 4-3-3 吸附量與pH值之關係...........................................106 4-3-4 吸附量與溫度之關係...........................................108 4-3-5 不同觸媒擔體量對吸附草酸之比較...............................110 4-3-6 反應機制探討.................................................117 第五章 結論與建議...........................................................122 5-1 結論................................................................122 5-2 建議................................................................125 參考文獻....................................................................126 附 錄....................................................................137 自 述....................................................................139 表目錄 表2.1 氧化電位表..........................................................13 表2.2 Fenton系統相關反應及速度常數........................................14 表2.3 高級氧化技術──Fenton之參考文獻整合................................15 表2.4 UV/H2O2系統中相關反應及速度常數.....................................19 表2.5 高級氧化技術──UV/H2O2之參考文獻整合...............................20 表2.6 高級氧化技術──Photo-Fenton均相反應參考文獻整合....................23 表2.7 高級氧化技術──Photo-Fenton異相反應參考文獻整合....................23 表2.8 Photo-Fenton系統相關反應及速度常數..................................24 表2.9 鐵離子與草酸相關平衡常數............................................25 表4.1 觸媒B1、T1、SiG吸附材料之物理性質分析...............................48 表4.2 有氧系統之背景實驗對反應性染料降解的操作條件........................72 表4.3 IC分析有機酸之面積值................................................83 表4.4 無氧系統之背景實驗對反應性染料降解的操作條件........................87 表4.5 草酸溶液體積量對B1擔體吸附程度之影響...............................102 表4.6 B1觸媒吸附草酸之動力學參數值.......................................112 表4.7 B1觸媒吸附草酸之各種平衡曲線方程及參數值...........................121 表4.8 B1觸媒吸附草酸之各種熱力學參數值...................................121 圖目錄 圖2.1 草酸與鐵氧化物相關反應之機制........................................27 圖3.1 異相光催化處理Reactive Black 5實驗流程圖............................30 圖3.2 觸媒吸附草酸之實驗流程圖............................................31 圖3.3 Reactive Black 5結構................................................36 圖3.4 反應裝置圖..........................................................37 圖3.5 Jar-test實驗裝置圖..................................................40 圖3.6 反應性染料Reactive Black 5 UV光譜圖.................................42 圖3.7 染料Reactive Black 5對不同pH值之UV光譜圖............................43 圖3.8 亞鐵離子濃度檢測之校正曲線..........................................45 圖3.9 草酸濃度(0~100 mg/L)檢測之校正曲線..................................46 圖3.10 草酸濃度(0~10 mg/L)檢測之校正曲線...................................46 圖4.1 B1磚粉擔體與觸媒的XRD圖譜...........................................49 圖4.2 T1磚粉擔體與觸媒的XRD圖譜...........................................50 圖4.3 SiG磚粉擔體與觸媒的XRD圖譜..........................................50 圖4.4 B1擔體底材Brick之SEM圖..............................................52 圖4.5 B1觸媒之SEM圖.......................................................52 圖4.6 T1擔體底材Brick之SEM圖..............................................53 圖4.7 T1觸媒之SEM圖.......................................................54 圖4.8 SiG擔體底材SiO2之SEM圖..............................................54 圖4.9 SiG觸媒之SEM圖......................................................55 圖4.10 B1底材磚粉表面元素EDS分析圖.........................................56 圖4.11 B1觸媒表面元素EDS分析圖.............................................56 圖4.12 T1底材磚粉表面元素EDS分析圖.........................................56 圖4.13 T1觸媒表面元素EDS分析圖.............................................57 圖4.14 SiG底材SiO2表面元素EDS分析圖........................................57 圖4.15 SiG觸媒表面元素EDS分析圖............................................57 圖4.16 B1底材以及觸媒的FTIR分析圖譜........................................59 圖4.17 T1底材以及觸媒的FTIR分析圖譜........................................60 圖4.18 SiG底材以及觸媒的FTIR分析圖譜.......................................60 圖4.19 不同鐵氧化物觸媒降解反應性偶氮染料之比較............................62 圖4.20 不同鐵氧化物觸媒對草酸吸附程度之影響................................64 圖4.21 不同鐵氧化物觸媒對草酸吸附量之影響..................................65 圖4.22 紫外光源UV光譜圖....................................................67 圖4.23 各試藥單一成分UV光譜圖..............................................68 圖4.24 雙成分試藥UV光譜圖..................................................68 圖4.25 反應性染料Reactive Black 5基本結構圖................................69 圖4.26 染料Reactive Black 5對不同pH值之UV光譜圖............................70 圖4.27 pH值對UV波長591 nm吸收值之影響......................................71 圖4.28 背景實驗對反應性染料降解的影響......................................73 圖4.29 不同草酸添加量對反應性染料吸附圖....................................74 圖4.30 pH對反應性染料降解圖................................................76 圖4.31 草酸添加量對反應性染料降解圖........................................78 圖4.32 Heterogeneous系統於空氣下之溶鐵曲線.................................79 圖4.33 草酸經B1觸媒對偶氮染料脫色效果的UV降解圖............................80 圖4.34 系統於空氣下之均相反應與異相反應的比較圖............................81 圖4.35 Reactive Black 5降解之中間有機酸的IC圖..............................83 圖4.36 Reactive Black 5 於有氧系統之TOC降解圖..............................84 圖4.37 有氧系統下，草酸、RB5與中間產物之礦化程度分析.......................84 圖4.38 反應性染料於氮氣系統之背景實驗圖....................................89 圖4.39 Reactive Black 5於氮氣系統之UV光譜圖................................90 圖4.40 Heterogeneous系統於氮氣下之溶鐵曲線.................................90 圖4.41 有無溶氧狀態對Reactive Black 5降解之影響............................91 圖4.42 觸媒重複利用對Reactive Black 5降解之探討............................93 圖4.43 草酸鹽在不同pH下存在物種的分佈圖....................................95 圖4.44 草酸與亞鐵離子於不同pH值下各物種之分佈圖............................98 圖4.45 草酸、亞鐵離子與其錯合物於不同pH值下各成分之分佈圖..................98 圖4.46 含氧系統中偶氮染料、草酸以及B1觸媒之反應機制探討...................100 圖4.47 無氧系統中偶氮染料、草酸以及B1觸媒之反應機制探討...................101 圖4.48 比較日光燈與無光源對於B1觸媒擔體吸附草酸之影響.....................103 圖4.49 不同背景電解質強度對B1觸媒擔體吸附草酸之影響.......................105 圖4.50 草酸平衡吸附量與pH值之關係.........................................107 圖4.51 改變溫度於B1觸媒吸附草酸之探討.....................................108 圖4.52 改變溫度於B1觸媒吸附草酸的飽和吸附量之探討.........................109 圖4.53 不同B1觸媒擔體量吸附草酸之研究.....................................113 圖4.54 草酸平衡吸附量於不同克數B1觸媒擔體.................................114 圖4.55 草酸吸附平衡對Lagergern first order model之探討....................115 圖4.56 草酸吸附平衡對Pseudo second order model之探討......................115 圖4.57 草酸吸附平衡對Webber-Morris model之探討............................116 圖4.58 草酸吸附平衡對Urano-Tachikawa model之探討..........................116 圖4.59 不同pH條件下草酸鐵離子錯合物之型態.................................119 圖4.60 草酸與三價鐵離子錯合物於不同pH條件下之分布圖.......................120 圖4.61 鐵氧化物觸媒與草酸根離子吸附之反應機制.............................121 圖A-1 IC分析硝酸之校正曲線...............................................137 圖A-2 IC分析硫酸之校正曲線...............................................137 圖A-3 IC分析草酸之校正曲線...............................................138 圖A-4 American Dye Manufacturers Institute (ADMI)分析....................138

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