臺灣博碩士論文加值系統

本研究利用電氧化法於人工及實際TFT-LCD製程鉻蝕刻廢液中回收Ce(IV)，並以 Ce(IV)-MEO(Mediated Electrochemical Oxidation)與電氧化法降解水中乙醯氨酚。實驗結果顯示，所測試電極對乙醯氨酚之電氧化降解效能為PbO2/Sn2O3-SnO2/Ti電極 >白金電極> BDD電極；電解槽使用不同分隔膜對乙醯氨酚之電氧化降解效能為Nafion212 > AMX > CMX。不同電極所展示的電回收人工廢液之Ce(IV)產率高低，依序為PbO2/Sn2O3-SnO2/Ti(b)≒PbO2/Sn2O3-SnO2/Ti(a) > 白金 > PbO2/Ti > 鑽石> BDD；前述最佳兩支電極對乙醯氨酚電氧化60 及240 min之降解率分別為~80%及>99%。以陽極PbO2/Sn2O3-SnO2/Ti電極(1cm2、0.88 A、25℃、AMI7001分隔膜)於實際TFT-LCD鉻蝕刻廢液電回收Ce(IV) 4小時，Ce(IV)產率可達100%。於4×10-4 M硫酸或10-3 M硝酸中添加不同濃度Ce(IV)氧化降解乙醯氨酚，所得Ce(IV)之較佳劑量為1500 ppm。乙醯氨酚在4M硝酸中之60 min氧化降解率達80%，而在4M硝酸中，無論是添加1500 ppm之Ce(IV)、人工廢液電回收之Ce(IV)或實際鉻蝕刻廢液電回收之Ce(IV)，均可於60 min完全氧化降解乙醯氨酚，且其對苯醌(中間產物)之240 min氧化降解率分別為95%、99%及95%。
關鍵字：乙醯氨酚(Acetaminophen)、Ce(IV)-MEO、鉻蝕刻廢液、Ce(IV)電再生、Ce(IV)產率、降解

The Contents of Abstract in This Thesis:
In this study, electro-regeneration of Ce(IV) from Ce(III) in prepared and spent Cr-ehtching solutions used in TFT-LCD manufacturing processes was performed. The regenerated Ce(IV) was used in a Ce(IV)-mediated electrochemical oxidation (MEO) process which was then compared with direct electro-oxidation for the degradation of acetaminophen. The results showed that the magnitude of acetaminophen degradation rate on tested anodes was in order PbO2/Sn2O3SnO2/Ti > Pt > BDD, while that in the electrolytic cell using different separators was in order Nafion212 > AMX > CMX. The magnitude of Ce(IV) yield (from Ce(III) electro-oxidation) in prepared solutions follow the order of PbO2/ Sn2O3-SnO2/Ti(b) ≒PbO2/ Sn2O3-SnO2/Ti(a) > Pt > PbO2/Ti > diamond > BDD. At 25oC, the Ce(IV) reached 100% for the electrolysis of 0.2 M Ce(III) in 4 M HNO3 for 4-hr using the PbO2/Sn2O3-SnO2/Ti anode (1cm2, at 0.88 A) in a divided cell equipped with an AMI-7100 separator, In 4×10-4 M H2SO4 and 10-3 M HNO3, the optimal dosages of Ce(IV) were the same (1500 ppm) for the degradation of acetaminophen. In 4 M HNO3, the addition of 1500 ppm Ce(IV), Ce(IV) electro-regenerated in prepared solution, or Ce(IV) electro-regenerated in spent Cr-ehtching solution achieved complete oxidation/degradation of acetaminophen at 60 min; moreover, the oxidation/degradation efficiencies of p-benzoquinone (one of intermediates from the acetaminophen oxidative degradation) were 95%, 99%, and 95%, respectively, in 240 min reaction.
Keywords: Acetaminophen,Ce(IV)-MEO, Cr-etching solution, Ce(IV) electro-regeneration, Ce(IV) yield, degradation

目錄
摘 要 I
Abstract II
謝 誌 III
目 錄 IV
表目錄 IX
圖目錄 XI
第1章 前言 1
第2章 文獻回顧 2
2.1 新興污染物 2
2.2 內分泌干擾物質 4
2.3 乙醯氨酚介紹、人體危害與對環境之影響 5
2.4氧氟沙星介紹、人體危害與對環境之影響 7
2.5乙醯氨酚與氧氟沙星之氧化降解 10
2.5.1（高級）化學氧化 10
2.5.2 電化學氧化 16
2.5.2.1電化學基本原理 16
2.5.2.2離子與電解 17
2.5.2.3氧化與還原 18
2.5.2.4循環伏安法及I-T定電流法 20
2.5.2.5法拉第定律 22
2.6 TFT-LCD廢液Ce(IV)電回收 23
2.6.1 TFT-LCD廢液 23
2.6.2 Ce(IV)電回收與應用 25
2.6.3 MEO技術 26
2.6.4 Ce-(IV)MEO技術 26
2.7 陽極材料選用與製備 28
第3章 研究設備及方法 35
3.1 實驗流程 35
3.2實驗儀器設備（藥品、電極材料及分隔膜） 37
3.2.1掃描式電子顯微鏡（SEM）及能量發散光譜儀（EDS） 41
3.2.2 X-光繞射儀（XRD） 42
3.2.3高效率液相層析儀(HPLC) 43
3.2.4紫外光/可見光分光光度計（UV） 44
3.2.5自動電位滴定儀 45
3.2.6電化學分析儀 46
3.3電極的製備 47
3.3.1 PbO2/Ti電極與鑽石電極的製備 47
3.3.2 PbO2/Sn2O3-SnO2/Ti電極、PLS/PbO2/Sn2O3 -SnO2/Ti及ppy/PbO2/Sn2O3 -SnO2/Ti電極的製備 47
3.3.3 PbO2/RuO2/Sn2O3-SnO2/Ti電極的製備 48
3.3.4 Au-Ag//Ti電極之製備 49
3.3.5 Au-Ag/Sn2O3-SnO2/Ti與PbO2/Au-Ag/Sn2O3-SnO2/Ti電極之製備 49
3.3.6 PbO2/SnO2/Ti、PLS/PbO2/ SnO2/Ti與ppy/PbO2/SnO2/Ti電極之製備 50
3.4乙醯氨酚及氧氟沙星之電降解 51
3.5 Ce(IV)之電再生 51
3.6以Ce(IV)氧化降解乙醯氨酚 53
第4章 結果與討論 56
4.1製備電極表面結構分析及元素分析 56
4.2製備電極結晶相分析 63
4.3 電極材料（白金、BDD及PbO2/ Sn2O3- SnO2/Ti電極）及不同分
隔膜（AMX、CMX及Nafion212）對乙醯氨酚電氧化之影響
67
4.4不同之製備電極對乙醯氨酚電氧化之影響分隔膜（Nafion212）
70
4.5不同之製備電極對氧氟沙星電氧化之影響分隔膜（Nafion212）
72
4.6 以不同電極電氧化對之Ce(IV)產率及電流效率 74
4.6.1 Ce(III)/Ce(IV)電化學特性 77
4.7以Ce(IV)氧化降解乙醯氨酚（4.8×10-4M硫酸） 80
4.8以Ce(IV)氧化降解乙醯氨酚（10-3M硝酸） 82
4.9於4M硝酸或4M硫酸中以Ce(IV)氧化降解乙醯氨酚 84
4.10人工廢液電再生之Ce(IV)氧化降解乙醯氨酚 87
4.11於實際TFT-LCD鉻蝕刻廢液電回收之Ce(IV)氧化降解乙醯氨酚
89
第5章 結論與建議 91
5.1 結論 91
5.2 建議 92
參考文獻 93
作者簡介 102
表目錄
表2-1環境中新興污染物化合物或來源 3
表2-2為氟喹諾酮類之藥物 8
表2-3 15種新興污染物最佳吸收波長 9
表2-4間接與直接氧化之差異性 11
表2-5各種Fenton法之比較 13
表2-6氧化劑的氧化還原反應及電位 15
表2-7各物種之形成電位 15
表2-8電化學之重點 16
表2-9法拉第參數說明 22
表2-10氧化還原電位 27
表3-1 實驗所使用的藥品中英文供應商及規格 37
表3-2 實驗所使用的電極材料、分隔膜供應商及型號 39
表3-3實驗所使用的設備器材 40
表4-1. PbO2/Ti、PbO2/ Sn2O3-SnO2/Ti (a)、PbO2/ Sn2O3-SnO2/Ti (b)、鑽石、BDD及白金電極速率常數(k)及質傳係數(kL)比較 76













圖目錄
圖2-1水環境中新興污染物之來源 4
圖2-2乙醯氨酚化學結構式 5
圖2-3酚類降解途徑-以BPA為例 6
圖2-4乙醯氨酚降解途徑 7
圖2-5 氧氟沙星化學結構式 8
圖2-6氧化與還原之運用及分類 19
圖2-7循環伏安圖 20
圖2-8可逆、半可逆及不可逆之循環伏安圖 21
圖2-9為定電位時間與電流變化圖 21
圖2-10蝕刻廢液產生示意圖 24
圖2-11 MEO系統 27
圖2-12α-PbO2之XRD圖 29
圖2-13β-PbO2之XRD圖 29
圖2-14α-PbO2之SEM圖 30
圖2-15與圖2-16β-PbO2之SEM圖分別為1000X與5000X 30
圖2-17不同的電沉積時間之SEM 32
圖2-18不同的電沉積時間之EDS 33
圖2-19不同的電沉積時間之XRD 33
圖3-1 實驗架構 36
圖3-2 掃描式電子顯微鏡（SEM）及能量發散光譜儀（EDS） 41
圖3-3 X-光繞射儀（XRD） 42
圖3-4 高效能液相層析儀（HPLC） 43
圖3-5紫外光/可見光分光光度計(UV) 44
圖3-6自動電位滴定儀 45
圖3-7電化學分析儀 46
圖3-8雙槽反應槽形式 53
圖3-9以Ce(IV)氧化降解乙醯氨酚流程圖 55
圖4-1 Sn2O3 -SnO2/Ti SEM(1000x) 57
圖4-2 Sn2O3 -SnO2/Ti SEM(5000x) 57
圖4-3 PbO2/ Sn2O3 -SnO2/Ti SEM(8000x) 57
圖4-4 PbO2/ Sn2O3 -SnO2/Ti SEM(15000x) 57
圖4-5 ppy/PbO2/Sn2O3 -SnO2/Ti SEM(1000x) 57
圖4-6 ppy/PbO2/Sn2O3 -SnO2/Ti SEM(5000x) 57
圖4-7 SnO2/Ti SEM(1000x) 58
圖4-8 SnO2/Ti SEM(5000x) 58
圖4-9 PbO2/SnO2/Ti SEM(1000x) 58
圖4-10 PbO2/SnO2/Ti SEM(5000x) 58
圖4-11 ppy/PbO2/SnO2/Ti SEM(1000x) 58
圖4-12 ppy/PbO2/SnO2/Ti SEM(5000x) 58
圖4-13 鑽石電極之SEM(1000x) 59
圖4-14 鑽石電極之SEM(3000x) 59
圖4-15 Au-Ag/Ti電極之SEM(1000x) 59
圖4-16 Au-Ag/Ti電極之SEM(2000x) 59
圖4-17 Sn2O3 -SnO2/Ti電極之EDS 60
圖4-18 PbO2/SnO2/Ti電極之EDS 60
圖4-19 ppy/PbO2/Sn2O3 -SnO2/Ti電極之EDS 60
圖4-20 SnO2/Ti電極之EDS 61
圖4-21 PbO2/SnO2/Ti電極之EDS 61
圖4-22 ppy/PbO2/SnO2/Ti電極之EDS 61
圖4-23 Au-Ag/Ti電極之EDS 62
圖4-24 鑽石電極之EDS 62
圖4-25 Au-Ag/Ti電極之XRD 63
圖4-26 PbO2/Au-Ag/Sn2O3-SnO2/Ti電極之XRD 64
圖4-27 PbO2/SnO2/Ti電極之XRD 64
圖4-28 ppy/PbO2/SnO2/Ti電極之XRD 65
圖4-29 PbO2/ Sn2O3-SnO2/Ti電極之XRD 65
圖4-30 ppy/PbO2/ Sn2O3-SnO2/Ti電極之XRD 66
圖4-31 鑽石電極之XRD 66
圖4-32 白金為陽極-以不同分隔膜(AMX、CMX、Nafion212)乙醯氨酚電氧化之影響 67
圖4-33 BDD為陽極-以不同分隔膜(AMX、CMX、Nafion212)乙醯氨酚電氧化之影響 68
圖4-34 PbO2/Sn2O3-SnO2/Ti為陽極-以不同分隔膜(AMX、CMX、Nafion212)乙醯氨酚電氧化之影響 69
圖4-35不同的陽極對乙醯氨酚電氧化之影響 71
圖4-36不同的製備電極對氧氟沙星電氧化之影響 73
圖4-37為各電極之Ce(IV)產率 75
圖4-38為各電極之Ce(III)電氧化電流效率 76
圖4-39 0.1M Ce(III)/4M HNO3之CV圖－BDD工作電極 77
圖4-40 0.1M Ce(III)/4M HNO3之CV圖－白金工作電極 78
圖4-41 0.1M Ce(III)/4M HNO3之CV圖－玻璃碳工作電極 78
圖4-42 0.1M Ce(III)/4M HNO3之CV圖－PbO2/Sn2O3-SnO2/Ti工作電極
79
圖4-43不同Ce(IV)濃度對乙醯氨酚之降解（4.8×10-4M硫酸） 81
圖4-44不同Ce(IV)濃度對中間產物(對苯醌)之降解（4.8×10-4M硫酸）
81
圖4-45不同Ce(IV)濃度對乙醯氨酚之降解（10-3M硝酸） 83
圖4-46不同Ce(IV)濃度對中間產物(對苯醌)之降解（10-3M硝酸） 83
圖4-47以Ce(IV) 於4M硝酸中氧化降解乙醯氨酚 84
圖4-48以Ce(IV) 於4M硝酸中氧化降解中間產物(對苯醌) 85
圖4-49以Ce(IV) 於4M硫酸中氧化降解乙醯氨酚 86
圖4-50以Ce(IV) 於4M硫酸中氧化降解中間產物(對苯醌) 86
圖4-51人工廢液中Ce(III)電氧化為Ce(IV)之最終產率及電流效率 88
圖4-52人工廢液電再生之Ce(IV)氧化降解乙醯氨酚及中間產物(對苯醌)
88
圖4-53陽極為PbO2/Sn2O3- SnO2/Ti(S) 1cm2，陰極為不銹鋼1 cm2，電流密度0.88A/cm2 90
圖4-54 TFT-LCD廢液電回收Ce(IV)氧化降解乙醯氨酚及中間產物(對苯醌) 90

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