臺灣博碩士論文加值系統

摘� 要

重金屬與有機污染物在環境污染上一直扮演著舉足輕重的地位，台灣地區由於工業快速成長，每年均產生大量的有毒廢水，舉凡電鍍業、金屬表面處理業、鋼鐵業、半導體業、電子業、光電業、印刷電路板業、冶煉業、醫藥業、油漆業及食品加工業等企業排放出的廢水中，無不含有對人體或環境有害之重金屬與有機污染物。有鑒於此，發展含重金屬與有機物之廢水處理技術更是值得推動。

� 本研究乃藉由Fenton程序之強氧化力先行去除廢水中之有機污染物EDTA，並於其後再以鐵氧磁體程序（Ferrite Process，簡稱FP）將重金屬離子一併納入尖晶石結構中而去除之，並藉以建立Fenton/Ferrite Processt（簡稱FFP）串聯最佳之處理操作模式。

在Fenton程序的批次反應中，主要探討之反應因子如溶液pH值、亞鐵離子濃度、過氧化氫添加量等對去除率之影響。實驗結果顯示，Fenton在酸性的條件(pH=2)下，EDTA呈現最佳之去除率。適當增加反應溶液中之亞鐵離子或過氧化氫可以增加EDTA之去除率，但當其量超過某一定值時，EDTA之去除率不增反減，其可能是因為過量之亞鐵離子或過氧化氫抑制氫氧自由基之生成所導致。

在Fenton程序完成後，接續以Ferrite Process進行串聯處理廢水；Ferrite Process主要以三個階段進行反應，操作條件為控制溫度及pH值，第一階段操作條件：70℃、pH值為9.0；第二階段操作條件：90℃、pH值為9.0；第三階段操作條件：80℃、pH值為10.0。
經串聯試驗結果可知，若以反應時間而言，A-4試驗條件之總反應時間為90分鐘時，可使上澄液中各重金屬濃度達放流水標準；若廢水中不含Hg時，則反應時間可縮短至50分鐘，因此最具時間上的效益；A-3試驗條件下，若廢水中不含Cd及Hg時，反應時間為56分鐘時，可使上澄液中各重金屬濃度達放流水標準，且此試驗條件所需之亞鐵離子添加量為最少，故此試驗條件兼具成本與時間上之經濟效益。


(註)
NO. Fenton Method(25℃) Ferrite Process
pH值 Fe2+濃度 H2O2濃度 Fe2+
添加量 第一
階段 第二
階段 第三
階段
A-3 2 10-3M 5×10-4M 0.098M
(7倍) 70℃
pH=9 90℃
pH=9 80℃
pH=10
A-4 10-2M




關鍵字：Fenton Process、Ferrite Process、EDTA、重金屬

Abstract

Heavy metals and organics are always presented an important rule in the pollution control. In Taiwan, there are large amounts of toxic wastewater produced from electrical plating, metal surface-treating, steel, IC, electrics, photo-electrics, printed PC board, refinery, medicals, oil painting and foods manufactory industries. Those wastewater are contained toxic and hazardous materials materials to human body or environment quality. Thus, we believe it need immediately to develop the innovative process on removal of wastewater containing heavy metals and organic compounds.

This study uses the strong oxidation of Fenton’s Process to first remove the organic pollutant, EDTA, and then uses Ferrite Process to incorporate heavy metal ions into spinel structure for facilitating removal of heavy metal ions, and through this work, the best operation model of series treatment “Fenton/Ferrite Process” is established.

With respect to batch reaction in Fenton’s Process, the emphasis in this work is placed the effect on EDTA removal by pH, ferrous ions concentration, and hydrogen peroxide . The results show that the best removal of EDTA occurs when Fenton is under acid condition (pH=2); and the removal of EDTA increase as the ferrous ions and hydrogen peroxide increase adequately, but when its quantity exceeds a certain value, the removal of EDTA would decrease as follows. Such a result may be caused by the excess of ferrous ions and hydrogen peroxide which could restain generation of hydroxyl radicals.
As followed the Fenton’s process, Ferrite Process is next used for treatment of wastewater in series; Ferrite Process has three stages, and the operating conditions are controlled temperature and pH. For the first stage, the operating condition is 70℃, and pH is 9.0; and the operating condition is 90℃, and pH is 9.0 in the second stage; and the operating condition is 80℃, and pH is 10.0 in the last stage.

From the results of series experiments, with respect to reaction time, each concentration of heavy metal in supernatant could meet the standards of discharge water when the total time of A-4 experimental condition is 90 minutes; if Hg ion is not included in wastewater, then the reaction time could be reduced to 50 minutes. I shows benefit for short reaction it the time. Under A-3 experimental condition, the reaction time is 56 minutes when Cd and Hg ions are not included in the wastewater, then each ions concentration of heavy metal could also reach the standards of discharge water, and this experiment need of ferrous ions is least of all. Thus, this experiment in this work has the economic benefits both for regarding time and cost-effectiveness.


Keywords：Fenton’s Process、Ferrite Process、EDTA、Heavy metal

目 錄

頁數
謝誌……………………………………………………………….. Ⅰ
中文摘要………………………………………………………….. Ⅱ
英文摘要………………………………………………………….. Ⅳ
目錄……………………………………………………………….. Ⅵ
表目錄…………………………………………………………….. Ⅹ
圖目錄…………………………………………………………….. VI


第一章 緒論……………………………………………………. 1-1
1-1 研究緣起………………………………………….. 1-1
1-2 研究目的………………………………………….. 1-4
1-3 預期成果………………………………………….. 1-4

第二章 文獻回顧………………………………………………. 2-1
2-1 EDTA之基本特性及相關研究…………………. 2-1
2-1-1 EDTA之基本特性……...………………….. 2-1
2-1-2 EDTA之應用概況…………………………. 2-4
2-1-3 EDTA之相關處理研究……………………. 2-7
2-2 重金屬污染之特性及相關研究………………… 2-10
頁數
2-2-1 重金屬污染之特性……………………….... 2-10
2-2-2 重金屬污染之相關研究…………………… 2-11
2-3 Fenton程序原理與影響因素………………….. 2-13
2-3-1 Fenton之氧化原理………………………… 2-13
2-3-2 Fentont程序去除有機物之影響因素……... 2-15
2-3-2 Fenton程序之相關研究…………………… 2-17
2-4 Ferrite Process之理論基礎與相關研究….…….. 2-20
2-4-1 Ferrite Process之原理……………… ……... 2-20
2-4-2 Ferrite Process之影響因子………… ……... 2-24
2-4-3 Ferrite Process之相關研究……………….... 2-26

第三章 研究方法與實驗設計…………………………………. 3-1
3-1 研究方法………………………………………… 3-1
3-2 Fenton-Ferrite Process批次反應系統簡介……... 3-4
3-3 實驗設計及步驟………………………………… 3-6
3-3-1 Fenton Method各項參數對去除EDTA之探� � �討……………………………………………. 3-6
3-3-2 Fettite Process對去除混合性重金屬能力之� � 探討…………………………………………. 3-8
頁數
3-4 實驗設備、分析項目及方法…………………….. 3-10
3-4-1 研究設備…………………………………… 3-10
3-4-2 實驗藥品與試劑…………………………… 3-12
3-4-3 實驗分析項目與方法……………………… 3-13
3-4-4 實驗操作條件……………………………… 3-15
3-5 實驗室之品質管制……………………………… 3-16
3-5-1 玻璃器皿之清洗…………………………… 3-16
3-5-2 儀器之校正及注意事項…………………… 3-16
3-5-3 試藥配藥注意事項………………………… 3-17

第四章 結果與討論……………………………………………. 4-1
4-1 Fenton法處理EDTA能力之探討……………… 4-1
4-1-1 pH值與處理效果之關係…………………... 4-1
4-1-2 亞鐵離子添加量對處理效果之影響……… 4-5
4-1-3 過氧化氫添加量對處理效果之影響……… 4-8
4-1-4 處理效能分析……………………………… 4-11
4-2 Fenton / Ferrite Process處理EDTA與重金屬廢水能力之探討…………………………………… 4-12
4-2-1 建立Ferrite Process操作條件……………... 4-12
頁數
4-2-2 建立Fenton / Ferrite Process操作條件……. 4-14
4-2-3 處理效能分析………………………………. 4-29
4-3 成本效益評估……………………………………. 4-30

第五章 結論與建議……………………………………………. 5-1
5-1 結論……………………………………………… 5-1
5-2 建議……………………………………………… 5-4

參考文獻………………………………………………………….. 參-1
附錄一 各重金屬檢量線………………………………………….. 附1-1
附錄二 QA /QC…………..……………………………………….. 附2-1
附錄三 物質安全資料表…………………..……………………… 附3-1
附錄四 審查委員意見回覆表……………..……………………… 附4-1

表 目 錄

頁數
表2.1 EDTA及其鈉鹽於水中溶解度與溫度之關係……… 2-3
表2.2 EDTA在不同pH值下與各重金屬螯合的置換能力.. 2-4
表2.3 EDTA在各行業中之應用概況………………………. 2-5
表2.4 重金屬排放之法規標準……………………………… 2-11
表2.5 不同重金屬分離技術之比較表……………………… 2-12
表2.6 以Fenton處理有機污染物之相關文獻彙整(1/2)…… 2-18
表2.6 以Fenton處理有機污染物之相關文獻彙整(2/2)…… 2-19
表2.7 尖晶石型鐵氧磁體可包含之金屬種類……………… 2-20
表2.8 鐵氧磁體化法影響因子之相關文獻彙整(1/4)……… 2-27
表2.8 鐵氧磁體化法影響因子之相關文獻彙整(2/4)……… 2-28
表2.8 鐵氧磁體化法影響因子之相關文獻彙整(3/4)……… 2-29
表2.8 鐵氧磁體化法影響因子之相關文獻彙整(4/4)……… 2-30
表3.1 模擬廢水重金屬藥品清單…………………………… 3-13
表4.1 系統pH值對Fenton反應之影響…………………… 4-1
表4.2 不同pH值下，EDTA殘餘率與反應時間之關係….. 4-2
表4.3 添加不同濃度之亞鐵離子，EDTA殘餘率與反應時間之關係……………………………………………… 4-6
表4.4 添加不同濃度之過氧化氫，EDTA殘餘率與反應時間之關係……………………………………………… 4-9
表4.5 Fenton / Ferrite Process處理EDTA與重金屬實驗操作條件………………………………………………… 4-14
表4.6 Fenton / Ferrite Process處理EDTA重金屬廢水之成效……………………………………………………… 4-15
表4.7 Ferrite Process對各項重金屬之處理效果(上澄液)… 4-19
表4.8 Ferrite Process對各項重金屬之處理效果(沈澱物)…………………………………………………….. 4-24
表4.9 Fenton/Ferrite Rrocess技術成本效益評估………….. 4-31

圖 目 錄

頁數
圖2.1 EDTA化學結構式…………………………………… 2-2
圖2.2 EDTA各種形式隨pH值變化之情形………………. 2-3
圖2.3 EDTA礦化之反應路徑……………………………… 2-9
圖2.4 鐵氧磁體尖晶石結構……………………………….. 2-21
圖2.5 形成鐵氧磁體之氧化條件………………………….. 2-23
圖3.1 整體研究流程……………………………………….. 3-3
圖3.2 Fenton-Ferrite Process批次反應系統………………. 3-5
圖3.3 Fenton試驗研究流程……………………………….. 3-7
圖3.4 Ferrite Process試驗研究流程………………………. 3-9
圖3.5 雙夾層玻璃反應器示意圖………………………….. 3-10
圖3.6 毒性溶出試驗旋轉裝置…………………………….. 3-11
圖3.7 毒性特性溶出程序( TCLP )………………………… 3-14
圖4.1 不同pH值下，EDTA殘餘率與反應時間之關係圖.. 4-3
圖4.2 添加不同濃度之亞鐵離子，EDTA殘餘率與反應時間之關係…………………………………………….. 4-7
圖4.3 添加不同濃度之過氧化氫，EDTA殘餘率與反應時間之關係…………………………………………….. 4-10
圖4.4 於Fenton / Ferrite Process下，EDTA之處理效果(一)…………………………………………………… 4-16
圖4.5 於Fenton / Ferrite Process下，EDTA之處理效果(二)…………………………………………………… 4-17
圖4.6 Ferrite Process於0min時，重金屬初始濃度(上澄液)……………………………………………………. 4-20
圖4.7 Fenton/ Ferrite Process亞鐵離子加藥量對Cd處理效果(上澄液)………………………………………… 4-20
圖4.8 Fenton/ Ferrite Process亞鐵離子加藥量對Cr處理效果(上澄液)…………………………………………… 4-21
圖4.9 Fenton/ Ferrite Process亞鐵離子加藥量對Cu處理效果(上澄液)………………………………………… 4-21
圖4.10 Fenton/ Ferrite Process亞鐵離子加藥量對Hg處理效果(上澄液)………………………………………… 4-22
圖4.11 Fenton/ Ferrite Process亞鐵離子加藥量對Ni處理效果(上澄液)…………………………………………… 4-22

頁數
圖4.12 Fenton/ Ferrite Process亞鐵離子加藥量對Pb處理效果(上澄液)…………………………………………… 4-23
圖4.13 Fenton/ Ferrite Process亞鐵離子加藥量對Zn處理效果(上澄液)………………………………………… 4-23
圖4.14 Fenton/ Ferrite Process亞鐵離子加藥量對Cd處理效果(沈澱物)………………………………………… 4-25
圖4.15 Fenton/ Ferrite Process亞鐵離子加藥量對Cr處理效果(沈澱物)…………………………………………… 4-25
圖4.16 Fenton/ Ferrite Process亞鐵離子加藥量對Cu處理效果(沈澱物)………………………………………… 4-26
圖4.17 Fenton/ Ferrite Process亞鐵離子加藥量對Hg處理效果(沈澱物)………………………………………… 4-26
圖4.18 Fenton/ Ferrite Process亞鐵離子加藥量對Ni處理效果(沈澱物)…………………………………………… 4-27
圖4.19 Fenton/ Ferrite Process亞鐵離子加藥量對Pb處理效果(沈澱物)…………………………………………… 4-27
圖4.20 Fenton/ Ferrite Process亞鐵離子加藥量對Zn處理效果(沈澱物)………………………………………… 4-28

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