本研究利用均勻沈澱法自行製備奈米級MgO，並從不同初始反應條件下，進行Reacitve Black-5（RB-5）與Reactive Blue-19（RB-19）染料廢水之破壞性吸附試驗。此外，本研究亦藉由使用UV-vis全波長分析、基質輔助雷射脫附游離法(MALDI)連接飛行時間質譜儀(TOF/MS)與氣相層析儀配置質譜儀檢知器(GC/MS)，針對破壞性吸附後之中間產物加以定性分析，據此推測其破壞性吸附之反應機制。
本研究利用均勻沈澱法合成奈米級MgO之最佳操作條件如下：(1) 反應劑(尿素/氯化鎂)莫耳比為9，(2) 添加水量250 mL，(3) 反應溫度125℃，(4) 震盪強度為90 strokes/min，(5) 反應時間為7 hr，(6) 以5 ℃/min之升溫速率加熱至450℃，維持4小時之煅燒，(7) 迴流加熱時間為24 hr，(8) 使用冷凍乾燥法進行乾燥，(9) 以兩階段式煅燒(以5 ℃/min之升溫速率加熱至300℃，維持1小時，並以相同升溫速率至500℃，維持4小時)。其所合成之奈米級MgO係屬於六角板，二維奈米結構，其六角形板厚約20〜30 nm ，BET比表面積介於120〜125 m2/g。
奈米級MgO對RB-5與RB-19之吸附模式較符合Langmuir equation，而其分別之吸附容量為196.08 mg/g和163.93 mg/g；兩者的吸附動力模式皆為擬二階動力方程式。奈米級MgO對於RB-5和RB-19之最佳操作條件為：(1)染料之初始濃度為1000 mg/L；(2)奈米級MgO添加量為15 g/L；(3)強烈攪拌時間為30 min；(4)系統pH值並不需調整，其ADMI與COD符合染整業廢水之法定放流標準。
經由UV-vis全波長掃描結果顯示，奈米級MgO對RB-5與RB-19反應後之色度去除結果十分良好，亦發現對於兩種染料之次波峰吸收值有下降趨勢，同時也都有生成新的吸收波峰，可證實染料分子產生斷鍵現象。由於RB-5之分子量較大、分子結構支鏈長、擁有較多可吸附在奈米級MgO的磺酸基與硫酸乙磺醯基，且RB-19之蔥醌結構不易被破壞，因此，奈米級MgO破壞性吸附RB-5之結果優於RB-19。
本研究係將奈米級MgO使用於水相環境，其破壞性吸附可能係以其表面反應位址為主：陰/陽離子空位、超氧離子O2-、邊、角、締合之-OH基、晶格鍵結之OH及孤立之OH。由MALDI-TOF/MS及GC/MS結果推測，RB-5之反應機制可分為：(1)吸附與水溶性基脫落階段，(2)發色團分解脫色階段，(3)淺色中間產物的進一步降解階段；RB-19則分為：(1)吸附與助色團脫落分解階段，(2)發色團分解脫色階段。

This study was to prepare nanoscale MgO using the homogeneous precipitation process and to investigate its destructive adsorption with dye wastewater of reactive black-5 and reactive blue-19. In addition, UV-vis Spectrophotometer, Matrix-Assisted Laser Desorption/Ionization Time of Flight Mass Spectrometry (MALDI-TOF/MS) and Gas Chromatograph/Mass Spectrometer (GC/MS) were used to analyze the intermediates resulting from destructive adsorption. Based on the results obtained, the destructive adsorption mechanisms for the treatment of dye wasterwater by nanoscale MgO were proposed in this study.

In this work, the optimal operating conditions for nanoscale MgO synthesis were determined to be the following: (1) a chemical reaction time of 7 hr, (2) reaction temperature of 125℃, (3) molar ratio of 9 for urea/MgCl2．6H2O, (4) water addition of 250 mL, (5) mixing intensity of 90 strokes per min, (6) calcination at 450℃ for 4 hr, (7) reflux time of 24 hr, (8) freeze-drying method, (9) two stage calcinations. Using these operating conditions one is able to prepare 2-D nanoscale MgO of hexagonal platelets with a thickness of 20-30 nm and BET surface area of 120-125 m2/g.

The adsorption model of nanoscale MgO for RB-5 and RB-19 was fitted to the Langmuir equation and their adsorption capacity were 196.08 mg/g and 163.93 mg/g, respectively. Both of them were fitted to the pseudo-second-order kinetic model equation. The optimal operating conditions of nanoscale MgO for destructive adsorption of both dyes were determined to be the following: (1) an initial dye concentration of 1000 mg/L, (2) a nanoscale MgO dose of 15 g/L, (3) a vigorous mixing of 30 min, (4) no need of system pH adjustment. Under such conditions, chemical oxygen demand (COD) and American Dye Manufacturers Institute (ADMI) of RB-5 and RB-19 were lower than the textile effluent standards.

According to the UV-vis spectrophotometer scanning results, the color removal of nanoscale MgO for RB-5 and RB-19 was good. At the same time, the absorbance of their second maximal peaks was decreased and some peaks were observed. Therefore, it proved that the model dyes were destroyed. Experimental results have shown that nanoscale MgO has a better performance of destructive adsorption on RB-5 than that of RB-19. This might be ascribed to the following reasons: (1) a greater molecular weight, (2) a longer molecule structure, (3) more sulfate ethyl sulfone groups for RB-5, and (4) a hard to be destroyed structure of anthraquinone for RB-19.

The destructive adsorption of dye wastewater by nanoscale MgO presumably took place mainly on the surface active sites of nanoscale MgO, including anion/cation vacancies, superoxide anion, edge, corner, isolated OH, lattice bound OH and assiocited-OH groups. According to the results of MALDI-TOF/MS and GC/MS analysis, the relevant reaction mechanism for RB-5 could be divided into three stages: (1) adsorption and water-soluble groups exfoliation stage, (2) chromophor decomposition and decolorization stage, and (3) further degradation stage for light-color intermediates. On the other hand, the relevant reaction mechanism for RB-19 might involve only the adsorption and auxochrome exfoliation stage and chromophor decomposition and decolorization stage.

聲明切結書………………………………………………………… i
謝誌………………………………………………………………… ii
摘要………………………………………………………………… iii
Abstract…………………………………………………………… v
目錄……………………………………………….……………… vii
表目錄……………………………………………………………… xiii
圖目錄……………………………………………………………… xv

第一章 前言……………………………………………………… 1
1-1 研究緣起…………………………………………………… 1
1-2 研究目的…………………………………………………… 3
1-3 研究內容…………………………………………………… 3
1-4 研究架構…………………………………………………… 5

第二章 文獻回顧………………………………………………… 6
2-1 染整廢水…………...……………………..…………….. 6
2-1-1 台灣染整廢水之污染情形……………………………. 6
2-1-2 染料簡介………………………………………………. 8
2-1-3 染料之發光團學說及基本結構………………… 11
2-1-4 反應性染料……………………………………………13
2-2 染整廢水之處理技術…………………………………………15
2-2-1 簡介………………………………………………… 15
2-2-2 國內外之處理技術………………………………… 16
2-2-3 染料降解途徑與機制……………………………… 25
2-3 氧化鎂……...……………………………............. 30
2-3-1 各國使用MgO之情形……………………………….. 30
2-3-2 奈米級MgO之用途…………………………………… 32
2-3-3 破壞性吸附………………………………………… 32
2-3-4 奈米級MgO之製備方法……………………………… 45
2-4 MALDI-TOF/MS….……………………………………….... 53
2-4-1 MALDI-TOF/MS之原理……………………………… 53
2-4-2 基質簡介...…………………………………………….. 56
2-4-3 MALDI游離機制……………………………………… 58
2-4-4 飛行時間偵測器（TOF）介紹……………………….. 58
2-4-5 MALDI-TOF/MS之應用……………………………… 60

第三章 實驗材料、設備與方法…………….…………………… 62
3-1 實驗材料…………………………………………………… 62
3-2 實驗設備…………………... …………………………… 64
3-3 實驗方法…………………………………………………… 68
3-3-1 利用均勻沉澱法製備奈米級MgO實驗..……………. 68
3-3-1-1 奈米級MgO製備…………………………… 68
3-3-1-2 奈米級MgO活化…………………………… 69
3-3-2 合成粉末之基本性質分析.…………………………… 70
3-3-2-1 晶形鑑定……………………………………. 70
3-3-2-2 粉末外觀型態……………………………….. 70
3-3-2-3 比表面積分析……………………………….. 71
3-3-2-4 熱分析……………………………………….. 71
3-3-3 破壞性吸附反應………………………………………. 71
3-3-3-1 奈米級MgO與RB-5之反應實驗…………. 71
3-3-3-2 奈米級MgO與RB-19之反應實驗………… 73
3-3-3-3 UV-vis全波長分析............... 74
3-3-3-4 MALDI-TOF/MS分析.................... 74
3-3-3-5 GC/MS分析……...………………………….. 75
3-3-3-6 破壞性吸附之反應機制…………………….. 75
3-3-4 與其他吸附劑比較……………………………………. 76
3-3-5 水質參數分析方法.…………………………………… 76

第四章 結果與討論…………………………………………….… 80
4-1 利用均勻沉澱法製備奈米級MgO實驗.……………………. 80
4-1-1 奈米級MgO製備…….……………………………….. 80
4-1-1-1 反應時間之效應…………………………….. 80
4-1-1-2 反應劑莫耳比之效應……………………….. 81
4-1-1-3 添加水量之效應…………………………….. 82
4-1-2 奈米級MgO活化……….......................... 83
4-1-2-1 迴流加熱時間與活化後之乾燥方法之效應.. 84
4-2 合成粉末之基本性質分析….................. 87
4-2-1 X-光繞射分析儀………………………………………. 87
4-2-2 熱重分析儀……………………………………………. 88
4-2-3 掃描式電子顯微鏡……………………………………. 90
4-3 奈米級MgO與RB-5之反應實驗…………………………… 92
4-3-1 攪拌時間之效應…………………………………… 92
4-3-1-1 ADMI分析………………………………… 92
4-3-1-2 COD分析…………………………………… 93
4-3-1-3 TOC分析…………………………………… 94
4-3-1-4 UV-vis分析……………………………… 95
4-3-1-5 吸附反應動力模式……………………… 96
4-3-1-6 綜合分析………………………………… 98
4-3-2 奈米級MgO添加量之效應……...…………….…… 99
4-3-2-1 ADMI分析…………………………………. 100
4-3-2-2 COD分析…………………………………… 101
4-3-2-3 TOC分析…………………………………… 101
4-3-2-4 UV-vis分析……………………………… 102
4-3-2-5 綜合分析…………………………………. 103
4-3-3 初始濃度之效應…………………………………… 104
4-3-3-1 ADMI分析………………………………… 105
4-3-3-2 COD分析…………………………………… 105
4-3-3-3 TOC分析…………………………………… 106
4-3-3-4 UV-vis分析……………………………… 107
4-3-3-5 等溫吸附模式…………………………… 108
4-3-3-6 綜合分析…………………………………. 112
4-3-4 初始pH值之效應……………………………………. 113
4-4 奈米級MgO與RB-19之反應實驗…………………………. 115
4-4-1 攪拌時間之效應…………………………………… 115
4-4-1-1 ADMI分析…………………………………. 115
4-4-1-2 COD分析…………………………………… 116
4-4-1-3 TOC分析…………………………………… 117
4-4-1-4 UV-vis分析……………………………… 118
4-4-1-5 吸附反應動力模式……………………… 119
4-4-1-6 綜合分析………………………………… 120
4-4-2 奈米級MgO添加量之效應……...…………….…… 120
4-4-2-1 ADMI分析…………………………………. 121
4-4-2-2 COD分析…………………………………… 121
4-4-2-3 TOC分析…………………………………… 122
4-4-2-4 UV-vis分析……………………………… 123
4-4-2-5 綜合分析…………………………………. 124
4-4-3 初始濃度之效應………………………………………. 125
4-4-3-1 ADMI分析………………………………….. 125
4-4-3-2 COD分析…………………………………… 126
4-4-3-3 TOC分析…………………………………… 127
4-4-3-4 UV-vis分析……………………………… 128
4-4-3-5 等溫吸附模式…………………………… 129
4-4-3-6 綜合分析…………………………………. 131
4-4-4 初始pH值之效應…………………………………… 131
4-5 奈米級MgO破壞性吸附RB-5之反應機制………………… 132
4-5-1 不同奈米級MgO劑量與RB-5反應之UV-vis全波長掃瞄分析………………………………………………............. 133
4-5-2 MALDI-TOF/MS分析…...…………………………… 135
4-5-3 GC/MS分析…...……………….……..…………… 137
4-5-4 奈米級MgO破壞性吸附RB-5之反應途徑………… 140
4-5-5 綜合分析…………………………………………… 142
4-6 奈米級MgO破壞性吸附RB-19之反應機制………………… 149
4-6-1 不同奈米級MgO之劑量與RB-19反應之UV-vis全波長掃瞄分析………………………………………….................. 150
4-6-2 MALDI-TOF/MS分析…...…………………………… 151
4-6-3 GC/MS分析...………………….……..…………… 152
4-6-4 奈米級MgO破壞性吸附RB-19之反應途徑.………. 153
4-6-5 綜合分析…………………………………………… 155
4-7 與其他吸附劑比較………………………………………… 158
4-8 綜合討論…………………………………………………… 161


第五章 結論與建議……………………………………………… 164
5-1 結論………………………………………………………… 164
5-2 建議………………………………………………………… 167

參考文獻………………………………………………………… 168

附錄………………………………………………………………… 177

碩士在學期間發表之學術論文……………………………… 185

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