臺灣博碩士論文加值系統

　　本研究於都市垃圾焚化飛灰中添加廢玻璃(30%~50%)，經1450℃高溫熔融技術熔製成熔渣，再經不同燒結再結晶熱處理條件(900~1100℃)製成玻璃陶瓷產品。藉由玻璃陶瓷產品特性、熔融及燒結反應活化能之分析結果，進一步評估焚化飛灰熔渣資源化製成玻璃陶瓷之最佳產品特性與操作條件。
根據熔融反應活化能分析結果顯示，焚化飛灰之熔融反應溫度高於1350℃，然當添加廢玻璃達30%以上時，熔融溫度反應溫度降至1285℃，明顯達到降低熔融溫度之目的。同時根據反應活化能分析結果，當廢玻璃添加比例由30%增加至50%，其活化能從109.9 kJ/mole降低至23.5kJ/mole。前述不同摻配比例製成之熔渣，其Cu、Zn、Cr、Cd及Pb之毒性溶出濃度皆符合法規標準。且熔渣中有害金屬Cd、Pb及Zn殘餘率皆為0%， 故利用此熔渣做為資源化再應用之安全性無慮。
為進一步探討熔渣燒結製成玻璃陶瓷之可行性，試驗結果顯示在燒結溫度900至1100℃之條件，添加30%之廢玻璃熔渣燒製成之玻璃陶瓷，其吸水率及抗壓強度等材料特性分別為11.29~14.03%及20.32~25.92MPa，均可符合國家標準建築磚材之標準規範，吸水率低於15%及抗壓強度大於15MPa。然而，添加50%之廢玻璃熔渣燒製成之玻璃陶瓷，須達燒結溫度1100℃，方可符合建築磚材之標準規範。此外，根據物種分析結果可知，試驗玻璃陶瓷主要以鈣鋁黃長石(Gehlenite，Ca2Al2SiO7)、鋁斜輝石(Augite,aluminian，Ca(Mg,Fe,Al)(SiAl)2O6)、斜輝石(Augite ，Ca(Mg,Fe)Si2O6)、透輝石(Diopside，Ca(Mg,Al)(Si,Al)2O6)及矽灰石(wollastonite，CaSiO3)等物種為主。
根據熔渣之燒結熱膨脹變化及其燒結活化能結果顯示，在5~15℃/ min升溫條件下，隨廢玻璃添加量從30%增加至50%時，熔渣總膨脹量(dL/L0)從1.83~2.53%增加至3.71~5.07%，而活化能從 22.00~24.34 kJ/mo增加至39.07~52.56 kJ/mol。表示廢玻璃添加量越多之熔渣燒結成玻璃陶瓷所需克服活化能越大。
考量玻璃陶瓷環境安全性評估結果顯示，所有試驗條件之玻璃陶瓷中Cu、Zn、Cr、Cd及Pb之毒性溶出濃度，皆低於法規標準值。而酸中和能力之試驗終點pH約4.00時，飛灰中添加30~50%廢玻璃共融熔渣製成玻璃陶瓷，其所需酸添加量高達8.18∼12.56 meq/g。在900~1100℃燒結溫度下，添加40~50%廢玻璃熔渣燒製成玻璃陶瓷之Cr、Pb及Cu之最大釋出量分別為0.002~3.51 mg/meq•kg、0.001~0.008 mg/meq•kg及0.001~1.434 mg/meq•kg，皆遠低於飛灰之最大釋出量3.70mg/meq•kg、94.39mg/meq•kg及25.31mg/meq•kg。

Abstract
This study investigates that the feasibility of glass ceramic products made from molten slag of municipal solid waste incinerator (MSWI) fly ash and waste glass cullet. The experiments were conducted at melting temperature 1450℃ and sintering-crystallization temperatures ranged from 900 to 1100℃. To assess the characteristics of glass-ceramic products and optimum operation conditions, the activation energy of melting an sintering reaction were also evaluated.
Based on the results of activation energy of melting process, the melting temperature of MSWI fly ash is higher than 1350℃. However, in case of the waste glass cullet addition above 30%, the melting temperature will be decreased to 1285℃. That is, the waste glass addition will enhance the reaction of melting and reduce the melting temperature. Meanwhile, the activation energy of melting decreased from 109.9 kJ/mole to 23.5 kJ/mole with an increase in waste glass cullet addition ranged from 30% to 50%.The TCLP concentrations of Cu、Zn、Cr、Cd and Pb in slag were all in compliant with Taiwan regulation thresholds. Besides, the results of residual rate of tested metals of slags, the residual rate of Cd, Pb and Zn were approximately 0%.
The experimental results of glass ceramic products indicated that the water absorption and compressive strength of glass-ceramic (slag produced from 30% waste glass cullet addition) were 11.29%~14.03% and 20.32 MPa~25.92 MPa, respectively. In case of slag produced from 50% waste glass cullet addition, the water absorption and compressive strength of glass ceramic products were 13.54% and 27.23MPa, respectively. The above results were all in compliant with Chinese National Standard (CNS) building brick criteria for construction work. Besides, the major speciation of glass ceramic products were Gehlenite (Ca2Al2SiO7), Augite-aluminian (Ca(Mg,Fe,Al)(SiAl)2O6), Augite (Ca(Mg,Fe)Si2O6), Diopside (Ca(Mg,Al)(Si,Al)2O6), and Wollastonite (CaSiO3), respectively.
According to results of linear swelling analysis and activation energy, the maximum swelling value (dL/dt) of slag increased from 1.83% ~2.53% to 3.71%~5.07% with waste glass cullet addition increased from 30% to 50%. The activation energy of sintering also increased from 22.00 kJ/mole~24.34 kJ/mole to 39.09 kJ/mole~52.56 kJ/mole with an increase in waste glass cullet addition. That is, the activation energy of sintering increased with waste glass cullet addition increased.
The assessment for environmental safety of glass ceramic products was conducted by the toxic characteristic leaching procedure (TCLP) concentration and acid neutralization capacity (ANC). The TCLP concentrations of Cu, Zn, Cr, Cd, and Pb were lower than regulation thresholds. The results of ANC test showed that the used amounts of acid titration were ranged from 8.18 meq/g to 12.56meq/g as pH = 4. The maximum released amounts of Cr、Pb and Cu of glass ceramic products (slags produced from 40% and 50% waste glass cullet addition) were 0.002 mg/meq•kg ~3.51 mg/meq•kg, 0.001 mg/meq•kg~0.008 mg/meq•kg, and 0.001 mg/meq•kg~1.434 mg/meq•kg, respectively. The released amounts of tested metals of glass ceramic products were far below the maximum released amounts of MSWI fly ash (3.70 mg/meq•kg for Cr, 94.37 mg/meq•kg for Pb, and 25.31 mg/meq•kg for Cu).

目 錄
致謝…………………………………………………………………………. ⅰ
中文摘要…………………………………………………………………… ii
英文摘要…………………………………………………………………… iv
目錄……………………………………………………………………..…... ⅵ
圖目錄……………………………………………………………...…….…. ⅸ
表目錄………………………………………………………….…..…….…. ⅹi
第一章 研究緣起與目的…………………………....................................... 1
第二章 文獻回顧…………………………..………………..………….….. 3
2-1 都市垃圾焚化飛灰產生量及處理技術………………………... 3
　2-1-1 飛灰產生量………………………………………................ 3
　2-1-2 飛灰處理技術及資源化再利用………………………….. 3
2-2 玻璃陶瓷………………………………………………………... 10
2-2-1 製備玻璃陶瓷之組成……………………………………... 10
2-2-2 製備玻璃陶瓷之熱處理程序…………………………….. 11
2-3國內外利用都市垃圾焚化灰渣製成玻璃陶瓷之相關研究…….. 13
第三章 實驗材料與方法...……………………………………………….... 20
3-1 實驗材料………………………………………………………... 20
3-2 實驗設備與條件…………………………………………........... 21
3-2-1 熔融試驗與條件.……………………….…………………. 23
3-2-2 玻璃陶瓷燒結試驗與條件……………………………….. 24
3-2-3 共熔反應之動力分析…………..…………………………. 25
3-2-4 玻璃陶瓷燒結反應之動力分析…………………………... 28
3-3 分析方法……………………………………………………….. 30
3-3-1 原料及熔渣之基本分析項目……………………………....... 30
3-3-2 玻璃陶瓷之分析項目………………………………….......... 33
第四章 結果與討論...……………………………………………….......… 36
4-1 研究材料基本性質分析………………………………………. . 36
4-1-1 物化特性分析結果……………………………………….. 36
4-1-2 物種鑑定及微結構分析………………………………….. 40
4-1-3 飛灰中酸中和能力……………………………………….. 43
4-2 焚化飛灰與廢玻璃共同熔融之熔渣特性分析……………. …. 46
4-2-1 減容比及減重比………………………………………….. 46
4-2-2 熔渣之TCLP分析………………………………….……. 47
4-2-3 熔渣之金屬殘留比…………………………………….…. 48
4-2-4 熔渣之化學組成分析…………………………………..… 51
4-2-5 熔渣之物種鑑定及微結構分析……………………..…… 51
4-3 焚化飛灰與廢玻璃共同熔融之反應動力分析……………...… 54
4-3-1 熔融反應之特徵溫度…………………………………..… 54
4-3-2 熔融反應級數及活化能………………………………….. 60
4-4 玻璃陶瓷特性分析……………………………………………... 63
4-4-1 燒失量……………………………………………………. 63
4-4-2 線性及體積變化……………….………………………… 64
4-4-3 吸水率及開孔孔隙率…………………………………… 66
4-4-4 抗壓強度…………………………………………………. 68
4-4-5 XDR物種鑑定…………………………………………… 69
4-4-6 SEM微觀結構………………..……………………….. 75
4-4-7 玻璃陶瓷之環境安全性評估……………………………. 79
4-4-8 不同pH值之玻璃陶瓷金屬溶出情形…………………. 82
4-5 燒結反應之動力分析………………………………………….. 99
4-5-1 燒結過程之線性熱膨脹變化………………………………... 99
4-5-2 燒結過程之活化能……………………..………………….... 102
第五章 結論與建議………………………………………………………. 104
5-1 結論………………………………………….………………………... 104
5-2 建議………………………………………….………………………... 107
參考文獻………………..…………………………………………………... 108
























圖 目 錄
圖1-1 研究架構圖……………………………………………………… 2
圖2-1 玻璃陶瓷之典型製程……………………………………………. 11
圖2-2 玻璃陶瓷兩階段熱處理示意圖…….………………………........ 13
圖2-3 玻璃陶瓷一階段熱處理示意圖….….…………………………… 15
圖3-1 採樣焚化廠處理流程及採樣點示意圖………………………… 20
圖3-2 實驗流程圖……………………………………………………… 22
圖3-3 高溫熔融爐設備示意圖…….……..……………………………. 23
圖3-4 熔融過程之溫度控制曲線……………………………………… 24
圖3-5 玻璃陶瓷燒結試驗之溫度控制曲線…………………………… 25
圖3-6 由DSC求取動力學參數的示意圖…………………………….. 27
圖3-7 燒結機制之表面傳遞與整體傳遞示意圖……………………… 28
圖4-1 焚化飛灰粒徑累積分佈曲線圖…………………………………. 37
圖4-2 焚化飛灰與廢玻璃之物種鑑定分析結果………………………. 41
圖4-3 焚化飛灰與廢玻璃之表面結構圖………………………………. 42
圖4-4 飛灰酸中和能力及重金屬溶出變化圖………………………….. 45
圖4-5 熔渣之物種鑑定…………………………………………………. 52
圖4-6 熔渣之表面結構圖……………………………………………….. 53
圖4-7 焚化飛灰、NaCl及KCl之差示掃描量熱-熱重分析圖…………… 55
圖4-8 焚化飛灰與廢玻璃之差示掃描量熱-熱重分析圖(10℃/min)….. 57
圖4-9 焚化飛灰與廢玻璃之差示掃描量熱-熱重分析圖(15℃/min)….. 58
圖4-10 焚化飛灰與廢玻璃在三種不同升溫速率下之差示掃瞄熱量圖.. 59
圖4-11 熔融過程反應級數的判定圖…………………………………… 60
圖4-12 飛灰與廢玻璃共同熔融熱動力參數圖………………………… 62
圖4-13 玻璃陶瓷之燒失量變化..………………………………………… 63
圖4-14 玻璃陶瓷之線性及體積變化圖…………………………………. 65
圖4-15 玻璃陶瓷之吸水率及視孔隙率變化圖………………………….. 67
圖4-16 玻璃陶瓷之抗壓強度圖………………………………………… 69
圖4-17 玻璃陶瓷(slag made from 30% glass / 70% fly ash)之晶相鑑定圖... 71
圖4-18 玻璃陶瓷(slag made from 40% glass / 60% fly ash)之晶相鑑定圖… 72
圖4-19 玻璃陶瓷(slag made from 50% glass / 50% fly ash)之晶相鑑定圖… 73
圖4-20 玻璃陶瓷(slag made from 30% glass / 70% fly ash)之微觀結構........ 76
圖4-21 玻璃陶瓷(slag made from 40% glass / 60% fly ash)之微觀結構........ 77
圖4-22 玻璃陶瓷(slag made from 50% glass / 50% fly ash)之微觀結構...... 78
圖4-23　 　玻璃陶瓷與飛灰之ANC曲線比較圖…………………………… 81
圖4-24 　玻璃陶瓷於不同pH之Cr金屬溶出情形………………………. 84
圖4-25 玻璃陶瓷於不同pH之Pb金屬溶出情形……………………….. 86
圖4-26 玻璃陶瓷於不同pH之Cu金屬溶出情形……………………… 87
圖4-27 玻璃陶瓷於不同pH之Na金屬溶出情形……………………… 89
圖4-28 玻璃陶瓷於不同pH之K金屬溶出情形……………………… 91
圖4-29 玻璃陶瓷於不同pH之Ca金屬溶出情形……………………… 93
圖4-30 玻璃陶瓷於不同pH之Mg金屬溶出情形……………………… 95
圖4-31 不同玻璃陶瓷之熱膨脹曲線圖………………………..………… 101








表 目 錄
表2-1 利用焚化灰渣製成玻璃陶瓷之組成成分、熱處理最佳條件及
要結晶相態之總整理表…………………………………………. 18
表4-1 焚化飛灰之粒徑分布累積重量分佈比例…………………….. 36
表4-2 焚化飛灰與廢玻璃之物化特性分析結果……………………. 39
表4-3 焚化飛灰與廢玻璃之化學組成成分……………………………. 40
表4-4 都市垃圾焚化飛灰酸中和試驗之金屬溶出量與最終環境釋出量… 44
表4-5 熔渣減容比………………………………………………………. 46
表4-6 熔渣減重比………………………………………………………. 47
表4-7 焚化飛灰與廢玻璃共熔熔渣之毒性特性熔出試驗分析結果…. 48
表4-8 不同廢玻璃掺配比例之混合灰共同熔融前後重金屬變化表... 50
表4-9 熔渣之化學組成成分……………………………………………. 51
表4-10 飛灰與廢玻璃熔融熱分析之特徵溫度…………………………. 59
表4-11 飛灰與廢玻璃共同熔融熱動力參數表…………………………. 62
表4-12 玻璃陶瓷之磚材材料特性之比較………………………………. 68
表4-13 玻璃陶瓷結晶物種彙整表……………………………………… 74
表4-14 玻璃陶瓷之毒性特性溶出試驗分析結果……………………… 79
表4-15 玻璃陶瓷之金屬溶出量與最終環境釋出量…………………… 96
表4-16 玻璃陶瓷與都市垃圾焚化飛灰之最終環境量之比較……….. 98
表4-17 不同玻璃陶瓷之熱膨脹參數……………………………………. 102
表4-17 玻璃陶瓷之燒結活化能…………………………………………. 103

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