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研究生：	段宇君 Tuan, Yeu-Juin
論文名稱：	實驗室廢棄物焚化灰渣及電漿熔渣之毒性物質研究 Tracking of toxic species in laboratory waste incineration ashes and plasma melting slags
指導教授：	王鴻博 Wang, H. Pual
學位類別：	博士 Doctor
系所名稱：	工學院 - 環境工程學系 Department of Environmental Engineering
論文出版年：	2012
畢業學年度：	100
語文別：	英文
論文頁數：	136
中文關鍵詞：	飛灰、熔渣、焚化、電漿熔融、洗灰、XANES 、DEA
外文關鍵詞：	ash, slag, incineration, plasma melting, ash washing, XANES, DEA
相關次數：	點閱：78 下載：3
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實驗室廢棄物焚化灰渣（ashes），因含毒性重金屬與戴奧辛（polychlorinated dibenzo-p-dioxins and dibenzofurans, PCDD/Fs）被視為有害廢棄物。焚化灰渣可以電漿熔融高溫安定化（1673-1773 K）生成熔渣（slag）。由於目前焚化灰渣及電漿熔渣之有害物質化學結構資料仍相當缺乏，因此，針對焚化灰渣及電漿熔渣中之有害物質（銅、鉻及PCDD/Fs）之安定化進行研究。尤其利用XANES，XAFS及XRD等光譜所獲得之分子尺度結果及數據，可更深入瞭解灰渣及熔渣中有害物質的物種及化學結構。
研究結果顯示CuO及CuSO4分別為焚化底渣及飛灰中主要之銅化合物。經電漿熔融處理後，金屬銅（76%）及Cu2O（15%）則為熔渣中之主要成分。此外，CuSiO2也在熔渣中發現，顯示銅可能被侷限（encapsulated）在SiO2晶格中，也是造成熔渣TCLP濃度相對低之原因，熔渣中以低氧化數銅（CuCl及Cu2O）及鉻（Cr及Cr2O3）為主。
為瞭解銅化合物對於灰渣中PCDD/Fs生成之影響，尤其在焚化煙道氣（flue gas）冷卻塔中灰渣之CuO及CuSO4比例及PCDD/Fs濃度進行關聯性研究。由焚化實廠數據之分析結果顯示，PCDD/Fs生成濃度可能與灰渣中CuO含量相關，而CuSO4可能抑制灰渣中PCDD/Fs的生成。
灰渣水洗可減少實驗室廢棄物焚化灰渣之氯含量（降低80~90%）及重量（減少65~99%），經不同液固比（L/S = 2、5、10、與20）測試結果，也考量用水量少與氯含量去除相對高之條件，發現液固比為5較有利於水洗實務應用。
為評估焚化操作效能，收集各空污防制設備（包括：冷卻塔及袋式集塵器）灰渣中重金屬之補集量，利用Data Envelopment Analysis (DEA)進行評估作業，結果發現，控制一次與二次燃燒室溫度分別為1173-1273 K及1273-1373 K時，可獲得較佳操作效率。
由同步輻射X光吸收光譜所獲得之分子尺度數據，可提供實驗室廢棄物焚化及電漿熔融實廠操作改善重要資料，也可作為後續系統效能提升之參考。

Ashes, which contain relatively high levels of toxic metals (e.g., copper and chromium) and polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs), discharged from laboratory wastes incineration are considered hazardous. The incineration ashes have been thermally stabilized with high-temperature plasma-assisted melting at the temperatures of 1673-1773 K. Detailed chemical structure of the toxic species in the ashes and slag is still lack in the literature. Thus the main objective of this work was to track toxic species, specifically copper, chromium, and PCDD/Fs, during incineration and melting. To better understand speciation of the toxic compounds in ashes and slags, their molecule-scale data were obtain by X-ray absorption (fine structure (EXAFS), X-ray absorption near edge structure (XANES)) and X-ray diffraction (XRD) spectroscopic methods.
Experimentally, by X-ray absorption spectroscopy, it is found that CuO and CuSO4 are the main copper compounds in the bottom and fly ashes, respectively. After thermal stabilization with the plasma melting, mainly metallic copper (Cu) (76%) and Cu2O (15%) are found in the slag. CuSiO2 is also observed, suggesting that copper may be encapsulated in the SiO2 matrix, which leads to formation of the thermally stable slag with a relatively low TCLP concentration of copper. The copper and chromium TCLP concentrations of slags sampled from the plasma melting reaction chamber are below the limit of Taiwan EPA. Low oxidation-state copper and chromium such as CuCl, Cu2O, Cr2O3 and Cr are found in the slag.
To learn how copper species play the key role in the formation of the relatively high PCDD/F concentrations in ashes, correlations of concentrations and fractions of CuO and CuSO4 with concentrations of PCDD/Fs in the cooling towers and baghouse filter ashes has been studied. The correlation between total concentrations of PCDD/Fs and fractions and concentrations of CuO or CuSO4 in the ash obtained from the commercial-scale incineration data suggest that the high PCDD/F concentrations may be associated with CuO in the ashes. Copper as CuSO4 can depress formation of PCDD/Fs in the ashes.
By washing, chloride contents and weight of incineration ashes can be reduced by 80-90% and 65-99%, respectively. Under liquid/solid (L/S) ratio of 5, low water consumption and relatively high chloride removal efficiency for ash washing is engineering feasible.
The incineration operation efficiency can be evaluated by effective capture of toxic metals in cooling towers and baghouse ashes. By data envelopment analysis (DEA), it is clear that the better operation temperature of the 1st and 2nd combustion chambers, are 1173-1273 and 1273-1373 K, respectively, which is to be applied in the practical operation.
It is also worth noting that the molecule-scale data obtained from synchrotron X-ray absorption spectra are well correlated with the findings from the full-scale laboratory waste incineration operation, which may be useful in process improvements.

CONTENTS
中文摘要	I
ABSTRACT	III
ACKNOWLEDGEMENT	V
CONTENTS	VI
TABLES	VIII
FIGURES	IX
ABBREVIATION LIST	XI
CHAPTER 1 INTRODUCTION	1
CHAPTER 2 LITERATURES REVIEW
2.1 Laboratory wastes managements	3
2.1.1 Incineration	3
2.1.2 Plasma melting	4
2.1.3 Available laboratory wastes treatment technologies	5
2.2 Toxic species in ashes and slags	22
2.2.1 Fate of toxic species in thermal treatment processes	22
2.2.2 Polychlorinated Dibenzo-p-dioxins and Dibenzofurans (PCDD/Fs)	27
2.2.3 Chemical structure analysis of ashes and slags	29
2.2.4 Application of molecular-scale data in engineering problem solving	30
2.3 Process efficiency analysis - Data Envelopment Analysis (DEA)	31
CHAPTER 3 EXPERIMENTS
3.1 Samples preparation	33
3.2 Characterization of toxic metals in ashes and slags	39
3.2.1 Total and TCLP concentration	39
3.2.1.1 X-ray fluorescence	39
3.2.1.2 Toxic characteristic leaching procedure	39
3.2.2 Chemical structure analysis	39
3.2.2.1 Extended X-Ray Absorption Fine Structure and X-ray Absorption Near Edge Structure	39
3.2.2.2 X-ray diffraction spectroscopy	40
3.3 Polychlorinated Dibenzo-p-dioxins and Dibenzofurans analyses	42
CHAPTER 4 RESULTS AND DISCUSSION
4.1 Fate of toxic metals in incineration and plasma melting processes	43
4.1.1 Speciation of copper in the thermally stabilized slag	43
4.1.2 Fate of copper in an ash/sludge plasma melting process	50
4.1.3 Tracking of chromium in an ash/sludge plasma melting process	58
4.2 Speciation of copper associated with PCDD/Fs formation during incineration flue gas cooling down	68
4.3 Washing of ashes and slag	77
4.4 Operation efficiency evaluation of laboratory waste incineration using Data Envelopment Analysis	90
CHAPTER 5 CONCLUSIONS	102
SUGGESTION	104
REFERENCES	105
APPENDIXES
	Appendix A Reduction benefits of laboratory wastes treatment intermediates	113
	Appendix B Primary Component Analysis (PCA) results of incineration ashes	114
Appendix C Free Energy of Copper compounds and metals chlorides	115
Appendix D Speciation of copper in slag discharged in the slag cart	117
Appendix E Publications	128
CURRICULUM VITAE	134
 
TABLES
Table 2.1.3.1 Experimental wastes classification and treatment procedures of the University of Tokyo	7
Table 2.1.3.2 Members of universities & schools in Taiwan	11
Table 2.1.3.3 Quantities of treated laboratory wastes in Taiwan (2005-2011)	12
Table 2.1.3.4 Laboratory wastes classifications and treatment procedures of ERMRC	14
Table 2.1.3.5 Typical contents of the ERMRC laboratory wastes	16
Table 2.2.1.1 Typical contents in ashes, sludges and slags	24
Table 2.2.1.2 Ashes characteristics of different wastes and treatment processes (Total)	25
Table 2.2.1.3 Ashes characteristics of different wastes and treatment processes (TCLP)	26
Table 2.3.1 Envelopment models with respect to the orientations and frontier types (Zhu, 2009)	32
Table 3.1.1 Ashes/slag washing and stabilization tests	38
Table 4.1.1.1 TCLP concentrations (mg/L) of toxic elements in incineration ashes and plasma melting slag	45
Table 4.1.1.2 Bond distances and coordination number (CN) of copper in the sludge, ashes and slag (obtained from refined EXAFS)	49
Table 4.1.2.1 Concentrations (mg/L) of leachable (TCLP) toxic elements in the incineration bag-house filters ash, inorganic wastewater sludge, and plasma melting	52
Table 4.1.2.2 Chemical structure parameters of copper in the ash, sludge and slags (determined by refined EXAFS)	54
Table 4.1.3.1 Concentrations of leachable chromium and fraction of Cr in the fly ash, sludge, and slags	62
Table 4.1.3.2 Speciation parameters of chromium in the slags (determined by refined EXAFS)	65
Table 4.2.1 Concentrations of total and leachable copper related to PCDD/F concentrations in the cooling towers and baghouse filter ashes	74
Table 4.3.1 Total metals contents in ashes	80
Table 4.3.2 Solid reduction of ashes washing process with water under L/S=10	81
Table 4.4.1 Operation parameters of incineration process	92
 
FIGURES
Fig. 2.1.3.1 Organic wastes treatment facilities of the University of Tokyo, Japan	8
Fig. 2.1.3.2 Inorganic wastes treatment facilities of the University of Tokyo, Japan	9
Fig. 2.1.3.3 Design concept of ERMRC treatment plant	13
Fig. 2.1.3.4 Incineration process of ERMRC	17
Fig. 2.1.3.5 Plasma melting process of ERMRC	19
Fig. 2.3.1.6 Physicochemical process of ERMRC	21
Fig. 3.1.1 Sampling points of incinerator of ERMRC	34
Fig. 3.1.2 Sampling points of plasma melting process of ERMRC	35
Fig. 3.1.3 Diagram of the plasma melting reaction chamber and slags sampling points	36
Fig. 3.1.4 Diagram of the cooling tower-I and ashes sampling points at various levels	37
Fig. 3.2.2.1 Scheme of typical X-ray absorption spectroscopic experiment	41
Fig. 4.1.1.1 XRD patterns of the incineration (a) bottom and (b) fly ashes and (c) plasma melting slag	46
Fig. 4.1.1.2 Component fitted XANES spectra of copper in the incineration (a) bottom and (b) fly ashes and (c) plasma melting slag	47
Fig. 4.1.2.1 XRD patterns of slags sampled at the melting zones of (a) 0 (surface), (b) -15, (c) -30, and (d) -50 cm (bottom) in the plasma melting chamber and (e) the slag discharged	55
Fig. 4.1.2.2 Component fitted XANES spectra of copper in slags sampled at the melting zones of (a) 0 (surface), (b) -15, (c) -30, and (d) -50 cm (bottom) in the plasma melting chamber and (e) the slag discharged	56
Fig. 4.1.3.1 Diagram of the plasma melting reaction chamber and slags sampling points	61
Fig. 4.1.3.2 XRD patterns of the slags (a) I, (b) II, (c) III, and (d) IV. (1: SiO2; 2: Cr2O3; 3: NaCl; 4: NaAlSiO4; 5: Na4AlSi3O12Cl)	63
Fig. 4.1.3.3 Component fitted XANES spectra of chromium in (a) sludge, (b) fly ash, and (c) slags	64
Fig. 4.1.3.4 Correlation between molar ratios of Cr/Cr2O3 and concentrations of leachable chromium in the slags at 1100-1700 K	67
 
FIGURES
Fig. 4.2.1 Total concentrations of toxic metals in the cooling tower-I ashes (deposited on the wall)	70
Fig. 4.2.2 Distribution of PCDD/F congeners in the cooling tower-I and baghouse filter ashes.	73
Fig. 4.2.3 Component fitted XANES spectra of copper in the (a) cooling tower-I, (b)                                                       cooling tower-II, and (c) baghouse filter ashes.	75	                                                                                                                                                                oncentrations of CuO or CuSO4 in 
Fig. 4.2.4 Correlation between PCDD/Fs and (a) fractions and (b) concentrations of CuO or CuSO4 in ashes.	76
Fig. 4.3.1 Chloride mass fractions in filtered liquids (FL) and washed residue (WR)	82
Fig. 4.3.2 Mass fractions of (a) Cu, (b) Zn, and (c) Ni in filtered liquids (FL) and washed residue (WR)	84
Fig. 4.3.3 Mass fractions of (a) Cr, (b) Hg, and (c) Pb in filtered liquids (FL) and washed residue (WR)	85
Fig. 4.3.4 Total contents of (a) Cu, (b) Zn, and (c) Ni in RM and WR	86
Fig. 4.3.5 Total contents of (a) Cr, (b) Hg, and (c) Pb in RM and WR	87
Fig. 4.3.6 TCLP concentrations of (a) Cu, (b) Zn, and (c) Ni in RM and WR	88
Fig. 4.3.7 TCLP concentrations of (a) Cr, (b) Hg, and (c) Pb in RM and WR	89
Fig. 4.4.1 Operation temperature zones of the incineration process	94
Fig. 4.4.2 Metals capture efficiencies in (a) cooling tower-I, (b) cooling tower-II, and (c) bag house	95
Fig. 4.4.3 Cr with sulfur/chlorine capture efficiencies in (a) cooling tower-I, (b) cooling tower-II, and (c) bag house	96
Fig. 4.4.4 Cu with sulfur/chlorine capture efficiencies in (a) cooling tower-I, (b) cooling tower-II, and (c) bag house	97
Fig. 4.4.5 Hg with sulfur/chlorine capture efficiencies in (a) cooling tower-I, (b) cooling tower-II, and (c) bag house	98
Fig. 4.4.6 Pb with sulfur/chlorine capture efficiencies in (a) cooling tower-I, (b) cooling tower-II, and (c) bag house	99
Fig. 4.4.7 Zn with sulfur/chlorine capture efficiencies in (a) cooling tower-I, (b) cooling tower-II, and (c) bag house	101

                                    

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