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研究生：	黃心亮 Huang, Hsin-Liang
論文名稱：	奈米銅鋅污染物之富集及再利用 Enrichment and Recycling of Nanosize Copper and Zinc Pollutants
指導教授：	王鴻博 Wang, H. Paul
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：	2007
畢業學年度：	95
語文別：	英文
論文頁數：	170
中文關鍵詞：	奈米污染物、離子熔液、分子篩、NMR 、EXAFS 、XANES
外文關鍵詞：	ionic liquids, nanopollutants, molecular sieves, XANES, EXAFS, NMR
相關次數：	點閱：114 下載：6
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長久以來，只重視次微米 (0.5 μm)大小以上之懸浮固體或氣膠之污染防冶及研究，毒性懸浮粒子可能包含奈米 (<100 nm)活性物質，特性也未完全了解，事實上奈米污染早已潛藏在環境之中，微奈米污染物之可能危害性，也是因最近幾年之奈米技術蓬勃發展而被挑起重視，對環境/公共衛生及人體健康可能是一重大隱憂，，因此奈米污染物質之分離及富集也因而成為重要研發課題。
本研究之主要目的是: (1) 研究化學機械研磨 (chemical mechanical plannarization (CMP))廢水中之奈米銅吸附於中孔洞分子篩(MCM-41)之微細結構；(2)以中孔洞分子篩富集含銅鋅水溶液廢中金屬之化學結構；(3) 利用EXAFS(X射線吸收光譜之延伸區微細結構)及XANES(X射線吸收近邊緣結構)研究空氣、水、土壤、廢觸媒及螢光粉中之奈米污染物，富集於常溫離子熔液(room temperature ionic liquid (RTIL) [C4mim][PF6])之化學結構變化。
實驗結果顯示，分子篩MCM-41及表面改質之MCM-41S及MCM-41N可富集CMP廢水中70~98%銅，XANES光譜圖顯示，銅在MCM-41、MCM-41S及MCM-41N中以吸附型態及奈米氧化銅為主，在富集過程MCM-41S及MCM-41N中也可提高奈米氧化銅之溶解度；吸附反應包括: (1)提高奈米氧化銅之溶解度及(2)銅離子吸附於MCM-41S及MCM-41N之孔洞中。
XANES光譜圖顯示，在573 K時，銅鋅合金可於MCM-41孔洞中形成，奈米金屬鋅及銅分別於T<573 K及923~1173 K；在1173 K下，由於奈米氧化銅之聚集，中心銅原子至第一層氧3.3個原子的距離增加為1.97 Å，鋅與MCM-41S之非結晶型態SiO2反應，中心鋅原子距第一層之氧原子的距離減少0.02 Å。
常溫離子熔液 [C4mim][PF6])可有效萃取化學機械研磨 (chemical mechanical plannarization (CMP))廢水中之奈米銅，在2分鐘內，萃取效率約94%，離子熔液亦可有效萃取空氣中之氧化銅、吸附於MCM-41中銅(模擬受銅污染之土壤)及奈米銅，萃取之反應機制是: (1)提高奈米金屬粒子之溶解度及(2)奈米金屬粒子形成離子態，並形成[Cu(MIm)4(H2O)2]2+於離子熔液中。離子熔液也可利用於萃取MCM-41之氧化銅(模擬廢觸媒)，萃取反應之活化能為475 cal/mole，反應機制包括: (1)奈米氧化銅由MCM-41遷移至離子熔液中及(2)奈米金屬粒子溶解形成離子態，並形成Cu (MIm)42+。離子熔液也可有效萃取螢光粉中之奈米鋅粒子，XANES光譜顯示，萃取之硫化鋅可於T<524 K氧化生成氧化鋅。
本論文研究之主要研究成果包括: (1) 了解奈米銅或鋅在環境介質中之分離、轉移及富集反應機制；(2)了解環境中毒性金屬(銅、鋅)之分子化學結構極可能涉及之反應機制，有利於應用昔知化學方法(而非嘗試性)解決污染防治問題；(3)應用綠色溶劑(離子熔液)選擇性回收或富集有害廢棄物中(例如螢光粉)之有價金屬。

Nano scale particles (<100 nm) that are generally negligible in the traditional air pollutant control device are directly emitted to environment. The impact of the hidden danger of nanopollutants on the environment and human health still lack in the literature. The main objective of this work was to study extraction of nanopollutants in air, waster, soils and spent catalysts with mesoporous molecular sieves (MCM-41) and a RTIL (room temperature ionic liquid ([C4mim][PF6], 1-butyl-3-methylimidazolium hexafluoro- phosphate)). In addition, molecular scale data of species involved in the extraction process were also determined by X-ray absorption fine structural (EXAFS) and X-ray absorption near edge structural (XANES) spectoscopies, nuclear magnetic resonance (NMR), X-ray diffraction (XRD) and transmission electron microscopy (TEM).
Experimentally, 70-98% of copper in the CMP wastewater can be extracted with MCM-41, MCM-41S (surface modified with (HS(CH2)3-Si(OM)3)) and MCM-41N (surface modified with (H2N(CH2)3-Si(OM)3)). By XANES, it is found that the main copper species in MCM-41, MCM-41S and MCM-41N are Cu(II)(ads) and nanosize CuO. An enchanced dissolution of nanosize CuO in the presence of MCM-41S and MCM-41N was also observed. At least two reaction paths may be involved in the extraction process: (1) an enhanced dissolution of nanosize CuO and (2) extraction of Cu2+ into MCM-41N and MCM-41S.
Experimentally, extraction of nanosize CuO in the CMP wastewater with a RTIL ([C4mim][PF6]) is very effective. In a very short contact time (about two minutes), 80-95% of nano CuO as well as other forms of copper (such as nano Cu, Cu2+, or Cu(II)(ads) (in the channels of MCM-41)) in the CMP wastewater can be extracted into the RTIL. At least two possible reaction paths for the rapid extraction of nanosize copper pollutants with the RTIL may occur: (1) an enhanced dissolution of nano CuO (to form Cu2+) and (2) formation of [Cu(MIm)4(H2O)2]2+ that acts as a carrier of copper into the RTIL matrix.
Extraction of nanosize CuO in the channels of MCM-41 at 298-373 K, that simulates recovery valuable metals in the spent catalysts, has been conducted. Three possibilities during extraction process are involved: (1) migration of nanosize CuO from channels of MCM-41 into the RTIL, (2) dissolution of nanosize CuO, and (3) formation of Cu(MIm)42+ in the RTIL. Enhanced extraction of Zn from phosphor particulates in the RTIL was also found. ZnS can be oxidized to form ZnO effectively at <523 K in the RTIL.
The main achievements of this work include: (1) an understanding of nature of nanosize copper and zinc during separation, transportation, and enrichment processes; (2) a molecular-scale observation of chemical structure of toxic elements (copper and zinc) in the environment, that may be very helpful in the development of effective methods for remediation; and (3) a finding of utilization of RTILs in selective recycling or enrichment of nanosize toxic pollutants in the phosphor wastes.

CONTENT
	Page	  
中文摘要	I
ABSTRACT	III
CONTENT	V
LIST OF TABLES	VIII
LIST OF FIGURES	X

CHAPTER 1	INTRODUCTION	1

CHAPTER 2	LITERATURE SURVEY	3
2.1	Nnaometal Pollutants	3
2.1.1 Nanoparticles in Phosphor waste	4
2.1.2 Nanoparticles in CMP Wastewater	6
2.1.3 Spent Catalysts	9
2.2	Toxicity of Nanoparticles	13
2.3	Absorbents	17
2.3.1 Molecular Sieves	17
2.3.2 Ionic Liquids	21

CHAPTER 3	EXPERIMENTAL METHODS	26
3.1	Preparation of Samples	26
3.1.1	Nanopollution	26
3.1.2	Absorbents	26
3.1.2.1 Synthesis of MCM-41	26
3.1.2.2 Synthesis of Modified MCM-41	29
3.1.2.3 Synthesis of Ionic Liquids	31
3.2	Extraction	31
3.2.1	Extraction of Nanosize Copper from CMP Wastewater in Molecular Sieves	31
3.2.2	Adsorption of Copper and Zinc in Molecular Sieves	31
3.2.3	Extraction of Nanometal Pollutants in an Ionic Liquid	31
3.3	Structural Analyses	34
3.3.1	X-ray Diffraction Spectroscopy (XRD)	34
3.3.2	Transmission Electron Mmicroscope (TEM)	34
3.3.3	Nuclear Magnetic Resonance (NMR) 	34
3.3.4	Atomic Absorption Spectroscopy (AA)	34
3.3.5	Elemental Analyzed (EA)	34
3.3.6	X-ray Absorption Spectroscopy (XAS)	35
	
CHAPTER 4	RESULTS AND DISCUSSION	41
4.1	Speciation of Nanosize Copper in CMP Wastewater Extracted with MCM-41 and Y	41
4.2	Extraction of Nanosize Copper in the CMP Wastewater with Modified MCM-41 	48
4.3	Interactions of Copper Extracted from the CMP Wastewater with Modified Surface of MCM-41	54
4.4	Interactions of Copper and Zinc in MCM-41	59
4.5	Speciation and Distribution of Copper and Zinc in Modified MCM-41	67
4.6	X-Ray Adsorption Studies of Copper in MCM-41	74
4.7	Speciation of Copper in Modified MCM-41	80
4.8	Extraction of Nanosize Copper Pollutants with an Ionic Liquid	87
4.9	Extraction of Copper in MCM-41 with an Ionic Liquid	97
4.10	Extraction of Nanosize Zinc in Phosphor Waste with an Ionic Liquid	107
4.11	Engineering Applications	116

CHAPTER 5 CONCLUSIONS	118

APPENDIXS	121
Appendix A Speciation of Chromium in Swarf during Pyrolysis	122
Appendix B Pyrolysis Kinetics of Swarf Waste	128
Appendix C Speciation of Chromium in Thermally Stabilized Swarf Waste	135
Appendix D Speciation Zinc in Channels of MCM-41S	143
Appendix E Interactions of Copper and Zinc in Modified MCM-41	146
Appendix F Copper Isotherms of Molecular Sieves	149
REFERENCES	153

CURRICULUM VITAE	167

 TABLES
	Page
Table 2.1.1	Emissive sources of heavy metals in nanopollutants	5
Table 2.1.2	Generally properties of CMP wastewater	9
Table 2.1.3	Major species in the CMP wastewater	10
Table 2.1.4	Concentrations of main elements in CMP wastewater	11
Table 2.1.5	Major species in spent catalysts	12
Table 2.3.1	The characteristics of several hydrophobic RTILs	23
Table 3.1.1	Properties of CMP wastewater from a semiconductor industry in the southern Taiwan.	27
Table 3.1.2	The concentrations of main elements in MCM-41, MCM-41S, MCM-41N, MCM-41-SH, and MCM-41-NH2.	32
Table 3.3.1	Purity, source and synthesis method of copper model compounds	37
Table 3.3.2	Purity, source and synthesis method of zinc model compounds	38
Table 4.1.1	Concentrations of copper extracted in MCM-41 and Y from the CMP wastewater	44
Table 4.1.2	Speciation parameters of copper in MCM-41 and Y	46
Table 4.2.1	Extraction of copper (mg/g) in the CMP wastewater with MCM-41, MCM-41S, and MCM-41N	50
Table 4.2.2	Speciation of adsorbed copper or MCM-41, MCM-41S, and MCM-41N	53
Table 4.3.1	Concentrations (mg/kg) of copper (in CMP wastewater) extracted in MCM-41-NH2	55
Table 4.3.2	Speciation data of copper (in CMP wastewater) extracted in MCM-41-NH2	58
Table 4.4.1	Structural parameters of copper and zinc in MCM-41 during calcination at 573-1173 K for two hrs	65
Table 4.5.1	Structural parameters of copper and zinc in MCM-41-SH after calcination at 573-1173 K for two hrs	73
Table 4.6.1	Fractions of copper extracted in (MCM-41) calcinated at 573-923 K for two hrs (studied by XANES)	76
Table 4.6.2	Speciation of copper in MCM-41 calcinated at 573-923 K for two hrs (studies by EXAFS)	79
Table 4.7.1	Speciation of copper in MCM-41-S calcinated at 573-1173 K for two hrs (studies by EXAFS)	85
Table 4.8.1	Speciation of copper in the CMP wastewater, Cu(II)/MCM-41 and nanosize Cu and those were extracted in the RTIL	96
Table 4.9.1	Speciation parameters of copper migrated from MCM-41 to the RTIL	106
Table 4.10.1	Speciation parameters of zinc in phosphor and phosphor-extracted RTIL at 298-523 K for 30 min	114
Table A.1	Speciation parameters of chromium in the swarf studies by EXAFS	127
Table B.1	Kinetic parameters for pyrolysis of swarf waste at 400-700 K	134
Table C.1	Speciation parameters of chromium in the swarf studies by EXAFS	141
Table D.1	Speciation changes of zinc in MCM-41-SH after calcination at 573-1173 K for two hrs	145
Table E.1	Structural parameters of copper and zinc in MCM-41S after calcination at 573-1173 K for two hrs	148


 
FIGURES
	Page
Figure 2.1.1	Schematic presentation of lateral friction instrument	7
Figure 2.2.1	Fraction of atoms on the outer surface (D) as a function of particle size (d)	14
Figure 2.2.2	Mechanisms of nanomaterials in medical application and toxicological effect	15
Figure 2.3.1	Schematic composite diagram of the surfactant silica organization in aqueous solution	18
Figure 2.3.2	Structures of thiols on SiO2	20
Figure 2.3.3	Dependence of melting point and phase diagram of [Cnmim][PF6] ionic liquids on the alkyl chain length (n)	22
Figure 2.3.4	Cations in the RTILs	24
Figure 3.1.1	X-ray diffraction pattern of the MCM-41	28
Figure 3.1.2	29Si SSNMR spectra of (a) MCM-41, (b) MCM-41S, and (c) MCM-41N	30
Figure 3.1.3	1H NMR spectrum of the RTIL ([C4min][PF6])	33
Figure 3.3.1	A schematic illustration of typical X-ray absorption spectroscopic experiment	39
Figure 3.3.2	Research scope of enrichment of nanosize copper and zinc pollutants	40
Figure 4.1.1	(a) Dark-field image and (b) diffraction pattern of nanosize CuO in the CMP wastewater	43
Figure 4.1.2	Experimental data (solid line) and the least-squares fits (circles) for the XANES spectra of copper species in (a) CMP wastewater and copper extracted in (b) MCM-41 and (c) Y.  The dotted line denotes the best fits of the XANES spectra	45
Figure 4.2.1	Experimental data (solid line) and the least-squares fits (circles) for the XANES spectra of copper species in (a) MCM-41, (b) MCM-41S and (c) MCM-41N.  The dotted line denotes the best fits of the XANES spectra	52
Figure 4.3.1	Experimental data (solid line) and the least-squares fits (circles) for the XANES spectra of copper in (a) MCM-41-NH2 and (b) calcined at 923 K for two hrs.  The dotted line denotes the best fits of the XANES spectra	57
Figure 4.4.1	XRD patterns of (a) dried (at 333 K for 16 hrs) and calcined CuO-ZnO/MCM-41 at (b) 573, (c) 923, and (d) 1173 K for two hrs. (1: SiO2, 2: Zn2SiO4, 3: CuO)	60
Figure 4.4.2	Experimental data (solid line) and the least-squares fits (circles) of XANES spectra of copper in (a) dried and calcined CuO-ZnO/MCM-41 at (b) 573, (c) 923, and (d) 1173 K	62
Figure 4.4.3	Experimental data of XANES spectra of zinc in (a) dried and calcined CuO-ZnO/MCM-41 at (d) 573, (e) 923, and (f) 1173 K for two hrs	63
Figure 4.4.4	Fourier transformed Cu and Zn K edge EXAFS of CuO-ZnO/MCM-41 which was (a) dried and calcined at (b) 573, (c) 923, and (d) 1173 K.	64
Figure 4.5.1	XRD patterns of (a) dried (at 383 K for 16 hours) and calcined (at (b) 573, (c) 923, and (d) 1173 K for two hrs) CuO-ZnO/MCM-41-SH. (1: Zn2SiO4; 2: CuO)	69
Figure 4.5.2	Experimental data (solid line) and the least-squares fits (circles) of XANES spectra of copper in (a) dried and calcined (at (b) 573, (c) 923, and (d) 1173 K) CuO-ZnO/MCM-41-SH and zinc in (e) dried and calcined CuO-ZnO/MCM-41-SH at (f) 573, (g) 923, and (h) 1173 K.	70
Figure 4.5.3	Temperature dependence for the Zn/Cu ratio in the channels of MCM-41-SH and the possible reaction path during calcination at 573-1173 K for two hrs	72
Figure 4.6.1	XRD patterns of (a) dried (at 383 K for 16 hrs) and calcined copper/MCM-41 at (b) 573 and (c) 923 for two hrs.	75
Figure 4.6.2	(a) Dark-field (calcined at 573 K) and (b) dark-field (923 K), bright-field (923 K) images and (d) diffraction pattern (923 K) of copper/MCM-41.	78
Figure 4.7.1	XRD patterns of (a) dried (at 383 K for 16 hrs) and calcined copper/MCM-41-SH at (b) 573, (c) 923, and (d) 1173 K for two hrs. (*: CuO)	81
Figure 4.7.2	X-ray absorption near edge structural (XANES) spectra of copper in (a) dried and calcined copper/MCM-41S at (b) 573, (c) 923, and (d) 1173 K	83
Figure 4.7.3	TEM image of copper/MCM-41S at 1173 K.	84
Figure 4.8.1	XANES spectra of (a) nanosize CuO and (b) that was extracted into the RTIL ([C4mim][PF6])	90
Figure 4.8.2	Experimental data (solid line) and the least-squares fits (circles) of XANES spectra of copper in (a) CMP wastewater, (b) Cu(II)/MCM-41 and (c) nanosize Cu (in 2-propanol) and that was extracted into the RTIL from (d) CMP wastewater, (e) Cu(II)/MCM-41 and (f) nanosize Cu	91
Figure 4.8.3	1H NMR spectra of (a) CMP wastewater and (b) nanosize CuO extracted in the RTIL and (c) RTIL ([C4min][PF6]))	93
Figure 4.8.4	1H NMR spectra of (a) nanosize CuO extracted in 1-methylimidazole (MIm) and (b) MIm	94
Figure 4.9.1	(a) Diffraction pattern and (b) dark-field image of nanosize CuO suspended in the RTIL	99
Figure 4.9.2	Time dependence for migration of copper into RTIL.	100
Figure 4.9.3	Diffusion kinetics for extraction of copper in MCM-41 with the RTIL	101
Figure 4.9.4	1H NMR spectra of (a) copper-extracted RTIL and (b) RTIL	103
Figure 4.9.5	XANES spectra of copper (a) in MCM-41 and extracted with the RTIL for (b) 30 min, (c) 12 hrs, and (d) one (e) three, and (f) 14 days.	104
Figure 4.10.1	1H NMR spectra of (a) RTIL ([C4min][PF6]) and (b) phosphor-extracted RTIL at 298 K.	109
Figure 4.10.2	XANES spectra of zinc in the (a) phosphor and extracted in the RTIL at (b) 298, (c) 423, and (d) 523 K for 30 min	110
Figure 4.10.3	(a) Diffraction pattern and (b) dark-field image of zinc species suspended in the RTIL at 298 K	111
Figure 4.10.4	1H NMR spectra of (a) Zn extracted 1-methylimidazole (MIm) at 298 K and (b) MIm.	113
Figure 4.11.1	Recovery of nano metal pollutants that escape from the traditional filtration processes.	117
Figure A.1	Thermal gravimetric analysis of the swarf waste	124
Figure A.2	Experimental data (solid line) and the least-squares fits (circles) of XANES spectra of chromium in the (a) swarf and that was pyrolyzed at (b) 673, (c) 773, and (d) 873 K	125
Figure B.1	Experimental data (solid line) and the least-squares fits (circles) of XANES spectra of chromium in (a) the swarf waste and (b) that were pyrolyzed at 873 K	130
Figure B.2	(A) TGA (thermogravimetric analysis) and DTA (differential thermal analysis) of the swarf waste at 360-1000 K in the 100 mL/min N2 and (B) FTIR spectra (CH stretchings) of gas products during TGA (denoted with in (a)-(e) in (A))	132
Figure C.1	Thermogravimetric analysis and (b) differential thermal analysis of the swarf waste	137
Figure C.2	SEM micrographs of (a) the swarf waste and that was thermally treated at (b) 673, (c) 1073, and (d) 1473 K for four hrs	139
Figure C.3	Experimental data (solid line) and the least-squares fits (circles) of XANES spectra of chromium in the swarf waste during thermal treatments at (a) 673 and (b) 1073, (c) 1473 K for four hrs.	140
Figure D.1	XRD patterns of (a) dried (at 383 K for 16 hrs) and calcined (at (b) 573, (c) 923, and (d) 1173 K for two hrs) ZnO/MCM-41-SH. (*: Zn2SiO4)	143
Figure D.2	Experimental data (solid line) and the least-squares fits (circles) of XANES spectra of zinc in (a) dried and calcined (at (b) 573, (c) 923, and (d) 1173 K) ZnO/MCM-41-SH.	144
Figure E.1	X-ray diffraction patterns of (a) dried and calcined CuO-ZnO/MCM-41S at (b) 573, (c) 923, and (d) 1173 K. (1: Zn2SiO4, 2: SiO2, 3: CuO)	146
Figure E.2	Experimental data (solid line) and the least-squares fits (circles) of XANES spectra of copper in (a) dried and calcined (at (b) 573, (c) 923, and (d) 1173 K) CuO-ZnO/MCM-41S and zinc in (e) dried and calcined CuO-ZnO/MCM-41S at (f) 573, (g) 923, and (h) 1173 K	147
Figure F.1	Copper isotherms of Y	149
Figure F.2	Copper isotherms of MCM-41	150
Figure F.3	Copper isotherms of MCM-41S	151
Figure F.4	Copper isotherms of MCM-41N	152
                                    

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