銅修飾二氧化鈦光催化降解新興污染物之研究:以BPA及SMX為例

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研究生：	江麗芬 Chiang, Li Fen
論文名稱：	銅修飾二氧化鈦光催化降解新興污染物之研究:以BPA及SMX為例 Copper modified-TiO2 photocatalysts for the degradation of BPA and SMX
指導教授：	董瑞安 Doong, Ruey An
口試委員:	盧明俊白曛綾盧重興吳劍侯王竹方
學位類別：	博士 Doctor
系所名稱：	原子科學院 - 生醫工程與環境科學系 Department of Biomedical Engineering and Environmental Sciences
論文出版年：	2015
畢業學年度：	103
語文別：	英文
論文頁數：	139
中文關鍵詞：	銅修飾二氧化鈦、磺胺甲噁唑、雙酚A
外文關鍵詞：	Cu-TiO2, SMX, BPA
相關次數：	點閱：2 下載：0
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銅修飾二氧化鈦為一新型環境淨化材料，其廣泛的被應用在光催化降解及氫能源還原的領域。在光催化降解部分，目前已有許多銅修飾二氧化鈦的合成方法，但因不同的方法所產生的銅物種的不同所造成的影響也不一樣，因此，系統性比較不同銅物種對二氧化鈦的影響為相當重要的課題。故本研究的主要目的是嘗試利用微波輔助浸滲(microwave-assisted impregnation)合成Cu2+-TiO2，高溫熱處理(high temperature heating)合成CuO-TiO2及化學還原(chemical reduction)合成Cu0-TiO2且利用雙酚A(BPA)及磺胺甲噁唑(SMX)來進行銅修飾二氧化鈦之光催化效能評估。
在Cu2+-TiO2部分，主要是利用微波輔助浸滲法來合成0.006-0.065 wt% Cu2+-P25和0.012-0.072 wt% Cu2+-ST01。Cu2+-TiO2主要是由二價的CuO修飾在二氧化鈦上。而Cu2+-TiO2中的Cu2+提供一個能階，故能縮短其電子跳躍的距離且降低電子電洞再結合的能力而有效的提升其可見光催化效能。在SMX的可見光催化降解部分，Cu2+-P25的反應速率為P25的2.9-14倍且0.045 wt% Cu2+-P25具有最佳的光催化效能。在BPA的可見光催化降解部分，Cu2+-P25的反應速率為P25的1.5-2.3倍且0.039 wt% Cu2+-P25具有最佳的光催化效能。而Cu2+-ST01的反應速率為ST01的1.5-3.7倍且0.055 wt% Cu2+-ST01具有最佳的光催化效能。
在CuO-TiO2部分，主要是利用高溫熱處理法來合成1.1-22.4 wt% CuO-TiO2奈米棒。CuO-TiO2奈米棒主要是由二價的CuO和Cu(OH)2修飾在二氧化鈦上。而CuO -TiO2奈米棒中的CuO提供一個儲存電子的位置，故能降低TiO2電子電洞再結合的能力而有效的提升其紫外光催化效能。在BPA的紫外光催化降解部分，CuO-TiO2奈米棒的反應速率為TiO2奈米棒的0.5-5.5倍。

在Cu0-TiO2部分，主要是利用化學還原法來合成0.4-20.0 wt% Cu0-TiO2奈米棒。Cu0-TiO2奈米棒主要是由Cu2O和Cu0修飾在二氧化鈦上。而Cu0-TiO2奈米棒中的Cu0提供一個儲存電子的位置，故能降低二氧化鈦電子電洞再結合的能力而有效的提升其紫外光催化效能。在可見光狀況下，可見光激發Cu2O產生光電子且經由Cu0到TiO2，故能在可見光下進行光催化反應且降低電子電洞再結合的能力而有效的提升其光催化效能。在BPA的紫外光催化降解部分，Cu0-TiO2奈米棒的反應速率為TiO2奈米棒的1.3-18.4倍且6.9 wt% Cu0-TiO2奈米棒具有最佳的光催化效能。在BPA的可見光催化降解部分，Cu0-TiO2奈米棒的反應速率為TiO2奈米棒的反應速率分別為P25跟Cu-P25的6跟5倍。
本研究結果顯示銅修飾TiO2催化劑能有效率被紫外光跟可見光激發來降解BPA跟SMX且銅修飾TiO2也極具潛力來降解其他新興汙染物。

Copper-based TiO2 have been demonstrated to be a potential photocatalyst for
photodegradation and hydrogen production. In the photodegradation area, many
method had been used to synthesize different Cu species-TiO2, which caused different
effects in the photodegradation. Therefore, a systematic comparison for different Cu
species on TiO2 is needed. The main purpose of this study is to use
microwave-assisted impregnation, high temperature heating and chemical reduction to
synthesize Cu2+-TiO2, CuO-TiO2 and Cu0-TiO2, respectively. Bisphenol A (BPA) and
sulfamethoxazole (SMX) were used as target compounds to evaluate the
photodegradation efficiency and rate of different Cu species-TiO2.
Cu2+-TiO2 was synthesized by microwave-assisted impregnation. The mass
loadings of Cu(II) were 0.006-0.065 wt% copper for P25 and 0.012-0.072 wt% copper
for ST01 and the major species of copper was CuO on the Cu-P25. Due to the redox
potential of Cu(II)/Cu(I) (0.3-0.5 V vs. SHE) and copper oxide as an electron
mediator, Cu2+-TiO2 have the potential to enable the absorption of light not only in the
ultraviolet but also in the visible light wavelength region and reduce the e/h
recombination to improve the photocatalytic efficiency. The pseudo-first-order rate
constants (kobs) for SMX photodegradation by Cu2+-P25 were 2.9–14.1 times higher
than that of pure Degussa P25 and the relative activity of Cu2+-P25 for BPA
photodegradation was 1.5-2.3 times. The relative activity of Cu2+-ST01 for BPA
photodegradation was 1.5-3.7 times. The optimal loading of Cu(II) to enhance the
photocatalytic activity of P25 and ST01 were 0.045 wt% and 0.055 wt%, respectively.

CuO-TiO2 nanorods were synthesized by high temperature heating and
CuO-TiO2 nanorods contain 1.1-22.4 wt% copper with CuO and Cu(OH)2 on
CuO-TiO2. CuO on the CuO-TiO2 nanorods was as an electron tank to reduce the e/h
recombination and improve the photocatalytic efficiency under the UV light
irradiation. BPA were used to evaluate the photodegradation efficiency and rate of
Cu-TiO2 nanorods under the irradiation of 365 nm UV light. The relative activity of
CuO-TiO2 nanorods were 0.5-5.5 times.
Cu0-TiO2 nanorods with 0.4-20.0 wt% copper were synthesized by chemical
reduction. The XRD and XPS results indicated that Cu species on the Cu-TiO2
nanorods were mainly Cu2O and Cu0. Cu0 as an electron tank on the Cu0-TiO2
nanorods reduce the e/h recombination and improve the photocatalytic efficiency
under the UV light irradiation. Cu2O was a semiconductor to excite by visible light
and produce electron to Cu0 and TiO2 to improve the photocatalytic efficiency. The
Cu0-TiO2 nanorods exhibited excellent photocatalytic activity towards BPA
photodegradation. The relative activity of Cu0-TiO2 nanorods were 1.3-18.4 times and
the optimal loading of Cu to enhance the photocatalytic activity of TiO2 nanorods
were 6.9 wt%. In addition, the kobs for BPA photodegradation by 6.9 wt% Cu0-TiO2
nanorods increases by factors of 6 for P25 and 5 for Cu0-P25 in the presence of 460 
40 nm visible light.
Results obtained in this study clearly demonstrate that Cu modified-TiO2
nanomaterials are an effective photocatalyst for degradation of BPA and SMX under
UV or visible light conditions and have potential to decompose emerging pollutants.

Content index
中文摘要    I
Abstract    III
Content index    V
Figure index    VIII
Table index    XII
Chapter 1 Introduction    1
1.1 Motivation    1
1.2 Objectives    3
Chapter 2. Background and theory    4
2.1Titanium dioxide    4
2.1.1 Progress in TiO2 photocatalysis: a shorthistorical overview    4
2.1.2 TiO2 structures and properties    4
2.1.3 Mechanisms of TiO2 photocatalysis    6
2.2 Synthetic methods for TiO2nanostructures    8
2.2.1 Sol−gel method    10
2.2.2 Nonhydrolytic sol-gel method    11
2.2.3 Hydrothermal method    13
2.2.4 Solvothermal method    13
2.2.5 Microwave-assisted method    14
2.3 Modification of TiO2 photocatalyst    16
2.3.1 Metal deposition    17
2.3.2 Heterostructures    18
2.3.3 Doping    20
2.4 The preparation of copper-based TiO2 photocatalyst    21
2.5 Emerging contaminants (ECs)    30
2.5.1 Bisphenol A    30
2.5.2 Sulfomethoxazole (SMX)    35
Chapter 3 Materials and methods    39
3.1 Experimental design    39
3.2 Experimental details for material synthesis    41
3.2.1 Chemicals    41
3.2.2 Synthesis of TiO2 nanomaterials    42
3.2.3 Fabrication of Cu2+-TiO2 composites by microwave-assisted impregnation method    44
3.2.4 Synthesis of CuO-TiO2 nanorod composites by high temperature heating method    45
3.2.5 Synthesis of Cu0-TiO2 nanorod composites by chemical reduction method    46
3.3 Photodegradation    47
3.3.1 Photodegradation of SMX and BPA by Cu-TiO2-based nanomaterials    ………………………………..…………………………………………………………………..47
3.3.2 pH effect    48
3.3.3 Stability    48
3.3.4 Visible light    49
3.3.5 BPA and SMX analysis    49
3.4 Characterization    50
3.4.1 TEM and EDX    52
3.4.2 BET    52
3.4.3 X-ray diffraction (XRD)    52
3.4.4 Thermal analysis (TGA)    53
3.4.5 Electron probe microanalyzer (EPMA)    53
3.4.6 X-ray adsorption near-edge structure (XANES)    53
3.4.7 High resolution X-ray Photoelectron Spectrometer (XPS)    54
3.4.8 Ultraviolet-Visible (UV-Vis) spectroscopy    54
3.4.9 Energy dispersive X-ray spectroscopy (EDX)    55
3.4.10 Inductively coupled plasma-optical emission spectroscopy (ICP-OES)        55
3.4.11 Particle size    55
Chapter 4 Results and discussion    56
4.1 Fabrication of Cu2+-TiO2 with commercial P25 and ST01    56
4.1.1 Morphology and Crystallization of Cu-TiO2    57
4.1.2 Specific surface area and pore textures of Cu2+-TiO2    64
4.1.3 Copper species characterizationof Cu2+-TiO2    68
4.1.4 Optical property of Cu2+-TiO2    70
4.1.5 Effect of copper concentration on photodegradation of SMX    72
4.1.5 Effect of pH on photodegradation of SMX    74
4.1.6 Effect of copper concentration on photodegradation of BPA (Cu2+-P25)    …    79
4.1.7 The photodegradation of BPA under the irradiation of visible light            81
4.1.8 Effect of pH on photodegradation of BPA    82
4.1.9 Effect of copper concentration on photodegradation of BPA (Cu2+-ST01)    83
4.2 Fabrication of TiO2 nanomaterials    88
4.2.1 Morphology and crystallization of TiO2 nanorods    88
4.2.2The photodegradation of BPA with TiO2 nanorods    91
4.3 Synthesis of different Cu species-TiO2 nanocomposties by different methods    92
4.3.1 Cu2+-TiO2 nanorod--Microwave-assisted impregnation method    92
4.3.2 CuO-TiO2 nanorod--High temperature heating method    95
4.3.2.1 Morphology and crystallization of CuO-TiO2 nanorods    95
4.3.2.2 Specific surface area and pore textures of CuO-TiO2 nanorods    98
4.3.2.3 Copper species characterization of CuO-TiO2 nanorods    101
4.3.2.3 The photodegradation of BPA of CuO-TiO2 nanorods    102
4.3.3 Cu0-TiO2 nanorod—Chemical reduction method    104
4.3.3.1 Morphology and crystallization of Cu0-TiO2 nanorods    104
4.3.3.1    Specific surface area and pore textures of Cu0-TiO2 nanorods            109
4.3.3.3 Photodegradation of BPA by Cu0-TiO2 nanorods under Visible light irradiation condition    119
4.3.3.4 Photodegradation of BPA by Cu-TiO2 nanorods by chemical reduction methodin the presence of humic acid    121
Chapter 5 Conclusions and suggestion    123
5.1 Conclusions    123
5.2 Suggestion    125
Reference    127

 
Figure index
Figure 1-1. Applications of TiO2 photocatalysis    2
Figure 2-1. Crystalline structures of titanium dioxide (a) anatase, (b) rutile, (c) brookite.    5
Figure 2-2. Schematic illustration of the formation of photogenerated charge carriers(hole and electron) upon absorption of UV light.    7
Figure 2-3. Processes occurring on bare TiO2 particles after UV excitation.    7
Figure 2-4. Various steps in the sol–gel process to control the final morphology of the product    11
Figure 2-5. Inverted temperature gradients in microwave versus oil-bath heating: difference in the temperature profiles after 1 min of microwave irradiation (left) and treatment in an oil-bath (right).    15
Figure 2-6. Various modification methods of TiO2 photocatalyst    16
Figure 2-7. Fermi level equilibration in a semiconductor-metal nanocomposite system    17
Figure 2-8. Schematic diagram showing the energy band structure and electron–hole pair separation in the p–n heterojunction.    19
Figure 2-9. The chemical structure of bisphenol A.    31
Figure 2-10. The chemical structure of SMX.    35
Figure 3-1. Flowchart of the fabrication Cu-TiO2 nanomaterials and their photocatalysis application.    40
Figure 3-2. Synthesis of TiO2 nanorod.    42
Figure 3-3. The ligand exchange procedure for TiO2 nanorods/nanowire.    43
Figure 3-4. Fabrication of Cu2+-P25 or Cu2+-ST01 or Cu2+-TiO2 nanorod by microwave-assisted impregnation method.    44
Figure 3-5. Fabrication of CuO-TiO2 nanorods by high temperature heating method.    45
Figure 3-6. Fabrication of Cu0-TiO2 nanorods by chemical reduction method.    46
Figure 3-7. The spectrum of fluorescent lamp. (a) UV light, (b) Visible light.    48
Figure 4-1. The TEM images of Degussa P25 (a) and Degussa P25 with different copper contents (b) 0.006, (c) 0.016, (d) 0.039, (e) 0.045, and (f) 0.063 wt%    58
Figure 4-2. The TEM images of ST01 (a) and ST01 with different copper contents (b) 0.012, (c) 0.022, (d) 0.045, (e) 0.055, and (f) 0.072 wt%.    59
Figure 4-3. The XRD patterns of Degussa P25 and Cu2+-P25. The mass loadings of Cu were in the range of 0.016-0.063 wt%.    60
Figure 4-4. The XRD patterns of pure ST01 and Cu2+-ST01. The mass loadings of Cu were inthe range of 0.012-0.072 wt%.    61
Figure 4-5. The EPMA elemental mapping of (a) Ti, (b) O, and (c) Cu, and (d) SEM
image of 0.045 wt% Cu2+-P25.    63
Figure 4-6. The EPMA elemental mapping of (a) Ti, (b) O, and (c) Cu, and (d) SEM image of 0.045 wt% Cu2+-ST01.    63
Figure 4-7. Nitrogen adsorption-desorption isotherms (a) and pore size distribution (b) of Degussa P25 and Cu2+-P25. The mass loadings of Cu were in the range 0.016-0.063 wt%.    65
Figure 4-8. Nitrogen adsorption-desorption isotherms (a) and pore size distribution (b) of ST01 and Cu2+-ST01. The mass loadings of Cu were in the range  0.012-0.072 wt%.    66
Figure 4-9. (a) The Cu K-edge XANES spectra of Cu, Cu2O, and CuO standards and 0.045 wt% Cu-P25 (b) The XPS spectra of 0.045 wt% Cu-P25.    69
Figure 4-10. UV-visible diffuse reﬂectance spectra of pure Degussa P25 and Cu2+-P25 at various mass loadings of 0.006–0.063 wt% Cu(a) and pure ST01 and Cu2+-ST01 at various mass loadings of 0.012–0.072 wt% Cu.    71
Figure 4-11. (a) The photodegradation of 4 mg/L SMX by various Cu loadings of Cu2+-P25 under the irradiation of 460  40 nm visible light at initial pH 5.2 and (b) the pseudo-first-order rate constant (kobs) for SMX photodegradation as a function of copper loading. The Cu loadings were in the range 0.006–0.063 wt%.    73
Figure 4-12. The pH effect on the photodegradation of SMX without the addition of buffer by Cu2+-P25 under the irradiation of 460  40 nm visible light.    75
Figure 4-13. The pH effect on the photodegradation of SMX with the addition of buffer by Cu2+-P25 under the irradiation of 460  40 nm visible light.    76
Figure 4-14. The recyclability of 1 mgL-1 SMX by 0.045 wt% Cu2+-TiO2 and Degussa P25 TiO2 under the irradiation of 460  40 nm visible light at initial pH 5.2.    78
Figure 4-15. (a) The photodegradation of 10 mg/L BPA by various Cu loadings of Cu2+-P25 under the irradiation of 460  40 nm visible light at initial pH 5.2 and (b) the pseudo-first-order rate constant (kobs) for BPA photodegradation and relative reactivity as a function of copper loading. The Cu loadings were in the range 0.006–0.063 wt%.    80
Figure 4-16. The photodegradation of 10 mg/L BPA by P25 and Cu2+-P25 under the irradiation of visible light (λ>420 nm) at initial pH 5.2.    81
Figure 4-17. The pH effect on the photodegradation of BPA with the addition of buffer by Cu2+-P25 under the irradiation of 460  40 nm visible light.    82
Figure 4-18. (a) The photodegradation of 10 mg/L BPA by various Cu loadings of Cu2+-ST01 under the irradiation of 460  40 nm visible light at initial pH 5.2 and (b) the pseudo-first-order rate constant (kobs) for BPA photodegradation and relative reactivity as a function of copper loading. The Cu loadings were in the range 0.012–0.072 wt%.    84
Figure 4-19. The TEM images of TiO2 nanorods.    88
Figure 4-20.The XRD patterns of TiO2 nanorods.    89
Figure 4-21. The TGA curves of TiO2 nanorods.    90
Figure 4-22. The photodegradation of 10 mg/L BPA by TiO2 nanorods under the irradiation of 460  40 nm visible light at initial pH 5.2.    91
Figure 4-23. (a) The photodegradation of 10 mg/L BPA by the TiO2 nanorods and Cu2+-TiO2 nanorods with different Cu(II) addition under the irradiation of 460  40 nm visible light at initial pH 5.2. (b) The pseudo-first-order rate constant (kobs) for BPA photodegradation and relative reactivity as a function of copper concentration.    94
Figure 4-24. The TEM images of CuO-TiO2 nanorods by high temperature heating at 110 °C with different copper contents (a) 1.1, (b) 2.7, (c) 8.1, and (d) 22.4 wt%.    96
Figure 4-25. The XRD patterns of CuO-TiO2 nanorods by high temperature heating at 110 °C. The mass loadings of Cu were in the range 1.1-22.4 wt%.    97
Figure 4-26. Nitrogen adsorption-desorption isotherms (a) and pore size distribution (b) of TiO2 nanorods and CuO-TiO2 nanorods. The mass loadings of Cu were in the range 1.1-22.4 wt%.    100
Figure 4-27. The XPS spectras of 8.1 wt% CuO-TiO2 nanorods by high temperature heating at 110 °C.    101
Figure 4-28. The photodegradation of 10 mg/L BPA by pure TiO2 nanorods, pure CuO and various Cu loadings of CuO-TiO2 nanorods by high temperature heating under the irradiation of 365 nm UV light at initial pH 5.2.    103
Figure 4-29. The TEM images of Cu0-TiO2 nanorod composites synthesized by using 0.8 mL TTIP as the precursor followed by reduction of various Cu loading of (a) 0.4 wt%, (b) 2.3 wt%, (c) 6.9 wt%, and (d) 20.0 wt% by NaBH4. Figures (e) and (f) are the HR-TEM image and EDS spectrum of Cu-TiO2 nanorod composites at 6.9 wt% Cu.    105
Figure 4-30. (a) XRD patterns of as-synthesized TiO2 nanorods and Cu0-TiO2 nanorods composite, (b) Cu 2p XPS spectra and (c) deconvolution of Cu 2p3/2 XPS spectra of 6.9 wt% Cu0-TiO2 nanorod composites.    107
Figure 4-31. The UV-visible diffuse reﬂectance spectra of as-synthesized TiO2 nanorods and Cu0-TiO2 nanorod composites at various mass loadings of Cu(II) ions ranging from 0.4-20 wt%    108
Figure 4-32. Nitrogen adsorption-desorption isotherms (a) and pore size distribution (b) of as-synthesized TiO2 and Cu0-TiO2 nanorods. The mass loadings of Cu were in the range 0.4-20.0 wt%.    110
Figure 4-33. (a) The photodegradation of 10 mg/L BPA by Cu0-TiO2 nanorod composites under UV light irradiation, and (b) kobs for BPA photodegradation as a function of copper loading.    112
Figure 4-34. (a) The photodegradation of 10 mg/L BPA by various TiO2-based nanomaterials under the irradiation of 365 nm UV light and (b) the comparison of kobs for BPA photodegradation in the presence of different TiO2-based materials.    115
Figure 4-35. The HPLC-MS spectra of intermediates produced from the photodegradation of bisphenol A by 6.9 wt% Cu-TiO2 nanorods.    117
Figure 4-36. (a) Photodegradation of 10 mg/L BPA by various TiO2-based nanomaterials under the irradiation of 460  40 nm visible light and (b) the kobs for BPA photodegradation by different TiO2 materials in the presence of visible light.    120
Figure 4-37. The photodegradation of 10 mg/L BPA in the presence of 1–25 mg/L humic acid by 6.9 wt% Cu0-TiO2 composites under the irradiation of 365 nm UV light.    122
Table index
Table 2-1. Physical and structural properties of anatase and rutile TiO2.    6
Table 2-2. Comparison with five main methods to synthesize TiO2 nanomaterials.    9
Table 2-3. The method to prepare the copper-based TiO2 photocatalyst and their photodegradation efficiency    26
Table 2-4. Physicochemical properties of bisphenol A    31
Table 2-5.Photocatalytic oxidation of BPA by various TiO2-based photocatalyst.    34
Table 2-6. The physical and chemical properties of SMX.    35
Table 2-7. Summary of the advanced oxidation processes (AOPs) applied in treatment of environmental matrices contaminated with SMX.    37
Table 2-8. Photocatalytic oxidation of SMX by various TiO2-based photocatalyst.    38
Table 3-1. The characteristics of physicochemical analytical instruments used in this study.    51
Table 4-1. The specific surface area (SBET) and pore size of Cu2+-P25 and Cu2+-ST01 TiO2 nanoparticles fabricated by microwave-assisted impregnation method at 120 °C.    67
Table 4-2. The pseudo-first-order rate constant (kobs) for BPA photodegradation by Cu2+-TiO2 with various Cu loadings under visible light region and the relative reactivity of Cu2+-TiO2.    87
Table 4-3. The specific surface area (SBET) and pore size of TiO2 nanorods and CuO-TiO2 nanorods fabricated by high temperature heating at 110 °C.    99
Table 4-4. The specific surface area (SBET) and pore size of TiO2 nanorods and Cu0-TiO2 nanorods fabricated by chemical reduction method.    109
Table 4-5. The proposed chemical structures of intermediates produced from the photodegradation of bisphenol A by Cu-TiO2 nanorods under the irradiation of 365 nm UV light.    118





                                

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