利用水熱法製備鈦酸鹽奈米管應用於水體環境中銅離子及雙酚A共處理研究

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研究生：	蔡嘉緯 Tsai, Chia-Wei
論文名稱：	利用水熱法製備鈦酸鹽奈米管應用於水體環境中銅離子及雙酚A共處理研究 Coupled removal of bisphenol A and Copper ion by one-dimensional titanate nanotubes fabricated by hydrothermal methods
指導教授：	董瑞安 Doong, Ruey-an
口試委員:
學位類別：	碩士 Master
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：	2010
畢業學年度：	99
語文別：	英文
論文頁數：	206
中文關鍵詞：	一維鈦酸鹽奈米材料、鹼性水熱法、吸附、光催化、銅離子、雙酚A
外文關鍵詞：	One-dimensional nanostructured materials, Alkaline hydrothermal, Adsorption, Photocatalytic, Copper ion, Bisphenol A
相關次數：	點閱：3 下載：0
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內分泌干擾物和製藥保健產品為典型的新興污染物，此類物質在極低濃度長期存在人體或生物體內時，可模擬天然荷爾蒙的功能，進而抑制內分泌系統或誘導造成內分泌系統失調，造成人體及生態環境的影響。因此，由環境永續與綠色科學的精神來看，開發高效能的先進光觸媒材料，來降解環境中對人體健康及生態環境潛在威脅的化學物質是相當重要的工作。利用水熱法合成之一維鈦酸鹽奈米材料具有相當高的潛力能廣泛的應用在能源和環境材料上。在本研究利用市售二氧化鈦在水熱環境中製備一維鈦酸鹽耐米管並進行後續鍛燒處理以強化光催化能力，以瞭解共處理重金屬(銅)及內分泌干擾物質(雙酚A)的可能性，同時瞭解環境參數包括pH、溫度、離子強度及濃度對處理效能的影響。使用商售之ST-01 (ISK) 二氧化鈦粉末做為初始材料，加入10 M氫氧化鈉水溶液中，在壓力釜系統下，調控水熱溫度在攝氏150度加熱24小時，即可成功製備具有管狀結構之一維鈦酸鹽奈米材料 (TNT)。掃描式及穿透式電子顯微鏡分析結果顯示，一維鈦酸鹽奈米材料的直徑介於7-10 nm，長度則在數百nm間，經在空氣下鍛燒4小時後，TNT在400□C會開始轉換成銳鈦礦TiO2，表面積則由最初的420 m2/g下降到鍛燒200-600□C後的43-396 m2/g。TNT對銅離子有相當好的吸附能力。研究結果顯示，鈦酸鹽奈米管材料吸附銅離子之最大飽和吸附量為160 ± 11 mg/g，而不同鍛燒溫度的TNT材料對重金屬能有不錯的吸附能力，但隨著鍛燒的溫度增高，其最大飽和吸附量也隨之降低至35-129 mg/g。另外，熱力學之結果顯示利用鈦酸鹽奈米管材料吸附銅離子為放熱反應，其最大飽和吸附量隨pH降低、離子強度增加及反應溫度增加時，而隨之減少。當水體環境中同時存在銅與雙酚A時，利用鍛燒溫度為500oC鍛燒處理之TNT(TNT_500)，在365 nm紫外光照環境下光催化雙酚A，反應速率高達0.33 min-1，高於商用P25二氧化鈦粉末6.7倍。而不同pH(2.9-8.5)對於TNT_500光催化雙酚A之反應速率，隨著pH增加而增加，其反應速率介於0.4±0.1×10-2到0.47±0.02 min-1。本研究結果顯示，利用鹼性水熱法所配製的鈦酸鹽奈米材料結構，可藉由鍛燒處理，產生二氧化鈦顆粒，但仍保有管狀結構與高比表面積，適合作為光催化材料，並可進行環境中混合污染物的共處理。

Endocrine disrupting chemicals (EDCs) and heavy metals are typical emerging pollutants. EDCs can cause the disorder of endocrine systems in biological bodies, which metal ions are poison chemicals to human health. From the environmental sustainability and green chemistry points of view, the development of a high efficient advanced photocatalyst that can remove emerging pollutants and metal ion in the environment is of great important. One-dimensional titanate nanobutes (TNTs) are promising materials for energy and environmental applications. However, the simultaneous removal of bisphenol A and copper ion by TNT are raely reported. In this study, the TNTs were originally obtained from ST-01 TiO2 at hydrothermal temperature of 150 oC for 1 d and then post heat-treatment at 200–600 °C in air for 4 h. The TNTs materials were characterized using SEM, TEM, BET surface area, XRD, UV-Vis, and XAS analyzer. The adsorption of copper ion onto as-synthesized and calcined TNTs was studied. The effects of copper ion concentration, pH value, ionic strength and temperature on adsorption of copper ion by TNTs were also evaluated. Results showed that the fabricated TNTs is a multi-layered tubular structures with diameters of 7-10 nm. The specific surface area of TNTs decreased with the increase in calcination temperature, presumably due to the collapse of tubular structures and formation of anatase TiO2 nanoparticles. The as-synthesized and calcined TNTs have good capacity for Cu(II) adsorption. The calculated maximum Langmurian adsorption capabilities (qm) were 160 ± 11 mg/g for as-synthesized TNTs, 129 ± 6 mg/g for TNT_200, 117 ± 6 mg/g for TNT_300, 105 ± 4 mg/g for TNT_400, 54 mg/g for TNT_500 and 35 mg/g for TNT_600. The adsorption kinetics was evaluated by the pseudo-first-order, pseudo-second-order and intraparticle diffusion model. The pseudo-second-order model fitted the experimental results quite well, and intraparticle diffusion was found to be not the rate limiting step. In addition, the negative value of enthalpy (ΔH) (−57.6 kJ mol−1) indicates the exothermic nature of the adsorption process, and the adsorbed amounts of copper ions onto the as-synthesized TNTs decreased with the increasing reaction temperature as well as the ionic strength. In addition, the photocatalytic activities of the catalyst obtained were evaluated by the degradation of bisphenol A in aqueous solution under UV light irradiation. The effect of environmental parameters including such concentration of bisphenol A and copper, and the pH were investigated by measurement of the rate constant for BPA degradation. Consequently, kinetic parameters were experimentally determined and a pseudo-first-order kinetic was observed. In this study, the photodegradation process of 10 mg/L BPA in the presence of copper ions by TNT_500 had higher rate constant than that in the absence of copper, which is 6.7 times higher than by Degussa P25 TiO2.

Content Index
中文摘要    I
Abstract    III
Content Index    V
Table Index    VIII
Figure Index    XII
Chapter 1 Introduction    1
1-1 Motivation    1
1-2 Objectives    2
Chapter 2 Background and Theory    4
2-1 Toxicity and removal of copper ions    4
2-2 Bisphenol A    8
2-3 Fabrication of 1-D titanate nanomaterials    16
2-3-1 Chemical (Template-directed) synthesis    18
2-3-2 Electrochemical synthesis (Anodization of Ti)    19
2-3-3 Alkaline hydrothermal method    19
2-4 Parameters influencing the morphology of titanate nanotubes    21
2-4-1 Effect of hydrothermal temperature and reaction time    24
2-4-2 Effect of alkaline concentration    25
2-4-3 Effect of starting materials    26
2-4-4 Effects of post treatment    31
2-5 Mechanism of 1-D titanate nanotube formation    32
2-6 Titanate nanotubes as catalysts in environmental applications    32


Chapter 3 Materials and methods    32
3-1 Regents and materials    32
3-2 Experimental design    32
3-3 Fabrication of 1-D TNTs materials by hydrothermal method    32
3-4 Evaluation of adsorption isothermal by titanate nanotubes    32
3-5 Evaluation of photocatalytic activity of bisphenol A by titanate nanotube    32
3-6 Characterization    32
3-6-1 Scanning electron microscopy (SEM)    32
3-6-2 Transmission electron microscopy (TEM)    32
3-6-3 Specific surface area    32
3-6-4 X-ray powder diffraction (XRPD)    32
3-6-5 Ultraviolet-Visible (UV-Vis) spectroscopy and band gap    32
3-6-6 X-ray absorption spectroscopy (XAS)    32
3-6-7 Zeta potential (ξ) measurement.    32
3-6-8 Electron paramagnetic resonance (EPR)    32
Chapter 4 Results and discussion    32
4-1 Optimization of hydrothermal conditions    32
4-2 Characterization of titanate naotube    32
4-2-1 Morphological properties    32
4-2-2 Microtsructures of as-synthesizd TNTs    32
4-2-3 Post heat-treatment TNT (calcined TNTs)    32
4-3 Adsorption of metal ions using titanate nanotube    32
4-3-1 Effect of contact time for adsorption    32
4-3-2 Effect of calcination temperatures on adsorption    32
4-3-3 Effect of pH value on adsorption of Cu(II)    32
4-3-4 Effect of ionic strength on Cu(II) adsorption    32
4-3-5 Adsorption thermodynamics    32
4-3-6 Adsorption kinetics    32
4-3-7 Desorption and reusability    32
4-4 Photocatalysis of Bisphenol A using titanate nanotube    32
4-4-1 Photocatalytic activity of titanate nanotubes (TNTs)    32
4-4-2 Couple removal of Cu and bisphenol A with various catalysts    32
4-4-3 Effect of pH value    32
4-4-4 Effect of copper concentration on photocatalytic activity of TNTs    32
4-4-5 Effect of BPA concentration on photocatalytic activity of TNTs    32
4-4-6 Analysis of TOC and reusability    32
4-4-7 Reusability of TNTs for photodegradation    32
4-4-8 Quantum efficiency results    32
4-4-9 Electron paramagnetic resonance (EPR) results    32
Chapter 5 Conclusions    32
References    32
Appendix    32



Table Index
Table 2-1. The adsorption capacities of various adsorbents towards Cu(II) adsorption under various environmental conditions.    6
Table 2-2. The physical and chemical properties of bisphenol A.    9
Table 2-3. The reaction mechanisms, advantages and disadvantages of various methods for removal of EDCs and PPCPs.    11
Table 2-4. The operational conditions and efficiency of different methods used for removal of bisphenol A in aqueous solutions.    12
Table 2-5. Photocatalytic oxidation of bisphenol A by various semiconductor photocatalyst.    15
Table 2-6. Comparisons with three main methods to prepare 1-D TiO2-derived nanomaterials.    17
Table 2-7. Effects of preparation parameters on the morphology of 1-D nanostructured titanate materials fabricated by hydrothermal method.    22
Table 2-8. Hydrothermal conditions and characteristics of products in previous studies.    27
Table 2-9. The potential applications of 1-D titanate nanomaterials by hydrothermal method.    32
Table 2-10. The photocatalysis in 1-D titanate nanomaterials by hydrothermal method.    32
Table 3-1. The characteristics of physicochemical analytical instruments used in this study.    32
Table 4-1-1. Specific surface area and pore size of TiO2-derived nanomaterials at various hydrothermal temperatures for 1d in the presence of 10 M NaOH solution.    32
Table 4-2-1. BET specific surface area and pore size of the ST-01 TiO2 and as-synthesized TNT.    32
Table 4-2-2. The BET specific surface area and pore size of 1-D TNT calcined at various temperatures ranging from 200 to 600 oC.    32
Table 4-2-3. The EDS of the as-synthesized and calcined TNTs at 200-600 □C.    32
Table 4-2-4. The bandgaps of as-synthesized and calcined TNTs at 200-600 □C derived from the UV-Vis spectroscopy.    32
Table 4-2-5. Quantity of TNTs surface functional groups with as-synthesized TNTs and TNT_500.    32
Table 4-2-6. The isoelectric points of as-synthesized and calcined TNTs at 200-600 oC.    32
Table 4-3-1. The removal efficiencies of different concentration of Cu(II) onto as-synthesized and calcined TNTs at 200-600 oC.    32
Table 4-3-2. Langmuir parameters for the adsorption of copper ions by difference TNTs materials at pH 5.0±0.1 and at 25 °C.    32
Table 4-3-3. Adsorption capacity of copper ions by various adsorbents.    32
Table 4-3-4. Freundlich parameters for the adsorption of copper ions onto difference TNTs materials at pH 5.0±0.1 and at 25 °C.    32
Table 4-3-5. The removal efficiency of copper ion onto as-synthesized TNTs at various pH values.    32
Table 4-3-6. Langmuir and Freundlich parameters for the adsorption of copper ions at various pH ranging from 2.8 to 6.2.    32
Table 4-3-7. The removal efficiency of copper ion onto as-synthesized TNTs at various ionic strength ranging from 0.01 to 0.1 M.    32


Table 4-3-8. Langmuir and Freundlich isotherm parameters for adsorption of copper ions onto 1-D as-synthesized TNTs at various ionic strengths ranging from 0.01 M to 0.1 M.    32
Table 4-3-9. The removal efficiency of copper ion onto as-synthesized TNTs at various temperatures ranging from 15 to 60 oC.    32
Table 4-3-10. Langmuir isotherm constants and correlation coefficients for the adsorption of copper ions at various temperatures ranging from 15 to 60 oC.    32
Table 4-3-11. Thermodynamic parameters for the adsorption of copper ions by as-synthesized TNTs at pH 5.0±0.1.    32
Table 4-3-12. The kinetic parameters for copper ions adsorption at various initial copper ions concentrations.    32
Table 4-3-13. The kinetic parameters for copper ions adsorption at various reaction temperature.    32
Table 4-3-14. The desorption efficiency of adsorbed Cu(II) onto as-synthesized TNTs as HCl and HNO3 was used.    32
Table 4-4-1. The specific surface area and pseudo-first-order rate constants for BPA photodegradation with different catalysts.    32
Table 4-4-2. The kobs for BPA photodegradation by different photocatalysts in the presence of absence of 1 mg/L Cu(II) under illumination of UV light at 365 nm at pH 6.5.    32
Table 4-4-3. The pseudo-first order rate constants (kobs) for BPA degradation and adsorption efficiency of Cu(II) at various pH in the presence of 20 mg/L Cu(II) under illumination of UV light at 365 nm.    32


Table 4-4-4. The pseudo-first-order rate constants (kobs) for BPA and adsorption efficiency of Cu(II) at various copper concentrations ranging from 1 to 50 mg/L under illumination of UV light at 365 nm.    32
Table 4-4-5. Parameters for Langmuir-Hsinshelwood kinetics of photodegradation of BPA by TNT_500 in the presence of 365 nm UV light.    32
Table 4-4-6. Rate constants (k, min-1), rate (r, μM min-1) and quantum efficiency (Φe), and Φ365 (μM /einstein) of BPA containing P25, TNT_500 and TNT_500 with 20mg/L Cu.    32


Figure Index
Figure 2-1. Chemical structure of bisphenol A.    9
Figure 2-2. Simplified milestones of the development and application of 1-D TiO2-derived nanostructured materials (Bavykin et al., 2009).    18
Figure 2-3. Five different morphologies synthesized by alkaline hydrothermal methods from TiO2. (a) Sheets, (b) spheroids, (c) rectangular-section fibers, (d) multiple-wall nanotubes, and (e) circular-section rods (Bavykin and Walsh, 2009).    20
Figure 2-4. Schematic illustration of the change in morphology of titanate nanotubes obtained from Degussa P-25 and ST-01 in 5 and 10 M NaOH at various hydrothermal temperatures ranging from 60 to 230 °C for 3 days.    25
Figure 2-5. Schematic representation of the thermal transformations pathways as a function of sodium content in titanate nanostructures (Morgado et al., 2006).    32
Figure 2-6. Schemes of three possible mechanisms for multi-walled titanate nanotubes (Bavykin et al., 2004).    32
Figure 2-7. Formation mechanism of the TiO2-derived nanotubes (Wang et al., 2002).    32
Figure 2-8. Schematic of the formation process of titanate nanosheets, nanotubes, and nanowires (Huang et al., 2009).    32
Figure 3-1. Flowchart of the fabrication 1-D titanate nanomaterials and its application.    32
Figure 3-2. Schematic diagram of the fabrication 1-D titanate nanotube.    32
Figure 3-3. Procedure of adsorption experiments by synthesized TNT.    32
Figure 3-4. Flowchart of the photocatalytic experiments by synthesized TNT.    32
Figure 4-1-1. SEM images of the morphology of 1-D titanate nanostructures fabricated from P25 TiO2 in 10 M NaOH(aq) solution at various hydrothermal temperatures for 1d. (a) 120 °C; (b) 150 °C; (c) 180 °C, and (d) 200 °C.    32
Figure 4-1-2. SEM images of the morphology of 1-D titanate nanostructures fabricated from ST-01 TiO2 in 10 M NaOH(aq) solution at various hydrothermal temperatures for 1d. (a) 120 °C; (b) 150 °C; (c), 180 °C and (d) 200 °C.    32
Figure 4-1-3. TEM images of titanate nanomaterials prepared by P25 TiO2 at (a)150 oC and (b) 200 oC, and by ST-01 TiO2 at (c)150 oC and (d) 200 oC for 1d in the 10 M NaOH solution.    32
Figure 4-1-4. Nitrogen adsorption-desorption isotherm at 77 K for titanate nano- materials from (a) P25 and (b) ST-01 at different hydrothermal temperatures of 120-200 □C for 1d in the presence of 10 M NaOH. The adsorption isotherms for the P25_120, P25_150, and P25_180 are vertically shifted 100, 400, 350 cm3 STP g-1, respectively, for clarity. The ST-01_120, ST-01_150, and ST-01_180 are vertically shifted 350, 150, 50 cm3 STP g-1, respectively, for clarity.    32
Figure 4-1-5. BJH pore size distribution for titanate nanomaterials from (a) P25 and (b)ST-01 prepared at different hydrothermal temperatures of 120-200 □C for 1d in the presence of 10 M NaOH.    32
Figure 4-2-1. SEM images of (a) ST-01 TiO2 and (b) as-synthesized TNTs obtained from ST-01 in 10 M NaOH solutions at hydrothermal temperature of 150°C for 24 h.    32
Figure 4-2-2. EDS of as-synthesized TNTs were obtained from ST-01 in 10 M NaOH solution at hydrothermal temperature of 150°C for 24 h.    32
Figure 4-2-3. (a) TEM images and (b) HRTEM images of as-synthesized TNTs were obtained from ST-01 in 10 M NaOH solutions at hydrothermal temperature of 150°C for 24 h.    32
Figure 4-2-4. Nitrogen adsorption–desorption isotherms of the ST-01 TiO2 and as-synthesized TNTs prepared in 10 M NaOH solution at hydrothermal temperature of 150°C for 24 h. Inseted is the BJH pore size distribution.    32
Figure 4-2-5. The XRD patterns of ST-01 TiO2 and as-synthesized TNT obtained from ST-01 in 10 M NaOH solutions at hydrothermal temperature of 150°C for 24 h.    32
Figure 4-2-6. The UV-Vis spectra of the ST-01 TiO2 and as-synthesized TNTs obtained from ST-01 in 10 M NaOH solutions at hydrothermal temperature of 150°C for 24 h.    32
Figure 4-2-7. SEM images of post heat treatment TNTs calcined at 200-600 □C. (a) TNT_200, (b) TNT_300, (c) TNT_400, (d) TNT_500, and (e) TNT_600.    32
Figure 4-2-8. TEM images of post heat treatment TNTs calcined at 200-600 □C. (a) TNT_200, (b) TNT_300, (c) TNT_400, (d) TNT_500, and (e) TNT_600.    32
Figure 4-2-9. HRTEM images of post heat treatment TNTs. (a) TNT_400, (b) TNT_500, (c) TNT_600.    32
Figure 4-2-10. Nitrogen adsorption–desorption isotherms of TNTs after calcination at various temperature..    32
Figure 4-2-11. The BJH pore size distribution of post heat treatment TNTs. The pore distribution for TNT_200, TNT_300, TNT_400, TNT_500, and TNT_600 are vertically shifted 0.1, 0.2, 0.3, 0.4, and 0.5 cm3 min g-1, respectively, for clarity.    32
Figure 4-2-12. Textural parameters of specific surface area and pore size of post heat treatment TNTs ranging from 200 to 600 □C.    32
Figure 4-2-13. The XRD patterns of the as-synthesized and calcined TNTs at various temperatures ranging from 200 to 600 □C..    32
Figure 4-2-14.  The UV-Vis spectra of the as-synthesized and post heat-treated TNTs. The TNTs were fabricated at 150 oC for 24 h in the presence of 10 M NaOH. The calcination temperatures were in the range 200-600 oC    32
Figure 4-2-15 The FTIR spectra of the as-synthesized and post heat-treated TNTs. The TNTs were fabricated at 150 oC for 24 h in the presence of 10 M NaOH. The calcination temperatures were in the range 200-600 oC    32
Figure 4-2-16. Ti K-edge XANES spectra of as-synthesized TNTs and TNT_500.    32
Figure 4-2-17. Pre-edge spectra of Ti K-edge XANES for as-synthesized TNTs and TNT_500.    32
Figure 4-2-18. Zeta potential of the as-synthesized and calcined TNTs at various pH values.    32
Figure 4-2-19. The isoelectric points (IEPs) of TNTs nanomaterials as a function of calcination temperatures ranging from 200 to 600 oC.    32
Figure 4-3-1. The adsorption of metal ions for as-synthesized TNTs as a function of time. The initial Cu(II) concentrations were in the range 50 mg/L, and the pH value and temperature were controlled at 5.0 and 25oC, respectively.    32
Figure 4-3-2. Adsorption isotherms of Cu(II) by different 1-D TNTs at 25 oC. The TNTs used included as-synthesized TNTs, TNT_200, TNT_300, TNT_400, TNT_500 and TNT_600. The pH value was controlled at 5.0±0.1 in 10 mM acetic acid buffer solution.    32
Figure 4-3-3. Concentration diagram of copper species in aqueous solution. Copper concentration: 10−4 M (Wang and Qin, 2005)    32
Figure 4-3-4. Effect of pH on adsorption of copper ions onto as-synthesized TNTs at 25 oC. The pHs were in the range 2.8-6.2.    32
Figure 4-3-5. Effect of ionic strength on adsorption of copper ions onto as-synthesized TNTs at 25 °C. The pH value was controlled at 5.0±0.1 and the ionic strengths were in the range 0.01 to 0.1 M using NaClO4 as the electrolyte.    32
Figure 4-3-6. The qm and KF values of the Langmuir and Freundlich at various ionic strengths ranging from 0.01 to 0.1 M. The pH value and temperature were controlled at 5.0±0.1 and 25 °C.    32
Figure 4-3-7. Adsorption isotherms of Cu(II) onto as-synthesized TNTs at various temperatures and at pH 5.0±0.1.    32
Figure 4-3-8. Plot of the Langmuir isotherm constant (ln b) vs. temperature (1/T).    32
Figure 4-3-9. The adsorption of metal ions for as-synthesized TNTs as a function of time. The initial Cu(II) concentrations were in the range 50-200 mg/L, and the pH value and temperature were controlled at 5.0 and 25 oC, respectively.    32
Figure 4-3-10. The adsorption of metal ions for as-synthesized TNTs as a function of time.  The reaction temperature were in the range 15-60 oC, and the pH value and initial Cu(II) concentrations were controlled at 5.0 and 50 mg/L, respectively.    32
Figure 4-3-11. Linear plot by pseudo-first-order model for adsorption of copper ions concentrations onto as-synthesized TNTs at different concentrations from 50 to 200 mg/L. (pH = 5.0±0.1 and T =25 oC)    32
Figure 4-3-12. Linear plot of pseudo-second-order model for adsorption of copper ions concentrations onto as-synthesized TNTs at different concentrations from 50 to 200 mg/L. (pH = 5.0±0.1 and T =25 oC)    32
Figure 4-3-13. Linear plot of intraparticle diffusion model for adsorption of copper ions concentrations onto as-synthesized TNTs at different concentrations from 50 to 200 mg/L. (pH = 5.0±0.1 and T =25oC)    32
Figure 4-3-14. Linear plot by pseudo-first-order model for adsorption of copper ions concentrations onto as-synthesized TNTs at various temperatures of 15-60 oC. (pH = 5.0±0.1 and initial concentration of Cu(II) = 100 mg/L)    32
Figure 4-3-15. Linear plot of pseudo-second-order model for adsorption of copper ions concentrations onto as-synthesized TNTs at various temperatures of 15-60 oC. (pH = 5.0±0.1 and initial concentration of Cu(II) = 100 mg/L)    32
Figure 4-3-16. Linear plot of intraparticle diffusion model for adsorption of copper ions concentrations onto as-synthesized TNTs at various temperatures of 15-60 oC. (pH = 5.0±0.1 and initial concentration of Cu(II) = 100 mg/L)    32
Figure 4-3-17. The desorption efficiency of adsorbed Cu(II) onto as-synthesized TNTs. (T=25 oC, pH=5.0±0.1 in 10 mM acetic acid buffer solution)    32
Figure 4-3-18. The performance of as-synthesized TNTs by multiple cycles of regeneration by 1 M HCl. (T=25oC, pH=5.0±0.1 in 10 mM acetic acid buffer solution)    32
Figure 4-3-19. The performance of as-synthesized TNTs by multiple cycles of regeneration by 1 M HNO3 (T=25oC, pH=5.0±0.1 in 10 mM acetic acid buffer solution).    32
Figure 4-4-1. The photodegradation of 10 mg/L BPA by the as-synthesized TNTs and commercial TiO2 (P25 and ST-01) in the presence of O2 under the UV irradiation of 365 nm (pH=6.5 and T=25oC).    32

Figure 4-4-2. Photocatalytic degradation of 10 mg/L BPA by TNTs calcined at various calcination temperatures in the presence of O2 under UV irradiation of 365 nm (pH=6.5 and T=25oC).    32
Figure 4-4-3. The linear relationship between the change in BPA concentration with time. The kobs for BPA photodegradation can be obtained from the slope of each line.    32
Figure 4-4-4. Coupled photodegradation of 10 mg/L BPA by different photocatalysts in the presence of 1 mg/L Cu(II) and O2 at pH 6.5 under UV irradiation conditions.  The photocatalysts used in this study were for P25, ST-01 and TNT_500.    32
Figure 4-4-5. Linear relationship between the change in BPA concentration and irradiation time.    32
Figure 4-4-6. Effect of pH on the photodegradation of 10 mg/L BPA in the presence of 20 mg/L Cu (II) at 25oC under the illumination of UV light at 365 nm.    32
Figure 4-4-7. The linear relationship of photodegradation of 10 mg/L BPA by TNT_500 in the presence of 20 mg/L Cu (II) at 25oC under illumination of UV light at 365 nm.    32
Figure 4-4-8. The pseudo-first-order rate constant (kobs) for BPA photodegradation as a function of pH at 25oC in the presence of 20 mg/L Cu(II).    32
Figure 4-4-9. The Cu(II) species as a function of pH in the presence of 10 mg/L BPA simulated using MINTEQ program. The initial concentration of Cu(II) was 20 mg/L.    32
Figure 4-4-10. The species distribution of Bisphenol A as a function of pH ranging from 4 to 12. The distribution was calculated based on pKa1 9.6 and pKa2 10.2 of BPA (Kosky et al., 1991).    32
Figure 4-4-11. The effect of Cu concentration on photodegradation of BPA by TNT_500 under the 365 nm UV irradiation conditions. The initial concentration of BPA was 10 mg/L at pH 7 and 25oC)    32
Figure 4-4-12. The kobs for BPA photodegradation by calcined TNTs as a function of Cu(II) concentration at pH 7 and at 25□C. The initial BPA concentration and wavelength of UV llight were 10 mg/L and 365 nm, respectively.    32
Figure 4-4-13. The initial rate for BPA photodegradation as a function of initial BPA concentration at pH 7 under UV-illumination conditions. Inset is the plot of the 1/r versus 1/C by L-H mode for photodegradation of BPA with 20 mg/L Cu by TNT_500.    32
Figure 4-4-14. The photomineralization of 10 mg/L BPA by various photocatalysts irradiated with 365 nm UV light. The photocatalytic system used were Degussa P25 TiO2 in the absence of Cu(II) and TNT_500 in the presence of 20 mg/L Cu(II).    32
Figure 4-4-15. The longevity of photocatalytic degradation of 10 mg/L BPA by Degussa P25 TiO2 and TNT_500 irradiated with 365 nm UV light at pH 6.5 and at 25 ºC.    32
Figure 4-4-16. Concentration of 2-NBA as a function of time under UV irradiated at 365 nm at pH 6.5 and 25oC.    32
Figure 4-4-17. Photodegradation of BPA by P25 TiO2 and TNT_500 catalysts in the presence and absence of Cu(II) ions under UV irradiated at 365 nm. The pH and temperature used in this study were at pH 6.5 and 25oC.    32
Figure 4-4-18. The EPR signals of DMPO-HO• adduct in the presence of DMPO solution under illumination of 250 W mercury lamps. The concentration of DMPO was 4.4×10-3 M.    32

Figure 4-4-19. The EPR spectra of radicals trapped by DMPO irradiated with 250 W UV lamp for 5 min. (a) P25 TiO2 and TNT_500 in DI water, (b) P25 TiO2 and TNT_500 in the presence of bisphenol A. DMPO concentration was 4.4×10-3 M.    32
Figure 4-4-20. EPR spectra of radicals obtained from the irradiation of TNT_500 by 250 W UV lamp fro 5 min after the addition of various concentrations of Cu(II) ranging from 5-40 mg/L to BPA solutions in the presence of DMPO.    32

                                

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