石墨材料固定鐵/鎳雙金屬奈米粒子增強還原脫氯

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研究生：	尚湖 Sahu, Rama Shanker
論文名稱：	石墨材料固定鐵/鎳雙金屬奈米粒子增強還原脫氯 Graphitic materials immobilized with Fe/Ni bimetallic nanoparticles for enhanced reductive dechlorination
指導教授：	董瑞安 Doong, Ruey-An
口試委員:	呂世源施养信連興隆 Shih, Yang-Hsin Lien, Hsing-Lung
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：	2018
畢業學年度：	106
語文別：	英文
論文頁數：	188
中文關鍵詞：	脫氯、鐵/鎳
外文關鍵詞：	NZVI, Dechclorination, TCE
相關次數：	點閱：2 下載：0
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地下水處理是環境科學領域之整體目標與專注方向。農業中使用過量化學藥劑、肥料及不適當的工業廢棄物處理導致許多環境污染，為現今受到關注且影響到千萬人的健康的污染物。三氯乙烯是其中一種因意外釋放到環境中並存在於地下水當中的 DNAPL (重質非水相液體)；另外，處理受污染的地下水是非常昂貴的，在過去的幾十年中，科學家們使用奈米等級的零價鐵處理水汙染並有著巨大的進展。鐵是一種天然、豐富且成本低廉的材料，這使得它比其他的奈米材料更有利。使用零價鐵降解有害的氯化烴-三氯乙烯(TCE)是最可行的技術之一。由於其特殊的材料性質和天然豐富度，研究人員對於奈米鐵處理氯化烴的應用具有濃厚的興趣。我們觀察到當添加第二種金屬作為催化劑後， TCE 降解效率有著大幅的增強。然而鐵處理系統中最常見的缺點，包括聚集、副產品的累積以及因反應時間的增長而造成的效率降低，影響了材料的性能及可續性。為了克服還原材料的聚集且穩定這些奈米粒子，我們迫切地需要找到合適的介面基質。鑒於此，本研究專注於利用奈米雙金屬粒子及其石墨碳奈米複合材料的製備。
目前的研究包括對合成奈米零價鐵、雙金屬奈米粒子、氧化石墨烯、還原氧化石墨烯、摻雜還原氧化石墨烯、石墨烯氮化碳和摻雜雙金屬奈米粒子的表面上的詳細研究；以及此奈米複合材料在環境領域相關應用。在合成新型高效雙金屬鐵/鎳奈米粒子，我們使用一種簡易的化學還原方法。其中，我們探討以石墨為基材的重要性質，包括表面積、穩定性、電導率、電子傳遞以及對水的限制能力，而這些具有影響的碳基材與雙金屬奈米粒子的特性被用於 TCE 的脫氯。

Groundwater and subsurface water treatment is the overall aim and focus of the environmental sciences. Excess use of chemicals and fertilizers in agriculture and inappropriate disposal of industrial waste are the major pollutants of concern, which affects the health of millions of people. Trichloroethylene is one of the notorious DNAPL (dense non-aqueous phase liquids) found in the ground water subsurface due to irregular and accidental release into the environment. Treatment of contaminated water in the subsurface and groundwater is tedious and expensive. Last few decades are the witnessed the use of nanoscale zero-valent iron for the treatment of toxic water and tremendous enhancement have been observed. Iron is naturally abundant and low cost, which make it more advantageous material among other nanomaterials. Application of in situ remediation of TCE (Trichloroethylene), a mostly hazardous chlorinated hydrocarbon, using zero-valent iron, is one of the most feasible technology. Due to its special physico-chemical properties and natural abundance, researchers have been interested in studying applications of nanoscale iron for the treatment of chlorinated hydrocarbons. However, enhanced TCE degradation have been observed after the addition of secondary metal as catalyst. The most common disadvantages of iron-based treatment system, include aggregation, accumulation of undesirable byproducts and a decrease in reactivity overlong time periods. To overcome the agglomeration of reductive materials and to stabilize these nanoparticles, it is urgent to find some suitable interface matrix. Keeping all this in view, the present study has been focused on fabrication of bimetallic nanoparticles with NZVI as a component and their nanocomposites with graphitic carbon.
Current research includes the detailed study to synthesis NZVI, bimetallic nanoparticles, graphene oxide, reduced graphene oxide, doped reduce graphene oxide, graphitic carbon nitride and immobilization of bimetallic nanoparticle onto the surface of respective matrixes. As synthesized nanocomposites were characterized and employed for the environmental applications. A facile chemical reduction method for the synthesis of novel and efficient bimetallic Fe/Ni nanoparticles. We have focused on important properties of graphitic matrix including surface area, stability, conductivity, electron transfer and also restricting ability toward the water. These influential properties of carbon matrix and bimetallic nanoparticles are exploited for the dechlorination of TCE.

Contents
Acknowledgement    i
Abstract    iii
摘要    iv
Abbreviations, units and symbols    v
List of figures and tables    xiv
Chapter 1    1
Introduction    1
1.1    Introduction    3
1.1.1    Environmental issues    3
1.1.2    Chlorinated hydrocarbons    3
1.2    Dechlorination technologies    7
1.3    Reductive materials for dechlorination    10
1.3.1    Zero-valent iron    11
1.3.2    Bimetallic nanoparticles    15
1.3.3    Factors influencing the reactivity of reducing metal    17
1.4    Functionalization of bimetallic nanoparticle with matrix    18
1.5    Graphitic material as the support    25
1.5.1    Activated carbon    25
1.5.2    Graphene based matrices    26
1.5.3    Carbon nitride    30
1.6    Motivation    34
1.7    Aim and Objectives    36
1.8    Experimental plan    37
Chapter 2    41
Experimental details    41
2.1.    Introduction    43
2.2.    Experimental Section    43
2.2.1.    Materials    43
2.2.2.    Sample Preparation    43
2.2.2.1. Synthesis of NZVI and bimetallic nanocomposites    43
2.2.2.2. Synthesis of graphene oxide (GO)    44
2.2.2.3. Synthesis of reduced graphene oxide (rGO)    44
2.2.2.4. Synthesis of boron doped reduced graphene oxide (B-rGO)    45
2.2.2.5. Synthesis of graphitic carbon nitride (g-C3N4)    46
2.2.2.6. Synthesis of rGO/Fe/Ni nanocomposites    46
2.2.2.7. Synthesis of B-rGO/Fe/Ni nanocomposites    47
2.2.2.8. Synthesis of Ni/Fe@g-C3N4 nanocomposite    48
2.3.    Characterization Techniques    48
2.3.1.    Scanning Electron Microscopy    48
2.3.2.    Scanning Transmission Electron Microscopy    48
2.3.3.    Transmission Electron Microscopy (TEM)    49
2.3.4.    X-ray Diffraction    49
2.3.5.    X-ray absorption near edge spectroscopy    49
2.3.6.    Raman Spectroscopy    50
2.3.7.    BET analysis    50
2.3.8.    X-ray photoelectron spectroscopy analysis (XPS)    50
2.3.9.    Electron probe microanalysis (EPMA)    51
2.3.10.    Thermogravimetric Analysis (TGA)    51
2.4.    Electrochemical Characterization    51
2.4.1.    Cyclic voltammogram (CV) and electrochemical impedance spectroscopy (EIS)    51
2.4.2.    Oxygen reduction reaction (ORR) analysis    51
2.5.    TCE dechlorination    52
2.6.    Gas Chromatography    53
2.7.    Kinetics and rate of reaction    54
2.8.    Conclusions    54
Chapter 3    55
Hydrodechlorination of trichloroethylene by reduced graphene oxide supported bimetallic Fe/Ni nanoparticles    55
3.1.    Introduction    58
3.2    Experimental procedure    59
3.2.1    Synthesis of rGO/Fe/Ni nanocomposites    59
3.3    Results and discussion    60
3.3.1    Physico-chemical properties    60
3.3.2    Electrochemical properties    66
3.3.3    TCE dechlorination    70
3.3.4    Effect of Ni loading and initial TCE concentration    76
3.3.5    Effect of dissolved organic matters    78
3.4    Conclusion    80
Chapter 4    83
Rapid dechlorination of trichloroethylene using bimetallic Fe/Ni immobilized boron doped reduced graphene oxide    83
4.1 Introduction    86
4.2    Experimental procedure    88
4.2.1    Synthesis of boron doped reduced graphene oxide    88
4.3    Results and discussion    88
4.3.1    Characterization    88
4.3.2    Dechlorination of TCE by B-rGO immobilized Fe/Ni nanoparticles    98
4.3.3    Effect of pH and initial TCE concentration on dechlorination    101
4.3.4    Stability and reusability of B-rGO/Fe/Ni    103
4.4    Conclusions    107
Chapter 5    109
Expending electron transport and masking properties of g-C3N4 in Fe/Ni nanoparticles: Dual applications for enhanced TCE dechlorination and successive ORR activity    109
5.1.    Introduction    112
5.2.    Experimental procedure    114
5.2.1.    Preparation of Fe/Ni@g-C3N4 nanocomposites    114
5.2.2.    Dechlorination analysis procedure    114
5.3.    Results and discussion    115
5.3.1.    Characterization of layered g-C3N4    115
5.3.2.    Characterization of Ni/Fe@g-C3N4 nanocomposite    118
5.3.3.    Electrochemical analysis of Ni/Fe@g-C3N4 nanocomposite    125
5.3.4.    TCE dechlorination    126
5.3.4.1. TCE degradation using various nanomaterials    126
5.3.4.2 Effect of applied voltage on TCE dechlorination    127
5.3.4.3. Effect of Ni loading on TCE dechlorination    128
5.3.4.4. Effect of dissolved organic matters on TCE dechlorination    129
5.3.4.5. TCE degradation in lake water    130
5.3.5.    Characterization Ni/Fe@g-C3N4 nanocomposite after dechlorination reaction    132
5.3.6.    ORR activity of Fe/Ni@g-C3N4 after dechlorination    134
5.3.7.    Stability test    136
5.4.    Conclusion    137
Chapter 6    139
Summary and proposed mechanism    139
Summary    140
Chapter 7    147
Conclusions    147
7.1.    Conclusions    149
7.2.    Future Scope of the Work    154
7.3. References    156
Author    185
List of publications    188

 
List of figures and tables
Figure 1. 1 Removal methods of chlorinated hydrocarbons    8
Figure 1. 2 Air sparging with soil vapor extraction process.    9
Figure 1. 3 Sequential and catalytic hydrodechlorination pathways of TCE.    10
Figure 1. 4 Schematic diagram for the synthesis of zerovalent iron using NaBH4 as reducing agent.    12
Figure 1. 5 Proposed reduction mechanism on NZVI surface under anoxic condition.    14
Figure 1. 6 Overview of pollutant treatment using nanoscales iron particles.    15
Figure 1. 7 Bimetallic NZVI immobilization onto the surface of different matrix as per literature.    23
Figure 1. 8 NZVI/HNT tubular particles that align along groundwater flow streamlines.    25
Figure 1. 9 Emergent applications and physico-chemical properties of graphene.    28
Figure 1. 10 Schematic illustration of synthesis, physico-chemical properties and emergent applications of graphitic carbon nitride.    31
Figure 1. 11 Multistep photoreduction of CO2 into CH4.    33
Figure 1. 12 Schematic representation of rGO/Fe/Ni and B-rGO/Fe/Ni nanocomposites in TCE dechlorination.    38
Figure 1. 13 Schematic representation displaying synthesis and application of Ni/Fe@g-C3N4 nanocomposites in dechlorination.    39
Figure 2. 1 Schematic illustration for the synthesis of graphene oxide according to modified hummer’s method.    45
Figure 2. 2 Schematic representing the synthesis of boron doped reduced graphene oxide    46
Figure 2. 3 Synthesis procedure for rGO/Fe/Ni and B-rGO/Fe/Ni nanocomposites    47
Figure 3. 1 Schematic illustration of rGO/Fe/Ni nanocomposite and possible reaction mechanism for TCE dechlorination.    59
Figure 3. 2 The (a) STEM image of rGO/Fe/Ni nanocomposites, (b) HRTEM image and (c) histogram of bimetallic Fe/Ni nanoparticles.    61
Figure 3. 3 (a) SEM of rGO/Fe/Ni nanocomposites with its corresponding EPMA images of (b) carbon, (c) Fe, (d) Ni distribution and (e) the energy-dispersive spectroscopic pattern.    62
Figure 3. 4 Specific surface areas of (a) GO, (b) rGO and (c) rGO/Fe/Ni nanocomposites.    63
Figure 3. 5 Thermogravimetric analysis of rGO and rGO/Fe/Ni nanocomposites.    64
Figure 3. 6 The XPS spectra of rGO/Fe/Ni nanocomposites, (a) survey, deconvoluted XPS of (b) C 1s, (c) Fe 2p and (d) Ni 2p.    65
Figure 3. 7  (a) Raman spectra of GO, rGO and rGO/Fe/Ni nanocomposite and (b) XRD pattern of GO, rGO, Fe0, rGO/Fe and rGO/Fe/Ni nanocomposite.    66
Figure 3. 8  (a) Cyclic voltammograms of rGO and rGO/Fe/Ni nanocomposites at a scan rate of 5 mV s-1 in the potential window of 0.0 – 1.0 V and (b) Nyquist plots of rGO and rGO/Fe/Ni nanocomposite.    67
Figure 3. 9  (a) LSV curve recorded for rGO/Fe/Ni nanocomposites at a san rate of 5 mV s-1 at different rotation speed and (b) K-L plot at different electrode potential window.    68
Figure 3. 10 (a) Dechlorination of TCE by using 1 g L-1 graphene based nanomaterials including rGO, as prepared NZVI, rGO/Fe, free Fe/Ni and rGO/Fe/Ni and (b) observed rate constant (kobs).    71
Figure 3. 11 The chromatographic results of TCE dechlorination (a) TCE degradation at different retention time (b) mass balance.    72
Figure 3. 12 Recyclability of rGO/Fe/Ni nanocomposites toward 20 mM TCE dechlorination and the rate of TCE.    74
Figure 3. 13  (a) TEM image, (b) histogram, the XPS spectra (c) deconvolution of Fe 2p and (d) Ni 2p of rGO/Fe/Ni nanocomposite after TCE degradation reaction.    75
Figure 3. 14  (a) Dechlorination efficiency and (b) kobs for TCE dechlorination as a function of loaded Ni amounts and (c) formation of ethane produced from the hydrodechlorination of TCE by various Ni amounts of rGO/Fe/Ni nanocomposites.    77
Figure 3. 15 (a) The initial rate of TCE dechlorination as a function of initial TCE concentration and (b) L-H kinetics.    78
Figure 3. 16  (a) Dechlorination efficiency (b) kobs for TCE dechlorination by rGO/Fe/Ni in the presence of 1 – 20 mg L-1 humic acid, (c) dechlorination efficiency in the presence of different ion concentration and (d) kobs for TCE dechlorination.    80
Figure 4. 1 Schematic illustration of synthesis of B-rGO/Fe/Ni nanocomposite for the dechlorination of TCE under anoxic conditions.    87
Figure 4. 2 The TEM images of (a) B-rGO, (b) B-rGO/Fe/Ni nanocomposites, (c) bimetallic Fe/Ni nanoparticles, (d) SEM image of B-rGO/Fe-Ni nanocomposite and (e) is the energy dispersion spectra of B-rGO/Fe/Ni nanocomposites, SEM image (inset) showing the spot of analysis.    89
Figure 4. 3 The electron probe microanalysis (EPMA) mappings of (a) carbon (C), (b) boron (B), (c) iron (Fe) and (d) nickel (Ni) elements in B-rGO/Fe/Ni nanocomposites.    91
Figure 4. 4 The Thermogravimetric analysis and DTA of (a) GO, (b) B-rGO and (c) B-rGO/Fe/Ni nanomaterials.    92
Figure 4. 5 N2 adsorption/desorption isotherms and pore size distribution curves of (a) GO, (b) B-rGO and (c) B-rGO/Fe/Ni nanocomposites.    93
Figure 4. 6 The (a) XRD patterns and (b) Raman spectra of GO-based materials and B-rGO/Fe/Ni nanocomposites.    95
Figure 4. 7 The X-ray photoelectron spectra of (a) survey scan and deconvolution of (b) B 1s, (c) C 1s, (d) Fe 2p and (e) Ni 2p in B-rGO/Fe/Ni nanocomposites.    96
Figure 4. 8 Nyquist plot of B-rGO, Fe/Ni and as-synthesized B-rGO/Fe/Ni nanocomposites in 1.0 M Na2SO4 electrolyte.    97
Figure 4. 9 FTIR spectrum of graphene oxide and B-rGO/Fe/Ni nanocomposites.    98
Figure 4. 10 (a) The dechlorination of 20 M TCE and (b) rate constants for TCE dechlorination by 1 g L-1 GO-based nanomaterials including B-rGO, free Fe/Ni and B-rGO/Fe/Ni at pH 7.    99
Figure 4. 11 Dechlorination of 20 M TCE degradation by 1.0 g L-1 GO/Fe/Ni nanocomposite.    100
Figure 4. 12 Effects of (a) pH and (b) various initial TCE concentrations (inset is the Langmuir-Hinshelwood relationship between initial rate and initial TCE concentration) on TCE dechlorination using 1 g L-1 B-rGO/Fe/Ni nanocomposite.    102
Figure 4. 13 Chromatograms of ethane production and (d) carbon mass balance during the of dechlorination of TCE by B-rGO/Fe/Ni nanocomposite under anoxic conditions. The pH and initial TCE concentrations used in the study are 4 – 9 and 10 – 80 M, respectively.    103
Figure 4. 14 The recyclability of 20 M TCE dechlorination by 1 g L-1 (a) free Fe/Ni, (b) rGO/Fe/Ni, (c) B-rGO/Fe/Ni nanocomposites at pH 7 under anoxic conditions and (d) is the kobs for TCE dechlorination by different Fe/Ni nanoparticles as a function of cycle    105
Figure 4. 15(a) XRD pattern and (b) SEM images of B-rGO/Fe/Ni nanocomposite before reaction and (c) SEM image after TCE dechlorination under anoxic conditions.    106
Figure 5. 1 (a) Schematic presentation on preparation of layered g-C3N4, (b) digital images of melamine and its products and (c) XRD pattern of exfoliated g-C3N4    116
Figure 5. 2  (a) TEM images and (b) high resolution TEM image of layered g-C3N4    117
Figure 5. 3 (a) XPS survey scan, (b) deconvoluted region of N 1S and (c) C 1S in layered g-C3N4    118
Figure 5. 4 (a) TEM [particle size distribution, histogram] (b) HRTEM image of Ni/Fe@g-C3N4 nanocomposite [Insets as particle size histogram and high magnified image].    119
Figure 5. 5 (a) SEM image and elemental mapping of (b) Fe distribution (c) Ni distribution in Ni/Fe@g-C3N4 nanocomposite and (e) normalized mass ration.    120
Figure 5. 6 XPS spectra, (a) survey scan, deconvoluted XPS of (b) C 1S (c) N 1S (d) Fe 2p and (e) Ni 2p of Ni/Fe@g-C3N4 nanocomposite.    121
Figure 5. 7 The XRD patterns of g- C3N4, Fe/Ni bimetallic nanoparticles and Ni/Fe@g-C3N4 nanocomposite    122
Figure 5. 8 N2 adsorption/desorption isotherms and porosity of (a) bulk g-C3N4 (b) layered g-C3N4 , and (c) Ni/Fe@ g-C3N4 nanocomposite    123
Figure 5. 9 Fe-L3-edge (a) XANES and (b) k3 weighted EXAFS spectra of the Fe0, Ni, Ni/Fe, and Ni/Fe@g-C3N4 nanocomposite    125
Figure 5. 10 (a) Cyclic voltammograms of Ni/Fe@g-C3N4 nanocomposite at a san rate of 5 mV s-1 in the potential window of -0.6 – 0.0 V using 1M Na2SO4 electrolyte (b) EIS of g-C3N4, Ni/Fe, and Ni/Fe@g-C3N4 nanocomposite, (inset) high resolution EIS    126
Figure 5. 11 (a) Dechlorination of TCE by using 1 g L-1 g-C3N4, bare NZVI, Ni/Fe bimetallic nanoparticles and Ni/Fe@g-C3N4 nanocomposites and (b) removal efficiency at different time span    127
Figure 5. 12  (a) Dechlorination of TCE by using Ni/Fe@g-C3N4 nanocomposites on applied voltage (0.2 – 0.6 V) and without applied voltage and (b) comparative TCE rate constant (kobs)    128
Figure 5. 13 Effect of Ni ion loading in TCE dechlorination and (b) TCE degradation rate constant    129
Figure 5. 14 (a) Effect of humic acid concentration on TCE dechlorination and (b) TCE degradation rate constant by using 1 g L-1 Fe/Ni@g-C3N4 nanocomposites, 20 mM HEPES buffer pH 7.0 with 120 rpm shaking under room temperature (27 ºC).    130
Figure 5. 15 (a) TCE degradation in lake water and simulated buffer and (b) TCE rate constant.    132
Figure 5. 16 Surface characterization after dechlorination reaction (a) TEM image (b) High resolution TEM image and (c) histogram of Ni/Fe@g- C3N4 nanocomposite    133
Figure 5. 17 Surface characterization after dechlorination reaction (a) XRD pattern, deconvoluted XPS pattern of (b) Fe 2p and (c) Ni 2p of Fe/Ni@g- C3N4 nanocomposites    134
Figure 5. 18  (a) Cyclic voltammograms of Fe/Ni@g-C3N4 nanocomposite at a san rate of 5 mV s-1 in the potential window of -0.9 – 0.0 V (b) LSV curve recorded at a san rate of 5 mV s-1 at different rotation speed (c) Koutecky-Levich plot at different electrode potent and (d) LSV curve recorded for standard Pt/C electrode.    135
Figure 5. 19  (a) LSV plot of bare Fe/Ni and g-C3N4 in comparison with Fe/Ni@g-C3N4 nanocomposites and (b) Stability test of Fe/Ni@g-C3N4 nanocomposites over 500 cycles    137
 
Table 1. 1 Physico-chemical properties of chlorinated hydrocarbons.    5
Table 1. 2. Major symptoms and sign in patient with TCE-induced hypersensitivity dermatitis (n=12).    6
Table 1. 3 Common functionalization matrices applied for metal nanoparticles and targeted pollutants.    20
Table 1. 4 The comparison of pseudo-first order rate constant (kobs) for TCE dechlorination by bimetallic Fe/Ni nanoparticles immobilized onto different supports under anoxic conditions.    21
Table 1. 5 Graphene based nanocomposites utilized for the degradation and adsorption of organic pollutants.    29
Table 1. 6 Summary of graphitic carbon nitride based nanocomposites application in the degradation of various organic compounds.    32
Table 3. 1 The comparison of pseudo-first order rate constant (kobs) for TCE dechlorination, conductivity and pH observed in the solution after the reaction by different nanocomposites in the presence of different ions.    69
Table 3. 2 The comparison of pseudo-first order rate constant (kobs) for TCE dechlorination by bimetallic Fe/Ni nanoparticles immobilized onto different supports under anoxic conditions.    72
Table 5. 1 The comparison of pseudo-first order rate constant (kobs), mass normalized rate (km), half-life, humic acid effect, and different Ni loading for TCE dechlorination.    131
Table 6. 1 Summarized characterizations, application and outcome of all Fe/Ni bimetallic nanoparticles immobilized on graphitic carbon matrices    142
Table 7. 1 The TCE dechlorination by NZVI, Fe/Ni and immobilized Fe/Ni with various graphitic carbon matrices    152



                                

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