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研究生：	馬漢德 Mahasti, Nicolaus Nezha Nunez
論文名稱：	以流體化床結晶法自廢水中回收金屬氧化物做為光芬頓程序之異相催化劑 Recycling of metal oxides from synthetic wastewater by fluidized-bed crystallization exemplified as a catalyst for UVA-assisted Fenton technology
指導教授：	黃耀輝 Huang, Yao-Hui
學位類別：	博士 Doctor
系所名稱：	工學院 - 化學工程學系 Department of Chemical Engineering
論文出版年：	2020
畢業學年度：	108
語文別：	英文
論文頁數：	117
外文關鍵詞：	fluidized-bed, homogeneous crystallization, iron oxyhydroxide, crystallization ratio, hydraulic condition
相關次數：	點閱：112 下載：8
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This work applied fluidized-bed crystallization (FBC) and fluidized-bed homogeneous crystallization (FBHC) to recover iron-contaminating from wastewater as iron oxide particles, such as FeOOH, Fe3O4, and FeCu@SiO2. The crystal of FeOOH was recovered from synthetic wastewater at the optimum value of pH 6.5 – 7.5, surface loading (L) of 0.6 kg/m2/h for an input ferrous concentration ([Fe2+]in) of 100-300 mg/L, resulting in the total iron removal (TR) of more than 99% and crystallization ratio (CR) of 85%. The X-ray diffractometry (XRD) analysis showed that the pellet product was a mixture of iron oxyhydroxide polymorph, including goethite (α-FeOOH), and lepidocrocite (γ-FeOOH). The magnetite (Fe3O4) was obtained under the conditions of pH = 8.5-9.5 and (Fe2+)in = 100 – 500 mg/l, the TR and CR values were 99% and 77%, respectively. The highly pure Fe3O4 pellets (average size: 0.5 – 0.7 mm) obtained from FBHC had high magnetization and low coercivity values of 79.45 emu/g and 5.6 Oe, respectively, indicating the property of superparamagnetism of recovered magnetite. A Fenton-like reaction of RB5 azo dye was catalyzed with the Fe3O4 pellets under conditions of UVA irradiation, pH = 2.75 – 3.0, initial peroxide concentration of 10 mM (340 mg/L), and catalyst loading of 2 g/l. The efficiencies of decolorization and mineralization reached about 99% and 68%, respectively. Iron and copper were also removed from synthetic wastewater as binary oxide compound coated on the surface of the silica seed. Under the optimum pH of 7.5 – 8.5, about 90% and >99% of iron and copper could be removed for CR and TR respectively.

CONTENTS
Abstract	II
Acknowledgement	III
Contents	IV
List of Tables	IX
List of Figures	X
I.   Introduction	1
1 Background	1
2 Research Objective	4
II  Literature Review	6
1 Iron Oxidation	8
2 Solubility Curve	10
3 Supersaturation condition	17
4 Fluidized-bed crystallization	18
5 Fluidization Velocity	21
6 Heterogeneous Fenton-Like Process	22
III  Materials and Methods	24
1 Framework of the research	24
2 Materials	25
3 Experiment Procedure	26
3.1 Jar Test Experiments	26
3.2 Synthesis of Iron Oxide crystals	27
3.3 Iron Removal Experiments	29
3.4 The synthesis of FeCu@SiO2	29
3.5 Magnetite product application in mineralization of organic pollutant	30
4 Analytical Methods	32
IV  Results and Discussions	35
1 Chemical Precipitation of FeOOH	35
2	FeOOH Synthesis by FBHC	39
3 Iron recovery as FeOOH by FBHC process	40
3.1 Iron Removal vs Time	42
3.2 Iron Removal vs pH	43
3.3 Dissolved Oxygen Consumption	44
3.4 Carbonate Consumption	46
3.5 Iron Removal vs Surface Loading	48
3.6 The Effect of supersaturation condition	50
4 FBHC Product Analysis for FeOOH	52
4.1 XRD Analysis	52
4.2 SEM Analysis	53
4.3 BET Analysis	54
5 Synthesis of Magnetite (Fe3O4) by FBHC	55
6 Iron recovery as Fe3O4 by FBHC process	56
6.1 Iron recovery as Fe3O4	57
6.2 Iron Removal vs pH	58
6.3 Dissolved Oxygen Consumption	59
6.4 Inorganic Carbon Residual	60
6.5 Ferrous ion consumption	61
6.6 Effect of cross-sectional loading	62
6.7 The Effect of supersaturation condition	63
7 Characterization of Magnetite Product	66
7.1 XRD Analysis	66
7.2 FTIR Analysis	67
7.3 SEM Analysis	68
7.4 SQUID-VSM	69
7.5 BET Surface Area Analysis	70
8 Recovery of iron and copper as of FeCu@SiO2 by FBC	70
9 FeCu@SiO2 Particle Characterization	71
9.1 Optical Camera	71
9.2 XPS	72
9.3 SEM	74
9.4 BET	75
10 Removal of iron and copper by FBC process	75
10.1 Effect of Initial [Fe2+] / [Cu2+] Ratio	75
10.2 Effect of Equilibrium pH on The Iron and Copper Removal Efficiency	76
10.3 The Iron – Copper Ratio Deposited onto the SiO2 Surface	78
10.4 Effect of pH on The Deposition Rate of Iron and Copper on SiO2 Surface	81
10.5 Effect of Organic Contaminant on The Removal Efficiency of Iron and Copper	82
11 Exemplification of Fe3O4 from FBHC Product in UVA-Assisted Three-Phases Fenton – Like Technology	85
11.1 The Decolorization and Degradation of RB5 by Three-Phase Fluidized Photo-Assisted Fenton-Like Process	86
11.2 The Type of ROS (Reactive Oxygen Spesies) In The Fenton – Like Reaction Catalyzed by Fe3O4	89
11.3 Kinetic Study	92
11.4 Effect of Light Irradiation	95
11.5 The Recyclability of Fe3O4 Catalyst	97
11.6 The Treatment of Real Wastewater by Three-Phase Fluidized Photo-Assisted Fenton-Like Process	98
V   Conclusions and Recommendations	101
1	Conclusions	101
2	Recommendation	103
References  104


                                    

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