利用廢面板玻璃製備奈米孔洞材料應用於水中重金屬去除及硼回收之研究

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研究生：	蔡正國 Tsai, Cheng-Kuo
論文名稱：	利用廢面板玻璃製備奈米孔洞材料應用於水中重金屬去除及硼回收之研究 Sustainable valorization of mesoporous material from display panel waste glass for removal of heavy metals and recovery of boron
指導教授：	董瑞安 Doong, Ruey-an
口試委員:	黃志彬 Huang, Chih-Pin 劉志成 Liu, Jhy-Chern 吳劍侯 Wu, Chien-Hou 洪肇嘉 Horng, Jao-Jia 黃耀輝 Huang, Yao-Hui
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：	2019
畢業學年度：	108
語文別：	英文
論文頁數：	158
中文關鍵詞：	廢面板玻璃、、田口實驗設計、流體化結晶床、吸附劑、中孔性奈米材料
外文關鍵詞：	TFT-LCD panel waste, Taguchi experimental design, Chemical –oxo precipitation fluidized bed crystallization (COP-FBC), Adsorbents, Mesoporous material
相關次數：	點閱：3 下載：0
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隨著地球資源不斷消耗面臨短缺之問題，為達永續環境之目的，藉循環經濟的理念，進行廢棄物的有效資源再利用，以製成各式產品為一重要課題。國內為液晶顯示器(TFT-LCD)主要生產國，佔全球生產量30%以上，TFT-LCD 廣泛應用於電子產品如手機、電視、平板電腦、車用顯示器等，然而這些電子產品仍有壽命之廢棄與製程過程中產生廢料之問題，未來將會有大量廢棄TFT-LCD面板玻璃待處理。TFT-LCD面板主要成分為含有高量氧化矽與氧化鋁等金屬氧化物的玻璃材料，藉此開發高值化低成本技術，以回收面板玻璃材料轉換製備奈米多孔性材料，將應用於水體水質淨化與回收再利用，達到「搖籃到搖籃」的環境永續目標。
本研究利用田口實驗設計法以L18直交表找出最佳化製程參數，研究顯示熔融溫度(1000 ℃)、廢面板玻璃與碳酸鈉重量比(1:2)、鹽酸濃度(0.1N)、酸洗時間 ( 4小時)、乾燥溫度與時間(110 ℃與12小時) 為最佳製程條件。利用BET 等溫氮氣吸附分析發現廢面板玻璃經由碳酸鈉活化結構形成相分離改質後比表面積高達175 (m2/g)，並搭配穿透式電子顯微鏡剖面影像鑑定平均孔洞大小為12 nm，為一中孔性矽酸鋁奈米材料；此材料具有電荷吸引性與高比表面積等特性功能，在酸性pH 3.5環境下對重金屬銅、鋅、鎳、鋇等有高吸附能力分別為64.5、34.0、23.1及105 mg/g；此外，進一步以放量填充管柱進行工業電鍍廢水中鎳重金屬去除試驗，結果顯示吸附能力達18.7 mg/g相當於實驗值，顯示此中孔性奈米材料在工業上為一高效率多孔性吸附劑。
此中孔性矽酸鋁奈米材料利用其對鋇具有高吸附能力特性，將此材料應用在過氧化流體化結晶(COP-FBC)技術作為結晶載體，能有效從高濃度硼廢水進行回收硼，研究結果顯示中孔性矽酸鋁奈米材料具有高結晶效率達93.4 % 形成硼化鋇氧化物(barium borate)，利用掃描式電子顯微鏡發現此載體具有特殊結晶路徑 (1) 此材料表面吸附二價鋇離子形成高結晶親和性、(2)富硼相氫氧化物離子與材料表面二價鋇離結合形成針狀結晶、(3)結晶經由材料孔隙往內層成長、(4)當材料已結晶成長飽和時，會自主架橋繼續長晶形程多層晶殼，達到高結晶特性。最後此結晶材料產物利用高溫X光繞射鑑定可知在600℃具相轉化形成硼化鋇材料，可作為光學玻璃原料再使用。本研究結果顯示利用廢棄面板玻璃可製備獲得新穎中孔性矽酸鋁奈米材料，且確實能有效應用於處理工業廢水中重金屬汙染去除及從高濃度硼廢水回收硼，以利達到永續環境之目標。

The recycling of the huge amount of thin film transistor liquid crystal display (TFT-LCD) glass wastes has become one of the worldwide environmental issues. Herein, a novel and cost-effective synthesis method for the fabrication of mesoporous aluminosilicate composite from the TFT-LCD waste has been developed to serve as the environmentally benign adsorbent for the removal of metal ions including Cu2+, Zn2+ and Ni2+, and as the carrier for recovery boron in terms of chemical –oxo precipitation fluidized bed crystallization (COP-FBC).
In this study, optimum parameters for fabrication of mesoporous aluminosilicate nanomaterial from TFT-LCD waste glass was been developed by using Taguchi experimental design technique. It is noteworthy that the parameters including melting temperature, added alkaline agent ratio, acid concentration, leaching time, calcinate temperature and time were optimized at 1000℃, 2 time agents, 0.1 N HCl, 4 hours, 110℃ and 12 hours, respectively. After melting procedure at 1000 C in the presence of Na2CO3 for phase separation, the mesoporous structure of aluminosilicate which had a surface area of 175 m2 g-1 and an average particle size of 12 nm was created. The surface functional groups of tailored mesoporous aluminosilicate nanocomposite (M-ANC) material were negatively charged .The adsorption capacity for Cu2+, Zn2+ ,Ni2+ and Ba2+ were 64.5, 34.0, 23.1 and 105mg g-1, respectively, at pH 3.5. Moreover, the environmental applicability of mesoporous aluminosilicate material is evaluated by column experiment in the presence of real electroplating wastewater. M-ANC can effectively remove Ni2+ in the electroplating wastewater with the adsorption capacity of 18.7 mg g-1.
On the other hand, the negatively charged surface and mesoporous structure of aluminosilicate material enhance the adsorption of Ba2+ onto surface, which is conducive to the enhancement of recovery of boron species. Moreover, the crystallization ratio of boron by mesoporous aluminosilicate material can be up to 93.4%. The cross-sectional SEM images and high-temperature X-ray diffraction (HT-XRD) results confirm the boron recovery mechanism in which the negatively charged functional group as well as the meso-porosity of mesoporous aluminosilicate material triggers the rapid formation of need-shaped precipitates of barium peroxoborate. The peroxoborate was converted to barium borate after calcination at 600 °C. Results obtained in this study clearly demonstrate the possibility of fabricating environmentally benign mesoporous aluminosilicate adsorbents from TFT-LCD waste to toward metal ion removal and sustainably recover and crystallize boron species from water and wastewater in COP-FBC.

Content index

中文摘要 .......................................................i
Abstract ......................................................iii
Abbreviations .................................................v
Content index .................................................vii
Figure index ..................................................xi
Table index ...................................................xvi
Chapter 1 .....................................................1
Introduction ..................................................1
1.1    Motivation .............................................2
1.2    Objective ..............................................5
Chapter 2 .....................................................7
Literature Review .............................................7
2.1    Patent Review for Recycling TFT-LCD Waste Glass Technologies ..................................................8
2.2    Removal of Heavy Metal Ions Technologies ...............10
2.2.1 Chemical Precipitation ..................................11
2.2.2 Membrane Filtration .....................................12
2.2.3 Reverse Osmosis .........................................14
2.2.4 Ion Exchange ............................................15
2.2.5 Adsorption ..............................................17
2.3    Removal of Non-metal Boron Technologies ................23
2.3.1 Removal of Boron by Chemical-oxo Precipitation ..........24
2.3.2 Removal of Non-metal Boron by Fluidized-bed Crystallized
..............................................................26
2.4    Fabrication of Mesoporous Material Methods .............30
2.4.1 Synthesis of Mesoporous Silica and Zeolite Methodologies
..............................................................32
2.4.2 Synthesis of Nanopore Glass Methodologies ...............34
2.5    Taguchi Optimization Studies ...........................40
2.6    Experimental Plan ......................................41
Chapter 3 .....................................................43
Experimental Detail ...........................................43
3.1    Introduction ...........................................44
3.2    Experimental Section ...................................44
3.2.1    Materials ............................................44
3.2.2    Fabrication of Mesoporous Aluminosilica ..............45
3.3    Characterization Techniques ............................48
3.3.1    Field-Emission Scanning Electron Microscopy ..........48
3.3.2    Field-Emission Transmission Electron Microscopy ......48
3.3.3    X-ray Diffraction ....................................48
3.3.4    High-temperature X-ray Diffraction ...................49
3.3.5    Raman Spectroscopy ...................................49
3.3.6    X-ray photoelectron spectroscopy analysis (XPS) ......49
3.3.7    Fourier Transformation Infrared (FTIR) ...............50
3.3.8    BET analysis .........................................50
3.3.9    Zeta Potential .......................................50
3.4    The quantity of metal oxide components .................51
3.5    Isothermal and Kinetics model ..........................51
Chapter 4 .....................................................54
Mesoporous Aluminosilicate Nanomaterial Optimization ..........54
Abstract ......................................................55
4.1    Introduction ...........................................56
4.2    Experimental design and statistical analysis ...........57
4.3    Results and discussion .................................58
4.3.1    Signal to noise ratio (S/N) analysis .................58
4.3.2    ANOVA analysis of variance for S/N ...................61
4.4    Summary ................................................62
Chapter 5 .....................................................64
Mesoporous Aluminosilicate Composite for Adsorption of Heavy Metal ions ..........................................................64
5.1    Introduction ...........................................65
5.2    Experimental procedure .................................68
5.2.1    Material and characterization ........................68
5.2.2    Fabrication of M-ANC .................................68
5.2.3    Adsorption of metal ions onto aluminosilicate materials
..............................................................68
5.2.4    Column experiment of adsorption from electroplating wastewater ....................................................69
5.3    Results and discussion .................................71
5.3.1    Surface characterization of aluminosilicate nanocomposites ................................................71
5.3.2    The pore texture of aluminosilicate materials ........79
5.3.3    Adsorption of metal ions by M-ANC ....................82
5.3.4    XPS analysis of adsorbent after the adsorption of metal ions ..........................................................94
5.3.5    Column experiment for Ni2+ adsorption from electroplating wastewater ....................................................97
5.4    Summary ................................................99
Chapter 6 .....................................................102
Development of Mesoporous Aluminosilicate Carriers for Boron Recovery and Crystallization ..................................102
6.1    Introduction ...........................................103
6.2    Experimental procure ...................................107
6.2.1    Material and characterization ........................107
6.2.2    Preparation of MAS ...................................107
6.2.3    Adsorption of Barium Ions by MAS .....................107
6.2.4    COP-FBC Experiments ..................................108
6.3    Results and discussion .................................110
6.3.1    Surface Characterization of Silica Sand and MAS ......110
6.3.2    The Pore Texture of Aluminosilicate Materials ........114
6.3.3    Adsorption of Ba2+ by MAS ............................117
6.3.4    Boron Recovery by COP-FBC ............................119
6.3.5    Identification of Peroxoborate Precipitates ..........125
6.3.6    The Crystallization Mechanism ........................128
6.4    Summary ................................................132
Chapter 7 .....................................................134
Conclusion ....................................................134
7.1    Overall Conclusion .....................................135
7.1    Recommendation .........................................137
References ....................................................139

 
Figure index
Figure2. 1 Different approaches for the recovery of glass from
waste TFT- LCD .....................................9
Figure2. 2 Removal mechanism by using membrane. (a) Size
exclusion/steric hindrance mechanism by low pressure
membrane; (b) adsorption by low pressure membrane; (c)
size exclusion/steric hindrance mechanism by TFC
membrane and; (d) Donnan exclusion/charge–charge
repulsion by TFC membrane...........................14
Figure2. 3 Anion ion exchange mechanism of adsorption Cr ( VI) by
EPIDMA/ D30164 .....................................16
Figure2. 4 Cation ion exchange mechanism of adsorption heavy metal
as (a,b,c) coordination bonding, (e) chelating
interaction between the electron donor species .....17
Figure2. 5 Surface functional groups of carbon-based adsorbents
for removal of heavy metal .........................18
Figure2. 6 Schematics of adsorption mechanisms of heavy metals
onto carbon-based adsorbents70......................19
Figure2. 7 Mechanisms of heavy metal ions Removal by silica- based
adsorbent72.........................................20
Figure2. 8 Reactions between boric acid, hydrogen peroxide,
perborates, and protons, and their stability constants
..............................................................25
Figure2. 9 Simulated species distribution in boric acid/hydrogen
peroxide system at different pH.....................26
Figure2. 10 Metastable zone for crystallization83 .............27
Figure2. 11 Precipitation mechanism in the fluidized-bed reactor
with seed material85 ..............................28
Figure2. 12 Proposed mechanisms of metal phosphate crystallization
in FBHC86 .........................................30
Figure2. 13 Schematics of the surface functionalization of SBA-15,
MCM-41, MCM-48 and KIT-6. .........................32
Figure2. 14 Schematic illustration of the templated synthesis of
a) a representative zeolite, b) a representative form
of mesoporous silica...............................34
Figure2. 15 Synthesis of porosification of nanopore glass
methodologies .....................................36
Figure2. 16 Synthesis of Zeolite and mesoporous silica (a) bottom
–up approach, mesoporous nanomaterial from TFT-LCD
waste panel glass (b) Top-down approach............39
Figure2. 17 Schematic representation displaying synthesis and
application of M-ANC and MAS nanomaterial for
adsorption heavy metal and recovery boron .........42

Figure 3.1 Fabrication of mesoporous aluminosilica nanomaterial
from NWTG procedures................................45

Figure 4.1 The effect of (a) melting temperature, (b) alkaline
agent ratio, (c) acid concentration (N), (d) acid
leaching time(hours), (e) calcinate temperature and (f)
calcinate time( hours) on the signal-to noise(S/N)
ratio for fabricate of mesoporous aluminosilica
nanomaterial .......................................59

Scheme 5.1 Schematic illustration of the fabrication and
activation of mesoporous aluminosilicate nanocomposites
(M-ANC) for the adsorption of metal ions ...........67
Scheme 5. 2 Graphic abstract illustration of the fabrication and
activation of mesoporous aluminosilicate
nanocomposites (M-ANC) for the removal of nickel ions
from electroplating ...............................101

Figure 5.1 SEM images of (a) original waste material (NWTG) and
(b) activated aluminosilicate material (M-ANC) ......72
Figure 5.2 FE-TEM image of activated aluminosilicate material (M-
ANC) (a) cross-sectional and (b) particle size
distribution of M-ANC................................73
Figure 5.3 XRD patterns of the TFT-LCD glass before (NWTG) and
after (M-ANC) the alkaline treatment at 1000 C in the
presence of Na2CO3...................................74
Figure 5.4 FTIR spectra of the TFT-LCD glass before (NWTG) and
after (M-ANC) the alkaline treatment at 1000 C in the
presence of Na2CO3...................................76
Figure 5.5 X-ray photoelectron spectroscopy (XPS) analysis of the
original (NWTG) and activated (M-ANC) aluminosilicate
materials. (a) Full scan survey and deconvoluted (b) Na
1s and (c) B 1s peaks ...............................78
Figure 5.6 The N2 adsorption-desorption isotherm and pore size
distribution of (a) the original (NWTG) and (b)
activated aluminosilicate material (M-ANC)...........80
Figure 5.7 (a) Adsorption capacity of mesoporous M-ANC materials
toward heavy metal ion adsorption and (b) isoelectric
point of original NWTG and activated M-ANC materials as
a function of pH. The initial concentration of metal
ions including Cu2+, Zn2+ and Ni2+ is 100 mg L-1 and
adsorbent dosage is 1 g L-1..........................83
Figure 5.8 Adsorption isotherms with fitted Langmuir model of
Cu2+, Ni2+ and Zn2+ onto M-ANC (a) and NWTG (b) at pH
3.5. The initial concentration of metal ion for
adsorption kinetic is 100 mg L-1 and the adsorbent
dosage is 1 g L-1...................................85
Figure 5.9 (a) Langmuir and (b)Freundlich adsorption isotherms of
metal ions onto M-ANC ..............................86
Figure 5.10 Adsorption kinetic curves with fitted pseudo-second-
order of Cu2+, Ni2+ and Zn2+ at pH 3.5. The initial
concentration of metal ion for adsorption kinetic is
100 mg L-1 and the adsorbent dosage is 1 g L-1.....92
Figure 5. 11 The (a) pseudo-first-order, (b) pseudo-second-order
kinetics and (c) intra-particle diffusion model of
adsorption of metal ions onto M-ANC nano-adsorbent.
...................................................93
Figure 5.12 (a) XPS spectra of M-ANC before and after the
adsorption of Cu2+, Zn2+ and Ni2+, (b) Cu 2p for M-
ANC_Cu; (c) Zn 2p for M-ANC_Zn and (d) Ni 2p for M-
ANC_Ni ............................................95
Figure 5. 13  (a) The XPS O 1s spectra of M-ANC, M-ANC_Cu, M-
ANC_Zn and M-ANC_Ni and the deconvolution of O 1s peak
after the adsorption of (b) Cu, (c) Zn, and (d) Ni
ions...............................................97
Figure 5. 14 The breakthrough curve of Ni2+ adsorption from
electroplating wastewater by 50 g M-ANC composite in a
column with bed volume of 150 mL at pH 3.5 ± 0.2. The
initial Ni2+ concentration is 30 mg L-1 and the flow
rate is 15 mL min -1 ..............................99

Scheme 6. 1 Illustration of the crystallization mechanism for the
recovery of boron species using mesoporous
aluminosilicate (MAS) as the carrier in chemical oxo-
precipitation fluidized bed crystallization (COP-FBC)
reactor. Photograph courtesy of ‘Cheng-Kuo Tsai’.
Copyright 2019.....................................106
Scheme 6. 2 Conceptual model of the crystallization of barium
peroxoborate in COP-FBC reactor using silica sand and
mesoporous MAS nanomaterials as the carriers.......131

Figure 6. 1 Schematic illustration of experimental set-up of the
chemical oxo-precipitation fluidized-bed
crystallization (COP-FBC)..........................109
Figure 6. 2 The SEM images of (a) silica sand and (b) MAS
nanomaterial, (c) cross sectional FE-TEM image of MAS,
and (d) particle size distribution of MAS..........111
Figure 6. 3 FTIR spectra of silica and MAS (a) and (b) the waste
TFT-LCD material ..................................112
Figure 6. 4 XRD patterns of TFT-LCD glass before and after the
activation treatment...............................113
Figure 6. 5 XPS spectra of silica and MAS nanomaterials derived
from the waste TFT-LCD ............................114
Figure 6. 6 N2 adsorption-desorption isotherm (a) and pore size
distribution (b) of the commercial silica sand and as-
prepared MAS nanomaterials derived from the waste TFT-
LCD. Insets in Figure (a) and (b) are the enlarged
figures of isotherm and pore size distribution of
silica sand, respectively .........................116
Figure 6. 7 Adsorption isotherms and the fitted Langmuir model of
silica sand and MAS for Ba2+ adsorption ...........118
Figure 6. 8 Comparison of the boron recovery performance of silica
sand and MAS in terms of (a) removal efficiency, (b)
crystallization ratio, and (c) effluent concentration
as the function of reaction time in the COP-FBC
process at pH 10.5.................................121
Figure 6. 9 COP-FBC system of commercial silica-sand (a) and MAS
(b) carrier for recovery boron ....................122
Figure 6. 10 Raman spectra of precipitates produced from the
recovery of boron in the presence of (a) silica sand
and (b) MAS as a function of reaction time .......126
Figure 6. 11 HT-XRD patterns for crystalized products by MAS
carrier in COP- FBC after 216 h of incubation.....128
Figure 6. 12 The cross-sectional SEM images of (a-d) MAS during
boron recovery at various reaction times..........129
Figure 6. 13 The EDS spectra and SEM image (inset) of the
mesoporous aluminosilicate (MAS) carrier-based
crystallization products..........................130
Figure 6. 14 The cross-sectional SEM images of (a-d) silica sand
during boron recovery at various reaction times ...130

Table index
Table2. 1 Different techniques for removing heavy metals from
water/ wastewater ...................................22
Table2. 2 Relation between pore volume and surface area at
different cooling condition .........................35
Table 3. 1 Experimental parameters and their levels ...........46
Table 3. 2 Modified orthogonal L18 (21*35) array ..............47
Table 4. 1 Standard orthogonal arrays of 18 different groups
following Taguchi’s suggestion .....................60
Table 4. 2 Analysis of variance for S/N ratios, using adjusted SS
for test ...........................................62
Table 5. 1 Characteristics of the electroplating wastewater
collected from Changhua Coastal Industrial Park, Taiwan
.....................................................70
Table 5. 2 Compositions of dominant constituents in NWTG and M-ANC
.....................................................76
Table 5. 3 The surface area, pore volume and pore size of the TFT-
LCD panel waste before (NWTG) and after (M-ANC) the
activation process .................................81
Table 5. 4 Isotherm parameters of copper, zinc and nickel
adsorption onto the M-ANC material .................87
Table 5. 5 Electronegativity of metal ion and the first stability
constants for metal hydroxide formation ............87
Table 5. 6 Comparison of the adsorption capacity of M-ANC toward
metal ion adsorption with reported data using a wide
variety of materials as the adsorbents .............90
Table 5. 7 Kinetics model constant for the adsorption of Cu(II),
Zn(II) and Ni(II) ions onto M-ANC nanocomposite ....94
Table 6. 1 The Experimental parameter of the commercial silica
sand and mesoporous aluminosilicate (MAS) carrier
seeds ..............................................109
Table 6. 2 The specific surface area and pore texture of the
commercial silica sand and mesoporous aluminosilicate
(MAS) carrier seeds ................................115
Table 6. 3 Isothermal parameters of Ba2+ adsorption onto the
silica sand and MAS materials ......................118
Table 6. 4 Comparison of the recovery efficiency and
crystallization ratio of boron using COP-based
treatment processes ................................124



                                

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