本實驗主要目的是在循環固定床中使用顆粒狀氫錳氧化物，以去除水溶液中鈷離子之研究。尖晶石鋰錳氧化物粉末係使用碳酸鋰和碳酸錳作為前驅物以固態法製備而成。並使用水玻璃粘合劑對LMO粉末進行造粒。而後經0.3N鹽酸酸洗以轉化成氫錳氧化物（HMO）顆粒。由XRD、 SEM、和EDS來確定吸附劑的晶體結構、形態和物理性質。
經由XRD分析的結果，粉末狀鋰錳氧化物在800oC煅燒溫度下展現出高的尖晶石純相。而顆粒狀氫錳氧化物加入60%水玻璃在500oC煅燒溫度下也展現出高的尖晶石純相。其吸附劑的吸附性能由 ICP-OES 測得水溶液鈷離子濃度來進行評估。
以HMO顆粒吸附劑在循環固定床下探討在不同操作條件如吸附劑用量，流率和溫度對於鈷離子吸附之能力。由實驗中得知HMO顆粒除去鈷的效果隨著反應溫度和吸附劑用量及流率的增加而增加。在循環固定床下，HMO顆粒之吸附過程利用一階速率方程式與鈷離子吸附能力之實驗數據相當符合。其高度的顆粒穩定性顯示HMO是一種良好的材料以去除水溶液鈷離子，故有良好的回收再利用特性以達到永續發展的效果。

This study was to adsorption of cobalt ions solution by using hydrogen manganese oxide granule in a recycle fixed bed. Spinel lithium manganese oxide material was prepared with solid-state method using lithium carbonate and manganese carbonate as the precursors. The LMO powder was granulated using a water glass binder. It was then acid washed with 0.3 N hydrochloric acid to convert LMO granule to manganese oxide (HMO) granule. Those materials were characterized by X-ray diffraction spectroscopy (XRD), Scanning Electron Microscopy with energy dispersive X-ray microanalysis (SEM), and Energy Dispersive Spectrometer (EDS).
XRD patterns show that the spinel LMO powder prepared at a calcination temperature of 800°C has a higher spinel pure phase. The HMO granule when added to 60% water glass, exhibits a high spinel purity phase at a calcination temperature of 500 °C. The cobalt adsorption capacities of adsorbents were evaluated by ICP-OES to detect the concentration of Co2+ in aqueous solution.
The ability to adsorb cobalt ions under different operating conditions such as adsorbent amount, flow rate and temperature was investigated using a recycle fixed bed in continuous system with HMO granule adsorbents. It is known from experiments that the cobalt adsorption capacities to HMO granule increases with the increase of reaction temperature, the amount of absorbent and flow rate. The adsorption process using the first-order rate with r=-K_1 (C-C_e) can fit well the experimental data of cobalt ion adsorption in a recycle fixed bed. The high particle stability shows that HMO granule can be a good material to remove cobalt ions from aqueous solution.

ACKNOWLEDGEMENTS i
ABSTRACT ii
摘要 iii
TABLE OF CONTENT iv
LIST OF TABLES vii
LIST OF FIGURES vii
NOMENCLATURE xi
CHAPTER 1 INTRODUCTION 1
1.1 Background 1
1.2 Objects and scope 10
CHAPTER 2 LITERATURE SURVEY 11
2.1 Basic cell chemistry 11
2.1.1 Lithium-metal systems 11
2.1.2 Lithium-ion batteries 13
2.2 Positive electrode materials 16
2.2.1 Transition metal oxides 20
2.2.2 Cathode materials 20
2.2.3 Spinel Lithium manganese oxide (LMO) 24
2.3 Lithium ion battery of recycling processes 27
2.3.1 Pretreatment method 27
2.3.2 Pyrometallurgical process 29
2.3.3 Hydrometallurgical process 30
2.4 Ion-sieve effect 35
2.5 Granulation of LMO powder 42
2.6 The fixed-bed column adsorption 45
2.6.1 Fixed-bed column adsorption experiments 46
2.6.2 Adsorption of metal ions 47
2.6.3 Evaluation of the mechanism of metal ion adsorption in a fixed bed column 51
2.6.4 Breakthrough curve modelling 51
CHAPTER 3 EXPERIMENTAL 55
3.1 Preparation of adsorbent 55
3.1.1 Preparation of spinel lithium manganese oxide (LMO) powder 55
3.1.2 Preparation of spinel lithium manganese oxide (LMO) granule 59
3.1.3 Preparation of HMO granule by acid treatment (Ryu et al., 2013) 61
3.2 Experimental procedure in a recycle fixed bed 65
3.2.1 Blank experiment 67
3.2.2 Cobalt adsorption by HMO granule 68
3.3 Characteristic analysis of adsorbent of HMO granule 68
3.3.1 X-Ray diffraction analysis 70
3.3.2 Scanning electron microscopy analysis 70
3.3.3 Inductively coupled plasma optical emission spectrometer analysis 71
CHAPTER 4 KIENETIC MODELLING OF RECYCLE FIXED BED 72
Kinetic Modelling 72
CHAPTER 5 RESULTS AND DISCUSSION 76
5.1 Characterizations of adsorbent 76
5.1.1 XRD patterns of the prepared adsorbents 76
5.1.2 SEM properties of the prepared adsorbent 82
5.1.3 EDS properties of the prepared adsorbent 86
5.2 Effect of calcination temperature in HMO granule stability 89
5.3 Adsorption performance of HMO granule with different water glass content 91
5.4 Adsorption experiment in recycle fixed bed 94
5.4.1 Effect of adsorbent amount 94
5.4.2 Effect of flow rate 94
5.4.3 Effect of temperature 96
5.4.4 Adsorption kinetic modelling 98
CHAPTER 6 CONCLUSIONS 106
REFERENCES 107
APPENDIX A 117
APPENDIX B 120

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