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Sustainable Selection of Copper Ions from Battery Wastewater Using Calcium-Activated Polyphenylene Oxide Derivatives

  • 이철 (서강대학교 일반대학원)

초록 (요약문)

Recycling valuable metals from battery wastewater is essential for sustainable resource management and environmental protection. This study presents a copper (Cu2+)-selective polyphenylene oxide (PPO)-based polymer adsorbent, functionalized with carboxyl (–COOH) and amide (–CONH–) groups and activated with calcium ions (Ca2+), to achieve efficient Cu2+ separation via ion exchange. While nickel (Ni2+) and cobalt (Co2+) are more economically valuable, Cu2+ poses significant environmental risks and requires selective removal to facilitate downstream recovery of Ni2+ and Co2+. The adsorbent exhibited high adsorption capacity and rapid kinetics for Cu2+, Ni2+, Co2+, and manganese (Mn2+) in single-component systems, and showed exceptional selectivity for Cu2+ in multi-component systems. The adsorption mechanism—driven by metal-ligand affinity and ligand transfer dynamics—was elucidated through spectroscopic analysis and density functional theory (DFT) calculations. When applied in a packed-bed configuration, the system enabled selective Cu2+ capture and Ca2+ recovery (85%), supporting adsorbent reusability and process sustainability. With Cu2+ selectivity coefficients ranging from 101 to 666, over 90% high-purity Cu2+ was recovered from a Cu2+/Ni2+/Co2+/Mn2+ mixture in a single pass. This work presents a scalable, eco-friendly approach for treating battery wastewater and recovering critical metals, advancing circular economy practices in industrial applications.

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Table of Contents
List of Figure vi
List of Tables xii
Abstract xiii
Chapter 1. Introduction 1
1.1 Background 2
1.2 Adsorbents for Metal Recovery 4
1.3 Polymeric Adsorbents for Metal Recovery 5
1.3.1 Adsorption 7
1.3.1.1 Langmuir Adsorption Model 8
1.3.1.2 Freundlich Adsorption Model 11
1.3.2 Adsorption Kinetics 12
1.3.2.1 Pseudo-First-Order Model 14
1.3.2.2 Pseudo-Second-Order Model 15
1.3.3 Adsorption Thermodynamics 16
1.3.4 Effects of pH on Adsorption and Desorption Processes 18
1.4 Metal Separation via Adsorption 20
1.4.1 Challenges in Selective Adsorption of Metal Ions 20
1.4.2 Selectivity Coefficients 22

Chapter 2. Materials and Experimental Methods 23
2.1 Introduction 24
2.2 Materials 25
2.3 Experimental Section 26
2.3.1 Synthesis of PPO-NO2 26
2.3.2 Synthesis of PPO-NH2 27
2.3.3 Synthesis of PPO-COOH 28
2.3.4 Synthesis of PPO-COOCa 29
2.3.5 Adsorption Isotherm Measurement 30
2.3.6 Adsorption Kinetic Measurement 31
2.3.7 Breakthrough Experiment 32
2.3.8 Computational Simulation 33
2.4 Characterizations 34
2.4.1 1H-Nuclear Magnetic Resonance (1H-NMR) 34
2.4.2 Fourier-Transform Infrared Spectroscopy (FT-IR) 35
2.4.3 Energy Dispersive Spectroscopy (EDS) 36
2.4.4 X-ray Diffraction (XRD) 37
2.4.5 Inductively Coupled Plasma Optical Emission Spectroscopy
(ICP-OES) 38
2.4.6 X-ray Photoelectron Spectroscopy (XPS) 39

Chapter 3. Results and Discussions 40
3.1 Chemical Structure Characterization 41
3.2 Metal Adsorption Performance in Single-Component Systems 46
3.2.1 Metal Adsorption Isotherm and Kinetic Analysis 46
3.2.2 Effect of pH on Adsorption Performance and Reusability 52
3.2.3 Temperature-Dependent Adsorption Performance 55
3.3 Selective Copper Ion Adsorption in Multi-Component Systems 58
3.3.1 Adsorption Selectivity 58
3.3.2 Selective Adsorption Kinetics 63
3.4 Investigation of the Metal Ion Adsorption Mechanisms 65
3.4.1 Ion-Exchange Mechanism 65
3.4.2 Selective Adsorption Driven by Affinity Differences 74
3.4.3 Density Functional Theory Calculations 80
3.5 Breakthrough Behavior in a Packed-Bed System under Quaternary Metal Ion Conditions 88

Chapter 4. Conclusions and Recommendations 92
4.1 Conclusions 93
4.2 Recommendations for Future Work 94

APPENDIX A 95
APPENDIX B 97

Reference 98

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