Recent developments and the future of the recycling of spent graphite for energy storage applications
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摘要: 本文对从废旧锂离子电池中获得的电池级石墨的回收和再生进行了广泛的分析。其主要目的是应对供需挑战，最大限度地减少环境污染。该综述主要包括获得、分离、纯化和再生废石墨的方法，以确保其可适用于高质量的储能为目的。为了提高石墨回收效率和去除残留污染物，研究者们探索了热处理、溶剂溶解和超声波处理等技术。本综述进一步评估了湿法和火法冶金的净化和再生方法，考虑了它们对环境的影响和能源消耗等问题。为了可持续和成本效益的提高，可以采用无酸纯化和低温石墨化。讨论了锂离子电池和超级电容器中再生石墨的具体要求，强调了包括酸浸、高温处理和表面涂层在内的回收工艺。这篇综述为开发高效和可持续的储能系统、解决环境问题和满足日益增长的石墨需求提供了宝贵的信息。Abstract: This review provides an extensive analysis of the recycling and regeneration of battery-grade graphite obtained from used lithium-ion batteries. The main objectives are to address supply-demand challenges and minimize environmental pollution. The study focuses on the methods involved in obtaining, separating, purifying, and regenerating spent graphite to ensure its suitability for high-quality energy storage. To improve the graphite recovery efficiency and solve the problem of residual contaminants, techniques like heat treatment, solvent dissolution, and ultrasound treatment are explored. Wet and pyrometallurgical purification and regeneration methods are evaluated, considering their environmental impact and energy consumption. Sustainable and cost-effective approaches, including acid-free purification and low-temperature graphitization, are highlighted. Specific requirements for regenerated graphite in lithium-ion batteries and supercapacitors are discussed, emphasizing customized recycling processes involving acid leaching, high-temperature treatment, and surface coating. Valuable information for the development of efficient and sustainable energy storage systems is provided, addressing environmental issues, and how to meet the increasing demand for graphite anodes.
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Key words:
- Spent graphite /
- Lithium-ion batteries /
- Regeneration /
- Anode /
- Reutilization
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Figure 2. (a) Recycling technology for spent graphite, (b) Separating electrode plates and active substances to obtain spent graphite. reprinted with permission from Ref.[21], Copyright © 2015 Elsevier Ltd. All rights reserved. (c) Separating cathode and anode electrode active materials to obtain spent graphite. reprinted with permission from Ref.[51], Copyright © 2018, American Chemical Society
Figure 3. (a) Flow chart of wet recovery of lithium and spent graphite, (b) Effect of S/L on metal recovery efficiency, (c) Cycle performance of regenerated graphite at room temperature at 1 C. reprinted with permission from Ref.[55], Copyright © 2019 Elsevier Ltd. All rights reserved. (d) Mechanism of graphite regeneration after high-temperature treatment, (e) Cycle stability of PG, HTT-700, HTT-900, HTT-1100, HTT-1300 and HTT-1500 samples under 100 cycles at 1 C. HRTEM images of (f) SG , (g) PG and (h) HTT-900 . reprinted with permission from Ref.[56], Copyright © 2021 Elsevier Ltd. All rights reserved
Figure 4. (a) Mechanism diagram of sulfuric acid solidification leaching high temperature calcination reaction, (b) RG spherical aberration electron microscope images, (c) Cycle stability of SG, PG, RG and CG at 0.1 C for 50 cycles. reprinted with permission from Ref.[58] , Copyright © 2020, American Chemical Society. (d) Flash recycling steps for spent batteries. reprinted with permission from Ref.[60], Copyright © 2022 Wiley-VCH GmbH. (e) Schematic diagram of the microwave assisted process for the regeneration and utilization of spent graphite recovered from spent LIBs. reprinted with permission from Ref.[59], Copyright © 2021 Elsevier B.V. All rights reserved
Figure 5. (a) Modification methods for fast charging graphite: expanding interlayer spacing, doping, and constructing defects. SEM images of (b) graphite, (c) expanded graphite (EG*) and (d) their thermally annealed version (EG), (e) comparison of interlayer spacing and domain size, (f) magnification performance of graphite, EG * and EG. reprinted with permission from Ref.[65], Copyright © Royal Society of Chemistry
Figure 6. (a) Schematic diagram of RG and DRG formation process, HRTEM images of (b) DRG and (c) CG reprinted with permission from Ref.[68], Copyright © 2022, Tsinghua University Press. (d) Schematic diagram of N-RG synthesis, (e) Cyclic performance of CG, SG, and N-RG half cells, (f) Schematic diagram of Li diffusion paths in CG and N-RG. reprinted with permission from Ref.[69], Copyright © 2022 Elsevier Ltd. All rights reserved
Figure 7. (a) Na intercalated EG schematic diagram. HRTEM images of (b) PG, (c) GO, (d) EG-1h and (e) EG-5h. reprinted with permission from Ref.[72], Copyright © 2014, Springer Nature Limited. (f) XRD diagram of graphite, (g) point change diagram of the first cycle at 0.1 C, (h) corresponding to the marked XRD pattern in b1. reprinted with permission from Ref.[73], Copyright © 2015, American Chemical Society. (i) XRD images of different temperature heat treatments and RG, and (j) HRTEM images of RG-1300. Cyclic performance of NIB and KIB at (k) 2 A g−1 and (l) 0.2 A g−1, respectively. reprinted with permission from Ref.[75], Copyright ©Royal Society of Chemistry. (m) Structural models of AG and RG, SEM images of (n) AG and (o) RG, cyclic performance of AG at 2000 mA g−1. reprinted with permission from Ref.[76], Copyright © 2020 Elsevier Ltd. All rights reserved
Figure 8. (a) Schematic diagram of preparation and working mechanism of Si/SG material, (b, c) HRTEM image of Si/SG, (d) Cycle performance of Si/AG and Si/SG at 1 A g−1 . reprinted with permission from Ref.[80], Copyright © Royal Society of Chemistry. (e) T-SGT/ Si@C Schematic diagram of the synthesis process of anode materials, (f) CGT/ Si@C and T-SGT/ Si@C cyclic performance. reprinted with permission from Ref.[82], Copyright © 2021 Elsevier B.V. All rights reserved. (g) Schematic diagram of adsorption performance and catalytic effect of SG modified separator, (h) Cycle performance of batteries with different separators at 1 C. reprinted with permission from Ref.[85], Copyright © Royal Society of Chemistry
Table 1. Recycling methods and high-quality utilization of spent graphite
Material Method Electrochemical performance High-quality application Ref. Defect-rich recycled graphite High-temperature shock 323 mAh g−1 (2 C) Fast-charging graphite material [68] N-RG Acid treated, gas-phase exfoliation
and element doping465 mAh g−1 (0.1 A g−1)
143.5 mAh g−1 (0.4 A g−1)Fast-charging graphite material [69] Recycled graphite Pyrolysis process 162 mAh g−1 (0.2 A g−1, SIB)
320 mAh g−1 (0.05 A g−1, PIB)Sodium/potassium battery [75] Regeneration graphite Sulfuric acid leaching and High
temperature heat treatment427 mAh g−1 (0.5 C, 200 cycle)
127 mAh g−1 (50 mA g−1, SIB)Sodium/potassium battery [76] Si/SG composite Mechanical ball milling 1321.8 mAh g−1 (0.05 A g−1)
69% (1 A g−1, 400 cycle)Silicon carbon composite materials [81] T-SGT/Si@C Heat treatment, sulfuric acid leaching
and calcination92.47% (500 mA g−1, 300 cycle)
434.1 mAh g−1 (500 mA g−1)Silicon carbon composite materials [82] SG-modified separator Surface coating 968 mAh g−1 (1 C) Lithium-sulfur batteries [85] CoO/CoFe2O4/EG Acid leaching, high-temperature treatment
and hydrometallurgy890 mAh g−1 (1 A g−1, 700 cycle)
208 mAh g−1 (5 A g−1)High-performance composites materials [29] PE/GRx, PP/GRx Solution intercalation Composite separator [86] Recovered graphite Ultrasonic peeling and High
temperature treatment185.54 Wh kg−1 (0.319 kW kg−1)
～75% (2000 cycle, 10 °C and 25 °C)Lithium-ion supercapacitors [90] 
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