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摘要: 近些年來，隨著全球新能源汽車和智能電子產品市場的逐漸擴大，鋰離子電池數量急劇增加，從保護生態環境和節約資源的角度來看，開展廢舊鋰電池的回收再生研究具有極大的社會和經濟價值。以三元鋰電池為例，介紹了三元鋰電池正極失效原因以及傳統火法冶金和濕法冶金浸出工藝的回收條件、應用現狀和優缺點，綜述了廢舊三元鋰電池濕法冶金浸出后再生和直接再生的研究進展。基于此，特別論述了再生后的三元鋰電池正極材料通過離子摻雜和表面包覆改性升級的創新策略。最后，展望了廢舊三元鋰電池回收再生工藝的發展前景，以期對廢舊鋰電池回收體系的完善提供一定的參考和建議，形成經濟效益好、綠色環保的鋰電池生產—回收閉路循環回收體系。Abstract: In recent years, with the gradual expansion of the global market for new energy vehicles, the supply and demand of lithium-ion batteries (LIBs) as a source of energy have been increasing, which directly promotes the significant increase in the number of used LIBs. Among them, ternary LIBs have been widely used because of their high specific capacity and excellent multiplying performance, which has aroused people’s concerns about their proper disposal. On the one hand, ternary LIBs contain rich nonferrous metals, such as lithium, nickel, cobalt, and manganese, with high recovery values. On the other hand, spent ternary LIBs contain a large number of toxic electrolytes and heavy metals, which will cause environmental pollution and damage human health if not handled properly. Therefore, research on the recycling and regeneration of spent ternary LIBs has been receiving considerable attention. Given the principles of low energy consumption, “green” recovery, and high recovery rate, this study briefly introduces the main failure causes of cathode materials for ternary LIBs and discusses the application scope and the advantages and disadvantages of traditional pyrometallurgy (such as chemical reduction and salinization roasting) and hydrometallurgical leaching processes (such as acid, alkali, and biological leaching). This review creatively summarizes the research progress on regeneration after hydrometallurgical leaching (such as coprecipitation and sol–gel methods) and direct regeneration (such as high-temperature solid-phase method, solvothermal treatment, and molten salt method) of spent ternary LIBs in recent years and analyzes the advantages and disadvantages of various regeneration technologies. Notably, compared with traditional pyrometallurgy and hydrometallurgy, the process of regeneration after hydrometallurgical leaching and direct regeneration considerably reduces the complexity of the process flow, maximizes the comprehensive utilization rate of nonferrous metals, and realizes the closed-loop recovery route of spent LIB cathode. Based on this, the innovative strategy of upgrading the cathode material of regenerated ternary LIBs through ion doping and surface coating modification, which effectively improved the poor thermal stability, short cycling, and low rate performance of ternary LIBs caused by high nickel content, was particularly discussed. Finally, from the perspective of recycling methods, multiple modification strategies, and mechanism research, the future development of recycling technology for spent ternary LIBs is proposed. This study aims to provide some references and suggestions for the improvement of the spent LIB recycling system and establish a closed-cycle recycling system for the production and recycling of spent LIBs.
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Key words:
- ternary lithium battery /
- cathode material /
- pyrometallurgy /
- hydrometallurgy /
- regenerate /
- cathode modification
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表 1 火法冶金—濕法冶金聯合回收有價金屬浸出率
Table 1. Leaching rates of valuable metals recovered by pyrometallurgy and hydrometallurgy
Recovery method Leaching rate/% Reference Li Ni Co Mm Graphite reduction roasting and sulfuric acid leaching 90.0 90.0 97.0 [20] Carbothermal reduction, carbonated water leaching and sulfuric acid leaching >80.0 98.0 96.0 96.0 [21] Carbothermal reduction and sulfuric acid leaching 93.67 93.33 98.08 98.68 [22] Carbothermal reduction, carbonated water leaching and sulfuric acid leaching 84.7 >99.0 [23] Microwave carbothermal reduction fumaric acid leaching 99.6 >97. 0 [24] Carbothermal reduction and carbonic acid water immersion 99.2 [25] Nitrate roasting and water leaching >99. 0 [26] Chlorination roasting and carbonic acid water leaching >90. 0 [27] 
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表 2 各浸出體系的舉例
Table 2. Examples of each leaching system
Technology Leaching system Optimal condition Leaching rate/% Reference Li Ni Co Mn Acid leaching Citric acid Sucrose Ambient temperature 60 min 99 [39] Trichloroacetic acid Hydrogen peroxide 60 ℃ 30 min 99.7 93.0 91.8 89.8 [40] Citric acid D-glucose 80 ℃ 120 min 99 91 92 94 [41] Ascorbic acid 69.26 ℃ 59.79 min 92.53 56.32 96.35 89.28 [42] Acetic acid Hydrogen peroxide 60 ℃ 60 min >99 [43] Phosphoric acid Hydrogen peroxide 40 ℃ 60 min 95.4 99.8 99.5 98.0 [44] Alkali leaching Ammonia water Ammonium sulfite 80 ℃ 1 h 25 80 1 [45] Ammonia Sodium sulfite 80 ℃ 2 h 79.1 85.3 86.4 [46] Ammonia water Ammonium chloride Ammonium sulfite 150 ℃ 30 min 90.3 98.3 100 [47] Bioleaching Iron–sulfur-oxidizing bacteria 30 ℃ 60 min 60.0 48.7 53.2 81.8 [48] Aspergillus niger 30 ℃ 30 days 100 45 38 72 [49] Thiobacillus ferrooxidans 30 ℃ 24 h 89 90 82 92 [50]
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表 3 共沉淀法不同沉淀體系的反應原理
Table 3. Reaction principles of different precipitation systems in the coprecipitation method
Type Reaction principle Reference Hydroxide coprecipitation $x{\text{Ni} }_{\text{aq} }^{\text{2+} }+{y}{\text{Co} }_{\text{aq} }^{\text{2+} }+{z}{\text{Mn} }_{\text{aq} }^{\text{2+} }+{n}{\text{NH} }_{\text{3} }\cdot{\text{H} }_{\text{2} }{\text{O} }_{\text{aq} }={\left[{\text{Ni} }_{ {x} }{\text{Co} }_{ {y} }{\text{Mn} }_{z}{\left({\text{NH} }_{\text{3} }\right)}_{ {n} }\right]}_{\text{aq} }^{\text{2+} }+{n\text{H} }_{\text{2} }\text{O}$ (x+y+z=1)
${\text{[}{\text{Ni} }_{ {x} }{\text{Co} }_{y}{\text{Mn} }_{ {z} }{\text{(}{\text{NH} }_{\text{3} }\text{)} }_{ {n} }\text{]} }_{\text{aq} }^{\text{2+} }+{\text{2OH} }^{ {-} }={\text{Ni} }_{x}{\text{Co} }_{ {y} }{\text{Mn} }_{ {z} }{\text{(OH)} }_{\text{2} }+{ {n}\text{NH} }_{\text{3} }$ (x+y+z=1)[52] Carbonate coprecipitation ${ {x}\text{Ni} }_{\text{aq} }^{\text{2+} }+{ {y}\text{Co} }_{\text{aq} }^{\text{2+} }+{z\text{Mn} }_{\text{aq} }^{\text{2+} }+n\text{NH} _{\text{3} }\cdot{\text{H} }_{\text{2} }{\text{O} }_{\text{aq} }={\left[{\text{Ni} }_{ {x} }{\text{Co} }_{ {y} }{\text{Mn} }_{z}{\left({\text{NH} }_{\text{3} }\right)}_{ {n} }\right]}_{\text{aq} }^{\text{2+} }+{ {n}\text{H} }_{\text{2} }\text{O}$ (x+y+z=1)
${\text{[}{\text{Ni} }_{x}{\text{Co} }_{ {y} }{\text{Mn} }_{z}{\text{(}{\text{NH} }_{\text{3} }\text{)} }_{ {n} }\text{]} }_{\text{aq} }^{\text{2+} }+{\text{CO} }_{\text{3} }^{ {2-} }{+}{ {n}\text{H} }_{\text{2} }\text{O=}\left({\text{Ni} }_{ {x} }{\text{Co} }_{ {y} }{\text{Mn} }_{{z} }\right){\text{CO} }_{\text{3} }+{{n}\text{NH} }_{\text{3} }\cdot{\text{H} }_{\text{2} }{\text{O} }_{\text{aq} }$ (x+y+z=1)[53] Oxalate coprecipitation $\text{4}{\text{H} }_{\text{2} }{\text{C} }_{\text{2} }{\text{O} }_{\text{4} }\text{+2Li}{\text{Ni} }_{{x} }{\text{Co} }_{y}{\text{Mn} }_{{z} }{\text{O} }_{\text{2} }{=2}\left({\text{Ni} }_{{x} }{\text{Co} }_{{y} }{\text{Mn} }_{{z} }\right){\text{C} }_{\text{2} }{\text{O} }_{\text{4} }{+4}{\text{H} }_{\text{2} }\text{O+2C}{\text{O} }_{\text{2} }$ (x+y+z=1) [54]
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表 4 傳統濕法冶金、火法冶金和直接再生的優缺點
Table 4. Advantages and disadvantages of traditional hydrometallurgy, pyrometallurgy, and direct regeneration
Recycling method Advantages Disadvantages References Hydrometallurgy Low-temperature operation
High material purity
Low energy consumptionComplex process
Secondary acid–base pollution
Large consumption of chemicals[59] Pyrometallurgy Simple process
Large processing capacityHigh energy consumption
Low metal recovery[65?66] Direct regeneration Simple process Low cost Single process at present
High requirements for battery classification[62, 67]
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