| 废旧锂电池中有价金属回收及三元正极材料的再制备 |
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| 引用本文： | 曹玲,刘雅丽,康铎之,李佳竺,陈湘萍,马宏瑞.废旧锂电池中有价金属回收及三元正极材料的再制备[J].化工进展,2019,38(5):2499-2505. |
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| 作者姓名： | 曹玲 刘雅丽 康铎之 李佳竺 陈湘萍 马宏瑞 |
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| 作者单位： | 陕西科技大学环境科学与工程学院,陕西西安,710021;湖南大学环境科学与工程学院,湖南长沙,410082 |
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| 基金项目： | 国家自然科学基金(51704189);陕西科技大学自然科学预研基金项目(2016QNBJ-06);国家水体污染控制与治理科技重大专项(2017ZX07602-001) |
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| 摘 要： | 探讨了磷酸体系下不同因素对废旧锂电池正极材料中有价金属浸出效率的影响，结果表明：在浸出时间60min，反应温度60℃，磷酸浓度2mol/L，液固比20mL/g，还原剂(H2O2)体积分数为4%时，可得最佳浸出效果，Co、Li、Mn、Ni浸出效率分别可达96.3%、100%、98.8%和99.5%；浸出液添加相应比例金属离子，采用草酸共沉淀法制备前体材料(Ni1/3Co1/3Mn1/3)C2O4，并得到相应再生磷酸溶液。再生磷酸进行循环浸出实验，实验研究结果表明：循环浸出5次之后Li的浸出率仍可保持在90.1%，而Co、Mn和Ni的浸出率在75.0%以上。前体添加锂源Li2CO3煅烧合成Li(Ni1/3Co1/3Mn1/3)O2材料，考察了不同温度对Li(Ni1/3Co1/3Mn1/3)O2材料合成的影响，结果显示，当合成温度为800℃时，得到的材料性能最优良，初次放电容量可达136.4mA·h/g。在0.2C下经过50圈循环后容量保持率为97.2%。
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| 关 键 词： | 废旧锂电池 回收 浸出 共沉淀 三元正极材料 |
| 收稿时间： | 2018-09-03 |
Recovery of valuable metals from spent lithium ion battery and the resynthesis of Li(Ni1/3Co1/3Mn1/3)O2 materials |
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| Ling CAO,Yali LIU,Duozhi KANG,Jiazhu LI,Xiangping CHEN,Hongrui MA.Recovery of valuable metals from spent lithium ion battery and the resynthesis of Li(Ni1/3Co1/3Mn1/3)O2 materials[J].Chemical Industry and Engineering Progress,2019,38(5):2499-2505. |
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| Authors: | Ling CAO Yali LIU Duozhi KANG Jiazhu LI Xiangping CHEN Hongrui MA |
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| Affiliation: | 1. School of Environmental Science and Engineering, Shanxi University of Science & Technology, Xi’an 710021，Shanxi，China
2. School of Environmental Science and Engineering，Hunan University，Changsha 410082，Hunan，China |
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| Abstract: | In this study, phosphoric acid was employed as efficient leaching reagent for the leaching of different valuable metals from waste cathode materials of spent lithium ion batteries (LIBs). Based on the leaching results, about 96.3% Co, 100% Li, 98.8% Mn and 99.5% Ni can be dissolved in phosphoric acidic medium under the optimized leaching conditions of acid concentration-2 mol/L, reductant dosage- 4% H2O2, retention time- 60 min, reaction temperature- 60°C and pulp density- 20 mL/g. After adjusting the molar ration with addition of a certain proportion of metal ions to the leachate, the precursor materials of (Ni1/3Co1/3Mn1/3)C2O4 can be obtained by co-precipitation method (adding stoichiometric oxalic acid to leaching solution). And phosphoric acid can be simultaneously regenerated during the above precipitating reaction. According to the circulating leaching results, it can be concluded that the regenerated acid can be reused to as leaching reagent with relatively sound leaching efficiencies for valuable metals (90.1% for Li and over 75.0% for Co, Mn and Ni) after 5 cycles of leaching. Finally, cathode materials of Li(Ni1/3Co1/3Mn1/3)O2 can be reprepared by calcination the precursor materials of (Ni1/3Co1/3Mn1/3)C2O4 with pure Li2CO3 in appropriate molar ratio. Analysis results of electrochemical performances of the regenerated cathode material indicated that the initial discharge capacity of Li(Ni1/3Co1/3Mn1/3)O2 was 136.4 mA·h/g with a remained capacity rate of 97.2% after 50 cycles at 0.2 C under the optimized synthesis temperature of 800 oC. |
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| Keywords: | spent lithium ion batteries recovery leaching co-precipitation Li(Ni1/3Co1/3Mn1/3)O2 materials |
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