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Upcycling Real Waste Mixed Lithium-Ion Batteries by Simultaneous Production of rGO and Lithium-Manganese-Rich Cathode Material
ACS Sustainable Chemistry & Engineering ( IF 7.1 ) Pub Date : 2021-09-24 , DOI: 10.1021/acssuschemeng.1c04690 Pier Giorgio Schiavi 1 , Robertino Zanoni 1 , Mario Branchi 1 , Camilla Marcucci 1 , Corrado Zamparelli 1 , Pietro Altimari 1 , Maria Assunta Navarra 1 , Francesca Pagnanelli 1
ACS Sustainable Chemistry & Engineering ( IF 7.1 ) Pub Date : 2021-09-24 , DOI: 10.1021/acssuschemeng.1c04690 Pier Giorgio Schiavi 1 , Robertino Zanoni 1 , Mario Branchi 1 , Camilla Marcucci 1 , Corrado Zamparelli 1 , Pietro Altimari 1 , Maria Assunta Navarra 1 , Francesca Pagnanelli 1
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The direct synthesis of high-value products from end-of-life Li-ion batteries (LIBs), avoiding the complex and costly separation of the different elements, can be reached through a competitive recycling strategy. Here, we propose the simultaneous synthesis of reduced graphene oxide (rGO) and lithium-manganese-rich (Li1.2Mn0.55Ni0.15Co0.1O2 - LMR) cathode material from end-of-life LIBs. The electrode powder recovered after LIBs mechanical pretreatment was directly subjected to the Hummers’ method. This way, quantitative extraction of the target metals (Co, Ni, Mn) and oxidation of graphite to graphene oxide (GO) were simultaneously achieved, and a Mn-rich metal solution resulted after GO filtration, owing to the use of KMnO4 as an oxidizing agent. This solution, which would routinely constitute a heavy-metal liquid waste, was directly employed for the synthesis of Li1.2Mn0.55Ni0.15Co0.1O2 cathode material. XPS measurements demonstrate the presence in the synthesized LMR of Cu2+, SO42–, and SiO44– impurities, which were previously proposed as effective doping species and can thus explain the improved electrochemical performance of recovered LMR. The GO recovered by filtration was reduced to rGO by using ascorbic acid. To evaluate the role of graphite lithiation/delithiation during battery cycling on rGO production, the implemented synthesis procedure was replicated starting from commercial graphite and from the graphite recovered by a consolidated acidic–reductive leaching procedure for metals extraction. Raman and XPS analysis disclosed that cyclic lithiation/delithiation of graphite during battery life cycle facilitates the graphite exfoliation and thus significantly increases conversion to rGO.
中文翻译：
通过同时生产 rGO 和富锂锰正极材料来升级回收真正的废混合锂离子电池
可以通过竞争性回收策略直接合成来自报废锂离子电池 (LIB) 的高价值产品，避免复杂且昂贵的不同元素分离。在这里，我们建议同时合成还原氧化石墨烯 (rGO) 和富锂锰 (Li 1.2 Mn 0.55 Ni 0.15 Co 0.1 O 2- LMR) 来自报废 LIB 的阴极材料。LIBs机械预处理后回收的电极粉末直接进行悍马法。通过这种方式，同时实现了目标金属（Co、Ni、Mn）的定量提取和石墨氧化成氧化石墨烯（GO），并且由于使用 KMnO 4作为GO 过滤后得到富含 Mn 的金属溶液一种氧化剂。该溶液通常构成重金属废液，直接用于合成 Li 1.2 Mn 0.55 Ni 0.15 Co 0.1 O 2正极材料。XPS 测量表明合成的 LMR 中存在 Cu 2+ , SO4 2–和 SiO 4 4–杂质，这些杂质以前被认为是有效的掺杂物质，因此可以解释回收的 LMR 的电化学性能的改善。通过使用抗坏血酸将通过过滤回收的 GO 还原为 rGO。为了评估石墨锂化/脱锂在电池循环过程中对 rGO 生产的作用，从商业石墨和通过用于金属提取的综合酸还原浸出程序回收的石墨开始复制所实施的合成程序。拉曼和 XPS 分析表明，电池生命周期中石墨的循环锂化/脱锂促进了石墨剥离，从而显着增加了向 rGO 的转化。
更新日期：2021-10-04
中文翻译：
通过同时生产 rGO 和富锂锰正极材料来升级回收真正的废混合锂离子电池
可以通过竞争性回收策略直接合成来自报废锂离子电池 (LIB) 的高价值产品，避免复杂且昂贵的不同元素分离。在这里，我们建议同时合成还原氧化石墨烯 (rGO) 和富锂锰 (Li 1.2 Mn 0.55 Ni 0.15 Co 0.1 O 2- LMR) 来自报废 LIB 的阴极材料。LIBs机械预处理后回收的电极粉末直接进行悍马法。通过这种方式，同时实现了目标金属（Co、Ni、Mn）的定量提取和石墨氧化成氧化石墨烯（GO），并且由于使用 KMnO 4作为GO 过滤后得到富含 Mn 的金属溶液一种氧化剂。该溶液通常构成重金属废液，直接用于合成 Li 1.2 Mn 0.55 Ni 0.15 Co 0.1 O 2正极材料。XPS 测量表明合成的 LMR 中存在 Cu 2+ , SO4 2–和 SiO 4 4–杂质，这些杂质以前被认为是有效的掺杂物质，因此可以解释回收的 LMR 的电化学性能的改善。通过使用抗坏血酸将通过过滤回收的 GO 还原为 rGO。为了评估石墨锂化/脱锂在电池循环过程中对 rGO 生产的作用，从商业石墨和通过用于金属提取的综合酸还原浸出程序回收的石墨开始复制所实施的合成程序。拉曼和 XPS 分析表明，电池生命周期中石墨的循环锂化/脱锂促进了石墨剥离，从而显着增加了向 rGO 的转化。
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