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Energies 2022, 15, 1611 13 of 23 acid solution to leach lithium from the spent cathode material for approximately 2–4 h, used phosphoric acid solution to leach nickel and cobalt, and utilized sulfuric acid to leach manganese for 1–3 h. The recoveries of Li, Ni, Co, and Mn are close to 100%, 99.5%, 98.2%, and 100%, respectively. Compared with the traditional “one leaching, multi-step separation” process, this “multiple leaching, multistep separation” process can improve the leaching rate by selectively leaching the metals from spent LIBs. Almost all leaching processes require large amounts of acid and the reducer/oxidizer to achieve the desired leaching results, with acid concentrations ranging from 1.0 M to 3.0 M and high consumption of the reducer/oxidizer (e.g., 2–6 vol% hydrogen peroxide). Furthermore, large amounts of acid or the reductant/oxidizer are practically ineffective for accurate recovery of the target metal, and any unreacted acid or reductant/oxidizer ends up in the effluent and causes secondary contamination. It can be observed that dif- ferent additives are used to reduce or oxidize the corresponding spent cathode materials (e.g., reductants for LCO and oxidizers for LFP), resulting in a single batch of different types of cathode materials that cannot be recovered synergistically. Therefore, the balance be- tween simplifying the recycling process and saving chemical/energy consumption should be fully considered in order to pursue the efficient and green recycling of different metals from spent LIBs. Unlike conventional leaching processes that require reducing or oxidizing agents, the different redox properties of LCO and LFP are fully utilized to avoid the use of additional reducing or oxidizing agents. Moreover, due to the intrinsic motivation of the redox reactions of LCO and LFP and the transformation of transition metals, especially Fe, the amount of acid is presumed to be significantly reduced. The dissolved metals in the leachate can then be recovered efficiently and selectively as different products depending on the differences in solubility. Liu et al. [51] mixed the cathode material NCM with LFP in a certain ratio, added 100 mL of the sulfuric acid solution and heated it in a water bath, and added FePO4·2H2O after 0.5 h. The reductant-free recycling of spent ternary LIBs is achieved via the introduction of FePO4·2H2O crystals and spent LFP. Jiang et al. [52] prepared diluted H2SO4 in a 250 mL conical flask reactor, and then added a fixed molar ratio of LCO and LFP mixed cathode materials for leaching experiments. During the leaching process, the reactor was kept in a water bath with magnetic stirring equipment to control the reaction temperature at 50 ◦C and the stirring speed at 500 rpm. A reducing environment can be provided for the leaching of LCO from rapidly dissolved Fe(II) in LFP, and the leaching of Co can be improved by reducing Co(III) to Co(II). Under the optimized leaching conditions of sulfuric acid (0.5 M), leaching time (20 min), S/L ratio (30 g/L), and LCO/LFP (1 molar ratio), more than 99% of Li, Fe, and P and 92.4% of Co:1 can be extracted. Mixed acid systems are often used to leach spent LIBs. Chan et al. [53] recovered lithium, cobalt, nickel, and manganese from LiNi0.15Mn0.15Co0.70O2, the cathode material of used LIBs for electric vehicles. A systematic experimental and theoretical approach based on experimental design and response surface methodology is used to determine the optimum leaching agent and optimal operating conditions for HCl with H2SO4 + H2O2. The recovery of all four metals is 100% using a mixture of 1.0 M H2SO4 and 0.62 wt% H2O2 with an L/S ratio of 25.8 mL/g, a leaching temperature of 51 ◦C, and a leaching time of 60 min. At pH above 11, cobalt, nickel, and manganese are coprecipitated as Ni0.15Mn0.15Co0.70(OH)2, and lithium is precipitated as lithium carbonate. These precipitates are mixed and sintered to form a new cathode material for the manufacturing of batteries with high electrochemical performance. Xing et al. [54] achieved ultrafast leaching of spent cathode materials (97.72% leaching of lithium and 97.25% leaching of cobalt in 10 min at an S/L ratio of 10 g/L and a temperature of 363 K) in a 0.5 M hydrochloric acid and 0.5 M L-ascorbic acid system. Yan et al. [55] proposed a hybrid organic acid (acetic acid and ascorbic acid) and sugarcane bagasse pith as leaching and reducing agents for the recovery of valuable metals (Li, Ni, Co, Mn) from ternary LIB cathode materials using a comprehensive hydrometallurgy system with the assistance of ultrasonic waves. More than 98% of the valuable metals can be leached at a temperature of 50 ◦C, a time of 40 min, an S/L ratio of 20 g/L, a bagassePDF Image | Recycling of Lithium Batteries
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