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Energies 2022, 15, 1611 14 of 23 pith dosage of 0.3 g, an acetic acid dosage of 0.5 M, an ascorbic acid dosage of 0.2 M, and an ultrasonic power of 450 W. Nayaka et al. [56] used organic acids iminodiacetic acid and maleic acid to dissolve used LIB cathode materials, allowing the recovery of 100% Li and 97% Co. 4.2. Chlorination Technology Process To reduce the use of inorganic acid and reduce environmental pressure. Liu et al. [57] and Nshizirungu et al. [58,59] proposed the use of chlorination technology to recycle spent LIBs without additional inorganic acid. Liu et al. [57] used an autoclave to treat used polyvinyl chloride (PVC) and spent LIBs. The PVC is dechlorinated and substituted to produce hydrochloric acid, which was used to leach the spent LIB cathode material. Under optimal conditions, Co recovery exceeds 95% and Li recovery is close to 98%. The whole process has no release of any toxic chlorine-containing organic compounds and recycles spent LIBs and PVC, which has good environmental benefits. Nshizirungu et al. [58] investigated the leaching efficiency of spent chlorinated polyvinyl chloride (CPVC) under subcritical hydrothermal conditions for lithium and cobalt from spent LIBs. The leaching efficiency is improved by using spent CPVC as a source of hydrochloric acid. His team compared the leaching of valuable metals from PVC and CPVC from ternary lithium battery cathode materials in closed containers. They found that CPVC outperforms PVC in the extraction of valuable metals from NCM cathode materials due to the higher Cl content in CPVC [59]. 4.3. Ammoniation Technology Process Some researchers have used an ammonia leaching process to recover spent LIBs. Liu et al. [60] used a solution consisting of ammonia sulfite, ammonia, ammonia carbon- ate, and deionized water to leach the cathode active material of used ion batteries. Co and Ni are converted into complexes [Ni(NH3)n]2+, [Co(NH3)m]2+, Mn is converted into (NH4)2Mn(SO3)2·H2O and (NH4)2Mn(SO4)3 precipitates, and Li is leached as metal ions. The leaching rates of Co, Li, Ni, and Mn were 84.56%, 90.31%, 64.13%, and 4.53%, respec- tively. Li et al. [61] used an ammonia-sodium sulfite-ammonium chloride system to leach LCO. After 5 h of ball milling, the leaching time of LCO is shortened from 48 h to 4 h. The Li and Co leaching rates are increased from 69.86% and 70.80% to 88.86% and 98.22%, respectively. Chen et al. [62] proposed a heat treatment–ammonia leaching process for the recovery of valuable metals from cathodically active powder. A new Co3O4 phase appears in the cathodically active powder roasted at 550 ◦C, indicating the collapse of the layered structure of LCO. In the spinel structure of LiMn2O4, the valence of manganese increases to form Li4Mn5O12. Ammonia leaching is conducted in a (NH4)2SO4-(NH4)2SO3 solution using calcined cathode powder as the raw material. Under optimum conditions, the leaching rates of 98%, 81%, 92%, and 98% are obtained for nickel, cobalt, manganese, and lithium, respectively. The ammonia solution can be reused after the recovery of the valuable metals. Overall, this new recovery method has the advantages of high metal recovery efficiency, availability of equipment, and environmental friendliness, which can meet the requirements of green chemistry and has great potential for industrial production. 4.4. Solvent Extraction Keller et al. [63] used an ion exchange agent (di(2-ethylhexyl)phosphoric acid to selectively extract manganese from the leachate, with up to 94% extraction under optimum conditions. Vakylabad et al. [64] selectively extracted cobalt and nickel ions with xanthate complexes at room temperature and then washed with ammonia to obtain pure cobalt complexes. The complexes are converted to pure Co3S4 nanospheres by mild treatment (250 ◦C, 1 h) with 98% extraction of Co. Choubey et al. [65] used a sulfuric acid–hydrogen peroxide system to leach spent LIBs, adding NaOH, and precipitation to remove impurities, such as aluminum, iron, and copper. The filtered liquid is further diluted prior to solvent extraction. Versatic acid is added to LIX84-I to synergistically extract nickel from thePDF Image | Recycling of Lithium Batteries
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