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Energies 2022, 15, 1611 12 of 23 76% with 2 M sulfuric acid. Introducing hydrogen peroxide as a reducing agent, leaching at 80 ◦C and a 50 g/L S/L ratio for 60 min can recover more than 99% of cobalt and lithium. Cheng et al. [39] used sulfuric acid as a leaching agent and hydrogen peroxide as a reducing agent to leach the cathode material powder and extracted Co2+ using Cyanex272 with a 99% extraction rate. Xin et al. [23] leached the treated active cathode material in a hydrogen peroxide sulfate system and prepared transition metal-doped α-MnO2 and β-MnO2 by deep oxidation with potassium permanganate and ozone, respectively, with the recovery of manganese up to 100%. Jiang et al. [40] used an ultrasonic-assisted sulfuric acid–hydrogen peroxide system to leach valuable metals from used lithium batteries with 94.63% for cobalt and 98.62% for lithium. The reactions involved are as follows: 2LiCoO2 + 3H2SO4 + H2O2→Li2SO4 + 2CoSO4 + 4H2O + O2 (10) 2LiMnO2 + 3H2SO4 + H2O2→Li2SO4 + 2MnSO4 + 4H2O + O2 (11) Castillo et al. [41] and Lee et al. [42,43] used HNO3 for the leaching of LMO. Castillo et al. [41] used 2 mol/L of nitric acid to leach LIBs, separating all the lithium and manganese from the other metals, allowing 100% of the lithium to be leached. The addition of NaOH solution to reach pH 10 selectively precipitates manganese hydroxide. Lee et al. [42,43] used HNO3 alone for the leaching of LiCoO2 with 40% leaching of Co and 75% of Li. The addition of 1.7 vol.% H2O2 as a reducing agent and leaching at 75 ◦C for 1 h increases the leaching of Co and Li to 95%. Because Co3+ is re-reduced to Co2+, it is easier to dissolve. The reactions involved are as follows: LiMn2O4 + 10HNO3→2Mn(NO3)2 + LiNO3 + 5NO2 + 5H2O + 2O2 (12) Meng et al. [44] used glucose as the reducing agent and phosphoric acid as the leaching agent to recover Co and Li from the LCO collected from spent LIBs, with leaching rates of approximately 98% and 100% for Co and Li. During the leaching process, glucose is sequentially oxidized and decomposed to form monocarboxylic acids, including gluconic acid, tartaric acid, oxalic acid, and formic acid. The leaching of spent LIBs using inorganic strong acids generates large amounts of spent liquids, as well as some harmful gases such as chlorine gas (Cl2) and sulfur trioxide (SO3), which can pollute the environment. These spent liquids are difficult in terms of being treated harmlessly. Researchers have tried to treat spent LIBs using organic acids, such as malic acid, citric acid, oxalic acid, malic acid, and ascorbic acid. Zhang et al. [45] used grape seeds as a reducing agent for the leaching of spent LCO materials. Under the optimized conditions of 0.6 g/g grape seeds, 1.5 mol/L malic acid, 180 min, 80 ◦C, and a slurry density of 20 g/L, approximately 92% Co and 99% Li can be leached. Zeba et al. [46] used formic acid to recover manganese, nickel, and lithium from spent LIBs by using it as a leaching and reducing agent for nickel and manganese. The addition of H2O2 in the leaching solution rapidly dissolves insoluble cobalt. Manganese, nickel, and cobalt are recovered by extraction. Lithium (99.5 wt%) is recovered as formate, a high-value-added by-product, by careful evaporation of the final aqueous solution, thereby reducing the final spent generation. Lei et al. [47] used 0.5 M ascorbic acid at 125 ◦C with an S/L ratio of 10 g/L. The closed-vessel microwave system can leach 100% of Li, Co, and Mn from the spent cathode material. Oxalic acid is used to recover Co and Mn, generating oxalate precipitates. Esmaeili et al. [48] investigated the leaching of valuable metals from spent LIBs using ultrasound-assisted bioacid. Organic acids from lemon juice and hydrogen peroxide are used as leaching agents. The three influencing factors of the S/L ratio, lemon juice content, and H2O2 volume fraction are optimized through response surface analysis. The recoveries of Li, Co, and Ni are 100%, 96%, and 96%, respectively, when the S/L in the leachate was 0.98% (w/v), the lemon juice was 57.8% (v/v), and the H2O2 was 8.07% (v/v). Pindar et al. [49] used citric acid to leach the spent LIB cathode material with microwave assistance, greatly improving the dissolution rate of manganese in citric acid (from 9% to 94%), and lithium is recovered as Li2CO3. Tao et al. [50] first used 0.5–2 mol/L oxalicPDF Image | Recycling of Lithium Batteries
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