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iScience ll OPEN ACCESS Ar ticle Extraction of Lithium from Single-Crystalline Lithium Manganese Oxide Nanotubes Using Ammonium Peroxodisulfate Kaiyuan Shi,1,6,* Mingwu Luo,1 Jie Ying,2 Shunying Zhen,3 Zhenyu Xing,3,* and Ri Chen4,5 SUMMARY In this work, a spinel single-crystalline Li1.1Mn1.9O4 has been successfully synthe- sized using b-MnO2 nanotubes as the self-sacrifice template. The tubular morphology was retained through solid-state reactions, attributed to a minimal structural reorganization from tetragonal b-MnO2 to spinel Li1.1Mn1.9O4. The ma- terials were investigated as sorbents for lithium recovery from LiCl solutions, re- cycled using H2SO4 and (NH4)2S2O8. Li1.1Mn1.9O4 nanotubes exhibited favorable lithium extraction behavior due to tubular nanostructure, single-crystalline na- ture, and high crystallinity. (NH4)2S2O8 eluent ensures the structural stability of Li1.1Mn1.9O4 nanotube, registering a Li+ adsorption capacity of 39.21 mg g1 ($89.73% of the theoretical capacity) with only 0.08% manganese dissolution af- ter eight adsorption/desorption cycles, compared to that of 1.21% for H2SO4. It reveals the degradation of sorbent involves with the volume change, Mn reduc- tion, and Li/Mn ratio depletion. New strategies, based on nanotube adsorbent and (NH4)2S2O8 eluent, can extract lithium ions at satisfactorily high degrees while effectively minimizing manganese dissolution. INTRODUCTION The demand for lithium production worldwide has significantly increased in recent years due to the growth of the rechargeable lithium-ion battery market (Li et al., 2018). The sources of lithium are mainly in forms of water resources and ore bodies, such as spodumene, lepidolite, and petalite ores. The grown interest in lithium extraction derived from water resources is attributed to its low cost, natural abundance, and envi- ronmental friendliness (Battistel et al., 2020). Great efforts have been devoted to selective recovery of Li+ from water resources, including precipitation (Biswal et al., 2018), evaporative crystallization (Ooi et al., 2017), solvent extraction (Zhang et al., 2020), electrochemical adsorption (Battistel et al., 2020; Du et al., 2016), and ion exchange adsorption (Lin et al., 2019; Wang et al., 2020). The precipitation and evaporative + Lithium-ion sieve technology represents a cost-effective green method, based on functional adsorbents capturing of lithium ions from the brines (Paranthaman et al., 2017; Tang et al., 2020; Xu et al., 2016). Among various materials, spinel-type lithium manganese oxides Lix ðMnIII MnIV ÞO4 or LMOs) attract more attention yz from academic researchers and, more recently, from the industry due to feasible production, excellent selectivity, and high lithium uptake capacity (Liu et al., 2019; Safari et al., 2020). A lithium-ion sieve is derived from the extraction of Li+ from spinel-type LMOs (Luo et al., 2016). In general, mild acids are employed for an ion exchange between Li+ and H+, yielded to a hydrogen manganese oxide (HMO) (Choi et al., 2020; Hong et al., 2018; Zhang et al., 2019). However, the promise of LMOs has been hampered by its low chem- ical stability in the acidic environment (Wang et al., 2020; Wei et al., 2020). It is known that the MnIII in the LMOs can undergo a disproportionation transaction and turn into MnII and MnIV upon delithiation (Hayashi 1School of Materials Science and Engineering, Sun Yat-Sen University, Guangzhou, Guangdong 510275, China 2School of Chemical Engineering and Technology, Sun Yat-Sen University, Zhuhai, Guangdong 519082, China 3School of Chemistry, South China Normal University, Guangzhou, Guangdong 510006, China 4School of Electromechanical Engineering, Guangdong Polytechnic Normal University, Guangzhou, Guangdong 510635, China 5School of Electromechanical Engineering, Guangdong University of Technology, Guangzhou, Guangdong 510006, China 6Lead Contact *Correspondence: shiky7@mail.sysu.edu.cn (K.S.), xingzhenyu@m.scnu.edu.cn (Z.X.) https://doi.org/10.1016/j.isci. 2020.101768 crystallization are limited for processing high concentrated Li tion process that entails tedious treatment and large energy consumption. Although the solvent extraction indicates high selectivity of lithium, the use of organic solvents generates significant environmental con- cerns. Electrochemical adsorption, based on the redox reactions of electrodes, has attracted increasing attention (Pasta et al., 2012; Tro ́ coli et al., 2017). In this technique, the materials are regenerated using an external power source, which avoided the use of chemicals for adsorbent regeneration; however, the method exhibits irreversible electrochemical reactions and limited lithium productions due to low energy efficiency (Pasta et al., 2012). solutions, which requires a pre-concentra- iScience 23, 101768, November 20, 2020 a 2020 The Author(s). 1 This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).PDF Image | Extraction of Lithium from Single-Crystalline Lithium
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