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Construction of truncated-octahedral LiMn2O4 for battery-like electrochemical lithium recovery from brine

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Green Energy & Environment 2023年第4期8卷 1081-1090页

作者： Guolang Zhou Linlin Chen Xiaowei Li Guiling Luo Zhendong Yu Jingzhou Yin Lei Fan Yanhong Chao Lei Jiang Wenshuai Zhu School of Chemistry and Chemical Engineering Jiangsu UniversityZhenjiang212013JiangsuChina School of Pharmacy Jiangsu UniversityZhenjiang212013JiangsuChina School of Chemistry and Chemical Engineering Huaiyin Normal UniversityHuai'an223001JiangsuChina School of Chemistry and Chemical Engineering Yangzhou UniversityYangzhou225002JiangsuChina Jiangsu Topfine New Materials Science&Technology Co. Ltd.Zhenjiang212013JiangsuChina

The extraction of lithium from salt lakes or seawater has attracted worldwide attention because of the explosive growth of global demand for lithium products. The LiMn_(2)O_(4)-based electrochemical lithium recovery system is one of the strongest candidates for commercial application due to its high inserted capacity and low energy consumption. However, the surface orientation of LiMn_(2)O_(4)that facilitates Li diffusion happens to be prone to manganese dissolution making it a great challenge to obtain high lithium inserted capacity and long life simultaneously. Herein, we address this problem by designing a truncated octahedral LiMn_(2)O_(4)(Tr-oh LMO) in which the dominant(111) facets minimize Mn dissolution while a small portion of(100) facets facilitate the Li diffusion. Thus, this Tr-oh LMO-based electrochemical lithium recovery system shows excellent Li recovery performance with high inserted capacity(20.25 mg g^(-1)per cycle) in simulated brine. In addition, the dissolution rate of manganese per 30 cycles is only 0.44% and the capacity maintained 85% of the initial after 30 cycles. These promising findings accelerate the practical application of LiMn_(2)O_(4)in electrochemical lithium recovery.

关键词： LiMn_(2)O_(4) Crystal facets Electrochemistry lithium recovery Brine

recovery of lithium using H_(4)Mn_(3.5)Ti_(1.5)O_(12)/reduced graphene oxide/polyacrylamide composite hydrogel from brine by Ads-ESIX process

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Chinese Journal of Chemical Engineering 2022年第4期35卷 20-28页

作者： Jingsi Cui Huanxi Xu Yanfeng Ding Jingjing Tian Xu Zhang Guanping Jin Anhui Key Lab of Controllable Chemical Reaction&Material Chemical Engineering School of Chemistry and Chemical EngineeringHefei University of TechnologyHefei 230009China

Powdery Li^(+)-imprinted manganese oxides adsorbent was widely used to the recovery of Li^(+),but there are some difficulties,such as poor stability in acid solution,inconvenience of operation and separation.In this work,a useful hydrogel composite based H_(4)Mn_(3.5)Ti_(1.5)O_(12)/reduced graphene oxide/polyacrylamide(HMTO-rGO/PAM)was fabricated by thermal initiation method with promising stable,conductive and selective properties.The resulting materials were characterized by field emission scanning electron microscope,infrared absorption spectrum,X-ray diffraction,X-ray photoelectron spectroscopy and electrochemical techniques.The recovery of Li^(+)was investigated using HMTO-rGO/PAM from brine by a separated two-stage sorption statically and electrically switched ion exchange desorption process.The adsorption capacity of 51.5 mg·g^(-1)could be achieved with an initial Li^(+)concentration of 200 mg·L^(-1)in pH 10,at 45℃ for 12 h.Li^(+)ions could be quickly desorbed by cyclic voltammetry(CV)in pH 3,0.1 mol·L^(-1)HCl/NH;Cl accompanying the exchange of Li^(+)and H+(NH;)and the transfer of LMTO-rGO/PAM to HMTO-rGO/PAM.

关键词： lithium recovery Titanium doped lithium ion sieve Hydrogel Adsorption-electrically switched ion exchange(Ads-ESIX)

Aqueous electrochemical delithiation of cathode materials as a strategy to selectively recover lithium from waste lithium-ion batteries

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Journal of Energy Chemistry 2024年第1期88卷 144-153,I0004页

作者： Pier Giorgio Schiavi Andrea Giacomo Marrani Olga Russina Ludovica D’Annibale Francesco Amato Francesca Pagnanelli Pietro Altimari Department of Chemistry Sapienza University of RomePiazzale Aldo Moro n.500185 RomeItaly

lithium recovery from end-of-life Li-ion batteries(LIBs)through pyro-and hydrometallurgical recycling processes involves several refining stages,with high consumption of reagents and energy.A competitive technological alternative is the electrochemical oxidation of the cathode materials,whereby lithium can be deintercalated and transferred to an electrolyte solution without the aid of chemical extracting compounds.This article investigates the potential to selectively recover Li from LIB cathode materials by direct electrochemical extraction in aqueous solutions.The process allowed to recovering up to 98%of Li from high-purity commercial cathode materials(LiMn_(2)O_(4),LiCoO_(2),and Li Ni_(1/3)Mn_(1/3)Co_(1/3)O_(2))with a faradaic efficiency of 98%and negligible co-extraction of Co,Ni,and Mn.The process was then applied to recover Li from the real waste LIBs black mass obtained by the physical treatment of electric vehicle battery packs.This black mass contained graphite,conductive carbon,and metal impurities from current collectors and steel cases,which significantly influenced the evolution and performances of Li electrochemical extraction.Particularly,due to concomitant oxidation of impurities,lithium extraction yields and faradaic efficiencies were lower than those obtained with high-purity cathode materials.Copper oxidation was found to occur within the voltage range investigated,but it could not quantitatively explain the reduced Li extraction performances.In fact,a detailed investigation revealed that above 1.3 V vs.Ag/Ag Cl,conductive carbon can be oxidized,contributing to the decreased Li extraction.Based on the reported experimental results,guidelines were provided that quantitatively enable the extraction of Li from the black mass,while preventing the simultaneous oxidation of impurities and,consequently,reducing the energy consumption of the proposed Li recovery method.

关键词： lithium recovery lithium-ion batteries recycling Electrochemical lithium extraction lithium selective Extraction

recovery of lithium from High Mg/Li Ratio Brines by Solvent Extraction Process

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Recovery of Lithium from High Mg/Li Ratio Brines by Solvent ...

Na_(2)SO_(4)-NaCl binary eutectic salt roasting to enhance extraction of lithium from pyrometallurgical slag of spent lithium-ion batteries

中国化学会第六届全国热分析动力学与热动力学学术会议

作者： Shangqing Chen Xiaoping Yu Yafei Guo Tianlong Deng Tianjin Key Laboratory of Marine Resources and Chemistry College of Chemical Engineering and Materials ScienceTianjin Univ of Sci & Technol College of Chemistry and Materials Science Northwest University

lithium regarded as one of the strategic elements, plays a more and more important role in national economy and has been extensively applied in various industrial fields, especially lithium-ion battery [1-2]. Natural lithium resources mainly associate with granite pegmatite type solid ores, and the liquid resources such as salt lake brine, seawater and geothermal water, and due to the high recovery costs and limited availability of spodumene minerals, seeking a feasible and economical approach to extract lithium ion from lithium-containing brines is an inevitable tendency in future lithium industry. Liquid brine resources with high concentrations of lithium ion in salt lake and underground brine are widely distributed in the western four provinces named Qinghai, Tibet,Sichuan and Inner Mongolia, China [3].It is worthy of mentioning that the mass ratio of magnesium and lithium is fairly high in the Qaidam Basin, Qinghai Province, and magnesium presents a major challenge for lithium extraction for similar chemical properties of magnesium and lithium. Aiming at that, in our present work, a novel co-extraction system of TBP-KPF was used in the extraction for lithium from brines and the technological parameters for lithium extraction and back-extraction were optimized. As a result, the single-stage extraction efficiency and back-extraction efficiency were no less than85%.

关键词： Solvent Extraction Process Solvent Mechanism lithium recovery Salt lakes

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Chinese Journal of Chemical Engineering 2022年第1期35卷 294-300页

作者： Hui Dang Zhidong Chang Xue Wu Sihang Ma Yifei Zhan Na Li Wenbo Liu Wenjun Li Hualei Zhou Changyan Sun Department of Chemistry and Chemical Engineering School of Chemistry and Biological EngineeringUniversity of Science and Technology BeijingBeijing 100083China Institute of Biophysics Chinese Academy of SciencesBeijing 100101China

Effectively extracting lithium at a relatively low temperature from the slag produced by the pyrometallurgical treatment of spent lithium-ion batteries remains a great challenge,which limits the acquirement of lithium.Herein,we proposed a eutectic system to roast slag at a lower temperature based on sodium sulfate-sodium chloride(Na_(2)SO_(4)-NaCl)binary eutectic salts.The optimal roasting conditions are as follows:the slag was roasted at 750℃with a(SO_(4)^(2-)+Cl^(-))/Li+molar ratio of 5:1 for 120 min.Followed by aqueous leaching 5 min at room temperature with a water/roasted samples mass ratio of 30:1,it can get 97.07%lithium extraction efficiency.

关键词： Spent lithium-ion battery lithium recovery Silicate structure Binary eutectic salt roasting

Extraction of lithium from the simulated pyrometallurgical slag of spent lithium-ion batteries by binary eutectic molten carbonates

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International Journal of Minerals,Metallurgy and Materials 2022年第9期29卷 1715-1721页

作者： Hui Dang Zhidong Chang Hualei Zhou Sihang Ma Min Li Jialing Xiang Department of Chemistry and Chemical Engineering School of Chemistry and Biological EngineeringUniversity of Science and Technology BeijingBeijing 100083China

The effective and low-temperature extraction of lithium from the pyrometallurgical slag of spent lithium-ion batteries(LIBs)remains a great challenge.Herein,potassium carbonate/sodium carbonate(K_(2)CO_(3)/Na_(2)CO_(3)),which could form a eutectic molten salt system at 720℃,was used as a roasting agent to extract lithium from pyrometallurgical slag.lithium was successfully extracted from the slag by K_(2)CO_(3)/Na_(2)CO_(3) roasting followed by water leaching.Theoretical calculation results indicate that the lengths of Li-O bonds increase after K^(+)/Na^(+)adsorption,resulting in the easy release of Li^(+)from the LiAlSi_(2)O_(6) lattice after roasting with K_(2)CO_(3)/Na_(2)CO_(3).Thermogravimetry-differential scanning calorimetry results indicate that the eutectic phenomenon of K_(2)CO_(3) and Na_(2)CO_(3) could be observed at 720℃ and that the reaction of the slag and eutectic molten salts occurs at temperatures above 720℃.X-ray diffraction results suggest that Li^(+)in the slag is exchanged by K^(+)in K_(2)CO_(3) with the concurrent formation of KAlSiO_(4),while Na_(2)CO_(3) mainly functions as a fluxing agent.The lithium extraction efficiency can reach 93.87%under the optimal conditions of a roasting temperature of 740℃,roasting time of 30 min,leaching temperature of 50℃,leaching time of 40 min,and water/roasted sample mass ratio of 10:1.This work provides a new system for extracting lithium from the pyrometallurgical slag of spent LIBs.

关键词： spent lithium-ion battery lithium recovery silicate structure low roasting temperature binary eutectic carbonates roasting

Enhanced leaching of metals from spent lithium-ion batteries by catalytic carbothermic reduction

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稀有金属:英文版 2023年第8期42卷 2688-2699页

作者： Ying-Chao Zhang Wen-Hao Yu Sheng-Ming Xu Institute of Nuclear and New Energy Technology Tsinghua UniversityBeijing 100084China China National Petroleum&Chemical Planning Institute Beijing 100013China Key Laboratory of Advanced Reactor Engineering and Safety of Ministry of Education Tsinghua UniversityBeijing 100084China Beijing Key Lab of Fine Ceramics Tsinghua UniversityBeijing 100084China

Spent Li-ion battery(LIB)recycling has become a challenge with the rapidly developing electric vehicle(EV)industry.To address the problems of high cost and low recovery of Li in the recycling of spent LIBs using traditional hydrometallurgical processes,we developed an alkali metal catalytic carbothermic reduction method to recover spent LiNi_(x)Co_(y)Mn_(z)O_(2)(NCM).Using alkali metal catalysts,such as NaOH,significantly reduced the temperature required for carbothermic NCM material reduction and realized targeted control of the phase of the reduction product,where Li was first separated by prior water leaching,followed by Ni,Co,and Mn recycling by acid leaching.The optimized carbothermic reduction conditions were a reaction time of 3 h,temperature of 550℃,NaOH dosage of 15 wt%,and graphite dosage of 15 wt%.The Li leaching efficiency reached 78.5 wt%during water leaching.And during acid leaching,the Ni,Co and Mn leaching efficiencies were 99.8 wt%,99.7 wt%,and 99.5wt%,respectively.This study provides strong technical support for the development of LIB industry.

关键词： Spent lithium-ion battery(LIB) Battery recycling Leaching lithium recovery Alkali metal catalytic carbothermic reduction

Performance comparison of lithium fractionation from magnesium via continuous selective nanofiltration/electrodialysis

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中国化学工程学报:英文版 2023年第7期59卷 42-50页

作者： Yong Xu Qingbai Chen Yang Gao Jianyou Wang Huiqing Fan Fei Zhao Tianjin Key Laboratory of Environmental Technology for Complex Trans-Media Pollution College of Environmental Science and EngineeringNankai UniversityTianjin 300350China College of Chemical Engineering and Material Quanzhou Normal UniversityQuanzhou 362000China Center for Water and Ecology State Key Joint Laboratory of Environment Simulation and Pollution ControlSchool of EnvironmentTsinghua UniversityBeijing 100084China

Although selective nanofiltration(SNF)and selective electrodialysis(SED)have been widely adopted in the field of Mg^(2+)/Li^(+)separation,their differences have not been illustrated systematically.In this study,for the first time,SNF and SED processes in continuous mode were studied for Li+fractionation from the same brine with high Mg/Li ratios and their differences were discussed in detail.For a fair analysis of the two processes,typical factors were optimized.Specifically,the optimal operating pressure and feed flow rate for SNF were 2.4 MPa and 140 L·h^(-1),respectively,while the optimal cell-pair voltage and replenishment flow rate for SED were 1.0 V and 14 L·h^(-1),respectively.Although the Li^(+)fractionation capacity of the two processes were similar,the selectivity coefficient of SNF was 24.7% higher than that of SED and,thus,the Mg/Li ratio in purified stream of the former was 19.0% lower than that of the latter.Due to higher ion driving force,SED had clear advantages in recovery ratio and concentration effects.Meanwhile,the specific energy consumption of SED was 20.1% lower than that of SNF.This study provided a better understanding and guidance for the application and improvement of the two technologies.

关键词： High Mg/Li brine Purification Membrane Nanofiltration Electrodialysis lithium recovery

Negatively charged organic–inorganic hybrid silica nanofiltration membranes for lithium extraction

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Chinese Journal of Chemical Engineering 2020年第3期28卷 749-757页

作者： Xiaoxian Wu Haoyue Liu Yibin Wei Ying Fei Hong Qi State Key Laboratory of Material-Oriented Chemical Engineering Membrane Science and Technology Research CenterNanjing Tech UniversityNanjing 210009China

Effective extraction of lithium from high Mg2+/Li+ratio brine lakes is of great challenge.In this work,organic–inorganic hybrid silica nanofiltration(NF)membranes were prepared by dip-coating a 1,2-bis(triethoxysilyl)ethane(BTESE)-derived separation layer on tubular TiO2 support,for efficient separation of LiC l and MgCl2 salt solutions.We found that the membrane calcinated at 400°C(M1–400)could exhibit a narrow pore size distribution(0.63–1.66 nm)owing to the dehydroxylation and the thermal degradation of the organic bridge groups.All as-prepared membranes exhibited higher rejections to LiCl than to MgCl2,which was attributed to the negative charge of the membrane surfaces.The rejection for LiCl and MgCl2 followed the order:LiCl N MgCl2,revealing that Donnan exclusion effect dominated the salt rejection mechanism.In addition,the triplecoated membrane calcined at 400°C(M3–400)exhibited a permeability of about 9.5 L·m-2·h-1·bar-1 for LiCl or MgCl2 solutions,with rejections of 74.7%and 20.3%to LiCl and MgCl2,respectively,under the transmembrane pressure at 6 bar.Compared with the previously reported performance of NF membranes for Mg2+/Li+separation,the overall performance of M3–400 is highly competitive.Therefore,this work may provide new insight into designing robust silica-based ceramic NF membranes with negative charge for efficient lithium extraction from salt lakes.

关键词： Nanofiltration Membrane BTESE Water lithium resource lithium recovery