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Recovery of Li, Ni, Co and Mn from spent lithium-ion batteries assisted by organic acids: Process optimization and leaching mechanism

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International Journal of Minerals,Metallurgy and Materials 2024年第3期31卷 518-530页

作者： Liuyi Ren Bo Liu Shenxu Bao Wei Ding Yimin Zhang Xiaochuan Hou Chao Lin Bo Chen School of Resources and Environmental Engineering Wuhan University of TechnologyWuhan 430070China State Environmental Protection Key Laboratory of Mineral Metallurgical Resources Utilization and Pollution Control Wuhan University of Science and TechnologyWuhan 430081China Zhejiang New Era Zhongneng Recycling Technology Co. LtdShaoxing 312000China Shenzhen Water Planning&Design Institute Co. LtdShenzhen 518000China

The proper recycling of spent lithium-ion batteries(LIBs)can promote the recovery and utilization of valuable resources,while also negative environmental effects resulting from the presence of toxic and hazardous substances.In this study,a new environmentally friendly hydro-metallurgical process was proposed for leaching lithium(Li),nickel(Ni),cobalt(Co),and manganese(Mn)from spent LIBs using sulfuric acid with citric acid as a reductant.The effects of the concentration of sulfuric acid,the leaching temperature,the leaching time,the solid-liquid ratio,and the reducing agent dosage on the leaching behavior of the above elements were investigated.Key parameters were optimized using response surface methodology(RSM)to maximize the recovery of metals from spent LIBs.The maxim-um recovery efficiencies of Li,Ni,Co,and Mn can reach 99.08%,98.76%,98.33%,and 97.63%.under the optimized conditions(the sulfuric acid concentration was 1.16 mol/L,the citric acid dosage was 15wt%,the solid-liquid ratio was 40 g/L,and the temperature was 83℃ for 120 min),respectively.It was found that in the collaborative leaching process of sulfuric acid and citric acid,the citric acid initially provided strong reducing CO_(2)^(-),and the transition metal ions in the high state underwent a reduction reaction to produce transition metal ions in the low state.Additionally,citric acid can also act as a proton donor and chelate with lower-priced transition metal ions,thus speeding up the dissolution process.

关键词： spent lithium-ion batteries leaching response surface methodology sulfuric acid citric acid

Converting intercalation-type cathode in spent lithium-ion batteries into conversion-type cathode

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Nano Research 2024年第5期17卷 4602-4609页

作者： Dingding Zhu Yong Su Jingzhao Chen Xiangze Ou Xuedong Zhang Wen Xie Yuyan Zhou Yunna Guo Qiushi Dai Peng Jia Jitong Yan Lin Geng Baiyu Guo Liqiang Zhang Yongfu Tang Qiao Huang Jianyu Huang School of Materials Science and Engineering Xiangtan UniversityXiangtan 411105China Clean Nano Energy Center State Key Laboratory of Metastable Materials Science and TechnologyYanshan UniversityQinhuangdao 066000China

The widespread applications of lithium-ion batteries(LIBs)generate tons of spent LIBs.Therefore,recycling LIBs is of paramount importance in protecting the environment and saving the resources.Current commercialized LIBs mostly adopt layered oxides such as LiCoO_(2)(LCO)or LiNi_(x)Co_(y)Mn_(1-x-y)O_(2)(NMC)as the cathode materials.Converting the intercalation-type spent oxides into conversion-type cathodes(such as metal fluorides(MFs))offers a valid recycling strategy and provides substantially improved energy densities for LIBs.Herein,two typical Co-based cathodes,LCO and LiNi_(0.6)Co_(0.2)Mn_(0.2)O_(2)(NMC622),in spent LIBs were successfully converted to CoF_(2) and(Ni_(x)Co_(y)Mn_(z))F_(2) cathodes by a reduction and fluorination technique.The as converted CoF_(2) and(Ni_(x)Co_(y)Mn_(z))F_(2) delivered cell energy densities of 650 and 700 Wh/kg,respectively.Advanced atomic-level electron microscopy revealed that the used LCO and NMC622 were converted to highly phase pure Co metal and Ni_(0.6)Co_(0.2)Mn_(0.2) alloys in the used graphite-assisted reduction roasting,simultaneously producing the important product of Li_(2)CO_(3) using only environment friendly solvent.Our study provided a versatile strategy to convert the intercalation-type Co-based cathode in the spent LIBs into conversion-type MFs cathodes,which offers a new avenue to recycle the spent LIBs and substantially increase the energy densities of next generation LIBs.

关键词： spent lithium-ion batteries recycling energy densities conversion-type cathode

Progresses in Sustainable Recycling Technology of spent lithium-ion batteries

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Energy & Environmental Materials 2022年第4期5卷 1012-1036页

作者： Kaidi Du Edison Huixiang Ang Xinglong Wu Yichun Liu Faculty of Chemistry Northeast Normal UniversityChangchunJilin 130024China MOE Key Laboratory for UV Light-Emitting Materials and Technology Northeast Normal UniversityChangchunJilin 130024China Natural Sciences and Science Education National Institute of EducationNanyang Technological UniversitySingapore 637616Singapore

The number of lithium-ion batteries(LIBs)is steadily increasing in order to meet the ever-growing demand for sustainable energy and a high quality of life for humankind.At the same time,the resulting large number of LIB waste certainly poses safety hazards if it is not properly disposed of and will seriously harm the environment due to its inherent toxicity due to the use of toxic substances.Moreover,the consumption of many scarce precious metal resources is behind the mass production of batteries.In the light of severe environmental,resources,safety and recycling problems,recycling spent LIBs have become an essential urgently needed action to achieve sustainable social development.This review therefore critically analyses the value and the need for recycling of spent LIBs from a variety of resources and the environment.A range of existing technologies for recycling and reusing spent LIBs,such as pretreatment,pyrometallurgy,hydrometallurgy,and direct recycled methods,is subsequently summarized exclusively.In addition,the benefits and problems of the methods described above are analyzed in detail.It also introduces recycling progress of other LIB components,such as anodes,separators,and electrolytes,as well as the high-value cathode.Finally,the prospects for recycling LIBs are addressed in four ways(government,users,battery manufacturers,and recyclers).This review should contribute to the development of the recycling of used LIBs,particularly in support of industrialization and recycling processes.

关键词： cathode materials pretreatment recycling spent lithium-ion batteries valuable metals

Direct reuse of LiFePO_(4)cathode materials from spent lithium-ion batteries:Extracting Li from brine

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Chinese Chemical Letters 2023年第6期34卷 556-562页

作者： Miao Du Jin-Zhi Guo Shuo-Hang Zheng Yan Liu Jia-Lin Yang Kai-Yang Zhang Zhen-Yi Gu Xiao-Tong Wang Xing-Long Wu Faculty of Chemistry Northeast Normal UniversityChangchun 130024China MOE Key Laboratory for UV Light-Emitting Materials and Technology Northeast Normal UniversityChangchun 130024China

Due to the serious imbalance between demand and supply of lithium,lithium extraction from brine has become a research hotspot.With the demand for power lithium-ion batteries(LIBs)increased rapidly,a large number of spent LiFePO_(4)power batteries have been scrapped and entered the recycling stage.Herein,a novel and efficient strategy is proposed to extract lithium from brine by directly reusing spent LiFePO_(4)powder without any treatment.Various electrochemical test results show that spent LiFePO_(4)electrode has appropriate lithium capacity(14.62 mg_(Li)/g_(LiFePO_(4))),excellent separation performance(α_(Li-Na)=210.5)and low energy consumption(0.768 Wh/g_(Li))in electrochemical lithium extraction from simulated brine.This work not only provides a novel idea for lithium extraction from brine,but also develops an effective strategy for recycling spent LIBs.The concept of from waste to wealth is of great significance to the development of recycling the spent batteries.

关键词： spent lithium-ion batteries Reuse LiFePO_(4) lithium extraction Brine

Upcycling the spent graphite/LiCoO_(2) batteries for high-voltage graphite/LiCoPO_(4)-co-workable dual-ion batteries

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International Journal of Minerals,Metallurgy and Materials 2024年第7期31卷 1745-1751页

作者： Miao Du Hongyan Lü Kaidi Du Shuohang Zheng Xiaotong Wang Xiaotong Deng Ronghua Zeng Xinglong Wu Key Laboratory for UV Light-Emitting Materials and Technology of Ministry of Education Northeast Normal UniversityChangchun 130024China Faculty of Chemistry Northeast Normal UniversityChangchun 130024China School of Chemistry South China Normal UniversityGuangzhou 510006China

The worldwide proliferation of portable electronics has resulted in a dramatic increase in the number of spent lithium-ion batteries(LIBs).However,traditional recycling methods still have limitations because of such huge amounts of spent LIBs.Therefore,we proposed an ecofriendly and sustainable double recycling strategy to concurrently reuse the cathode(LiCoO_(2))and anode(graphite)materials of spent LIBs and recycled LiCoPO_(4)/graphite(RLCPG)in Li^(+)/PF^(-)_(6) co-de/intercalation dual-ion batteries.The recycle-derived dualion batteries of Li/RLCPG show impressive electrochemical performance,with an appropriate discharge capacity of 86.2 mAh·g^(-1) at25 mA·g^(-1) and 69%capacity retention after 400 cycles.Dual recycling of the cathode and anode from spent LIBs avoids wastage of resources and yields cathode materials with excellent performance,thereby offering an ecofriendly and sustainable way to design novel secondary batteries.

关键词： recycle lithium cobalt oxide lithium cobalt phosphate graphite dual-ion batteries spent lithium-ion batteries

Direct regeneration of LiNi_(0.5)Co_(0.2)Mn_(0.3)O_(2) cathode material from spent lithium-ion batteries

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Chinese Journal of Chemical Engineering 2021年第12期34卷 278-286页

作者： Xiaodong Tang Qiankun Guo Miaomiao Zhou Shengwen Zhong Faculty of Materials Melallurgy and Chemistry Jiangxi University of Science and TechnologyGanzhou 341000China

At present,metal ions from spent lithium-ion batteries are mostly recovered by the acid leaching procedure,which unavoidably introduces potential pollutants to the environment.Therefore,it is necessary to develop more direct and effective green recycling methods.In this research,a method for the direct regeneration of anode materials is reported,which includes the particles size reduction of recovered raw materials by jet milling and ball milling,followed by calcination at high temperature after lithium supplementation.The regenerated LiNi_(0.5)Co_(0.2)Mn_(0.3)O_(2) single-crystal cathode material possessed a relatively ideal layered structure and a complete surface morphology when the lithium content was n(Ni+Co+Mn):n(Li)=1:1.10 at a sintering temperature of 920 0 C,and a sintering time of 12 h.The first discharge specific capacity was 154.87 mA·h·g^(-1) between 2.75 V and 4.2 V,with a capacity retention rate of 90% after 100 cycles.

关键词： spent lithium-ion batteries LiNi_(0.5)Co_(0.2)Mn_(0.3)O_(2)cathode material Direct regeneration

Surplus energy utilization of spent lithium-ion batteries for high-profit organolithiums

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Carbon Energy 2023年第6期5卷 11-20页

作者： Jian Lu Yun Zhao Yuqiong Kang Chenglei Li Yawen Liu Liguang Wang Hao Du Meicen Fan Yunan Zhou John Wozny Tao Li Naser Tavajohi Feiyu Kang Baohua Li Shenzhen Key Laboratory on Power Battery Safety Tsinghua Shenzhen International Graduate School(SIGS)Shenzhen Geim Graphene CenterShenzhenChina College of Chemical and Biological Engineering Zhejiang UniversityHangzhouChina Institute of Zhejiang University QuzhouChina Department of Chemistry and Biochemistry Northern Illinois UniversityDeKalbIllinoisUSA Department of Chemistry UmeåUniversityUmeåSweden

It is challenging to efficiently and economically recycle many lithium-ion batteries(LIBs)because of the low valuation of commodity metals and materials,such as LiFePO_(4).There are millions of tons of spent LIBs where the barrier to recycling is economical,and to make recycling more feasible,it is required that the value of the processed recycled material exceeds the value of raw commodity materials.The presented research illustrates improved profitability and economics for recycling spent LIBs by utilizing the surplus energy in lithiated graphite to drive the preparation of organolithiums to add value to the recycled lithium materials.This study methodology demonstrates that the surplus energy of lithiated graphite obtained from spent LIBs can be utilized to prepare high-value organolithiums,thereby significantly improving the economic profitability of LIB recycling.Organolithiums(R-O-Li and R-Li)were prepared using alkyl alcohol(R-OH)and alkyl bromide(R-Br)as substrates,where R includes varying hindered alkyl hydrocarbons.The organolithiums extracted from per kilogram of recycled LIBs can increase the economic value between$29.5 and$226.5 kg^(−1) cell.The value of the organolithiums is at least 5.4 times the total theoretical value of spent materials,improving the profitability of recycling LIBs over traditional pyrometallurgical($0.86 kg^(−1) cell),hydrometallurgical($1.00 kg^(−1) cell),and physical direct recycling methods($5.40 kg^(−1) cell).

关键词： lithiated graphite lithium-ion batteries recycling regeneration spent lithium-ion batteries

Hydrometallurgical recycling of valuable metals from spent lithium-ion batteries by reductive leaching with stannous chloride

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International Journal of Minerals,Metallurgy and Materials 2021年第6期28卷 991-1000页

作者： Liu-ye Sun Bo-rui Liu Tong Wu Guan-ge Wang Qing Huang Yue-feng Su Feng Wu School of Materials Science and Engineering Beijing Institute TechnologyBeijing 100081China

The reductant is a critical factor in the hydrometallurgical recycling of valuable metals from spent lithium-ion batteries(LIBs).There is limited information regarding the use of SnCl_(2) as a reductant with organic acid(maleic acid)for recovering valuable metals from spent Li-CoO_(2) material.In this study,the leaching efficiencies of Li and Co with 1 mol·L^(−1) of maleic acid and 0.3 mol·L^(−1) of SnCl_(2) were found to be 98.67%and 97.5%,respectively,at 60°C and a reaction time of 40 min.We investigated the kinetics and thermodynamics of the leaching process in this study to better understand the mechanism of the leaching process.Based on a comparison with H_(2)O_(2) with respect to leaching efficiency,the optimal leaching parameters,and the activation energy,we determined that it is feasible to replace H_(2)O_(2) with SnCl_(2) as a leaching reductant in the leaching process.In addition,when SnCl_(2) is used in the acid-leaching process,Sn residue in the leachate may have a positive effect on the re-synthesis of nickel-rich cathode materials.Therefore,the results of this study provide a potential direction for the selection of reductants in the hydrometallurgical recovery of valuable metals from spent LIBs.

关键词： spent lithium-ion batteries recovery maleic acid reductant stannous chloride

Technology for recycling and regenerating graphite from spent lithium-ion batteries

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Chinese Journal of Chemical Engineering 2021年第11期34卷 37-50页

作者： Chenxing Yi Lijie Zhou Xiqing Wu Wei Sun Longsheng Yi Yue Yang School of Minerals Processing and Bioengineering Central South UniversityChangsha 410083China Beijing Battery Green Resources Technology Co. LtdBeijing 100081China

With the annual increase in the amount of lithium-ion batteries(LIBs),the development of spent LIBs recycling technology has gradually attracted attention.Graphite is one of the most critical materials for LIBs,which is listed as a key energy source by many developed countries.However,it was neglected in spent LIBs recycling,leading to pollution of the environment and waste of resources.In this paper,the latest research progress for recycling of graphite from spent LIBs was summarized.Especially,the processes of pretreatment,graphite enrichment and purification,and materials regeneration for graphite recovery are introduced in details.Finally,the problems and opportunities of graphite recycling are raised.

关键词： spent lithium-ion batteries Graphite Anode materials Recycle