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Article(id=1241081040039629689, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241081025531540408, articleNumber=null, orderNo=null, doi=10.3969/j.issn.0253-6099.2024.04.023, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1716739200000, receivedDateStr=2024-05-27, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773826378115, onlineDateStr=2026-03-18, pubDate=1722441600000, pubDateStr=2024-08-01, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773826378115, onlineIssueDateStr=2026-03-18, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773826378115, creator=13701087609, updateTime=1773826378115, updator=13701087609, issue=Issue{id=1241081025531540408, tenantId=1146029695717560320, journalId=1235980550691926019, year='2024', volume='44', issue='4', pageStart='1', pageEnd='258', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773826374657, creator=13701087609, updateTime=1773827517159, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1241085817590960730, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241081025531540408, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1241085817590960731, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241081025531540408, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=120, endPage=125, ext={EN=ArticleExt(id=1241081041339864059, articleId=1241081040039629689, tenantId=1146029695717560320, journalId=1235980550691926019, language=EN, title=Research Progress in Comprehensive Recycling Graphite Anode in Spent Lithium-Ion Batteries, columnId=1241081026567533498, journalTitle=Mining and Metallurgical Engineering, columnName=SPECIAL ISSUE: BATTERY MATERIALS, runingTitle=null, highlight=null, articleAbstract=

A review of comprehensive recycling technologies for graphite anodes in spent lithium-ion batteries is presented, including hydrometallurgical process, a combination of pyrometallurgical and hydrometallurgical process, as well as mechanical recycling. And then, an in-depth analysis of advantages and disadvantages of each technology is also presented. It is particularly pointed out that there are various recycling technologies, but the development of an efficient and environmentally-friendly closed-circuit recycling process still faces challenges. The recycling approaches of graphite anodes in spent lithium-ion batteries are discussed in details, such as usage as anodes of rechargeable batteries, or for preparation of graphene. The research direction in the future is also forecasted aiming to provide theoretical and technical support for reutilization of graphite anodes in spent lithium-ion batteries with high-value added. It is suggested that research should focus on developing a simple, efficient and clean closed-circuit recycling processes to improve the recovery rate and purity of graphite anode materials while reducing environmental pollution. The research hotspots in the future should include lattice reconstruction and repairing technologies for graphite anode materials, as well as exploration of new applications of graphite anode materials in the fields of energy storage materials, catalysts, adsorbents among others.

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综述了废锂离子电池石墨负极的综合回收利用技术，包括湿法、火法-湿法联合以及物理法回收工艺，并对各工艺的优缺点进行了深入分析。特别指出，尽管目前存在多种回收技术，但高效、环保的闭环回收工艺仍面临挑战。探讨了废石墨负极材料的资源化再利用途径，如作为二次电池负极材料、制备石墨烯等，并对未来研究方向进行了展望，旨在为废锂离子电池石墨负极的高值化利用提供理论支持和技术支持。建议未来的研究关注开发简单、高效、清洁的闭环回收工艺，提高石墨负极材料的回收率和纯度，同时减少环境污染。未来研究的热点应包括石墨负极材料的晶格重构修复技术，以及探索石墨负极材料在储能材料、催化剂、吸附剂等领域的新应用。

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仲奇凡（1990—），男，山东济宁人，教授，博士研究生导师，主要从事碳基/硅基电极材料的制备与仿真模拟、铝电解与炭素、冶金固废的无害化处理和高值化利用和半导体硅基材料高纯化制备等方面研究。E-mail：，
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赵朝显（1999—），男，贵州毕节人，硕士研究生，主要从事锂离子电池废石墨负极综合回收利用研究和大型预焙阳极铝电解槽多物理场耦合数值仿真研究。E-mail：

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赵朝显（1999—），男，贵州毕节人，硕士研究生，主要从事锂离子电池废石墨负极综合回收利用研究和大型预焙阳极铝电解槽多物理场耦合数值仿真研究。E-mail：

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赵朝显（1999—），男，贵州毕节人，硕士研究生，主要从事锂离子电池废石墨负极综合回收利用研究和大型预焙阳极铝电解槽多物理场耦合数值仿真研究。E-mail：

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废锂离子电池石墨负极综合回收利用研究进展
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赵朝显 1 , 肖劲 1, 2 , 诸向东 1 , 仲奇凡 1, 2
矿冶工程杂志 | 电池材料专题 2024,44(4): 120-125
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矿冶工程杂志 | 电池材料专题 2024, 44(4): 120-125
废锂离子电池石墨负极综合回收利用研究进展
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赵朝显1 , 肖劲1, 2, 诸向东1, 仲奇凡1, 2
作者信息
  • 1.中南大学 冶金与环境学院，湖南 长沙 410083
  • 2.中南大学 低碳有色冶金国家工程研究中心，湖南 长沙 410083

    • 赵朝显（1999—），男，贵州毕节人，硕士研究生，主要从事锂离子电池废石墨负极综合回收利用研究和大型预焙阳极铝电解槽多物理场耦合数值仿真研究。E-mail：

通讯作者:

仲奇凡（1990—），男，山东济宁人，教授，博士研究生导师，主要从事碳基/硅基电极材料的制备与仿真模拟、铝电解与炭素、冶金固废的无害化处理和高值化利用和半导体硅基材料高纯化制备等方面研究。E-mail：，
Research Progress in Comprehensive Recycling Graphite Anode in Spent Lithium-Ion Batteries
Chaoxian ZHAO1 , Jin XIAO1, 2, Xiangdong ZHU1, Qifan ZHONG1, 2
Affiliations
  • 1.School of Metallurgy and Environment, Central South University, Changsha 410083, Hunan, China
  • 2.National Engineering Research Center for Low-Carbon Nonferrous Metallurgy, Central South University, Changsha 410083, Hunan, China
出版时间: 2024-08-01 doi: 10.3969/j.issn.0253-6099.2024.04.023
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摘要
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综述了废锂离子电池石墨负极的综合回收利用技术，包括湿法、火法-湿法联合以及物理法回收工艺，并对各工艺的优缺点进行了深入分析。特别指出，尽管目前存在多种回收技术，但高效、环保的闭环回收工艺仍面临挑战。探讨了废石墨负极材料的资源化再利用途径，如作为二次电池负极材料、制备石墨烯等，并对未来研究方向进行了展望，旨在为废锂离子电池石墨负极的高值化利用提供理论支持和技术支持。建议未来的研究关注开发简单、高效、清洁的闭环回收工艺，提高石墨负极材料的回收率和纯度，同时减少环境污染。未来研究的热点应包括石墨负极材料的晶格重构修复技术，以及探索石墨负极材料在储能材料、催化剂、吸附剂等领域的新应用。

废锂离子电池  /  石墨负极  /  综合回收  /  资源化再利用  /  环境效益

A review of comprehensive recycling technologies for graphite anodes in spent lithium-ion batteries is presented, including hydrometallurgical process, a combination of pyrometallurgical and hydrometallurgical process, as well as mechanical recycling. And then, an in-depth analysis of advantages and disadvantages of each technology is also presented. It is particularly pointed out that there are various recycling technologies, but the development of an efficient and environmentally-friendly closed-circuit recycling process still faces challenges. The recycling approaches of graphite anodes in spent lithium-ion batteries are discussed in details, such as usage as anodes of rechargeable batteries, or for preparation of graphene. The research direction in the future is also forecasted aiming to provide theoretical and technical support for reutilization of graphite anodes in spent lithium-ion batteries with high-value added. It is suggested that research should focus on developing a simple, efficient and clean closed-circuit recycling processes to improve the recovery rate and purity of graphite anode materials while reducing environmental pollution. The research hotspots in the future should include lattice reconstruction and repairing technologies for graphite anode materials, as well as exploration of new applications of graphite anode materials in the fields of energy storage materials, catalysts, adsorbents among others.

spent lithium-ion battery  /  graphite anode  /  comprehensive recycling  /  resources reutilization  /  environmental benefit
赵朝显, 肖劲, 诸向东, 仲奇凡. 废锂离子电池石墨负极综合回收利用研究进展. 矿冶工程杂志, 2024 , 44 (4) : 120 -125 . DOI: 10.3969/j.issn.0253-6099.2024.04.023
Chaoxian ZHAO, Jin XIAO, Xiangdong ZHU, Qifan ZHONG. Research Progress in Comprehensive Recycling Graphite Anode in Spent Lithium-Ion Batteries[J]. Mining and Metallurgical Engineering, 2024 , 44 (4) : 120 -125 . DOI: 10.3969/j.issn.0253-6099.2024.04.023
正文
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化石能源的大量使用带来了资源枯竭、环境污染和全球气候变暖等一系列严重问题[1-3]。在此背景下，为了实现“碳达峰和碳中和”的目标，大力发展可再生清洁能源对世界能源体系的脱碳和转型具有至关重要的作用[4]。为了最大限度地利用可再生清洁能源，开发清洁、安全和可持续的能源存储和转换技术至关重要。
锂离子电池具有高能量密度、高充电效率和良好循环性能等特点[5-6]，被广泛应用于便携式电子设备和电动汽车。石墨负极材料因导电性好、结晶度高、锂嵌入电位低、膨胀系数小等特点[7]，已成为目前商用锂离子电池负极材料的主流，占负极总市场的份额超过94%[8]。随着新能源汽车产量爆发式增长[2]，我国石墨资源供需矛盾日渐凸显，预计到2025年，全球锂离子电池所需石墨材料将达到150万吨[9]。同时，随着锂离子电池退役潮的到来，我国每年产生的退役锂离子电池数量正在呈指数级增长，据EVTank数据统计，预计到2030年中国锂离子电池回收量将达到602.8万吨，市场规模将突破千亿元，但到目前为止，全行业的名义产能利用率仅16.4%[10]。
目前国内外对于废锂离子电池回收主要集中于回收高价值的镍、钴、锰、锂等有价金属元素，而对石墨负极材料的回收和再利用却很少关注，其产业化高效清洁回收技术尤为欠缺[1]。石墨负极材料在整个锂离子电池组中的质量占比达到10%以上，其中绝大部分是石墨化程度很高的石墨资源，废石墨负极材料的不当处置极大浪费了宝贵的石墨资源，还极易产生严重的环境问题[11]。因此，通过高效回收循环再利用废锂离子电池中的负极石墨不仅可以有效缓解石墨资源严重短缺问题、降低能源行业环境保护压力，还可以减少我国对有限战略资源的依赖，保障关键资源供给能力[12]。
我国废锂离子电池的处理与回收工艺主要以湿法冶金为主，采用硫酸还原浸出，得到的浸出渣（废石墨负极）中残留的主要杂质元素为微量的镍、钴、锰、铝、铁和锂等有价组分。目前对于这部分废石墨负极的处理与回收工艺主要包括湿法、火法-湿法联合、物理法及其他回收法。本文针对这几种废锂离子电池石墨负极的处理方法进行综述，分析各方法的优缺点。
1 湿法回收工艺
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湿法冶金提纯废石墨负极（SGA）是利用无机酸、碱性溶液或其他溶液将石墨中的有价成分浸出到溶液中，该工艺可以在回收有价金属的同时回收高纯度石墨产品[13]。文献[14]采用3 mol/L的HCl和H2O2溶液对SGA进行还原浸出，在浸出温度80 ℃、液固比50∶1和浸出时间80 min的最佳条件下，可浸出99.4%的Li，同时可回收利用晶体结构更好的石墨材料。文献[15]通过SGA的物相组成和结构表征，发现SGA仍保持着石墨的原始结构特征，导致电池失效的主要原因是石墨表面包含大量电解质分解产物及SEI膜的过度形成，因此提出用简单的水处理来纯化SGA，打开锂离子的传输通道，恢复石墨的电化学性能。在0.1C电流密度下循环100圈后，再生比容量仍保持在345 mAh/g左右，可与商业石墨（347 mAh/g）相媲美（见图1）。
文献[16]将SGA经过两段简单的热处理后，用1.5 mol/L的HCl浸出60 min，可浸出SGA中几乎所有的锂、铜和铝，浸出液通过先调节pH值至7后再调节pH值至9，可将浸出液中99.9%的铝和铜除去，随后加入Na2CO3可以制备高纯度Li2CO3（>99%），同时，再生石墨表现出了优异的循环性能。文献[17]将SGA通过超声处理后，分离铜箔与石墨，并采用绿色溶剂水作为浸出剂，在最佳条件下，可浸出99.9%的Li，同时将浸出液中的Li+以Li2CO3形式回收，纯度为99.4%，通过简单的乙酸和水溶液作为浸出剂，分别回收了正极材料和负极材料。
2 火法-湿法联合回收工艺
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火法工艺是指将预处理后的SGA进行高温焙烧，在去除其中有机物的同时还能使有价金属及其氧化物发生氧化还原反应得到合金和炉渣，是处理废电池的常用方法之一。在当前“双碳”目标背景下，在废锂离子电池回收技术中，火法工艺通常结合湿法工艺形成火法-湿法联合回收工艺，典型的SGA的热处理技术包括原位处理、石墨纯化以及晶格或缺陷的高温修复[18]，如图2所示。
2.1 石墨的活化纯化
文献[19]通过简单的高温焙烧和筛分工艺从废锂离子电池中成功地再生石墨负极，在氮气氛围下1 673 K焙烧4 h，使负极集流体中的铜箔变成球形颗粒，并根据铜与石墨颗粒的粒度分布差异，用简单的超声波振动和筛分将铜与石墨颗粒彼此分离，回收得到的再生石墨纯度高达99.5%，达到了锂离子电池对石墨的标准要求。文献[20]开发了一种机械分离和热处理工艺，分别从废锂离子电池中回收有价金属和石墨产品，并研究了热处理温度和时间对石墨回收的影响，结果表明，在450 ℃下焙烧15 min，能除去混合电极材料表面大部分的有机物，焙烧还恢复了LiCoO2和石墨的润湿性，通过浮选工艺可以有效分离LiCoO2和石墨。文献[21]提出了一种以氟化钠为助剂的改进硫酸化焙烧方法，在250 ℃下焙烧可回收纯度超过99.55%的高纯石墨，该石墨表现出优越的电化学性能。此外，利用超高温（2 600～3 300 ℃）将石墨中残留的有价组分气化去除是目前商业上制备高纯石墨的方法[22]。
2.2 原位处理
文献[23]在回收正极材料过程中，在700 ℃下高温热处理2 h除去碳粉。文献[24]采用以废石墨粉作为还原剂和水浸的还原焙烧工艺，在焙烧温度650 ℃、废石墨粉用量5%和焙烧时间1 h的最佳工艺条件下，破坏了正极材料的层状结构，并通过水浸优先回收了82.2%的Li，随后采用氨水浸出工艺从水浸渣中直接分离Co和Ni。文献[25]通过环保真空热解技术从废钴酸锂电池中回收Li和Co，以废石墨为还原剂，在真空和873～1 273 K下通过碳热还原选择性地将LiCoO2转化为Co或CoO和Li2CO3，通过控制合适的C/LiCoO2质量比和热解温度，Li和Co回收率分别达到93%和99%以上。然而，原位处理过程中废石墨被作为配料而不是产品使用，无法很好地反映石墨本身的价值。
2.3 石墨晶格缺陷的高温修复
文献[26]研究了SGA在高温热处理中的再生机制，重点考察了热处理温度、时间以及气氛对石墨晶格恢复的影响，结果表明，在氮气氛围下，热处理温度3 000 ℃和热处理时间6 h是消除内应力和实现最高石墨化程度的最优参数（见图3）。再生石墨表现出优异的电化学性能，初始充电比容量为352.5 mAh/g，1 000次循环后容量保持率为97.3%。文献[27]提出了一种硫酸固化和酸浸相结合的工艺提纯石墨，再经过1 500 ℃的高温热处理修复石墨的缺陷和内部晶格，获得了纯度超过99.6%的高纯石墨并具有良好的电化学性能。文献[28]通过酸处理和碳热还原修复了废石墨的结构，重构的石墨用作锂离子电池负极材料，具有较高的可逆容量和较长的循环寿命。综上所述，废石墨的晶格缺陷都需要经过高温热处理来进行修复。
3 物理法回收工艺
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物理法回收工艺主要指采用机械或浮选的方法提纯石墨。其中浮选法主要利用材料天然可浮性和表面性质，同时借助捕收剂、起泡剂和调整剂的作用，选择性地将疏水材料与亲水材料分开[29-30]。废锂离子电池的浮选过程如图4所示。
机械研磨-浮选法能破坏石墨的层状结构，暴露大量新生疏水表面的同时还能破坏LiCoO2颗粒表面的有机包覆膜，恢复其原有的亲水表面，提高浮选效率。文献[31]系统分析了正负极混合颗粒在研磨前后的表面形态、元素化学状态和元素分布，并借助此方法分别获得了品位高达97.13%和73.56%的LiCoO2和石墨。文献[32]则提出了一种低温研磨后泡沫浮选的新方法，改进后的浮选法能将LiCoO2精矿品位从55.36%提高到91.75%，回收率高达89.83%，同时还能获得高纯度的石墨。
采用研磨法虽然可以恢复颗粒润湿性能，但无法去除混合样品中的黏结剂，导致部分石墨和LiCoO2出现相互黏结的现象，降低了石墨的纯度。因此，文献[20]提出一种热处理后再进行浮选的工艺，先将混合正负极材料在450 ℃下热处理15 min，去除绝大部分包裹在电极表面的有机包覆层，恢复LiCoO2的原始润湿性，再通过浮选法分离石墨和LiCoO2，Co、Mn、Cu和Al回收率分别达到了97.66%、93.66%、90.14%和86.29%。文献[33]则利用Fenton试剂的高氧化性，辅助浮选回收废锂离子电池中的LiCoO2和石墨材料，结果表明，Fe2+/H2O2比为1∶120，液固比为75∶1时，可去除电极表面大部分的有机包覆层，在Fenton试剂存在的情况下，聚偏二氟乙烯（PVDF）等高分子材料被分解成小分子，最后被氧化为CO和H2，经过Fenton试剂改性后，能高效回收废锂离子电池中的LiCoO2和石墨。
4 其他回收工艺
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除了上述提到的常用的三大回收工艺，其他回收工艺主要包括电化学法、超或亚临界二氧化碳热解法、微波处理法等[34]。文献[35]提出了采用电解法将负极片中的石墨与铜箔分离的工艺，分离后的铜箔和石墨（纯度为95%）可直接重复使用，石墨直接制备成新的负极材料后表现出优异的循环稳定性和倍率性能。文献[36]建议以不同的方式处理废锂离子电池的废石墨，将废石墨从铜箔上剥离出来以后，加入乙二醇溶液中进行低温搅拌，然后将混合物在微波炉中反应，将悬浮液通过带有乙醇/水溶液的喷雾干燥器来制备具有sp2+sp3杂化碳表面的重建石墨。文献[37]研究了从石墨中去除电解质和SEI膜的三种方法：热蒸发、使用亚临界二氧化碳和乙腈、使用超临界二氧化碳，结果表明，使用亚临界二氧化碳获得的再生石墨表现出比人造石墨更好的电化学性能。
应用以上方法获得的再生石墨，其资源化利用领域主要包括：再生成二次可充电池负极材料，制备成石墨烯、超级电容器、催化剂、吸附剂、电化学传感器以及储气库等[38]，如图5所示。
5 结论与展望
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在“双碳”目标背景下，新能源汽车产量的快速增长导致石墨负极材料的需求持续增加。由于石墨化技术的高门槛限制，石墨资源严重短缺。从废锂离子电池中再生石墨是解决电池级石墨短缺的有效方法。本文综述了废锂离子电池石墨负极的回收处理技术，并对未来研究方向进行了展望。
1）SGA的回收再利用在环保和经济效益方面具有实质性意义。现有的SGA再生工艺由于加工成本高、附加值低、需求大，多数仍停留在实验室阶段。环境污染仍然是回收技术难以应用的主要原因。再生石墨是未来SGA大规模有效处置研究的主要方向。
2）由于SGA特殊的物化性能，目前主要的技术难点是在保持石墨晶体结构完整的情况下，开发一种简单、高效、清洁的闭环净化工艺来净化SGA，以获得纯度高于99.9%的石墨产品。
3）锂离子电池的容量衰减机制及其回收过程中的结构演变决定了未来的研究重点将是采用先进的石墨晶格重构修复技术，使SGA高值再生为全新的二次电池负极材料。
基金
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  • 国家自然科学基金面上项目(52174338)
  • 国家自然科学基金面上项目(52374421)
  • 湖南省自然科学基金(2022JJ20086)
  • 中国科协青年人才托举工程(YESS20210258)
  • 中南大学创新驱动项目(2023CXQD005)
  • 云南省科技计划项目(202202AB080017)
  • 贵州省科技计划项目([2023]General212)
文献
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2024年第44卷第4期
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doi: 10.3969/j.issn.0253-6099.2024.04.023
  • 接收时间：2024-05-27
  • 首发时间：2026-03-18
  • 出版时间：2024-08-01
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  • 收稿日期：2024-05-27
基金
国家自然科学基金面上项目(52174338)
国家自然科学基金面上项目(52374421)
湖南省自然科学基金(2022JJ20086)
中国科协青年人才托举工程(YESS20210258)
中南大学创新驱动项目(2023CXQD005)
云南省科技计划项目(202202AB080017)
贵州省科技计划项目([2023]General212)
作者信息
    1.中南大学 冶金与环境学院，湖南 长沙 410083
    2.中南大学 低碳有色冶金国家工程研究中心，湖南 长沙 410083

通讯作者:

仲奇凡（1990—），男，山东济宁人，教授，博士研究生导师，主要从事碳基/硅基电极材料的制备与仿真模拟、铝电解与炭素、冶金固废的无害化处理和高值化利用和半导体硅基材料高纯化制备等方面研究。E-mail：，
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2种不同金属材料的力学参数
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Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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