废旧锂离子电池负极石墨深度除杂及除杂液循环再生规律研究  

Research on Deep Impurity Removal of Negative Graphite of Waste Lithium Ion Battery and Recycling of Impurity Removal Liquid

作　　者：赵浩含 蔡龙浩 李祥龙 周瑞 童翠婷 吴昊 许江斌 黄硕 沈璟昊 曾桂生[1] 刘春力 ZHAO Haohan;CAI Longhao;LI Xianglong;ZHOU Rui;TONG Cuiting;WU Hao;XU Jiangbin;Huang Shuo;SHEN Jinghao;ZENG Guisheng;LIU Chunli(School of Environmental and Chemi cal Engineering,Nanchang Hangkong Uni versity,Nanchang 330063,China;Binzhou Tongbo Engi neering Technology Co.,Ltd.,Binzhou 527299,Shandong,China)

机构地区：[1]南昌航空大学环境与化学工程学院,南昌330063 [2]滨州通渤工程技术有限公司,山东滨州527299

出　　处：《有色金属(冶炼部分)》2025年第4期225-233,共9页Nonferrous Metals(Extractive Metallurgy)

基　　金：江西省自然科学基金(面上)项目(20224BAB203027)。

摘　　要：废旧锂离子电池的资源化回收具有环保和经济双重效益,然而目前研究主要集中在正极回收,对负极石墨的回收报道相对较少。提出一种负极石墨低温氟化氢铵焙烧—水浸深度除杂的新工艺,系统考察了不同工艺条件对杂质去除的影响规律。发现在优化条件下,负极石墨中的锂、镍、钴、锰、铝、铜去除率分别达到99.78%、99.84%、99.99%、99.94%、95.18%、92.35%,除杂后石墨纯度高于99.9%。此外,还研究了浸出液中的杂质离子分步去除规律。结果发现,先通过联合利用同离子效应和溶析结晶方法,浸出液中杂质铝离子去除率可达到88%,再通过铁粉还原处理,浸出液中铜离子的去除率达到76%;接着通过pH调控实现浸出液中钴、镍、锰等金属的被高效去除;最后,浸出液经过蒸发结晶可回收得到氟化氢铵固体,从而实现除杂剂的再生循环利用。The resource recovery of spent lithium-ion batteries has both environmental and economic benefits,however,the current research mainly focuses on the recovery of positive electrode,and there are relatively few reports on the recovery of anode graphite.A new process of low temperature ammonium hydrogen fluoride roasting-water immersion depth impurity removal of anode graphite was proposed,and the influence of different process conditions on the removal of impurities was systematically investigated.It is found that under the optimized conditions,the removal rate of lithium,nickel,cobalt,manganese,aluminum and copper in anode graphite reaches 99.78%,99.84%,99.99%,99.94%,95.18%,and 92.35%,respectively,and the purity of the graphite is higher than 99.9%after removal of impurities.In addition,the step-by-step removal of impurity ions in the leach solution was also studied.It is found that,firstly,through the joint use of the homoionic effect and solventing-out crystallization method,the removal rate of impurity aluminum ions in the leach solution can reach 88%,then through the reduction of iron powder treatment,the removal rate of copper ions in the leach solution reaches 76%.Then,through pH value regulation,cobalt,nickel,manganese and other metals in the leaching solution can be efficiently removed.Finally,ammonium hydrogen fluoride solid can be recovered from the leaching solution by evaporation and crystalli zation,so as to realize the recycli ng and recycli ng of the i mpurity removal agent.

关 键 词：负极石墨 低温焙烧 同离子效应 溶析结晶 浸出液 分步除杂 

分 类 号：TF803.25[冶金工程—有色金属冶金]