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Article(id=1241081031185461291, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241081025531540408, articleNumber=null, orderNo=null, doi=10.3969/j.issn.0253-6099.2024.04.024, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1717776000000, receivedDateStr=2024-06-08, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773826376005, onlineDateStr=2026-03-18, pubDate=1722441600000, pubDateStr=2024-08-01, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773826376005, onlineIssueDateStr=2026-03-18, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773826376005, creator=13701087609, updateTime=1773826376005, 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=126, endPage=131, ext={EN=ArticleExt(id=1241081032519250044, articleId=1241081031185461291, tenantId=1146029695717560320, journalId=1235980550691926019, language=EN, title=Flotation of Electrode Materials in Spent LiFePO4 Batteries Enhanced by Selective Flocculation, columnId=1241081026567533498, journalTitle=Mining and Metallurgical Engineering, columnName=SPECIAL ISSUE: BATTERY MATERIALS, runingTitle=null, highlight=null, articleAbstract=

In the flotation process of electrode materials from spent LiFePO4 batteries, the occurrence of entrainment and entrapment usually leads to poor separation effect. Aiming at such problem, selective flocculation with polyvinylpiroxanone (PVP) and polyacrylic acid (PAA) was adopted to enhance the flotation effect in an experimental study, and the interaction mechanism between PVP and PAA and electrode materials was also analyzed. Results show that the firstly added PVP can be selectively adsorbed on the graphite surface by hydrogen bonding, thus inhibiting the spontaneous hydrophobic flocculation of graphite. Then, due to site-blocking effect, the subsequently-added PAA is inhibited to be adsorbed on the graphite surface, leading to selective flocculation of LiFePO4 by PAA. A combined usage of PVP and PAA can not only make graphite effectively dispersed, but also lead to apparent particle size (D50) of LiFePO4 cathode material increased from 15.01 μm to 26.17 μm. As a result, the loss of LiFePO4 due to entrainment in the flotation process of mixed electrode can be effectively reduced, thus the recovery rate of LiFePO4 cathode material by flotation process can be improved from 71.41% to 83.59%.

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针对废旧磷酸铁锂电池电极材料浮选过程中的夹带和夹杂导致分离效果不佳的问题，利用聚乙烯吡络烷酮（PVP）和聚丙烯酸（PAA）选择性絮凝强化废旧磷酸铁锂电池混合电极材料的浮选分离过程，并分析PVP和PAA与电极材料的作用机理。结果表明：先加入的PVP通过氢键作用选择性吸附在石墨表面从而抑制石墨自发的疏水性絮凝，同时通过位点阻断后加入的PAA在石墨表面的吸附，使PAA选择性絮凝LiFePO4；PVP和PAA的联合使用在有效分散石墨的同时使LiFePO4正极材料表观粒径（D50）由15.01 μm增至26.17 μm，有效减少了LiFePO4在混合电极浮选过程中的夹带损失，使LiFePO4正极材料的浮选回收率由71.41%提升到83.59%。

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张明（1985—），男，湖北咸宁人，博士研究生，副教授，主要研究方向为微细粒矿物浮选，固废资源化利用。E-mail：
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赵梅（1999—），女，湖北应城人，硕士研究生，主要研究方向为废旧锂离子电池的回收，固废资源化利用。E-mail：

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赵梅（1999—），女，湖北应城人，硕士研究生，主要研究方向为废旧锂离子电池的回收，固废资源化利用。E-mail：

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赵梅（1999—），女，湖北应城人，硕士研究生，主要研究方向为废旧锂离子电池的回收，固废资源化利用。E-mail：

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articleId=1241081031185461291, doi=null, pmid=null, pmcid=null, year=2022, volume=42, issue=1, pageStart=85, pageEnd=89, url=null, language=null, rfNumber=[1], rfOrder=0, authorNames=廖财斌, 任国兴, 赵卫夺, journalName=矿冶工程, refType=null, unstructuredReference=廖财斌, 任国兴, 赵卫夺, 等. 三元正极材料废粉氢还原-水浸提锂过程典型杂质的影响[J]. 矿冶工程, 2022, 42(1): 85-89., articleTitle=三元正极材料废粉氢还原-水浸提锂过程典型杂质的影响, refAbstract=null), Reference(id=1241081048570851349, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081031185461291, doi=null, pmid=null, pmcid=null, year=2022, volume=42, issue=6, pageStart=100, pageEnd=104, url=null, language=null, rfNumber=[2], rfOrder=1, authorNames=乔延超, 邓浩臻, 阮丁山, journalName=矿冶工程, refType=null, unstructuredReference=乔延超, 邓浩臻, 阮丁山, 等. 废旧三元锂电池回收中间产物铝渣的资源化研究[J]. 矿冶工程, 2022, 42(6): 100-104., articleTitle=废旧三元锂电池回收中间产物铝渣的资源化研究, refAbstract=null), Reference(id=1241081048671514652, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081031185461291, doi=null, 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International Journal of Mineral Processing, 1995, 43(3): 235-247., articleTitle=Selective flocculation of iron oxide from its synthetic mixtures with clays: a comparison of polyacrylic acid and starch polymers, refAbstract=null)], funds=[Fund(id=1241081048298222592, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081031185461291, awardId=51704215, language=CN, fundingSource=国家自然科学基金(51704215), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1241081037250425276, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081031185461291, xref=1., ext=[AuthorCompanyExt(id=1241081037258813886, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081031185461291, companyId=1241081037250425276, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.School of Resources and Environmental Engineering, Wuhan University of Science and Technology, Wuhan 430081, Hubei, China), AuthorCompanyExt(id=1241081037267202494, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081031185461291, companyId=1241081037250425276, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.武汉科技大学 资源与环境工程学院，湖北 武汉 430081)]), AuthorCompany(id=1241081037418197452, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081031185461291, xref=2., ext=[AuthorCompanyExt(id=1241081037430780366, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081031185461291, companyId=1241081037418197452, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2.Hubei Xingfa Chemical Group Co., Ltd., Yichang 443000, Hubei, China), AuthorCompanyExt(id=1241081037439168976, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081031185461291, companyId=1241081037418197452, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2.湖北兴发化工集团股份有限公司，湖北 宜昌 443000)])], figs=[ArticleFig(id=1241081043957117685, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081031185461291, language=EN, label=null, caption=null, figureFileSmall=/R/UnzlnP81/aNzHa3T4Gw==, figureFileBig=yhlZ3UHU4xlHLSbA/VhF9Q==, tableContent=null), ArticleFig(id=1241081044074558204, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081031185461291, language=CN, label=图1, caption=电极材料破碎流程, figureFileSmall=/R/UnzlnP81/aNzHa3T4Gw==, figureFileBig=yhlZ3UHU4xlHLSbA/VhF9Q==, tableContent=null), ArticleFig(id=1241081044301050644, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081031185461291, language=EN, label=null, caption=null, figureFileSmall=9OUJ63gU0lJezfH6O2v3OA==, figureFileBig=zgzK7pDFm4qUaNmPjFivnQ==, tableContent=null), ArticleFig(id=1241081044397519646, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081031185461291, language=CN, label=图2, caption=混合电极材料浮选流程, figureFileSmall=9OUJ63gU0lJezfH6O2v3OA==, figureFileBig=zgzK7pDFm4qUaNmPjFivnQ==, tableContent=null), ArticleFig(id=1241081044506571560, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081031185461291, language=EN, label=null, caption=null, figureFileSmall=g8OdpwxkspLpkdA/n7hEpQ==, figureFileBig=Fb6/NYDLfmPMijDiDQnciQ==, tableContent=null), ArticleFig(id=1241081044628206390, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081031185461291, language=CN, label=图3, caption=混合电极材料选择性絮凝试验结果, figureFileSmall=g8OdpwxkspLpkdA/n7hEpQ==, figureFileBig=Fb6/NYDLfmPMijDiDQnciQ==, tableContent=null), ArticleFig(id=1241081044846310213, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081031185461291, language=EN, label=null, caption=null, figureFileSmall=oE04VqIGSyw0l3LD/3j+1A==, figureFileBig=TSBWhZbfxk5KnD4rrIIeUw==, tableContent=null), ArticleFig(id=1241081044946973516, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081031185461291, language=CN, label=图4, caption=混合电极材料浮选试验结果, figureFileSmall=oE04VqIGSyw0l3LD/3j+1A==, figureFileBig=TSBWhZbfxk5KnD4rrIIeUw==, tableContent=null), ArticleFig(id=1241081045110551389, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081031185461291, language=EN, label=null, caption=null, figureFileSmall=pwEE6z2VYPDTxg3YgaohtA==, figureFileBig=d7meOvLEzisa82BEUuRs+w==, tableContent=null), ArticleFig(id=1241081045261546342, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081031185461291, language=CN, label=图5, caption=PVP和PAA对石墨和LiFePO4粒度分布的影响

（a）石墨；（b）LiFePO4

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（a）石墨；（b）LiFePO4

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（a）PVP；（b）PAA；（c）石墨+药剂；（d）LiFePO4+药剂

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试验组石墨粒度特征参数/μmLiFePO4粒度特征参数/μm
D10D50D90D10D50D90
空白组9.4917.1430.112.0915.0154.25
PVP9.5216.5328.301.7015.8055.68
PAA8.5019.7939.303.0223.7984.53
PVP+PAA8.8316.9230.353.8726.1783.03
), ArticleFig(id=1241081046524031962, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081031185461291, language=CN, label=表1, caption=

正、负极电极材料粒度分布

, figureFileSmall=null, figureFileBig=null, tableContent=
试验组石墨粒度特征参数/μmLiFePO4粒度特征参数/μm
D10D50D90D10D50D90
空白组9.4917.1430.112.0915.0154.25
PVP9.5216.5328.301.7015.8055.68
PAA8.5019.7939.303.0223.7984.53
PVP+PAA8.8316.9230.353.8726.1783.03
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试验组ENTFMR2
空白组0.954.330.996 3
PVP+PAA0.762.260.999 5
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混合电极粉浮选夹带模型拟合结果

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试验组ENTFMR2
空白组0.954.330.996 3
PVP+PAA0.762.260.999 5
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选择性絮凝强化废旧磷酸铁锂电池电极材料浮选分离
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赵梅 1 , 崔瑞 1 , 李盼武 2 , 张明 1
矿冶工程杂志 | 电池材料专题 2024,44(4): 126-131
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矿冶工程杂志 | 电池材料专题 2024, 44(4): 126-131
选择性絮凝强化废旧磷酸铁锂电池电极材料浮选分离
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赵梅1 , 崔瑞1, 李盼武2, 张明1
作者信息
  • 1.武汉科技大学 资源与环境工程学院，湖北 武汉 430081
  • 2.湖北兴发化工集团股份有限公司，湖北 宜昌 443000

    • 赵梅（1999—），女，湖北应城人，硕士研究生，主要研究方向为废旧锂离子电池的回收，固废资源化利用。E-mail：

通讯作者:

张明（1985—），男，湖北咸宁人，博士研究生，副教授，主要研究方向为微细粒矿物浮选，固废资源化利用。E-mail：
Flotation of Electrode Materials in Spent LiFePO4 Batteries Enhanced by Selective Flocculation
Mei ZHAO1 , Rui CUI1, Panwu LI2, Ming ZHANG1
Affiliations
  • 1.School of Resources and Environmental Engineering, Wuhan University of Science and Technology, Wuhan 430081, Hubei, China
  • 2.Hubei Xingfa Chemical Group Co., Ltd., Yichang 443000, Hubei, China
出版时间: 2024-08-01 doi: 10.3969/j.issn.0253-6099.2024.04.024
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摘要
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针对废旧磷酸铁锂电池电极材料浮选过程中的夹带和夹杂导致分离效果不佳的问题，利用聚乙烯吡络烷酮（PVP）和聚丙烯酸（PAA）选择性絮凝强化废旧磷酸铁锂电池混合电极材料的浮选分离过程，并分析PVP和PAA与电极材料的作用机理。结果表明：先加入的PVP通过氢键作用选择性吸附在石墨表面从而抑制石墨自发的疏水性絮凝，同时通过位点阻断后加入的PAA在石墨表面的吸附，使PAA选择性絮凝LiFePO4；PVP和PAA的联合使用在有效分散石墨的同时使LiFePO4正极材料表观粒径（D50）由15.01 μm增至26.17 μm，有效减少了LiFePO4在混合电极浮选过程中的夹带损失，使LiFePO4正极材料的浮选回收率由71.41%提升到83.59%。

磷酸铁锂  /  废旧电池回收  /  正极材料  /  石墨  /  电极材料  /  选择性絮凝  /  浮选

In the flotation process of electrode materials from spent LiFePO4 batteries, the occurrence of entrainment and entrapment usually leads to poor separation effect. Aiming at such problem, selective flocculation with polyvinylpiroxanone (PVP) and polyacrylic acid (PAA) was adopted to enhance the flotation effect in an experimental study, and the interaction mechanism between PVP and PAA and electrode materials was also analyzed. Results show that the firstly added PVP can be selectively adsorbed on the graphite surface by hydrogen bonding, thus inhibiting the spontaneous hydrophobic flocculation of graphite. Then, due to site-blocking effect, the subsequently-added PAA is inhibited to be adsorbed on the graphite surface, leading to selective flocculation of LiFePO4 by PAA. A combined usage of PVP and PAA can not only make graphite effectively dispersed, but also lead to apparent particle size (D50) of LiFePO4 cathode material increased from 15.01 μm to 26.17 μm. As a result, the loss of LiFePO4 due to entrainment in the flotation process of mixed electrode can be effectively reduced, thus the recovery rate of LiFePO4 cathode material by flotation process can be improved from 71.41% to 83.59%.

lithium iron phosphate  /  spent battery recycling  /  cathode material  /  graphite  /  electrode material  /  selective flocculation  /  flotation
赵梅, 崔瑞, 李盼武, 张明. 选择性絮凝强化废旧磷酸铁锂电池电极材料浮选分离. 矿冶工程杂志, 2024 , 44 (4) : 126 -131 . DOI: 10.3969/j.issn.0253-6099.2024.04.024
Mei ZHAO, Rui CUI, Panwu LI, Ming ZHANG. Flotation of Electrode Materials in Spent LiFePO4 Batteries Enhanced by Selective Flocculation[J]. Mining and Metallurgical Engineering, 2024 , 44 (4) : 126 -131 . DOI: 10.3969/j.issn.0253-6099.2024.04.024
正文
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废旧锂电池是重要的富锂二次资源[1]，若不采取措施有效回收将会造成资源浪费与环境污染问题[2]。直接回收工艺具有可持续、能源需求低以及排放物少等优点。浮选是利用正极金属氧化物的亲水性和负极石墨天然疏水性分离微细混合电极材料的一种直接回收手段[3]。但正、负极材料表面的有机黏结剂附着导致二者润湿性差异变小，直接浮选难以实现高效分离[4]，因此在进行浮选前需对电极材料进行预处理，去除电极材料表面的有机黏结剂。为了尽可能回收电极材料，在直接回收时通常需要将活性材料碎磨至很细的粒度[4-5]，后续浮选过程中，过细的正极材料颗粒容易以夹带的形式进入泡沫产品（主要是石墨）中。同时，负极石墨在矿浆中自发的疏水性絮凝会将正极材料包裹在其中，最终导致浮选分离精度不高。因此，如何抑制石墨自发的疏水性絮凝并减少过细的正极材料的夹带是强化废旧电池电极材料浮选分离的关键。
本文以聚乙烯吡络烷酮（PVP）为分散剂、聚丙烯酸（PAA）为絮凝剂，探究通过选择性絮凝提高混合电极材料中LiFePO4和石墨浮选分离效果的可行性，并分析了PVP和PAA与电极材料的作用机理。
1 试验
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1.1 材料准备
试验原料为18650型废旧磷酸铁锂电池。试验药剂包括氯化钠（分析纯）、聚乙烯吡络烷酮（PVP，平均分子质量58 000）、聚丙烯酸（PAA，平均分子质量3 000 000）、煤油（工业纯）、甲基异丁基甲醇（MIBC，纯度99%）等。
为保证试验安全，在拆解废旧磷酸铁锂电池前需进行放电处理：将电池浸泡在质量分数5%的氯化钠溶液中放电48 h后取出，待其自然风干后进行手工拆解处理，分别得到正极片与负极片[5]。将正、负极片按片数比例1∶1裁剪成小片后与水混合加入MJ-BL1036A型破碎机中，经两段湿式破碎处理后收集0.074 mm筛下部分，真空抽滤，将所得电极材料置于烘箱中80 ℃干燥、105 ℃过夜以去除多余电解液，收集备用，制备正极材料（LiFePO4）、负极材料（石墨）及二者的混合电极材料。电极材料破碎流程如图1所示。
1.2 试验方法与表征
1.2.1 选择性絮凝试验
在自制的250 mL沉降管中进行絮凝试验[6]。将7.5 g混合电极材料与200 mL去离子水混合，加入所需量的PVP或PAA。将矿浆转移至250 mL沉降管中并补加去离子水至250 mL，上下翻转沉降管10次后置于水平桌面静止30 s，打开阀门，收集上部悬浮液，将排出的矿浆与管内矿浆烘干、称重并检测Fe质量分数，计算产品中LiFePO4品位[5]。结合式（1）[7]对混合电极材料絮凝的选择性进行分析。
式中：S为选择性指数；RL-RG为管内矿浆中LiFePO4回收率与管内矿浆中石墨回收率的差值，百分点。
1.2.2 浮选试验
浮选设备为100 mL XFGC实验室浮选机，设置浮选机叶轮转速1 800 r/min、充气量0.04 m3/h。在浮选槽中加入4 g混合电极材料和100 mL去离子水后搅拌混匀，调节矿浆pH值为8.8。以图2所示浮选流程开展浮选试验，并分别在30 s、60 s、120 s、180 s收集泡沫产品，将所得4组泡沫产品与槽内产品分别称重、过滤、烘干、称重、检测Fe质量分数。
1.2.3 检测方法
根据浮选条件进行调浆，采用激光粒度分析仪（Malvern Mastersizer 2000）测定LiFePO4和石墨与PVP或PAA作用前后的粒度分布情况。
将50 mg石墨或LiFePO4加入50 mL的1 mmol/L的KCl溶液中，加入所需量PVP或PAA，用稀盐酸或氢氧化钠调节矿浆pH值，矿浆沉淀5 min后，采用电位分析仪（Malvern Zetasizer Nano ZS90）测试上清液Zeta电位。
将1 g石墨或LiFePO4与50 mL去离子水混合，加入所需量PVP或PAA，根据浮选条件进行调浆，再将抽滤后所得样品在真空烘箱中干燥。采用傅里叶红外光谱仪（美国Thermo Scientific Nicolet 6700）的KBr压片程序测量样品红外光谱。
2 结果与讨论
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2.1 选择性絮凝试验
PVP和PAA单独或联合作用下混合电极材料的絮凝效果如图3所示。可以看出，与空白组（不添加PVP和PAA）相比，单独添加PVP时，管内矿浆LiFePO4品位由43.89%提升到46.77%，回收率由61.54%提升到65.41%，S值由空白组的0.14增加到0.19，说明单独使用PVP可以对混合电极材料石墨与LiFePO4的分离产生积极影响；单独添加PAA时，管内矿浆中LiFePO4品位反而降至40.72%，虽然回收率高达94.91%，但其S值仅0.10，这可能是由于PAA没有选择性絮凝能力，LiFePO4颗粒与石墨颗粒均被絮凝形成没有选择性的团聚物，使得二者更难分离；将PAA和PVP联合使用时管内矿浆中LiFePO4品位和LiFePO4回收率分别达到45.24%和85.57%，且S值增加到0.22，说明二者联合作用可以提高PAA对LiFePO4的选择性絮凝能力。
2.2 浮选试验
PVP和PAA对混合电极材料浮选效果的影响如图4所示。可以看出，空白组槽内产品LiFePO4品位和回收率分别为76.29%和71.41%。PVP单独作用时，LiFePO4浮选回收率提高至81.28%，原因可能是PVP通过分散石墨抑制其自发的疏水性絮凝，进而抑制了石墨对LiFePO4的非选择性包裹（夹杂），但同时亲水的PVP作用于石墨表面后降低了石墨的可浮性，从而影响槽内LiFePO4品位。PAA单独作用时，虽然LiFePO4回收率上升但品位却大幅下降，原因可能是PAA没有选择性絮凝作用，产生了LiFePO4和石墨的夹杂絮凝物。先添加PVP再添加PAA能在保证LiFePO4品位小幅降低的情况下大幅提高回收率到83.59%，说明二者联合选择性絮凝LiFePO4有利于正、负极材料的浮选分离。
2.3 PVP和PAA对粒度分布的影响
PVP和PAA对石墨和LiFePO4粒度分布的影响见图5，石墨和LiFePO4粒度分布情况如表1所示。由图5及表1可知，单独加入PVP时，石墨粒度分布变得更加分散；单独加入PAA时，石墨粒度分布曲线发生了明显的右移，说明PAA使石墨团聚；先加PVP再加PAA，PVP的加入明显抑制了PAA对石墨的絮凝作用，石墨依旧处于相对分散的状态。添加PVP对LiFePO4的分散与团聚并没有明显作用，添加PAA可以使LiFePO4团聚；先加PVP再加PAA，PVP的加入并没有影响PAA对LiFePO4的絮凝作用，LiFePO4表观粒径（D50）由空白组的15.01 μm增加至26.17 μm，而石墨粒度无明显变化。
由此可见，PAA对石墨和LiFePO4没有明显的选择性絮凝作用，PVP会抑制PAA对石墨的絮凝，但不影响PAA对LiFePO4的絮凝。这表明PVP和PAA联合使用可以分散石墨，抑制其自发的疏水性絮凝，并使PAA选择性絮凝LiFePO4，增大LiFePO4的表观粒径，从而有望减少LiFePO4在混合电极材料浮选过程中的夹带损失[8]。
2.4 PVP和PAA对夹带的影响
PVP和PAA作用前后泡沫产品中LiFePO4回收率和水回收率的关系如图6所示。由图6可以发现，泡沫产品中LiFePO4回收率与水回收率呈线性关系，说明夹带是LiFePO4进入泡沫相的重要方式[8]。
与空白组相比，混合电极材料在加入PVP和PAA后，泡沫产品中水回收率和LiFePO4回收率均有所降低。为更直观展现PVP和PAA对混合电极材料夹带行为的影响，采用经典Warren模型[9]对混合电极材料浮选过程LiFePO4回收率与水回收率进行拟合分析，拟合公式为：
式中：RM为LiFePO4在泡沫产品中的总回收率，%；FM为LiFePO4在泡沫产品中的真浮选回收率，%；ENT为浮选夹带指数，介于0～1之间，其值越大，夹带越严重[10]；RW为水回收率，%。
式（2）拟合结果如表2所示。由表2可知，添加PVP和PAA后，混合电极材料的真浮选回收率FM降低。更重要的是，PVP和PAA的添加使浮选夹带指数ENT由空白组的0.95降至0.76，说明PVP和PAA的联合作用降低了混合电极材料浮选过程中的夹带程度，减少了LiFePO4进入泡沫产品中的量。
2.5 Zeta电位测试
石墨和LiFePO4颗粒与药剂作用前后的Zeta电位随pH值的变化关系见图7。由图7可见，石墨与PVP单独作用后Zeta电位发生正向偏移，而与PAA单独作用后Zeta电位发生负向偏移，说明PVP和PAA均能与石墨作用。但石墨先与PVP作用后再加入PAA时，其Zeta电位发生正向偏移且偏移量较单独添加PVP时小，说明此时PVP和PAA都在石墨表面吸附，同时PVP有效阻碍了PAA在石墨表面的吸附。LiFePO4与PVP单独作用后Zeta电位无明显偏移，说明PVP与LiFePO4几乎不作用；LiFePO4先与PVP作用后再加入PAA，其Zeta电位相较于单独与PAA作用时未发生明显偏移，表明PVP的加入并未影响PAA在LiFePO4表面的吸附。综上可知，PVP先一步与石墨作用后能够有效抑制PAA在石墨表面吸附，但PVP并不影响PAA在LiFePO4表面的吸附。
2.6 红外光谱分析
图8（a）为PVP的红外光谱图。由图8（a）可以看出，PVP有几个明显的特征峰，分别出现在2 948.22 cm-1、1 661.71 cm-1、1 425.50 cm-1和1 280.79 cm-1处。3500～3000 cm-1的钝峰归因于水的O—H拉伸振动[11]。
图8（b）为PAA的红外光谱图，3 450.34 cm-1、1 709.25 cm-1、1 453.74 cm-1和1 415.11 cm-1处的峰均为PAA的特征峰。
图8（c）为石墨与PVP和PAA作用前后的红外光谱图。经PVP处理后，谱图中3 442.29 cm-1和1 636.52 cm-1处的新峰来自PVP的O—H的拉伸振动和伸缩振动[12]，其中1 500～600 cm-1范围内出现了谱带消失或强度降低，这是PVP与石墨之间形成氢键[13]造成的。经PAA处理后，谱图中3 440.40 cm-1和1 640.92 cm-1处的新峰来自PAA的—COOH基团O—H拉伸振动和—COO—反对称拉伸振动[14]。PAA中的—COOH基团可以与C表面的OH基团形成强氢键[15]。经PVP和PAA联合作用后，石墨800～600 cm-1范围内谱带的消失或强度降低表明PVP通过氢键作用吸附在石墨表面；同时谱图中发现了来自PAA的—COOH基团O—H拉伸振动以及—COO—反对称拉伸振动，说明此时PAA与PVP共同吸附在石墨表面。
图8（d）为LiFePO4与PVP和PAA作用前后的红外光谱图，PVP处理前后LiFePO4峰型几乎没有变化，由此可知PVP并未吸附在LiFePO4表面。有研究[16]表明，非离子型聚合物在氧化矿物表面的吸附多由氢键作用驱动，LiFePO4自身水化作用很强，导致PVP很难替换LiFePO4表面牢固结合的水分子形成吸附[17]。LiFePO4经PAA处理后在3 445.31 cm-1和1 636.52 cm-1处分别出现了来自PAA的—COOH基团O—H拉伸振动和—COO—反对称拉伸振动。PAA能通过—COO—基团与LiFePO4共氢表面位点间的氢键作用在后者表面形成吸附[18]。先经PVP处理、再经PAA处理的LiFePO4出现了与单独添加PAA时几乎一样的新带，表明PAA可以吸附在经PVP处理后的LiFePO4表面，添加PVP对LiFePO4吸附PAA无明显影响。
2.7 选择性絮凝机理分析
由上述试验结果可知，先加PVP、再加PAA，PAA虽然能与PVP共同吸附在石墨表面，但此时石墨与PAA的作用强度和石墨颗粒的絮凝程度相较于单独添加PAA时均大幅降低。这说明石墨经PVP处理后，再加入的PAA对石墨的絮凝作用十分有限，它只选择性絮凝LiFePO4，原因在于经PVP处理的石墨表面可供PAA吸附的氢键作用位点数量大幅减少。
PVP和PAA选择性分散絮凝石墨和LiFePO4的机理如图9所示。可见PVP和PAA实现选择性絮凝浮选电极材料可分为三个阶段：
1）分散阶段：分散剂PVP选择性吸附在石墨表面而不与LiFePO4作用，PVP抑制了石墨自发的疏水性絮凝，从而减少LiFePO4因石墨疏水性絮凝而被夹带进入泡沫产品的量。
2）选择性絮凝阶段：石墨表面的作用位点被先加入的PVP占据，从而阻碍了PAA对石墨的絮凝；LiFePO4不与PVP作用，使得PAA可通过氢键作用吸附在其表面，进而实现LiFePO4的选择性絮凝。
3）浮选阶段：充气浮选时，疏水的石墨被气泡捕获进入泡沫产品，亲水的LiFePO4颗粒絮团留在浮选槽内。
3 结论
收起
1）分散剂PVP和絮凝剂PAA的联合作用可以实现石墨和LiFePO4的选择性分散和絮凝。先PVP后PAA的加药方式可以使LiFePO4正极材料的浮选回收率由常规浮选的71.41%提升到83.59%。
2）单独使用PVP或PAA时，PVP可以通过氢键作用吸附在石墨表面，但并不作用于LiFePO4表面；PAA能通过氢键作用同时吸附在石墨和LiFePO4表面。PVP和PAA联合作用时，PVP先一步与石墨作用，然后有效阻碍后加入的PAA在石墨表面吸附，使石墨保持分散状态；而PVP不影响PAA对LiFePO4的絮凝，从而实现LiFePO4的选择性絮凝。
3）PVP和PAA通过选择性絮凝LiFePO4有效降低了LiFePO4在混合电极材料浮选过程中的夹带损失。
基金
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  • 国家自然科学基金(51704215)
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doi: 10.3969/j.issn.0253-6099.2024.04.024
  • 接收时间：2024-06-08
  • 首发时间：2026-03-18
  • 出版时间：2024-08-01
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  • 收稿日期：2024-06-08
基金
国家自然科学基金(51704215)
作者信息
    1.武汉科技大学 资源与环境工程学院，湖北 武汉 430081
    2.湖北兴发化工集团股份有限公司，湖北 宜昌 443000

通讯作者:

张明（1985—），男，湖北咸宁人，博士研究生，副教授，主要研究方向为微细粒矿物浮选，固废资源化利用。E-mail：
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2种不同金属材料的力学参数
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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
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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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