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Article(id=1240689591091516234, tenantId=1146029695717560320, journalId=1234093305789726721, issueId=1240689590315569990, articleNumber=null, orderNo=null, doi=null, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1719763200000, receivedDateStr=2024-07-01, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773733049414, onlineDateStr=2026-03-17, pubDate=1739980800000, pubDateStr=2025-02-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773733049414, onlineIssueDateStr=2026-03-17, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773733049414, creator=13701087609, updateTime=1773733049414, updator=13701087609, issue=Issue{id=1240689590315569990, tenantId=1146029695717560320, journalId=1234093305789726721, year='2025', volume='45', issue='2', pageStart='593', pageEnd='1184', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773733049228, creator=13701087609, updateTime=1773733150042, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1240690013239825123, tenantId=1146029695717560320, journalId=1234093305789726721, issueId=1240689590315569990, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1240690013239825124, tenantId=1146029695717560320, journalId=1234093305789726721, issueId=1240689590315569990, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=759, endPage=767, ext={EN=ArticleExt(id=1240689591347368779, articleId=1240689591091516234, tenantId=1146029695717560320, journalId=1234093305789726721, language=EN, title=Degradation of Rhodamine B by FeMnCoNi-O activated potassium persulfate, columnId=1234106386360103680, journalTitle=China Environmental Science, columnName=Water Pollution Control, runingTitle=null, highlight=null, articleAbstract=

FeMnCoNi-O nanoparticles (NPs) with outstanding structural stability and catalytic performance were synthesized by coprecipitation and consequent calcination method. The FeMnCoNi-O NPs were carefully characterized by X-Ray diffraction (XRD), transmission electron microscope (TEM), Fourier transform infrared spectroscopy (FT-IR), thermal gravimetric analyzer (TG) and X-ray photoelectron spectroscopy (XPS) techniques. Furthermore, the obtained catalyst was applied to activate potassium persulfate (PMS) and degrade Rhodamine B (RhB). The effects of reaction conditions such as the concentration of the RhB, PMS and catalysts concentration, the kinds of pollutant and aqueous pH values, on the degradation process and the recycling performance were systematically investigated. Via the calcined treatment (200℃, 2h), the final product was the multi-metal oxide, which exhibited enhanced catalytic performance for the RhB degradation. FeMnCoNi-O NPs can achieve complete degradation of RhB (20mg/L) in 10minutes by activating trace amounts of PMS (0.2mmol/L). With the help of free radical quenching experiment and XPS analysis, it is found the main active substances in the degradation system were 1O2 and SO4·- generated via persulfate activation.

, correspAuthors=Feng FANG, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, authorCompany=null, fund=null, authors=null, authorsList=Bang-li XU, Hai-xian YAN, Shi-ya WENG, Shi-qi WANG, Feng FANG), CN=ArticleExt(id=1240689600155406537, articleId=1240689591091516234, tenantId=1146029695717560320, journalId=1234093305789726721, language=CN, title=FeMnCoNi-O活化过硫酸氢钾降解罗丹明B, columnId=1234106386565624579, journalTitle=中国环境科学, columnName=水污染与控制, runingTitle=null, highlight=null, articleAbstract=

以乙酸盐和柠檬酸钠为原料,通过共沉淀-热处理法合成了结构稳定且性能优良的FeMnCoNi-O纳米颗粒,使用XRD，TEM，FT-IR，TG，ICP，XPS等手段对其进行表征,并将其应用于常温常压下活化过硫酸氢钾(PMS)降解罗丹明B(RhB),探究PMS浓度、RhB浓度、污染物种类、FeMnCoNi-O浓度、初始pH值、水中阴离子种类等反应条件对降解效果的影响,以及FeMnCoNi-O纳米颗粒的循环使用性能.结果表明,经过200℃保温2h后样品从普鲁士蓝类似物转变为多元金属氧化物,活化PMS降解RhB能力显著提高.FeMnCoNi-O纳米颗粒可以通过活化微量的PMS(0.2mmol/L),在10min内实现RhB(20mg/L)的完全降解.自由基淬灭和XPS结果表明,体系中主要活性物质为过硫酸氢根活化生成的1O2和SO4·—.

, correspAuthors=方峰, authorNote=null, correspAuthorsNote=
*责任作者，教授，
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徐邦利(1998-)，女，安徽淮北人，东南大学硕士研究生，主要从事污水中有机污染物降解研究.发表论文2篇. .

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徐邦利(1998-)，女，安徽淮北人，东南大学硕士研究生，主要从事污水中有机污染物降解研究.发表论文2篇. .

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徐邦利(1998-)，女，安徽淮北人，东南大学硕士研究生，主要从事污水中有机污染物降解研究.发表论文2篇. .

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Journal of Inorganic Materials，2023，38:469., articleTitle=Enhanced degradation of methyl orange with CoFe2O4@Zeolite catalyst as peroxymonosulfate activator: Performance and mechanism, refAbstract=null)], funds=[Fund(id=1240689611962372143, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1240689591091516234, awardId=52171110, language=CN, fundingSource=国家自然科学基金资助项目(52171110), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1240689600658723055, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1240689591091516234, xref=null, ext=[AuthorCompanyExt(id=1240689600667111665, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1240689591091516234, companyId=1240689600658723055, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=School of Materials Science and Engineering, Southeast University, Nanjing 211189, China), AuthorCompanyExt(id=1240689600675500275, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1240689591091516234, companyId=1240689600658723055, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=东南大学材料科学与工程学院，江苏 南京 211189)])], figs=[ArticleFig(id=1240689605385704070, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1240689591091516234, language=EN, label=Fig.1, caption=HRTEM and EDS-mapping of FeMnCoNi PBA and FeMnCoNi-O, figureFileSmall=aXl9mp253jxGyvYAHlB62g==, figureFileBig=SRmC4JPZNJUupCBIA4hF9g==, tableContent=null), ArticleFig(id=1240689605469590163, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1240689591091516234, language=CN, label=图1, caption=FeMnCoNi PBA及氧化物的HRTEM和EDS-Mapping, figureFileSmall=aXl9mp253jxGyvYAHlB62g==, figureFileBig=SRmC4JPZNJUupCBIA4hF9g==, tableContent=null), ArticleFig(id=1240689605763191480, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1240689591091516234, language=EN, label=Fig.2, caption=XRD spectra of FeMnCoNi-O and PBA, figureFileSmall=Y1sPJKEMbvQB7mxeV4evQg==, figureFileBig=lrN9tnX4H5jl1b5zyxS8Tw==, tableContent=null), ArticleFig(id=1240689607331861193, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1240689591091516234, language=CN, label=图2, caption=FeMnCoNi PBA及氧化物的XRD图谱, figureFileSmall=Y1sPJKEMbvQB7mxeV4evQg==, figureFileBig=lrN9tnX4H5jl1b5zyxS8Tw==, tableContent=null), ArticleFig(id=1240689607445107413, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1240689591091516234, language=EN, label=Fig.3, caption=TG and FT-IR results of FeMnCoNi-O and PBA, figureFileSmall=mt3XFzwyzD6D9THHlitysg==, figureFileBig=fmpUvqAwHB3TYXvkZY4fsw==, tableContent=null), ArticleFig(id=1240689607562547941, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1240689591091516234, language=CN, label=图3, caption=FeMnCoNi PBA及氧化物的TG和FT-IR图谱, figureFileSmall=mt3XFzwyzD6D9THHlitysg==, figureFileBig=fmpUvqAwHB3TYXvkZY4fsw==, tableContent=null), ArticleFig(id=1240689607663211252, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1240689591091516234, language=EN, label=Fig.4, caption=Removal rate of RhB in different system, figureFileSmall=k63G2Ibi+wOIOg7bLtKj2A==, figureFileBig=h2DuVfndI3j+QkJU/tHiug==, tableContent=null), ArticleFig(id=1240689607780651778, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1240689591091516234, language=CN, label=图4, caption=不同催化体系下的RhB去除率

实验条件:20ppm RhB, 1mL 0.02mol/L PMS (a), 0.5mL 0.02mol/L PMS(b), pH=7

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RhB:罗丹明B，MB:亚甲基蓝,MO:甲基橙,CR:刚果红,MG:孔雀石绿

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EDS of FeMnCoNi-O

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元素(at%)OMnFeCoNi
FeMnCoNi-O46.6620.258.329.0015.77
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FeMnCoNi-O的EDS

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元素(at%)OMnFeCoNi
FeMnCoNi-O46.6620.258.329.0015.77
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First order kinetic fitting parameters for radical quenching experiments

, figureFileSmall=null, figureFileBig=null, tableContent=
样品名称对照组2mol/L MeOH0.5mol/L MeOH0.1mol/L TBA1mol/L TBA1mmol/L L-Histidine10mmol/L L-Histidine
k(min-1)0.238910.084550.189680.18290.266530.109620.00406
R20.986980.982790.99290.999720.998610.988170.97259
), ArticleFig(id=1240689610116879361, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1240689591091516234, language=CN, label=表2, caption=

淬灭实验的一阶动力学拟合参数

, figureFileSmall=null, figureFileBig=null, tableContent=
样品名称对照组2mol/L MeOH0.5mol/L MeOH0.1mol/L TBA1mol/L TBA1mmol/L L-Histidine10mmol/L L-Histidine
k(min-1)0.238910.084550.189680.18290.266530.109620.00406
R20.986980.982790.99290.999720.998610.988170.97259
), ArticleFig(id=1240689610255290381, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1240689591091516234, language=EN, label=Table 3, caption=

The ion leakage during reaction

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元素FeMnCoNi
单位(mg/L)<0.0012<0.0001<0.00210.2999
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反应中离子泄露情况

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元素FeMnCoNi
单位(mg/L)<0.0012<0.0001<0.00210.2999
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FeMnCoNi-O活化过硫酸氢钾降解罗丹明B
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徐邦利 , 严海线 , 翁诗雅 , 王世琦 , 方峰 *
中国环境科学 | 水污染与控制 2025,45(2): 759-767
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中国环境科学 | 水污染与控制 2025, 45(2): 759-767
FeMnCoNi-O活化过硫酸氢钾降解罗丹明B
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徐邦利 , 严海线, 翁诗雅, 王世琦, 方峰*
作者信息
  • 东南大学材料科学与工程学院，江苏 南京 211189

    • 徐邦利(1998-)，女，安徽淮北人，东南大学硕士研究生，主要从事污水中有机污染物降解研究.发表论文2篇. .

通讯作者:

*责任作者，教授，
Degradation of Rhodamine B by FeMnCoNi-O activated potassium persulfate
Bang-li XU , Hai-xian YAN, Shi-ya WENG, Shi-qi WANG, Feng FANG*
Affiliations
  • School of Materials Science and Engineering, Southeast University, Nanjing 211189, China
出版时间: 2025-02-20
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摘要
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以乙酸盐和柠檬酸钠为原料,通过共沉淀-热处理法合成了结构稳定且性能优良的FeMnCoNi-O纳米颗粒,使用XRD，TEM，FT-IR，TG，ICP，XPS等手段对其进行表征,并将其应用于常温常压下活化过硫酸氢钾(PMS)降解罗丹明B(RhB),探究PMS浓度、RhB浓度、污染物种类、FeMnCoNi-O浓度、初始pH值、水中阴离子种类等反应条件对降解效果的影响,以及FeMnCoNi-O纳米颗粒的循环使用性能.结果表明,经过200℃保温2h后样品从普鲁士蓝类似物转变为多元金属氧化物,活化PMS降解RhB能力显著提高.FeMnCoNi-O纳米颗粒可以通过活化微量的PMS(0.2mmol/L),在10min内实现RhB(20mg/L)的完全降解.自由基淬灭和XPS结果表明,体系中主要活性物质为过硫酸氢根活化生成的1O2和SO4·—.

污水处理  /  高级氧化  /  多元金属氧化物  /  PMS活化  /  罗丹明B降解

FeMnCoNi-O nanoparticles (NPs) with outstanding structural stability and catalytic performance were synthesized by coprecipitation and consequent calcination method. The FeMnCoNi-O NPs were carefully characterized by X-Ray diffraction (XRD), transmission electron microscope (TEM), Fourier transform infrared spectroscopy (FT-IR), thermal gravimetric analyzer (TG) and X-ray photoelectron spectroscopy (XPS) techniques. Furthermore, the obtained catalyst was applied to activate potassium persulfate (PMS) and degrade Rhodamine B (RhB). The effects of reaction conditions such as the concentration of the RhB, PMS and catalysts concentration, the kinds of pollutant and aqueous pH values, on the degradation process and the recycling performance were systematically investigated. Via the calcined treatment (200℃, 2h), the final product was the multi-metal oxide, which exhibited enhanced catalytic performance for the RhB degradation. FeMnCoNi-O NPs can achieve complete degradation of RhB (20mg/L) in 10minutes by activating trace amounts of PMS (0.2mmol/L). With the help of free radical quenching experiment and XPS analysis, it is found the main active substances in the degradation system were 1O2 and SO4·- generated via persulfate activation.

wastewater treatment  /  advanced oxidation  /  multi-metal oxides  /  PMS activation  /  RhB degradation
徐邦利, 严海线, 翁诗雅, 王世琦, 方峰. FeMnCoNi-O活化过硫酸氢钾降解罗丹明B. 中国环境科学, 2025 , 45 (2) : 759 -767 .
Bang-li XU, Hai-xian YAN, Shi-ya WENG, Shi-qi WANG, Feng FANG. Degradation of Rhodamine B by FeMnCoNi-O activated potassium persulfate[J]. China Environmental Science, 2025 , 45 (2) : 759 -767 .
正文
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人类活动给自然水体带去大量有机污染物[1]，如有机染料、有机农药、抗生素等.传统处理技术如活性炭吸附[2]、膜分离法[3]、生物吸附和降解[4]等存在一定局限性，无法满足污水处理需求，长此以往将严重影响我国水资源安全.
高级氧化工艺（AOPs）是目前应用前景最广阔的污水处理技术之一，它通过生成强氧化性自由基（如SO4·—和⋅OH）而高效的氧化和降解污染物[5-6].相关研究中，H2O2只有在初始pH为碱性时才能正常被活化[7]，且通过掺杂金属离子活化H2O2生成强氧化性自由基（⋅OH和O2·—），离子泄露严重[8].但过硫酸氢钾（PMS）同样可以活化生成强氧化性物质且受pH值影响较小.PMS可以被超声、光、热、电、过渡金属离子等活化，以过渡金属活化最为经济高效，其中又以Co金属[9]性能最佳，Wang等[10]通过水热法制备的Co-MOF在10min内完全降解10mg/L的RhB.当前的研究中也多采用Co及其化合物来活化PMS[11].但Co金属本身价格昂贵且有较大毒性，制备的金属有机骨架（MOF）结构下离子泄露会导致严重后果[12]，因此研究人员希望得到Co含量低但性能优异的PMS活化剂.
过渡金属催化活化PMS有诸多研究应用，但常用的非Co单金属基催化剂往往活化效率低[13]，如α-MnO2降解20mg/L的RhB耗时近60min[14].双金属主元催化剂能够利用金属间的协同作用提高活化性能[15]，如Fe3O4-MnO2协同活化PMS在30min内完全降解50mg/L的4-氯酚[16]，通过促进反应中的电子转移，提高降解有机物效率[17]，因此可以通过制备多金属氧化物，在降低Co含量的同时高效降解有机污染物.普鲁士蓝类似物（PBA）是依靠金属离子和氰化物之间的配位作用形成的多金属化合物[18-19]，目前在储能[20]与能量转换应用[21]等领域已有深入研究，其独特分子构型为导电金属离子提供支撑结构，易制备得到多金属主元产物.常见的PBA制备方法有水热法[22]和共沉淀[23]，但PBA本身结构稳定性差[24]，多通过对其进行煅烧改性从而稳定其性能[25].
本文采用共沉淀法制备了FeMnCoNi PBA，然后通过煅烧改性得到其稳定的氧化物（FeMnCoNi-O），以RhB为目标污染物探究其活化PMS去除有机污染物的能力及相关因素的影响，并通过多种测试手段分析反应过程中的变化，为FeMnCoNi-O活化PMS降解有机污染物的应用研究提供适当的实验支撑和理论依据.
1　材料与方法
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1.1　实验药品
实验以罗丹明B（AR，天津市致远化学试剂有限公司）为模型污染物，亚甲基蓝（MB，97%）、甲基橙（MO，85%）、刚果红（CR，98%）、孔雀石绿（MG，99%）等有机污染物购自天津市致远化学试剂有限公司，钴氰化钾（AR）、铁氰化钾（99%）、三醋酸锰二水合物（98%）、乙酸镍四水合物（AR）、过硫酸氢钾（4.50%）、L-组氨酸（99%）购自上海麦克林生化科技有限公司，十二水合磷酸钠（98.00%）、甲醇（99.50%）、叔丁醇（98%）购自上海凌峰化学试剂有限公司，除此之外涉及到的药品皆为分析纯，购自国药集团化学试剂有限公司.
1.2　FeMnCoNi基金属氧化物的制备
1）取0.746g乙酸镍四水合物、1.0724g三醋酸锰二水合物和2.0587g二水合柠檬酸钠加入60mL去离子水中，搅拌30min获得溶液A.
2）取0.066g铁氰化钾和0.066g钴氰化钾加入40mL去离子水中，搅拌30min获得溶液B.
3）将溶液B逐滴加入溶液A中并搅拌，滴加完毕后再搅拌30min.
4）将混合物密封静置老化24h，得到的沉淀物离心后分别使用去离子水和乙醇洗涤，60℃下真空干燥后研磨，得到FeMnCoNi PBA.
5）将FeMnCoNi PBA置于200℃下保温2h，最终得到FeMnCoNi基金属氧化物（FeMnCoNi-O）.
1.3　表征
FeMnCoNi PBA及氧化物的结构表征如下：通过X射线衍射仪（XRD，型号D8-Discover）对样品的晶相进行分析，以Cu Kα1为射线源，扫描角度（2θ）在10°~80°，扫描速度为0.15s/step；通过高分辨透射电镜（型号Talos F200X）及其配备的EDS能谱仪对样品的结构和元素分布进行分析；通过傅里叶红外光谱仪（FT-IR，型号Nicolet iS10）对样品的化学键变化进行分析；通过紫外可见分光光度计（UV-Vis，型号Cary 5000）进行污染物的定量测定；通过电感耦合等离子体光谱仪（ICP，型号SPECTROBLUE ICP-OES）进行离子泄露情况分析；通过X射线光电子能谱（XPS）分析样品表面化学价态.
1.4　性能测试
在室温（25℃）下，以浓度为40mg/L的RhB溶液为污染物代表，以浓度为20g/L的Na2S2O3为淬灭剂.量取100mL配制好的RhB溶液倒入烧杯中，搅拌10min后取样记为初始样品，然后加入10mg的FeMnCoNi-O，黑暗条件下搅拌反应0.5h后取样，加入1mL 0.02mol/L的PMS溶液，搅拌并自加入PMS时开始计时，每隔相同时间取样，至溶液完全变为无色.将水样通过0.22µm滤膜过滤，测其在554nm处的吸光度，即可得到RhB的剩余量.探究催化剂对不同污染物（RhB，MB，MO，CR，MG，浓度为40mg/L）的催化效果，以及不同阴离子（PO43-，HPO42-，Cl-，SO42-，SO32-，CO32-，浓度为0.2mol/L）影响、不同催化剂投加量（5，10，15，20，25，30mg）、不同PMS浓度（0.01，0.02，0.03，0.04，0.05mol/L）、不同pH值（3，5，7，9，11）和样品的重复性时，实验条件与上述保持一致.且为避免实验的偶然性，性能类实验均做3组平行实验，取平均值.
加入一定量的淬灭剂如L-组氨酸（L-Histidine）、甲醇（MeOH）和叔丁醇（TBA），进行催化RhB实验，确定系统中的活性氧物种（ROS）类型.L-组氨酸可以清除单线态氧（1O2），甲醇能同时捕获羟基自由基（⋅OH）和硫酸根自由基（SO4·-），当羟基自由基和硫酸根自由基共存时，叔丁醇会捕获羟基自由基[26].
2　结果和讨论
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2.1　FeMnCoNi-O的表征
图1（a）（h）与（i）（m）分别为FeMnCoNi PBA与氧化物的高角度环形暗场图像，可以看到PBA样品具有规则的立方体结构，而氧化物的立方体结构被部分破坏形成较不规则的块状堆积物；图1（b）~（d），（f）~（h）为FeMnCoNi PBA的EDS-Mapping，能明显的看出PBA样品元素均匀分布在立方体内外，不存在聚集情况；但图1（k）和（p）中可以看出氧化物中Fe和Ni元素分布不均匀，Fe元素在立方体内部有明显聚集，而Ni元素存在于立方体表面内外Fe原子稀疏的地方，形成较为明显的实心核壳结构.Mn元素和Co元素分布较为均匀，且O元素分布情况证明保温后的生成物中氧元素均匀分布.表1为FeMnCoNi-O样品的具体元素含量，其中以Mn元素含量居多.
合成的FeMnCoNi PBA与氧化物的XRD图谱如图2所示，可以看到FeMnCoNi PBA与标准卡片（JCPDS#77-1161）基本匹配，2θ在17.374°、24.666°、35.164°和39.477°处的衍射峰分别对应钴氰化物的（2 0 0）、（2 2 0）、（4 0 0）和（4 2 0）晶面；FeMnCoNi-O粉末样品的衍射峰与标准样品（JCPDS#88-1937）基本匹配，2θ在35.472°、43.111°和62.608°处的衍射峰分别对应镁铁矿（MgFe2O4）的（3 1 1）、（2 0 0）、（4 4 0）晶面.证明经过热处理后，样品的晶体结构由PBA向金属氧化物转变.
图3（a）所示为FeMnCoNi PBA的热重分析结果，可以看出约在150℃左右时PBA开始向氧化物发生转变，在250℃时完全转变为氧化物，因此可通过在200℃时的长时间热处理使PBA转变为金属氧化物.通过傅里叶红外光谱仪来分析转变中化学键变化如图3（b）所示，光谱中位于2149和2048cm-1处的尖峰表示的是金属氰化物的拉伸振动，这是普鲁士蓝类似物的特征峰[27]，FeMnCoNi-O的FT-IR图谱中没有氰化物的特征峰.1600和1400cm-1左右的峰可能源于羧酸（-COO-）基团的对称和不对称振动[28]，保温后羧酸基团部分被氧化故检测信号变弱.
2.2　FeMnCoNi-O的有机物降解
图4（a）是RhB降解性能空白对照试验，在降解实验前首先对样品进行吸附平衡试验，以消除可能存在的样品吸附对实验结果的影响，即时间0之前的数据.如图所示，在只加入FeMnCoNi-O或PMS时RhB几乎不发生降解，表明FeMnCoNi-O或PMS本身没有降解RhB的能力；FeMnCoNi PBA活化PMS能力弱，反应8min时残余污染物浓度高于60%；FeMnCoNi-O因其具有尖晶石结构，且热处理后原PBA结构被破坏金属离子容易与外界发生电子转移，故而拥有较强的活化PMS能力，在反应8min左右时污染物基本完全降解[29].Wang等[30]研究了NiFe2O4活化PMS降解苯甲酸的性能，实验证明双组元过渡金属催化活化效果高于单组元，本实验进行了三组元与四组元的样品性能对比.如图4（b）所示，在相同的实验条件下，四元FeMnCoNi-O的降解速率最高，三元FeMnNi-O的降解效率最低，与Wei等[31]描述的过渡金属活化PMS能力强弱程度（Co>Ni>Mn>Fe）一致.过渡金属元素通过电子转移激活PMS，相较于Ni4+/Ni2+（E0=1.59V）、Mn3+/Mn2+（E0=1.50V）、Fe3+/Fe2+（E0=0.771V）、Co3+/Co2+（E0=1.92V）具有较高的标准还原电位，因此Co单元素的活化能力最强，三元FeMnNi-O的电子转移能力在同样情况下最弱，而在金属协同作用存在的情况下，四元FeMnCoNi-O的电子转移能力最强.
由图5（a）可以看到，降解效率随PMS浓度的增加先提高后降低，在样品投加量为10mg，PMS浓度在0.04mol/L时达到样品活化能力顶点.之后，过量的硫酸根自由基发生了自淬灭（式（1））或与过硫酸氢根发生反应失去活性[18]（式（2））.
由图5（b）可以看出，降解效率随着投加量的增加呈正相关，理论上随着投加量增加会有更多的催化活性位点，但投加量在10~25mg时活化PMS效果接近，可能是由于同时生成的过量强氧化性自由基间存在竞争性自淬灭[32].
由图6（a）可以看出，FeMnCoNi-O样品能活化PMS降解多种有机污染物，普适性良好.由图6（b）可以看出，FeMnCoNi-O样品受OH-的影响比较大，在弱碱情况下降解效果最好，但强碱性情况下很难活化PMS发生作用，这与前人的研究结果相吻合[12]；样品受H+影响较小，在中性和酸性条件下降解效果都较好.图6（c）为在高浓度（0.2mol/L）的不同种类阴离子影响下的降解情况，可以看出Cl-和SO42-对PMS的活化起到轻微的促进作用，氯离子促进是因为ClOH·-生成速率与其分解速率相近，酸性条件下会倾向于形成强氧化性的Cl2·-[33]；HPO42-因为会与生成的硫酸根自由基反应所以有一定的抑制作用；PO43-、SO32-、CO32-在高浓度下会与自由基离子进行电子争夺从而生成对应的弱氧化性磷酸氢根自由基、亚硫酸氢根自由基、碳酸氢根自由基等，导致完全抑制样品对PMS的活化[34].综上所述，样品在较宽的pH值对多种有色污染物都有较好的降解能力，且适合在氯盐和硫酸盐浓度高的废水中使用.
2.3　活性物种的鉴定
实验分别采用不同浓度的甲醇、叔丁醇、L-组氨酸作为淬灭剂，来鉴定体系中存在的活性氧物种及其在反应体系中对RhB降解的贡献，实验结果如图7（a）所示.为更清晰的比较各淬灭剂对降解反应的抑制情况，使用伪一阶反应动力学模型（方程（3））来描述RhB的降解.
式中：C是时间t处RhB的浓度；C0是初始RhB的浓度；k是伪一阶速率常数. RhB降解与伪一级反应动力学模型拟合良好，如图7（b）所示，拟合参数见表2.
自由基淬灭反应中，TBA浓度从0.1mol/L提升到1mol/L时，样品活化PMS效果反而有轻微提高，说明反应过程中羟基自由基完全不发挥作用.但MeOH浓度从0.5mol/L提高到2mol/L时，k值从约0.19min-1降低到0.085min-1，反应速率降低一半，说明硫酸根自由基（SO4·-）在反应中发挥一定作用[35].非自由基淬灭反应可以看出L-组氨酸对反应速率的影响非常明显，L-组氨酸浓度为1mmol/L时k值从约0.24min-1降低到0.11min-1，L-组氨酸浓度从1mmol/L增加到10mmol/L时样品降解效果几乎完全被抑制.拟合结果直观的展现了L-组氨酸的抑制效果，10mmol/L的L-组氨酸对应的一阶速率常数接近于0，因此认为反应过程中单线态氧（1O2）起到关键作用[36]，可能是主要活性物质或者关键步骤反应物质.
为进一步了解FeMnCoNi-O在PMS活化过程中的作用，采用XPS测定了其反应前后的化学态.如图8所示，每种元素的结合能由C1s峰（284.8eV）校正.图8（a）（e）、（c）（g）、（d）（h）分别为反应前后Fe、Co、Ni的XPS精细谱图，分峰结果表明这3种金属离子的化学价态没有明显变化，说明反应后这些元素没有明显电子得失，结合前文三元金属氧化物实验结果，推测Fe、Co、Ni 3种金属离子参与反应中的电子传输.图8（b）（f）为Mn 2p能级反应前后精细谱图，可以看到反应前的Mn 2p在640.6、646.4、651.3、657.6eV处呈现4个峰，反应后的Mn 2p在637.3、642.9、647.8、654.4eV处呈现4个峰，根据文献，646.4和657.6eV处的峰归因于Mn（Ⅲ），642.9和654.4eV处的峰归因于Mn（Ⅱ）[37]，反应后Mn元素化学价态由+3价变为+2价说明在反应过程中Mn元素得到电子被还原.
基于自由基淬灭实验和上述研究结果，FeMnCoNi-O活化PMS降解RhB的机理如图9所示.根据图4（a）实验结果可知PMS会发生自分解（见反应式（4））但较为缓慢[38]，而PMS在弱碱性条件下降解效果最优（图6（b））是因为有少量PMS水解为SO52-，与HSO5—反应生成1O2（反应式（5~6））.图1（k）（p）明显看出FeMnCoNi-O样品为实心核壳结构，故PMS被样品吸附后表面Co，Mn，Ni的活性位点先接触到HSO5—发生氧化还原反应，如反应式（7~10）所示，产生SO4·-和SO5·-[33].由于不同金属间的标准氧化还原电位不同，高价态的金属离子与二价Mn、Fe离子间发生电子转移（反应式（11~12，15~16））[39-41]，反应式（7~8，10~12，15~16）中金属离子之间形成循环，协同活化PMS.SO5·-能与自身反应生成1O2，也能在水环境中生成HSO4—和1O2（反应式（13~14））[42].Fe元素因聚集在催化剂内部，活性位点未暴露在外，在反应中起电子传输作用（反应式（15~16））[37]，加速反应中各部分的电子得失.最后，RhB被SO4·-和1O2降解为小分子无毒物质（反应式（17））.
2.4　FeMnCoNi-O的稳定性
对样品进行多轮循环试验，取反应30min时的样品与反应前做污染物残留对比，结果如图10所示，可以看出样品在反应中表现较为良好，第4轮仍然在30min内降解了80%以上，活化PMS性能未发生大幅度下降.图11（a）（b）分别为反应前后的FT-IR图和XRD图谱，反应前后物质的基本峰型和强度几乎未变化，表明反应前后样品物相结构未发生明显变化，稳定性较好.表3为ICP测定的反应时离子泄漏情况，Co离子的析出浓度小于0.0021mg/L，离子泄露程度低.Jing Di等人通过在稻壳上生长Co3O4纳米片以减少Co的析出[12]，ICP测得其析出最少的Co3O4-0.5RHA中浸出离子浓度为0.0125mg/L，比本样品高出一个数量级，而制备的Co3O4纳米颗粒Co离子泄露浓度是本样品的百倍以上.
3　结论
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3.1　以乙酸盐和柠檬酸钠为原料，通过共沉淀-热处理法合成了具有实心核壳结构的FeMnCoNi-O纳米颗粒.
3.2　在0.10g/L FeMnCoNi-O和0.04mol/L PMS条件下，催化体系对60mg/L RhB在10min内去除率达到100%.
3.3　该催化体系的pH值适用范围广，适合在富含氯盐和硫酸盐的水体中使用，FeMnCoNi-O纳米颗粒的结构和催化性能稳定，具有较好的重复性能且Co离子泄露小于0.0021mg/L，对环境友好.
3.4　自由基淬灭实验和XPS实验分析表明，1O2和SO4·—是主要的活性物质，金属离子间的协同作用有效促进PMS活化.
基金
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  • 国家自然科学基金资助项目(52171110)
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  • 首发时间：2026-03-17
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  • 收稿日期：2024-07-01
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    东南大学材料科学与工程学院，江苏 南京 211189

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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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