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Article(id=1234106387282850568, tenantId=1146029695717560320, journalId=1234093305789726721, issueId=1234106384963400440, 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=1732550400000, receivedDateStr=2024-11-26, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1772163491316, onlineDateStr=2026-02-27, pubDate=1750348800000, pubDateStr=2025-06-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1772163491316, onlineIssueDateStr=2026-02-27, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1772163491316, creator=13701087609, updateTime=1772163491316, updator=13701087609, issue=Issue{id=1234106384963400440, tenantId=1146029695717560320, journalId=1234093305789726721, year='2025', volume='45', issue='6', pageStart='2961', pageEnd='3552', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=1, specialIssue=null, createTime=1772163490763, creator=13701087609, updateTime=1772163969484, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1234108392948682946, tenantId=1146029695717560320, journalId=1234093305789726721, issueId=1234106384963400440, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1234108392948682947, tenantId=1146029695717560320, journalId=1234093305789726721, issueId=1234106384963400440, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=3063, endPage=3072, ext={EN=ArticleExt(id=1234106388205597450, articleId=1234106387282850568, tenantId=1146029695717560320, journalId=1234093305789726721, language=EN, title=Activated carbon catalytic membrane for persulfate activation of ammonia nitrogen oxidation in water, columnId=1234106386360103680, journalTitle=China Environmental Science, columnName=Water Pollution Control, runingTitle=null, highlight=null, articleAbstract=

A novel catalytic membrane (AC-MgO@PVDF) was fabricated by loading activated carbon (AC) and MgO onto a poly (vinylidene fluoride) (PVDF) membrane using a vacuum filtration method. The as-prepared catalytic membrane (AC-MgO@PVDF) was employed to activate persulfate (PS) for the oxidation of ammonia nitrogen (NH4+-N) in aqueous solution. The structure and elemental composition of the catalytic membrane were characterized by SEM, Raman and XPS. The efficiency and mechanism of NH4+-N oxidation by the AC-MgO@PVDF/PS system were investigated. The results showed that under the conditions of a flow rate of 1mL/min, a PS dosage of 8g/L and an AC loading of 4.8mg/cm2, the removal rate of 30mg N/L NH4+-N and the nitrogen gas (N2) selectivity of the NH4+-N oxidation products reached 100% and 91.7%, respectively, after 25min of operation. The system exhibited a broad pH tolerance range (3~12) and was barely affected by common anions and natural organic matters in water body. Even after 240min of continuous operation, the system could still achieve a removal rate of over 60% for NH4+-N. Quenching experiments, EPR measurements, and electrochemical tests revealed that f NH4+-N was primarily oxidized through a non-radical pathway, with direct electron transfer being the main mechanism for its oxidation to N2.

, correspAuthors=Yong LIU, 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=Han-ling JIANG, Chen-xi WU, Ai-juan ZHOU, Xiao-bo GONG, Jin-wen WANG, Yong LIU), CN=ArticleExt(id=1234106397756027164, articleId=1234106387282850568, tenantId=1146029695717560320, journalId=1234093305789726721, language=CN, title=活性碳催化膜活化过硫酸盐氧化水中氨氮, columnId=1234106386565624579, journalTitle=中国环境科学, columnName=水污染与控制, runingTitle=null, highlight=null, articleAbstract=

通过真空抽滤的方法，以聚偏氟乙烯(PVDF)膜为基底，制得负载活性碳(AC)与MgO的催化膜(AC-MgO@PVDF)，搭建了一个用于活化过硫酸盐(PS)的膜体系(AC-MgO@PVDF/PS)，用于氧化水中的氨氮(NH4+-N).采用SEM、Raman和XPS等对催化膜的结构和元素组成进行了表征，探讨了NH4+-N在AC-MgO@PVDF/PS中的氧化效能和机制.结果表明，在流速1mL/min、PS投加量8g/L和AC负载量4.8mg/cm2的条件下运行25min后，对浓度为30mg N/L的NH4+-N的去除率和氧化产物的氮气(N2)选择性分别达到100%和91.7%.该体系具有较宽的初始pH值适用范围(3~12)，基本不受水体中常见阴离子和天然有机物的影响.体系连续运行240min仍能达到60%以上的NH4+-N去除率.猝灭实验、EPR测定及电化学测试结果表明，水中NH4+-N主要通过非自由基途径被氧化去除，其中直接电子转移途径是其氧化为N2的主要机制.

, correspAuthors=刘咏, authorNote=null, correspAuthorsNote=
* 责任作者，教授，
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蒋函灵(1999-)，女，四川中江人，四川师范大学硕士研究生，主要从事氨氮废水处理技术方向研究.发表论文2篇..

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蒋函灵(1999-)，女，四川中江人，四川师范大学硕士研究生，主要从事氨氮废水处理技术方向研究.发表论文2篇..

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蒋函灵(1999-)，女，四川中江人，四川师范大学硕士研究生，主要从事氨氮废水处理技术方向研究.发表论文2篇..

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Water Research，221:118797., articleTitle=Peroxydisulfate activation by sulfur-doped ordered mesoporous carbon: insight into the intrinsic relationship between defects and 1O2 generation, refAbstract=null)], funds=[Fund(id=1234106411593036040, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1234106387282850568, awardId=52070136, language=CN, fundingSource=国家自然科学基金(52070136), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1234106398196429137, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1234106387282850568, xref=1., ext=[AuthorCompanyExt(id=1234106398204817747, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1234106387282850568, companyId=1234106398196429137, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.College of Chemistry and Materials Science, Sichuan Normal University, Chengdu 610066, China), AuthorCompanyExt(id=1234106398217400662, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1234106387282850568, companyId=1234106398196429137, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.四川师范大学化学与材料科学学院，四川 成都 610066)]), AuthorCompany(id=1234106398372589933, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1234106387282850568, xref=2., ext=[AuthorCompanyExt(id=1234106398393561456, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1234106387282850568, companyId=1234106398372589933, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2.Key Laboratory of Treatment for Special Wastewater of Sichuan Province Higher Education System, Chengdu 610066, China), AuthorCompanyExt(id=1234106398557139321, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1234106387282850568, companyId=1234106398372589933, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2.四川省高校特种废水处理重点试验室，四川 成都 610066)])], figs=[ArticleFig(id=1234106404454331281, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1234106387282850568, language=EN, label=Fig.1, caption=Photographs of PVDF and AC-MgO@PVDF catalytic membrane, SEM images of AC-MgO@PVDF catalytic membrane and AC before and after reaction, figureFileSmall=PRnIeE77tHfRx1knnfRNwQ==, figureFileBig=aUifuep/R+BHKK7y9hoeiA==, tableContent=null), ArticleFig(id=1234106405934920613, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1234106387282850568, language=CN, label=图1, caption=PVDF膜和AC-MgO@PVDF催化膜的实物及反应前后AC-MgO@PVDF催化膜和AC的SEM图, figureFileSmall=PRnIeE77tHfRx1knnfRNwQ==, figureFileBig=aUifuep/R+BHKK7y9hoeiA==, tableContent=null), ArticleFig(id=1234106406283047870, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1234106387282850568, language=EN, label=Fig.2, caption=Raman spectra of AC before and after reaction, infrared spectra of AC before and after reaction, figureFileSmall=+G9C9XP0kqRKR4qBc9wHpw==, figureFileBig=ynqf9s523jvOZzwHxWfKIQ==, tableContent=null), ArticleFig(id=1234106406408877004, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1234106387282850568, language=CN, label=图2, caption=反应前后AC的拉曼光谱图，反应前后AC的红外谱, figureFileSmall=+G9C9XP0kqRKR4qBc9wHpw==, figureFileBig=ynqf9s523jvOZzwHxWfKIQ==, tableContent=null), ArticleFig(id=1234106406639563743, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1234106387282850568, language=EN, label=Fig.3, caption=XPS spectra of AC before and after reaction, figureFileSmall=rZENzWFRDhkTX+/3t60ehg==, figureFileBig=2eI+2jcs2+ADkG2zGDxREg==, tableContent=null), ArticleFig(id=1234106406803141612, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1234106387282850568, language=CN, label=图3, caption=反应前后AC的XPS光谱, figureFileSmall=rZENzWFRDhkTX+/3t60ehg==, figureFileBig=2eI+2jcs2+ADkG2zGDxREg==, tableContent=null), ArticleFig(id=1234106406991885301, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1234106387282850568, language=EN, label=Fig.4, caption=Removal efficiency of NH4+-N in different systems, figureFileSmall=WtPN7dSC3l8jpmTL9J/7Jg==, figureFileBig=zBp7ECMPV1f6IECV4H+Lnw==, tableContent=null), ArticleFig(id=1234106407168045057, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1234106387282850568, language=CN, label=图4, caption=不同体系中NH4+-N的去除率

实验条件为PS:8g/L，MgO:5g/L，AC:4.8mg/cm2，流速：1mL/min，NH4+-N:30mg N/L

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活性碳催化膜活化过硫酸盐氧化水中氨氮
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蒋函灵 1 , 吴晨曦 1 , 周艾娟 1 , 龚小波 1, 2 , 王晶文 1, 2 , 刘咏 1, 2, *
中国环境科学 | 水污染与控制 2025,45(6): 3063-3072
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中国环境科学 | 水污染与控制 2025, 45(6): 3063-3072
活性碳催化膜活化过硫酸盐氧化水中氨氮
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蒋函灵1 , 吴晨曦1, 周艾娟1, 龚小波1, 2, 王晶文1, 2, 刘咏1, 2, *
作者信息
  • 1.四川师范大学化学与材料科学学院，四川 成都 610066
  • 2.四川省高校特种废水处理重点试验室，四川 成都 610066

    • 蒋函灵(1999-)，女，四川中江人，四川师范大学硕士研究生，主要从事氨氮废水处理技术方向研究.发表论文2篇..

通讯作者:

* 责任作者，教授，
Activated carbon catalytic membrane for persulfate activation of ammonia nitrogen oxidation in water
Han-ling JIANG1 , Chen-xi WU1, Ai-juan ZHOU1, Xiao-bo GONG1, 2, Jin-wen WANG1, 2, Yong LIU1, 2, *
Affiliations
  • 1.College of Chemistry and Materials Science, Sichuan Normal University, Chengdu 610066, China
  • 2.Key Laboratory of Treatment for Special Wastewater of Sichuan Province Higher Education System, Chengdu 610066, China
出版时间: 2025-06-20
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摘要
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通过真空抽滤的方法，以聚偏氟乙烯(PVDF)膜为基底，制得负载活性碳(AC)与MgO的催化膜(AC-MgO@PVDF)，搭建了一个用于活化过硫酸盐(PS)的膜体系(AC-MgO@PVDF/PS)，用于氧化水中的氨氮(NH4+-N).采用SEM、Raman和XPS等对催化膜的结构和元素组成进行了表征，探讨了NH4+-N在AC-MgO@PVDF/PS中的氧化效能和机制.结果表明，在流速1mL/min、PS投加量8g/L和AC负载量4.8mg/cm2的条件下运行25min后，对浓度为30mg N/L的NH4+-N的去除率和氧化产物的氮气(N2)选择性分别达到100%和91.7%.该体系具有较宽的初始pH值适用范围(3~12)，基本不受水体中常见阴离子和天然有机物的影响.体系连续运行240min仍能达到60%以上的NH4+-N去除率.猝灭实验、EPR测定及电化学测试结果表明，水中NH4+-N主要通过非自由基途径被氧化去除，其中直接电子转移途径是其氧化为N2的主要机制.

废水处理  /  高级氧化  /  催化膜  /  氨氮  /  氮气选择性

A novel catalytic membrane (AC-MgO@PVDF) was fabricated by loading activated carbon (AC) and MgO onto a poly (vinylidene fluoride) (PVDF) membrane using a vacuum filtration method. The as-prepared catalytic membrane (AC-MgO@PVDF) was employed to activate persulfate (PS) for the oxidation of ammonia nitrogen (NH4+-N) in aqueous solution. The structure and elemental composition of the catalytic membrane were characterized by SEM, Raman and XPS. The efficiency and mechanism of NH4+-N oxidation by the AC-MgO@PVDF/PS system were investigated. The results showed that under the conditions of a flow rate of 1mL/min, a PS dosage of 8g/L and an AC loading of 4.8mg/cm2, the removal rate of 30mg N/L NH4+-N and the nitrogen gas (N2) selectivity of the NH4+-N oxidation products reached 100% and 91.7%, respectively, after 25min of operation. The system exhibited a broad pH tolerance range (3~12) and was barely affected by common anions and natural organic matters in water body. Even after 240min of continuous operation, the system could still achieve a removal rate of over 60% for NH4+-N. Quenching experiments, EPR measurements, and electrochemical tests revealed that f NH4+-N was primarily oxidized through a non-radical pathway, with direct electron transfer being the main mechanism for its oxidation to N2.

wastewater treatment  /  advanced oxidation  /  catalytic membrane  /  ammonia nitrogen  /  nitrogen gas selectivity
蒋函灵, 吴晨曦, 周艾娟, 龚小波, 王晶文, 刘咏. 活性碳催化膜活化过硫酸盐氧化水中氨氮. 中国环境科学, 2025 , 45 (6) : 3063 -3072 .
Han-ling JIANG, Chen-xi WU, Ai-juan ZHOU, Xiao-bo GONG, Jin-wen WANG, Yong LIU. Activated carbon catalytic membrane for persulfate activation of ammonia nitrogen oxidation in water[J]. China Environmental Science, 2025 , 45 (6) : 3063 -3072 .
正文
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目前，废水中NH4+-N的去除方法主要包括物理化学分离法(膜分离、吸附、吹脱和离子交换法等)、生物转化法(硝化-反硝化法和厌氧氨氧化法)和化学氧化法(折点加氯法和高级氧化法)等[1-3].其中，膜分离法和高级氧化法(AOPs)因其性能优异、操作简便而日益受到水处理领域的关注[4].膜分离法面临着高浓度NH4+-N浓缩液的处理难题;过硫酸盐(PS)AOPs通过产生羟基自由基(HO•,E0=1.9~2.8V)、硫酸根自由基(SO4•−,E0=2.5~3.1V)和单线态氧(1O2,E0=2.2V)等强氧化性活性物种(ROS)[5-6]，能有效氧化水中的NH4+-N.但是PS活化剂主要是微纳米颗粒，存在易流失、分离困难等缺点，难以实际工程应用[7].为此，将活化剂负载在膜材料上的催化膜技术兼具膜分离和AOPs优点，在去除废水中NH4+-N方面具有很大的潜力.
活化PS会导致溶液酸化，使水中NH4+-N主要以NH4+形态存在，会降低其反应活性[8].在反应体系中加入环保、经济且来源广泛的固体碱可有效解决此问题.基于PS的AOPs体系(PS-AOPs)氧化NH4+-N过程中存在的一个最大难题是产生的ROS容易将NH4+-N过度氧化为亚硝酸盐(NO2−)或硝酸盐(NO3−)，造成二次污染[9].针对此难题，课题组前期的工作中发现，在光活化PS的AOPs体系中加入还原助剂如低价铁、亚硫酸盐等作为调节剂，可以极大地提高氧化NH4+-N为氮气(N2)的选择性[10-11].已有研究发现在Cl−存在的条件下，通过Fe2+活化PS氧化NH4+-N，反应120min后，NH4+-N去除率为96%，产物的N2选择性达100%[12].尽管如此，这些过程需光、热等能量以及大量化学药剂的添加，既增加了运行成本，又操作不便，难以实际应用.因此，发展一种常温常压下、不添加还原助剂、且能氧化NH4+-N为N2的PS-AOPs具有较强的竞争力.
在PS活化剂中，碳材料具有来源广泛、廉价易得、环境友好等催化剂特性[13].在碳材料中，活性碳(AC)不仅含有丰富的含氧官能团如-OH、C=O、COOH等，还含有多种硫成分[14].这不仅有利于PS的高效活化，而且一些成分具有还原性，有助于抑制NH4+-N的过度氧化.
本文采用将PS-AOPs与膜分离技术相耦合的方式氧化水中NH4+-N，选择耐酸碱、具有较稳定和较长使用寿命的聚偏氟乙烯(PVDF)膜作为基底，将AC和MgO抽滤至PVDF膜上，构建一种动态的AC-MgO@PVDF催化膜体系;系统地研究了AC-MgO@PVDF催化膜体系氧化NH4+-N的效能与机制，探究AC活化PS过程中NH4+-N的氧化去除效果，探讨PS用量、AC负载量和溶液初始pH值等因素影响NH4+-N去除的规律，揭示AC-MgO@PVDF催化膜体系氧化去除NH4+-N的作用机制;并应用AC-MgO@PVDF催化膜体系去除实际废水中的NH4+-N.
1　材料和方法
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1.1　试剂
化学品包括过硫酸钾、氧化镁、浓硫酸、氢氧化钠、硫酸铵、PVDF膜(0.22µm)由成都市科龙化工试剂厂提供.叔丁醇(TBA)、甲醇(MeOH)、糠醇(FFA)、酒石酸钾钠、纳氏试剂等其他化学品购自阿拉丁试剂(上海)有限公司.除非另有说明，化学药品均为分析纯，活性炭(AC)由杭州回水科技股份有限公司提供.实验用水均为去离子水.
1.2　AC-MgO@PVDF催化膜的制备
称取60mgAC与50mgMgO置于装有50mL去离子水的100mL烧杯中，室温下磁力搅拌30min，得到AC与MgO共存的混合溶液，将该混合溶液真空抽滤到PVDF膜基底上，获得湿润的AC-MgO@PVDF催化膜，最后，自然风干12h得到AC-MgO@PVDF催化膜.
1.3　材料表征
采用15kV的扫描电镜(SEM，JSM-7500F，Jeol，日本)观察AC和AC-MgO@PVDF催化膜的表面形貌.利用LabRAM HR800光谱仪(Horiba Jobin Yvon，France)以激发波长为523nm的光源，在室温下记录拉曼光谱.使用光谱仪(Bruker Optics-Vertex 70，德国)测定材料的傅里叶变换红外(FT-IR)光谱.利用X射线光电子能谱仪(XPS，ESCALAB Xi，Thermo Scientific)对材料中所含元素进行测定.电子顺磁波谱仪(EMXnano，Bruker，德国)用于活性物种的检测.
1.4　NH4+-N氧化去除实验
将AC-MgO@PVDF催化膜安装在膜过滤装置中，为增加过滤器中AC负载量，将多层膜串联安装，采用动态流方式去除水中的NH4+-N.具体操作如下：将PS先加入到NH4+-N废水中，混匀，然后将添加有PS的废水通过蠕动泵引入到膜过滤器.混合物在重力作用下，废水穿透催化膜，产生干净的过滤水.NH4+-N浓度为30mg N/L，流速设置为1mL/min，过滤装置流出第一滴液体时开始计时.每隔一定时间采集2mL样品.在整个过程中，进料流流过膜，渗透流没有循环回进料罐.
1.5　分析测试方法
1.5.1　膜通量计算
通过测量25mL去离子水在真空泵作用下通过AC-MgO@PVDF催化膜所需的时间来计算膜通量J(LMH)，计算见公式(1).
式中：V为膜的渗透体积，L;A为膜的有效过滤面积，m2;T为膜过滤时间，h.
1.5.2　N2选择性计算
式中：S(N2)为N2选择性;ΔC(TN)、ΔC(NH4+-N)、ΔC(N2O)和ΔC(NOx)分别为总氮(TN)、NH4+-N、N2O和NOx的浓度变化量.
1.5.3　分析方法
pH计(上海利奇仪器有限公司，中国)用于测定反应溶液的pH值;采用纳氏比色法在420nm处测定NH4+-N浓度;采用碱性过硫酸钾紫外分光光度法测定水中TN浓度;用对二甲氨基苯甲醛分光光度法测定肼(N2H4)的浓度;反应过程中产生的NOx采用分光光度计测定，其原理是NOx先被三氧化铬吸收氧化为NO2，与对氨基苯磺酸和盐酸萘乙二胺反应后，生成的产物在波长为540nm处进行定量分析;一氧化二氮(N2O)采用气相色谱法测定;用空气采样器收集可能溢出的NH3，用4mmol/L硼酸吸收测定;采用离子色谱法测定溶液中生成的亚硝酸盐和硝酸盐(NOx−)的浓度.使用微软Office Excel 2010对原始数据进行处理，利用Avantage对XPS数据进行处理，其余绘图均由Origin 2021和WPS Office完成.
2　结果与讨论
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2.1　AC与AC-MgO@PVDF催化膜的表征
图1(a~d)表明，AC/MgO通过真空抽滤成功负载至PVDF膜上.由图1(b~e)发现，反应前后AC-MgO@PVDF催化膜平面较为粗糙，形貌一致，表明AC-MgO@PVDF催化膜结构相对稳定.同时，对反应前后AC的形貌进行扫描(图1c~f)，可以观察到反应前后AC的层状结构保存良好.
通过拉曼光谱仪测得拉曼图谱，并根据ID/IG的强度比评估了反应前后AC的缺陷程度.如图2(a)所示，反应后AC的ID/IG从0.91上升到了0.92，缺陷水平略微上升，这表明在活化PS氧化NH4+-N的过程中，AC的石墨化碳不断受到攻击，反应后AC的缺陷增加.
在C 1s和O 1s的XPS谱图中(图3)，反应后AC的C-O/C=O官能团(287.7eV)和C=O官能团(520.7eV)的相对强度减弱，表明C=O官能团在氧化NH4+-N的过程中被消耗[15-16]，与FT-IR结果一致，因此推测AC中的C=O官能团可能是活化PS的活化位点之一.此外，由图3(c)和3(f)可知，反应后C-S-C(165.9eV)的峰强明显降低，这可能是因为在NH4+-N氧化过程中，C-S-C作为活化PS的活性位点被消耗.除此以外，对比反应前后S 2p的光谱图，可以发现，S2−(162.4eV)的峰强有所减弱，这可能与S2−的还原性有关[17].综上，反应后催化剂AC中C=O和C-S-C的含量明显减少，说明AC中的C=O和C-S-C是AC-MgO@PVDF催化膜活化PS的主要活性位点.
2.2　催化性能
以NH4+-N去除率为指标，采用终端过滤方式对AC-MgO@PVDF催化膜的性能进行了评价.如图4所示，单独的PVDF膜对NH4+-N的去除率为0%，表明PVDF膜不能吸附去除NH4+-N.在加入PS后，PVDF/PS体系对NH4+-N的去除率为18.3%，这表明，单独的PS对NH4+-N的氧化能力是有限的.在PVDF膜上负载MgO，发现25min后NH4+-N的溢出量为0.6mg N/L，表明碱性逸散的NH4+-N对体系去除NH4+-N的影响可以忽略.在此基础上，进一步投加PS，反应25min后，MgO@PVDF/PS体系对NH4+-N的去除率为13.3%，说明单独MgO活化PS在NH4+-N氧化过程中的作用不大.同时，单独的AC-MgO@PVDF膜在25min后，对NH4+-N的去除率为11.7%，可能由于AC-MgO@PVDF催化膜对NH4+-N具有良好的吸附能力.在加入PS后，AC-MgO@PVDF催化膜对NH4+-N的去除有明显的促进作用，且NH4+-N的去除率达100%.这一结果表明AC-MgO@PVDF催化膜活化PS体系(AC-MgO@PVDF/PS)能高效氧化水中的NH4+-N.
2.3　单因素实验
2.3.1　AC负载量的影响
如图5所示，当AC负载量为2.4mg/cm2时，25min后NH4+-N去除率为77.5%(N2选择性为79.8%).当AC负载量上升到4.8mg/cm2，NH4+-N去除率升为100%(N2选择性为91.7%).这可能是由于更多的AC可以为PS活化提供更多的活性位点，从而提高ROS的生成速率，加快NH4+-N的氧化[18].然而，进一步提高AC负载量分别为9.6和19.2mg/cm2后，NH4+-N去除率分别降低为87.8%和68.6%，这是因为AC负载过多，可能屏蔽了部分活性位点，并且影响了NH4+-N在膜表面的扩散速率，导致NH4+-N氧化率下降.因此，选择4.8mg/cm2为后续研究的AC负载量.
2.3.2　PS投加量的影响
由图6可知，PS投加量从4g/L增至8g/L，体系运行25min后NH4+-N的去除率从66.6%增大到100%.这是由于PS是体系中ROS的前驱物，适量加大PS投量可增加溶液中ROS数量，从而加强NH4+-N氧化.然而，当PS投加量继续增加为12和16g/L时，NH4+-N去除率分别为88.0%和83.4%，N2选择性为90.9%和90.6%.这与PS的自淬灭有关[19]，且过量的PS会氧化NH4+-N为NOx−，导致NH4+-N的氧化效果受到抑制.进一步测定了PS投加量为8g/L的体系的出水PS浓度，发现反应25min后，有5.9g/L的PS被消耗，表明添加的PS可以在该体系中得到很好的利用，为增加PS的利用效率，将在下一步的工作中采取出水中PS循环利用的策略.
2.3.3　废水流速的影响
如图7所示，当废水流速从0.5mL/min提高到1mL/min时，NH4+-N去除率从86.3%升至100%，且N2选择性从79.8%升高为91.7%，说明AC-MgO@PVDF/PS氧化NH4+-N的性能在此范围内受传质速率控制.然而，当流速增加到2mL/min时，NH4+-N去除效率开始下降，进一步将流速增加到4mL/min时NH4+-N去除率下降至33%.这说明，在此流速条件下，NH4+-N和催化剂AC之间的传质不再是决定NH4+-N氧化速率的关键步骤.同时，单位时间内NH4+-N的负荷量随着流速的加快而增加，AC-MgO@PVDF膜上活性位点的数量成为决定NH4+-N氧化效率的主要因素.因此，后续实验采用废水流速为1mL/min.
2.3.4　初始pH值的影响
水中的NH4+-N主要以NH4+和NH3两种形式存在，并且NH3的还原性强于NH4+[20].因此，用NaOH和H2SO4调节NH4+-N溶液的初始pH值，考察溶液初始pH值对AC-MgO@PVDF/PS去除NH4+-N效能的影响.如图8所示，在初始pH值为3~12范围内，反应25min后，溶液的出水pH值均为9~10，且NH4+-N的去除率没有明显差异，均大于97%，同时均实现了较高的N2选择性(>90%).结果表明，AC-MgO@PVDF/PS可以在较宽的pH值范围内(3~12)氧化NH4+-N.这可归功于催化膜上的MgO.MgO作为固体碱能将NH4+-N转化为NH3，并且具有维持溶液pH值的缓冲作用[21].
2.3.5　NH4+-N初始浓度的影响
如图9(a)所示，当NH4+-N初始浓度从15mg N/L增加到60mg N/L时，NH4+-N去除效率从100%下降到77.7%.这是因为在固定PS投加量(8g/L)下，去除较高浓度的NH4+-N需要更多ROS.由图9(b)知，反应25min后，随着NH4+-N浓度从30mg N/L增加到60mg N/L，N2选择性从91.7%下降到83.3%.这可能是由于NH4+-N氧化过程中，AC-MgO@PVDF膜中的还原性活性位点可以抑制其过度氧化.高浓度NH4+-N需要更多的还原性活性位点才能不被ROS氧化成NOx−.因此，在AC-MgO@PVDF膜中还原性活性位点固定的条件下，NH4+-N浓度过高会产生较多NOx−，导致其N2选择性降低.
2.4　共存离子和实际废水
催化膜体系的抗干扰能力是评判其实际应用潜力的一项重要参数.Cl−、SO42−、CO32−和NO3−广泛存在于实际水体中，可能影响AC-MgO@PVDF/PS中NH4+-N的氧化去除.由图10(a~b)可知，上述阴离子对NH4+-N的氧化具有轻微的抑制作用.其原因是它们能与ROS发生反应，生成氧化能力更弱的其他自由基[22].尽管如此，在上述离子存在的情况下，NH4+-N氧化仍具有较高的N2选择性(89.4%).进一步探究有机质(腐殖酸(HA)和富里酸(FA))和水质对NH4+-N去除效能的影响.如图10(c~d)所示，向AC-MgO@PVDF/PS中分别加入10mg/L HA和10mg/L FA，NH4+-N去除率分别为85.3%和80.4%.这可能是由于有机质会与NH4+-N争夺吸附位点，导致膜表面活性位点被堵塞，也可能是因为有机质会与NH4+-N竞争ROS[23].此外，AC-MgO@PVDF/PS在处理几种实际废水时，NH4+-N的去除效率与去离子水相比稍有所降低，NH4+-N去除效率依次为城市污水(80.7%)<稀土废水(84.0%)<泡菜废水(91.6%)(图10(e~f))，这可能是由于上述实际废水中存在一些矿物质、有机质以及微生物等，它们会影响NH4+-N的氧化.尽管如此，处理实际废水时的N2选择性均在93.7%以上.这说明AC-MgO@PVDF/PS在处理实际废水方面具有较大的应用潜力.
2.5　作用机制
2.5.1　活性氧化物种的鉴定
为了明晰AC-MgO@PVDF/PS氧化NH4+-N的机制，进行了EPR、猝灭实验和电化学测试.首先，对该体系中可能存在的ROS(如：HO•、SO4•−和1O2)进行EPR测试，并以DMPO作为HO•和SO4•−的捕获剂，TEMP作为1O2的捕获剂[24].测得的DMPO•-OH与TEMP-1O2加合物谱峰如图11(a)所示，HO•和1O2的生成是符合预期的，但SO4•−加合物(DMPO•-OSO3−)的强度可以忽略不计，因为AC-MgO@PVDF催化膜中存在固体碱MgO，使得溶液pH值保持在9~10的范围内，而碱性条件下SO4•−加合物容易向DMPO•-OH转变[25].进一步通过猝灭实验揭示了HO•、SO4•−和1O2对NH4+-N氧化去除的贡献.MeOH、TBA和FFA被广泛用作活性物种的猝灭剂来区分HO•、SO4•−和1O2对污染物去除的贡献[26].由图11(b)知，MeOH、TBA和FFA(10mmol/L)均能抑制AC-MgO@PVDF/PS对NH4+-N的氧化，并且25min时NH4+-N的去除率分别为81.9%、85.0%和66.4%.进一步添加足量的猝灭剂(20mmol/L)，反应25min后，NH4+-N的去除率分别为79.9%、82.0%和58.6%.说明ROS中的1O2对NH4+-N的氧化起主要作用.除此以外，当1O2被完全捕获时，仍然有38.5%的NH4+-N被氧化去除.为此，本研究利用电化学测试(i-t和LSV测试)对AC-MgO@PVDF/PS氧化NH4+-N的电子转移过程进行了验证.由图11(c)知，在使用AC修饰玻碳旋转环形圆盘电极为工作电极、碱性硫酸钠溶液(pH=10.5)作为电解质，依次添加PS和NH4+-N分别检测到了明显的负电流和正电流响应信号，其中，负电流的产生可能是由于PS与AC表面相互作用，形成的不稳定的AC-PS*中间体，致使电子从AC向PS移动，而后，随着NH4+-N的加入，AC-PS*与NH4+-N接触时，形成AC-PS*与NH4+-N之间的电荷转移配合物，AC-PS*直接从NH4+-N中夺取电子，导致正电流的产生[27-28].该结果直接证实了AC与PS两者之间以及AC、PS与NH4+-N三者之间存在直接电子转移过程.另外，LSV的检测结果如图11(d)所示，以AC修饰玻碳旋转环形圆盘电极为工作电极时，体系在有和无NH4+-N条件下测得的LSV电流响应强度差别不大，但当NH4+-N与PS共存时的电流响应强度明显高于仅NH4+-N存在时的电流响应强度，进一步证明了AC介导了NH4+-N与PS间的电子转移.
2.5.2　NH4+-N氧化产物的鉴定
由于AC-MgO@PVDF/PS中存在ROS，可能氧化NH4+-N为NOx.为此，对可能产生的NOx进行了吸收和光谱测定，未检测到NOx，表明在NH4+-N氧化过程中没有NOx产生.此外，采用离子色谱和紫外分光光度法对NH4+-N氧化过程的中间产物进行分析测定(图12(a~b))，共检测出了NO3−、NO2−和N2H4,3种产物.为进一步探讨NH4+-N氧化途径，用PS与N2H4进行了反应，发现生成的产物是N2.这说明N2H4中间物在反应过程中不断地生成和消耗，也可解释图12(b)中N2H4的浓度在10min后基本维持在一个很低的浓度.
基于前面的表征分析、试验结果和相关文献，本文提出了AC-MgO@PVDF/PS氧化NH4+-N的作用机制(图13).在AC-MgO@PVDF/PS中，AC中含有大量的含氧基团和噻吩S，能将PS活化为ROS;同时，MgO表面丰富的碱性位点和溶于水后形成的Mg(OH)2使得NH4+-N主要以NH3存在.进一步地，NH4+-N通过两种途径被氧化.途径一：PS与AC相互作用形成AC-PS*中间体，当AC-PS*与NH4+-N接触时，形成AC-PS*与NH4+-N之间的电荷转移配合物，其中，NH4+-N将电子转移给AC-PS*后自身转化为N2;途径二：NH4+-N被ROS氧化，生成NO3−、NO2−和N2H4，其中N2H4可被PS直接氧化为N2.在这两种途径中，电子直接转移途径主导了NH4+-N选择性氧化为N2，而ROS中的1O2起到了辅助作用.
此外，与本文前期对UV/PS/CaO体系氧化NH4+-N的研究相比，NH4+-N氧化机理的差异主要体现在两个方面[27].一方面，AC-MgO@PVDF/PS主要由非自由基途径氧化NH4+-N，而UV/PS/CaO体系主要通过自由基途径氧化NH4+-N;另一方面，在UV/PS/CaO体系中，N2选择性高的主要原因是N2H4在UV和CaO的作用下与NO2−反应生成N2，而在AC-MgO@PVDF/PS中，AC中的多种硫成分促进了NH4+-N与PS之间的非自由基作用途径，从而提高了N2选择性.
2.6　实际应用潜力
催化膜能否连续稳定运行是判断其性能的关键依据.因此，探究了长期运行过程中AC-MgO@PVDF/PS对NH4+-N的去除效果(图14(a)).在NH4+-N浓度为30mg N/L，PS投加量为8g/L，AC负载量为4.8mg/cm2以及NH4+-N通量为47.8LMH的条件下，连续运行240min时，NH4+-N仍然能达到60%以上的去除效率.这表明AC-MgO@PVDF/PS具有一定的连续氧化去除NH4+-N的能力.为了使AC-MgO@PVDF/PS更高效的持续氧化NH4+-N，以25min为一个周期更换进水的表层膜片，如图14(b)所示，在125min内更换5次表层膜，每次更换后NH4+-N去除率和N2选择性分别大于96%和89%，因此，更换表层膜片可能是提高AC-MgO@PVDF/PS持续去除NH4+-N的有效手段.此外，考虑到MgO的引入会导致处理后废水呈碱性(pH=10.5)，不利于后续处理.因此，通过调整MgO的负载量，可以进一步控制处理出水的pH值.如图14(c)所示，最底层膜片不负载MgO的条件下，AC-MgO@PVDF/PS实现了88.9%的NH4+-N去除率和85.7%的N2选择性且处理后废水的pH值降至7.1，降低了实际应用过程中与溶液pH值有关的潜在风险.根据AC，MgO和PS的价格及其在水处理中的消耗，计算每去除1mg NH4+-N的药剂成本约为0.14元.此外，膜分离技术与AC活化PS的AOPs耦合，不仅减少了光电输入，使得装置简单、便于实际操作，而且NH4+-N转化为无害的N2，大大减少了二次污染，具有明显的环境效益.
3　结论
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3.1　采用真空抽滤技术制备了AC-MgO@PVDF催化膜.AC-MgO@PVDF催化膜由于AC具有丰富的活性位点(C=O与C-S-C)，能有效活化PS选择性氧化NH4+-N为N2.
3.2　AC负载量为4.8mg/cm2，废水流速为1mL/min时，AC-MgO@PVDF/PS中NH4+-N(30mg N/L)的去除率达100%，N2选择性达91.7%.
3.3　猝灭实验、EPR和电化学测试证实了1O2和直接电子转移途径对AC-MgO@PVDF/PS氧化NH4+-N的显著贡献.
3.4　常见阴离子(Cl−、SO42−、CO32−和NO3−)、有机质(HA和FA)以及实际废水对AC-MgO@PVDF/PS氧化NH4+-N的影响较小.即使在连续运行240min后，NH4+-N的去除率仍保持在60%以上.
3.5　更换表层膜能高效连续氧化NH4+-N，每次更换后NH4+-N去除率和N2选择性分别大于96%和89%.
3.6　通过减少膜片上MgO的负载量能使处理出水的pH值呈中性，且可达到88.9%的NH4+-N去除率和85.7%的N2选择性.综上，本研究开发的AC-MgO@PVDF/PS具有膜材料制备简单、运行操作简便、NH4+-N去除效率高且产物主要为N2等优点，在实际废水处理中具有广阔的应用前景.
基金
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  • 国家自然科学基金(52070136)
文献
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参考文献 引证文献
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2025年第45卷第6期
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  • 接收时间：2024-11-26
  • 首发时间：2026-02-27
  • 出版时间：2025-06-20
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  • 收稿日期：2024-11-26
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国家自然科学基金(52070136)
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    1.四川师范大学化学与材料科学学院，四川 成都 610066
    2.四川省高校特种废水处理重点试验室，四川 成都 610066

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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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