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Article(id=1234106391833662181, 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=1732118400000, receivedDateStr=2024-11-21, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1772163492401, onlineDateStr=2026-02-27, pubDate=1750348800000, pubDateStr=2025-06-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1772163492401, onlineIssueDateStr=2026-02-27, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1772163492401, creator=13701087609, updateTime=1772163492401, 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=3046, endPage=3053, ext={EN=ArticleExt(id=1234106393997923175, articleId=1234106391833662181, tenantId=1146029695717560320, journalId=1234093305789726721, language=EN, title=HA driven PM/PMS system for removing emerging contaminants and controlling membrane fouling, columnId=1234106386360103680, journalTitle=China Environmental Science, columnName=Water Pollution Control, runingTitle=null, highlight=null, articleAbstract=

The study used humic acid (HA) to drive the potassium permanganate/persulfate (PM/PMS+HA) system to investigate the removal of small molecule organic pollutants and the effectiveness of membrane fouling control. The experimental results showed that the PM/PMS+HA system exhibited excellent removal performance for different small molecule organic compounds, including Atrazine (ATZ), Phenol (Phenol), Diclofenac Sodium (DCF), Carbamazepine (CBZ), Ibuprofen (IBP) and Sulfamethoxazole (SMX). The first-order kinetic constants of the PM/PMS+HA system were all higher than 18×10-2min-1, far higher than the PM/PMS system, PM system, and ultrafiltration system alone. At the same time, the PM/PMS system has a good membrane fouling alleviation effect. When HA was used as the pollutant, the effluent specific flux of the PM/PMS system only decreased to 0.919 within 15 minutes, much higher than the 0.393 obtained by HA filtration alone. Meanwhile, when using the PM/PMS system for membrane cleaning, the membrane flux recovery rate reached 98.51%. The mechanism of the PM/PMS+HA system was explored through capture experiments and measurements using a UV spectrophotometer. The experimental results indicate that during the filtration process of PM/PMS+HA, it is mainly the rich electronic HA in the system that triggers the decomposition of the composite oxidant (PM-PMS). The decompositionof composite oxidants produces reactive oxygen species (•OH、SO4•-、1O2) and reactive manganese(Mn(V)and Mn(VI)). The generated reactive oxygen species and reactive manganese oxidize pollutants, leading to the removal of new pollutants and a decrease in the molecular weight of membrane pollutants, thereby achieving the removal of new pollutants and the control of membrane pollution. The PM/PMS system driven by pollutants has achieved the coupling of ultrafiltration membranes with advanced oxidation technology, providing new ideas for the removal of small molecule organic compounds and membrane fouling control in ultrafiltration technology.

, correspAuthors=Chun ZHAO, 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=Chao ZHANG, Qi-bin XU, Ying WANG, Suo LIU, Chun ZHAO), CN=ArticleExt(id=1234106402629800410, articleId=1234106391833662181, tenantId=1146029695717560320, journalId=1234093305789726721, language=CN, title=HA驱动PM/PMS体系去除新污染物及膜污染控制, columnId=1234106386565624579, journalTitle=中国环境科学, columnName=水污染与控制, runingTitle=null, highlight=null, articleAbstract=

本研究采用腐殖酸(HA)驱动高锰酸钾/过一硫酸盐(PM/PMS+HA)体系的方法，研究小分子有机污染物的去除并探究膜污染控制效能的内容.结果表明，对于不同小分子有机物(阿特拉津(ATZ)、苯酚(Phenol)、双氯芬酸钠(DCF)、卡马西平(CBZ)、布洛芬(IBP)磺胺甲噁唑(SMX))，PM/PMS+HA体系去除效果良好，其一级动力学常数均高于18×10-2min-1，远高于单独超滤体系、PM体系和PM/PMS体系.与此同时，PM/PMS+HA体系在膜污染缓解方面也表现良好.采用HA作为膜污染物，15min内，PM/PMS+HA体系的出水比通量仅下降至0.919，远高于单独HA过滤时的0.393.同时，采用PM/PMS体系进行膜清洗时，膜通量恢复率达到98.51%.捕获试验以及紫外分光光度计的测定探究PM/PMS+HA体系的机理表明，PM/PMS+HA过滤过程中主要是体系中富电子特性的HA引发了复合氧化剂(PM-PMS)的分解.复合氧化剂的分解产生了活性氧(•OH、SO4•-、1O2)以及活性锰(Mn(V)和Mn(VI)).产生的活性氧和活性锰对污染物的氧化导致了新污染物的去除以及膜污染物分子量的降低，从而实现了新污染的去除和膜污染的控制.污染物驱动的PM/PMS体系实现了超滤膜与高级氧化技术的耦合.

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* 责任作者，教授，;
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张超(2000-)，男，四川德阳人，重庆大学硕士研究生，主要从事过硫酸盐体系的高级氧化研究.发表论文1篇..

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张超(2000-)，男，四川德阳人，重庆大学硕士研究生，主要从事过硫酸盐体系的高级氧化研究.发表论文1篇..

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张超(2000-)，男，四川德阳人，重庆大学硕士研究生，主要从事过硫酸盐体系的高级氧化研究.发表论文1篇..

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Detection methods for different pollutants

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污染物柱温(℃)流动相(V,%)紫外波长(nm)
水甲醇乙腈0.1%3%冰0.5%
甲酸乙酸冰乙酸
IBP357030220
SMX353862265
DCF308020276
Phenol302080270
CBZ303070284
ATZ253070225
), ArticleFig(id=1234106413354635480, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1234106391833662181, language=CN, label=表1, caption=

不同污染物的检测方法

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污染物柱温(℃)流动相(V,%)紫外波长(nm)
水甲醇乙腈0.1%3%冰0.5%
甲酸乙酸冰乙酸
IBP357030220
SMX353862265
DCF308020276
Phenol302080270
CBZ303070284
ATZ253070225
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HA驱动PM/PMS体系去除新污染物及膜污染控制
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张超 1 , 许岐斌 1 , 王颖 2 , 刘索 1 , 赵纯 1, *
中国环境科学 | 水污染与控制 2025,45(6): 3046-3053
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中国环境科学 | 水污染与控制 2025, 45(6): 3046-3053
HA驱动PM/PMS体系去除新污染物及膜污染控制
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张超1 , 许岐斌1, 王颖2, 刘索1, 赵纯1, *
作者信息
  • 1.重庆大学，煤矿灾害动力学与控制全国重点实验室，三峡库区生态环境教育部重点实验室，重庆 400045
  • 2.重庆大学，建筑规划设计研究总院有限公司，重庆 400045

    • 张超(2000-)，男，四川德阳人，重庆大学硕士研究生，主要从事过硫酸盐体系的高级氧化研究.发表论文1篇..

通讯作者:

* 责任作者，教授，;
HA driven PM/PMS system for removing emerging contaminants and controlling membrane fouling
Chao ZHANG1 , Qi-bin XU1, Ying WANG2, Suo LIU1, Chun ZHAO1, *
Affiliations
  • 1.Key Laboratory of the Three Gorges Reservoir Region's Eco-Environment, Ministry of Education, State Key Laboratory of Coal Mine Disaster Dynamics and Control, Chongqing University, Chongqing 400045, China
  • 2.General Research Institute of Architecture & Planning Design Co., Ltd, Chongqing University, Chongqing 400045, China
出版时间: 2025-06-20
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摘要
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本研究采用腐殖酸(HA)驱动高锰酸钾/过一硫酸盐(PM/PMS+HA)体系的方法，研究小分子有机污染物的去除并探究膜污染控制效能的内容.结果表明，对于不同小分子有机物(阿特拉津(ATZ)、苯酚(Phenol)、双氯芬酸钠(DCF)、卡马西平(CBZ)、布洛芬(IBP)磺胺甲噁唑(SMX))，PM/PMS+HA体系去除效果良好，其一级动力学常数均高于18×10-2min-1，远高于单独超滤体系、PM体系和PM/PMS体系.与此同时，PM/PMS+HA体系在膜污染缓解方面也表现良好.采用HA作为膜污染物，15min内，PM/PMS+HA体系的出水比通量仅下降至0.919，远高于单独HA过滤时的0.393.同时，采用PM/PMS体系进行膜清洗时，膜通量恢复率达到98.51%.捕获试验以及紫外分光光度计的测定探究PM/PMS+HA体系的机理表明，PM/PMS+HA过滤过程中主要是体系中富电子特性的HA引发了复合氧化剂(PM-PMS)的分解.复合氧化剂的分解产生了活性氧(•OH、SO4•-、1O2)以及活性锰(Mn(V)和Mn(VI)).产生的活性氧和活性锰对污染物的氧化导致了新污染物的去除以及膜污染物分子量的降低，从而实现了新污染的去除和膜污染的控制.污染物驱动的PM/PMS体系实现了超滤膜与高级氧化技术的耦合.

超滤膜  /  过一硫酸盐  /  高锰酸钾  /  膜污染

The study used humic acid (HA) to drive the potassium permanganate/persulfate (PM/PMS+HA) system to investigate the removal of small molecule organic pollutants and the effectiveness of membrane fouling control. The experimental results showed that the PM/PMS+HA system exhibited excellent removal performance for different small molecule organic compounds, including Atrazine (ATZ), Phenol (Phenol), Diclofenac Sodium (DCF), Carbamazepine (CBZ), Ibuprofen (IBP) and Sulfamethoxazole (SMX). The first-order kinetic constants of the PM/PMS+HA system were all higher than 18×10-2min-1, far higher than the PM/PMS system, PM system, and ultrafiltration system alone. At the same time, the PM/PMS system has a good membrane fouling alleviation effect. When HA was used as the pollutant, the effluent specific flux of the PM/PMS system only decreased to 0.919 within 15 minutes, much higher than the 0.393 obtained by HA filtration alone. Meanwhile, when using the PM/PMS system for membrane cleaning, the membrane flux recovery rate reached 98.51%. The mechanism of the PM/PMS+HA system was explored through capture experiments and measurements using a UV spectrophotometer. The experimental results indicate that during the filtration process of PM/PMS+HA, it is mainly the rich electronic HA in the system that triggers the decomposition of the composite oxidant (PM-PMS). The decompositionof composite oxidants produces reactive oxygen species (•OH、SO4•-、1O2) and reactive manganese(Mn(V)and Mn(VI)). The generated reactive oxygen species and reactive manganese oxidize pollutants, leading to the removal of new pollutants and a decrease in the molecular weight of membrane pollutants, thereby achieving the removal of new pollutants and the control of membrane pollution. The PM/PMS system driven by pollutants has achieved the coupling of ultrafiltration membranes with advanced oxidation technology, providing new ideas for the removal of small molecule organic compounds and membrane fouling control in ultrafiltration technology.

ultrafiltration membrane  /  peroxymonosulfate  /  permanganate  /  membrane fouling
张超, 许岐斌, 王颖, 刘索, 赵纯. HA驱动PM/PMS体系去除新污染物及膜污染控制. 中国环境科学, 2025 , 45 (6) : 3046 -3053 .
Chao ZHANG, Qi-bin XU, Ying WANG, Suo LIU, Chun ZHAO. HA driven PM/PMS system for removing emerging contaminants and controlling membrane fouling[J]. China Environmental Science, 2025 , 45 (6) : 3046 -3053 .
正文
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超滤膜孔径介于微滤和纳滤之间，是一种低压膜过滤技术(0.1~0.5MPa).通过膜孔筛分作用，超滤膜能够有效截留溶液中悬浮固体、胶体、大分子有机物等物质，从而实现高效的水净化效果[1-3].但小分子有机物(SMOP)难以去除以及膜污染问题限制了超滤膜技术在实际中的大规模应用[4-6].
高级氧化技术(AOPs)可产生强活性物质来降解和矿化水中污染物，因此，耦合AOPs的超滤技术越来越受到研究学者的青睐[7].硫酸根自由基-高级氧化技术(SR-AOPs)已被证明可有效去除各种污染物[8]，并且与羟基自由基(•OH)相比，硫酸根自由基(SO4•-)的氧化还原电位更高(E0=2.5~3.1eV)，半衰期更长(30~40us)[9-10].因此，SR-AOPs耦合超滤膜技术成为了当前的研究热点[11].目前，过硫酸盐高级氧化耦合膜过滤技术主要通过膜表面涂层或掺杂过渡金属来实现过硫酸盐的原位活化[12-13].这种方法具有良好的过硫酸盐活化效果，但也会造成金属泄露的风险，而过渡金属的泄露会造成二次污染并降低膜过滤系统的耐久性[14-15]，并且超滤膜的功能化处理工艺复杂，无疑会增加成本，导致其难以在实际中进行应用[16].与此同时，与单氧化剂的高级氧化技术相比，双氧化剂的高级氧化技术氧化能力更强，对污染物的氧化去除效果更好[17].相关研究表明，高锰酸钾(PM)与过硫酸氢钾(PMS)的双氧化剂体系能够在未引入催化剂的条件下实现对小分子有机物的快速去除[18].因此，理论上将PM/PMS与超滤膜技术结合能够有效解决超滤技术面临的问题.然而，对于双氧化剂膜过滤体系的研究较少.
天然有机物(NOM)能造成严重的超滤膜不可逆膜污染[19].而腐殖酸是NOM中的主要种类，是造成膜污染的主要因素之一[20].因此NOM污染是限制超滤技术的一个重要问题.故本文以腐殖酸(HA)作为目标膜污染物，探究了其在超滤膜表面及膜孔内驱动PM/PMS体系对多种小分子污染物(ATZ、Phenol、CBZ、SMX、DCF和IBP)的去除效果.研究了PM/PMS+HA体系对膜污染的控制，并通过捕获试验确定了体系的清洗机理，同时采用紫外分光光度计对中间价态锰进行测量.
1　材料与方法
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1.1　实验药品
聚偏氟乙烯粉末(PVDF)购自美国苏威有限公司;腐殖酸(HA)和甲醇(MeOH)购自西格玛奥德里奇(上海)贸易有限公司;布洛芬(IBP)、磺胺甲噁唑(SMX)、卡马西平(CBZ)和过硫酸氢钾(KHSO5)购自阿拉丁有限公司;苯酚(Phenol)、高锰酸钾(KMnO4)和N，N-二甲基甲酰胺(DMF)购自成都科隆有限公司;焦磷酸钠(PP)购自重庆川东化工有限公司;双氯芬酸钠(DCF)、阿特拉津(ATZ)、叔丁醇(TBA)、糠醇(FFA)、5，5-二甲基-1-吡咯啉-N-氧化物(DMPO)、四甲基哌啶醇(TMPO)和聚乙烯吡咯烷酮(PVP)购自麦克林生化科技有限公司.实验中溶液配制均采用超纯水(电阻率18.25 MΩ/cm).
1.2　实验仪器
磁力搅拌器(85-2A型，金坛市城东新瑞仪器厂)、磁力搅拌转子(A35,35mm)、紫外分光光度计(T6新世纪，北京普析通用仪器有限公司)、高效液相色谱仪(Waters 2695，沃特世科技有限公司)、电子顺磁共振仪(A300，美国Bruker).
1.3　超滤膜的制备
聚偏氟乙烯超滤膜的制作方法为非溶剂诱导相分离方法.首先为膜液制备，在锥形瓶中加入83g N，N-二甲基甲酰胺，1g聚乙烯吡咯烷酮和16g聚偏氟乙烯(PVDF)于60℃下搅拌12h.制好的膜液放入60℃烘箱中静置12h脱气[21].其次是超滤膜刮取，用刮膜棒将膜液快速均匀刮于干净刮膜板上，然后立即浸入水中，凝固后将其转移至去离子水中浸泡48h去除残余溶剂[22].实验所用超滤膜直径为64cm，比表面积为32.15cm2.
1.4　实验方法
对ATZ、IBP、SMX、DCF、Phenol和CBZ的去除实验采用错流过滤和浓水回流模式进行，反应装置如图1所示，采用蠕动泵为进水提供动力，跨膜压力控制在0.05MPa.每组实验开始前，使用超纯水对超滤膜进行预压30min，预压结束后向进水烧杯中加入小分子有机物，打开蠕动泵开关，一旦部分进水流经反应器回到原水，迅速加入HA、PMS及PM并开始计时.实验过程中，在规定时间点用针管对出水进行取样并采用0.22µm滤膜过滤到液相小瓶中.实验中PM投加量为20µmol/L，PMS投加量为2mmol/L，HA投加量为5mg/L，小分子有机物投加量为3µmol/L.所有样品进行测量前均保存在4℃条件下.
膜污染缓解实验采用的过滤、回流模式以及实验前超滤膜预压同小分子有机物去除实验.选用HA作为模拟膜污染物.污染缓解实验先向烧杯中投加所需浓度HA，打开蠕动泵后，流经反应器时迅速加入PMS以及PM并开始计时.膜清洗实验先采用HA溶液进行过滤使超滤膜污染，后采用PM/PMS清洗液进行过滤清洗.当PM/PMS清洗液流经反应器时开始计时.污染缓解和清洗实验中PM浓度均为0.15mmol/L，PMS浓度均为5mmol/L.由电子天平记录出水质量.
超滤膜的纯水通量J0通过式(1)计算[23]:
式中：V为单位时间内通过膜的渗透量，L;A为相关有效面积，m2;t为过滤时间，min.
1.5　分析方法
小分子有机物去除实验中相关污染物为ATZ、IBP、SMX、DCF、Phenol和CBZ，采用高效液相色谱(HPLC)检测其浓度，进样体积为10μL.色谱柱为Cosmosil 5C18-ms-II柱(4.6mm×150mm).各污染物具体检测条件见表1.初始浓度为C0，不同时刻取样测得的浓度为C，去除率为1-C/C0.
膜表面形貌由扫描电子显微镜(MIRA3TESCAN，Czech)观察测定.
焦磷酸钠(PP)会与三价锰形成络合物(Mn(III)-PP)，使用紫外分光光度计在258nm处监测是否有Mn(III)生成[24].使用紫外可见分光光度计在660,610nm处监测Mn(V)、Mn(VI)生成情况.
2　结果与讨论
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2.1　不同体系对ATZ的去除
如图2所示，反应10min后，单独超滤体系和单独PM体系对ATZ几乎没有去除效果.PMS和PM/PMS体系对ATZ的去除率也十分有限，仅为17.17%和25.64%.而当加入HA后，PM/PMS+HA体系对ATZ的去除率得到显著提升，在10min时可达到97.30%的去除率，明显优于单独超滤体系和PM/PMS体系.这一结果表明，污染物的加入可以提高PM/PMS体系的氧化能力.这可能是由于PM/PMS体系中形成的络合物的氧化能力不足以去除ATZ，而当HA加入后，HA向PM与PMS络合物提供电子使其分解产生活性物种，实现了对ATZ的去除.为验证PM/PMS+HA体系对ATZ去除的稳定性，对该体系进行了循环实验，如图3所示.循环20次后，PM/PMS+HA体系对ATZ的去除基本保持不变，去除率维持在97%左右，而PM/PMS体系对ATZ的去除率从27.26%降低至10.32%.表明PM/PMS+HA体系对小分子有机物的去除具有更好的稳定性.
2.2　PM/PMS+HA体系对不同小分子的去除
如图4所示，对于Phenol、CBZ、DCF和SMX，PM/PMS体系和HA驱动的PM/PMS体系都能对其进行快速去除，其一级反应动力学常数均高于25×10-2min-1.而对于ATZ和IBP，单独PM、单独PMS和PM/PMS体系对其几乎没有去除效果.加入HA后，该体系对这两种污染物的去除效率得到了显著提升，远高于单独PM、单独PMS和PM/PMS体系.以ATZ为例，单独PM或PMS体系和PM/PMS体系对ATZ的去除速率分别为0.2133×10-2，1.8367×10-2，2.8867×10-2min-1，而PM/PMS+HA体系对ATZ的一级反应动力学常数为36.8267×10-2min-1.表明PM/PMS+HA体系对其他小分子污染物的去除仍具有显著效果，也进一步说明污染物的加入可以提高PM/PMS体系的氧化能力.
2.3　PM/PMS+HA体系对膜污染的缓解
如图5所示，实验开始5min内，超滤膜的出水通量(J/J0)快速下降，最终稳定在0.393左右，在过滤过程中，可能由于HA沉积在膜组分表面并且造成严重的膜孔堵塞而导致出水通量迅速下降[25].PM+HA与PMS+HA体系与HA有着相似的出水通量衰减情况，其J/J0最终分别稳定在0.451和0.449左右.而当体系中加入PM/PMS后(即PM/PMS+HA体系),15min时J/J0维持在0.919左右，膜污染得到有效缓解，主要原因是HA为PM与PMS的络合物提供电子使其产生更多的活性物种，将HA大分子氧化成分子量小的有机成分，从而缓解了膜孔的堵塞.
膜过滤的性能与其表面形貌有着密切关系[26-27].超滤膜的形貌如图6所示，原始超滤膜的表面光滑、致密，没有污染物的沉积.而经过HA原水污染后的超滤膜，能清晰地看见膜表面形成了一层致密的饼层，这种滤饼造成了严重的不可逆膜污染[28].在PM/PMS+HA体系中，HA被活性物种氧化为分子量更小的有机成分，膜表面仅有少量污染物附着，并且膜表面依旧光滑.这一结果表明过滤过程中污染物造成的膜孔堵塞导致的膜通量降低，采用PM/PMS+HA体系可以有效去除污染物、缓解膜污染，使超滤膜恢复本身的表面形貌.
2.4　对污染膜通量的恢复
由图7可知，采用物理清洗后，污染膜的出水通量恢复到71.42%.采用单独PMS和单独PM清洗后，出水通量分别恢复到72.86%和77.46%.而采用PM/PMS清洗后，出水通量恢复到98.51%.说明单独的PM或PMS清洗，并不能有效实现膜通量的恢复，而采用PM/PMS清洗能实现接近完全的膜通量恢复.
2.5　活性物种鉴定
PM/PMS+HA体系中PMS和PM两者均作为氧化剂，可能产生•OH、SO4•-和中间价态锰等多种活性物种.选取甲醇(MeOH)作为•OH和SO4•-淬灭剂，选取叔丁醇(TBA)作为•OH淬灭剂，选取糠醇(FFA)作为1O2淬灭剂[28].如图8所示，当未加入淬灭剂时，PM/PMS+HA体系的一级反应动力学常数为36.83×10-2min-1，当过量的TBA加入到体系中，一级反应动力学常数降低到9.29×10-2min-1，这表明该体系中•OH参与了对ATZ的去除.将过量的MeOH加入到体系中，一级反应动力学常数进一步降低为4.23×10-2min-1，表明除了•OH外，SO4•-也参与了对ATZ的去除.接着将过量的FFA加入到体系中，发现一级反应动力学常数变为5.13×10-2min-1，说明1O2也存在于体系中.最后，向体系中加入过量的焦磷酸盐，一级反应动力学常数降低到0.83×10-2min-1，其原因可能是PP的络合作用导致PM与PMS的络合物无法分解从而无法产生活性物种实现对小分子污染物的去除.
采用电子顺磁共振实验来确定PM/PMS+HA体系中具体的活性物种种类. 5,5-二甲基-1-吡咯啉-N-氧化(DMPO)可用于鉴定•OH和SO4•-，四甲基哌啶醇(TMPO)可用于鉴定1O2[29-31].在PM/PMS+HA体系中加入相应捕获剂，由图9(a)可知，当加入DMPO后，PM/PMS+HA体系中出现了明显的1:2:2:1的DMPO-•OH信号特征峰和1:1:1:1:1:1的DMPO-SO4•-信号特征峰，表明体系中产生了•OH和SO4•-，而PM/PMS体系在未污染的膜过滤过程中未出现任何特征峰.由图9(b)可知，当加入TMPO后，PM/PMS+HA体系中出现了明显的1:1:1的TMPO-1O2的信号特征峰，表明体系中产生了1O2，而PM/PMS体系中也未出现任何特征峰.通过以上实验结果可推断出，PM/PMS+HA体系在膜过滤过程中产生的活性物种为•OH、SO4•-和1O2，并且需要污染物存在的条件下活性氧才能产生.
PM/PMS+HA体系中，活性物种是两种氧化剂相互作用产生的，因此中间价态锰也可能是缓解膜污染的活性物种.为了探究Mn(III)在膜污染缓解中是否发挥作用，在焦磷酸盐(PP)浓度10mmol/L条件下，对PM/PMS+HA体系进行了紫外全扫描，如图10所示，反应后Mn(VII)的紫外吸收峰强度有所降低，同时在258nm处也并没有出现Mn(III)-PP的紫外吸收峰，该结果证明在污染膜的过滤过程中污染物驱动两种氧化物相互作用产生活性物种，故PM的浓度有所降低，同时Mn(III)不是PM/PMS+HA体系中缓解膜污染的活性中间价态锰，这一结果与之前的中间价态锰研究的氧化结果不同[32].PM分解除了产生Mn(III)，还可能会产生Mn(V)和Mn(VI).
Mn(V)和Mn(VI)的特征吸收峰所对应的波长分别是660nm和610nm[33-34].如图11所示，每间隔一段时间进行取样并采用紫外分光光度计分别对Mn(V)和Mn(VI)进行扫描，结果显示Mn(V)和Mn(VI)的吸收峰在反应开始后1min内迅速升高.接下来Mn(V)峰强度维持在0.06左右，Mn(VI)也有着相同的规律，峰强度维持在0.055左右.表明Mn(V)和Mn(VI)是PM/PM+HA体系中控制膜污染的中间价态锰.根据现有研究[35-36]，推测PM/PMS+HA体系产生活性物质的反应式如式(2) ~式(8)所示：
2.6　电子转移机制
在小分子有机物去除实验中，PM与PMS络合后通过歧化反应产生活性物种，从而实现对小分子有机物的去除.同时，在膜清洗实验中需要污染物HA存在，才会产生活性物种实现膜清洗，在未污染的膜过滤过程中PM并不会分解.并且本研究中反应时间均较短，与之前报道的PM与PMS的歧化时间较长不同[37].这说明该体系需要污染物存在才能实现清洗作用，污染物可能起到一个“活化剂”的作用.考虑到污染物可能与PM与PMS的络合物之间存在电子转移，因此，对PM-PMS+HA体系进行了电流时间曲线测试验证电子转移[38].如图12所示，60s时加入PMS到溶液中，响应电流急剧下降，随后又慢慢增加.随后在120s时加入PM，电流再一次迅速下降，随后又慢慢增加.加入污染物HA后，响应电流进一步增加.结果表明，污染物HA与PM和PMS的络合物之间发生了电子转移，污染物向络合物提供电子，络合物得到电子后分解产生活性物种.
3　结论
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3.1　富电子污染物HA驱动的PM/PMS体系在没有外加电场和催化剂的条件下实现了对小分子污染物的去除以及膜通量的恢复.HA引发PM与PMS相互作用产生活性氧和中间价态锰.
3.2　PM/PMS+HA体系对几种不同污染物(ATZ、SMX、DCF、Phenol、CBZ和IBP)的一级反应动力学常数均高于18×10-2min-1，远高于单独超滤、PM和PM/PMS体系.采用PM/PMS体系进行污染膜清洗，通量恢复率能够达到98.51%，远高于单独PMS和单独PM清洗的通量恢复率.
3.3　机理实验结果证实了体系中产生了•OH、SO4•-和1O2以及中间价态锰.活性氧以及锰对有机污染物的氧化作用实现了PM/PMS过滤体系对小分子有机物的去除以及膜污染控制.
基金
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  • 国家自然科学基金资助项目(22076015; 52370126)
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2025年第45卷第6期
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  • 接收时间：2024-11-21
  • 首发时间：2026-02-27
  • 出版时间：2025-06-20
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  • 收稿日期：2024-11-21
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国家自然科学基金资助项目(22076015; 52370126)
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    1.重庆大学，煤矿灾害动力学与控制全国重点实验室，三峡库区生态环境教育部重点实验室，重庆 400045
    2.重庆大学，建筑规划设计研究总院有限公司，重庆 400045

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