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Article(id=1241116646870405523, tenantId=1146029695717560320, journalId=1234093305789726721, issueId=1241116641321350143, 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=1723392000000, receivedDateStr=2024-08-12, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773834867446, onlineDateStr=2026-03-18, pubDate=1742400000000, pubDateStr=2025-03-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773834867446, onlineIssueDateStr=2026-03-18, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773834867446, creator=13701087609, updateTime=1773834867446, updator=13701087609, issue=Issue{id=1241116641321350143, tenantId=1146029695717560320, journalId=1234093305789726721, year='2025', volume='45', issue='3', pageStart='1185', pageEnd='1776', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773834866123, creator=13701087609, updateTime=1773881366030, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1241311676130193619, tenantId=1146029695717560320, journalId=1234093305789726721, issueId=1241116641321350143, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1241311676130193620, tenantId=1146029695717560320, journalId=1234093305789726721, issueId=1241116641321350143, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=1298, endPage=1307, ext={EN=ArticleExt(id=1241116647214338472, articleId=1241116646870405523, tenantId=1146029695717560320, journalId=1234093305789726721, language=EN, title=Visible light-assisted copper oxide efficient activation of peroxydisulfate for tetracycline degradation, columnId=1234106386360103680, journalTitle=China Environmental Science, columnName=Water Pollution Control, runingTitle=null, highlight=null, articleAbstract=

The advanced oxidation technology of persulfate（PDS）activation by CuO have been hotly sought as one of the effective strategies for degrading organic pollutants in water. However, there are still certain issues such as the low efficiency of PDS activation, the small specific surface area of CuO, and the low conversion efficiency of Cu（II）/Cu（I）. Herein, the flake copper oxide（CCB-300）with high activity and large specific surface area（32.8m2/g）was successfully synthesized through a two-step hydrothermal-calcination method. Multiple characterization analysis, such as X-ray powder diffractometry（XRD）, N2 adsorption-desorption analysis, Scanning electron microscopy（SEM）, Transmission electron microscopy（TEM）and X-ray photoelectron spectroscopy（XPS）, were utilized to analyze crystal structure, morphology and element composition of CCB-300. Furthermore, the performance of the CCB-300 for degradation of tetracycline（TC）via peroxydisulfate activation under visible light（Vis）was investigated. The findings revealed that the TC removal rate reached 96.9% within 60minutes under the circumstances of 0.05g/L CCB-300, 0.5mmol/L PDS, 50mg/L TC and unadjusted initial pH. Electron paramagnetic resonance spectroscopy（EPR）and radical quenching experiments indicated that both 1O2 produced by the non-radical pathways and and ⋅OH generated via the radical pathways were involved in the degradation reaction. Ultraviolet-visible diffuse reflectance spectroscopy and photoelectrochemical tests confirmed that CCB-300 exhibited excellent visible light absorption capacity and charge transfer performance. The photogenerated electrons excited by visible light accelerate the redox cycle of Cu（II）/Cu（I）, facilitating the conversion of PDS to and ⋅OH, and further enhancing the efficiency of TC degradation. The repeatable experiments demonstrated that CCB-300exhibited favorable reusability and stability. Finally, the possible reaction mechanism was proposed. This study provided a novel method for tetracycline degradation through synergistic persulfate activation by visible light and heterogeneous catalysts.

, correspAuthors=Shi-jia LI, 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=Shi-jia LI, Er-nan PANG), CN=ArticleExt(id=1241116664016720504, articleId=1241116646870405523, tenantId=1146029695717560320, journalId=1234093305789726721, language=CN, title=可见光协同CuO高效活化过二硫酸盐降解四环素, columnId=1234106386565624579, journalTitle=中国环境科学, columnName=水污染与控制, runingTitle=null, highlight=null, articleAbstract=

基于CuO活化过二硫酸盐(PDS)的高级氧化技术已成为降解有机污染物的有效策略之一，但仍存在活化PDS效率较低、CuO比表面积小和Cu(Ⅱ)/Cu(Ⅰ)转换效率低等问题，本文采用低温水热-煅烧两步法成功制备了具有高催化活性和大比表面积(32.8m2/g)的片状氧化铜(CCB-300).通过X射线粉末衍射仪(XRD)、比表面及孔径分析仪(BET)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X射线光电子能谱仪(XPS)等表征分析了CCB-300的晶体结构、形貌和元素组成等理化性质.研究其在可见光(Vis)协同作用下活化PDS降解四环素(TC)的性能.在不调整初始pH值、催化剂用量为0.05g/L、PDS浓度为0.5mmol/L、TC浓度为50mg/L条件下，反应60min后TC去除率达到96.9%.电子顺磁共振谱(EPR)和自由基淬灭实验表明非自由基途径产生的1O2和自由基途径生成的和⋅OH均参与了降解反应.紫外可见漫反射光谱及光电化学测试结果表明CCB-300具有优异的可见光吸收能力和电荷传输性能，在可见光激发下产生的光生电子加速了Cu(Ⅱ)/Cu(Ⅰ)的氧化还原循环，促进了PDS向和⋅OH的转化，从而进一步提高其降解TC的效率.重复性实验结果表明CCB-300具有较好的重复使用性和稳定性.最后，提出了CCB-300协同可见光活化PDS降解TC的可能反应机理.本研究为可见光协同非均相催化剂活化过硫酸盐降解四环素类抗生素提供一种新的方法和思路.

, correspAuthors=李世嘉, authorNote=null, correspAuthorsNote=
* 责任作者，副教授，
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李世嘉(1982-)，山西应县人，副教授，博士，主要从事高级氧化法降解水中有机污染物研究.发表论文10余篇..

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李世嘉(1982-)，山西应县人，副教授，博士，主要从事高级氧化法降解水中有机污染物研究.发表论文10余篇..

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李世嘉(1982-)，山西应县人，副教授，博士，主要从事高级氧化法降解水中有机污染物研究.发表论文10余篇..

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caption=催化剂重复性（a）及反应前后CCB-300的XRD谱（b）, figureFileSmall=Ao/QqksPB2DtYDsQY1a9bA==, figureFileBig=sHhDJYytsrdC/AeO0c/2zg==, tableContent=null), ArticleFig(id=1241116672409522356, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1241116646870405523, language=EN, label=Table 1, caption=

The specific surface area of CCB-300 and CuO reported in other literatures

, figureFileSmall=null, figureFileBig=null, tableContent=
样品名称制备方法比表面积(m2/g)参考文献
MSCuO-300煅烧9.14[30]
CuO-10水热+煅烧3.19[31]
CuOµm商用0[24]
CuO-3煅烧3.19[32]
CCB-300水热+煅烧32.8本文
), ArticleFig(id=1241116672547934398, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1241116646870405523, language=CN, label=表1, caption=

CCB-300与其他文献报道CuO的比表面积比较

, figureFileSmall=null, figureFileBig=null, tableContent=
样品名称制备方法比表面积(m2/g)参考文献
MSCuO-300煅烧9.14[30]
CuO-10水热+煅烧3.19[31]
CuOµm商用0[24]
CuO-3煅烧3.19[32]
CCB-300水热+煅烧32.8本文
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可见光协同CuO高效活化过二硫酸盐降解四环素
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李世嘉 1, * , 庞尔楠 2
中国环境科学 | 水污染与控制 2025,45(3): 1298-1307
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中国环境科学 | 水污染与控制 2025, 45(3): 1298-1307
可见光协同CuO高效活化过二硫酸盐降解四环素
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李世嘉1, * , 庞尔楠2
作者信息
  • 1.山西工程科技职业大学交通工程学院，山西 太原 030619
  • 2.中北大学材料科学与工程学院，山西 太原 030051

    • 李世嘉(1982-)，山西应县人，副教授，博士，主要从事高级氧化法降解水中有机污染物研究.发表论文10余篇..

通讯作者:

* 责任作者，副教授，
Visible light-assisted copper oxide efficient activation of peroxydisulfate for tetracycline degradation
Shi-jia LI1, * , Er-nan PANG2
Affiliations
  • 1.Institute of Traffic Engineering, Shanxi Vocational University of Engineering Science and Technology, Taiyuan 030619, China
  • 2.School of Materials Science and Engineering, North University of China, Taiyuan 030051, China
出版时间: 2025-03-20
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基于CuO活化过二硫酸盐(PDS)的高级氧化技术已成为降解有机污染物的有效策略之一，但仍存在活化PDS效率较低、CuO比表面积小和Cu(Ⅱ)/Cu(Ⅰ)转换效率低等问题，本文采用低温水热-煅烧两步法成功制备了具有高催化活性和大比表面积(32.8m2/g)的片状氧化铜(CCB-300).通过X射线粉末衍射仪(XRD)、比表面及孔径分析仪(BET)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X射线光电子能谱仪(XPS)等表征分析了CCB-300的晶体结构、形貌和元素组成等理化性质.研究其在可见光(Vis)协同作用下活化PDS降解四环素(TC)的性能.在不调整初始pH值、催化剂用量为0.05g/L、PDS浓度为0.5mmol/L、TC浓度为50mg/L条件下，反应60min后TC去除率达到96.9%.电子顺磁共振谱(EPR)和自由基淬灭实验表明非自由基途径产生的1O2和自由基途径生成的和⋅OH均参与了降解反应.紫外可见漫反射光谱及光电化学测试结果表明CCB-300具有优异的可见光吸收能力和电荷传输性能，在可见光激发下产生的光生电子加速了Cu(Ⅱ)/Cu(Ⅰ)的氧化还原循环，促进了PDS向和⋅OH的转化，从而进一步提高其降解TC的效率.重复性实验结果表明CCB-300具有较好的重复使用性和稳定性.最后，提出了CCB-300协同可见光活化PDS降解TC的可能反应机理.本研究为可见光协同非均相催化剂活化过硫酸盐降解四环素类抗生素提供一种新的方法和思路.

高级氧化法  /  氧化铜  /  可见光  /  过二硫酸盐  /  四环素

The advanced oxidation technology of persulfate（PDS）activation by CuO have been hotly sought as one of the effective strategies for degrading organic pollutants in water. However, there are still certain issues such as the low efficiency of PDS activation, the small specific surface area of CuO, and the low conversion efficiency of Cu（II）/Cu（I）. Herein, the flake copper oxide（CCB-300）with high activity and large specific surface area（32.8m2/g）was successfully synthesized through a two-step hydrothermal-calcination method. Multiple characterization analysis, such as X-ray powder diffractometry（XRD）, N2 adsorption-desorption analysis, Scanning electron microscopy（SEM）, Transmission electron microscopy（TEM）and X-ray photoelectron spectroscopy（XPS）, were utilized to analyze crystal structure, morphology and element composition of CCB-300. Furthermore, the performance of the CCB-300 for degradation of tetracycline（TC）via peroxydisulfate activation under visible light（Vis）was investigated. The findings revealed that the TC removal rate reached 96.9% within 60minutes under the circumstances of 0.05g/L CCB-300, 0.5mmol/L PDS, 50mg/L TC and unadjusted initial pH. Electron paramagnetic resonance spectroscopy（EPR）and radical quenching experiments indicated that both 1O2 produced by the non-radical pathways and and ⋅OH generated via the radical pathways were involved in the degradation reaction. Ultraviolet-visible diffuse reflectance spectroscopy and photoelectrochemical tests confirmed that CCB-300 exhibited excellent visible light absorption capacity and charge transfer performance. The photogenerated electrons excited by visible light accelerate the redox cycle of Cu（II）/Cu（I）, facilitating the conversion of PDS to and ⋅OH, and further enhancing the efficiency of TC degradation. The repeatable experiments demonstrated that CCB-300exhibited favorable reusability and stability. Finally, the possible reaction mechanism was proposed. This study provided a novel method for tetracycline degradation through synergistic persulfate activation by visible light and heterogeneous catalysts.

advanced oxidation  /  CuO  /  visible light  /  peroxydisulfate  /  tetracycline
李世嘉, 庞尔楠. 可见光协同CuO高效活化过二硫酸盐降解四环素. 中国环境科学, 2025 , 45 (3) : 1298 -1307 .
Shi-jia LI, Er-nan PANG. Visible light-assisted copper oxide efficient activation of peroxydisulfate for tetracycline degradation[J]. China Environmental Science, 2025 , 45 (3) : 1298 -1307 .
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四环素类抗生素由于具有抗菌活性好和成本低廉的特点，广泛应用于水产养殖、畜牧业和人类疾病诊疗.目前四环素类抗生素在中国的产量和用量均排第一[1].四环素在人类和动物消化系统难以完全代谢，50%~80%随着排泄物排到自然环境中稳定存在且不易降解，在水生和土壤环境中大量积累，对生态系统和公众健康造成严重影响[2].传统的物理分离[3]、化学吸附[4]和生物降解[5]等废水处理方法不能有效去除四环素，且存在诸多问题.膜分离需要消耗大量外部能量来提供足够高的工作压力；化学吸附只是将四环素从废水中分离出来，四环素并没有降解为小分子产物；由于四环素对细菌的抑制作用，生物降解四环素效率也不高.近些年基于过二硫酸盐(PDS)的高级化学氧化法因其氧化能力强、效率高、适应性广等优点，已被证实是一种有效的四环素降解策略[6-11].
PDS可通过外部能量输入(紫外光照射[12]、超声波[13]、加热[14]、微波[15]等)或者是使用均相[16]、非均相催化剂[17-18]活化产生高氧化还原电位的硫酸根自由基()和羟基自由基(⋅OH)来去除难降解有机污染物.太阳能是绿色可再生能源，其中可见光占到47%.基于可见光与非均相催化剂协同活化PDS的高级氧化法已成为降解水中有机污染物的有效策略之一.实现这种协同活化PDS的关键是选择具有合适带隙的光催化剂.类似的高级氧化技术近几年正逐渐成为新的研究热点[19-22].
CuO是一种典型的过渡金属氧化物，具有多样化的形态结构和较强的电子转移能力，可以通过自由基或非自由基途径活化PDS产生、•OH、、1O2和Cu(Ⅲ)等活性物质降解有机污染物[23-24]. Liang等[25]首次提出CuO可以在不同pH条件下活化PDS降解有机污染物对氯苯胺，降解反应过程中、⋅OH和Cu(Ⅲ)均起作用.CuO也可以激活其表面吸附的PDS形成活化态PDS降解富电子有机污染物.Xu等[26]指出带负电的PDS阴离子吸附于带正电的CuO表面形成活化态的PDS，活化态的PDS在降解有机污染物莫西沙星起主要作用.Xing等[27]指出CuO活化PDS降解环丙沙星过程中主要活性物质有、⋅OH、和1O2.Li等[28]指出CuO活化PS的方式与其表面暴露晶面有关，活性物质既有自由基途径产生和⋅OH，也有非自由基途径生成1O2和Cu(Ⅲ).综上，CuO能以多种途径活化PDS产生不同的活性物质降解有机污染物，但是仍存在Cu(Ⅱ)向Cu(Ⅰ)转化速率较低、活化PDS效率不高的问题.
本文通过低温水热-煅烧两步法合成碱式碳酸铜衍生氧化铜，发现其具有较大比表面积和优异的可见光吸收能力，不仅可以直接活化PDS降解TC，而且，当有可见光照射时其活化PDS降解TC性能大幅提高.利用可见光协同CuO活化PDS降解TC的研究此前鲜有报道.可见光、CuO和PDS的协同作用，不仅抑制了CuO光生电子与空穴的复合，同时，加速了表面Cu(Ⅱ)/Cu(Ⅰ)的氧化还原循环，促进了PDS产生更多的和⋅OH.通过电子顺磁共振光谱仪(EPR)和自由基淬灭实验证实反应过程中可能生成的活性物质，进一步结合光电化学测试和X射线光电子能谱测试结果提出可能的活化机理.此外，探究了PDS用量、初始溶液pH值、共存阴离子等反应条件对降解TC的影响.最后通过重复性实验及反应前后XRD结果证实催化剂具有优异的重复使用性和稳定性.本研究为高级氧化法高效降解四环素类抗生素有机废水提供借鉴和参考.
1　材料与方法
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1.1　材料
硝酸铜(Cu(NO3)2⋅3H2O)、尿素(urea)、盐酸四环素(TC)、过硫酸钠(Na2S2O8)、甲醇(MeOH，色谱级)、甲酸(CH2O2，色谱级)、叔丁醇(TBA)、高碘酸钠(NaIO4)氧化铜(纳米级，99%)购买自阿拉丁试剂有限公司；5，5-二甲基-1-吡咯啉-N-氧化物(DMPO，97%)、2，2，6，6-四甲基哌啶(TEMP)、糠醇(FFA)等购买自国药化学试剂有限公司；药品没有特别说明均为分析纯.实验用水均为去离子水.
1.2　催化剂制备
采用水热和煅烧两步法制备催化剂.称取2mmol Cu(NO3)2⋅3H2O和8mmol urea溶于30mL去离子水中，将混好的溶液转移至聚四氟乙烯高压反应釜中，加热至120℃保温12h自然冷却至室温，将反应产物通过孔径为0.22µm的聚四氟乙烯滤膜分离纯化，60℃烘箱干燥12h.水热后产物命名为CCB.将CCB研磨并置于管式炉中，空气气氛加热至300℃煅烧4h，升温速率为5℃/min，自然冷却得到最终样品.为了研究煅烧温度对煅烧产物的影响，改变煅烧温度为250℃和350℃，煅烧后产物根据煅烧温度不同分别命名为CCB-250、CCB-300、CCB-350.
1.3　催化剂表征
采用Bruker D8型X射线衍射仪(XRD)分析催化剂晶体结构；采用型号为Micromeritics ASAP2020比表面和孔隙度分析仪测定催化剂比表面积和孔径分布；采用型号为JEM-2800型透射电子显微镜(TEM)和型号为Hitachi S-4 800的扫描电子显微镜(SEM)观察催化剂微观形貌；采用型号为Thermo Scientific K-Alpha的X射线光电子能谱仪(XPS)测试样品的表面元素组成和价态；使用上海辰华CHI 650E电化学工作站测定催化剂的循环伏安曲线、光电流和电化学阻抗谱等；使用型号为岛津UV-2450的紫外可见分光光度计测定样品的紫外-可见漫反射光谱(UV-vis DRS).采用型号为EMXPLUS10/12的电子顺磁共振光谱仪测定自由基类别.
1.4　试验方法
在光催化反应器进行可见光协同催化剂活化PDS降解TC实验，光源为LED白光灯(100W)，未加滤波片，实测光强为100mW/cm2.将3mg催化剂分散于50mL(50mg/L)TC溶液中.黑暗处搅拌30min，确保TC与催化剂达到吸附-解吸平衡.随后在溶液中滴加0.25mL PDS(100mmol/L)溶液，同时，开启光源开始反应.每间隔一定时间取0.5mL反应溶液并向其中加入0.5mL甲醇中止反应.然后用0.22µm的针头过滤器过滤后采用高效液相色谱仪测定溶液残余TC浓度.TC降解过程采用一阶动力学模型进行拟合，可以表示为ln(ct/c0)=-kt，其中，k为表观速率常数(min-1)，t为反应时间(min)，Ct为t时刻的污染物浓度，C0为初始污染物浓度.根据TC的去除率和反应速率常数来考察催化剂的降解效果.实验过程中用0.1mol/L NaOH或H2SO4调节溶液初始pH值.催化剂的可重复性和稳定性实验中，反应后的催化剂采用0.22µm的PTFE聚四氟乙烯滤膜过滤收集，用去离子水冲洗3次.然后置于60℃的烘箱中干燥12h，用于下一轮的重复性使用实验.
活性物质捕获实验中，在催化反应前分别在溶液中加入MeOH(100mmol/L)、TBA(100mmol/L)、FFA(1mmol/L)作为活性物质淬灭剂，考察其对TC降解率的影响.在考察无机阴离子对催化反应影响实验中，Cl-、SO42-、NO3-、HCO3-浓度均为5mmol/L.
2　结果与讨论
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2.1　催化剂表征
热解温度对催化剂的物相组成有重要影响.如图1(a)所示，CCB-250与CCB的XRD衍射峰峰位基本相同，与Cu2(OH)2CO3的标准谱图(PDF#76-0660)相一致.CCB-300和CCB-350的衍射峰峰位发生明显变化，与CuO标准谱图(PDF#80-0076)的特征衍射峰相吻合，说明热解温度高于300℃时，Cu2(OH)2CO3会发生相转变生成CuO，而且随着热解温度增加衍射峰强度增强，半峰宽变窄，样品结晶度更好.从图1(b)可以看到，CCB-300的N2吸附-脱附等温线属于Ⅳ型等温线，回滞环为H3型，为介孔材料特征.CCB-300的BET比表面积为32.8m2/g，是CCB的65.6倍，是商用氧化铜(C-CuO)的7.6倍.CuO作为催化剂普遍存在比表面积较小的缺点[29]，由表1可以看出，CCB-300的比表面积远大于其他文献报道氧化铜的比表面积.说明催化剂具有较大比表面积可以为催化反应提供更多潜在的活性位点.
通过SEM和TEM研究催化剂的微观形貌和晶体结构，如图2(a)，(d)所示为催化剂的SEM照片，CCB和CCB-300的微观形貌类似，均为片状结构堆积而成，CCB-300表面更加粗糙一些，存在丰富的孔隙结构，这是由CCB高温分解转变为CCB-300过程中产生的CO2和H2O等挥发性气体导致.此外，TEM图像进一步证实CCB和CCB-300具有典型的不规则多边形片状结构(图2(b)，(e).在高分辨透射电镜(HRTEM)图像上，可以观察到明显的间距为0.252nm的晶格条纹，对应于碱式碳酸铜的(2 4 0)晶面(图2(c)).同样在图(图2(f))中可以观察到间距为0.252nm的晶格条纹，与CuO的(-1 1 1)晶面相对应利用XPS技术探究催化剂中Cu和O的化学价态.如图3(a)所示，Cu 2p反应前样品表面只存在Cu(Ⅱ)(534.02eV)，反应后样品表面除Cu(Ⅱ)外，还出现Cu(Ⅰ)(532.03eV)的特征峰，这说明在活化PDS过程中催化剂表面存在Cu(Ⅱ)/Cu(Ⅰ)的价态转变[32].图3(b)是O 1s的XPS精细谱图，在结合能为529.9eV、531.6eV和533eV处的峰分别归属于晶格氧(Olatt)、表面羟基氧(Oads)和表面吸附水氧(Owater)，反应后的Olatt占比下降，Oads占比增加，这可能是由于催化剂表面有部分CuO转化为Cu2O所致.这也说明在活化PDS过程中催化剂表面存在Cu(Ⅱ)/Cu(Ⅰ)的价态转变.
从图4(a)可以看到CCB-300比CCB具有更加优异的可见光吸收能力.图4(b)是催化剂的瞬态光电流响应曲线，其中CCB-300的光电流响应显著增强，光电流密度约是CCB的30倍.说明CCB-300中的光生电子和空穴不易复合，具有更多的光生载流子.进一步从电化学阻抗谱(EIS)图可以看到(图4(c))，与CCB相比，CCB-300的Nyquist曲线具有更小的半径，表明其具有更低的界面电荷传输阻力，有利于电荷的传输与分离.如图4(d)所示为CCB和CCB-300的循环伏安(CV)曲线，其中两个峰p1和p2分别对应于Cu(Ⅰ)/Cu(Ⅱ)的氧化还原峰，可以看到CCB-300的CV曲线面积和电流响应信号强度比CCB都大，说明CCB-300具有更好的电荷传输能力，而且存在Cu(Ⅰ)/Cu(Ⅱ)的价态转变，这也与反应前后XPS测试结果相一致.UV-Vis DRS和电化学测试结果表明CCB-300具有优异的可见光吸收能力和电荷传输特性，为可见光催化降解有机污染物提供便利条件.
2.2　催化性能
以盐酸四环素(TC)作为目标污染物，评估不同体系的催化降解性能.如图5(a)所示，黑暗条件下催化剂与TC吸附解吸30min后，TC的去除率低于10%，说明CCB-300对TC的吸附能力有限.反应60min后，CCB-300+Vis，CCB-300+PDS和CCB-300+PDS+Vis体系对TC的去除率分别为10.5%、57.4%和96.9%，CCB-300+PDS+Vis比单纯CCB-300+PDS体系对TC去除率提高近1倍.不同体系降解TC均符合伪一级动力学方程，拟合后得到的表观反应速率常数k如图5(b)所示，CCB-300+PDS+Vis体系的k值是CCB+PDS体系的4.3倍.进一步探究了CCB-250、CCB-350、C-CuO和CCB在可见光协同作用下活化PDS降解TC性能.如图5(c，d)所示，对TC的去除率分别为91%、85.8%、28.3%和76.5%，k值也均小于CCB-300.特别是C-CuO对TC的去除率仅为CCB-300的1/3.以上结果说明CCB-300在可见光协同作用下具有最优异的活化PDS降解TC能力.
2.3　活性物质鉴定
采用自由基淬灭实验探究CCB-300+PDS+Vis体系中哪些活性物种参与了TC降解反应.其中，MeOH作为和⋅OH的淬灭剂，TBA作为⋅OH的淬灭剂，FFA作为1O2的淬灭剂.如图6(a)，(b)所示，加入过量的MeOH(100mmol/L)和TBA(100mmol/L)后，反应60min后TC的去除率由不加淬灭剂的96.9%分别降至80.7%和87.1%，k值分别减小为0.026min-1和0.033min-1.说明体系中和⋅OH对降解TC均有贡献.当加入FFA(1mmol/L)后，体系对TC去除率降至41%，k值减小为0.008min-1，k值仅为不加淬灭剂的1/7.FFA对TC降解抑制效果明显，说明1O2可能是降解TC的主要活性物种.Cu(Ⅲ)作为一种具有强氧化性的中间产物，可作为活性物质降解有机污污染物，但是非常不稳定[24,33].Cu(Ⅲ)可以和高碘酸盐形成络合物，在415nm处具有特征吸收峰.本文发现在CCB-300+PDS+Vis体系中加入高碘酸盐后在415nm处出现明显的特征吸收峰，而CCB-300和CCB-300+PDS体系均不能产生特征吸收峰(图6(c)).说明CCB-300+PDS+Vis体系中出现了Cu(Ⅲ).
采用电子顺磁共振(EPR)光谱进一步验证反应体系中哪些活性物种对TC降解起作用.以TEMP作为1O2的自旋捕获剂，以DMPO作为、⋅OH和的自旋捕获剂.如图6(d)所示，CCB-300+PDS+Vis体系中检测到强烈的TEMP-1O2加合物信号，结合自由基淬灭实验说明1O2在催化反应中起主要作用.体系中没有检测到和DMPO-⋅OH加合物信号，但是出现DMPO-X(1：2：1：2：1：2：1)的加合物信号.DMPO-X一般是认为是和DMPO-⋅OH被快速氧化的产物，CCB-300+PDS+Vis体系中的1O2可以氧化和DMPO-⋅OH生成DMPO-X[34].DMPO-X加合物信号的产生从侧面也说明在该体系中存在和⋅OH.此外，在该体系中检测到微弱的加合物的特征吸收峰.
2.4　反应机理分析
基于以上实验结果和讨论，提出可见光协同CCB-300活化PDS降解TC的可能催化反应机理.如图7a所示为降解反应机理图，反应过程中涉及的主要反应如式(1)~(6)所示.首先，在可见光激发下，CCB-300导带(ECB)产生光生电子(e-)，价带(EVB)产生光生空穴(h+)，由Tauc-plot图和VB-XPS图可得出CCB-300的带隙(Eg)和EVB分别为1.92eV和1.9V (vs. NHE) (图7b)，通过计算得到ECB电位为-0.02V (vs. NHE).Cu(Ⅱ)/Cu(Ⅰ)的氧化还原电位为0.153V，所以，ECB上的光生e-很容易将Cu(Ⅱ)还原为Cu(Ⅰ)，这就促进了Cu(Ⅱ)/Cu(Ⅰ)之间的价态转变，有利于产生更多的和⋅OH.由于的氧化还原电位(-0.33V vs. NHE)更负于ECB电位，所以，ECB上的光生e-不能与吸附于催化剂表面的氧分子生成，EPR
测试结果也证实只有微量的生成.EPR测试结果证实本反应过程有大量1O2产生，我们推断CCB-300与PDS形成的亚稳态络合物(CCB-300≡PDS)与H2O直接反应生成1O2[10].最终，1O2、和⋅OH共同参与TC降解反应.其中，非自由基途径产生的1O2起主要作用.
之前的高碘酸盐捕获Cu(Ⅲ)实验表明CCB-300+PDS+Vis体系有Cu(Ⅲ)生成，我们猜测EVB上具有强氧化性的光生h+可能将低价态铜氧化成为Cu(Ⅲ)(式(7))，此外，也可以与Cu(Ⅰ)或Cu(Ⅱ)直接反应生成Cu(Ⅲ)(式(8))[24,35].在此反应中Cu(Ⅲ)和CCB- 300≡PDS也可能参与了TC降解.
2.5　反应条件对催化反应影响
考察了PDS用量、初始溶液pH值、无机阴离子对降解反应的影响.如图8(a)所示，在其他条件保持不变的情况下，PDS的用量从0.1mmol/L增加至0.5mmol/L，TC的去除率从62.5%增加至96.9%，继续增加为1mmol/L时，TC的去除率为93.4%，略有下降，这可能是过量的PDS会按照方程式(9)淬灭反应体系中的[35].无机阴离子(Cl-、SO42-、NO3-等)普遍存在于实际水体，这些阴离子会与和⋅OH反应生产氧化能力较低的Cl⋅、和NO3⋅等
自由基，抑制催化降解反应.图8(b)是在反应体系中加入浓度为5mmol/L的Cl-、SO42-、NO3-、HCO3-几种无机阴离子后对TC降解性能的影响，可以看到加入几种无机阴离子后TC的去除率仍能在80%以上，总体来说对催化反应的影响不大.这也符合以非自由基途径活化PDS降解有机污染物不易受无机阴离子影响的特点.
图8(c)是溶液不同初始pH值条件下对降解TC的影响.在pH=3.1~10.0条件下，TC去除率均可达到92.3%以上.当pH=11时，TC去除率降至76.9%.这可能是由于在不同pH值条件下TC可电离成不同的离子态化合物，在pH<7.7条件下，TC主要以TCH3+和TCH2存在，当pH>7.7时，TC主要以TCH−、TC2−存在[36-37]，而对于CCB-300来说，如图8(d)所示，在pH=3.1-11.0条件下，Zeta电位由-7.0mV降至-21.5mV，说明催化剂表面均带负电荷，所以说在碱性条件下，CCB-300与TC分子之间存在静电斥力，不利于催化反应的进行.
2.6　催化剂的可重复使用性和稳定性
如图9(a)所示，CCB-300在连续循环使用6次后，CCB-300+PDS+Vis体系对TC去除率仍能够达到85.9%，去除率降低仅为11%.说明该催化剂具有较强的可重复使用性.催化剂活性稍有减弱的原因可能是部分降解中间有机产物或TC附着到CCB-300表面并占据其催化活性位点[26,38-40].图9(b)是反应前后催化剂的XRD谱图，可以看到反应前后的物相组成没有发生变化，说明CCB-300具有优异的稳定性.
3　结论
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3.1　通过低温水热加煅烧法成功制备碱式碳酸铜衍生片状氧化铜(CCB-300)，比表面积达到32.8m2/g，远高于碱式碳酸铜、C-CuO及其它文献报道氧化铜.较大的比表面积为催化反应提供更多潜在的活性位点.
3.2　相比于CCB-300+PDS、CCB-300+Vis和CCB+PDS+Vis体系，CCB-300+PDS+Vis体系降解TC的效率最高.这是由于CCB-300具有合适的带隙和优异的可见光吸收能力，在可见光照射下，其光生e-促进了Cu(Ⅱ)/Cu(Ⅰ)的循环转变，有利于PDS活化产生更多的和⋅OH.
3.3　CCB-300+PDS+Vis体系中以非自由基途径产生的1O2和以自由基路径生成的、⋅OH共同参与TC的降解反应，其中1O2起主导作用.
基金
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  • 山西工程科技职业大学校科技创新基金(202229)
  • 山西工程科技职业大学横向项目(2023HX021)
文献
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  • 接收时间：2024-08-12
  • 首发时间：2026-03-18
  • 出版时间：2025-03-20
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  • 收稿日期：2024-08-12
基金
山西工程科技职业大学校科技创新基金(202229)
山西工程科技职业大学横向项目(2023HX021)
作者信息
    1.山西工程科技职业大学交通工程学院，山西 太原 030619
    2.中北大学材料科学与工程学院，山西 太原 030051

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* 责任作者，副教授，
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2种不同金属材料的力学参数
科
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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