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Article(id=1234106385810649849, 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=1730563200000, receivedDateStr=2024-11-03, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1772163490965, onlineDateStr=2026-02-27, pubDate=1750348800000, pubDateStr=2025-06-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1772163490965, onlineIssueDateStr=2026-02-27, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1772163490965, creator=13701087609, updateTime=1772163490965, 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=3073, endPage=3083, ext={EN=ArticleExt(id=1234106386540458754, articleId=1234106385810649849, tenantId=1146029695717560320, journalId=1234093305789726721, language=EN, title=Deep purification for multiple pollutants in wet desulphurization wastewater, columnId=1234106386360103680, journalTitle=China Environmental Science, columnName=Water Pollution Control, runingTitle=null, highlight=null, articleAbstract=

This study implemented an integrated precipitation-air stripping-electrochemical oxidation process to treat limestone wet desulfurization wastewater, systematically investigating the effects of operational parameters on chloride removal, nitrogen elimination, and organic pollutant degradation. The removal mechanisms of multiple contaminants were comprehensively elucidated. Through response surface methodology (RSM) optimization, the salt precipitation achieved 66.9% chloride ion removal efficiency under optimal conditions (Ca/Al/Cl molar ratio of 6.8:1.9:1, operational temperature 37.5℃). Air stripping was conducted under alkaline condition, which attained 76.5% ammonia nitrogen removal efficiency. Finally, after 180min electrochemical oxidation, the effluent ammonia nitrogen and COD concentrations were significantly reduced to 7mg/Land 165mg/L, respectively. Mechanistic analysis revealed that the introduction of calcium-aluminum salts facilitated the transformation of tetrahedral Al(OH)4- into Ca-O-Al octahedral under high Ca/Al ratios and appropriate thermal conditions. Cl- were immobilized through adsorption or ion exchange by calcium-aluminum bimetallic layered hydroxide, then the Ca4Al2(OH)12Cl2•10H2O was formed and precipitated from the water. After precipitation-air stripping process, the residual Cl- concentration in the effluent was high, enabling its participation in electrochemical activation, and generating reactive species such as •Cl, •OH and 1O2, Thus those pollutants such as ammonia nitrogen and organic matters in the effluent was efficiently purified by direct anodic oxidation and indirect oxidation of active substances.

, correspAuthors=Yan-ling ZHANG, Shu-gen 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=Zheng-chao LI, Yan-ling ZHANG, Dao-ping ZHAN, Peng ZHAO, Sen-lin TIAN, Shu-gen LIU), CN=ArticleExt(id=1234106398800408984, articleId=1234106385810649849, tenantId=1146029695717560320, journalId=1234093305789726721, language=CN, title=湿法脱硫废水多污染物深度净化及作用机制, columnId=1234106386565624579, journalTitle=中国环境科学, columnName=水污染与控制, runingTitle=null, highlight=null, articleAbstract=

本研究采用沉淀-吹脱-电解工艺技术处理石灰石湿法脱硫废水，考察了工艺条件对除氯、脱氮、有机污染物去除的影响，并探究多污染物去除机制.基于RSM试验方法优化了复盐沉淀除氯工艺条件，在Ca/Al/Cl比例6.8:1.9:1、操作温度37.5℃条件下，脱硫废水中氯离子去除率为66.9%;碱性条件下空气吹脱处理，氨氮去除率为76.5%;再经电化学氧化处理180min，水体中氨氮和难降解有机物明显下降，出水氨氮和COD浓度分别降低至7mg/L与165mg/L.脱硫废水中投加钙铝复盐后，较高Ca/Al比以及适宜的反应温度促进四面体Al(OH)4-向Ca-O-Al八面体骨架转化，Cl-通过吸附或离子交换这类途径与钙铝双金属层状氢氧化物结合，生成固相物Ca4Al2(OH)12Cl2•10H2O并从水体沉淀析出;沉淀-吹脱处理后的尾水氯离子含量较高，在电化学作用下激发产生•Cl、•OH、1O2，水体中氨氮和难降解有机物通过阳极直接氧化与活性物质间接氧化得以高效净化.

, correspAuthors=张燕玲, 刘树根, authorNote=null, correspAuthorsNote=
* 责任作者，高级工程师，；
** 教授，
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李正超(1998-)，男，云南普洱人，昆明理工大学硕士研究生，主要从事水污染控制方面研究工作..

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李正超(1998-)，男，云南普洱人，昆明理工大学硕士研究生，主要从事水污染控制方面研究工作..

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李正超(1998-)，男，云南普洱人，昆明理工大学硕士研究生，主要从事水污染控制方面研究工作..

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Factors and their levels for dechloridation via double-salt coprecipitation

, figureFileSmall=null, figureFileBig=null, tableContent=
变量因子水平
-101
Ca/ClX1357
Al/ClX2123
反应温度(℃)X3204060
), ArticleFig(id=1234153445809246938, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1234106385810649849, language=CN, label=表1, caption=

复盐沉淀除氯各因子与水平设计

, figureFileSmall=null, figureFileBig=null, tableContent=
变量因子水平
-101
Ca/ClX1357
Al/ClX2123
反应温度(℃)X3204060
), ArticleFig(id=1234153445901521629, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1234106385810649849, language=EN, label=Table 2, caption=

Experiment design and test results based on RSM analysis

, figureFileSmall=null, figureFileBig=null, tableContent=
序号X1(Ca/Cl)X2(Al/Cl)X3(℃)Cl-去除率(%)模型预测值(%)
1524060.760.6
2524060.260.6
3334019.518.5
4512036.036.2
5714038.739.7
6326038.039.2
7734054.656.4
8516038.038.6
9726063.361.7
10524059.260.6
11536041.741.5
12524060.760.6
13532040.439.8
14314030.228.5
15322033.535.1
16524060.060.6
17722062.961.7
), ArticleFig(id=1234153445993796318, tenantId=1146029695717560320, journalId=1234093305789726721, articleId=1234106385810649849, language=CN, label=表2, caption=

基于RSM分析方法的试验方案及测试结果

, figureFileSmall=null, figureFileBig=null, tableContent=
序号X1(Ca/Cl)X2(Al/Cl)X3(℃)Cl-去除率(%)模型预测值(%)
1524060.760.6
2524060.260.6
3334019.518.5
4512036.036.2
5714038.739.7
6326038.039.2
7734054.656.4
8516038.038.6
9726063.361.7
10524059.260.6
11536041.741.5
12524060.760.6
13532040.439.8
14314030.228.5
15322033.535.1
16524060.060.6
17722062.961.7
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湿法脱硫废水多污染物深度净化及作用机制
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李正超 1 , 张燕玲 2, * , 詹道平 3 , 赵鹏 2 , 田森林 1 , 刘树根 1, **
中国环境科学 | 水污染与控制 2025,45(6): 3073-3083
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中国环境科学 | 水污染与控制 2025, 45(6): 3073-3083
湿法脱硫废水多污染物深度净化及作用机制
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李正超1 , 张燕玲2, * , 詹道平3, 赵鹏2, 田森林1, 刘树根1, **
作者信息
  • 1.昆明理工大学环境科学与工程学院，云南 昆明 650500
  • 2.云南天朗节能环保集团有限公司，云南 安宁 650300
  • 3.武钢集团昆明钢铁股份有限公司，云南 安宁 650300

    • 李正超(1998-)，男，云南普洱人，昆明理工大学硕士研究生，主要从事水污染控制方面研究工作..

通讯作者:

* 责任作者，高级工程师，；
** 教授，
Deep purification for multiple pollutants in wet desulphurization wastewater
Zheng-chao LI1 , Yan-ling ZHANG2, * , Dao-ping ZHAN3, Peng ZHAO2, Sen-lin TIAN1, Shu-gen LIU1, **
Affiliations
  • 1.Faculty of Environmental Science and Engineering, Kunming University of Science and Technology, Kunming 650500, China
  • 2.Yunnan Tianlang Energy-saving & Environment-Protection Co., Ltd., Anning 650300, China
  • 3.Wisco Group Kunming Iron & Steel Co., Ltd, Anning 650300, China
出版时间: 2025-06-20
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摘要
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本研究采用沉淀-吹脱-电解工艺技术处理石灰石湿法脱硫废水，考察了工艺条件对除氯、脱氮、有机污染物去除的影响，并探究多污染物去除机制.基于RSM试验方法优化了复盐沉淀除氯工艺条件，在Ca/Al/Cl比例6.8:1.9:1、操作温度37.5℃条件下，脱硫废水中氯离子去除率为66.9%;碱性条件下空气吹脱处理，氨氮去除率为76.5%;再经电化学氧化处理180min，水体中氨氮和难降解有机物明显下降，出水氨氮和COD浓度分别降低至7mg/L与165mg/L.脱硫废水中投加钙铝复盐后，较高Ca/Al比以及适宜的反应温度促进四面体Al(OH)4-向Ca-O-Al八面体骨架转化，Cl-通过吸附或离子交换这类途径与钙铝双金属层状氢氧化物结合，生成固相物Ca4Al2(OH)12Cl2•10H2O并从水体沉淀析出;沉淀-吹脱处理后的尾水氯离子含量较高，在电化学作用下激发产生•Cl、•OH、1O2，水体中氨氮和难降解有机物通过阳极直接氧化与活性物质间接氧化得以高效净化.

脱硫废水  /  多污染物  /  深度净化  /  复盐沉淀  /  电化学氧化

This study implemented an integrated precipitation-air stripping-electrochemical oxidation process to treat limestone wet desulfurization wastewater, systematically investigating the effects of operational parameters on chloride removal, nitrogen elimination, and organic pollutant degradation. The removal mechanisms of multiple contaminants were comprehensively elucidated. Through response surface methodology (RSM) optimization, the salt precipitation achieved 66.9% chloride ion removal efficiency under optimal conditions (Ca/Al/Cl molar ratio of 6.8:1.9:1, operational temperature 37.5℃). Air stripping was conducted under alkaline condition, which attained 76.5% ammonia nitrogen removal efficiency. Finally, after 180min electrochemical oxidation, the effluent ammonia nitrogen and COD concentrations were significantly reduced to 7mg/Land 165mg/L, respectively. Mechanistic analysis revealed that the introduction of calcium-aluminum salts facilitated the transformation of tetrahedral Al(OH)4- into Ca-O-Al octahedral under high Ca/Al ratios and appropriate thermal conditions. Cl- were immobilized through adsorption or ion exchange by calcium-aluminum bimetallic layered hydroxide, then the Ca4Al2(OH)12Cl2•10H2O was formed and precipitated from the water. After precipitation-air stripping process, the residual Cl- concentration in the effluent was high, enabling its participation in electrochemical activation, and generating reactive species such as •Cl, •OH and 1O2, Thus those pollutants such as ammonia nitrogen and organic matters in the effluent was efficiently purified by direct anodic oxidation and indirect oxidation of active substances.

desulfurization wastewater  /  multiple pollutants  /  deep purification  /  double-salt precipitation  /  electrochemical oxidation
李正超, 张燕玲, 詹道平, 赵鹏, 田森林, 刘树根. 湿法脱硫废水多污染物深度净化及作用机制. 中国环境科学, 2025 , 45 (6) : 3073 -3083 .
Zheng-chao LI, Yan-ling ZHANG, Dao-ping ZHAN, Peng ZHAO, Sen-lin TIAN, Shu-gen LIU. Deep purification for multiple pollutants in wet desulphurization wastewater[J]. China Environmental Science, 2025 , 45 (6) : 3073 -3083 .
正文
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石灰石湿法脱硫技术已经在燃煤电厂、钢铁企业、冶金行业广泛应用，但工艺过程定期废弃的脱硫废水含有高浓度的氯离子、氨氮、酚类、多环芳烃等有毒有害组分[1]，且具有盐度高、气味重、污染物难降解等典型特征.现今，较多采用离子交换、膜分离、吸附法等技术净化处理含氯废水，而蒸发浓缩技术如多效蒸发、机械蒸汽再压缩热泵蒸发，一般用于高盐度苦咸水或海水脱盐处理[2-3];也有研究指出，向含氯废水中投加特定化学试剂如硝酸银、硫酸钡等，可以促使氯离子形成不溶性沉淀物而从水体中得以分离[4].受设备腐蚀与结垢、潜在的二次污染、投资或运行成本高等因素制约，该类技术鲜少直接应用于脱硫废水的深度净化处理.基于常规的氯盐沉淀法，相关研究利用氢氧化钙和偏铝酸钠与水体中氯离子结合形成沉淀物[5]，在有效降低火电厂脱硫废水中氯离子的同时，对水体中Mn2+以及其他重金属也有较好的吸附效果;同样，该类技术也可应用于稀土冶炼废水的脱氯处理，在超声协同的单段式废水处理体系中，氯离子去除效率可达88.2%[6].复盐沉淀法具有反应速率快、能耗低、操作简便等优势，在石灰石湿法脱硫废水、冶金与化工等行业高浓度含氯废水处理方面具有良好应用前景，但工艺技术的基础研究尚不充分，过程调控与污染物迁移转化机制有待深入探究.
就废水中氨氮脱除而言，离子交换、折点加氯氧化、生物转化这类技术通常用于低浓度含氨废水处理[7-8];而中高浓度氨氮工业废水往往通过化学沉淀法或吹脱法予以处理[9].化学沉淀法在碱性条件下投加镁盐与磷酸盐以生成微溶沉淀物Mg(NH4)PO4，降低水体中氨氮的同时回收氮磷肥料.吹脱法则基于气液相平衡和传质速度理论，将废水中离子态NH4+转化为游离态NH3并向解吸的空气相转移，达到氨氮脱除的目的[10];该类工艺技术流程简单、运行费用较低，但同时存在低温时去除效率低、出水氨氮浓度偏高等不足之处.石灰石湿法脱硫废水氨氮浓度有时高达2500mg/L，如何经济、高效降低氨氮含量以满足废水处理与尾水回用的既定要求，尚缺少适宜的工艺技术与工程应用案例.
目前，钢铁企业与火电厂通常采用三联箱沉淀法处理石灰石湿法脱硫废水[11-12]，通过中和、沉淀、絮凝3个连续的处理单元去除废水中的重金属与悬浮物，该工艺对水体中氯离子、氨氮以及有机污染物去除效果甚为有限，处理后的出水无法直接回用或排放.本研究采用复盐沉淀+吹脱+电化学氧化工艺技术对钢铁企业石灰石湿法脱硫废水进行深度净化，将氯离子与钙铝双金属氢氧化物共沉淀，水体中余氯继而在电化学作用下原位产生活性物质并氧化氨氮与有机类组分，在考察水体中氯离子、氨氮、有机物去除效果的基础上，探讨多污染物迁移转化规律与去除作用机制，为脱硫废水深度净化与尾水回用提供参考.
1　材料与方法
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1.1　废水来源与特性
从昆明某钢铁企业采集石灰石湿法脱硫废水，其主要理化指标为：氯离子浓度9910~10350mg/L，COD含量1030~1150mg/L，氨氮含量2040~2250mg/L，硫酸根2010~2120mg/L，碳酸根425~460mg/L，硝酸根390~440mg/L，pH值6.5~6.8，总盐度3.9%~4.2%，电导率20.1~22.6ms/cm.
1.2　废水深度净化工艺
如图1所示，脱硫废水经一级反应器进行混凝沉淀预处理，所得上清液引入二级反应器中，投加复合药剂并调整水体pH值至碱性条件，缓慢搅拌处理以促进碱式钙铝氯复盐沉淀物生成;有效分离沉淀物后，对碱性上清液进行空气吹脱处理，用清水吸收吹脱尾气回收得到稀氨水，所得尾水引至电化学装置;利用电化学作用激发残余氯离子产生强氧化活性物质，进一步分解与去除水体中氨氮与难降解有机物.
1.3　试验方案
1.3.1　复盐沉淀除氯
脱硫废水中投加CaO将pH值调整至(9.0±0.2)，搅拌均匀后静置沉降10min，将上清液转移至二级反应器中，按比例投加CaO和NaAlO2，在转速50r/min条件下搅拌并反应90min.基于前期预试验结果，原水中共存阴离子如硝酸根、碳酸根、硫酸根浓度低于500mg/L均不会影响复盐沉淀进程.
本研究选择Ca/Cl、Al/Cl物质的量比以及反应温度3个影响甚为明显的因素，考察其对复盐沉淀除氯效果的影响，响应曲面法(RSM)试验方案设计如表1所示.
1.3.2　吹脱法脱除氨氮
将复盐沉淀除氯的废水固液分离，所得液体转入孟氏洗瓶，通入空气进行吹脱除氨，采用清水吸收吹脱气.开展批次对照试验时，工艺条件如下：气液比0.5,1.0,1.5,2.0,2.5(L/min:L)，操作温度25,35,45,55,65℃，初始pH值4.0,6.0,8.0,10.0,12.0，吹脱时间均为150min.
1.3.3　电化学氧化处理
脱硫废水经沉淀-吹脱处理后，所得尾水引入电化学装置予以净化处理.该装置的圆柱形阳极固定于反应器中央，阳极基体材料表层均匀镀覆Ti/Pt以提升极板电化学性能;将钛箔卷成环状构成阴极板，安装于圆形反应器内侧.在不同溶液初始pH值、极板间距、电流密度条件下开展对照试验，测试水体中氨氮和有机污染物(以化学需氧量COD表示)浓度变化.在典型体系中分别加入硝基苯NB、甲醇MeOH、糠醇FFA[13-14]，其溶液浓度均为25mmol/L，进行自由基猝灭对照试验，剖析氯、氧活性物质与水体污染物迁移转化的内在关联.
1.4　分析与表征
采用离子色谱仪(CIC-D100，青岛盛瀚)测定废水中氯离子浓度，基于纳氏比色法与重铬酸钾快速消解--分光光度法(DR 6000，美国HACH)分别测定水体中氨氮和COD含量.
电化学体系中，分别添加5,5-二甲基-1-吡啶-N-氧化物(DMPO)、2,2,6,6-四甲基哌啶(TEMP)和N-叔丁基-α-苯基硝酮(PBN)以捕获溶液中•OH、1O2、•Cl[15-16]，利用EPR波谱仪(A300，德国Bruker)检测样本中活性物质的信号强度.
利用X射线衍射仪(XRD，SmartLab SE，日本Rigaku)对复盐沉淀物2θ为5°~90°区域进行扫描，分析沉淀物的物相组成及相对含量变化情况.采用X射线光电子能谱仪(XPS，K-Alpha，美国Thermo Fisher)对沉淀物表面组成及化学状态进行分析.
2　结果与讨论
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2.1　复盐沉淀除氯
基于RSM分析法设计了3因素3水平系列试验，不同工艺条件下废水中氯离子去除率变化情况如图2所示.
利用Design-Expert 10软件对试验结果(表2)进行分析，得到氯离子去除率(Y)与Ca/Cl(X1)、Al/Cl(X2)以及反应温度(X3)3个因素之间的二次多项式如下：
该模型表达式中，R2 = 0.993,P<0.0001，失拟项水平不显著(P>0.05)，表明模型拟合度和可信度良好.从交互项系数来看，Ca/Cl(X1)与Al/Cl(X2)对氯离子去除效果的影响交互作用最为显著，而Ca/Cl(X1)与反应温度(X3)、Al/Cl(X2)与反应温度(X3)这两组双因素之间并没有明显的交互作用.
基于响应面的参数优化，得到氯离子去除率的最佳试验条件为：Ca/Cl、Al/Cl比例分别为6.8与1.9，反应温度为37.5℃，氯离子去除率预测值为66.5%.在此条件下开展复盐沉淀除氯验证试验，3次平行试验中氯离子去除效果分别为66.7%、67.1%、67.0%，其均值为66.9%，与理论值甚为吻合.对钢铁企业石灰石湿法脱硫废水而言，原水温度通常为50~60℃，经预处理送至复盐沉淀操作单元的待处理水水温一般为33~42℃，与复盐沉淀工艺的最适反应温度37.5℃较为接近.因此，开发的工艺技术应用于钢铁企业、燃煤电厂深度净化处理石灰石湿法脱硫废水时，在无需额外加热条件下即可维持良好的水体除氯效果.
2.2　吹脱法脱除氨氮
如图3所示，随着吹脱空气的流速增大以及操作温度的上升，水体中氨氮浓度均呈现下降趋势;当气液比为2.0L/min:L且操作温度为45℃时，氨氮去除率达到76.5%.继续增大气液比或提高操作温度能够降低氨气在水体中的溶解度、促进气液传质过程从而强化氨氮吹脱效率[17-18]，但提升率并不十分明显(图3);另外，较高的气液比以及操作温度必然导致动力消耗与高温能耗等水处理运行成本明显增加.综上考虑，选择气液比2.0L/min:L、操作温度45℃作为吹脱法脱除氨氮的适宜工艺技术参数.
待处理的脱硫废水由酸性提升至碱性条件时，水体中氨氮吹脱效率明显提升(图3(c)).酸性条件下，水体中氨氮浓度高达1900mg/L，其去除率均低于6.3%;当pH值分别调整至10.0、12.0时，氨氮去除率分别上升至68.3%、74.4%.基于溶液中氨离子解离作用，废水中游离态NH3所占比例为：NH3(%)=100/[1+([H+]/Ka)][18](Ka为氨解离常数).高pH值条件下，氨氮主要以游离NH3分子态形式存在，因而能够通过吹脱方式得以有效去除;而低pH值条件下，氨氮以不易挥发的NH4+离子形式存在，难以吹脱去除.本次设计的脱硫废水深度净化工艺中，复盐沉淀除氯后所得废水pH值通常为12.0~12.5，为氨氮吹脱去除提供了合适的pH值条件.综合考虑连续运行及水处理成本，选取pH值12.0、气液比2L/min：L、操作温度45℃作为氨氮吹脱的适宜工艺条件，连续运行处理150min，水体中氨氮浓度下降至415mg/L；COD浓度为1150mg/L，无明显降低.
2.3　电化学氧化处理
如图4所示，净化处理前期，酸性条件下水体中COD去除率略高于碱性条件;当净化时间大于120min后，不同初始pH值的4个电化学体系中COD去除率均较为接近.而从氨氮浓度变化看，初始pH值从4.0上升至10.0时，同一时期氨氮去除率略有差异，近中性条件时相对稍高;初始pH值为8.0的电化学体系，在运行时间120、180min时氨氮去除率分别高达95.6%、98.0%(图4 (a、b)).
当电化学体系的极板间距设置为4cm时，待处理水体的氨氮与COD去除率在180min时分别为97.9%与84.0%;当极板间距扩大至6cm时，同期的氨氮与COD去除率分别下降至70.6%与42.7%(图4(c、d)).极板间距过小时，电极板表面钝化而导致电解效率降低、能耗增加[19];但极板间距过大时，电极之间电阻增大、电压升高，能耗同样随之增加，且电化学体系中氨氮与COD去除效能也明显下降[20].
电流密度从30mA/cm2增加至70mA/cm2时，水体中污染物去除效能随之提升(图4(e、f))，其原因主要归因于电流密度的增加能够加快电子在电极表面的迁移速率，进而激发产生活性物质并氧化分解水体中污染物.电流密度增大至90mA/cm2时，过高的电流密度导致阳极发生明显的析氧反应，不但降低了电流利用效率和污染物氧化分解能力，还会增加能量消耗，不利于净化体系稳定运行.综合考虑水体污染物效能提升与能耗需求，确定电流密度50mA/cm2为脱硫废水净化处理适宜的工艺技术参数.
2.4　废水中典型污染物的迁移转化途径
2.4.1　复盐沉淀产物的表征与分析
复盐沉淀除氯过程中，在Ca：Al：Cl物质的量比分别为6.8：1.9：1,1：1：1,1：3：1(操作温度均为37.5℃)以及操作温度分别为60,37.5,20℃(Ca：Al：Cl物质的量比均为6.8：1.9：1)条件下开展对照试验，收集沉淀产物并分析其物相组成.XRD图谱在11.3°、23.3°、31.0°、34.0°、50.8°等处存在不同强度的衍射峰，表明复盐沉淀产物中存在含氯弗里德尔盐(Friedel’s Salt)Ca4Al2(OH)12Cl2•10H2O.相比而言，所得沉淀物在Ca/Al/Cl物质的量比6.8：1.9：1、操作温度37.5℃这一工况条件下Ca4Al2(OH)12Cl2•10H2O衍射峰强度最大，但同时也存在Ca(OH)2、Ca3Al2(OH)12、Al(OH)3低强度衍射峰(图5(a、b))，表明脱硫废水投加复盐后存在多个沉淀反应进程.低Ca/Cl且高Al/Cl(即Ca：Al：Cl比例1：3：1)以及过高/过低操作温度(即60/20℃)条件下，沉淀产物中Ca3Al2(OH)12、Al(OH)3衍射峰均有所增强.有其他研究表明，弗里德尔盐生成进程中，n(Ca)：n(Al)<2时副反应甚为明显;随着含钙/铝试剂添加量的增加，Cl-去除率逐步上升，Ca4Al2(OH)12Cl2•10H2O衍射峰不断增强[21].可见，工艺操作条件明显影响复盐沉淀过程，减少沉淀副反应有助于提升水体除氯效果.
利用X射线光电子能谱仪(XPS)分析不同钙铝氯比例以及操作温度条件下所得沉淀物的表面状态(图5(c~e)).根据NaCl中Cl2p谱线，Cl2p3/2结合能峰在198.4eV附近[22]，本研究199.5、198.8eV附近的结合能峰归属于Cl2p，证实脱硫废水中的氯离子已经转移至固相沉淀物钙铝氧类复盐之中.从O1s结合能来看，530.2~530.6eV处的峰归属于晶格氧(O2-，符号为Oa)[23]，而531.5~531.7eV处的峰则对应于表面吸附氧(O22-，符号为Ob)[24].晶格氧容易与金属离子形成较强的配位键，Oa百分比越高则沉淀物越稳定[25]，水体中Cl-也就难以进入弗里德尔盐中间层交换OH-并得以固定与沉淀去除;与此同时，沉淀物表面吸附氧Ob可以选择性地被其他阴离子取代而生成新的物质[26].本次对照试验中，在Ca: Al: Cl物质的量比6.8: 1.9: 1、操作温度37.5℃条件下所得沉淀产物中Oa与Ob所占比例分别为18.6%与81.4%，此条件下脱硫废水除氯效果最为明显.同样，Al2p能谱可分为两个峰，分别对应四面体(Al4)与六面体配位(Al6);而CaAl氧化物转变为层状双金属氢氧化物LDHs是以Al配位变化为特征，由四方Al(OH)4-重构形成Al-O八面体骨架，进而转化为Ca-O-Al框架的双金属沉淀物[22].可见，当Al6所占比例较大时，更有利于形成稳定的含氯弗里德尔复盐沉淀物从而提升水体除氯效果.
2.4.2　电化学体系中活性物种及其贡献
鉴于•OH、1O2和•Cl这类活性物质对电化学体系污染物降解的重要贡献[14-15]，本研究在氨氮吹脱后的废水中引入不同类型的猝灭剂以考察水体中存在的活性物种及其贡献.考虑到硝基苯NB等猝灭剂均为有机物质，添加后会导致水体COD发生变化，故采用氨氮去除率作为污染物降解效果的重要评价指标.不添加猝灭剂的对照组电化学处理120min时，水体中氨氮和COD的去除效率分别为95.6%和64.6%;在运行时间为30min时，分别利用DMPO、TEMP和PBN作为捕获剂时检测水体中活性物质，EPR谱图中存在DMPO-OH四重特征峰、TEMP-1O2三重特征峰以及PBN-Cl八重特征峰(图6 (b-d))，证实该水处理体系中同时存在活性组分•OH、1O2与•Cl.当吹脱后的脱硫废水中分别加入硝基苯NB、甲醇MeOH以及糠醇FFA后，氨氮去除率均有不同程度的降低.净化处理时间达120min时，添加NB、MeOH、FFA的3个水处理体系氨氮去除率分别为73.7%、47.6%、81.5%，较不添加猝灭剂的对照组降低值分别为21.9%、48.0%和14.1%(图6(a)).氨氮与•OH、•Cl、1O2的反应速率常数分别为1.8×108,1.1×109,3.2×106L/(mol·s)[27-29]；MeOH能与•OH与•Cl反应，其速率常数分别为9.7×108、5.5×109L/(mol·s)；NB与•Cl不发生反应，其与•OH的反应速率为3.9×109L/(mol·s)[15];而FFA与1O2反应速率为1.2×107L/(mol·s)[30].据此测算，单独猝灭水体中活性组分•OH、1O2、•Cl后，氨氮去除率降低值分别为21.9%、14.1%、26.1%，这就反映出脱硫废水中的Cl-对污染物电化学氧化进程具有极为重要的贡献.
2.4.3　水体中污染物的迁移转化
(1)氯离子迁移转化：采用复盐沉淀+吹脱+电化学氧化工艺深度净化石灰石湿法脱硫废水时，Cl-主要通过生成弗里德尔盐而从水体转移至固体沉淀物中(图7).脱硫废水中投加CaO和NaAlO2后，反应生成Ca(OH)2和Al(OH)3，由于水体中存在大量Cl-，将较好阻止水化产物Ca3Al2O6•6H2O形成[31]，进而诱导水体中的Al转化为四面体Al(OH)4-(式. 1).高Ca/Cl、Al/Cl条件下，水体中Ca2+与Al(OH)4-进一步结合，形成含有Ca、Al的层状结构[Ca4Al(OH)12•10H2O]2+(式. 2).该物质表面吸附氧Ob含量明显高于晶格氧Oa(图5(d))，且带两个单位正电荷，有利于带负电的Cl-迁移至弗里德尔盐骨架的层间区域[6]，最终形成含氯固体物质Ca4Al2(OH)12Cl2•10H2O(式.3).与此同时，较高的Ca/Al比以及适宜的反应温度能够促进Al(OH)4-与Ca(OH)2反应，四面体Al(OH)4-转化成Al-O八面体骨架(图5(e))，形成中间体Ca4Al2(OH)14•10H2O，部分Cl-与中间体层内的OH-发生离子交换(式.4~5)，生成固相物Ca4Al2(OH)12Cl2•10H2O(图5(a-b))，经后续沉淀分离后实现水体中氯离子去除.
(2)氨氮和难降解有机物迁移转化：脱硫废水的电化学净化体系中，氨氮和难降解有机物(R)的去除与阳极(M)直接氧化以及活性物质(•OH、•Cl、1O2、HClO)间接氧化密切相关(图7).水体中氨氮包括离子态NH4+和游离态NH3，溶液pH值影响氨电离平衡并决定NH4+与NH3相对含量.氨氮可以在阳极板表面失去电子而被直接氧化成氮气[32]，同样，难降解有机物R也会发生阳极直接氧化[33]，最终矿化生成CO2和H2O这类产物(式.6~7).此外，高氯脱硫废水的电化学体系中，产生大量活性物质如•OH、•Cl、1O2(图6)，也会在电解作用下生成Cl2并进一步解离产生HClO(式.8).除HClO可以氧化水体中氨氮外，电化学体系产生的活性组分•OH、1O2、•Cl也有很好的脱氮效果(式.9~10)，其对水体氨氮去除的贡献率分别为21.9%、14.1%、26.1%(图6(a))，含氯活性物质对氨氮的氧化去除贡献尤为突出.
脱硫废水经沉淀-吹脱处理后Cl-含量通常为3300~3600mg/L，采用电化学手段进行后续净化处理时，水体中原位产生大量含氯活性组分，同时激发形成含氧活性物质，除氧化氨氮外，也能氧化分解水体中难降解的污染物R，生成系列中间产物(如RCl、R′等)，并最终矿化为CO2和H2O这类小分子末端产物(式.11~12).本次试验研究中，吹脱后的脱硫废水电化学处理180min时，水体中氨氮和COD去除效率分别达到97.9%和84.0%(图4)，出水氨氮和COD浓度分别下降至7mg/L与165mg/L，取得了良好的深度净化效果.
3　结论
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3.1　复盐沉淀阶段，Ca/Al/Cl比例6.8:1.9:1、操作温度37.5℃条件下Cl-去除率达66.9%，此时复盐沉淀物Ob和Al6含量较高，促进了四面体Al(OH)4-向Ca-O-Al八面体骨架转化，Cl-通过吸附作用或离子交换形成稳定固相物Ca4Al2(OH)12Cl2•10H2O，显著降低水体Cl-含量.
3.2　氨氮吹脱阶段，初始pH值为12.0、气液比2L/min:L、操作温度45℃条件下，连续运行150min，氨氮去除率达76.4%.优化条件提升了氨氮的传质效率和吹脱速率，增强氨氮从水相向气相的转移.
3.3　经该工艺全流程处理后，出水氨氮、COD和重金属离子分别低于9.3，180，0.033mg/L，符合《钢铁工业水污染物排放标准》(GB13456-2012)间接排放规定的污染物浓度限值.EPR及自由基猝灭实验表明，OH、•Cl、1O2等活性物质参与了氨氮和COD氧化降解过程.
基金
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  • 云南省中青年学术与技术带头人后备人才项目(202105AC160096)
文献
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2025年第45卷第6期
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  • 接收时间：2024-11-03
  • 首发时间：2026-02-27
  • 出版时间：2025-06-20
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  • 收稿日期：2024-11-03
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云南省中青年学术与技术带头人后备人才项目(202105AC160096)
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    1.昆明理工大学环境科学与工程学院，云南 昆明 650500
    2.云南天朗节能环保集团有限公司，云南 安宁 650300
    3.武钢集团昆明钢铁股份有限公司，云南 安宁 650300

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* 责任作者，高级工程师，；
** 教授，
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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
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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