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Article(id=1240689596250518197, 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=1721577600000, receivedDateStr=2024-07-22, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773733050644, onlineDateStr=2026-03-17, pubDate=1739980800000, pubDateStr=2025-02-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773733050644, onlineIssueDateStr=2026-03-17, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773733050644, creator=13701087609, updateTime=1773733050644, 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=803, endPage=809, ext={EN=ArticleExt(id=1240689596477010623, articleId=1240689596250518197, tenantId=1146029695717560320, journalId=1234093305789726721, language=EN, title=Study on recovery efficiency and mechanism of high concentration fluoride by a nucleation crystallization pelleting process in photovoltaic wastewater, columnId=1234106386360103680, journalTitle=China Environmental Science, columnName=Water Pollution Control, runingTitle=null, highlight=null, articleAbstract=

In response to the challenge of coexisting high concentrations of fluoride (F-) and sulfate (SO42-) in photovoltaic wastewater, based on the principle of nucleation crystallization pelleting process (NCP), its efficacy and mechanisms for removing F-in such ion coexistence systems were thoroughly investigated. Our study demonstrated that under conditions (nucleation inducer dosage 4.46gMgCl2/gF, flow rate 67.8×10-4m3/h, static bed height 30%, and seed particle size 80~100mesh, F- removal efficiency reached up to 90%. To further validate the stability of the process system, continuous flow defluorination experiments were conducted over 120h. In the first stage (0~40hours), F- removal efficiency stabilized at approximately 89%, increasing to over 92% in the second stage (40~120hours), with granule purity exceeding 90%. Analysis using XRD and Roman revealed that F- predominantly adhered to seed surfaces in the forms of magnesium fluoride (MgF2) and sodium magnesium fluoride (NaMgF3). Static water contact angle tests and SEM-EDS characterization indicated that granules exhibited greater hydrophobicity compared to the raw seeds and formed a loose porous structure, thereby increasing their specific surface area and enhancing F- removal. The ZP revealed that in pH 6~8, the seed surface was positively charged, and F- was mainly concentrated around the surface of the seeds by electrostatic attraction, and then driven by the inducer to nucleate and grow into dense granulation on the surface of the seeds, effectively separating F- from water.

, correspAuthors=Peng-kang JIN, 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=Ya-dong WANG, Zhi-hao FU, Dan-heng ZHOU, Xiao-chang WANG, Peng-kang JIN, Xin JIN, Zhi-lin LI), CN=ArticleExt(id=1240689600549680014, articleId=1240689596250518197, tenantId=1146029695717560320, journalId=1234093305789726721, language=CN, title=光伏行业废水中高浓度氟离子核晶造粒回收效能与机制研究, columnId=1234106386565624579, journalTitle=中国环境科学, columnName=水污染与控制, runingTitle=null, highlight=null, articleAbstract=

针对光伏废水中高浓度氟离子与硫酸根共存的特征,基于核晶造粒技术原理,深入解析了该技术对于上述离子共存体系中氟离子的回收效能与机制.研究结果表明:当诱晶剂投加量为4.46gMgCl2/gF,进水流量为67.8×10-4m3/h,静态床高为30%,且晶种粒径为80~100目时,氟离子去除率高达90%.为进一步验证工艺系统稳定性,开展了为期120h的连续流除氟实验,第一阶段(0~40h)系统出水除氟效能可稳定在89%左右,第二阶段(40~120h)增加至92%左右,最终形成的造粒体纯度可达90%以上.结合X射线衍射(XRD)及拉曼光谱(Raman)等表征结果发现氟离子主要以氟化镁及氟镁酸钠的形式附着于晶种表面,且由静态水接触角测试结果及扫描电镜-能谱(SEM-EDS)表征结果发现造粒体表面相较于原晶种更为疏水,且形成了疏松多孔的结构,致使其比表面积更大,强化了造粒体对于氟离子的富集去除.经晶种表面电势电位(ZP)的测定发现,在pH值为6~8内,晶种表面荷正点,且氟离子主要通过静电引力富集于晶种表面,并在诱晶剂的驱动下,在晶种表面成核并生长成致密的造粒体,从水中分离.

, correspAuthors=金鹏康, authorNote=null, correspAuthorsNote=
*责任作者，教授，
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王亚东(1994-)，男，江苏南通人，西安建筑科技大学博士研究生，主要研究方向为污废水深度处理与资源化利用.发表论文2篇. .

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王亚东(1994-)，男，江苏南通人，西安建筑科技大学博士研究生，主要研究方向为污废水深度处理与资源化利用.发表论文2篇. .

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王亚东(1994-)，男，江苏南通人，西安建筑科技大学博士研究生，主要研究方向为污废水深度处理与资源化利用.发表论文2篇. .

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光伏行业废水中高浓度氟离子核晶造粒回收效能与机制研究
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王亚东 1 , 付梽浩 2 , 周丹姮 2 , 王晓昌 1 , 金鹏康 1, 2, * , 金鑫 2 , 李志林 3
中国环境科学 | 水污染与控制 2025,45(2): 803-809
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中国环境科学 | 水污染与控制 2025, 45(2): 803-809
光伏行业废水中高浓度氟离子核晶造粒回收效能与机制研究
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王亚东1 , 付梽浩2, 周丹姮2, 王晓昌1, 金鹏康1, 2, * , 金鑫2, 李志林3
作者信息
  • 1.西安建筑科技大学环境与市政工程学院，陕西 西安 710055
  • 2.西安交通大学人居环境与建筑工程学院，陕西 西安 710049
  • 3.云南氟业环保科技股份有限公司，云南 昆明 652199

    • 王亚东(1994-)，男，江苏南通人，西安建筑科技大学博士研究生，主要研究方向为污废水深度处理与资源化利用.发表论文2篇. .

通讯作者:

*责任作者，教授，
Study on recovery efficiency and mechanism of high concentration fluoride by a nucleation crystallization pelleting process in photovoltaic wastewater
Ya-dong WANG1 , Zhi-hao FU2, Dan-heng ZHOU2, Xiao-chang WANG1, Peng-kang JIN1, 2, * , Xin JIN2, Zhi-lin LI3
Affiliations
  • 1.Department of Environmental and Municipal Engineering, Xi’an University of Architecture and Technology, Xi’an 710055, China
  • 2.School of Human Settlements and Architectural Engineering, Xi’an Jiaotong University, Xi’an 710049, China
  • 3.Fluorine Industry Environmental Protection Technology (YUNNAN) Co., Ltd, Kunming 652199, China
出版时间: 2025-02-20
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摘要
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针对光伏废水中高浓度氟离子与硫酸根共存的特征,基于核晶造粒技术原理,深入解析了该技术对于上述离子共存体系中氟离子的回收效能与机制.研究结果表明:当诱晶剂投加量为4.46gMgCl2/gF,进水流量为67.8×10-4m3/h,静态床高为30%,且晶种粒径为80~100目时,氟离子去除率高达90%.为进一步验证工艺系统稳定性,开展了为期120h的连续流除氟实验,第一阶段(0~40h)系统出水除氟效能可稳定在89%左右,第二阶段(40~120h)增加至92%左右,最终形成的造粒体纯度可达90%以上.结合X射线衍射(XRD)及拉曼光谱(Raman)等表征结果发现氟离子主要以氟化镁及氟镁酸钠的形式附着于晶种表面,且由静态水接触角测试结果及扫描电镜-能谱(SEM-EDS)表征结果发现造粒体表面相较于原晶种更为疏水,且形成了疏松多孔的结构,致使其比表面积更大,强化了造粒体对于氟离子的富集去除.经晶种表面电势电位(ZP)的测定发现,在pH值为6~8内,晶种表面荷正点,且氟离子主要通过静电引力富集于晶种表面,并在诱晶剂的驱动下,在晶种表面成核并生长成致密的造粒体,从水中分离.

光伏行业  /  高浓度含氟废水  /  核晶造粒  /  氟离子  /  硫酸根离子

In response to the challenge of coexisting high concentrations of fluoride (F-) and sulfate (SO42-) in photovoltaic wastewater, based on the principle of nucleation crystallization pelleting process (NCP), its efficacy and mechanisms for removing F-in such ion coexistence systems were thoroughly investigated. Our study demonstrated that under conditions (nucleation inducer dosage 4.46gMgCl2/gF, flow rate 67.8×10-4m3/h, static bed height 30%, and seed particle size 80~100mesh, F- removal efficiency reached up to 90%. To further validate the stability of the process system, continuous flow defluorination experiments were conducted over 120h. In the first stage (0~40hours), F- removal efficiency stabilized at approximately 89%, increasing to over 92% in the second stage (40~120hours), with granule purity exceeding 90%. Analysis using XRD and Roman revealed that F- predominantly adhered to seed surfaces in the forms of magnesium fluoride (MgF2) and sodium magnesium fluoride (NaMgF3). Static water contact angle tests and SEM-EDS characterization indicated that granules exhibited greater hydrophobicity compared to the raw seeds and formed a loose porous structure, thereby increasing their specific surface area and enhancing F- removal. The ZP revealed that in pH 6~8, the seed surface was positively charged, and F- was mainly concentrated around the surface of the seeds by electrostatic attraction, and then driven by the inducer to nucleate and grow into dense granulation on the surface of the seeds, effectively separating F- from water.

photovoltaic industry  /  high concentration fluoride-containing wastewater  /  nucleation crystallization pelleting process (NCP)  /  fluoride  /  sulfate
王亚东, 付梽浩, 周丹姮, 王晓昌, 金鹏康, 金鑫, 李志林. 光伏行业废水中高浓度氟离子核晶造粒回收效能与机制研究. 中国环境科学, 2025 , 45 (2) : 803 -809 .
Ya-dong WANG, Zhi-hao FU, Dan-heng ZHOU, Xiao-chang WANG, Peng-kang JIN, Xin JIN, Zhi-lin LI. Study on recovery efficiency and mechanism of high concentration fluoride by a nucleation crystallization pelleting process in photovoltaic wastewater[J]. China Environmental Science, 2025 , 45 (2) : 803 -809 .
正文
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近年来，我国光伏等可再生能源正在迅猛发展，同时储能行业规模也在不断扩大.光伏电池制造过程中使用的氢氟酸会导致大量酸性含氟废水的产生，这种废水具有低pH值、高硝酸盐氮、高氟离子含量、低生物降解性和高重金属含量等特点，若直接排放，将严重威胁生态环境和人体健康[1-2].
目前常用的光伏废水处理技术包括化学沉淀法、吸附法、离子交换法以及膜技术等[3-6].吸附法由于其高效、简单、经济等优点，近年来得以广泛应用.唐婧等采用改性膨润土作为吸附剂，发现其在含氟废水中的吸附容量较大，且可通过简单的再生处理进行循环利用[7].离子交换法主要基于阴离子交换树脂与氟的交换从而实现氟的高效去除. Meenakshi等[8]比较了螯合树脂和阴离子交换树脂的除氟能力，发现前者对于氟离子具有高选择性但除氟容量较低.膜处理技术作为一种高效分离技术，在含氟废水处理中也取得了显著进展.Damite等[9]采用反渗透膜对氟化物废水进行处理，发现该技术可将废水中的氟浓度由10mg/L降至0.5mg/L以下，且处理效率较高.
然而，在含氟废水处理过程中，上述方法也普遍存在一些弊端；就吸附法而言，其应用常受限于吸附材料的处理效率，尤其是在高浓度含氟废水的处理方面[10]；离子交换法同样无法适应高浓度含氟废水的处理且其操作工艺复杂[11].膜处理技术常存在膜污染、能耗高以及膜更换频繁等问题[12].化学沉淀法因其具有操作简便，处理效率高以及处理成本低等优势而得以广泛使用，但其会产生大量高含水率污泥[13]，后续常需耦合沉淀、板框压滤等处置单元，极大增加了处理系统的占地面积及吨水处理成本[14].此外，氟作为一种有限资源，广泛应用于工业生产、农业以及医药等领域[15]，然而，上述方法无法有效实现废水中氟资源的回收，造成了资源浪费.因而，亟需开发一种高效、低耗、短流程的水处理技术，实现氟与硫酸根共存光伏废水中氟离子的高效回收.
化学结晶造粒技术能够诱导水中氟化钙的结晶，该工艺不仅降低了水中氟的浓度，而且生成了纯度更高的氟化钙颗粒，最大限度地减少了副产物的产生[16-17]，然而，现有研究仅针对100~400mg/L，对于更高浓度工业含氟废水（500~1000mg/L）的研究较少；此外，光伏废水中通常存在硫酸盐与氟离子共存的情况，常规的化学结晶造粒除氟技术常以钙盐为沉淀剂[18-19]，硫酸根的存在会与氟离子竞争水体中游离的钙离子及填料表面的活性位点[20]，造成处理效能的降低；同时，硫酸根与钙离子结合所形成的硫酸钙将造成最终产物纯度的下降[21].
针对上述问题，本文以云南某光伏企业高浓度含氟废水（共存硫酸根）为研究对象，采用本研究团队研发的核晶造粒技术（NCP），以氯化镁为诱晶剂，探究了水力学及水化学参数对核晶造粒处理高浓度含氟复合废水中氟离子及硫酸根离子去除的影响.并通过系列表征进一步解析了核晶造粒工艺在硫酸根共存下的氟离子回收的内在机制，以期为后续的工程应用提供依据.
1　材料与方法
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1.1　试验水质
试验所用原水取自云南某光伏公司，该企业废水主要为酸性电板清洗废水及浓碱水，按体积比4：1混合后进行集中处理（酸性水量为碱性水量的4倍）.
该光伏废水氟离子含量为896mg/L，同时含有207.5mg/L的硫酸根，浊度为0.5NTU，原水pH值仅为4.5，由于氟化镁沉淀的最佳pH值区间为6~8之间，为更好的诱导氟离子沉淀，需预调原水pH值.实验用水从厂区酸性电板清洗水出水管及浓碱水出水管处取回，保存于实验室阴凉避光处.
1.2　试验材料
试验所使用的填料为氟专用晶种（灵寿县安达矿物粉体厂，80~120目），该晶种具有比表面积大、无磁性以及耐冲击负荷等特性，初始粒径约为0.18mm；诱晶剂种类较多，由于水体中含有硫酸根，为避免硫酸根对于造粒体纯度的影响，特选取无水氯化镁为诱晶剂（阿拉丁）.
1.3　试验装置与方法
试验装置如图1所示，反应器主体由有机玻璃加工而成，底部设有进水口，在进水泵的作用下，注入含氟原水，进水流量为67.8×10-4m3/h，侧面底部设有加药口，在专用晶种充分流化的前提下，通过侧面加药口注入诱晶剂，驱动氟离子在晶种限域内达到过饱和，实现氟离子的附着沉淀；采用单因素实验分别研究诱晶剂投加量、进水流量、静床高度以及晶种粒径对核晶造粒工艺除氟效能的影响；其中，诱晶剂投加量通过加药泵流量及诱晶剂母液协同控制，固定加药泵流量为2.26×10-4m3/h，调整诱晶剂母液浓度，使反应体系内的诱晶剂投加量为1.12~5.58gMgCl2/gF；最后，处理水经顶部出水口流出，装置连续运行120h，每4h从出水口取样测定.上述核晶造粒反应器主要参数如下：高1.2m，内径20mm，壁厚3mm.
1.4　方法与仪器
pH值：奥豪斯ST3100型pH计；氟离子、硫酸根离子：DioNEXICS-600型离子色谱仪（GB/T 39305-2020）；浊度：哈纳HI93703-11浊度仪；形貌及元素分布表征：GeminiSEM360+牛津能谱；表面基团、晶型结构分析：日本-岛津-IRTracer100型傅里叶漫反射红外光谱仪，美国-Thermo Fisher-Dxr 2xi型拉曼光谱仪；Bruker-D8Advance型X射线衍射仪；材料亲疏水性：DSA100S型光学接触角/表面张力测量仪；氟化镁的过饱和指数以及不同pH值下氟离子的形态分布采用visual MINTEQ进行计算[22].
氟离子去除率及回收率的计算方法如下：
式中：C0为进水氟离子浓度；Cf为出水经0.45mm滤膜过滤后的浓度.
2　结果与讨论
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2.1　核晶造粒技术氟资源回收效能分析
核晶造粒技术运行参数对于光伏废水中氟离子与硫酸根的去除效能如图2所示.本文选用氯化镁为诱晶剂，依据溶度积原理，氟化镁的过饱和度是推动氟结晶过程的驱动力，其中镁离子浓度是影响氟去除效果的关键因素.如图2（a）所示，随着氯化镁投加量的增加（1.12~5.58gMgCl2/gF），废水中氟离子的去除率先增加后降低，且在氯化镁投加量为4gMgCl2/0.896gF时达到最大，为92.4%.此外，硫酸根的去除率随着诱晶剂的投加量持续增加，最大去除率为3%左右，硫酸根的去除主要归结为以下两个原因：一方面，在反应pH值区间内，晶种表面带正电（图3（b）），与硫酸根之间通过静电作用将其从水中吸附去除；另一方面，在诱晶剂加入的情况下，氟离子在晶种表面成核生长，同步裹挟部分硫酸根离子，使其发生共沉淀去除.当投加量由4.46gMgCl2/gF增加至5.58gMgCl2/gF时，浊度呈现出小幅增加，这可能归因于因诱晶剂过量而导致局部区域内氟离子的自成核作用.
在诱晶剂投加的基础上，反应体系中的上升流速、静床高度以及晶种粒径也对出水氟离子以及硫酸根的去除有着较大的影响；其中上升流速是影响氟离子与晶种之间传质的关键因素，如图2（b）所示，当进水流量为67.8×10-4m3/h时，氟离子的去除率达最佳，此时出水浊度较低（不超过5.0NTU），这表明在该流速下氟离子的回收效能最高；当流速过低时，晶种流化状态差，暴露的活性位点少；而过高的流速会直接将附着在晶种表面的氟化镁晶核冲刷下来；造成浊度的升高以及回收率的降低[23].静床高度即晶种填充量与晶种粒径与单位反应区域内除氟活性点位数呈正相关，但在一定流速下，填充量过大将直接干扰体系中晶种的流化状态，造成出水水质的下降；此外，粒径过小也将直接影响出水水质，小粒径晶种可有效增加比表面积，但在一定的上升流速下，也更易被上升水流带出体系，造成反应体系出水水质的下降及浊度的升高；在本研究中，最佳静床高度为装置有效高度的30%；最佳粒径为80~100目.
2.2　进水pH值、温度以及共存硫酸根浓度对于出水水质的影响
核晶造粒过程中进水pH值、温度及共存离子对于水处理效果存在一定干扰，就进水pH值而言，pH值的改变直接影响氟离子在废水中的赋存形态，如图3（d）所示，经环境水化学平衡软件Visual MINTEQ 3.1的模拟，氟离子在不同pH值条件下分别以F-、HF以及HF2-形态存在（如图3（d）），且随着pH值的升高，水体中的HF及HF2-逐渐减少，F-逐渐成为氟在水体中的主要存在形式，当pH值大于7时，主要以F-形态存在于水体中，诱晶剂的投加使氟离子达到过饱和状态，并于晶种表面成核析出，提高了氟离子的去除效能.随着pH值的进一步升高，晶种表面逐渐荷负电（图3（e）），氟离子与晶种表面之间的作用力由最初的静电引力逐渐变为斥力；此外，pH值的增加致使水体中OH-的浓度逐渐增加，与氟离子竞争水体中投加的镁离子而形成Mg（OH）2，造成出水浊度的增加以及氟离子去除率的下降（图3（a））.
进水温度是影响核晶造粒除氟的热力学因素，如图3（b）所示，氟离子与硫酸根的去除率随温度的升高而升高，这归因于，随着温度的升高，氟离子、诱晶剂的热运动增加，其与晶种之间的碰撞频率更高，更易于其表面成核生长；此外，如图3（f）所示，温度的升高致使生成氟化镁的过饱和指数越低，即在相同的诱晶剂投加量下，氟离子更易在晶种表面析出氟化镁晶核，进而强化水处理效能；
在光伏废水中，硫酸根往往与氟离子共存；如图3（c）所示，在不同的共存硫酸根浓度下，使用氯化镁作为诱晶剂对于氟离子去除的干扰较小，这归因于硫酸镁的溶度积较大，易溶于水；相比于硫酸根离子，氟离子更易与镁离子形成氟化镁晶核附着于晶种表面，且由于在反应区间内，晶种表面荷正电，在静电作用下，硫酸根离子与氟离子竞争晶种表面的活性位点，导致了硫酸根的吸附去除及氟离子去除效能的下降，经研究发现，在1200mg/L硫酸根离子共存的前提下，其对氟离子去除的干扰小于4%，因而可以忽略硫酸根离子对于晶种捕获氟离子的影响.
2.3　连续流实验及造粒体微观形貌表征
为进一步探究核晶造粒除氟工艺的稳定性，为现场中试实验奠定基础，本研究开展了为期120h的连续流稳定实验；如图4（a）所示，连续运行期间，出水pH值稳定在6~8，浊度稳定在5~10NTU，氟离子去除率前3d为89%左右，经过连续运行，后期去除率呈现出小幅度增加，为92%左右，同时结晶率也呈现出同样的趋势.这可能是因为晶种表面新生成物质强化了氟离子晶核的形成，促进了结晶反应的进行[24].
经过120h的运行后，将造粒体取出烘干，表征了其表观形貌，如图4（b）~（f）所示，图4（b）、4（d）为原晶种在不同倍率下的扫描电镜图像，原晶种表面平整，无明显的孔状结构；相较于原晶种，由于在诱晶剂的作用下，氟沉淀不断在原晶种表面成核生长，导致造粒体表面更加粗糙，由于硫酸根的存在，增加了空间位阻，使晶种表面形成了一种较为疏松多孔的结构（如图4（c）、4（e）所示），吸附诱导面积也相应增加，同时增加了氟离子的作用活性位点，使氟离子的去除效率得以进一步强化[25]，这也与图4（a）效果中的连续流性能数据规律一致.图4（f）为EDS能谱图，由图4可知，造粒体表面主要为镁，氟，钠3种元素，且占比分别为25.1%，40.35%以及19.45%，这表明在氟离子的去除过程中少量钠离子嵌入了氟化镁晶核.
2.4　造粒体组成成分及表面特性解析
为探究造粒前后晶种表面组成的变化，以及造粒后晶种表面的亲疏水性，分别对原晶种及造粒体进行了XRD，Roman以及表面亲疏水性表征；如图5（a）所示，为造粒前后的XRD谱图，相较于原晶种而言，运行120h后的造粒体在2θ=32.91°、35.28°、39.06°、43.41°及60.80°等多处出现氟化镁的衍射峰，说明含氟废水中的氟离子以氟化镁的形式附着与晶种表面；此外，造粒体在2θ=23.13°、37.27°、47.34°以及53.34°等多处出现了氟镁酸钠的衍射峰[26]，这是因为在起始含氟废水为酸性，为使其位于最佳pH值反应区间，加入氢氧化钠进行pH值回调，过程中残留的钠离子在氟化镁结晶时部分嵌入其晶格中，导致了氟镁酸钠的形成；此结果与图4（f）中的结果相一致.
上述结论也可由造粒体的拉曼光谱谱图得以证实；如图5（b）所示，相较于原晶种的拉曼谱图，造粒体谱图中在206cm-1、265cm-1以及467cm-1处出现了新的衍射峰，为氟化镁的拉曼衍射峰[27]，这与XRD谱图中造粒体表面形成了氟化镁与氟镁酸钠的结论相一致.由于在水溶液晶种表面存在水化层，核晶造粒的成核生长过程均需透过水化层而发生，因而晶种表面的亲疏水性与氟离子的去除效能息息相关[28]，如图5（c）所示，原晶种表面的静态水接触角为24.7°，为亲水性表面，成核阻力较大，造粒体表面的静态水接触角为95.6°，相比于原晶种，造粒体表面更为疏水，因而水化层更薄，氟离子成核阻力减小，去除效能得以增加，这也与连续流实验后期，氟离子去除效率增强相一致.
2.5　去除机理分析
基于上述表征分析，含氟废水的核晶造粒除氟机制如图（6）所示.由XRD图可知，氟离子主要以氟化镁的形式成核并结晶附着与晶种表面，由于钠离子的存在，部分钠离子嵌入晶核，形成了氟镁酸钠.具体机制如下：在反应pH值区间内，晶种表面荷正电（图3（e），在晶种的诱导下，氟离子优先富集与晶种表面，随着诱晶剂的投加，并辅以水力学（上升流速）调控，强化了晶种、氟离子与诱晶剂之间的碰撞机率，促进了氟化镁在晶种表面的成核；此外，由于前期为了调节含氟水pH值至6~8时引入了氢氧化钠，氢氧根离子用于中和废水中的氢离子，从而被消耗，残留的钠离子在氟化镁形成的过程中，部分嵌入氟化镁晶格中，形成了氟镁酸钠晶核并生长.如扫描电镜图所示，原晶种表面由于氟化镁（氟镁酸钠）不断的成核生长使其逐渐长大，由于硫酸根的存在，增加了空间位阻，形成了疏松多孔的结构，使其比表面积增大；此外，后期由于原晶种表面形成的氟化镁（氟镁酸钠）组成成分与待诱导产物类似且形成的表面更为疏水，因而在水化层变薄的同时，表面成核能垒降低；强化了氟离子的去除.
3　结论
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3.1　核晶造粒技术可有效回收水体中的氟离子，当诱晶剂投加量为4.46gMgCl2/gF，进水流量为67.8×10-4m3/h，静态床高为30%，且晶种粒径为80~100目时，氟离子去除效率最高可达90%以上，回收造粒体（氟化镁）纯度可达90%以上.
3.2　在晶种的诱导及诱晶剂（氯化镁）的协同驱动下，通过水力剪切作用，强化传质，使氟离子以氟化镁及氟镁酸钠的形式附着沉淀于晶种表面；且氟离子的去除机制主要为非均相成核.
3.3　硫酸根的共存造成了空间位阻的增强，致使造粒体表面呈现出疏松多孔的结构，比表面积增加，强化了氟离子的去除，致使连续流运行后期氟离子去除率提升3%以上.
基金
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  • 国家自然科学基金资助项目(52230001)
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2025年第45卷第2期
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  • 接收时间：2024-07-22
  • 首发时间：2026-03-17
  • 出版时间：2025-02-20
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  • 收稿日期：2024-07-22
基金
国家自然科学基金资助项目(52230001)
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    1.西安建筑科技大学环境与市政工程学院，陕西 西安 710055
    2.西安交通大学人居环境与建筑工程学院，陕西 西安 710049
    3.云南氟业环保科技股份有限公司，云南 昆明 652199

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