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Article(id=1149776966775173766, tenantId=1146029695717560320, journalId=1146123166801305609, issueId=1149776900194791454, articleNumber=null, orderNo=null, doi=10.12404/j.issn.1671-1815.2403980, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1716912000000, receivedDateStr=2024-05-29, revisedDate=1727193600000, revisedDateStr=2024-09-25, acceptedDate=null, acceptedDateStr=null, onlineDate=1752057790701, onlineDateStr=2025-07-09, pubDate=1744905600000, pubDateStr=2025-04-18, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1752057790701, onlineIssueDateStr=2025-07-09, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1752057790701, creator=13701087609, updateTime=1752057790701, updator=13701087609, issue=Issue{id=1149776900194791454, tenantId=1146029695717560320, journalId=1146123166801305609, year='2025', volume='25', issue='11', pageStart='4397', pageEnd='4826', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=0, createTime=1752057774827, creator=13701087609, updateTime=1768456666677, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1218558837930512931, tenantId=1146029695717560320, journalId=1146123166801305609, issueId=1149776900194791454, language=EN, specialIssueTitle=, coverIllustrator=, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1218558837930512932, tenantId=1146029695717560320, journalId=1146123166801305609, issueId=1149776900194791454, language=CN, specialIssueTitle=, coverIllustrator=, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=4801, endPage=4808, ext={EN=ArticleExt(id=1149776966959723143, articleId=1149776966775173766, tenantId=1146029695717560320, journalId=1146123166801305609, language=EN, title=Optimization of Tetracycline Adsorption Performance by Sludge Biochar and Adsorption Mechanism Research, columnId=1156262729993277777, journalTitle=Science Technology and Engineering, columnName=Papers·Environmental and Safe Science, runingTitle=null, highlight=null, articleAbstract=

The transformation of sludge into biochar adsorbents for the removal of tetracycline contaminants in water bodies represents one of the effective approaches for the resource utilization of sludge and enables the realization of the circular economy concept of “treating waste with waste”. Municipal sludge was employed as the raw material, and sludge biochar was fabricated through pyrolysis for the adsorption and removal of tetracycline. The adsorption and removal efficacy of tetracycline was investigated, and the preparation conditions of sludge biochar and adsorption environmental conditions were optimized. Additionally, by combining methods such as scanning electron microscopy, infrared spectroscopy, and BET(Brunauer,Emmett,Teller) specific surface area testing, the structural characteristics of sludge biochar and the underlying mechanism of its adsorption behavior towards tetracycline were explored. The results indicate that the sludge biochar prepared under a pyrolysis temperature of 800 ℃ and a pyrolysis duration of 4 hours exhibits the optimal adsorption performance for tetracycline. The pH value exerts a significant influence on the adsorption effect. In a weakly acidic environment, the adsorption effect of sludge biochar on tetracycline is the most favorable, with a maximum adsorption capacity reaching 45.33 mg/g. Thermodynamic and kinetic analyses demonstrate that the pseudo-second-order kinetic model and the Langmuir adsorption isotherm model can appropriately fit the adsorption process of tetracycline by sludge biochar. The adsorption process is primarily monolayer adsorption, dominated by surface chemical adsorption. In conjunction with the analysis of characterization test results, the chemical adsorption mainly involves processes such as electrostatic attraction, cation exchange, complex precipitation, π-π conjugation, and hydrogen bonding. Simultaneously, the pore structure characteristics of sludge biochar result in the adsorption process of tetracycline also encompassing pore filling and Van der Waals force.

, correspAuthors=Duo MENG, 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=Wei LIU, Duo MENG, Shu-ping CHU, Xiang LI), CN=ArticleExt(id=1149776982889690009, articleId=1149776966775173766, tenantId=1146029695717560320, journalId=1146123166801305609, language=CN, title=污泥生物炭对四环素吸附性能的优化及吸附机理, columnId=1156262730140078420, journalTitle=科学技术与工程, columnName=论文·环境科学、安全科学, runingTitle=null, highlight=null, articleAbstract=

将污泥转化为生物炭吸附剂,用于去除水体中的四环素污染物,是污泥资源化利用的有效途径之一,且能够实现“以废治废”的循环经济理念。以市政污泥为原料,采用热解法制备污泥生物炭并吸附去除四环素,面向四环素吸附去除效果考察并优化了污泥生物炭制备条件及吸附环境条件,并结合扫描电镜、红外光谱及BET(Brunauer、Emmett和Teller)比表面积测试等手段,探究了污泥生物炭结构特性及其对四环素吸附行为的内在机理。结果表明:热解温度为800 ℃,热解时间为4 h条件下所制备的污泥生物炭对四环素具有最佳的吸附性能; pH对吸附效果影响较大,在弱酸性环境下,污泥生物炭对四环素的吸附效果最优,最大吸附量达到45.33 mg/g。热力学及动力学分析表明,准二级动力学模型和Langmuir吸附等温模型能较好拟合污泥生物炭吸附四环素的过程,吸附过程主要为单分子层吸附,且以表面化学吸附为主,结合表征测试结果分析,化学吸附主要涉及静电吸引、阳离子交换、络合沉淀、π—π共轭作用及氢键作用等过程;同时,污泥生物炭的孔结构特性使其对四环素的吸附过程还包含孔隙填充及范德华力作用。

, correspAuthors=孟多, authorNote=null, correspAuthorsNote=
* 孟多(1981—),女,汉族,辽宁阜新人,教授,博士。研究方向:固体废弃物综合利用技术。E-mail:。
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刘炜(2000—),男,土家族,重庆市忠县人,硕士研究生。研究方向:污泥资源化利用。E-mail:。

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刘炜(2000—),男,土家族,重庆市忠县人,硕士研究生。研究方向:污泥资源化利用。E-mail:。

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刘炜(2000—),男,土家族,重庆市忠县人,硕士研究生。研究方向:污泥资源化利用。E-mail:。

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figureFileBig=ajVyX4KgAw9Q7EiCo7CPoA==, tableContent=null), ArticleFig(id=1218843919731835711, tenantId=1146029695717560320, journalId=1146123166801305609, articleId=1149776966775173766, language=CN, label=图10, caption= SBC 800 ℃ , 4 h的孔径分布图, figureFileSmall=UfBfOHCLSBLA49owoqzieA==, figureFileBig=ajVyX4KgAw9Q7EiCo7CPoA==, tableContent=null), ArticleFig(id=1218843919849276225, tenantId=1146029695717560320, journalId=1146123166801305609, articleId=1149776966775173766, language=EN, label=Table 1, caption=

Preparation conditions for SBCs

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编号 热解
温度/℃		 热解
时间/h		 编号 热解
温度/℃		 热解
时间/h
1 500 2 7 700 2
2 500 3 8 700 3
3 500 4 9 700 4
4 600 2 10 800 2
5 600 3 11 800 3
6 600 4 12 800 4
), ArticleFig(id=1218843919970911050, tenantId=1146029695717560320, journalId=1146123166801305609, articleId=1149776966775173766, language=CN, label=表1, caption=

SBC的制备条件

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编号 热解
温度/℃		 热解
时间/h		 编号 热解
温度/℃		 热解
时间/h
1 500 2 7 700 2
2 500 3 8 700 3
3 500 4 9 700 4
4 600 2 10 800 2
5 600 3 11 800 3
6 600 4 12 800 4
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污泥生物炭对四环素吸附性能的优化及吸附机理
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刘炜 1 , 孟多 1, * , 褚书平 1 , 李响 2
科学技术与工程 | 论文·环境科学、安全科学 2025,25(11): 4801-4808
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科学技术与工程 | 论文·环境科学、安全科学 2025, 25(11): 4801-4808
污泥生物炭对四环素吸附性能的优化及吸附机理
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刘炜1 , 孟多1, * , 褚书平1, 李响2
作者信息
  • 1 辽宁工业大学土木建筑工程学院, 锦州 121000
  • 2 辽宁城建设计院有限公司沈阳分公司, 沈阳 110015

    • 刘炜(2000—),男,土家族,重庆市忠县人,硕士研究生。研究方向:污泥资源化利用。E-mail:。

通讯作者:

* 孟多(1981—),女,汉族,辽宁阜新人,教授,博士。研究方向:固体废弃物综合利用技术。E-mail:。
Optimization of Tetracycline Adsorption Performance by Sludge Biochar and Adsorption Mechanism Research
Wei LIU1 , Duo MENG1, * , Shu-ping CHU1, Xiang LI2
Affiliations
  • 1 School of Civil and Architectural Engineering, Liaoning University of Technology, Jinzhou 121000, China
  • 2 Shenyang Branch of Liaoning Urban Construction Design Institute Corp. Ltd., Shenyang 110015, China
出版时间: 2025-04-18 doi: 10.12404/j.issn.1671-1815.2403980
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摘要
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将污泥转化为生物炭吸附剂,用于去除水体中的四环素污染物,是污泥资源化利用的有效途径之一,且能够实现“以废治废”的循环经济理念。以市政污泥为原料,采用热解法制备污泥生物炭并吸附去除四环素,面向四环素吸附去除效果考察并优化了污泥生物炭制备条件及吸附环境条件,并结合扫描电镜、红外光谱及BET(Brunauer、Emmett和Teller)比表面积测试等手段,探究了污泥生物炭结构特性及其对四环素吸附行为的内在机理。结果表明:热解温度为800 ℃,热解时间为4 h条件下所制备的污泥生物炭对四环素具有最佳的吸附性能; pH对吸附效果影响较大,在弱酸性环境下,污泥生物炭对四环素的吸附效果最优,最大吸附量达到45.33 mg/g。热力学及动力学分析表明,准二级动力学模型和Langmuir吸附等温模型能较好拟合污泥生物炭吸附四环素的过程,吸附过程主要为单分子层吸附,且以表面化学吸附为主,结合表征测试结果分析,化学吸附主要涉及静电吸引、阳离子交换、络合沉淀、π—π共轭作用及氢键作用等过程;同时,污泥生物炭的孔结构特性使其对四环素的吸附过程还包含孔隙填充及范德华力作用。

污泥  /  污泥生物炭  /  四环素  /  吸附  /  资源化利用

The transformation of sludge into biochar adsorbents for the removal of tetracycline contaminants in water bodies represents one of the effective approaches for the resource utilization of sludge and enables the realization of the circular economy concept of “treating waste with waste”. Municipal sludge was employed as the raw material, and sludge biochar was fabricated through pyrolysis for the adsorption and removal of tetracycline. The adsorption and removal efficacy of tetracycline was investigated, and the preparation conditions of sludge biochar and adsorption environmental conditions were optimized. Additionally, by combining methods such as scanning electron microscopy, infrared spectroscopy, and BET(Brunauer,Emmett,Teller) specific surface area testing, the structural characteristics of sludge biochar and the underlying mechanism of its adsorption behavior towards tetracycline were explored. The results indicate that the sludge biochar prepared under a pyrolysis temperature of 800 ℃ and a pyrolysis duration of 4 hours exhibits the optimal adsorption performance for tetracycline. The pH value exerts a significant influence on the adsorption effect. In a weakly acidic environment, the adsorption effect of sludge biochar on tetracycline is the most favorable, with a maximum adsorption capacity reaching 45.33 mg/g. Thermodynamic and kinetic analyses demonstrate that the pseudo-second-order kinetic model and the Langmuir adsorption isotherm model can appropriately fit the adsorption process of tetracycline by sludge biochar. The adsorption process is primarily monolayer adsorption, dominated by surface chemical adsorption. In conjunction with the analysis of characterization test results, the chemical adsorption mainly involves processes such as electrostatic attraction, cation exchange, complex precipitation, π-π conjugation, and hydrogen bonding. Simultaneously, the pore structure characteristics of sludge biochar result in the adsorption process of tetracycline also encompassing pore filling and Van der Waals force.

sludge  /  sludge biochar  /  tetracycline  /  adsorption  /  resource utilization
刘炜, 孟多, 褚书平, 李响. 污泥生物炭对四环素吸附性能的优化及吸附机理. 科学技术与工程, 2025 , 25 (11) : 4801 -4808 . DOI: 10.12404/j.issn.1671-1815.2403980
Wei LIU, Duo MENG, Shu-ping CHU, Xiang LI. Optimization of Tetracycline Adsorption Performance by Sludge Biochar and Adsorption Mechanism Research[J]. Science Technology and Engineering, 2025 , 25 (11) : 4801 -4808 . DOI: 10.12404/j.issn.1671-1815.2403980
正文
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污泥是污水处理的副产品,其来源和成分十分复杂,包括动植物残体、微生物以及有机物[1],同时含有一定量的病原体、寄生虫和重金属[2]等,如果随意排放污泥,很可能会二次污染环境。目前,中国有超过2 600 座污水处理厂投入运行,辽宁省锦州市10 余座污水厂每天产生含水率超80%的污泥70 t以上,如此庞大的污泥产量为城市污水处理带来不可避免的固体废弃物处理处置问题。目前常用的污泥处理处置方法可能存在资源浪费和环境二次污染等问题,因此国内外已经开始探索污泥资源化利用的新模式,例如,将污泥制成有机肥、燃料、吸附剂等,不仅能够有效解决污泥的排放问题,还能够产生一定的经济效益和社会效益。
利用热解法将污泥制成污泥生物炭(sludge biochar,SBC)是对污泥进行无公害化处理,实现污泥资源化利用的有效途径之一。热解是一种通过加热生物质在无氧或限氧条件下分解产生生物炭、生物油和气态产物的技术。不同的热解方式会产生不同的产物,这取决于操作条件如加热温度、速率和停留时间。以污泥为原料进行热解制备生物炭可以解决生物炭制备中原料成本过高的问题,并且高温热解后重金属会以更稳定的形式存在于生物炭中,降低了污泥对环境可能造成污染的风险,是一种污泥资源化利用的新型处理方法。
四环素(tetracycline,TC)是一种广谱抗生素,水溶性强,具有一定致突变性和致畸性,生物降解性差[3],如果四环素废水无节制排放到环境中,不仅会破坏生态平衡,也会增加细菌的耐药性。因此,加强对四环素废水的处理和提高其排放标准显得尤为重要。吸附法因操作简单,吸附剂制备简单、成本低等优点被广泛用于吸附去除水体中的TC。近年来,使用污泥制备SBC用于吸附水体中的抗生素、有机物、重金属、染料等新兴污染物在被不断尝试。余江芳等[4]等通过3 种不同温度来制备污泥生物炭,结果表明随着热解温度的升高,SBC的比表面积和孔容均有所增大,吸附TC的能力也显著增强;何丽文泽等[5]在热解温度400 ℃、热解4 h的条件下制备SBC,对TC的吸附量为58 mg/g。Zhao等[6]研究Fe3O4-污泥生物炭高效去除水中的四环素,当生物炭用量为1.5 g/L、pH=7、TC初始浓度为30 mg/L、吸附时间为8 h时,生物炭对TC的去除率达到98%。目前,采用污泥制备生物炭去除抗生素类污染物的研究较多,但对于SBC吸附某一特定污染物的优化制备条件及吸附机制的研究还相对欠缺,特别是基于面向工业化的简单SBC制备工艺及吸附能力提升方面的研究还需进一步补充完善,且SBC对不同类型污染物的吸附应用具有较大潜力和发展空间,对其吸附能力和吸附机理进行深入研究具有必要性及实际价值。
本研究采用热解法制备污泥生物炭,考察不同热解温度和热解时间对SBC吸附TC的影响,以确定具有最优TC吸附能力的污泥生物炭制备工艺条件,并探讨SBC对TC吸附过程中,TC初始浓度、SBC投加量、溶液pH、吸附时间等条件对SBC吸附性能的影响作用规律,结合SBC性能表征手段,探究SBC对TC的吸附机制,以期实现对废水中TC的高效去除,为污泥资源化利用及水体净化技术提供实践依据与技术支持。
1 实验
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1.1 实验材料与仪器
实验污泥取自辽宁省锦州市女儿河污水处理厂,含水率99.5%。四环素,分析纯,上海阿拉丁生化科技股份有限公司;氢氧化钠、盐酸,化学纯,天津市鑫铂特化工有限公司;去离子水为实验室自制。
实验仪器:电子天平(FA1004B,上海佑科仪表有限公司),恒温震荡箱(HZQ-F160A,上海一恒科学仪器有限公司),鼓风干燥箱(LG-50,上海跃进医疗器械厂),循环水式多用真空泵(SHZ-D(Ⅲ),河南省予华仪器有限公司),智能箱式高温炉(DC-B40/15,北京独创科技有限公司),粉碎机(2500Y,北京独创科技有限公司),紫外可见分光光度计(TU-1810,北京普析通用仪器有限责任公司)。
1.2 污泥生物炭的制备
将污泥静置24 h进行沉淀,去除上清液后,采用真空泵对沉淀污泥进行抽滤以脱除多余水分,然后放入80 °C干燥箱中干燥24 h至水分蒸发完全,冷却至室温后用研磨机粉碎,过100 目筛得到污泥粉末。将适量污泥粉末放入50 mL的坩埚中,用双层锡纸包裹坩埚以增强气密性,置于马弗炉中,升温速率10 ℃/min进行热解。热解结束后冷却至室温,取出坩埚内热解得到的污泥生物炭,放入去离子水中浸泡24 h,经烘干、冷却、研磨后得到最终产品SBC。
采用上述方法选取不同的热解温度和热解时间作为热解条件,制备得到如表1所示的12 种污泥生物炭,考察不同热解条件对SBC性能和吸附能力的影响。
1.3 四环素吸附实验
依次称取12 种SBC各0.06 g,分别加入到50 mL离心管中,然后加入40 mL TC浓度为20 mg/L的溶液,调节初始pH=7。将离心管置于25 ℃恒温振荡器中,以150 r/min的振动速率反应24 h至吸附平衡。吸附后用0.45 μm水系膜过滤,利用紫外可见分光光度计检测水样中剩余TC的吸光度,并计算TC剩余浓度。计算平衡吸附量qe和去除率R,所有批量实验均进行3次平行实验,取平均值。计算公式为
q e = ( C 0 - C e ) V M
q t = ( C 0 - C t ) V M
R = C 0 - C e C 0 × 100 %
式中:C0为TC的初始浓度,mg/L;Ce为TC的平衡浓度,mg/L;Ct为接触时间t的TC浓度,mg/L;qe为吸附平衡后生物炭对TC的吸附量,mg/g;qt为接触时间为t时生物炭吸附TC的吸附量,mg/g;M为生物炭的质量,g;V为溶液体积,L;R为去除率,%。
1.4 性能表征
采用扫描电子显微镜(scanning electron microscope,SEM,德国蔡司公司Sigma 500)测试分析SBC的表观形貌;采用傅里叶变换红外吸收光谱仪(Fourier transform infrared spectroscopy,FTIR,美国赛默飞公司Nicolet 6700)分析检测原污泥和SBC所含表面官能团的类型,并利用比表面积孔隙度分析仪(Brunner-Emmet-Teller,BET,美国康塔公司AUTOSORB IQ2)测定SBC样品的比表面积、总孔容和平均孔径。
1.5 吸附等温线实验
在设定的实验参数条件下,分别配置TC初始浓度为10~100 mg/L的TC溶液,并加入0.06 g SBC进行对四环素的吸附实验。根据式(4)、式(5)利用Langmuir和Freundlich吸附等温线模型,在不同初始吸附质浓度下,对SBC吸附TC的结果进行拟合分析。
Langmuir吸附等温线模型:
1 q e = 1 q m + 1 q m K L C e
Freundlich吸附等温线模型:
l n q e = l n K F + 1 n l n C e
式中:KL和KF分别为Langmuir模型和Freundlich模型的模型常数,L/mg、mg/g;qm为生物炭对TC吸附量的最大值,mg/g;Ce为吸附平衡后的平衡浓度,mg/L;1/n为吸附过程的异质性因子。
1.6 吸附动力学实验
称取0.3 g SBC加入200 mL浓度为100 mg/L的TC溶液;然后,在25 ℃和150 r/min下进行吸附实验。分别在2、4、6、8、10、12、24、36 h对样品进行测定。根据式(6)、式(7)对实验数据进行准一级和准二级动力学模型拟合,并分析结果。
准一级动力学模型:
l n ( q e - q t ) = l n q e - k 1 t
准二级动力学模型:
t q t = 1 k 2 q e 2 + t q e
式中:qe为吸附平衡后生物炭对TC的吸附量,mg/g;qt接触时间t时生物炭对TC的吸附量,mg/g;k1和k2分别为准一级和准二级动力学模 型 的 速 率 常 数, h - 1、g/(mg·h);t为吸附时间,h。
2 结果与讨论
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2.1 SBC最佳制备条件的确定
不同热解温度和热解时间条件下所制备的SBC对TC的吸附效果如图1 所示。由图1可知, SBC对TC的去除率随着热解温度的增加而增加;热解时间t对TC去除率R的影响与热解温度呈现一定的相关性,当热解温度为500 ℃时,热解时间的增加并不影响SBC对TC的吸附能力;当热解温度为600 ~700 ℃时,TC的吸附去除率随着热解时间的增加而下降,且去除率均低于70%,去除效果不理想。当热解温度升高至 800 ℃且热解时间增加至 4 h 时, SBC对TC的去除率陡升至 90%,达最大吸附去除率,表现出极高的 TC 吸附去除能力。这表明在热解温度为 800 ℃、热解时间为 4 h 时,SBC 对 TC 具有最强吸附性能。经3次重复实验,SBC 对 TC 呈现最佳吸附效果的制备条件均为热解温度 800 ℃、热解时间 4 h。鉴于此,确定该条件作为污泥生物炭的最佳制备条件,将此生物炭记作 SBC 800 ℃ , 4 h。
2.2 SBC吸附TC的影响因素
2.2.1 SBC投加量的影响
在pH为7,TC浓度20 mg/L,溶液体积40 mL,反应温度25 ℃,吸附24 h的条件下, SBC 800 ℃ , 4 h投加量对TC吸附影响如图2 所示。图2 表明,随着 SBC 800 ℃ , 4 h投加量的增加,为吸附TC提供了更多的活性位点[7],TC的去除率由53%提高到95%。由于污染物的总浓度相同,生物炭的增加会降低吸附活性点的驱动力,从而使得吸附量呈下降趋势,TC的吸附量从28 mg/g下降到10 mg/g,因此,综合考虑到吸附速率和经济效益的影响,选取0.06 g投加量。
2.2.2 初始pH的影响
溶液pH对吸附剂和吸附质的表面电荷会产生一定影响,从而使两者之间存在静电引力作用。TC有3个电离平衡常数(pKa=3.3、7.7、9.7),TC的主要离子种类:pH<3.3时的TC+,3.3<pH<7.7时的TC±,7.7<pH<9.7时的TC-,pH>9.7时的TC2- [8]。
在TC浓度20 mg/L、体积40 mL,反应温度25 ℃,吸附时间24 h, SBC 800 ℃ , 4 h投加量0.06 g时,SBC对TC的去除率达90%以上,此条件下不易观察初始pH对实验的影响;因此配置TC浓度100 mg/L,其他条件不变探究初始pH与TC吸附去除率的关系,吸附曲线如图3所示。由图3可见,溶液初始pH为5时, SBC 800 ℃ , 4 h对TC的吸附去除效果最佳,去除率为64.14%,这是由于此条件下的SBC表面带少量正电荷,TC的优势种为TC±,产生的静电吸引或排斥作用均较弱。当溶液pH由3增加5时,TC的正电性逐渐减弱,与吸附剂的静电斥力逐渐减小,吸附量产生增加。当pH>7时, SBC 800 ℃ , 4 h表面带负电荷,以TC-产生静电排斥,从而大大降低了TC的去除率。在酸性条件下, SBC 800 ℃ , 4 h表面吸附H+使其带有正电荷,TC此时又以阳离子形式存在,两者之间存在静电斥力,但在此次研究中,酸性条件下的TC去除率比中性和碱性条件下都高,说明此时可能存在配位络合或离子交换等其他作用力影响吸附过程[8]。同时,当溶液呈弱酸性时,生物炭中的金属离子被溶解,金属阳离子与TC发生配位反应,TC聚合后发生吸附或沉淀去除;且以阳离子形式存在的TC还可能与生物炭的表面配位位点结合,发生阳离子交换反应[9]。综上所述,弱酸条件下 SBC 800 ℃ , 4 h对TC的吸附能力更强,因此反应环境pH确定为5。
2.2.3 吸附时间的影响
在溶液pH=5,反应温度25 ℃的条件下,称取0.3 g SBC 800 ℃ , 4 h加入到200 mL浓度为100 mg/L的TC溶液中,考察吸附时间对TC吸附去除效果的影响,结果如图4所示。由图4可见,当反应时间小于12 h时, SBC 800 ℃ , 4 h对TC的吸附去除率随着反应时间的增加而迅速增加,表明此时吸附剂中存在大量未被占据的吸附点位,吸附速率增长较快。当吸附时间达到至12~24 h时,TC的吸附去除率的继续增加,但吸附速率逐渐变小,24 h后SBC的吸附容量基本饱和,TC去除率趋于稳定,36 h的吸附去除率与24 h几乎相等,说明反应时间为24 h时SBC对TC的吸附已达到吸附平衡,因此选取24 h作为最优的吸附时间。
2.2.4 TC浓度的影响
吸附质浓度是影响吸附速率的显著因素之一,在 SBC 800 ℃ , 4 h投加量为0.06 g,溶液pH=5,反应温度25 ℃,吸附时间24 h条件下,探究吸附质初始浓度对去除TC影响作用规律如图5所示。由图5可见,随着四环素浓度的升高,SBC对TC的去除率逐渐下降,去除率从94.6%下降到64.14%;吸附量逐渐上升,从15 mg/g上升到45.33 mg/g。根据图能够看出当TC初始浓度为100 mg/L时,SBC对TC的吸附量最大,且日常中TC废水浓度较浓,较符合实际情况;选取高浓度条件下进行实验也可对以后实际应用提供一定的帮助,因此选取TC浓度为100 mg/L作为实验中TC的初始浓度。
2.3 吸附热力学及动力学分析
2.3.1 吸附等温线
利用Langmuir和Freundlich吸附等温线模型对不同初始吸附质浓度下,SBC对TC吸附结果进行拟合分析,结果如图6所示。由图6可见,Langmuir等温吸附模型能够更加准确地描述 SBC 800 ℃ , 4 h对水中TC的吸附过程,拟合方程的R2=0.997 0(Freundlich模型中R2=0.881 6),相关性较高。由Langmuir等温吸附模型的基本理论可知, SBC 800 ℃ , 4 h的表面活性位点是均匀分布的,被吸附的分子之间没有相互作用力,且在单分子层的条件下达到平衡,吸附为均匀的单层吸附[10]。在当前实验条件下,Langmuir模型预测 SBC 800 ℃ , 4 h对TC的理论最大吸附量为48.01 mg/g,与实验得出的最大吸附量(45.33 mg/g)相接近,进一步证明 SBC 800 ℃ , 4 h对TC的吸附过程符合Langmuir模型。
2.3.2 吸附动力学
为探究SBC对TC的去除率随吸附时间变化而产生的影响,利用准一级和准二级动力学模型对吸附时间的影响数据进行拟合分析,拟合结果如图7所示。由图7可知,在此条件下SBC对TC的吸附过程可以通过准二级动力学模型精准表达(准二级R2=0.992 9>准一级R2=0.983 9),且准二级动力学模型得出的SBC对TC的理论平衡吸附量qe为53.62 mg/g,与实验最大吸附量(45.33 mg/g)更接近。由准二级动力学分析可知,TC在SBC上的吸附过程以化学吸附和表面控制为主[11],这意味着在吸附过程中,TC分子先与SBC表面形成一个单分子层,然后逐渐扩散到SBC孔隙中,这种吸附过程相对较慢,需要一定的时间完成最终吸附。
2.4 吸附机理探究
2.4.1 红外光谱分析
图8为原污泥与 SBC 800 ℃ , 4 h的红外吸收光谱。由原污泥的吸收光谱可见,3 427 cm-1处存在一宽而强的吸收峰,由—OH基的伸缩振动引起;2 925 cm-1和1 460 cm-1处的吸收峰为污泥脂类物质中烷基的伸缩振动吸收峰和不对称剪式振动吸收峰;波数1 640 cm-1附近为酰胺中C=O基团的伸缩振动吸收峰,1 037 cm-1为污泥中多糖类物质的芳香环中C—O的伸缩振动峰;461 cm-1处的吸收峰则归属于Si—O键的对称伸缩振动峰。在 SBC 800 ℃ , 4 h的红外光谱中,部分吸收峰出现变化,其中3 427 cm-1处—OH的吸收峰强度有所降低,表明热解过程产生脱水反应,且由于在热解过程中不稳定脂肪族化合物的持续减少以及去甲基化,波数2 925 cm-1和1 460 cm-1处的烷基吸收峰几近消失。1 640 cm-1处吸收峰强度显著减弱,说明800 ℃的热解温度使C=O键变少,而1 037 cm-1处吸收峰强度有所增强,可见芳香环中含氧官能团的数量有所增加,同时Si—O的振动吸收峰也明显增强,说明生物炭中Si的质量分数有所增加。根据Zhang等[12]、Ma等[13]的研究,SBC中2 925 cm-1处的脂肪族C—H键在吸附TC后消失,可能是由于生物炭的C—H基团与TC分子表面的酚羟基之间形成了氢键;生物炭的—OH、C=O与TC的含氟、含氮、含氧基团之间形成氢键,生物炭上的—OH因其对炔单元的π—电子供体能力而充当π—电子供体,而TC的苯环因存在强吸电子的氟和N—杂芳香环而被视为π—电子受体,π—π共轭作用参与了生物炭的—OH和TC的苯环之间的相互作用,这证实了SBC吸附TC的吸附过程含有氢键和π—π键共轭作用。由红外光谱分析可知,经高温热解后,大部分脂类化合物都产生分解,部分含氧官能团如C=O、C—O的含量有所保留或增加,这有利于TC所包含的质子化基团与 SBC 800 ℃ , 4 h的含氧官能团通过氢键、静电引力等作用实现对TC的吸附去除,同时 SBC 800 ℃ , 4 h中的芳香环结构可以与TC分子的芳香环结构形成较稳定的π—π键,达到去除TC的目的。
2.4.2 扫描电镜分析
图9所示为污泥原料、 SBC 800 ℃ , 4 h的表观形貌图,经对比可见,污泥经过高温煅烧成生物炭后,污泥表面的颗粒块状物经过高温热解后形成了较丰富的片状结构,其表面变得凹凸不平,颗粒表面粗糙度增大,使 SBC 800 ℃ , 4 h具有更大的比表面积,因而吸附位点和活性位点数量增多。由图9(b)可见,污泥生物炭表面形成很多片状结构和部分孔隙结构,这是由于污泥中的部分有机物通过受热分解,使块状物变成一些立体片状结构,增大了污泥生物炭的比表面积;有机物的分解,使结构更加松散,呈现一定的孔隙结构,使其孔隙度更加丰富。比表面积的增加和孔隙结构的产生,是SBC拥有较强吸附能力的关键因素之一。
2.4.3 孔结构分析
SBC的孔隙结构为SBC优越的吸附性能提供前提和基础,采用BET技术对 SBC 800 ℃ , 4 h的孔结构特性进行表征,得到 SBC 800 ℃ , 4 h的比表面积为107.70 m2/g,孔容0.1 845 cm3/g,其孔径分布如图10所示。由图9可见,该SBC的孔径分布主要集中在2~8 nm,平均孔径6.065 nm,属于介孔结构,一般介孔用于运输污染物分子,微孔用于吸附分子,微孔结构和高比表面积有利于离子交换和扩散。
由于TC分子的尺寸约为1.27 nm,远远小于吸附剂 SBC 800 ℃ , 4 h的平均孔径,能够轻易扩散到孔隙所形成的通道和空间中,因此推测孔隙填充可能是TC被吸附到 SBC 800 ℃ , 4 h上的机制之一[14]。
2.4.4 吸附机理分析
从SBC的物理结构、性能表征分析,污泥生物炭具有较大的比表面积和较丰富的介孔结构,其表面拥有较多的吸附位点和活性位点以及含有丰富的官能团,其较强的物理化学性能为其吸附四环素提供了强有力的保障。SBC的丰富孔隙结构可实现孔隙填充作用,其表面与TC分子间存在范德华力作用。其次,SBC表面拥有丰富的含氧官能团,能使TC分子通过氧化、吸附等方式作用到生物炭上,且SBC中所含物质的芳香环结构可以与TC分子的芳香环结构发生共轭反应,基于电子云的相互吸引,使得TC分子能够稳定地吸附在SBC的芳香环结构上;同时,SBC表面的羟基可以与TC分子中的羟基、氨基等形成氢键,实现对TC的吸附去除。由实验结果可知,在弱酸性条件下,SBC对TC的吸附能力最强,此时,SBC与TC分子产生不同电性由此产生静电相互吸引。在弱酸环境中,SBC中的金属阳离子会溶解在溶液中,TC分子在溶液中与金属阳离子发生阳离子交换反应和络合沉淀作用,从而被吸附到SBC上。因此,SBC对TC的吸附行为既包含孔隙填充、范德华力作用等,也包含氢键作用、π—π共轭作用、静电引力、离子交换以及络合沉淀作用等化学吸附过程。由吸附热力学、动力学分析及表征测试结果可知,SBC对TC的吸附过程主要以化学吸附为主。
3 结论
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(1)采用热解法将污水处理厂污泥转化为高效吸附剂—污泥生物炭,用于去除水中的TC污染物,通过批量实验确定对TC具有最佳吸附能力的SBC制备条件为热解温度800 ℃,热解时间4 h。
(2)在弱酸性水质环境中,SBC对TC的吸附效率达到峰值,最大吸附容量可达45.33 mg/g。 其吸附过程符合Langmuir吸附等温模型和准二级动力学模型,表明 SBC对TC的吸附过程为均匀的单分子层吸附,TC分子扩散到SBC孔隙中的速率较缓慢,需要一定的时间完成最终吸附。
(3)由SBC对TC的吸附实验结果与SBC表征结果综合分析得出:SBC对TC的吸附过程主要以化学吸附为主,氢键、π—π键、阳离子交换和络合沉淀作用为SBC吸附TC提供主要助力;同时由于SBC丰富的孔隙结构以及较大的比表面积,对TC的吸附过程中含有孔隙填充和范德华力作用。
基金
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  • 辽宁省自然科学基金面上项目(2022-MS-380)
  • 辽宁省教育厅科研基金面上项目(JYTMS20230864)
文献
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2025年第25卷第11期
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doi: 10.12404/j.issn.1671-1815.2403980
  • 接收时间：2024-05-29
  • 首发时间：2025-07-09
  • 出版时间：2025-04-18
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  • 收稿日期：2024-05-29
  • 修回日期：2024-09-25
基金
辽宁省自然科学基金面上项目(2022-MS-380)
辽宁省教育厅科研基金面上项目(JYTMS20230864)
作者信息
    1 辽宁工业大学土木建筑工程学院, 锦州 121000
    2 辽宁城建设计院有限公司沈阳分公司, 沈阳 110015

通讯作者:

* 孟多(1981—),女,汉族,辽宁阜新人,教授,博士。研究方向:固体废弃物综合利用技术。E-mail:。
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https://castjournals.cast.org.cn/joweb/kxjsygc/CN/10.12404/j.issn.1671-1815.2403980
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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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