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Article(id=1322594856816460040, tenantId=1146029695717560320, journalId=1225396423026438145, issueId=1322594813749350688, 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=1714060800000, receivedDateStr=2024-04-26, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1793260786489, onlineDateStr=2026-10-29, pubDate=1740412800000, pubDateStr=2025-02-25, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1793260786489, onlineIssueDateStr=2026-10-29, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1793260786489, creator=13701087609, updateTime=1793260786489, updator=13701087609, issue=Issue{id=1322594813749350688, tenantId=1146029695717560320, journalId=1225396423026438145, year='2025', volume='45', issue='2', pageStart='1', pageEnd='288', issueExtLink='null', onlineDate='null', pubDate='1740412800000', pubDateStr='2025-02-25', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1793260776220, creator='13701087609', updateTime=1793260776220, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext=null, issueFiles=null, downloadFileDto=null}, startPage=279, endPage=288, ext={EN=ArticleExt(id=1322594858666148105, articleId=1322594856816460040, tenantId=1146029695717560320, journalId=1225396423026438145, language=EN, title=Study on the Adsorption Properties of Lead Ions in Coal Gangue Modified by Amino and Sulfhydryl Bifunctional Groups, columnId=null, journalTitle=Mining Research and Development, columnName=null, runingTitle=null, highlight=null, articleAbstract=

The solid waste coal gangue produced in the process of coal mining and washing and the discharge of Pb(Ⅱ) from industrial wastewater will bring great harm to the ecosystem and human health, and it is of great significance to study the efficient removal method of Pb(Ⅱ) and the rational utilization of coal gangue for ecological and environmental protection. A low-cost aminothiol difunctional modified coal gangue (CG-SHNH) composite material was prepared by grafting 3-mercaptopropyl trimethoxysilane (MPTMS) and 3-aminopropyl triethoxysilane (APTES) with coal gangue. The physical and chemical properties of the adsorbed materials were investigated by means of XRD, XRD-EDS, XFR, FTIR, SEM, Zeta potential, and so on. And it is found that new bands appeare at 2 930 cm−1 and 2 560 cm−1, corresponding to C—H and S—H tensile vibrations, respectively, and a new peak appeares at 3 367 cm−1, which is the absorption peak of N—H bonds, indicating that the surface of CG-SHNH is rich in amino and sulfhydryl functional groups. The results of N2 adsorption-desorption analysis indicate that the average pore size of CG-SHNH increases significantly, from 17.33 nm to 24.54 nm. The study on the adsorption performance of CG-SHNH for Pb(Ⅱ) shows that the optimal adsorption capacity of CG-SHNH for Pb(Ⅱ) is 125 mg/g when the addition amount of CG-SHNH is 1 g/L, the contact time is 20 h, the temperature is 25 ℃, the pH is 6.6, and the initial concentration of Pb(Ⅱ) is 600 mg/L. The adsorption mechanism shows that CG-SHNH amino and sulfhydryl bifunctional groups can synergistically promote the chelation adsorption of Pb(Ⅱ), exhibiting excellent heavy metal ion adsorption ability.

, authors=Rui LEII, Xianshu DONGI, Yuping FANI, Xiaomin MAI, authorsList=Rui LEI, Xianshu DONG, Yuping FAN, Xiaomin MA, authorCompany=null, correspAuthors=Xianshu DONG, 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, fund=null), CN=ArticleExt(id=1322594867893616938, articleId=1322594856816460040, tenantId=1146029695717560320, journalId=1225396423026438145, language=CN, title=氨基和巯基双官能团修饰煤矸石对铅离子的吸附性能研究, columnId=1226462297560892399, journalTitle=矿业研究与开发, columnName=选矿与资源综合利用, runingTitle=null, highlight=null, articleAbstract=

煤炭开采和洗选过程中产生的固体废物煤矸石以及工业废水排放的Pb(Ⅱ)给生态系统和人类健康带来了巨大危害，研究Pb(Ⅱ)的高效去除方法和煤矸石的合理利用对生态环境保护具有重要意义。提出以煤矸石接枝3-巯基丙基三甲氧基硅烷(MPTMS)和3-氨基丙基三乙氧基硅烷(APTES)制备一种低成本氨基巯基双官能团改性煤矸石(CG-SHNH)复合材料。通过XRD、XRD-EDS、XFR、FTIR、SEM、Zeta电位等手段对吸附材料的物理和化学特性进行全面分析，发现复合材料在2 930 cm−1和2 560 cm−1处出现新的谱带，分别对应C—H和S—H拉伸振动，在3 367 cm−1处出现了新的峰，为N—H键的吸收峰，说明CG-SHNH表面分布有丰富的氨基和巯基官能团。N2吸附脱附分析结果表明，CG-SHNH平均孔径明显增加，从17.33 nm增加到24.54 nm。CG-SHNH对Pb(Ⅱ)的吸附性能研究结果表明，在CG-SHNH添加量为1 g/L、接触时间为20 h、温度为25 ℃，pH为6.6,Pb(Ⅱ)溶液初始浓度为600 mg/L时，CG-SHNH对Pb(Ⅱ)的吸附效果最佳，吸附容量为125 mg/g。吸附机理研究表明，CG-SHNH氨基和巯基双官能团对Pb(Ⅱ)螯合吸附能够协同促进，展现出优异的重金属离子吸附能力。

, authors=雷锐I, 董宪姝I, 樊玉萍I, 马晓敏I, authorsList=雷锐, 董宪姝, 樊玉萍, 马晓敏, authorCompany=null, correspAuthors=董宪姝, authorNote=

雷锐（1995—），女，山西闻喜人，硕士研究生，主要从事煤炭固废煤矸石综合利用方面的研究。E-mail:

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董宪姝（1964—），女，辽宁葫芦岛人，教授，博士生导师，主要从事煤炭洗选加工与综合利用研究。E-mail:
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雷锐（1995—），女，山西闻喜人，硕士研究生，主要从事煤炭固废煤矸石综合利用方面的研究。E-mail:

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雷锐（1995—），女，山西闻喜人，硕士研究生，主要从事煤炭固废煤矸石综合利用方面的研究。E-mail:

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Journal of Hazardous Materials, 2013 (252/253):428-461., articleTitle=A review on zinc and nickel adsorption on natural and modified zeolite, bentonite and vermiculite: Examination of process parameters, kinetics and isotherms, refAbstract=null), Reference(id=1322594896993698201, tenantId=1146029695717560320, journalId=1225396423026438145, articleId=1322594856816460040, doi=null, pmid=null, pmcid=null, year=2023, volume=17, issue=3, pageStart=761, pageEnd=773, url=null, language=null, rfNumber=[22], rfOrder=34, authorNames=熊茹婷, 张志恒, 林海英, journalName=环境工程学报, refType=null, unstructuredReference=熊茹婷，张志恒，林海英，等.巯基改性壳聚糖复合材料的制备及其用于高容量去除水中Hg(Ⅱ)[J].环境工程学报，2023，17(3):761-773., articleTitle=巯基改性壳聚糖复合材料的制备及其用于高容量去除水中Hg(Ⅱ), refAbstract=null), Reference(id=1322594897081778586, tenantId=1146029695717560320, journalId=1225396423026438145, articleId=1322594856816460040, doi=null, pmid=null, pmcid=null, year=2023, volume=17, issue=3, pageStart=761, pageEnd=773, url=null, language=null, rfNumber=[22], rfOrder=35, authorNames=XIONG Ruting, ZHANG Zhiheng, LIN Haiying, journalName=Chinese Journal of Environmental Engineering, refType=null, unstructuredReference=XIONG Ruting, ZHANG Zhiheng, LIN Haiying, et al. 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Chinese Journal of Environmental Engineering, 2023, 17(3):761-773., articleTitle=A facile synthesis of thiol-modified chitosan composite for high-capacity capture of mercury from aqueous solution, refAbstract=null)], funds=null, companyList=[AuthorCompany(id=1322594869550367020, tenantId=1146029695717560320, journalId=1225396423026438145, articleId=1322594856816460040, xref=null, ext=[AuthorCompanyExt(id=1322594869562949933, tenantId=1146029695717560320, journalId=1225396423026438145, articleId=1322594856816460040, companyId=1322594869550367020, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=School of Mining Engineering, Taiyuan University of Technology, Taiyuan, Shanxi 030024, China), AuthorCompanyExt(id=1322594869579727150, tenantId=1146029695717560320, journalId=1225396423026438145, articleId=1322594856816460040, companyId=1322594869550367020, language=CN, country=null, province=null, city=null, postcode=null, 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articleId=1322594856816460040, language=CN, label=图13, caption=氨基以及巯基修饰后的煤矸石对Pb(Ⅱ)的吸附机制, figureFileSmall=GEGsd61JmgyDigALxc05GQ==, figureFileBig=Z2euxXKPaQq91kurAYPLbw==, tableContent=null), ArticleFig(id=1322594887959167336, tenantId=1146029695717560320, journalId=1225396423026438145, articleId=1322594856816460040, language=EN, label=Table 1, caption=

XRF analysis of coal gangue and two modified coal gangues

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材料类别Al2O3SiO2SO3K2OFe2O3
CG50.4942.095.220.1720.545
CG-SH44.9739.0013.030.1420.450
CG-SHNH43.4835.6914.830.1120.413
), ArticleFig(id=1322594888064024937, tenantId=1146029695717560320, journalId=1225396423026438145, articleId=1322594856816460040, language=CN, label=表1, caption=

煤矸石及两种改性煤矸石的 XRF 分析

, figureFileSmall=null, figureFileBig=null, tableContent=
材料类别Al2O3SiO2SO3K2OFe2O3
CG50.4942.095.220.1720.545
CG-SH44.9739.0013.030.1420.450
CG-SHNH43.4835.6914.830.1120.413
), ArticleFig(id=1322594888386986346, tenantId=1146029695717560320, journalId=1225396423026438145, articleId=1322594856816460040, language=EN, label=Table 2, caption=

Pore structure analysis results of CG, CG-SH, CG-SHNH

, figureFileSmall=null, figureFileBig=null, tableContent=
吸附剂类型比表面积/(m2/g)总孔容积/(cm2/g)平均孔径/nm
CG17.970.077917.33
CG-SH8.700.062028.33
CG-SHNH5.780.035024.54
), ArticleFig(id=1322594890014376299, tenantId=1146029695717560320, journalId=1225396423026438145, articleId=1322594856816460040, language=CN, label=表2, caption=

CG、CG-SH、CG-SHNH 的孔隙结构分析结果

, figureFileSmall=null, figureFileBig=null, tableContent=
吸附剂类型比表面积/(m2/g)总孔容积/(cm2/g)平均孔径/nm
CG17.970.077917.33
CG-SH8.700.062028.33
CG-SHNH5.780.035024.54
), ArticleFig(id=1322594890081485164, tenantId=1146029695717560320, journalId=1225396423026438145, articleId=1322594856816460040, language=EN, label=Table 3, caption=

Fitting parameters of Langmuir model and Freundlich model

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模型qm/(mg/g)KL/(L/mg)R2
Langmuir125.790.0840.997
模型qe(mg/g)K2R2
Freundlich74.73112.330.948
), ArticleFig(id=1322594890144399725, tenantId=1146029695717560320, journalId=1225396423026438145, articleId=1322594856816460040, language=CN, label=表3, caption=

Langmuir 与 Freundlich 模型拟合参数

, figureFileSmall=null, figureFileBig=null, tableContent=
模型qm/(mg/g)KL/(L/mg)R2
Langmuir125.790.0840.997
模型qe(mg/g)K2R2
Freundlich74.73112.330.948
), ArticleFig(id=1322594890219897198, tenantId=1146029695717560320, journalId=1225396423026438145, articleId=1322594856816460040, language=EN, label=Table 4, caption=

Fitting parameters for quasi-first-order kinetics and quasi-second-order kinetics

, figureFileSmall=null, figureFileBig=null, tableContent=
动力学qe/(mg/g)K1R2
准一级83.870.001 170.895
动力学qe/(mg/g)K2R2
准二级111.110.000 20.999
), ArticleFig(id=1322594890295394671, tenantId=1146029695717560320, journalId=1225396423026438145, articleId=1322594856816460040, language=CN, label=表4, caption=

准一级动力学、准二级动力学拟合参数

, figureFileSmall=null, figureFileBig=null, tableContent=
动力学qe/(mg/g)K1R2
准一级83.870.001 170.895
动力学qe/(mg/g)K2R2
准二级111.110.000 20.999
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氨基和巯基双官能团修饰煤矸石对铅离子的吸附性能研究
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雷锐 I , 董宪姝 I , 樊玉萍 I , 马晓敏 I
矿业研究与开发 | 选矿与资源综合利用 2025,45(2): 279-288
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矿业研究与开发 |选矿与资源综合利用 2025 , 45 (2) : 279 -288
氨基和巯基双官能团修饰煤矸石对铅离子的吸附性能研究
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雷锐I , 董宪姝I , 樊玉萍I, 马晓敏I
作者信息
  • 太原理工大学 矿业工程学院，山西　太原　030024
通讯作者:
董宪姝（1964—），女，辽宁葫芦岛人，教授，博士生导师，主要从事煤炭洗选加工与综合利用研究。E-mail:
作者简介:

雷锐（1995—），女，山西闻喜人，硕士研究生，主要从事煤炭固废煤矸石综合利用方面的研究。E-mail:

Study on the Adsorption Properties of Lead Ions in Coal Gangue Modified by Amino and Sulfhydryl Bifunctional Groups
Rui LEII , Xianshu DONGI , Yuping FANI, Xiaomin MAI
Affiliations
  • School of Mining Engineering, Taiyuan University of Technology, Taiyuan, Shanxi 030024, China
出版时间: 2025-02-25
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煤炭开采和洗选过程中产生的固体废物煤矸石以及工业废水排放的Pb(Ⅱ)给生态系统和人类健康带来了巨大危害，研究Pb(Ⅱ)的高效去除方法和煤矸石的合理利用对生态环境保护具有重要意义。提出以煤矸石接枝3-巯基丙基三甲氧基硅烷(MPTMS)和3-氨基丙基三乙氧基硅烷(APTES)制备一种低成本氨基巯基双官能团改性煤矸石(CG-SHNH)复合材料。通过XRD、XRD-EDS、XFR、FTIR、SEM、Zeta电位等手段对吸附材料的物理和化学特性进行全面分析，发现复合材料在2 930 cm−1和2 560 cm−1处出现新的谱带，分别对应C—H和S—H拉伸振动，在3 367 cm−1处出现了新的峰，为N—H键的吸收峰，说明CG-SHNH表面分布有丰富的氨基和巯基官能团。N2吸附脱附分析结果表明，CG-SHNH平均孔径明显增加，从17.33 nm增加到24.54 nm。CG-SHNH对Pb(Ⅱ)的吸附性能研究结果表明，在CG-SHNH添加量为1 g/L、接触时间为20 h、温度为25 ℃，pH为6.6,Pb(Ⅱ)溶液初始浓度为600 mg/L时，CG-SHNH对Pb(Ⅱ)的吸附效果最佳，吸附容量为125 mg/g。吸附机理研究表明，CG-SHNH氨基和巯基双官能团对Pb(Ⅱ)螯合吸附能够协同促进，展现出优异的重金属离子吸附能力。

煤矸石  /  吸附剂  /  Pb（Ⅱ）  /  巯基  /  氨基

The solid waste coal gangue produced in the process of coal mining and washing and the discharge of Pb(Ⅱ) from industrial wastewater will bring great harm to the ecosystem and human health, and it is of great significance to study the efficient removal method of Pb(Ⅱ) and the rational utilization of coal gangue for ecological and environmental protection. A low-cost aminothiol difunctional modified coal gangue (CG-SHNH) composite material was prepared by grafting 3-mercaptopropyl trimethoxysilane (MPTMS) and 3-aminopropyl triethoxysilane (APTES) with coal gangue. The physical and chemical properties of the adsorbed materials were investigated by means of XRD, XRD-EDS, XFR, FTIR, SEM, Zeta potential, and so on. And it is found that new bands appeare at 2 930 cm−1 and 2 560 cm−1, corresponding to C—H and S—H tensile vibrations, respectively, and a new peak appeares at 3 367 cm−1, which is the absorption peak of N—H bonds, indicating that the surface of CG-SHNH is rich in amino and sulfhydryl functional groups. The results of N2 adsorption-desorption analysis indicate that the average pore size of CG-SHNH increases significantly, from 17.33 nm to 24.54 nm. The study on the adsorption performance of CG-SHNH for Pb(Ⅱ) shows that the optimal adsorption capacity of CG-SHNH for Pb(Ⅱ) is 125 mg/g when the addition amount of CG-SHNH is 1 g/L, the contact time is 20 h, the temperature is 25 ℃, the pH is 6.6, and the initial concentration of Pb(Ⅱ) is 600 mg/L. The adsorption mechanism shows that CG-SHNH amino and sulfhydryl bifunctional groups can synergistically promote the chelation adsorption of Pb(Ⅱ), exhibiting excellent heavy metal ion adsorption ability.

Coal gangue  /  Adsorbent  /  Pb (Ⅱ)  /  Sulfhydryl  /  Amino group
雷锐, 董宪姝, 樊玉萍, 马晓敏. 氨基和巯基双官能团修饰煤矸石对铅离子的吸附性能研究. 矿业研究与开发, 2025 , 45 (2) : 279 -288 .
Rui LEI, Xianshu DONG, Yuping FAN, Xiaomin MA. Study on the Adsorption Properties of Lead Ions in Coal Gangue Modified by Amino and Sulfhydryl Bifunctional Groups[J]. Mining Research and Development, 2025 , 45 (2) : 279 -288 .
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0　引言
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煤矸石是煤炭采选过程中产生的固体废物，其大量堆积对工业生产和矿区的环境造成了严重的影响和负担[1]。我国煤矸石利用率仅为50%~60%[2]，堆积的煤矸石若不加以利用，会引起环境污染和资源浪费。因此，合理开发和利用煤矸石资源已成为我国亟待解决的问题。煤矸石中富含丰富的硅铝酸盐矿物，经过化学改性后对重金属的吸附效果明显。因此煤矸石被视为有应用前景的废水处理吸附剂和土壤重金属污染修复剂。
近年来国内外在采用吸附法处理重金属废水污染方面的研究取得了很大进展[3-4]。现有研究表明，通过高温煅烧、生物炭、沸石分子筛等手段包覆改性煤矸石合成复合材料，可显著提升煤矸石的离子交换能力[5]、比表面积以及平均孔径，从而增强了煤矸石的活性[6]，可制备为煤矸石基功能性复合材料，使其广泛应用于废水处理领域。煤矸石基功能性复合材料的应用不仅为解决我国固体废弃物堆存的环境污染问题提供了新思路，同时也将煤矸石转化为一种高效的吸附材料，用于去除废水中的污染物。铅及其可溶化合物均具有毒性，而含铅的废水对人类健康以及动植物的成长带来了显著的负面影响[7]。当重金属铅经由消化道被人体摄入后，会在体内形成一种称作“储存库”的聚集，随后会逐渐释放，通过血液循环传播至全身，并最终沉积在骨骼内，导致严重的积累性中毒现象[8-9]。
刘瑞等[10]的研究将壳聚糖接枝到改性煤基高岭土上制备Pb(Ⅱ)吸附剂CK-CTAC/CTS。在吸附温度为25 ℃，溶液pH为6，吸附时间为100 min的条件下，该吸附剂对Pb(Ⅱ)的吸附容量可达到195.37 mg/g。尚中博等通过运用3-巯基丙基三甲氧基硅烷(3-Mercaptopropyltriethoxysilane, MPTMS)对煤矸石进行化学改性处理，成功制备出了一种经济效益高且成本低的巯基煤矸石(CG-SH)。巯基非常活跃，可以与重金属离子如Pb(Ⅱ)形成稳定的化合物。研究结果表明，大量巯基(S—H)成功地引入到煤矸石表面，使Pb(Ⅱ)的吸附量大大提升，最大吸附量为332.8 mg/g。此外，煤矸石中含有大量的SiO2，能够接枝氨基基团制备功能化吸附材料。孙静静等[11]用3-氨基丙基三乙氧基硅烷(3-Aminopropyltriethoxysilane, APTES)处理介孔二氧化硅，使氨基团接枝到其表面，该材料对Pb(Ⅱ)具有选择的吸附特性，材料的吸附能力随着APTES含量的增加而提高。这些改进研究不仅增强了煤矸石的活性，还使其在废水处理领域的应用潜力得到显著提升。这一创新应用不仅为解决我国固体废弃物的环境污染问题提供了新思路，同时也使煤矸石转化为一种高效的吸附材料，展现出良好的环保价值与实用价值。
本研究以煤矸石(CG)为原料，在酸化除杂预处理后，APTES及MPTMS分别和煤矸石反应得到氨基和巯基双官能团修饰煤矸石(CG-SHNH)的复合吸附材料。本研究制备的煤矸石功能材料能有效地吸收多种污染物，具有很好的吸附能力，又可进行分离回收及再生利用。
1　材料与方法
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1.1　试验材料与仪器
本试验原料为煤矸石(CG)，试验过程中所用的主要试剂包括3-氨基丙基三乙氧基硅烷(APTES，国药试剂)及3-巯基丙基三甲氧基硅烷(MPTMS，国药试剂）、乙醇（C2H5OH，国药试剂）、甲醇(CH3OH，国药试剂）、水合肼（N2H4⋅H2O，国药试剂）、甲苯(C6H5CH3，国药试剂)等，均为分析纯。所用的试验仪器有集热式恒温加热磁力搅拌器、中速离心机、高速离心机、电感耦合等离子体(ICP-MS)、扫描电子显微镜、全自动比表面及孔隙度分析仪、X射线衍射仪、Zeta电位分析仪等。
1.2　样品制备
（1）对煤矸石进行研磨、筛分，取大约200目粒度的煤矸石进行干燥处理。
（2）将5 g煤矸石与40 mL浓度为20%的硫酸溶液混合。
（3）使用去离子水多次清洗离心管中的固体颗粒，直至洗涤至固体颗粒的pH达到中性状态。并在55 ℃的条件下进行烘干。
（4）将干燥完成的CG放入浓度为18.5%的200 mL盐酸溶液中，在水浴锅30 ℃环境中进行12 h的加热回流。
（5）随后取5 g经过两次酸处理的CG，分散在80 ℃的硫酸和水混合溶液中（体积比1:1,50 mL)，并在持续搅拌的同时加入15 mL高锰酸钾溶液。完成氧化后，使用去离子水清洗经过氧化的煤矸石，直到其pH恢复至中性。最后，将样品放入真空干燥器中，并在60 ℃环境中进行干燥。
（6）采用冷凝回流方法制备氨基和巯基双官能化煤矸石复合吸附材料。在制备CG-SH时，将处理后的4 g CG加入含有40 mL甲醇的100 mL圆底烧瓶中回流30 min，加入4 mL N2H4⋅H2O后回流2 h。最后加入3.77 mL MPTMS溶液，水浴锅69.6 ℃环境中继续回流12 h，然后用甲醇和去离子水洗涤至pH为中性。制备的样品在60 ℃下烘干，并在使用前保存在干燥器中。
（7）将接枝成功的巯基煤矸石(CG-SH)悬浮在20 mL甲苯中，并加入4.11 mL 3-氨基丙基三乙氧基硅烷(APTES)。水浴锅71.39 ℃环境下混合物冷凝回流54 h，对悬浮液进行过滤，分别用过量的甲苯和乙醇对固体悬浮物进行洗涤。
（8）样品置于真空干燥器中，并在60 ℃的条件下进行干燥处理。最终制备出具有氨基和巯基双官能团的煤矸石(CG-SHNH)复合吸附材料。
1.3　表征方法
利用Malvern Mastersizer 3000(XRD)，对CG材料的粒度分布进行详细分析，以准确描绘出材料的粒度特征。利用傅里叶变换红外光谱仪(FTIR)对CG及其CG表面成功接枝的产物进行表征。用扫描电子显微镜(SEM)对煤矸石粉末及其改性后的煤矸石粉末进行微观结构的采集。继续进行能量色散X射线光谱（Energy-Dispersive X-ray Spectroscopy, EDS)点扫描，即获得样品元素组成信息。采用单四极杆电感耦合等离子体质谱仪(ICP-MS)精确测量模拟废水溶液中的Pb(Ⅱ)浓度。
1.4　吸附试验
采用水体批量吸附试验进行CG-SHNH对Pb（Ⅱ)的吸附性能研究。将吸附剂CG-SHNH放入模拟Pb(Ⅱ)废水溶液中，溶液pH调整至7，振荡速度为180 r/min，温度25 ℃，持续吸附20 h。试验完成后，通过过滤稀释上清液，随后运用电感耦合等离子体质谱(ICP-MS)技术，测定Pb(Ⅱ)浓度。此外，通过使用0.1 mol/L的HCl或NaOH调整溶液的pH（范围为1~7)，研究不同pH对Pb(Ⅱ)的吸附效果。调整Pb（Ⅱ）初始浓度进一步探究了CG-SHNH对Pb(Ⅱ)的吸附性能。
2　结果与讨论
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2.1　氨基和巯基双官能修饰煤矸石的特性
2.1.1　XRD分析
煤矸石的XRD图谱如图1所示。由图1可知，煤矸石中高岭石为主要矿物。同时，伊利石、蒙脱石和石英等矿物成分的含量相对较低[12]。
2.1.2　XRF分析
表1为煤矸石改性前后的XRF分析。由CG、CG-SH及CG-SHNH中的主要化合物的含量（以氧化物的形式计算)可知，元素硫的含量增加了约2.5倍，表明在改性过程中巯基已成功地引入CG中。Al、K和Fe的损失可能归因于酸化过程[13]。
2.1.3　FTIR分析
煤矸石及两种改性煤矸石的FTIR图谱见图2。
由图2可知，CG在790 cm−1和470 cm−1处各有一个吸收峰[14]，对应Si—O—Si的对称伸缩振动；在1 034 cm−1附近的吸收峰是Si—O振动峰的特点，对应Si—O—Si的不对称伸缩振动。CG-SH与CG对比，在2 930 cm−1和2 560 cm−1处出现新的谱带，分别对应C—H和S—H拉伸振动，且CG-SH中的S主要以S—H的形式存在。证实了MPTMS已成功地修饰在CG上。此外，CG和CG-SH在3 703 cm−1、3 624 cm−1、3 439 cm−1和1 632 cm−1处都具有谱带，归因于Si—OH和H2O的振动。当APTES接枝到CG后，CG-SHNH的红外谱图中出现上述同样的吸收峰，CG-SHNH与CG及CG-SH相比，1 450 cm−1到1 600 cm−1吸收峰分别对应O—C—O的不对称伸缩振动和对称伸缩振动，对应于氨基，在3 367 cm−1处出现了新的峰[15]，为N—H键的吸收峰。结果表明APTES成功接枝到了CG上。
2.1.4　SEM形貌分析图
图3(a)和图3(b)为CG和CG-SH的表面形态。CG明显呈现片状，并且略显光滑，孔隙结构并不明显。与CG相比，CG-SH表面相对粗糙，这是因为氧化剂K2MnO4和H2SO4的氧化以及改性过程中N2H4的加入。
图3(c)为CG-SHNH的表面形态，与图3(a)和图3(b)相比，在保持原有形貌同时，CG-SHNH的表面明显粗糙，其外表面被一层氨丙基硅烷膜包覆[16]，与氨基功能化材料的形态一致，晶体颗粒会发生团聚，形成了块状的晶体，颗粒接枝良好且相对分散均匀，也为Pb(Ⅱ)提供更多的吸附位点，从而提高CG-SHNH对Pb(Ⅱ)的吸附能力。图3(d)为对Pb(Ⅱ)吸附完成后的CG-SHNH, CG-SHNH吸附了很多不规则多边形的片状物体，同时通过SEM-EDS的观察，不规则多边形的片状物体为Pb(Ⅱ)，表明CG-SHNH已吸附上Pb(Ⅱ)。
2.1.5　SEM-EDS分析
图4为CG-SHNH未吸附Pb(Ⅱ)的SEM-EDS，样品中未观察到Pb(Ⅱ)。图5为CG-SHNH吸附完Pb(Ⅱ)的样品，从图中观察到样品中有O、Al、Si、Pb 4种元素，并且明显观察到Pb(Ⅱ)的信号[17]，表明CG-SHNH对Pb(Ⅱ)的有效吸附。
2.1.6　N2吸附-脱附分析
图6为CG、CG-SH和CG-SHNH的氮气吸附—脱附等温线及其孔径分布，三种吸附剂的孔隙结构分析结果见表2。从图6可以观察到三种吸附剂均呈现出Ⅳ型吸附等温线的特征。在较低的相对压力下，吸附曲线表现为温和上升，表明此阶段主要发生的是单层吸附。随着相对压力的提升，吸附量显著增加，表明发生了多层吸附。孔隙结构主要分布在介孔区域(2~50 nm)，孔径集中在2~50 nm之间，说明了样品具有显著的介孔结构特点。CG-SHNH孔径介于2~50 nm之间的数量明显多于CG-SH及CG, CG-SH及CG-SHNH的比表面积和总孔容积较CG有明显减小，而平均孔径增加明显。CG经过2次接枝后，CG的比表面积从17.97 m2⋅g−1降至8.70 m2⋅g−1再到5.78 m2⋅g−1，孔体积也有所减小。但是，接枝后的2种CG产物的平均孔径都有明显增大。CG的平均孔径从17.33 nm增加到24.54 nm。在孔隙内部，由于烷基链的填充占据了空间，此外，在氨基接枝的阶段，硅醇基团间可能发生聚合反应，这一过程将导致微孔隙的堵塞及位阻效应的形成，造成了比表面积、孔径和孔体积的减少。小孔隙的阻塞使得CG-SHNH的平均孔径增大。虽然CG-SHNH的比表面积较小，但是其对Pb(Ⅱ)的吸附量反而更高，这表明在此过程中，化学吸附起着主导作用[18]。
2.1.7　Zeta电位分析
在溶液中，细粒物质的电动性质对于阐释固体颗粒表面吸附机制具有显著重要性。CG、CG-SH和CG-SHNH的Zeta电位分别为–6.755 mV、–45.45 mV和–19.05 mV。巯基能够赋予颗粒表面正电荷的官能团，氨基能够赋予颗粒表面负电荷的官能团。根据斯特恩双电层模型，在矿物-溶液界面上，当矿物表面经过氨基改性处理后，由于氨基团的引入，会形成一个电离层。这个过程导致矿物表面带有正电荷CG，对比经过MPTMS和APTES处理的CG，具有较高的电位值，这表明CG表面通过巯基和氨基的修饰，成功地接枝了大量的巯基和氨基。结合对Pb(Ⅱ)的吸附量的分析，说明CG表面巯基和氨基的接枝率是决定其吸附效能的关键。
2.2　CG-SHNH去除水中Pb(Ⅱ)影响因素的研究
2.2.1　添加量
图7为CG、CG-SH、CG-SHNH的添加量对吸附效果的影响曲线。由图7可知，CG对Pb(Ⅱ)的吸附率伴随着添加量的增加而缓慢上升，该曲线的斜率较小，表明添加量的增加对铅的吸附效率影响较小。CG-SH的吸附率高于CG，且随着添加量的增加，吸附率提高的速度也比CG快。CG-SHNH对Pb(Ⅱ)溶液的吸附率随添加量的增加逐渐升高，吸附率从13.6%提升至81.68%，相较于CG和CG-SH吸附效率更高。当CG-SHNH的添加量从0.2 g/L(0.01 g，溶液50 mL)提升至1 g/L(0.05 g，溶液50 mL)时，Pb(Ⅱ)吸附率不断升高，因为溶液中Pb(Ⅱ)的浓度一定，CG-SHNH添加量的增加使表面活性位点的数量增加，可供Pb(Ⅱ)吸附的表面扩大，使得CG-SHNH对Pb(Ⅱ)的吸附更加充分。当添加量超过1 g/L时，CG-SHNH对Pb(Ⅱ)的吸附已经趋于饱和，溶液中过量的吸附剂CG-SHNH未充分利用，因此确定1 g/L为最佳吸附剂添加量。
2.2.2　接触时间
图8为吸附率随接触时间的变化曲线。图8表明，随着接触时间的增加，CG吸附铅的效率逐渐上升，但整体上升幅度不大。CG-SH在接触的初始阶段，因大量未占用的—SH官能团与金属阳离子的相互作用非常强烈，其吸附效率快速上升，达到60%后上升幅度减缓，总体明显高于CG的吸附率。CG-SHNH吸附效率最好，CG-SHNH对Pb（Ⅱ）的吸附随时间的延长分为三个阶段：快速吸附阶段、慢速吸附阶段和平衡阶段。在吸附反应初期的0~30 min, CG-SHNH的Pb（Ⅱ）吸附量迅速上升至56.6 mg/g，此阶段主要是CG-SHNH表面的氨基、羟基对Pb（Ⅱ）的化学吸附，是快速吸附阶段[19]；在吸附反应的30~600 min内，吸附速度放缓，此阶段物理吸附和化学吸附共同作用，是慢速吸附阶段；在吸附反应的600~2 000 min内，吸附剂对Pb（Ⅱ）的物理吸附作用和化学吸附作用均达到平衡，吸附量趋于稳定，是吸附平衡阶段。在20 h时，吸附率达到81.6%，并在此后基本保持稳定，表明已达到吸附平衡状态。因此，最佳接触时间为20 h。
2.2.3　初始pH
图9为吸附溶液初始pH对吸附性能的影响曲线。从图9可以看出，在不同的溶液初始pH条件下，CG-SHNH的吸附效率均高于CG和CG-SH。CG-SHNH的Pb(Ⅱ)吸附量随溶液初始pH的升高而增大。吸附量的增大是因为酸性条件下溶液中H+会与重金属在其表面上的吸附产生竞争，但随着pH的升高，H+浓度逐渐降低[20]，竞争吸附逐渐减弱。但吸附量提高幅度有限，是因为氨基与Pb(Ⅱ)的吸附过程是化学吸附，吸附过程受pH变化的影响较小。由此可见，CG-SHNH不仅对Pb(Ⅱ)的吸附量有很大的提升，还在较宽的pH范围内保持较高的吸附量，这种特性使CG-SHNH对重金属废水的处理方面具备优势。后续试验中铅溶液的pH均控制在6.6。
由图10可知，在不同的初始浓度下，CG-SHNH的吸附性能始终优于CG和CG-SH。随着Pb(Ⅱ)溶液的初始质量浓度从50 mg/L提升至600 mg/L, CG-SHNH对Pb(Ⅱ)的吸附容量从49 mg/g提升至125 mg/g。当质量浓度超过120 mg/L后，吸附容量基本不变。说明CG-SHNH对Pb(Ⅱ)的吸附逐渐达到饱和状态，达到最大吸附容量。
综合分析表明，吸附剂对重金属离子的去除效率受多重因素控制，包括了吸附剂的添加量、与重金属离子的接触时长、溶液的初始pH及离子的初始质量浓度等变量。各影响因素条件下，CG-SHNH均表现了更优的吸附性能。试验条件中，当CG-SHNH吸附剂的添加量为1 g/L，接触时间设定为20 h，溶液初始pH为6.6，温度控制在25 ℃时，CG-SHNH对Pb(Ⅱ)离子的吸附性能最佳，其最大吸附容量达到了125 mg/g。
2.3　CG-SHNH对Pb(Ⅱ)吸附行为研究
2.3.1　吸附等温线
为了研究特定温度[21]下Pb(Ⅱ)离子在CG-SHNH 吸附剂上的平衡吸附量与溶液中浓度的相关性，本研究应用了 Langmuir和 Freundlich 两个等温吸附模型对试验数据进行分析 (见图11)。在室温条件下(25 ℃), 应用浓度为1 g/L的 CG-SHNH 复合吸附材料，对浓度在50~600 mg/L之间的Pb(Ⅱ)溶液进行了吸附研究。
式中：qe为平衡时的吸附容量，mg/g;Ce表示溶液中未吸附的Pb(Ⅱ)浓度，mg/L;qm表示最大Pb(Ⅱ)吸附容量，mg/g;b是朗缪尔常数；KF是吸附容量常数，L/g;n是吸附强度常数。
表3为两个模型的拟合参数取值，线性相关系数R2分别是0.997和0.948。试验结果表明，Langmuir等温模型的qm值125.79 mg/g与实际试验Pb(Ⅱ)吸附量qe值125 mg/g接近，说明Pb(Ⅱ)的吸附以单层吸附为主。
2.3.2　吸附动力学
为了说明CG-SHNH对水体中Pb(Ⅱ)的吸附机制[22]，在本研究中，运用了一级和二级动力学方程进行线性拟合，拟合参数取值见表4，拟合结果见图12。依据表4所示数据，二级动力学模型展现出的相关系数显著高于一级动力学模型。这表明准二级动力学模型能够较为准确地描述CG-SHNH对Pb(Ⅱ)的吸附过程。结果显示，该吸附过程主要是通过化学吸附机制进行，而物理吸附作用则起辅助作用。
2.3.3　吸附机理初步分析
CG-SH和CG-SHNH的Zeta电位分别为–6.755、–45.45和–19.05 mV，氨基显正电性，CG、巯基显负电性，此外，CG表面富含活性羟基等基团，通过离子交换作用及与Pb（Ⅱ）之间的Si—O键相互作用，促成了以化学吸附为主导的过程，进而大幅增强了对Pb（Ⅱ）的吸附效果。吸附过程的机理见图13。
3　结论
收起
（1）利用XRD、XRF、FTIR、氮气吸附解吸和孔径及Zeta电位等手段对CG-SHNH吸附材料的物理和化学特性进行分析，结果表明CG表面已经成功地接枝了氨基和巯基。
（2）对CG-SHNH复合材料在模拟含Pb(Ⅱ)废水中吸附特性进行了深入研究。在25 ℃室温条件下，当溶液pH为6.6，且初始Pb(Ⅱ)浓度为600 mg/L时，该材料在20 h内达到接近平衡的吸附状态，其吸附效率和容量均显著高于CG和CG-SH吸附剂。APTES中的氨基和MPTMS中的巯基元素对Pb(Ⅱ)的吸附呈现显著的协同效应，大幅提升了复合材料的吸附效果。
（3）准二级动力学模型更好地描述了CG-SHNH吸附铅离子的吸附容量和吸附时间的关系，显示出了以化学吸附为主导的特性。此外，在吸附等温线的研究中，吸附结果更贴近Langmuir吸附模型，说明CG-SHNH材料的吸附主要为单分子层吸附。

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  • 接收时间：2024-04-26
  • 首发时间：2026-10-29
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    太原理工大学 矿业工程学院，山西　太原　030024

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董宪姝（1964—），女，辽宁葫芦岛人，教授，博士生导师，主要从事煤炭洗选加工与综合利用研究。E-mail:
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2种不同金属材料的力学参数
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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
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