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Article(id=1148109995352256812, tenantId=1146029695717560320, journalId=1146120122248306696, issueId=1148109990923072455, articleNumber=1009-2617(2025)02-0238-09, orderNo=null, doi=10.13355/j.cnki.sfyj.2025.02.013, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1730736000000, receivedDateStr=2024-11-05, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1751660353744, onlineDateStr=2025-07-05, pubDate=1745769600000, pubDateStr=2025-04-28, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1751660353744, onlineIssueDateStr=2025-07-05, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1751660353744, creator=13701087609, updateTime=1751660353744, updator=13701087609, issue=Issue{id=1148109990923072455, tenantId=1146029695717560320, journalId=1146120122248306696, year='2025', volume='44', issue='2', pageStart='133', pageEnd='279', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=0, createTime=1751660352687, creator=13701087609, updateTime=1758246043500, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1175732380301148501, tenantId=1146029695717560320, journalId=1146120122248306696, issueId=1148109990923072455, language=EN, specialIssueTitle=, coverIllustrator=, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1175732380301148502, tenantId=1146029695717560320, journalId=1146120122248306696, issueId=1148109990923072455, language=CN, specialIssueTitle=, coverIllustrator=, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=238, endPage=246, ext={EN=ArticleExt(id=1148109995608109367, articleId=1148109995352256812, tenantId=1146029695717560320, journalId=1146120122248306696, language=EN, title=Removal of Iron from Coal Gangue by Thermally Activated Enhancement—Hydrochloric Acid Leaching Process, columnId=1152626641181700664, journalTitle=Hydrometallurgy of China, columnName=Experiment Research, runingTitle=null, highlight=null, articleAbstract=

Removal of iron from high silicon-aluminum ratio and high iron coal gangue using thermally activated enhanced—hydrochloric acid leaching process was studied. The effects of calcination temperature, calcination time, hydrochloric acid concentration, leaching temperature, liquid-to-solid mass ratio, and leaching time on the iron leaching rate were examined, and the process conditions were optimized through orthogonal experiments. The results show that under the optimized conditions of calcination temperature of 500 ℃, calcination time of 1 h, hydrochloric acid concentration of 20%, leaching time of 3 h, leaching temperature of 90 ℃, and liquid-to-solid mass ratio of 4/1, leaching rate of Fe can reach 94.25%. The method can efficiently remove iron from coal gangue while effectively enriching Si and Al elements, providing technical reference for the resource utilization of coal gangue.

, correspAuthors=Aiyuan MA, 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=Mingxian ZHANG, Fuqin YUAN, Aiyuan MA, Jinsong DU), CN=ArticleExt(id=1148110007306023179, articleId=1148109995352256812, tenantId=1146029695717560320, journalId=1146120122248306696, language=CN, title=热活化强化盐酸浸出煤矸石中的铁试验研究, columnId=1152626641328501305, journalTitle=湿法冶金, columnName=试验研究, runingTitle=null, highlight=null, articleAbstract=研究了采用热活化强化盐酸浸出法从高硅铝比、高铁煤矸石中脱除铁,考察了煅烧温度、煅烧时间、盐酸浓度、浸出温度、液固质量比、浸出时间对铁浸出率的影响,并通过正交试验优化了工艺条件。结果表明:在煅烧温度500 ℃、煅烧时间1 h、盐酸浓度20%、浸出时间3 h、浸出温度90 ℃、液固质量比4/1的优化条件下,Fe浸出率为94.25%。该法能高效脱除煤矸石中的铁,同时使Si、Al元素得到有效富集,可为煤矸石资源化利用提供一定技术参考。, correspAuthors=马爱元, authorNote=null, correspAuthorsNote=
马爱元(1988—),男,博士,教授,主要研究方向为固废资源综合利用。E-mail:。
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张明贤(1994—),男,硕士,讲师,主要研究方向为工业固体废弃物资源化。

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张明贤(1994—),男,硕士,讲师,主要研究方向为工业固体废弃物资源化。

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张明贤(1994—),男,硕士,讲师,主要研究方向为工业固体废弃物资源化。

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label=Fig.1, caption=XRD pattern of coal gangue, figureFileSmall=ZW0Bfg7l217ltp4maS6Tlg==, figureFileBig=uxeKl39yAR2a+xZVXl7AdA==, tableContent=null), ArticleFig(id=1174444176260350146, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1148109995352256812, language=CN, label=图1, caption=煤矸石的XRD图谱, figureFileSmall=ZW0Bfg7l217ltp4maS6Tlg==, figureFileBig=uxeKl39yAR2a+xZVXl7AdA==, tableContent=null), ArticleFig(id=1174444176398762179, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1148109995352256812, language=EN, label=Fig.2, caption=SEM-EDS characterization results of coal gangue, figureFileSmall=7SmQK9lpfLfYPlfmn0xZAg==, figureFileBig=wmtOG6CqOSvk52BbzLd0qw==, tableContent=null), ArticleFig(id=1174444176574922948, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1148109995352256812, language=CN, label=图2, caption=煤矸石的SEM-EDS表征结果, figureFileSmall=7SmQK9lpfLfYPlfmn0xZAg==, figureFileBig=wmtOG6CqOSvk52BbzLd0qw==, 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a、b—煅烧前;c、d—煅烧后。

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Chemical composition of coal gangue %

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SiO2 Al2O3 Fe2O3 TiO2 CaO K2O MgO P2O5 ZrO2 Cr2O3
44.8 17.4 20.6 6.64 3.54 3.11 1.14 0.27 0.218 0.106
), ArticleFig(id=1174444178579800284, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1148109995352256812, language=CN, label=表1, caption=

煤矸石原料的化学组成

, figureFileSmall=null, figureFileBig=null, tableContent=
SiO2 Al2O3 Fe2O3 TiO2 CaO K2O MgO P2O5 ZrO2 Cr2O3
44.8 17.4 20.6 6.64 3.54 3.11 1.14 0.27 0.218 0.106
), ArticleFig(id=1174444178638520541, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1148109995352256812, language=EN, label=Table 2, caption=

Factors and levels of orthogonal test

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水平 因素
A
浸出温度/℃		 B
浸出时间/h		 C
液固质量比		 D
盐酸浓度/%
1 70 1 3/1 10
2 80 2 4/1 15
3 90 3 5/1 20
), ArticleFig(id=1174444178709823710, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1148109995352256812, language=CN, label=表2, caption=

正交试验的因素及水平

, figureFileSmall=null, figureFileBig=null, tableContent=
水平 因素
A
浸出温度/℃		 B
浸出时间/h		 C
液固质量比		 D
盐酸浓度/%
1 70 1 3/1 10
2 80 2 4/1 15
3 90 3 5/1 20
), ArticleFig(id=1174444178831458527, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1148109995352256812, language=EN, label=Table 3, caption=

Orthogonal test results

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试验
编号		 浸出
温度/℃		 浸出
时间/h		 液固
质量比		 盐酸
浓度/%		 铁浸出
率/%
1 70 1 5/1 15 83.63
2 80 1 3/1 10 46.74
3 90 1 4/1 20 95.83
4 70 2 4/1 10 64.42
5 80 2 5/1 20 94.44
6 90 2 3/1 15 89.12
7 70 3 3/1 20 92.17
8 80 3 4/1 15 91.56
9 90 3 5/1 10 86.68
K1 240.22 226.20 228.03 197.84
K2 232.74 247.98 251.81 264.31
K3 271.63 270.41 264.75 282.44
k1 80.07 75.40 76.01 65.95
k2 77.58 82.66 83.94 88.10
k3 90.54 90.14 88.25 94.15
R 12.96 14.74 12.24 28.20
), ArticleFig(id=1174444178898567392, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1148109995352256812, language=CN, label=表3, caption=

正交试验结果

, figureFileSmall=null, figureFileBig=null, tableContent=
试验
编号		 浸出
温度/℃		 浸出
时间/h		 液固
质量比		 盐酸
浓度/%		 铁浸出
率/%
1 70 1 5/1 15 83.63
2 80 1 3/1 10 46.74
3 90 1 4/1 20 95.83
4 70 2 4/1 10 64.42
5 80 2 5/1 20 94.44
6 90 2 3/1 15 89.12
7 70 3 3/1 20 92.17
8 80 3 4/1 15 91.56
9 90 3 5/1 10 86.68
K1 240.22 226.20 228.03 197.84
K2 232.74 247.98 251.81 264.31
K3 271.63 270.41 264.75 282.44
k1 80.07 75.40 76.01 65.95
k2 77.58 82.66 83.94 88.10
k3 90.54 90.14 88.25 94.15
R 12.96 14.74 12.24 28.20
), ArticleFig(id=1174444178965676257, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1148109995352256812, language=EN, label=Table 4, caption=

Chemical composition of leaching residue %

, figureFileSmall=null, figureFileBig=null, tableContent=
SiO2 Al2O3 Fe2O3 TiO2 CaO K2O MgO P2O5 ZrO2 Cr2O3
70.9 12.0 2.95 9.82 0.143 2.97 0.423 0.091 3 0.229 —
), ArticleFig(id=1174444179020202210, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1148109995352256812, language=CN, label=表4, caption=

煤矸石浸出渣的化学组成

, figureFileSmall=null, figureFileBig=null, tableContent=
SiO2 Al2O3 Fe2O3 TiO2 CaO K2O MgO P2O5 ZrO2 Cr2O3
70.9 12.0 2.95 9.82 0.143 2.97 0.423 0.091 3 0.229 —
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热活化强化盐酸浸出煤矸石中的铁试验研究
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张明贤 1 , 袁富琴 2 , 马爱元 2 , 杜金松 2
湿法冶金 | 试验研究 2025,44(2): 238-246
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湿法冶金 | 试验研究 2025, 44(2): 238-246
热活化强化盐酸浸出煤矸石中的铁试验研究
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张明贤1, 袁富琴2, 马爱元2 , 杜金松2
作者信息
  • 1 六盘水师范学院 土木与规划学院, 贵州 六盘水 553004
  • 2 六盘水师范学院 化学与材料工程学院, 贵州 六盘水 553004

    • 张明贤(1994—),男,硕士,讲师,主要研究方向为工业固体废弃物资源化。

通讯作者:

马爱元(1988—),男,博士,教授,主要研究方向为固废资源综合利用。E-mail:。
Removal of Iron from Coal Gangue by Thermally Activated Enhancement—Hydrochloric Acid Leaching Process
Mingxian ZHANG1, Fuqin YUAN2, Aiyuan MA2 , Jinsong DU2
Affiliations
  • 1 School of Civil Engineering and Urban Planning, Liupanshui Normal University, Liupanshui 553004, China
  • 2 School of Chemistry and Materials Engineering, Liupanshui Normal University, Liupanshui 553004, China
出版时间: 2025-04-28 doi: 10.13355/j.cnki.sfyj.2025.02.013
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摘要
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研究了采用热活化强化盐酸浸出法从高硅铝比、高铁煤矸石中脱除铁,考察了煅烧温度、煅烧时间、盐酸浓度、浸出温度、液固质量比、浸出时间对铁浸出率的影响,并通过正交试验优化了工艺条件。结果表明:在煅烧温度500 ℃、煅烧时间1 h、盐酸浓度20%、浸出时间3 h、浸出温度90 ℃、液固质量比4/1的优化条件下,Fe浸出率为94.25%。该法能高效脱除煤矸石中的铁,同时使Si、Al元素得到有效富集,可为煤矸石资源化利用提供一定技术参考。
煤矸石  /  铁  /  浸出  /  煅烧  /  活化  /  盐酸

Removal of iron from high silicon-aluminum ratio and high iron coal gangue using thermally activated enhanced—hydrochloric acid leaching process was studied. The effects of calcination temperature, calcination time, hydrochloric acid concentration, leaching temperature, liquid-to-solid mass ratio, and leaching time on the iron leaching rate were examined, and the process conditions were optimized through orthogonal experiments. The results show that under the optimized conditions of calcination temperature of 500 ℃, calcination time of 1 h, hydrochloric acid concentration of 20%, leaching time of 3 h, leaching temperature of 90 ℃, and liquid-to-solid mass ratio of 4/1, leaching rate of Fe can reach 94.25%. The method can efficiently remove iron from coal gangue while effectively enriching Si and Al elements, providing technical reference for the resource utilization of coal gangue.

coal gangue  /  iron  /  leaching  /  calcination  /  activation  /  hydrochloric acid
张明贤, 袁富琴, 马爱元, 杜金松. 热活化强化盐酸浸出煤矸石中的铁试验研究. 湿法冶金, 2025 , 44 (2) : 238 -246 . DOI: 10.13355/j.cnki.sfyj.2025.02.013
Mingxian ZHANG, Fuqin YUAN, Aiyuan MA, Jinsong DU. Removal of Iron from Coal Gangue by Thermally Activated Enhancement—Hydrochloric Acid Leaching Process[J]. Hydrometallurgy of China, 2025 , 44 (2) : 238 -246 . DOI: 10.13355/j.cnki.sfyj.2025.02.013
正文
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煤矸石作为富含SiO2、Al2O3的固体废物,常被用作生产各类沸石、陶瓷、气凝胶等功能材料的原材料。但高铁煤矸石中以Fe2O3为主的各种杂质组分会极大地影响这些硅基材料的合成与性能,从而阻碍煤矸石的再生回收[1-6]。目前,从煤矸石中去除铁的技术主要包括磁选法[7]、浮选法[8]和重选法[9]等。磁选法是利用磁性物质的吸附作用,将含铁矿物质从煤矸石中分离出来;浮选法是利用矿物表面的亲水性和疏水性差异,将含铁煤矸石从煤矸石中分离出来;重选法则是利用煤矸石中不同密度的组分分选原理,将含铁煤矸石从煤矸石中分离出来。这些方法在实际应用中各有优缺点,需要根据原料的性质和产品的需求选择合适的技术路线。
为了进一步提高煤矸石除铁的效果和效率,近些年研究人员经过不断探索和优化,提出了多种方法,其中较为有效的方法是化学酸浸法[10]。研究表明在浸出前进行粉碎研磨或高温煅烧预处理,或将这两种方法结合进行预处理[8,11],之后再进行酸浸的除铁效果更佳。这是因为:粉碎研磨能明显减小煤矸石的颗粒尺寸,增加表面积,改善表面结构,从而增大煤矸石与酸浸剂的接触概率,提高浸出率;高温煅烧能破坏分解煤矸石中大部分的含杂质矿物相,释放其中的杂质成分,使煤矸石颗粒尺寸进一步减小,同时还能去除煤矸石内的有机质[12-16]。
试验以某高硅铝比、高铁煤矸石为原料,研究了采用热活化强化酸浸法从煤矸石深度回收铁,富集硅、铝,考察了热活化强化焙烧条件、浸出优化工艺条件对铁浸出率的影响,并探讨了煤矸石热活化强化溶铁机制,以期为开发煤矸石制备陶瓷等高附加值材料及煤矸石资源综合利用提供一定技术参考。
1 试验部分
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1.1 试验原料、试剂及设备
试验用煤矸石取自贵州省六盘水某煤矿企业,具有高硅铝比、含铁量高等特征。煤矸石的化学组成见表1,硅铝比达2.5以上,硅铝组分占煤矸石总质量的62.2%,可作为生产陶瓷等硅基材料的原材料。
图1为煤矸石原料的XRD图谱。
煤矸石中的SiO2、Al2O3主要来自石英相、高岭石相及斜绿泥石相,而Fe2O3则来自菱铁矿相和斜铁辉石相,另有少量TiO2来自锐钛矿相。除石英及锐钛矿相外,其余矿物相均可通过高温煅烧实现有效分解,基于此,试验选用高温热处理方式对煤矸石进行活化。
对煤矸石样品进行SEM-EDS形貌分析,结果如图2所示。由图2(a)、(b)可知:通过粉碎球磨步骤,煤矸石颗粒尺寸得到有效控制,基本保持在微米级别,且颗粒表面十分粗糙,使得其表面积明显增加,有利于提高后续酸浸效果。图2(c)为煤矸石的面扫能谱峰图及具体的元素占比。可以看出:各元素质量百分比由大到小依次为O、Si、Al、Fe、Mg、K、Ti、Ca,这与XRF的分析结果大体一致,O原子百分比远大于其他元素,说明该煤矸石基本由各种含氧矿物相组成,这与XRD的分析结果相吻合。
1.2 试验试剂及设备
主要试剂:浓盐酸,36%~38%,分析纯,购自重庆川东化工集团有限公司。
主要设备:PM2L型行星式球磨机(上海卓的仪器设备有限公司),SXP-4-13型马弗炉(北京科伟永兴仪器有限公司),DF-101S型恒温加热磁力搅拌器(巩义市予华仪器有限责任公司),DZF-6090型真空干燥箱(北京中科环试仪器有限公司)。
1.3 试验原理及方法
煤矸石中,铁通常以菱铁矿、斜铁辉石形式存在,经高温煅烧后,部分菱铁矿会氧化转化为铁氧化物,并与盐酸反应,通过活化能实现铁浸出率的提升。
4FeCO3+O2═══════2Fe2O3+4CO2↑;
Fe2O3+6HCl═══════2FeCl3+3H2O;
FeCO3+2HCl═══════FeCl2+CO2↑+H2O。
煤矸石破碎后球磨40 min,得煤矸石粉末,过200目筛。取一定量煤矸石粉末放入坩埚中,再将坩埚置于马弗炉中,在空气气氛中于一定温度下煅烧一定时间;取10 g煤矸石煅烧样,在相同浸出条件下用盐酸浸出Fe,考察各因素对Fe浸出率的影响,确定煤矸石煅烧热活化脱铁的最优工艺参数。浸出液中的Fe质量浓度通过紫外-可见分光光度计以邻二氮菲比色法测定,煤矸石原料(高温煅烧、微波消解处理实现消解)中Fe质量分数通过ICP-OES进行测定,Fe浸出率x通过下式计算:
x=$\frac{n\rho V}{mw}$×100%。
式中:ρ—浸出液中Fe质量浓度,mg/L;n—浸出液稀释倍数;V—浸出液总体积,L;m—煤矸石质量,g;w—煤矸石中Fe质量分数,%。
2 试验结果与讨论
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2.1 煤矸石煅烧热活化
2.1.1 煅烧温度和时间对Fe浸出率的影响
取固定量的煤矸石原料放入坩埚中,再将坩埚转移至马弗炉中,在空气气氛中,分别于400、500、600 ℃温度下煅烧一定时间,之后取煅烧后煤矸石10 g,在盐酸浓度15%、浸出时间2 h、浸出温度80 ℃、液固质量比4/1条件下浸出,并在相同条件下以未煅烧的煤矸石进行常规浸出作对比研究,不同煅烧温度下煅烧时间对Fe浸出率的影响如图3所示。可以看出:煅烧热活化后的煤矸石中Fe浸出率明显高于未煅烧的煤矸石;在不同煅烧温度下,Fe浸出率随煅烧时间延长呈先上升后下降再上升趋势,且煅烧时间为60 min、煅烧温度为500 ℃下的活化效果最好,Fe浸出率最高。
2.1.2 热活化后煤矸石的表征
为研究煤矸石热活化强化脱铁机制,对高温煅烧后煤矸石的XRD、SEM及粒度分布进行表征,分析了煅烧活化对煤矸石物相、微观形貌结构及粒度变化的影响,结果如图4~6所示。
通过对比图1、4可知:煤矸石煅烧前后的物相发生明显变化,其中大部分菱铁矿相和斜铁辉石相均消失,另有少量残余峰强度也明显减弱,充分说明通过煅烧,煤矸石内的含Fe相得到了有效活化;除含Fe物相外,煤矸石中含Al斜绿泥石相及部分高岭石相也遭到了一定程度破坏,出现了峰形减弱乃至消失的现象,使得Al离子流失。因高岭石在750 ℃时可转变为偏高岭石实现完全活化[17],故试验选择在500 ℃下煅烧,以确保最大程度地破坏含Fe相,同时保留大部分含Al相,防止Al离子过量流失;煅烧后煤矸石中石英相及锐钛矿相未发生明显变化,表明这2个物相在该煅烧条件下未被破坏。
图5为煤矸石原料和煤矸石煅烧样的SEM表征结果。通过对比发现,扫描区域内煅烧活化后的煤矸石中小型粉末颗粒的数量明显增加,粒度呈变小趋势。
图6为煤矸石煅烧样的SEM-EDS分析结果,与图2相比,煅烧后煤矸石颗粒表面变得疏松多孔,可见高温煅烧可使煤矸石中部分物质得到活化,在其内部产生大量孔隙,形成疏松多孔结构,从而为后续酸浸提供了有利条件,促进Fe浸出。
煤矸石原料及煅烧样的粒度分布如图7所示。可以看出:煤矸石原料颗粒粒径主要分布在8.023~80.225 μm之间,平均粒径为32.734 μm;煅烧样颗粒粒径主要分布在6.412~77.338 μm,平均粒径为29.336 μm之间,通过煅烧煤矸石的整体粒度明显减小,这与SEM的表征结果相吻合。这可能是因为菱铁矿、斜铁辉石、斜绿泥石等矿物晶体,以及存在于矿物晶体间的残留有机质在高温煅烧下被破坏发生分解,使较大的煤矸石颗粒分裂成数个小块造成的[18-19]。煤矸石颗粒尺寸的减小可增大后续酸浸过程的反应接触面,提升Fe浸出率。
2.2 煤矸石煅烧样的酸浸
2.2.1 盐酸浓度对Fe浸出率的影响
取煤矸石煅烧样10 g,控制浸出温度70 ℃、液固质量比3/1、浸出时间2 h,考察盐酸浓度对煤矸石中Fe浸出率的影响,试验结果如图8所示。
由图8可知:用5%盐酸进行浸出时,煤矸石中Fe离子浸出率仅为10.15%;随盐酸浓度增大,Fe浸出率迅速提高,在盐酸浓度增至15%时,Fe浸出率提升至80%左右,说明此时溶液中的H+与焙烧活化后煤矸石中可溶的FeCO3、Fe2O3接触较为充分,有利于反应进行;之后继续增大盐酸浓度,Fe浸出率升高幅度变缓,浓度超过20%时,Fe浸出率提升不明显,趋于稳定,说明此时浸出基本达到平衡状态,未被浸出的Fe可能属于少量未完全活化的斜铁辉石,在现有条件下无法快速溶出,需要更剧烈的反应条件。故选择20%盐酸进行后续试验。
2.2.2 浸出温度对Fe浸出率的影响
取煤矸石煅烧样10 g,控制盐酸浓度20%、液固质量比3/1、浸出时间2 h,考察浸出温度对煤矸石中Fe浸出率的影响,试验结果如图9所示。
由图9可知:升高浸出温度可有效提升Fe浸出率,在50~60 ℃范围内,提升十分明显,而后提升幅度逐渐趋缓;温度升至90 ℃时,Fe浸出率达90%左右。这是因为高温环境有效增加了H+和煤矸石的扩散速率和碰撞概率,使Fe离子的浸出速率大大提升,剧烈的反应环境使少量未被完全活化的菱铁矿和斜铁辉石溶解,释放其中的Fe[20]。考虑到浸出温度达80 ℃后,Fe浸出率提升不明显,故在浸出温度80 ℃下进行后续试验。
2.2.3 液固质量比对Fe浸出率的影响
取煤矸石煅烧样10 g,控制盐酸浓度20%、浸出温度80 ℃、浸出时间2 h,考察液固质量比对煤矸石中Fe浸出率的影响,试验结果如图10所示。
由图10可知:Fe浸出率随液固质量比增大而升高,这是因为液固质量比越大,反应体系黏度降低,有利于溶质的扩散,使盐酸与煤矸石充分接触,促进Fe浸出率;液固质量比增至5/1时,Fe浸出率升至95%左右;继续增大液固质量比,Fe浸出率提升幅度不大。故选择液固质量比5/1进行后续试验[21]。
2.2.4 浸出时间对Fe浸出率的影响
取煤矸石煅烧样10 g,控制盐酸浓度20%、浸出温度80 ℃、液固质量比4/1,考察浸出时间对煤矸石中Fe浸出率的影响,试验结果如图11所示。
由图11看出:,随浸出时间延长,Fe浸出率升高;浸出1 h时,煤矸石中大部分Fe被浸出;随浸出继续进行,Fe浸出率变化不大,趋于稳定。这是因为随浸出时间延长,可溶Fe不断浸出,盐酸不断消耗,Fe浸出速率降低,浸出1 h后,煤矸石中Fe浸出率已基本维持稳定。
根据单因素试验结果确定,煤矸石酸浸脱除铁的最优工艺参数为:盐酸浓度20%,浸出时间2 h,浸出温度80 ℃,液固质量比5/1。
2.2.5 正交优化试验
为实现以较低成本实现高铁脱除率目的,对煤矸石煅烧样进行酸浸正交试验,以优化浸出工艺参数。根据单因素试验结果设计了4因素3水平L9(34)正交试验,因素及水平见表2,试验结果见表3。
由表3可知:各因素对Fe浸出的影响顺序为盐酸浓度>浸出时间>浸出温度>液固质量比;盐酸浓度的影响因子明显高于其他因素,R值达28.20,而其他3个因素的R值相近,因此在选择优化条件时应在保证盐酸浓度20%前提下,尽可能降低其他因素带来的时间及成本损耗。综合考虑,确定优化酸浸方案为A3B3C2D3,即浸出温度90 ℃,浸出时间3 h,液固质量比4/1,盐酸浓度20%。在该条件下对煤矸石进行酸浸,酸浸液中Fe质量浓度为764.31 mg/L,经计算可知,Fe浸出率为94.25%。
2.3 煤矸石浸出渣的分析
2.3.1 XRF分析
煤矸石浸出渣的化学组成见表4。与表1对比可知:酸浸后煤矸石中的Fe2O3组分基本实现了脱除分离,CaO、MgO含量也大幅减少,而SiO2和大部分Al2O3组分都留在渣中,两者总质量分数达80%以上,说明通过热活化—酸浸,煤矸石有效组分质量分数得到了有效提升。
2.3.2 XRD分析
图12为煤矸石浸出渣的XRD图谱。对比图1、4可知:少量未被煅烧活化的含Fe相基本已被酸浸,因此仅残余的少量微弱的斜铁辉石峰;此外,高岭石相的峰强也因酸浸明显变弱,这是因为在剧烈酸浸条件下,高岭石相被破坏,使Al离子被浸出;而石英相及锐钛矿相在酸浸前后基本保持稳定,说明二者没有被破坏。
2.3.3 SEM-EDS分析
煤矸石及煤矸石浸出渣的扫描电镜图及能谱面扫分析结果如图13所示,图13(a)、(b)为煤矸石原料的扫描电镜图,图13(d)、(e)为煤矸石浸出渣的扫描电镜图。经对比可知:扫描区域内酸浸后的煤矸石颗粒粒度进一步减少,且表面更粗糙,呈不规则鳞片状,这是由于煤矸石内的活化组分被破坏溶解所致。图13(c)是煤矸石原料的能谱面扫分析结果,图13(f)是煤矸石浸出渣的能谱面扫分析结果。经对比可知:煤矸石原料内的O、Si、Al、Fe、Mg、K、Ti、Ca元素分布十分均匀,浸出后Fe、Mg、K、Ca的信号明显减弱,说明这些元素经酸浸基本脱除,而Si、Ti和大部分Al留在渣中,这与XRF的分析结果相吻合。
3 结论
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针对某高硅铝比、高铁煤矸石,采用热活化强化盐酸浸出法酸浸工艺脱除铁是可行的。在500 ℃下煅烧1 h,煤矸石中大部分含Fe相能得到有效活化,颗粒尺寸进一步减小。通过单因素试验和正交试验确定优化工艺条件为:盐酸浓度20%,浸出时间3 h,浸出温度90 ℃,液固质量比4/1,在该条件下,Fe浸出率为94.25%。煤矸石浸出渣中Fe等杂质成分能基本脱除,Si、Al元素得到有效富集,可作为生产陶瓷材料的原材料。
该法对于解决此类煤矸石的大量堆存、综合利用不足等问题,具有重要的实践指导意义和实际应用价值。但该法对于Si、Al组分的回收处理技术仍有待深入研究与优化,从而进一步提升回收效率,全面高效推进煤矸石资源的综合回收利用。
基金
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  • 贵州省教育厅项目(黔教技[2024]157号,黔教技[2024]152号)
  • 六盘水市科技局科技发展项目(52020-2024-0-2-8)
  • 六盘水师范学院重点学科建设项目(LPSSYZDXK2022001)
  • 贵州省大学生创新训练计划项目(S202310977119)
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2025年第44卷第2期
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文章信息
doi: 10.13355/j.cnki.sfyj.2025.02.013
  • 接收时间：2024-11-05
  • 首发时间：2025-07-05
  • 出版时间：2025-04-28
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  • 收稿日期：2024-11-05
基金
贵州省教育厅项目(黔教技[2024]157号,黔教技[2024]152号)
六盘水市科技局科技发展项目(52020-2024-0-2-8)
六盘水师范学院重点学科建设项目(LPSSYZDXK2022001)
贵州省大学生创新训练计划项目(S202310977119)
作者信息
    1 六盘水师范学院 土木与规划学院, 贵州 六盘水 553004
    2 六盘水师范学院 化学与材料工程学院, 贵州 六盘水 553004

通讯作者:

马爱元(1988—),男,博士,教授,主要研究方向为固废资源综合利用。E-mail:。
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https://castjournals.cast.org.cn/joweb/sfyj/CN/10.13355/j.cnki.sfyj.2025.02.013
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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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