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Article(id=1148106701267530100, tenantId=1146029695717560320, journalId=1146031787341344770, issueId=1148106698197295351, articleNumber=1003-3033(2025)02-0057-09, orderNo=null, doi=10.16265/j.cnki.issn1003-3033.2025.02.0698, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1726156800000, receivedDateStr=2024-09-13, revisedDate=1732204800000, revisedDateStr=2024-11-22, acceptedDate=null, acceptedDateStr=null, onlineDate=1751659568373, onlineDateStr=2025-07-05, pubDate=1740672000000, pubDateStr=2025-02-28, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1751659568373, onlineIssueDateStr=2025-07-05, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1751659568372, creator=13701087609, updateTime=1751659568372, updator=13701087609, issue=Issue{id=1148106698197295351, tenantId=1146029695717560320, journalId=1146031787341344770, year='2025', volume='35', issue='2', pageStart='1', pageEnd='252', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=0, createTime=1751659567641, creator=13701087609, updateTime=1757401525528, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1172190215188894212, tenantId=1146029695717560320, journalId=1146031787341344770, issueId=1148106698197295351, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1172190215188894213, tenantId=1146029695717560320, journalId=1146031787341344770, issueId=1148106698197295351, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=57, endPage=65, ext={EN=ArticleExt(id=1149767846005223751, articleId=1148106701267530100, tenantId=1146029695717560320, journalId=1146031787341344770, language=EN, title=Influence of coal metamorphism on microstructure and pyrolysis parameters: a correlation analysis, columnId=1149733269173878863, journalTitle=China Safety Science Journal, columnName=Safety engineering technology, runingTitle=null, highlight=null, articleAbstract=

To reveal the impact of coal metamorphism on the self-ignition process，experimental and quantitative analysis methods was combined to analyze the pyrolysis characteristics，microstructural changes，and their correlations during coal self-ignition. First，Fourier-transform infrared spectroscopy (FTIR) was employed to determine changes in the content of active functional groups in coal samples. Then，thermogravimetric analysis (TGA) was conducted to obtain pyrolysis characteristic parameters for coal samples with varying degrees of metamorphism. Finally，Pearson correlation coefficient method was applied to quantify the relationship between microstructure and characteristic temperatures during coal self-ignition. The results indicate that as the degree of coal metamorphism increases，the content of aromatic and aliphatic hydrocarbons(Ar-CH) rises，while oxygen-containing functional groups(C-O-C) significantly decrease. Low-rank coal samples exhibit the highest proportion of oxygen-containing functional groups，whereas high-rank coal samples contain more than 50% aromatic hydrocarbons. Increased metamorphism delays weight loss curves and shifts them to higher temperature regions，leading to an increase in characteristic temperatures. Ar-CH show a significant positive correlation with characteristic temperatures，while C-O-C exhibit a negative correlation. Overall，the increase in Ar-CH and the decrease in C-O-C in coal samples are identified as the primary microstructural factors responsible for the rise in characteristic temperatures and the reduction in self-ignition propensity.

, correspAuthors=Ximan GUO, 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=Zhengliang YE, Ximan GUO, Bo SHANG, Mian HU), CN=ArticleExt(id=1148106711837175993, articleId=1148106701267530100, tenantId=1146029695717560320, journalId=1146031787341344770, language=CN, title=煤变质程度对微观结构与热解参数的影响及关联性分析, columnId=1149733269727526997, journalTitle=中国安全科学学报, columnName=安全工程技术, runingTitle=null, highlight=null, articleAbstract=

为揭示煤变质程度对煤自燃过程的影响，结合试验与定量分析方法分析煤自燃过程中热解参数、微观结构的变化特征及二者之间关联性特征。首先，利用傅立叶变换红外光谱(FTIR)试验分析煤样中主要活性官能团的含量变化；然后，通过热重分析(TGA)试验获取不同变质程度煤样的热解特征参数；最后，基于Pearson相关系数法量化煤自燃过程中微观结构与特征温度之间的关联性。结果表明：随着煤样变质程度的提高，芳香烃(Ar-CH)和脂肪烃含量增加，含氧官能团(如C-O-C)显著减少;低阶煤样中含氧官能团占比最高，高阶煤样中芳香烃含量超过50%；变质程度提高使失重曲线滞后并向高温区移动，特征温度随之升高;芳香烃与特征温度呈显著正相关关系，而含氧官能团与特征温度呈负相关关系。煤样中芳香烃含量的增加和含氧官能团的减少，是特征温度升高及自燃倾向性降低的主要微观结构因素。

, correspAuthors=郭曦蔓, authorNote=null, correspAuthorsNote=
**郭曦蔓(1998—)，女，甘肃兰州人，硕士，助理工程师，主要从事煤矿火灾防控与治理方面的研究。E-mail：。
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叶正亮 (1981—)，男，江苏盐城人，硕士，正高级工程师，主要从事煤矿自燃火灾防治相关的基础理论、工艺技术和装备材料的研究。E-mail：。

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叶正亮 (1981—)，男，江苏盐城人，硕士，正高级工程师，主要从事煤矿自燃火灾防治相关的基础理论、工艺技术和装备材料的研究。E-mail：。

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叶正亮 (1981—)，男，江苏盐城人，硕士，正高级工程师，主要从事煤矿自燃火灾防治相关的基础理论、工艺技术和装备材料的研究。E-mail：。

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Coal Science and Technology, 2023, 51(1):304-312., articleTitle=Study on the influence of gas on the microstructure and thermal reactivity of coal in low temperature oxidation process, refAbstract=null), Reference(id=1165682049290608702, tenantId=1146029695717560320, journalId=1146031787341344770, articleId=1148106701267530100, doi=null, pmid=null, pmcid=null, year=2022, volume=29, issue=3, pageStart=62, pageEnd=70, url=null, language=null, rfNumber=[20], rfOrder=34, authorNames=王秋红, 靳松灵, 罗振敏, journalName=安全与环境工程, refType=null, unstructuredReference=王秋红, 靳松灵, 罗振敏, 等. 煤变质程度对煤燃烧动力学参数的影响[J]. 安全与环境工程, 2022, 29(3):62-70., articleTitle=煤变质程度对煤燃烧动力学参数的影响, refAbstract=null), Reference(id=1165682049504518207, tenantId=1146029695717560320, journalId=1146031787341344770, articleId=1148106701267530100, doi=null, pmid=null, pmcid=null, year=2022, volume=29, issue=3, pageStart=62, pageEnd=70, url=null, language=null, rfNumber=[20], rfOrder=35, authorNames=WANG Qiuhong, JIN Songling, LUO Zhenmin, journalName=Safety and Environmental Engineering, refType=null, unstructuredReference=WANG Qiuhong, JIN Songling, LUO Zhenmin, et al. 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Safety and Environmental Engineering, 2022, 29(3):62-70., articleTitle=Effect of coal metamorphic grade on kinetic parameters of coal combustion, refAbstract=null), Reference(id=1165682049680678976, tenantId=1146029695717560320, journalId=1146031787341344770, articleId=1148106701267530100, doi=null, pmid=null, pmcid=null, year=2024, volume=49, issue=4, pageStart=1906, pageEnd=1916, url=null, language=null, rfNumber=[21], rfOrder=36, authorNames=潘荣锟, 胡代民, 贾海林, journalName=煤炭学报, refType=null, unstructuredReference=潘荣锟, 胡代民, 贾海林, 等. 深部开采高温热液侵蚀煤自燃特性研究[J]. 煤炭学报, 2024, 49(4):1906-1916., articleTitle=深部开采高温热液侵蚀煤自燃特性研究, refAbstract=null), Reference(id=1165682049919754305, tenantId=1146029695717560320, journalId=1146031787341344770, articleId=1148106701267530100, doi=null, pmid=null, pmcid=null, year=2024, volume=49, issue=4, pageStart=1906, pageEnd=1916, url=null, language=null, rfNumber=[21], rfOrder=37, authorNames=PAN Rongkun, HU Daimin, JIA Hailin, journalName=Journal of China Coal Society, refType=null, unstructuredReference=PAN Rongkun, HU Daimin, JIA Hailin, et al. Study on spontaneous combustion characteristics of high temperature hydrothermal erosion coal in deep mining[J]. Journal of China Coal Society, 2024, 49(4):1906-1916., articleTitle=Study on spontaneous combustion characteristics of high temperature hydrothermal erosion coal in deep mining, refAbstract=null)], funds=[Fund(id=1165682041459843097, tenantId=1146029695717560320, journalId=1146031787341344770, articleId=1148106701267530100, awardId=2023YFF0615404, language=CN, fundingSource=国家重点研发计划(2023YFF0615404), fundOrder=null, country=null), Fund(id=1165682041648586778, tenantId=1146029695717560320, journalId=1146031787341344770, articleId=1148106701267530100, awardId=U23B2093, language=CN, fundingSource=国家自然科学基金联合重点项目资助(U23B2093), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1165682028130345943, tenantId=1146029695717560320, journalId=1146031787341344770, articleId=1148106701267530100, xref=null, ext=[AuthorCompanyExt(id=1165682028134540248, tenantId=1146029695717560320, journalId=1146031787341344770, articleId=1148106701267530100, companyId=1165682028130345943, language=EN, 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articleId=1148106701267530100, language=EN, label=Fig.5, caption=Peak fitting curve of 1 800-1 000 cm-1band, figureFileSmall=YCM+ZnCVQ5xnjIb3W2OQBQ==, figureFileBig=eqNTUR7d/SXQuBaxTyJ2Bg==, tableContent=null), ArticleFig(id=1165682036615421956, tenantId=1146029695717560320, journalId=1146031787341344770, articleId=1148106701267530100, language=CN, label=图5, caption=1 800~1 000 cm-1波段的分峰拟合曲线, figureFileSmall=YCM+ZnCVQ5xnjIb3W2OQBQ==, figureFileBig=eqNTUR7d/SXQuBaxTyJ2Bg==, tableContent=null), ArticleFig(id=1165682036665753605, tenantId=1146029695717560320, journalId=1146031787341344770, articleId=1148106701267530100, language=EN, label=Fig.6, caption=Changes in relative content of functional groups of coal with different metamorphic degrees, figureFileSmall=dFdGz0bBBqXJrybISKZpxA==, figureFileBig=BVhPyZuEYtSw8Pe5HEZ4wg==, tableContent=null), ArticleFig(id=1165682036724473862, tenantId=1146029695717560320, journalId=1146031787341344770, articleId=1148106701267530100, language=CN, 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figureFileBig=ngGz3/7Dm4FCJmTQaM2wyw==, tableContent=null), ArticleFig(id=1165682039262027793, tenantId=1146029695717560320, journalId=1146031787341344770, articleId=1148106701267530100, language=EN, label=Table 1, caption=

Industrial analysis test results %

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煤种 水分 灰分 挥发分 固定碳
含量
方家畔煤业褐煤 5.06 9.58 40.22 59.90
兴隆庄煤矿气煤 2.45 8.85 33.42 65.28
云驾岭矿无烟煤 1.88 16.56 2.35 97.12
), ArticleFig(id=1165682039442382866, tenantId=1146029695717560320, journalId=1146031787341344770, articleId=1148106701267530100, language=CN, label=表1, caption=

工业分析测试结果

, figureFileSmall=null, figureFileBig=null, tableContent=
煤种 水分 灰分 挥发分 固定碳
含量
方家畔煤业褐煤 5.06 9.58 40.22 59.90
兴隆庄煤矿气煤 2.45 8.85 33.42 65.28
云驾岭矿无烟煤 1.88 16.56 2.35 97.12
), ArticleFig(id=1165682039610155027, tenantId=1146029695717560320, journalId=1146031787341344770, articleId=1148106701267530100, language=EN, label=Table 2, caption=

Peak area of infrared absorption vibration region of 3 coal samples

, figureFileSmall=null, figureFileBig=null, tableContent=
煤种 峰面积
羟基 脂肪烃 芳香烃 含氧官能团
Ar-CH C=C 多种取
代芳烃		 -COOH C=O R-O-R'
方家畔煤业褐煤 107.735 75.85 14.12 21.088 15.664 5.189 8.445 61.085
兴隆庄煤矿气煤 2.376 15.295 4.585 10.915 21.388 — 3.841 6.705
云驾岭矿无烟煤 16.743 2.832 2.640 2.054 8.838 — 0.306 33.299
), ArticleFig(id=1165682039836647444, tenantId=1146029695717560320, journalId=1146031787341344770, articleId=1148106701267530100, language=CN, label=表2, caption=

3种煤样红外吸收振动区峰面积

, figureFileSmall=null, figureFileBig=null, tableContent=
煤种 峰面积
羟基 脂肪烃 芳香烃 含氧官能团
Ar-CH C=C 多种取
代芳烃		 -COOH C=O R-O-R'
方家畔煤业褐煤 107.735 75.85 14.12 21.088 15.664 5.189 8.445 61.085
兴隆庄煤矿气煤 2.376 15.295 4.585 10.915 21.388 — 3.841 6.705
云驾岭矿无烟煤 16.743 2.832 2.640 2.054 8.838 — 0.306 33.299
), ArticleFig(id=1165682040092499989, tenantId=1146029695717560320, journalId=1146031787341344770, articleId=1148106701267530100, language=EN, label=Table 3, caption=

Relative content of functional groups with different metamorphic degrees %

, figureFileSmall=null, figureFileBig=null, tableContent=
煤种 羟基 脂肪烃 芳香烃 含氧官能团
褐煤 29.10 10.49 13.74 46.68
气煤 25.10 14.25 20.31 40.37
无烟煤 3.65 23.49 56.66 16.20
), ArticleFig(id=1165682040348352534, tenantId=1146029695717560320, journalId=1146031787341344770, articleId=1148106701267530100, language=CN, label=表3, caption=

不同变质程度官能团相对含量

, figureFileSmall=null, figureFileBig=null, tableContent=
煤种 羟基 脂肪烃 芳香烃 含氧官能团
褐煤 29.10 10.49 13.74 46.68
气煤 25.10 14.25 20.31 40.37
无烟煤 3.65 23.49 56.66 16.20
), ArticleFig(id=1165682040646148119, tenantId=1146029695717560320, journalId=1146031787341344770, articleId=1148106701267530100, language=EN, label=Table 4, caption=

Characteristic temperature points of coal samples ℃

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煤样 特征温度点
t1 t2 t3 t4 t5 t6 t7
临界温度 干裂温度 活性温度 增速温度 着火温度 速率最大温度 燃尽温度
方家畔煤业褐煤 66.25 175.25 250.00 292.25 420.25 508.75 633.75
兴隆庄煤矿气煤 69.50 174.50 334.00 365.25 511.64 643.00 787.00
云驾岭矿无烟煤 72.5 261.25 341.75 405.25 615.42 690.25 788.00
), ArticleFig(id=1165682040927166488, tenantId=1146029695717560320, journalId=1146031787341344770, articleId=1148106701267530100, language=CN, label=表4, caption=

煤样的特征温度点

, figureFileSmall=null, figureFileBig=null, tableContent=
煤样 特征温度点
t1 t2 t3 t4 t5 t6 t7
临界温度 干裂温度 活性温度 增速温度 着火温度 速率最大温度 燃尽温度
方家畔煤业褐煤 66.25 175.25 250.00 292.25 420.25 508.75 633.75
兴隆庄煤矿气煤 69.50 174.50 334.00 365.25 511.64 643.00 787.00
云驾岭矿无烟煤 72.5 261.25 341.75 405.25 615.42 690.25 788.00
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煤变质程度对微观结构与热解参数的影响及关联性分析
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叶正亮 , 郭曦蔓 ** , 尚博 , 胡冕
中国安全科学学报 | 安全工程技术 2025,35(2): 57-65
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中国安全科学学报 | 安全工程技术 2025, 35(2): 57-65
煤变质程度对微观结构与热解参数的影响及关联性分析
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叶正亮 , 郭曦蔓** , 尚博, 胡冕
作者信息
  • 中煤能源研究院有限责任公司，陕西 西安 710054

    • 叶正亮 (1981—)，男，江苏盐城人，硕士，正高级工程师，主要从事煤矿自燃火灾防治相关的基础理论、工艺技术和装备材料的研究。E-mail：。

通讯作者:

**郭曦蔓(1998—)，女，甘肃兰州人，硕士，助理工程师，主要从事煤矿火灾防控与治理方面的研究。E-mail：。
Influence of coal metamorphism on microstructure and pyrolysis parameters: a correlation analysis
Zhengliang YE , Ximan GUO** , Bo SHANG, Mian HU
Affiliations
  • China Coal Energy Research Institute Co.，Ltd.，Xi'an Shaanxi 710054，China
出版时间: 2025-02-28 doi: 10.16265/j.cnki.issn1003-3033.2025.02.0698
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摘要
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为揭示煤变质程度对煤自燃过程的影响，结合试验与定量分析方法分析煤自燃过程中热解参数、微观结构的变化特征及二者之间关联性特征。首先，利用傅立叶变换红外光谱(FTIR)试验分析煤样中主要活性官能团的含量变化；然后，通过热重分析(TGA)试验获取不同变质程度煤样的热解特征参数；最后，基于Pearson相关系数法量化煤自燃过程中微观结构与特征温度之间的关联性。结果表明：随着煤样变质程度的提高，芳香烃(Ar-CH)和脂肪烃含量增加，含氧官能团(如C-O-C)显著减少;低阶煤样中含氧官能团占比最高，高阶煤样中芳香烃含量超过50%；变质程度提高使失重曲线滞后并向高温区移动，特征温度随之升高;芳香烃与特征温度呈显著正相关关系，而含氧官能团与特征温度呈负相关关系。煤样中芳香烃含量的增加和含氧官能团的减少，是特征温度升高及自燃倾向性降低的主要微观结构因素。

变质程度  /  微观结构  /  热解参数  /  关联性  /  煤自燃  /  官能团

To reveal the impact of coal metamorphism on the self-ignition process，experimental and quantitative analysis methods was combined to analyze the pyrolysis characteristics，microstructural changes，and their correlations during coal self-ignition. First，Fourier-transform infrared spectroscopy (FTIR) was employed to determine changes in the content of active functional groups in coal samples. Then，thermogravimetric analysis (TGA) was conducted to obtain pyrolysis characteristic parameters for coal samples with varying degrees of metamorphism. Finally，Pearson correlation coefficient method was applied to quantify the relationship between microstructure and characteristic temperatures during coal self-ignition. The results indicate that as the degree of coal metamorphism increases，the content of aromatic and aliphatic hydrocarbons(Ar-CH) rises，while oxygen-containing functional groups(C-O-C) significantly decrease. Low-rank coal samples exhibit the highest proportion of oxygen-containing functional groups，whereas high-rank coal samples contain more than 50% aromatic hydrocarbons. Increased metamorphism delays weight loss curves and shifts them to higher temperature regions，leading to an increase in characteristic temperatures. Ar-CH show a significant positive correlation with characteristic temperatures，while C-O-C exhibit a negative correlation. Overall，the increase in Ar-CH and the decrease in C-O-C in coal samples are identified as the primary microstructural factors responsible for the rise in characteristic temperatures and the reduction in self-ignition propensity.

metamorphic degree  /  microstructur  /  pyrolysis parameters  /  correlation  /  spontaneous combustion of coal  /  functional groups
叶正亮, 郭曦蔓, 尚博, 胡冕. 煤变质程度对微观结构与热解参数的影响及关联性分析. 中国安全科学学报, 2025 , 35 (2) : 57 -65 . DOI: 10.16265/j.cnki.issn1003-3033.2025.02.0698
Zhengliang YE, Ximan GUO, Bo SHANG, Mian HU. Influence of coal metamorphism on microstructure and pyrolysis parameters: a correlation analysis[J]. China Safety Science Journal, 2025 , 35 (2) : 57 -65 . DOI: 10.16265/j.cnki.issn1003-3033.2025.02.0698
正文
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0 引言
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鉴于我国多煤少油的能源结构，以及国家发展的综合需求，未来数十年，煤炭资源依旧是我国多能互补的现代化能源体系中不可或缺的主体资源[1]。近年来，我国煤炭开采强度增加导致安全事故频发，其中超过90%的煤层具有自燃或容易自燃的特性，因此，矿井火灾成为制约矿井安全高效生产的主要因素[2]。煤矿内因火灾具有产生机制复杂、发生地点隐蔽、传播速度迅速等特征，导致火灾防治和救援难度较大[3-4]。据统计[5]，我国(不含港澳台地区)25个主要产煤区共约5 300处煤矿，有70%以上的煤矿存在煤自燃隐患，因此，探究煤自燃的演化过程，揭示其机制对预防事故发生至关重要。
煤自燃过程可根据其热失重的特征温度划分其自燃的反应阶段及反应特性，而煤自然发火的本质是煤分子中复杂的微观结构发生氧化反应并产生热量积聚的结果。文虎等[6]利用程序升温试验，优选出高瓦斯矿井自燃早期预报指标。贾廷贵等[7]利用联用试验，得出烟煤自燃过程中的热解参数，并建立了动力学方程，计算出煤样的热动力参数。ZHANG Duo等[8]采用特征温度分析法，建立了唐家汇矿煤的6个特征温度及阈值，得出各阶段的预警标准和特征参数阈值，成功预测了煤自燃程度。朱建芳等[9]采用热重(Thermogravimetry)/傅里叶变换红外光谱(Fourier Transform Infrared Spectroscopy，TFTIR)联用试验得出煤中硫含量会提高煤分子的化学活性，加速煤自燃进程。耿济世等[10]自主研发了热解试验装置，测出富油煤原位热解工艺参数选择的关键数据。张玉涛等[11]采用Arrhenius公式拟合得出煤质指标和煤自燃危险性的关联性，其中，挥发分和燃料比与临界温度前后的相关联性最大。ZHAO Jinyu等[12]采用贫氧环境下的试验分析方法研究煤自燃过程中煤微观结构的演变，得出氧浓度对活性基团影响的规律。SHI Quanlin等[13]采用试验分析探究预氧化温度对煤微观结构及自然特性的影响，得出当预氧化温度低于临界温度时，预氧化处理会增加煤自燃风险。李美芬等[14]采用在线热解试验法，探究伊敏褐煤结构演化特征与热解行为的关系，得出低阶煤高效开发利用和煤基石墨演化的关键数据。XIAO Yang等[15]通过差示扫描量热(Differential Scanning Calorimetry，DSC)试验计算出碳化和氧化煤粉的自燃热解参数，得出碳化和氧化粉末的活化能等热动力参数，为煤质活性炭的制备提供了理论基础。综上所述，学者们对煤自燃过程的特征参数、热动力参数以及煤分子的微观结构分析做了大量研究，但大多以单一煤种为研究对象分析其宏观演化特征和微观机制，且二者间的关联性分析仍有不足。然而，煤的形成过程受多种因素影响，导致煤质成分存在差异，因此，不同变质程度的煤在自燃反应过程中特征参数和微观结构展现出一定不同，而煤样的微观结构从本质上影响自燃过程特征参数的变化。
鉴于此，笔者分别以陕西榆林方家畔煤业的褐煤、山东济宁兴隆庄煤矿的气煤(烟煤)和河北邯郸云驾岭矿的无烟煤等为研究对象，采用TG和FTIR试验，分析计算不同变质程度煤样的热解参数、官能团种类及含量、微观基团和特征温度的关联性，以期明确煤的变质程度对煤自燃过程在宏观和微观角度下的影响，为类似煤种矿区自然发火防控提供理论基础。
1 煤样工业测试及热解试验
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根据《煤样的制备方法》[16]，将方家畔煤业褐煤、兴隆庄煤矿气煤和云驾岭矿无烟煤3种不同变质程度的煤样放置在75℃恒温干燥箱中干燥2 h，然后采用标准试验将煤样研磨至粒径为0.212~0.180 mm，制备完成后将其置于广口瓶中并确保密封良好。工业分析测试结果见表1。由表1可知：煤样变质程度的增加使固定碳含量占比增大，反之水分和挥发分的比例降低。总体上褐煤中的水分和灰分含量较低，均未超过10%，挥发分含量较高，在高挥发分条件下自燃危险性较高。煤样组分随变质程度增加而变化，说明变质程度对其微观结构造成了一定影响，导致不同煤阶的煤种在煤自然发火过程中存在一定差异。
试验采用FTIR仪测定官能团，采用专业型同步热分析仪测定不同变质程度的煤样在升温热解过程中的质量变化，设置试验升温速率为15 ℃/min，升温范围为30~800 ℃。
2 煤变质程度对微观结构的影响
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煤自燃的本质是煤大分子中的官能团与氧气发生化学反应导致热量积聚的结果，因此，研究不同变质程度煤种的主要活性官能团，可分析煤样变质程度对自燃过程影响的微观机制。煤样红外光谱如图1所示，图1中纵坐标为红外光谱中的Kubelka-Munk变换，是一种用于处理反射光谱数据的数学处理方法。Kubelka-Munk变换的基本方程为F(R)=(1-R)2/2R，其中，F(R)为Kubelka-Munk函数，R为样品的漫反射率(即1减去透射率)。通过变换，原本的漫反射率数据可以转换成一个类似于吸收系数的值，从而使得光谱图更易于解释和分析。
由图1可知：随煤样变质程度的增加，各煤样的吸收光谱也存在不同。根据文献[17]可得，组成煤低分子化合物的主要官能团分别有：羟基、脂肪烃、芳香烃(Ar-CH)和含氧官能团(C-O-C、-COOH、-C=O和-OH)。通过Gaussian公式[18]分峰处理3种煤样的吸收光谱图，半定量表征各官能团的相对含量。Gaussian公式如下：
y = y 0 + A θ · e x p - 4 l n 2 ( x - x c ) 2 w 2 w · π 4 l n 2
式中：y为Kubelka-Munk变换;x为波数，cm-1；y0为基线;Aθ为峰面积;xc为峰中心位置;w为半峰宽。
3种煤样各波段的分峰拟合如图2—图5所示，对应的红外吸收振动区峰面积见表2。由图2—图5及表2可知：试验分析的3种煤样红外光谱中均含有常见的脂肪烃、芳香烃及含氧官能团。但随着煤阶的不同，官能团的种类及含量均有差别。煤的变质程度与煤分子中芳香烃结构有关，芳香烃含量越高，煤分子越稳定，越不易发生自燃[19]。芳香烃类主要包括取代苯、-C=C-和Ar-CH，不同变质程度煤样官能团相对含量及变化见表3和图6，由表3和图6可知：褐煤的芳香烃含量仅占13.74%，气煤占20.31%，而无烟煤56.66%，所以芳香烃的含量随着煤变质程度的增加而增加。含氧官能团主要分为C-O-C、-COOH、-C=O和-OH，是煤中最活泼的官能团，无烟煤中含氧官能团含量为16.20%，是3种煤样中含量最低的，气煤和褐煤分别为40.37%和46.68%，因此，相较之下，无烟煤不易与氧气发生自燃反应。脂肪烃中-CH3含量最高，其次是-CH2，2种官能团含量也随着变质程度的增加而增加。气煤和无烟煤中脂肪烃-CH3、-CH2-的变形振动和C-O伸缩振动的吸收强度与褐煤相比更弱，说明煤变质程度的增加使煤中侧链和某些含氧官能团呈减少趋势。在低变质程度的褐煤中，其侧链和活性官能团较多，因此，在受热过程中容易发生氧化反应。
3 煤变质程度对热解参数的影响
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特征温度是煤氧化过程中的关键热解参数，其变化特征对研究煤自燃过程的宏观特征变化具有理论指导作用。不同煤样的TG/微分热重分析(Derivative Thermogravimetry，DTG)曲线如图7—图9所示，各煤样的特征温度点见表4。由图7—图9和表4可知：随着煤变质程度的增加，特征温度也会随之升高，表明煤样的燃烧温度升高，煤样的燃烧温度越高，煤样越不易自燃。根据煤热解失重曲线的变化可将煤的燃烧过程划分为[20]:水分蒸发脱附、动态平衡、吸氧增重、受热分解、燃烧和燃尽6个不同阶段。
3种煤样的TG/DTG曲线如图10所示。由图10可知：随着煤变质程度的增加，其受热分解温度t4和燃尽温度t7均有所增加，使得TG/DTG曲线向右偏移，同时煤样最大失重速率对应温度也随之升高。煤的化学构造和组成成分因煤变质程度的不同而产生差异，通过第2节试验可得，煤化过程的加深导致芳香族化合物的比例上升、芳香层有序性提高，进而增强了煤样的热稳定性。临界温度t1越低意味煤氧复合加速过程越迅速，煤的自燃倾向性就越高，因此，褐煤相较于无烟煤具有更高的自燃倾向性；着火温度t5是煤样起火的温度，随煤化程度的增加，t5逐渐增大，表明煤样越不容易燃烧。此外，兴隆庄煤矿气煤在700 ℃后有一个小的失重峰，这可能由于煤中存在不稳定的矿物成份，此时发生热解。
4 微观结构与热解参数关联性分析
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煤自燃特性与其微观结构密切相关，同时特征温度反映煤的自燃进程，因此，煤自燃过程中的特征温度与微观基团之间必定存在某种关联。采用Pearson相关系数法[21]确定自燃过程中对特征温度影响最大的官能团，根据下式计算结果可准确反应出特征温度和微观基团之间的内在关系。
r = ∑ i = 1 n ( x i - x - ) ( y i - y - ) ∑ i = 1 n ( x i - x - ) 2 ∑ i = 1 n ( y i - y - ) 2
式中：r为相关系数；n为样本量；x和y为2个变量的观测值；xi、yi为变量x和y的第i个观测值；计算结果越接近1，表明该特征温度与某种官能团正相关性越强;越接近-1，则表明二者之间的负相关性越强。
微观基团与特征温度之间相关性如图11所示。由图11可知：煤样在氧化升温至燃烧过程中，各官能团与特征温度之间的相互关联存在差异，表明煤样在不同特征温度点下所参与的化学发应不同。在低温氧化阶段，与特征温度关联性强的官能团分别是:C-O-C、Ar-CH、-CH3和-CH2-、-OH。其中，t1~t5正相关性最强的官能团为芳香烃Ar-CH，关联系数越大，意味着这一官能团对此阶段的煤自燃过程影响最大，这是因为芳香烃控制煤的结构紧密度，引起特征温度点滞后使得煤自燃难以发生，因此，芳香烃含量越高，煤自燃的特征温度越高;t1~t5负相关性最强的官能团分别为：C-O-C、-CH3和-CH2-、-OH，表明在低温氧化阶段含氧官能团和脂肪烃的含量对氧化反应影响大，尤其是C-O-C越多、煤的特征温度越小，煤自燃倾向性越大。起火燃烧阶段t6~t7，-OH与特征温度的负关联性最大，表明在起火阶段，会消耗大量的-OH、-OH基团，该阶段的特征温度越低，起火危险性越大。
5 结论
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1) 随着煤样变质程度的增加，羟基及含氧官能团的占比逐渐降低，而脂肪烃和芳香烃的比例则不断上升。在低阶煤样中，含氧官能团的相对含量最多；在高阶煤样中，芳香族化合物的占比最大，超过了50%。
2) 随着煤样变质程度的增加，3种煤样的特征温度逐渐升高，热解失重进程开始滞后，TG和DTG曲线逐渐向高温区移动。
3) 根据Pearson相关系数计算结果，煤样在低温氧化过程中，Ar-CH与特征温度之间呈现最显著的正相关性，C-O-C、-OH与特征温度呈现最大的负相关性；在燃烧阶段，-OH与特征温度的负关联性最大。
4) 煤自燃的难易程度受芳香烃和含氧官能团的影响，芳香族化合物含量越多、含氧官能团含量越少，煤自燃越难发生。
基金
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  • 国家重点研发计划(2023YFF0615404)
  • 国家自然科学基金联合重点项目资助(U23B2093)
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2025年第35卷第2期
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doi: 10.16265/j.cnki.issn1003-3033.2025.02.0698
  • 接收时间：2024-09-13
  • 首发时间：2025-07-05
  • 出版时间：2025-02-28
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  • 收稿日期：2024-09-13
  • 修回日期：2024-11-22
基金
国家重点研发计划(2023YFF0615404)
国家自然科学基金联合重点项目资助(U23B2093)
作者信息
    中煤能源研究院有限责任公司，陕西 西安 710054

通讯作者:

**郭曦蔓(1998—)，女，甘肃兰州人，硕士，助理工程师，主要从事煤矿火灾防控与治理方面的研究。E-mail：。
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