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Article(id=1149735804496425595, tenantId=1146029695717560320, journalId=1146031787341344770, issueId=1149735800964825832, articleNumber=1003-3033(2024)11-0073-08, orderNo=null, doi=10.16265/j.cnki.issn1003-3033.2024.11.0678, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1717862400000, receivedDateStr=2024-06-09, revisedDate=1723564800000, revisedDateStr=2024-08-14, acceptedDate=null, acceptedDateStr=null, onlineDate=1752047976850, onlineDateStr=2025-07-09, pubDate=1732723200000, pubDateStr=2024-11-28, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1752047976850, onlineIssueDateStr=2025-07-09, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1752047976850, creator=13701087609, updateTime=1752047976850, updator=13701087609, issue=Issue{id=1149735800964825832, tenantId=1146029695717560320, journalId=1146031787341344770, year='2024', volume='34', issue='11', 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=1752047976008, creator=13701087609, updateTime=1756361988347, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1167830080236565470, tenantId=1146029695717560320, journalId=1146031787341344770, issueId=1149735800964825832, language=EN, specialIssueTitle=, coverIllustrator=, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1167830080236565471, tenantId=1146029695717560320, journalId=1146031787341344770, issueId=1149735800964825832, language=CN, specialIssueTitle=, coverIllustrator=, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=73, endPage=80, ext={EN=ArticleExt(id=1149735804718723708, articleId=1149735804496425595, tenantId=1146029695717560320, journalId=1146031787341344770, language=EN, title=Characteristics of gas desorption energy change after liquid CO2 treatment at high temperature point in goaf, columnId=1149733269173878863, journalTitle=China Safety Science Journal, columnName=Safety engineering technology, runingTitle=null, highlight=null, articleAbstract=

In order to study the effect of liquid CO2 injection on coal spontaneous combustion heat production and gas release in the gob with high gas content and easy spontaneous combustion，the gas desorption test system was composed of a self-made variable temperature chamber and desorption instrument to simulate the influence of liquid CO2 injected into a high-temperature point of gob on coal sample temperature and coal gas desorption amount and analyze the change of gas desorption energy of coal sample under corresponding coal body gas pressure and different temperature during the process of "falling to rising" temperature change. The results show that the temperature of the coal sample will stabilize at a lower level，and the gas will stop desorbing within 60 minutes to 100 minutes after the liquid CO2 is injected. After 100 minutes，the cold energy gradually runs out，and the coal continues to oxidize and heat up，and the gas resumes desorbing with an increasing desorption rate. The cold energy released by the liquefied CO2 gasification and the CO2 gas has an excellent inhibitory effect on reducing coal temperature and gas desorption. When the coal sample temperature is between 10 and 30 ℃，the coal is in a low energy state. In this temperature range，the internal coal is more likely to cause the adsorption heat value to stabilize. The decrease in the surface free energy of the coal body will also present a stable trend.

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为研究在高瓦斯易自燃煤层采空区内注入液态CO2后，其对抑制煤自燃产热和瓦斯释放的效果，利用自制的变温腔体、解吸仪器等装置组成瓦斯解吸测试系统，模拟液态CO2注入采空区高温点后对煤样温度和煤瓦斯解吸量的影响，分析降-升温变化过程中煤样在相应煤体瓦斯压力及不同温度下的瓦斯解吸能量变化特性。结果表明：煤样在注入液态CO2后的60~100 min内温度会降至稳定，瓦斯也停止解吸；100 min后冷量逐渐耗尽，煤继续氧化升温，煤瓦斯也恢复解吸，且解吸量以较快速度上升；液态CO2气化释放的冷量和CO2气体对煤体降温和瓦斯解吸具有良好抑制作用；当煤样温度处于10~30 ℃时，煤呈现低能量状态，且在该温度区间内进行解吸，煤内部更易使吸附热值趋向于平衡，煤体表面自由能降低值也会呈现平稳态势。

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鲁义(1986—)，男，江西新干人，博士，教授，博士生导师，主要从事火灾科学与技术方面的研究。E-mail：。

王俏，讲师

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鲁义(1986—)，男，江西新干人，博士，教授，博士生导师，主要从事火灾科学与技术方面的研究。E-mail：。

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鲁义(1986—)，男，江西新干人，博士，教授，博士生导师，主要从事火灾科学与技术方面的研究。E-mail：。

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王俏，讲师

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王俏，讲师

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采空区高温点液态CO2处理后瓦斯解吸能量变化特性
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鲁义 1 , 颜晴琼 1 , 王俏 1 , 丁仰卫 2 , 史正景 3 , 谷旺鑫 1
中国安全科学学报 | 安全工程技术 2024,34(11): 73-80
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中国安全科学学报 | 安全工程技术 2024, 34(11): 73-80
采空区高温点液态CO2处理后瓦斯解吸能量变化特性
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鲁义1 , 颜晴琼1, 王俏1, 丁仰卫2, 史正景3, 谷旺鑫1
作者信息
  • 1 湖南科技大学 资源环境与安全工程学院，湖南 湘潭 411201
  • 2 山东鲁泰控股集团有限公司鹿洼煤矿，山东 济宁 272004
  • 3 中煤新集能源股份有限公司 技术中心，安徽 淮南 232000

    • 鲁义(1986—)，男，江西新干人，博士，教授，博士生导师，主要从事火灾科学与技术方面的研究。E-mail：。

    王俏，讲师

Characteristics of gas desorption energy change after liquid CO2 treatment at high temperature point in goaf
Yi LU1 , Qingqiong YAN1, Qiao WANG1, Yangwei DING2, Zhengjing SHI3, Wangxin GU1
Affiliations
  • 1 School of Resource & Environment and Safety Engineering，Hunan University of Science and Technology，Xiangtan Hunan 411100，China
  • 2 Luwa Coal Mine，Shangdong Lutai Hold Group Co.，Ltd.，Jining Shandong 272004，China
  • 3 Technical Center，China Coal Xinji Energy Co.，Ltd.，Huainan Anhui 232000，China
出版时间: 2024-11-28 doi: 10.16265/j.cnki.issn1003-3033.2024.11.0678
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摘要
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为研究在高瓦斯易自燃煤层采空区内注入液态CO2后，其对抑制煤自燃产热和瓦斯释放的效果，利用自制的变温腔体、解吸仪器等装置组成瓦斯解吸测试系统，模拟液态CO2注入采空区高温点后对煤样温度和煤瓦斯解吸量的影响，分析降-升温变化过程中煤样在相应煤体瓦斯压力及不同温度下的瓦斯解吸能量变化特性。结果表明：煤样在注入液态CO2后的60~100 min内温度会降至稳定，瓦斯也停止解吸；100 min后冷量逐渐耗尽，煤继续氧化升温，煤瓦斯也恢复解吸，且解吸量以较快速度上升；液态CO2气化释放的冷量和CO2气体对煤体降温和瓦斯解吸具有良好抑制作用；当煤样温度处于10~30 ℃时，煤呈现低能量状态，且在该温度区间内进行解吸，煤内部更易使吸附热值趋向于平衡，煤体表面自由能降低值也会呈现平稳态势。

采空区  /  高温点  /  液态CO2  /  瓦斯解吸  /  吸附热  /  表面自由能

In order to study the effect of liquid CO2 injection on coal spontaneous combustion heat production and gas release in the gob with high gas content and easy spontaneous combustion，the gas desorption test system was composed of a self-made variable temperature chamber and desorption instrument to simulate the influence of liquid CO2 injected into a high-temperature point of gob on coal sample temperature and coal gas desorption amount and analyze the change of gas desorption energy of coal sample under corresponding coal body gas pressure and different temperature during the process of "falling to rising" temperature change. The results show that the temperature of the coal sample will stabilize at a lower level，and the gas will stop desorbing within 60 minutes to 100 minutes after the liquid CO2 is injected. After 100 minutes，the cold energy gradually runs out，and the coal continues to oxidize and heat up，and the gas resumes desorbing with an increasing desorption rate. The cold energy released by the liquefied CO2 gasification and the CO2 gas has an excellent inhibitory effect on reducing coal temperature and gas desorption. When the coal sample temperature is between 10 and 30 ℃，the coal is in a low energy state. In this temperature range，the internal coal is more likely to cause the adsorption heat value to stabilize. The decrease in the surface free energy of the coal body will also present a stable trend.

goaf  /  high temperature point  /  liquid CO2  /  gas desorption  /  heat of adsorption  /  surface free energy
鲁义, 颜晴琼, 王俏, 丁仰卫, 史正景, 谷旺鑫. 采空区高温点液态CO2处理后瓦斯解吸能量变化特性. 中国安全科学学报, 2024 , 34 (11) : 73 -80 . DOI: 10.16265/j.cnki.issn1003-3033.2024.11.0678
Yi LU, Qingqiong YAN, Qiao WANG, Yangwei DING, Zhengjing SHI, Wangxin GU. Characteristics of gas desorption energy change after liquid CO2 treatment at high temperature point in goaf[J]. China Safety Science Journal, 2024 , 34 (11) : 73 -80 . DOI: 10.16265/j.cnki.issn1003-3033.2024.11.0678
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0 引言
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受遗煤和垮落岩石的影响，矿井采空区内部易产生复杂且动态变化的冒落空间及次生裂隙，形成多种可燃气体共存的状态[1]。当采空区内遗煤氧化升温至47.3~102.5℃时，热源附近出现瓦斯积聚现象，导致综采面瓦斯涌出量增加，扩大瓦斯爆炸范围[2];当环境温度达650~750℃时，适当条件下积聚的瓦斯会被引爆，并沿富氧通道蔓延到综采面，形成耦合事故[3]。因此，同时抑制采空区内煤体升温和煤瓦斯积聚对防治瓦斯与煤自燃共生灾害具有重要意义。
众学者为达到消灭热源和降低瓦斯体积分数的双重目标，有利用泡沫、稠化浆体、凝胶等防灭火材料，动态隔离防治采空区高温点与瓦斯爆炸[4-5];另外，还有利用液态N2、CO2降低煤体发热量和煤瓦斯体积分数[6]进行防治。液态CO2因具有降温、惰化及抑爆等优点被广泛使用[7]，其对煤瓦斯爆炸极限和氧化反应的影响也被深入探究，如CAO Naifu等[8]分析了液态CO2的相变及扩散运移特征，探讨了其对高温煤体的冷却影响；BENEDETTO等[9]测试研究了液态CO2对瓦斯爆炸峰值压力、临界氧气体积分数和层流燃烧速度的惰化效果。
这些研究分别揭示了液态CO2抑制煤温和瓦斯爆炸的作用，但未深入探讨液态CO2如何持续防治煤自燃和瓦斯共生灾害。基于此，笔者拟利用自制的瓦斯解吸测试系统，分析液态CO2对煤体升温速率和煤瓦斯解吸的影响，研究解吸过程中的能量变化特性，以期得出抑制煤自然产热与瓦斯释放的温度条件，为矿井采空区工程灾害防治提供理论依据。
1 瓦斯解吸模拟测试系统
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1.1 煤样制备
从山东鲁泰控股集团有限公司鹿洼煤矿中取新鲜煤样，按《煤样的制备方法》(GB474—2008)破碎和筛分后，制备成粒径为60~80目的煤粉，随后利用图1所示模具制成型煤。
1.2 测试系统及步骤
自制煤瓦斯解吸模拟测试系统，如图2所示，该装置由吸附平衡、解吸测定、抽真空、控温和数据收集等单元组成。
测试步骤如下：①真空脱气；②吸附平衡：煤样罐被高压气源充气至最大吸附压力值(0.5、1.0、1.5、2.0MPa)后保持3h不变至充分吸附平衡状态；③注入冷量：当充入瓦斯压力达到0.5MPa时，利用冷气管注入2kg液态CO2。基于热传导理论，得出煤体导热速率和瓦斯解吸发热率。再控制加热板模拟煤自身产热量，在10℃下充分解吸平衡后再依次升温至30、50和70℃。煤样在这些温度点下充分解吸后进行重启，再将压力分别升到1、1.5和2.0MPa，重复步骤③;④数据采集：记录煤表面温度值、煤瓦斯解吸量及压力变化数据。
2 瓦斯解吸能量变化特性试验分析
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2.1 煤体瓦斯压力对瓦斯解吸特性的影响
液态CO2在不同煤体瓦斯压力条件下对煤体温度和瓦斯解吸量的影响如图3所示。
可以看出，解吸过程中前60min内煤温快速下降，瓦斯持续被较快解吸。随后40min内，煤样降温趋于稳定，瓦斯停止解吸，解吸量保持不变。经过100min后，煤温迅速上升，解吸得到恢复。当加热温度达到70℃时，无论瓦斯压力的变化，煤温在冷却温度(低于0℃)维持的时间最短，140 ~150min后便开始升温，比30℃时稳定时长低43%。表明：在相同加热条件下瓦斯压力的增加，瓦斯的解吸量呈逐渐增加的趋势；且不同煤体瓦斯压力对煤样温度有一定的影响，但其影响程度相对较小。
2.2 煤样温度对瓦斯解吸特性的影响
图4表示煤样温度对瓦斯解吸能量变化特性的影响(p为压力，MPa)。在初始解吸的前1min内，瓦斯解吸速率急剧下降，而瓦斯累计解吸量急剧增加，接着持续一段时间暂停解吸。升至一定温度时，瓦斯解吸量突增，解吸速率也随着煤温升高而加快。
同时，温度升高会使瓦斯重新解吸的时间缩短，也会使瓦斯解吸速率更高，解吸量的增加速度更迅速。升温阶段较降温阶段相比，煤瓦斯解吸量会呈现显著的差异，但在高温条件下，瓦斯解吸速率在迅速增加后开始逐渐减小。
2.3 煤样瓦斯解吸过程能量变化特性
2.3.1 解吸过程中吸附热变化特性
运用 Clausius-Clapeyron方程，在特定吸附量n下，等温吸附热 q s t可以表示为[10]:
d l n f d T = q s t R T 2
根据文献[11-12]，得出逸度f和压力p的符合关系式f=pZ，其中，Z为压缩因子；利用 q s t=-RB和吸附量n，得lnf-n的关系式，其中，R=8.314 J/(mol·K)，为气体常数；B为lnf-1/T的线性拟合关系的斜率，其中，T为绝对温度，K，文中取273.15+θ(θ为煤样温度，℃);绘制等温吸附线后，利用lnf-1/T的线性关系，得出煤的等量和等温吸附量的良好线性关系。Z通过Factuer 得到[11]。
根据式(1)计算得出液态CO2作用前后不同煤体瓦斯压力对解吸过程吸附曲线的影响，如图5所示。发现随着加热温度和瓦斯压力的上升，煤样第1次降低到-20℃时解吸量与煤样第2次升高到-20℃时相比都有较低增幅。这是由于在升温过程中瓦斯分子在加热的影响下，更易成为游离态。随着吸附压力增加，瓦斯分子间相互作用力增大，吸附态瓦斯分子与游离态瓦斯分子之间进行了引力叠加，使游离态瓦斯分子解吸时会释放更多热量。
2.3.2 解吸过程表面自由能变化特性
根据表面化学理论得出表面自由能变化值Δγ为[13]:
Δ γ = V L   R T V 0 S   l n 1 + p p L
式中：VL为Langmuir体积，cm3/g;V0为标准状态条件下气体的摩尔体积，22.4×103 cm3/mol; S为煤比表面积，m2/g;pL为Langmuir压力，MPa。
通过对式(2)进行微分，得各个压力点表面自由能变化值Δγp为：
Δ γ p = V L R T ( p + p L ) V 0   S
根据式(2)和式(3)计算不同加热温度和瓦斯压力条件下，煤的表面自由能总降低值及各压力点表面自由能降低值，结果如图6、图7所示。
图6、图7反映了液态CO2对煤表面能自由能的总降低值和各压力点降低值的影响。温度稳定时，压力与煤表面自由能总降低值呈正相关，与各压力点降低值呈负相关。煤样受液态CO2吸热降温影响，游离态瓦斯分子因热量散失内能减小，动能降低，运动减慢，煤体高势能位点更容易吸附瓦斯分子，导致煤表面自由能显著下降。当已被占据的吸附位点数量达到饱和状态时，建立新的煤体表面自由能平衡状态，此时表现为解吸过程停止。
当冷量耗尽，煤受热继续升温，瓦斯分子的内能和动能增加，使吸附在煤体上的瓦斯分子挣脱范德华力的束缚，煤体表面自由能平衡被打破，导致吸附在煤中的瓦斯分子逐渐解吸。此时，宏观表现为恢复解吸。
每千克液态CO2气化后体积约为0.56m3，2种物理状态下的吸热量差距为45~65 K[14]。因此，液态CO2气化后也会影响煤瓦斯解吸能力。针对气化后对煤的表面自由能降低值及各压力点表面自由能降低值的变化再进行探讨，得出结果如图8所示。
由图8可知：温度为10~30℃时，处于累计表面自由能降低值和各压力点表面自由能降低值升降缓慢的阶段。此时，解吸与吸附过程中的等量吸附热相互匹配，煤基质表面瓦斯分子间的相互作用力达到了平衡状态，使吸附热值趋向于平衡，煤表面自由能维持着相对稳定，导致该温度区间内煤瓦斯解吸能力较其他温度条件下也会减弱。
2.4 现场应用及效果
鹿洼煤矿6301工作面为3煤层开采，部分开采区域位于4301采空区下方；2个工作面层位重叠关系及开采时裂隙发育情况如图9所示。
开采推进至4301采空区下方时，将揭露采空区内落差大于3m的断层，并诱使顶板煤岩应力重新分布，导致裂隙发育较完全。随后，氧气通过裂隙对上覆采空区内遗煤进行氧化形成高温点，同时，也易引发采空区内积存的瓦斯发生爆炸。
发现自然发火征兆后，向封闭的采空区高温点处大流量灌注液态CO2，从而抑制出现煤体升温和煤瓦斯积聚现象，灌注工艺流程及应用效果如图10所示。
其中降低煤体温度及抑制瓦斯爆炸的灌注量为[14]:
Q = α V ( τ 1 - τ 2 ) + 2 Δ t Q 0 ( τ 0 - τ 2 ) Δ t τ 2
式中：Q为注入火区内CO2强度，m3 /h;α为富裕系数，1.2~ 1.5;V为封闭区域内的体积，m3;τ1为火区内初期氧气平均体积分数，14%;τ2为火区内灭火临界氧气体积分数，3%~5%;Q0为火区漏风量，m3/h; Δ t为CO2的预计注入时间，h;τ0为火区周边巷道空气中的氧体积分数，20%。其中封闭火区空间总体积V为：
V = V 1 + V 2 + L 1 H L 2 λ
式中：V1为工作面密闭体积，m3;V2为巷道封闭体积，m3;L1为采空区走向长度，m;H为煤层厚度，m;L2为采空区倾向长度，m;λ为顶板岩石垮落碎胀系数的取值，1.1~1.3。
封闭火区总容积为514 608 m3，此时所需的CO2气体总量为144 090.24 m3，1t液态CO2转换成气体时的体积为560m3，理论上所需液态CO2约为257t，即需要约234m3的液态CO2。据式 (4) 计算需连续注入225h，既当液态CO2以1.14 t/h的注入量进入采空区高温点后，能达到稳定防治煤自燃和瓦斯共生灾害的目的。
利用气体和温度传感器，实时监测数据并绘制变化曲线，如图11所示。
由图11可知：随着液态CO2的注入采空区内温度由78℃降至57℃，在持续注入10天后，温度稳定在22℃;煤温的降低也抑制了采空区内遗煤和原始煤层中瓦斯的继续解吸释放，使瓦斯体积分数由1.18%降至0.68%后稳定在0.1%左右；使采空区高温点处的煤体温度和瓦斯含量得到有效抑制。
3 结论
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1) 煤瓦斯解吸过程受高温影响显著，在较低温度时，瓦斯解吸量和解吸速率差异不明显；但在高温情况下，会使瓦斯解吸量更高，解吸量的增加速度更快。
2) 温度处于10~30℃时，煤瓦斯解吸过程较其他温度区间内更易使煤基质表面的相互作用力达到稳定，促使解吸过程中和吸附过程中的等量吸附热相互等值，煤体表面自由能也维持平衡。
3) 在现场持续注入液态CO2后，采空区内遗煤和原始煤层中煤自燃和瓦斯解吸都能得到抑制，煤温和瓦斯体积分数会稳定在22℃和0.1%左右，说明液态CO2能有效抑制采空区煤氧化自燃的同时阻止产生瓦斯积聚。
基金
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  • 国家自然科学基金(52174180)
  • 湖南省杰出青年科学基金(2022JJ10026)
  • 国家重大人才工程青年项目(2022QB06801)
文献
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2024年第34卷第11期
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文章信息
doi: 10.16265/j.cnki.issn1003-3033.2024.11.0678
  • 接收时间：2024-06-09
  • 首发时间：2025-07-09
  • 出版时间：2024-11-28
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出版历史
  • 收稿日期：2024-06-09
  • 修回日期：2024-08-14
基金
国家自然科学基金(52174180)
湖南省杰出青年科学基金(2022JJ10026)
国家重大人才工程青年项目(2022QB06801)
作者信息
    1 湖南科技大学 资源环境与安全工程学院，湖南 湘潭 411201
    2 山东鲁泰控股集团有限公司鹿洼煤矿，山东 济宁 272004
    3 中煤新集能源股份有限公司 技术中心，安徽 淮南 232000
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https://castjournals.cast.org.cn/joweb/zgaqkxxb/CN/10.16265/j.cnki.issn1003-3033.2024.11.0678
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