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煤系页岩瓦斯吸附−解吸迟滞效应核磁共振谱实验研究

唐巨鹏 田虎楠 潘一山

唐巨鹏, 田虎楠, 潘一山. 煤系页岩瓦斯吸附−解吸迟滞效应核磁共振谱实验研究. 力学学报, 2021, 53(8): 2193-2204 doi: 10.6052/0459-1879-21-264
引用本文: 唐巨鹏, 田虎楠, 潘一山. 煤系页岩瓦斯吸附−解吸迟滞效应核磁共振谱实验研究. 力学学报, 2021, 53(8): 2193-2204 doi: 10.6052/0459-1879-21-264
Tang Jupeng, Tian Hunan, Pan Yishan. Experiment of adsorption-desorption hystersis of gas in coal shale by using nuclear magnetic resonance spectrums. Chinese Journal of Theoretical and Applied Mechanics, 2021, 53(8): 2193-2204 doi: 10.6052/0459-1879-21-264
Citation: Tang Jupeng, Tian Hunan, Pan Yishan. Experiment of adsorption-desorption hystersis of gas in coal shale by using nuclear magnetic resonance spectrums. Chinese Journal of Theoretical and Applied Mechanics, 2021, 53(8): 2193-2204 doi: 10.6052/0459-1879-21-264

煤系页岩瓦斯吸附−解吸迟滞效应核磁共振谱实验研究

doi: 10.6052/0459-1879-21-264
基金项目: 国家自然科学基金面上项目(51874165)和辽宁省兴辽英才计划项目(XLYC1902106)资助
详细信息
    作者简介:

    田虎楠, 博士研究生, 主要研究方向: 煤系页岩瓦斯开采理论及相关实验研究. E-mail: tangjupeng@lntu.edu.cn

  • 中图分类号: TE327

EXPERIMENT OF ADSORPTION-DESORPTION HYSTERSIS OF GAS IN COAL SHALE BY USING NUCLEAR MAGNETIC RESONANCE SPECTRUMS

  • 摘要: 煤系页岩瓦斯主要以吸附态和游离态形式存在, 其解吸过程相对吸附过程具有普遍滞后现象, 因此从微细观角度定量研究其吸附−附解吸迟滞规律对页岩气井后期稳产增产具有重要意义. 在前人研究基础上结合核磁共振谱理论推导出能够准确表征煤系页岩瓦斯吸附−解吸迟滞效应微细观评价模型, 并采用核磁共振谱测试技术, 以双鸭山盆地东保卫煤矿三采区36# 煤层底板煤系页岩为研究对象, 进行煤系页岩瓦斯吸附−解吸迟滞效应核磁共振谱实验, 模拟不同储层原位应力状态煤系页岩瓦斯迟滞效应发生全过程, 进一步对吸附态瓦斯、游离态瓦斯以及微细观方法测定的宏观瓦斯迟滞规律进行定量化研究, 并对其发生机理以及其对深部煤系页岩瓦斯开采影响进行了初步探究. 结果表明: 应力状态下吸附态和游离瓦斯均有滞后效应; 瓦斯宏观迟滞系数与平均有效应力呈幂函数关系, 而瓦斯宏观迟滞效应中由吸附态或游离态瓦斯引起的迟滞系数与平均有效应力关系均可采用二次多项式拟合; 孔裂隙应力损伤和微孔隙瓦斯扩散受限耦合或许是煤系页岩瓦斯吸附−解吸迟滞效应产生根本原因之一.

     

  • 图  1  吸附−解吸迟滞效应示意图

    Figure  1.  Schematic diagram of adsorption-desorption hysteresis

    图  2  迟滞评价模型示意图

    Figure  2.  Schematic diagram of hysteresis model

    图  3  煤系页岩瓦斯吸附−解吸迟滞效应现场实验

    Figure  3.  Field experiment on hysteresis effect of gas adsorption-desorption in coal shale

    图  4  煤系页岩瓦斯吸附−解吸迟滞效应实验装置连接示意图

    Figure  4.  Connection diagram of gas adsorption-desorption hysteresis effect experiment device for coal shale

    图  5  自由态瓦斯T2

    Figure  5.  T2 spectrum of free gas

    图  6  吸附过程T2

    Figure  6.  T2 spectrum of shale gas adsorption

    图  7  解吸过程T2

    Figure  7.  T2 spectrum of shale gas desorption

    图  8  吸附态瓦斯迟滞效应评价模型

    Figure  8.  Evaluation model for hysteresis effect of adsorbed gas

    图  9  游离态瓦斯迟滞效应评价模型

    Figure  9.  Evaluation model for hysteresis effect of porous medium-confined gas

    图  10  瓦斯迟滞系数与平均有效应力关系

    Figure  10.  Relationship between hysteresis index of gas and average effective stress

    表  1  迟滞效应宏观定量评价指标

    Table  1.   Macro quantitative evaluation index of hysteresis

    Evaluation indexFormulaParameterReference
    Freundlich${S_{{\rm{ad}}}} = {K_{{\rm{ad}}}}{C_{{\rm{ad}}}}^{1/{n_{{\rm{ad}}}}}$,
    ${S_{{\rm{de}}}} = {K_{{\rm{de}}}}{C_{{\rm{de}}}}^{1/{n_{{\rm{de}}}}}$,
    $HI = \dfrac{{{n_{{\rm{de}}}}}}{{{n_{{\rm{ad}}}}}}$
    ${S_{{\rm{ad}}}}$—equilibrium concentration of solid phase adsorption
    ${S_{{\rm{de}}}}$—equilibrium concentration of solid phase desorption
    K—adsorption parameter
    C—equilibrium concentration of adsorbent
    ${n_{{\rm{ad}}}}$—Freundlich adsorption index
    ${n_{{\rm{de}}}}$ —Freundlich desorption index
    [21-22]
    slope$HI = \dfrac{{{f_{{\rm{ad}}}}^\prime (C) - {f_{{\rm{de}}}}^\prime (C)}}{{{f_{{\rm{ad}}}}^\prime (C)}}$${f_{{\rm{ad}}}}^\prime (C)$, ${f_{{\rm{de}}}}^\prime (C)$—first derivative of characteristic equation[23]
    solid phase concentration$HI = \dfrac{{\max ({S_{{\rm{de}}}} - {S_{{\rm{ad}}}})}}{{{S_{{\rm{ad}}}}}}$,
    $HI = {\left. {\dfrac{{\max ({S_{{\rm{de}}}} - {S_{{\rm{ad}}}})}}{{{S_{{\rm{ad}}}}}}} \right|_{T,C}}$
    ${S_{{\rm{ad}}}}$—equilibrium concentration of solid phase adsorption
    ${S_{{\rm{de}}}}$—equilibrium concentration of solid phase desorption
    C—equilibrium concentration of adsorbent
    T—test temperature
    [24]
    area$HI = 100\left(\dfrac{{{A_{{\rm{de}}}} - {A_{{\rm{ad}}}}}}{{{A_{{\rm{ad}}}}}}\right)$${A_{{\rm{de}}}}$—area under desorption curve
    ${A_{{\rm{ad}}}}$—area under adsorption curve
    [25]
    下载: 导出CSV

    表  2  页岩特征参数

    Table  2.   Shale characteristic parameters

    Nameρ/(g·cm−3)φ/%σbc/MPaE/GPa
    shale2.431.6 ~ 5.03.0 ~ 18.713.5
    下载: 导出CSV

    表  3  自由态瓦斯核磁共振谱特性实验方案

    Table  3.   Experiment of free gas by NMR spectrums

    No.Confining
    pressure
    /MPa
    Axial
    pressure
    /MPa
    Pore
    pressure
    /MPa
    11.792.131.35
    23.093.542.46
    34.034.933.52
    44.995.714.43
    56.026.465.44
    67.017.566.50
    78.899.418.29
    下载: 导出CSV

    表  4  吸附过程核磁共振谱实验方案

    Table  4.   Experimental adsorption of gas by NMR spectrums

    No.Confining
    pressure
    /MPa
    Axial
    pressure
    /MPa
    Pore
    pressure
    /MPa
    11.782.241.31
    22.973.612.24
    34.044.473.37
    45.025.434.39
    56.026.445.65
    67.017.456.33
    78.799.347.89
    下载: 导出CSV

    表  5  解吸过程核磁共振谱实验方案

    Table  5.   Experimental desorption of gas by NMR spectrums

    No.Confining
    pressure
    /MPa
    Axial
    pressure
    /MPa
    Pore
    pressure
    /MPa
    18.799.347.89
    27.498.186.94
    36.547.235.76
    45.476.244.48
    54.525.153.41
    63.514.162.40
    72.493.251.41
    80.951.470.40
    下载: 导出CSV

    表  6  常用吸附模型

    Table  6.   Common adsorption models

    ModelModel expressionAdsorption R2
    L $V = P{V_{\rm{L}}}/({P_{\rm{L}}} + P)$ 0.80002
    F $V = {K_{\rm{b}}}{P^m}$ 0.93634
    E-L $V = {K_{\rm{b}}}P{V_{\rm{L}}}/(1 + {K_{\rm{b}}}P + m\sqrt {{K_{\rm{b}}}P} )$ 0.99038
    T $V = {K_{\rm{b}}}P{V_{\rm{L}}}/{[1 + {({K_{\rm{b}}}P)^m}]^{1/m}}$ 0.75002
    B-BET $V = \dfrac{{{V_{\rm{m}}}CP}}{{({P^0} - P)[1 + (C - 1)(P/{P^0})]}}$ 0.76401
    T-BET $V = \dfrac{{{V_{\rm{m}}}CP[1 - (n - 1)(P/{P^0}) + n{{(P/{P^0})}^{n + 1}}]}}{{({P^0} - P)[1 + (C - 1)(P/{P^0}) - C{{(P/{P^0})}^{n + 1}}]}}$ 0.93211
    D-R $V = {V_0}\exp [ - D{\ln ^2}({P^0}/P)]$ 0.99475
    D-A $V = {V_0}\exp [ - D{\ln ^m}({P^0}/P)]$ 0.56960
    注: PL—Langmuir压力, MPa; VL—Langmuir体积, cm3/g; Vm—单层极限吸附量, cm3/g; P0—饱和蒸汽压力, MPa; C—吸附热常数; V0—最大吸附量, cm3/g; Kb—吸附经验常数; m—吸附剂非均质参数; n—模型参数; D—净吸附热常数.
    Notes: PL—Langmuir pressure, MPa; VL—Langmuir volume, cm3/g; Vm—monolayer limit adsorption capacity, cm3/g; P0—saturated steam pressure, MPa; C—adsorption heat constant; V0—maximum adsorption capacity, cm3/g; Kb—adsorption empirical constant; m—adsorbent heterogeneity parameters; n—model parameter; D—final adsorption heat constant.
    下载: 导出CSV

    表  7  常用解吸模型

    Table  7.   Common desorption models

    ModelModel expressionDesorption R2
    Weibull $V = {V_0}[1 - \exp ( - b{p^q})]$ 0.99660
    desorption function $V = \dfrac{{abp}}{{1 + bp}} + c$ 0.97953
    注: a—煤系页岩最大吸附量, cm3/g; b—吸附热、吸附速度与解吸速度综合函数, MPa−1; c—残余吸附量, cm3/g; V0—最大吸附量, cm3/g; b—吸附热常数; q—吸附质在孔隙表面的占位比.
    Notes: a—maximum adsorption capacity of coal shale, cm3/g; b—comprehensive function of adsorption heat, adsorption rate and desorption rate, MPa−1; c—residual adsorption capacity, cm3/g; V0—maximum adsorption capacity, cm3/g; b—adsorption heat constant; q—occupation ratio of adsorbate on pore surface.
    下载: 导出CSV
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  • 收稿日期:  2021-06-13
  • 录用日期:  2021-08-03
  • 网络出版日期:  2021-08-04
  • 刊出日期:  2021-08-18

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