富油煤经中低温热解可以获得焦油和煤气，是一种集煤、油、气属性于一体的矿产资源，对减缓我国油气资源对外依存度具有重要意义。富油煤热解流体运移析出依赖于煤体孔隙结构在加热过程中的演变。开展富油煤热解过程中孔隙结构演化规律研究有助于深化热解流体运移和析出行为的认识。本研究以鄂尔多斯盆地延安组富油煤为研究对象，利用管式马弗炉在氮气气氛下进行热解实验，得到不同温度热处理残煤样品。通过体视、光学和扫描电子显微镜、低场核磁共振、低温氮气吸附等测试方法对热解过程中煤样孔隙结构（开放孔隙和封闭孔隙）的表面形貌以及演化特征进行了深入研究，结合热重分析、X射线衍射、红外光谱和¹³C核磁共振手段揭示了孔隙演化的微观机制。

研究发现：（1）煤体孔隙热演化呈现3个阶段：30-300℃时微孔占据主体地位，此阶段煤样不同组分由于热膨胀差异性产生水平及垂直裂隙；300-500℃时大量热解产物生成及逸出导致中大孔占比逐步升高，煤基质的流变性增强，且孔隙之间出现合并现象；>500℃时孔径整体增大，此阶段煤基质的收缩性明显增强，还出现大孔中发育小孔的现象。此外孔隙分形维数在热解过程中先降低后增加，分别对应热解孔隙生长合并和孔隙嵌套演化两个过程。（2）不同手段测得的封闭孔隙与开放孔隙的协同演化不一致。低温氮气吸附法测得2-50nm孔隙得出封闭孔随温度的演化规律与开放孔一致，表现为随着温度的升高均逐渐降低，500℃时达到最低，700℃时急剧增加。低场核磁共振法测得<450nm孔隙发现该孔径范围内封闭孔随温度的升高逐渐增多，而开放孔则是先减小后增大。（3）煤样在热解过程中孔隙结构的演化受控于大分子结构，剧烈热分解阶段孔隙结构的演化受控于脂肪结构，含氧结构次之。随着脂肪结构和含氧结构的减小，微孔占比减小，大孔占比增大。而热缩聚阶段孔隙的演化则与芳香结构密不可分。随着芳香环之间的不断缩合，芳香层片堆叠度和延展度增大，导致微孔占比升高，大孔占比降低。

Tar-rich coal can gain tar and gas through medium and low temperature pyrolysis, which is a special mineral resource combining coal, oil and gas properties, and has great significance for reducing China's external dependence on oil and gas resources. The pyrolysis fluids produced by the pyrolysis of tar-rich coals transport and precipitate through channels such as pores. Therefore, the evolution of the pore structure largely influences the transport and precipitation behaviour of the pyrolysis fluids. Moreover, it may even enhance the secondary reaction of the pyrolysis fluid in the temperature field, affecting the yield of the pyrolysis fluid. Therefore, the study of the pore structure evolution during the tar-rich coal pyrolysis process can help to deepen the understanding of the transport and precipitation characteristics of the pyrolysis fluid during the tar-rich coal pyrolysis process.

In this study, using the tar-rich coal of the Yan'an Formation in the Ordos Basin as the research object, and pyrolysis experiments were carried out using a tube muffle furnace under an N₂ atmosphere to obtain thermal treatment coal samples at different temperatures. The surface morphology and evolutionary characteristics of the pore structure (open and closed pores) of the coal samples during pyrolysis were investigated in depth using body vision microscopy, optical microscopy and scanning electron microscopy, low-field NMR, low-temperature nitrogen adsorption, thermogravimetric analysis, X-ray diffraction, Fourier transform infrared spectroscopy and ¹³C-NMR, revealing the microscopic mechanisms of pore evolution.

The main conclusions include: (1) the thermal evolution of the pores in the coal matrix exhibited three stages: 30-300°C, the micropores occupied the dominant position, and at this stage the different components of the coal sample produced horizontal and vertical fractures due to the difference in thermal expansion. 300-500°C, a large number of pyrolysis products were generated and escaped leading to the gradual increase the ratio of mesopores and macropores, the rheology of the coal matrix was enhanced, and the coalescence between pores appeared. >500°C, where the pore size increased overall. The shrinkage of the coal matrix enhanced significantly at this stage, and the development of small pores within large pores occurred. In addition, the pore fractal dimension decreased and then increased during the pyrolysis process, corresponding to the two processes of pyrolysis pore growth and coalescence and pore nesting evolution, respectively. (2) The synergistic evolution of closed and open pores was not consistent based on the different methods measured. Pore size of 2-50 nm pores measured by low-temperature nitrogen adsorption showed that the evolution of closed pores with temperature was consistent with that of open pores, showing a gradual decrease in closed pores with increasing temperature, reaching a minimum at 500°C and a sharp increase at 700°C. The pore size of <450 nm pores measured by low-field NMR showed a gradual increase in closed pores with increasing temperature, open pores were consistent with the evolution of the pore structure measured by low-temperature nitrogen adsorption. (3) The evolution of the coal pore structure during pyrolysis was controlled by the macromolecular structure. During the violent thermal decomposition stages, the evolution of the pore structure was controlled by aliphatic structure, followed by the oxygenated structure. As the aliphatic and oxygenated structures decreased, the ratio of micropores decreased and the ratio of macropores increased. During the thermal polycondensation stage, the evolution of the pore structure was closely linked to the aromatic structure. As the aromatic rings continue to condense with each other, the aromatic lamellae increased in stacking and ductility, resulting in a higher ratio of micropores and a lower ratio of macropores.

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