Evolutionary Characteristics of Pore Structure for Over-Matured Shales in Semi-Closed Thermal Simulation Experiment
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摘要: 为研究过熟页岩孔隙结构的演化规律及控制因素，选用上扬子寒武系牛蹄塘组和志留系龙马溪组2套过熟页岩开展热模拟实验，结合X-衍射、氮气和二氧化碳吸附以及扫描电镜研究其孔隙结构的演化特征.龙马溪组样品孔体积在500℃时得到最大提高，为原样的1.35倍; 牛蹄塘组样品孔体积在450℃时上升为最高，较原样提高到1.13倍.利用吸附数据计算出牛蹄塘组样品微孔体积是龙马溪组样品的1.72倍，龙马溪组中孔体积是牛蹄塘组样品的1.44倍.结果表明：（1）牛蹄塘组页岩有机质生烃潜力弱且原始微孔体积高，生烃量少又不易排出，孔隙结构改善较差; （2）龙马溪组页岩石英含量较高抗压能力较强，利于中-大孔隙的发育与保存，也有利于烃类生成后排出，孔体积得到较大提高.Abstract: In order to study the evolution law of pore structure of over-matured shale, two groups of over-matured shales, which were collected from Cambrian Niutitang Formation and Silurian Longmaxi Formation in the Upper Yangtze region, were selected to carry out semi-closed thermal simulation experiments. Meanwhile, X-ray diffraction analysis, CO2 and N2 isotherm adsorption as well as FE-SEM observations were used to determine mineralogical compositions and study the nanopore evolution characteristics. The pore volume of Longmaxi samples increases to the maximum at 500℃, and the pore volume is 1.35 times higher than that of the original sample. The pore volume of shale samples in Niutitang Formation rises to the maximum at 450℃, which is 1.13 times higher than the original sample. Combined with N2 and CO2 adsorption data, the micro-meso-macro pore volume of the samples in the two groups was calculated. The micropore volume of the samples in the Niutitang Formation is 1.72 times higher than that in the Longmaxi Formation, and the mesopore volume of the samples in the Longmaxi Formation is 1.44 times higher than that in the Niutitang Formation. These results show that follows (1) The shale of Niutitang Formation has weak hydrocarbon generation potential and high original micropore volume, with little hydrocarbon generation and difficulty in discharging, resulting in relatively poor pore structure improvement.(2) Longmaxi Formation has high quartz content and strong compressive resistance, which is conducive to the development and preservation of meso-macropores, as well as hydrocarbon generation and subsequent extraction, so the pore volume is greatly improved.
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图 1 剖面地质图
a.中国南方早志留世龙马溪组沉积古地理简图; b.寒武世牛蹄塘组沉积古地理简图(徐政语等, 2015)
Fig. 1. Geographical map of the sampling location
图 3 页岩样品原样与热模拟样品低温氮气吸附
CN-1.CN原样氮气吸附曲线; LTZ-1.LTZ原样氮气吸附曲线; CN-***/LTZ-***.CN/LTZ各模拟温度下的氮气吸附曲线
Fig. 3. Low temperature N2 adsorption and desorption isotherms for the original and pyrolyzed samples
图 4 物理吸附等温线和滞留环类型
a.曲线类型; b.滞留环类型; 据Sing(1985)
Fig. 4. Types of physisorption isotherms and hysteresis loops
图 5 页岩样品最大吸附量对比
Fig. 5. Comparison of the maximum adsorption for the original and pyrolyzed samples
图 6 页岩样品低温二氧化碳吸附
a.CN样品; b.LTZ样品
Fig. 6. Low temperature CO2 adsorption isotherms for the original and pyrolyzed samples
图 7 场发射-扫描电镜照片
CN-0.原样发育大量的粒间孔，大孔径有机孔以及少量粒内孔; CN-450.450 ℃样品发育粒间孔、大孔径有机孔; CN-525.525 ℃样品发育长石溶解粒内孔; LTZ-0.原样发育有少量小孔径有机孔、粒内孔、粒间孔; LTZ-450.450 ℃样品发育有较多的小孔径有机孔; LTZ-525.525 ℃样品发育有粒间孔、长石溶蚀粒内孔，少量较大孔径有机孔
Fig. 7. FE-SEM images for the original and pyrolyzed samples
图 8 孔体积分布
a.CN样品; b.LTZ样品
Fig. 8. The distributions of pore volume with the pore size for the original and pyrolyzed samples
表 1 热模拟实验参数
Table 1. Pyrolysis experimental conditions
样品号 样品重量（g） 模拟深度（m） 加热温度（℃） 静岩压力（MPa） 流体压力（MPa） CN-400 62.169 5 000 400 120 50 CN-450 61.290 6 000 450 144 60 CN-500 61.556 7 000 500 168 70 CN-525 60.470 8 000 525 192 80 LTZ-400 76.173 5 000 400 120 50 LTZ-450 73.087 6 000 450 144 60 LTZ-500 60.918 7 000 500 168 70 LTZ-525 58.773 8 000 525 192 80 
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表 2 样品有机质丰度与矿物组成
Table 2. The TOC and mineral compositions for the original and pyrolyzed samples
样品号 石英（%） 钾长石（%） 斜长石（%） 方解石（%） 白云石（%） 黄铁矿（%） 粘土矿物(%） 其他（%） TOC（%） CN-0 73.0 0 1.5 4.3 5.0 2.8 13.4 0 5.74 CN-400 80.1 0 1.4 5.8 0 0 12.7 0 5.91 CN-450 81.7 0 1.8 5.3 0 0 11.2 0 5.62 CN-500 77.0 0 1.8 5.4 0 0 5.9 9.9 5.79 CN-525 83.1 1.7 2.7 5.0 0 0 7.5 0 5.62 LTZ-1 37.4 1.9 12.2 1.6 5.0 9.5 28.4 4.0 10.60 LTZ-400 34.9 2.5 11.9 2.3 11.5 8.7 26.4 1.8 10.47 LTZ-450 34.3 2.6 11.2 1.8 7.7 0 29.8 12.6 9.44 LTZ-500 40.4 2.7 13.8 6.6 9.1 6.5 18.8 2.1 9.47 LTZ-525 40.6 4.0 13.4 9.1 0 3.0 22.2 7.7 9.33
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表 3 页岩样品孔体积变化
Table 3. Transformation of pore volume for the original and pyrolyzed samples
样品 总孔体积(cm3/g) 微孔 中孔 大孔 (%) (cm3/g) (%) (cm3/g) (%) (cm3/g) CN-0 0.612 7 53.29% 0.326 5 38.76% 0.237 5 7.95% 0.048 7 CN-400 0.667 3 46.79% 0.312 2 46.25% 0.308 6 6.95% 0.046 4 CN-450 0.785 8 44.10% 0.346 5 45.20% 0.355 2 10.70% 0.084 1 CN-500 0.824 8 38.22% 0.315 2 48.28% 0.398 2 13.49% 0.111 3 CN-525 0.708 3 38.63% 0.273 6 45.24% 0.320 4 16.14% 0.114 3 LTZ-0 0.783 0 67.89% 0.531 6 24.76% 0.193 9 7.34% 0.057 5 LTZ-400 0.767 2 69.59% 0.533 9 23.75% 0.182 2 6.67% 0.051 2 LTZ-450 0.881 1 66.17% 0.583 0 31.79% 0.280 1 2.03% 0.017 9 LTZ-500 0.827 2 66.03% 0.546 2 31.87% 0.263 6 2.10% 0.017 4 LTZ-525 0.810 6 62.25% 0.504 6 24.87% 0.201 6 12.89% 0.104 5
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表 4 低压氮气、二氧化碳等温吸附孔隙结构参数
Table 4. Pore structure parameters of N2 and CO2 sorption for the original and pyrolyzed samples under low pressure condition
样品 氮气吸附 二氧化碳吸附 BET比表面积（m2/g) BJH孔体积（cm3/g） BJH平均孔径（nm） 微孔体积（cm3/g） 微孔比表面积（m2/g） CN-0 27.756 4 0.031 4 7.688 8 0.003 81 36.788 0 CN-400 31.249 0 0.038 3 7.656 9 0.004 03 35.874 0 CN-450 29.056 9 0.032 2 9.402 8 0.003 70 36.402 0 CN-500 29.249 6 0.042 7 9.228 1 0.003 63 33.708 0 CN-525 28.718 7 0.041 0 9.431 1 0.003 17 32.480 0 LTZ-0 28.357 5 0.023 7 5.572 5 0.006 72 49.111 0 LTZ-400 30.788 8 0.029 8 5.926 7 0.006 13 48.766 0 LTZ-450 31.731 2 0.031 3 5.075 2 0.006 51 48.982 0 LTZ-500 24.875 0 0.027 7 5.508 1 0.006 89 50.327 0 LTZ-525 20.564 3 0.025 4 7.917 1 0.006 09 45.434 0
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