Evaluation of evaporative loss of hydrocarbon in shale samples and its geological implications
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摘要: 游离烃含量是页岩油资源评价中最关键参数之一，但由于烃类散失的影响，实验测得的游离烃含量往往与真实含量差异较大，从而导致含油性评价结果“失真”。为研究含油泥页岩烃类散失过程，获取烃类散失量及校正系数，本文利用成熟度相近、不同岩相的新鲜含油岩心样品，对不同放置时间后样品的烃类残留量及残留组分开展实验并进行综合分析。研究认为，页岩样品烃类散失分早期快速散失和后期缓慢散失2个过程，挥发组分主要为C13—C15以前的低碳数烃类，中质—重质组分受影响较小；储集物性条件及原始含油量共同控制了烃类散失量及散失过程。原始含油量越高、储集物性越好的泥页岩样品烃类散失量越大，因此，在评价储集物性好的高含油的页岩油“甜点”段时，更需要注意原始烃含量的恢复。Abstract: Free hydrocarbon content is one of the key parameters for resource assessment of shale oil.However, due to the evaporative loss of hydrocarbon, the measured results from lab analysis differ greatly from real value, which leads to the "distortion" of shale oil resource assessment.To investigate the process of the evaporative loss and obtain the hydrocarbon loss amount and correction coefficient, a time-series of analysis has been carried out on fresh oil-bearing shale samples with similar maturity and different lithofacies for both the amount and the composition of the hydrocarbons retained in shale.Results suggest that there are two processes of early rapid and later slow evaporative loss. The volatile components are mainly light hydrocarbons with carbon numbers smaller than C13-C15, while the medium to heavy components are less affected. Both the amount and processes of hydrocarbon evaporative loss are controlled by the physical properties and original oil content of shale samples.The oil-bearing shale samples with higher original oil content and better physical properties appear to have more evaporative loss of hydrocarbons.Results also indicate that more attention should be exercised on original hydrocarbon content when conducting the shale oil resource assessment of "sweet spot" section with high oil content and good physical properties.
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图 1 热解S1测量值与样品放置时间的关系
Figure 1. Relationships between Rock-Eval S1 value and sample storing time
图 2 不同含油程度的样品放置后S1测量值变化
Figure 2. Rock-Eval S1 value changes of samples with different oil contents after storing
图 3 页岩岩心样品不同放置周期后散失烃类组分变化特征
Figure 3. Characteristics of hydrocarbon component changes of shale core samples with different storing time
图 4 不同放置周期后样品游离烃含量与原始游离烃含量的关系
Figure 4. Free hydrocarbon contents before and after different storing time
图 5 样品早期散失量与孔隙度、渗透率及原始含油量的关系
Figure 5. Early loss vs. porosity, permeability and original oil content of samples
图 7 泥页岩样品长时间放置后烃类损失比例与原始含油量关系
Figure 7. Hydrocarbon loss ratio vs. original oil content of shale samples after long-time storing
图 8 不同泥页岩样品原始含油量与长时间放置后含油量对比
Figure 8. Original S1 value vs. S1 value of different shale samples after storing for five months
表 1 实验样品基础数据
Table 1. Basic information of experimental samples
井号 样品号 岩性 深度/m S1/(mg·g-1) S2/(mg·g-1) ω(TOC)/% Tmax/℃ 主要矿物含量/% 孔隙度/% 黏土 石英 长石 方解石 白云石 石膏 钙芒硝 BYY1 45 灰色纹层状白云质泥岩 3 124.07 4.45 2.96 2.07 408 29.6 14.5 7.4 5.8 28.8 1.1 8.0 1.1 55 灰色纹层状泥质白云岩 3 124.39 5.72 3.91 2.17 414 19.2 9.2 8.1 16.5 40.2 1.4 2.3 8.4 61 灰黑色纹层状白云质泥岩 3 124.70 3.23 2.86 1.46 416 18.7 9.2 8.3 19.6 34.9 2.1 1.2 1.0 67 灰黑色纹层状白云质泥岩 3 124.88 3.66 2.26 1.28 414 38.6 17.8 7.9 18.6 5.0 1.2 2.4 3.1 143 灰色泥质白云岩 3 127.33 5.54 3.36 1.75 407 18.5 10.2 6.5 12.1 47.6 0.9 0.6 7.5 161 灰色纹层状泥质白云岩 3 127.76 7.79 1.55 1.16 402 13.9 9.4 7.8 16.9 43.1 0.8 4.3 2.5 192 灰黄色含穿层钙芒硝白云岩 3 129.07 5.34 1.22 0.80 398 17.1 9.0 6.5 6.7 25.4 1.8 27.9 2.8 205 灰黄色纹层状白云岩 3 129.56 12.60 1.21 1.40 393 8.0 7.5 8.1 4.0 54.1 1.0 13.3 1.6 220 浅灰色白云岩 3 130.12 3.93 0.69 0.60 403 7.6 12.6 11.4 3.6 56.7 1.2 1.2 13.4 224 灰色细纹层状白云岩 3 130.27 7.60 4.22 1.68 408 34.1 20.3 5.0 5.3 3.7 1.5 24.1 3.8 197 灰色含钙芒硝白云质泥岩 3 129.29 4.43 1.68 1.04 397 31.3 22.2 10.3 11.3 7.0 1.6 5.1 3.8 253 灰白色块状钙芒硝岩 3 131.40 2.92 0.77 0.66 391 27.6 15.3 4.0 3.6 1.9 1.8 37.4 0.7 264 灰黄色块状白云岩 3 131.73 4.75 1.18 0.85 405 13.3 8.7 4.4 2.7 58.1 0.6 1.2 8.2 BYY2 1111 灰黑色纹层状白云质泥岩 3 400.29 10.88 5.22 4.13 428 15.5 8.6 13.7 21.3 29.0 5.1 0.3 1.3 1076 灰黑色纹层状白云质泥岩 3 399.37 2.43 0.69 2.27 400 12.4 6.1 18.5 8.7 35.3 16.7 0.7 6.0 注：S1、S2、TOC及Tmax数据为原始新鲜样品分析结果。 
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表 2 泥页岩样品不同常温放置时间后S1测试值
Table 2. Rock-Eval S1 value of shale samples after a time-series of storing in normal conditions
放置时间/h S1/(mg·g-1) 样品1111 样品1076 2 10.88 2.43 8 10.54 1.64 32 9.70 1.45 56 9.41 1.27 794 8.20 1.08 1 394 8.16 0.98
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表 3 不同样品的S1恢复系数计算结果
Table 3. Calculation results of corrective coefficients of Rock-Eval S1 for different samples
样品号 原始S1含量/(mg·g-1) 缓慢散失阶段S1含量/(mg·g-1) S1损失比例/% S1恢复系数 205 12.6 55 5.72 224 7.60 2.63 65.39 2.89 161 7.79 4.11 47.24 1.90 264 4.75 2.83 40.42 1.68 67 3.66 2.75 24.86 1.33 143 5.54 3.84 30.69 1.44 192 5.34 3.55 33.52 1.50 61 3.23 2.43 24.77 1.33 220 3.93 2.73 30.53 1.44 注：样品205和55由于尚未进入缓慢散失阶段，故本文未计算其恢复系数。
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