Evaluation of oil content in shale by sealed thermal desorption: a case study of Jurassic Da'anzhai Member, Sichuan Basin
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摘要: 为解决页岩含油性评价受限于游离烃蒸发损失的难题，并考虑页岩含油性评价目的和井场快速分析的需求，在结合井场低温密闭粉碎技术、改进传统岩石热解方法的基础上，建立了一种岩石密闭热释方法定量评价岩石中游离烃含量的方法。对四川盆地侏罗系自流井组大安寨段页岩进行方法对比分析表明，岩石热解方法获得S0值为0.001~0.046 mg/g，S1值为0.165~4.648 mg/g，而密闭热释方法获得S0值为0.026~0.984 mg/g，S1值为0.113~5.989 mg/g；密闭热释方法获得的S1值与岩石热解方法获得的S1值基本相等，而S0值提高了1~2个数量级。通过改进升温程序，井场密闭热释方法分别获得不加热条件下、90℃以前、90~300℃时单位质量岩石中的烃含量，这不仅获得了更加丰富的含油性数据，而且缩短了检测周期，满足了井场快速分析的需求。结合泥浆气测、页岩地化参数、储层流体性质等参数，评价了研究井大安寨段页岩含油量“甜点”，为页岩油含油性评价提供了一种新的实验手段。Abstract: The oil content in shale is still a contentious issue due to the evaporative losses of free hydrocarbon. Considering the objective of the evaluation of oil content in shale and the demand of fast analysis at wellsite, a newly developed sealed rock thermal desorption method is introduced to quantify the content of free hydrocarbon in rock samples which combined the technique of sealed crushing at low temperature and improved the traditional rock pyrolysis (Rock-Eval). Comparison experiments have been conducted on Jurassic Da'anzhai shale from the Sichun Basin. The S0 value ranges from 0.001 to 0.046 mg/g, with S1 value from 0.165 to 4.648 mg/g by routine method of rock pyrolysis. The S0 value by the sealed thermal desorption method, which ranges from 0.026 to 0.984 mg/g, is about 1-2 order of magnitude higher than that of Rock-Eval. By improving the heating program, the sealed thermal desorption method can obtain the hydrocarbon content per unit mass of rock at temperatures of 5, 5-90 and 90-300℃, which not only obtains abundant oil-bearing data, but also shortens detection time. Combined with parameters such as mud gas measurement, shale geochemical parameters, and reservoir fluid properties, the "sweet spots" of shale oil in the Da'anzhai Member of the study well were evaluated, providing a new experimental method for evaluating the oil content of shale oil.
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Key words:
- sealed crushing /
- thermal release /
- free hydrocarbon content /
- shale oil /
- Da'anzhai Member /
- Jurassic /
- Sichuan Basin
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图 2 不同温度段密闭热释烃气相色谱
Figure 2. Gas chromatograms of hydrocarbons released at different temperatures
图 3 四川盆地侏罗系自流井组大安寨段页岩岩石热解和密闭热释S0和S1对比
Figure 3. Comparisons of S0 and S1 between Rock-Eval and sealed thermal release of Da'anzhai shale, Jurassic Ziliujing Formation, Sichuan Basi
图 4 四川盆地侏罗系自流井组大安寨段页岩TOC与岩石热解S0和井场密闭热释S0之间的关系
Figure 4. Relationship between TOC and S0 by Rock-Eval and sealed thermal release, respectively, of Da'anzhai shale in Jurassic Ziliujing Formation, Sichuan Basin
图 5 四川盆地侏罗系自流井组大安寨段页岩TOC与岩石热解S1和井场密闭热释S1之间的关系
Figure 5. Relationship between TOC and S1 by Rock-Eval and sealed thermal release, respectively, of Da'anzhai shale in Jurassic Ziliujing Formation, Sichuan Basin
图 6 四川盆地L1井侏罗系自流井组大安寨段含油性综合评价
Figure 6. Comprehensive evaluation of oil-content properties of Da'anzhai shale from well L1, Sichuan Basin
表 1 四川盆地L1井侏罗系大安寨段取心层段岩石热解和井场密闭粉碎热解实验数据对比
Table 1. The comparisons of Rock-Eval and in-site sealed thermal release of core samples from Jurassic Da'anzhai member of well L1, Sichuan Basin
编号 深度/m 岩性1) ω(TOC)/% 岩石热解 井场密闭热释 OSI/(mg·g-1)3) Ro/%4) 可动油量/(mg·g-1) S0/(mg·g-1) S1/(mg·g-1) S2/(mg·g-1) Tmax/℃ Sg/(mg·g-1) S0*/(mg·g-1) S0/(mg·g-1)2) S1/(mg·g-1) D-1 3 511.01 MS 1.77 0.001 2.333 2.830 465 0.065 0.741 0.806 5.989 384 1.21 5.025 D-2 3 511.54 MS 1.56 0.034 4.648 4.746 446 0.184 0.801 0.984 5.828 437 0.87 5.252 D-3 3 511.91 MS 1.28 0.046 2.425 2.444 450 0.148 0.450 0.598 2.835 269 0.94 2.156 D-4 3 512.56 LS 0.39 0.006 0.364 0.598 458 0.012 0.034 0.046 0.292 86 1.08 0.000 D-5 3 513.42 LS 1.05 0.001 3.789 4.181 451 0.105 0.331 0.436 2.717 300 0.96 2.103 D-6 3 514.30 LS 1.34 0.022 2.361 2.412 446 0.070 0.374 0.444 2.601 228 0.87 1.707 D-7 3 515.51 MS 0.63 0.007 0.763 1.017 463 0.033 0.066 0.099 0.707 127 1.17 0.172 D-8 3 516.06 MS 0.67 0.003 1.329 1.199 465 0.044 0.309 0.352 1.474 271 1.21 1.152 D-9 3 517.20 MS 0.86 0.029 0.908 1.548 464 0.059 0.253 0.312 0.977 150 1.19 0.429 D-10 3 518.17 LS 0.18 0.013 0.165 0.324 448 0.017 0.009 0.026 0.113 77 0.90 0.000 D-12 3 519.92 LS 0.84 0.001 0.605 1.078 466 0.084 0.247 0.331 1.027 162 1.23 0.521 D-14 3 521.60 LS 0.71 0.006 0.653 1.077 465 0.074 0.144 0.217 0.606 116 1.21 0.116 D-15 3 522.07 MS 0.77 0.011 0.522 0.961 462 0.060 0.175 0.235 0.393 81 1.16 0.000 D-17 3 523.42 MS 0.74 0.001 0.599 0.779 467 0.011 0.126 0.137 0.617 102 1.25 0.015 D-18 3 524.59 LS 0.88 0.001 1.208 1.430 455 0.052 0.217 0.268 1.335 182 1.03 0.721 D-19 3 525.70 LS 1.41 0.026 2.321 2.650 462 0.137 0.424 0.561 1.297 132 1.16 0.447 D-21 3 528.41 MS 0.90 0.011 0.713 0.882 469 0.108 0.260 0.368 0.734 123 1.28 0.203 D-23 3 530.43 MS 1.04 0.003 0.811 1.112 467 0.079 0.266 0.345 1.214 150 1.25 0.520 D-25 3 532.88 LS 0.99 0.011 1.007 1.431 468 0.106 0.334 0.440 1.196 166 1.26 0.651 D-26 3 534.01 MS 1.34 0.022 1.788 1.777 468 0.102 0.376 0.478 1.803 171 1.26 0.944 D-27 3 535.60 MS 1.54 0.038 2.209 2.750 462 0.125 0.404 0.528 2.939 226 1.16 1.931 D-31 3 541.30 MS 0.85 0.005 0.623 0.949 466 0.097 0.196 0.294 0.726 120 1.23 0.173 D-33 3 543.30 MS 1.13 0.027 1.707 1.745 461 0.056 0.285 0.341 1.697 181 1.14 0.909 D-35 3 545.20 MS 2.27 0.002 1.253 1.929 464 0.110 0.497 0.607 1.818 107 1.19 0.155 D-37 3 547.39 MS 1.32 0.040 2.549 2.965 461 0.097 0.493 0.591 2.674 248 1.14 1.946 D-39 3 549.90 MS 1.28 0.017 1.611 1.808 462 0.069 0.306 0.375 2.139 197 1.16 1.238 D-41 3 552.30 LS 1.43 0.001 1.644 2.492 464 0.132 0.405 0.537 1.151 118 1.19 0.260 D-42 3 553.70 LS 0.69 0.026 0.361 0.618 474 0.011 0.078 0.089 0.220 45 1.37 0.000 D-43 3 554.80 MS 0.79 0.001 0.368 0.886 473 0.054 0.158 0.212 0.414 80 1.35 0.000 1) MS表示泥页岩，LS表示介壳灰岩；
2)S0=Sg+S0*；
3)OSI基于井场密闭粉碎热释结果计算，OSI=100(Sg+S0*+S1)/ω(TOC)；
4)Ro=0.018Tmax-7.16[14]。
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