二维核磁共振技术表征页岩所含流体特征的应用——以松辽盆地青山口组富有机质页岩为例

doi:10.11743/ogg20210613

Abstract

Abstract:

Shale may contain a large amount of oil and gas that can be commericially exploited. Clarifying the content and occurrence of different fluids in shale is crucial to the development of shale oil. High frequency (23 MHz) two-dimensional (2D) NMR technology that can be used to quickly, nondestructively and quantitatively measure protium-containing (¹H) fluids in shale is employed to test shale samples (from the Qingshankou Formation in Songliao Basin) before and after extraction as well as during spontaneous imbibition and constant temperature rising experiments. The content and occurrence of different fluids in the samples as well as the loss of fluid from the samples after a period of static settlement are quantified and analyzed. The results show that on the 2D NMR maps, the signals of analogous solid organic matter and movable hydrocarbons, roughly separated by T₂=0.1ms, are mostly distributed in the region above T₁>10 ms. Good linear correlations can be observed between the signals and TOCs or S₁. Oil is either free or absorbed in shale samples from the Qingshankou Formation. Higher clay content means more absorbed oil and less free oil in shale. The 2D NMR spectrum obtained during spontaneous imbibition experiment indicates water swelling of clay minerals. The vacuum heating process of the samples shows both volatilization of light hydrocarbons and significant loss of water. Samples from sealing core drilling combined with 2D NMR can be used effectively in the restoration of the original oil saturation and water saturation.

Key words: two-dimensional NMR, abundance of organic matter, shale, Qingshankou Formation, Songliao Basin

CLC Number:

TE122.1

Longhui Bai, Bo Liu, Yaao Chi, Shichao Li, Xun Wen. 2D NMR studies of fluids in organic-rich shale from the Qingshankou Formation, Songliao Basin[J]. Oil & Gas Geology, 2021, 42(6): 1389-1400.

Figures/Tables 12

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References 32

1	邹才能, 杨智, 崔景伟, 等. 页岩油形成机制、地质特征及发展对策[J]. 石油勘探与开发, 2013, 40 (1): 14- 27.
	Zou Caineng , Yang Zhi , Cui Jingwei , et al. Formation mechanism, geological characteristic and development strategy of nonmarine shale oil in China[J]. Petroleum Exploration and Development, 2013, 40 (1): 14- 27.
2	姜在兴, 张文昭, 梁超, 等. 页岩油储层基本特征及评价要素[J]. 石油学报, 2014, 35 (1): 184- 197.
	Jiang Zaixing , Zhang Wenzhao , Liang Chao , et al. Characteristic and evaluation elements of shale oil reservoir[J]. Acta Petroleum Since, 2014, 35 (1): 184- 197.
3	孙龙德, 刘合, 何文渊, 等. 大庆古龙页岩油重大科学问题与研究路径探析[J]. 石油勘探与开发, 2021, 48 (03): 453- 463.
	Sun Longde , Liu He , He Wenyuan , et al. An analysis of major scientific problems and research paths of Gulong shale oil in Da-qing Oilfield, NE China[J]. Petroleum Exploration and Development, 2021, 48 (03): 453- 463.
4	贾承造, 庞雄奇, 宋岩. 论非常规油气成藏机理: 油气自封闭作用与分子间作用力[J]. 石油勘探与开发, 2021, 48 (03): 437- 452.
	Jia Chengzao , Pang Xiongqi , Song Yan . The mechanism of unconventional hydrocarbon formation: Hydrocarbon self-containment and intermolecular forces[J]. Petroleum Exploration and Development, 2021, 48 (03): 437- 452.
5	柳波, 何佳, 吕延防, 等. 页岩油资源评价指标与方法--以松辽盆地北部青山口组页岩油为例[J]. 中南大学学报, 2014, 45 (11): 3846- 3853.
	Liu Bo , He jia , Lu Yanfang , et al. Parameters and method for shale oil assessment: Taking Qinshankou Formation shale oil of Northern Songliao Basin[J]. Journal of Central south University (Since and Technology), 2014, 45 (11): 3849- 3853.
6	周磊, 王永诗, 于雯泉, 等. 基于物性上、下限计算的致密砂岩储层分级评价-以苏北盆地高邮凹陷阜宁组一段致密砂岩为例[J]. 石油与天然气地质, 2019, 40 (6): 1308- 1316, 1323.
	Zhou Lei , Wang Yongshi , Yu Wenquan , et al. Classification assessment of tight sandstone reservoir based on calculation of lower and upper limits of physical properties-A case study of the tight sandstone reservoir in the 1st member of Funing Formation in Gaoyou Sag, North Jiangsu Basin[J]. Oil & Gas Geology, 2019, 40 (6): 1308- 1316, 1323.
7	牛小兵, 冯胜斌, 刘飞, 等. 低渗透致密砂岩储层中石油微观赋存状态与油源关系--以鄂尔多斯盆地三叠系延长组为例[J]. 石油与天然气地质, 2013, 34 (03): 288- 293.
	Niu Xiaobing , Feng Shengbin , Liu Fei , et al. Microscopic occurrence of oil in tight sandstones and its relation with oil sources-a case study from the Upper Triassic Yanchang Formation, Ordos Basin[J]. Oil & Gas Geology, 2013, 34 (03): 288- 293.
8	Birdwell J E. , Washburn K E . Multivariate analysis relating oil shale geochemical properties to NMR relaxometry[J]. Energy & Fuels, 2015, 29 (4): 2234- 2243.
9	顾兆斌, 刘卫, 孙佃庆, 等. 基于核磁共振二维谱技术识别储层流体类型[J]. 西安石油大学学报(自然科学版), 2010, 32 (005): 83- 86.
	Gu Zhaobin , Liu Wei , Sun Dianqing , et al. Identify reservoir fluid types with two dimensional NMR techniques[J]. Journal of Southwest Petroleum University (Science & Technology Edition), 2010, 32 (5): 83- 87.
10	Liu B , Bai L , Chi Y , et al. Geochemical characterization and quantitative evaluation of shale oil reservoir by two-dimensional nuclear magnetic resonance and quantitative grain fluorescence on extract: A case study from the Qingshankou Formation in Southern Songliao Basin, northeast[J]. Marine and Petroleum Geology, 2019, 109, 561- 573. doi: 10.1016/j.marpetgeo.2019.06.046
11	Liu B , Sun J , Zhang Y , et al. Reservoir space and enrichment model of shale oil in the first member of Cretaceous Qingshankou Formation in the Changling sag, southern Songliao Basin, NE China[J]. Petroleum Exploration and Development, 2021, 48 (2): 1- 16.
12	Li J , Jiang C , Wang M , et al. Adsorbed and free hydrocarbons in unconventional shale reservoir: A new insight from NMR T₁-T₂ maps[J]. Marine and Petroleum Geology, 2020, 116, 104311. doi: 10.1016/j.marpetgeo.2020.104311
13	Khatibi S. , Ostadhassan M. , Xie Z H. , et al. NMR relaxometry a new approach to detect geochemical properties of organic matter in tight shales[J]. Fuel, 2018, 235 (1): 167- 177.
14	Rueslåtten H , Eidsemo T , Lehne K A , et al. The use of NMR spectroscopy to validate NMR logs from deeply buried reservoir sandstones[J]. Journal of Petroleum Science and Engineering, 1998, 19, 33- 43. doi: 10.1016/S0920-4105(97)00033-8
15	Howard J J. , Kenyon W E. , Straley C . Proton magnetic resonance and pore size variations in reservoir sandstones[J]. SPE Formation Evaluation, 1993, 8 (03): 194- 200. doi: 10.2118/20600-PA
16	Gao Z , Hu Q . Wettability of Mississippian Barnett Shale samples at different depths: Investigations from directional spontaneous imbibition[J]. AAPG Bulletin, 2016, 100 (1): 101- 114. doi: 10.1306/09141514095
17	Wei Y , Qwab C , Yan S , et al. New scaling model of the spontaneous imbibition behavior of tuffaceous shale: Constraints from the tuff-hosted and organic matter-covered pore system[J]. Journal of Natural Gas Science and Engineering, 2020, 81103389.
18	Bechtel A , Jia J , Strobl S , et al. Palaeoenvironmental conditions during deposition of the Upper Cretaceous oil shale sequences in the Songliao Basin (NE China): Implications from geochemical analysis[J]. Organic Geochemistry, 2012, 46, 76- 95. doi: 10.1016/j.orggeochem.2012.02.003
19	Liu B , Wang H , Fu X , et al. Lithofacies and depositional setting of a highly prospective lacustrine shale oil succession from the Upper Cretaceous Qingshankou Formation in the Gulong sag, northe-rn Songliao Basin, northeast China[J]. AAPG Bulletin, 2019, 103 (2): 405- 432. doi: 10.1306/08031817416
20	柳波, 刘阳, 刘岩, 等. 低熟页岩电加热原位改质油气资源潜力数值模拟--以松辽盆地南部中央坳陷区嫩江组一, 二段为例[J]. 石油实验地质, 2020, (4): 533- 544.
	Liu Bo , Liu Yang , Liu Yan , et al. Prediction of low-maturity shale oil produced by in situ conversion: a case study of the first and second members of Nenjiang Formation[J]. Petroleum Geology & Experiment, 2020, (4): 533- 544.
21	Espitalie , Deroo G , Marquis F . Rock-Eval pyrolysis and its applications (Part One)[J]. Revue del'Institut Français du Pétrole, 1985, 40 (5): 563- 579.
22	Langford F F , Blanc-Valleron M M . Interpreting Rock-Eval pyrolysis data using graphs of pyrolizable hydrocarbons vs[J]. AAPG Bulletin, 1990, 74 (6): 799- 804.
23	Dahl B , Bojesen-Koefoed J , Holm A , et al. A new approach to interpreting Rock-Eval S₂ and TOC data for kerogen quality assessment[J]. Organic Geochemistry, 2004, 35 (11): 1461- 1477.
24	Fleury M , Romero-Sarmiento M . Characterization of shales using T₁-T₂ NMR maps[J]. Journal of Petroleum Science and Engineering, 2016, 137, 55- 62. doi: 10.1016/j.petrol.2015.11.006
25	Gong L , Wang J , Gao S , et al. Characterization, controlling factors and evolution of fracture effectiveness in shale oil reservoirs[J]. Journal of Petroleum Science and Engineering, 2021, 203, 108655. doi: 10.1016/j.petrol.2021.108655
26	Liu B , Yang Y , Li J , et al. Stress sensitivity of tight reservoirs and its effect on oil saturation: A case study of Lower Cretaceous tight clastic reservoirs in the Hailar Basin, Northeast China[J]. Journal of Petroleum Science and Engineering, 2020, 184, 106484. doi: 10.1016/j.petrol.2019.106484
27	赵清民, 伦增珉, 章晓庆, 等. 页岩油注CO₂动用机理[J]. 石油与天然气地质, 2019, 40 (6): 1333- 1338.
	Zhao Qingmin , Lun Zengmin , Zhang Xiaoqing , et al. Mechanism of shale oil mobilization under CO₂ injection[J]. Oil &Gas Geology, 2019, 40 (6): 1333- 1338.
28	郎东江, 伦增珉, 吕成远, 等. 页岩油注二氧化碳提高采收率影响因素核磁共振实验[J]. 石油勘探与开发, 2021, 48 (03): 603- 612.
	Lang Dongjiang , Lun Zengmin , Lv Chengyuan , et al. Nuclear magnetic resonance experimental study of CO2 injection to enhance shale oil recovery[J]. Petroleum Exploration and Development, 2021, 48 (03): 603- 612.
29	张炜, 李义连, 郑艳, 等. 二氧化碳地质封存中的储存容量评估: 问题和研究进展[J]. 地球科学进展, 2008, (10): 1061- 1069. doi: 10.3321/j.issn:1001-8166.2008.10.008
	Zhang Wei , Li Yilian , Zheng Yan , et al. CO₂ storage capacity estimation in geological sequestration: issus and Research Progress[J]. Advances in Earth Science, 2008, (10): 1061- 1069. doi: 10.3321/j.issn:1001-8166.2008.10.008
30	Li C , Shen Y , Ge H , et al. Analysis of capillary rise in asymmetric branch-like capillary[J]. Fractals, 2016, 24 (2): 1650024. doi: 10.1142/S0218348X16500249
31	Mmab C , Hg C , Ys C , et al. The effect of clay-swelling induced cracks on imbibition behavior of marine shale reservoirs[J]. Journal of Natural Gas Science and Engineering, 2020, 83, 103525. doi: 10.1016/j.jngse.2020.103525
32	李进步, 卢双舫, 陈国辉, 等. 热解参数S₁的轻烃与重烃校正及其意义-以渤海湾盆地大民屯凹陷E₂ s⁴⁽²⁾段为例[J]. 石油与天然气地质, 2016, 37 (4): 538- 545.
	Li Jinbu , Lu Shuangfang , Chen guohui , et al. Correction of light and heavy hydrocarbon loss for residual hydrocarbon S₁ andits significance to assessing resource potential of E₂s⁴⁽²⁾ member in Damintun Sag, Bohai Bay Basin[J]. Oil &Gas Geology, 2016, 37 (4): 538- 545.

样品编号	深度/ m	TOC/ %	T_max/ ℃	S₁/（mg·g^-1）	S₂/（mg·g^-1）	PI	DCM	矿物组分含量/%
样品编号	深度/ m	TOC/ %	T_max/ ℃	S₁/（mg·g^-1）	S₂/（mg·g^-1）	PI	DCM	石英	长石	方解石	白云石	黄铁矿+ 菱铁矿	粘土
1	1 480.28	2.49	450	1.20	21.10	0.05	0.50	31.0	18.7	0.9	3.6	8.8	37.0
2	1 486.94	2.68	449	1.50	19.20	0.07	0.72	30.2	20.2	1.5	0	10.1	38.0
3	1 492.70	2.40	448	1.20	17.20	0.07	0.63	31.9	16.4	0	0	10.4	41.3
4	1 498.13	2.84	447	2.00	20.60	0.09	0.84	33.6	23.5	1.7	0	8.0	33.2
5	1 506.95	3.49	448	1.50	26.90	0.05	0.66	29.6	18.5	5.8	2.3	9.7	34.1
6	1 510.72	2.27	449	1.00	22.40	0.04	0.47	32.6	17.2	0	0	8.5	41.7
7	1 512.78	3.39	451	1.10	30.10	0.03	0.61	63.9	10.1	0	2.1	2.9	52.6
8	1 524.64	1.81	447	2.20	14.90	0.13	0.88	31.4	10.5	1.3	4.8	21.2	30.9
9	1 527.86	3.41	449	1.80	25.70	0.07	0.77	39.2	10.7	0	0	6.9	43.1
10	2 046.55	4.10	445	4.63	25.28	0.15	—	35.8	9.0	3.4	12.1	2.0	37.7
11	2 055.80	2.56	438	2.56	16.68	0.13	—	32.2	10.1	0	2.0	9.0	46.7

样品编号	抽提前						抽提后
样品编号	样品质量/g	总化合物量/μL	类固体有机质含量/（μL·g^-1）	轻质烃含量/（μL·g^-1）	羟基化合物/（μL·g^-1）	水含量/（μL·g^-1）	样品质量/ g	总化合物量/μL	类固体含量有机质/（μL·g^-1）	轻质烃含量/（μL·g^-1）	羟基化合物含量/（μL·g^-1）	水含量/（μL·g^-1）
1	20.62	863	6.2	1.7	15.3	18.6	19.4	645	4.0	1.6	20.3	7.4
2	20.79	853	5.9	2.3	15.5	17.3	19.9	653	3.3	1.3	24.5	3.7
3	20.68	987	5.0	2.2	22.4	18.1	20.0	696	3.4	1.5	24.9	5.0
4	20.98	730	6.5	3.1	12.5	12.7	20.0	564	1.7	1.3	20.4	4.7
5	20.96	803	7.8	2.4	13.2	14.9	20.0	602	3.1	1.3	23.7	2.2
6	20.86	871	7.4	1.9	18.5	14.1	20.0	780	6.7	1.1	27.8	3.5
7	20.50	1 006	9.1	2.2	23.1	14.7	19.7	814	7.5	2.1	28.3	3.4
8	20.41	869	4.5	3.9	19.1	15.1	19.0	798	1.4	2.2	33.8	4.6
9	20.96	961	7.6	3.3	17.7	17.3	19.5	723	4.3	1.4	27.9	3.4

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2D NMR studies of fluids in organic-rich shale from the Qingshankou Formation, Songliao Basin

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