CN110595953B - Experimental test device and method for shale mixing wettability - Google Patents
Experimental test device and method for shale mixing wettability Download PDFInfo
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- 238000012360 testing method Methods 0.000 title claims abstract description 47
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- 230000015572 biosynthetic process Effects 0.000 claims abstract description 24
- 239000012530 fluid Substances 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000004088 simulation Methods 0.000 claims abstract 8
- 239000011435 rock Substances 0.000 claims description 53
- 238000005481 NMR spectroscopy Methods 0.000 claims description 33
- 229920006395 saturated elastomer Polymers 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 12
- 239000011148 porous material Substances 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000010998 test method Methods 0.000 claims description 7
- 230000014509 gene expression Effects 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 2
- 238000009738 saturating Methods 0.000 claims description 2
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- 238000002474 experimental method Methods 0.000 description 10
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- 239000007789 gas Substances 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 238000011160 research Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 4
- 238000009736 wetting Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000003345 natural gas Substances 0.000 description 3
- 239000002734 clay mineral Substances 0.000 description 2
- 239000002283 diesel fuel Substances 0.000 description 2
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- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N24/00—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
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Abstract
The invention discloses an experimental test device and method for shale mixed wettability, wherein the experimental test device comprises a stratum temperature simulation system, a stratum confining pressure simulation system and a mixed wettability test system; the formation temperature simulation system is a heater; the stratum confining pressure simulation system is a confining pressure pump; the mixed wettability testing system comprises a constant-speed constant-pressure pump, a constant-speed constant-pressure pump outlet valve, an intermediate container outlet valve, a vacuum pump inlet valve and a reaction kettle, wherein the constant-speed constant-pressure pump, the constant-speed constant-pressure pump outlet valve, the intermediate container and the intermediate container outlet valve are sequentially connected to the reaction kettle, the vacuum pump and the vacuum pump inlet valve are sequentially connected to the reaction kettle, and fluids with different wettability are pumped into the reaction kettle by the constant-speed constant-pressure pump to test mixed wettability. The method can consider the influences of the formation temperature, the formation pressure and the shale mixed wettability, and can quantitatively represent the shale hydrophilic index, the oleophilic index and the mixed wettability index.
Description
Technical Field
The invention relates to the field of petroleum and natural gas engineering, in particular to an experimental test method for shale mixed wettability in a shale reservoir development process.
Background
The shale gas fracturing realizes the multi-section multi-cluster large-scale volume transformation of the horizontal well by injecting water-based fracturing fluid of the top ten thousand into a shale stratum, and the formation of a complex fracture network is a key technology for effectively utilizing shale oil gas. Compared with the conventional sandstone, the fracturing fluid has more prominent and deep interaction with the shale reservoir due to the difference in geological characteristics, fracturing process and the like. Shale after volume compaction exhibits flowback characteristics that are distinct from conventional reservoirs: the method is characterized by comprising the following steps of (1) low fracturing fluid flowback rate, negative correlation between gas production rate and flowback rate, reduction of water production after soaking and increase of gas production rate, and the like (billows, lie directions, Yang standing peaks, and shut-in opportunities influence the flowback rate and the productivity of the shale gas well [ J ] natural gas industry, 2017,37(8): 48-58). The wettability is a key factor influencing the microscopic distribution state of the fluid in the shale pore canal and the interaction between the fluid and the rock, so that the characteristics of shale wettability are accurately and quantitatively represented by using an indoor experimental method, and the method has important effects on clearing the seepage rule of the fracturing fluid in the shale reservoir, explaining the special flowback characteristics of the fractured shale gas well, objectively evaluating the seepage and absorption capacity of the shale reservoir and the like.
Researches show that the shale reservoir is rich in organic matters and clay minerals, and the surface of the shale reservoir has complex mixed wettability characteristics, namely the shale is hydrophilic and oleophilic. The micro-pore structure and mineral components of shale, formation confining pressure, formation temperature and the like have important influence on the wettability of fluid in the shale, but at present, experimental research does not consider the factors at the same time, and most of the experimental research focuses on the surface wettability research of the shale at normal temperature and normal pressure. At present, the wettability testing method mainly takes experiments as main content, and the specific content is as follows:
(1) liu jun, etc. (Liu jun, bear jian, Lilianxi, Longma xi shale wettability analysis and influence discussion [ J ] natural gas geoscience, 2014,25(10):1645 one 1652) adopt optical contact angle measuring instrument to the contact angle of deionized water, white oil and diesel oil on the surface of Longma xi underground and outcrop rock core under normal temperature and heating condition, research shows that the contact angle of shale and deionized water is 10.7-38.7 degrees, white oil and diesel oil can be completely spread, the shale surface is both hydrophilic and oleophilic, shows the characteristic of mixed wettability, and the contact angle is reduced along with the temperature increase. The method does not consider the influence of the formation temperature and the confining pressure simultaneously, only tests the wettability of the shale surface, and does not quantitatively characterize the mixed wettability of the shale pore throat.
(2) Su et al (Su S, Jiang Z, Shan X, et al. the wetability of shale by NMR measurements and its controlling factors [ J ]. Journal of Petroleum Science & Engineering 2018,169,309-316.) use nuclear magnetic resonance techniques to qualitatively measure shale wettability and analyze factors that influence shale wettability control, studies have shown that the presence of organic matter is the root cause of shale oil-wetting, the formation of pores between organic matter and clay minerals is characteristic of shale mixed wettability, and the inorganic mineral carbonate salt content in water-wetted shale samples is higher. The method also does not consider the influence of the formation temperature and the confining pressure, and the shale mixed wettability is not quantitatively characterized.
The method does not comprehensively consider the influence of factors such as formation temperature, confining pressure and the like on the wettability of the fluid in the shale pore throat, and at present, no method simultaneously considers the factors and qualitatively and quantitatively represents the factors, so that an experimental test device and a related test method for the mixed wettability of the shale reservoir under the condition of a real formation need to be developed, and a basis is provided for analyzing the distribution and migration rule of the fluid in the shale reservoir.
Disclosure of Invention
The invention aims to provide a shale mixing wettability experiment testing device and a method for testing shale mixing wettability by using the device.
The utility model provides a shale mixes wettability experiment testing arrangement mainly comprises constant speed constant pressure pump, constant speed constant pressure pump outlet valve, intermediate container outlet valve, vacuum pump inlet valve, reation kettle, heating jacket, reation kettle outlet valve, rock core holder, cylindrical cushion, rock core holder outlet valve, confining pressure pump. The core is placed in the core holder, one end face of the core holder is in contact with experimental liquid, the other end face of the core holder is in contact with a cylindrical cushion block, and confining pressure is loaded to the core through a confining pressure pump during experiment; heating the experimental liquid and the rock core by a heater; a diversion trench is arranged on the contact surface of the cylindrical cushion block and the rock core, an eyelet for fluid to flow is arranged in the center of the cushion block, and the fluid can flow to an outlet valve of the rock core holder through the eyelet;
an experimental test method for shale mixed wettability comprises the steps of processing an underground core or a same-layer outcrop rock of a shale storage interval into a standard core with the diameter of 2.5cm and the length of 5cm, and drying the standard core till the standard core is constantHeavy, the dried sample T is tested by a low-field nuclear magnetic resonance apparatus2And (5) obtaining the area of the nuclear magnetic resonance signal of the original sample by using a map curve. Secondly, determining confining pressure and temperature of a shale wettability test experiment according to formation parameters of a fracturing layer section, loading confining pressure on a shale sample, heating to a set temperature, placing deionized water into a reaction kettle, contacting and saturating the end face of a rock core for 48 hours, and then testing T2Obtaining a spectrum curve to obtain the nuclear magnetic resonance hydrophilic signal area of the rock core, and using MnCl to test the tested rock core2Soaking in water for 24 h; finally, after the soaked rock core is saturated with oil for 48 hours, testing T2Obtaining core nuclear magnetic resonance oleophylic signal area according to the graph curve and T under different states2And calculating the shale hydrophilic index, the oleophylic index and the mixed wettability index by the signal area of the map curve, thereby quantitatively testing and evaluating the mixed wettability of the shale under the conditions of confining pressure and temperature.
In order to achieve the above technical objects, the present invention provides the following technical solutions. An experimental test device and method for shale mixed wettability sequentially comprises the following steps:
(1) preparing a core: preparing a standard core with the diameter of 2.5cm and the length of 5cm from an underground core or a same-layer-position outcrop rock of a shale storage layer section, and drying the standard core in a 100 ℃ drying oven to constant weight;
(2) testing the shale rock core T dried in the step (1) by using a low-field nuclear magnetic resonance instrument2Obtaining the nuclear magnetic resonance signal area S of the original sample by using a map curve;
(3) determining an experimental loading condition according to the formation stress and the temperature, wherein the specific determination method comprises the following steps: determining the experimental loading confining pressure according to the expressions (1) to (4), wherein the formation temperature is the experimental temperature;
σ'z＝σz-αPp (1)
σ'H＝σH-αPp (2)
σ'h＝σh-αPp (3)
σenclose＝(σ'z+σ'H+σ'h)/3 (4)
In the formula: sigma'zIs vertically provided withEffective stress, MPa; sigma'HMaximum horizontal effective principal stress, MPa; sigma'hIs the minimum level effective principal stress, MPa; sigmazIs vertical stress, MPa; sigmaHMaximum horizontal principal stress, MPa; sigmahMinimum horizontal principal stress, MPa; alpha is the effective stress coefficient, decimal; sigmaEncloseIs experimental confining pressure, MPa; pPThe formation pore pressure, MPa.
(4) Pouring the experimental liquid into an intermediate container of a constant-speed constant-pressure pump, loading the tested rock core in the step (2) into a rock core holder, and loading initial confining pressure of 5MPa to the rock core by using a confining pressure pump;
(5) heating the core and the core holder to the experimental temperature determined in the step (3) by using a heater, and setting the loading pressure of the confining pressure pump according to the confining pressure determined in the step (3);
(6) evacuating the air in the pipeline and the reaction kettle by using a vacuum pump, closing an inlet valve of the vacuum pump after evacuation is finished, and pumping the experimental liquid in the intermediate container into the reaction kettle by using a constant-speed constant-pressure pump;
(7) after the end face of the rock core and liquid in the reaction kettle are saturated for 48 hours, unloading the pressure of the confining pressure pump, turning off the heater, cooling for 2 hours, taking out the rock core, and testing T2Obtaining nuclear magnetic resonance hydrophilic signal area S of rock core by using atlas curvews，
(8) Using MnCl for the rock core after the test in the step (7)2The solution is saturated in a beaker at normal temperature and normal pressure for 24 hours;
(9) repeating the steps (4) to (7) on the saturated rock core obtained in the step (8), wherein the experimental liquid is oil, and testing the T of the saturated rock core for 48 hours2Obtaining core nuclear magnetic resonance oleophylic signal area S by using atlas curveos；
(10) Testing the nuclear magnetic resonance signal area, the nuclear magnetic resonance hydrophilic signal area after saturated water and the nuclear magnetic resonance oleophylic signal area after saturated oil of the original sample according to the steps (2), (7) and (9), and respectively defining a hydrophilic index, an oleophylic index and a mixed wettability index to quantitatively represent the hydrophilic ability, the oleophylic ability and the mixed wettability of the shale, wherein the expression is as follows:
hydropathic index:
WIw＝(Sws-S)/(Sws+Sos-2S) (5)
lipophilicity index:
WIo＝(Sos-S)/(Sws+Sos-2S) (6)
mixed wettability index:
WIwo＝WIw-WIo (7)
in the formula: WI (Wireless electric appliance)wHydrophilic index, dimensionless; WI (Wireless electric appliance)oThe oil is oleophylic index and has no dimension; WI (Wireless electric appliance)woThe mixed wetting index is zero; s is the area of the nuclear magnetic resonance signal of the original sample and has no dimension; swsThe area of a nuclear magnetic resonance hydrophilic signal of the rock core after saturated water is zero; sosThe area of a nuclear magnetic resonance oleophylic signal of the rock core after saturated oil is zero dimension.
(11) Comprehensively evaluating the shale mixed wettability index calculated in the step (10) when the mixed wettability index WI iswoShale is strongly hydrophilic as 1; when mixed wetting index WIwoShale is strongly lipophilic-1; when mixed wetting index WIwoShale is neutral wet 0. When WI iswoWhen the value is more than 0, the integral shale is hydrophilic, and the larger the value is, the stronger the hydrophilicity of the rock core is; when WI iswoLess than 0, the shale is wholly oleophilic, and the smaller the value, the stronger the oleophilicity of the rock core.
Compared with the prior art, the invention has the following beneficial effects:
the invention designs a shale mixed wettability experiment testing device and method considering the influences of formation temperature and confining pressure simultaneously, defines a hydrophilic index, a lipophilic index and a mixed wettability index to comprehensively evaluate and quantitatively characterize the shale wettability, is simple to operate, is more accurate than the conventional wettability testing method, and provides a new idea for testing and evaluating the shale mixed wettability.
Drawings
FIG. 1 is a schematic diagram of an experimental testing device for shale mixing wettability.
FIG. 2 is the bookNuclear magnetic resonance T of shale core S1-1 in different states2Graph curves.
Experimental set-up picture description
The shale mixed wettability experiment testing device is composed of a constant-speed constant-pressure pump 1, a constant-speed constant-pressure pump outlet valve 2, an intermediate container 3, an intermediate container outlet valve 4, a vacuum pump 5, a vacuum pump inlet valve 6, a reaction kettle 7, a heater 8, a reaction kettle outlet valve 9, a rock core 10, a rock core holder 11, a cylindrical cushion block 12, a confining pressure pump 13 and a rock core holder outlet valve 14. The rock core 10 is placed in a lithology holder 11, one end face of the rock core is in contact with experimental liquid, the other end face of the rock core is in contact with a cylindrical cushion block 12, and confining pressure is loaded to the rock core 10 through a confining pressure pump 13 during experiment; heating experiment liquid and a rock core 10 in a reaction kettle 9 through a heating sleeve 8; the contact surface of the cylindrical cushion block 12 and the rock core is provided with a diversion trench, the center of the cushion block 12 is provided with an eyelet 12-1 for fluid to flow, and the fluid can flow to an outlet valve 14 of the rock core holder through the eyelet.
Detailed Description
The invention is further illustrated below with reference to the figures and examples.
Example 1
Embodiments of the invention are described in detail below with reference to the drawings and the downhole core of a shale well in the rampart of the Sichuan basin, by way of example. The method comprises the following specific steps:
(1) and preparing a core: actual underground rock cores at different positions of a Longmaxi reservoir section with the length of 2420-22460 m from an H1 well are respectively processed into standard rock cores S1-1 with the diameter of 2.5cm and the length of 5cm, and the standard rock cores are placed in a 100 ℃ drying oven to be dried to constant weight;
(2) and (3) testing the T of the dried rock core S1-1 in the step (1) by using a low-field nuclear magnetic resonance instrument2Obtaining the nuclear magnetic resonance signal area S of the original sample as 2152.91 by a graph curve;
(3) the temperature of a shale stratum of the H1 well is 80 ℃, the pressure of a stratum pore is 42MPa, the maximum horizontal well main stress is 46MPa, the minimum horizontal main stress is 38MPa, the vertical stress is 44MPa, and the effective stress coefficient is 0.5. The experimental temperature can be determined to be 80 ℃ according to the formation temperature, the maximum horizontal well effective main stress can be determined to be 25MPa, the minimum horizontal effective main stress can be determined to be 17MPa and the vertical effective stress can be determined to be 23MPa by using the formulas (1) to (3), and the experimental loading confining pressure can be determined to be 22MPa by using the formula (4);
(4) pouring the test liquid deionized water into an intermediate container 3 of a constant-speed constant-pressure pump, loading the tested rock core 10 in the step (2) into a rock core holder 11, and loading initial confining pressure of 5MPa to the rock core 10 by using a confining pressure pump 13;
(5) heating the core 10 and the core holder 11 to the experimental temperature determined in the step (3) by using a heater 8, and setting the loading pressure of a confining pressure pump 13 according to the confining pressure determined in the step (3);
(6) evacuating air in the pipeline and the reaction kettle 7 by using a vacuum pump 5, closing an inlet valve 6 of the vacuum pump after evacuation is finished, and pumping the experimental liquid deionized water in the intermediate container 3 into the reaction kettle 7 by using a constant-speed constant-pressure pump 1;
(7) after the end face of the core 10 and deionized water in the reaction kettle 7 are saturated for 48 hours, the pressure of the confining pressure pump 13 is unloaded, the heater 8 is turned off, the core 10 is taken out after being cooled for 2 hours, and the T is tested2Obtaining a hydrophilic signal area S of nuclear magnetic resonance of the rock core 10 by a graph curvews8866.16;
(8) using MnCl for the core 10 tested in the step (7)2The solution is saturated in a beaker at normal temperature and normal pressure for 24 hours;
(9) and (5) repeating the steps (4) - (7) on the saturated rock core 10 in the step (8), wherein the experimental liquid is oil, and testing the T of the saturated rock core 10 for 48 hours2Obtaining the nuclear magnetic resonance oleophylic signal area S of the rock core 10 rock sample by using a graph curveos5886.23;
(10) testing the nuclear magnetic resonance signal area S of the original sample and the nuclear magnetic resonance hydrophilic signal area S of the rock core 10 after saturated water according to the steps (2), (7) and (9)ws Core 10 NMR oleophilic signal area S after saturated oilosRespectively calculating the shale hydropathic index WI by using expressions (5) to (7)w0.64, lipophilicity index 0.36, mixed wettability index WIwoIs 0.28;
(11) the shale mixed wettability index WI calculated according to the step (10)wo0.28, which is greater than zero, and overall appears hydrophilic.
While the present invention has been described in detail by way of examples, it should be understood, however, that the present invention is not limited to the particular forms disclosed, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein. But all the modifications and simple changes made by those skilled in the art without departing from the technical idea and scope of the present invention belong to the protection scope of the technical solution of the present invention.
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| CN111175169A (en) * | 2019-12-31 | 2020-05-19 | 中国地质大学（北京） | Rock wettability evaluation method |
| CN113295569B (en) * | 2020-02-24 | 2023-04-25 | 中国石油天然气股份有限公司 | Shale oil-gas reservoir protection effect detection method and device |
| CN112112641B (en) * | 2020-10-10 | 2021-05-11 | 西南石油大学 | Experimental test method for soaking time of horizontal well of shale reservoir |
| CN112382345B (en) * | 2020-11-11 | 2023-06-06 | 东北石油大学 | A method and system for calculating contact angle of shale oil reservoir |
| CN112505085B (en) * | 2021-02-05 | 2021-04-09 | 西南石油大学 | Method for measuring porosity effective stress coefficient based on nuclear magnetic resonance |
| CN113820249B (en) * | 2021-11-22 | 2022-03-01 | 中国矿业大学(北京) | Device and method for evaluating wettability of sediment based on imbibition nuclear magnetic resonance |
| CN115616022B (en) * | 2022-10-10 | 2025-04-08 | 中国矿业大学(北京) | Shale mixing wettability evaluation method |
| CN117110349B (en) * | 2023-06-28 | 2024-05-28 | 东北石油大学 | A quantitative evaluation method for the wettability of multi-scale reservoir space in shale oil reservoir rocks |
| CN118392910B (en) * | 2024-06-27 | 2024-10-15 | 陕西延长石油（集团）有限责任公司 | Nuclear magnetic resonance-based compact oil microscopic pore wettability evaluation method |
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