CN110595953A - 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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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. 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 testing device and 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. Different from the conventional sandstone, the interaction between the fracturing fluid and the shale reservoir is more prominent and profound 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 flowback rate of fracturing fluid is low, the gas production rate and the flowback rate are in a negative correlation relationship, the water production after stewing is reduced, the gas production rate is increased, and the like (the influence of the open wave, the Lichen square, the Yangtze vertical peak and the shut-in opportunity on the flowback rate and the productivity of the shale gas well is J, the 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 a complex mixed wettability characteristic, 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 the factors are not considered simultaneously in the current experimental research, and most of the experimental research focuses on the shale surface wettability research under normal temperature and normal pressure. At present, the wettability test method mainly takes experiments as main points, and the specific contents are as follows:
(1) liu jun, etc. (Liu jun, bear jian, Lilianxi, Longma xi shale wettability analysis and influence discussion [ J ] natural gas earth science 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 core under the condition of normal temperature and heating, the research shows that the contact angle of shale and deionized water is 10.7-38.7 degrees, the white oil and diesel oil can be completely spread, the shale surface is both hydrophilic and oleophilic, the mixed wettability is shown, 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, 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 et al. shale wettability research and influence factor analysis [ J ] petroleum science and engineering based on nuclear magnetic resonance, 2018,169,309-316.) utilize nuclear magnetic resonance technology to qualitatively measure shale wettability, and analyze influence shale wettability control factors, and research shows that the existence of organic matters is the root cause of shale organic matter mineral oil wetting, and the pore formed by the organic matters and clay mineral leads the shale to have the characteristic of mixed wettability, and the content of inorganic mineral carbonate rock salt in the water-wet shale sample 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.
A shale mixed wettability experiment testing device comprises a formation temperature simulation system, a formation confining pressure simulation system and a mixed wettability testing system;
the formation temperature simulation system is a heater;
the stratum confining pressure simulation system is a confining pressure pump, and the confining pressure pump applies stratum confining pressure to the rock core through the rock core holder;
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, fluid is pumped into the reaction kettle by the constant-speed constant-pressure pump, and the vacuum pump applies pressure to the fluid in.
Further, the fluid pumped into the reaction kettle is deionized water or oil.
Furthermore, the experimental test device also comprises a cylindrical cushion block, a diversion trench is arranged on the contact surface of the cylindrical cushion block and the rock core, one end face of the rock core is in contact with the fluid in the reaction kettle during experimental test, and the other end face of the rock core is in contact with the cylindrical cushion block.
Further, the center of the cylindrical pad has an aperture for fluid flow therethrough to the core holder outlet valve.
Further, the experimental test device further comprises a vacuum pump and a vacuum pump inlet valve, wherein the vacuum pump and the vacuum pump inlet valve are sequentially connected to the reaction kettle.
An experimental test method for shale mixed wettability sequentially comprises the following steps:
(1) preparing a core: preparing a downhole core of a shale storage interval or a same-layer exposed rock into a core, and placing the core in an oven to dry to constant weight;
(2) testing the dried rock core T in the step (1) by using a low-field nuclear magnetic resonance instrument2Obtaining a nuclear magnetic resonance signal area S of the rock core by using a graph curve;
(3) determining an experiment loading condition according to the formation stress and the temperature, determining an experiment loading confining pressure according to the expressions (1) to (4), wherein the formation temperature is the experiment 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 vertical effective 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; pPIs the formation pore pressure, MPa;
(4) pouring fluid into an intermediate container of a constant-speed constant-pressure pump, loading the core tested in the step (2) into a core holder, and loading initial confining pressure on the 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 fluid in the intermediate container into the reaction kettle by using a constant-speed constant-pressure pump;
(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 in the step (8), wherein the fluid is replaced by oil, and testing the T after the saturated rock core2Obtaining 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 core nuclear magnetic resonance hydrophilic signal after water saturation is zero; sosThe area of a nuclear magnetic resonance oleophylic signal of the rock core after saturated oil is zero;
(11) and (4) comprehensively evaluating the shale mixed wettability according to the shale mixed wettability index calculated in the step (10).
Further, the comprehensive evaluation of the shale mixed wettability comprises the following steps:
when mixed wetting index WIwoWhen the shale is neutral, the shale is wet;
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 test device and method which simultaneously consider the influences of formation temperature and confining pressure, 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 test 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 shows NMR T of a shale core S1-1 of the present invention under different conditions2Graph curves.
Wherein, 1, a constant-speed constant-pressure pump; 2. a constant speed constant pressure pump outlet valve; 3. an intermediate container; 4. an intermediate container outlet valve; 5. a vacuum pump; 6. a vacuum pump inlet valve; 7. a reaction kettle; 8. a heater; 9. an outlet valve of the reaction kettle; 10. a core; 11. a core holder; 12. a cylindrical cushion block; 13. a confining pressure pump; 14. a core holder outlet valve.
Detailed Description
The details of the present invention can be more clearly understood in conjunction with the accompanying drawings and the description of the embodiments of the present invention. However, the specific embodiments of the present invention described herein are for the purpose of illustration only and are not to be construed as limiting the invention in any way. Any possible variations on the invention may be conceived by the skilled person in the light of the teachings of the invention, and these should be considered to fall within the scope of the invention.
The utility model provides a shale mixes wettability experiment testing arrangement is by constant speed constant pressure pump 1, includes constant speed constant pressure pump outlet valve 2, intermediate container 3, intermediate container outlet valve 4, vacuum pump 5, vacuum pump inlet valve 6, reation kettle 7, heater 8, reation kettle outlet valve 9, rock core 10, core holder 11, cylindrical cushion 12, confined pressure pump 13, core holder outlet valve 14.
Wherein, the heater 8 is used for heating the experimental test device to simulate the formation temperature.
The confining pressure pump 13 applies formation confining pressure to the core 10 through the core holder 11 to simulate formation confining pressure experienced by downhole rock.
The constant-speed constant-pressure pump 1, the constant-speed constant-pressure pump outlet valve 2, the intermediate container 3 and the intermediate container outlet valve 4 form a mixed wettability testing system of the experimental testing device through the reaction kettle 7. Wherein the constant-speed constant-pressure pump 1, the constant-speed constant-pressure pump outlet valve 2, the intermediate container 3 and the intermediate container outlet valve 4 are sequentially connected to the reaction kettle 5, and the vacuum pump 5 and the vacuum pump inlet valve 6 are sequentially connected to the reaction kettle 5. And pumping fluid into the reaction kettle 6 by the constant-speed constant-pressure pump 1, wherein the pumped fluid is respectively deionized water or oil according to experimental requirements so as to test different wettabilities of the rock core.
During experimental test, the core 10 is placed in the core holder 11, one end surface is in contact with experimental liquid, the other end surface is in contact with the cylindrical cushion block 12, a diversion trench is arranged on the contact surface of the cylindrical cushion block 12 and the core 10, a hole for fluid to flow is formed in the center of the cylindrical cushion block 12, and the fluid can flow to the outlet valve 14 of the core holder through the hole.
When the experimental device is used for testing the shale mixing wettability, the method sequentially comprises the following steps:
(1) preparing a core: preparing a downhole core of a shale storage interval or a same-layer exposed rock into a core, and placing the core in an oven to dry to constant weight; when the core is prepared, the core can be prepared into a standard core with the diameter of 2.5cm and the length of 5cm, and the standard core is placed in an oven at 100 ℃ and dried 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 expression formulas (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 vertical effective stress, MPa; sigma'HMaximum horizontal effective principal stress, MPa; sigma'hIs the minimum level effective principal stress, MPa;σzis 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 core nuclear magnetic resonance hydrophilic signal after water saturation 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 whole shale is hydrophilic, and the larger the value is, the stronger the hydrophilicity of the rock core is; when WI iswoLess than 0, the integral shale is oleophilic, and the smaller the value, the stronger the oleophilicity of the rock core.
Example calculation
In order to facilitate the understanding of technical solutions and advantages of the present invention for those skilled in the art, a shale downhole core of a longmaxi section of the four-Sichuan basin is taken as an example to describe in detail a specific embodiment of the present invention. The method comprises the following steps:
(1) and preparing a core: actual underground rock cores at different positions of a Kyoma xi reservoir section of 2.5cm in diameter and 5cm in length are respectively processed into standard rock cores S1-1, and the standard rock cores are placed in an oven at 100 ℃ and 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 the graph spectrum curve;
(3) the shale formation temperature of the XXX well is 80 ℃, the formation pore pressure 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, 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 the 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)wsCore 10 NMR oleophilic signal area S after saturated oilosUse of the watchRespectively calculating shale hydropathic index WI by the expressions (5) to (7)w0.64, oleophilic 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 the embodiments, it should be understood that the present invention is not limited to the embodiments disclosed herein, but is intended to cover other embodiments as well. 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.
Claims (7)
1. A shale mixed wettability experiment testing device comprises a formation temperature simulation system, a formation confining pressure simulation system and a mixed wettability testing system;
the formation temperature simulation system is a heater;
the stratum confining pressure simulation system is a confining pressure pump, and the confining pressure pump applies stratum confining pressure to the rock core through the rock core holder;
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, and fluid is pumped into the reaction kettle by the constant-speed constant-pressure pump.
2. The shale mixing wettability experiment testing apparatus of claim 1, wherein the fluid pumped into the reaction kettle is deionized water or oil.
3. The shale mixed wettability experiment testing device as claimed in claim 1, further comprising a cylindrical cushion block, wherein a diversion trench is arranged on a contact surface of the cylindrical cushion block and the rock core, one end surface of the rock core is in contact with fluid in the reaction kettle during experiment testing, and the other end surface of the rock core is in contact with the cylindrical cushion block.
4. The shale mixing wettability experiment testing device as claimed in claim 3, wherein a hole for fluid flow is formed in the center of the cylindrical pad, and fluid can flow to the outlet valve of the core holder through the hole.
5. The experimental testing device for shale mixing wettability of claim 1, further comprising a vacuum pump and a vacuum pump inlet valve, wherein the vacuum pump and the vacuum pump inlet valve are sequentially connected to the reaction kettle.
6. A shale mixed wettability experiment test method which adopts the shale mixed wettability experiment test of any one of claims 1 to 5 and sequentially comprises the following steps:
(1) preparing a core: preparing a rock core from a downhole rock pillar of a shale storage layer section or a rock with a head exposed at the same layer position, and placing the rock core in an oven to dry to constant weight;
(2) testing the dried rock core T in the step (1) by using a low-field nuclear magnetic resonance instrument2Obtaining a nuclear magnetic resonance signal area S of the rock core by using a graph curve;
(3) determining an experiment loading condition according to the formation stress and the temperature, determining an experiment loading confining pressure according to the expressions (1) to (4), wherein the formation temperature is the experiment 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 vertical effective stress, MPa; sigmaHMaximum horizontal effective principal stress, MPa; sigma'hIs the minimum level effective principal stress, MPa; sigmazIs vertical stress, MPa; sigmaHMaximum horizontal principal stress, MPa; sigmahTo a minimumHorizontal principal stress, MPa; alpha is the effective stress coefficient, decimal; sigmaEncloseIs experimental confining pressure, MPa; pPIs the formation pore pressure, MPa;
(4) pouring fluid into an intermediate container of a constant-speed constant-pressure pump, loading the core tested in the step (2) into a core holder, and loading initial confining pressure on the 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 fluid in the intermediate container into the reaction kettle by using a constant-speed constant-pressure pump;
(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 in the step (8), wherein the fluid is replaced by oil, and testing the T after the rock core is saturated2Obtaining 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;WIwothe 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;
(11) and (4) comprehensively evaluating the shale mixed wettability according to the shale mixed wettability index calculated in the step (10).
7. The test method of claim 6, wherein the comprehensive evaluation of shale mixed wettability comprises:
when mixed wetting index WIwoWhen the shale is neutral, the shale is wet;
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.
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