CN117433977B - Supercritical CO 2 Device and method for detecting in-situ permeability of shale reaction - Google Patents
Supercritical CO 2 Device and method for detecting in-situ permeability of shale reaction Download PDFInfo
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- 230000035699 permeability Effects 0.000 title claims abstract description 42
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 36
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title abstract description 16
- 230000000087 stabilizing effect Effects 0.000 claims abstract description 14
- 238000006073 displacement reaction Methods 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 76
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 34
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- 238000001514 detection method Methods 0.000 claims description 9
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 4
- 238000012360 testing method Methods 0.000 abstract description 15
- 238000005516 engineering process Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 3
- 239000011435 rock Substances 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/082—Investigating permeability by forcing a fluid through a sample
- G01N15/0826—Investigating permeability by forcing a fluid through a sample and measuring fluid flow rate, i.e. permeation rate or pressure change
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N7/10—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing diffusion of components through a porous wall and measuring a pressure or volume difference
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P90/00—Enabling technologies with a potential contribution to greenhouse gas [GHG] emissions mitigation
- Y02P90/70—Combining sequestration of CO2 and exploitation of hydrocarbons by injecting CO2 or carbonated water in oil wells
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Abstract
The invention belongs to the technical field of shale gas exploitation, and provides a supercritical CO 2 Device and method for detecting in-situ permeability of shale reaction, pressure stabilizing tank and CO filling 2 Both the intermediate container and the core holder are positioned in the incubator; the outlet end of the booster pump is communicated with the air inlet of the pressure stabilizing tank; the air outlet of the pressure stabilizing tank is connected with a valve I of the three-way valve; the intermediate container is provided with a bottom bin and a top bin, and the top bin is filled with CO 2 A piston which can be driven by pressure is arranged in the middle; the displacement pump is communicated with a liquid inlet at the bottom end of the intermediate container; the outlet at the top of the middle container is connected with a second valve of the three-way valve; the core holder is provided with a confining pressure loading portThe gas inlet is connected with a valve III of the three-way valve. The invention can ensure the supercritical CO 2 The method can fully react with the shale core at preset temperature and pressure, and can also realize accurate permeability test under in-situ high-temperature and high-pressure conditions.
Description
Technical Field
The invention provides a supercritical CO 2 The invention discloses a device and a method for detecting in-situ permeability of shale reaction, and belongs to the technical field of shale gas exploitation.
Background
Unlike conventional hydrocarbon reservoirs, shale reservoirs have very low porosity and permeability, develop a large number of nanoscale pores, and can be produced industrially by means of horizontal well hydraulic fracturing technology. The existing shale gas horizontal well hydraulic fracturing technology has the problems of large water consumption, reservoir damage, difficult treatment of flowback water and the like, and the 'low water' or 'anhydrous' green fracturing technology is required to be sought.
Research has shown that supercritical CO 2 The fracturing is a fracturing technology with extremely low water consumption and stronger seam making capability, and supercritical CO 2 The injection into shale gas reservoir not only can effectively improve the shale gas recovery ratio, but also can simultaneously inject a large amount of CO 2 Sealed in the underground reservoir space, and effectively reduces carbon emission. Supercritical stateCO 2 After entering the shale reservoir, a series of complex physicochemical reactions with the rock minerals in the reservoir can occur during long-term contact, thereby causing reservoir permeability changes. Clear supercritical CO 2 The variation rule of shale permeability after reaction is an important basis for realizing dynamic and accurate prediction and analysis of shale gas well postpressure production.
Existing test methods in the literature are all to test and supercritical CO under relatively low temperature and low pressure conditions 2 The permeability of the shale rock sample after reaction is greatly different from the in-situ high-temperature and high-pressure condition of a shale reservoir, the temperature and the pressure have obvious influence on the permeability of the reservoir rock, and the supercritical CO under the high-temperature and high-pressure condition of the reservoir is estimated by using the test result under the low-pressure condition 2 The effect on shale permeability may be subject to large errors.
Patent CN108760602A provides a method for utilizing supercritical CO 2 An anti-reflection ultra-low permeability compact shale test system and method have the following disadvantages: the pressure of the gas cylinder is limited, the conventional upper limit pressure is not more than 15MPa, and supercritical CO under high-temperature and high-pressure conditions of a real shale reservoir cannot be effectively simulated 2 Interactions with shale; failure to achieve supercritical CO under high temperature and high pressure conditions 2 And testing shale permeability before and after action.
Disclosure of Invention
The present invention provides a supercritical CO for solving the above technical problems 2 An in-situ permeability detection device and method for reaction with shale. Typically sample and supercritical CO 2 The reaction is carried out under specific temperature and pressure, after the reaction is finished, the sample is taken out, and the permeability is measured by nitrogen under the condition of normal temperature and low pressure, so that the measurement result is inevitably distorted. By using the experimental device and the method disclosed by the invention, the supercritical CO can be ensured 2 The shale permeability testing process is carried out in the same temperature and pressure environment after the reaction with the shale, so that the supercritical CO can be ensured 2 The method can fully react with the shale core at preset temperature and pressure, and can also realize accurate permeability test under in-situ high-temperature and high-pressure conditions.
The invention adopts the following technical scheme:
supercritical CO 2 The in-situ permeability detection device for the reaction with shale comprises a nitrogen cylinder, a booster pump, a surge tank, an intermediate container, a core holder, a confining pressure pump, a displacement pump, a gas flowmeter and an incubator;
pressure stabilizing tank filled with CO 2 Both the intermediate container and the core holder are positioned in the incubator.
The outlet end of the booster pump is communicated with the air inlet of the pressure stabilizing tank; the air outlet of the pressure stabilizing tank is connected with a valve I of the three-way valve;
the intermediate container is provided with a bottom bin and a top bin, and the top bin is filled with CO 2 A piston which can be driven by pressure is arranged in the middle. The displacement pump is communicated with a liquid inlet at the bottom end of the intermediate container, and the top CO is discharged through a piston in the middle of the intermediate container 2 The pressure applied by the air bin reaches a preset value. The outlet at the top of the middle container is connected with a second valve of the three-way valve;
the shale sample is sealed and clamped in the core holder, a confining pressure loading port is arranged on the core holder, and the confining pressure pump applies confining pressure to the ultralow permeability compact shale sample in the core holder through the confining pressure loading port. The core holder is also provided with a gas inlet and a gas outlet respectively, the gas inlet of the core holder is connected with a valve III of the three-way valve, and the effect of controlling different fluids to enter the core holder is achieved by opening or closing the corresponding switch;
a first stop valve and a first pressure gauge are respectively arranged on a pipeline between the gas outlet of the nitrogen gas cylinder and the gas inlet of the pressure stabilizing tank; a second pressure gauge is arranged between the gas outlet at the top of the intermediate container and a second valve pipeline of the three-way valve, a third pressure gauge is arranged on a pipeline between a third valve of the three-way valve and an inlet of the core holder, and a fourth pressure gauge and a second stop valve are respectively arranged on a pipeline between an outlet of the core holder and an inlet of the gas flowmeter; and a fifth pressure gauge and a third stop valve are respectively arranged on a pipeline between the confining pressure loading port of the core holder and the confining pressure pump. The top of the intermediate container is provided with a thermometer, and the CO in the top bin of the intermediate container is monitored in real time through the thermometer 2 The temperature of the gas.
Supercritical CO 2 The in-situ permeability detection method for the reaction with shale specifically comprises the following steps:
step one: starting the constant temperature box, controlling the temperature in the box to a preset temperature (determined according to the actual shale gas reservoir temperature), and enabling a first valve, a second valve, a third valve and a first valve, a second valve and a third valve of the three-way valve to be in a closed state;
step two: opening a nitrogen cylinder and a booster pump, simultaneously opening a first stop valve, filling nitrogen gas into a pressure stabilizing tank, and waiting for 30min after the pressure reaches a preset value until the gas state in the tank is stable; the preset value is determined according to the actual shale gas reservoir pressure;
step three: turning on the displacement pump to drive CO in the top bin of the intermediate container by using constant pressure mode 2 Pressurizing the gas to a preset pressure (determined according to the actual shale gas reservoir pressure and equal to the pressure in the second step), and under the conditions of the actual shale reservoir pressure and the actual shale gas reservoir temperature, CO in the top bin of the intermediate container 2 The gas is in a supercritical state; step three and step two can be performed simultaneously;
step four: and opening a third stop valve, and applying confining pressure to the shale sample in the core holder through a confining pressure pump, wherein the confining pressure is usually 2-3 MPa higher than the inlet pressure of the core holder. After waiting for at least 30min until the deformation of the shale sample is stable, closing a third stop valve;
step five: and opening a first valve and a third valve of the three-way valve to enable nitrogen to enter the core holder. Simultaneously opening a second stop valve, observing readings of a third pressure gauge, a fourth pressure gauge and a gas flowmeter, and recording the inlet pressure P of the clamp holder after the pressure and the flow reach stability 1 Outlet pressure P 2 A gas flow rate q;
step six: the CO is calculated according to the following formula 2 Permeability k of shale sample prior to reaction with shale:
k＝(2*q*μ*L*P 0 )/{A*[(P 1 +P 0 ) 2 -(P 2 +P 0 ) 2 ]}*10 2
wherein: k-permeability in millidarcy (mD);
a-shale sample cross-sectional area in square centimeters (cm) 2 )；
P 0 -measured atmospheric pressure in megapascals (MPa);
P 1 -inlet pressure in megapascals (MPa);
P 2 -outlet pressure in megapascals (MPa);
l-shale sample length in centimeters (cm);
mu-viscosity of the test gas at the current temperature in millipascal seconds (mPas);
q-gas flow per unit time in milliliters per second (mL/s);
step seven: closing a first valve of the three-way valve, opening a second valve to enable supercritical CO in a top bin of the intermediate container 2 Gas flows into the core holder inlet;
step eight: observing the readings of a third pressure gauge, a fourth pressure gauge and a gas flowmeter, keeping for 10 minutes after the pressure and the flow reach stability, and then sequentially closing a second stop valve, a second valve and a third valve of the three-way valve to enable supercritical CO to be obtained 2 Fully contacting and reacting with the shale sample;
step nine: to be supercritical CO 2 After the contact reaction with the shale sample reaches the set time, repeating the steps five to six, and measuring and recording the inlet pressure P of the clamp holder 1 ' outlet pressure P 2 'steady gas flow q' through core, calculating supercritical CO according to the formula in step six 2 Permeability k' of shale sample after reaction with shale.
The booster pump in the detection device provided by the invention can effectively solve the problem that the air source pressure cannot exceed 15MPa, the booster pump can boost and output a low-pressure air source (such as the air bottle pressure below 15 MPa) to a set high-pressure condition (the upper limit is 100 MPa), and the booster pump can be utilized to boost the air to a high-pressure environment preset in an experiment.
Supercritical CO 2 The fracturing shale reservoir can effectively solve the problem of large water consumption of hydraulic fracturing of the conventional shale reservoir, and can improve shale gasThe underground sealing and storage of carbon dioxide gas are realized while the recovery ratio is reserved. Clear supercritical CO 2 Shale permeability change after shale interaction, shale gas well postpressure production dynamic prediction, shale gas recovery rate improvement and CO realization 2 Effective sealing is important.
The invention can ensure supercritical CO 2 The shale permeability measuring process is carried out in the same temperature and pressure environment before and after the shale reaction, so that supercritical CO can be ensured 2 The method is fully contacted with the shale sample for reaction under the conditions of real reservoir temperature and pressure, and can also realize accurate testing of shale permeability of the reservoir in situ under high temperature and high pressure environments before and after reaction. The technology dynamically predicts shale gas well postpressure and CO 2 The effective sealing evaluation has important significance.
Drawings
FIG. 1 is a schematic view of the structure of the device of the present invention;
the reference numerals are: the core holder 1, the surge tank 2, the nitrogen cylinder 3, the intermediate container 4, the displacement pump 5, the three-way valve 6, the confining pressure pump 7, the gas flowmeter 8, the incubator 9, the first pressure gauge 10, the second pressure gauge 11, the third pressure gauge 12, the fourth pressure gauge 13, the fifth pressure gauge 14, the first valve 15, the second valve 16, the third valve 17, the first stop valve 18, the second stop valve 19, the third stop valve 20, the thermometer 21 and the booster pump 22.
Detailed Description
The specific technical scheme of the invention is described with reference to the accompanying drawings.
As shown in FIG. 1, a supercritical CO 2 The in-situ permeability detection device for the reaction with shale comprises a nitrogen cylinder 3, a booster pump 22, a surge tank 2, an intermediate container 4, a core holder 1, a confining pressure pump 7, a displacement pump 5, a gas flowmeter 8 and an incubator 9;
surge tank 2 filled with CO 2 Both the intermediate container 4 and the core holder 1 are located in an incubator 9.
The air outlet of the nitrogen cylinder 3 is communicated with the inlet end of the booster pump 22, and the outlet end of the booster pump 22 is communicated with the air inlet of the pressure stabilizing tank 2; the air outlet of the pressure stabilizing tank 2 is connected with a valve 15 of the three-way valve 6;
the intermediate container 4 is provided with a bottom bin and a top bin, and the top bin is filled with CO 2 A piston which can be driven by pressure is arranged in the middle. The displacement pump 5 is communicated with a liquid inlet at the bottom end of the intermediate container 4, and the top CO is arranged at the top through a piston in the middle of the intermediate container 4 2 The pressure applied by the air bin reaches a preset value. The outlet at the top of the intermediate container 4 is connected with a valve II 16 of the three-way valve 6;
the shale sample is sealed and clamped in the core holder 1, a confining pressure loading port is arranged on the core holder 1, and a confining pressure pump 7 applies confining pressure to the ultra-low permeability compact shale sample in the core holder 1 through the confining pressure loading port. The core holder 1 is also provided with a gas inlet and a gas outlet respectively, the gas inlet of the core holder 1 is connected with a valve No. three 17 of the three-way valve 6, and the effect of controlling different fluids to enter the core holder 1 is achieved by opening or closing corresponding switches;
a first stop valve 18 and a first pressure gauge 10 are respectively arranged on a pipeline between the air outlet of the nitrogen cylinder 3 and the air inlet of the surge tank 2; a second pressure gauge 11 is arranged between the air outlet at the top of the intermediate container 4 and a pipeline of a valve II 16 of the three-way valve 6, a third pressure gauge 12 is arranged on a pipeline between a valve III 17 of the three-way valve 6 and an inlet of the core holder 1, and a fourth pressure gauge 13 and a second stop valve 19 are respectively arranged on a pipeline between an outlet of the core holder 1 and an inlet of the gas flowmeter 8; a fifth pressure gauge 14 and a third stop valve 20 are respectively arranged on the pipeline between the confining pressure loading port of the core holder 1 and the confining pressure pump 7. A thermometer 21 is arranged at the top of the intermediate container 4, and CO in the top bin of the intermediate container 4 is monitored in real time through the thermometer 21 2 The temperature of the gas.
By using the device, supercritical CO is carried out 2 The in-situ permeability detection method for the reaction with shale specifically comprises the following steps:
step one: the thermostat 9 is started, the temperature in the thermostat is controlled to a preset temperature (determined according to the actual shale gas reservoir temperature), and the first stop valve 18, the second stop valve 19, the third stop valve 20, the first valve 15, the second valve 16 and the third valve 17 of the three-way valve 6 are all in a closed state;
step two: opening the nitrogen cylinder 3 and the booster pump 22, simultaneously opening the first stop valve 18, filling nitrogen gas into the surge tank 2, and waiting for 30 minutes until the gas state in the tank is stable after the pressure reaches a preset value (determined according to the actual shale gas reservoir pressure);
step three: turning on the displacement pump 5 to use constant pressure mode to drive CO in the top bin of the intermediate container 4 2 Pressurizing the gas to a preset pressure (determined according to the actual shale gas reservoir pressure and equal to the pressure in the second step), and under the conditions of the actual shale reservoir pressure and the actual shale gas reservoir temperature, CO in the top bin of the intermediate container 4 2 The gas is in a supercritical state; step three and step two can be performed simultaneously;
step four: the third stop valve 20 is opened, and a confining pressure is applied to the shale sample in the core holder 1 by the confining pressure pump 7, wherein the confining pressure is generally 2-3 MPa higher than the inlet pressure of the core holder 1. After waiting at least 30min until the deformation of the shale sample is stable, closing the third stop valve 20;
step five: and opening a first valve 15 and a third valve 17 of the three-way valve 6 to enable nitrogen to enter the core holder 1. Simultaneously opening the second stop valve 19, observing the readings of the third pressure gauge 12, the fourth pressure gauge 13 and the gas flowmeter 8, and recording the inlet pressure P of the clamp after the pressure and the flow reach stability 1 Outlet pressure P 2 A gas flow rate q;
step six: the CO is calculated according to the following formula 2 Permeability k of shale sample prior to reaction with shale:
k＝(2*q*μ*L*P 0 )/{A*[(P 1 +P 0 ) 2 -(P 2 +P 0 ) 2 ]}*10 2
wherein: k-permeability in millidarcy (mD);
a-shale sample cross-sectional area in square centimeters (cm) 2 )；
P 0 -measured atmospheric pressure in megapascals (MPa);
P 1 -inlet pressure in megapascals (MPa);
P 2 -outlet pressure in megapascals (MPa);
l-shale sample length in centimeters (cm);
mu-viscosity of the test gas at the current temperature in millipascal seconds (mPas);
q-gas flow per unit time in milliliters per second (mL/s);
step seven: closing the valve number one 15 of the three-way valve 6, and opening the valve number two 16 to enable supercritical CO in the top bin of the intermediate container 4 2 Gas flows into the inlet of the core holder 1;
step eight: observing the readings of the third pressure gauge 12, the fourth pressure gauge 13 and the gas flowmeter 8, keeping for 10 minutes after the pressure and the flow reach the stable state, and then sequentially closing the second stop valve 19, the second valve 16 and the third valve 17 of the three-way valve 6 to enable supercritical CO to be discharged 2 Fully contacting and reacting with the shale sample;
step nine: to be supercritical CO 2 After the contact reaction with the shale sample reaches the set time, repeating the steps five to six, and measuring and recording the inlet pressure P of the clamp holder 1 ' outlet pressure P 2 'steady gas flow q' through core, calculating supercritical CO according to the formula in step six 2 Permeability k' of shale sample after reaction with shale.
By supercritical CO 2 In practice of fracturing to improve shale gas reservoir recovery ratio, supercritical CO 2 Contact with the shale reservoir and reaction are all carried out under high temperature and pressure conditions of the reservoir. To accurately evaluate and predict supercritical CO 2 Shale gas well production dynamics after reaction with shale requires accurate acquisition of supercritical CO 2 Shale permeability after action, under in situ high temperature and pressure conditions of the reservoir. Existing experimental device and method in literature for supercritical CO 2 Reacts with shale and supercritical CO 2 The shale permeability test after the reaction is often carried out separately, namely supercritical CO under high temperature and high pressure conditions 2 After the reaction with shale, taking out the shale sample, and testing the permeability of the shale sample by using nitrogen under the low-temperature and low-pressure conditions, wherein the obtained permeability test result has a larger difference from the permeability test result under the high-temperature and high-pressure conditions, so that the dynamic prediction of gas well production has a larger deviation. The invention realizes different fluid delivery through the three-way valve 6The parallel connection of the equipment can ensure the supercritical CO 2 The shale permeability measurement process is carried out in the same temperature and pressure environment after the shale reaction, and can truly simulate the supercritical CO under the conditions of the temperature and the pressure of a real reservoir 2 And the method reacts with shale samples, and can also realize accurate testing of shale permeability before and after reaction under the conditions of real reservoir temperature and pressure.
Claims (2)
1. Supercritical CO 2 The in-situ permeability detection device for the shale reaction is characterized by comprising a nitrogen gas cylinder (3), a booster pump (22), a pressure stabilizing tank (2), an intermediate container (4), a core holder (1), a confining pressure pump (7), a displacement pump (5), a gas flowmeter (8) and a constant temperature box (9);
pressure stabilizing tank (2) filled with CO 2 The intermediate container (4) and the core holder (1) are both positioned in the incubator (9);
the air outlet of the nitrogen cylinder (3) is communicated with the inlet end of the booster pump (22), and the outlet end of the booster pump (22) is communicated with the air inlet of the surge tank (2); the air outlet of the pressure stabilizing tank (2) is connected with a valve I (15) of the three-way valve (6);
the intermediate container (4) is provided with a bottom bin and a top bin, and the top bin is filled with CO 2 A piston which can be driven by pressure is arranged in the middle; the displacement pump (5) is communicated with a liquid inlet at the bottom end of the intermediate container (4), and the top CO is opposite to the top CO through a piston in the middle of the intermediate container (4) 2 The pressure applied by the air bin reaches a preset value; the top outlet of the intermediate container (4) is connected with a second valve (16) of the three-way valve (6);
the shale sample is sealed and clamped in the core holder (1), a confining pressure loading port is arranged on the core holder (1), and a confining pressure pump (7) applies confining pressure to the ultralow-permeability compact shale sample in the core holder (1) through the confining pressure loading port; the core holder (1) is also provided with a gas inlet and a gas outlet respectively, the gas inlet of the core holder (1) is connected with a valve III (17) of the three-way valve (6), and the effect of controlling different fluids to enter the core holder (1) is achieved by opening or closing the corresponding switch;
a first stop valve (18) and a first pressure gauge (10) are respectively arranged on a pipeline between the air outlet of the nitrogen gas cylinder (3) and the air inlet of the pressure stabilizing tank (2); a second pressure gauge (11) is arranged between a gas outlet at the top of the intermediate container (4) and a pipeline of a second valve (16) of the three-way valve (6), a third pressure gauge (12) is arranged on a pipeline between a third valve (17) of the three-way valve (6) and an inlet of the core holder (1), and a fourth pressure gauge (13) and a second stop valve (19) are respectively arranged on a pipeline between an outlet of the core holder (1) and an inlet of the gas flowmeter (8); a fifth pressure gauge (14) and a third stop valve (20) are respectively arranged on a pipeline between the confining pressure loading port of the core holder (1) and the confining pressure pump (7); a thermometer (21) is arranged at the top of the intermediate container (4), and the CO in the top bin of the intermediate container (4) is monitored in real time through the thermometer (21) 2 The temperature of the gas.
2. Supercritical CO 2 An in-situ permeability detection method for shale reaction, characterized in that the supercritical CO as claimed in claim 1 is adopted 2 The in-situ permeability detection device for reaction with shale comprises the following steps:
step one: starting a constant temperature box (9) to control the temperature in the box to a preset temperature; the preset value is determined according to the actual shale gas reservoir temperature; the first stop valve (18), the second stop valve (19), the third stop valve (20) and the first valve (15), the second valve (16) and the third valve (17) of the three-way valve (6) are all in a closed state;
step two: opening a nitrogen cylinder (3) and a booster pump (22), simultaneously opening a first stop valve (18), filling nitrogen gas into a surge tank (2), and waiting for 30min after the pressure reaches a preset value until the gas state in the tank is stable; the preset value is determined according to the actual shale gas reservoir pressure;
step three: turning on a displacement pump (5) to use a constant pressure mode to drive CO in a top bin of an intermediate container (4) 2 Pressurizing the gas to a preset pressure, and under the conditions of actual shale reservoir pressure and temperature, obtaining an intermediate capacityCO in the top bin of the device (4) 2 The gas is in a supercritical state;
or the third step and the second step are carried out simultaneously;
step four: opening a third stop valve (20), and applying confining pressure to the shale sample in the core holder (1) through a confining pressure pump (7), wherein the confining pressure is 2-3 MPa higher than the inlet pressure of the core holder (1); closing the third stop valve (20) after waiting at least 30 minutes until the deformation of the shale sample is stable;
step five: opening a first valve (15) and a third valve (17) of the three-way valve (6) to enable nitrogen to enter the core holder (1); simultaneously opening a second stop valve (19), observing the readings of a third pressure gauge (12), a fourth pressure gauge (13) and a gas flowmeter (8), and recording the inlet pressure P of the clamp holder after the pressure and the flow reach stability 1 Outlet pressure P 2 A gas flow rate q;
step six: the CO is calculated according to the following formula 2 Permeability k of shale sample prior to reaction with shale:
k=(2*q*μ*L*P 0 )/{A*[( P 1 + P 0 ) 2 -( P 2 + P 0 ) 2 ]}*10 2 ；
wherein: k-permeability in millidarcy (mD);
a-shale sample cross-sectional area in square cm, cm 2 ；
P 0 -measured atmospheric pressure in MPa;
P 1 inlet pressure in MPa;
P 2 outlet pressure in MPa;
the length of the L-shale sample is in cm;
mu-viscosity of the experimental gas at the current temperature, wherein the unit is milliPa sec, mPa.s;
q-gas flow per unit time in milliliters per second, mL/s;
step seven: the valve number one (15) of the three-way valve (6) is closed, the valve number two (16) is opened, and the top bin of the intermediate container (4) is enabled to be inSupercritical CO 2 The gas flows into the inlet of the core holder (1);
step eight: observing the readings of the third pressure gauge (12), the fourth pressure gauge (13) and the gas flowmeter (8), keeping for 10 minutes after the pressure and the flow reach the stability, and then sequentially closing the second stop valve (19), the second valve (16) and the third valve (17) of the three-way valve (6) to enable supercritical CO to be discharged 2 Fully contacting and reacting with the shale sample;
step nine: to be supercritical CO 2 After the contact reaction with the shale sample reaches the set time, repeating the steps five to six, and measuring and recording the inlet pressure P of the clamp holder 1 ' outlet pressure P 2 'steady gas flow q' through core, calculating supercritical CO according to the formula in step six 2 Permeability k' of shale sample after reaction with shale.
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