CN106525687B - Supercritical carbon dioxide soaks shale experimental apparatus - Google Patents

Supercritical carbon dioxide soaks shale experimental apparatus Download PDF

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CN106525687B
CN106525687B CN201610968585.5A CN201610968585A CN106525687B CN 106525687 B CN106525687 B CN 106525687B CN 201610968585 A CN201610968585 A CN 201610968585A CN 106525687 B CN106525687 B CN 106525687B
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pressure
carbon dioxide
shale
bearing container
heating
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CN106525687A (en
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康勇
蔡灿
王晓川
胡毅
黄满
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Wuhan University WHU
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    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
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    • G01N15/082Investigating permeability by forcing a fluid through a sample

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Abstract

The invention discloses an experimental device for soaking shale with supercritical carbon dioxide, which comprises an end enclosure and a pressure-bearing container barrel positioned below the end enclosure, wherein a safety accessory is arranged on the end enclosure, the end enclosure is connected with the pressure-bearing container barrel through a flange, a heating sleeve for heating and keeping constant temperature is arranged in the pressure-bearing container barrel, the heating sleeve and the pressure-bearing container barrel form a double-layer structure for separating heating and pressure bearing, a rock sample fixing basket for containing and fixing rock samples is arranged in the inner space of the heating sleeve, and an inlet pipe and an outlet pipe with a stop valve are arranged on the side wall of the pressure-bearing container barrel. The heating sleeve comprises a base body made of ceramic material and a spiral heating coil arranged in the base body. The device also considers the shale soaking experiment under the influence of water saturation, and a visible transparent water tank is connected to the inlet pipeline of the container. The device is small in size, the temperature and the pressure can be flexibly adjusted, and the soaked shale is convenient to carry to a shale mechanical property experiment place for subsequent experiments.

Description

Supercritical carbon dioxide soaks shale experimental apparatus
Technical Field
The invention relates to an experimental device for soaking shale, in particular to an experimental device for soaking shale in supercritical carbon dioxide. And the soaking temperature and pressure can be adjusted according to the subsequent mechanical experiment requirements of the rock sample.
Background
Because the supercritical carbon dioxide has low viscosity, high diffusivity and small damage to a reservoir, the yield of the shale gas can be obviously improved, and the industrially generated carbon dioxide can be permanently sealed in a deep stratum when the shale gas is developed, the development of the shale gas by the supercritical carbon dioxide is considered as a key technology for the development of the shale gas in the future. The interaction mechanism between the supercritical carbon dioxide and the rock is the basic problem of 'efficient development of shale gas by supercritical carbon dioxide' in the national 973 project, so that a series of experimental researches on rock mechanics and microstructures are urgently needed.
However, most of the current domestic and foreign research on rock mechanics and microstructures is carried out on the basis of no effect of supercritical carbon dioxide, and is not consistent with the actual working condition that the stratum is infiltrated in a supercritical carbon dioxide medium. Therefore, experts at home and abroadThe mechanical testing of shale has been conducted in an effort to place shale in an environment of high temperature, high pressure and fracturing fluids similar to deep substrates. The research on the fracturing of the shale by the supercritical carbon dioxide is still in an initial stage at home and abroad, and related shale soaking experimental devices are also in a blank stage. An Australian scholars adds a carbon dioxide gas injection device on an original rock mechanics triaxial apparatus so as to establish an interaction environment of supercritical carbon dioxide and rocks. Due to the limitation of the function of the triaxial apparatus, the pressure can only reach about 7Mpa, and the method can not meet the requirements of supercritical carbon dioxide at high pressure (more than 7 Mpa) and temperature (more than 40 MPa) higher than the environment temperatureO) Mechanical experimental requirements within the range. Meanwhile, due to the limitation of a triaxial apparatus, the soaked rock sample cannot be used for carrying out other tensile strength and shear strength experiments, and is very unfavorable for researching the mechanical properties of the shale under the action of supercritical carbon dioxide.
Therefore, the development of the supercritical carbon dioxide shale soaking experimental device with adjustable pressure and temperature is very important for promoting the basic research of the 973 project and improving the shale gas development technology. And this kind of device still need separate with triaxial experimental apparatus, portable is favorable to developing rock compressive strength, tensile strength and shear strength experiment.
Disclosure of Invention
The invention aims to solve the technical problem of designing and manufacturing a portable supercritical carbon dioxide soaked shale experimental device, which not only can flexibly control the temperature and the pressure of the soaked shale, but also has the advantages of small volume, corrosion resistance and convenient carrying so as to be convenient for developing the later rock mechanics experiment.
According to the research requirement of 'high-efficiency development of shale gas by supercritical carbon dioxide' in the current 973 project, the invention designs an experimental device for soaking shale by supercritical carbon dioxide, wherein the energy of a pressurized carbon dioxide gas source is injected into a container, and simultaneously, the soaked shale and carbon dioxide are heated by a corrosion-resistant lining so as to ensure the supercritical state of the carbon dioxide in a pressure-bearing container. The equipment can flexibly adjust the temperature and pressure of the shale soaking according to the environmental temperature and pressure of the rock, and truly simulate the action process of the shale subjected to the supercritical carbon dioxide. In the soaking experimental equipment, a plurality of groups of soaking experiments with different time from several hours to one month can be carried out on the shale, and then the shale sample is taken out in situ to carry out subsequent rock mechanical property tests so as to measure shale mechanical property parameters close to the bottom layer under the working condition of high temperature and high pressure.
The invention mainly completes the shale soaking experiment of supercritical carbon dioxide under the conditions of set pressure and temperature, and relates to the functions of heating, pressurizing, measuring, monitoring, stabilizing pressure and preserving heat of a shale soaking working environment.
In order to solve the technical problems, the invention adopts the technical scheme that:
the utility model provides a supercritical carbon dioxide soaks shale experimental apparatus, includes head and the pressure-bearing container barrel that is located the head below, its characterized in that: the sealing head is provided with a safety accessory, the sealing head is connected with the pressure-bearing container barrel through a flange, a heating sleeve used for heating and keeping constant temperature is arranged in the pressure-bearing container barrel, the heating sleeve and the pressure-bearing container barrel form a double-layer structure for separating heating and pressure bearing, a rock sample fixing basket used for containing and fixing rock samples is arranged in the inner space of the heating sleeve, and an inlet pipe and an outlet pipe with a cut-off valve are arranged on the side wall of the pressure-bearing container barrel.
As a refinement, the safety accessories include a safety valve, a pressure gauge, and a temperature sensor.
As an improvement, the heating sleeve is composed of a base body made of ceramic materials and a heating device arranged in the base body, the heating device of the heating sleeve is isolated from an external space by being embedded in the base body, and the heating device is a three-grade heater capable of realizing high grade, medium grade and low grade.
As an improvement, a sealing device is arranged on the flange connecting surface of the end socket and the pressure-bearing container cylinder, and the sealing device is a sealing ring or a gasket which is resistant to carbon dioxide corrosion and pressure; the stop valves on the inlet pipe and the outlet pipe are ball valves with good sealing performance, the outlet pipe is arranged on the upper part of the pressure-bearing container cylinder, and the inlet pipe is arranged on the lower part of the pressure-bearing container cylinder.
As an improvement, a heating device of the heating sleeve is a spiral heating coil, a pressure-resistant connector for preventing high-pressure carbon dioxide from leaking is arranged at the bottom of a cylinder body of the pressure-bearing container, the spiral heating coil is connected with the pressure-resistant connector through an insulated wire, and the pressure-resistant connector is connected with an external power supply.
As an improvement, the pressure-resistant connector comprises a socket shell and a socket inner core, a small hole is formed in the bottom of the pressure-bearing container cylinder, the socket shell is arranged in the small hole, a rubber sealing ring is arranged between the socket shell and the bottom of the pressure-bearing container cylinder, and the socket inner core is connected with the spiral heating coil through an insulated wire.
As an improvement, a heat-insulating layer is arranged outside the pressure-bearing container cylinder body, and the heat-insulating layer is a polyester fiber or asbestos heat-insulating layer.
As an improvement, the internal volume of the pressure-bearing container cylinder is less than 5000mL, and gaps are arranged between the heating sleeve and the pressure-bearing container cylinder and between the rock sample fixing basket and the rock sample.
As an improvement, the heating sleeve and the pressure-bearing container barrel are made of corrosion-resistant alloy steel, and the rock sample fixing basket is hollow and made of transparent plastic resistant to carbon dioxide corrosion.
As an improvement, the bottom of the pressure-bearing container cylinder body is provided with a skirt, a reinforcing rib is arranged between the pressure-bearing container cylinder body and the skirt, and the seal head is provided with a plurality of reserved expansion holes.
The invention has the beneficial effects that:
1. compared with the existing equipment for soaking shale in a vacuum container, the equipment for soaking shale in supercritical carbon dioxide can realize the pressure of 0-10 Mpa and the temperature of 0-100 MPaoThe requirement of the large-range soaking environment of the C can simulate the pressure and temperature environment of shale in the stratum more truly.
2. Compared with a shale soaking small container modified by a rock true triaxial apparatus, the supercritical carbon dioxide shale soaking device can realize the soaking of a group of five rock samples at one time, and the quantity is more. This time cost that will greatly reduced follow-up rock mechanics experiment has improved experimental efficiency. Meanwhile, the mechanical property difference of shale soaked in the true rock triaxial apparatus for two times independently is avoided.
3. At present, carbon dioxide in shale soaking is in a gas state due to the limitation of temperature and pressure regulation. The experimental device for soaking shale in supercritical carbon dioxide can really realize the soaking of shale in supercritical carbon dioxide with different pressure temperatures due to flexible pressure and temperature regulation.
4. Because the volume of the experimental device for soaking the shale by the supercritical carbon dioxide is only 4300mL, the supercritical carbon dioxide is injected in a pressurizing way and the temperature is raised more quickly, and the experimental device is more convenient to carry. After the inlet and outlet ball valves are closed, the device can be carried to a rock mechanical property test experiment site, so that the experiment can be conveniently and rapidly carried out on the spot after the soaking is finished, and the true validity of the shale soaking state is ensured.
Drawings
Fig. 1 is an isometric view of an experimental apparatus for soaking shale with supercritical carbon dioxide.
Fig. 2 is a front sectional view of an experimental device for soaking shale with supercritical carbon dioxide.
Fig. 3 is an exploded view of an experimental apparatus for soaking shale with supercritical carbon dioxide.
Fig. 4 is an exploded view of a heating device of an experimental device for soaking shale with supercritical carbon dioxide.
Fig. 5 is a sectional view of a heating device of an experimental device for soaking shale with supercritical carbon dioxide.
Fig. 6 is a partial cross-sectional view of the pressure resistant connector of fig. 5.
In the figure: 1-safety valve, 2-temperature sensor, 3-reserved connector, 4-end socket, 5-hexagon bolt, 6-hexagon nut, 7-rock sample, 8-inlet ball valve, 9-rock sample fixing basket, 10-heating sleeve, 11-pressure-bearing container barrel, 12-inlet pipe, 13-pressure-resistant connector, 14-pressure gauge, 15-outlet ball valve, 16-spiral heating coil, 17-outlet pipe, 18-skirt, 19-insulated wire positive wire, 20-rubber sealing ring, 21-insulated wire negative wire, 22-socket inner core and 23-socket shell.
Detailed Description
As shown in fig. 1 and 2, the experimental device for soaking shale with supercritical carbon dioxide comprises a seal head 4 and a pressure-bearing container barrel 11 located below the seal head, wherein a safety accessory is arranged on the seal head 4, the seal head 4 is connected with the pressure-bearing container barrel 11 through a flange, a heating sleeve 10 used for heating and keeping constant temperature is arranged in the pressure-bearing container barrel 11, the heating sleeve 10 and the pressure-bearing container barrel 11 form a double-layer structure for separating heating and pressure-bearing, a rock sample fixing basket 9 used for containing and fixing a rock sample 7 is arranged in the inner space of the heating sleeve 10, and an inlet pipe 12 and an outlet pipe 17 are arranged on the side wall of the pressure-bearing container.
As shown in fig. 1, the safety attachment includes a safety valve 1, a pressure gauge 14, and a temperature sensor 2.
As shown in fig. 2 and 4, the heating sleeve 10 is composed of a base body made of a ceramic material and a spiral heating coil 16 arranged in the base body, the spiral heating coil 16 is isolated from an external space by being embedded in the base body, the spiral heating coil 16 is a three-gear heater capable of realizing high-grade, medium-grade and low-grade heating, the high-grade is mainly used for rapid heating of the shale 7 soaking environment, the medium-grade is used for normal-speed heating, and the low-grade is used for temperature compensation in a long-time soaking process. The pressure-bearing vessel cylinder 11 is provided at the bottom with a pressure-resistant connector 13 for preventing leakage of high-pressure carbon dioxide and isolating the lead wire connection from the carbon dioxide medium.
And a heat-insulating layer is arranged outside the pressure-bearing container barrel body 11, and is a polyester fiber or asbestos heat-insulating layer.
As shown in fig. 5 and 6, the voltage-resistant connector 13 includes a socket housing 23 and a socket inner core 22, a small hole is formed in the bottom of the pressure-bearing container cylinder 11, the socket housing 23 is disposed in the small hole, a rubber seal ring 20 is disposed between the socket housing 23 and the bottom of the pressure-bearing container cylinder 11, the socket inner core 22 is connected to the spiral heating coil 16 through an insulated conductor positive wire 19 and an insulated conductor negative wire 21, and the socket inner core 22 of the voltage-resistant connector 13 is connected to an external power supply.
As shown in fig. 1, a sealing device is arranged on a flange connecting surface of the end socket 4 and the pressure-bearing container cylinder 11, and the sealing device is a sealing ring or gasket which is resistant to carbon dioxide corrosion and pressure; the inlet pipe 12 and the outlet pipe 17 are respectively provided with an inlet ball valve 8 and an outlet ball valve 15 with good sealing performance. The outlet pipe 17 is arranged at the upper part of the pressure-bearing container cylinder 44, so that gas can be conveniently discharged after the experiment is finished, and the inlet pipe 17 is arranged at the lower part of the pressure-bearing container cylinder 11, so that liquid carbon dioxide can conveniently enter the container.
Because the shale soaking pressure control range sets up to 0~10Mpa, consequently design 4 shapes of head for oval head to improve its bearing capacity. The end socket 4 is formed by punching 35CrMo high alloy steel which is resistant to carbon dioxide corrosion in one step, and the end socket is subjected to heat treatment so as to improve the corrosion resistance and high temperature resistance of the material. The upper part of the seal head 4 adopts a measuring hole with the diameter of 6mm in drilling tool machining engineering, a pressure gauge 14, a temperature sensor 2 and a safety valve 1 are respectively installed, and the rest two measuring holes are temporarily sealed to be used as a reserved interface 3 for reserved later-stage experiment expansion.
The seal head 4 is connected with the pressure-bearing container barrel body 11 through a flange, and the flange is fastened through a hexagon bolt 5 and a hexagon nut 6. In order to ensure the sealing effect of the upper and lower flanges under high pressure, a corrosion-resistant sealing device is additionally arranged on the contact surface of the flanges, the sealing device is a gasket or a sealing ring, the gasket is a carbon dioxide corrosion-resistant metal gasket or a polytetrafluoroethylene gasket with the pressure grade of PN 10Mpa, and even if the shale is soaked for one month, the main sealing surface of the shale is not leaked.
The internal volume of the pressure-bearing container cylinder body 11 is less than 5000mL, and gaps are arranged between the heating sleeve 10 and the pressure-bearing container cylinder body 11 and between the rock sample fixing basket 9 and the rock sample 7. The equal clearance between fixed basket 9 of rock specimen and the rock specimen 7 is less than 2mm, and when cutting off exit ball valve, with experimental facilities area to next experimental place in-process, the rock specimen can not damage because of colliding with empting. The rock sample fixing basket 9 and the rock sample 7 are placed in the pressure-bearing vessel cylinder 11 before the experiment is started, and then heating and pressurizing are performed.
The heating sleeve and the pressure-bearing container barrel are made of corrosion-resistant alloy steel, and the rock sample fixing basket 9 is hollow and made of transparent plastic resistant to carbon dioxide corrosion.
The bottom of the pressure-bearing container cylinder body is provided with a skirt 18, and a reinforcing rib is arranged between the pressure-bearing container cylinder body 11 and the skirt 18.
The experimental device for soaking shale in carbon dioxide also considers that a visible transparent water tank is connected to the inlet pipe 12 of the pressure-bearing container barrel 11. The shale soaking experiment under the influence of water saturation can be carried out, and the shale soaking experiment under the combined action of supercritical carbon dioxide and water can also be carried out.
In the pressurization process before the equipment works, the vacuum pump connected with the outlet ball valve 15 firstly vacuumizes the interior of the container to-0.1 MPa, so that the interior of the container does not contain air components, and then the subsequent processes of carbon dioxide injection, heating and soaking are carried out. In order to ensure that the air in the container is completely replaced, when the carbon dioxide is injected, a small amount of carbon dioxide is injected, the carbon dioxide is discharged through the outlet ball valve 15, then the carbon dioxide is injected through the inlet ball valve 8, the circulation is performed for about three times, almost pure carbon dioxide is contained in the container, then the outlet ball valve 15 is closed, the carbon dioxide is continuously injected through the booster pump connected with the inlet pipe 12, the pressure is increased to the designed pressure, and then the heating and soaking processes are performed.
In the working process of the equipment, as shown in fig. 1 and 2, the pressure-bearing container cylinder 11 is a main experiment carrier for injecting supercritical carbon dioxide, heating and soaking shale. In order to ensure that the rock sample 7 of the shale reaches the set temperature in the soaking process, the shale experimental device is divided into an inner layer and an outer layer: the outer layer mainly comprises a pressure-bearing container cylinder body 11, an inlet ball valve 8, an outlet ball valve 15 and a skirt 18, and the outer layer mainly has the functions of bearing pressure load and keeping the internal pressure of the whole device stable in the shale soaking process. The inner layer mainly comprises a rock sample fixing basket 9, a heating sleeve 10 made of ceramic, a spiral heating coil 16 and a pressure-resistant connector 13, the main function of the inner layer is to fix the shale rock sample and prevent the shale from being accidentally damaged, and meanwhile, the shale and supercritical carbon dioxide are heated by adopting a heating lining structure, so that the temperature is constant in the soaking process. The heating device is provided with three selectable gears, namely a high gear, a medium gear and a low gear. High gear heating mainly used container inside rapid heating, normal heating in the well shelves mainly used container, keep out and mainly carry out heat compensation and heat preservation in soaking to the container.
In the whole soaking process of the experiment, the pressure gauge 14 and the temperature sensor 2 keep monitoring at any time, and meanwhile, when the pressure in the pressure container is abnormally increased to a set limit value, the safety valve 1 can be automatically communicated with the atmosphere to relieve the pressure of the pressure container. Because the maximum value of the soaking time is designed to be two months, in order to avoid temperature drop and pressure drop in the soaking process, heat compensation and pressure boosting compensation are required to be periodically adopted for equipment, so that the equipment is maintained at the designed temperature and pressure.
During the heating process of the equipment, it should be noted that due to the particularity of the supercritical carbon dioxide medium, the spiral heating coil 16 must be embedded in the ceramic matrix of the heating sleeve 10 by the manufacturer before assembly, so as to prevent it from being exposed to the supercritical carbon dioxide medium, so as not to cause the risks of corrosion, electric leakage, electric shock, etc. Meanwhile, the spiral heating coil 16 is connected to the voltage-resistant connector 13 through a sealed insulated wire and then connected to a power supply outside the pressure-containing vessel. The heating device can realize a high-grade, medium-grade and low-grade three-grade heater: after the equipment is pressurized, high-grade rapid heating is adopted, medium-grade and low-grade adjustment is adopted after the temperature approaches a designed temperature range, and heat compensation is carried out by adopting a low-grade position in the soaking process of the equipment.
After the equipment soaks the shale, the power is firstly cut off, the heating work of the spiral heating coil 16 is suspended, then the booster pump for compensating and boosting is stopped, the inlet ball valve 8 and the outlet ball valve 15 are kept in a closed state, and the equipment is waited to carry the shale to a shale mechanical test experiment field.
In the process of carrying the equipment, because a gap exists between the rock sample 7 and the heating sleeve 10 in the pressure-bearing container, the rock sample 7 of the shale possibly collides with the inner wall surface in the process of carrying and transporting the equipment; and also forms a low-speed jet when supercritical carbon dioxide enters from the inlet ball valve 8 to the inside. The adverse factors can cause damage to the internal shale rock sample, and influence the subsequent mechanical property test of the shale. Therefore, the hollow rock sample fixing basket 9 is made of transparent carbon dioxide corrosion resistant organic glass or other plastics, and the rock sample 7 is placed in the hollow rock sample fixing basket to effectively reduce the damage to the shale caused by the two conditions.
The pressure release process, equipment are carried behind shale mechanical properties experiment place, select spacious ventilation place, open the export ball valve 15 of upper end at first and wait for high-pressure gas slowly to exhaust to the manometer reading and be close atmospheric pressure, then open entry ball valve 8 and wait for the air admission to displace surplus carbon dioxide, and manometer 14 reading and the 2 readings of temperature sensor of container can be close atmospheric pressure and room temperature at last. And finally, opening the end socket 4, and taking out the rock sample to perform a shale mechanical property experiment as soon as possible.

Claims (9)

1. The utility model provides a supercritical carbon dioxide soaks shale experimental apparatus, includes head and the pressure-bearing container barrel that is located the head below, its characterized in that: the sealing head is provided with a safety accessory, the sealing head is connected with the pressure-bearing container barrel through a flange, a heating sleeve for heating and keeping constant temperature is arranged in the pressure-bearing container barrel, the heating sleeve and the pressure-bearing container barrel form a double-layer structure for separating heating and pressure bearing, a rock sample fixing basket for containing and fixing rock samples is arranged in the heating sleeve, and an inlet pipe and an outlet pipe with a cut-off valve are arranged on the side wall of the pressure-bearing container barrel; the heating device of the heating sleeve is a spiral heating coil, a pressure-resistant connector for preventing high-pressure carbon dioxide from leaking is arranged at the bottom of the pressure-bearing container barrel, the spiral heating coil is connected with the pressure-resistant connector through an insulated wire, and the pressure-resistant connector is connected with an external power supply.
2. The supercritical carbon dioxide soaking shale experimental device according to claim 1, wherein: the safety accessories include a safety valve, a pressure gauge, and a temperature sensor.
3. The supercritical carbon dioxide soaking shale experimental device according to claim 2, wherein: the heating sleeve is composed of a base body made of ceramic materials and a heating device arranged in the base body, the heating device of the heating sleeve is isolated from the external space by being pre-embedded in the base body, and the heating device is a three-grade heater capable of realizing high grade, medium grade and low grade.
4. The supercritical carbon dioxide soaking shale experimental device according to claim 3, wherein: a sealing device is arranged on the flange connecting surface of the end socket and the pressure-bearing container cylinder, and the sealing device is a sealing ring or a gasket which is resistant to carbon dioxide corrosion and pressure; the stop valves on the inlet pipe and the outlet pipe are ball valves with good sealing performance, the outlet pipe is arranged on the upper part of the pressure-bearing container cylinder, and the inlet pipe is arranged on the lower part of the pressure-bearing container cylinder.
5. The supercritical carbon dioxide soaking shale experimental device according to claim 4, wherein: the pressure-resistant connector comprises a socket shell and a socket inner core, a small hole is formed in the bottom of the pressure-bearing container cylinder, the socket shell is arranged in the small hole, a rubber sealing ring is arranged between the socket shell and the bottom of the pressure-bearing container cylinder, and the socket inner core is connected with the spiral heating coil through an insulated wire.
6. The supercritical carbon dioxide soaking shale experimental device according to claim 5, wherein: and the pressure-bearing container cylinder body is externally provided with a heat-insulating layer, and the heat-insulating layer is a polyester fiber or asbestos heat-insulating layer.
7. The supercritical carbon dioxide soaking shale experimental device according to claim 6, wherein: the internal volume of the pressure-bearing container cylinder is less than 5000mL, and gaps are arranged between the heating sleeve and the pressure-bearing container cylinder and between the rock sample fixing basket and the rock sample.
8. The supercritical carbon dioxide shale soaking experimental device according to any one of claims 1 to 7, wherein: the heating sleeve and the pressure-bearing container barrel are made of alloy steel, and the rock sample fixing basket is hollow and made of transparent plastic resistant to carbon dioxide corrosion.
9. The supercritical carbon dioxide shale soaking experimental device according to claim 8, wherein: the bottom of the pressure-bearing container barrel is provided with a skirt, a reinforcing rib is arranged between the pressure-bearing container barrel and the skirt, and the seal head is provided with a plurality of reserved expansion holes.
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