CN111537697A - Indoor simulation device and method for supercritical water and shale reaction - Google Patents
Indoor simulation device and method for supercritical water and shale reaction Download PDFInfo
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Abstract
The invention relates to an indoor simulation device and method for supercritical water and shale reaction, which comprises a high-temperature high-pressure reaction kettle, a vacuum pump, an air compressor, a booster pump and a heating device, wherein the high-temperature high-pressure reaction kettle is connected with the vacuum pump; the high-temperature high-pressure reaction kettle comprises a kettle body, a kettle cavity, a kettle cover, a rock core jacket and a filter screen support, wherein the kettle cavity is arranged in the kettle body, the upper part of the kettle cavity extends out of the kettle body, the kettle cover is arranged at the top of the kettle cavity, pressure fluid is injected through a communicating valve port to realize rock core confining pressure control, the kettle cavity is placed on the filter screen support at the bottom of the inner side of the kettle cavity, and the filter screen support is vertically arranged in the middle of the bottom of the kettle cavity and used for placing the rock core jacket; a heating device is arranged outside the kettle cavity; an air injection pipeline, an air exhaust pipeline and a detection pipeline are arranged on the kettle cover and extend to the outside from the kettle cavity through the kettle cover, and the air injection pipeline is connected with the booster pump. The invention can realize that the rock sample reacts with water under the condition that the critical temperature and pressure of the water are exceeded in a specific gas environment, and the indoor simulation of the reaction of the shale and the supercritical water is completed.
Description
Technical Field
The invention relates to an indoor simulation device and method for supercritical water and shale reaction, and belongs to the technical field of energy and environment.
Background
The shale reservoir bed block is compact, and has the characteristics of low porosity and poor seepage capability. In order to realize commercial exploitation of shale gas, long-distance horizontal wells and staged fracturing technologies are required. In the flowback process after hydraulic fracturing, the flowback rate is often low, a large amount of fracturing fluid is retained in a reservoir, the retained fracturing fluid can cause the problems of water phase trapping damage and the like of the reservoir, and the flowing fracturing fluid is an important factor for restricting the yield increasing effect of the hydraulic fracturing.
Existing research and mine tests indicate that artificially increasing the temperature of shale reservoirs may remove water phase trapping damage and even form thermally induced fractures. Further, if the reservoir temperature is increased to be higher than the critical temperature of water, namely 374.2 ℃, and the formation pressure of the shale reservoir is higher than the critical pressure of water, namely 22.4MPa, the fracturing fluid retained in the reservoir can be converted into a supercritical state in situ. Obviously, the formation pressure of the shale reservoirs developed at present is greater than the critical pressure of water, namely 22.4 MPa. The existing research shows that the supercritical water has the characteristics of low density, low viscosity, strong oxidizing property, high organic matter and gas solubility and the like, and can react with reducing components such as pyrite and the like in the shale pores. The retained fracturing fluid is converted into a supercritical state, theoretically, a large number of complex chemical reactions can occur and the thermal effect is accompanied, so that the gas seepage capability of a shale reservoir matrix or the gas flow conductivity of cracks is influenced.
Therefore, the indoor experiment of the reaction of the shale and the supercritical water is carried out indoors, and the analysis of the action mechanism of the supercritical water on the shale is facilitated. Related research institutions have conducted certain exploration, such as academic paper "near-critical water simulation extraction and product analysis of oil shale in different regions". The supercritical fluid in the industry is more an experiment for supercritical carbon dioxide and shale at present, for example, the application number 201610105722.2, "test piece manufacturing method for supercritical carbon dioxide cracking shale under triaxial stress". The conventional indoor simulation device can realize indoor experiments of high-temperature treatment of rock samples or displacement experiments of specific fluids, but at present, an indoor simulation device and a matching method aiming at a complete system of supercritical water and shale reaction do not exist, the indoor simulation experiments of the supercritical water and shale reaction cannot be realized aiming at the supercritical water specifically, and further quantitative evaluation research and reaction mechanism research cannot be deeply developed.
Disclosure of Invention
The invention aims to provide an indoor simulation device and method for supercritical water and shale reaction, which can realize that a rock sample reacts with water under the condition that the critical temperature and pressure of the water are exceeded in a specific gas environment, and complete the indoor simulation of the supercritical water reaction of the shale.
In order to achieve the purpose, the invention adopts the technical scheme that:
an indoor simulation device for supercritical water and shale reaction comprises a high-temperature high-pressure reaction kettle, a vacuum pump, an air compressor, a booster pump and a heating device;
the high-temperature high-pressure reaction kettle comprises a kettle body, a kettle cavity, a kettle cover, a rock core jacket and a filter screen support, wherein the kettle cavity is arranged in the kettle body, the upper part of the kettle cavity extends out of the kettle body, the kettle cover is arranged at the top of the kettle cavity, and the rock core jacket is used for clamping experimental rock cores and is at least 2; fluid is injected through a communicating valve port on the core jacket shell to control the core confining pressure, and the core confining pressure is placed on a filter screen support at the bottom of the inner side of the kettle cavity, and the filter screen support is vertically arranged in the middle of the bottom of the kettle cavity and is used for placing the core jacket, providing an exhaust pipeline channel and preventing micro particles from entering and blocking the exhaust pipeline; a heating device is arranged on the outer side of the kettle cavity, and the heating device penetrates through the kettle body through a circuit to be connected to the outside;
still be equipped with the gas injection pipeline on the kettle cover to pass the kettle cover from the cauldron chamber and extend to the outside, be connected with the booster pump, be equipped with the three-way valve in the booster pump, be connected to air compressor and outside gas container respectively.
Further, the kettle cover consists of a pressure gauge, a vacuum gauge, a pressure transmitter, an air injection pipeline, an exhaust pipeline, a temperature transmitter and a handle; the pressure gauge, the vacuum gauge, the pressure transmitter and the temperature transmitter are all arranged on the same pipeline, the pipeline penetrates through the kettle cover and extends into the kettle cavity, and the handle is arranged on the side face of the kettle cover.
The core jacket comprises an upper shell, a lower shell and a middle sleeve, wherein a core is placed in the sleeve and is compacted through the shells, and the shells are provided with communicating valve ports; the pressure fluid is injected inwards through the communicating valve port to apply certain confining pressure to the rock core required by the experiment, and the shale with certain confining pressure and the supercritical water reaction are simulated.
Further, the filter screen support, including upper portion support, lower part filter screen and bottom reducing pipe, the upper portion support is the cavity pipeline, for the exhaust pipe line in the cauldron provides the passageway, the lower part filter screen mainly used places the rock core and presss from both sides the cover, bottom reducing pipe is located under the filter screen, can be used to prevent that tiny granule from getting into intraductal jam pipeline along with the fluid.
The exhaust pipeline penetrates through the kettle cover from the kettle cavity, and a sampling port and an exhaust port are arranged at the far end of the exhaust pipeline, and the sampling port faces downwards and is used for collecting liquid in the kettle; the direction of the exhaust port is consistent with the extending direction of the exhaust pipeline, and the supercritical fluid core displacement test device can be used for transferring fluid in the kettle to the core holder to carry out the supercritical fluid core displacement test. The sampling port and the exhaust port are both provided with valves. The exhaust line can also be connected to a vacuum pump to realize vacuum treatment in the kettle.
The vacuum pump can eliminate the interference of initial gas conditions before increasing the gas pressure in the kettle body, and the air compressor provides power for the booster pump to inject the external gas in the external gas container into the kettle cavity when boosting the pressure in the kettle body.
And the external gas is one or more of air, nitrogen, helium, methane and carbon dioxide. The function is that the pressure in the kettle body can be increased, and a specific gas phase environment can be built in the kettle body.
Furthermore, the heating device is composed of a ring of electric heating rods, the electric heating rods are arranged on the outer wall of the kettle cavity in a surrounding mode, and electric wires connected together at the bottom of the electric heating rods extend to the outside.
Further, the device also comprises a controller, wherein the controller is respectively connected with the pressure transmitter, the temperature transmitter and the heating device, so that the pressure and temperature conditions in the kettle can be observed in real time, and the target temperature and the heating rate can be controlled.
The invention also provides an experimental method for carrying out supercritical water treatment on the shale sample by using the indoor simulation device, which comprises the following steps:
step 1, pretreating a rock sample, cutting a rock block, drilling a rock core or grinding rock debris according to the research purpose, drying the rock sample in a 60 ℃ drying oven to constant weight, and measuring the mass and geometric dimension data of the rock sample;
and 5, firstly, completing vacuum treatment, then opening a booster pump and an air compressor, injecting specific gas into the kettle cavity, improving the pressure in the kettle cavity, simultaneously starting a heating device, and setting a target temperature and a heating rate. When the set pressure and temperature are reached and the pressure and temperature are kept for a period of time, because the pressure and temperature of the fluid in the kettle cavity are greater than the pore pressure and temperature of the rock core, the pressure and temperature in the rock core are changed under the action of pressure difference and heat transfer, after the critical pressure and critical temperature of water are exceeded, the fracturing fluid in the rock core is converted into a supercritical state, on one hand, the fracturing fluid in the supercritical state reacts with organic matters or reducing components in the rock core, on the other hand, the special properties of high temperature and high pressure of the fracturing fluid can be used for displacing other fluids in the rock core, and the fluid distribution condition in the pores of the rock core is changed; finally stopping heating, cooling and releasing pressure through an exhaust pipeline;
and 6, opening the kettle cover and taking out the rock sample.
By applying the indoor simulation device, the reaction of rock core-supercritical water is simulated, so that the pore structure of the rock core, the content of organic carbon and the retention condition of internal fluid are changed. The rock core after the experiment can be used for continuously carrying out seepage capability evaluation experiment, nitrogen adsorption experiment and organic carbon content determination experiment after the shale and supercritical water act, and further disclosing the reaction mechanism of the shale and the supercritical water.
The indoor experimental device and the method for the supercritical water and shale reaction provided by the invention have the following advantages:
(1) the supercritical water and shale reaction is objectively and truly simulated. Because the critical temperature of water is 374 ℃ and the critical pressure of water is 22.4MPa, although the existing indoor operating device for core heat treatment, such as an atmosphere furnace, can realize the core treatment at the temperature of over 374 ℃ under certain atmosphere conditions, the strength of an atmosphere tube is limited, the internal pressure of the atmosphere tube cannot be increased to 22.4MPa, and therefore, the shale-supercritical water series reaction cannot be truly and objectively simulated; although the existing core holder equipment can displace fluid with the pressure of more than 22.4MPa, if the temperature of the fluid reaches the critical temperature 374 ℃ of water, the sealing performance of the core holder is difficult to guarantee, so that the series reaction of shale-supercritical water cannot be truly and objectively simulated. According to the indoor simulation device and the experimental method, the industrial current situation of a fracturing fluid retention reservoir in shale gas development engineering is simulated through self-absorption fracturing fluid treatment before experiment; applying a certain confining pressure to the experimental core through a specially-made core jacket, and simulating the stress condition of the core in an actual reservoir; the process that the reserved reservoir fracturing fluid is converted into a supercritical state in situ and reacts with organic matters and reducing components in the rock core or is moved in pores is simulated by taking the rock core treated by the self-priming fracturing fluid at the critical temperature and the critical pressure of the super-water as an object and using the booster pump, the air compressor, the heating device and the controller in a matched manner in a high-temperature high-pressure reaction kettle with special design.
(2) A specific gas phase environment can be created. Under the condition that the vacuum pump is used for vacuumizing and removing initial gas, the air compressor is used for providing power, and the specific gas in the external gas container is injected into the kettle cavity through the booster pump, so that the pressure is controlled, and meanwhile, a specific gas phase environment is created.
(3) Real-time sampling can be realized. A filter screen support is arranged in the kettle cavity, and a sampling tube containing a reducer tube is arranged at the bottom of the kettle cavity at the lower part of the filter screen support, so that real-time sampling can be realized. Meanwhile, as the cross-sectional area of the fluid at the reducer pipe is changed, part of the tiny residues flowing along with the fluid are attached to the reducer pipe, and part of the tiny residues are settled due to the change of the fluid speed, so that the purpose of preventing the tiny residues generated by the reaction from blocking the sampling pipe is achieved. The principle is that the reducer pipe is designed, so that the speed of fluid changes when passing through, because the inertia of tiny solid particles is larger than that of the fluid, the fluid cannot provide enough momentum for the solid particles when the pipe diameter is reduced and the speed rises, so that the solid particles are settled and cannot enter a subsequent pipeline, and in addition, part of the tiny particles rising along with airflow possibly collide with the wall surface of the reducer pipe and cannot rise into the pipeline. In addition, after the experiment, tiny residues generated in the experiment can be discharged and collected in a mode of gas purging the reducer pipe, specifically, the filter screen bracket can be taken out, and tiny particles attached to the pipe can be blown out by using airflow with small flow so as to be collected and detected.
(4) The experimental conditions are visual and controllable. The controller is connected with the pressure transmitter and the temperature transmitter, so that the pressure and temperature conditions in the kettle cavity can be monitored in real time; the controller is matched with the heating equipment, and can control the target temperature and the heating rate; the pressure control can be realized by manually operating the booster pump by matching with the pressure data observed in real time.
(5) And a foundation is laid for the subsequent research on the action of supercritical water and rocks. Under the support of the indoor experimental device, the evaluation experiment of the change of the pore structure and the permeability of the shale after the reaction of supercritical water and the shale can be further carried out by combining other detection means.
Drawings
FIG. 1 is a schematic diagram showing the construction of an indoor simulation apparatus for supercritical water and shale reaction according to the present invention;
FIG. 2 is an enlarged view of area A of FIG. 1;
3a-3c are schematic diagrams of a screen support configuration, including pictorial, top and bottom views;
4a-4c are schematic diagrams of core jacket structures, including perspective, front and cross-sectional views c-c;
FIG. 5 is a flow chart of an experimental method of an indoor simulation device for supercritical water and shale reaction according to the present invention.
Shown in the figure:
1-kettle body, 2-kettle cavity, 3-kettle cover, 4-filter screen support, 5-vacuum gauge, 6-pressure gauge, 7-pressure transmitter, 8-temperature transmitter, 9-handle, 10-heating device, 11-controller, 12-booster pump, 13-air compressor, 14-external gas container, 15-vacuum pump, 16-sampling port, 17-core jacket, 18-gas injection pipeline and 19-gas exhaust pipeline.
Detailed Description
The indoor simulation apparatus and method for supercritical water and shale reaction provided by the present invention are further described with reference to the accompanying drawings and embodiments.
An indoor simulation device for supercritical water and shale reaction comprises a high-temperature high-pressure reaction kettle, a vacuum pump, an air compressor, a booster pump, a heating device and a controller; the high-temperature high-pressure reaction kettle comprises a kettle body, a kettle cavity, a kettle cover, a core jacket and a filter screen support, wherein the kettle cavity is arranged in the kettle body, the upper part of the kettle cavity extends out of the kettle body, the kettle cover is arranged at the top of the kettle cavity, the core jacket is used for clamping an experimental core, the core jacket is arranged at the bottom of the inner side of the kettle cavity, the number of the core jacket can be set according to experimental requirements and is at least 2, and the filter screen support is vertically arranged in the middle of the bottom of the kettle cavity and separates a plurality of core jackets; a heating device is arranged on the outer side of the kettle cavity, and the heating device penetrates through the kettle body through a circuit to be connected to the outside; still be equipped with the pipeline on the kettle cover to pass the kettle cover from the cauldron chamber and extend to the outside, be connected with the booster pump, be equipped with the three-way valve in the booster pump, be connected to air compressor and outside gas container respectively. The kettle cover consists of a pressure gauge, a vacuum gauge, a pressure transmitter, an air injection pipeline, an exhaust pipeline, a temperature transmitter and a handle; the pressure gauge, the vacuum gauge, the pressure gauge air supply and the temperature transmitter are all arranged on the same pipeline, the pipeline penetrates through the kettle cover and extends into the kettle cavity, and the handle is arranged on the side face of the kettle cover. The core jacket comprises an upper shell, a lower shell and a middle sleeve, wherein a core is placed in the sleeve and is compacted through the shells, and the shells are provided with communicating valve ports; the core jacket applies certain confining pressure to the core in the experimental process, and the shale with certain confining pressure is simulated to react with supercritical water. The filter screen support comprises an external support and an internal filter screen, the filter screen is fixed at the bottom of the kettle cavity, the support is a hollow pipeline, the upper part of the support passes through the kettle cover through a pipeline, branch pipelines are arranged on the external pipeline and are respectively used as an exhaust pipeline and a sampling port, the exhaust pipeline is also connected to a vacuum pump, the direction of the sampling port is downward, and valves are arranged on the sampling port and the exhaust pipeline; the vacuum pump can eliminate the interference of initial gas conditions before increasing the gas pressure in the kettle body, and the air compressor provides power for the booster pump to inject the external gas in the external gas container into the kettle cavity when boosting the pressure in the kettle body. And the external gas is one or more of air, nitrogen, helium, methane and carbon dioxide.
The specific experimental steps comprise:
step 1, rock sample pretreatment. Selecting a rock sample of a research block, drilling a core column or collecting rock debris according to the research purpose, drilling the core column meeting the requirements of quantitative evaluation experiments or cutting the core column into rock blocks if quantitative evaluation experiments such as permeability and the like are required to be carried out, and grinding the rock debris or other rock blocks into the particle size required by the experiments by using equipment such as a scanning electron microscope, an organic carbon-sulfur analyzer and the like if nitrogen adsorption experiments and X-ray diffraction experiments are required to be carried out. In the embodiment, according to the experimental requirement, a core pillar with the diameter of 3.5cm and the length of 5cm is drilled, the rock debris in the drilling process and other rock blocks with similar positions are collected by more than 40g, and the core pillar is ground to the grain size of 12 meshes to 20 meshes. And (3) placing the treated core pillar and rock debris samples in an oven at 60 ℃ to be dried to constant weight, and numbering and recording basic data (such as dry weight, length and diameter).
And 2, measuring initial data (such as initial porosity, initial permeability and initial total organic carbon) according to the requirements of subsequent experiments, and soaking the rock sample in fracturing fluid or formation water to enable the rock sample to be self-absorbed so as to simulate the condition that the fracturing fluid stays in the well in actual engineering. In the embodiment, the processed rock debris is divided into 3 parts randomly, namely, group A, group B and group C, wherein the group A is used for measuring the initial organic carbon content, the group B and the group C are placed into a high-temperature high-pressure reaction kettle for participating in the reaction, and the group C is used for standby. The initial permeability of the core pillar and the initial organic carbon content of the group a cuttings were determined as required. The core column and B, C sets of cuttings loaded into the screen were then immersed in the fracturing fluid and the core column and screen bags were suspended at the bottom of the analytical balance while the analytical balance data was transmitted to the computer to allow for the understanding of the self-absorption of the rock sample.
And 3, detecting the airtightness of the high-temperature high-pressure reaction kettle and the functional conditions of other equipment. In the embodiment, after connecting each line, firstly, the vacuum pump 15 is used to pump the empty kettle cavity 2 to the negative pressure of 0.098MPa and keep the negative pressure for 10min, if the pressure keeps normal, the booster pump 12 is connected to boost the pressure to 11MPa and stabilize the pressure for 10min to detect the condition of stable pressure, if the pressure keeps normal, the heating device 10 is started to gradually increase the temperature to 400 ℃ and simultaneously detect the sealing condition of each connection part, and if the pressure can reach stability for 30min, the high-temperature high-pressure reaction kettle can be judged to be qualified in tightness and other devices are good in function condition. And (4) after the detection is finished, closing the heating system 10, and releasing the pressure after all the equipment is cooled, so as to prepare the experiment.
And 4, injecting a fluid for providing the rock core column confining pressure into the rock core jacket 17 placed in the rock core column through the communicating valve port, placing the fluid on the filter screen support 4, fixing the filter screen support 4 in the kettle cavity 2, closing the kettle cover 3, and fixing and sealing. In the embodiment, firstly, a core column required by an experiment is placed in the core jacket 17 and a certain confining pressure is applied, then the core column is vertically placed on the filter screen bracket 4, the rock debris of the group B and the group C are respectively placed in the crucibles and placed on the filter screen bracket 4, and then the filter screen bracket 4 is placed in the kettle cavity 2 and fixed. The vessel lid 3 is closed and sealed, and the temperature transmitter 8, pressure transmitter 7, heating device 10 and other lines are checked for connections.
And 5, firstly, using a vacuum pump 15 to enable the kettle cavity 2 to reach a negative pressure of 0.098MPa and keep the negative pressure for 10min, then starting a booster pump 12 and an air compressor 13, injecting the gas in an external gas container 14 into the kettle cavity 2 to increase the pressure, and simultaneously starting a heating device 10 to increase the temperature of the kettle cavity 2, so that the temperature and the pressure of the kettle cavity 2 are finally enabled to reach the supercritical conditions of water preset in the experiment. In the embodiment, the vacuum pump 15 is turned on to make the inside of the kettle cavity 2 reach the condition of 0.098MPa negative pressure, and is kept for 10min to exhaust the interfering gas in the kettle, and then the vacuum pump is turned off, the booster pump 12 and the air compressor 13 are connected, and the specific gas in the external gas container 14 is injected into the kettle cavity 2. Firstly, the pressure in the kettle cavity 2 is increased to 10MPa, then the heating device 10 is started, the set temperature is 380 ℃, and after the temperature is 380 ℃, the controller 11 displays that the pressure in the kettle cavity 2 is 22.87MPa and does not reach 24MPa of the experimental design, so that the booster pump 12 and the air compressor 13 are started to increase the pressure to 24 MPa. And (3) keeping the temperature and the pressure in the kettle cavity 2 stable for 4h, so that the self-absorption fracturing fluid in the rock core in the kettle is converted into a supercritical state under the action of a high-temperature and high-pressure environment in the kettle, and the supercritical state and the shale matrix or organic matter in the rock core generate certain thermodynamic or chemical reaction to change the pore structure and the organic matter content of the rock core. Meanwhile, the supercritical fracturing fluid taking supercritical water as a main component migrates in the pores of the core due to the reduction of viscosity, so that the distribution of fluid in the pores is changed, the seepage capability of part of the pores which are damaged by water lock is recovered, and the permeability of the core is changed. And finally, after the temperature is reduced to the room temperature, the pressure in the kettle cavity 2 is unloaded. If a traditional atmosphere tube type heating furnace is used, because of the strength problem of the atmosphere tube, the pressure condition of 22.4MPa cannot be achieved for a long time, so that most of self-absorption fracturing fluid in the rock core cannot be converted into a supercritical state, and further relevant reactions of shale and supercritical water cannot occur. And if can realize the contact of supercritical water and rock core in inputing the supercritical water to the rock core holder, but the relevant connecting line of rock core holder is many, and is difficult to optimize to thermal-insulated keeping warm, so the supercritical water that flows in its pipeline is difficult to guarantee to be in supercritical state, and the nature of rock core holder's sealing washer under the critical temperature condition that surpasss water can change, causes certain influence to the sealing performance of rock core holder. Therefore, by using the indoor simulation equipment and the method, a continuous, stable and real shale-supercritical water treatment process can be realized. The pressurization and temperature rise operation is realized in the kettle cavity 2, so that the energy loss in the external flowing process is reduced; through the cooperation of the controller 11 and the heating device 10 and the manual operation of the booster pump 12, the pressure and temperature conditions in the kettle cavity 2 are maintained above the critical pressure and critical temperature of water and kept for more than 4 hours, so that the reaction is carried out for sufficient time, and the experimental result can show the real reaction process of the shale and the supercritical water.
And 6, opening the kettle cover 3, taking out the rock sample, arranging equipment, and carrying out subsequent seepage capability evaluation experiment, low-pressure nitrogen adsorption experiment and organic carbon content detection so as to research the reaction mechanism of the shale and the supercritical water. In this embodiment, the core pillar and the crucibles filled with the group B and group C rock debris are taken out, the core pillar is used for the subsequent measurement experiment of parameters such as permeability, and the group B, C rock debris is used for the subsequent measurement experiment of parameters such as organic carbon content.
Although the present invention has been described with reference to the above embodiments, it should be understood that the present invention is not limited to the above embodiments, and those skilled in the art can make various changes and modifications without departing from the scope of the present invention.
Claims (8)
1. An indoor simulation device for supercritical water and shale reaction is characterized by comprising a high-temperature high-pressure reaction kettle, a vacuum pump, an air compressor, a booster pump and a heating device;
the high-temperature high-pressure reaction kettle comprises a kettle body, a kettle cavity, a kettle cover, a rock core jacket and a filter screen support, wherein the kettle cavity is arranged in the kettle body, the upper part of the kettle cavity extends out of the kettle body, the kettle cover is arranged at the top of the kettle cavity, the rock core jacket is used for clamping an experimental rock core and comprises a shell and a sleeve, the rock core confining pressure control is realized through a communicating valve port on the shell, the rock core confining pressure control is placed on the filter screen support at the bottom of the inner side of the kettle cavity, and the filter screen support is vertically arranged in the middle of the bottom of the kettle cavity and is used for placing the rock core jacket and providing an exhaust; a heating device is arranged on the outer side of the kettle cavity, and the heating device penetrates through the kettle body through a circuit to be connected to the outside;
still be equipped with the gas injection pipeline on the kettle cover to pass the kettle cover from the cauldron chamber and extend to the outside, be connected with the booster pump, be equipped with the three-way valve in the booster pump, be connected to air compressor and outside gas container respectively.
2. The indoor simulation device of supercritical water and shale reaction of claim 1, wherein the kettle cover is composed of a pressure gauge, a vacuum gauge, a pressure transmitter, an air injection pipeline, an exhaust pipeline, a temperature transmitter and a handle; the pressure gauge, the vacuum gauge, the pressure transmitter and the temperature transmitter are all arranged on the same pipeline, the pipeline penetrates through the kettle cover and extends into the kettle cavity, and the handle is arranged on the side surface of the kettle cover;
the core jacket comprises an upper shell, a lower shell and a middle sleeve, wherein a core is placed in the sleeve and is compacted through the shells, and the shells are provided with communicating valve ports; can exert certain confining pressure to the required rock core of experiment through the communicating valve port, the simulation has the shale and the supercritical water reaction of certain confining pressure.
3. The indoor simulation device of supercritical water and shale reaction of claim 2, wherein the filter screen support comprises an upper support, a lower filter screen and a bottom reducer, the upper support is a hollow pipeline and provides a channel for an exhaust pipeline in the kettle, the lower filter screen is mainly used for placing a core jacket, and the bottom reducer is located below the filter screen and can be used for preventing fine particles from blocking the pipeline in the pipeline along with fluid entering the pipeline.
The exhaust pipeline penetrates through the kettle cover from the kettle cavity, and a sampling port and an exhaust port are arranged at the far end of the exhaust pipeline, and the sampling port faces downwards and is used for collecting liquid in the kettle; the direction of the exhaust port is consistent with the extending direction of the exhaust pipeline, and the supercritical fluid core displacement test can be carried out by transferring the fluid in the kettle to the core holder; the sampling port and the exhaust port are provided with valves; the exhaust line can also be connected to a vacuum pump to realize vacuum treatment in the kettle.
4. The apparatus of claim 3, wherein the vacuum pump, the booster pump, and the air compressor are configured to remove the disturbance of the initial gas condition before increasing the gas pressure in the autoclave body, and the air compressor is configured to provide power to the booster pump to inject the external gas from the external gas container into the autoclave cavity when the autoclave body is pressurized.
5. The indoor simulation device for supercritical water and shale reaction of claim 4, wherein the external gas is one or more of air, nitrogen, helium, methane, carbon dioxide.
6. The indoor simulation device of supercritical water and shale reaction of claim 5, wherein the heating device is composed of a ring of electric heating rods, the electric heating rods are arranged around the outer wall of the kettle cavity, and electric wires connected together at the bottom of the electric heating rods extend to the outside.
7. The indoor simulation device of supercritical water and shale reaction of claim 6, further comprising a controller, wherein the controller is respectively connected with the pressure transmitter, the temperature transmitter and the heating device, so as to realize real-time observation of pressure and temperature conditions in the kettle and control target temperature and heating rate.
8. An experimental method for supercritical water treatment of shale samples by using the indoor simulation device for supercritical water and shale reaction of claim 7, characterized by comprising the following steps:
step 1, pretreating a rock sample, cutting a rock block, drilling a rock core or grinding rock debris according to the research purpose, drying the rock sample in a 60 ℃ drying oven to constant weight, and measuring the mass and geometric dimension data of the rock sample;
step 2, after the initial data of the rock sample is measured, immersing the rock sample in a liquid phase environment required by an experiment, wherein the liquid comprises water-based fracturing fluid and formation water, so that the rock sample is self-absorbed and the retention of working fluid in shale is simulated;
step 3, detecting the airtightness of the high-temperature high-pressure reaction kettle and the functional conditions of other equipment;
step 4, putting the pretreated rock core into a rock core jacket, applying a certain confining pressure, placing the rock core on a filter screen support, putting the filter screen support into a kettle cavity, closing a kettle cover, connecting a pipeline, a temperature transmitter and a pressure transmitter, and well performing examination before an experiment;
and 5, firstly, completing vacuum treatment, then opening a booster pump and an air compressor, injecting specific gas into the kettle cavity, improving the pressure in the kettle cavity, simultaneously starting a heating device, and setting a target temperature and a heating rate. When the set pressure and temperature are reached and the pressure and temperature are kept for a period of time, because the pressure and temperature of the fluid in the kettle cavity are greater than the pore pressure and temperature of the rock core, the pressure and temperature in the rock core are changed under the action of pressure difference and heat transfer, after the critical pressure and critical temperature of water are exceeded, the fracturing fluid in the rock core is converted into a supercritical state, on one hand, the fracturing fluid in the supercritical state reacts with organic matters or reducing components in the rock core, on the other hand, the special properties of high temperature and high pressure of the fracturing fluid can be used for displacing other fluids in the rock core, and the fluid distribution condition in the pores of the rock core is changed; finally stopping heating, cooling and releasing pressure through an exhaust pipeline;
and 6, opening the kettle cover and taking out the rock sample.
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