An apparatus and method for in-situ pyrolysis of laboratory bulk shale

Abstract

The present application belongs to the technical field of pyrolysis equipment, and particularly relates to a device and method for in-situ pyrolysis of laboratory block shale, which comprises a clamping shell, a copper pipe, a sealing shaft, a shaft pressing rod and a sealing flange; further comprises a sealing mechanism installed inside the clamping shell and located at both ends of the copper pipe, and the sealing mechanism is used for enhancing the sealing property of the clamping shell; through a simple magnetic mechanical positioning mechanism, the present application realizes intuitive inspection of the filling state of quartz sand, and the core components include an internal magnetic isolation sheet and an external magnetic positioning ring; an operator only needs to observe whether the position of the external magnetic positioning ring is deviated, so as to determine whether the internal reaction cavity has reached a "true compaction" state.

Description

Technical Field

[0001] This invention belongs to the field of pyrolysis equipment technology, specifically a device and method for in-situ pyrolysis of blocky shale in the laboratory. Background Technology

[0002] With the increasing depletion of conventional oil and gas resources, unconventional oil and gas resources such as shale oil have become a research focus. Shale reservoirs are characterized by low porosity and permeability, and strong heterogeneity. Their oil and gas generation, discharge, and retention processes are closely coupled. Accurately simulating the in-situ pyrolysis behavior under high temperature and high pressure in the laboratory is the core means to assess their "hydrocarbon generation potential" and "recoverability".

[0003] High-temperature in-situ pyrolysis operations require the use of pyrolysis equipment.

[0004] The existing shale pyrolysis device has the following key defects: (1) poor sealing performance, light hydrocarbons are prone to leak from the edge of the cavity at high temperature, resulting in inaccurate yield calculation and inability to assess the "retention effect" and "discharge efficiency"; (2) unknown internal filling state, the density and uniformity of quartz sand filling cannot be monitored, resulting in distortion of temperature transmission and stress distribution, making it difficult to restore the real formation conditions; (3) insufficient assembly alignment accuracy, small deviations cause stress concentration under high pressure, accelerate the damage of seals or cause device instability, resulting in high experiment failure rate and poor repeatability.

[0005] For example, Chinese patent document CN120703146A discloses a comprehensive simulation experimental device for hydrocarbon generation in gold tubes. This device achieves the basic function of loading and compacting internal samples, but it lacks a monitoring mechanism to ensure that the internal filling state is adequate. It cannot ensure that the quartz sand filling is uniform and dense, which affects the realism of heat transfer and stress simulation. It fails to effectively solve the core problems faced in the development of unconventional energy, such as sealing reliability, the realism of the internal environment, and the repeatability of operation.

[0006] Chinese patent document CN120063799A discloses a method, apparatus, equipment, and medium for evaluating shale hydrocarbon expulsion efficiency. This prior art mainly focuses on "calculating" and "evaluating" hydrocarbon expulsion efficiency by measuring a series of static parameters such as TOC, water saturation, porosity, and crude oil density, and using charts. Although this method involves the concept of hydrocarbon expulsion efficiency, it is essentially an indirect calculation method based on static parameter measurements. It does not involve any hardware devices for conducting physical simulation experiments, and in particular, it cannot provide a realistic, controllable high-temperature and high-pressure in-situ environment for blocky shale samples in a laboratory. Therefore, it fundamentally fails to solve the core problem that this invention aims to address: "how to accurately simulate and directly obtain the products of the pyrolysis process."

[0007] Therefore, in order to meet the standard requirements for the accuracy of pyrolysis experimental data in unconventional shale oil and gas exploration and development, there is an urgent need for a shale pyrolysis device that can ensure sufficient and uniform internal filling, reliable sealing, and rapid and accurate assembly, so as to meet the requirements for the accuracy of experimental data in unconventional oil and gas exploration and development.

[0008] In view of this, the present invention proposes an apparatus and method for in-situ pyrolysis of blocky shale in the laboratory, in order to solve the above-mentioned technical problems. Summary of the Invention

[0009] To overcome the shortcomings of existing technologies and solve the aforementioned technical problems, this invention proposes an apparatus and method for in-situ pyrolysis of blocky shale in the laboratory.

[0010] The technical solution adopted by the present invention to solve its technical problem is: the device for in-situ pyrolysis of blocky shale in the laboratory, as described in the present invention, includes a clamping shell, a copper tube, a sealing shaft, a axial pressure rod and a sealing flange;

[0011] The copper tube is installed inside the clamping housing, and the inner cavity of the copper tube forms a reaction chamber. The sealing shaft and the sealing flange are detachably fixed at both ends of the clamping housing. The inner cavities of the sealing shaft and the sealing flange are slidably sealed with axial pressure rods.

[0012] The clamping housing is provided with an outlet and an injection port, and the top axial pressure rod is equipped with an air injection channel.

[0013] It also includes a sealing mechanism, which is installed inside the clamping housing and located at both ends of the copper tube. The sealing mechanism is used to enhance the sealing performance of the clamping housing and includes a pressure transmitting medium, a graphite sealing ring, and an isolation positioning element.

[0014] The pressure-transmitting medium and the pyrolysis sample are filled together in the reaction chamber, with the pyrolysis sample located in the middle of the reaction chamber and the pressure-transmitting medium located at both ends of the reaction chamber.

[0015] The isolation positioning element is installed on the copper tube and extends into the pressure transmission medium. The isolation positioning element is used to perform layered isolation and thickness positioning of the pressure transmission medium.

[0016] The graphite sealing ring is installed in the inner cavity of the clamping housing, and the graphite sealing ring is sleeved at the joint between the axial pressure rod and the copper tube.

[0017] Preferably, the isolation positioning component includes a magnetic positioning ring and a magnetic isolation plate. The magnetic positioning ring is sleeved and installed on the outside of the copper tube, and the magnetic isolation plate is installed in the reaction chamber. The magnetic positioning ring and the magnetic isolation plate correspond one-to-one.

[0018] The magnetic separator is a sieve-like structure. The magnetic separators located at the same end of the reaction chamber are arranged in a gradient of mesh size, and the magnetic separators closer to the pyrolysis sample have a larger mesh size than the magnetic separators farther away from the pyrolysis sample.

[0019] Preferably, a central long tube with a porous structure is installed inside the clamping housing.

[0020] Preferably, it also includes a precision filling mechanism, which is used to fill the isolation positioning element and the pressure transmitting medium. The precision filling mechanism includes a mounting frame, a control element, a control pump, and a rangefinder.

[0021] The mounting bracket is detachably mounted on the end of the clamping housing. The mounting bracket is magnetically connected to the clamping housing. The control component is fixedly mounted on the mounting bracket. The control component is a length-adjustable telescopic structure. The control component is divided into two groups, and the two groups of control components correspond to a magnetic positioning ring and a magnetic isolation plate, respectively.

[0022] The control pump is mounted on the mounting bracket, and the control component has a pressure transmission chamber. The control input terminal is connected to the pressure transmission chamber. The control component uses negative pressure to adsorb and fix the magnetic positioning ring and magnetic isolation plate.

[0023] A rangefinder is installed on the control component corresponding to the magnetic positioning ring. The rangefinder is used to detect the distance between the magnetic positioning ring and the bottom end of the control component.

[0024] Preferably, the control component consists of an adjustable telescopic rod, a connecting plate, a telescopic suction rod, and a support spring;

[0025] The adjustable telescopic rod is fixedly installed on the mounting frame. The adjustable telescopic rod and the telescopic adsorption rod are fixedly connected by a connecting plate. The support spring is installed inside the telescopic adsorption rod. The rangefinder is installed on the adjustable telescopic rod.

[0026] Preferably, a rubber ring is fixedly installed at the bottom end of the telescopic adsorption rod. The rubber ring is used to enhance the negative pressure adsorption effect between the pressure transmission chamber and the magnetic positioning ring and magnetic isolation sheet.

[0027] Preferably, the mounting bracket is equipped with an air jet rod, which corresponds to the magnetic isolation plate. The air jet rod is an elastic telescopic rod and is electrically connected to the output end of the control pump.

[0028] Preferably, an adjusting component is installed between the telescopic adsorption rod and the control pump. The adjusting component has a conductive cavity, which is electrically connected to both the telescopic adsorption rod and the control pump. The adjusting component has a release hole, and a distribution ring is rotatably installed inside the adjusting component. One side of the distribution ring is located between the telescopic adsorption rod and the control pump. The distribution ring has a docking hole. In the initial state, the distribution ring blocks the release hole, and the docking hole is used to connect the release hole and the conductive cavity.

[0029] Preferably, uniformly distributed elastic sheets are fixedly installed on the circumferential surface of the distribution ring, and the elastic sheets are used to enhance the rotation effect of the distribution ring under the action of directional airflow.

[0030] Preferably, a display is fixedly mounted on the mounting bracket, the display is electrically connected to the rangefinder, and the display is used to display the rangefinder test data.

[0031] A method for in-situ pyrolysis of massive shale in a laboratory setting, the method comprising the following steps:

[0032] S1. Experimental preparation: Select cylindrical shale samples and clean them thoroughly;

[0033] S2. Assembly of the device and confirmation of the internal filling status: With the assistance of the fine filling mechanism, the shale sample and quartz sand are filled into the reaction chamber, and the sealing mechanism is assembled.

[0034] S3. Sealing system closure and pressure application: After the sealing flange and sealing shaft complete the sealing at the upper and lower ends, pressure is applied by the shaft pressure rod;

[0035] S4. Sealing effect test: Close the outlet, and while maintaining the pressure of the axial pressure cylinder, inject gas through the injection port to test the sealing performance of the reaction chamber.

[0036] S5. Pyrolysis Experiment and Product Collection: High temperature is applied to the outside of the clamping shell, and pyrolysis products are collected from the outlet. Finally, the pressure transmission medium is extracted with organic solvent and the yield is calculated to complete the pyrolysis experiment.

[0037] The beneficial effects of this invention are as follows:

[0038] 1. The apparatus and method for in-situ pyrolysis of blocky shale in the laboratory, as described in this invention, achieves intuitive inspection of the quartz sand filling state through a simple magnetic mechanical positioning mechanism. The core components include an internal magnetic isolation plate and an external magnetic positioning ring. When the quartz sand is not densely filled, the internal magnetic isolation plate can be attracted by the external magnetic positioning ring under the action of magnetic force, causing displacement and resulting in the magnetic positioning ring deviating from its initial installation position. When the quartz sand is densely filled, the dense quartz sand firmly fixes the internal magnetic isolation plate in its original position, preventing it from being attracted by magnetic force and moving. At this time, the external magnetic positioning ring will stably remain in its initial positioning position. Therefore, the operator only needs to observe whether the position of the external magnetic positioning ring has shifted to determine whether the reaction chamber has reached a "true compaction" state.

[0039] 2. The apparatus and method for in-situ pyrolysis of blocky shale in the laboratory, as described in this invention, utilizes a precision filling mechanism to provide positioning services for the isolation and positioning components during installation of the isolation and positioning components and the pressure transmission medium. This ensures a more accurate initial installation position and assists in determining the filling limit of the quartz sand. Simultaneously, during the quartz sand filling process, the repeated opening and closing of the pump, combined with the distance detection of the magnetic positioning ring by a rangefinder, facilitates the judgment of the quartz sand filling status by the staff. This provides significant assistance for the staff's observation in a confined space. Attached Figure Description

[0040] The invention will now be further described with reference to the accompanying drawings.

[0041] Figure 1 This is a partial three-dimensional view of the structure of the present invention;

[0042] Figure 2 This is a partial structural cross-sectional view of the present invention;

[0043] Figure 3 It is a 3D assembly diagram of the sealing mechanism and the precision filling mechanism;

[0044] Figure 4 This is an assembly diagram of the sealing mechanism and the precision filling mechanism;

[0045] Figure 5 It is a 3D diagram of the precision loading mechanism;

[0046] Figure 6 This is a partial sectional view of the control component;

[0047] Figure 7 This is a diagram of the internal structure of the adjusting component;

[0048] Figure 8 This is a flowchart of the method of the present invention;

[0049] In the diagram: 1. Clamping shell; 11. Copper tube; 12. Reaction chamber; 13. Sealing shaft; 14. Sealing flange; 15. Shaft pressure rod; 16. Outlet; 17. Inlet; 18. Gas injection channel; 2. Graphite sealing ring; 21. Magnetic positioning ring; 22. Magnetic isolation plate; 23. Central long tube; 24. Mounting bracket; 25. Control pump; 26. Rangefinder; 27. Adjustable telescopic rod; 28. Connecting plate; 29. ​​Telescopic adsorption rod; 3. Support spring; 31. Pressure transmission chamber; 32. Rubber ring; 33. Air jet rod; 4. Adjusting component; 41. Conducting chamber; 42. Release hole; 43. Distribution ring; 44. Docking hole; 45. Elastic sheet; 5. Display. Detailed Implementation

[0050] To make the technical means, creative features, objectives and effects of this invention easier to understand, the invention will be further described below in conjunction with specific embodiments.

[0051] like Figures 1 to 8 As shown, the device for in-situ pyrolysis of blocky shale in the laboratory according to the present invention includes a clamping shell 1, a copper tube 11, a sealing shaft 13, a axial pressure rod 15, and a sealing flange 14.

[0052] The copper tube 11 is installed inside the clamping housing 1, and the inner cavity of the copper tube 11 forms a reaction chamber 12. The sealing shaft 13 and the sealing flange 14 are respectively detachably fixed at both ends of the clamping housing 1. The inner cavities of the sealing shaft 13 and the sealing flange 14 are slidably sealed with axial pressure rods 15.

[0053] The clamping housing 1 is provided with an outlet 16 and an injection port 17, and the top axial pressure rod 15 is equipped with an air injection channel 18.

[0054] It also includes a sealing mechanism, which is installed inside the clamping housing 1 and located at both ends of the copper tube 11. The sealing mechanism is used to enhance the sealing performance of the clamping housing 1. The sealing mechanism includes a pressure transmitting medium, a graphite sealing ring 2, and an isolation positioning element.

[0055] The pressure-transmitting medium and the pyrolysis sample are filled together in the reaction chamber 12, with the pyrolysis sample located in the middle of the reaction chamber 12 and the pressure-transmitting medium located at both ends of the reaction chamber 12.

[0056] The isolation positioning element is installed on the copper tube 11 and extends into the pressure transmission medium. The isolation positioning element is used to perform layered isolation and thickness positioning of the pressure transmission medium.

[0057] The graphite sealing ring 2 is installed in the inner cavity of the clamping housing 1, and the graphite sealing ring 2 is sleeved at the joint between the axial pressure rod 15 and the copper tube 11.

[0058] The isolation and positioning component includes a magnetic positioning ring 21 and a magnetic isolation plate 22. The magnetic positioning ring 21 is sleeved and installed on the outside of the copper tube 11, and the magnetic isolation plate 22 is installed inside the reaction chamber 12. The magnetic positioning ring 21 and the magnetic isolation plate 22 correspond one-to-one.

[0059] The magnetic isolation sheet 22 is a sieve-like structure. The magnetic isolation sheets 22 located at the same end of the reaction chamber 12 are arranged in a gradient of mesh size, and the magnetic isolation sheets 22 closer to the pyrolysis sample have a larger mesh size than the magnetic isolation sheets 22 farther away from the pyrolysis sample.

[0060] The reaction chamber 12 is equipped with a central long tube 23 with a porous structure.

[0061] In this embodiment, the following method flow for the pyrolysis of massive shale is provided, as detailed below:

[0062] 1. Experimental preparation:

[0063] Take a cylindrical blocky shale sample with an average diameter of about 24 mm and a height of about 30 mm, and clean its surface.

[0064] Prepare the quartz sand: use 30-50 mesh quartz sand as the main pressure transmission medium, and reserve a small amount of 100 mesh fine quartz sand. Use organic solvents to clean the quartz sand to remove excess impurities and ensure its cleanliness.

[0065] Inspect all components: Confirm that the reaction chamber 12 (inner diameter 25mm), upper and lower magnetic isolation plates 22 (upper plate 100 mesh, lower plate 200 mesh), graphite sealing ring 2, axial pressure rod 15 and other components are intact.

[0066] 2. Confirmation of device assembly and internal filling status:

[0067] The lower magnetic isolation plate 22 is placed at the bottom of the reaction chamber 12; its magnetic material is neodymium iron boron, and its outer edge is tightly attached to the inner wall of the reaction chamber 12.

[0068] The blocky shale sample was placed upright at the center of reaction chamber 12;

[0069] Different mesh sizes of quartz sand were slowly and evenly filled into the annular space between the shale sample and the reaction chamber 12, while the chamber was slightly vibrated to promote the compaction of the sand.

[0070] When the quartz sand is filled to the level of the top of the sample, cover it with the upper magnetic isolation sheet 22;

[0071] A central tube 23 with a porous structure is inserted into the clamping housing 1. The central tube 23 is used to guide fluid and distribute pressure.

[0072] 3. Sealing system closure and pressure application:

[0073] After confirming that the internal filling is dense, the graphite sealing ring 2 and the magnetic positioning ring 21 are installed on the outside of the copper tube 11 in sequence. The graphite material deforms and tightens at high temperature, laying the foundation for subsequent high-pressure sealing.

[0074] The sealing flange 14 and the sealing shaft 13 are installed to complete the sealing of the upper and lower ends; the sealing cylinder at the lower end continuously pushes upward to achieve the sealing of the lower end.

[0075] When the axial pressure rod 15 is installed, due to the magnetic attraction between the magnetic sealing ring and the magnetic isolation plate 22, the axial pressure rod 15 is automatically guided to the correct position during the descent, achieving automatic centering and avoiding uneven wear with the graphite sealing ring 2. At the same time, during installation, its end contacts the magnetic isolation plate 22. The presence of the magnetic isolation plate 22 provides a clear force reference surface for the axial pressure rod 15, as well as magnetic positioning with the outer end, ensuring that the axial pressure can be uniformly transmitted and completely filled through the quartz sand layer.

[0076] Hydraulic oil is injected into the system through injection port 17. With the sealing effect of the graphite sealing rings at both ends, a closed space is formed inside the clamp. Simultaneously, the axial pressure rod 15 is pushed upward by the axial pressure cylinder at the bottom to apply axial pressure. The axial pressure rod 15 transmits the pressure to the upper magnetic isolation plate 22. Then, through the compacted quartz sand filling layer, the axial pressure is efficiently and uniformly converted into lateral stress acting on the shale sample, which truly simulates the triaxial stress state of the formation. Finally, the axial pressure is efficiently converted into uniform confining pressure, which ultimately stabilizes the system under a confining pressure of 10 MPa.

[0077] 4. Sealing effect inspection:

[0078] A sealing test must be conducted before formal pyrolysis.

[0079] With outlet 16 closed, while maintaining the pressure of the axial pressure cylinder, inject gas at 5-8 MPa through injection port 17.

[0080] Observe whether the pressure gauge reading of the system remains stable. If the pressure does not drop significantly, it proves that the sealing system composed of the graphite sealing ring and the magnetic centering component is reliable and meets the experimental requirements of high temperature and high pressure.

[0081] 5. Pyrolysis experiment and product collection:

[0082] The heating system enclosed in the clamping housing 1 is activated, and the system is heated to the target temperature of 450°C at a heating rate of 5°C / min, and the temperature is maintained for 24 hours.

[0083] Throughout the pyrolysis process, the system pressure remains stable, and the sealing system consisting of the magnetic isolation plate 22, the magnetic positioning ring 21, and the graphite sealing ring effectively prevents the leakage of volatile hydrocarbons under high temperature and high pressure.

[0084] The generated liquid pyrolysis products are discharged through the outlet 16 at the bottom of the clamping shell 1 and collected into the condensation system;

[0085] Disassemble the device, extract the quartz sand with organic solvents, and calculate the yield;

[0086] After the experiment, wait for the device to cool to room temperature, observe that there is no damage to any of the components, and that the magnetic positioning ring 21 on the outside is in the correct position. Then, disassemble the device in the reverse order of assembly.

[0087] Since high temperatures may cause the magnet's performance to degrade or even demagnetize, the magnetic strength of the magnetic isolation plate 22 and the magnetic sealing ring was checked step by step after disassembly. To ensure the accuracy of subsequent experiments and the precision of positioning, the demagnetized magnetic components were remagnetized or replaced with new components to ensure the reliability of their functions.

[0088] In this invention, the isolation positioning component is the core magnetic functional component of the system. Its positioning principle is to achieve intuitive inspection of the quartz sand filling state through a simple magnetic mechanical positioning mechanism. The core component includes an internal magnetic isolation plate 22 and an external magnetic positioning ring 21. When the quartz sand is not densely filled, the internal magnetic isolation plate 22 can be attracted by the external magnetic positioning ring 21 under the action of magnetic force, causing displacement and causing the magnetic positioning ring 21 to deviate from its initial installation position. When the quartz sand is densely filled, the dense quartz sand firmly fixes the internal magnetic isolation plate 22 in its original position, preventing it from being attracted by magnetic force and moving. At this time, the external magnetic positioning ring 21 will be stably maintained in its initial positioning position. Therefore, the operator only needs to observe whether the position of the external magnetic positioning ring 21 has shifted to determine whether the reaction chamber has reached the state of "true compaction".

[0089] At the same time, compared with the prior art, the present invention also has the following significant improvements:

[0090] 1. Pressure transmission technology based on gradient quartz sand filling: By designing a sandwich structure of "magnetic isolation sheet 22 - specific mesh quartz sand - magnetic isolation sheet 22", the confining pressure that is difficult to apply directly is transformed into a uniform confining pressure that can be achieved through axial pressure, which effectively solves the technical problem of simulating formation pressure in blocky shale.

[0091] 2. Internal state monitoring technology based on magnetic isolator 22: The function of magnetic isolator 22 is extended from simple physical isolation to a non-destructive testing sensor for internal filling density, realizing the "visualization" and "controllability" of the initial state before the experiment;

[0092] 3. Automatic alignment and sealing technology based on magnetic adsorption: By utilizing the magnetic self-alignment characteristics of the magnetic positioning ring 21, the assembly process is simplified, the fitting accuracy of the sealing pair is improved, and the risk of leakage and damage caused by assembly deviation is eliminated structurally.

[0093] 4. High-temperature dynamic sealing technology based on graphite material: Graphite sealing ring 2 was selected and a corresponding sealing structure was designed. Taking advantage of its high-temperature stability and deformation self-tightening characteristics, a reliable sealing solution suitable for high-temperature and high-pressure conditions of pyrolysis equipment was constructed.

[0094] As a preferred embodiment of the present invention, it further includes a precision filling mechanism for filling the isolation positioning element and the pressure transmitting medium. The precision filling mechanism includes a mounting frame 24, a control element, a control pump 25 and a rangefinder 26.

[0095] The mounting bracket 24 is detachably mounted on the end of the clamping housing 1. The mounting bracket 24 is magnetically connected to the clamping housing 1. The control component is fixedly mounted on the mounting bracket 24. The control component is a length-adjustable telescopic structure. The control component is divided into two groups, and the two groups of control components correspond to the magnetic positioning ring 21 and the magnetic isolation plate 22, respectively.

[0096] The control pump 25 is mounted on the mounting bracket 24. The control component has a pressure transmission chamber 31. The control input terminal is connected to the pressure transmission chamber 31. The control component fixes the magnetic positioning ring 21 and the magnetic isolation plate 22 by negative pressure adsorption.

[0097] A rangefinder 26 is installed on the control component corresponding to the magnetic positioning ring 21. The rangefinder 26 is used to detect the distance between the magnetic positioning ring 21 and the bottom end of the control component.

[0098] The control component consists of an adjustable telescopic rod 27, a connecting plate 28, a telescopic suction rod 29, and a support spring 3.

[0099] The adjustable telescopic rod 27 is fixedly installed on the mounting frame 24. The adjustable telescopic rod 27 and the telescopic adsorption rod 29 are fixedly connected by the connecting plate 28. The support spring 3 is installed inside the telescopic adsorption rod 29. The rangefinder 26 is installed on the adjustable telescopic rod 27. The pressure transmission chamber 31 is opened inside the telescopic adsorption rod 29 and the adjustable telescopic rod 27, and is connected to the input end of the control pump 25 through a pipe.

[0100] A rubber ring 32 is fixedly installed at the bottom of the telescopic adsorption rod 29. The rubber ring 32 is used to enhance the negative pressure adsorption effect between the pressure transmission chamber 31 and the magnetic positioning ring 21 and the magnetic isolation plate 22. It should be noted that in order to enhance the adsorption effect of the telescopic adsorption rod 29 on the magnetic isolation plate 22 and the magnetic positioning ring 21, the bottom of the telescopic adsorption rod 29 is made of ferromagnetic material, so that the telescopic adsorption rod 29 and the magnetic isolation plate 22 and the magnetic positioning ring 21 have a magnetic attraction effect. Combined with the negative pressure traction effect, the telescopic adsorption rod 29 can stably attract the magnetic isolation plate 22 and the magnetic positioning ring 21. When the negative pressure traction effect disappears, the telescopic adsorption rod 29 detaches from the magnetic isolation plate 22 and the magnetic positioning ring 21.

[0101] In the experiment, to enhance the installation accuracy and convenience of the quartz sand and the isolation positioning components, a precision filling mechanism was also provided in this invention. During actual filling, the pyrolysis sample was first installed in the reaction chamber 12. Then, one end of the reaction chamber 12 was sealed with a soft material such as cotton, with the unsealed end facing upwards. The precision filling mechanism was then adjusted. Since the installation depth of the magnetic positioning ring 21 is clearly defined, the staff actively adjusted the length of the adjustable telescopic rod 27. After adjustment, the control pump 25 was started. The control pump 25 is a conventional circulating air pump, which delivers air during operation. Air is drawn in at the inlet and discharged at the outlet. Since the input end of the control pump 25 is connected to the telescopic suction rod 29, the telescopic suction rod 29 continuously draws in outside air. The operator manually places the magnetic positioning ring 21 and the magnetic separator at the ends of the two sets of telescopic suction rods 29 respectively. When the pressure transmission chamber 31 on the telescopic suction rod 29 is blocked, under the continuous suction action of the control pump 25, the telescopic suction rod 29 is finally in a fully retracted state. At this time, it is inserted into the clamping housing 1. During the process of the mounting bracket 24 approaching and combining with the end of the clamping housing 1, the magnetic positioning ring 21 and the magnetic separator are... 22 is installed to the designated depth. At this point, the reaction chamber 12 is filled with a pressure-transmitting medium, which is quartz sand with a smaller aperture than the current magnetic isolation plate 22. As the quartz sand gradually passes over the magnetic isolation plate 22 and fills the gap between the reaction chamber 12 and the pyrolysis sample, the height of the quartz sand gradually approaches that of the magnetic isolation plate 22. At this point, the control pump 25 is turned off. After the negative pressure traction is lost, under the action of the support spring 3 and gravity, the magnetic isolation plate 22 has a downward tendency to move. Therefore, when the quartz sand at the bottom of the magnetic isolation plate 22 is not compacted, both the magnetic isolation plate 22 and the magnetic positioning ring 21 move downward. When the bottom of the magnetic isolation plate 22 is filled with quartz sand, the magnetic isolation plate 22 is supported by the quartz sand and is in a stable state. Under the magnetic attraction, the magnetic positioning ring 21 is also in a stable and immobile state. During this process, the rangefinder 26 continuously tests the distance of the magnetic positioning ring 21. When the data of the rangefinder 26 changes, the control pump 25 is restarted and quartz sand is filled. When the data of the rangefinder 26 does not change during this process, the precision filling mechanism is removed and the above actions are repeated to install the next set of isolation positioning components until the isolation positioning components are completely installed.

[0102] This invention, by setting up a precision filling mechanism, provides positioning services for the isolation positioning component during the installation of the isolation positioning component and the pressure transmission medium, ensuring a more accurate initial installation position and assisting in the filling limit of the quartz sand. At the same time, during the quartz sand filling process, by controlling the repeated opening and closing of the pump 25, and cooperating with the distance measuring instrument 26 to detect the distance of the magnetic positioning ring 21, the operator can judge the filling status of the quartz sand. This provides great assistance to the operator's observation in a confined space.

[0103] In a preferred embodiment of the present invention, an air jet rod 33 is mounted on the mounting bracket 24. The air jet rod 33 corresponds to the magnetic isolation plate 22. The air jet rod 33 is an elastic telescopic rod and is electrically connected to the output end of the control pump 25.

[0104] An adjusting component 4 is installed between the telescopic adsorption rod 29 and the control pump 25. A conduction cavity 41 is provided inside the adjusting component 4. The conduction cavity 41 is conductively connected to both the telescopic adsorption rod 29 and the control pump 25. A release hole 42 is provided on the adjusting component 4. A distribution ring 43 is rotatably installed inside the adjusting component 4. One side of the distribution ring 43 is located between the telescopic adsorption rod 29 and the control pump 25. A docking hole 44 is provided on the distribution ring 43. In the initial state, the distribution ring 43 blocks the release hole 42. The docking hole 44 is used to connect the release hole 42 and the conduction cavity 41.

[0105] The distribution ring 43 has uniformly distributed elastic plates 45 fixedly installed on its circumferential surface. The elastic plates 45 are used to enhance the rotation effect of the distribution ring 43 under the action of directional airflow.

[0106] A display 5 is fixedly mounted on the mounting bracket 24. The display 5 is electrically connected to the rangefinder 26 and is used to display the test data of the rangefinder 26.

[0107] To further enhance the ease of filling the pressure-transmitting medium, during the actual filling process, the jet rod 33 continuously injects air drawn by the control pump 25 onto the magnetic isolation plate 22, and through the mesh of the magnetic isolation plate 22, it injects air below it. The impact of the airflow assists in dispersing the quartz sand. Simultaneously, as the control pump 25 continues to operate, the airflow flows through the transmission cavity 41 on the adjusting component 4 and flows from one side of the distribution ring 43. With the cooperation of the elastic plate 45, it drives the distribution ring 43 to rotate continuously, thereby causing the docking hole 44 and the release hole 42 to... The periodic overlap occurs when the two overlap, making the conduction cavity 41 connected to the outside world. This reduces the negative pressure intensity inside the telescopic adsorption rod 29, causing the magnetic isolation plate 22 and the magnetic positioning ring 21 to tend to move downwards. This causes periodic oscillations in the filled quartz sand. Combined with the external oscillations on the clamping shell 1, this promotes rapid compaction of the quartz sand. Therefore, during the filling process, the value on the display 5 fluctuates periodically. When the value on the display 5 stabilizes, it indicates that the quartz sand filling is complete at the current stage, further facilitating the filling of quartz sand.

[0108] A method for in-situ pyrolysis of massive shale in a laboratory setting, the method comprising the following steps:

[0109] S1. Experimental preparation: Select cylindrical shale samples and clean them thoroughly;

[0110] S2. Assembly of the device and confirmation of the internal filling status: With the assistance of the fine filling mechanism, the shale sample and quartz sand are filled into the reaction chamber, and the sealing mechanism is assembled.

[0111] S3. Sealing system closure and pressure application: After the sealing flange 14 and sealing shaft 13 complete the sealing at the upper and lower ends, pressure is applied by the shaft pressure rod 15.

[0112] S4. Sealing effect test: Close outlet 16, and while maintaining the pressure of the axial pressure cylinder, inject gas through injection port 17 to test the sealing performance of the reaction chamber.

[0113] S5. Pyrolysis Experiment and Product Collection: High temperature is applied to the outside of the clamping shell 1, and the pyrolysis products are collected through the outlet 16. Finally, the pressure transmission medium is extracted with organic solvent and the yield is calculated to complete the pyrolysis experiment.

[0114] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely illustrative of the principles of the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the present invention as claimed. The scope of protection of the present invention is defined by the appended claims and their equivalents.

Claims

1. An apparatus for in-situ pyrolysis of blocky shale in the laboratory, comprising a clamping shell (1), a copper tube (11), a sealing shaft (13), a axial pressure rod (15), and a sealing flange (14). The copper tube (11) is installed inside the clamping shell (1), and the inner cavity of the copper tube (11) forms a reaction chamber (12). The sealing shaft (13) and the sealing flange (14) are respectively detachably fixed at both ends of the clamping shell (1). The inner cavities of the sealing shaft (13) and the sealing flange (14) are slidably sealed with axial pressure rods (15). The clamping housing (1) is provided with an outlet (16) and an injection port (17), and an air injection channel (18) is installed on the top shaft pressure rod (15). Its features are: It also includes a sealing mechanism, which is installed inside the clamping housing (1) and located at both ends of the copper tube (11). The sealing mechanism is used to enhance the sealing performance of the clamping housing (1). The sealing mechanism includes a pressure transmission medium, a graphite sealing ring (2), and an isolation positioning element. The pressure-transmitting medium and the pyrolysis sample are filled together in the reaction chamber (12), with the pyrolysis sample located in the middle of the reaction chamber (12) and the pressure-transmitting medium located at both ends of the reaction chamber (12); The isolation positioning element is installed on the copper tube (11) and extends into the pressure transmission medium. The isolation positioning element is used to perform layered isolation and thickness positioning of the pressure transmission medium. The graphite sealing ring (2) is installed in the inner cavity of the clamping shell (1) and is sleeved on the joint between the axial pressure rod (15) and the copper tube (11); The isolation positioning component includes a magnetic positioning ring (21) and a magnetic isolation plate (22). The magnetic positioning ring (21) is sleeved and installed on the outside of the copper tube (11), and the magnetic isolation plate (22) is installed in the reaction chamber (12). The magnetic positioning ring (21) and the magnetic isolation plate (22) correspond one-to-one. The magnetic isolation sheet (22) is a sieve-like structure. The magnetic isolation sheets (22) located at the same end of the reaction chamber (12) are arranged in a gradient of mesh number, and the magnetic isolation sheets (22) closer to the pyrolysis sample have a larger mesh number than the magnetic isolation sheets (22) farther away from the pyrolysis sample.

2. The apparatus for in-situ pyrolysis of blocky shale in the laboratory according to claim 1, characterized in that: The clamping housing (1) is equipped with a central long tube (23) with a porous structure.

3. The apparatus for in-situ pyrolysis of blocky shale in the laboratory according to claim 2, characterized in that: It also includes a precision filling mechanism for filling isolation positioning components and pressure transmission medium, the precision filling mechanism including a mounting frame (24), a control component, a control pump (25) and a rangefinder (26). The mounting bracket (24) is detachably mounted on the end of the clamping shell (1). The mounting bracket (24) is magnetically attached to the clamping shell (1). The control component is fixedly mounted on the mounting bracket (24). The control component is a length-adjustable telescopic structure. The control component is divided into two groups, and the two groups of control components correspond to the magnetic positioning ring (21) and the magnetic isolation plate (22) respectively. The control pump (25) is mounted on the mounting bracket (24). The control component has a pressure transmission chamber (31). The input end of the control pump (25) is connected to the pressure transmission chamber (31). The control component fixes the magnetic positioning ring (21) and the magnetic isolation plate (22) by negative pressure adsorption. A rangefinder (26) is installed on the control component corresponding to the magnetic positioning ring (21). The rangefinder (26) is used to detect the distance between the magnetic positioning ring (21) and the bottom end of the control component.

4. The apparatus for in-situ pyrolysis of blocky shale in the laboratory according to claim 3, characterized in that: The control component consists of an adjustable telescopic rod (27), a connecting plate (28), a telescopic suction rod (29), and a support spring (3); The adjustable telescopic rod (27) is fixedly installed on the mounting frame (24). The adjustable telescopic rod (27) and the telescopic adsorption rod (29) are fixedly connected by a connecting plate (28). The support spring (3) is installed inside the telescopic adsorption rod (29). The rangefinder (26) is installed on the adjustable telescopic rod (27).

5. The apparatus for in-situ pyrolysis of blocky shale in the laboratory according to claim 4, characterized in that: A rubber ring (32) is fixedly installed at the bottom of the telescopic adsorption rod (29). The rubber ring (32) is used to enhance the negative pressure adsorption effect between the pressure transmission chamber (31) and the magnetic positioning ring (21) and the magnetic isolation sheet (22).

6. An apparatus for in-situ pyrolysis of blocky shale in a laboratory, as described in claim 4 or 5, characterized in that: The mounting bracket (24) is equipped with an air jet rod (33), which corresponds to the magnetic isolation plate (22). The air jet rod (33) is an elastic telescopic rod, and the air jet rod (33) is connected to the output end of the control pump (25).

7. The apparatus for in-situ pyrolysis of blocky shale in the laboratory according to claim 6, characterized in that: An adjusting component (4) is installed between the telescopic adsorption rod (29) and the control pump (25). A conduction cavity (41) is provided in the adjusting component (4). The conduction cavity (41) is conductively connected to the telescopic adsorption rod (29) and the control pump (25). A release hole (42) is provided on the adjusting component (4). A distribution ring (43) is rotatably installed in the adjusting component (4). One side of the distribution ring (43) is located between the telescopic adsorption rod (29) and the control pump (25). A docking hole (44) is provided on the distribution ring (43). In the initial state, the distribution ring (43) blocks the release hole (42). The docking hole (44) is used to connect the release hole (42) and the conduction cavity (41).

8. The apparatus for in-situ pyrolysis of blocky shale in the laboratory according to claim 7, characterized in that: The distribution ring (43) has uniformly distributed elastic plates (45) fixedly installed on its circumferential surface. The elastic plates (45) are used to enhance the rotation effect of the distribution ring (43) under the action of directional airflow. The mounting bracket (24) has a display (5) fixedly installed on it. The display (5) is electrically connected to the rangefinder (26). The display (5) is used to display the test data of the rangefinder (26).

9. A method for in-situ pyrolysis of massive shale in a laboratory setting, characterized in that: This method uses the in-situ pyrolysis apparatus of claim 8, and includes the following steps: S1. Experimental preparation: Select cylindrical shale samples and clean them thoroughly; S2. Assembly of the device and confirmation of the internal filling status: With the assistance of the fine filling mechanism, the shale sample and quartz sand are filled into the reaction chamber, and the sealing mechanism is assembled. S3. Sealing system closure and pressure application: After the sealing flange (14) and sealing shaft (13) complete the sealing at the upper and lower ends, pressure is applied by the shaft pressure rod (15); S4. Sealing effect test: Close the outlet (16), and under the condition of maintaining the pressure of the axial pressure cylinder, inject gas through the injection port (17) to test the sealing performance of the reaction chamber; S5. Pyrolysis Experiment and Product Collection: High temperature is applied to the outside of the clamping shell (1), and pyrolysis products are collected from the outlet (16). Finally, the yield is calculated after organic solvent extraction of the pressure transmission medium to complete the pyrolysis experiment.

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