An in-situ high-temperature and high-pressure visual reactor capable of taking gravity into account and its application

Abstract

The present invention discloses an in-situ high-temperature and high-pressure visual reactor that can take into account the effect of gravity and its application, which belongs to the technical field of multiphase fluid mechanics experimental equipment. The in-situ high-temperature and high-pressure visual reactor provided by the present invention utilizes the linkage and tilt adjustment (0~90°) of the fiber-coupled laser light source and the model clamping device to realize the in-situ simulation of the gravity vector under non-rotating conditions; the multi-prism reflection system corrects the optical path offset in real time to form an orthogonal collimated optical path, ensuring the observation field stability and data accuracy of processes such as oil-water separation and CO2 diffusion under high-temperature and high-pressure environments. In addition, the present invention eliminates the alternating stress effect of the rotational torque on the sealing interface through the split clamp body and the rigid locking sealing structure, significantly reducing the risk of high-pressure dynamic seal failure, while simplifying the device volume, avoiding interference from peripheral equipment, and improving experimental safety and spatial adaptability.

Description

Technical Field

[0001] The present invention relates to the technical field of multiphase fluid mechanics experimental equipment, and in particular to an in-situ high-temperature and high-pressure visual reactor capable of taking gravity into account and applications thereof. Background Art

[0002] The information disclosed in the background of the invention is only intended to enhance understanding of the overall background of the invention and should not necessarily be regarded as an admission or any form of suggestion that the information constitutes the prior art already known to a person skilled in the art.

[0003] High-temperature, high-pressure reactors precisely simulate deep, high-temperature, and high-pressure geological conditions to replicate in situ processes such as multiphase fluid seepage and mineral phase transitions. They have become core equipment for studying the displacement dynamics of multiphase fluids within micro- and nanoscale pore throats in deep geotechnical projects like oil and gas development and underground energy storage. However, when using this equipment to observe gravity-driven dynamic behaviors such as phase separation, sedimentation, and buoyancy during fluid migration in deep geotechnical projects, the spatial angle between the observation axis and the gravity vector directly affects the accuracy of the experimental data.

[0004] Existing technologies generally employ an integrated design in which the reactor body, optical imaging system, and light source module rotate synchronously. While this design can adjust the spatial angle between the observation axis and the gravity vector, it presents significant technical bottlenecks. On the one hand, this solution requires a high-rigidity rotating base to resist the torque generated by large-angle rotation and reserve redundant space to prevent interference from peripheral equipment. This results in a bulky and redundant device, making it difficult to adapt to complex experimental environments. On the other hand, during dynamic rotation, the sealing interface between the high-pressure reaction chamber and the external pipeline is subjected to long-term alternating stress and frictional wear. Under high-temperature and high-pressure coupling conditions, the sealing material is prone to plastic deformation or fatigue cracking, which poses a risk of medium leakage and seriously restricts the long-term operational stability of the device and experimental safety. Furthermore, the mechanical vibration caused by the overall rotation can easily interfere with the precision optical observation system, causing image blur or data distortion, further reducing the accuracy of gravity field simulation experiments. Therefore, achieving multi-angle dynamic gravity field simulation under non-rotating conditions while ensuring high-temperature and high-pressure sealing performance and observation accuracy has become a technical challenge that urgently needs to be overcome in fields such as deep-earth oil and gas resource development and carbon sequestration monitoring. Summary of the Invention

[0005] In view of this, the present invention provides an in-situ high-temperature and high-pressure visual reactor and its application that can take into account the effect of gravity; the in-situ high-temperature and high-pressure visual reactor provided by the present invention can realize the in-situ simulation of the gravity vector under non-rotating conditions, has a small size, is easy to operate and provides clear images, thereby providing reliable technical support for the successful implementation of displacement experiments in real reservoir environments.

[0006] In a first aspect, the present invention provides an in-situ high-temperature and high-pressure visual reactor that can take into account the effect of gravity, comprising a reactor body and an optical path observation system;

[0007] The optical path observation system includes a fiber-coupled laser light source, a model clamping device, a multi-prism reflection system, a rotation angle adjustment device and an optical image acquisition system; the model clamping device is used to clamp the model to be observed;

[0008] The reactor body includes a reaction chamber and a visualization window, and the reaction chamber is provided with a fiber-coupled laser light source, a model clamping device, and a multi-prism reflection system;

[0009] The fiber-coupled laser light source is rigidly connected to the model clamping device to form a linkage body, and an inclination adjustment of 0 to 90 degrees is achieved through a rotation angle adjustment device to simulate different gravitational inclination conditions; the laser beam emitted by the fiber-coupled laser light source is vertically incident on the model to be observed placed on the model clamping device, and the laser beam passes through the model to be observed to the multi-prism reflection system. After the multi-prism reflection system performs spectroscopic correction, an orthogonal collimated light path perpendicular to the visualization window is formed. The orthogonal collimated light path passes through the visualization window and enters the optical image acquisition system to realize image observation.

[0010] In some embodiments of the present invention, the reactor body further includes a reactor cover, and the reaction chamber and the reactor cover form a rigid locking sealing structure through a split clamp body, a first sealing ring, and circumferentially distributed connecting screws.

[0011] In some embodiments of the present invention, the split clamp body is composed of two independent semi-annular components, the material of which is 1Cr18Ni9Ti austenitic stainless steel, and the inner curved surface thereof is precisely machined to form a clearance fit structure with the reactor body.

[0012] In some embodiments of the present invention, the reactor body is provided with a confining pressure delivery pipeline, an optical fiber inlet, a pressure gauge and a temperature gauge; a confining pressure ring cavity is formed inside the reaction chamber, and the confining pressure ring cavity is connected to the confining pressure delivery pipeline.

[0013] In some embodiments of the present invention, the reactor body is further provided with an explosion-proof valve and a horizontal bubble tube. The explosion-proof valve is used for safe pressure release, and the horizontal bubble tube is used for leveling control of the reactor body.

[0014] In some embodiments of the present invention, the rotation angle adjustment device includes a drive shaft, a knob and a second sealing ring, the knob is located outside the reaction chamber and is used to adjust the rotation angle of the drive shaft; the drive shaft is fixedly connected to the model clamping device and the polygonal mirror reflection system; the drive shaft passes through a preset hole on the side wall of the reaction chamber and is connected to the knob; a second sealing ring is provided at the contact portion between the drive shaft and the reaction chamber.

[0015] In some embodiments of the present invention, the fiber-coupled laser light source is connected to the fiber inlet via an optical fiber.

[0016] In some embodiments of the present invention, the light transmittance of the visualization window is greater than 95%, and the visualization window is connected to the reaction chamber via a sealing assembly. Furthermore, the visualization window is made of sapphire glass, and the sealing assembly is a combination of metal and fluororubber. Furthermore, the visualization window is coated with a gold coating as a conductive layer, with a thickness of 40-60 nm, to prevent contamination by electrostatic adsorption particles.

[0017] In some embodiments of the present invention, the visualization window is arranged at the bottom of the reaction chamber; the model clamping device is arranged near the top of the reaction chamber; the center point of the projection of the model clamping device on the bottom of the reaction chamber, the center point of the visualization window and the center point of the bottom of the reaction chamber are located in the same straight line, and the center point of the projection of the model clamping device on the bottom of the reaction chamber and the center point of the visualization window are located on both sides of the center point of the bottom of the reaction chamber.

[0018] In some embodiments of the present invention, the multi-prism reflection system includes a first prism and a second prism, the first prism is located below the model clamping device and is arranged close to the bottom of the reaction chamber; the second prism is located above the visualization window and is arranged close to the top of the reaction chamber; the first prism and the second prism are arranged opposite to each other; the angle of the first prism and the second prism is adjustable, and is used to perform spectral correction on the laser beam of the fiber-coupled laser light source through the observation model to form an orthogonal collimated light path, and then penetrate the visualization window into the optical image acquisition system.

[0019] In some embodiments of the present invention, the optical image acquisition system is located outside the reactor body and includes a microscope and a high-speed camera, with the microscope facing the visualization window. The microscope is used to magnify the pore throat structure and microscopic distribution of multiphase fluids (oil, water, CO2, etc.) within the observation model (such as a rock core or micro-nanochip); the high-speed camera is used to record transient behaviors such as gravity-driven phase separation, sedimentation, and buoyancy at a high frame rate, acquiring dynamic data with millisecond-level time resolution.

[0020] In some embodiments of the present invention, the in-situ high-temperature and high-pressure visual reactor further includes a temperature-pressure coordinated control system, which includes a temperature control box and a heating jacket coated on the outer wall of the reaction chamber.

[0021] In some embodiments of the present invention, the heating jacket and the temperature control box are linked for control. The heating jacket wraps around the outer wall of the reaction chamber, achieving uniform heat distribution and a temperature gradient of less than 2°C through a serpentine winding layout. The temperature control box incorporates a built-in PID control module that dynamically adjusts the heating jacket's power output by providing real-time temperature feedback from a K-type thermocouple embedded in the reaction chamber wall. Furthermore, the heating jacket is constructed of an aluminum silicate fiber matrix and a nickel-chromium alloy heating wire.

[0022] In some embodiments of the present invention, a pressure sensor is configured inside the reactor body to monitor the pressure inside the reactor in real time and to generate an overpressure buzzer alarm.

[0023] In some embodiments of the present invention, the reaction chamber adopts an integral weld-free structure, and the material is 1Cr18Ni9Ti stainless steel, which is pressure-resistant and corrosion-resistant; the sealing ring is made of fluororubber; and the reactor body is cylindrical.

[0024] In a second aspect, the present invention provides an application of the above-mentioned in-situ high-temperature and high-pressure visual reactor that can take into account the effect of gravity, wherein the application is an application in the study of multiphase displacement mechanism;

[0025] The specific application method is as follows: the model to be observed is clamped and fixed by a model clamping device and placed inside the reaction chamber; the fiber-coupled laser light source and the model clamping device are controlled to rotate within an angle range of 0 to 90 degrees by a rotation angle adjustment device to realize the simulation of the model to be observed under different gravitational inclination angles; the laser beam of the fiber-coupled laser light source is vertically incident on the model to be observed, and the laser beam passes through the model to be observed to the multi-prism reflection system, and is split and corrected by the multi-prism reflection system to form an orthogonal collimated light path perpendicular to the visualization window. The orthogonal collimated light path penetrates the visualization window and enters the optical image acquisition system to realize image observation.

[0026] Specific application scenarios include oil and gas reservoir seepage, CO2 storage, underground hydrogen storage, etc.

[0027] Compared with the prior art, the present invention has achieved the following beneficial effects:

[0028] (1) The present invention utilizes the linkage and tilt adjustment (0-90°) of the fiber-coupled laser light source and the model clamping device to realize the in-situ simulation of the gravity vector under non-rotating conditions; the multi-prism reflection system corrects the optical path offset in real time to form an orthogonal collimated optical path, ensuring the observation field stability and data accuracy of processes such as oil-water separation and CO2 diffusion under high temperature and high pressure environments.

[0029] (2) The present invention supports multimodal dynamic observations such as fluorescence labeling, particle tracking, and interferometric imaging through the collaboration of visualization windows, microscopes, and high-speed cameras. The integrated temperature and pressure collaborative control system enables accurate simulation of deep-earth environments, is compatible with the experimental requirements of micro-nano chips and real rock cores, and provides a full-scale experimental platform for high-temperature and high-pressure displacement dynamics research.

[0030] (3) The present invention breaks through the traditional integral rotation design. Through the split clamp body and rigid locking seal structure, the alternating stress effect of the rotational torque on the sealing interface is eliminated, which significantly reduces the risk of high-pressure dynamic seal failure. At the same time, it simplifies the device volume, avoids interference from peripheral equipment, and improves experimental safety and spatial adaptability. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] The drawings, which constitute part of the present invention, are intended to provide a further understanding of the present invention. The exemplary embodiments of the present invention and their descriptions are intended to explain the present invention and do not constitute undue limitations thereon. It is obvious that one of ordinary skill in the art could derive other drawings based on these drawings without inventive effort.

[0032] Figure 1 Schematic diagram of the overall structure of the in-situ high-temperature and high-pressure visual reactor device of Example 1 of the present invention;

[0033] Figure 2 Schematic diagram of the cross-sectional structure of the reaction chamber of the in-situ high-temperature and high-pressure visual reactor device of Example 1 of the present invention;

[0034] Figure 3 1. This is a schematic diagram of the top view of the reaction chamber of the in-situ high-temperature and high-pressure visual reactor device according to Example 1 of the present invention;

[0035] Figure 4 This is a partial schematic diagram of the in-situ high-temperature and high-pressure visual reactor device of Example 1 of the present invention;

[0036] Figure 5 Schematic diagram of light path propagation when the model to be observed is placed horizontally according to Example 2 of the present invention;

[0037] Figure 6 Schematic diagram of light path propagation when the model to be observed is rotated 30° counterclockwise in Example 2 of the present invention;

[0038] Figure 7 Schematic diagram of light path propagation when the model to be observed is rotated 60° counterclockwise in Example 2 of the present invention;

[0039] Figure 8 Schematic diagram of light path propagation when the model to be observed is rotated 90° counterclockwise in Example 2 of the present invention;

[0040] In the figure, 1. reaction chamber; 2. reactor cover; 3. split clamp body; 4. connecting screw; 5. first sealing ring; 6. explosion-proof valve; 7. confining pressure delivery pipe inlet; 8. horizontal bubble tube; 9. temperature gauge; 10. pressure gauge; 11. inlet duct; 12. outlet duct; 13. visualization window; 14. sealing assembly; 15. confining pressure delivery pipe; 16. confining pressure ring cavity; 17. heating jacket; 18. temperature control box; 19. optical fiber; 20. optical fiber coupled laser light source; 21. model clamping device; 22. knob; 23. microscope; 24. first drive shaft; 25. optical fiber inlet; 26. first prism; 27. second prism; 28. second drive shaft; 29. ​​third drive shaft; 30. second sealing ring. DETAILED DESCRIPTION

[0041] It should be noted that the specific embodiments of the present invention described herein are intended for illustrative purposes only and are not to be construed as limiting the invention in any way. Given the teachings of this invention, skilled artisans may conceive of any possible variations based on the invention, all of which should be considered within the scope of the invention. It should be noted that when an element is referred to as being "disposed on" another element, it may be directly on the other element or with an intervening element. When an element is referred to as being "connected to" another element, it may be directly connected to the other element or with an intervening element. Unless otherwise expressly specified or limited, the terms "disposed," "mounted," "connected," and "connected" should be interpreted broadly. For example, they may refer to fixed, removable, or integral connections; mechanical or electrical connections; direct or indirect connections through an intermediary; or internal communication between two elements. A person of ordinary skill in the art will understand the specific meanings of these terms based on the specific circumstances. The terms "vertical," "horizontal," "upper," "lower," "left," "right," and similar expressions used herein are for illustrative purposes only and do not represent the only embodiments. The terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.

[0042] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those skilled in the art to which the present invention pertains. The terms used herein in the specification of the present invention are for the purpose of describing specific embodiments only and are not intended to limit the present invention. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.

[0043] The technical solution of the present invention is further described below with reference to specific embodiments.

[0044] Example 1

[0045] This embodiment provides an in-situ high-temperature and high-pressure visual reactor device that can take into account the effect of gravity, such as Figure 1 and Figure 2 As shown, it includes a reactor body, a temperature and pressure coordinated control system and an optical path observation system.

[0046] The reactor body is cylindrical and consists of a reaction chamber 1, a reactor cover 2, a split clamp 3, connecting screws 4, and a first sealing ring 5. The reactor body is equipped with an explosion-proof valve 6, a confining pressure delivery pipe inlet 7, a horizontal bubble tube 8, a thermometer 9, a pressure gauge 10, and a fiber optic inlet 25. The reaction chamber 1 is a seamless, cylindrical structure with a diameter of 14.5 cm and a height of 10.5 cm. It is constructed of 1Cr18Ni9Ti stainless steel, which is pressure-resistant and corrosion-resistant. The reaction chamber 1 and reactor cover 2 are sealed together by the split clamp 3, connecting screws 4, and the first sealing ring 5 to ensure the device's tightness. The split clamp 3 is composed of two independent semi-annular components made of 1Cr18Ni9Ti austenitic stainless steel. Its inner curved surface is precisely machined to create a clearance fit with the reactor body. The split clamp body 3 aligns the reactor lid 2 with the flange of the reaction chamber 1 (not shown). Connecting screws 4 are screwed evenly along the circumference, and a pre-tightening torque of 120 N·m is applied to ensure uniform compressive stress distribution across the flange surface. The first sealing ring 5, made of fluororubber, is embedded in the flange sealing groove of the reaction chamber 1. The pre-tightening force of the screws produces axial compression deformation with a compression ratio of 15-20%, establishing an airtight barrier with a pressure rating of ≥35 MPa.

[0047] The horizontal bubble tube 8 on the upper part of the reactor cover 2 is used to control the leveling of the reactor body; the temperature gauge 9 and the pressure gauge 10 transmit the temperature information and pressure information inside the reactor body to the outside; the explosion-proof valve 6 is located on the pressure gauge 10 for safe pressure release.

[0048] A visualization window 13 is located at the bottom of the reaction chamber 1 for easy observation. This window is made of sapphire glass, which boasts a high light transmittance exceeding 95%, meeting the requirements for high-definition in-situ observation. It is also heat- and pressure-resistant, meeting the design temperature of 100°C and the design pressure of 35 MPa. The visualization window 13 is connected to the reaction chamber 1 via a sealing assembly 14, made of a combination of metal and fluororubber. The visualization window 13 is mounted below the reaction chamber 1. The inner surface of the visualization window 13, near the reaction chamber 1, is coated with a 50nm thick gold coating as a conductive layer to prevent electrostatic adsorption of particles.

[0049] The reactor body features an inlet conduit 11 and an outlet conduit 12 on either side; these conduits serve as channels for the injection and discharge of the model fluid to be observed. Both conduits 11 and 12 are constructed from 1Cr18Ni9Ti austenitic stainless steel, resistant to high temperatures and pressures. Furthermore, the semi-annular split clamp body 3 is provided with coaxial threaded holes with a diameter of 2.5 ± 0.02 mm, which accommodate the flange connections of the inlet and outlet conduits 11 and 12.

[0050] A confining pressure ring cavity 16 is formed within reaction chamber 1 and communicates with confining pressure delivery pipe 15, which in turn communicates with confining pressure delivery pipe inlet 7. A pressure sensor (not shown) is also located within the reactor body to monitor the pressure within the reactor in real time and provide an overpressure alarm.

[0051] In this embodiment, the sealing of the reactor body is verified as follows: the confining pressure liquid is injected into the reaction chamber 1 to 35 MPa, and the pressure is maintained for 24 hours. The leakage rate detector shows that the leakage is less than 1×10 -6 Pa·m 3 / s, meeting ASME B16.20 standards.

[0052] The temperature and pressure coordinated control system includes a heating jacket 17 and a temperature control box 18; the heating jacket 17 and the temperature control box 18 realize linkage control to achieve the purpose of adjusting the experimental temperature in the reaction chamber 1. The heating jacket 17 is coated on the outer wall of the reaction chamber 1, and a uniform distribution of the heat field is achieved through a serpentine winding layout, with a temperature gradient of <2°C. The temperature control box 18 has a built-in PID adjustment module, which uses a K-type thermocouple embedded in the inner wall of the reaction chamber 1 to measure the temperature with an accuracy of ±0.5°C and real-time feedback of the temperature signal, dynamically adjusts the power output of the heating jacket 17, and adjusts the response time to ≤1s. The winding layout of the heating jacket 17 cooperates with the PID algorithm to achieve a temperature fluctuation of the medium in the reaction chamber 1 of <1.5°C, so as to achieve thermal control accuracy. The material of the heating jacket 17 is an aluminum silicate fiber matrix and a nickel-chromium alloy heating wire. The experimental temperature of this embodiment is from room temperature to 100°C.

[0053] like Figure 2 and Figure 3 As shown, the optical path observation system consists of a fiber-coupled laser light source 20, a model holding device 21, a rotation angle adjustment device, a multi-prism reflection system, a microscope 23, and a high-speed camera (not shown). Microscope 23 faces the visualization window 13. Microscope 23 is a Nikon inverted microscope equipped with a long working distance objective lens with a numerical aperture (NA) of 0.45 and a working distance of 25 mm. Its objective lens faces the visualization window 13. After being corrected by the multi-prism reflection system, the optical path passes through the visualization window 13 and enters the objective lens of microscope 23. Real-time image capture and analysis are controlled by IS Elements software.

[0054] The model clamping device 21 is used to secure the model to be observed. In this embodiment, it uses a spring-loaded clamping method, but those skilled in the art may also choose other clamping methods as needed. The model clamping device 21 is positioned near the top of the reaction chamber 1. The center point of the model clamping device 21's projection on the bottom of the reaction chamber 1, the center point of the visualization window 13, and the center point of the bottom of the reaction chamber 1 are located on the same straight line. The center point of the model clamping device 21's projection on the bottom of the reaction chamber 1 and the center point of the visualization window 13 are located on either side of the center point of the bottom of the reaction chamber 1.

[0055] The fiber-coupled laser light source 20 is rigidly connected to the model clamping device 21 via a flange, forming a linked assembly. The axes of the two components remain parallel. The fiber-coupled laser light source 20 is connected to the fiber inlet 25 via the optical fiber 19. The fiber inlet 25 provides a passage for the optical fiber 19 to enter the reactor. The optical fiber 19 serves as the "transmission medium," while the fiber-coupled laser light source 20 serves as the "generator" of the optical signal.

[0056] The multi-prism reflection system includes a first prism 26 and a second prism 27. The first prism 26 is located below the model holding device 21, and the second prism 27 is located above the visualization window 13. Figure 2 、 Figure 3 and Figure 4 As shown, the rotation angle adjustment device includes a knob 22, a first drive shaft 24, a second drive shaft 28, a third drive shaft 29, and a second sealing ring 30. The knob 22 is located outside the reaction chamber 1 and is provided with angle scale lines on its surface. There are three knobs 22 in total, which independently drive the first drive shaft 24, the second drive shaft 28, and the third drive shaft 29 to adjust the rotation angle. The knob 22 can also be further provided with a locking device. After the knob 22 is rotated to the target angle, the locking device circumferentially fixes the first drive shaft 24, the second drive shaft 28, and the third drive shaft 29 through mechanical interference or friction constraint. The first drive shaft 24, the second drive shaft 28, and the third drive shaft 29 pass through a pre-set hole in the side wall of the reaction chamber 1 and are connected to the knob 22. A second sealing ring 30 is provided at the contact portion of the first drive shaft 24, the second drive shaft 28, and the third drive shaft 29 with the reaction chamber 1. The second sealing ring 30 is made of fluororubber and has an interference fit with the first drive shaft 24, the second drive shaft 28, and the third drive shaft 29 to ensure a good sealing of the reactor and to some extent prevent angular deviation. In another embodiment of the present invention, the knob 22 can be replaced with a rotary motor, and the rotation and pause of the first drive shaft 24, the second drive shaft 28, and the third drive shaft 29 can be independently controlled by an external control system.

[0057] The first drive shaft 24 is fixedly connected to the model clamping device 21, for example, by means of a slot and bolts, or by welding. The first drive shaft 24 is used to adjust the rotation angle of the rigid linkage formed by the fiber-coupled laser light source 20 and the model clamping device 21, allowing it to rotate within a range of 0 to 90 degrees. The second drive shaft 28 is fixedly connected to the first prism 26 for adjusting the rotation angle of the first prism 26, and the third drive shaft 29 is fixedly connected to the second prism 27 for adjusting the rotation angle of the second prism 27. The fixed connection between the second drive shaft 28 and the first prism 26, and between the third drive shaft 29 and the second prism 27, can be a combination of a slot, a fastening bolt, and a flexible gasket.

[0058] The laser beam emitted by the fiber-coupled laser source 20 is perpendicularly incident on the model to be observed, which is placed in the model holding device 21. The laser beam then passes through the model to the multi-prism reflection system. The first prism 26 and the second prism 27 are used for angle adjustment and beam splitting correction to form an orthogonal collimated optical path. The light then passes through the visualization window 13 and enters the microscope 23, where it is synchronously captured with a high-speed camera for dynamic phase state images. "Orthogonalization" here means that the optical path is orthogonal to the visualization window 13, that is, the light path after reflection by the multi-prism reflection system enters the visualization window 13 perpendicularly. This operation ensures image quality.

[0059] In this embodiment, the center of the bottom surface of the kettle is taken as the origin ( O )Establish xyz Cylindrical coordinate system, the coordinates of any point M in the reaction chamber 1 are ( r , θ , z ),in: r is the radial distance, θ is the azimuth, z The first prism 26 has a size of 60 mm × 30 mm × 2 mm and is made of quartz. The coordinates of its rotation axis are ( r =42 mm, θ =180°, z =38 mm). The second prism 27 has a size of 40 mm × 30 mm × 2 mm and is made of quartz. The coordinates of its rotation axis are ( r =5 mm, θ =0°, z =92 mm). Figure 3 As shown, in the initial state, the normal direction of the working surface of the first prism 26 and the second prism 27 is parallel to the axis direction of the kettle body.

[0060] Example 2

[0061] This example uses the in-situ high-temperature and high-pressure visual reactor apparatus of Example 1 to study the process of gas phase H2 displacing liquid phase water under different gravity inclination conditions.

[0062] In this embodiment, the model to be observed (microfluidic chip) is fixed on the model clamping device 21 by means of spring fastening. A cylindrical coordinate system is established with the center of the bottom circle of the kettle as the origin. The normal direction of the working surface of the model to be observed is parallel to the axis direction of the kettle. The size of the model to be observed is determined to be 20 mm × 10 mm × 2 mm, and the coordinates of the center of its rotation axis are ( r =38 mm, θ =180°, z =60 mm), a microfluidic channel (width 25 μm, depth 10 μm) is machined in the model to be observed, and a fluid injection port and an outflow port are provided at both ends of the microfluidic channel, both with an inner diameter of 20 μm, and are respectively connected to the inlet conduit 11 and the outlet conduit 12 through stainless steel pipelines. The chip is rigidly connected to the fiber-coupled laser light source 20 through a stainless steel flange (outer diameter 20 mm, thickness 5 mm), and the axis of the flange is aligned with the center of the etched area to ensure that the outgoing light beam of the light source is vertically incident on the surface of the model to be observed.

[0063] The two-phase flow involved in this embodiment uses H2-water displacement as an example, with water as the liquid phase and H2 as the gas phase. Before the experiment, the experimental temperature in reaction chamber 1 was maintained at a constant 100±0.5°C using a temperature-pressure coordinated control system. A high-precision syringe pump (not shown) was connected to inlet conduit 11 to enable fluid injection. Inlet conduit 11 was connected to the microfluidic channel injection port via a stainless steel pipeline. Simulated water was first injected into the model to be observed through inlet conduit 11 at an injection pressure of 25 MPa until the model to be observed and its pores were completely filled with water. H2, the displacement phase, was then injected into the water-filled model to study the displacement dynamics of H2 relative to water.

[0064] The specific steps for tilt adjustment are as follows:

[0065] (1) The first driving shaft 24 is used to drive the model to be observed and the fiber-coupled laser light source 20 to rotate counterclockwise from the horizontal position by 0° / 30° / 60° / 90° respectively. After adjustment, the model to be observed is locked to prevent displacement.

[0066] (2) In order to correct the optical path deviation caused by the chip tilt, the polygonal mirror reflection system is adjusted as follows: two independent knobs 22 are used to control the second drive shaft 28 to rotate the first prism 26, and the third drive shaft 29 is controlled to drive the second prism 27 to rotate (resolution ≤ 0.5°) to achieve dynamic optical path alignment. After adjustment, the first prism 26 and the second prism 27 are locked to prevent displacement. After adjustment, the optical path penetrates the visualization window 13 and enters the microscope 23 vertically. At the same time, the high-speed camera (frame rate 1000 fps) is controlled by IS Elements software to synchronously shoot the two-phase flow process in the microfluidic channel, and the bubble size distribution and flow velocity field in the image are analyzed in combination with ImageJ software. Among them, the specific rotation angle parameters are shown in Table 1, and the rotation schematic diagram is shown in Figure 4 、 Figure 5 、 Figure 6 and Figure 7 As shown, the first prism 26 is marked as A and the second prism 27 is marked as B.

[0067] Table 1 Rotation angle parameters of the observed model, the first prism 26 and the second prism 27

[0068]

[0069] Note: In Table 1, the rotation angles of the first prism 26 and the second prism 27 are positive when the drive axis rotates counterclockwise around the horizontal position, negative when it rotates clockwise, and the horizontal direction is 0°; the angle descriptions in Table 1 are all the same as x The angle in the positive direction of the axis.

[0070] The foregoing description is merely a preferred embodiment of the present invention and is not intended to limit the present invention. Those skilled in the art will readily appreciate that various modifications and variations of the present invention are possible. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of the present invention are intended to be within the scope of protection of the present invention.

Claims

1. An in-situ high-temperature and high-pressure visual reactor that can take into account the effect of gravity, characterized in that: Including reactor body and optical path observation system; The optical path observation system includes a fiber-coupled laser light source, a model clamping device, a multi-prism reflection system, a rotation angle adjustment device and an optical image acquisition system; the model clamping device is used to clamp the model to be observed; The reactor body includes a reaction chamber and a visualization window, and the reaction chamber is provided with a fiber-coupled laser light source, a model clamping device and a multi-prism reflection system; The visualization window is provided at the bottom of the reaction chamber; the model clamping device is provided near the top of the reaction chamber; the center point of the projection of the model clamping device on the bottom of the reaction chamber, the center point of the visualization window, and the center point of the bottom of the reaction chamber are located in the same straight line, and the center point of the projection of the model clamping device on the bottom of the reaction chamber and the center point of the visualization window are located on both sides of the center point of the bottom of the reaction chamber; The fiber-coupled laser light source is rigidly connected to the model clamping device to form a linkage body, and the rotation angle adjustment device can achieve 0-90° inclination adjustment to simulate different gravity inclination conditions; The laser beam emitted by the fiber-coupled laser light source is vertically incident on the model to be observed placed on the model clamping device, and the laser beam passes through the model to be observed to the multi-prism reflection system. After the multi-prism reflection system performs spectroscopic correction, an orthogonal collimated light path perpendicular to the visualization window is formed. The orthogonal collimated light path passes through the visualization window and enters the optical image acquisition system to realize image observation.

2. The in-situ high-temperature and high-pressure visual reactor capable of taking gravity into account according to claim 1, characterized in that: The reactor body further comprises a reactor cover, and the reaction chamber and the reactor cover form a rigid locking sealing structure through a split clamp body, a first sealing ring and circumferentially distributed connecting screws.

3. The in-situ high-temperature and high-pressure visual reactor capable of taking gravity into account according to claim 2, characterized in that: The split hoop body is composed of two independent semi-annular components, and the inner curved surface thereof is precisely machined to form a clearance fit structure with the reactor body.

4. The in-situ high-temperature and high-pressure visual reactor capable of taking gravity into account according to claim 1, characterized in that: The rotation angle adjustment device includes a drive shaft, a knob, and a second sealing ring. The knob is located outside the reaction chamber and is used to adjust the rotation angle of the drive shaft. The drive shaft is fixedly connected to the model clamping device and the polygonal mirror reflection system. The drive shaft passes through a preset hole on the side wall of the reaction chamber and is connected to the knob. A second sealing ring is provided at the contact portion between the drive shaft and the reaction chamber.

5. The in-situ high-temperature and high-pressure visual reactor capable of taking gravity into account according to claim 1, characterized in that: The multi-prism reflection system includes a first prism and a second prism. The first prism is located below the model clamping device and is arranged near the bottom of the reaction chamber; the second prism is located above the visualization window and is arranged near the top of the reaction chamber; the first prism and the second prism are arranged opposite to each other; the angles of the first prism and the second prism are adjustable, and are used to perform spectroscopic correction on the laser beam of the fiber-coupled laser light source through the observation model to form an orthogonal collimated light path, and then penetrate the visualization window into the optical image acquisition system.

6. The in-situ high-temperature and high-pressure visual reactor capable of taking gravity into account according to claim 1, characterized in that: The optical image acquisition system is arranged outside the reactor body, and includes a microscope and a high-speed camera, wherein the microscope faces the visualization window.

7. The in-situ high-temperature and high-pressure visual reactor capable of taking gravity into account according to claim 1, characterized in that: The in-situ high-temperature and high-pressure visual reactor further includes a temperature-pressure coordinated control system, which includes a temperature control box and a heating jacket.

8. The in-situ high-temperature and high-pressure visual reactor capable of taking gravity into account according to claim 7, characterized in that: The heating jacket is linked to the temperature control box for control; the heating jacket is wrapped around the outer wall of the reaction chamber, and a serpentine winding layout is used to achieve uniform heat field distribution; the temperature control box has a built-in PID adjustment module, which uses a K-type thermocouple embedded in the reaction chamber wall to provide real-time feedback of the temperature signal and dynamically adjust the power output of the heating jacket.

9. The use of the in-situ high-temperature and high-pressure visual reactor capable of taking gravity into account according to any one of claims 1 to 8, characterized in that: The application is in the study of multiphase displacement mechanism; The specific application method is as follows: the model to be observed is clamped and fixed by a model clamping device and placed inside the reaction chamber; the fiber-coupled laser light source and the model clamping device are controlled to rotate within an angle range of 0 to 90 degrees by a rotation angle adjustment device to realize the simulation of the model to be observed under different gravitational inclination angles; the laser beam of the fiber-coupled laser light source is vertically incident on the model to be observed, and the laser beam passes through the model to be observed to the multi-prism reflection system, and is split and corrected by the multi-prism reflection system to form an orthogonal collimated light path perpendicular to the visualization window. The orthogonal collimated light path penetrates the visualization window and enters the optical image acquisition system to realize image observation.

Images