In-situ high-temperature and high-pressure visible reaction kettle capable of considering gravity action and application thereof

Abstract

The invention discloses an in-situ high-temperature and high-pressure visible reaction kettle capable of considering the action of gravity and application of the in-situ high-temperature and high-pressure visible reaction kettle, and belongs to the technical field of multiphase fluid mechanics experimental equipment. According to the in-situ high-temperature and high-pressure visible reaction kettle provided by the invention, in-situ simulation of a gravity vector under a non-rotation condition is realized by utilizing linkage and inclination angle adjustment (0-90 degrees) of the optical fiber coupling laser light source and the model clamping device; the polygon prism reflection system corrects light path offset in real time to form an orthogonalization collimation light path, and the observation view field stability and the data accuracy in the processes of oil-water separation, CO2 diffusion and the like in the high-temperature and high-pressure environment are ensured. Besides, through a split type hoop body and a rigid locking sealing structure, the alternating stress effect of rotating torque on a sealing interface is eliminated, the high-pressure dynamic sealing failure risk is remarkably reduced, meanwhile, the device size is simplified, interference of peripheral equipment is avoided, and the experiment safety and the space adaptability are improved.

Description

Technical Field

[0001] The 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 consideration and application thereof. Background Art

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

[0003] High-temperature and high-pressure reactors accurately simulate deep-layer high-temperature and high-pressure geological conditions to achieve in-situ environmental reproduction of multiphase fluid seepage, mineral phase change and other processes. They have now become the core equipment for the study of multiphase fluid displacement dynamics in micro-nanoscale pore throats in deep-earth engineering projects such as oil and gas development and underground energy storage. However, when using this equipment to observe dynamic behaviors such as phase separation, sedimentation, and floating dominated by gravity during the migration of fluids in deep-earth engineering projects, the spatial angle between the observation axis and the gravity vector directly affects the accuracy of the experimental data.

[0004] The existing technology generally adopts an integrated design in which the reactor body, optical imaging system and light source module rotate synchronously. Although the spatial angle between the observation axis and the gravity vector can be adjusted, there are significant technical bottlenecks. On the one hand, the scheme needs to be equipped with a high-rigidity rotating base to resist the torque generated by large-angle rotation, and reserve redundant space to avoid interference from peripheral equipment, resulting in a large device size and redundant structure, which is difficult to adapt to complex experimental environments; on the other hand, during the dynamic rotation process, the sealing interface between the high-pressure reaction chamber and the external pipeline is subjected to alternating stress and friction wear for a long time. The sealing material is prone to plastic deformation or fatigue cracking under high-temperature and high-pressure coupling conditions, causing the risk of medium leakage, which seriously restricts the long-term operation stability and experimental safety of the equipment. In addition, the mechanical vibration caused by the overall rotation is easy to interfere with the precision optical observation system, causing image blur or data distortion, further reducing the accuracy of the gravity field simulation experiment. Therefore, how to achieve multi-angle gravity field dynamic simulation under non-rotating conditions, while ensuring high-temperature and high-pressure sealing performance and observation accuracy, has become a technical problem that needs to be broken through in the fields of deep oil and gas resource development and carbon storage 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 has 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 consider the effect of gravity, comprising a reactor body and an optical path observation system; The optical path observation system includes a fiber-optic 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 for clamping the model to be observed; The reactor body includes a reaction chamber and a visualization window, and the fiber-optic coupled laser light source, the model clamping device, and the multi-prism reflection system are arranged in the reaction chamber; The fiber-optic coupled laser light source is rigidly connected to the model clamping device to form a linkage body, and realizes an inclination angle adjustment of 0 to 90° through the rotation angle adjustment device, for simulating different gravity inclination situations; the laser beam emitted by the fiber-optic coupled laser light source is vertically incident on the model to be observed placed by the model clamping device, and the laser beam passes through the model to be observed to the multi-prism reflection system, and after being spectroscopically corrected by the multi-prism reflection system, an orthogonally collimated optical path perpendicular to the visualization window is formed, and the orthogonally collimated optical path passes through the visualization window and enters the optical image acquisition system to realize image observation.

[0007] 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 and sealing structure through a split-type hoop body, a first sealing ring, and circumferentially uniformly distributed connecting screws.

[0008] In some embodiments of the present invention, the split-type hoop body is composed of two independent semi-circular members, and the material is 1Cr18Ni9Ti austenitic stainless steel, and its inner curved surface is precisely processed to form a clearance fit structure with the reactor body.

[0009] In some embodiments of the present invention, a confining pressure conveying pipeline, a fiber-optic inlet, a pressure gauge, and a thermometer are provided on the reactor body; a confining pressure ring cavity is formed inside the reaction chamber, and the confining pressure ring cavity is communicated with the confining pressure conveying pipeline.

[0010] In some embodiments of the present invention, an explosion-proof valve and a spirit level tube are further provided on the reactor body, the explosion-proof valve is used for safe pressure relief, and the spirit level tube is used for leveling control of the reactor body.

[0011] 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 for adjusting the rotation angle of the drive shaft; the drive shaft is fixedly connected to the model clamping device and the multi-prism 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 arranged at the contact part of the drive shaft and the reaction chamber.

[0012] In some embodiments of the present invention, the fiber-coupled laser light source is communicated with the fiber inlet through a fiber optic.

[0013] In some embodiments of the present invention, the light transmittance of the visualization window is above 95%; the visualization window is connected to the reaction chamber through a sealing assembly. Further, the visualization window is made of sapphire glass; the sealing assembly is a combination of metal and fluororubber. Further, a gold plating coating is provided on the surface of the visualization window as a conductive layer, and the thickness of the gold plating coating is 40 - 60 nm to prevent electrostatic adsorption of particulate contamination.

[0014] In some embodiments of the present invention, the visualization window is disposed at the bottom of the reaction chamber; the model clamping device is disposed 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 on 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 on both sides of the center point of the bottom of the reaction chamber.

[0015] 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 near the bottom of the reaction chamber; the second prism is located above the visualization window and near the top of the reaction chamber; the first prism and the second prism are oppositely arranged; the angles of the first prism and the second prism are adjustable for splitting and correcting the laser beam transmitted through the observation model by the fiber-coupled laser light source to form an orthogonally collimated light path, and then penetrating through the visualization window into the optical image acquisition system.

[0016] In some embodiments of the present invention, the optical image acquisition system is disposed outside the reaction kettle body. The optical image acquisition system includes a microscope and a high-speed camera, and the microscope is directly opposite to the visualization window. The microscope is used to magnify the pore-throat structure and the microscopic distribution pattern of multiphase fluids (such as oil, water, CO2, etc.) in the observation model (such as core, micro-nano chip); the high-speed camera is used to record transient behaviors such as gravity-dominated phase separation, sedimentation, and floating at a high frame rate to obtain dynamic data with millisecond-level time resolution.

[0017] In some embodiments of the present invention, the in-situ high-temperature and high-pressure visible reaction kettle further includes a temperature and pressure coordinated control system, and the temperature and pressure coordinated control system includes a temperature control box and a heating jacket wrapped around the outer wall of the reaction chamber.

[0018] In some embodiments of the present invention, the heating jacket is in linkage control with the temperature control box; the heating jacket is wrapped around the outer wall of the reaction chamber, and the heat field is evenly distributed through a serpentine winding layout, with a temperature gradient < 2 °C; the temperature control box is internally provided with a PID adjustment module, and the temperature signal is real-time fed back through a K-type thermocouple embedded in the reaction chamber wall, and the power output of the heating jacket is dynamically adjusted. Further, the material of the heating jacket is a silica-aluminum fiber matrix and a nickel-chromium alloy heating wire.

[0019] In some embodiments of the present invention, a pressure sensor is configured inside the reaction kettle body to monitor the pressure inside the kettle in real time for overpressure buzzer alarm.

[0020] In some embodiments of the present invention, the reaction chamber adopts an integral seamless structure, and the material is selected as 1Cr18Ni9Ti stainless steel, which is pressure-resistant and corrosion-resistant; the material of the sealing ring is fluororubber; the reaction kettle body is in a cylindrical shape.

[0021] In a second aspect, the present invention provides an application of the above-mentioned in-situ high-temperature and high-pressure visible reaction kettle that can consider the gravity effect, and the application is in the research of multiphase displacement mechanism; The specific application method is as follows: the model to be observed is clamped and fixed through 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° through a rotation angle adjustment device to simulate the model to be observed under different gravity inclinations; 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 prism reflection system, and is spectroscopically corrected by the prism reflection system to form an orthogonally collimated light path perpendicular to the visualization window, and the orthogonally collimated light path penetrates the visualization window and enters the optical image acquisition system to realize image observation.

[0022] Specific application scenarios include oil and gas reservoir seepage, CO2 sequestration, underground hydrogen storage, etc.

[0023] Compared with the prior art, the present invention has achieved the following beneficial effects: (1) The present invention realizes the in-situ simulation of the gravity vector under non-rotating conditions by using the linkage and inclination angle adjustment (0 to 90°) of the fiber-coupled laser light source and the model clamping device; the prism reflection system real-time corrects the optical path deviation to form an orthogonally collimated light 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.

[0024] (2) The present invention collaborates with a visualization window, a microscope, and a high-speed camera to support multi-modal dynamic observations such as fluorescence labeling, particle tracking, and interference imaging; integrates a temperature-pressure collaborative control system to accurately simulate the deep-earth environment, and is compatible with the experimental requirements of micro-nano chips and real rock cores, providing a full-scale experimental platform for the study of high-temperature and high-pressure displacement dynamics.

[0025] (3) The present invention breaks through the traditional overall rotation design. Through a split-type hoop body and a rigid locking and sealing structure, it eliminates the alternating stress effect of the rotation torque on the sealing interface, significantly reduces the risk of high-pressure dynamic seal failure, simplifies the device volume, avoids interference from peripheral equipment, and improves the experimental safety and space adaptability. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] The accompanying drawings forming a part of this specification are used to provide a further understanding of the present invention. The schematic embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation of the present invention. Obviously, for those of ordinary skill in the art, other drawings can be obtained based on these drawings without creative efforts.

[0027] Figure 1 is a schematic diagram of the overall structure of the in-situ high-temperature and high-pressure visible reaction kettle device according to Embodiment 1 of the present invention; Figure 2 is a schematic cross-sectional view of the reaction chamber of the in-situ high-temperature and high-pressure visible reaction kettle device according to Embodiment 1 of the present invention; Figure 3 is a schematic top view of the reaction chamber of the in-situ high-temperature and high-pressure visible reaction kettle device according to Embodiment 1 of the present invention; Figure 4 is a partial schematic diagram of the in-situ high-temperature and high-pressure visible reaction kettle device according to Embodiment 1 of the present invention; Figure 5 is a schematic diagram of the optical path propagation when the model to be observed in Embodiment 2 of the present invention is placed horizontally; Figure 6 is a schematic diagram of the optical path propagation when the model to be observed in Embodiment 2 of the present invention is rotated counterclockwise by 30°; Figure 7 is a schematic diagram of the optical path propagation when the model to be observed in Embodiment 2 of the present invention is rotated counterclockwise by 60°; Figure 8 is a schematic diagram of the optical path propagation when the model to be observed in Embodiment 2 of the present invention is rotated counterclockwise by 90°; In the figure, 1 is a reaction chamber; 2 is a reaction kettle cover; 3 is a split hoop body; 4 is a connecting screw; 5 is a first sealing ring; 6 is an explosion-proof valve; 7 is an inlet of the confining pressure conveying pipeline; 8 is a spirit level tube; 9 is a thermometer; 10 is a pressure gauge; 11 is an inlet conduit; 12 is an outlet conduit; 13 is a visualization window; 14 is a sealing assembly; 15 is a confining pressure conveying pipeline; 16 is a confining pressure ring cavity; 17 is a heating jacket; 18 is a temperature control box; 19 is an optical fiber; 20 is an optical fiber coupled laser light source; 21 is a model clamping device; 22 is a knob; 23 is a microscope; 24 is a first driving shaft; 25 is an optical fiber inlet; 26 is a first prism; 27 is a second prism; 28 is a second driving shaft; 29 is a third driving shaft; 30 is a second sealing ring. Detailed implementation manners

[0028] It should be noted that the specific implementation manners of the present invention described herein are only for the purpose of explaining the present invention and cannot be understood in any way as a limitation to the present invention. Under the teaching of the present invention, those skilled in the art can conceive any possible deformations based on the present invention, and these should all be regarded as belonging to the scope of the present invention. It should be noted that when an element is referred to as being "disposed on" another element, it can be directly on the other element or there may also be an intermediate element. When an element is considered to be "connected" to another element, it can be directly connected to the other element or there may be an intermediate element at the same time. Unless otherwise clearly defined and limited, the terms "disposed", "installed", "connected", and "coupled" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium, and it can be the communication inside two elements. For those of ordinary skill in the art, the specific meanings of the above terms can be understood according to specific situations. The terms "vertical", "horizontal", "upper", "lower", "left", "right" and similar expressions used herein are only for the purpose of illustration and do not represent the only implementation manner. The terms "first", "second", and "third" are only used for descriptive purposes and cannot be understood as indicating or implying relative importance.

[0029] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those of ordinary skill in the technical field to which the present invention belongs. The terms used in the description of the present invention herein are only for the purpose of describing specific implementation manners and are not intended to limit the present invention. The term "and / or" used herein includes any and all combinations of one or more of the related listed items.

[0030] The technical solution of the present invention will be further described below in conjunction with specific embodiments.

[0031] Embodiment 1 This embodiment provides an in-situ high-temperature and high-pressure visible reaction kettle device that can consider the action of gravity, as Figure 1 and Figure 2 shown. It includes a reaction kettle body, a temperature and pressure coordinated control system, and an optical path observation system.

[0032] The reaction kettle body is cylindrical in shape and is composed of a reaction chamber 1, a reaction kettle cover 2, a split hoop body 3, connecting screws 4, and a first sealing ring 5. An explosion-proof valve 6, a confining pressure conveying pipeline inlet 7, a spirit level tube 8, a thermometer 9, a pressure gauge 10, and an optical fiber inlet 25 are provided on the reaction kettle body. The reaction chamber 1 adopts an integral seamless structure, is cylindrical in shape, has a diameter of 14.5 cm, and a height of 10.5 cm. The material is selected as 1Cr18Ni9Ti stainless steel, which is pressure-resistant and corrosion-resistant. The reaction chamber 1 and the reaction kettle cover 2 are hermetically connected through the split hoop body 3, connecting screws 4, and the first sealing ring 5 to ensure the tightness of the device. The split hoop body 3 is composed of two independent semi-circular members, and the material is selected as 1Cr18Ni9Ti austenitic stainless steel. Its inner curved surface is precision machined to form a clearance fit structure with the reaction kettle body. The split hoop body 3 aligns the flange of the reaction kettle cover 2 with the reaction chamber 1 (not shown in the figure), evenly screws in the connecting screws 4 along the circumferential direction, and applies a pre-tightening torque of 120 N·m to ensure uniform distribution of the flange surface compressive stress. The first sealing ring 5 is made of fluororubber material and is embedded in the flange sealing groove of the reaction chamber 1. It generates an axial compression deformation with a compression rate of 15-20% under the action of the screw pre-tightening force to establish an airtight barrier, and the pressure resistance level is ≥35 MPa.

[0033] The spirit level tube 8 on the upper part of the reaction kettle cover 2 is used to level the reaction kettle body; the thermometer 9 and the pressure gauge 10 transmit the temperature information and pressure information inside the reaction kettle body to the outside; the explosion-proof valve 6 is located on the pressure gauge 10 and is used for safe pressure relief.

[0034] A visual window 13 for easy observation is provided at the bottom of the reaction chamber 1. The visual window 13 is made of sapphire glass, which has a high light transmittance of more than 95% and meets the requirements of high-definition in-situ observation. It is also high-temperature and high-pressure resistant and meets the requirements of a design temperature of 100 °C and a design pressure of 35 MPa. The visual window 13 is connected to the reaction chamber 1 through a sealing component 14. The sealing component 14 is obtained by combining metal and fluororubber. The visual window 13 is installed at the lower part of the reaction chamber 1. At the same time, a gold-plated coating is provided on the inner surface of the visual window 13 close to the reaction chamber 1 as a conductive layer to avoid electrostatic adsorption of particles, and the thickness of the gold-plated coating is 50 nm.

[0035] The inlet duct 11 and the outlet duct 12 are provided on the left and right sides of the reactor body; the inlet duct 11 and the outlet duct 12 are reserved for the injection or discharge of the model fluid to be observed. The inlet duct 11 and the outlet duct 12 are made of 1Cr18Ni9Ti austenitic stainless steel, which can withstand high temperature and high pressure. In addition, the semi-annular split clamp body 3 is respectively provided with coaxial threaded holes with a hole diameter of Φ2.5±0.02mm, which are used to adapt to the flange connection of the inlet duct 11 and the outlet duct 12.

[0036] A confining pressure ring cavity 16 is formed inside the reaction chamber 1, which is connected to the confining pressure delivery pipeline 15, and the confining pressure delivery pipeline 15 is connected to the confining pressure delivery pipeline inlet 7. At the same time, a pressure sensor (not shown in the figure) is configured inside the reactor body to monitor the pressure inside the reactor in real time to issue an overpressure buzzer alarm.

[0037] 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 a pressure of 35 MPa, and the pressure is maintained for 24 hours. The leakage rate detector shows that the leakage amount is less than 1×10 -6 Pa·m 3 / s, meeting ASME B16.20 standard.

[0038] The temperature-pressure coordinated control system includes a heating sleeve 17 and a temperature control box 18; the heating sleeve 17 and the temperature control box 18 are linked to achieve the purpose of adjusting the experimental temperature in the reaction chamber 1. The heating sleeve 17 is coated on the outer wall of the reaction chamber 1, and a uniform distribution of the thermal field is achieved through a serpentine winding layout, and the temperature gradient is <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 to feed back the temperature signal in real time, dynamically adjust the power output of the heating sleeve 17, and adjust the response time to ≤1s. The winding layout of the heating sleeve 17 cooperates with the PID algorithm to achieve a medium temperature fluctuation of <1.5°C in the reaction chamber 1, so as to achieve thermal control accuracy. The material of the heating sleeve 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.

[0039] like Figure 2 and Figure 3 As shown, the optical path observation system consists of a fiber-coupled laser light source 20, a model clamping device 21, a rotation angle adjustment device, a multi-prism reflection system, a microscope 23, and a high-speed camera (not shown in the figure). The microscope 23 faces the visualization window 13. The microscope 23 adopts a Nikon inverted microscope, equipped with a long working distance objective lens, whose numerical aperture (NA) is 0.45 and the working distance is 25 mm. Its objective lens faces the visualization window 13. After the optical path is corrected by the multi-prism reflection system, it penetrates the visualization window 13 and enters the objective lens of the microscope 23. The real-time image capture and analysis are controlled by IS Elements software.

[0040] The model clamping device 21 is used to fix the model to be observed. In this embodiment, its clamping method is spring pre-tightening type. Those skilled in the art can also select other clamping methods according to needs. The model clamping device 21 is arranged near the top of the reaction chamber 1; the center point of the projection of the model clamping device 21 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, and the center point of the projection of the model clamping device 21 on the bottom of the reaction chamber 1 and the center point of the visualization window 13 are located on both sides of the center point of the bottom of the reaction chamber 1.

[0041] The fiber-coupled laser light source 20 is rigidly connected to the model clamping device 21 through a flange to form a linkage body, and their axes always remain parallel. The fiber-coupled laser light source 20 is connected to the fiber inlet 25 through the optical fiber 19. The fiber inlet 25 is the channel for the optical fiber 19 to enter the reaction kettle. The optical fiber 19 is the "transmission medium", and the fiber-coupled laser light source 20 is the "generator" of the optical signal.

[0042] The multi-prism reflection system includes a first prism 26 and a second prism 27. The first prism 26 is located below the model clamping device 21, and the second prism 27 is located above the visualization window 13. As Figure 2 、 Figure 3 and Figure 4 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 its surface is provided with angle scale lines. A total of three knobs 22 are provided to independently drive the first drive shaft 24, the second drive shaft 28, and the third drive shaft 29 to rotate and adjust the rotation angle. A locking device can be further provided on the knob 22. After the knob 22 rotates to the target angle, the first drive shaft 24, the second drive shaft 28, and the third drive shaft 29 are circumferentially fixed through mechanical interference or frictional restraint. The first drive shaft 24, the second drive shaft 28, and the third drive shaft 29 pass through the preset holes on the side wall of the reaction chamber 1 and are connected to the knob 22. The contact parts of the first drive shaft 24, the second drive shaft 28, and the third drive shaft 29 with the reaction chamber 1 are provided with a second sealing ring 30. The second sealing ring 30 is made of fluororubber material, and it is in interference fit with the first drive shaft 24, the second drive shaft 28, and the third drive shaft 29 to ensure good sealing of the reaction kettle. At the same time, it can also play a role in preventing angle deviation to a certain extent. 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 through an external control system.

[0043] The first drive shaft 24 is fixedly connected to the model clamping device 21. For example, it can be fixedly connected through a card slot and bolts, or it can be welded or other methods. The first drive shaft 24 is used to adjust the rotation angle of the rigid linkage body composed of the fiber-coupled laser light source 20 and the model clamping device 21, so that it rotates within the range of 0 to 90°. The second drive shaft 28 is fixedly connected to the first prism 26 and is used to adjust the rotation angle of the first prism 26. The third drive shaft 29 is fixedly connected to the second prism 27 and is used to adjust the rotation angle of the second prism 27. The fixed connection between the second drive shaft 28 and the first prism 26 and the fixed connection between the third drive shaft 29 and the second prism 27 can adopt a combination of a card slot, a fastening bolt and a flexible gasket.

[0044] The laser beam emitted by the fiber-coupled laser light source 20 is vertically incident on the model to be observed placed by the model clamping device 21. The laser beam passes through the model to be observed and reaches the multi-prism reflection system. The first prism 26 and the second prism 27 form an orthogonally collimated optical path through angle adjustment and spectroscopic correction, penetrate the visualization window 13 and enter the microscope 23, and cooperate with the high-speed camera to synchronously capture dynamic phase images. The "orthogonalization" here means that the optical path is orthogonal to the visualization window 13, that is, the optical path reflected by the multi-prism reflection system is vertically incident on the visualization window 13. This operation can ensure the imaging quality.

[0045] In this embodiment, taking the center of the bottom surface of the kettle body as the origin ( O ) to establish xyz a cylindrical coordinate system. The coordinates of any point M in the reaction chamber 1 are ( r , θ , z ), where: r is the radial distance, θ is the azimuth angle, z is the distance from the bottom surface of the kettle body. The size of the first prism 26 is 60 mm × 30 mm × 2 mm, and it is made of quartz. The center coordinates of its rotation axis are ( r = 42 mm, θ = 180°, z = 38 mm). The size of the second prism 27 is 40 mm × 30 mm × 2 mm, and it is made of quartz. The center coordinates of its rotation axis are ( r = 5 mm, θ = 0°, z = 92 mm). As Figure 3 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.

[0046] Embodiment 2 This embodiment uses the in-situ high-temperature and high-pressure visual reactor device of Embodiment 1 to study the process of gas-phase H2 displacing liquid-phase water under different gravity inclination conditions.

[0047] 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 surface of the kettle body 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 body. The size of the model to be observed is determined to be 20 mm × 10 mm × 2 mm, and the center coordinates 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. Fluid injection ports and outlets are provided at both ends of the microfluidic channel, with an inner diameter of 20 μm each, 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-optic coupled laser light source 20 through a stainless steel flange (outer diameter 20 mm, thickness 5 mm). The axis of the flange is aligned with the center of the etched area to ensure that the light beam emitted by the light source is perpendicularly incident on the surface of the model to be observed.

[0048] Taking the H2 displacement of water as an example for the two-phase flow involved in this embodiment, where water is the liquid phase and H2 is the gas phase. Before the experiment, the experimental temperature in the reaction chamber 1 is kept constant at 100 ± 0.5 °C through the temperature and pressure coordinated control system. A high-precision injection pump (not shown in the figure) is connected to the inlet conduit 11 to achieve fluid injection. The inlet conduit 11 is connected to the injection port of the microfluidic channel through a stainless steel pipeline. First, simulated water is injected into the model to be observed through the inlet conduit 11 at an injection pressure of 25 MPa until the model to be observed and its pores are filled with water; then, the displacement phase H2 is injected into the water-filled model to be observed to study the displacement dynamics of H2 relative to water.

[0049] The specific steps for inclination adjustment are as follows: (1) Use the first drive shaft 24 to drive the model to be observed and the fiber-optic coupled laser light source 20 to rotate counterclockwise from the horizontal position by 0° / 30° / 60° / 90° respectively, and lock the model to be observed after adjustment to prevent displacement.

[0050] (2) To correct the optical path offset caused by the chip tilt, the following adjustments are made to the multi-prism reflection system: Two independent knobs 22 are used to control the rotation of the first prism 26 by the second drive shaft 28 and the rotation of the second prism 27 driven by the third drive shaft 29 (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 vertically enters the microscope 23. At the same time, the high-speed camera (frame rate 1000 fps) is controlled by the IS Elements software to synchronously capture the two-phase flow process in the microfluidic channel, and the ImageJ software is used to analyze the bubble size distribution and velocity field in the image. Among them, the specific rotation angle parameters are shown in Table 1, and the rotation schematic diagrams are as shown in Figure 4 , Figure 5 , Figure 6 and Figure 7 . The first prism 26 is denoted as A, and the second prism 27 is denoted as B.

[0051] Table 1 Rotation angle parameters of the model to be observed, the first prism 26 and the second prism 27

[0052] Note: In Table 1, the rotation angles of the first prism 26 and the second prism 27 are positive when the drive shaft rotates counterclockwise around the horizontal position and negative when it rotates clockwise, with the horizontal direction being 0°. The angle descriptions in Table 1 are all the included angles with the positive direction of the x axis.

[0053] The above are only the preferred embodiments of the present invention and are not used to limit the present invention. For those skilled in the art, the present invention can have various changes and modifications. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.

Claims

1. An in-situ high-temperature and high-pressure visible reaction kettle that can consider the action of gravity, characterized in that, It includes a reactor body and an 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 fiber-coupled laser light source, the model clamping device, and the multi-prism reflection system are arranged in the reaction chamber; The fiber-coupled laser light source is rigidly connected to the model clamping device to form a linkage body, and realizes an inclination angle adjustment of 0 to 90° through the rotation angle adjustment device, and is used to simulate different gravity inclination situations; The laser beam emitted by the fiber-coupled laser light source is vertically incident on the model to be observed placed by the model clamping device, and the laser beam passes through the model to be observed to the multi-prism reflection system. After being split and corrected by the multi-prism reflection system, an orthogonalized collimated optical path perpendicular to the visualization window is formed, and the orthogonalized collimated optical 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 visible reaction kettle capable of considering the gravity effect as described in claim 1, wherein The reactor body further includes a reactor cover, and the reaction chamber and the reactor cover form a rigid locking and sealing structure through a split clamp body, a first sealing ring, and circumferentially uniformly distributed connecting screws.

3. The in-situ high-temperature and high-pressure visible reaction kettle capable of considering the gravity effect as described in claim 2, wherein The split clamp body is composed of two independent semi-circular members, and its inner curved surface is precisely processed to form a clearance fit structure with the reactor body.

4. The in-situ high-temperature and high-pressure visual reactor capable of considering the gravity effect as claimed in claim 1, wherein 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 multi-prism 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 arranged at the contact part of the drive shaft and the reaction chamber.

5. The in-situ high-temperature and high-pressure visible reaction kettle capable of considering the action of gravity as claimed in claim 1, wherein, 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 on 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 on both sides of the center point of the bottom of the reaction chamber.

6. The in-situ high-temperature and high-pressure visible reaction kettle capable of considering the action of gravity as described in claim 5, 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 split and correct the laser beam transmitted through the observation model by the fiber-coupled laser light source to form an orthogonalized collimated optical path, and then penetrate the visualization window and enter the optical image acquisition system.

7. The in-situ high-temperature and high-pressure visible reaction kettle capable of considering the action of gravity according to claim 1, characterized in that, The optical image acquisition system is arranged outside the reactor body, and the optical image acquisition system includes a microscope and a high-speed camera, and the microscope is directly opposite to the visualization window.

8. The in-situ high-temperature and high-pressure visible reaction kettle capable of considering the action of gravity according to claim 1, characterized in that, The in-situ high-temperature and high-pressure visible reactor further includes a temperature and pressure coordinated control system, and the temperature and pressure coordinated control system includes a temperature control box and a heating jacket.

9. The in-situ high-temperature and high-pressure visible reaction kettle capable of considering the action of gravity according to claim 8, characterized in that The heating jacket is in linkage control with the temperature control box; the heating jacket is wrapped around the outer wall of the reaction chamber, and the heat field is evenly distributed through a serpentine winding layout; the temperature control box is internally provided with a PID adjustment module, and the temperature signal is real-time fed back through a K-type thermocouple embedded in the reaction chamber wall, and the power output of the heating jacket is dynamically adjusted.

10. Application of the in-situ high-temperature and high-pressure visible reaction kettle capable of considering the action of gravity according to any one of claims 1 to 9, characterized in that, The application is for the study of multiphase displacement mechanism; The specific application method is as follows: the model to be observed is clamped and fixed through 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° through a rotation angle adjustment device to simulate the model to be observed under different gravity 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 prism reflection system, and after being spectroscopically corrected by the prism reflection system, an orthogonally collimated light path perpendicular to the visualization window is formed, and the orthogonally collimated light path penetrates the visualization window and enters the optical image acquisition system to realize image observation.

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