High-temperature and high-pressure all-visible phase state and foam behavior characterization device and use method thereof

Abstract

The invention provides a high-temperature and high-pressure all-visible phase state and foam behavior characterization device. The device comprises a high-temperature-resistant and high-pressure-resistant visual observation cavity, an atomization spraying module, a volume adjusting module, a temperature control module, a pressure control module, a stirring and rotating module, a visual imaging module and a data acquisition and computer control module. The observation cavity is sealed through an upper flange and a lower flange to form a pressure-resistant visual cavity, and an upper visual window and a lower visual window are arranged to achieve double-view-angle imaging. The volume adjusting module is driven by a piston to change the effective volume in the cavity, and the temperature and the pressure are controlled in a closed-loop mode through a heating / circulating constant-temperature device and piston driving and / or a high-pressure pump. The method comprises the steps of device pretreatment, establishment of a high-pressure carbon dioxide environment and formula injection, volume / pressure scanning to obtain phase boundary parameters, stirring disturbance and visual recording, temperature switching repeated experiments, water adding disturbance and foam performance evaluation, and realization of phase-foam behavior coupling characterization.

Description

Technical Field

[0001] This invention relates to the field of oil and gas field development engineering, and in particular to a high-temperature and high-pressure fully visible phase and foam behavior characterization device. Background Technology

[0002] The phase changes, interfacial behavior, and foam formation-collapse mechanisms of high-temperature and high-pressure multiphase systems are of great significance in reservoir development, supercritical fluid utilization, chemical engineering, and energy geology. Especially in supercritical CO2 development, foam-driven oil recovery, gas-liquid two-phase mixing, and the study of fluid properties in deep oil and gas reservoirs, systems often experience significant temperature and pressure gradients within wellbores or pipelines. Their internal phase transitions, interfacial configuration evolution, and foam stability changes directly affect oil and gas recovery efficiency, lift process safety, and surface process stability. With the rapid development of technologies such as ultra-deep reservoir development, supercritical CO2 phase regulation, and foam-enhanced recovery, the dissolution, volatilization, miscibility, and precipitation of CO2 under high-temperature and high-pressure conditions, along with their accompanying transient microdynamic behaviors such as interfacial abrupt changes, bubble collapse, and droplet coalescence, have received widespread attention. Therefore, there is an urgent need to establish experimental devices capable of simulating complex temperature and pressure conditions and achieving visualized characterization to reveal the physical mechanisms of high-temperature and high-pressure multiphase systems and guide engineering optimization.

[0003] Currently, various experimental devices and schemes have been proposed for studying the phase behavior and foam stability of CO2-fluid systems. For example, Chinese patent CN105865963A discloses a supercritical carbon dioxide phase equilibrium instrument and its usage method, which realizes gas-liquid phase observation through a pressure-resistant window and temperature and pressure control. However, its visualization range is small and it is mainly used for static phase observation, making it difficult to capture high-speed dynamic processes. It also lacks a system linkage for rotation, atomization spraying, and image processing. Chinese patent CN103969407A discloses a device for evaluating the foaming performance of aerosol surfactants and its application, which can realize foam visualization. However, it achieves pressure reduction testing through an intermediate container and has insufficient capabilities in cloud point acquisition, atomization spraying, adjustable volume, and transient high-speed recording. Chinese patent CN117434209 discloses a dynamic visualization testing device for high-temperature and high-pressure foam performance, which can realize dynamic observation of foam to a certain extent. However, it usually focuses on continuous foaming and flow observation, and lacks the ability to perform phase scanning (such as obtaining turbidity point / clarity point), non-depressurized step formula switching, and continuous adjustment of effective volume through piston displacement within the same high-temperature and high-pressure visible chamber. Chinese patent CN112098602 discloses a high-temperature and high-pressure foam evaluation device and evaluation method, which can observe foam and measure foam half-life and liquid half-life under high-temperature and high-pressure conditions. However, its foaming method is mainly based on stirring or container inversion, which is difficult to simulate the transient foaming process induced by high-pressure jet / atomization mixing. At the same time, it lacks volume-pressure linkage control and quantitative closed-loop means based on adjustable volume.

[0004] Existing technologies still have the following shortcomings: the phase testing device and the foam evaluation device are functionally separate, making it difficult to achieve continuous coupled characterization of processes such as phase testing, mixing and foaming, foam generation / collapse, and liquid precipitation decay within the same chamber; existing devices are insufficient in simulating interface changes and foaming behavior induced by jet / spray mixing, and cannot cover the transient dynamic processes caused by jet atomization under high pressure conditions; existing devices often cannot be equipped with high-speed visualization systems, making it difficult to capture and quantitatively analyze rapid evolution behaviors such as droplet dispersion, critical phase transitions, and interface mutations; existing devices lack the ability to coordinate and link multiple modules such as stirring, atomizing spray, rotation, full visualization, temperature and pressure control, data acquisition, and image processing, and lack a mechanism for achieving volume-pressure linkage control and quantitative closed-loop through adjustable volume, making it difficult to meet the comprehensive characterization requirements of integrated "phase-foam" analysis, wide temperature and pressure range, and high time resolution. Therefore, there is an urgent need to develop a high-temperature and high-pressure multifunctional characterization device that covers a wide temperature and pressure range, has full visibility, can perform high-speed transient capture, has atomization injection and volume adjustment functions, and supports multi-system collaborative simulation, data acquisition and image processing integration, so as to meet the experimental needs of fields such as oil and gas development, supercritical fluid technology and foam drive mechanism research. Summary of the Invention

[0005] The purpose of this invention is to address the shortcomings existing in the field by proposing a high-temperature, high-pressure, fully visible phase and foam behavior characterization device.

[0006] To overcome the shortcomings of the prior art, the present invention adopts the following technical solution: A high-temperature and high-pressure fully visible phase and foam behavior characterization device includes: a cavity for high-temperature and high-pressure visual observation, an atomizing spray module, a volume adjustment module, a temperature control module, a pressure control module, a stirring and rotation module, a visualization imaging module, and a data acquisition and computer control module. The observation cavity is formed by a sealed connection between the upper and lower flanges to form a pressure-resistant visualization cavity, and an upper viewing window and a lower viewing window are respectively set at the top and bottom of the cavity to achieve dual-view imaging. The temperature control module includes a heating jacket and an external circulating constant temperature device; the pressure control module includes a pressure sensor, a piston drive device, and / or an external high-pressure pump. The volume adjustment module includes a volume adjustment piston, a guide and limiting structure, and a displacement sensor. The volume adjustment piston moves linearly along the axial direction under the drive of the piston driving device to change the effective volume inside the cavity. The atomizing spray module includes an atomizing nozzle and a replaceable atomizing connector; The visualization imaging module includes a camera and an adjustable camera bracket, which work together with a front light source group and a rear light source group to form an image; The data acquisition and computer control module is used to acquire temperature, pressure, displacement, rotation speed and image data, and to perform linkage control of temperature, pressure and volume or piston displacement.

[0007] Furthermore, the upper viewing window and the lower viewing window are respectively equipped with imaging devices or acquire image sequences from different perspectives. The data acquisition and computer control module performs geometric calibration and registration on the dual-view images at the same time, and performs three-dimensional characterization or three-dimensional reconstruction of the interface and / or foam structure based on the cavity geometry.

[0008] Furthermore, a limiting groove or limiting structure is provided on the inner wall of the observation chamber or at the part that cooperates with the piston and / or stirring assembly to limit the installation position and axial travel range of the stirring assembly, the spraying assembly or the guide limiting structure.

[0009] Furthermore, the data acquisition and computer control module includes a data acquisition unit and a control unit. The data acquisition unit includes a temperature acquisition channel, a pressure acquisition channel, and a displacement acquisition channel, which are used to acquire the cavity temperature, cavity pressure, and piston displacement, respectively. Among them, the piston displacement is used for subsequent calculation of the effective volume inside the cavity. The data acquisition unit also acquires the actual rotation speed of the stirring device and acquires real-time images or videos of the cavity obtained by the camera. The control unit uses computer control to set, switch, and control the temperature, pressure, volume, or piston displacement, and performs interlock monitoring of overpressure, overtemperature, and / or overtorque.

[0010] Furthermore, the control software calculates the displacement volume based on the piston displacement collected by the displacement sensor, and robustly fuses it with the volume calculated from the image to obtain an estimate of the effective cavity volume, which is used for volume-pressure linkage closed-loop control; the robust fusion satisfies the following relationship: ; in, For displacement volume With image volume The effective volume estimate of the cavity obtained through robust fusion; The displacement volume is obtained from the piston displacement. The image volume obtained from image processing. The fusion coefficient is... As a consistency threshold, This indicates that the volume difference value is truncated at upper and lower limits to suppress abnormal volume jumps caused by window fogging, reflection, or recognition errors; where displacement volume... The piston displacement is collected by a displacement sensor and calculated by combining the effective cross-sectional area A of the piston with the reference effective volume V0. A is obtained by piston structural dimension calibration or given by the cavity factory parameters. V0 can be obtained by geometric calibration or weighing calibration under the condition that the piston displacement is zero and the cavity is empty or filled with reference medium.

[0011] Furthermore, the control software also constructs consistency verification statistics for anomaly detection and control degradation switching: ; in, As a consistency indicator; It is a positive constant; To represent a unit of time The magnitude of the change is used to normalize the volume difference under different capacity change rates, thereby reducing misjudgments during rapid voltage regulation; when z≥z0, it is determined that the volume estimates of the two channels are inconsistent, the control software triggers an alarm and switches to the normalized value. A feedback-based closed-loop control strategy is adopted to improve the stability and data reliability of pressure-volume closed-loop control.

[0012] Furthermore, the control software is in the target area. The image is then normalized for illumination and a turbidity index is constructed. ,satisfy: ; in, For the first The turbidity index corresponding to the frame image. After grayscale processing of the k-th frame image captured by the camera, at the pixel... Pixel value at; A dark field reference image is used to eliminate camera dark current and fixed pattern noise; This is a reference image used to compensate for fill light intensity drift, reflection differences, and non-uniform background lighting. This represents an image gradient operator used to extract edge / texture variation features of fog droplet scattering, interface texture, and foam structure. The gradient operator can be implemented using existing Sobel operators, Scharr operators, Prewitt operators, or adjacent difference operators. And based on turbidity sequence Cumulative and change point statistics Automatically determine the phase transition point, wherein the statistics satisfy: ; in, This is a sign function; it takes the value 1 when the value inside the parentheses is greater than 0, 0 when it is equal to 0, and -1 when it is less than 0. To find the maximum value function, The mean of the sliding window. Tolerance bandwidth, H is the trigger threshold; when ≥H and relatively When the offset is continuously increasing, the real-time feedback pressure of the pressure sensor at the trigger moment is defined as the turbidity point Pc; when ≥H and relatively When the offset is continuously decreasing, the real-time feedback pressure of the pressure sensor at the trigger moment is defined as the clarification point P1.

[0013] A method for using a high-temperature, high-pressure, fully visible phase and foam behavior characterization device includes the following steps: S1. Assembly and Pretreatment of the Device: Assemble the device according to the prescribed assembly process. Select either a short or long atomizing connector as needed, and install the appropriate agitator type onto the agitator interface. Check the sealing of each sealing part. Adjust the effective volume of the chamber to the maximum and use a vacuum pump to evacuate for 6 hours to remove residual water vapor and air. Pre-fill each intermediate container with carbon dioxide, surfactant system, ethanol or ethanol-surfactant composite system, and aqueous phase. Heat the chamber using a heating jacket and heat the intermediate containers accordingly to ensure that each gas, liquid, and composite system reaches the expected temperature. S2. Establishing a high-pressure carbon dioxide environment and injecting the formulation: Pressurize the carbon dioxide in the carbon dioxide cylinder to the fourth intermediate container using a booster, and after stabilization, inject a quantitative amount of high-pressure carbon dioxide into the chamber through a high-pressure pump to increase and stabilize the chamber pressure, and record the temperature and pressure data; open the first to fifth valves according to the experimental design, and dynamically switch different reagents under high pressure conditions through a six-way valve; inject surfactant solutions and ethanol or composite systems into the chamber through a high-pressure pump and atomizing nozzle; S3. Phase Scanning and Quantitative Characterization of Phase Behavior: Under isothermal conditions, the effective volume within the cavity is adjusted by changing the piston displacement through a piston-driven device, thereby causing pressure changes within the cavity. This enables pressure boosting or depressurization scanning, or the execution of a preset volume trajectory in constant pressure mode. During pressure scanning, a turbidity index is constructed based on images acquired by a camera, and change point detection is performed. When the turbidity statistic meets the preset triggering condition and shows a continuous upward shift, the real-time feedback pressure of the pressure sensor at that triggering moment is recorded as the turbidity point Pc. When the turbidity statistic meets the preset triggering condition and shows a continuous downward shift, the real-time feedback pressure of the pressure sensor at that triggering moment is recorded as the clarification point P1, in order to obtain quantitative information on phase boundaries, critical behavior, and gas-liquid transition processes. S4. Disturbance and Visualization Recording: Based on the recording of Pc and P1 in step S3, the fluid in the cavity is disturbed by rotation and shearing using the stirring and rotation module; the phase interface changes, atomization dispersion morphology and foam evolution process are visualized and observed by the camera; and temperature, pressure, displacement and image data are recorded by the data acquisition and computer control module. S5. Temperature condition switching and repeated experiments: Change the temperature setpoint and stabilize it, then repeat steps S3 and S4 to obtain the phase behavior or dispersion morphology at different temperatures. S6. Study on phase behavior changes under water disturbance: A quantitative water phase is added into the cavity through a high-pressure pump and atomizing nozzle to cause water disturbance in the system. The phase behavior changes are observed and the effect of water addition on the phase behavior of the system is studied. S7. Foam generation and foam performance evaluation: Under set temperature and pressure conditions, increase the stirring and rotation intensity and maintain it for a predetermined time, and record the foam volume and liquid separation half-life; if necessary, replace the high-speed camera to record the foam evolution and liquid separation process at high speed.

[0014] The beneficial effects achieved by this invention are: 1. This invention utilizes a high-temperature and high-pressure resistant visual observation chamber to construct a controllable environment. Through the coordinated action of a volume adjustment module and a pressure control module, the temperature, pressure, and volume inside the experimental chamber can be continuously adjusted within a wide range to simulate the environment in wellbore and reservoir, obtaining a more realistic phase evolution process. An atomization injection module and a stirring module are set up to simulate the injection mixing conditions at the injection end and the shear disturbance conditions inside the wellbore, respectively, so that the atomization, phase behavior changes, foam generation and collapse behavior of the carbon dioxide-surfactant / auxiliary agent-water composite system can be continuously completed in the same device.

[0015] 2. The visualization imaging module of this invention achieves real-time high-definition observation through multiple light sources and different sapphire viewing windows. Equipped with a high-definition camera and a high-speed camera, it can observe the occurrence / dissolution state of surfactants or composite systems in carbon dioxide and the entire process of foam formation / collapse. Combined with the light source system, it can obtain clear images of interface changes for quantitative analysis of atomization scale, foam stability, and gas-liquid distribution characteristics. Simultaneously, the data acquisition and computer control module can collect and automatically record temperature, pressure, volume, jet speed, stirring speed, and image information in real time, realizing the linkage control of experimental parameters, automatic execution of preset steps, and data visualization processing. This effectively overcomes the problems of scattered data, excessive manual intervention, and poor repeatability in existing technologies.

[0016] 3. This invention integrates multiple experimental functions such as phase observation, atomization mixing, foam generation, and foam stability evaluation into a single system. It can continuously observe and evaluate the phase behavior and foam performance of the carbon dioxide system under unified conditions, providing experimental data with good repeatability and low fidelity for reservoir development, foam flooding design, and phase behavior research. Attached Figure Description

[0017] The invention will be further understood from the following description taken in conjunction with the accompanying drawings. The components in the drawings are not necessarily drawn to scale, but rather the emphasis is on illustrating the principles of the embodiments. In different views, the same reference numerals designate corresponding parts.

[0018] Figure 1 This is a cross-sectional structural schematic diagram of the high-temperature and high-pressure fully visible phase and foam behavior characterization device of the present invention.

[0019] Figure 2 This is another cross-sectional structural schematic diagram of the high-temperature and high-pressure fully visible phase and foam behavior characterization device of the present invention.

[0020] Figure 3 Appendix of the present invention Figure 2 A magnified schematic diagram of the structure at point A in the middle.

[0021] Figure 4 Appendix of the present invention Figure 2 Enlarged schematic diagram of the structure at point B.

[0022] Figure 5 This is a schematic cross-sectional view of the high-temperature, high-pressure, multifunctional, fully visualized phase and foam behavior integrated characterization device of the present invention.

[0023] Figure 6 This is a visualization image of the atomized surfactant entering the supercritical CO2 environment in Example 2 of the present invention.

[0024] Figure 7 This is a graph showing the change of phase transition point (Pc / P1) with the mass fraction of ethanol in Embodiment 2 of the present invention.

[0025] Explanation of reference numerals: 1. High-temperature and high-pressure resistant visual observation chamber; 2. Upper flange of the vessel body; 3. Volume adjustment piston; 4. Sapphire lower viewing window; 5. Lower viewing window cover; 6. Lower viewing window PEEK ring; 7. Flat head bolt; 8. Stirring device; 9. Contouring sleeve; 10. Sapphire upper viewing window; 11. Upper viewing window PEEK gasket; 12. Upper viewing window PEEK ring; 13. Upper viewing window Waldner gasket; 14. Replaceable short atomizing connector; 15. Replaceable long atomizing connector; 16. O-ring; 17. Lower viewing window PEEK gasket; 18. O-ring; 19. O-ring; 20. Guide ring; 21. Piston retaining ring; 22. Stirring motor fixing clamp; 23. Stirring motor fixing support; 24. Extended protective connector; 25. Heating jacket; 26. Retaining ring; 27. O-ring; 28. 29. Atomizing nozzle; 30. Copper gasket; 31. Upper flange retaining ring; 32. O-ring; 33. Agitator interface; 34. Piston drive device; 35. Rotary shaft one; 36. Rotary shaft two; 37. Connecting flange; 38. Piston flange; 39. Oil-free bushing; 40. Bushing baffle; 41. Lower flange of cylinder; 42. Displacement sensor; 43. Scale; 44. Support plate one; 45. Support plate two; 46. Adjustable camera bracket; 47. Camera; 48. ISCO pump; 49. Six-way valve; 50. Carbon dioxide cylinder; 51. Booster; 52. First intermediate container; 53. Second intermediate container; 54. Third intermediate container; 55. Fourth intermediate container; 56. First valve; 57. Second valve; 58. Third valve; 59. Fifth valve. Detailed Implementation

[0026] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to its embodiments. It should be noted that the specific embodiments described herein are for illustrative purposes only and are not intended to limit the scope of this invention. Other systems, methods, and / or features of this embodiment will become apparent to those skilled in the art after reviewing the following detailed description. Furthermore, the terminology used to describe positional relationships in the accompanying drawings is for illustrative purposes only and should not be construed as limiting this patent. Those skilled in the art can understand the specific meaning of the above terms according to the specific circumstances.

[0027] Example 1: Combined with Appendix Figure 1 Appendix Figure 2 Appendix Figure 3 Appendix Figure 4 and attached Figure 5 This embodiment constructs a high-temperature and high-pressure fully visible phase state and foam behavior characterization device, including a high-temperature and high-pressure resistant visual observation cavity, an atomizing spray module, a volume adjustment module, a temperature control module, a pressure control module, a stirring and rotation module, a visualization imaging module, and a data acquisition and computer control module.

[0028] The high-temperature and high-pressure visual observation cavity 1 is sealed and connected to the upper flange 2 of the vessel body and the lower flange 40 of the cylinder body to form a pressure-resistant visual cavity. A sapphire upper viewing window 10 and a sapphire lower viewing window 4 are respectively provided at the top and bottom of the cavity to achieve dual-view imaging. The upper viewing window consists of an upper viewing window PEEK gasket 11, an upper viewing window PEEK ring 12, and an upper viewing window Walka gasket 13, forming an upper sealing assembly. Preferably, a contour sleeve 9 is provided at the mounting location of the upper viewing window. The contour sleeve 9 cooperates with the outer edge of the upper viewing window and the upper flange step and / or the upper flange retaining ring to achieve coaxial positioning, stress buffering, and force uniformity, thereby reducing the risk of local stress concentration of the sapphire window under high pressure and thermal cycling conditions. An upper flange retaining ring 30 is provided on the outside of the upper sealing assembly to axially limit and compress the upper viewing window 10; preferably, an O-ring 16 and an O-ring 31 are also provided at the sealing location of the upper viewing window 10 to form a multi-stage sealing structure together with the copper gasket 29. This improves the sealing reliability and thermal cycling resistance under high-pressure conditions. The lower viewing window cover 5, lower viewing window PEEK ring 6, lower viewing window PEEK gasket 17, and O-rings 18 and 19 constitute the lower sealing structure. The lower viewing window cover 5 is connected to the cavity body via flat-head bolts 7, achieving preload compression of the lower viewing window 4 and facilitating disassembly and maintenance. The heating jacket 25 covers the outside of the cavity, enabling overall temperature control of the cavity 1, achieving a constant temperature range of -20 to 180℃.

[0029] Preferably, imaging devices are arranged in the upper and lower viewing windows respectively, or image sequences are acquired from different perspectives. The control software can perform geometric calibration and registration on the dual-view images at the same time, and perform three-dimensional characterization or three-dimensional reconstruction of the interface / foam structure based on the known cavity geometry, thereby obtaining three-dimensional information on the spatial morphology of the atomized plume, the foam height distribution, and the interface spatial configuration. Furthermore, a limiting groove or limiting structure can be provided on the inner wall of the cavity or at the part that mates with the piston / stirring assembly to limit the installation position and axial travel range of the stirring assembly, jetting assembly, or guide ring, so as to improve the positioning accuracy and operational stability under high pressure conditions.

[0030] The atomizing injection module, which can replace either the short atomizing connector 14 or the long atomizing connector 15, forms a multiphase system injection component. It can create an atomized dispersion system within the cavity for studying processes such as carryover behavior and atomization effects. An injection pressure regulating valve / throttle valve can be installed on the atomizing injection path to further adjust the injection pressure difference based on the ISCO pump output pressure, or to achieve rapid opening and closing and pressure stabilization at the start and stop of injection, thereby obtaining the set injection pressure difference and injection flow rate. Preferably, a retaining ring 26 is provided at the connection between the replaceable atomizing connector and the atomizing nozzle 28 for axial limiting and quick-release positioning, and an O-ring 27 is provided for high-pressure sealing, thus ensuring reliable connection and repeatability when replacing the short atomizing connector 14 or the long atomizing connector 15. The replaceable nozzle can be a direct injection type, a conical injection type, or a thin-film injection type, etc., to control the injection angle, droplet size distribution, and spray pattern, thereby adapting to atomization dispersion experiments under different phase ranges and different shear intensities.

[0031] In the volume adjustment module, the volume adjustment piston 3 is driven by the piston drive device 33 and achieves axial linear movement through the guide ring 20 and the oil-free bushing 38 for guidance and limitation. Preferably, a piston retaining ring 21 is provided on the outer periphery of the volume adjustment piston 3. The piston retaining ring 21 cooperates with the guide ring 20 to limit the axial movement of the piston assembly and maintain the stability of the guide clearance. Preferably, a bushing baffle 39 is provided on the outer side of the oil-free bushing 38 to limit the axial movement of the oil-free bushing 38 and prevent it from falling off, and to maintain the stability of the guide assembly position under high-pressure vibration conditions. The displacement sensor 41 collects the displacement of the piston 3 in real time and transmits it to the computer control software. The control software calculates the effective volume in the cavity based on the effective cross-sectional area of ​​the piston and the displacement, and can perform closed-loop control of the piston drive device 33 accordingly to achieve constant volume, programmed variable volume, or fine control according to a set volume trajectory. The maximum effective volume of the chamber is 300 mL, and the minimum effective volume is 100 mL. The effective volume corresponding to the piston stroke is continuously adjustable within the range of 100–300 mL. The above volume range can be set by those skilled in the art based on actual conditions, according to the chamber size and piston stroke design.

[0032] The temperature control module consists of a heating jacket 25 and an external circulating thermostat. The heating jacket 25 can be a flexible heating jacket or a fully enclosed thermostat. The temperature of the cavity 1 is collected in real time by a temperature sensor and input into the computer control software. The control software adjusts the output power of the heating jacket 25 and / or the operating conditions of the external circulating thermostat according to the temperature setpoint and feedback value, thereby achieving constant temperature or programmed temperature rise and fall control of the cavity 1.

[0033] The pressure control module consists of a pressure sensor, a piston drive device 33, and / or an external ISCO pump 47. The pressure sensor collects the pressure of the cavity 1 in real time and inputs it into the computer control software. In constant pressure mode, the control software drives the piston drive device 33 to adjust the displacement of the piston 3 and / or controls the output of the ISCO pump 47 based on pressure feedback, achieving pressure closed-loop stability. In programmed pressure increase or decrease mode, the control software executes control according to the set pressure step or pressure trajectory, and simultaneously records temperature-pressure-volume data for phase boundary and critical behavior analysis. The piston drive device 33 is connected to the volume regulating piston 3 via a connecting flange 36 and a piston flange 37 to reliably transmit the axial push / pull force output by the drive to the volume regulating piston 3, and to ensure transmission coaxiality and sealing stability.

[0034] The stirring and rotating module achieves cavity rotation via rotating shaft 34 and rotating shaft 35, and is equipped with a scale 42 to indicate the cavity rotation angle, thus providing fine angle adjustment. Stirring is achieved through stirring device 8, stirring motor fixing clamp 22, stirring motor fixing support 23, and stirring paddle interface 32, achieving high-speed stirring and stable power output. Rotating shaft 34 and rotating shaft 35 are respectively mounted on support plate 43 and support plate 44, which provide load-bearing and positioning references to ensure coaxiality, rigidity, and angle adjustment stability during cavity rotation.

[0035] The visualization imaging module, comprising a high-definition camera or high-speed camera 46, is connected to the cavity 1 via an adjustable camera bracket 45. The imaging distance can be adjusted by changing the bracket height. It provides supplementary lighting for imaging through a front light source group and a rear light source group. These light source groups are conventional supplementary lighting devices, ensuring clear imaging. Preferably, an extended protective connector 24 is provided on the camera mounting side. This extended protective connector 24 is used for heat insulation and impact protection of the imaging port, and provides structural leeway for the camera / light source mounting distance and focusing stroke.

[0036] The data acquisition and computer control module includes a data acquisition unit and a control unit. The data acquisition unit includes a temperature acquisition channel, a pressure acquisition channel, and a displacement acquisition channel: the temperature sensor acquires the temperature of the cavity 1, the pressure sensor acquires the pressure of the cavity 1, the displacement sensor 41 acquires the piston displacement to calculate the effective volume inside the cavity; the stirring device 8 provides feedback on the actual rotation speed; and the camera 46 acquires real-time images or videos inside the cavity.

[0037] The control unit is electrically connected to the heating jacket 25, the piston drive device 33 and the external ISCO pump 47 through computer control software to realize the setting, switching and linkage control of temperature, pressure and volume or piston displacement, and to perform interlock monitoring of overpressure, overtemperature and / or overtorque.

[0038] Specifically, the control software calculates the displacement volume based on the piston displacement collected by the displacement sensor 41, and robustly fuses it with the volume calculated from the image to obtain an estimate of the effective cavity volume, which is used for volume-pressure linkage closed-loop control; the robust fusion satisfies the following relationship: ; in, For displacement volume With image volume The effective volume estimate of the cavity obtained through robust fusion; The displacement volume is obtained from the piston displacement. The image volume obtained from image processing. The fusion coefficient is... As a consistency threshold, This indicates that the volume difference value is truncated at upper and lower limits to suppress abnormal volume jumps caused by window fogging, reflection, or recognition errors; where displacement volume... The piston displacement is acquired by displacement sensor 41 and calculated by combining the effective cross-sectional area A of the piston and the reference effective volume V0. A can be obtained from piston structural dimension calibration or given by the cavity's factory parameters. V0 can be obtained through geometric calibration or weighing calibration under conditions where the piston displacement is zero and the cavity is empty or filled with a reference medium. Image volume Images are acquired by camera 46. After establishing a mapping relationship based on pixel-length calibration using the effective size of the viewport and / or the known structural dimensions inside the cavity, the phase interface height or foam height is identified and calculated by combining the internal geometric dimensions or equivalent cross-sectional area of ​​the cavity. Fusion coefficient The correction weight used to characterize the image volume to the displacement volume is preferably adaptively set according to image quality: a larger value is used when the image clarity is high, the contrast of the visible phase boundary is high, or the window is unobstructed; a smaller value is used when fogging, reflection, or unclear visible boundaries occur. As one implementation method, a short-term calibration experiment can be conducted under clear, unobstructed conditions to compare... and The consistency and noise level are determined by combining the signal-to-noise ratio or edge contrast index of the image channels. The value range is determined and updated based on real-time image quality during the experiment. Consistency threshold. The maximum injection amplitude for limiting the volume difference is preferably determined by the normal fluctuation range of the system: the volume difference is collected over a period of time under stable operating conditions. - Calculate its statistical distribution (e.g., mean and standard deviation), and then... The range of the difference is set to the upper limit under normal operating conditions (e.g., the amplitude corresponding to several times the standard deviation) to ensure effective fusion under normal conditions and automatic amplitude limiting during abnormal jumps.

[0039] The control software also constructs consistency verification statistics for anomaly detection and control degradation switching: ; in, As a consistency indicator; It is a positive constant; To represent a unit of time The magnitude of the change is used to normalize the volume difference under different capacity change rates, thereby reducing misjudgments during rapid voltage regulation; when z≥z0, it is determined that the volume estimates of the two channels are inconsistent, the control software triggers an alarm and switches to the normalized value. A feedback-based closed-loop control strategy is adopted to improve the stability and data reliability of pressure-volume closed-loop control. To avoid zero denominators and normalize the static segment, the threshold z0 is preferably taken as the lower limit of the minimum resolvable volume change or displacement volume change rate of the system, which can be calculated from the displacement sensor resolution, sampling period, and effective cross-sectional area of ​​the piston. The threshold z0 is used for consistency anomaly detection, preferably determined through offline calibration or pre-experimentation: the range of consistency indicators is statistically analyzed under normal operating conditions and typical abnormal operating conditions (e.g., window fogging, strong reflection, recognition failure), and z0 is set as the discrimination threshold that can effectively distinguish between normal and abnormal conditions; when z ≥ z0, the control software triggers an alarm and switches to [the threshold value is missing here]. A feedback control strategy is adopted to ensure closed-loop stability.

[0040] In terms of image processing, the control software establishes a pixel-length mapping based on the known structural dimensions inside the cavity and / or the effective size of the viewing window as the image calibration benchmark, thereby identifying the phase interface position and foam height in the image. Among them, the displacement sensor collects the piston displacement as the benchmark quantity of the change in length inside the cavity, and combines it with the effective cross-sectional area of ​​the piston to calculate the effective volume inside the cavity. In addition, it combines the internal geometric dimensions or equivalent cross-sectional area of ​​the cavity to convert and allocate the effective volume, calculate the liquid volume, gas phase volume and / or foam volume and their changes over time, and use them to obtain evaluation parameters related to cloud point or clear point, foam volume and liquid precipitation decay.

[0041] Among them, the control software is in the target area The image is then normalized for illumination and a turbidity index is constructed. ,satisfy: ; in, For the first The turbidity index corresponding to the frame image. After grayscale processing of the k-th frame image captured by camera 46, at the pixel... Pixel value at; The dark field reference image is used to eliminate camera dark current and fixed pattern noise. It is preferably obtained by acquiring multiple dark field images under shading conditions and averaging them. The shading conditions are turning off the light source, blocking the lens, or acquiring the image under conditions without incident light. The reference image is used to compensate for the drift of the supplementary light intensity, the difference in reflection, and the non-uniform background illumination. It is preferable to select the reference frame in the clear and stable state of the system as a static reference; or the moving average of the most recent frames can be used as a dynamic reference to adapt to the slow changes in illumination during the experiment. This represents an image gradient operator used to extract edge / texture variation features of fog droplet scattering, interface textures, and foam structures. The gradient operator can be implemented using existing Sobel, Scharr, Prewitt, or adjacent difference operators. The norm of the gradient is squared and... The gradient energy type turbidity index can be obtained by summing / averaging the inner values, which is used to characterize the overall structural changes caused by enhanced texture and scattering as the turbidity changes.

[0042] And based on turbidity sequence Cumulative and change point statistics Automatically determine the phase transition point, wherein the statistics satisfy: ; in, This is a sign function; it takes the value 1 when the value inside the parentheses is greater than 0, 0 when it is equal to 0, and -1 when it is less than 0. To find the maximum value function, The mean of the sliding window. Tolerance bandwidth, H is the trigger threshold; when ≥H and relatively When the offset is continuously increasing, the real-time feedback pressure of the pressure sensor at the trigger moment is defined as the turbidity point Pc; when ≥H and relatively When the offset is continuously decreasing, the real-time feedback pressure of the pressure sensor at the trigger moment is defined as the clarification point P1. The target area is preferably a sub-region of the image covering the phase interface or the main evolution area of ​​the foam within the effective field of view of the viewing window, avoiding fixed structures such as the edges of the viewing window, bolts, and sealing rings. The target area can be manually selected by the operator during initial setup, or it can be automatically extracted by the software based on the geometry of the viewing window (e.g., taking the inscribed area after detecting the boundary of a circular / elliptical window frame).

[0043] The sliding window, used as a turbidity baseline, preferably has a window length preset based on the sampling frequency and system response time, or determined through pre-experiments. The mean of the sliding window can be achieved using existing moving average methods; if necessary, exponential moving averages can also be used to reduce storage and computational overhead. The tolerance bandwidth is used to suppress small turbidity shifts caused by imaging noise, minor fluctuations in illumination, or single-frame reflections. It is preferably set based on the fluctuation scale of the T1 sequence in the clear stable segment (e.g., using a multiple of the fluctuation amplitude of that segment as the tolerance bandwidth), so that the statistic only accumulates for persistent and significant shifts. The trigger threshold is used to determine the triggering condition for the accumulation and statistic to reach a phase transition. It is preferably calibrated through pre-experiments to ensure reliable triggering when a phase transition occurs, even if no trigger occurs in the clear stable segment. The pre-experiment can be conducted by collecting T1 sequence data from the clear stable segment in typical clear segments and typical turbid segments, and adjusting the H value to meet the requirements for false trigger rate and false detection rate. The accumulation and change point detection belong to existing sequence change point detection methods, and the software can perform calculations based on sampling time. Real-time updates are performed, and the corresponding pressure sensor values ​​are read upon triggering to determine Pc and P1 respectively.

[0044] like Figure 2 As shown, the device is externally connected to a first intermediate container 51, a second intermediate container 52, a third intermediate container 53, and a fourth intermediate container 54. Each intermediate container 51–54 is connected to different channels of a six-way valve 48 via a first valve 55, a second valve 56, a third valve 57, and a fourth valve 58, respectively. The common end of the six-way valve 48 is connected to an ISCO pump 47, and the other end of the ISCO pump 47 is connected to the cavity injection port and / or the atomizing jet channel to achieve dynamic switching and quantitative injection of different reagents under high pressure conditions. Among them, the first intermediate container 51 is preferably used for pre-filling a surfactant system, the second intermediate container 52 is preferably used for pre-filling ethanol, the third intermediate container 53 is preferably used for pre-filling an ethanol-surfactant composite system and / or an aqueous phase, and the fourth intermediate container 54 is preferably used for pre-filling pressurized high-pressure carbon dioxide and serving as a pressure stabilizing buffer container. The pre-filling includes sealing the container after filling with the medium, evacuating the container and its connecting pipelines and / or replacing them with carbon dioxide to remove residual air and water vapor, and ensuring that the temperature of the medium inside the intermediate container is consistent with the set temperature of the cavity under the matching heating conditions. The carbon dioxide cylinder 49 establishes a high-pressure carbon dioxide supply path to the fourth intermediate container 54 via the booster 50 and the fifth valve 59. After the fourth valve 58 is turned on, the fourth intermediate container 54 supplies high-pressure carbon dioxide to the cavity via the six-way valve 48 and the ISCO pump 47. The fifth valve 59 is used to open or isolate the carbon dioxide supply branch to achieve shut-off and safe isolation during filling, pressure stabilization or maintenance.

[0045] The above structure ensures that this device can simultaneously achieve multiple functions such as high temperature and high pressure, visualization, atomized injection, interchangeable injection methods, precise stirring, volume adjustment, and computer data acquisition and control, providing basic conditions for the study of phase behavior and foam laws.

[0046] A method for using a high-temperature, high-pressure, multifunctional, fully visualized device for summarizing and characterizing phase states and foam behavior includes the following steps: S1. Assembly and Pretreatment of the Device: Assemble the device according to the prescribed assembly process. Select either the short atomizing connector 14 or the long atomizing connector 15 as required, and install the stirring paddle type to the stirring paddle interface 32. Check the sealing of each sealing part. Adjust the effective volume of the chamber to the maximum and use a vacuum pump to evacuate for 6 hours to remove residual water vapor and air. Pre-fill each intermediate container with carbon dioxide, surfactant system, ethanol or ethanol-surfactant composite system and aqueous phase. Heat the chamber through the heating jacket 25 and heat the intermediate containers accordingly to bring each gas, liquid and composite system to the expected temperature. S2. Establishing a high-pressure carbon dioxide environment and injecting the formulation: The carbon dioxide in the carbon dioxide cylinder 49 is pressurized to the fourth intermediate container 54 by the booster 50, and after stabilization, a quantitative amount of high-pressure carbon dioxide is injected into the chamber through the ISCO pump 47 to increase and stabilize the chamber pressure, and the temperature and pressure data are recorded; according to the experimental design, the first to fifth valves 55-59 are opened, and the dynamic switching of different reagents is achieved under high pressure conditions through the six-way valve 48; the surfactant solution and ethanol or a composite system are injected into the chamber through the ISCO pump 47 and the atomizing nozzle 28; S3. Phase Scanning and Quantitative Characterization of Phase Behavior: Under isothermal conditions, the effective volume within the cavity is adjusted by changing the piston displacement through a piston-driven device, thereby causing pressure changes within the cavity. This enables pressure boosting or depressurization scanning, or the execution of a preset volume trajectory in constant pressure mode. During pressure scanning, a turbidity index is constructed based on images acquired by a camera, and change point detection is performed. When the turbidity statistic meets the preset triggering condition and shows a continuous upward shift, the real-time feedback pressure of the pressure sensor at that triggering moment is recorded as the turbidity point Pc. When the turbidity statistic meets the preset triggering condition and shows a continuous downward shift, the real-time feedback pressure of the pressure sensor at that triggering moment is recorded as the clarification point P1, in order to obtain quantitative information on phase boundaries, critical behavior, and gas-liquid transition processes. S4. Disturbance and Visualization Recording: Based on the recording of Pc and P1 in step S3, the fluid in the cavity is disturbed by rotation and shearing using the stirring and rotation module; the phase interface changes, atomization dispersion morphology and foam evolution process are visualized and observed by the camera; and temperature, pressure, displacement and image data are recorded by the data acquisition and computer control module. S5. Temperature condition switching and repeated experiments: Change the temperature setpoint and stabilize it, then repeat steps S3 and S4 to obtain the phase behavior or dispersion morphology at different temperatures. S6. Study on phase behavior changes under water addition disturbance: A quantitative water phase is added to the cavity through ISCO pump 47 and atomizing nozzle 28 to cause water addition disturbance in the system. The phase behavior changes are observed and the effect of water addition on the phase behavior of the system is studied. S7. Foam generation and foam performance evaluation: Under set temperature and pressure conditions, increase the stirring and rotation intensity and maintain it for a predetermined time, and record foam performance indicators such as foam volume and liquid separation half-life; if necessary, replace the high-speed camera 46 to record the foam evolution and liquid separation process at high speed.

[0047] Example 2: Combined with Appendix Figure 1 Appendix Figure 2 Appendix Figure 3 Appendix Figure 4 and attached Figure 5 In addition to the content of the above embodiments, the experimental procedure of Example 2 is as follows: In order to simulate the phase transition and foam generation-attenuation behavior of the CO2-surfactant-ethanol / water composite system under high temperature and high pressure conditions during the formulation step injection and pressure scanning process, the experimental procedure of Example 2 is as follows: S11. Assembly and Pretreatment of the Device in Example 2: Assemble the device according to the prescribed assembly process. Select either the short atomizing connector 14 or the long atomizing connector 15 as needed, and install the stirring paddle type onto the stirring paddle interface 32. Check the sealing performance of each sealing part. Adjust the effective volume of the cavity to the maximum and use a vacuum pump to evacuate for 6 hours to remove residual water vapor and air. Heat the cavity through the heating jacket 25 and heat the intermediate container accordingly to bring the gases, liquids, and composite system to the expected temperature. The set temperature T is 40°C. Prepare a surfactant solution with a surfactant concentration of 0.5 wt%. S12. Establishment of a high-pressure carbon dioxide environment and initial state recording in Example 2: The carbon dioxide in the carbon dioxide cylinder 49 is pressurized to the fourth intermediate container 54 using a booster 50, and after stabilization, a quantitative amount of high-pressure carbon dioxide is injected into the cavity through an ISCO pump 47 to increase and stabilize the cavity pressure; wherein, the total mass of injected carbon dioxide is 100g, and the initial pressure P0 is recorded after the pressure stabilizes, and the corresponding temperature and pressure data are recorded. S13. Stepwise injection and phase stabilization of the formulation in Example 2: According to the experimental design, valves 55-59 from the first to the fifth valve were opened, and different reagents were dynamically switched under high pressure through the six-way valve 48; a quantitative surfactant solution was first added under high pressure through the intermediate container and the six-way valve 48, and then ethanol was added sequentially, with an increment of 0.1 wt% each time; after each addition, the stirring motor was turned on and stirred at a low speed of 500 r / min, and then allowed to stand for 20 min until the phase was stable; S14. Pressure scanning and phase transition point acquisition in Example 2: Keep the temperature constant, adjust the displacement of piston 3 by changing the volume of piston 3 through piston drive device 33 to adjust the effective volume in the cavity and cause pressure changes, thereby realizing pressure boosting or depressurization scanning; the pressure is adjusted once every 0.5MPa, and the pressure is adjusted once every 0.1MPa near the turbidity point; during the pressure scanning process, the cavity image is acquired synchronously and the trigger time of turbidity transition and clarification transition is identified by control software / image processing criteria, and the pressure sensor feedback pressure at the corresponding trigger time is recorded as turbidity point Pc and clarification point P1 respectively, and the average value is obtained by repeating three times; S15, Temperature switching and repeated pressure scan in Example 2: Change the temperature setpoint and stabilize it, repeat S14 to obtain the value of Pc at different temperatures; S16. Observation of water addition disturbance and phase behavior changes in Example 2: Under the condition of maintaining the target temperature and pressure, a quantitative amount of deionized water in the aqueous intermediate container was added into the cavity through the device injection passage by ISCO pump 47. After the system stabilized, the phase behavior changes in the cavity were observed and the images and data were recorded. S17. Evaluation of foam performance and high-speed imaging in Example 2: Under set temperature and pressure conditions, turn on the stirrer and set the high-speed stirring to 3000 r / min for 180 s; then stop stirring and record the foam volume V and the half-life t1 / 2 of the liquid separation; if necessary, replace the high-speed camera 46 to record the foam decay and liquid separation process at high speed.

[0048] like Figure 6 This is a visualization of the atomized surfactant entering the supercritical CO2 environment in Example 2; like Figure 7 This is a graph showing the change of phase transition point (Pc / P1) with the mass fraction of ethanol in Example 2. Table 1 shows the foam performance data of Embodiment 2 of the present invention: Table 1

[0049] Depend on Figure 6 As can be seen, after the surfactant solution is sprayed into supercritical CO2 through the atomizing nozzle, it forms a distinct droplet dispersion / spray plume within the visible cavity. Under stirring and temperature / pressure control conditions, rapid mixing and interfacial morphology evolution occur, providing a visual basis for subsequent phase transitions and foam generation processes. Figure 7It is evident that under different temperature conditions, the phase transition point Pc / P1 of the system exhibits a clear and regular difference with the change in ethanol mass fraction, and the phase transition point shifts systematically with increasing temperature, indicating that temperature and the content of co-solvent components have a significant regulatory effect on the phase boundary of the system. Further analysis of Table 1 shows that, under the condition of 0.3% ethanol mass fraction, when the temperature increases from 313.15 K to 333.15 K, the half-life of the liquid precipitation decreases from 851 min to 738 min, and the foaming ratio decreases from 620% to 560%, indicating that under the conditions of this embodiment, increasing the temperature reduces foam stability and foaming performance. This result is consistent with the trend of phase boundary changes with temperature, indicating that this device can achieve coupled characterization of phase-foam behavior and can be used to evaluate the influence of temperature, pressure, and formulation factors on the stability of foam-driven systems.

[0050] Example 3: Combined with Appendix Figure 1 Appendix Figure 2 Appendix Figure 3 Appendix Figure 4 and attached Figure 5 Based on the apparatus and general usage method of Example 1, this example differs from Example 2 in that, in addition to the general steps S1–S7, it focuses on forming a dispersion system by atomization spraying under liquid or supercritical carbon dioxide conditions, and evaluates the presence, dispersion uniformity, and stability of surfactants or additive-surfactant composite systems in carbon dioxide. Compared with Example 2, Example 3 generally does not perform water addition disturbance and foam evaluation steps, but focuses on atomization dispersion morphology criteria and stabilization time / deposition behavior as the main outputs.

[0051] S21. Assembly and pretreatment of the device in Example 3: Assemble the device according to the prescribed assembly process. Select either the short atomizing connector 14 or the long atomizing connector 15 as required, and select the stirring paddle type to install on the stirring paddle interface 32. Check the sealing of each sealing part. Adjust the effective volume of the cavity to the maximum and use a vacuum pump to evacuate for 6 hours to remove residual water vapor and air. Select a suitable nozzle and install it on the atomizing nozzle 28. Heat the cavity through the heating jacket 25 and heat the intermediate container accordingly to ensure that the medium required for subsequent experiments reaches the expected temperature. S22. Establishment and stabilization of liquid or supercritical carbon dioxide operating conditions in Example 3: The carbon dioxide in the carbon dioxide cylinder 49 is pressurized to the fourth intermediate container 54 using the booster 50, and after stabilization, high-pressure carbon dioxide is injected into the cavity through the ISCO pump 47; the temperature T and pressure P are set so that the carbon dioxide is in the liquid range and the supercritical range respectively; each group of experiments is allowed to stand until the temperature and pressure stabilize and the temperature and pressure data are recorded. S23. Sample preparation and high-pressure connection switching in Example 3: Add surfactant or auxiliary agent-surfactant composite system to the intermediate container in advance; open the first valve to the fifth valve 55-59 according to the experimental design, and realize the dynamic switching of different reagents under high pressure through the six-way valve 48; connect the intermediate container and the atomizing nozzle 28 through the ISCO pump 47 to establish a high-pressure injection path from the sample to the cavity. S24. Execution and Visual Recording of Atomization Spraying in Example 3: Set the pressure difference to 2MPa, flow rate to 5mL / min, and spraying time to 1min. Start the ISCO pump 47 to perform atomization spraying through the atomizing nozzle 28. During the spraying process, the camera 46 continuously records the images, and the temperature, pressure, and image data are recorded synchronously through the data acquisition and computer control module. S25. Criteria for determining the form of existence in Example 3: The form of existence is determined based on the image within the field of view of camera 46: If there are no droplets or particles in the field of view, and no interfaces, stripes or sedimentary traces, it is determined to be true dissolution or sub-visible scale existence; if visible droplets or particles appear, or stripes or agglomeration zones appear, it is determined to be the dispersed existence of droplets or particles; if obvious sedimentary zones or sedimentary layer growth are observed on the wall or bottom, it is determined to be the existence of solid phase precipitation or gravity-driven sedimentation morphology. S26. Evaluation of dispersion uniformity and stability in Example 3: At the same time, the field of view is divided into four regions, the visible phase area fraction in each region is calculated, and the dispersion uniformity is characterized by the difference between the area fraction of each region and the total area fraction. After the spraying stops, imaging continues, and the change law of visible phase area fraction or deposition area fraction over time is recorded. The dispersion retention time is corresponding to the time when the visible phase disappears, and the time when the deposition area fraction reaches a stable value is taken as the deposition completion time. S27. Operating condition switching and repeating experiment of Example 3: Change the temperature setpoint and / or pressure setpoint and stabilize them to switch carbon dioxide between the liquid range and the supercritical range. Repeat S23 to S26 respectively to obtain the evaluation results of the dispersion morphology and stability under different phase ranges.

[0052] Example 3 enables the full-process visualization and quantitative evaluation of the atomized spray-formed dispersion system under liquid or supercritical carbon dioxide conditions. The control software, based on images / videos acquired by camera 46, identifies and statistically analyzes the spatiotemporal evolution of the atomized plume, droplet / particle dispersion, strip / agglomeration, and deposition zone, outputting the dispersion morphology determination results and providing dispersion uniformity and stability indices. The dispersion uniformity index can be characterized by the dispersion degree of the visible phase area fraction in each zone, and the stability index can be determined by the holding time corresponding to the decay of the visible phase area fraction to a preset threshold and the deposition completion time corresponding to the deposition area fraction reaching a stable value. This allows for comparative evaluation of the dissolution, dispersion, and precipitation behavior of surfactants or additive-surfactant composite systems in carbon dioxide under different temperature T and pressure P conditions, providing a basis for optimal formulation, screening operating conditions, and analyzing dispersion instability mechanisms.

[0053] While the invention has been described above with reference to various embodiments, it should be understood that many changes and modifications can be made without departing from the scope of the invention. That is, the methods, systems, and devices discussed above are examples. Various configurations can be appropriately omitted, substituted, or added to various processes or components. For example, in alternative configurations, methods can be performed in a different order than described, and / or various components can be added, omitted, and / or combined. Moreover, features described with respect to certain configurations can be combined in various other configurations, such as different aspects and elements of the configuration can be combined in a similar manner. Furthermore, the elements therein can be updated as the technology develops; many elements are examples and do not limit the scope of this disclosure or the claims. It should also be understood that after reading the description of this invention, those skilled in the art can make various alterations or modifications to the invention, and these equivalent changes and modifications also fall within the scope defined by the claims of this invention.

Claims

1. A high-temperature, high-pressure, fully visible phase state and foam behavior characterization device, characterized in that, include: The high-temperature and high-pressure resistant visualization observation chamber, atomizing jet module, volume adjustment module, temperature control module, pressure control module, stirring and rotation module, visualization imaging module, and data acquisition and computer control module; The observation cavity is formed by a sealed connection between the upper and lower flanges to form a pressure-resistant visualization cavity, and an upper viewing window and a lower viewing window are respectively set at the top and bottom of the cavity to achieve dual-view imaging. The temperature control module includes a heating jacket and an external circulating constant temperature device; the pressure control module includes a pressure sensor, a piston drive device, and / or an external high-pressure pump. The volume adjustment module includes a volume adjustment piston, a guide and limiting structure, and a displacement sensor. The volume adjustment piston moves linearly along the axial direction under the drive of the piston driving device to change the effective volume inside the cavity. The atomizing spray module includes an atomizing nozzle and a replaceable atomizing connector; The visualization imaging module includes a camera and an adjustable camera bracket, which work together with a front light source group and a rear light source group to form an image; The data acquisition and computer control module is used to acquire temperature, pressure, displacement, rotation speed and image data, and to perform linkage control of temperature, pressure and volume or piston displacement.

2. The high-temperature and high-pressure fully visible phase and foam behavior characterization device as described in claim 1, characterized in that, The upper and lower viewing windows are respectively equipped with imaging devices or acquire image sequences from different perspectives. The data acquisition and computer control module performs geometric calibration and registration on the dual-view images at the same time, and performs three-dimensional characterization or three-dimensional reconstruction of the interface and / or foam structure based on the cavity geometry.

3. The high-temperature and high-pressure fully visible phase and foam behavior characterization device as described in claim 2, characterized in that, The inner wall of the observation chamber or the part that mates with the piston and / or stirring assembly is provided with a limiting groove or limiting structure to limit the installation position and axial travel range of the stirring assembly, the spraying assembly or the guide limiting structure.

4. The high-temperature and high-pressure fully visible phase and foam behavior characterization device as described in claim 3, characterized in that, The data acquisition and computer control module includes a data acquisition unit and a control unit. The data acquisition unit includes a temperature acquisition channel, a pressure acquisition channel, and a displacement acquisition channel, which are used to acquire the cavity temperature, cavity pressure, and piston displacement, respectively. Among them, the piston displacement is used for subsequent calculation of the effective volume inside the cavity. The data acquisition unit also acquires the actual rotation speed of the stirring device and acquires real-time images or videos of the cavity obtained by the camera. The control unit uses computer control to set, switch, and control the temperature, pressure, volume, or piston displacement, and performs interlock monitoring of overpressure, overtemperature, and / or overtorque.

5. The high-temperature and high-pressure fully visible phase and foam behavior characterization device as described in claim 4, characterized in that, The control software calculates the displacement volume based on the piston displacement collected by the displacement sensor, and robustly fuses it with the volume calculated from the image to obtain an estimate of the effective cavity volume, which is used for volume-pressure linkage closed-loop control; the robust fusion satisfies the following relationship: ； in, For displacement volume With image volume The effective volume estimate of the cavity obtained through robust fusion; The displacement volume is obtained from the piston displacement. The image volume obtained from image processing. The fusion coefficient is... As a consistency threshold, This indicates that the volume difference value is truncated at upper and lower limits to suppress abnormal volume jumps caused by window fogging, reflection, or recognition errors; where displacement volume... The piston displacement is collected by a displacement sensor and calculated by combining the effective cross-sectional area A of the piston with the reference effective volume V0. A is obtained by piston structural dimension calibration or given by the cavity factory parameters. V0 can be obtained by geometric calibration or weighing calibration under the condition that the piston displacement is zero and the cavity is empty or filled with reference medium.

6. The high-temperature and high-pressure fully visible phase and foam behavior characterization device as described in claim 5, characterized in that, The control software also constructs consistency verification statistics for anomaly detection and control degradation switching: ； in, As a consistency indicator; It is a positive constant; To represent a unit of time The magnitude of the change is used to normalize the volume difference under different capacity change rates, thereby reducing misjudgments during rapid voltage regulation; when z≥z0, it is determined that the volume estimates of the two channels are inconsistent, the control software triggers an alarm and switches to the normalized value. A feedback-based closed-loop control strategy is adopted to improve the stability and data reliability of pressure-volume closed-loop control.

7. The high-temperature and high-pressure fully visible phase and foam behavior characterization device as described in claim 6, characterized in that, Control software in the target area The image is then normalized for illumination and a turbidity index is constructed. ,satisfy: ； in, For the first The turbidity index corresponding to the frame image. After grayscale processing of the k-th frame image captured by the camera, at the pixel... Pixel value at; A dark field reference image is used to eliminate camera dark current and fixed pattern noise; This is a reference image used to compensate for fill light intensity drift, reflection differences, and non-uniform background lighting. This represents an image gradient operator used to extract edge / texture variation features of fog droplet scattering, interface texture, and foam structure. The gradient operator can be implemented using existing Sobel operators, Scharr operators, Prewitt operators, or adjacent difference operators. And based on turbidity sequence Cumulative and change point statistics Automatically determine the phase transition point, wherein the statistics satisfy: ； in, This is a sign function; it takes the value 1 when the value inside the parentheses is greater than 0, 0 when it is equal to 0, and -1 when it is less than 0. To find the maximum value function, The mean of the sliding window. H is the tolerable bandwidth and the trigger threshold. when ≥H and relatively When the offset is continuously rising, the real-time feedback pressure of the pressure sensor at the trigger moment is defined as the turbidity point Pc. when ≥H and relatively When the offset is continuously decreasing, the real-time feedback pressure of the pressure sensor at the trigger moment is defined as the clarification point P1.

8. A method of using the high-temperature, high-pressure, fully visible phase and foam behavior characterization device according to any one of claims 1-7, comprising the following steps: S1. Assembly and Pretreatment of the Device: Assemble the device according to the prescribed assembly process. Select either a short or long atomizing connector as needed, and install the appropriate agitator type onto the agitator interface. Check the sealing of each sealing part. Adjust the effective volume of the chamber to the maximum and use a vacuum pump to evacuate for 6 hours to remove residual water vapor and air. Pre-fill each intermediate container with carbon dioxide, surfactant system, ethanol or ethanol-surfactant composite system, and aqueous phase. Heat the chamber using a heating jacket and heat the intermediate containers accordingly to ensure that each gas, liquid, and composite system reaches the expected temperature. S2. Establishing a high-pressure carbon dioxide environment and injecting the formulation: Pressurize the carbon dioxide in the carbon dioxide cylinder to the fourth intermediate container using a booster, and after stabilization, inject a quantitative amount of high-pressure carbon dioxide into the chamber through a high-pressure pump to increase and stabilize the chamber pressure, and record the temperature and pressure data; open the first to fifth valves according to the experimental design, and dynamically switch different reagents under high pressure conditions through a six-way valve; inject surfactant solutions and ethanol or composite systems into the chamber through a high-pressure pump and atomizing nozzle; S3. Phase Scanning and Quantitative Characterization of Phase Behavior: Under isothermal conditions, the effective volume within the cavity is adjusted by changing the piston displacement through a piston-driven device, thereby causing pressure changes within the cavity. This enables pressure boosting or depressurization scanning, or the execution of a preset volume trajectory in constant pressure mode. During pressure scanning, a turbidity index is constructed based on images acquired by a camera, and change point detection is performed. When the turbidity statistic meets the preset triggering condition and shows a continuous upward shift, the real-time feedback pressure of the pressure sensor at that triggering moment is recorded as the turbidity point Pc. When the turbidity statistic meets the preset triggering condition and shows a continuous downward shift, the real-time feedback pressure of the pressure sensor at that triggering moment is recorded as the clarification point P1, in order to obtain quantitative information on phase boundaries, critical behavior, and gas-liquid transition processes. S4. Disturbance and Visualization Recording: Based on the recording of Pc and P1 in step S3, the fluid in the cavity is disturbed by rotation and shearing using the stirring and rotation module; the phase interface changes, atomization dispersion morphology and foam evolution process are visualized and observed by the camera; and temperature, pressure, displacement and image data are recorded by the data acquisition and computer control module. S5. Temperature condition switching and repeated experiments: Change the temperature setpoint and stabilize it, then repeat steps S3 and S4 to obtain the phase behavior or dispersion morphology at different temperatures. S6. Study on phase behavior changes under water disturbance: A quantitative water phase is added into the cavity through a high-pressure pump and atomizing nozzle to cause water disturbance in the system. The phase behavior changes are observed and the effect of water addition on the phase behavior of the system is studied. S7. Foam generation and foam performance evaluation: Under set temperature and pressure conditions, increase the stirring and rotation intensity and maintain it for a predetermined time, and record the foam volume and liquid separation half-life; if necessary, replace the high-speed camera to record the foam evolution and liquid separation process at high speed.

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