Testing device and testing method

Abstract

The invention provides a testing device and a testing method, the device comprises a micron-sized reaction chamber, a temperature control device, a pressure control device and a phase state acquisition device, and the reaction chamber is connected with the temperature control device and the pressure control device; the reaction cavity is used for containing reaction substances for generating hydrates, the temperature control equipment is used for controlling the temperature in the reaction cavity, the pressure control equipment is used for controlling the pressure in the reaction cavity, the temperature control equipment comprises a cold and hot table and a temperature control assembly, and the cold and hot table is used for loading the reaction cavity; the temperature control assembly is connected with the cooling and heating table and used for controlling the temperature of the reaction cavity according to the cooling and heating table; the phase state acquisition equipment is used for acquiring the phase state information of the hydrate in the reaction cavity, so that the generation rate and the dissolution rate of the hydrate are determined according to the phase state information. According to the invention, the generation rate and the dissolution rate of the hydrate can be quantitatively measured.

Description

Technical Field

[0001] The present application relates to the field of new energy technology, and in particular to a testing device and a testing method. Background Art

[0002] With the rapid development of the world's industry, the demand and consumption of traditional fossil energy have increased dramatically, and energy shortage has become one of the problems that every country has to face. Hydrates have attracted widespread attention from countries around the world due to their huge reserves and high energy density.

[0003] Hydrate growth and dissolution are important research areas in the foundation of hydrate application technology. Most of the related technologies are based on macroscopic qualitative descriptions of the hydrate formation and dissolution process based on temperature and pressure changes, and it is difficult to quantitatively measure key parameters (such as formation rate and dissolution rate). Summary of the invention

[0004] In view of the above, it is necessary to provide a testing device and a testing method that can solve the technical problem of difficulty in quantitatively measuring the formation rate and dissolution rate of hydrates.

[0005] In a first aspect, an embodiment of the present application provides a testing device, comprising a micron-scale reaction chamber, a temperature control device, a pressure control device, and a phase state acquisition device, wherein the reaction chamber is connected to the temperature control device and the pressure control device; the reaction chamber is used to accommodate a reaction substance that generates a hydrate, the temperature control device is used to control the temperature in the reaction chamber, and the pressure control device is used to control the pressure in the reaction chamber, wherein the temperature control device comprises a hot and cold stage and a temperature control component: the hot and cold stage is used to load the reaction chamber; the temperature control component is connected to the hot and cold stage, and is used to control the temperature of the reaction chamber according to the hot and cold stage; the phase state acquisition device is used to collect phase state information of the hydrate in the reaction chamber, so that the generation rate and dissolution rate of the hydrate are determined according to the phase state information.

[0006] In a feasible embodiment, the temperature control component includes a temperature control component and a liquid nitrogen storage component, the liquid nitrogen storage component connects the hot and cold stage and the temperature control component; the liquid nitrogen storage component is used to store liquid nitrogen, and the temperature control component is used to control the liquid nitrogen storage component to release liquid nitrogen to the hot and cold stage to reduce the temperature of the hot and cold stage; the hot and cold stage transfers heat to the reaction chamber to reduce the temperature in the reaction chamber.

[0007] In a feasible embodiment, the hot and cold stage includes a heating component, and the heating component is used to generate heat to increase the temperature of the hot and cold stage; the hot and cold stage transfers heat to the reaction chamber to increase the temperature in the reaction chamber.

[0008] In a feasible embodiment, the pressure control device includes an injection component, a pressure control component and a high-pressure pipeline, the injection component is used to inject a first liquid into the reaction chamber, the high-pressure pipeline is used to connect the pressure control component and the reaction chamber, and a second liquid is stored in the high-pressure pipeline; the pressure control component is used to control the pressure of the reaction chamber by controlling the second liquid in the high-pressure pipeline.

[0009] In a feasible embodiment, the phase state acquisition device includes a Raman spectrometer, a laser and a processor, and the Raman spectrometer is connected to the processor; the laser is used to irradiate the hydrate in the reaction chamber to generate a Raman spectrum, the Raman spectrometer is used to collect the Raman spectrum, and the processor is used to determine the phase state information of the hydrate in the reaction chamber based on the Raman spectrum, and determine the generation rate and dissolution rate of the hydrate based on the phase state information.

[0010] In a second aspect, an embodiment of the present application provides a testing method, which is applied to a testing device, wherein the testing device includes a reaction chamber, wherein the reaction chamber is used to accommodate a reaction substance for generating a hydrate, and the reaction substance includes a reaction gas. The method includes: controlling the initial hydrate in the reaction chamber to dissociate into a target crystal; controlling the pressure in the reaction chamber to allow the target crystal to grow until a phase equilibrium state is reached to obtain a target hydrate; collecting first phase state information of the target crystal, and determining a generation rate of the target crystal based on the first phase state information, as well as determining a dissolution rate of the reaction gas in the reaction chamber, and determining a cage entry rate corresponding to the reaction gas based on the dissolution rate; controlling the pressure in the reaction chamber to dissociate the target hydrate; collecting second phase state information of the target hydrate, and determining the dissolution rate of the target hydrate based on the second phase state information.

[0011] In a feasible embodiment, the testing device includes a hot and cold stage, a liquid nitrogen storage component and a heating component, the hot and cold stage is used to load the reaction chamber, the liquid nitrogen storage component is connected to the hot and cold stage, and the controlling the initial hydrate in the reaction chamber to dissociate into the target crystal includes: determining a first temperature control rate and a second temperature control rate of the reaction chamber; determining a liquid nitrogen flux corresponding to the liquid nitrogen storage component according to the first temperature control rate, and determining heating information of the heating component according to the second temperature control rate; according to the liquid nitrogen flux, controlling the liquid nitrogen storage component to release liquid nitrogen to the hot and cold stage, cooling the reaction chamber according to the first temperature control rate, so that the initial hydrate is generated in the reaction chamber; according to the heating information, adjusting the temperature of the hot and cold stage through the heating component, heating the reaction chamber according to the second temperature control rate, so that the initial hydrate is dissociated into the target crystal.

[0012] In a feasible embodiment, controlling the pressure in the reaction chamber so that the target crystals grow until a phase equilibrium state is reached to obtain a target hydrate comprises: injecting a first liquid into the reaction chamber; controlling the pressure in the reaction chamber based on the first liquid so that the target crystals grow until a phase equilibrium state is reached to obtain a target hydrate.

[0013] In a feasible embodiment, the phase state acquisition device includes a Raman spectrometer, a laser and a processor. The acquisition of the first phase state information of the target crystal and determining the generation rate of the target crystal based on the first phase state information include: irradiating the target crystal in the reaction chamber with the laser to generate a Raman spectrum; acquiring the Raman spectrum through the Raman spectrometer; determining the first phase state information of the target crystal based on the Raman spectrum, and determining the generation rate of the target crystal based on the first phase state information.

[0014] In a feasible embodiment, the phase state acquisition device also includes a microscope, and the method also includes: determining the crystal video in the reaction chamber through the microscope; determining the growth rate of the target crystal in the crystal video based on a preset image recognition model, and determining the dissolution rate of the target hydrate in the crystal video.

[0015] In a feasible embodiment, determining the growth rate of the target crystal in the crystal video includes: based on the image recognition model, determining the crystal contour of the target crystal corresponding to each frame of the crystal image in the crystal video to obtain multiple crystal contours; and determining the growth rate of the target crystal based on the multiple crystal contours.

[0016] In a feasible embodiment, before determining the growth rate of the target crystal based on the multiple crystal contours, the method also includes: determining the structural information of the reaction chamber; if the structural information is a preset structure, determining the growth rate of the target crystal based on the multiple crystal contours; if the structural information is not the preset structure, determining multiple crystal volumes based on the multiple crystal contours, and determining the growth rate of the target crystal based on the multiple crystal volumes.

[0017] In the testing device of the present embodiment, when controlling the temperature in the reaction chamber, the reaction chamber is placed in a hot and cold stage, and the temperature of the reaction chamber is controlled according to the hot and cold stage. Since the heat transfer performance of the hot and cold stage is good, the temperature control accuracy and rate can be improved, and the hydrate formation and dissolution process can be accurately controlled, and the accuracy of determining the formation rate and dissolution rate can be improved. In addition, the present application collects the phase information of the hydrate in the reaction chamber according to the phase acquisition device, and then combines the temperature, pressure and other information in the reaction chamber to achieve quantitative measurement of the hydrate formation rate and dissolution rate. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] The following specific implementation manner will further illustrate the present invention in conjunction with the above-mentioned drawings.

[0019] Figure 1 It is a schematic diagram of the structure of the testing device provided in the embodiment of the present application.

[0020] Figure 2 It is a flow chart of the testing method provided in the embodiment of the present application.

[0021] Figure 3 It is a flow chart of the temperature control method for forming target crystals provided in an embodiment of the present application.

[0022] Figure 4 It is a flow chart of the method for determining growth rate and dissolution rate provided in the embodiment of the present application.

[0023] Figure 5 It is a schematic diagram of the growth process of the hydrate provided in the examples of the present application.

[0024] Figure 6 It is a schematic diagram of the hydrate generation rate provided in the examples of the present application.

[0025] Figure 7 It is a schematic diagram of the dissolution process of the hydrate provided in the examples of the present application.

[0026] Figure 8 4 is a graph showing the relationship between the crystal size of the hydrate and the heating rate provided in the examples of the present application.

[0027] Fig. 9 4 is a graph showing the relationship between the dissolution rate and the heating rate of the hydrate provided in the examples of the present application.

[0028] Fig.10 It is a schematic diagram of the dissolution process of the reaction gas during the hydrate growth process provided in the embodiment of the present application.

[0029] Fig.11 It is a schematic diagram of the formation process of the composite hydrate provided in the examples of the present application.

[0030] Description of component symbols: testing device 1, temperature control equipment 12, hot and cold stage 121, temperature control component 122, temperature control component 1221, liquid nitrogen storage component 1222, pressure control equipment 13, injection component 131, pressure control component 132, high pressure pipeline 133, pressure sensor 134, phase state acquisition equipment 14, Raman spectrometer 141, microscope 142, processor 143, adjustment equipment 15. DETAILED DESCRIPTION

[0031] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art of the present invention. The terms used in the specification of the present invention herein are only for the purpose of describing specific embodiments and are not intended to limit the present invention.

[0032] With the rapid development of the world's industry, the demand and consumption of traditional fossil energy have increased dramatically, and the problem of energy shortage has become one of the problems that every country has to face. Hydrate is a non-stoichiometric cage-shaped crystalline compound formed by gas and water under appropriate temperature and pressure conditions. Hydrates have attracted widespread attention from countries around the world due to their huge reserves and high energy density. Hydrate technology has broad application prospects in the fields of energy and climate, such as hydrate-based carbon dioxide storage, hydrate-based seawater desalination, hydrate-based gas separation, etc. Hydrate technology is expected to become a key technology to meet energy challenges and climate change.

[0033] In the foundation of hydrate application technology, hydrate growth and dissolution are important research parts. In the related technologies, there are shortcomings in the study of hydrate formation and dissolution, such as difficulty in quantitatively measuring the formation rate and dissolution rate of hydrates, which hinders the widespread application of hydrate technology in industrialization. For example, phase equilibrium research determines whether hydrates can be formed by analyzing the phase state of hydrates under specific temperature and pressure conditions. It is a macroscopic qualitative description of the hydrate formation and dissolution process based on temperature and pressure changes, and cannot achieve a dynamic description of the hydrate formation and dissolution process, making it difficult to quantitatively measure key parameters (such as formation rate and dissolution rate).

[0034] In view of this, it is necessary to provide a testing device and a testing method that can achieve quantitative measurement of the formation rate and dissolution rate of hydrates.

[0035] Figure 1 1 is a schematic diagram of the structure of the test device provided in the embodiment of the present application. The test device 1 is used to quantitatively measure the formation rate and dissolution rate of hydrates. Figure 1 As shown, the testing device 1 includes a reaction chamber ( Figure 1The reaction chamber is used to contain the reaction substances that generate hydrates. The reaction substances may include reaction gases and reaction liquids. The reaction gases and reaction liquids may be determined according to the generation requirements of hydrates and are not limited here. The temperature control device 12 is used to control the temperature in the reaction chamber, and the pressure control device 13 is used to control the pressure in the reaction chamber. The phase state acquisition device 14 is used to collect the phase state information of the hydrates in the reaction chamber, and determine the generation rate and dissolution rate of the hydrates based on the phase state information.

[0036] In some embodiments, the reaction chamber may include a micrometer-level high-pressure molten silicon capillary tube, and the size of the molten silicon capillary tube may be set according to actual needs. For example, the diameter of the molten silicon capillary tube may be 100-300 micrometers, which is not limited here. One end of the molten silicon capillary tube is welded using a hydrogen flame, and the other end is connected to the pressure control device 13. In some embodiments, an observation window may be provided on the reaction chamber, through which the morphological characteristics, growth process and dissolution process of the hydrate may be observed.

[0037] In some embodiments, the temperature control device 12 includes a hot and cold stage 121 and a temperature control component 122. The hot and cold stage 121 is disposed on the phase acquisition device 14 and is used to load the reaction chamber. The temperature control component 122 is connected to the hot and cold stage 121 and is used to control the temperature of the reaction chamber according to the hot and cold stage 121.

[0038] In some embodiments, the temperature control device 12 also includes an interactive interface, which is used to realize the interaction between the user and the temperature control device 12. Exemplarily, the user can output the temperature control rate to the temperature control device 12 through the interactive interface, so that the temperature control device 12 realizes the temperature control of the reaction chamber according to the temperature control rate. Among them, the temperature control rate represents the rate at which the temperature in the reaction chamber rises or falls. The temperature control rate may include a first temperature control rate and a second temperature control rate, the first temperature control rate is used to describe the temperature in the reaction chamber to decrease at a specified rate, and the second temperature control rate is used to describe the temperature in the reaction chamber to increase at a specified rate. Among them, the first temperature control rate and the second temperature control rate can be set according to actual needs, and are not limited here.

[0039] In some embodiments, the temperature control device 12 may also include a temperature sensor ( Figure 1 (not shown), a high-precision temperature sensor is connected to the reaction chamber to monitor the temperature in the reaction chamber in real time.

[0040] In some embodiments, the hot and cold stage 121 may include a silver stage ( Figure 1 not shown) with a silver cap ( Figure 1 The silver platform (not shown) can be made of a material with good thermal conductivity (such as silver or copper). The silver platform is used to load the reaction chamber and heat or cool the reaction chamber through a conduction mechanism. The silver cover is used to cover the silver platform to protect the reaction chamber from interference from the external environment, for example, to prevent impurities from entering or to reduce the impact of ambient temperature fluctuations on the reaction chamber.

[0041] In some embodiments, the temperature control component 122 includes a temperature control component 1221 and a liquid nitrogen storage component 1222, wherein the liquid nitrogen storage component 1222 connects the hot and cold stage 121 and the temperature control component 1221. For example, one end of the liquid nitrogen storage component 1222 is connected to the temperature control component 1221, and the other end is connected to the silver plate of the hot and cold stage 121. The liquid nitrogen storage component 1222 is used to store liquid nitrogen; the temperature control component 1221 is used to control the liquid nitrogen storage component 1222 to release liquid nitrogen to the hot and cold stage 121, thereby reducing the temperature in the silver plate of the hot and cold stage 121; the silver plate transfers heat to the reaction chamber, thereby reducing the temperature in the reaction chamber.

[0042] In some embodiments, the hot and cold stage 121 further includes a heating component ( Figure 1 (not shown in the figure), the heating component may include a high-voltage resistor. The heating component is used to generate heat to increase the temperature of the silver stage in the hot and cold stage 121; the silver stage transfers heat to the reaction chamber to increase the temperature in the reaction chamber. In the present application, the hot and cold stage 121 is used as a temperature conduction medium. Due to the good temperature conduction effect of the hot and cold stage 121, the temperature control accuracy and rate in the reaction chamber are high. The temperature control accuracy can reach 0.01K, and the temperature control rate can reach 0.01K / h, so that the formation conditions of hydrates can be quickly achieved and the formation rate of hydrates can be accelerated; in addition, due to the high temperature control accuracy, the embodiments of the present application can also control the formation of hydrates into single crystals or polycrystalline and other states, making the growth process of hydrates more controllable.

[0043] In some embodiments, the pressure control device 13 includes an injection component 131, a pressure control component 132 and a high-pressure pipeline 133. The injection component 131 is used to inject a first liquid into the reaction chamber. The first liquid is used to seal the reaction chamber. The first liquid may be liquid mercury. The high-pressure pipeline 133 is used to connect the pressure control component 132 and the reaction chamber. The second liquid is stored in the high-pressure pipeline 133. The second liquid is used as a pressure transmission medium. The second liquid may include ultrapure water. The pressure control component 132 is used to control the pressure of the reaction chamber by controlling the second liquid in the high-pressure pipeline 133. The embodiment of the present application is based on the second liquid for liquid pressure transmission, which can improve the pressure control accuracy, and the pressure control accuracy can reach 0.1psi.

[0044] In some embodiments, the injection assembly 131 is a detachable assembly, and the number of injection assemblies 131 can be multiple, and the first liquid stored in each injection assembly 131 can be different. For example, there are two injection assemblies, recorded as injection assembly A and injection assembly B, wherein injection assembly A can be connected to the reaction chamber, and pure water, electrolyte or promoter solution (for example, tetrahydrofuran (THF), tetrahydrofuran, 1,4-dioxane and acetone) and other liquids required for generating hydrates are injected into the reaction chamber; the injection assembly A is removed from the reaction chamber, the injection assembly B is connected to the reaction chamber, and mercury liquid is injected into the reaction chamber. The embodiment of the present application sets the injection assembly 131 as a detachable assembly, so that the injection assembly 131 can be disassembled according to actual needs, and the required liquid can be input into the reaction chamber, thereby improving the flexibility of the test device 1.

[0045] In some embodiments, the pressure control device 13 may further include a pressure sensor 134, which may be connected to the reaction chamber and monitor the pressure in the reaction chamber in real time. The embodiment of the present application can monitor key parameters (e.g., pressure) in the growth and dissolution process of hydrates in real time by providing a high-precision pressure sensor, thereby increasing the frequency of data acquisition and enhancing the accuracy and reliability of the experimental results.

[0046] In some embodiments, the pressure control device 13 further includes a valve assembly ( Figure 1 (not shown in the figure), the type of valve assembly can be set according to actual needs. For example, the valve assembly can include a three-way valve, a four-way valve, etc. By setting the valve assembly, the injection assembly 131, the high-pressure pipeline 133, the pressure sensor 134 and other equipment can be connected to the reaction chamber at the same time.

[0047] In some embodiments, the pressure control device 13 may also include a gas storage tank ( Figure 1(not shown), a gas storage tank is connected to the reaction chamber. The reaction gas required for generating hydrates can be stored in the gas storage tank, for example, carbon dioxide can be stored in the gas storage tank. By opening the gas storage tank, the reaction gas in the gas storage tank can be transferred to the reaction chamber, so that hydrates can be generated in the reaction chamber.

[0048] In some embodiments, the phase state acquisition device 14 includes a Raman spectrometer 141, a laser ( Figure 1 The laser is used to irradiate the hydrate in the reaction chamber to generate a Raman spectrum, the Raman spectrometer 141 is used to collect the Raman spectrum, and the processor 143 is used to determine the phase information of the hydrate in the reaction chamber based on the Raman spectrum, and determine the generation rate and dissolution rate of the hydrate based on the phase information. In some embodiments, the dissolution rate of the reaction gas in the reaction chamber can also be determined based on the Raman spectrum, and the corresponding cage entry rate of the reaction gas can be determined based on the dissolution rate. The embodiment of the present application identifies the structure of the hydrate and the guest molecules (for example, gas molecules of the reaction gas) by collecting the Raman spectrum of the hydrate under different temperature and pressure conditions during the phase change process, and can perform in-situ real-time and non-invasive monitoring of the growth process of the hydrate at the molecular scale.

[0049] In some embodiments, the phase state acquisition device 14 also includes a microscope 142, which is used to collect crystal videos in the reaction chamber, observe local details of hydrate nucleation, growth and dissolution processes in the X-axis and Y-axis directions in the reaction chamber, so that the phase state acquisition device 14 can analyze and calculate the generation rate and dissolution rate of the hydrate.

[0050] In some embodiments, the testing device 1 further includes an adjustment device 15, and the adjustment device 15 is used to load the pressure control device 13. For example, the adjustment device 15 is used to load the valve assembly in the pressure control device 13, and adjust the position of the valve assembly according to a preset direction to drive the reaction chamber in the hot and cold stage 121 to move so that the reaction chamber is within the observation field of the laser. In some embodiments, the preset direction of the adjustment device 15 may include the X-axis direction, the Y-axis direction, and the Z-axis direction.

[0051] In some embodiments, the testing device 1 may also include a preset environmental monitoring sensor ( Figure 1(not shown), the environmental monitoring sensor is connected to the reaction chamber to monitor the environmental parameters of the hydrate in the reaction chamber. The environmental parameters can be set according to actual needs. For example, the environmental parameters can be the intensity and frequency of the electromagnetic field, and the corresponding environmental monitoring sensor can be an electromagnetic sensor. By setting the electromagnetic sensor, the influence of the intensity and frequency of the electromagnetic field on the formation and dissolution process of the hydrate can be monitored. For another example, the environmental parameter can be the flow state in the reaction chamber, and the corresponding environmental monitoring sensor can be a flow sensor. By setting the flow sensor, the influence of the flow state of the liquid in the reaction chamber on the formation and dissolution process of the hydrate can be monitored.

[0052] In some embodiments, the testing device 1 may further include a mass spectrometer ( Figure 1 (not shown in the figure), a mass spectrometer is used to monitor the chemical composition of the hydrate in the reaction chamber.

[0053] In some embodiments, the specific testing process of the testing device 1 may be as follows: After the reaction chamber is cleaned and dried, the liquid required for generating hydrate is injected into the reaction chamber through the injection assembly 131 in the pressure control device 13 .

[0054] The gas storage tank is opened to transmit the reaction gas in the gas storage tank to the reaction chamber, and the liquid required for generating hydrate in the reaction chamber is pushed to one end of the reaction chamber.

[0055] The first liquid, mercury liquid, is injected into the reaction chamber through the injection assembly 131 in the pressure control device 13, so that the reaction chamber is closed.

[0056] The reaction chamber is placed in the silver stage of the hot and cold stage 121 and covered with a silver cover; then, the movement of the adjustment device 15 is adjusted so that the reaction chamber in the hot and cold stage 121 is within the observation field of the laser, so as to accurately and quickly collect the formation and dissolution process of the hydrate in the reaction chamber. The preset direction may include the X-axis direction, the Y-axis direction and the Z-axis direction.

[0057] Under the initial conditions, the temperature and pressure in the test device 1 are maintained outside the preset hydrate phase boundary, the temperature of the reaction chamber under the initial conditions is recorded as the initial temperature, and the pressure of the reaction chamber under the initial conditions is recorded as the initial pressure. The hydrate phase boundary can be the physical boundary of hydrate formation under specific temperature and pressure conditions. For example, under specific temperature and pressure conditions, the gas molecules of the reaction gas (such as methane, carbon dioxide) can combine with the water molecules of the reaction liquid to form a stable hydrate crystal structure. By maintaining the temperature and pressure in the test device 1 outside the preset hydrate phase boundary, it can be ensured that there is no hydrate crystal in the reaction chamber at the beginning of the test.

[0058] The temperature control component 1221 controls the liquid nitrogen storage component 1222 to release liquid nitrogen to the hot and cold stage 121, thereby reducing the temperature of the silver stage in the hot and cold stage 121; the silver stage transfers heat to the reaction chamber, thereby reducing the initial temperature in the reaction chamber to below the first preset temperature, thereby promoting the formation of hydrates in the reaction chamber. The first preset temperature can be set according to actual needs and is not limited here. In some embodiments, a temperature sensor is used to monitor the temperature in the reaction chamber in real time.

[0059] The laser is turned on, and the laser is used to irradiate the hydrate in the reaction chamber to generate a Raman spectrum. The Raman spectrometer 141 is used to collect the Raman spectrum, and the processor 143 is used to determine whether the hydrate in the reaction chamber (for the convenience of description, this application also refers to "initial hydrate") is generated based on the Raman spectrum. Among them, Raman spectroscopy is a non-destructive analysis technology that obtains chemical structure information of a substance by analyzing the wavelength change of scattered light. For hydrates, the Raman spectrum will show characteristic peaks related to the combination of water molecules and gas molecules. For example, methane hydrate will show characteristic peaks of the interaction between methane molecules and water molecules in the Raman spectrum, and each substance has its own unique Raman spectrum characteristic peaks, which correspond to specific vibration modes of the molecules of the substance. In some embodiments, in the test device 1, it can be determined whether the initial hydrate is generated by detecting whether the characteristic peak appears in the Raman spectrum. When the characteristic peak appears in the Raman spectrum, it is determined that the initial hydrate is generated; if the characteristic peak does not appear in the Raman spectrum, it is determined that the initial hydrate is not generated.

[0060] After the initial hydrate in the reaction chamber is formed, heat is generated by the heating component to increase the temperature of the silver stage in the hot and cold stage 121, and the silver stage transfers heat to the reaction chamber to increase the first preset temperature in the reaction chamber to the second preset temperature. Among them, the second preset temperature can be set according to actual needs and is not limited here. When the temperature in the reaction chamber is raised from the first preset temperature to the second preset temperature, the initial hydrate in the reaction chamber gradually dissociates. In some embodiments, a temperature sensor is used to monitor the temperature in the reaction chamber in real time.

[0061] When the initial hydrate dissociates into a small amount of crystal particles, the temperature control component 1221 controls the liquid nitrogen storage component 1222 to release liquid nitrogen to the hot and cold table 121, thereby reducing the temperature in the silver table in the hot and cold table 121, and the silver table transfers heat to the reaction chamber, thereby reducing the second preset temperature in the reaction chamber to below the third preset temperature, so that the initial hydrate in the reaction chamber dissociates into target crystals, thereby avoiding complete dissolution of the initial hydrate. Among them, the third preset temperature can be set according to actual needs and is not limited here. The target crystals may include single crystals and polycrystalline. In some embodiments, a temperature sensor is used to monitor the temperature in the reaction chamber in real time.

[0062] When the initial hydrate in the reaction chamber dissociates into the target crystal, the pressure in the reaction chamber is increased by the pressure control component 132, and the pressure in the reaction chamber is monitored in real time by the pressure sensor 134. When the pressure in the reaction chamber increases, the target crystal begins to grow. At a certain temperature (for example, a third preset temperature), the pressure in the reaction chamber is continuously increased by the pressure search method until the target crystal neither grows nor dissociates and reaches a phase equilibrium state, and the hydrate in the reaction chamber is used as the target hydrate.

[0063] In the process of the target crystal growing into the target hydrate, the laser is turned on, the target crystal in the reaction chamber is irradiated with the laser to generate a Raman spectrum, the Raman spectrometer 141 is used to collect the Raman spectrum, the processor 143 is used to determine the first phase information of the target crystal in the reaction chamber according to the Raman spectrum, and the generation rate of the target crystal is determined according to the first phase information. In some embodiments, the dissolution rate of the reaction gas in the reaction chamber can also be determined according to the Raman spectrum, and the corresponding cage entry rate of the reaction gas can be determined according to the dissolution rate. In some embodiments, the generation rate of the target crystal and the dynamic change process of the temperature and pressure in the reaction chamber can also be quantitatively measured to achieve quantitative measurement of the hydrate generation rate. In other embodiments, the generation size of the target crystal and the dynamic change process of the temperature and pressure in the reaction chamber can also be quantitatively measured to achieve quantitative measurement of the hydrate generation size. After determining the generation rate of the target crystal, the pressure in the reaction chamber is reduced by opening the pressure relief valve on the reaction chamber, and the pressure in the reaction chamber is monitored in real time by the pressure sensor 134. When the pressure in the reaction chamber decreases, the target hydrate begins to dissociate; the pressure in the reaction chamber continues to decrease until the dissociation of the target hydrate is complete.

[0064] During the dissociation process of the target hydrate, the laser is turned on, and the target hydrate in the reaction chamber is irradiated with the laser to generate a Raman spectrum, and the Raman spectrometer 141 is used to collect the Raman spectrum, and the processor 143 is used to determine the second phase information of the target hydrate in the reaction chamber based on the Raman spectrum, and the dissolution rate of the target hydrate is determined based on the second phase information. In some embodiments, the dissolution rate of the target crystal and the dynamic change process of the temperature and pressure in the reaction chamber can also be quantitatively measured to achieve quantitative measurement of the dissolution rate of the hydrate. In other embodiments, the dissolution size of the target crystal and the dynamic change process of the temperature and pressure in the reaction chamber can also be quantitatively measured to achieve quantitative measurement of the dissolution size of the hydrate.

[0065] In the testing device provided in the embodiment of the present application, when controlling the temperature in the reaction chamber, the reaction chamber is placed in a hot and cold stage, and the temperature of the reaction chamber is controlled according to the hot and cold stage. Since the heat transfer performance of the hot and cold stage is good, the temperature control accuracy and rate can be improved, and the hydrate formation and dissolution process can be accurately controlled, and the accuracy of determining the formation rate and dissolution rate can be improved; in addition, the present application can control the temperature and pressure information in the reaction chamber according to the temperature control device and the pressure control device, and can quantitatively measure the temperature and pressure information in the reaction chamber, and then collect the phase state information of the hydrate in the reaction chamber according to the phase state collection device, and can realize quantitative measurement of the hydrate formation rate and dissolution rate according to the phase state information of the hydrate.

[0066] Figure 2 is a flow chart of a test method provided in an embodiment of the present application, and the test method is applied to a test device (for example, Figure 1 Test setup 1). Figure 2 As shown, the following steps are included: S11, controlling the initial hydrate in the reaction chamber to dissociate into target crystals.

[0067] In at least one embodiment of the present application, the target crystal can be set according to the test requirements. For example, the target crystal can include a single crystal and a polycrystalline. The embodiment of the present application achieves precise control of the state of the hydrate in the reaction chamber by accurately controlling the temperature and pressure in the reaction chamber. The embodiment of the present application is described by taking the target crystal as a single crystal as an example. The single crystal can include an initial hydrate that decomposes under specific conditions, releases water molecules therein, and rearranges into a single crystal structure that does not contain water molecules. The temperature in the reaction chamber can be adjusted by a temperature control device and a heating component, so that an initial hydrate is generated in the reaction chamber, and then the initial hydrate is dissociated into a target crystal.

[0068] S12, controlling the pressure in the reaction chamber so that the target crystal grows until a phase equilibrium state is reached to obtain a target hydrate.

[0069] In at least one embodiment of the present application, when the initial hydrate in the reaction chamber dissociates into target crystals, controlling the pressure in the reaction chamber so that the target crystals grow until a phase equilibrium state is reached to obtain the target hydrate comprises: controlling the pressure of the reaction chamber based on a second liquid so that the target crystals grow until a phase equilibrium state is reached to obtain the target hydrate.

[0070] In some embodiments, the pressure in the reaction chamber is increased by the pressure control assembly, and the pressure in the reaction chamber is monitored in real time by a pressure sensor. When the pressure in the reaction chamber increases, the target crystal begins to grow. At a certain temperature, the pressure in the reaction chamber is continued to be increased by a pressure search method until the target crystal neither grows nor dissociates, and a phase equilibrium state is reached, and the hydrate in the reaction chamber is used as the target hydrate. The embodiment of the present application can accelerate the formation rate of hydrates by accurately controlling the pressure in the reaction chamber at a constant temperature, significantly reducing the test time and improving the test efficiency.

[0071] S13, collecting the first phase information of the target crystal, and determining the generation rate of the target crystal according to the first phase information, and determining the dissolution rate of the reaction gas in the reaction chamber, and determining the corresponding cage entry rate of the reaction gas according to the dissolution rate.

[0072] In at least one embodiment of the present application, during the growth of the target crystal into the target hydrate, the laser is turned on, the target crystal in the reaction chamber is irradiated with the laser to generate a Raman spectrum, the Raman spectrometer is used to collect the Raman spectrum, the processor is used to determine the first phase state information of the target crystal in the reaction chamber based on the Raman spectrum, and the generation rate of the target crystal is determined based on the first phase state information.

[0073] In some embodiments, the first phase state information can be used to describe the existence form of the target crystal under specific temperature and pressure conditions. For example, the first phase state information can be the concentration information of the gas molecules in the hydrate. In some embodiments, the concentration of the gas molecules in the hydrate can be quantitatively analyzed by the intensity of the corresponding peak of the Raman spectrum. For example, the corresponding relationship between the peak intensity and the concentration of the gas molecules can be established in advance. By querying the corresponding relationship, the concentration of the corresponding gas molecules can be determined according to the peak intensity of the gas molecules in the Raman spectrum.

[0074] In some embodiments, when the target crystal forms a hydrate in a solution, it will bind a certain amount of gas molecules. By monitoring the gas concentration in the hydrate by Raman spectroscopy, the size of the hydrate can be determined. By monitoring the change in the gas concentration in the hydrate by Raman spectroscopy, the growth rate of the hydrate can be determined. For example, if the concentration of gas molecules in the hydrate increases significantly within a certain period of time, this indicates that the hydrate is rapidly generating and capturing gas molecules. In some embodiments, the corresponding relationship between the concentration of gas molecules and the hydrate growth rate can be pre-set, and by querying the corresponding relationship, the generation rate of the hydrate can be determined.

[0075] In some embodiments, in the Raman spectrum, the peak intensity ratio of the guest molecule (such as a gas molecule) and the water molecule can reflect the relative content of the gas molecule in the hydrate. By monitoring the change of the ratio in real time, the process and mechanism of the guest molecule entering the hydrate cage can be determined. For example, when the peak intensity of the guest molecule increases relative to the peak intensity of the water molecule, it indicates that more guest molecules are incorporated into the hydrate structure.

[0076] In some embodiments, while collecting the first phase state information of the target crystal, the method also includes: determining environmental information in the reaction chamber, wherein the environmental information includes at least one of the temperature and pressure in the reaction chamber; based on the environmental information and the first phase state information, a quantitative measurement relationship between the environmental information and the generation rate of the target crystal can be determined, and based on the environmental information and the first phase state information, a quantitative measurement relationship between the environmental information and the generation size of the target crystal can be determined.

[0077] In some embodiments, the dissolution rate of the reaction gas in the reaction chamber can also be quantitatively analyzed by the intensity change information of the corresponding spectral peak of the Raman spectrum. The corresponding relationship between the dissolution rate of the reaction gas and the corresponding cage entry rate of the reaction gas in the hydrate formation process is preset, and by querying the corresponding relationship, the cage entry rate corresponding to the determined dissolution rate can be obtained. Among them, the cage entry rate may include the rate at which the reaction gas enters the hydrate cage. The greater the cage entry rate, the greater the hydrate generation rate; the smaller the cage entry rate, the smaller the hydrate generation rate.

[0078] The embodiment of the present application can realize real-time, non-invasive monitoring of the growth process of the target crystal by collecting Raman spectra of the hydrate under different temperature and pressure conditions during the phase change process. In addition, the embodiment of the present application can realize quantitative measurement of information such as the generation rate and generation size of the hydrate by real-time measurement of environmental information such as temperature and pressure in the reaction chamber.

[0079] S14, controlling the pressure in the reaction chamber to dissociate the target hydrate.

[0080] In at least one embodiment of the present application, after determining the generation rate of the target crystal, the pressure in the reaction chamber is reduced by opening the pressure relief valve on the reaction chamber, and the pressure in the reaction chamber is monitored in real time using a pressure sensor. When the pressure in the reaction chamber is reduced, the target hydrate begins to dissociate; the pressure in the reaction chamber is continuously reduced until the dissociation of the target hydrate is completed.

[0081] S15, collecting second phase information of the target hydrate, and determining the dissolution rate of the target hydrate according to the second phase information.

[0082] In at least one embodiment of the present application, during the dissociation process of the target hydrate, the laser is turned on, the target hydrate in the reaction chamber is irradiated with the laser to generate a Raman spectrum, the Raman spectrometer is used to collect the Raman spectrum, the processor is used to determine the second phase information of the target hydrate in the reaction chamber based on the Raman spectrum, and the dissolution rate of the target hydrate is determined based on the second phase information.

[0083] In some embodiments, the second phase state information can be used to describe the existence form of the target hydrate under specific temperature and pressure conditions. For example, the second phase state information can be the concentration information of the gas molecules in the target hydrate. In some embodiments, the Raman spectrum can quantitatively analyze the concentration of the gas molecules in the hydrate by the intensity of the spectrum peak. For example, the corresponding relationship between the spectrum peak intensity and the concentration of the gas molecules can be established in advance. By querying the corresponding relationship, the concentration of the corresponding gas molecules can be determined according to the spectrum peak intensity of the gas molecules in the Raman spectrum.

[0084] In some embodiments, when the target hydrate begins to dissociate, a certain amount of gas molecules will be released. By monitoring the gas concentration in the hydrate by Raman spectroscopy, the solubility size of the hydrate can be determined, and the solubility size refers to the size of the hydrate after dissolution. By monitoring the concentration change of gas molecules in the target hydrate by Raman spectroscopy, the dissolution rate of the target hydrate can be determined. Exemplarily, if the concentration of gas molecules in the target hydrate decreases significantly within a certain period of time, this indicates that the target hydrate is rapidly dissociating and releasing gas molecules. In some embodiments, the corresponding relationship between the concentration of gas molecules and the dissolution rate of hydrates can be pre-set, and by querying the corresponding relationship, the dissolution rate of the target hydrate can be determined.

[0085] In some embodiments, while collecting the second phase information of the target hydrate, the method further includes: determining environmental information in the reaction chamber, wherein the environmental information includes at least one of the temperature and pressure in the reaction chamber; based on the environmental information and the second phase information, the quantitative measurement relationship between the environmental information and the dissolution rate of the target crystal can be determined, and based on the environmental information and the second phase information, the quantitative measurement relationship between the environmental information and the dissolution size of the target crystal can be determined. The embodiments of the present application can achieve quantitative measurement of information such as the dissolution rate and dissolution size of the hydrate by measuring environmental information such as the temperature and pressure in the reaction chamber in real time.

[0086] In the testing method provided in the embodiment of the present application, the temperature and pressure information in the reaction chamber are determined based on the temperature control device and the pressure control device, and the phase information of the hydrate in the reaction chamber is collected based on the phase acquisition device, so that the formation rate and dissolution rate of the hydrate can be quantitatively measured.

[0087] In at least one embodiment of the present application, the temperature in the reaction chamber can be adjusted by a temperature control device and a heating component, so that an initial hydrate is generated in the reaction chamber, and then the initial hydrate is dissociated into target crystals. Figure 3 is a flow chart of a temperature control method for forming a target crystal provided in an embodiment of the present application, such as Figure 3 As shown, the following steps are included: S21, determining a first temperature control rate and a second temperature control rate of the reaction chamber.

[0088] In at least one embodiment of the present application, the first temperature control rate is used to describe that the temperature in the reaction chamber decreases at a specified rate, so that an initial hydrate is generated in the reaction chamber; the second temperature control rate is used to describe that the temperature in the reaction chamber increases at a specified rate, so that the initial hydrate in the reaction chamber dissociates into target crystals. The first temperature control rate and the second temperature control rate can be set according to actual needs and are not limited here.

[0089] S22: determining a liquid nitrogen flux corresponding to the liquid nitrogen storage component according to the first temperature control rate, and determining heating information of the heating component according to the second temperature control rate.

[0090] In at least one embodiment of the present application, a correspondence between the first temperature control rate and the liquid nitrogen flux may be preset, and the liquid nitrogen flux may be determined by querying the correspondence, wherein the liquid nitrogen flux may include a liquid nitrogen discharge amount and a liquid nitrogen discharge rate.

[0091] In some embodiments, a correspondence between the second temperature control rate and the heating information may be preset, and the heating information may be determined by querying the correspondence, wherein the heating information may include a heating duration.

[0092] S23, according to the liquid nitrogen flux, controlling the liquid nitrogen storage component to release liquid nitrogen to the hot and cold stage, and cooling the reaction chamber according to the first temperature control rate, so that the initial hydrate is generated in the reaction chamber.

[0093] In at least one embodiment of the present application, the temperature control component controls the liquid nitrogen storage component to release liquid nitrogen to the hot and cold stages according to the liquid nitrogen flux, thereby reducing the temperature in the silver stage in the hot and cold stages, and the silver stage transfers heat to the reaction chamber, and reduces the initial temperature in the reaction chamber according to the first temperature control rate, thereby promoting hydrate formation in the reaction chamber.

[0094] S24, adjusting the temperature of the hot and cold stage by the heating component according to the heating information, and heating the reaction chamber according to the second temperature control rate, so that the initial hydrate dissociates into the target crystal.

[0095] In at least one embodiment of the present application, after the hydrate in the reaction chamber is formed, the heating component generates heat to increase the temperature of the silver stage in the hot and cold stage, and the silver stage transfers heat to the reaction chamber to increase the temperature in the reaction chamber. When the temperature in the reaction chamber is increased at the second temperature control rate, the initial hydrate in the reaction chamber gradually dissociates.

[0096] In some embodiments, when the initial hydrate dissociates into a small amount of crystal particles, the temperature control component controls the liquid nitrogen storage component to release liquid nitrogen to the hot and cold stages, thereby reducing the temperature in the silver stage in the hot and cold stages, and the silver stage transfers heat to the reaction chamber, thereby reducing the temperature in the reaction chamber, so that the initial hydrate in the reaction chamber dissociates into target crystals, thereby avoiding complete dissolution of the initial hydrate.

[0097] The embodiment of the present application is based on the temperature control device that can accurately control the temperature in the reaction chamber, so that the initial hydrate can dissociate into the target crystal that meets the test requirements, making the hydrate generation and dissociation process highly controllable; in addition, the embodiment of the present application can deeply understand the physicochemical mechanism of hydrate formation, including nucleation, growth and decomposition processes, by studying the generation and dissolution rate of a single hydrate crystal.

[0098] In at least one embodiment of the present application, the phase state acquisition device further includes a microscope, which is used to collect crystal videos in the reaction chamber. By performing image processing on the crystal videos and analyzing the crystal images of the crystals at different time points, it is possible to determine the generation rate and dissolution rate of the crystals. Figure 4 is a flow chart of a method for determining growth rate and dissolution rate provided in an embodiment of the present application, such as Figure 4 As shown, the following steps are included: S31, determining the crystal video in the reaction chamber through the microscope.

[0099] In at least one embodiment of the present application, the growth process of the target crystal and the dissolution process of the target hydrate in the reaction chamber can be recorded regularly by an image acquisition device such as a microscope to obtain a crystal video.

[0100] In some embodiments, after determining the crystal video in the reaction chamber by the microscope, the method further comprises: preprocessing the crystal video. The preprocessing may include but is not limited to denoising, contrast enhancement, and background removal. By preprocessing the crystal video, the video quality can be improved, thereby improving the accuracy of determining the growth rate and dissolution rate.

[0101] S32, based on a preset image recognition model, determining the growth rate of the target crystal in the crystal video, and determining the dissolution rate of the target hydrate in the crystal video.

[0102] In at least one embodiment of the present application, the image recognition model is used to identify the outline of the crystal in the crystal video, the input data of the image recognition model is the crystal video or multiple frames of crystal images, and the output data is the crystal outline sorted according to the time series. In other embodiments, the input data of the image recognition model is a single frame of crystal image, and the output data is the crystal outline. The image recognition model may include but is not limited to convolutional neural network models such as LeNet-5, AlexNet, VGGNet, ResNet, Inception, or supervised learning models such as support vector machines, and the present application does not limit this.

[0103] In some embodiments, when training an image recognition model, the method further includes: obtaining an initial crystal image set; preprocessing the initial crystal image set to obtain a target crystal image set; training the image recognition model based on the target crystal image set to obtain a trained image recognition model. Preprocessing may include rotation and scaling processing, random cropping processing, and color transformation processing. By randomly rotating or scaling the crystal image, the image recognition model's ability to recognize crystals of different angles and sizes can be enhanced; by randomly cropping the crystal image, the effects of different focal lengths and shooting positions on the model output can be simulated, thereby improving the accuracy of the model output; by randomly adjusting the brightness, contrast, color, etc. of the crystal image, it can adapt to changes in illumination under different experimental conditions, thereby improving the accuracy of the model output.

[0104] In some embodiments, since the growth and dissolution process of the crystal follows certain physical laws, for example, the shape of the crystal must satisfy symmetry and edge smoothness, and for example, the growth and dissolution of the crystal is a continuous process, and the growth and dissolution of the crystal must conform to the actual growth and dissolution trend. The embodiment of the present application incorporates physical laws into the training process of the image recognition model. The output of the image recognition model is constrained by physical priors to improve the physical rationality of the model output. In some embodiments, when training the image recognition model, the method also includes: obtaining an initial crystal image set; marking the outline frame of the crystal in the initial crystal image set to obtain a target crystal image set; obtaining an initial loss function, and adding penalty terms of shape constraints and time series constraints to the initial loss function to obtain a target loss function; training the image recognition model based on the crystal image set and the target loss function to obtain a trained image recognition model. The implementation of the present application can reduce the model's excessive sensitivity to noise or background interference by introducing geometric feature constraints (such as edge smoothness, symmetry, etc.) of the crystal shape during the training of the image recognition model; and the present application introduces time series information for constraints during the training of the image recognition model, so that the predicted crystal contour changes in time conform to the actual growth and dissolution trends.

[0105] In some embodiments, the image recognition model is a multi-task model, and the crystal contour extraction and region recognition are used as different subtasks to train the multi-task model. The above method can improve the overall performance of the image recognition model by sharing representation information to simultaneously learn multiple related tasks. In some embodiments, the subtasks of the image recognition model include contour extraction tasks and region recognition tasks, wherein the contour extraction task is used to extract the edge contour of the crystal and identify the complete shape of the crystal; the region recognition task is used to identify the specific area where the crystal grows or dissolves, and assist in understanding the rate change. Each task has corresponding training data, for example, the input data corresponding to the contour extraction task is a crystal video or crystal image, and the output data is the crystal contour; the input data corresponding to the region recognition task is a crystal video or crystal image, and the output data is a specific area where the crystal grows or dissolves.

[0106] In some embodiments, the image recognition model is called to process the crystal video of the target crystal during the growth process, and the crystal contour of the target crystal can be obtained, and then the growth rate of the target crystal is determined based on the crystal contour of the target crystal at different time points. Similarly, the image recognition model is called to process the crystal video of the target hydrate during the dissolution process, and the crystal contour of the target hydrate can be obtained, and then the dissolution rate of the target hydrate can be determined based on the crystal contour of the target hydrate at different time points.

[0107] In the above-mentioned testing method provided in the embodiment of the present application, by continuously collecting and analyzing crystal images, real-time monitoring of crystal growth and dissolution can be achieved, thereby improving the timeliness of determining the growth rate and dissolution rate; and the present application processes crystal videos through image recognition models, thereby accurately identifying the complex morphology of crystals and improving the accuracy of determining the crystal growth rate and dissolution rate.

[0108] In at least one embodiment of the present application, by comparing the change information of the crystal contour at different time points, the growth rate or dissolution rate of the crystal can be determined. The determination of the growth rate of the target crystal in the crystal video includes: based on the image recognition model, determining the crystal contour of the target crystal corresponding to each frame of the crystal image in the crystal video, and obtaining multiple crystal contours; based on the multiple crystal contours, determining the growth rate of the target crystal. Among them, the crystal contour can be measured by a geometric measurement tool, and the geometric measurement tool can include a vernier caliper, an inner diameter measuring instrument, a laser measuring instrument, etc.

[0109] In at least one embodiment of the present application, the reaction chamber can be a two-dimensional plane or a three-dimensional structure. When the reaction chamber is a two-dimensional plane, the growth rate of the target crystal and the dissolution rate of the target hydrate can be determined based on the crystal contour; when the reaction chamber is a three-dimensional structure, the crystal contour needs to be processed accordingly, and then the growth rate of the target crystal and the dissolution rate of the target hydrate are determined. The embodiment of the present application is described by taking the determination of the growth rate of the target crystal as an example. Before determining the growth rate of the target crystal based on the multiple crystal contours, the method also includes: determining the structural information of the reaction chamber; if the structural information is a preset structure, then determining the growth rate of the target crystal based on the multiple crystal contours; if the structural information is not the preset structure, then determining multiple crystal volumes based on the multiple crystal contours, and determining the growth rate of the target crystal based on the multiple crystal volumes. Wherein, the structural information includes a two-dimensional plane structure and a three-dimensional structure. The preset structure can represent a two-dimensional plane structure.

[0110] In some embodiments, when the structural information of the reaction chamber is a two-dimensional structure, determining the growth rate of the target crystal based on the multiple crystal contours may include: determining a first contour length of each crystal contour in the X-axis direction and a second contour length in the Y-axis direction; determining the growth rate of the target crystal in the X-axis direction based on the multiple first contour lengths, and determining the growth rate of the target crystal in the Y-axis direction based on the multiple second contour lengths.

[0111] In some embodiments, when the structural information of the reaction chamber is a three-dimensional structure, multiple crystal volumes are determined based on the multiple crystal contours, and the growth rate of the target crystal is determined based on the multiple crystal volumes. Among them, the method for determining multiple crystal volumes based on the multiple crystal contours may include: treating the target crystal as a symmetrical three-dimensional shape, for example, a sphere, a cylinder, or an ellipsoid, and determining the crystal volume by rotating the contour around an axis. Alternatively, by photographing the target crystal in the reaction chamber from different angles, obtaining multiple crystal contours of the target crystal at the same time point, reconstructing the three-dimensional shape of the target crystal through a computer vision algorithm (such as a three-dimensional reconstruction algorithm), and determining the crystal volume of the target crystal. The embodiment of the present application can improve the accuracy of the growth rate determination by determining the structural information of the reaction chamber and selecting the corresponding growth rate determination method based on the structural information.

[0112] In some embodiments, after determining multiple crystal contours or multiple crystal volumes, a rate curve can be constructed to represent the relationship between the crystal contour or crystal volume and the time point. The horizontal axis of the rate curve can represent the time point, and the vertical axis can represent the crystal contour or crystal volume. By constructing the rate curve, the growth rate of the target crystal and the dissolution rate of the target hydrate can be intuitively seen.

[0113] In some embodiments, the first data of the target crystal during the growth process and the second data of the target hydrate during the dissolution process are collected. According to the first data, the relationship between the change of the crystal size over time during the growth process can be fitted, and according to the second data, the relationship between the change of the crystal size over time during the dissolution process can be fitted. Among them, the first data may include the volume, surface area, mass and other information of the target crystal at different time points under specific temperature, pressure and other conditions, and the second data may include the volume, surface area, mass and other information of the target hydrate at different time points under specific temperature, pressure and other conditions. The present application can fit the growth trend of the crystal under different temperature, pressure and other conditions by learning the first data, and can fit the dissolution trend of the crystal under different temperature, pressure and other conditions by learning the second data. The fitting method may include a linear regression method, a polynomial regression method and an exponential regression method, which are not limited here.

[0114] Figure 5 is a schematic diagram of the growth process of the hydrate provided in the examples of the present application, Figure 6 Schematic diagram of the hydrate generation rate provided in the embodiment of the present application. Taking carbon dioxide hydrate as an example, Figure 5 As shown in Figure 1, from (a) to (j), the crystal shape of the hydrate is a polygonal cage, and it gradually expands. Figure 6 As shown in FIG. 1 , the relationship between the growth time and the growth rate of the hydrate in the X-axis direction and the Y-axis direction is compared. As time goes by, the growth rate of the hydrate in the X-axis direction and the Y-axis direction gradually decreases, and the acceleration of the decrease in the X-axis direction is greater than that in the Y-axis direction.

[0115] Figure 7 is a schematic diagram of the dissolution process of the hydrate provided in the examples of the present application, Figure 8 is a graph showing the relationship between the crystal size of the hydrate and the heating rate provided in the examples of the present application, Fig. 9 : is a graph showing the relationship between the dissolution rate and the heating rate of the hydrate provided in the embodiment of the present application. Taking carbon dioxide hydrate as an example, Figure 7 As shown in the figure, from (a) to (f), as the temperature rises, the hydrate gradually dissolves and shrinks from a polyhedral shape to a flat ellipsoidal shape. Figure 8 and 9 As shown, the size of the hydrate gradually becomes smaller and the dissolution rate gradually increases with increasing temperature.

[0116] Fig.10 Schematic diagram of the dissolution process of the reaction gas during the hydrate growth process provided in the embodiment of the present application. Fig.10As shown, in the test of observing the growth characteristics of hydrates, in order to obtain clear observation results, low supercooling is generally maintained to facilitate slow growth of crystals. After reaching the set low supercooling conditions (<2°C), one of the hydrate clusters grew significantly (as shown below (a) to (f)), and the other small crystals showed little obvious growth. At the same time, in the early stage of hydrate growth, two carbon dioxide bubbles appeared in the solution (as shown in (a)). As the hydrate crystals grow, the dissolved carbon dioxide enters the hydrate cage, and then only one carbon dioxide bubble (as shown in (b)) or even no carbon dioxide bubble (as shown in (c)) remains in the field of view. Finally, when all the free gas (CO2 bubbles) disappears, there is no source of dissolved gas in the solution, the hydrate crystals grow slowly (as shown in (d)-(f)), and eventually stop growing. Fig.10 It can be seen that carbon dioxide gas forms hydrates after dissolving.

[0117] Fig.11 Schematic diagram of the formation process of the composite hydrate provided in the embodiment of the present application. It is known that the type II hydrate formed by carbon dioxide and tetrahydrofuran fills the large cage and the small cage respectively. In order to better understand the structure of type II carbon dioxide hydrate, an experiment was conducted to observe the composite hydrate crystals in tetrahydrofuran solution. In the low supercooling hydrate growth experiment, the embodiment of the present application found some characteristics that are different from the growth of carbon dioxide hydrate crystals in pure water. During the growth process, the ring-shaped growth pattern (such as Fig.11 In (a)-(f)), the uniform zonal growth indicates that when there is sufficient space and material source, there is no obvious difference in the growth rate of hydrate in various directions.

[0118] then Figure 1 In the description of the test device 1, in some embodiments, the test device 1 further includes a memory and at least one communication bus, and the at least one communication bus is configured to realize connection and communication between the memory and the processor 143. The memory stores a computer program; the processor 143 is used to implement the test method when executing the computer program stored in the memory.

[0119] In some embodiments, a computer program is stored in the memory, and when the computer program is executed by at least one processor 143, all or part of the steps in the above-mentioned test method are implemented. The memory includes a read-only memory (ROM), a programmable read-only memory (PROM), an erasable programmable read-only memory (EPROM), a one-time programmable read-only memory (OTPROM), an electronically erasable programmable read-only memory (EEPROM), a compact disc read-only memory (CD-ROM) or other optical disc storage, magnetic disk storage, magnetic tape storage, or any other computer-readable medium that can be used to carry or store data.

[0120] In some embodiments, the computer-readable storage medium may mainly include a program storage area and a data storage area, wherein the program storage area may store an operating system, an application required for at least one function, etc.; the data storage area may store data created according to the use of the test device 1, etc.

[0121] In some embodiments, at least one processor 143 is the control core (Control Unit) of the test device 1, which uses various interfaces and lines to connect the various components of the entire test device 1, and executes various functions and processes data of the test device 1 by running or executing programs or modules stored in the memory, and calling data stored in the memory. For example, when at least one processor 143 executes a computer program stored in the memory, all or part of the steps of the test method in the embodiment of the present application are implemented. At least one processor 143 can be composed of an integrated circuit, for example, it can be composed of a single packaged integrated circuit, or it can be composed of multiple integrated circuits with the same function or different functions, including one or more central processing units (CPU), microprocessors, digital processing chips, graphics processors, and various control chips. Combination, etc.

[0122] The above integrated unit implemented in the form of software function modules can be stored in a computer-readable storage medium. The above software function modules are stored in a storage medium and include several instructions for enabling a test device 1 or a processor to execute parts of the methods of various embodiments of the present application.

[0123] In the several embodiments provided in this application, it should be understood that the disclosed devices and methods can be implemented in other ways. For example, the device embodiments described above are only schematic, for example, the division of modules is only a logical function division, and there may be other division methods in actual implementation.

[0124] The modules described as separate components may or may not be physically separated, and the components shown as modules may or may not be physical units, and may be located in one place or distributed on multiple network units. Some or all of the modules may be selected according to actual needs to achieve the purpose of the solution of this embodiment.

[0125] In addition, each functional module in each embodiment of the present application can be integrated into one processing unit, or each unit can exist physically separately, or two or more units can be integrated into one unit. The above integrated unit can be implemented in the form of hardware or in the form of hardware plus software functional modules.

[0126] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present application and are not intended to limit it. Although the present application has been described in detail with reference to the preferred embodiments, a person of ordinary skill in the art should understand that the technical solution of the present application may be modified or replaced by equivalents without departing from the spirit and scope of the technical solution of the present application.

Claims

1. A testing device, characterized in that: The testing device comprises a micron-scale reaction chamber, a temperature control device, a pressure control device and a phase state acquisition device, wherein the reaction chamber is connected to the temperature control device and the pressure control device; the reaction chamber is used to accommodate the reaction substances that generate hydrates, the temperature control device is used to control the temperature in the reaction chamber, and the pressure control device is used to control the pressure in the reaction chamber, wherein the temperature control device comprises a hot and cold stage and a temperature control component: The hot and cold stage is used to load the reaction chamber; The temperature control component is connected to the hot and cold stage and is used to control the temperature of the reaction chamber according to the hot and cold stage; The phase state acquisition device is used to collect the phase state information of the hydrate in the reaction chamber, so that the generation rate and dissolution rate of the hydrate can be determined according to the phase state information.

2. The testing device according to claim 1, characterized in that: The temperature control assembly includes a temperature control component and a liquid nitrogen storage component, wherein the liquid nitrogen storage component connects the hot and cold stage and the temperature control component; the liquid nitrogen storage component is used to store liquid nitrogen, and the temperature control component is used to control the liquid nitrogen storage component to release liquid nitrogen to the hot and cold stage to reduce the temperature of the hot and cold stage; the hot and cold stage transfers heat to the reaction chamber to reduce the temperature in the reaction chamber.

3. The testing device according to claim 1, characterized in that: The hot and cold stage includes a heating component, and the heating component is used to generate heat to increase the temperature of the hot and cold stage; the hot and cold stage transfers heat to the reaction chamber to increase the temperature in the reaction chamber.

4. The testing device according to claim 1, characterized in that: The pressure control device includes an injection component, a pressure control component and a high-pressure pipeline. The injection component is used to inject a first liquid into the reaction chamber. The high-pressure pipeline is used to connect the pressure control component and the reaction chamber. A second liquid is stored in the high-pressure pipeline. The pressure control component is used to control the pressure of the reaction chamber by controlling the second liquid in the high-pressure pipeline.

5. The testing device according to claim 1, characterized in that: The phase state acquisition device includes a Raman spectrometer, a laser and a processor, and the Raman spectrometer is connected to the processor; the laser is used to irradiate the hydrate in the reaction chamber to generate a Raman spectrum, the Raman spectrometer is used to collect the Raman spectrum, and the processor is used to determine the phase state information of the hydrate in the reaction chamber based on the Raman spectrum, and determine the generation rate and dissolution rate of the hydrate based on the phase state information.

6. A testing method, applied to a testing device, characterized in that: The testing device comprises a micrometer-scale reaction chamber, the reaction chamber is used to contain a reaction substance for generating hydrates, the reaction substance comprises a reaction liquid and a reaction gas, and the method comprises: Controlling the initial hydrate in the reaction chamber to dissociate into target crystals; Controlling the pressure in the reaction chamber so that the target crystal grows until a phase equilibrium state is reached to obtain a target hydrate; Collecting first phase information of the target crystal, and determining the generation rate of the target crystal according to the first phase information, and determining the dissolution rate of the reaction gas in the reaction chamber, and determining the corresponding cage entry rate of the reaction gas according to the dissolution rate; controlling the pressure in the reaction chamber to dissociate the target hydrate; The second phase state information of the target hydrate is collected, and the dissolution rate of the target hydrate is determined according to the second phase state information.

7. The testing method according to claim 6, characterized in that: The testing device comprises a hot and cold stage, a liquid nitrogen storage component and a heating assembly, wherein the hot and cold stage is used to load the reaction chamber, the liquid nitrogen storage component is connected to the hot and cold stage, and the control of the initial hydrate in the reaction chamber to dissociate into target crystals comprises: Determining a first temperature control rate and a second temperature control rate of the reaction chamber; Determining a liquid nitrogen flux corresponding to the liquid nitrogen storage component according to the first temperature control rate, and determining heating information of the heating component according to the second temperature control rate; According to the liquid nitrogen flux, controlling the liquid nitrogen storage component to release liquid nitrogen to the hot and cold stage, cooling the reaction chamber according to the first temperature control rate, so that the initial hydrate is generated in the reaction chamber; According to the heating information, the temperature of the hot and cold stage is adjusted by the heating component, and the temperature of the reaction chamber is increased according to the second temperature control rate, so that the initial hydrate is dissociated into the target crystal.

8. The testing method according to claim 6, characterized in that: The step of controlling the pressure in the reaction chamber so that the target crystal grows until a phase equilibrium state is reached to obtain a target hydrate comprises: The pressure of the reaction chamber is controlled according to the second liquid, so that the target crystal grows until a phase equilibrium state is reached to obtain a target hydrate.

9. The testing method according to claim 6, characterized in that: The testing device includes a phase state acquisition device, which includes a Raman spectrometer, a laser and a processor. The first phase state information of the target crystal is acquired, and the generation rate of the target crystal is determined according to the first phase state information, including: irradiating a target crystal in the reaction chamber with the laser to generate a Raman spectrum; Acquire the Raman spectrum by the Raman spectrometer; The first phase information of the target crystal is determined based on the Raman spectrum, and the generation rate of the target crystal is determined according to the first phase information.

10. The testing method according to claim 6, characterized in that: The testing device includes a phase state acquisition device, and the phase state acquisition device also includes a microscope. The method further includes: Determine the crystal video in the reaction chamber through the microscope; Based on a preset image recognition model, the growth rate of the target crystal in the crystal video is determined, and the dissolution rate of the target hydrate in the crystal video is determined.

11. The testing method according to claim 10, characterized in that: Determining the growth rate of the target crystal in the crystal video includes: Based on the image recognition model, determining the crystal contour of the target crystal corresponding to each frame of the crystal image in the crystal video, and obtaining a plurality of crystal contours; The growth rate of the target crystal is determined according to the multiple crystal contours.

12. The testing method according to claim 11, characterized in that: Before determining the growth rate of the target crystal according to the multiple crystal profiles, the method further includes: Determining structural information of the reaction chamber; If the structure information is a preset structure, determining the growth rate of the target crystal according to the multiple crystal contours; If the structure information is not the preset structure, multiple crystal volumes are determined based on the multiple crystal contours, and the growth rate of the target crystal is determined according to the multiple crystal volumes.

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