Visual reaction device and method for measuring hydrate gas storage capacity

Abstract

The present application provides a visualization reaction device, including a reactor, a gas supply component, a plurality of shooting components, two arc-shaped light sources, a temperature and pressure sensor, a temperature control component and a computer. The reactor includes a reactor body, a cover body and a sample stage. The cover body and the reactor body are both provided with a transparent part. The reactor body has two transparent parts. The gas supply component is connected to the cavity. Each shooting component is arranged relative to a transparent part. The shooting component includes a microscope and a camera. The camera is used to shoot the bubble image generated by the hydrate through the microscope. The two arc-shaped light sources are both bent relative to the sample stage. The temperature and pressure sensors are arranged in the cavity. The temperature control component is used to control the temperature in the cavity. The computer is used to process the bubble image captured by the camera and is also used to obtain the temperature and pressure values ​​detected by the temperature and pressure sensor. The device of the present application is conducive to assisting in improving the processing quality of the bubble image. The present application also provides a method for measuring the gas storage capacity of hydrates that is conducive to improving the measurement accuracy.

Description

Technical Field

[0001] The present invention relates to the technical field of hydrate measurement, and in particular to a reaction device and a method for measuring the gas storage capacity of hydrate. Background Art

[0002] Natural gas hydrates, also known as combustible ice, are cage-shaped crystals formed by small gas molecules and water. Water molecules are connected by hydrogen bonds to form polyhedral cages, and small gas molecules fill these polyhedral cages, making them thermodynamically stable. The unique structural characteristics of hydrates give them the advantages of high gas storage capacity (theoretically, 1 cubic meter of hydrate can store 160 cubic meters of methane gas) and mild storage and transportation conditions. It has attracted the attention of many scholars at home and abroad and is considered to be a new type of gas storage and transportation technology carrier with great potential.

[0003] However, due to the randomness of the gas molecule filling process, the measurement of the actual gas storage capacity of hydrates has always been a key issue restricting the gas storage and transportation technology based on the hydrate principle. At present, the main methods for measuring the gas storage capacity of hydrates are the decomposition gas method and the pressure drop method. The decomposition gas method: collects the decomposition gas of hydrates, decomposes the hydrates, and uses the drainage method and other methods to determine the volume of the decomposition gas, and then calculates the gas storage capacity of the hydrates. The pressure drop method: based on the pressure drop during the hydrate formation process, the hydrate gas storage capacity is calculated by theoretical calculation. The decomposition gas method is easily affected by the free gas in the reactor, and the pressure drop method is a theoretical calculation method. Both methods have certain shortcomings.

[0004] In addition, existing visualization reaction devices usually place the light source outside the reactor, causing the bubbles to reflect light from the lamp beads. As a result, the contrast between the edge of the bubble and the background is not obvious, resulting in poor quality of subsequent image processing, which in turn affects the measurement accuracy of the hydrate gas storage capacity. Summary of the invention

[0005] In order to overcome the deficiencies of the prior art, an object of the present invention is to provide a visual response device that is beneficial to improving the contrast between the bubble image and the background so as to assist in improving the processing quality of the bubble image.

[0006] The present application also provides a method for measuring the gas storage capacity of hydrates. The measurement method proposed in the present application can detect the gas storage capacity of hydrates in situ, thereby avoiding the problem of free gas affecting the measurement result of the gas storage capacity of hydrates, thereby improving the measurement accuracy. To solve the above problems, the technical solution adopted by the present invention is as follows:

[0007] A visual reaction device, comprising:

[0008] A reaction kettle, comprising a kettle body, a cover body and a sample stage, wherein the kettle body and the cover body are detachably connected to form a cavity, the sample stage is arranged in the cavity for fixing a wafer forming a liquid bridge, the cover body and the kettle body are both provided with a transparent portion so that the cavity is exposed outside the reaction kettle, and the kettle body has two transparent portions arranged opposite to each other;

[0009] a gas supply assembly connected to the cavity for providing a reaction gas into the cavity, wherein the reaction gas forms a hydrate with the liquid bridge;

[0010] A plurality of photographing components, all disposed outside the reactor, each of the photographing components being disposed relative to one of the transparent parts, the photographing components comprising a microscope and a camera, the microscope being disposed between the camera and the transparent part, the camera being used to photograph the bubble image generated by the hydrate through the microscope;

[0011] Two arc-shaped light sources are both arranged in the cavity and bent relative to the sample stage, and each of the arc-shaped light sources is installed between the transparent portion of the kettle body and the transparent portion of the cover body;

[0012] A temperature and pressure sensor is disposed in the cavity;

[0013] A temperature control component, disposed outside the reactor, for regulating the temperature in the cavity; and

[0014] The computer is used to process the bubble image captured by the camera and to obtain the temperature and pressure values ​​detected by the temperature and pressure sensor.

[0015] In some possible implementations, the arc light source includes:

[0016] A diffusion plate is installed on the kettle body, and the diffusion plate is an arc-shaped structure bent relative to the sample stage; and

[0017] A plurality of LED lamp beads are evenly arranged on an end surface of the diffusion plate opposite to the sample stage.

[0018] In some possible implementations, the temperature control component includes:

[0019] A temperature control sleeve is provided at least on the outer side of the kettle body, and the transparent portion is exposed to the temperature control sleeve; and

[0020] A temperature controller is arranged outside the reaction kettle and connected to the temperature control sleeve, and the temperature controller is used to adjust the temperature of the temperature control sleeve.

[0021] In some possible implementations, the gas supply assembly includes:

[0022] A gas cylinder, connected to the cavity through an air inlet pipe, and used to store the reaction gas;

[0023] An air pressure and temperature detection system, installed on the air inlet pipe and connected to the temperature and pressure sensor, the air pressure and temperature detection system is used to display and detect the output pressure of the gas cylinder, and is also used to display the temperature value and pressure value of the temperature and pressure sensor;

[0024] An air outlet pipe, comprising a first pipe portion and a second pipe portion, wherein the first pipe portion is connected between the cavity and the air pressure and temperature detection system, and the second pipe portion connects the air pressure and temperature detection system to the atmosphere;

[0025] a first valve installed in the air inlet pipe between the gas cylinder and the air pressure and temperature detection system;

[0026] a second valve installed on the first pipe portion;

[0027] The third valve is installed on the second pipe portion.

[0028] In some possible implementations, a light absorbing coating is fixed to at least one of the surface of the sample stage and the inner surface of the kettle body.

[0029] The present application also provides a method for measuring the gas storage capacity of hydrates, which is performed using the above-mentioned visualization reaction device, and the method comprises the following steps:

[0030] A liquid bridge is formed on the sample stage, the gas supply component supplies a reaction gas into the cavity, and the temperature control component adjusts the reaction temperature to a preset value, so that the liquid bridge and the reaction gas form a hydrate;

[0031] Decomposing the hydrate, each of the photographing components collects continuous images of the decomposition process, the continuous images contain bubbles, and the temperature and pressure sensor monitors the pressure P and temperature T in the cavity during the decomposition process;

[0032] processing the continuous images to separate the bubbles from the background;

[0033] Constructing a bubble image classification model with shapes including a sphere, an ellipsoid and a hemisphere, and performing MIM training on the bubble image classification model, so as to restore the contour of the incomplete bubble after separation;

[0034] Mark the repeat bubble;

[0035] Monitoring the shape and size of the bubbles before they disappear, and identifying the repeated bubbles when monitoring the bubbles;

[0036] Calculate the volume of a single target bubble based on the bubble contour before disappearance;

[0037] The volumes of all the target bubbles are added together to obtain the volume of hydrate decomposition gas, and the hydrate gas storage capacity can be calculated in combination with the hydrate volume.

[0038] In some possible implementations, the processing steps include:

[0039] Processing the continuous images using an image distortion elimination algorithm to obtain a first image;

[0040] The first image is converted into a grayscale image, and an image segmentation algorithm is used to process the grayscale image to separate the bubbles from the background.

[0041] In some possible implementations, marking a repeat bubble comprises the steps of:

[0042] For the restored bubble images obtained by at least two of the shooting components arranged relative to the kettle body, the restored bubble images are divided into a proximal bubble image and a global bubble image by setting high and low thresholds, and the distal bubble image is obtained by subtracting the global bubble image from the proximal bubble image, and the pixel area where the proximal bubble image of one of the shooting components and the distal bubble image of another relatively arranged shooting component overlap at the same moment is marked as a repeated bubble.

[0043] In some possible implementations, between the step of monitoring the shape and size of the bubble before it disappears and the step of marking as repeated bubbles, the following steps are also included:

[0044] The missing pixels of the proximal bubble image and the global bubble image are filled using a bilinear or cubic spline interpolation method.

[0045] In some possible implementations, after the step of filling the missing pixels, the method further comprises the steps of:

[0046] The boundary of the bubble is identified and extracted by using an edge detection algorithm, and the MIM training step of the bubble image classification model is repeated for the far-end bubble image to restore the bubble shape.

[0047] Compared with the prior art, the present invention has the following beneficial effects:

[0048] In the present application, the arc light source is changed to be located in the cavity, the arc light source is bent relative to the sample stage, and is also located between the transparent parts of the cover body and the kettle body, so that the light emitted by the light source is more uniform, thereby being able to reduce the reflection phenomenon caused by the bubbles, thereby helping to improve the contrast between the bubble image and the background, thereby helping to assist in improving the processing quality of the bubble image, and therefore, helping to assist in improving the measurement accuracy of the hydrate gas storage capacity. In addition, the present application arranges multiple shooting components at multiple angles for shooting, which is conducive to distinguishing overlapping bubbles during later image processing, reducing the measurement error introduced by bubble overlap, and thereby helping to assist in improving the measurement accuracy of the hydrate gas storage capacity.

[0049] In the present application, the structure of the visualization reaction device is improved to improve the image quality collected by the shooting component. In addition, a method is proposed to track and analyze the bubbles generated during the decomposition of the hydrate sample, and then obtain the gas storage capacity based on the total volume of the bubbles. This allows the measurement method proposed in the present application to detect the gas storage capacity of the hydrate in situ, thereby avoiding the problem of poor measurement accuracy caused by the decomposition of the hydrate before measurement. Therefore, the measurement method provided in the present application is conducive to improving measurement accuracy.

[0050] The present invention is further described in detail below in conjunction with the accompanying drawings and specific embodiments. BRIEF DESCRIPTION OF THE DRAWINGS

[0051] Figure 1 A schematic diagram of the structure of a visual reaction device provided in one embodiment of the present application;

[0052] Figure 2 for Figure 1 A schematic structural diagram of the reactor and the temperature control jacket from another perspective shown;

[0053] Figure 3 for Figure 1 The structural schematic diagram of the arc light source shown;

[0054] Figure 4 Taking images of bubbles obtained by prior art;

[0055] Figure 5 for Figure 4 The image obtained after preprocessing;

[0056] Figure 6 The bubble image obtained in the embodiment of the present application;

[0057] Figure 7 for Figure 6 The image obtained after preprocessing;

[0058] Figure 8 A flow chart of a method for measuring hydrate gas storage capacity provided in one embodiment of the present application.

[0059] Description of Figure Numbers:

[0060] 100-visual reaction device; 10-reactor; 11-reactor body; 12-cover body; 13-sample stage; 101-cavity; 110-transparent part; 121-body; 122-anti-fog lens; 120-through hole; 20-gas supply assembly; 21-gas cylinder; 22-intake pipe; 23-air pressure and temperature detection system; 24-exhaust pipe; 241-first pipe; 242-second pipe; 25-first valve; 26-second valve; 27-first Three valves; 30 - shooting assembly; 31 - microscope; 32 - camera; 40 - arc light source; 41 - diffusion plate; 42 - LED lamp beads; 43 - shell; 50 - temperature and pressure sensor; 60 - temperature control assembly; 61 - temperature control sleeve; 62 - temperature control machine; 70 - computer; 200 - chip; 201 - liquid bridge; S101, S102, S103, S104, S105, S108, S109, S1010 - steps. DETAILED DESCRIPTION

[0061] The following will be combined with the drawings in the embodiments of the present application to clearly and completely describe the technical solutions in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.

[0062] The terms "first", "second", etc. in the specification and claims of this application and the above-mentioned drawings are used to distinguish different objects, rather than to describe a specific order. In addition, the terms "including" and "having" and any variations thereof are intended to cover non-exclusive inclusions. It should be noted that when an element is referred to as "fixed to" another element, it can be directly on the other element or there can be a centered element. When an element is referred to as "connected to" another element, it can be directly connected to the other element or there can be a centered element. When an element is referred to as "arranged on" another element, it can be arranged on the other element or there can be a centered element.

[0063] Reference Figure 1 In one embodiment of the present application, a visualization reaction device 100 is provided. Specifically, the visualization reaction device 100 includes a reaction kettle 10, a gas supply component 20, a plurality of shooting components 30, two arc light sources 40 (combined with reference to Figure 3), temperature and pressure sensor 50, temperature control assembly 60 and computer 70. The reaction kettle 10 includes a kettle body 11, a cover body 12 and a sample stage 13. The kettle body 11 and the cover body 12 are detachably connected to form a cavity 101. For example, the kettle body 11 and the cover body 12 can be threaded or clamped. The sample stage 13 is arranged in the cavity 101 to fix the wafer 200 forming the liquid bridge 201 (combined with reference to Figure 2 ), exemplarily, the number of wafers 200 can be two, so that water source is dripped into the gap between the two wafers 200 to form a liquid bridge 201. Exemplarily, the wafer 200 can be fixed by a card slot. The cover 12 and the kettle body 11 are both provided with a transparent portion 110, so that the cavity 101 is exposed outside the reactor 10, that is, the cavity 101 can be observed from the outside of the reactor 10 along the transparent portion 110. The kettle body 11 has two transparent portions 110 arranged opposite to each other. Exemplarily, the reactor 10 can be partially transparent or fully transparent.

[0064] The gas supply assembly 20 is connected to the cavity 101 to provide a reaction gas into the cavity 101. The reaction gas forms a hydrate with the liquid bridge 201. For example, the reaction gas may include one of methane or ethane. For example, the liquid bridge 201 may include an aqueous solution. A plurality of shooting assemblies 30 are arranged outside the reactor 10. Each shooting assembly 30 is arranged relative to a transparent portion 110. The shooting assembly 30 includes a microscope 31 and a camera 32. The microscope 31 is arranged between the camera 32 and the transparent portion 110. The camera 32 is used to shoot the bubble image generated by the hydrate through the microscope 31. For example, the camera 32 can shoot continuous video images or continuous multi-frame photo images. Each arc light source 40 is installed between a transparent portion 110 of a reactor body 11 and a transparent portion 110 of a cover body 12. The arc light source 40 is arranged in the cavity 101 and is bent relative to the sample stage 13. The temperature and pressure sensor 50 is arranged in the cavity 101 so as to detect the temperature and pressure of the reaction. The temperature control assembly 60 is disposed outside the reactor 10 to control the temperature in the cavity 101. The computer 70 is used to process the bubble image captured by the camera 32 and to obtain the temperature and pressure values ​​detected by the temperature and pressure sensor 50.

[0065] Figure 4 The bubble images obtained by the prior art disclosed in the background art are Figure 5 for Figure 4 The image obtained after preprocessing to separate bubbles from the background, Figure 6 The bubble shooting image obtained by the visualization reaction device 100 provided in the present application is Figure 7 for Figure 6 The image obtained after preprocessing to separate bubbles from the background.

[0066] In the present application, the arc light source 40 is changed to be arranged in the cavity 101, and the arc light source 40 is bent relative to the sample stage 13, and is also arranged between the transparent parts 110 of the cover body 12 and the kettle body 11, so that the light emitted by the light source is more uniform, thereby being able to reduce the reflection phenomenon caused by the bubbles, thereby helping to improve the contrast between the bubble image and the background, making the bubble outline more obvious, thereby helping to assist in improving the processing quality of the bubble image, and therefore, helping to assist in improving the measurement accuracy of the hydrate gas storage capacity. In addition, the present application arranges multiple shooting components 30 at multiple angles for shooting, which is conducive to distinguishing overlapping bubbles during later image processing, reducing the measurement error introduced by bubble overlap, and thereby helping to assist in improving the measurement accuracy of the hydrate gas storage capacity.

[0067] In some embodiments, reference Figure 3 The arc light source 40 includes a diffuser plate 41 and a plurality of LED lamp beads 42. The diffuser plate 41 is mounted on the kettle body 11. The diffuser plate 41 is an arc-shaped structure bent relative to the sample stage 13. The plurality of LED lamp beads 42 are evenly arranged on one end surface of the diffuser plate 41 relative to the sample stage 13. The diffuser plate 41 is conducive to further improving the uniformity of light, thereby further assisting in improving the processing quality of the bubble image.

[0068] Exemplarily, the diffusion plate 41 and the plurality of LED lamp beads 42 may be installed in the housing 43 .

[0069] In some embodiments, the arc-shaped light source 40 emits blue light, thereby facilitating slowing down the evaporation rate of the liquid bridge 201 .

[0070] In some embodiments, reference Figure 1 The temperature control assembly 60 includes a temperature control sleeve 61 and a temperature control machine 62. The temperature control sleeve 61 is at least arranged on the outer side of the kettle body 11, and the transparent part 110 is exposed to the temperature control sleeve 61. For example, the temperature control sleeve 61 can be provided with an opening so that the transparent part 110 is exposed to the opening, or the temperature control sleeve 61 can be a transparent body, so that the microscope 31 can collect images from one side of the temperature control sleeve 61. The temperature control machine 62 is arranged outside the reactor 10 and connected to the temperature control sleeve 61. The temperature control machine 62 is used to adjust the temperature of the temperature control sleeve 61. For example, the temperature control sleeve 61 can include a water bath jacket, and for example, the temperature control machine 62 can include a water bath circulator. The temperature control sleeve 61 is arranged on the outer side of the kettle body 11 to facilitate heat dissipation of the arc light source.

[0071] In some embodiments, reference Figure 1The gas supply assembly 20 includes a gas cylinder 21, an air inlet pipe 22, an air pressure and temperature detection system 23, an air outlet pipe 24, a first valve 25, a second valve 26 and a third valve 27. The gas cylinder 21 is connected to the cavity 101 through the air inlet pipe 22, and the gas cylinder 21 is used to store the reaction gas. The air pressure and temperature detection system 23 is installed on the air inlet pipe 22 and connected to the temperature and pressure sensor 50, so that the value of the temperature and pressure sensor 50 can be transmitted to the air pressure and temperature detection system 23 for display. The air pressure and temperature detection system 23 is used to display the output pressure of the detection gas cylinder 21, and is also used to display the temperature value and pressure value of the temperature and pressure sensor 50. Exemplarily, the air pressure and temperature detection system 23 may include an electronic barometer. The air outlet pipe 24 includes a first pipe portion 241 and a second pipe portion 242, the first pipe portion 241 is connected between the cavity 101 and the air pressure and temperature detection system 23, and the second pipe portion 242 connects the air pressure and temperature detection system 23 to the atmosphere. The first valve 25 is installed on the air inlet pipe 22 between the gas cylinder 21 and the air pressure and temperature detection system 23 , the second valve 26 is installed on the first pipe portion 241 , and the third valve 27 is installed on the second pipe portion 242 .

[0072] In specific application, after opening the gas cylinder 21, the first valve 25 can be adjusted (the second valve 26 and the third valve 27 are closed at this time) so that the gas supply pressure reaches the preset value, and then the second valve 26 is unscrewed to allow the reaction gas to pass into the cavity 101, and then the second valve 26 can be closed to form a sealed space in the cavity 101. At this time, the measured value of the temperature and pressure sensor 50 is transmitted to the air pressure and temperature detection system 23 for display, so as to facilitate the adjustment of the gas supply pressure of the gas cylinder 21. When the temperature control component 60 adjusts the reaction temperature to the preset temperature, the hydration reaction begins. At this time, the measured value of the temperature and pressure sensor 50 is transmitted to the computer 70. In addition, the third valve 27 and the first valve 25 can be opened while the second valve 26 and the gas cylinder 21 are closed to discharge the residual gas in the tube into the atmosphere. In addition, the second valve 26 and the third valve 27 can be opened while the first valve 25 is closed, so that the hydrate is decomposed by reducing pressure. It can be seen from this that the structure of the gas supply component 20 can realize the functions of reducing pressure, cleaning residual gas, pressure detection and numerical display.

[0073] In other embodiments, hydrates may be decomposed by heating or adding inhibitors, and accordingly, the structure of the gas supply assembly 20 may be simplified, and illustratively, may only include the gas cylinder 21 .

[0074] In some embodiments, at least one of the surface of the sample stage 13 and the inner surface of the kettle body 11 is fixed with a light-absorbing coating (not shown). Exemplarily, the light-absorbing coating can be a black coating. The light-absorbing coating can reduce the negative impact of stray light on imaging quality, thereby helping to further assist in improving the processing quality of the bubble image.

[0075] In some embodiments, reference Figure 2 The cover 12 includes a body 121 and an anti-fog lens 122. The body 121 is provided with a through hole 120 connected to the cavity 101. The anti-fog lens 122 is fixed in the through hole 120. The mirror surface of the anti-fog lens 122 is arranged relative to the cavity 101. The structure of the cover 12 can reduce fogging caused by the temperature difference between the inside and outside of the kettle.

[0076] In some embodiments, the inner surface of the kettle body 11 is sunken to form a groove, and the arc light source 40 is fixed in the groove. The way in which the arc light source 40 is fixed in the groove facilitates assembly and disassembly of the device.

[0077] Another embodiment of the present application also provides a method for measuring the gas storage capacity of hydrates, which is performed using the visualization reaction device 100 of the above embodiment, referring to Figure 8 , the method comprises the following steps:

[0078] Step S101 : forming a liquid bridge 201 on the sample stage 13 , the gas supply component 20 supplies reaction gas into the cavity 101 , and the temperature control component 60 adjusts the reaction temperature to a preset value, so that the liquid bridge 201 and the reaction gas form a hydrate.

[0079] Specifically, the cover 12 can be opened to drip a water source between the gaps of the two wafers 200 on the sample stage 13 to form a liquid bridge 201. For example, the water source can be deionized water. In some embodiments, the gas cylinder 21 can be opened, and the first valve 25 can be unscrewed (at this time, the second valve 26 and the third valve 27 are closed) so that the outlet pressure of the gas cylinder 21 reaches a preset value. After that, the second valve 26 is also unscrewed to allow the reaction gas to pass into the cavity 101. After that, according to the pressure measurement value of the temperature pressure sensor 50 displayed by the air pressure and temperature detection system 23, the gas cylinder 21 and the second valve 26 are closed, and the third valve 27 is also unscrewed to remove the residual gas. Finally, the gas cylinder 21, the first valve 25, the second valve 26 and the third valve 27 are closed to complete the step of supplying the reaction gas.

[0080] Step S102: Decomposing hydrates, each shooting component 30 collects continuous images of the decomposition process, the continuous images contain bubbles, the temperature and pressure sensor 50 monitors the pressure P and temperature T in the cavity 101 during the decomposition process, and the corresponding monitoring values ​​are sent to the computer 70 for recording.

[0081] Exemplarily, the hydrate decomposition may be promoted by reducing pressure, heating or adding an inhibitor. Exemplarily, the shooting component 30 may collect video continuous images including bubbles.

[0082] In some embodiments, the second valve 26 and the third valve 27 can be unscrewed (the gas cylinder 21 and the first valve 25 remain closed at this time) to reduce the gas pressure in the cavity 101, thereby causing the hydrate to decompose under reduced pressure.

[0083] Step S103: Process the continuous images to separate the bubbles from the background.

[0084] In some embodiments, the step of processing the continuous images includes:

[0085] The continuous images are processed by an image distortion elimination algorithm to obtain a first image. The image distortion elimination algorithm can eliminate the image distortion problem caused by the refraction of the liquid bridge curved liquid surface, thereby obtaining a true image of the bubble. Exemplarily, the image distortion elimination algorithm can adopt a fully convolutional residual network algorithm based on GAN training.

[0086] The first image is converted into a grayscale image. For example, the first image can be binarized to form a grayscale image, and the grayscale image can be processed using an image segmentation algorithm to separate the bubbles from the background. For example, an image threshold segmentation method can be used to segment the image.

[0087] Step S104: constructing a bubble image classification model whose shapes include a sphere, an ellipsoid and a hemisphere, and performing MIM training on the bubble image classification model, so as to restore the contours of the incomplete bubbles after separation.

[0088] Step S105: Mark repeated bubbles.

[0089] In some embodiments, for the restored bubble images obtained by at least two shooting components 30 arranged relative to the kettle body 11, by setting high and low thresholds, the restored bubble images are divided into proximal bubble images and global bubble images, and the global bubble images are subtracted from the proximal bubble images to obtain the distal bubble images, and the pixel areas where the proximal bubble images of one shooting component 30 and the distal bubble images of another shooting component 30 arranged relatively at the same time overlap are marked as repeated bubbles. Exemplarily, the proximal bubble images collected by one shooting component 30 and another shooting component 30 arranged relative to the kettle body 11 are removed from the repeated bubble images to obtain the entire horizontally collected image (i.e., the image in the depth direction). In addition, the shooting component 30 arranged relative to the cover body 12 obtains the bubble images in the length direction and the width direction, and the size of the bubble group can be obtained from the bubble images in the depth direction, the length direction and the width direction. According to the size of the bubble group, the influence of the behavior of all bubbles that are completely blocked and cannot be observed on the volume can be obtained, thereby obtaining the empirical coefficient k. That is, the position coordination of all the shooting components 30 is also conducive to improving the measurement accuracy.

[0090] In some embodiments, after step S105, a further step is included: using a bilinear or cubic spline interpolation method to fill in missing pixels of the proximal bubble image and the global bubble image, thereby improving the image resolution.

[0091] In some embodiments, after the step of filling the missing pixels, the method also includes the steps of: using an edge detection algorithm to identify and extract the boundaries of the bubbles, and repeatedly using the bubble image classification model to perform the MIM training step on the far-end bubble image to restore the bubble shape, thereby solving the incomplete bubble edge of the far-end bubble image obtained by subtraction.

[0092] In other embodiments, step S106 and / or step S107 may be omitted.

[0093] Step S108: monitor the shape and size of the bubble before it disappears, and identify repeated bubbles when monitoring the bubble. For example, the bubble trajectory can be tracked using the method provided by Chinese invention patent CN116563342A (published on August 8, 2023) or Chinese invention patent CN116580059A (published on August 11, 2023).

[0094] Step S109: Calculate the volume of a single target bubble based on the bubble contour shape before disappearance, and calculate the gas storage capacity of each target bubble based on n=PV / RT (ideal gas state equation). The bubble volume can be calculated based on the parameter formula of the bubble image classification model corresponding to the shape detected by the edge. The target bubble refers to the part of the bubble excluding the overlapping bubbles.

[0095]

[0096] Exemplarily, when the bubble is classified as spherical by the model, the volume is calculated using this formula, where V is the volume of the bubble and A is the projected area of ​​the bubble, that is, the equivalent diameter method is used for calculation.

[0097]

[0098] When the bubble is classified as an ellipsoid by the model, the volume is calculated using this formula, where V is the bubble volume, a is the major axis, b is the minor axis, the longest chord intercepted by the bubble boundary of a straight line passing through the bubble horizontally is the bubble major axis, and the chord intercepted by the bubble boundary of a straight line passing through the midpoint of the major axis and perpendicular to the major axis is the bubble minor axis. c can be determined by the ratio of a to b. When the ratio is large, it is considered that the axis length in the third direction that cannot be reflected in the image is equal to the major axis of the bubble in the image. When the ratio is small, it is considered that the axis length in the third direction that cannot be reflected in the image is equal to the minor axis of the bubble in the image.

[0099] When the bubble is classified as hemispherical by the model, the adaptive slicing method proposed in the study of image processing technology based on high-speed photography to measure the bubble volume (Tang Huapeng, Wen Jiming, Gu Haifeng) can be used to calculate the bubble model.

[0100] Step S1010: Add up the volumes of all target bubbles and compare with the hydrate volume to obtain the gas storage capacity of the hydrate.

[0101] A gas balance equation is established to convert the volume of gas in the bubble into the volume of gas at the target temperature and pressure (such as normal temperature and pressure), and then the volume of all target gases is added to obtain the volume of hydrate decomposition gas. The volume of hydrate decomposition gas is divided by the hydrate volume to obtain the hydrate gas storage capacity.

[0102]

[0103] V g is the gas volume, T s and p s Normal temperature and pressure

[0104]

[0105] The amount of gaseous material obtained by the vertical / horizontal camera and the volume of decomposed gas are calculated using this formula, N_(x / y) is the total amount of material in the horizontal or vertical camera position, p is the pressure, v is the bubble volume, T is the temperature, and R is the molar gas constant, where i is the bubble parameter in the bubble group area. Since bubble aggregation will lead to complete occlusion of bubbles, an empirical coefficient α is used to correct the influence of the behavior of bubbles that are completely blocked and cannot be observed in the bubble group on the volume. The size of the α value is positively correlated with the size of the bubble group. The size of the bubble group is jointly determined by multiple shooting components 30 relative to the cover body 12 and the kettle body 11. That is, the larger the bubble group, the more bubbles that may be blocked, and the data obtained by the original formula will be smaller, so α is used for correction. k is the bubble parameter in the non-bubble group area.

[0106]

[0107]

[0108] The final amount of gas and decomposition gas volume are obtained by weighted average of the amount of substance obtained by the horizontal camera and the vertical camera (refer to the above formula). Due to the uncertainty of hydrate decomposition, sometimes there are more horizontal bubbles and sometimes more vertical bubbles, so the weight can be adjusted by artificially observing the behavior of hydrates during decomposition. ε1 and ε2 are determined according to the number of bubbles observed in the corresponding direction.

[0109] The volume of hydrate can be calculated by the amount of gas substance. For example, the chemical formula of methane hydrate is CH4﹒nH2O. According to the amount of methane substance and the amount of water used to construct the liquid bridge, n can be obtained. The amount of gas substance at this time is the amount of hydrate substance. Then the amount of hydrate substance is multiplied by the molar volume of the hydrate under the current n to get the hydrate volume.

[0110]

[0111] N1 is the amount of water, μ is the liquid bridge evaporation coefficient, V1 is the volume used to build the liquid bridge, V m1 is the molar volume of water

[0112]

[0113] V gh =N·V mgh

[0114] Gas storage capacity:

[0115] In the present application, the structure of the visualization reaction device 100 is improved to improve the image quality collected by the shooting component 30. In addition, a method is proposed to track and analyze the bubbles generated during the decomposition of the hydrate sample, and then obtain the gas storage capacity based on the total volume of the bubbles. This allows the measurement method proposed in the present application to detect the gas storage capacity of the hydrate in situ, thereby avoiding the problem of poor measurement accuracy caused by hydrate decomposition before measurement. Therefore, the measurement method provided in the present application is conducive to improving measurement accuracy.

[0116] The above-mentioned embodiments are only preferred embodiments of the present invention and cannot be used to limit the scope of protection of the present invention. Any non-substantial changes and substitutions made by technicians in this field on the basis of the present invention shall fall within the scope of protection required by the present invention.

Claims

1. A visual reaction device, characterized in that: include: A reaction kettle, comprising a kettle body, a cover body and a sample stage, wherein the kettle body and the cover body are detachably connected to form a cavity, the sample stage is arranged in the cavity for fixing a wafer forming a liquid bridge, the cover body and the kettle body are both provided with a transparent portion so that the cavity is exposed outside the reaction kettle, and the kettle body has two transparent portions arranged opposite to each other; a gas supply assembly connected to the cavity for providing a reaction gas into the cavity, wherein the reaction gas forms a hydrate with the liquid bridge; A plurality of photographing components, all disposed outside the reactor, each of the photographing components being disposed relative to one of the transparent parts, the photographing components comprising a microscope and a camera, the microscope being disposed between the camera and the transparent part, the camera being used to photograph the bubble image generated by the hydrate through the microscope; Two arc-shaped light sources are both arranged in the cavity and bent relative to the sample stage, and each of the arc-shaped light sources is installed between the transparent portion of the kettle body and the transparent portion of the cover body; A temperature and pressure sensor is disposed in the cavity; A temperature control component, disposed outside the reactor, for regulating the temperature in the cavity; as well as The computer is used to process the bubble image captured by the camera and to obtain the temperature and pressure values ​​detected by the temperature and pressure sensor.

2. The visual reaction device according to claim 1, characterized in that: The arc light source comprises: A diffusion plate is installed on the kettle body, and the diffusion plate is an arc-shaped structure bent relative to the sample stage; and A plurality of LED lamp beads are evenly arranged on an end surface of the diffusion plate opposite to the sample stage.

3. The visual reaction device according to claim 1, characterized in that: The temperature control component comprises: A temperature control sleeve is provided at least on the outer side of the kettle body, and the transparent portion is exposed to the temperature control sleeve; and A temperature controller is arranged outside the reaction kettle and connected to the temperature control sleeve, and the temperature controller is used to adjust the temperature of the temperature control sleeve.

4. The visual reaction device according to claim 1, characterized in that: The gas supply assembly comprises: A gas cylinder, connected to the cavity through an air inlet pipe, and used to store the reaction gas; An air pressure and temperature detection system, installed on the air inlet pipe and connected to the temperature and pressure sensor, the air pressure and temperature detection system is used to display and detect the output pressure of the gas cylinder, and is also used to display the temperature value and pressure value of the temperature and pressure sensor; An air outlet pipe, comprising a first pipe portion and a second pipe portion, wherein the first pipe portion is connected between the cavity and the air pressure and temperature detection system, and the second pipe portion connects the air pressure and temperature detection system to the atmosphere; a first valve installed in the air inlet pipe between the gas cylinder and the air pressure and temperature detection system; a second valve installed on the first pipe portion; The third valve is installed on the second pipe portion.

5. The visual reaction device according to any one of claims 1 to 4, characterized in that: A light absorbing coating is fixed to at least one of the surface of the sample stage and the inner surface of the kettle body.

6. A method for measuring hydrate gas storage capacity, characterized in that: The method is carried out using the visualization reaction device according to any one of claims 1 to 5, and comprises the following steps: A liquid bridge is formed on the sample stage, the gas supply component supplies a reaction gas into the cavity, and the temperature control component adjusts the reaction temperature to a preset value, so that the liquid bridge and the reaction gas form a hydrate; Decomposing the hydrate, each of the photographing components collects continuous images of the decomposition process, the continuous images contain bubbles, and the temperature and pressure sensor monitors the pressure P and temperature T in the cavity during the decomposition process; processing the continuous images to separate the bubbles from the background; Constructing a bubble image classification model with shapes including a sphere, an ellipsoid and a hemisphere, and performing MIM training on the bubble image classification model, so as to restore the contour of the incomplete bubble after separation; Mark the repeat bubble; Monitoring the shape and size of the bubbles before they disappear, and identifying the repeated bubbles when monitoring the bubbles; Calculate the volume of a single target bubble based on the bubble contour before disappearance; The volumes of all the target bubbles are added together to obtain the volume of hydrate decomposition gas, and the hydrate gas storage capacity can be calculated in combination with the hydrate volume.

7. The method according to claim 6, characterized in that The steps of the process include: Processing the continuous images using an image distortion elimination algorithm to obtain a first image; The first image is converted into a grayscale image, and an image segmentation algorithm is used to process the grayscale image to separate the bubbles from the background.

8. The method according to claim 6, characterized in that Marking duplicate bubbles includes the following steps: For the restored bubble images obtained by at least two of the shooting components arranged relative to the kettle body, the restored bubble images are divided into a proximal bubble image and a global bubble image by setting high and low thresholds, and the distal bubble image is obtained by subtracting the global bubble image from the proximal bubble image, and the pixel area where the proximal bubble image of one of the shooting components and the distal bubble image of another relatively arranged shooting component overlap at the same moment is marked as a repeated bubble.

9. The method according to claim 8, characterized in that Between the step of monitoring the shape and size of the bubble before it disappears and the step marked as repeating the bubble, there are also steps: The missing pixels of the proximal bubble image and the global bubble image are filled using a bilinear or cubic spline interpolation method.

10. The method according to claim 9, characterized in that After the step of filling the missing pixels, the method further comprises the steps of: The bubble boundary is identified and extracted by using an edge detection algorithm, and the MIM training step is repeated using the bubble image classification model on the far-end bubble image to restore the bubble shape.

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