CN117740754A - Gas hydrate micro-dynamics in-situ test device and method - Google Patents
Gas hydrate micro-dynamics in-situ test device and method Download PDFInfo
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Abstract
The gas hydrate micro-dynamics in-situ testing device comprises a reaction kettle, a gas-liquid two-phase injection unit, a temperature-pressure control and monitoring unit, a visual operation unit and a hydrate generation area intelligent identification and calculation unit, wherein the gas-liquid two-phase injection unit is connected with the reaction kettle and is used for injecting multiphase samples into the reaction kettle, the temperature-pressure control and monitoring unit is used for controlling and monitoring the temperature and the pressure in the reaction process of a reaction kettle system, the reaction kettle is provided with an observable window, the visual operation unit is used for observing the morphological characteristics and the growth process of the hydrate reaction system through the observable window, and the hydrate generation area intelligent identification and calculation unit is used for identifying the generation and decomposition of the hydrate and calculating the thermodynamic information of the hydrate in real time according to the observation information of the visual operation unit. The invention can realize the synthesis and decomposition of the hydrate under the condition of controllable temperature and pressure, and inject multiphase samples and accurately determine the generation and decomposition positions of the gas hydrate.
Description
Technical Field
The invention relates to the technical field of gas hydrate dynamics measurement, in particular to a gas hydrate micro-dynamics in-situ test device and method.
Background
To realize CO 2 Trapping and sequestration, the traditional geological sequestration method is usually to sequester CO 2 The method is characterized in that the method is injected into geological bodies such as depleted oil and gas reservoirs, deep gas reservoirs, salty water layers and the like in a supercritical state, wherein the mainly related sealing mechanism comprises dissolution sealing, mineralization sealing, structural sealing and residual sealing. Although this approach is relatively mature, it is overly dependent on the integrity of the cap layer, once the cap layer is broken, supercritical CO with high buoyancy 2 Is easy to escape to the atmosphere again through cracks or faults. In addition, some high carbon emission areas lack the above-described bodies suitable for conventional sequestration. Therefore, there is an urgent need to explore a new way of geological sequestration that is efficient, safe and more versatile, complementary to the advantages of conventional geological sequestration. Hydrate process CO 2 The liquid CO is stored 2 Injecting CO into submarine sediment under proper temperature and pressure conditions 2 The hydrate is used for realizing long-term stable sealing. The method not only covers four main sealing mechanisms in the traditional mode, but also generates CO 2 The hydrate can be used as a hypotonic cover layer to block CO 2 And can self-seal the primary fracture of the stratum to prevent CO possibly generated 2 Escape along the fissure. The huge pore space in the submarine sediment is also hydrate method CO 2 The sealing and storing provides a wide application prospect.
The Raman spectrum technology can provide basic information such as hydrate cage structure, guest molecule components, cage occupation rate, hydration number and the like, and represents CO on a microscopic scale 2 Important for hydrate formation and decomposition processMeans of the method. However, CO is now concerned with 2 The raman test device of hydrates has the following limitations: (1) Most of the detection can only be performed under specific temperature and pressure, and the CO of different Wen Yaxia cannot be tested 2 Hydrate microstructure; (2) Failure to accurately determine CO 2 Generating a position of the hydrate in the reaction kettle; (3) CO 2 The injection mode is single, and most of the injection modes only can inject gaseous CO 2 。
Disclosure of Invention
In order to solve the problems of temperature and pressure limitation, difficulty in determining a generation position, single injection mode and the like in the prior art, the invention provides a gas hydrate micro-dynamics in-situ test device and method.
The technical problems of the invention are solved by the following technical scheme:
the utility model provides a gas hydrate micromechanics normal position testing arrangement, includes reation kettle, gas-liquid two-phase injection unit, temperature and pressure control and monitoring unit, visual operation unit and hydrate formation area intelligence discernment and calculation unit, gas-liquid two-phase injection unit connects reation kettle for pour into multiphase sample into reation kettle into, temperature and pressure control and monitoring unit are set up with control and monitoring reation kettle reaction in-process's temperature and pressure, reation kettle is provided with observable window, visual operation unit is set up with through observable window survey hydrate reaction system's morphological feature and growth process (can include guest molecule cage ratio, microstructure evolution etc.), hydrate formation area intelligence discernment and calculation unit is set up with according to visual operation unit's observation information, discernment hydrate formation and decomposition and calculation hydrate thermodynamic information.
In some embodiments, the thermodynamic information of the hydrate includes one or more of induction time, nucleation region, saturation, decomposition behavior of the hydrate.
In some embodiments, the gas-liquid two-phase injection unit comprises a storage tank, a piston container and a multi-phase carbon dioxide injection pump, wherein the storage tank is connected with the piston container, and the piston container is connected with the reaction kettle through the multi-phase carbon dioxide injection pump; wherein the storage tank comprises a gas phase storage tank and a liquid phase storage tank.
In some embodiments, the reaction kettle is a jacketed temperature control reaction kettle, the temperature and pressure control and monitoring unit comprises a liquid nitrogen tank and a liquid nitrogen pump, the liquid nitrogen tank is connected with a jacket of the jacketed temperature control reaction kettle through the liquid nitrogen pump, and the liquid nitrogen pump drives liquid nitrogen to circulate so that a reaction system in the reaction kettle is in a set low-temperature condition.
In some embodiments, the visual operation unit comprises a CCD camera, and the CCD camera is used for observing and recording the morphological expressions of the hydrate in different reaction stages in the whole injection-sealing process in real time, so that the intelligent identification and calculation unit of the hydrate generation area can analyze and calculate the hydrate.
In some embodiments, the visual operation unit comprises a microscope, and the microscope is used for observing local details of the hydrate nucleation and growth process so as to enable the hydrate generation area intelligent identification and calculation unit to analyze and calculate.
In some embodiments, the visual manipulation unit comprises a raman spectrometer for illuminating the sample to produce a raman spectrum and a laser for collecting the raman spectrum to monitor and identify hydrate microstructure and micro-kinetic reaction processes for analysis and calculation by the hydrate generation region intelligent identification and calculation unit.
In some embodiments, the visual operation unit comprises an XYZ electric displacement table and a precision displacement operation sliding table, the reaction kettle is connected with the XYZ electric displacement table, and the precision displacement operation sliding table is used for operating the displacement of the XYZ electric displacement table to control the position of the reaction kettle so as to adjust the observation field of view of the visual operation unit on the reaction kettle.
In some embodiments, the reactor is filled with mineral particles and injected with multi-phase CO 2 Sample to simulate hydrate process CO 2 Sealing and storing, namely intelligent through the visual operation unit and the hydrate generation areaAnd the identification and calculation unit is used for monitoring the phase state conversion of the sample in the reaction kettle in real time and evaluating the stability of geological carbon sequestration.
The invention also provides a gas hydrate micro-dynamics in-situ test method, which uses the device to perform gas hydrate micro-dynamics in-situ test.
The beneficial effects of the invention include:
the gas hydrate micro-dynamics in-situ test device and the method thereof provided by the invention are coupled with a gas-liquid two-phase injection unit and a temperature-pressure control and monitoring unit, and can inject gas-phase or liquid-phase CO under the specified temperature-pressure condition 2 Realizing CO under the condition of controllable temperature and pressure 2 The synthesis and decomposition of the hydrate solve the limitation of detection under specific temperature and pressure; by arranging the visual operation unit to observe the visual window of the kettle body, the generation position of the gas hydrate in the reaction kettle can be effectively and accurately determined, and the CO in the whole injection-sealing process can be observed and recorded in real time 2 Hydrate morphology characterization, CO was observed 2 The nucleation and growth process of the hydrate can obtain clear CO in different reaction systems 2 The evolution rule of the morphology of the hydrate crystal is used for clarifying the CO under different reaction systems 2 The mechanism of the thermodynamic of the hydrate lays a morphological foundation; meanwhile, the gas-liquid two-phase injection unit can inject the multiphase sample into the reaction kettle, so that the problem of single injection mode is solved; and by arranging the intelligent recognition and calculation unit of the hydrate generation area, the generation and decomposition of the hydrate are recognized according to the observation information of the visual operation unit, and the thermodynamic information of the hydrate is calculated, and the recognition calculation result and the temperature and pressure monitoring result are subjected to cross verification so as to ensure the accuracy of the system. The invention can accurately describe different temperature pressures and CO 2 CO under the condition of phase injection 2 Microcosmic nucleation, growth and decomposition behavior of hydrate followed by clearing CO 2 The thermodynamic characteristics of the hydrate, the development of high-efficiency thermodynamic promoters and the optimization of injection-sealing schemes lay an experimental foundation.
Other advantages of embodiments of the present invention are further described below.
Drawings
FIG. 1 is a schematic diagram of a system architecture of a gas hydrate micro-kinetic in situ test apparatus in an embodiment of the present invention.
FIG. 2 is a flow chart of a method of in situ testing of gas hydrate micro-dynamics in an embodiment of the invention.
Fig. 3a to 3d are raman spectrum identification graphs of hydrates under different systems tested in the examples of the present invention.
Reference numerals illustrate: 1. a piston container; 2. high-precision multiphase carbon dioxide injection pump; 3. a liquid nitrogen tank; 4. a liquid nitrogen pump; 5. a laser; 6. a microscope; 7. jacket test temperature control reaction kettle; 8. an XYZ electric displacement table; 9. operating the sliding table by precision displacement; 10. a data acquisition system; 11. high-precision full-automatic back pressure valve; 12. a raman spectrometer; 13. a data processing and computing computer; 14. a gas storage tank; 15. a pressure sensor; 16. a temperature sensor; 17. a pressure control needle valve; 18. a pressure control valve; 19. a high pressure gas cylinder.
Detailed Description
The following describes embodiments of the present invention in detail. It should be emphasized that the following description is merely exemplary in nature and is in no way intended to limit the scope of the invention or its applications.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the embodiments of the present invention, the meaning of "plurality" is two or more, unless explicitly defined otherwise.
Fig. 1 is a schematic system structure diagram of an in-situ test device for gas hydrate micro dynamics in an embodiment of the invention. It can be seen that the embodiment of the invention provides a gas hydrate micro-dynamics in-situ testing device, which comprises a reaction kettle, a gas-liquid two-phase injection unit, a temperature-pressure control and monitoring unit, a visual operation unit and a hydrate generation area intelligent identification and calculation unit, wherein the gas-liquid two-phase injection unit is connected with the reaction kettle and is used for injecting a multiphase sample into the reaction kettle, the temperature-pressure control and monitoring unit is used for controlling and monitoring the temperature and pressure in the reaction process of the reaction kettle, the reaction kettle is provided with an observable window, the visual operation unit is used for observing the morphological characteristics and the growth process of a hydrate reaction system through the observable window, the hydrate generation area intelligent identification and calculation unit is used for identifying the generation and decomposition of a hydrate according to the observation information of the visual operation unit, and the thermal dynamics information of the hydrate comprises one or more of the induction time, the nucleation area, the saturation and the decomposition behavior of the hydrate.
Aiming at the defects existing in the prior art, the embodiment of the invention designs a novel gas hydrate micro-dynamics in-situ test device, which is used for carrying out gas hydrate micro-dynamics in-situ test and is coupled with a gas-liquid two-phase injection unit, a temperature and pressure control and monitoring unit, a hydrate generation area intelligent identification and calculation unit and a visual operation unit on the basis of the existing in-situ Raman test device, so that different temperature and pressure and CO can be accurately depicted 2 CO under the condition of phase injection 2 Microcosmic nucleation, growth and decomposition behavior of hydrate followed by clearing CO 2 The thermodynamic characteristics of the hydrate, the development of high-efficiency thermodynamic promoters and the optimization of injection-sealing schemes lay an experimental foundation.
Specifically, the gas-liquid two-phase injection unit comprises a storage tank, a piston container 1 and a multi-phase carbon dioxide injection pump, wherein the storage tank is connected with the piston container 1, and the piston container 1 is connected with the reaction kettle through the multi-phase carbon dioxide injection pump; wherein, the storage tank includes gaseous phase storage tank and liquid phase storage tank. The gas phase storage tank can comprise a high-pressure gas cylinder 19 and a gas storage tank 14, and the multiphase carbon dioxide injection pump is preferably a high-precision multiphase carbon dioxide injection pump 2; the gas-liquid two-phase injection unit further comprises: a pressure control valve 18, a pressure control needle valve 17, a pressure sensor 15, and a temperature sensor 16; the reaction kettle is a jacketed temperature control reaction kettle 7; the temperature and pressure control and monitoring unit comprises a liquid nitrogen tank 3 and a liquid nitrogen pump 4, the liquid nitrogen tank 3 is connected with a jacket of a jacket type temperature control reaction kettle 7 through the liquid nitrogen pump 4, and the liquid nitrogen pump 4 drives liquid nitrogen to circulate so that a reaction system in the reaction kettle is in a set low temperature condition, and the temperature and pressure control and monitoring unit further comprises: a high-precision fully automatic back pressure valve 11; the visual operation unit comprises a CCD (Charge-Coupled Device) camera, a microscope 6, a Raman spectrometer 12, a laser 5, an XYZ electric displacement table 8 and a precise displacement operation sliding table 9, wherein the CCD camera is used for observing and recording the morphological expressions of the hydrate in different reaction stages in the whole injection-sealing process in real time, so as to carry out analysis and calculation by the intelligent recognition and calculation unit of the water-hydrate generation area; the microscope 6 is used for observing the local details of the nucleation and growth processes of the hydrate, so as to analyze and calculate the intelligent recognition and calculation unit of the hydrate generation area; the laser 5 is used for irradiating a sample to generate a Raman spectrum, and the Raman spectrometer 12 is used for collecting the Raman spectrum to monitor and identify the microstructure and the micro-dynamics reaction process of the hydrate, so that the hydrate generation area intelligent identification and calculation unit can analyze and calculate the hydrate generation area intelligent identification and calculation; the reaction kettle is connected with the XYZ electric displacement table 8, and the precise displacement operation sliding table 9 is used for operating the displacement of the XYZ electric displacement table 8 to control the position of the reaction kettle so as to adjust the observation field of view of the visual operation unit on the reaction kettle; the hydrate generation area intelligent recognition and calculation unit comprises a data acquisition system 10 and a data processing and calculation computer 13.
Mineral particles can be filled in the reaction kettle according to the embodiment of the invention, and multi-phase CO is injected 2 To simulate hydrate method CO in submarine sediment 2 And sealing, namely, monitoring the phase transformation of a sample in the reaction kettle in real time through a visual operation unit and an intelligent identification and calculation unit of a hydrate generation area, and evaluating the stability of geological carbon sealing.
The embodiment of the invention also provides a gas hydrate micro-dynamics in-situ test method, which uses the device to perform gas hydrate micro-dynamics in-situ test.
FIG. 2 is a flow chart showing a method for in situ testing of gas hydrate micro-dynamics in accordance with an embodiment of the present invention. The specific test flow of the gas hydrate micro-dynamics in-situ test device provided by the embodiment of the invention is as follows:
after the jacket type temperature control reaction kettle 7 is cleaned and dried, pure water and additive solution are injected, the jacket type temperature control reaction kettle 7 is connected with an XYZ electric displacement table 8, the position of the jacket type temperature control reaction kettle 7 is controlled through a precise displacement operation sliding table 9 (XYZ electric displacement table-operation part), so that the jacket type temperature control reaction kettle 7 is positioned at the center of a visual field of a microscope 6, and after the jacket type temperature control reaction kettle 7 is sealed, the jacket type temperature control reaction kettle 7 is purged for 3 times by using 0.5MPa gas, so that the influence of gas impurities in a system is removed. The liquid nitrogen tank 3 and the liquid nitrogen pump 4 of the temperature control and monitoring unit are connected with the jacketed temperature control reaction kettle 7, so that the temperature change in the reaction process is accurately controlled and monitored. Then injecting the gas-liquid two-phase injection unit and CO 2 The hydrate reaction system is connected, a pressure control valve 18 is opened, and a pressure control needle valve 17 is used for controlling CO in a high-pressure gas cylinder 19 2 The gas or flue gas mixture is injected into the gas storage tank 14, and the storage tank gas injection is monitored by the pressure sensor 15 and the temperature sensor 16. When simulating in situ hydrate process CO 2 When in sealing, the high-precision full-automatic back pressure valve 11 is opened to enable CO to be discharged 2 Is injected into the piston container 1 in the form of gas-liquid or gas-liquid mixture, and the multiphase CO in the piston container 1 is injected into the piston container 1 2 The high-precision multiphase carbon dioxide is injected into a jacket temperature-controlled reaction kettle 7 through a high-precision multiphase carbon dioxide injection pump 2. The liquid nitrogen pump 4 drives the liquid nitrogen 3 to circulate so as to cool the reaction system to a set low temperature condition, the precise displacement operation sliding table 9 is regulated so as to enable the XYZ electric displacement table 8 to be linked with the reaction kettle, the reaction system is regulated to the height of the working distance of the microscope 6, the laser 5 is turned on, the Raman spectrometer 12 is regulated so as to monitor and collect the Raman spectrum of the hydrate system, after the hydrate is generated in the system, the image recognition system can recognize the hydrate generation area, signals are transmitted to the data processing and computing computer 13, the XYZ electric displacement table 8 moves so that the hydrate generation area is in the center of the visual field, and the Raman spectrum evolution of the hydrate generation (and decomposition) dynamic process is recorded in real time.
The embodiment of the invention has the following beneficial effects:
(1) The gas hydrate micro-dynamics in-situ testing device and the method thereof provided by the embodiment of the invention are coupled with the gas-liquid two-phase injection unit and the temperature-pressure control and monitoring unit, and can inject gas phase or liquid phase under the specified temperature-pressure conditionCO 2 And realize CO under the condition of controllable temperature and pressure 2 Synthesis and decomposition of hydrates.
(2) The visual operation unit shoots a visual window of the kettle body through a high-definition CCD camera with adjustable focal length, and observes and records CO in the whole injection-sealing process in real time 2 Hydrate morphology characterization, CO was observed 2 The nucleation and growth process of the hydrate, and clear CO in different reaction systems are obtained 2 The evolution rule of the morphology of the hydrate crystal is further used for elucidating the CO under different reaction systems 2 The mechanism of the thermodynamic of the hydrate lays a morphological foundation.
(3) The intelligent recognition and calculation unit of the hydrate generation region can analyze the nucleation time and the generation region of the hydrate by utilizing the shape picture shot by the intelligent image recognition algorithm in real time by analyzing the CCD camera, calculate the saturation of the hydrate, and carry out cross verification on the recognition calculation result and the temperature and pressure monitoring result so as to ensure the accuracy of the recognition calculation result.
Compared with the conventional Raman test technology, the embodiment of the invention realizes the integrated integration of the gas-liquid two-phase injection unit, the temperature and pressure control and monitoring unit, the intelligent identification and calculation unit of the hydrate generation area and the visual operation unit, and can accurately describe controllable temperature and pressure and multiphase CO from macroscopic (temperature and pressure, saturation and morphology) and microscopic scale (cage occupying behavior) at the same time 2 CO under injection conditions 2 -CO 2 Dynamic evolution law of a hydrate system can more comprehensively reveal CO under different reaction systems 2 The mechanism of the thermodynamic of the hydrate is a site-scale hydrate method CO under the coupling action of complex factors 2 The containment provides theoretical support. Meanwhile, the gas hydrate micro-dynamics in-situ testing device and the method thereof provided by the embodiment of the invention realize dynamic controllable hydrate identification and monitoring by coupling the multi-phase gas and liquid injection system (namely, the gas-liquid two-phase injection unit), and the device has flexible operation, environment-friendly experimental technology and suitability for CO in a hydrate method 2 The sealing technology and the hydration solidification hydrogen storage technology adopt Raman spectrum to monitor and identify the microstructure and dynamic reaction process of the hydrate in the experiment, so as to analyze CO 2 Microcosmic mechanism and saturation evolution rule of hydrate guest molecules entering a cage.
In various embodiments of the present invention, the injection system may inject the gas as follows: methane, carbon dioxide, hydrogen, ethane, nitrogen, etc., or a mixture of several of the above gases, the injectable liquids are: liquid carbon dioxide, liquid water, promoter or inhibitor solution, or pre-loaded with solution in the reaction system; by coupling multi-phase CO 2 Constant pressure or constant flow injection, in-situ reaction and identification of the hydrate, and microstructure test by combining with Raman spectrum, and multi-scale (microscopic molecular vibration, mesoscopic morphology and macroscopic dynamics) reveal the mechanism of the gas hydrate generation and decomposition process.
Referring to fig. 3a to 3d, raman spectrum identification diagrams of hydrates under different systems in the embodiment of the present invention are shown,
experimental example 1:
tetrahydrofuran (THF) -CO 2 Hydrate microstructure and kinetics of formation
(1) And cleaning and drying the reaction kettle, injecting the prepared tetrahydrofuran solution into the reaction kettle, covering the reaction kettle, sealing the reaction kettle by a cover, and sealing a reaction system.
(2) The circulating temperature of a liquid nitrogen pump is regulated by program temperature control, the reaction system is cooled to 2 ℃ from room temperature, the data acquisition system records the reaction temperature and pressure change in real time, the raman characteristic peak monitoring shows that the phase of THF is changed from solution to hydrate phase along with the temperature rise when the THF generates the hydrate, and the saturation of the THF hydrate is captured by the image recognition system and changed in real time.
(3) After the temperature is stable, CO is injected through the gas injection system 2 The reaction kettle is purged 3 times under the pressure of 0.5 MPa.
(4) Slow CO injection 2 The gas was brought to 4.5MPa.
(5) Along with CO 2 Gas injection, THF-CO 2 Binary hydrate formation, an exothermic process, observed temperature rise, CO 2 From the gas phase into the hydrate phase, occupying the binary hydrate gabion, CO 2 Fermi resonance (1273, 1381 cm) -1 ) Is detected.
(6) Along with CO 2 Continuously feeding the material into the cage, and the pressure in the systemGradually reducing the area of the hydrate identified by the image, enlarging the area of the hydrate identified by the image, and calculating key parameters such as the growth rate of the hydrate, the cage ratio of the guest molecule and the like by combining the growth dynamics process of the hydrate.
(7) When the pressure change in the kettle is less than 0.1MPa/h, the generation of the hydrate is basically finished.
(8) The hydrate can be decomposed by controlling the temperature, and the CO is calculated according to the temperature and the pressure 2 The rate of hydrate dissociation and the rate of release of different guest molecules from the cage.
The in-situ testing device and the method for the micromechanics of the gas hydrate provided by the embodiment of the invention aim to realize the observation, recording and automatic analysis of the gas hydrate in a laboratory, such as the simulation of CO 2 The hydrate sealing process comprises the steps of CO 2 Multi-phase injection, phase inversion, long-term stability monitoring of hydrates, and the like. The invention can reduce the workload of the experimenter in observation and analysis, provide more detailed information in the whole process of hydrate generation and decomposition, clarify the morphological evolution rule of the hydrate, reveal the basic thermodynamic characteristics of the hydrate, and provide a site scale hydrate method CO under the coupling effect of multiple complex factors for practical conditions 2 The containment provides theoretical support.
Compared with the prior art, the gas hydrate micro-dynamics in-situ testing device and the method provided by the embodiment of the invention have the following innovation points:
a. the embodiment of the invention is provided with a whole-course visual operation unit and a microscope to acquire morphology detail information. The high-definition CCD camera with adjustable focal length is used for shooting the visible window of the kettle body in the whole process, so that the CO in different reaction systems in the whole injection-sealing process can be observed and recorded in real time 2 The morphological characteristics of the hydrate, and the local details of the nucleation and growth processes of the hydrate can be clearly observed by a microscope, so that more observation supplementary evidence is provided for analysis.
b. The embodiment of the invention is coupled with the intelligent recognition and calculation unit of the hydrate generation area, can utilize an intelligent image recognition algorithm to process the morphology picture shot by the CCD camera in real time, automatically search and recognize the generated hydrate, and further analyze the nucleation time and the growth time of the hydrateZoning and calculating hydrate saturation. The Raman spectrum surface scanning mapping function in the identification unit can simulate the CO of the change of the submarine deposition environment 2 Effect of hydrate storage stability.
c. The embodiment of the invention realizes the integrated integration of a gas-liquid two-phase injection unit, a temperature-pressure control and monitoring unit, a visual operation unit and an intelligent identification and calculation unit of a hydrate generation area, and can accurately describe controllable temperature-pressure and multiphase CO from macroscopic (temperature-pressure, saturation and morphology) and microscopic scale (cage-occupying behavior) at the same time 2 CO under injection conditions 2 -CO 2 Dynamic evolution law of a hydrate system.
d. Although the embodiment of the invention uses CO 2 Hydrate is taken as an example, but experimental apparatus and methods are not limited to study of CO 2 The hydrate has adaptability to injection, generation and decomposition researches of other gas hydrates, and can be expanded only by properly modifying an image recognition algorithm, so that the application range is wide.
The embodiment of the invention provides a gas hydrate micro-dynamics in-situ test device and a method thereof, which comprehensively consider CO 2 Polymorphic injection, CO 2 The hydrate phase transformation identification and the sealing stability are obtained, and the multi-scale and whole-process information of macroscopic temperature and pressure evolution, mesoscopic morphology characteristics and microscopic Raman spectrum is obtained. And the CO proposed by the invention 2 The in-situ test method of the hydrate can control CO aiming at the actual water depth and the buried depth of different sea areas 2 Injection sequestration pressure and deposition environment, revealing CO in laboratory 2 The thermodynamic characteristics of the hydrate provide microscopic Raman spectrum characteristics, and the surface scanning mapping function of the Raman spectrum can simulate the change of the submarine deposition environment to CO 2 Effect of hydrate storage stability. The invention provides in-situ CO 2 The hydrate in-situ test device and method are simple to operate and low in cost, and can be used for sealing and storing CO in actual submarine deposition environment 2 The phase evolution process provides theoretical guidance.
It can be seen that the embodiments of the present invention have the following bright points:
1. CO for realizing static temperature-pressure controllable system 2 In the formation of hydrate,Carrying out thermodynamic and morphological observation on the whole decomposition process;
2. coupling multiple phase CO 2 The injection unit can study the influence of different phases of gas on the nucleation, generation, decomposition and stability of the hydrate;
3. the key areas of the hydrate are automatically searched and identified by combining the intelligent image identification algorithm, and related parameters are calculated in an auxiliary mode, so that the data processing workload of scientific researchers is reduced;
4. the experimental device provided by the invention is a visual device additionally provided with the CCD camera with adjustable focal length, the microscope and the in-situ Raman tester, and can obtain the morphological and spectral characteristics of hydrate in real time, high definition and detail, wherein the in-situ Raman spectrum surface scanning mapping function can accurately identify CO 2 Phase transformation in submarine sealing process to fully reveal hydrate method CO in submarine deposition environment 2 A microcosmic phase change mechanism in the sealing process;
5. the integrated intelligent in-situ Raman spectrum experimental device and method integrating the gas-liquid two-phase injection unit, the temperature-pressure control and monitoring unit, the visual operation unit and the hydrate generation area intelligent identification and calculation unit are provided for the first time, and CO in different reaction systems can be obtained 2 The macro temperature and pressure evolution of the hydrate, mesoscopic morphological characteristics and microscale and whole-process information of the microcosmic cage occupying behavior.
The invention provides a gas hydrate micro-dynamics in-situ test device and method, which are used for controlling and monitoring the temperature and pressure change of the whole process of a system through circulating liquid nitrogen, a high-precision pressure control valve and a multi-point temperature and pressure sensor, and are used for controlling and monitoring the reaction device and gaseous CO 2 Liquid CO 2 Storage tank connection for realizing multi-phase CO 2 Injecting, observing the morphology of the reaction system through a sapphire glass window, and identifying and calculating CO through an intelligent image identification algorithm and a volume conservation method 2 Hydrate nucleation time, nucleation region, and saturation.
The embodiment of the invention also makes corresponding adjustment to realize the following deformation scheme:
(1) By using mixed gas injection, different gas components are distinguished in a mode of generating hydrate, namely, gas hydrate with lower thermodynamic conditions is generated, and gas types difficult to generate hydrate are in gas phase;
(2) First let in CH 4 The gas generates hydrate and then is injected into CO 2 Combined CO from depressurization recovery 2 Sealing the hydrate, identifying mining efficiency and sealing proportion in real time, and identifying the composition of the hydrate guest molecules in real time;
the deformation scheme still needs to be coupled with a multiphase injection system, the hydrate generation dynamics is automatically identified by adopting an image identification mode, and the intelligent identification and monitoring of the hydrate structure are carried out by combining a high-precision XYZ electric displacement platform; the embodiment and the modification scheme of the invention are characterized in that: the multi-phase (gas, liquid) and controllable (constant pressure and constant flow) injection, the temperature and pressure controllable reaction system, and the full-automatic identification of the hydrate structure.
The gas hydrate micro-dynamics in-situ test device and method provided by the embodiment of the invention can also be used for a hydrate method CO 2 And the corresponding fields of trapping and sealing, gas storage and transportation by a solid hydrate method, sea water desalination by a hydrate method, cold accumulation by a hydrate method, gas separation by a hydrate method and the like.
The foregoing is a further detailed description of the invention in connection with specific/preferred embodiments, and it is not intended that the invention be limited to such description. It will be apparent to those skilled in the art that several alternatives or modifications can be made to the described embodiments without departing from the spirit of the invention, and these alternatives or modifications should be considered to be within the scope of the invention. In the description herein, reference to the terms "one embodiment," "some embodiments," "preferred embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Those skilled in the art may combine and combine the features of the different embodiments or examples described in this specification and of the different embodiments or examples without contradiction. Although embodiments of the present invention and their advantages have been described in detail, it should be understood that various changes, substitutions and alterations can be made herein without departing from the scope of the invention as defined by the appended claims.
Claims (10)
1. The gas hydrate micro-dynamics in-situ testing device is characterized by comprising a reaction kettle, a gas-liquid two-phase injection unit, a temperature-pressure control and monitoring unit, a visual operation unit and a hydrate generation area intelligent identification and calculation unit, wherein the gas-liquid two-phase injection unit is connected with the reaction kettle and is used for injecting multiphase samples into the reaction kettle, the temperature-pressure control and monitoring unit is used for controlling and monitoring the temperature and pressure in the reaction process of the reaction kettle, the reaction kettle is provided with an observable window, the visual operation unit is used for observing the morphological characteristics and the growth process of a hydrate reaction system through the observable window, and the hydrate generation area intelligent identification and calculation unit is used for identifying the generation and decomposition of a hydrate and calculating the thermodynamic information of the hydrate according to the observation information of the visual operation unit.
2. The gas hydrate micro-kinetic in situ test device according to claim 1, wherein the thermodynamic information of the hydrate comprises one or more of induction time, nucleation area, saturation, guest-molecule cage ratio, decomposition behavior of the hydrate.
3. The gas hydrate micro-dynamics in-situ test device according to claim 1 or 2, wherein the gas-liquid two-phase injection unit comprises a storage tank, a piston container and a multi-phase carbon dioxide injection pump, the storage tank is connected with the piston container, and the piston container is connected with the reaction kettle through the multi-phase carbon dioxide injection pump; wherein the storage tank comprises a gas phase storage tank and a liquid phase storage tank.
4. A gas hydrate micro-kinetic in-situ test device according to any one of claims 1 to 3, wherein the reaction kettle is a jacketed temperature-controlled reaction kettle, the temperature-pressure control and monitoring unit comprises a liquid nitrogen tank and a liquid nitrogen pump, the liquid nitrogen tank is connected with a jacket of the jacketed temperature-controlled reaction kettle through the liquid nitrogen pump, and the liquid nitrogen pump drives liquid nitrogen to circulate so that a reaction system in the reaction kettle is in a set low-temperature condition.
5. The gas hydrate micro-dynamics in-situ test device according to any one of claims 1 to 4, wherein the visual operation unit comprises a CCD camera and an XYZ electric displacement table, the CCD camera is used for observing and recording the morphological performance of the hydrate in different reaction stages in the whole injection-sealing process in real time, and the XYZ electric displacement table can automatically move according to the existence of the hydrate in an observation area so as to be used for the intelligent recognition and calculation unit of the hydrate generation area to analyze and calculate.
6. The gas hydrate micro-kinetic in-situ test device according to any one of claims 1 to 5, wherein the visual operation unit comprises a microscope for observing local details of a hydrate nucleation and growth process for analysis and calculation by the hydrate generation region intelligent recognition and calculation unit.
7. The gas hydrate micro-kinetic in-situ test device according to any one of claims 1-6, wherein the visualization operation unit comprises a raman spectrometer and a laser, the laser is used for irradiating a sample to generate a raman spectrum, and the raman spectrometer is used for collecting the raman spectrum to monitor and identify the hydrate microstructure and micro-kinetic reaction process for the intelligent identification and calculation unit of the hydrate generation area to analyze and calculate.
8. The gas hydrate micro-dynamics in-situ test apparatus according to any one of claims 1 to 7, wherein the visual operation unit comprises an XYZ electric displacement table and a precision displacement operation sliding table, the reaction kettle is connected with the XYZ electric displacement table, the precision displacement operation sliding table is used for operating the displacement of the XYZ electric displacement table to control the position of the reaction kettle so as to adjust the observation field of view of the visual operation unit on the reaction kettle, and preferably, intelligent recognition of a plurality of states of CO is realized 2 And CO 2 A hydrate.
9. The gas hydrate micro-dynamics in-situ test device according to any one of claims 1-8, wherein the reaction kettle is filled with mineral particles, and a multiphase CO2 sample is injected to simulate hydrate method CO 2 And sealing, namely monitoring the phase state conversion of the sample in the reaction kettle in real time through the visual operation unit and the hydrate generation area intelligent identification and calculation unit, and evaluating the stability of geological carbon sealing.
10. A method of gas hydrate micromechanics in situ testing, characterized in that the gas hydrate micromechanics in situ testing is performed using the device according to any one of claims 1 to 9.
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