CN114088684A - Carbon dioxide sequestration experiment simulation device and method - Google Patents
Carbon dioxide sequestration experiment simulation device and method Download PDFInfo
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- CN114088684A CN114088684A CN202111303301.8A CN202111303301A CN114088684A CN 114088684 A CN114088684 A CN 114088684A CN 202111303301 A CN202111303301 A CN 202111303301A CN 114088684 A CN114088684 A CN 114088684A
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 207
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 105
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 103
- 230000009919 sequestration Effects 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 41
- 238000002474 experimental method Methods 0.000 title claims abstract description 33
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- 238000012360 testing method Methods 0.000 claims abstract description 25
- 230000008569 process Effects 0.000 claims abstract description 24
- 238000005070 sampling Methods 0.000 claims abstract description 22
- 238000007789 sealing Methods 0.000 claims abstract description 22
- 239000007788 liquid Substances 0.000 claims abstract description 18
- VTVVPPOHYJJIJR-UHFFFAOYSA-N carbon dioxide;hydrate Chemical compound O.O=C=O VTVVPPOHYJJIJR-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000523 sample Substances 0.000 claims description 77
- 239000013049 sediment Substances 0.000 claims description 48
- 239000007791 liquid phase Substances 0.000 claims description 40
- 238000002347 injection Methods 0.000 claims description 19
- 239000007924 injection Substances 0.000 claims description 19
- 238000001069 Raman spectroscopy Methods 0.000 claims description 15
- 238000013401 experimental design Methods 0.000 claims description 15
- 238000005192 partition Methods 0.000 claims description 15
- 238000011049 filling Methods 0.000 claims description 13
- 239000004576 sand Substances 0.000 claims description 13
- 239000013535 sea water Substances 0.000 claims description 13
- 238000011160 research Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 238000001237 Raman spectrum Methods 0.000 claims description 7
- 239000011148 porous material Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 4
- 230000001276 controlling effect Effects 0.000 claims description 4
- 238000012216 screening Methods 0.000 claims description 4
- 239000002344 surface layer Substances 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000004458 analytical method Methods 0.000 claims description 2
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01D—MEASURING NOT SPECIALLY ADAPTED FOR A SPECIFIC VARIABLE; ARRANGEMENTS FOR MEASURING TWO OR MORE VARIABLES NOT COVERED IN A SINGLE OTHER SUBCLASS; TARIFF METERING APPARATUS; MEASURING OR TESTING NOT OTHERWISE PROVIDED FOR
- G01D21/00—Measuring or testing not otherwise provided for
- G01D21/02—Measuring two or more variables by means not covered by a single other subclass
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/06—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a liquid
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Abstract
The invention discloses a carbon dioxide sequestration experiment simulation device and a method, which comprises a high-pressure reaction kettle, a gas supply and liquid supply system, a temperature and pressure acquisition system and a sample acquisition and test system, wherein the gas supply and liquid supply system is connected with the high-pressure reaction kettle; combining a plurality of groups of independent temperature control jackets to realize a simulation experiment on the instability condition of the carbon dioxide hydrate; the test of the concentration of carbon dioxide in the water body in the experimental process is completed through a real-time sampling device; the method adopts the method of excessive water to realize the simulation of the carbon dioxide on the seabed sealing, is more consistent with the process in the actual sealing, can simulate the processes of diffusion mechanism, hydrate formation and the like of the carbon dioxide in different forms on the seabed sealing, can simulate the carbon dioxide sealing instability process through the temperature control, and can more comprehensively know the law of the carbon dioxide seabed sealing process.
Description
Technical Field
The invention belongs to the technical field of carbon dioxide sequestration, and particularly relates to an experimental device and method for simulating the sequestration state of carbon dioxide on the seabed.
Background
Fossil fuels are one of the most important energy sources today, and provide about 80-85% of the world's energy usage today. Since fossil fuels have great advantages in energy density, storage, and price, it will remain the main means for human energy in the foreseeable future. However, the heavy use of fossil fuels necessarily faces the heavy emission of carbon dioxide. The carbon dioxide content of the atmosphere has risen by about 30% since the industrial revolution (Siegenthaler and Oeschager, 1987; Keeling et al, 1995), and most of these have come from the combustion of fossil fuels. The impact of carbon dioxide on global climate change is receiving increasing attention due to its greenhouse effect, and the threat posed by global warming has increased public concern about anthropogenic carbon emissions.
In 9 months in 2020, China announces the goals of realizing carbon peak reaching before 2030 and realizing carbon neutralization before 2060 to the world, which is the strategic demand of long-term growth in China. To achieve this goal, not only is it necessary to improve energy efficiency and the use of new energy to reduce Carbon dioxide emissions, but it is more important to develop Carbon Capture and sequestration technology (CCS). This technology does not require a reduction in the amount of fossil fuel used, and the captured carbon is expected to be sequestered as a solid at lower processing costs and to be of commercial value.
According to different modes of sequestration, CO2The sealing techniques of (a) can be roughly classified into 3 types: (1) geological sequestration, in geological formations such as abandoned oil and natural gas fields, non-exploitable coal fields, and high salt aquifer formations; (2) sequestration of the ocean, i.e. CO via fixed pipelines or moving vessels2And injecting the mixture into a water body or an ocean bottom (below 1000 m). The effectiveness and the influence on the seabed ecological environment are still in the research stage; (3) and (4) sealing the minerals, namely solidifying carbon dioxide into inorganic carbonate.
At present, a plurality of technologies related to carbon dioxide emission reduction or sequestration exist in China, for example, a method and a device for carbon dioxide emission reduction and comprehensive utilization (patent number ZL 200910195171.3), the invention proposes that ammonia gas is contacted with wet soil to be ammoniated to generate NH4OH, obtaining ammoniated soil; then the carbon dioxide is contacted with ammoniated soil to carbonize the ammoniated soil to obtain NH4HCO3Can be fixed in the soil. Patent "sequestration of CO2The method of (1) (patent No. ZL 200880023216.2), which proposes precipitating a storage-stable carbon dioxide sequestering product in an alkaline earth metal-containing water and then disposing of the product by placing the product in a disposal site or using the product as a component of a manufactured composition. The patent 'a method for reducing emission and recycling carbon dioxide in flue gas of a coal-fired power plant and a special system thereof' (patent number ZL200610047522.2), the patent proposes that after pre-dedusting is carried out on the tail part of a coal-fired boiler, amino substance solution is sprayed into the flue gas in a carbon dioxide absorption system to absorb carbon dioxide generated in coal combustion in the form of ammonium salt, and 20-95% of carbon dioxide in the flue gas is reduced; the carbon dioxide absorbed in the form of ammonium salt is separated and purified into high-purity carbon dioxide gas, and can be used for industry, chemical industry, food processing, oil extraction and oil displacement.
Subsea sequestration of carbon dioxide is stably sequestered in a subsea formation by injecting carbon dioxide into the subsea formation, by high pressure carbon dioxide forming carbon dioxide hydrates with seawater in the formation. Compared with other carbon dioxide sequestration technologies, the technology for sequestering carbon dioxide by utilizing the seabed has many characteristics. Although the storage density of the carbon dioxide hydrate is not superior to that of other carbon dioxide sequestration storage modes, the thermodynamic conditions required for the stable existence of the carbon dioxide hydrate are mild, and carbon dioxide can be spontaneously combined with free water molecules in the formation to form the carbon dioxide hydrate in the low-temperature high-pressure submarine formation environment. And in the submarine sediment, the temperature and the pressure are basically stable, and the long-term sequestration of the carbon dioxide can be realized once the carbon dioxide forms the hydrate.
At present, there are also a few technical solutions for seabed sequestration of carbon dioxide, for example, patent of invention "system for seabed sequestration of greenhouse gas and method for using the same" (patent No. CN201010179202.9), which utilizes the characteristics of low temperature and high pressure of seawater in deep sea to make seawater and greenhouse gas, especially carbon dioxide gas, generate carbon dioxide hydrate, and since the density of carbon dioxide hydrate is greater than that of seawater, the generated carbon dioxide hydrate will deposit on seabed and sequester in solid form. The patent "a deep sea carbon sequestration and power generation system" (patent No. CN201922162695.4) proposes to generate power by waste heat of power plant exhaust gas and to separate carbon dioxide, apply the separated carbon dioxide to the subsea geothermal brayton cycle, and finally store the carbon dioxide in the deep sea sequestration hole in the form of carbon dioxide hydrate.
The research on the seabed sequestration of carbon dioxide is at the starting stage at present, and a gas excess method is mostly adopted, which is not consistent with the actual condition of seabed water excess, although seabed temperature and pressure conditions can meet the generation of carbon dioxide hydrate, the migration process and the formation and decomposition characteristics of the carbon dioxide hydrate are still to be researched after the carbon dioxide is injected into the seabed specific environment. The knowledge of the processes has important significance for determining the mode and the position of carbon dioxide seabed injection and evaluating the sealing amount and the safety of carbon dioxide seabed sealing.
Disclosure of Invention
The invention provides a carbon dioxide sequestration experiment simulation device and a carbon dioxide sequestration experiment simulation method, aiming at overcoming the defects that the existing carbon dioxide sequestration method is not consistent with the actual situation and the like.
The invention is realized by adopting the following technical scheme: the utility model provides a carbon dioxide seals up deposits experiment analogue means, includes high pressure batch autoclave, the air feed liquid supply system that is connected with high pressure batch autoclave, temperature pressure collection system and sample acquisition and test system, and high pressure batch autoclave includes reation kettle barrel and end cover, air feed liquid supply system includes constant pressure pump, liquid phase filling opening, and a vacuum pump is connected through the valve to the liquid phase filling opening:
the temperature and pressure acquisition system comprises a plurality of groups of water bath jackets with independent temperature control, the water bath jackets are sequentially arranged along the outer side wall of the high-pressure reaction kettle from top to bottom, circulating cooling liquid is injected through a matched low-temperature constant-temperature bath, and the temperatures of different positions of a sample in the high-pressure reaction kettle are controlled; a plurality of groups of pressure sensors and temperature sensors connected with a data collector are arranged at different height positions in the high-pressure reaction kettle;
in order to change the experimental defect of traditional device gas excess, not co-altitude is equipped with the multiunit mounting groove on the inside wall of reation kettle barrel, and the inside two sets of detachable movable partition that set up of reation kettle barrel, movable partition adopt ventilative material of permeating water to install the mounting groove department at co-altitude position according to the experimental design requirement, be used for restricting the position of deposit.
Furthermore, a piston and a piston rod are arranged at the upper end of the inner cavity of the high-pressure reaction kettle, a hydraulic cavity is formed between the end cover and the piston, the hydraulic cavity is connected with the constant-pressure pump through a pipeline, and constant pressure is applied to the water in the high-pressure reaction kettle through the piston; the piston rod is of a hollow structure, one end of the piston rod is connected with the piston, the other end of the piston rod extends out of the end cover, and the hollow part of the piston rod is communicated with the piston and the end cover to form a liquid phase inlet and a liquid phase outlet of the high-pressure reaction kettle and is connected with the liquid phase injection port.
Further, the sample collecting and testing system comprises a liquid phase collecting terminal, a high-voltage sample bin, a Raman spectrum probe and a Raman tester; the Raman spectrum probe is arranged in the high-pressure sample bin and is connected with the Raman tester, the liquid phase acquisition terminal comprises a sampling filter screen and a sampling valve, a plurality of groups of sampling ports are arranged in the axial direction of the high-pressure reaction kettle, the sampling filter screen is installed in the reaction kettle barrel and is led out through the sampling ports, the sampling ports are connected with the high-pressure sample bin through the sampling valve, the acquired samples are tested in real time through the in-situ Raman probe, and the samples are analyzed based on the Raman spectrometer.
Furthermore, a sample discharge port is formed in the bottom of the high-pressure sample bin, an air release valve is arranged at the sample discharge port, and after the sample is discharged by controlling the switch of the air release valve, sampling and testing are performed again.
Further, the gas and liquid supply system comprises a high-pressure gas cylinder, a pressure reducing valve, a liquefaction system and an injection pump; the high-pressure gas cylinder is connected with a liquefaction system through a pressure reducing valve, and liquefied carbon dioxide is divided into two paths through an injection pump and is connected with the high-pressure reaction kettle.
Furthermore, a resistivity test port is further arranged on the side wall of the high-pressure reaction kettle, and the sealing capacity of carbon dioxide in the seabed environment is evaluated by testing the generation condition of carbon dioxide hydrate in sediments in the high-pressure reaction kettle body through the resistivity test.
The invention also provides an experimental method based on the carbon dioxide sequestration experiment simulation device, which comprises the following steps:
step A, preparation of a sediment sample: screening natural or artificial sand samples with proper grain sizes according to the experimental design requirements, or mixing artificial sand samples with different grain sizes according to the actual sediment composition to simulate the pore conditions of the submarine sediment, cleaning the sediment sample, and drying the sediment sample in a drying box for later use;
step B, sediment filling: adjusting the position of a movable partition plate in the high-pressure reaction kettle according to the experimental design requirements, and filling and compacting a sediment sample to a required position;
step C, injecting a water sample:
(1) closing the high-pressure reaction kettle, opening a valve with an upper cover connected with a vacuum pump, opening the vacuum pump to vacuumize the high-pressure reaction kettle, and closing the valve and the vacuum pump;
(2) injecting deionized water or artificial seawater into the high-pressure reaction kettle, and stopping injecting when the liquid level in the high-pressure reaction kettle is higher than the sediment;
(3) opening the vacuum pump and the connecting valve again to vacuumize, discharging bubbles in the sediment, standing for a plurality of hours, and repeating the process until the sediment is completely filled with the water sample;
(4) filling a water sample into the high-pressure reaction kettle, and opening the constant pressure pump to push a piston at the upper end of the high-pressure reaction kettle so that the pressure in the high-pressure reaction kettle reaches the pressure required by the experiment;
step D, experimental simulation:
(1) according to the experimental design, a circulating water bath is started to enable the temperature in the high-pressure reaction kettle to reach a simulation condition;
(2) and opening a carbon dioxide liquefaction system and an injection pump, injecting liquid-phase carbon dioxide into the high-pressure reaction kettle, recording the amount of the injected liquid-phase carbon dioxide through a flow meter, and starting a hydrate sealing experiment.
And further, in the process of carrying out the sealing experiment in the step D, starting a sample collecting and testing system at fixed time intervals, taking the liquid phase at the corresponding position in the high-pressure reaction kettle into the high-pressure sample bin, testing by using a Raman probe, and simultaneously recording the temperature and pressure values of each measuring point in the high-pressure reaction kettle.
Furthermore, in the step D, the temperature in the high-pressure reaction kettle is regulated by controlling a plurality of groups of water bath jackets so as to research the sealing or dissipation condition of the carbon dioxide under different conditions.
Further, in actual work, the simulation research of the sealing condition when the liquid-phase carbon dioxide is injected into the surface layer or the inner part of the sediment is realized through the adjustment of the position of the movable partition plate.
Compared with the prior art, the invention has the advantages and positive effects that:
1. the method adopts the method of excessive water to realize the simulation of the carbon dioxide sequestration at the seabed, and the process is more consistent with the process in the actual sequestration;
2. the experimental process is controlled by a movable partition plate in the reaction kettle so as to comprehensively simulate the process of injecting liquid-phase carbon dioxide into each position of the sediment;
3. the multiple groups of independent temperature control jackets can realize a simulation experiment on the instability condition of the carbon dioxide hydrate;
4. the real-time sampling device in the reaction kettle is combined to complete the test of the concentration of carbon dioxide in the water body in the experimental process, which is helpful for estimating the dissipation capacity of the carbon dioxide;
the method can simulate the migration and diffusion process of the carbon dioxide after the carbon dioxide is injected into the seabed surface layer or sediment and the formation process of the carbon dioxide hydrate relatively truly, is beneficial to knowing the evolution law and the migration mechanism of the carbon dioxide during the sealing and storage of the seabed stratum, and has practical application value.
Drawings
FIG. 1 is a schematic structural diagram of a simulation apparatus for a carbon dioxide sequestration experiment according to an embodiment of the present invention;
wherein, 1, a liquid phase injection port; 2. a constant pressure pump; 3. an end cap; 4. a Raman spectrometer; 5. a Raman spectrum probe; 6. a high pressure sample compartment; 7. a sampling valve; 8. sampling a filter screen; 9. a temperature sensor; 10. a pressure sensor; 11. a movable partition plate; 12. a data acquisition unit; 13. a liquefaction system; 14. a gas phase injection port; 15. an atmospheric valve; 16. a vacuum pump; 17. a high pressure liquid flow meter; 18. a reaction kettle barrel; 19. a water bath jacket; 20. a piston rod; 21. a piston.
Detailed Description
In order to make the above objects, features and advantages of the present invention more clearly understood, the present invention will be further described with reference to the accompanying drawings and examples. It should be noted that the embodiments and features of the embodiments of the present application may be combined with each other without conflict. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced in other ways than those described herein, and thus, the present invention is not limited to the specific embodiments disclosed below.
Embodiment 1, a simulation apparatus for a carbon dioxide sequestration experiment, as shown in fig. 1, includes a high-pressure reaction vessel, a gas and liquid supply system connected to the reaction vessel, a temperature and pressure acquisition system, and a sample acquisition and test system;
the high-pressure reaction kettle comprises a reaction kettle barrel 18 with a cylindrical inner cavity and an end cover 3 arranged at the upper end of the reaction kettle barrel 18, wherein a piston 21 is arranged at the upper end of the inner cavity of the high-pressure reaction kettle, a hydraulic cavity is formed between the end cover 3 and the piston 21 and is connected with a constant pressure pump 2 through a pipeline, constant pressure is applied to a water body in the high-pressure reaction kettle through the piston 21, so that a pressure environment similar to the seabed is formed in the high-pressure reaction kettle, and the constant pressure pump controls the pressure in the kettle body to keep constant by applying pressure to seawater sealed in the kettle body; the piston rod 20 is a hollow structure, one end of the piston rod is connected with the piston 21, the other end of the piston rod extends out of the end cover 3, the hollow part of the piston rod 20 is communicated with the piston 21 and the end cover 3 to form a liquid phase inlet and outlet of the high-pressure reaction kettle and is connected with the liquid phase injection port 1, in order to completely discharge the air in the high-pressure reaction kettle, the liquid phase injection port 1 is connected with the vacuum pump 16 through a valve, and the air in the pores can be discharged by vacuumizing the kettle body after sediment and part of water are added;
the gas and liquid supply system comprises a high-pressure gas cylinder, a pressure reducing valve, a liquefaction system 13 and a liquid-phase carbon dioxide injection pump; the high-pressure gas cylinder is connected with the liquefaction system 13 through a pressure reducing valve, and the liquefied carbon dioxide is divided into two paths through an injection pump to be connected with the reaction kettle; the liquid phase injection port of the high-pressure reaction kettle is also divided into two paths, one path is connected with the vacuum pump 16 through a valve, and the other path is connected with the constant flow pump through the valve and is injected into the liquid phase; the lower part of the reaction kettle cylinder 18 is provided with two carbon dioxide injection ports which are connected with the liquefaction system 13, and carbon dioxide gas can be injected into different positions of the sample in the high-pressure reaction kettle through the liquefaction system 13, the high-pressure liquid flowmeter 17 and the control valve. In consideration of the fact that the gas and liquid supply pipeline is a relatively common system module, the attached drawing of the embodiment is partially simplified, and the function and purpose of the system are relatively clear and are not described herein again;
the temperature and pressure acquisition system comprises a plurality of groups of water bath jackets 19, temperature sensors 10, pressure sensors 9 and a data acquisition unit 12 connected with the temperature sensors 10 and the pressure sensors 9, wherein the water bath jackets 19 are arranged along the outer side wall of the reaction kettle barrel 18 from top to bottom, the temperature can be independently controlled, circulating cooling liquid is injected through a matched low-temperature constant temperature bath, and the temperatures of different positions of a sample in the high-pressure reaction kettle are controlled; in addition, a plurality of groups of temperature and pressure measuring points are axially arranged on the side wall of the reaction kettle cylinder 18, and a pressure sensor 10 and a temperature sensor 9 are arranged on the side wall;
the sample collecting and testing system comprises a liquid phase collecting terminal, a high-voltage sample bin 6, a Raman spectrum probe 5 and a Raman tester 4; continuing to refer to fig. 1, in order to research the sequestration effect of carbon dioxide, be equipped with a plurality of liquid phase acquisition terminals on the reation kettle barrel 18, including sample filter screen 8 and sampling valve 7, be equipped with the multiunit sample connection on the high-pressure reaction kettle axial direction, sample filter screen 8 installs in the reation kettle barrel, establish at the sample connection end, prevent that sediment granule from blockking up the sampling passageway, the sample connection passes through valve 7 and links to each other with high-pressure sample storehouse 6, be equipped with normal position raman probe 5 in the high-pressure sample storehouse 6, the sample of gathering can carry out real-time test with fiber-type raman spectrum probe 5, and carry out the analysis based on raman spectrometer 4, confirm the quantity of carbon dioxide in the sample, in order to estimate the carbon dioxide sequestration condition. And a sample discharge port is formed in the bottom of the high-pressure sample bin, and the sample can be discharged by controlling the switch of the emptying valve 15 and then sampled and tested again.
In order to change the experimental defect of traditional device gas excess, not co-altitude is equipped with the multiunit mounting groove on the inside wall of reation kettle barrel 18, and reation kettle barrel 18 is inside to be set up two sets of detachable movable partition plate 11, and movable partition plate 11 adopts the material of permeating water of breathing freely to make, can install the mounting groove department at co-altitude position according to experimental design requirement for the position of restriction deposit.
Furthermore, the side wall of the high-pressure reaction kettle can also be provided with a resistivity test port, and the sealing capacity of carbon dioxide in the seabed environment is evaluated by testing the generation condition of carbon dioxide hydrate in sediments in the reaction kettle body through the resistivity test.
step A, preparation of a sediment sample: screening natural or artificial sand samples with proper grain sizes according to the experimental design requirements, or mixing artificial sand samples with different grain sizes according to the actual sediment composition to simulate the pore conditions of the submarine sediment, cleaning the sediment sample, and drying the sediment sample in a drying box for later use;
step B, sediment filling: adjusting the position of an inner clapboard of the high-pressure kettle according to the experimental design requirement, and filling and compacting a sediment sample to a required position;
step C, injecting a water sample: and closing the reaction kettle, opening a valve with an upper end cover connected with a vacuum pump, opening the vacuum pump to vacuumize the reaction kettle, and closing the valve and the vacuum pump. Injecting deionized water or artificial seawater into the reaction kettle through the constant-flow pump, and closing the constant-flow pump and the valve when the liquid level in the kettle is higher than the sediment. Opening the vacuum pump and the connecting valve again to vacuumize so as to discharge bubbles possibly existing in the sediment, standing for 12 hours, repeating the process twice so as to completely fill the sediment with the water sample, finally filling the water sample into the reaction kettle through the advection pump, and opening the constant pressure pump to push a piston at the upper end of the reaction kettle so as to enable the pressure in the reaction kettle to reach the pressure required by the experiment;
step D, experimental simulation: and setting and starting three groups of circulating water baths outside the reaction kettle according to the experimental design to ensure that the temperature in the reaction kettle reaches the simulation condition, opening a carbon dioxide liquefaction system and an injection pump, injecting liquid-phase carbon dioxide into the high-pressure kettle, recording the amount of the injected liquid-phase carbon dioxide through a flowmeter, and starting a hydrate sealing experiment.
The experimental method for seabed sequestration of carbon dioxide is further described by taking the sequestration process of liquid-phase carbon dioxide in natural sand with the particle size of 200 mu m and carbon dioxide at the temperature of 3 ℃ and under the pressure of 10MPa as an example:
step 1, screening out natural sand with the particle size of 200 mu m before the experiment, cleaning the natural sand, and drying the cleaned natural sand in a drying oven at 70 ℃.
And 2, opening an upper end cover, detaching a partition plate inside the high-pressure reaction kettle, adding a sand sample into the high-pressure reaction kettle, compacting until the sand sample reaches the height of the experimental design position, and then installing the partition plate on the upper part of the sediment to prevent the sediment from disturbing in the experimental process to influence sampling.
And 3, after the sand sample is filled, the upper cover is arranged back to seal the high-pressure kettle. Preparing artificial seawater according to the salinity of the seawater, and injecting the prepared artificial seawater into the high-pressure kettle until the sediment in the high-pressure kettle is immersed at the liquid level.
And 4, opening a valve connected with the water phase injection port and a vacuum pump to vacuumize the high-pressure kettle and discharge air in the pores of the sediment. After standing for several hours, the above process is repeated twice, so that the artificial seawater is completely filled in the sediment pores. And continuously injecting artificial seawater into the reaction kettle until the interior of the reaction kettle is completely filled.
And 5, starting a constant pressure pump at the upper part of the reaction kettle, and enabling the constant pressure pump to push a piston to pressurize the reaction kettle until the pressure in the reaction kettle reaches an experimental design pressure value.
And 6, opening a carbon dioxide gas cylinder and a liquefaction system connected with the carbon dioxide gas cylinder, selecting a position for injecting liquid-phase carbon dioxide into the reaction kettle according to the experimental design, opening a corresponding valve, injecting quantitative liquid-phase carbon dioxide into sediments in the reaction kettle, and starting a simulation experiment. Temperature and pressure values of all positions in the reaction kettle can be recorded in real time through a temperature and pressure probe in the kettle in the whole experiment process, and liquid in the reaction kettle can be sampled and subjected to Raman testing at a fixed time point. If the reaction kettle is provided with resistivity measuring points, the resistivity between the measuring points can be recorded for inverting the generation condition of the carbon dioxide hydrate in the kettle.
Further, in the experimental process, the temperature in the reaction kettle can be adjusted through three groups of water bath jackets outside the reaction kettle, so that the sealing or dissipation conditions of the liquid-phase carbon dioxide under different conditions can be studied.
The above embodiments only describe the research process of the sequestration experiment for injecting the liquid-phase carbon dioxide into the sediment, and in practical work, the simulation research of the sequestration situation when the liquid-phase carbon dioxide is injected into the surface layer or the lower layer of the sediment can also be realized by adjusting the position of the partition plate.
The above description is only a preferred embodiment of the present invention, and not intended to limit the present invention in other forms, and any person skilled in the art may apply the above modifications or changes to the equivalent embodiments with equivalent changes, without departing from the technical spirit of the present invention, and any simple modification, equivalent change and change made to the above embodiments according to the technical spirit of the present invention still belong to the protection scope of the technical spirit of the present invention.
Claims (10)
1. The utility model provides a carbon dioxide seals up deposits experiment analogue means, includes high-pressure batch autoclave, the air feed liquid supply system that is connected with high-pressure batch autoclave, temperature pressure collection system and sample collection and test system, and high-pressure batch autoclave includes reation kettle barrel (18) and end cover (3), air feed liquid supply system includes constant pressure pump (21), liquid phase filling opening (1), and a vacuum pump (16), its characterized in that are connected through the valve in liquid phase filling opening (1):
the temperature and pressure acquisition system comprises a plurality of groups of water bath jackets (19) with independent temperature control, and the water bath jackets (19) are sequentially arranged along the outer side wall of the high-pressure reaction kettle from top to bottom; a plurality of groups of pressure sensors (10) and temperature sensors (9) connected with a data collector (12) are arranged at different height positions in the high-pressure reaction kettle;
different heights are equipped with the multiunit mounting groove on the inside wall of reation kettle barrel (18), and reation kettle barrel (18) is inside to be set up two sets of detachable movable partition (11), and movable partition (11) adopt ventilative material of permeating water to install the mounting groove department at the co-altitude position according to the experimental design requirement, be used for restricting the position of deposit.
2. The carbon dioxide sequestration experiment simulation device of claim 1, characterized in that: a piston (21) and a piston rod (20) are arranged at the upper end of the inner cavity of the high-pressure reaction kettle, a hydraulic cavity is formed between the end cover (3) and the piston (21), the hydraulic cavity is connected with the constant-pressure pump (2) through a pipeline, and constant pressure is applied to the water in the high-pressure reaction kettle through the piston (21); the piston rod (20) is of a hollow structure, one end of the piston rod is connected with the piston (21), the other end of the piston rod extends out of the end cover (3), and the hollow part of the piston rod (20) is communicated with the piston (21) and the end cover (3) to form a liquid phase inlet and a liquid phase outlet of the high-pressure reaction kettle and is connected with the liquid phase injection port (1).
3. The carbon dioxide sequestration experiment simulation device of claim 1, characterized in that: the sample collecting and testing system comprises a liquid phase collecting terminal, a high-voltage sample bin (6), a Raman spectrum probe (5) and a Raman tester (4); the Raman spectrum probe (5) is arranged in the high-pressure sample bin (6) and is connected with the Raman tester (4); the liquid phase acquisition terminal comprises a sampling filter screen (8) and a sampling valve (7), a plurality of groups of sampling ports are arranged in the axial direction of the high-pressure reaction kettle, the sampling filter screen (8) is installed in the reaction kettle barrel and is led out through the sampling ports, the sampling ports are connected with a high-pressure sample bin (6) through the sampling valve (7), the samples acquired are tested in real time through an in-situ Raman probe (5), and analysis is carried out based on a Raman spectrometer (4).
4. The carbon dioxide sequestration experiment simulation device of claim 3, characterized in that: the bottom of the high-pressure sample bin (6) is provided with a sample discharge port, and the sample discharge port is provided with an air release valve (15).
5. The carbon dioxide sequestration experiment simulation device of claim 1, characterized in that: the gas and liquid supply system comprises a high-pressure gas cylinder, a pressure reducing valve, a liquefaction system (13) and an injection pump; the high-pressure gas cylinder is connected with a liquefaction system (13) through a pressure reducing valve, and liquefied carbon dioxide is divided into two paths through an injection pump to be connected with the high-pressure reaction kettle.
6. The carbon dioxide sequestration experiment simulation device of claim 1, characterized in that: and a resistivity test port is also arranged on the side wall of the high-pressure reaction kettle, and the sealing capacity of carbon dioxide in the seabed environment is evaluated by testing the generation condition of carbon dioxide hydrate in sediments in the high-pressure reaction kettle body through the resistivity test.
7. The experimental method of the carbon dioxide sequestration experimental simulation device based on any one of claims 1-6, characterized by comprising the following steps:
step A, preparation of a sediment sample: screening natural or artificial sand samples with proper grain sizes according to the experimental design requirements, or mixing artificial sand samples with different grain sizes according to the actual sediment composition to simulate the pore conditions of the submarine sediment, cleaning the sediment sample, and drying the sediment sample in a drying box for later use;
step B, sediment filling: adjusting the position of a movable partition plate (11) in the high-pressure reaction kettle according to the experimental design requirement, and filling and compacting a sediment sample to a required position;
step C, injecting a water sample:
(1) closing the high-pressure reaction kettle, opening a valve connecting the upper cover (3) and the vacuum pump (16), opening the vacuum pump (16) to vacuumize the high-pressure reaction kettle, and closing the valve and the vacuum pump (16);
(2) injecting deionized water or artificial seawater into the high-pressure reaction kettle, and stopping injecting when the liquid level in the high-pressure reaction kettle is higher than the sediment;
(3) opening the vacuum pump and the connecting valve again to vacuumize, discharging bubbles in the sediment, standing for a plurality of hours, and repeating the process until the sediment is completely filled with the water sample;
(4) filling a water sample into the high-pressure reaction kettle, and opening the constant pressure pump (2) to push a piston (21) at the upper end of the high-pressure reaction kettle so that the pressure in the high-pressure reaction kettle reaches the pressure required by the experiment;
step D, experimental simulation:
(1) according to the experimental design, a circulating water bath (19) is started to ensure that the temperature in the high-pressure reaction kettle reaches the simulation condition;
(2) and opening a carbon dioxide liquefaction system and an injection pump, injecting liquid-phase carbon dioxide into the high-pressure reaction kettle, recording the amount of the injected liquid-phase carbon dioxide through a flow meter, and starting a hydrate sealing experiment.
8. The experimental method based on the carbon dioxide sequestration experimental simulation device according to claim 7, characterized in that: and D, in the process of carrying out a sealing experiment in the step D, starting a sample collecting and testing system at fixed time intervals, taking the liquid phase at the corresponding position in the high-pressure reaction kettle into the high-pressure sample bin, testing by using a Raman probe, and simultaneously recording the temperature and pressure values of each measuring point in the high-pressure reaction kettle.
9. The experimental method based on the carbon dioxide sequestration experimental simulation device according to claim 7, characterized in that: in the step D, the temperature in the high-pressure reaction kettle is regulated by controlling a plurality of groups of water bath jackets (19) so as to research the sealing or dissipation condition of the carbon dioxide under different conditions.
10. The experimental method based on the carbon dioxide sequestration experimental simulation device according to claim 7, characterized in that: in actual work, the simulation research of the sequestration condition when liquid-phase carbon dioxide is injected into the surface layer or the inner part of the sediment is realized through the adjustment of the position of the movable partition plate (11).
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