CN114062191A - Displacement adsorption experimental device and experimental method for binary gas in porous medium - Google Patents
Displacement adsorption experimental device and experimental method for binary gas in porous medium Download PDFInfo
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- 238000001179 sorption measurement Methods 0.000 title claims abstract description 129
- 238000006073 displacement reaction Methods 0.000 title claims abstract description 30
- 238000002474 experimental method Methods 0.000 title claims abstract description 25
- 239000007789 gas Substances 0.000 claims abstract description 175
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 76
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 42
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 38
- 238000004458 analytical method Methods 0.000 claims abstract description 24
- 230000000694 effects Effects 0.000 claims abstract description 5
- 238000012360 testing method Methods 0.000 claims abstract description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical group C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 66
- 239000000523 sample Substances 0.000 claims description 29
- 238000002347 injection Methods 0.000 claims description 11
- 239000007924 injection Substances 0.000 claims description 11
- 238000004868 gas analysis Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 5
- 238000004364 calculation method Methods 0.000 claims description 3
- 238000011156 evaluation Methods 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 238000009489 vacuum treatment Methods 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 2
- 238000012544 monitoring process Methods 0.000 claims 1
- 238000012545 processing Methods 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract description 3
- 239000011148 porous material Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000003079 shale oil Substances 0.000 description 2
- 238000004088 simulation Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002156 adsorbate Substances 0.000 description 1
- 229910052729 chemical element Inorganic materials 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N7/02—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder
- G01N7/04—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder by absorption or adsorption alone
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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Abstract
The invention discloses a displacement adsorption analysis experimental device and an experimental method for binary gas on a porous medium, which comprises the following steps: a vacuum system, a gas supply system, an adsorption system and an analysis system. The vacuum system can exhaust gas in the adsorption device; the gas supply system is characterized in that two gas storage tanks are respectively filled with different gases. The adsorption system comprises a heating thermostat, a first gas storage tank, a second gas storage tank and a sample tank. The gas in the first gas storage tank is adsorbed on the sample in advance, and then is injected into the sample tank after the balance is achieved, and due to the difference of adsorption capacity, the gas which is injected later can replace the gas which is adsorbed in advance and achieve the balance; the analysis system can detect the components of the free gas in the sample tank and calculate the replacement efficiency of the gas. The device can simulate and test the replacement effect of injected carbon dioxide on the adsorbed shale gas at high temperature and high pressure, and has important significance for improving the recovery ratio of the shale gas and the geological storage of the carbon dioxide.
Description
Technical Field
The invention relates to the technical field of improving the recovery ratio of a shale oil reservoir by injecting carbon dioxide, in particular to a replacement adsorption experimental device and an experimental method of binary gas on a porous medium.
Background
At present, the common exploitation technical means of shale oil and gas resources are hydraulic fracturing completion and horizontal drilling technology, but the technology causes a plurality of environmental problems, such as underground water pollution, chemical element migration, deep earthquake induction and the like. Meanwhile, the exploitation efficiency of the technology is not high, only 15%, especially the shale gas existing in the micropores in the reservoir in an adsorption state is not exploited, and the part accounts for 40% -80% of the total reserve volume.
The sizes of micro pores of the shale are mostly nano-scale, water cannot effectively enter the micro pores without damaging the original pore structures, and gas molecules can quickly diffuse into the micro pores and are adsorbed on the surface of a solid through weak van der waals force, electrostatic force and other coupling effects. The conventional experimental device can only measure the adsorption capacity of single gas, and the displacement effect is estimated by comparing the adsorption capacity of pure gas. When the replacement of two kinds of gas adsorbs in the simulation actual exploitation in-process, there are three main problems in current absorption measurement mode:
(1) two gases cannot be introduced simultaneously or sequentially. If the gas is introduced simultaneously, the component proportion of the gas in the gas storage tank is unknown, and the adsorption quantity of each component cannot be calculated. If the adsorption quantity is introduced successively, the calculation error of the adsorption quantity is overlarge due to the pressure change caused by the temperature fluctuation.
(2) The components of the composition of the adsorbed gas cannot be separated. The change of pressure or temperature breaks the adsorption equilibrium between solid and gas phases, and new adsorption/desorption occurs. There is no technology to directly observe and analyze the adsorbed methane and carbon dioxide in shale.
(3) The temperature at the interface where adsorption occurs cannot be accurately monitored. Because the high-temperature and high-pressure environment in an actual reservoir is simulated, the temperature detector is difficult to normally work under high pressure, and the temperature in the constant temperature box is taken as the experimental temperature in the conventional detection method, but the experimental temperature is different from the temperature in the adsorption tank.
Therefore, the experimental device for simulating the displacement adsorption of the binary gas in the shale under the conditions of high temperature and high pressure is designed, the temperature in the adsorption tank and the pressure in each tank are monitored, the adsorption capacity under the experimental conditions is calculated, the ratio of methane to carbon dioxide in an adsorption state can be analyzed, and the experimental device has important significance for researching the injection of the carbon dioxide to improve the recovery ratio of the shale gas and realizing the underground storage of the carbon dioxide.
Disclosure of Invention
The embodiment of the invention aims to provide an experimental device for a displacement adsorption reaction of binary gas in a porous medium, which is used for solving the problem of the existing simulation of injecting carbon dioxide into a displacement adsorption state shale gas.
To achieve the above object, an embodiment of the present invention provides:
a displacement adsorption analysis experimental device and an experimental method of binary gas on a porous medium comprise: a vacuum system, a gas supply system, an adsorption system and a free gas analysis system. The vacuum system can exhaust gas in the adsorption device; the gas supply system is characterized in that two gas storage tanks are respectively filled with different gases. The adsorption system comprises a heating thermostat, a first gas storage tank, a second gas storage tank and a sample tank. The gas in the first gas storage tank is adsorbed on the sample in advance, and then is injected into the sample tank after the balance is achieved, and due to the difference of adsorption capacity, the gas which is injected later can replace the gas which is adsorbed in advance and achieve the balance; the free gas analysis system can detect the components of the free gas in the sample tank and calculate the replacement efficiency of the gas.
The embodiment of the invention provides a displacement adsorption experimental method of a binary gas in a porous medium, which relates to a displacement adsorption experiment and comprises the following steps:
(1) sample treatment: and grinding and drying the shale core and putting the shale core into an adsorption tank.
(2) And (3) air tightness test: the experiment was started after all devices were connected and a certain amount of helium was injected and monitored for 24 hours to determine that there was no gas leakage.
(3) And (3) vacuum treatment: the vacuum pump 20 is turned on to evacuate the entire apparatus.
(4) Preheating gas: the temperature of the constant temperature box is set as the experimental temperature, and methane and carbon dioxide are respectively injected into the two gas storage tanks to wait for gas heating.
(5) Methane pre-adsorption: and (3) allowing methane in the gas storage tank to preferentially enter the adsorption tank for pre-adsorption, and calculating the injection amount and the adsorption amount.
(6) Carbon dioxide displacement adsorption: and (3) allowing the carbon dioxide in the gas storage tank to enter an adsorption tank for displacement adsorption, and calculating the injection amount and the adsorption amount.
(7) Gas component analysis: and after the replacement adsorption in the adsorption tank reaches the balance, allowing the mixed gas of the free methane and the carbon dioxide to enter a gas chromatograph for component analysis.
(8) And (3) separation calculation of adsorbed gas components: the amount of each component adsorbed in the state of adsorption can be obtained by subtracting the amount of each component gas injected from their respective free amounts by the law of conservation of mass.
(9) Evaluation of replacement Effect: the replacement efficiency of carbon dioxide can be demonstrated by comparing the methane adsorption amount after replacement with the amount at the time of preliminary adsorption.
The embodiment of the invention has the following advantages:
1. the invention provides an experimental method and an experimental device for realizing binary gas displacement adsorption by sequentially introducing two adsorbates.
2. The invention provides a convenient and efficient way for analyzing the free gas in the adsorption tank, and avoids errors caused by multiple intervention gas taking.
3. The invention provides a temperature detection mode, which can not only avoid the influence of high pressure on a temperature probe, but also accurately measure the temperature in an adsorption tank.
Drawings
Fig. 1 is a schematic structural diagram of a displacement adsorption experimental apparatus of a binary gas in a porous medium according to embodiment 1 of the present invention.
The numbers used in the figures are as follows:
1. a methane cylinder; 2. a pressure gauge; 3. a valve; 4. a carbon dioxide cylinder; 5. a pressure gauge; 6. a valve; 7. a first gas storage tank; 8. a valve; 9. a pressure gauge; 10. an adsorption tank; 11. a porous media (shale) powder sample; 12. a temperature probe; 13. a valve; 14. a pressure gauge; 15. a valve; 16. a second gas storage tank; 17. a valve; 18. a pressure gauge; 19. a valve; 20. a vacuum pump; 21. a valve; 22. a pressure reducing valve; 23. a gas chromatograph; 24. an incubator.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Examples
Referring to fig. 1, the present invention provides a displacement adsorption experimental apparatus for binary gas in a porous medium, including: a vacuum system, a gas supply system, an adsorption system and a free gas analysis system.
The vacuum system is a vacuum pump 20. The gas supply system is composed of a methane gas cylinder 1, a pressure gauge 2, a valve 3, a carbon dioxide gas cylinder 4, a pressure gauge 5 and a valve 6. The adsorption system comprises a first gas storage tank 7, a valve 8, a pressure gauge 9, an adsorption tank 10, a porous medium (shale) powder sample 11, a temperature probe 12, a valve 13, a pressure gauge 14, a valve 15, a second gas storage tank 16, a valve 17, a pressure gauge 18, a valve 19 and a thermostat 24. The free gas analysis system consists of a valve 21, a pressure reducing valve 22 and a gas chromatograph 23.
The cover of the sample tank 10 is provided with a cavity which is concave downwards, the temperature probe 12 is placed in the cavity, the influence of high pressure in the tank can be isolated, and the temperature in the adsorption tank can be measured due to good thermal conductivity of metal.
When the vacuum system 20 is in operation, the valves 8, 13, 15, 19, 17 and 21 are opened, and the other valves are kept closed.
The gas in the methane gas cylinder 1 enters a first gas storage tank 7 through a valve 3 and a valve 8. Other valves are kept closed during the gas injection process.
The gas in the carbon dioxide gas bottle 4 enters a second gas storage tank 16 through a valve 6 and a valve 17. Other valves are kept closed during the gas injection process.
Methane in the first gas storage tank 7 is injected into the adsorption tank 10 through a valve 8, a valve 15 and a valve 13. Other valves are kept closed during the gas injection process.
The carbon dioxide in the second gas storage tank 16 is injected into the adsorption tank 10 through the valve 17, the valve 19 and the valve 13. Other valves are kept closed during the gas injection process.
The free gas mixture in the canister 10 is fed at a low flow rate into the gas chromatograph 23 for analysis by control of the valve 21 and the pressure reducing valve 22.
The invention provides a displacement adsorption experimental device and an experimental method of binary gas in a porous medium, which comprises the following steps:
(1) sample treatment: shale cores were ground and sieved into 200 mesh powder samples to reduce the time for gas diffusion to adsorption sites in the shale micro-pore structure. The sample is put into an oven and dried for 12-14 hours at 105 ℃ to eliminate the influence of moisture in the pores.
(2) And (3) air tightness test: helium gas of 7MPa is injected into the adsorption system through the gas supply system, the temperature required by the experiment is set in the constant temperature box, and the pressure of the first gas storage tank, the second gas storage tank and the adsorption tank is observed for 24 hours. The pressure variation within. + -. 0.01MPa is regarded as good airtightness.
(3) And (3) vacuum treatment: and (3) loading the powder sample scale into a sample tank, and vacuumizing the adsorption system for 15 minutes by using a vacuum system to eliminate the interference of air existing in sample pores, various tanks and pipelines on the experimental precision.
(4) Preheating gas: setting the temperature of the constant temperature box as the experiment temperature, respectively injecting methane and carbon dioxide with the pressure required by the experiment into the first air storage tank and the second air storage tank, and standing for 2 hours until the gas is heated to reach the set temperature.
(5) Methane pre-adsorption: after the preheated methane gas enters the adsorption tank, a communication valve between the gas storage tank and the adsorption tank is closed, and the amount N of the injected gas is recordedCH4. And observing and recording pressure data in the adsorption tank when the gas diffuses into the pores of the shale sample and generates an adsorption reaction. When the pressure in the sample tank did not change within 1 hour, methane pre-adsorption was considered to reach equilibrium. Calculating the adsorption n of methane by pressure differenceCH4Usually 8 hours.
(6) Carbon dioxide displacement adsorption: and injecting the carbon dioxide in the second gas storage tank into the adsorption tank. Pressure difference exists between the two tanks, and methane in the adsorption tank cannot diffuse to the storage tankIn the second gas tank, the amount N of the injected gas is recordedCO2. Because the pressure in the tank rises, the mixed gas in the free state can continue to be adsorbed in the sample pores, and meanwhile, the free carbon dioxide can replace the methane in the original adsorption state. And observing pressure data in the adsorption tank, and considering that the carbon dioxide displacement adsorption reaches the equilibrium if no change occurs within one hour. Due to competitive adsorption, the process can take longer than a single gas adsorption time, about 10-12 hours.
(7) Gas component analysis: and (4) allowing the free gas in the adsorption tank to pass through a pressure reducing valve, and entering a gas chromatograph at low pressure and low speed for component analysis. The gas amount analyzed only needs 2ml, and the influence on the pressure in the adsorption tank can be ignored. Analyzing the amount W of methane and carbon dioxide in the free gasCH4And WCO2。
(8) Separation of adsorbed gas components: injection amount N of methane and carbon dioxide gasCH4And NCO2Respectively deducting the amount W of methane and carbon dioxide in the free gas after the replacement adsorption balanceCH4And WCO2The ratio of methane to carbon dioxide in the displaced adsorption state can be obtained.
(9) Evaluation of replacement Effect: the replacement efficiency of carbon dioxide can be demonstrated by comparing the methane adsorption amount after replacement with the amount at the time of preliminary adsorption.
The experiment can realize the replacement adsorption experiment of the binary gas in the porous medium under the temperature condition of the simulated actual reservoir, and simultaneously can accurately analyze the component content of each gas in the adsorption state and evaluate the replacement efficiency of the carbon dioxide injection on the shale gas.
Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114740118A (en) * | 2022-04-21 | 2022-07-12 | 云南电网有限责任公司电力科学研究院 | Analysis method of decomposition product of organic hydrogen storage material |
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