CN110514748B - Shale gas occurrence conversion and isotope response simulation device and method - Google Patents
Shale gas occurrence conversion and isotope response simulation device and method Download PDFInfo
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Abstract
The invention discloses a shale gas occurrence conversion and isotope response simulation device which comprises a saturation-desorption tank, a chromatography-isotope mass spectrometry system and a sampling and sample-conveying mechanism. The saturation-desorption tank is used for carrying out gas high-pressure saturation on the rock core and desorbing the rock core after high-pressure saturation; the chromatographic-isotope mass spectrometry system is used for monitoring the change of carbon isotopes or hydrogen isotopes in real time; and the sampling and conveying mechanism is used for collecting gas after the rock core desorption and conveying the gas after the rock core desorption into the chromatographic-isotope mass spectrometry system. The shale gas occurrence conversion and isotope response simulation device is used for shale core gas high-pressure saturation-desorption experiments, the output process of shale gas is simulated in a laboratory, the change of carbon isotopes or hydrogen isotopes is monitored in real time, and basic data and theoretical support are provided for tracing the development state of a shale gas well and predicting the productivity.
Description
Technical Field
The invention relates to the technical field of oil-gas geological exploration, in particular to a shale gas occurrence conversion and isotope response simulation device and method.
Background
The shale gas yield in the blocks of the Job rock dam, Weiyuan and the like in the Sichuan basin of China reaches 5.1 multiplied by 109m3At present, the shale gas production process is in a key stage of exploration and development, and the problems of the adsorbed gas/free gas ratio, the shale gas well development state, the productivity prediction and the like are all important concerns of oil field units. Recent isotope methods are gaining attention and have preliminarily demonstrated the potential for application to the above problems. In principle, in the adsorption/desorption and diffusion processes, an obvious methane isotope fractionation effect can occur, so that an isotope fractionation phenomenon can be caused. It has been found that the carbon isotope value of methane in shale gas drilling mud gas is lighter than that of rock debris degassing, and the methane isotope delta in shale gas production process13C tends to become heavier with mining time. Obviously, the method is related to isotope fractionation in the adsorption/desorption and diffusion processes of the shale gas.
In the analysis of the rock core of the rock shale of the Longmaxi group and the rock core of the Tuoyou group, the composition of the methane carbon isotope (delta) of the rock shale gas in the processes of absorption/desorption and diffusion is observed in the Dangning (2016) and the like13C1) Can produce fractionation effect as high as 7-14.4 per mill. For the obvious isotope fractionation effect, the isotope fractionation effect of the shale gas desorption-diffusion process is simulated and calculated by using SIMEDWin software developed by the university of New Nanwegian Australia and CSIRO by adopting a multi-component adsorption and double-pore gas flow model. According to the simulation calculation result, the proportion of free gas/adsorbed gas in the analysis gas at different moments and the change of the proportion along with the analysis time are further solved.
At present, the research of the isotope method is just started, and the isotope method has great potential for researching the transformation of the shale gas occurrence state and the tracing of the shale gas development state. The key point is to master the isotope fractionation rule in the shale gas analysis (adsorption/desorption, diffusion) process and establish a fractionation effect quantitative characterization model with a theoretical basis.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides a shale gas occurrence conversion and isotope response simulation device and method. According to one aspect of the invention, the shale gas occurrence conversion and isotope response simulation device comprises:
the saturation-desorption tank is used for carrying out gas high-pressure saturation on the rock core and desorbing the rock core after the high-pressure saturation;
a chromatograph-isotope mass spectrometry system for monitoring the change of carbon isotopes or hydrogen isotopes in real time;
and the sampling and sample-feeding mechanism is used for collecting the gas after the core desorption and feeding the gas after the core desorption into the chromatographic-isotope mass spectrometry system.
In one embodiment, a pressure reducing valve and a flow controller are sequentially arranged between the saturation-desorption tank and the sampling mechanism along the gas flow direction.
In one embodiment, the sampling and sample-feeding mechanism is a six-way valve, and a sampling tube is arranged in the six-way valve.
In one embodiment, the chromatography-isotope mass spectrometry system comprises a chromatograph and an isotope mass spectrometer which are arranged in sequence along the gas flowing direction, and a combustion furnace is arranged between the chromatograph and the isotope mass spectrometer and is used for oxidizing gas or pyrolyzing gas.
In one embodiment, the saturation-desorption tank is externally provided with a heating jacket for providing a suitable temperature for the saturation-desorption tank.
In one embodiment, an inlet of the saturation-desorption tank is connected with a high-pressure air storage tank, an outlet of the high-pressure air storage tank is provided with a first pressure gauge, and an outlet of the saturation-desorption tank is provided with a second pressure gauge.
In one embodiment, the lower portion of the saturation-desorption tank is connected to a vacuum pump.
According to another aspect of the invention, the method for shale gas occurrence conversion and isotope response simulation comprises the following steps:
s1, vacuumizing the saturation-desorption tank with the core, and performing high-pressure gas saturation on the saturation-desorption tank by using a high-pressure gas storage tank;
s2, desorbing the core after the gas saturation, and sampling the gas after the core desorption;
and S3, sending the obtained sample to the chromatography-isotope mass spectrometry system to monitor the change of the carbon isotope or the hydrogen isotope in real time.
In one embodiment, before the step S1, the method further includes a step S0:
placing the dried rock core in the saturation-desorption tank, and vacuumizing the saturation-desorption tank;
introducing inert gas into the saturation-desorption tank by using the high-pressure gas storage tank until the pressure of the high-pressure gas storage tank and the pressure of the saturation-desorption tank reach balance;
acquiring the volume of the void space of the saturation-desorption tank according to the pressure change before and after the high-pressure gas storage tank feeds the inert gas into the saturation-desorption tank;
and calculating the volume of the gas required to be filled in the high-pressure gas storage tank according to the obtained volume of the empty space of the saturation-desorption tank.
In one embodiment, the core saturated gas is methane or shale gas.
Compared with the prior art, the shale gas occurrence conversion and isotope response simulation device has the advantages that the shale gas occurrence conversion and isotope response simulation device is used for shale core gas high-pressure saturation-desorption experiments, the shale gas production process is simulated in a laboratory, the change of isotopes is monitored in real time, the change rule and the fractionation mechanism of the isotopes in the mass transfer and migration process in the shale gas production process are determined, the relationship between the shale gas occurrence conversion and the isotope response is cleared, and the development state of a shale gas well is traced.
Drawings
Preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings. In the figure:
fig. 1 shows a schematic structural diagram of a shale gas occurrence conversion and isotope response simulation apparatus according to an embodiment of the present invention.
Fig. 2 shows a flow chart of a shale gas occurrence conversion and isotope response simulation method according to an embodiment of the present invention.
In the drawings, like parts are provided with like reference numerals. The figures are not drawn to scale.
Detailed Description
The invention will be further explained with reference to the drawings.
Fig. 1 shows a shale gas occurrence transformation and isotope response simulation device according to the present invention, which comprises a saturation-desorption tank 1, a chromatography-isotope mass spectrometry system 2 and a sampling mechanism 3. The saturation-desorption tank 1 is used for performing gas high-pressure saturation on the rock core and desorbing the rock core after high-pressure saturation. The chromatograph-isotope mass spectrometry system 2 is used to monitor the change of isotopes in real time. The sampling and sample-feeding mechanism 3 is used for collecting gas after core desorption, and sending the gas after core desorption into the chromatographic-isotope mass spectrometry system 2. When the core is saturated with gas under high pressure, the gas used may be pure methane or shale gas.
According to the method, a certain corresponding relation exists between the isotope change of methane and the recovery ratio of the shale gas well in the shale gas development process, so that the development state of the shale gas well is traced by utilizing the isotope change of methane. By utilizing the principle, the shale gas occurrence conversion and isotope response simulation device is used for a shale core gas high-pressure saturation-desorption experiment, and can also be used for a full-diameter shale core (a columnar core which is not cut or split and is used for analysis and determination in a laboratory in the whole section) gas high-pressure saturation-desorption experiment, the shale gas production process is simulated in the laboratory, the isotope change is monitored in real time, and the development state of a shale gas well is traced.
In one embodiment, a pressure reducing valve 11 and a flow controller 12 are sequentially arranged between the saturation-desorption tank 1 and the sampling mechanism 3 along the gas flowing direction (as shown by an arrow b in fig. 1). A pressure reducing valve 11 is used to reduce the pressure at the outlet of the saturation-desorption tank 1, and a flow controller 12 is used to control the flow of gas, preferably 5.0 ml/min.
In one embodiment, the sampling mechanism 3 is a six-way valve, a sampling tube 31 is disposed in the six-way valve, and a gas supply device (not shown) is further disposed at an inlet of the six-way valve 3, and an inert gas (as indicated by arrow a in fig. 1) supplied by the gas supply device is used as a carrier to supply the gas collected in the sampling tube 31 to the chromatograph-isotope mass spectrometry system 2. In the six-way valve shown in fig. 1, the gas not collected in the sampling pipe 31 is discharged through the pipes indicated by the symbols (r), (c), and (c). Preferably, the sampling tube is 10ul in length. The inert gas used as the carrier may be helium or other inert gases.
In one embodiment, the chromatograph-isotope mass spectrometry system 2 includes a chromatograph 21 and an isotope mass spectrometer 22 sequentially arranged along a gas flow direction (as indicated by an arrow c in the figure), and a combustion furnace 23 is provided between the chromatograph 21 and the isotope mass spectrometer 22. The combustion furnace 23 may be an oxidation furnace or a cracking furnace.
When the core is saturated at high pressure with pure methane, the chromatograph 21 is used to remove any impurity gases that may be present to avoid interference with the methane. The gas separated by the chromatograph 21 is oxidized into carbon dioxide by an oxidation furnace, or is cracked into hydrogen at high temperature by a cracking furnace. Thereafter, the carbon isotope or the hydrogen isotope is detected by the isotope mass spectrometer 22.
When the gas used is shale gas, chromatograph 21 is used to separate methane and ethane in addition to removing impurity gases that may be present. The gas separated by the chromatograph 21 is oxidized into carbon dioxide by an oxidation furnace, or is pyrolyzed into hydrogen by a pyrolysis furnace. Then, the carbon isotope chromatographic peaks of methane and ethane, or the hydrogen isotope chromatographic peaks of methane and ethane, respectively, can be detected by the isotope mass spectrometer 22.
In an embodiment, the saturation-desorption tank 1 is externally provided with a heating jacket 13, and the heating jacket 13 is used for providing a proper temperature for the saturation-desorption tank 1. Typically, the temperature is set to the temperature of the formation in which the core is located to maximize modeling of the environment of the core in its formation.
In one embodiment, the inlet of the saturation-desorption tank 1 is connected with the high-pressure air storage tank 14, and a valve is arranged between the saturation-desorption tank 1 and the high-pressure air storage tank 14. The outlet of the high-pressure gas storage tank 14 is provided with a first pressure gauge 15, and the outlet of the saturation-desorption tank 1 is provided with a second pressure gauge 17. In this embodiment, the lower portion of the saturation-desorption tank 1 is connected to a vacuum pump 16. Before performing a methane gas or shale gas saturation-desorption experiment on the core, the high-pressure gas storage tank 14 is filled with an inert gas (preferably, helium) with a pressure P, and the pressure value of the high-pressure gas storage tank 14 is observed through the first pressure gauge 15. Then, the rock core is placed in the saturation-desorption tank 1, then the saturation-desorption tank is vacuumized by using the vacuum pump 16, after the vacuumization, a valve between the high-pressure gas storage tank 14 and the saturation-desorption tank 1 is opened until the pressures of the high-pressure gas storage tank 14 and the saturation-desorption tank 1 reach balance (whether the pressures of the high-pressure gas storage tank 14 and the saturation-desorption tank 1 reach balance is observed through the first pressure gauge 15 and the second pressure gauge 17), and the volume of the void space of the saturation-desorption tank 1 is calculated through the change of the pressure of the first pressure gauge 15. The void space is the sum of the space in the saturation-desorption tank 1 in which the core is placed and the core pores.
According to another aspect of the invention, the method for shale gas occurrence conversion and isotope response simulation comprises the following steps:
s1, vacuumizing the saturation-desorption tank with the core, and performing high-pressure gas saturation on the saturation-desorption tank by using a high-pressure gas storage tank;
s2, desorbing the core after gas saturation, and sampling the gas after core desorption;
and S3, sending the obtained sample to the chromatography-isotope mass spectrometry system to monitor the change of the isotope in real time.
In one embodiment, before the step S1, the method further includes a step S0:
placing the dried rock core in a saturation-desorption tank, and vacuumizing the saturation-desorption tank;
introducing inert gas into the saturation-desorption tank by using a high-pressure gas storage tank until the pressure of the high-pressure gas storage tank and the pressure of the saturation-desorption tank reach balance;
acquiring the volume of the void space of the saturation-desorption tank according to the pressure change before and after the inert gas is introduced into the saturation-desorption tank by the high-pressure gas storage tank;
and calculating the volume of the gas required to be filled in the high-pressure gas storage tank according to the obtained volume of the empty space of the saturation-desorption tank.
In one embodiment, the method for shale gas evolution transformation and isotope response simulation is as follows:
1) filling high-purity helium gas with a certain pressure into the high-pressure gas storage tank 14, and recording the pressure value of the first pressure gauge 15;
2) placing the core to be tested in a vacuum oven for fully degassing and dehydrating, wherein the temperature is set to be 85 ℃ under the vacuum condition, and the drying time is set to be 1 hour;
3) placing the dried rock core into a saturation-desorption tank 1, sealing the saturation-desorption tank 1, and vacuumizing for about 1 hour;
4) after vacuumizing, communicating the high-pressure gas storage tank 14 with the saturation-desorption tank 1 until the pressures of the high-pressure gas storage tank 14 and the saturation-desorption tank 1 reach balance, and calculating the volume of a void space of the saturation-desorption tank 1 in which the rock core is placed according to the change of the pressure value of the first pressure gauge 15;
5) vacuumizing the saturation-desorption tank 1 with the core again;
6) calculating the pressure required to be filled with methane in the high-pressure gas storage tank 14 according to the volume of the obtained void space of the saturation-desorption tank 1 with the core, and filling the high-pressure gas storage tank 14 with methane at the pressure;
7) opening a valve between the high-pressure gas storage tank 14 and the saturation-desorption tank 1 to enable methane in the high-pressure gas storage tank to flow into the saturation-desorption tank 1 to perform methane high-pressure saturation on the rock core, and detecting pressure change in the saturation-desorption tank 1 according to a second pressure gauge 17 until the rock core is fully saturated;
8) closing a valve between the high-pressure gas storage tank 14 and the saturation-desorption tank 1, starting desorption, controlling the flow rate of methane gas to be 5ml/min through a flow controller in the desorption process, and accumulating the gas outflow in real time;
9) when methane gas flowing out from the core desorption flows through the six-way valve 3, sampling is performed by using the sampling pipe 31. The sampling time interval of the sampling pipe 31 can be set, and when sampling is not needed, methane gas is discharged through pipelines shown as the first pipeline, the fourth pipeline, the fifth pipeline and the sixth pipeline of the six-way valve 3;
10) using helium as a carrier, as shown by an arrow a in fig. 1, sending the methane gas collected in the sampling pipe 31 into a chromatography-isotope mass spectrometry system, separating components of the methane gas in a chromatograph 21, and converting the methane gas into CO through an oxidation furnace2Or is pyrolyzed to H by a pyrolysis furnace2The carbon isotope or hydrogen isotope is then monitored by the isotope mass spectrometer 22.
According to the experimental method, the carbon isotope or hydrogen isotope change conditions under the conditions of different time, different pressure and different gas flow rate can be designed to simulate the isotope fractionation mechanism in the shale core production process, and the isotope change rule in the shale gas development process is inverted.
In another embodiment, shale gas may be used instead of methane gas to perform high pressure shale saturation of the core in the saturation-desorption tank, and after desorption, the collected gas is sent to chromatograph 21 for component separation and converted to CO by oxidation furnace2Or is pyrolyzed to H by a pyrolysis furnace2The change in the carbon isotope or hydrogen isotope is then monitored by the isotope mass spectrometer 22. The other steps are the same as the above-mentioned steps for introducing methane gas.
The above description is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily make changes or variations within the technical scope of the present invention disclosed, and such changes or variations should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (4)
1. A method for shale gas occurrence conversion and isotope response simulation according to a shale gas occurrence conversion and isotope response simulation device is characterized in that,
the shale gas occurrence conversion and isotope response simulation device comprises:
the saturation-desorption tank is used for carrying out gas high-pressure saturation on the rock core and desorbing the rock core after the high-pressure saturation;
a chromatography-isotope mass spectrometry system for monitoring the change of isotopes in real time;
the sampling and sample-feeding mechanism is used for collecting the gas after the rock core desorption and feeding the gas after the rock core desorption into the chromatographic-isotope mass spectrometry system;
the chromatographic-isotope mass spectrometry system comprises a chromatograph and an isotope mass spectrometer which are sequentially arranged along the gas flowing direction, wherein a combustion furnace is arranged between the chromatograph and the isotope mass spectrometer, and the combustion furnace is used for oxidizing gas or cracking the gas at high temperature;
a pressure reducing valve and a flow controller are sequentially arranged between the saturation-desorption tank and the sampling and sample-sending mechanism along the gas circulation direction;
an inlet of the saturation-desorption tank is connected with a high-pressure gas storage tank, an outlet of the high-pressure gas storage tank is provided with a first pressure gauge, and an outlet of the saturation-desorption tank is provided with a second pressure gauge;
the method comprises the following steps:
filling inert gas with a certain pressure into the high-pressure gas storage tank, and recording the pressure value of the first pressure gauge;
placing the dried rock core in a saturation-desorption tank, sealing the saturation-desorption tank and vacuumizing the saturation-desorption tank;
after vacuumizing, communicating the high-pressure gas storage tank with the saturation-desorption tank until the pressures of the high-pressure gas storage tank and the saturation-desorption tank reach balance, and calculating the volume of a void space of the saturation-desorption tank in which the core is placed according to the change of the pressure value of the first pressure meter;
vacuumizing the saturation-desorption tank with the core again;
calculating the pressure of the high-pressure gas storage tank required to be filled with the core saturated gas according to the obtained volume of the void space of the saturation-desorption tank with the core, and filling the high-pressure gas storage tank with the core saturated gas with the pressure;
opening a valve between the high-pressure gas storage tank and the saturation-desorption tank to enable saturated gas of the rock core in the high-pressure gas storage tank to flow into the saturation-desorption tank to perform high-pressure gas saturation on the rock core, and detecting pressure change in the saturation-desorption tank according to a second pressure gauge until the rock core is fully saturated;
closing a valve between the high-pressure gas storage tank and the saturation-desorption tank, starting desorption, and controlling the flow rate of the desorbed gas through a flow controller in the desorption process;
sampling the gas desorbed from the rock core by a sampling and conveying mechanism;
feeding the obtained sample into the chromatography-isotope mass spectrometry system to monitor the change of the isotope in real time;
wherein the introduced core saturated gas is methane or shale gas.
2. The method for shale gas occurrence conversion and isotope response simulation as claimed in claim 1, wherein the sampling mechanism is a six-way valve, and a sampling tube is arranged in the six-way valve.
3. The method for shale gas occurrence conversion and isotope response simulation of claim 1, wherein a heating jacket is provided outside the saturation-desorption tank, and the heating jacket is used for providing a suitable temperature for the saturation-desorption tank.
4. The method for shale gas occurrence conversion and isotope response simulation as claimed in claim 1, wherein a vacuum pump is connected to a lower portion of the saturation-desorption tank.
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| CN111749685B (en) * | 2020-07-03 | 2023-04-07 | 承德石油高等专科学校 | Method and device for determining exploitation degree of oil and gas reservoir |
| CN111855481A (en) * | 2020-07-13 | 2020-10-30 | 中国石油大学(北京) | Method and device for measuring fractionation data of adsorbed gas isotope |
| CN114112787B (en) * | 2020-09-01 | 2024-07-09 | 中国石油化工股份有限公司 | Method for identifying single-well shale gas dessert segment |
| CN112151124B (en) * | 2020-09-24 | 2022-11-04 | 中国石油大学(华东) | Shale in-situ gas-containing parameter determination method and system based on carbon isotope fractionation |
| CN112149306B (en) * | 2020-09-27 | 2021-05-18 | 中国科学院地质与地球物理研究所 | Carbon isotope fractionation calculation method in natural gas analysis process and application |
| CN112461912A (en) * | 2020-11-03 | 2021-03-09 | 中能化江苏地质矿产设计研究院有限公司 | Method for indicating shale gas high-yield horizon by inversion of alkane carbon isotope sequence |
| CN112331366B (en) * | 2020-11-21 | 2022-12-13 | 中国工程物理研究院材料研究所 | Deuterium-tritium fuel storage and supply demonstration system and application |
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