CN115165951B - Supercritical CO determination under reservoir temperature and pressure conditions 2 Method and device for displacing shale gas efficiency - Google Patents
Supercritical CO determination under reservoir temperature and pressure conditions 2 Method and device for displacing shale gas efficiency Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 42
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- 229910052731 fluorine Inorganic materials 0.000 claims description 16
- 239000011737 fluorine Substances 0.000 claims description 16
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- 238000012544 monitoring process Methods 0.000 claims description 9
- 238000003825 pressing Methods 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a method for measuring supercritical CO under the reservoir temperature and pressure condition 2 The method and the device for displacing shale gas efficiency comprise the steps of calibrating the relation between the amount of methane substances and the integral of the signal intensity of nuclear magnetic resonance T2 spectrum peak by using a polytetrafluoroethylene sample; saturating the shale sample with methane under reservoir temperature and pressure conditions; determination of supercritical CO by nuclear magnetic resonance 2 T2 spectrum change of rock core in methane process in shale sample displacement process, and supercritical CO is calculated 2 And (3) displacing shale gas efficiency under different occurrence states. The invention solves the problems of the current research of supercritical CO 2 The shale gas displacement efficiency is not in the reservoir temperature and pressure condition, so that the production practice is more met; the methane in different occurrence states is distinguished according to the length of the relaxation time, the weight change of the shale sample or the pressure change of the system is not required to be measured, the occurrence state and the content of the methane in the shale sample are accurately and quantitatively analyzed through nuclear magnetic resonance technology, and the supercritical CO is helpful to be deeply understood 2 A mechanism for displacing shale gas.
Description
Technical Field
The invention relates to the technical field of shale gas exploration and development, in particular to a method for measuring supercritical CO under the reservoir temperature and pressure condition 2 Method for displacing shale gas efficiency, and simultaneously relates to method for measuring supercritical CO under reservoir temperature and pressure conditions 2 And a device for displacing shale gas efficiency.
Background
The economic recoverable reserve of the global shale gas is about 4.56 multiplied by 10 14 Cubic meters are expected to be one of the most important successor energy sources in the 21 st century. Chinese shale gas geological resource reaches 95.00 multiplied by 10 12 Cubic meters, the economic and recoverable resource amount reaches 12.86 multiplied by 10 12 Cubic meters, and has wide prospect in exploration and development. However, shale reservoirs are different from general oil and gas reservoirs in nature, have extremely low pores and permeability, have a large number of nano-scale pores distributed, have high exploitation difficulty and have low recovery ratio. Supercritical CO 2 The injection into the shale gas reservoir can not only effectively improve the shale gas recovery ratio, but also can simultaneously inject a large amount of CO 2 Sealed in the underground reservoir space, and effectively reduces carbon emission.
At present, CO is studied through experimental means in China 2 There has been little research on the efficiency of displacing shale gas. At present, the experimental samples studied at present mostly use shale powder, and the mode destroys the pore structure of the rock core and cannot be used for CO 2 The mechanism of enhancing shale gas recovery is being studied intensively. Meanwhile, shale powder cannot be placed in an effective pressure state, the difference between the shale powder and the current situation of an actual project is large, and the obtained experimental result has limited guiding significance on the actual project. The monitoring means is also single in the experimental process, and often, the measurement and the analysis of CO are carried out through the pressure change in the reaction kettle or the total mass change of the system 2 The shale gas efficiency is displaced, and the monitoring means is too simple. The main component of shale gas is methane, and the methane has three occurrence states in shale: adsorbed state, free state and free state. The measurement and analysis by pressure change or quality change cannot further study the occurrence of methane in CO in three different occurrence states 2 Law of variation in the displacement process. The experiment core is not in a reservoir temperature and pressure state and lacks microscopic monitoring means to greatly limit CO 2 Research progress in displacing shale gas.
In summary, a set of reservoir temperature and pressure conditions were developed to measure supercritical CO 2 The method and the device for displacing the shale gas efficiency are urgent and have important significance for relieving the energy crisis of the current country.
Disclosure of Invention
Based on the defects existing in the prior art, the invention aims to solve the technical problems thatFor measuring supercritical CO under reservoir temperature and pressure conditions 2 The method for displacing the shale gas efficiency is easy to operate, is simple and convenient to operate, does not need to measure the weight change of the shale sample or the pressure change of the system, and can accurately and quantitatively analyze the occurrence state and the content of methane in the shale sample through a nuclear magnetic resonance technology.
It is another object of the present invention to provide a method for determining supercritical CO at reservoir temperature and pressure 2 The device for displacing the shale gas efficiency is simple in structure and convenient to use. The invention can realize the development of supercritical CO under the condition of true triaxial stress by placing the shale core 2 And the shale gas displacement experiment is more in line with the actual stratum condition. The invention also realizes the differentiation and quantification of methane in different occurrence states by measuring by using nuclear magnetic resonance technology.
In order to achieve the above object, the present invention adopts the following technical measures:
supercritical CO determination under reservoir temperature and pressure conditions 2 The method for displacing shale gas efficiency comprises the following steps:
s1, calibrating the relation between the amount of methane substances and the integral of the signal intensity of the nuclear magnetic resonance T2 spectrum peak by using a polytetrafluoroethylene sample; placing a polytetrafluoroethylene sample into a core holder, applying axial pressure to the polytetrafluoroethylene sample by using an axial pressure pump, then introducing a heated FC40 solution into a confining pressure chamber of the core holder by using a confining pressure circulating heating pump, applying confining pressure to the polytetrafluoroethylene sample, and heating the core holder to a specified temperature; under the condition of constant temperature and constant pressure, vacuumizing a pipeline by using a vacuum pump, injecting methane into a polytetrafluoroethylene sample at different pore pressures by using a methane injection pump, testing the nuclear magnetic resonance T2 spectrum of the polytetrafluoroethylene sample by using nuclear magnetic resonance equipment, and obtaining the linear relation between the amount of methane substances and the integral of the peak signal intensity of the nuclear magnetic resonance T2 spectrum by using a universal gas law:
M＝k*Amp (1)
wherein M is the amount of methane substance, k is a linear correlation coefficient, and Amp is the integral of the signal intensity of the nuclear magnetic resonance T2 spectrum peak, namely T 2 Envelope area formed by spectrum and x-axis;
s2, using methane to saturate shale samples under the reservoir temperature and pressure condition; placing a shale sample into a core holder, applying axial pressure to the shale sample by using an axial pressure pump, introducing a heated FC40 solution into a confining pressure chamber of the core holder by using a confining pressure circulating heating pump, applying confining pressure to the shale sample, and heating the shale sample to a specified temperature; using a methane injection pump to saturate methane gas with a certain pore pressure to a shale sample, and using nuclear magnetic resonance equipment to test a T2 spectrum of the shale sample in a reservoir temperature and pressure state in a saturated methane state;
s3, measuring supercritical CO by utilizing nuclear magnetic resonance 2 T2 spectrum change of rock core in methane process in shale sample displacement process, and supercritical CO is calculated 2 Displacing shale gas efficiency in different occurrence states; by CO 2 Displacement pump will be supercritical CO 2 Injecting the mixture into a rock core under the reservoir temperature and pressure condition by a certain pore pressure, and monitoring the T2 spectrum change of the shale sample in real time by using nuclear magnetic resonance equipment and distinguishing methane in different occurrence states in the shale sample:
M sat ＝k*Amp sat (2)
wherein M is sat Amp, which is the amount of methane substances in different occurrence forms in shale samples in saturated methane state under reservoir temperature and pressure sat Integrating peak signal intensities of different relaxation time ranges in a T2 spectrum of the shale sample;
according to the morphology of the T2 spectrum of the shale sample, different occurrence states of methane in the shale sample are distinguished, and the methane passes through supercritical CO 2 T2 spectrum change of shale sample in displacement process, and supercritical CO is calculated 2 Shale gas efficiency in different occurrence states is displaced:
M exp ＝k*Amp exp (3)
wherein M is exp At CO for shale sample 2 Shale internal methane in methane displacement processAmp, the amount of substance in (a) exp For rock sample at CO 2 T2 spectrum peak signal intensity integration in methane displacement process, E is supercritical CO 2 Shale gas displacement efficiency.
In the above test step, the relationship between the measured methane substance amount in step S1 and the integral of the nuclear magnetic resonance T2 spectrum peak signal intensity is the calculation basis of step S3; step S2, placing a shale sample in a reservoir temperature and pressure environment by using a core holder is an important point of the invention; step S3, monitoring the CO of methane in different occurrence states by using nuclear magnetic resonance equipment 2 Variations in the displacement process are also a bright spot of the present invention.
By the technical method, the supercritical CO in the current research is solved 2 The shale gas displacement efficiency is not in the reservoir temperature and pressure condition, so that the production practice is more met; meanwhile, the methane in different occurrence states is distinguished according to the length of relaxation time, which is helpful for deep understanding of supercritical CO 2 A mechanism for displacing shale gas.
In addition, another object of the invention is to provide a method for determining supercritical CO under reservoir temperature and pressure conditions 2 The device for displacing shale gas efficiency has the advantages of simple structure and convenient use, and the experimental device comprises a set of nuclear magnetic resonance equipment, a set of warm-pressing loading unit and a set of displacement seepage unit and is used for accurately measuring supercritical CO under the reservoir warm-pressing condition 2 Shale gas displacement efficiency.
The invention can measure supercritical CO under the reservoir temperature and pressure condition 2 The device for displacing the shale gas efficiency comprises a warm-pressure loading unit, nuclear magnetic resonance equipment and a displacement seepage unit;
the warm-pressing loading unit comprises a left end cushion block, a right end cushion block, a heat shrinkage pipe, a core holder, a shaft pressure pump, a fluorine oil storage tank, a first needle valve, a first pressure gauge and a confining pressure circulation heating pump, wherein the polytetrafluoroethylene sample, the left end cushion block and the right end cushion block are spliced together, the three are connected into a whole through the heat shrinkage pipe and put into the core holder, the shaft pressure pump, the fluorine oil storage tank, the first needle valve and the first pressure gauge are connected through pipelines, and the core holder and the confining pressure circulation heating pump are connected through pipelinesAre connected; the nuclear magnetic resonance equipment comprises an NMR control console, a permanent magnet and a nuclear magnetic probe coil, which are connected through a USB data line; the displacement seepage unit comprises a second needle valve, a vacuum pump, a methane injection pump, a methane gas cylinder, a third needle valve, a second pressure gauge and CO 2 Displacement pump, CO 2 The second needle valve and the vacuum pump are connected with the core holder through pipelines; the methane injection pump, the methane gas cylinder, the third needle valve and the second pressure gauge are connected with the core holder through pipelines; the CO 2 Displacement pump, CO 2 The gas cylinder, the fourth needle valve and the third pressure gauge are connected with the core holder through pipelines; the fifth needle valve and the back pressure valve are connected with the core holder through pipelines.
Further, the axial pressure pump is used for injecting the fluorine oil in the fluorine oil storage tank into the core holder and is used for applying axial pressure to the polytetrafluoroethylene sample and the shale sample; the confining pressure circulating heat pump is used for applying confining pressure to the polytetrafluoroethylene sample and the shale sample and heating the polytetrafluoroethylene sample and the shale sample to a specified temperature.
Further, the nuclear magnetic probe coil is used for transmitting nuclear magnetic resonance pulse sequences and receiving relaxation signals of methane gas in the sample; the permanent magnet is used for manufacturing a main magnetic field environment with constant field intensity; the NMR console is used for controlling the nuclear magnetic probe coil to transmit pulse sequences, receive and process relaxation signals of methane gas.
In the device, the core holder is a key component, and by using the core holder, supercritical CO can be developed under the temperature and pressure of a reservoir 2 And (3) displacing shale gas experiments. The NMR control console, the permanent magnet and the nuclear magnetic probe coil are also key components and are connected through USB data lines, so that accurate quantitative analysis of the occurrence state and the content of methane in shale samples is realized.
Compared with the prior art, the invention has the core that the nuclear magnetic resonance technology is utilized to monitor the supercritical CO in the shale sample in the reservoir temperature and pressure state 2 Displacement of methaneNuclear magnetic resonance signals of methane with different forms in the process, and further calculating and measuring supercritical CO 2 The method is more suitable for shale gas reservoir development. Compared with the prior art, the invention has at least the following advantages:
1. the experimental rock core is under the real reservoir temperature and pressure conditions, and particularly can be under the conventional triaxial stress state.
2. Methane in different occurrence states can be studied in CO by distinguishing the methane in different occurrence states through a T2 spectrum 2 Law of variation in the displacement process.
3. The method is matched with nuclear magnetic resonance technology, realizes one machine with multiple parameters, and can obtain multiple parameters such as porosity, permeability, relative permeability curve and the like of the core under the condition of reservoir temperature and pressure through one experiment.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiments of the application and together with the description serve to explain the application and do not constitute an undue limitation to the application.
FIG. 1 is a graph of the determination of supercritical CO under reservoir temperature and pressure conditions of the present invention 2 A structural schematic diagram of a device for displacing shale gas efficiency;
FIG. 2 is a graph showing the T2 spectrum of methane (FIG. 2 a) and the amount of methane material versus the integral of the peak signal intensity of the T2 spectrum (FIG. 2 b) for different Kong Yaxia samples of the examples;
FIG. 3 is a graph of T2 spectrum of shale samples in saturated methane state;
FIG. 4 is supercritical CO 2 A core T2 spectrum change result schematic diagram in the process of displacing methane in the shale sample;
FIG. 5 is supercritical CO 2 Variation of the amount of methane species in different occurrence states during displacement of methane inside shale samples (FIG. 5 a) and CO 2 Displacement efficiency (fig. 5 b) is schematically represented.
Wherein:
1-polytetrafluoroethylene sample, 2-left end pad, 3-right end pad, 4-heat shrinkage tube, 5-core holder (oxidation)Zirconium material), 6-axis pressure pump, 7-fluorooil storage tank (316L material), 8-first needle valve, 9-first pressure gauge, 10-confining pressure circulation heat pump, 11-second needle valve, 12-vacuum pump, 13-methane injection pump, 14-methane gas cylinder, 15-third needle valve, 16-second pressure gauge, 17-NMR control console, 18-permanent magnet, 19-nuclear magnetic probe coil, 20-shale sample, 21-CO 2 Displacement pump, 22-CO 2 Gas cylinder, 23-fourth needle valve, 24-third pressure gauge, 25-fifth needle valve, 26-back pressure valve.
Detailed Description
As shown in fig. 1 to 5, the supercritical CO is measured under the reservoir temperature and pressure conditions of the present invention 2 The method for displacing shale gas efficiency is characterized by monitoring the occurrence state and content change of methane in an experimental rock core by using nuclear magnetic resonance equipment, and comprises the following specific steps:
s1, calibrating the relation between the amount of methane substances and the integral of the signal intensity of the nuclear magnetic resonance T2 spectrum peak by using a polytetrafluoroethylene sample 1; placing a polytetrafluoroethylene sample 1 into a core holder 5, applying axial pressure to the polytetrafluoroethylene sample 1 by using an axial pressure pump 6, then introducing a heated FC40 solution into a confining pressure chamber of the core holder 5 by using a confining pressure circulating heating pump 10, applying confining pressure to the polytetrafluoroethylene sample 1 and heating the core holder 5 to a specified temperature; under the condition of constant temperature and constant pressure, the pipeline is vacuumized by utilizing the vacuum pump 12, methane is injected into the polytetrafluoroethylene sample 1 by utilizing the methane injection pump 13 at different pore pressures, the nuclear magnetic resonance T2 spectrum of the polytetrafluoroethylene sample 1 is tested by utilizing nuclear magnetic resonance equipment, and the linear relation between the amount of methane substances and the peak signal intensity integral of the nuclear magnetic resonance T2 spectrum is obtained by utilizing the universal gas law:
m=k×amp formula 1
Wherein M is the amount of methane substance, and Amp is the integral of the signal intensity of the nuclear magnetic resonance T2 spectrum peak, namely T 2 The envelope area formed by the spectrum and the x-axis, k is a linear correlation coefficient. Amp and K were each determined from specific experimental data.
S2, saturating the shale sample 20 with methane under the reservoir temperature and pressure condition; placing the shale sample 20 into a core holder 5, applying axial pressure to the shale sample 20 by using an axial pressure pump 6, introducing the heated FC40 solution into a confining pressure chamber of the core holder 5 by using a confining pressure circulating heating pump 10, applying confining pressure to the shale sample 20, heating the shale sample 20 to a specified temperature, and setting the axial pressure, confining pressure and temperature of a test core according to the temperature and pressure conditions of the reservoir core; after the displacement system is vacuumized by the vacuum pump 12, the shale sample 20 is saturated by methane gas at a certain pore pressure by the methane injection pump 13, and the T2 spectrum of the shale sample 20 in a reservoir temperature and pressure state in a saturated methane state is tested by nuclear magnetic resonance equipment.
S3, measuring supercritical CO by utilizing nuclear magnetic resonance 2 T2 spectrum change of rock core in methane process in shale sample displacement process, and supercritical CO is calculated 2 Displacing shale gas efficiency in different occurrence states; by CO 2 The displacement pump 21 will be supercritical CO 2 Injecting the mixture into a rock core under the reservoir temperature and pressure condition at a certain pore pressure, and monitoring the T2 spectrum change of the shale sample 20 in real time by using nuclear magnetic resonance equipment and distinguishing methane in different occurrence states in the shale sample 20:
M sat ＝k*Amp sat equation 2
Wherein M is sat Amp, which is the amount of methane substances in different occurrence forms in shale samples in saturated methane state under reservoir temperature and pressure sat Integrating peak signal intensities of different relaxation time ranges in a T2 spectrum of the shale sample;
according to the morphology of the T2 spectrum of the shale sample, different occurrence states of methane in the shale sample are distinguished, and the methane passes through supercritical CO 2 The T2 spectrum change of the shale sample in the displacement process is utilized to calculate the supercritical CO by using the following formulas 3 and 4 2 Shale gas efficiency in different occurrence states is displaced:
M exp ＝k*Amp exp equation 3
Wherein M is exp At CO for shale sample 2 Amount of methane material in shale during methane displacement, amp exp For rock testSample at CO 2 T2 spectrum peak signal intensity integration in methane displacement process, E is supercritical CO 2 Shale gas displacement efficiency.
Example 1:
supercritical CO determination under reservoir temperature and pressure conditions 2 The method for displacing shale gas efficiency comprises the following steps:
(1) And connecting a polytetrafluoroethylene sample 1 with an outer diameter of 25mm, an inner diameter of 5mm and a height of 50mm, a left end cushion block 2 and a right end cushion block 3 together. And the polytetrafluoroethylene sample 1, the left end cushion block 2 and the right end cushion block 3 are tightly connected by utilizing the heat shrink tube 4. The aggregate of polytetrafluoroethylene sample 1, left-end pad 2, right-end pad 3 and heat shrink tubing 4 is then placed in core holder 5.
(2) And sucking the fluorine oil from the fluorine oil storage tank 7 by utilizing the axial pressure pump 6, opening the first needle valve 8, introducing the fluorine oil into an axial pressure chamber of the core holder 5, applying axial pressure to the polytetrafluoroethylene sample 1, setting the pressure to be 12Mpa, and using a first pressure gauge 9 for axial pressure monitoring.
(3) And introducing the heated FC40 solution into a confining pressure chamber of the core holder 5 by using a confining pressure circulating heat pump 10, and applying certain confining pressure to the polytetrafluoroethylene sample 1, wherein the pressure is set to be 10MPa. While the core holder 5 was heated to a specified temperature, which was set to 45 ℃.
(4) The second needle valve 11 was opened and the line was evacuated for a duration of 2 hours using the vacuum pump 12.
(5) High purity methane gas is extracted from the methane cylinder 14 by the methane injection pump 13. The third needle valve 15 was opened and methane was injected into the polytetrafluoroethylene sample 1 at different pore pressures of 2MPa, 4MPa, 6MPa and 8MPa, respectively. The second pressure gauge 16 is used to monitor the pore pressure value. Nuclear magnetic radio frequency pulses are transmitted by means of the NMR console 17 to the polytetrafluoroethylene sample 1 in the permanent magnet 18 and nuclear magnetic relaxation signals are received by means of the nuclear magnetic probe coil 19. The results of the T2 spectrum of methane of different Kong Yaxia in this example are shown in figure 2 a. According to the universal gas law, the relation between the amount of methane substances and the integral of the signal intensity of the peak of the T2 spectrum is calculated, and the calculation result is shown in fig. 2b and formula 5:
M＝8.425×10 -3 * Amp equation 5
Where M is the amount of methane species and Amp is the integral of the signal intensity of the peak of the T2 spectrum.
(6) The pressure was released, and the polytetrafluoroethylene sample 1 was taken out of the core holder 5.
(7) Shale samples 20 with a diameter of 25mm and a length of 50mm, left end pad 2 and right end pad 3 are connected together. The shale sample 20, the left end cushion block 2 and the right end cushion block 3 are tightly connected by utilizing the heat shrink tube 4. The aggregate of shale sample 20, left pad 2, right pad 3 and heat shrink tubing 4 is then placed in core holder 5.
(8) An axial pressure was applied to the shale sample 20 by the axial pressure pump 6, and the axial pressure was set to 12MPa. The confining pressure and the temperature were set to 10MPa and 45 ℃ respectively by applying confining pressure and heating to the shale sample 20 using the confining pressure circulation heating pump 10. The line was evacuated using vacuum pump 12 for a duration of 24 hours. Methane was injected into shale sample 20 at a pore pressure of 6MPa using methane injection pump 13 for 48 hours. Nuclear magnetic radio frequency pulses are transmitted using NMR console 17 and T2 spectra of shale sample 20 in saturated methane state at reservoir temperature and pressure are received using nuclear magnetic probe coil 19, the results of which are shown in fig. 3. Methane gas in the shale sample 20 may be classified into an adsorbed state (P1), a free state (P2), and a free state (P3) according to the nuclear magnetic resonance T2 spectrum morphology of the shale sample 20. Using equation 6, the amount of methane species in different occurrence forms of the shale sample 20 in the saturated methane state can be calculated.
M sat ＝8.425×10 -3 *Amp sat Equation 6
Wherein M is sat Amp, which is the amount of methane substances in different occurrence forms in shale samples in saturated methane state under reservoir temperature and pressure sat Peak signal intensities for different relaxation time ranges in the T2 spectrum of the shale sample are integrated.
| Methane state | Adsorption state | Free state | Free state | All methane |
| Integration of signal intensity | 96.72 | 694.65 | 184.87 | 976.24 |
| Methane substance amount (mmole) | 0.81 | 5.85 | 1.56 | 8.2 |
(9) By CO 2 Displacement pump 21 is from CO 2 High purity CO extraction from cylinder 22 2 And (3) gas. Open fourth needle valve 23, CO 2 Is injected into the shale sample 20 at a pore pressure of 8MPa. The pore pressure value is monitored using a third pressure gauge 24. The fifth needle valve 25 is opened, and the methane gas displaced is introduced into the atmosphere through the back pressure valve 26. Nuclear magnetic resonance is used to monitor the T2 spectrum changes of shale samples 20. CO in the present embodiment 2 The T2 spectrum of shale sample 20 during injection varies as shown in fig. 4. The nuclear magnetic signal intensity integral of methane in different states in shale sample 20 is calculated as shown in the following table:
the shale sample 20 of the embodiment of the invention is supercritical CO at an axial pressure of 12MPa, a confining pressure of 10MPa and a temperature of 45 DEG C 2 The amount and efficiency of the substance displacing methane can be found from equations 7 and 8:
M exp ＝8.425×10 -3 *Amp exp equation 7
Wherein M is ini And M exp In saturated methane state and CO for shale samples 2 Amount of methane material in shale during methane displacement, amp exp In saturated methane state and CO for rock sample 2 T2 spectrum peak signal intensity integration in methane displacement process, E is supercritical CO 2 Shale gas displacement efficiency.
The methane in the shale sample 20 in this example has 3 different states: adsorbed state (P1), free state (P2) and free state (P3), and the amount change of methane in the shale sample 20 and methane substances in the whole sample and CO are obtained through calculation 2 The result of the displacement efficiency calculation is shown in fig. 5.
The device and the method can be used for measuring supercritical CO under the reservoir temperature and pressure condition 2 Shale gas displacement efficiency, and the change rule of methane in different occurrence states is distinguished through screening of T2 spectrums.
Example 2:
supercritical CO determination under reservoir temperature and pressure conditions 2 The device for displacing shale gas efficiency comprises a warm-pressing loading unit, nuclear magnetic resonance equipment and a displacement seepage unit. The warm-pressing loading unit comprises a left end cushion block 2, a right end cushion block 3, a heat shrinkage tube 4, a core holder 5, a shaft pressing pump 6, a fluorine oil storage tank 7, a first needle valve 8, a first pressure gauge 9 and a surrounding wallThe pressure circulation heating pump 10 is connected through a pipeline, so that the sample is under the reservoir temperature and pressure conditions.
The polytetrafluoroethylene sample 1, the left end cushion block 2 and the right end cushion block 3 are spliced together, and the heat shrinkage tube 4 connects the above three into a whole and is put into the core holder 5. The axial pressure pump 6, the fluorine oil storage tank 7, the first needle valve 8, the first pressure gauge 9 and the axial pressure chamber of the core holder 5 are sequentially connected through pipelines. The axial pressure pump 6 sucks in the fluorine oil from the fluorine oil storage tank 7, and supplies the fluorine oil to the axial pressure chamber of the core holder 5 through the first needle valve 8, and applies an axial pressure to the polytetrafluoroethylene sample 1, the axial pressure being set to 12MPa. The confining pressure circulating heat pump 10 is connected with the confining pressure chamber of the core holder 5 through a pipeline and is used for applying confining pressure and temperature to the polytetrafluoroethylene sample 1. The confining pressure circulating heat pump 10 introduces the heated FC40 solution into the confining pressure chamber of the core holder 5, and applies confining pressure and temperature to the polytetrafluoroethylene sample 1, the pressure and temperature being set to 10MPa and 45 ℃.
The nuclear magnetic resonance equipment comprises an NMR control console 17, a permanent magnet 18 and a nuclear magnetic probe coil 19, which are connected through USB data lines. The NMR console 17 emits nuclear magnetic radio frequency pulses to the polytetrafluoroethylene sample 1 in the permanent magnet 18 and receives nuclear magnetic relaxation signals with the nuclear magnetic probe coil 19 for calculating the relation between the amount of methane material and the T2 spectral peak signal intensity integral.
The displacement seepage unit comprises a second needle valve 11, a vacuum pump 12, a methane injection pump 13, a methane gas cylinder 14, a third needle valve 15, a second pressure gauge 16 and CO 2 Displacement pump 21, CO 2 The gas cylinder 22, the fourth needle valve 23, the third pressure gauge 24, the fifth needle valve 25 and the back pressure valve 26, and the second needle valve 11 and the vacuum pump 12 are connected with the core holder 5 through pipelines. The second needle valve 11 and the vacuum pump 12 are connected by a pipe for evacuating the inside of the displacement system. The methane injection pump 13, the methane gas cylinder 14, the third needle valve 15, the second pressure gauge 16 and the displacement pipeline of the core holder 5 are sequentially connected through pipelines. The methane injection pump 13 extracts high purity methane gas from the methane cylinder 14, and the methane gas is introduced into the polytetrafluoroethylene sample 1 through the third needle valve 15 at different pore pressures, which are set to 2MPa, 4MPa, 6MPa, and 8MPa, respectively. CO 2 Displacement pump 21, CO 2 The gas cylinder 22, the fourth needle valve 23 and the third pressure gauge 24 are sequentially connected with the displacement pipeline of the core holder 5 through pipelines. CO 2 Displacement pump 21 is from CO 2 High purity CO extraction from cylinder 22 2 CO is fed through the fourth needle valve 23 2 Introducing a constant pressure into the shale sample 20 to develop CO 2 And (3) displacing methane experiments. The shale sample 20 is monitored for T2 spectral variation using nuclear magnetic resonance equipment.
The invention uses the polytetrafluoroethylene sample 1 to determine the relation between the amount of methane substances and the T2 spectrum peak signal intensity integral, and uses the shale sample 20 to develop CO 2 And (3) displacing methane experiments. The shale sample 20 and the polytetrafluoroethylene sample 1 occupy spatially the same position but in a different order of use in time.
The above is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should understand that the obtained changes or substitutions are included in the scope of the present invention.
Claims (4)
1. Supercritical CO determination under reservoir temperature and pressure conditions 2 The method for displacing shale gas efficiency is characterized by comprising the following steps:
s1, calibrating the relation between the amount of methane substances and the integral of the signal intensity of the nuclear magnetic resonance T2 spectrum peak by using a polytetrafluoroethylene sample; placing a polytetrafluoroethylene sample into a core holder, applying axial pressure to the polytetrafluoroethylene sample by using an axial pressure pump, then introducing a heated FC40 solution into a confining pressure chamber of the core holder by using a confining pressure circulating heating pump, applying confining pressure to the polytetrafluoroethylene sample, and heating the core holder to a specified temperature; under the condition of constant temperature and constant pressure, vacuumizing a pipeline by using a vacuum pump, injecting methane into a polytetrafluoroethylene sample at different pore pressures by using a methane injection pump, testing the nuclear magnetic resonance T2 spectrum of the polytetrafluoroethylene sample by using nuclear magnetic resonance equipment, and obtaining the linear relation between the amount of methane substances and the integral of the peak signal intensity of the nuclear magnetic resonance T2 spectrum by using a universal gas law:
M=k*Amp （1）
wherein M is the amount of methane substance, k is a linear correlation coefficient, and Amp is the integral of the peak signal intensity of the nuclear magnetic resonance T2 spectrum, namely the envelope area formed by the T2 spectrum and the x axis;
s2, using methane to saturate shale samples under the reservoir temperature and pressure condition; placing a shale sample into a core holder, applying axial pressure to the shale sample by using an axial pressure pump, introducing a heated FC40 solution into a confining pressure chamber of the core holder by using a confining pressure circulating heating pump, applying confining pressure to the shale sample, and heating the shale sample to a specified temperature; using a methane injection pump to saturate methane gas with a certain pore pressure to a shale sample, and using nuclear magnetic resonance equipment to test a T2 spectrum of the shale sample in a reservoir temperature and pressure state in a saturated methane state;
s3, measuring supercritical CO by utilizing nuclear magnetic resonance 2 T2 spectrum change of rock core in methane process in shale sample displacement process, and supercritical CO is calculated 2 Displacing shale gas efficiency in different occurrence states; by CO 2 Displacement pump will be supercritical CO 2 Injecting the mixture into a rock core under the reservoir temperature and pressure condition by a certain pore pressure, and monitoring the T2 spectrum change of the shale sample in real time by using nuclear magnetic resonance equipment and distinguishing methane in different occurrence states in the shale sample:
=k*/> （2）
wherein,the amount of methane substances with different occurrence forms in the shale sample in the saturated methane state under the reservoir temperature and pressure state is +.>Integrating peak signal intensities of different relaxation time ranges in a T2 spectrum of the shale sample;
according to the morphology of the T2 spectrum of the shale sample, different occurrence states of methane in the shale sample are distinguished, and the methane passes through supercritical CO 2 T2 spectrum change of shale sample in displacement process, and supercritical CO is calculated 2 Shale gas efficiency in different occurrence states is displaced:
=k*/> （3）
（4）
wherein,CO for shale sample 2 Amount of methane material in shale during displacement of methane,/->For rock sample at CO 2 T2 spectral peak signal intensity integration during methane displacement, +.>Is supercritical CO 2 Shale gas displacement efficiency.
2. Supercritical CO determination under reservoir temperature and pressure conditions 2 The device for displacing the shale gas efficiency is characterized by comprising a warm-pressing loading unit, nuclear magnetic resonance equipment and a displacement seepage unit;
the warm-pressing loading unit comprises a left end cushion block, a right end cushion block, a heat shrinkage pipe, a core holder, a shaft pressure pump, a fluorine oil storage tank, a first needle valve, a first pressure gauge and a confining pressure circulating heating pump, wherein the polytetrafluoroethylene sample, the left end cushion block and the right end cushion block are spliced together, the heat shrinkage pipe is connected into a whole and is placed into the core holder, the shaft pressure pump, the fluorine oil storage tank, the first needle valve and the first pressure gauge are connected through pipelines, and the core holder is connected with the confining pressure circulating heating pump through the pipelines;
the nuclear magnetic resonance equipment comprises an NMR control console, a permanent magnet and a nuclear magnetic probe coil, which are connected through a USB data line;
the displacement seepage unit comprises a second needle valve, a vacuum pump, a methane injection pump, a methane gas cylinder, a third needle valve, a second pressure gauge and CO 2 Displacement pump, CO 2 The second needle valve and the vacuum pump are connected with the core holder through pipelines; the methane injection pump, the methane gas cylinder, the third needle valve and the second pressure gauge are connected with the core holder through pipelines; the CO 2 Displacement pump, CO 2 The gas cylinder, the fourth needle valve and the third pressure gauge are connected with the core holder through pipelines; the fifth needle valve and the back pressure valve are connected with the core holder through pipelines.
3. The method for determining supercritical CO under the reservoir temperature and pressure conditions of claim 2 2 The device for displacing shale gas efficiency is characterized in that the axial pressure pump is used for injecting the fluorine oil in the fluorine oil storage tank into the core holder and applying axial pressure to the polytetrafluoroethylene sample and the shale sample; the confining pressure circulating heat pump is used for applying confining pressure to the polytetrafluoroethylene sample and the shale sample and heating the polytetrafluoroethylene sample and the shale sample to a specified temperature.
4. The method for determining supercritical CO under the reservoir temperature and pressure conditions of claim 2 2 The device for displacing the shale gas efficiency is characterized in that the nuclear magnetic probe coil is used for transmitting a nuclear magnetic resonance pulse sequence and receiving a relaxation signal of methane gas in a sample;
the permanent magnet is used for manufacturing a main magnetic field environment with constant field intensity;
the NMR control console is used for controlling the nuclear magnetic probe coil to transmit pulse sequences, and receiving and processing relaxation signals of methane gas.
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