CN117538236B - Shale overburden pore infiltration combined measurement device and method - Google Patents

Shale overburden pore infiltration combined measurement device and method Download PDF

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CN117538236B
CN117538236B CN202410020573.4A CN202410020573A CN117538236B CN 117538236 B CN117538236 B CN 117538236B CN 202410020573 A CN202410020573 A CN 202410020573A CN 117538236 B CN117538236 B CN 117538236B
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shale
pressure
gas
sample
valve
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CN117538236A (en
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杨峰
聂思嘉
徐尚
蒋恕
刘亚松
王欢
罗隆
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China University of Geosciences
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China University of Geosciences
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Abstract

The invention discloses a shale overburden pressure hole infiltration combined measurement device and a shale overburden pressure hole infiltration combined measurement method, wherein the device comprises a helium gas source, a reference chamber, a differential pressure sensor, a sample clamping system, a temperature control system, a confining pressure loading system, a shaft pressure loading system, a vacuumizing system and a pipe valve system; the reference chamber is respectively connected with the sample clamping system, the helium source and the vacuumizing system through the pipe valve system; the vacuumizing system is respectively connected with the sample clamping system, the reference chamber and the external environment through the pipe valve system; the confining pressure loading system and the axial pressure loading system are respectively connected with the sample clamping system; the differential pressure sensor is respectively arranged at the reference chamber, the axial pressure loading system and the confining pressure loading system; the reference chamber, the differential pressure sensor, the sample clamping system, and the tube valve system are all disposed within the temperature control system. The combined test of shale porosity and permeability in situ is realized.

Description

Shale overburden pore infiltration combined measurement device and method
Technical Field
The invention relates to the technical field of rock physical property measurement of shale porosity, permeability and the like, in particular to a shale overburden pore permeation combined measurement device and method.
Background
Shale oil gas is taken as a typical unconventional oil gas resource, is an important successor resource for increasing the storage and the production in the petroleum field of China, and has important strategic significance for guaranteeing the resource energy safety of China. Shale oil and gas refers to oil and gas resources contained in shale-based reservoirs, including oil and gas in shale pores and cracks, and oil and gas in adjacent and interbedded organic-lean reservoirs, wherein the geological storage of shale gas in China is up to 134.42 ×10 12 m 3 Shale oil geological storage amounts to 335 x 10 8 t. The porosity and permeability of shale reflect the storage and flow capacities of the reservoir, respectively, so that accurate calculation of the porosity and permeability of shale is critical to the exploration and development of shale oil and gas.
At present, a low-pressure helium expansion method based on Boyle's law of gas is mainly adopted for testing shale porosity, and a pulse testing method based on gas diffusion is mainly adopted for testing shale permeability. The two methods are widely used because of simple test instruments, low test cost and simple test flow. Both of the above devices typically operate under low pressure conditions and require separate individual testing of the samples in sequence. However, the shale porosity and permeability under the actual formation pressure are more practical, and the sample after the porosity or permeability test is completed is likely to generate new changes, and the test result is easily influenced by another test, so that the deviation between the test result and the actual condition of the formation in-situ state is caused.
Disclosure of Invention
In view of the above, the invention provides a shale overburden pore infiltration combined measurement device and a shale overburden pore infiltration combined measurement method, which realize accurate quantitative calculation of shale porosity and permeability in a stratum in-situ state, greatly simplify the test flow of the existing device and have higher accuracy. Meanwhile, the device can be used for displacement experiments under different temperature and pressure conditions, and has multiple purposes.
According to one aspect of the invention, there is provided a shale overburden pore infiltration combined measuring device, the device comprising a helium source, a reference chamber, a differential pressure sensor, a sample clamping system, a temperature control system, a confining pressure loading system, an axial pressure loading system, a vacuum pumping system and a pipe valve system;
the reference chamber is respectively connected with the sample clamping system, the helium source and the vacuumizing system through the pipe valve system;
the vacuumizing system is respectively connected with the sample clamping system, the reference chamber and the external environment through the pipe valve system;
the confining pressure loading system and the axial pressure loading system are respectively connected with the sample clamping system;
the differential pressure sensor is respectively arranged at the reference chamber, the axial pressure loading system and the confining pressure loading system;
The reference chamber, the differential pressure sensor, the sample clamping system, and the tube valve system are all disposed within the temperature control system.
Optionally, the pipe valve system comprises a first valve, a second valve, a third valve, a pipeline and a three-way joint on the pipeline;
the first valve is arranged on a pipeline between the reference chamber and the helium source;
the three-way joint is connected with the reference chamber through the second valve, is connected with the second top shaft of the sample clamping system through the third valve and is connected with the first top shaft of the sample clamping system, wherein the third valve is a four-way valve, and a connecting pipeline forms a passage and is connected with the external environment and the vacuumizing system.
Optionally, the confining pressure loading system is composed of a confining pressure loading pump; the axial pressure loading system consists of an axial pressure loading pump;
the confining pressure loading pump is used for loading confining pressure to the sample clamping system;
the axial pressure loading pump is used for loading axial pressure to the sample holding system.
Optionally, the temperature control system is an incubator with a temperature adjusting function, and the incubator is used for controlling the temperature of the shale overburden pore infiltration combined measuring device.
Optionally, the vacuumizing system comprises a vacuum pump with an exhaust pipe, and the vacuum pump is used for vacuumizing the shale overburden pore infiltration combined measuring device.
Optionally, the reference chamber has a volume of V ref =2cm 3 The pipeline volume between the reference chamber and the second valve is V l1 The pipeline volume between the second valve and the three-way joint is V l2 The volume of the pipeline between the three-way joint and the upstream of the sample clamping system is V l3 The pipeline volume between the three-way joint and the third valve is V l4 The volume of the pipeline between the third valve and the downstream of the sample clamping system is V l5 And the total volume of the pipelines of each part is V l =V l1 +V l2 +V l3 +V l4 +V l5 =3.440553cm 3
Optionally, sample clamping system is the structure that inside has the cavity, including the outside steel of holder, heat preservation, annular circle, tubular rubber sleeve, first apical axis, second apical axis and sample storehouse, the sample storehouse is used for placing the shale sample that awaits measuring.
Optionally, the differential pressure sensor includes a first differential pressure sensor, a second differential pressure sensor, a third differential pressure sensor;
the differential pressure sensor arranged at the reference chamber is the first differential pressure sensor;
The differential pressure sensor arranged at the axle pressure loading system is the second differential pressure sensor;
and the differential pressure sensor arranged at the confining pressure loading system is the third differential pressure sensor.
According to another aspect of the invention, a shale coverage hole seepage joint measurement method is provided, and the shale coverage hole seepage joint measurement method is applied to the shale coverage hole seepage joint measurement device, wherein the pipe valve system comprises a first valve, a second valve, a third valve, a pipeline and a three-way joint on the pipeline; the reference chamber and the reference chamberThe first valve is arranged on a pipeline between the helium sources; the three-way joint is connected with the reference chamber through the second valve, is connected with a second top shaft of the sample clamping system through the third valve and is connected with a first top shaft of the sample clamping system, wherein the third valve is a four-way valve, and a connecting pipeline forms a passage and is simultaneously connected with the external environment and the vacuumizing system; the differential pressure sensor arranged at the reference chamber is the first differential pressure sensor; the volume of the reference chamber is V ref The pipeline volume between the reference chamber and the second valve is V l1 The pipeline volume between the second valve and the three-way joint is V l2 The volume of the pipeline between the three-way joint and the upstream of the sample clamping system is V l3 The pipeline volume between the three-way joint and the third valve is V l4 The volume of the pipeline between the third valve and the downstream of the sample clamping system is V l5 And the total volume of the pipelines of each part is V l =V l1 +V l2 +V l3 +V l4 +V l5 =3.440553cm 3
The method comprises the following steps:
acquiring a shale sample to be tested in a preset mode, recording the apparent diameter d and the apparent length L of the shale sample to be tested, and placing the shale sample to be tested into a sample bin of a sample clamping system so as to test at each temperature and pressure point;
under any temperature and pressure point, a first valve, a second valve and a third valve are opened, a vacuumizing system is started to vacuumize the shale covering pressure hole seepage joint measuring device, air tightness inspection is carried out, and when the air tightness inspection is qualified, the first valve, the second valve and the third valve are closed;
setting the temperature of the temperature control system according to the temperature required by the test;
according to the test requirement, loading the axial pressure and the confining pressure of the sample clamping system by using a confining pressure loading system and an axial pressure loading system;
opening the valveThe first valve is closed when the reading of the first differential pressure sensor is kept unchanged within a first preset time period, and the reading of the first differential pressure sensor is recorded to obtain the initial gas pressure p of the reference chamber after the helium is introduced into the reference chamber ref The method comprises the steps of carrying out a first treatment on the surface of the Opening the second valve and the third valve to enable the gas of the reference chamber to be introduced into the sample clamping system, and recording the reading of the first differential pressure sensor to obtain the gas pressure p in the shale overburden pore permeation combined measuring device in the process of diffusing the gas to the shale sample to be measured t The method comprises the steps of carrying out a first treatment on the surface of the When the reading of the first differential pressure sensor is kept unchanged within a second preset time period, recording the reading of the first differential pressure sensor to obtain the gas pressure p after the pressure in the shale overburden pore permeation combined measuring device is balanced eq
Based on the volume V of the reference chamber ref Total volume V of the pipelines of each part l Initial gas pressure p of the reference chamber after introducing helium into the reference chamber ref The pressure p of the gas after pressure balance in the shale overburden pressure hole seepage joint measuring device eq, Calculating the overburden pore volume V in the shale sample to be measured p The method comprises the steps of carrying out a first treatment on the surface of the Based on the overburden pore volume V p Calculating the overburden porosity of the shale sample to be measured, the apparent diameter d of the shale sample to be measured and the apparent length L of the shale sample to be measured
Acquiring initial gas pressure p in shale overburden pore infiltration combined measuring device when gas starts to infiltrate into shale sample to be measured max Gas viscosity of helium at the temperature and pressure point Gas compression coefficient c of helium at said temperature and pressure point g Based on initial gas pressure p in shale overburden pore infiltration combined measurement device when gas starts to infiltrate into shale sample to be measured max The gas viscosity->The place of saleThe gas compression coefficient c g The appearance length L of the shale sample to be tested and the overburden porosity +.>Volume V of the reference chamber ref Total volume V of the pipelines of each part l The pore volume V of the coating p The pressure p of the gas after pressure balance in the shale overburden pressure hole seepage joint measuring device eq The gas pressure p in the shale overburden pore permeation combined measuring device in the diffusion process of the gas to the shale sample to be measured t Calculating the overburden permeability k of the shale sample to be measured;
unloading the confining pressure and the axial pressure of the sample clamping system, and discharging residual gas in the shale overburden pore infiltration combined measuring device by opening one end of the third valve connected with the external environment;
and continuing iteration until the test of the shale sample to be tested at all temperature and pressure points is completed.
By means of the technical scheme, the shale overburden pore infiltration combined testing device and the shale overburden pore infiltration combined testing method are capable of simulating the temperature and the pressure of the shale reservoir under the in-situ condition by connecting the reference chamber with the known volume and the pipeline with the known volume with the sample clamping system and simultaneously arranging the accurate confining pressure loading system, the shaft pressure loading system and the temperature control system, overcome the defect that the shale porosity test and the permeability test are separated in the prior art, greatly simplify the testing flow, and realize the accurate test of shale pore infiltration under the in-situ condition of the stratum. The invention has important roles in the effective exploration and development of shale oil gas.
The foregoing description is only an overview of the present invention, and is intended to be implemented in accordance with the teachings of the present invention in order that the same may be more clearly understood and to make the same and other objects, features and advantages of the present invention more readily apparent.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and do not constitute a limitation on the invention. In the drawings:
fig. 1 shows a schematic structural diagram of a shale overburden pore infiltration combined measurement device according to an embodiment of the present invention;
FIG. 2 is a schematic diagram showing a pressure curve of a gas in a process of diffusing the gas into a shale sample to be tested after a gas pulse is applied to a testing device according to an embodiment of the present invention;
fig. 3 is a schematic diagram showing a ratio change curve of the cumulative amount of gas entering pores of a shale sample to be tested at different moments and the amount of all gases in the pore space of the shale sample in a final state in the process of diffusing the gas to the shale sample to be tested in the test process provided by the embodiment of the invention;
FIG. 4 shows a test time lnF provided by an embodiment of the invention r Graph with time t.
Reference numerals in fig. 1 are respectively expressed as:
1-helium source, 2-first valve, 3-first differential pressure sensor, 4-reference room, 5-second valve, 6-three way connection, 7-first jackshaft, 8-second differential pressure sensor, 9-axle pressure booster pump, 10-third differential pressure sensor, 11-sample storehouse, 12-confining pressure booster pump, 13-second jackshaft, 14-third valve, 15-vacuum pump, 16-holder external steel, 17-heat preservation, 18-annular ring, 19-tubular rubber sleeve, 20-thermostated container.
Detailed Description
The invention will be described in detail hereinafter with reference to the drawings in conjunction with embodiments. It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other.
In this embodiment, a shale overburden pore permeability testing device is provided, as shown in fig. 1, and the device includes: helium gas source 1, reference chamber 4, differential pressure sensor, sample clamping system, temperature control system, confining pressure loading system, shaft pressure loading system, evacuation system, and pipe valve system.
The reference chamber 4 is connected to the sample holding system, the helium source 1 and the evacuation system, respectively, by the tube valve system.
The vacuum pumping system is respectively connected with the sample clamping system, the reference chamber 4 and the external environment through the pipe valve system.
The confining pressure loading system and the axial pressure loading system are respectively connected with the sample clamping system.
The differential pressure sensors are respectively arranged at the reference chamber 4, the axle pressure loading system and the confining pressure loading system.
The reference chamber 4, the differential pressure sensor, the sample clamping system and the tube valve system are all placed within the temperature control system.
The shale overburden pore infiltration combined measurement device provided by the embodiment of the invention is suitable for combined measurement of shale porosity and permeability under the in-situ condition of the stratum. In this embodiment, the shale overburden pore penetration testing device comprises a helium gas source 1, a reference chamber 4, a differential pressure sensor, a sample clamping system, a temperature control system, a confining pressure loading system, an axial pressure loading system, a vacuumizing system and a pipe valve system; the reference chamber 4 is respectively connected with the sample clamping system, the helium source 1 and the vacuumizing system through a pipe valve system and is used for receiving helium gas fed by the helium source 1 through the pipe valve system and feeding the helium gas into the sample clamping system. The vacuumizing system is respectively connected with the sample clamping system, the reference chamber 4 and the external environment through the pipe valve system and is used for vacuumizing the shale overburden pressure hole seepage joint measuring device. The confining pressure loading system and the axial pressure loading system are respectively connected with the sample clamping system and are used for loading confining pressure and axial pressure on the sample clamping system respectively. The differential pressure sensors are respectively arranged at the reference chamber 4, the shaft pressure loading system and the confining pressure loading system and are used for respectively measuring gas pressure data corresponding to the reference chamber 4, the shaft pressure loading system and the confining pressure loading system. The reference chamber 4, the differential pressure sensor, the sample holding system and the tube valve system are all placed in a temperature control system for controlling the temperature of the whole set of apparatus. The sample clamping system is used for placing the shale sample to be tested.
Optionally, the pipe valve system comprises a first valve 2, a second valve 5, a third valve 14, a pipeline and a three-way connection 6 on the pipeline; the first valve 2 is arranged on a pipeline between the reference chamber 4 and the helium source 1; the three-way joint 6 is connected with the reference chamber 4 through the second valve 5, is connected with the second top shaft 13 of the sample clamping system through the third valve 14, and is connected with the first top shaft 7 of the sample clamping system, wherein the third valve 14 is a four-way valve, and a connecting pipeline forms a passage and is simultaneously connected with the external environment and the vacuumizing system.
In this embodiment, the pipe valve system comprises a first valve 2, a second valve 5, a third valve 14, a line and a three way connection 6 on the line, wherein the first valve 2 is arranged on the line between the reference chamber 4 and the helium source 1. The three-way joint 6 is connected with the reference chamber 4 through the second valve 5, is connected with the second top shaft 13 of the sample clamping system through the third valve 14 and is connected with the first top shaft 7 of the sample clamping system, wherein the first valve 2 and the second valve 5 are two-way valves which can be connected with pipelines to form a gas passage, and the third valve 14 is a four-way valve which can be connected with the pipelines to form a gas passage and be communicated with the external atmospheric environment and is also connected with the vacuumizing system.
Optionally, the confining pressure loading system is composed of a confining pressure loading pump 12; the axial pressure loading system consists of an axial pressure loading pump 9; the confining pressure loading pump 12 is used for loading confining pressure to the sample clamping system; the axial pressure loading pump 9 is used for loading axial pressure to the sample holding system.
In this embodiment, the loading or unloading process of the confining pressure and the axial pressure is manually set by keys on the confining pressure pressurizing pump 12 and the axial pressure pressurizing pump 9, and the confining pressure can be loaded at the maximum of 70MPa and the axial pressure can be loaded at the maximum of 70MPa.
Optionally, the temperature control system is an incubator 20 with a temperature adjusting function, and the incubator 20 is used for controlling the temperature of the shale coverage hole infiltration combined measuring device.
In this embodiment, the temperature control system is an incubator 20 with a temperature adjusting function, and is used for controlling the temperature of the whole set of device, the temperature adjusting range of the incubator 20 is room temperature to 300 ℃, and the temperature control precision is 0.5 ℃. The reference chamber 4, differential pressure sensor, sample holding system, and tube valve system are all placed within an incubator 20.
Optionally, the vacuumizing system is composed of a vacuum pump 15 with an exhaust pipe, and the vacuum pump 15 is used for vacuumizing the shale overburden pore infiltration combined measuring device.
In this embodiment, the vacuum pumping system is composed of a vacuum pump 15 with an exhaust pipe, and is connected with the reference chamber 4, the sample clamping system and the external atmospheric environment through a pipe valve system, so as to perform vacuum pumping treatment on the shale overburden pore infiltration combined measuring device.
Optionally, the reference chamber has a volume of V ref =2cm 3 The pipeline volume between the reference chamber 4 and the second valve 5 is V l1 The pipeline volume between the second valve 5 and the three-way joint 6 is V l2 The volume of the pipeline between the three-way joint 6 and the upstream of the sample clamping system is V l3 The pipeline volume between the three-way joint 6 and the third valve 14 is V l4 The line volume between the third valve 14 and downstream of the sample holding system is V l5 And the total volume of the pipelines of each part is V l =V l1 +V l2 +V l3 +V l4 +V l5 =3.440553cm 3
In the present embodiment, the volume of the reference chamber 4, the volume of the pipeline between the reference chamber 4 and the second valve 5, the volume of the pipeline between the second valve 5 and the three-way joint 6, the volume of the pipeline between the three-way joint 6 and the upstream of the sample holding system, the volume of the pipeline between the three-way joint 6 and the third valve 14, and the volume of the pipeline between the third valve 14 and the downstream of the sample holding system are all known, and are precisely calibrated and respectively known as V ref 、V l1 、V l2 、V l3 、V l4 、V l5 And V is ref =2cm 3 The total volume of the pipelines of each part is V l =V l1 +V l2 +V l3 +V l4 +V l5 =3.440553cm 3
Optionally, the sample clamping system is a structure with a cavity inside, and comprises a clamp holder outer steel 16, a heat insulation layer 17, an annular ring 18, a cylindrical rubber sleeve 19, a first top shaft 7, a second top shaft 13 and a sample bin 11, wherein the sample bin 11 is used for placing a shale sample to be tested.
In this embodiment, the inside of the sample clamping system is provided with a cavity structure, and the sample clamping system comprises a first top shaft 7, a second top shaft 13, a clamp holder external steel 16, a heat insulation layer 17, an annular ring 18, a cylindrical rubber sleeve 19 and a sample bin 11, wherein the sample bin 11 is used for placing a shale sample to be tested, the internal diameter is 2.6cm, and the internal length is 10cm. The steel 16 outside the clamp is made of 316L stainless steel, and the highest bearing confining pressure and the highest bearing shaft pressure of the sample clamping system are 75MPa and 75MPa respectively.
Optionally, the differential pressure sensor includes a first differential pressure sensor 3, a second differential pressure sensor 8, and a third differential pressure sensor 10; the differential pressure sensor arranged at the reference chamber 4 is the first differential pressure sensor 3; the differential pressure sensor arranged at the axle pressure loading system is the second differential pressure sensor 8; the differential pressure sensor arranged at the confining pressure loading system is the third differential pressure sensor 10.
In this embodiment, the first differential pressure sensor 3, the second differential pressure sensor 8 and the third differential pressure sensor 10 are all configured with communication interfaces to be connected with a computer, and pressure data is recorded in real time through computer software. The first differential pressure sensor 3 registers the initial gas pressure p of the reference chamber after the introduction of helium into the reference chamber 4 ref And gas pressure p in shale overburden pore infiltration combined measuring device in diffusion process of gas to shale sample to be measured t Pressure p of gas after pressure balance in shale overburden pressure hole seepage combined measuring device eq Namely, the first differential pressure sensor 3 can measure the gas pressure in the shale overburden pore infiltration combined measuring device in real time during the test; the second differential pressure sensor 8 registers the axial pressure p of the axial pressure loading pump to the sample holding system a The method comprises the steps of carrying out a first treatment on the surface of the The third differential pressure sensor 10 registers the confining pressure p applied by the confining pressure loading pump to the sample clamping system c The method comprises the steps of carrying out a first treatment on the surface of the The highest withstand voltage of the first differential pressure sensor 3 is 30MPa, and the measurement accuracy is 0.05 percent, namely 15KPa; second differential pressure sensor8. The highest pressure resistance of the third differential pressure sensor 10 is 50MPa, and the measurement accuracy is 0.05 percent, namely 25KPa.
By applying the technical scheme of the embodiment, the reference chamber 4 with known volume and the pipeline with known volume are connected with the sample clamping system, and meanwhile, the accurate confining pressure loading system, the axial pressure loading system and the temperature control system are arranged, so that the temperature and the pressure of the shale reservoir under the in-situ condition can be simulated, the defect that the shale porosity test and the permeability test are separated in the prior art is overcome, the test flow is greatly simplified, and the accurate test of shale pore permeation under the stratum in-situ condition is realized. The invention has important roles in the effective exploration and development of shale oil gas.
Further, as a refinement and expansion of the specific implementation of the above embodiment, in order to fully describe the specific implementation process of the embodiment, another shale overburden pore permeability testing method is provided, which is applied to the shale overburden pore permeability combined testing device, where the pipe valve system includes a first valve 2, a second valve 5, a third valve 14, a pipeline and a three-way joint 6 on the pipeline; the first valve 2 is arranged on a pipeline between the reference chamber 4 and the helium source 1; the three-way joint 6 is connected with the reference chamber 4 through the second valve 5, is connected with the second top shaft 13 of the sample clamping system through the third valve 14 and is connected with the first top shaft 7 of the sample clamping system, wherein the third valve 14 is a four-way valve, and a connecting pipeline forms a passage and is simultaneously connected with the external environment and the vacuumizing system; the differential pressure sensor arranged at the reference chamber 4 is the first differential pressure sensor 3; the volume of the reference chamber 4 is V ref The pipeline volume between the reference chamber 4 and the second valve 5 is V l1 The pipeline volume between the second valve 5 and the three-way joint 6 is V l2 The volume of the pipeline between the three-way joint 6 and the upstream of the sample clamping system is V l3 The pipeline volume between the three-way joint 6 and the third valve 14 is V l4 The line volume between the third valve 14 and downstream of the sample holding system is V l5 And the total volume of the pipelines of each part is V l =V l1 +V l2 +V l3 +V l4 +V l5 =3.440553cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The method comprises the following steps:
step 201, obtaining a shale sample to be tested in a preset mode, recording the appearance diameter d of the shale sample to be tested and the appearance length L of the shale sample, and placing the shale sample to be tested into a sample clamping system so as to test at each temperature and pressure point.
In the embodiment, a test sample is prepared firstly, namely, an obtained shale sample is drilled into a cylindrical rock core with the diameter of 2.5cm and the length of not more than 10cm, two ends of the sample are polished smoothly, when the length of the sample is measured, the error of three times of measurement is not more than 0.05mm, and the shale sample is dried at the temperature required by the test for 24 hours, so that the shale sample to be measured in a preset mode is obtained. After obtaining the predetermined pattern of the shale sample to be tested, the diameter d and the length L thereof are recorded, and the predetermined pattern of the shale sample to be tested is placed into the sample compartment 11 of the sample holding system for testing at each warm-pressing point.
Step 202, under any temperature and pressure point, opening the first valve 2, the second valve 5 and the third valve 14, starting a vacuum pumping system to perform vacuum pumping treatment on the shale overburden pore permeation testing device, performing air tightness inspection, and closing the first valve 2, the second valve 5 and the third valve 14 when the air tightness inspection is qualified.
Then, vacuumizing the shale covered pore infiltration combined measuring device and checking the air tightness, namely, after a shale sample to be measured in a preset mode is placed into a sample bin 11 of a sample clamping system, opening a first valve 2, a second valve 5 and a third valve 14, starting a vacuum pump 15 in a vacuumizing system to vacuumize the shale covered pore infiltration combined measuring device, wherein the vacuumizing time is 3-6 h, and completing the vacuumizing step when the reading of a pressure gauge of the vacuum pump 15 is reduced to-0.1 MPa. And then, performing air tightness inspection of the device, closing the vacuum pump 15 for 3 hours, and if the reading of the pressure gauge of the vacuum pump 15 is unchanged, indicating that the whole set of device is good in air tightness, namely, qualified in air tightness inspection, and closing the first valve 2, the second valve 5 and the third valve 14 after the air tightness inspection is finished.
And 203, setting the temperature of the temperature control system according to the temperature required by the test.
Then, a test temperature is set, that is, the temperature of the incubator 20 of the temperature control system is set according to the temperature environment required by the test, after the temperature is set, the incubator 20 waits for 1 hour, and after the temperature environment in the incubator 20 is stabilized, the next step is performed and the set temperature T is recorded.
And 204, pressurizing the sample clamping system by using a confining pressure loading system and an axial pressure loading system according to the test requirements.
Then, the confining pressure and the shaft pressure are loaded, namely, according to the test requirement, the shaft pressure pressurizing pump 9 in the shaft pressure loading system and the keys on the confining pressure pressurizing pump 12 in the confining pressure loading system are used for loading the shaft pressure and the confining pressure on the sample clamping system, and the attention is paid to the fact that the confining pressure and the shaft pressure are set to be slowly pressurized according to the pressurizing gradient not exceeding 2MPa, and each time one pressure gradient is added, the next pressurizing is needed to be carried out after waiting for 5 minutes. And the final confining pressure and the axial pressure are not more than 70MPa, and after the confining pressure and the axial pressure are loaded, the shale sample to be tested is ensured to be stable under the pressure environment and then is tested after waiting for 24 hours.
Step 205, opening the first valve 2, introducing helium into the reference chamber 4, closing the first valve 2 when the reading of the first differential pressure sensor 3 remains unchanged for a first preset period of time, and recording the reading of the first differential pressure sensor 3 to obtain an initial gas pressure p of the reference chamber 4 after introducing helium into the reference chamber 4 ref The method comprises the steps of carrying out a first treatment on the surface of the Opening the second valve 5 and the third valve 14 to enable the gas in the reference chamber 4 to be introduced into the sample clamping system, and recording the reading of the first differential pressure sensor 3 to obtain the gas pressure p in the shale overburden pore permeation combined measuring device in the process of diffusing the gas to the shale sample to be measured t The method comprises the steps of carrying out a first treatment on the surface of the When the reading of the first differential pressure sensor 3 is kept unchanged within a second preset time period, recording the reading of the first differential pressure sensor 3 to obtain the gas pressure p after the pressure in the shale overburden pore permeation combined measuring device is balanced eq
Next, a test is performed, i.e. the helium source 1 and the first valve 2 are opened, andhelium gas is fed into the reference chamber 4 from the helium gas source 1, wherein the pressure of the fed helium gas can be controlled by adjusting a pressure regulating valve on the helium gas source 1. After helium is introduced into the reference chamber 4, monitoring the reading of the first differential pressure sensor 3, closing the first valve 2 when the reading of the first differential pressure sensor 3 reaches a preset upstream gas pressure value and remains unchanged for a first preset period of time, and recording the reading of the first differential pressure sensor 3 at the moment to obtain the initial gas pressure p of the reference chamber 4 after helium is introduced into the reference chamber 4 ref Wherein the first preset duration is at least 10min. Then, the gas of the reference chamber 4 is introduced into the sample clamping system by opening the second valve 5 and the third valve 14, and the reading of the first differential pressure sensor 3 is monitored and recorded in real time to obtain the gas pressure p in the shale overburden pore infiltration combined measuring device in the process of diffusing the gas to the shale sample to be measured t . The gas pressure p in the shale overburden pore infiltration combined measuring device in the process of diffusing the obtained gas to the shale sample to be measured t After that, continuously monitoring the reading of the first differential pressure sensor 3 until the reading of the first differential pressure sensor 3 is kept unchanged within a second preset time, recording the reading of the first differential pressure sensor 3, and obtaining the gas pressure p after the pressure in the shale overburden pore infiltration combined measuring device is balanced eq Wherein the second preset duration may be 1h. The gas pressure p after pressure balance in the shale overburden pore infiltration combined measuring device is obtained eq And then ending the test of the temperature and pressure point.
Step 206, based on the volume V of the reference chamber 4 ref Total volume V of the pipelines of each part l The initial gas pressure p of the reference chamber 4 after the helium is introduced into the reference chamber 4 ref The pressure p of the gas after pressure balance in the shale overburden pressure hole seepage joint measuring device eq, Calculating the overburden pore volume V in the shale sample to be measured p The method comprises the steps of carrying out a first treatment on the surface of the Based on the overburden pore volume V p Calculating the overburden porosity of the shale sample to be measured, the apparent diameter d of the shale sample to be measured and the apparent length L of the shale sample to be measured
Then, based on an ideal gas state equation, the shale sample to be tested is subjected to overburden porosity at the temperature and pressure point And calculating, wherein the state equation expression of the ideal gas is as follows:
(equation I)
Wherein p is the gas pressure, bar; v is the gas volume, m 3 The method comprises the steps of carrying out a first treatment on the surface of the n is the amount of gaseous material, mol; r is molar gas constant, J/mol.K; t is the gas temperature, K.
In this embodiment, the gas temperature T is kept constant and the amount n of the gas substance is kept constant and the molar gas constant R is also kept constant during the test at each temperature and pressure point. Therefore, the whole set of testing device in the testing process meets the following formula:
(equation II)
Wherein p is ref For the initial gas pressure of the reference chamber 4 after the introduction of helium into the reference chamber 4, bar,; v (V) ref For reference of the volume of the chamber 4 cm 3 Known as 2cm 3 ;p eq The pressure of the gas after pressure balance in the shale overburden pore permeation measurement device is bar; v (V) l Cm is the total volume of each part of pipeline 3 Known as 3.440553cm 3 ;V p To be measured of the volume of the overburden pore in the shale sample in cm 3
Wherein, the overburden pore volume V in the shale sample to be measured p The calculation formula of (2) is as follows:
(equation three)
Then, calculating the overburden porosity of the shale sample to be measuredThe calculation formula is as follows:
(equation IV)
Wherein,the porosity of the shale sample to be measured is in percent; vs is the apparent volume, cm, of the shale sample to be tested 3 The method comprises the steps of carrying out a first treatment on the surface of the L is the appearance length of the shale sample to be measured, cm; d is the apparent diameter of the shale sample to be measured, cm;
step 207, obtaining initial gas pressure p in shale overburden pore permeation testing device when gas begins to permeate into shale sample to be tested max Gas viscosity of helium at the temperature and pressure pointGas compression coefficient c of helium at said temperature and pressure point g Based on initial gas pressure p in shale overburden pore infiltration combined measurement device when gas starts to infiltrate into shale sample to be measured max The gas viscosity->The gas compression coefficient c g The appearance length L of the shale sample to be tested and the overburden porosity +.>Volume V of the reference chamber ref Total volume V of the pipelines of each part l The pore volume V of the coating p The pressure p of the gas after pressure balance in the shale overburden pressure hole seepage joint measuring device eq The gas pressure p in the shale overburden pore permeation combined measuring device in the diffusion process of the gas to the shale sample to be measured t And calculating the overburden permeability k of the shale sample to be measured.
Then, the overburden permeability of the shale sample to be measured at the temperature and pressure point is calculated, and the specific calculation process is as follows:
as shown in fig. 2, after a pulse pressure is applied to the test gas in the shale coverage hole infiltration combined measuring device, the test gas permeates into the core along the upper end and the lower end of the holder in the axial direction, in the process, the gas pressure in the shale coverage hole infiltration combined measuring device is gradually attenuated until the gas pressure tends to be balanced, in the process, the ratio of the accumulated gas quantity in the pores of the shale sample to be measured at any moment to all the gas quantities in the pore space of the shale sample to be measured in the final balanced state is calculated, and the calculation formula is as follows:
(equation five)
Wherein F is U The method is characterized in that the ratio of the accumulated gas quantity in the pores of the shale sample to be measured at the moment A to all the gas quantities in the pore space of the shale sample to be measured in the final balance state is dimensionless; m is M t Accumulating the amount of the gas entering the pores of the shale sample to be measured at the moment A, and mol; m is M The method comprises the steps of (1) determining the mol of all gas quantities in the pore space of a shale sample to be measured in a final equilibrium state; p is p max The method comprises the steps that when gas starts to permeate into a shale sample to be measured, the initial gas pressure in a shale overburden pressure hole permeation combined measuring device is measured by a first differential pressure sensor 3, wherein bar is measured; p is p t The method comprises the steps of 1, performing gas pressure and bar in a shale overburden pore infiltration combined measurement device in the process of diffusing gas into a shale sample to be measured;
further, calculating the proportion of the part which is not filled with gas in the pore space of the shale sample to be measured at the moment AThe calculation formula is as follows:
(equation six)
Fr is the proportion of the part which is not filled by gas in the pore space of the shale sample to be measured at the moment A.
Further, according to the ratio Fr of the part which is not filled by the gas in the pore space of the shale sample to be measured at the moment A, lnF is obtained r Relation with time t, and selecting from the relationTaking a section of curve with smaller curvature, fitting by using a trend line, and generating the slope S of the selected curve 1
Further, calculating the ratio of the sum of the total volume of each part of pipelines and the volume of the reference chamber 4 to the pore volume in the shale sample to be measuredThe calculation formula is as follows:
wherein,the ratio of the sum of the total volume of each part of pipelines and the volume of the reference chamber 4 to the pore volume in the shale sample to be measured is dimensionless; a is the sum of the total volume of each part of the pipeline and the volume of the reference chamber 4, cm 3
Further, a first order solution q of the transcendental equation is calculated 1 The calculation formula is as follows:
wherein q n And (3) solving the n-order of the transcendental equation, and obtaining no dimension.
Further, the gas viscosity of helium at the temperature and pressure point is obtainedCoefficient of gas compression c g Wherein, the gas viscosity->Coefficient of gas compression c g The gas data corresponding to the temperature and pressure point are all obtained by inquiring.
Further, the overburden permeability k of the shale sample to be measured at the temperature and pressure point is calculated, and the calculation formula is as follows:
(equation nine)
Wherein k is the overburden permeability of the shale sample to be tested, cm 2 I.e. 10 17 nD;Is the gas viscosity, pa.s; c g Is the gas compression coefficient, 1/Pa; s is S 1 Selecting the slope of the curve, 1/s; l is the appearance length of the shale sample to be measured, cm; />The method comprises the steps of (1) obtaining the overburden porosity of a shale sample to be measured; q 1 Is a first order solution to the transcendental equation.
And the overburden permeability of the shale sample to be measured at the temperature and pressure point can be obtained by using the method.
And step 208, unloading the confining pressure and the axial pressure, and discharging the residual gas in the shale overburden pore infiltration combined measuring device by opening one end of the third valve 14 connected with the external environment.
And then unloading the confining pressure and the shaft pressure, namely manually unloading the confining pressure and the shaft pressure by utilizing keys on the confining pressure pressurizing pump 12 and the shaft pressure pressurizing pump 9, paying attention to the pressure relief amplitude of each time not to exceed 2MPa, opening one end of the third valve 14 connected with the external environment after the confining pressure and the shaft pressure drop are 0, and exhausting the residual gas in the device.
And step 209, continuing iteration until the test of the shale sample to be tested at all temperature and pressure points is completed.
And finally, testing the next temperature and pressure point, namely repeating the steps 202-208, and testing the overburden porosity and the overburden permeability of the shale sample to be tested in other temperature and pressure environments. And after the experimental test of all the temperature and pressure points is finished, taking out a shale sample to be tested, closing the shale overburden pressure hole seepage joint testing device and finishing the test.
The procedure and test results for measuring shale overburden porosity and overburden permeability using the present invention are described below with a set of examples.
In this test example, the shale sample to be tested used was diameter dCore column with length of L= 2.746cm and 2.575cm, mass m of dried sample 0 31.824g, the test ambient temperature T is constant 27.5℃and the confining pressure p c =20mpa, axial pressure p a =20 MPa. The test gas is helium with a compression coefficient c g =2.20×10 -6 Pa -1 The gas viscosity was μ=1.95×10 -5 The initial gas pressure given to the reference chamber 4 during the test is p ref = 15.2065bar, opening the second valve 5 to allow the gas in the reference chamber 4 to flow into the sample clamping system to diffuse into the shale sample to be measured, and finally balancing the gas pressure p eq =4.2995bar。
Substituting the data into the formula III and the formula IV to calculate the overburden pore volume V of the shale sample to be measured p And the overburden porosity
And then, calculating the overburden permeability of the shale sample to be measured. Substituting the data into a formula seven to calculate:
substituting α into equation eight, the resulting override equation is as follows:
solving the above overrun equation to obtain a first-order solution q 1 =1.671327。
According to the process of diffusing the gas into the shale sample to be tested in the testing process, the ratio FU of the accumulated gas quantity in the pores of the shale sample to be tested at different moments to all the gas quantities in the pore space of the shale sample in the final state is obtained, and the result is shown in figure 3.
Will F U Substituting into the formula six to obtain the corresponding F r Values are further derived lnF r The time t is plotted as shown in fig. 4.
Selecting a curve with stable curvature in FIG. 4 to generate its slope to obtain S 1 =-0.008030999。
Long L and overburden porosity of shale sample to be measuredViscosity μ and gas compression coefficient cg, S of helium 1 Q 1 Substituting the formula III to obtain:
from the above results, the shale sample to be tested in this example had a porosity of 11.42% and a permeability of 2670nD at a confining pressure of 20MPa, an axial pressure of 18MPa, and a temperature of 27.5 ℃.
The foregoing has outlined and described the features, principles, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the foregoing embodiments, and that the foregoing embodiments and description are merely illustrative of the principles of this invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (1)

1. The shale overburden pore infiltration combined measurement method is characterized by being applied to a shale overburden pore infiltration combined measurement device, and the device comprises: helium source, reference chamber, differential pressure sensor, sample clamping system, temperature control system, confining pressure loading system, shaft pressure loading system, vacuumizing system and pipe valve system;
The reference chamber is respectively connected with the sample clamping system, the helium source and the vacuumizing system through the pipe valve system;
the vacuumizing system is respectively connected with the sample clamping system, the reference chamber and the external environment through the pipe valve system;
the confining pressure loading system and the axial pressure loading system are respectively connected with the sample clamping system, wherein the confining pressure loading system consists of confining pressure loading pumps; the axial pressure loading system consists of an axial pressure loading pump; the confining pressure loading pump is used for loading confining pressure to the sample clamping system, and the highest loadable confining pressure is 70MPa; the axial pressure loading pump is used for loading axial pressure to the sample holding system, and the maximum loadable axial pressure is 70MPa;
the differential pressure sensor is respectively arranged at the reference chamber, the axial pressure loading system and the confining pressure loading system;
the reference chamber, the differential pressure sensor, the sample clamping system and the pipe valve system are all arranged in the temperature control system, wherein the temperature control system is an incubator with a temperature adjusting function, the incubator is used for controlling the temperature of the shale overburden pressure hole seepage joint measuring device, the temperature adjusting range of the incubator is room temperature-300 ℃, and the temperature control precision is 0.5 ℃;
The pipe valve system comprises a first valve, a second valve, a third valve, a pipeline and a three-way joint on the pipeline; the first valve is arranged on a pipeline between the reference chamber and the helium source;
the three-way joint is connected with the reference chamber through the second valve, is connected with a second top shaft of the sample clamping system through the third valve and is connected with a first top shaft of the sample clamping system, wherein the third valve is a four-way valve, and a connecting pipeline forms a passage and is simultaneously connected with the external environment and the vacuumizing system;
the volume of the reference chamber is V ref =2cm 3 The pipeline volume between the reference chamber and the second valve is V l1 The saidThe pipeline volume between the second valve and the three-way joint is V l2 The volume of the pipeline between the three-way joint and the upstream of the sample clamping system is V l3 The pipeline volume between the three-way joint and the third valve is V l4 The volume of the pipeline between the third valve and the downstream of the sample clamping system is V l5 And the total volume of the pipelines of each part is V l =V l1 +V l2 +V l3 +V l4 +V l5 =3.440553cm 3
The differential pressure sensor arranged at the reference chamber is a first differential pressure sensor;
the method comprises the following steps:
Acquiring a shale sample to be tested in a preset mode, recording the apparent diameter d and the apparent length L of the shale sample to be tested, and placing the shale sample to be tested into a sample clamping system so as to test at each temperature and pressure point;
under any temperature and pressure point, a first valve, a second valve and a third valve are opened, a vacuumizing system is started to vacuumize the shale covering pressure hole seepage joint measuring device, air tightness inspection is carried out, and when the air tightness inspection is qualified, the first valve, the second valve and the third valve are closed;
setting the temperature of the temperature control system according to the temperature required by the test;
according to the test requirement, loading the axial pressure and the confining pressure of the sample clamping system by using a confining pressure loading system and an axial pressure loading system;
opening the first valve, introducing helium into the reference chamber, closing the first valve when the reading of the first differential pressure sensor is kept unchanged within a first preset time period, and recording the reading of the first differential pressure sensor to obtain the initial gas pressure p of the reference chamber after introducing helium into the reference chamber ref The method comprises the steps of carrying out a first treatment on the surface of the Opening the second valve and the third valve to enable the gas of the reference chamber to be introduced into the sample clamping system, and recording the reading of the first differential pressure sensor to obtain the gas pressure p in the shale overburden pore permeation combined measuring device in the process of diffusing the gas to the shale sample to be measured t The method comprises the steps of carrying out a first treatment on the surface of the When the reading of the first differential pressure sensor is kept unchanged within a second preset time period, recording the reading of the first differential pressure sensor to obtain the gas pressure p after the pressure in the shale overburden pore permeation combined measuring device is balanced eq
Based on the volume V of the reference chamber ref Total volume V of the pipelines of each part l Initial gas pressure p of the reference chamber after introducing helium into the reference chamber ref The pressure p of the gas after pressure balance in the shale overburden pressure hole seepage joint measuring device eq, Calculating the overburden pore volume V in the shale sample to be measured p The method comprises the steps of carrying out a first treatment on the surface of the Based on the overburden pore volume V p Calculating the overburden porosity of the shale sample to be measured, the apparent diameter d of the shale sample to be measured and the apparent length L of the shale sample to be measured
Acquiring initial gas pressure p in shale overburden pore infiltration combined measuring device when gas starts to infiltrate into shale sample to be measured max Gas viscosity of helium at the temperature and pressure pointGas compression coefficient c of helium at said temperature and pressure point g Based on initial gas pressure p in shale overburden pore infiltration combined measurement device when gas starts to infiltrate into shale sample to be measured max The gas viscosity->The gas compression coefficient c g The appearance length L of the shale sample to be tested and the overburden porosity +. >Volume V of the reference chamber ref Total volume V of the pipelines of each part l The pore volume V of the coating p The pressure p of the gas after pressure balance in the shale overburden pressure hole seepage joint measuring device eq The gas is directed to be treatedGas pressure p in shale overburden pore permeation combined measuring device in shale sample diffusion process t Calculating the overburden permeability k of the shale sample to be measured;
unloading the confining pressure and the axial pressure of the sample clamping system, and discharging residual gas in the shale overburden pore infiltration combined measuring device by opening one end of the third valve connected with the external environment;
continuing iteration until the test of the shale sample to be tested at all temperature and pressure points is completed;
the overburden permeability k of the shale sample to be measured is calculated specifically as follows:
when a pulse pressure is applied to test gas in the shale coating hole infiltration combined measuring device, the test gas can axially infiltrate into the core along the upper end and the lower end of the clamp holder, in the process, the gas pressure in the shale coating hole infiltration combined measuring device can be gradually attenuated until the gas pressure tends to balance, in the process, the ratio of the accumulated gas quantity in the pore space of the shale sample to be measured at any moment to all the gas quantities in the pore space of the shale sample to be measured in the final balance state is calculated, and the calculation formula is as follows:
Wherein F is U The method is characterized in that the ratio of the accumulated gas quantity in the pores of the shale sample to be measured at the moment A to all the gas quantities in the pore space of the shale sample to be measured in the final balance state is dimensionless; m is M t Accumulating the amount of the gas entering the pores of the shale sample to be measured at the moment A, and mol; m is M The method comprises the steps of (1) determining the mol of all gas quantities in the pore space of a shale sample to be measured in a final equilibrium state; p is p max When gas starts to permeate into a shale sample to be measured, the initial gas pressure in the shale overburden pressure hole permeation combined measuring device is bar, and the bar is measured by a first differential pressure sensor; p is p t The method comprises the steps of 1, performing gas pressure and bar in a shale overburden pore infiltration combined measurement device in the process of diffusing gas into a shale sample to be measured;
calculating the proportion of the part which is not filled by gas in the pore space of the shale sample to be measured at the moment AThe calculation formula is as follows:
wherein Fr is the proportion of the part which is not filled by gas in the pore space of the shale sample to be measured at the moment A;
according to the ratio Fr of the part which is not filled by gas in the pore space of the shale sample to be measured at the moment A, lnF is obtained r A curve with time t is selected from a section of curve with smaller curvature, and a trend line fitting is utilized to generate a slope S of the selected curve 1
Calculating the ratio of the sum of the total volume of each part of pipelines and the volume of the reference chamber to the pore volume in the shale sample to be measuredThe calculation formula is as follows:
wherein,the ratio of the sum of the total volume of each part of pipelines and the volume of the reference chamber to the pore volume in the shale sample to be measured is dimensionless; a is the sum of the total volume of each part of pipeline and the volume of the reference chamber, cm 3
Calculating a first order solution q to the transcendental equation 1 The calculation formula is as follows:
wherein q n An n-order solution of the transcendental equation is dimensionless;
acquiring the gas viscosity of helium at the temperature and pressure pointCoefficient of gas compression c g Wherein, the gas viscosity->Coefficient of gas compression c g All the gas data corresponding to the temperature and pressure point are inquired;
the overburden permeability k of the shale sample to be measured at the temperature and pressure point is calculated according to the following calculation formula:
wherein k is the overburden permeability of the shale sample to be tested, cm 2 I.e. 10 17 nD;Is the gas viscosity, pa.s; c g Is the gas compression coefficient, 1/Pa; s is S 1 Selecting the slope of the curve, 1/s; l is the appearance length of the shale sample to be measured, cm; />The method comprises the steps of (1) obtaining the overburden porosity of a shale sample to be measured; q 1 Is a first order solution to the transcendental equation.
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