CN117147414B - Device and method for determining occurrence of water in shale organic and inorganic pores - Google Patents
Device and method for determining occurrence of water in shale organic and inorganic pores Download PDFInfo
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- CN117147414B CN117147414B CN202311432952.6A CN202311432952A CN117147414B CN 117147414 B CN117147414 B CN 117147414B CN 202311432952 A CN202311432952 A CN 202311432952A CN 117147414 B CN117147414 B CN 117147414B
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- 239000011148 porous material Substances 0.000 title claims abstract description 63
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 204
- 238000003860 storage Methods 0.000 claims abstract description 9
- 238000002474 experimental method Methods 0.000 claims description 18
- 238000010521 absorption reaction Methods 0.000 claims description 13
- 230000006835 compression Effects 0.000 claims description 11
- 238000007906 compression Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 8
- 238000012360 testing method Methods 0.000 claims description 7
- 229920006395 saturated elastomer Polymers 0.000 claims description 5
- 229910010272 inorganic material Inorganic materials 0.000 claims description 3
- 239000011147 inorganic material Substances 0.000 claims description 3
- 150000002894 organic compounds Chemical class 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 239000008398 formation water Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 8
- 230000008859 change Effects 0.000 abstract description 5
- 238000011161 development Methods 0.000 abstract description 4
- 239000003345 natural gas Substances 0.000 abstract description 3
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 18
- 239000000243 solution Substances 0.000 description 13
- 235000011164 potassium chloride Nutrition 0.000 description 9
- 239000001103 potassium chloride Substances 0.000 description 9
- 239000007789 gas Substances 0.000 description 4
- 238000012937 correction Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000036962 time dependent Effects 0.000 description 2
- 238000012824 chemical production Methods 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000013100 final test Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000002737 fuel gas Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000005213 imbibition Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000005514 two-phase flow Effects 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/088—Investigating volume, surface area, size or distribution of pores; Porosimetry
Abstract
The invention discloses a device and a method for determining occurrence of water in shale organic and inorganic pores, which relate to the field of natural gas exploration and development and comprise the following steps: the liquid outlet end of the dropper is communicated with the first liquid outlet pipeline, the first liquid outlet pipeline is communicated with the liquid inlet pipeline, the liquid inlet end of the booster pump is communicated with the liquid storage tank, experimental liquid is filled in the liquid storage tank and the dropper, the liquid outlet end of the booster pump is communicated with the second liquid outlet pipeline, the second liquid outlet pipeline is communicated with the liquid inlet pipeline, and the vacuum pump is communicated with the vacuumizing pipeline; the volume of the inorganic pore occurrence water of shale can be accurately measured through the scale change of the experimental liquid in the dropper, the volume of the inorganic pore occurrence water in the organic pore is further obtained, the experimental liquid is pressurized through the booster pump, the experimental liquid gradually enters the organic pore along with the pressure increase, the volume of the experimental liquid entering the organic pore is further calculated, the volume of the inorganic pore occurrence water in the organic pore is determined, and the result is accurate and reliable.
Description
Technical Field
The invention relates to the field of natural gas exploration and development, in particular to a device and a method for determining occurrence of water in shale organic and inorganic pores.
Background
Shale gas is a natural gas resource which is reserved in the pores of a shale layer and can be mined, takes adsorption and free states as main existence modes, takes methane as main components, is a clean and efficient energy resource and chemical raw material, is mainly used for resident fuel gas, urban heat supply, power generation, automobile fuel, chemical production and the like, and has wide application range. The shale gas production process generally does not need drainage, the production period is long, generally 30-50 years, the exploration and development success rate is high, and the shale gas production process has higher industrial economic value. According to the prediction, the main basin and the regional resource amount of China are about 36 trillion cubic meters, the economic value is huge, and the resource prospect is wide.
However, shale pores are complex in type, diverse in pore structure, and huge in wettability difference between organic pores and inorganic pores, and the wettability difference is expressed as: normally, water can wet the surfaces of inorganic pores, but cannot wet the surfaces of organic pores, and the difference controls the occurrence state and flow mechanism of formation water in the shale gas reservoir in the organic pores and the inorganic pores. Therefore, the method accurately represents the occurrence volume of water in the shale inorganic pores and the shale organic pores, and has important theoretical research and practical significance for revealing the gas-water two-phase flow mechanism in shale and predicting the actual effect after exploration and development. In view of this, it would be a matter of urgent need in the art to provide an apparatus or method that can characterize the volume of water within shale inorganic and organic voids.
Disclosure of Invention
The invention aims to provide a device for determining occurrence of water in shale organic and inorganic pores, so as to solve the problems in the prior art and realize accurate measurement of shale inorganic pores and organic pores.
In order to achieve the above object, the present invention provides the following solutions: the invention provides a device for determining occurrence of water in organic and inorganic pores of shale, which comprises the following components:
the sample chamber is used for placing shale core samples, the sample chamber is communicated with a liquid inlet pipeline, and a first valve is arranged on the liquid inlet pipeline;
the dropper is provided with scale marks and is vertically arranged, a liquid outlet end of the dropper is communicated with a first liquid outlet pipeline, the first liquid outlet pipeline is communicated with the liquid inlet pipeline, and a second valve is arranged on the first liquid outlet pipeline;
the liquid inlet end of the booster pump is communicated with the liquid storage tank, experimental liquid is filled in the liquid storage tank and the dropper, the liquid outlet end of the booster pump is communicated with the second liquid outlet pipeline, the second liquid outlet pipeline is communicated with the liquid inlet pipeline, a third valve and a pressure sensor are arranged on the second liquid outlet pipeline, the operating end of the booster pump is provided with a dial, and the dial can record the output volume of the experimental liquid;
the vacuum pump is communicated with the vacuumizing pipeline, the vacuumizing pipeline is communicated with the liquid inlet pipeline and/or the first liquid outlet pipeline and/or the second liquid outlet pipeline, a fourth valve is arranged on the vacuumizing pipeline, and the vacuum pump can vacuumize the sample chamber, the liquid inlet pipeline, the first liquid outlet pipeline and the second liquid outlet pipeline.
Further, when the first valve and the fourth valve are opened and the second valve and the third valve are closed, the vacuum pump can pump the sample chamber, the liquid inlet pipeline, the first liquid outlet pipeline and the second liquid outlet pipeline to a vacuum state.
Further, the experimental liquid is deionized water or simulated shale water solution.
The invention also provides a method for determining occurrence of water in organic and inorganic pores of shale, which comprises the following steps:
s1: drying the shale core sample;
s2: placing a shale core sample into a sample chamber, and vacuumizing the sample chamber, a liquid inlet pipeline, a first liquid outlet pipeline and a second liquid outlet pipeline to a vacuum state by using a vacuum pump;
s3: closing a fourth valve on the vacuumizing pipeline, opening a first valve on the liquid inlet pipeline and a second valve on the first liquid outlet pipeline, filling the sample chamber with experimental liquid in a dropper from the dropper along the first liquid outlet pipeline and the liquid inlet pipeline, recording residual liquid scales in the dropper through scale marks on the dropper, recording the residual liquid scales in the dropper after the shale core sample absorbs the experimental liquid to be saturated, and calculating the volume of the experimental liquid absorbed by inorganic pores of the shale core sample;
s4: closing the second valve, opening the third valve, rotating the operating end of the booster pump until the pressure of the second liquid outlet pipeline is constant, recording the experiment time and recording the rotation angle when the pressure is constant through the dial;
s5: the output pressure of the booster pump is increased, the operation end of the booster pump is rotated again until the pressure of the second liquid outlet pipeline is constant, the experiment time is recorded, and the rotation angle when the pressure is constant is recorded through the dial;
s6: and (5) repeating the step (S5) and calculating the organic pore absorption experiment liquid volume of the shale core sample under different output pressure conditions.
Further, in the step S1, the shale core sample is weighed every a period of time in the drying process of the shale core sample, and when the continuous three weighing results are the same, the shale core sample is dried.
Further, the vacuum degree of the vacuum pump evacuation in the step S2 is 0.101MPa, and this state is maintained for at least 3 hours.
Further, in step S3, when the sample chamber is filled with the experimental liquid, the scale of the residual liquid in the dropper is V Front part When the shale core sample absorbs experimental liquid to be saturated, the scale of the residual liquid in the dropper is V Rear part (S) Inorganic pore absorption experiment liquid volume V of shale core sample Inorganic material =V Front part -V Rear part (S) 。
Further, in steps S4 to S6, the volume of the experimental liquid output by the booster pump is an apparent volume, the apparent volume is calculated by the rotation angle of the dial, the volume of the experimental liquid after output is compressed, and the real volume of the experimental liquid output by the booster pump is:
in the method, in the process of the invention,is P i The j-th rotation booster pump under pressure outputs the apparent volume of the experimental liquid, V i C is the volume of experimental liquid in the shale core sample wi The compression coefficient of the experimental liquid; p (P) i Is the ith constant pressure; when the compression coefficient of the experimental liquid is calculated, the output pressure is adopted to calculate the compression coefficient of the experimental liquid from P 0 Pressurizing to P 1 、P 1 Pressurizing to P 2 、P 2 Pressurizing to P 3 ……P n-1 Pressurizing to P n Wherein P is 0 =0; sequentially calculating P 1 、P 2 、P 3 … … and P n The real volume V of the experimental liquid output by the booster pump under the output pressure 1 、V 2 、V 3 … … and V n Organic pore absorption experiment liquid volume V of shale core sample Organic compound =V 1 +V 2 +V 3 ……+V n ，
The invention discloses the following technical effects:
according to the method, the volume of the inorganic pore of shale can be accurately measured through the scale change of the experimental liquid in the dropper, the volume of the inorganic pore is further obtained, the experimental liquid is pressurized through the booster pump when the volume of the water in the organic pore is measured, the experimental liquid gradually enters the organic pore along with the pressure increase, the volume of the experimental liquid entering the organic pore is calculated, and the occurrence volume of the water in the organic pore is accurately and reliably determined.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of the structure of the device of the present invention;
FIG. 2 is a graph showing the results of the test liquid compressibility factor measurement;
FIG. 3 is a graph of imbibition volume versus time for shale core samples;
FIG. 4 is a schematic volume of a total occurrence test liquid for shale core samples;
FIG. 5 is a schematic illustration of the volumes of experimental liquids in the inorganic and organic pores at different output pressures;
wherein, 1, a dropper; 2. a vacuum pump; 3. a sample chamber; 4. a liquid storage tank; 5. a booster pump; 6. a dial; 7. a first valve; 8. a second valve; 9. a third valve; 10. and a fourth valve.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In order that the above-recited objects, features and advantages of the present invention will become more readily apparent, a more particular description of the invention will be rendered by reference to the appended drawings and appended detailed description.
Examples
Referring to fig. 1, an embodiment of the present invention provides an apparatus for determining the occurrence of water in organic and inorganic pores of shale, comprising: the sample chamber 3 is used for placing shale core samples, the sample chamber 3 is communicated with a liquid inlet pipeline, and a first valve 7 is arranged on the liquid inlet pipeline; the dropper 1 has the capacity of 10ml and the precision of 0.05ml, the dropper 1 is provided with scale marks and is vertically arranged, a liquid outlet end of the dropper 1 is communicated with a first liquid outlet pipeline, the first liquid outlet pipeline is communicated with a liquid inlet pipeline, and a second valve 8 is arranged on the first liquid outlet pipeline; the liquid inlet end of the booster pump 5 is communicated with the liquid storage tank 4, experimental liquid is filled in the liquid storage tank 4 and the dropper 1, the liquid outlet end of the booster pump 5 is communicated with a second liquid outlet pipeline, the second liquid outlet pipeline is communicated with the liquid inlet pipeline, a third valve 9 and a pressure sensor are arranged on the second liquid outlet pipeline, the operating end of the booster pump 5 is provided with a dial 6, and the dial 6 can record the output experimental liquid volume; the vacuum pump 2, the vacuum pump 2 is communicated with a vacuumizing pipeline, as shown in fig. 1, the liquid inlet pipeline, the first liquid outlet pipeline, the second liquid outlet pipeline and the vacuumizing pipeline are intersected at one place, so that the vacuumizing pipeline is communicated with the liquid inlet pipeline and the first liquid outlet pipeline and the second liquid outlet pipeline, and a fourth valve 10 is arranged on the vacuumizing pipeline, and the vacuum pump 2 can vacuumize the sample chamber 3, the liquid inlet pipeline, the first liquid outlet pipeline and the second liquid outlet pipeline. In this embodiment, when the first valve 7 and the fourth valve 10 are opened and the second valve 8 and the third valve 9 are closed, the vacuum pump 2 can pump the sample chamber 3, the liquid inlet pipe, the first liquid outlet pipe and the second liquid outlet pipe to a vacuum state. The experimental liquid is potassium chloride solution.
The device for determining occurrence of water in shale organic and inorganic pores disclosed in the following application examples is used for experiments, and specifically comprises the following steps:
s1: drying shale core samples, taking a plurality of shale core samples, putting the shale core samples into a drying box, arranging a gravity sensor in the drying box, drying the shale core samples until the weight of the shale core samples is not changed any more, and measuring that the weight of the shale core samples is 56.12g;
s2: placing a shale core sample into a sample chamber 3, and pumping the sample chamber 3, a liquid inlet pipeline, a first liquid outlet pipeline and a second liquid outlet pipeline to a vacuum state by using a vacuum pump 2, wherein the pipeline pressure is-0.101 MPa;
s3: closing a fourth valve 10 on the vacuumizing pipeline, opening a first valve 7 on the liquid inlet pipeline and a second valve 8 on the first liquid outlet pipeline, filling the sample chamber 3 with experimental liquid in the dropper 1 from the dropper 1 along the first liquid outlet pipeline and the liquid inlet pipeline (actually, the second liquid outlet pipeline on the left side of the third valve 9 and the vacuumizing pipeline on the right side of the fourth valve 10 are also filled with the experimental liquid due to the negative pressure of each pipeline), recording the residual liquid scale in the dropper 1 through the scale mark on the dropper 1, recording the residual liquid scale in the dropper 1 after the shale core sample absorbs the experimental liquid to be saturated, and calculating the inorganic pore absorption experimental liquid volume of the shale core sample; when the sample chamber 3 is full of experimental liquid, the scale of the residual liquid in the dropper 1 is V Front part Recording the scale of the residual liquid every 30s within 30 minutes, recording the reading of the scale tube every hour after 30 minutes, and along with the experiment, the reading time interval of the scale tube becomes longer until the reading is not changed any more, and stopping the absorption of the experimental liquid by the shale core sample, wherein the scale of the residual liquid in the dropper 1 is V Rear part (S) Inorganic pore absorption test liquid volume V of shale core sample Inorganic material =V Front part -V Rear part (S) 。
S4: closing the second valve 8, opening the third valve 9, rotating the operating end of the booster pump 5 until the pressure of the second liquid outlet pipeline is constant, wherein the output pressure of the booster pump 5 is 2MPa, recording the experiment time and recording the rotation angle when the pressure is constant through the dial 6;
s5: raising the output pressure of the booster pump 5 to 6MPa, rotating the operation end of the booster pump 5 again until the pressure of the second liquid outlet pipeline is constant, recording the experiment time and recording the rotation angle when the pressure is constant through the dial 6;
s6: and repeating the step S5 twice, so that the output pressure of the booster pump 5 is sequentially increased to 10MPa and 14MPa, and calculating the volume of the organic pore absorption experiment liquid of the shale core sample under different output pressure conditions.
In steps S4 to S6, the volume of the experimental liquid output by the booster pump 5 is an apparent volume, the apparent volume is calculated by the rotation angle of the dial 6, the volume of the experimental liquid after output is compressed, and the real volume of the experimental liquid output by the booster pump 5 is:
in the method, in the process of the invention,is P i The j-th rotation booster pump under pressure outputs the apparent volume of the experimental liquid, V i C is the volume of experimental liquid in the shale core sample wi The compression coefficient of the experimental liquid; p (P) i Is the ith constant pressure; when the compression coefficient of the experimental liquid is calculated, the output pressure is adopted to calculate the compression coefficient of the experimental liquid from P 0 Pressurizing to P 1 、P 1 Pressurizing to P 2 、P 2 Pressurizing to P 3 ……P n-1 Pressurizing to P n Wherein P is 0 =0; sequentially calculating P 1 、P 2 、P 3 … … and P n Real volume V of experimental liquid output by booster pump 5 under output pressure 1 、V 2 、V 3 … … and V n Organic pore absorption test liquid volume V of shale core sample Organic compound =V 1 +V 2 +V 3 ……+V n 。
As shown in FIG. 3, the experimental data recorded in the above steps S4-S6 are used to obtain the time-dependent change of the rotation angle, which is converted into the time-dependent change of the volume of the existing potassium chloride solution as shown in FIG. 4, and the volume of the 1-degree injected potassium chloride solution and the compression coefficients thereof at the output pressures of 2MPa, 6MPa, 10MPa and 14MPa (as shown in FIG. 2) of the dial 6 are measured, which shows that 5.92 mu L of the potassium chloride solution is injected every 1-degree injection, and the compression coefficients thereof at 2MPa, 6MPa, 10MPa and 14MPa are respectively 1.22GPa -1 、0.652GPa -1 、0.519GPa -1 And 0.498GPa -1 . The residual amount of the potassium chloride solution in the organic pores at different output pressures shown in FIG. 4 can be obtained, the apparent volume in the parameters is corrected to be the real volume, the real volume of the potassium chloride solution entering the shale core sample is obtained through calculation by a formula after correction, the residual amount schematic diagram shown in FIG. 5 is obtained (the curve difference before correction and after correction is very small and basically coincides in FIG. 5), and the residual amount of the potassium chloride solution in the inorganic pores is 0.790cm 3 The occurrence of potassium chloride solution in the organic pores at output pressures of 2MPa, 6MPa, 10MPa and 14MPa was 0.148cm, respectively 3 、0.189cm 3 、0.203cm 3 And 0.232cm 3 . As is clear from FIG. 4, when the output pressure of the booster pump 5 reached 14MPa, the occurrence of the increase in the amount of potassium chloride solution in the organic pores was 0.148cm, since the increase in the amount of water absorbed by the organic pores was considered to be saturated 3 +0.189cm 3 +0.203cm 3 +0.232cm 3 =0.772cm 3 。
When the second valve 8 is closed and the third valve 9 is opened, the second liquid outlet pipe on the left side of the third valve 9 and the vacuuming pipe on the right side of the fourth valve 10 are already filled with the test liquid due to the negative pressure of each pipe in step S3, so that the volume of the test liquid output by the booster pump 5 can be regarded as the liquid suction volume of the organic pore, and the error is small, so that the final test result is not affected and can be ignored.
The invention discloses a device and a method for determining occurrence of water in shale organic and inorganic pores, which can accurately measure the absorption experiment liquid volume of the shale inorganic pores through the scale change of experiment liquid in a dropper 1 so as to obtain the volume of the inorganic pores, and the measurement of the water volume in the organic pores is to pressurize the experiment liquid through a booster pump 5 so that the experiment liquid gradually enters the organic pores along with the pressure increase, and then the occurrence volume of the water in the organic pores is determined through calculation of the experiment liquid volume entering the organic pores, so that the result is accurate and reliable.
In the description of the present invention, it should be understood that the terms "longitudinal," "transverse," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like indicate or are based on the orientation or positional relationship shown in the drawings, merely to facilitate description of the present invention, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be construed as limiting the present invention.
The above embodiments are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope defined by the claims of the present invention without departing from the design spirit of the present invention.
Claims (8)
1. An apparatus for determining the occurrence of water in shale organic and inorganic voids, comprising:
the sample chamber (3), the sample chamber (3) is used for placing shale core samples, the sample chamber (3) is communicated with a liquid inlet pipeline, and a first valve (7) is arranged on the liquid inlet pipeline;
the dropper (1) is provided with scale marks and is vertically arranged, a liquid outlet end of the dropper (1) is communicated with a first liquid outlet pipeline, the first liquid outlet pipeline is communicated with the liquid inlet pipeline, and a second valve (8) is arranged on the first liquid outlet pipeline;
the liquid inlet end of the booster pump (5) is communicated with the liquid storage tank (4), experimental liquid is filled in the liquid storage tank (4) and the dropper (1), the liquid outlet end of the booster pump (5) is communicated with a second liquid outlet pipeline, the second liquid outlet pipeline is communicated with the liquid inlet pipeline, a third valve (9) and a pressure sensor are arranged on the second liquid outlet pipeline, the operation end of the booster pump (5) is provided with a dial (6), and the dial (6) can record the volume of the output experimental liquid;
the vacuum pump (2), vacuum pump (2) and evacuation pipeline intercommunication, the evacuation pipeline with feed liquor pipeline and/or first drain pipeline and/or second drain pipeline intercommunication just be provided with fourth valve (10) on the evacuation pipeline, vacuum pump (2) can with sample room (3) feed liquor pipeline first drain pipeline with the second drain pipeline evacuation reaches the vacuum state.
2. The device for determining occurrence of water in organic and inorganic pores of shale according to claim 1, wherein the vacuum pump (2) can pump the sample chamber (3), the liquid inlet pipeline, the first liquid outlet pipeline and the second liquid outlet pipeline to a vacuum state when the first valve (7) and the fourth valve (10) are opened and the second valve (8) and the third valve (9) are closed.
3. The apparatus for determining the occurrence of water in organic and inorganic voids of shale according to claim 1, wherein said experimental liquid is deionized water or a simulated formation water solution.
4. A method for determining the occurrence of water in shale organic and inorganic voids, characterized in that the device for determining the occurrence of water in shale organic and inorganic voids according to any of claims 1-3 is used, comprising the following steps:
s1: drying the shale core sample;
s2: placing shale core samples into a sample chamber (3), and vacuumizing the sample chamber (3), a liquid inlet pipeline, a first liquid outlet pipeline and a second liquid outlet pipeline by using a vacuum pump (2);
s3: closing a fourth valve (10) on the vacuumizing pipeline, opening a first valve (7) on the liquid inlet pipeline and a second valve (8) on the first liquid outlet pipeline, filling the sample chamber (3) with experimental liquid in the drip tube (1) from the drip tube (1) along the first liquid outlet pipeline and the liquid inlet pipeline, recording residual liquid scales in the drip tube (1) through scale marks on the drip tube (1), recording residual liquid scales in the drip tube (1) after the experimental liquid absorbed by the shale core sample reaches saturation, and calculating the inorganic pore absorption experimental liquid volume of the shale core sample;
s4: closing the second valve (8), opening the third valve (9), rotating the operating end of the booster pump (5) until the pressure of the second liquid outlet pipeline is constant, recording the experiment time and recording the rotation angle when the pressure is constant through the dial (6);
s5: the output pressure of the booster pump (5) is increased, the operation end of the booster pump (5) is rotated again until the pressure of the second liquid outlet pipeline is constant, the experiment time is recorded, and the rotation angle when the pressure is constant is recorded through the dial (6);
s6: and (5) repeating the step (S5) and calculating the volume of the organic pore absorption experimental liquid of the shale core sample under different output pressure conditions.
5. The method according to claim 4, wherein in the step S1, the shale core sample is weighed at intervals during the drying process, and the shale core sample is dried when the results of three consecutive weighing are the same.
6. The method for determining occurrence of organic and inorganic voids in shale according to claim 4, wherein said vacuum degree of said vacuum pump (2) vacuumized in said step S2 is 0.101MPa, and maintained in this state for at least 3 hours.
7. The method for determining occurrence of organic and inorganic pores in shale according to claim 4, wherein in step S3, when the sample chamber (3) is filled with experimental liquid, the scale of the residual liquid in the dropper (1) is V Front part When the shale core sample absorbs experimental liquid to be saturated, the scale of the residual liquid in the dropper (1) is V Rear part (S) Inorganic pore absorption experiment liquid volume V of shale core sample Inorganic material =V Front part -V Rear part (S) 。
8. A method of determining the occurrence of water in shale organic and inorganic voids as recited in claim 4,
the method is characterized in that in the steps S4-S6, the volume of the experimental liquid output by the booster pump (5) is an apparent volume, the apparent volume is calculated through the rotation angle of the dial (6), the volume of the experimental liquid after output is compressed, and the real volume of the experimental liquid output by the booster pump (5) is as follows:
in which, is V j Is P i The j-th rotation under pressure of the booster pump (5) outputs the apparent volume of the experimental liquid, V i C is the volume of experimental liquid in the shale core sample wi The compression coefficient of the experimental liquid; p (P) i Is the ith constant pressure; when the compression coefficient of the experimental liquid is calculated, the output pressure is adopted to calculate the compression coefficient of the experimental liquid from P 0 Pressurizing to P 1 、P 1 Pressurizing to P 2 、P 2 Pressurizing to P 3 ……P n-1 Pressurizing to P n Wherein P is 0 =0; sequentially calculating P 1 、P 2 、P 3 … … and P n The real volume V of the experimental liquid output by the booster pump (5) under the output pressure 1 、V 2 、V 3 … … and V n Organic pores of the shale core sampleGap absorption test liquid volume V Organic compound =V 1 +V 2 +V 3 ……+V n 。
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| CA2750405A1 (en) * | 2009-02-23 | 2010-08-26 | Exxonmobil Upstream Research Company | Water treatment following shale oil production by in situ heating |
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| CN113340928B (en) * | 2021-05-28 | 2022-04-22 | 中国石油大学(华东) | Experimental device and method for developing shale oil through supercritical CO2/H2O mixed fluid throughput |
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