CN117309720A - Method for representing pore throat lower limit of fluid in shale oil-gas layer by neutron scattering - Google Patents
Method for representing pore throat lower limit of fluid in shale oil-gas layer by neutron scattering Download PDFInfo
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- CN117309720A CN117309720A CN202311282614.9A CN202311282614A CN117309720A CN 117309720 A CN117309720 A CN 117309720A CN 202311282614 A CN202311282614 A CN 202311282614A CN 117309720 A CN117309720 A CN 117309720A
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- 239000011148 porous material Substances 0.000 title claims abstract description 142
- 238000001956 neutron scattering Methods 0.000 title claims abstract description 83
- 239000012530 fluid Substances 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000002474 experimental method Methods 0.000 claims abstract description 31
- 239000013598 vector Substances 0.000 claims abstract description 24
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 14
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 14
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 14
- 239000003079 shale oil Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims description 12
- 239000011159 matrix material Substances 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052753 mercury Inorganic materials 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 16
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 15
- 239000007789 gas Substances 0.000 description 10
- 150000003613 toluenes Chemical class 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 4
- 238000001998 small-angle neutron scattering Methods 0.000 description 4
- 238000012512 characterization method Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
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- Chemical & Material Sciences (AREA)
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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Abstract
A method for characterizing a pore throat lower limit of a fluid in a shale hydrocarbon reservoir by utilizing neutron scattering, comprising the following steps: preparing a shale sample, and performing neutron scattering experiments on the shale sample to obtain scattering vectors of the shale sample and scattering intensities of corresponding full-scale pores; using a solution to saturate the shale sample, and performing a full-contrast matching neutron scattering experiment to obtain a full-contrast matching neutron scattering vector of the shale sample and scattering intensity of a corresponding fluid which cannot enter a pore; obtaining pore diameter and corresponding pore volume distribution data, and drawing a pore diameter distribution curve of a vacuum environment; obtaining pore diameter and corresponding pore volume distribution data, and drawing a pore diameter distribution curve of a full-contrast matching neutron scattering experiment; the lower limit of the pore throat of the fluid in the shale oil and gas layer can be obtained. The method can not damage the pore structure of the sample, can accurately characterize the pores which can not be accessed by mercury, and finally determines the true pore throat lower limit of shale.
Description
Technical Field
The invention belongs to the field of unconventional natural gas characterization, and particularly relates to a method for characterizing the pore throat lower limit of fluid in a shale oil-gas layer by utilizing neutron scattering.
Background
The shale oil gas reserves in China are huge, but the problem of difficult development still exists, and because the pore throats of a compact oil reservoir are tiny and the structure is complex, the transportation and the accumulation of oil gas in the reservoir are affected by the pore throats, so that the accurate judgment of the lower limit of the pore throats is particularly important. The pore throat lower limit refers to the minimum pore throat radius at which reservoir shale oil is effectively passed in and out. The traditional method generally uses invasive characterization methods such as mercury intrusion method to measure the lower limit of pore throat, but the method can damage the original pore structure of the sample to a certain extent, thereby affecting the judgment of the pore structure and the lower limit of pore throat of the sample.
Disclosure of Invention
The invention aims to nondestructively characterize the pore-throat lower limit of fluid in a shale oil-gas layer, and based on the pore-throat lower limit, a method for characterizing the pore-throat lower limit of the fluid in the shale oil-gas layer by utilizing neutron scattering is provided.
The technical scheme of the invention is as follows:
a method for characterizing a pore throat lower limit of a fluid in a shale hydrocarbon reservoir by utilizing neutron scattering, comprising the following steps:
s1, preparing a shale sample, and drying the shale sample;
s2, carrying out neutron scattering experiments on the shale sample to obtain scattering vectors of the shale sample and scattering intensities of corresponding full-scale pores;
s3, after the neutron scattering experiment is finished, using a solution to saturate the shale sample, and performing a full-contrast matching neutron scattering experiment to obtain a full-contrast matching neutron scattering vector of the shale sample and the scattering intensity of a corresponding fluid non-accessible pore;
s4, obtaining pore diameter and corresponding pore volume distribution data based on the scattering vector in the S2 and the scattering intensity of the corresponding full-scale pore, and drawing a pore diameter distribution curve of a vacuum environment;
s5, drawing a pore diameter distribution curve of the full-contrast matching neutron scattering experiment based on the scattering vector of the full-contrast matching neutron scattering experiment in S3 and the scattering intensity of the corresponding fluid inaccessible pore to obtain pore diameter and corresponding pore volume distribution data.
S6, obtaining the pore throat lower limit of the fluid in the shale oil and gas layer based on all the pore diameter distribution curves of neutron scattering and the full-contrast matched neutron scattering pore diameter distribution curve.
Further, the method for preparing shale samples is as follows:
and weighing shale with certain mass, grinding the shale into slices with the thickness of 0.5mm and the thickness of 1.0cm < 2 >, and obtaining the shale sample.
Further, the drying treatment method comprises the following steps:
and placing the shale sample into a drying box, and drying for 48 hours at 60-100 ℃.
Further, the S2 specifically is:
s21, vacuumizing the sample cabin to enable the vacuum degree in the sample cabin to be 0.05-0.1 Pa;
s22, operating a neutron scattering instrument in the vacuum environment to obtain neutron scattering data.
S23, processing the neutron scattering data by using IGOR software to obtain scattering vectors of the sample vacuum environment and scattering intensity of the corresponding full-scale pores.
Further, the step S3 specifically includes:
s31, soaking the shale sample in a solution for 24 hours;
s32, operating a neutron scattering instrument after the accessible hole of the shale sample is filled with the solution to obtain the full-contrast matched neutron scattering data;
s33, processing the full-contrast matched neutron scattering data by using IGOR software to obtain a full-contrast matched neutron scattering vector of the shale sample and the scattering intensity of the corresponding fluid inaccessible pore.
Further, the scattering length density of the solution is equal to the scattering length density of the shale sample matrix.
Further, in S4, the scattering vector of the sample vacuum environment and the scattering intensity of the corresponding full-scale pore are processed by using a PDSP model in the IGOR software, so as to obtain pore diameter and corresponding pore volume distribution data.
Further, in S5, the method uses a PDSP model in the IGOR software to process the scattering vector of the sample full-contrast matching neutron scattering experiment and the scattering intensity of the corresponding fluid inaccessible pore, so as to obtain the pore diameter and the corresponding pore volume distribution data.
Further, the step S6 specifically includes:
and the aperture corresponding to the intersection point of all aperture distribution curves of neutron scattering and the full-contrast matched neutron scattering aperture distribution curve is the pore throat lower limit of the fluid in the shale oil-gas layer, and the difference value of the two curves corresponds to the distribution condition of the accessible aperture.
Further, the full-scale pores include accessible pores and inaccessible pores.
The invention has the technical effects that:
according to the pore throat lower limit characterization method of the fluid in the shale oil and gas layer, through a neutron scattering experiment in a vacuum environment and a full contrast matching neutron scattering experiment, the neutron scattering experiment in the vacuum environment can obtain information of all pores (the fluid can enter the pores and the fluid cannot enter the pores) of the shale sample; the solution is used as a substitute of petroleum hydrocarbon, the sample is saturated for a sufficient time, the solution is ensured to fill all accessible pores of the sample, occurrence of shale oil in a reservoir is simulated, the scattering length density of the solution is equal to that of a sample matrix, and the fluid non-accessible pore information of the shale sample is ensured to be obtained through a full-contrast matching neutron scattering experiment; by drawing pore size distribution curves of shale samples under two experiments, the intersection point of the two curves represents that all pores corresponding to the pore sizes in the shale are fluid non-accessible pore information, namely the pore throat lower limit of the fluid. Meanwhile, the neutron scattering experiment is to collect the collision condition of neutrons between shale matrixes and pores, so that the pore structure and pore size distribution of shale can be represented nondestructively.
Drawings
The accompanying drawings illustrate various embodiments by way of example in general and not by way of limitation, and together with the description and claims serve to explain the inventive embodiments. Wherever possible, the same reference numbers will be used throughout the drawings to refer to the same or like parts. Such embodiments are illustrative and not intended to be exhaustive or exclusive of the present apparatus or method.
FIG. 1 shows a schematic of an experimental flow scheme of the present invention;
FIG. 2 shows a scattering vector-scattering intensity diagram of vacuum ambient neutron scattering and full contrast matched neutron scattering using a toluene and deuterated toluene mixed solution saturated shale sample in an embodiment of the invention;
fig. 3 shows a pore size distribution schematic of a shale sample of an embodiment of the invention.
Detailed Description
It should be noted that, in the case of no conflict, the embodiments and features in the embodiments may be combined with each other. The present application will be described in detail below with reference to the accompanying drawings in conjunction with embodiments.
The invention uses the small angle neutron scattering technique to nondestructively characterize the pore throat lower limit of the reservoir. The small-angle neutron scattering technology utilizes neutron rays to penetrate shale, and due to the difference between the sample matrix and the density of the scattering length of the pores, the pore structure information of the shale can be obtained by measuring the scattering radiation intensity in a specific scattering angle range. And preparing a hydrocarbon solution with the scattering length density equal to that of the matrix, and using the solution to saturate the sample, and filling the accessible pores of the shale sample with the solution, so that accessible pore structure information of the sample can be obtained through a full-contrast matching experiment, and meanwhile, occurrence of shale oil in a reservoir is simulated. Therefore, the method can not damage the pore structure of the sample, can accurately characterize the pores which can not be accessed by mercury, and finally determines the true pore throat lower limit of shale.
As shown in fig. 1-3, an embodiment of the present invention provides a method for characterizing a pore throat lower limit of a fluid in a shale hydrocarbon reservoir by using neutron scattering, including the following steps:
s1, preparing a shale sample, and drying the shale sample;
specifically, the method for preparing shale samples is as follows:
weighing shale with certain mass, and grinding the shale into 1.0-1.0 cm 2 A sheet of 0.5mm thickness, the shale sample was obtained.
The drying treatment method comprises the following steps:
in this embodiment, the temperature of the drying oven is set to 70 ℃ for drying for 48 hours.
S2, carrying out neutron scattering experiments on the shale sample in a vacuum environment, and obtaining scattering vectors of the sample in the vacuum environment and scattering intensity (accessible pores and inaccessible pores) of corresponding full-scale pores;
in step S2, the neutron scattering experimental method includes the following steps:
s21, vacuumizing the sample cabin to enable the vacuum degree in the sample cabin to be 0.06Pa;
s22, operating a neutron scattering instrument in the vacuum environment to obtain neutron scattering data.
S23, processing the neutron scattering data by using IGOR software to obtain scattering vectors of the sample vacuum environment and scattering intensity (accessible pore and inaccessible pore) of the corresponding full-scale pore.
S3, after the neutron scattering experiment in the vacuum environment is finished, using a solution to saturate the shale sample, and performing a full-contrast matching neutron scattering experiment to obtain a full-contrast matching neutron scattering vector of the sample and the scattering intensity of a corresponding fluid inaccessible pore;
in step S3, the contrast matching neutron scattering experimental method includes the following steps:
s31, soaking the shale sample in a mixed solution of toluene and deuterated toluene for 24 hours;
s32, operating a neutron scattering instrument after the accessible hole of the shale sample is filled with the solution to obtain the full-contrast matched neutron scattering data;
s33, processing the neutron scattering data by using IGOR software to obtain a full-contrast matched neutron scattering vector of the sample and the scattering intensity of the corresponding fluid inaccessible pore.
The solution has a scattering length density equal to the scattering length density of the shale sample matrix.
In this example, the shale sample matrix has a scattering length density of 3.39X10 10 cm -2 The solution is a mixed solution of toluene and deuterated toluene, and the scattering length density of toluene is 0.94 multiplied by 10 10 cm -2 The scattering length density of deuterated toluene is 5.64×10 10 cm -2 The method comprises the steps of carrying out a first treatment on the surface of the The mixed solution was prepared in a proportion of 30% toluene and 55% deuterated toluene.
S4, using a PDSP model in IGOR software to process the scattering vector of the vacuum environment and the scattering intensity (accessible pore and inaccessible pore) of the corresponding full-scale pore, obtaining pore diameter and corresponding pore volume distribution data, and drawing a pore diameter distribution curve of the vacuum environment;
s5, using a PDSP model in IGOR software to process a scattering vector of the full-contrast matching neutron scattering experiment and scattering intensity of a corresponding fluid inaccessible pore, obtaining pore diameter and corresponding pore volume distribution data, and drawing a pore diameter distribution curve of the full-contrast matching neutron scattering experiment.
S6, pore diameters corresponding to the intersection points of all the neutron scattering pore diameter distribution curves (accessible pore and inaccessible pore) and the full-contrast matched neutron scattering pore diameter distribution curve (inaccessible pore) are pore throat lower limits of fluid in the shale oil-gas layer, and the difference value of the two lines corresponds to the distribution condition of accessible pore.
In step S6, the curve corresponding to the small-angle neutron scattering experiment represents the pore size distribution curve of the full-scale pore (the pore which can be accessed by fluid and the pore which can not be accessed by fluid) of the sample; the curve corresponding to the contrast matching small-angle neutron scattering experiment represents the pore diameter distribution curve of the pores which can not be accessed by fluid; the aperture corresponding to the intersection point of the neutron scattering aperture distribution curve and the full-contrast matched neutron scattering aperture distribution curve is 3nm, and refer to figure 2. The above is not relevant and is applicable to the prior art.
In this context, the experimental materials are referred to only for the sake of clarity and convenience in expressing the technical solutions. It should be understood that the use of the experimental materials should not limit the scope of the protection claimed herein.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical solution of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (10)
1. A method for characterizing the pore throat lower limit of a fluid in a shale hydrocarbon reservoir by utilizing neutron scattering, which is characterized by comprising the following steps:
s1, preparing a shale sample, and drying the shale sample;
s2, carrying out neutron scattering experiments on the shale sample to obtain scattering vectors of the shale sample and scattering intensities of corresponding full-scale pores;
s3, after the neutron scattering experiment is finished, using a solution to saturate the shale sample, and performing a full-contrast matching neutron scattering experiment to obtain a full-contrast matching neutron scattering vector of the shale sample and the scattering intensity of a corresponding fluid non-accessible pore;
s4, obtaining pore diameter and corresponding pore volume distribution data based on the scattering vector in the S2 and the scattering intensity of the corresponding full-scale pore, and drawing a pore diameter distribution curve of a vacuum environment;
s5, drawing a pore diameter distribution curve of the full-contrast matching neutron scattering experiment based on the scattering vector of the full-contrast matching neutron scattering experiment in S3 and the scattering intensity of the corresponding non-accessible pores of the fluid to obtain pore diameter and corresponding pore volume distribution data;
s6, obtaining the pore throat lower limit of the fluid in the shale oil and gas layer based on all the pore diameter distribution curves of neutron scattering and the full-contrast matched neutron scattering pore diameter distribution curve.
2. The method for characterizing pore throat boundaries of fluids in shale hydrocarbon reservoirs using neutron scattering according to claim 1, wherein the method for preparing shale samples is as follows:
weighing shale with certain mass, and grinding the shale into 1.0-1.0 cm 2 And (3) obtaining the shale sample by using a sheet with the thickness of 0.5 mm.
3. The method for characterizing pore throat boundaries of fluids in shale hydrocarbon reservoirs using neutron scattering according to claim 1, wherein said method for drying treatment comprises the steps of:
and placing the shale sample into a drying box, and drying for 48 hours at 60-100 ℃.
4. The method for characterizing pore throat boundaries of fluids in shale hydrocarbon reservoirs using neutron scattering according to claim 1, wherein S2 is specifically:
s21, vacuumizing the sample cabin to enable the vacuum degree in the sample cabin to be 0.05-0.1 Pa;
s22, operating a neutron scattering instrument in the vacuum environment to obtain neutron scattering data.
S23, processing the neutron scattering data by using IGOR software to obtain scattering vectors of the sample vacuum environment and scattering intensity of the corresponding full-scale pores.
5. The method for characterizing pore throat boundaries of fluids in shale hydrocarbon reservoirs using neutron scattering according to claim 1, wherein S3 is specifically:
s31, soaking the shale sample in a solution for 24 hours;
s32, operating a neutron scattering instrument after the accessible hole of the shale sample is filled with the solution to obtain the full-contrast matched neutron scattering data;
s33, processing the full-contrast matched neutron scattering data by using IGOR software to obtain a full-contrast matched neutron scattering vector of the shale sample and the scattering intensity of the corresponding fluid inaccessible pore.
6. The method of characterizing the pore throat restriction of a fluid in a shale hydrocarbon reservoir using neutron scattering according to claim 5, wherein the solution has a scattering length density equal to the scattering length density of the shale sample matrix.
7. The method for characterizing pore throat boundaries of fluids in shale hydrocarbon reservoirs by neutron scattering according to claim 1, wherein in S4, a PDSP model in the IGOR software is used to process scattering vectors of the sample vacuum environment and scattering intensities of corresponding full-scale pores to obtain pore diameter and corresponding pore volume distribution data.
8. The method for characterizing pore throat boundaries of fluids in shale hydrocarbon reservoirs by neutron scattering according to claim 1, wherein in S5, the scattering vectors of the sample full contrast matched neutron scattering experiment and the scattering intensities of the corresponding fluid inaccessible pores are processed by a PDSP model in the IGOR software to obtain pore diameter and corresponding pore volume distribution data.
9. The method for characterizing a pore throat lower limit of a fluid in a shale hydrocarbon reservoir by utilizing neutron scattering according to claim 1, wherein the step S6 is specifically:
and the aperture corresponding to the intersection point of all aperture distribution curves of neutron scattering and the full-contrast matched neutron scattering aperture distribution curve is the pore throat lower limit of the fluid in the shale oil-gas layer, and the difference value of the two curves corresponds to the distribution condition of the accessible aperture.
10. The method of characterizing pore throat boundaries of fluids in shale hydrocarbon reservoirs using neutron scattering of claim 1, wherein the full-scale pores comprise accessible pores and inaccessible pores.
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| CN113176186A (en) * | 2021-03-22 | 2021-07-27 | 中国地质大学（武汉） | Method for judging carbonate rock crude oil injection pressure and pore throat lower limit |
| CN113552149A (en) * | 2021-06-22 | 2021-10-26 | 中国石油化工股份有限公司江汉油田分公司勘探开发研究院 | Method for quantitatively representing shale wettability by using small-angle neutron scattering |
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| CN115728202A (en) * | 2022-11-04 | 2023-03-03 | 西南石油大学 | Method for determining radius lower limit of shale movable throat |
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- 2023-10-07 CN CN202311282614.9A patent/CN117309720A/en active Pending
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| CN114894692A (en) * | 2022-04-26 | 2022-08-12 | 重庆大学 | Method for determining full-scale pore diameter of compact reservoir |
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