CN114778581A - Coal micro-nano intercommunicating pore fracture tracking method - Google Patents
Coal micro-nano intercommunicating pore fracture tracking method Download PDFInfo
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- CN114778581A CN114778581A CN202210449554.4A CN202210449554A CN114778581A CN 114778581 A CN114778581 A CN 114778581A CN 202210449554 A CN202210449554 A CN 202210449554A CN 114778581 A CN114778581 A CN 114778581A
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- 239000003245 coal Substances 0.000 title claims abstract description 75
- 239000011148 porous material Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 25
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical group [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 72
- 239000001103 potassium chloride Substances 0.000 claims abstract description 35
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 35
- 239000011435 rock Substances 0.000 claims abstract description 4
- 239000003795 chemical substances by application Substances 0.000 claims abstract 2
- 238000001035 drying Methods 0.000 claims description 20
- 238000004891 communication Methods 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 5
- 239000012466 permeate Substances 0.000 claims 2
- 239000000700 radioactive tracer Substances 0.000 abstract description 14
- 238000011161 development Methods 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 abstract description 3
- 238000001291 vacuum drying Methods 0.000 abstract description 3
- 238000005213 imbibition Methods 0.000 abstract description 2
- 229920006395 saturated elastomer Polymers 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 244000137852 Petrea volubilis Species 0.000 description 8
- 229910052500 inorganic mineral Inorganic materials 0.000 description 7
- 235000010755 mineral Nutrition 0.000 description 7
- 239000011707 mineral Substances 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 239000012530 fluid Substances 0.000 description 6
- 238000009826 distribution Methods 0.000 description 5
- 239000002105 nanoparticle Substances 0.000 description 5
- 238000005520 cutting process Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 238000005065 mining Methods 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 239000012463 white pigment Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 238000000095 laser ablation inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 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
- 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
- G01N23/22—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 measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/30—Staining; Impregnating ; Fixation; Dehydration; Multistep processes for preparing samples of tissue, cell or nucleic acid material and the like for analysis
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
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Abstract
The invention discloses a coal micro-nano intercommunicating pore fracture tracking method; the adopted tracer is potassium chloride, 3mol/L potassium chloride solution is saturated into a coal rock sample in a vacuum imbibition mode, then the sample is dried in a vacuum drying oven until the weight of the sample is not reduced, the coal sample is polished by abrasive paper with different meshes under the anhydrous condition, the polished sample is subjected to a scanning electron microscope test, and the potassium chloride filled in communicated pore cracks in a scanning electron microscope picture is bright and easy to identify. The tracer agent is simple in preparation method, micron-scale and nano-scale intercommunicating pore cracks can be observed through a scanning electron microscope, and the types and the development conditions of intercommunicating pore cracks in coal can be directly observed.
Description
Technical Field
The invention belongs to the technical field of coal bed gas development, and particularly relates to a coal micro-nano intercommunicating pore fracture tracing method.
Background
Coal bed gas mining difficulty in China is high, and low-yield and low-efficiency areas of coal bed gas wells generally exist, so that the coal bed gas mining method becomes one of main bottlenecks restricting development of coal bed gas industry in China. The development rule of the communicated pore gaps of different microscopic components is deeply known, and the yield of the coal reservoir is increased. However, determination and characterization of pore-fracture connectivity is a scientific problem to be solved in the fields of coal bed gas geology and engineering. At present, a theoretical method for researching reservoir pore fracture connectivity mainly comprises the steps of obtaining a three-dimensional pore fracture structure through CT and FIB-SEM, qualitatively analyzing pore fracture connectivity by utilizing a water absorption curve slope, disclosing the reservoir communication pore fracture distribution condition by adopting LA-ICP-MS and combining a tracer, and reflecting the pore fracture connectivity according to MIP and NMR curve difference. However, the above method can only qualitatively analyze reservoir connectivity on one hand, and is limited by the difficulty in comprehensively characterizing reservoir connectivity due to sample size and resolution on the other hand. Therefore, the current method is difficult to be applied to coal reservoirs with strong heterogeneity.
The invention discloses 202010840547.8 shale pore structure fluid flow channel tracer, a preparation method and a tracing method, wherein the tracer comprises gold nanoparticles or ferroferric oxide nanoparticles and composite nanoparticles containing any one of the components; the tracing method comprises the steps of introducing a nano tracer with a proper concentration into a shale fluid spontaneous imbibition experiment or utilizing an external magnetic field to absorb a fluid containing a magnetic nano tracer into a shale micro-nano pore structure, drying the fluid and then carrying out electron microscope scanning on a shale sample, and revealing a flow channel of the fluid in the shale micro-nano pore structure by utilizing position information of the nano tracer. The tracer and the tracing method disclosed by the invention solve the problem that the existing tracer and tracing method cannot intuitively acquire the migration information of the fluid in the shale micro-nano pores, and have higher resolution compared with the traditional CT and micro optical microscopic imaging. However, the used tracer is gold nanoparticles or ferroferric oxide nanoparticles, is difficult to prepare, and simultaneously enters the cracks of coal uniformly and thoroughly.
Disclosure of Invention
The invention mainly aims to solve the technical problem and provide a cheap tracer and a tracing method, which are convenient for permeation operation.
The method comprises the following specific steps:
preparing a potassium chloride solution;
preparing a coal sample with the diameter of 2.5 cm and the height of 2 cm;
placing the prepared coal sample in a potassium chloride solution, and saturating the coal sample with the potassium chloride solution in a negative pressure environment;
drying a coal sample of a saturated potassium chloride solution;
and polishing one end of the dried coal rock.
Wherein, preparing the potassium chloride solution comprises:
pouring deionized water into a beaker, and placing the beaker in a drying box;
wherein the temperature of the drying oven is set to be 20 ℃, and the drying oven is heated for 1-2 hours to ensure that the temperature of the deionized water reaches 20 ℃;
adding potassium chloride into deionized water to prepare a potassium chloride solution;
wherein the concentration of the potassium chloride solution is 3 mol/L.
Wherein, preparing the coal sample comprises:
selecting a large unoxidized coal sample, and marking a target area by using white pigment;
cutting off the coal sample in the target area by using a linear cutting instrument, wherein the specification of the coal sample is a cylinder with the diameter of 2.5 cm;
and (3) polishing two ends of the cylindrical coal sample by using an angle grinder to prepare the coal sample with the diameter of 2.5 cm and the height of 2 cm.
Wherein, the saturated potassium chloride solution of coal sample includes:
placing the coal sample in a beaker filled with a potassium chloride solution;
placing the beaker into a vacuum drying oven, and setting the temperature to be 20 ℃;
and opening the vacuum pump to vacuumize for 1-2 days until no bubbles are generated in the beaker.
Wherein, the coal sample feeding drying comprises:
taking out the coal sample from the beaker, and putting the coal sample into a drying box;
the temperature of the drying oven is set to be 105 ℃, and the drying is continued for more than 48 hours;
and taking out the coal sample every 6 hours, weighing until the weight of the coal sample is not reduced, and finishing drying.
Wherein, give the sample of coal and polish and include:
respectively adopting 1000 meshes of sand paper, 2000 meshes of sand paper, 3000 meshes of sand paper and 5000 meshes of sand paper to polish one end of the coal sample;
the sanding process must avoid contact with water to avoid re-dissolution of the potassium chloride into the water.
And (3) carrying out a scanning electron microscope test on the sample, wherein the potassium chloride mineral observed in the scanning electron microscope picture is filled in the original coal sample because the potassium chloride mineral does not exist. In addition, the main component of the coal is organic matter, and the mineral is mainly clay mineral with the atomic number smaller than that of potassium chloride. Therefore, the color of the potassium chloride mineral is brighter and easier to identify in the scanning electron micrograph.
And (3) performing element analysis by adopting X-ray energy spectrum scanning to determine that the mineral filled into the interconnected pore cracks in the coal is potassium chloride.
Due to the adoption of the technical scheme, the invention has the following advantages:
1. the tracer potassium chloride is commonly and easily obtained, the solution is neutral and harmless after being dissolved in water, and the preparation process is simple and easy to operate.
2. The potassium chloride has high solubility at 20 ℃, so that the content of solute in the potassium chloride solution is high, the fluidity of the aqueous solution is good, and the potassium chloride can be ensured to be completely filled in communicated micro-nano pore cracks after the coal sample is dried.
3. The coal has hydrophilic characteristic, and potassium chloride solution is saturated into the coal sample in a vacuumizing mode. The method can not damage the sample, and the coal sample is broken to generate small cracks.
4. The potassium chloride is used as a tracer, has higher brightness in a scanning electron microscope picture, and is obviously compared with coal organic matters and minerals so as to be convenient to distinguish.
Drawings
FIG. 1 is a diagram of filling potassium chloride in a fracture;
FIG. 2 is a diagram of the spectrum analysis of potassium chloride in a fracture;
FIG. 3 is a plot of the distribution of chlorine in the fracture;
FIG. 4 is a plot of the distribution of potassium in the crevices.
Detailed Description
The technical scheme of the invention is further explained by combining the attached drawings.
A coal micro-nano intercommunicating pore crack tracing method comprises pouring deionized water into a beaker, and placing in a drying oven; the temperature of the drying box is set to be 20 ℃, and the drying box is heated for 1-2 hours to ensure that the temperature of the deionized water reaches 20 ℃; potassium chloride solution having a concentration of 3mol/L was prepared by adding potassium chloride to deionized water.
Selecting a large unoxidized coal sample, and marking a target area by using white pigment; cutting off the coal sample in the target area by using a linear cutting instrument, wherein the specification of the coal sample is a cylinder with the diameter of 2.5 cm; and (3) polishing two ends of the cylindrical coal sample by adopting an angle grinder to prepare the coal sample with the diameter of 2.5 cm and the height of 2 cm.
Placing the coal sample in a beaker filled with potassium chloride solution; placing the beaker into a vacuum drying oven, and setting the temperature to be 20 ℃; and opening the vacuum pump to vacuumize for 1-2 days until no bubbles are generated in the beaker.
Taking out the coal sample from the beaker, and putting the coal sample into a drying box; the temperature of the drying oven is set to be 105 ℃, and the drying is continued for more than 48 hours; taking out the coal sample every 6 hours, weighing until the weight of the coal sample is not reduced, and finishing drying; respectively adopting 1000 meshes of sand paper, 2000 meshes of sand paper, 3000 meshes of sand paper and 5000 meshes of sand paper to polish one end of the coal sample; the polished surface of the sample is subjected to a scanning electron microscope test, so that the fracture of the intercommunicating pores in the coal can be observed and analyzed, as shown in figure 1. FIG. 3 is a graph showing a distribution of chlorine in fractures; FIG. 4 is a distribution diagram of potassium element; can verify that the cracks are full of potassium chloride and can be analyzed easily.
Elemental analysis was performed using X-ray energy spectrum scanning, and as shown in fig. 2, it was determined that the mineral filling the interconnected pore fractures in the coal was potassium chloride.
The above-described embodiments are preferred aspects of the present invention, and the scope of the present invention is defined by the claims.
Claims (8)
1. A coal micro-nano intercommunicating pore fracture tracing method is characterized by comprising the steps of preparing a coal sample, using a potassium chloride solution as a tracing agent, enabling the potassium chloride solution to permeate into the coal sample, drying to be constant in weight, polishing one end of dried coal rock under a waterless condition, examining the coal sample by using a scanning electron microscope, and distinguishing the color of potassium chloride from the coal sample in a scanning electron microscope photo so as to observe the condition of intercommunicating pore fractures in coal.
2. The coal micro-nano communication hole crack tracing method according to claim 1, wherein the concentration of the potassium chloride solution is 3 mol/L.
3. The coal micro-nano communication hole crack tracing method according to claim 1, wherein the drying is performed at a temperature of 105 ℃.
4. The coal micro-nano communication hole fracture tracking method according to claim 1, wherein the constant weight means that the sample is weighed once every 6 hours in a drying process until the weight of the sample is not reduced.
5. The coal micro-nano intercommunicating pore fracture tracking method according to claim 1, wherein the coal sample is in a cylindrical shape with a diameter of 2.5 cm and a height of 2 cm, and both ends are polished before permeation.
6. The coal micro-nano intercommunicating pore fracture tracing method according to claim 1, wherein the polishing of one end of the dried coal rock is performed by using 1000 mesh, 2000 mesh, 3000 mesh and 5000 mesh sandpaper respectively.
7. The coal micro-nano intercommunicating pore fracture tracing method according to claim 1, wherein said potassium chloride solution is allowed to permeate into the coal sample at a temperature of 20 ℃ for a certain time in a vacuum environment.
8. The coal micro-nano communication hole crack tracing method according to claim 7, wherein the time is 1-2 days until no bubbles are generated in the beaker.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101718800A (en) * | 2009-11-09 | 2010-06-02 | 水利部交通运输部国家能源局南京水利科学研究院 | Haplopore dilution method for determining seepage direction by electrical conductivity |
| CN106323840A (en) * | 2016-09-13 | 2017-01-11 | 西南石油大学 | Shale porosity measurement method |
| CN106525688A (en) * | 2016-11-21 | 2017-03-22 | 中国石油大学(华东) | Experimental method for saturated shale pore fluid separation and saturation degree calculation |
| CN107923236A (en) * | 2015-08-27 | 2018-04-17 | 通用电气(Ge)贝克休斯有限责任公司 | For assessing and improving the method and material of geographical specific page rock reservoir production |
| US20190218907A1 (en) * | 2018-01-18 | 2019-07-18 | Saudi Arabian Oil Company | Tracers for petroleum reservoirs |
| CN112304998A (en) * | 2020-08-20 | 2021-02-02 | 成都理工大学 | Shale pore structure fluid flow channel tracer, preparation method and tracing method |
| CN114184444A (en) * | 2021-11-27 | 2022-03-15 | 中国石油大学(华东) | Visualization system and method for initiating migration of coal powder in fracture induced by gas-water two-phase flow |
-
2022
- 2022-04-27 CN CN202210449554.4A patent/CN114778581A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101718800A (en) * | 2009-11-09 | 2010-06-02 | 水利部交通运输部国家能源局南京水利科学研究院 | Haplopore dilution method for determining seepage direction by electrical conductivity |
| CN107923236A (en) * | 2015-08-27 | 2018-04-17 | 通用电气(Ge)贝克休斯有限责任公司 | For assessing and improving the method and material of geographical specific page rock reservoir production |
| CN106323840A (en) * | 2016-09-13 | 2017-01-11 | 西南石油大学 | Shale porosity measurement method |
| CN106525688A (en) * | 2016-11-21 | 2017-03-22 | 中国石油大学(华东) | Experimental method for saturated shale pore fluid separation and saturation degree calculation |
| US20190218907A1 (en) * | 2018-01-18 | 2019-07-18 | Saudi Arabian Oil Company | Tracers for petroleum reservoirs |
| CN112304998A (en) * | 2020-08-20 | 2021-02-02 | 成都理工大学 | Shale pore structure fluid flow channel tracer, preparation method and tracing method |
| CN114184444A (en) * | 2021-11-27 | 2022-03-15 | 中国石油大学(华东) | Visualization system and method for initiating migration of coal powder in fracture induced by gas-water two-phase flow |
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| 胡钦红等: "东营凹陷沙河街组页岩油储集层润湿性、孔隙连通性和流体―示踪剂运移", 石油学报, vol. 39, no. 03, pages 278 - 289 * |
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