CN116337707A - Shale core porosity measurement method - Google Patents
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- 238000000691 measurement method Methods 0.000 title description 11
- 238000003763 carbonization Methods 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 34
- 238000005406 washing Methods 0.000 claims abstract description 33
- 239000001307 helium Substances 0.000 claims abstract description 29
- 229910052734 helium Inorganic materials 0.000 claims abstract description 29
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000005259 measurement Methods 0.000 claims abstract description 26
- 238000000197 pyrolysis Methods 0.000 claims abstract description 16
- 239000007789 gas Substances 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 238000012360 testing method Methods 0.000 claims abstract description 9
- 238000005481 NMR spectroscopy Methods 0.000 claims description 14
- 239000011435 rock Substances 0.000 claims description 10
- 238000012545 processing Methods 0.000 claims description 3
- 239000003208 petroleum Substances 0.000 abstract description 2
- 230000000452 restraining effect Effects 0.000 abstract description 2
- 238000012795 verification Methods 0.000 abstract description 2
- 239000003921 oil Substances 0.000 description 67
- 239000011148 porous material Substances 0.000 description 10
- 239000003079 shale oil Substances 0.000 description 9
- 238000004364 calculation method Methods 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000000084 colloidal system Substances 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 235000011850 desserts Nutrition 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 238000012937 correction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000000655 nuclear magnetic resonance spectrum Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000010426 asphalt Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011707 mineral Substances 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
- 238000001225 nuclear magnetic resonance method Methods 0.000 description 1
- 230000005311 nuclear magnetism Effects 0.000 description 1
- 239000004058 oil shale Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- 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
- G01N24/00—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
- G01N24/08—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
- G01N24/081—Making measurements of geologic samples, e.g. measurements of moisture, pH, porosity, permeability, tortuosity or viscosity
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- Y02A90/30—Assessment of water resources
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Abstract
The invention discloses a method for measuring shale core porosity, and belongs to the field of petroleum. The shale core plunger sample is directly heated by a temperature-control carbonization method, so that the residual oil gas is removed completely, the core plunger sample is not changed, the porosity is directly measured by helium porosity measuring equipment, and a verification method for measuring the porosity accuracy is also provided. In order to accurately measure the porosity of the shale core, the method of the invention is characterized in that the dry distillation process which can completely remove residual oil and preserve the original appearance of a core sample is finally determined on the basis of repeatedly testing and restraining the increasing speed of the dry distillation temperature, the heating time and the highest temperature, and then the porosity of the shale core is directly obtained by using helium porosity measurement equipment. The porosity measured by the method is compared with the total effective porosity obtained by adding the helium porosity measured after oil washing and the residual oil porosity measured after oil washing, and the difference between the two is less than 0.5%, so that the accuracy is sufficiently verified.
Description
Technical Field
The invention belongs to the field of petroleum, and relates to a shale core porosity measurement method.
Background
Accurate measurement of shale oil reservoir porosity is an important parameter for evaluating the oiliness of desserts and is also a worldwide problem. The difficulty in measurement is that the shale oil reservoir mainly develops nanoscale and microscale pores, and the residual oil gas of the nanoscale and microscale pores cannot be completely cleaned in the conventional oil washing link in the helium measurement method, so that the measurement result is smaller than the real pore value. In addition, the shale oil has very low porosity, so that the measured small value occupies a larger proportion in the total pores and cannot be ignored. How to accurately measure the porosity of shale oil reservoirs is a key element for restricting the physical property evaluation and resource amount calculation of desserts, and researchers in the shale oil field have made a great deal of effort to face the difficult problem.
Current patents on shale oil porosity measurements can be divided into four categories. One type is to calculate porosity indirectly by establishing a functional relationship with other components, such as: chen Fangwen in 2014 et al (CN 103822866 a) estimated porosity using scanning electron microscope data; in 2015, wang Xingjian and the like (CN 104977771U), the porosity is indirectly measured by utilizing the adsorption quantity of shale samples; yang Zhenheng in 2019 (CN 112231882 a) determined porosity values indirectly from material composition by establishing a functional relationship between porosity and mineral composition; he Chencheng in 2019 et al (CN 111122408A) calculated the porosity of pore size between 0.3-10nm by establishing a relationship between pore volume and TOC content. The calculation method has high accuracy requirement on establishing functions, the accuracy is difficult to judge, and the porosity is difficult to accurately characterize. The second type is to find the porosity by nuclear magnetic resonance technology, such as 2014, xu Hao (CN 104075974 a), and determine the porosity by different echo times and waiting times of nuclear magnetic resonance; 2016, zhang Pengfei et al (CN 105866002A) characterized oil shale reservoir physical properties by nuclear magnetic resonance T2 spectral distribution; 2018, wang Min, et al (CN 108458960A) found porosity values by establishing different component nuclear magnetic resonance T1-T2 spectra and comparing the difference of the T2 spectra. The calculation method has long test period, different areas of different basins have different nuclear magnetic characteristics, and the calculation method has no universality. The third category is to calculate the porosity by the difference method, such as 2019 Tao Guoliang et al (CN 111855521 a) using the mass difference; the porosity (total rock volume-skeletal volume-particle volume-dust volume) was calculated using the volume difference in 2020, qu et al (CN 111650108 a). The method has more measurement data and large system error. The fourth class discharges the residual oil by means of distillation, extraction, pyrolysis and the like, and then obtains the porosity by the residual oil mass, and the residual oil gas is discharged by a distillation extraction method as selected in Tian Hua and the like (CN 102252948A) in 2011; the porosity is obtained by extracting the rock sample of 2016 (CN 106323840A) and the like with a solution after vacuumizing; the residual oil gas in the crushed stone is pyrolyzed out by Xie Xiaomin in 2020 (CN 111487176A), and the porosity of the residual oil gas is calculated by weighing the residual oil gas. The distillation and extraction time is long, and the total discharge of the residual oil is difficult to achieve. Under the condition of no temperature constraint, pyrolysis is easy to cause rock sample damage, weight, density and other parameter measurement, and the unavoidable errors exist, so that the porosity is difficult to be accurate.
In view of the foregoing, there is a need to develop a technique for accurately and simply measuring shale core porosity.
Disclosure of Invention
The invention aims to overcome the defects of large error and inconvenient measurement in the shale core porosity measurement method in the prior art, and provides a shale core porosity measurement method.
In order to achieve the above purpose, the invention is realized by adopting the following technical scheme:
a shale core porosity measurement method comprises the following steps:
step 1) processing shale rock core into a plunger sample, and washing oil from the plunger sample;
step 2) measuring the porosity of the plunger sample after oil washing to obtain the porosity of the plunger sample after oil washing and the porosity of residual oil;
step 3) performing carbonization heating on the plunger sample after oil washing, and measuring the porosity of the plunger sample after carbonization heating to obtain the porosity after carbonization;
and 4) adding the porosity of the plunger-like wash oil and the porosity of the residual oil to obtain a sum of the porosities, comparing the sum of the porosities with the porosity after carbonization, and calculating an absolute error, wherein when the absolute error is less than or equal to 0.5%, the porosity after carbonization is the total porosity of the shale core.
Preferably, in step 3), the conditions of destructive distillation heating are: the temperature is 350-400 ℃ and the time is 40-50 h.
Preferably, in the step 3), the dry distillation heating process is as follows:
the core plunger sample is heated to 100 ℃, 100-200 ℃ at the temperature of 10 ℃ per hour, and 10 ℃ per 2 hours after 200 ℃ until reaching 350-400 ℃.
Preferably, in step 4), the absolute error is calculated by:
wherein, phi 1 is the porosity after plunger-like wash oil, phi 2 is the residual oil porosity after plunger-like wash oil, and phi 3 is the porosity after carbonization.
Preferably, in step 2), the test gas is helium during the porosity measurement.
Preferably, in step 2), the test pressure is 200psi when measured for porosity.
Preferably, in step 2) and step 3), the porosity measurement is performed by means of a nuclear magnetic resonance measuring device.
Preferably, step 1) is performed on the plunger sample for a wash oil period of 30 days.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a method for measuring the porosity of a shale core, which directly heats a shale core plunger sample by a temperature-control carbonization method, ensures that the core plunger sample is not changed while all residual oil gas is removed, directly measures the porosity by helium porosity measuring equipment, and further provides a verification method for measuring the accuracy of the porosity. In order to accurately measure the porosity of the shale core, the method of the invention is characterized in that the dry distillation process which can completely remove residual oil and preserve the original appearance of a core sample is finally determined on the basis of repeatedly testing and restraining the increasing speed of the dry distillation temperature, the heating time and the highest temperature, and then the porosity of the shale core is directly obtained by using helium porosity measurement equipment. The porosity measured by the method is compared with the total effective porosity obtained by adding the helium porosity measured after oil washing and the residual oil porosity measured after oil washing, and the difference between the two is less than 0.5%, so that the accuracy is sufficiently verified. Meanwhile, the operation steps are convenient, the direct measurement is not needed to be calculated, the system error is small, the time is short, the direct measurement can be completed within two days, the precision is high, the influence of artificial calculation factors and multi-step external factors is reduced, the system error is reduced, and the experimental flow is convenient.
Drawings
FIG. 1 is a flow chart of a method of measuring shale core porosity in accordance with the present invention;
FIG. 2 is a plot of residual oil porosity versus nuclear magnetic T2 relaxation time for example 3;
FIG. 3 is a plot of residual oil porosity versus nuclear magnetic T2 relaxation time for example 14.
Detailed Description
The invention is described in further detail below with reference to the attached drawing figures:
example 1
The accurate measurement method of the shale core porosity is adopted to analyze 17 samples of the shale oil cores of the set of the concave wind city of the marc lake of the songaric basin, and is carried out according to the following steps, the flow is shown in figure 1,
step S1, processing a shale core into a plunger sample, and washing oil of the shale core plunger sample by using oil washing equipment to reach helium porosity measurement standard;
step S2, measuring the porosity of the washed shale core plunger sample by using helium porosity measuring equipment to obtain the porosity phi 1 of the washed shale core plunger sample;
step S3, measuring the residual oil porosity phi 2 of the shale core plunger sample after oil washing by using nuclear magnetic resonance measuring equipment;
step S4, performing carbonization heating on the shale core plunger sample by using a temperature control carbonization method, wherein the core plunger sample is slowly heated to 100 ℃ at first, the temperature is raised to 10 ℃ every hour, the temperature is raised to 10 ℃ every 2 hours after 200 ℃ until the required highest temperature is reached to 350 ℃, and carbonization is performed for about 40 hours;
s5, measuring the porosity of the shale core plunger sample subjected to temperature control carbonization by using helium porosity measurement equipment, and obtaining the porosity phi 3 of the shale core plunger sample subjected to temperature control carbonization;
s6, after the measurement of a batch of shale core plunger samples is completed, adding the helium porosity phi 1 after oil washing of each sample and the residual oil porosity phi 2 measured by nuclear magnetism, and comparing with the helium porosity phi 3 measured after temperature control carbonization, wherein the absolute error is less than or equal to 0.5%, which indicates that the accuracy of the porosity measured by the temperature control carbonization method is higher;
and S7, taking the helium porosity value phi 3 measured after temperature control carbonization as the porosity of the shale core plunger sample.
Example 2
The accurate measurement method for the shale core porosity is used for analyzing 17 samples of shale oil cores of the set of the air city of the concave air city of the marc lake of the songaric basin, and comprises the following steps (refer to figure 1): the shale core is processed into a plunger sample, so that the shale core meets the requirement of measuring the porosity by using helium. And (3) washing oil by using oil washing equipment, wherein the fluorescence series of the shale core plunger sample after washing oil is lower than that of chloroform asphalt in SY/T5118-2005 rock in the oil and natural gas industry standard of the people's republic of China, and the 3-level fluorescence reaches helium porosity measurement standard for about 30 days. The porosity of the washed shale core plunger sample was measured by helium porosity measuring equipment (ultra pore300 helium porosimeter from american core company) to obtain porosity Φ1 (see table 1) after washing the shale core plunger sample. The residual oil porosity Φ2 (see fig. 2) of the shale core plunger sample after oil washing is measured by using nuclear magnetic resonance measuring equipment. Nuclear magnetic resonance technology quantitatively characterizes the fluid content by detecting the relaxation signals of hydrogen nuclei in a unit volume of fluid, and current laboratory nuclear magnetic resonance instruments (model GEOSPEC2 nmr from oxford instruments, england) are capable of measuring substantially all of the fluid information in tight rock pores. Under the condition of not considering hydrogen correction, the hydrogen index of oil and water can be considered to be close to 1, and the nuclear magnetic resonance spectrum of the core after the washing oil treatment can be measured to obtain the volume of the residual oil and the porosity information of the residual oil. And (3) carrying out destructive distillation heating on the shale core plunger sample by using a temperature control destructive distillation method, wherein the core plunger sample is slowly heated to 100 ℃ at 10 ℃ per hour, and is heated to 10 ℃ per 2 hours after 200 ℃ until the required maximum temperature is reached, and the maximum temperature is controlled between 400 ℃ and takes about 40 hours. And measuring the porosity of the shale core plunger sample subjected to temperature control carbonization by using helium porosity measurement equipment, and obtaining the porosity phi 3 of the shale core plunger sample subjected to temperature control carbonization. And after the 17 shale core plunger samples are measured, adding the helium porosity phi 1 measured after oil washing of each sample and the residual oil porosity phi 2 measured by nuclear magnetic resonance, and comparing with the helium porosity phi 3 measured after temperature control carbonization, wherein the helium porosity value measured after temperature control carbonization is used as the porosity value of the shale core plunger samples.
The result of the relation between the residual oil porosity and the nuclear magnetic T2 relaxation time measured in the example 3 is shown in fig. 2, the result of the example 14 is shown in fig. 3, the porosity measured by the temperature-controlled carbonization method is consistent with the porosity measured by the nuclear magnetic after conventional oil washing, the time is saved compared with the conventional method, the calculation is not needed, and the accuracy is high.
TABLE 1 shale core porosity analysis statistics table
The results in Table 1 show that the absolute error is between 0 and 0.5 percent, which shows that the porosity measured by the temperature-controlled carbonization method has high accuracy and meets the requirements of the oil and gas industry standard SY/T5336-2006 core analysis method of the people's republic of China.
The residual oil porosity measured by nuclear magnetic resonance is obtained by measuring nuclear magnetic resonance spectrum of a core sample after oil washing treatment, wherein the hydrogen index of oil and water is close to 1 under the condition of not considering hydrogen correction. The same batch of samples are washed oil first, helium porosity after washing oil is measured, residual oil porosity is measured by a nuclear magnetic resonance method, total porosity is calculated by adding the two, then temperature control carbonization is carried out, helium porosity after temperature control carbonization is measured, and the experimental sequence is used for verifying the accuracy of the measured porosity data, so the sequence is not reversible. When the method is used for measuring the shale porosity, the steps 1, 2 and 3 can be omitted, and the shale porosity is directly pyrolyzed, so that the time-consuming and longer procedure of core washing is saved.
The shale core porosity measured by the method can be directly used for evaluating desserts and calculating geological reserves, and does not need to carry out additional calculation. The helium porosity measurement device used in the present invention was an ultra pore300 helium porosimeter from core company, U.S. and the test gas was helium at a test pressure of 200psi. The nuclear magnetic resonance instrument used in the invention is GEOSPEC2 type of oxford instrument company in England, and can measure all fluid information in the tight rock pore. The invention can be widely applied to shale cores and other compact rock cores with difficult development of nano and micro pores and oil washing.
In order to avoid the problems of deformation or cracks of a plunger sample and the like in the carbonization heating process, and simultaneously, residual oil gas can be carbonized, the carbonization heating speed is strictly controlled, and the highest temperature is controlled between 350 and 400 ℃ in order to prevent colloid and asphaltene from being pyrolyzed. The highest dry distillation temperature is determined according to the following steps: according to the pyrolysis temperature range of different oil components in the oil and gas industry standard SY/T5117-1996 rock pyrolysis analysis method of the people's republic of China, kerosene and diesel oil are pyrolyzed at 200-350 ℃, heavy oil is pyrolyzed at 350-450 ℃, colloid and asphaltene are pyrolyzed at 450-600 ℃, in order to avoid the pyrolysis of colloid and asphaltene and influence the accuracy of shale core plunger-like porosity measurement, the carbonization temperature is controlled at 350-400 ℃, and the specific temperature can be determined according to the oil quality of the core oil.
In summary, the measurement method fully considers the influence of effective pore development characteristics of shale cores and residual oil caused by incomplete washing oil on the measurement of the porosity, directly adopts a temperature-control carbonization method to remove the residual oil, eliminates the influence of the residual oil on the measurement of the porosity, avoids pyrolysis of colloid and asphaltene by controlling the highest temperature, and further verifies the accuracy of the measurement method by adding the measured helium porosity after washing oil and the residual oil porosity measured by nuclear magnetic resonance after washing oil. The method solves the problems of long period, large difficulty and inaccuracy of shale core porosity measurement, so that the shale physical properties can be accurately analyzed by a person skilled in the art, reasonable exploration and development can be further carried out, and the development of shale oil industry is facilitated.
The above is only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited by this, and any modification made on the basis of the technical scheme according to the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (8)
1. The method for measuring the porosity of the shale core is characterized by comprising the following steps of:
step 1) processing shale rock core into a plunger sample, and washing oil from the plunger sample;
step 2) measuring the porosity of the plunger sample after oil washing to obtain the porosity of the plunger sample after oil washing and the porosity of residual oil;
step 3) performing carbonization heating on the plunger sample after oil washing, and measuring the porosity of the plunger sample after carbonization heating to obtain the porosity after carbonization;
and 4) adding the porosity of the plunger-like wash oil and the porosity of the residual oil to obtain a sum of the porosities, comparing the sum of the porosities with the porosity after carbonization, and calculating an absolute error, wherein when the absolute error is less than or equal to 0.5%, the porosity after carbonization is the total porosity of the shale core.
2. The method for measuring shale core porosity according to claim 1, wherein in the step 3), conditions of dry distillation heating are as follows: the carbonization temperature is 350-400 ℃, and the carbonization time is 40-50 h.
3. The method for measuring shale core porosity according to claim 1, wherein in the step 3), the carbonization heating process is as follows:
the core plunger sample is heated to 100 ℃ firstly, the temperature is raised to 10 ℃ per hour, and the temperature is raised to 10 ℃ per 2 hours after 200 ℃ until reaching 350-400 ℃.
4. The method for measuring shale core porosity according to claim 1, wherein in the step 4), the absolute error is calculated as follows:
wherein, phi 1 is the porosity after plunger-like wash oil, phi 2 is the residual oil porosity after plunger-like wash oil, and phi 3 is the porosity after carbonization.
5. The method for measuring the porosity of the shale core according to claim 1, wherein in the step 2), the test gas is helium gas during the measurement of the porosity.
6. The method for measuring the porosity of the shale core according to claim 1, wherein in the step 2) and the step 3), the porosity measurement is performed by a nuclear magnetic resonance measurement device.
7. The method for measuring the porosity of the shale core according to claim 1, wherein in the step 2), the test pressure is 200psi when measuring the porosity.
8. The method for measuring shale core porosity according to claim 1, wherein the oil washing period is 30 days when the plunger sample is washed in step 1).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118603847A (en) * | 2024-08-07 | 2024-09-06 | 中国石油集团西部钻探工程有限公司 | Coal seam porosity determination method and device based on rock pyrolysis technology |
| CN119643401A (en) * | 2023-09-15 | 2025-03-18 | 中国石油天然气股份有限公司 | Characterization method, plate construction method and measurement method of shale oil reservoir space |
| CN120467993B (en) * | 2025-05-28 | 2025-10-17 | 中国石油大学(华东) | Method for determining primary porosity of shale oil reservoir |
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2021
- 2021-12-24 CN CN202111605185.5A patent/CN116337707A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN119643401A (en) * | 2023-09-15 | 2025-03-18 | 中国石油天然气股份有限公司 | Characterization method, plate construction method and measurement method of shale oil reservoir space |
| CN118603847A (en) * | 2024-08-07 | 2024-09-06 | 中国石油集团西部钻探工程有限公司 | Coal seam porosity determination method and device based on rock pyrolysis technology |
| CN120467993B (en) * | 2025-05-28 | 2025-10-17 | 中国石油大学(华东) | Method for determining primary porosity of shale oil reservoir |
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