CN106706496A - Measurement method for nano-scale oil bearing aperture distribution of dense oil/shale oil - Google Patents
Measurement method for nano-scale oil bearing aperture distribution of dense oil/shale oil Download PDFInfo
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- 238000009826 distribution Methods 0.000 title claims abstract description 73
- 239000003079 shale oil Substances 0.000 title claims abstract description 15
- 238000000691 measurement method Methods 0.000 title abstract 4
- 239000011148 porous material Substances 0.000 claims abstract description 46
- 238000012360 testing method Methods 0.000 claims abstract description 8
- 239000003960 organic solvent Substances 0.000 claims abstract description 5
- 238000003556 assay Methods 0.000 claims description 23
- 239000004576 sand Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 10
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical group ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000002474 experimental method Methods 0.000 abstract description 26
- 239000011435 rock Substances 0.000 abstract description 8
- 239000003921 oil Substances 0.000 description 62
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 26
- 229910002092 carbon dioxide Inorganic materials 0.000 description 15
- 238000001179 sorption measurement Methods 0.000 description 15
- 239000001569 carbon dioxide Substances 0.000 description 14
- 239000007788 liquid Substances 0.000 description 14
- 229910052757 nitrogen Inorganic materials 0.000 description 13
- 238000002336 sorption--desorption measurement Methods 0.000 description 12
- 239000010779 crude oil Substances 0.000 description 11
- 239000007789 gas Substances 0.000 description 8
- 239000004215 Carbon black (E152) Substances 0.000 description 7
- 229930195733 hydrocarbon Natural products 0.000 description 7
- 150000002430 hydrocarbons Chemical class 0.000 description 7
- 238000003775 Density Functional Theory Methods 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 238000003795 desorption Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000000197 pyrolysis Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000005481 NMR spectroscopy Methods 0.000 description 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
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- 238000013459 approach Methods 0.000 description 1
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- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000010997 low field NMR spectroscopy Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000005311 nuclear magnetism Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
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- 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
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- G01N15/088—Investigating volume, surface area, size or distribution of pores; Porosimetry
- G01N15/0893—Investigating volume, surface area, size or distribution of pores; Porosimetry by measuring weight or volume of sorbed fluid, e.g. B.E.T. method
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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Abstract
The invention discloses a measurement method for nano-scale oil bearing aperture distribution of dense oil/shale oil. The measurement method comprises the following steps: smashing a dense sandstone sample or shale sample to obtain a powdered sample, extracting one part of the powdered sample through an organic solvent to obtain an extracted sample, and taking the other part of the powdered sample as a non-extracted sample; respectively carrying out aperture distribution test on the non-extracted sample and the extracted sample to obtain aperture distribution curves of the non-extracted sample and the extracted sample; respectively fitting the two curves to obtain micropore-mesoporous-macropore aperture distribution of the non-extracted sample and the extracted sample, and taking a difference value between the specific pore volume of the extracted sample and the specific pore volume of the non-extracted sample as a specific pore volume of an oil bearing pore space, thus obtaining the nano-scale oil bearing aperture distribution of the dense oil/shale oil. According to the measurement method, the oil bearing aperture distribution obtained in the experiment is compared with the total oil content of rock, so that the overall distribution of oil bearing apertures of the rock can be objectively evaluated.
Description
Technical field
The present invention relates to a kind of assay method of the nanoscale oil-containing pore-size distribution of fine and close oil/shale oil.
Background technology
With being deepened continuously to fine and close oil and shale oil work of exploration and development both at home and abroad, focus is from initial money
Evaluate progressively steering mechanism research in source.Wherein, it explored due to the supporting environment of fine and close oil and shale oil, develop and have important
Meaning, has therefore suffered from the extensive concern of domestic and foreign scholars.The oil-containing pore-size distribution of fine and close oil and shale oil is its supporting environment
Important component, but have no rational analytical plan all the time, therefore be all the time section's knowledge of puzzlement domestic and foreign scholars
One of topic.
It is containing a large amount of nanoscale holes therefore right because average pore size is far below common reservoir in tight sand and shale
The analysis difficulty of its pore-size distribution is larger.Mainly there is following several method in the prior art：
Scheme one：
To tight sand/shale samples saturation crude oil or water, the rock sample to different saturation carries out nuclear-magnetism T2Spectrum point
Analysis, using T2The difference of spectrum obtains oil-containing pore-size distribution (M.Fleury, Characterization of shales with
low field NMR,in:The International Symposium of Core Analysts,Avignon,France,
8e11September,SCA2014-014,2014.；J.Li,J.Yin,Y.Zhang,S.Lu,W.Wang,J.Li,F.Chen,
Y.Meng,A comparison of experimental methods for describing shale pore
features—A case study in the Bohai Bay Basin of eastern China,International
Journal of Coal Geology,152,Part B(2015)39-49.；A.Tinni,E.Odusina,
I.Sulucarnain,C.Sondergeld,C.Rai,NMR Response of Brine,Oil and Methane in
Organic Rich Shales,in:SPE Unconventional Resources Conference,Society of
Petroleum Engineers,2014.).Oil-containing pore-size distribution obtained by the program is the pore-size distribution of saturated oils, not
The pore-size distribution of initial oil, because filling mechanism is different, the two and non-equivalence.
Scheme two：
To extracting, forward and backward high maturation shale samples carry out carbon dioxide and liquid nitrogen pore-size distribution is analyzed, from
And obtain influence (J.Li, S.Zhou, Y.Li, Y.Ma, Y.Yang, C.Li, Effect of of the asphalitine to shale pore-size distribution
organic matter on pore structure of mature lacustrine organic-rich shale:A
case study of the Triassic Yanchang shale,Ordos Basin,China,Fuel,185(2016)
421-431.).The object that the program is studied is maturation shale samples high, thus crude oil in shale almost total number is converted into
Gas, thus the research object not crude oil of the program pore-size distribution, the only influence of residual asphalt confrontation shale pore-size distribution.
In addition, be not further analyzed for pore-size distribution combination oil-containing total amount by the program, therefore certain pore size scope is not obtained
The relation of interior oil content and total oil content amount.
The content of the invention
It is an object of the invention to provide a kind of assay method of the nanoscale oil-containing pore-size distribution of fine and close oil/shale oil, this
By being stripped removal crude oil in samples to rock sample, the pore-size distribution to extracting forward and backward tight sand/shale enters for invention
Row experiment test, and the two is carried out, than analysis, oil-containing pore-size distribution to be reflected using the difference between the two；In addition, to extracting forward and backward cause
Close sandstone/shale samples carry out pyrolysis analysis, and then obtain oil-containing total amount.Respective aperture interval is included into oil volume and total oil content
Amount is analyzed, and finally determines the oil-containing ratio in the interval of the aperture.
The assay method of the nanoscale oil-containing pore-size distribution of fine and close oil/shale oil provided by the present invention, including following step
Suddenly：
(1) tight sand sample or shale samples obtain powder sample after crushed, and the part powder sample is had
Machine solvent extraction, sample after being extracted, the part powder sample is used as sample before extracting；
(2) sample after sample before the extracting and the extracting is carried out into pore-size distribution test respectively, obtains the extracting
The pore size distribution curve of sample after the pore size distribution curve of preceding sample and the extracting；
(3) pore size distribution curve of sample enters respectively after pore size distribution curve to sample before the extracting and the extracting
Row fitting, obtains micropore-Jie of sample after the pore-size distribution in the micropore-mesopore-grand hole of sample and the extracting before the extracting
The pore-size distribution in hole-grand hole；
The pore-size distribution refers to the relation between aperture and specific pore volume；
(4) difference after the extracting before the specific pore volume of sample and the extracting between the specific pore volume of sample is containing oilhole
The specific pore volume in gap space, so far obtains the nanoscale oil-containing pore-size distribution of fine and close oil or shale oil.
In above-mentioned assay method, micropore refers to hole of the aperture less than 2nm, and the mesoporous aperture that refers to is for 2~50nm
Between hole, grand hole refer to aperture more than 50nm hole.
In above-mentioned assay method, in step (1), the granularity of the powder sample can be 80~100 mesh.
In above-mentioned assay method, in step (1), the solvent that the organic solvent extracting is used can be chloroform, using rope
The mode of family name's extracting；
The time of the organic solvent extracting is not less than 72 hours, fully to remove the crude oil in sample.
In above-mentioned assay method, before step (2), methods described also includes to sample before the extracting and the extracting
The step of sample is pre-processed as follows afterwards：
Sample after sample before the extracting and the extracting is heated above 100 DEG C, such as 105 DEG C, it is therefore an objective to fully remove
Water is removed, and the operation for being vacuumized simultaneously；
The process duration of the pretreatment is not less than 12 hours；
By moisture and other impurities in the pretreatment fully removal sample.
In above-mentioned assay method, in step (2), the pore-size distribution test can be carried out using existing method, such as be inhaled
Attached-detachment assays, nuclear magnetic resonance or Electronic Speculum etc.；
The adsorption-desorption experiment can be tested using carbon dioxide adsorption-detachment assays and liquid nitrogen adsorption-desorption, wherein,
Carbon dioxide adsorption-detachment assays typically can test microvia (be less than 2nm), and the experiment of liquid nitrogen adsorption-desorption can typically test 2~
Hole between 150nm.
The present invention can respectively obtain institute using the carbon dioxide adsorption experiment and the experiment of liquid nitrogen adsorption-desorption for carrying out successively
The preceding sample of extracting is stated to carbon dioxide adsorption thermoisopleth and to sample after liquid nitrogen adsorption-desorption isothermal, the extracting to dioxy
Change carbon adsorption thermoisopleth and to liquid nitrogen adsorption-desorption isothermal.
The condition of the carbon dioxide adsorption experiment is as follows：
Temperature is 0 DEG C, and absolute pressure is 0.002~0.1MPa.
The condition of the liquid nitrogen adsorption-desorption experiment is as follows：
Temperature is -195.70 DEG C, and absolute pressure is 0.0006~0.1112MPa.
In above-mentioned assay method, in step (3), the fitting can be carried out using existing model；
Such as using carbon dioxide adsorption experiment and liquid nitrogen adsorption-desorption test when, can using NLDFT models, DR models,
BJH models or DFT models are fitted to the adsorption-desorption isothermal curve for obtaining.
In above-mentioned assay method, methods described also includes the step of determining nanoscale aperture oil content as follows：
1) sample before the extracting is pyrolyzed, product S is collected at 300 DEG C1, received during 300~650 DEG C
Collection product S2；
The product S1Predominantly free hydrocarbon；
The product S2Both the heavy hydrocarbon in shale samples had been included, and had been received including kerogen in shale samples (Oil source bed)
The cracked hydrocarbon produced in thermal process；
Sample after the extracting is pyrolyzed, product S is collected during 300~650 DEG C2′；
The product S1With the product S2Quality sum and the product S2' difference be the tight sand sample
Or the oil-containing total amount of the shale samples；
2) the nanoscale aperture oil content of the tight sand sample or the shale samples and the tight sand sample
Or the ratio of the oil-containing total amount of the shale samples is the nanoscale aperture of the tight sand sample or the shale samples
Oil content；
The nanoscale aperture oil content of the tight sand sample or the shale samples is by the fine and close oil or shale oil
Nanoscale oil-containing pore-size distribution and oil density obtain, i.e., respective aperture distributed area is obtained according to nanoscale oil-containing pore-size distribution
Interior total specific pore volume, is multiplied with oil density and just obtains corresponding oil content.
Assay method of the present invention has the following advantages that：
Pore-size distribution of the present invention by contrast containing oil samples (sample before extracting) and without oil samples (sample after extracting),
The oil-containing pore-size distribution of rock can objectively be obtained.It is past during due to being tested the pore-size distribution of rock using different experiments
Toward having some limitations, the pore-size distribution in a certain pore diameter range can only be measured, such as carbon dioxide adsorption is tested, typically
The pore size distribution range of micropore (aperture is less than 2nm) can only be reflected, this will cause the oil-containing aperture for only being obtained by particular experiment
Distribution has significant limitations.For this problem, the present invention always contains the oil-containing pore-size distribution measured by experiment and rock
Oil mass is contrasted, and then overall distribution to rock oil-containing aperture makes objective evaluation.
Brief description of the drawings
Fig. 1 is the flow chart of assay method of the present invention.
Fig. 2 for the present invention extracting before sample and extracting after sample to carbon dioxide adsorption thermoisopleth.
Fig. 3 for the present invention extracting before sample and extracting after sample to liquid nitrogen adsorption-desorption isothermal.
Fig. 4 is the pore-size distribution of sample after the preceding sample of present invention extracting and extracting.
Fig. 5 is oil-containing graph of pore diameter distribution in the nano-pore that the present invention is determined.
Specific embodiment
Experimental technique used in following embodiments is conventional method unless otherwise specified.
Material used, reagent etc. in following embodiments, unless otherwise specified, commercially obtain.
The present embodiment is with Damintun Depression E2s4 LAs a example by section shale samples, pore-size distribution is by carbon dioxide and liquid
N2 adsorption detachment assays are measured, and flow chart is as shown in Figure 1.
Step 1：Sample pretreatment
Cleaning shale samples surface, and by sample comminution to 80~100 mesh, powder dress sample is divided into two parts, to wherein
A sample carries out soxhlet type using chloroformic solution, and extracting continues more than 72 hours, fully to remove the crude oil in sample.
So far, the powdered samples before extracting and after extracting are respectively obtained.
Step 2：Carbon dioxide and liquid nitrogen adsorption experiment
The forward and backward shale samples powder of extracting is chosen respectively, carries out carbon dioxide and liquid nitrogen absorption/detachment assays.
Sample is pre-processed first, is heated to 105 DEG C and while is vacuumized, preprocessing process continues 12 hours
More than, fully to remove the moisture and other impurities in sample.
Carbon dioxide adsorption experiment is carried out to sample after pretreatment, this experiment is using Micromeritics ASAP-
2460 instruments, experimental temperature is 0 DEG C, and experiment relative pressure is 5.00 × 10-4~2.89 × 10-2(absolute pressure is about 0.002
~0.1MPa), obtain adsorption isothermal curve (as shown in Figure 2).
Followed by the experiment of liquid nitrogen adsorption/desorption, still using Micromeritics ASAP-2460 instruments, experimental temperature
It it is -195.70 DEG C, relative pressure was 0.005~1.0 (absolute pressure is about 0.0006~0.1112MPa), is adsorbed/is desorbed
Thermoisopleth (as shown in Figure 3).
Be can be seen that on the whole by Fig. 2 and Fig. 3, no matter for adsorption isotherm or desorption isotherm, extracted sample
Adsorbance be all higher than not extracting the adsorbance of sample, illustrate that the presence of crude oil in samples hinders the entrance of gas.
Step 3：Pore-size distribution is asked for using NLDFT models
Non-localized density functional theory (NLDFT) can make accurate aperture point in the range of larger aperture to porous media
Cloth evaluates (P.I.Ravikovitch, G.L.Haller, A.V.Neimark, Density functional theory model
for calculating pore size distributions:pore structure of nanoporous
catalysts,Adv Colloid Interfac,76(1998)203-226.).Therefore, the present embodiment by taking NLDFT as an example to
Extracting and the shale samples not extracted carry out pore-size distribution evaluation.
NLDFT principles are based on to the CO obtained by experiment using the softwares of MicroActive for ASAP 24602、N2Inhale
Attached/desorption isotherm is fitted, and the micropore for having extracted and not extracted sample is obtained respectively (based on CO2Adsorption isotherm) and be situated between
Hole-grand hole (is based on N2Adsorption-desorption isothermal) pore-size distribution.
In NLDFT, the pore-size distribution of porous media can be by the fitting to calculating absorption/desorption isotherm and measured value
Ask for.Measured absorption/desorption isotherm the N (P) of experiment can be expressed as follows (P.I.Ravikovitch, G.L.Haller,
A.V.Neimark,Density functional theory model for calculating pore size
distributions:pore structure of nanoporous catalysts,Adv Colloid Interfac,76
(1998)203-226.；C.Lastoskie,K.E.Gubbins,N.Quirke,Pore-Size Distribution
Analysis of Microporous Carbons-a Density-Functional Theory Approach,J
PhysChem-Us,97(1993)4786-4796.；P.Tarazona,Free-Energy Density Functional for
Hard-Spheres,Phys Rev A,31(1985)2672-2679.；P.Tarazona,U.M.B.Marconi,R.Evans,
Phase-Equilibria of Fluid Interfaces and Confined Fluids-Nonlocal Versus
Local Density Functionals,MolPhys,60(1987)573-595.)：
In formula, HminAnd HmaxThe minimum value and maximum in respectively analyzed aperture, f (H) are the pore-size distribution letter of sample
Number, when ρ (P, H) is pressure for P (MPa), aperture is averag density of the Adsorbate Gas in hole in the hole of H (nm).
Assuming that the crack type hole in shale is respectively provided with specific geometry, and can be contacted with Adsorbate Gas.It is huge
Canonical assemblage can preferably describe the macroscopic property in shale pore system, wherein chemical potential μ (J/mol), temperature T (K)
With volume V (cm3) be designated.Density Distribution (ρL) can be minimized by potential-energy function Ω and asked for：
Ω[ρL(r)]=F [ρL(r)]-∫drρL(r)[μ-Vext(r)] (2)
In formula, F is Helmholtz free energy (J), ρL(r)(g/cm3) be specify aperture hole in position r gas
Density, is integrated for formula 2 to pore volume.Vext(J) it is surface potential energy, by gas-gas and the effect gesture of gas solids
Can be determined.
According to the Density Distribution of gas in different pore size, the integration type of formula 1 can obtain pore-size distribution by Optimization Solution
Function f (H).In solution procedure, realize seeking f (H) by calculated value and the error sum of squares of experiment value minimize
Solution：
In formula, E is the average value of error sum of squares, npIt is the points of adsorption isotherm, nHIt is in numerical integration process mesopore
The number in footpath size subinterval.
Using principles above, respectively by carbon dioxide adsorption data and liquid nitrogen absorption/desorption data obtain micropore and mesoporous-
The pore-size distribution in grand hole, and the two is docked, obtain the pore-size distribution (as shown in Figure 4) in micropore-mesopore-grand hole.
Step 4：Nano-pore oil-containing pore-size distribution is asked for
As shown in Figure 4, on the whole, in respective aperture is interval, the specific pore volume of sample has been extracted generally more than not extracting sample
The specific pore volume of product, illustrates that the crude oil in sample occupies interstitial space.Using the difference of the two specific pore volume, for corresponding aperture
Interval, the specific pore volume for not extracting sample is subtracted using the specific pore volume for having extracted sample, obtains the specific pore volume of oil-containing interstitial space, its
Result is as shown in Figure 5.
Step 5：Nano-pore oil content is asked for
Pyrolysis Experiment is carried out to the sample for having extracted He do not extract respectively, experiment is carried out by Rock-Eval instruments.For
The sample not extracted, in Pyrolysis Experiment, free hydrocarbon (S is measured at 300 DEG C1), during 300~650 DEG C, measure S2, S2
Both the heavy hydrocarbon in shale samples, and the cracking produced in thermal histories including kerogen in shale samples (Oil source bed) had been included
Hydrocarbon.For the sample for having extracted, in Pyrolysis Experiment, S is measured during 300~650 DEG C2', due to chloroform process
Through eliminating the crude oil in sample, therefore S2' in only include kerogen cracking hydrocarbon.From S1And S2S is subtracted in sum2', you can
Crude oil total amount in sample.
In the present embodiment, S1It is 6.57mg/g, S2It is 42.43mg/g, S2' it is 35.85mg/g, oil-containing total amount is
13.15mg/g。
Meanwhile, to micropore and it is mesoporous in oil-containing specific pore volume sum up, you can obtain micropore and it is mesoporous in oil-containing it is total
Specific pore volume, (this example Central Plains oil density is 0.84g/cm with oil density3) be multiplied, you can obtain its oil content, the present embodiment
In its value be 1.8mg/g.
By to micropore and it is mesoporous in oil content contrasted with total oil content amount, it is known that micropore and it is mesoporous in oil content
Only the 13.7% of oil-containing total amount, illustrates in the sample, and most crude oil preservations are in grand aerial more than 50nm.
Claims (5)
1. a kind of assay method of the nanoscale oil-containing pore-size distribution of fine and close oil/shale oil, comprises the following steps：
(1) tight sand sample or shale samples obtain powder sample after crushed, and the part powder sample carries out organic molten
Agent is extracted, sample after being extracted, and the part powder sample is used as sample before extracting；
(2) sample after sample before the extracting and the extracting is carried out into pore-size distribution test respectively, obtains sample before the extracting
The pore size distribution curve of sample after the pore size distribution curve of product and the extracting；
(3) pore size distribution curve of sample is intended respectively after pore size distribution curve to sample before the extracting and the extracting
Close, obtain the micropore-mesopore of sample after the pore-size distribution in the micropore-mesopore-grand hole of sample and the extracting before the extracting-grand
The pore-size distribution in hole；
The pore-size distribution refers to the relation between aperture and specific pore volume；
(4) to be oil-containing hole empty for the difference after the extracting before the specific pore volume of sample and the extracting between the specific pore volume of sample
Between specific pore volume, so far obtain the nanoscale oil-containing pore-size distribution of fine and close oil or shale oil.
2. assay method according to claim 1, it is characterised in that：In step (1), the granularity of the powder sample is 80
~100 mesh.
3. assay method according to claim 1 and 2, it is characterised in that：In step (1), the organic solvent extracting is adopted
Solvent is chloroform；
The time of the organic solvent extracting is not less than 72 hours.
4. the assay method according to any one of claim 1-3, it is characterised in that：Before step (2), methods described is also
The step of including being pre-processed as follows to sample after sample before the extracting and the extracting：
Sample after sample before the extracting and the extracting is heated above 100 DEG C and while the operation for being vacuumized；
The process duration of the pretreatment is not less than 12 hours.
5. the assay method according to any one of claim 1-4, it is characterised in that：Methods described also includes following measure
The step of nanoscale aperture oil content：
1) sample before the extracting is pyrolyzed, product S is collected at 300 DEG C1, collected during 300~650 DEG C and produced
Thing S2；
Sample after the extracting is pyrolyzed, product S is collected during 300~650 DEG C2′；
The product S1With the product S2Quality sum and the product S2' difference be the tight sand sample or institute
State the oil-containing total amount of shale samples；
2) the nanoscale aperture oil content of the tight sand sample or the shale samples and the tight sand sample or institute
The ratio for stating the oil-containing total amount of shale samples is the nanoscale aperture oil-containing of the tight sand sample or the shale samples
Rate；
The nanoscale aperture oil content of the tight sand sample or the shale samples is received by the fine and close oily or shale oil
Meter level oil-containing pore-size distribution and oil density are obtained.
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| CN107907461A (en) * | 2017-11-03 | 2018-04-13 | 中国石油化工股份有限公司 | The research method of the main preservation pore diameter range of shale oil |
| CN109856176A (en) * | 2019-03-27 | 2019-06-07 | 中国石油大学(华东) | The full-scale hole quantitatively characterizing method of compact reservoir based on NMR and LTNA |
| WO2019184429A1 (en) * | 2018-03-27 | 2019-10-03 | 中国石油大学(华东) | Evaluation method for hydrogen containing ingredient, porosity and aperture of shale rich in organic matters |
| CN112304837A (en) * | 2020-06-24 | 2021-02-02 | 成都理工大学 | Method for judging shale oil reservoir organic matter microscopic occurrence structure |
| CN113504257A (en) * | 2021-08-06 | 2021-10-15 | 科正检测(苏州)有限公司 | Method for detecting oil content of shale |
| CN113670787A (en) * | 2020-05-14 | 2021-11-19 | 中国石油天然气股份有限公司 | Method for testing pore diameters of micropores and mesopores of organic matters and other minerals in shale |
| CN113970512A (en) * | 2021-01-05 | 2022-01-25 | 中国石油天然气股份有限公司 | Method for determining enrichment pore size range of free hydrocarbon |
| CN114428043A (en) * | 2020-09-18 | 2022-05-03 | 中国石油化工股份有限公司 | Porous medium pore size distribution characterization method and electronic equipment |
| CN117571582A (en) * | 2024-01-16 | 2024-02-20 | 中国地质大学（武汉） | Method for determining porosity occupied by light hydrocarbon and heavy hydrocarbon in shale oil reservoir |
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| CN107907461A (en) * | 2017-11-03 | 2018-04-13 | 中国石油化工股份有限公司 | The research method of the main preservation pore diameter range of shale oil |
| WO2019184429A1 (en) * | 2018-03-27 | 2019-10-03 | 中国石油大学(华东) | Evaluation method for hydrogen containing ingredient, porosity and aperture of shale rich in organic matters |
| CN109856176A (en) * | 2019-03-27 | 2019-06-07 | 中国石油大学(华东) | The full-scale hole quantitatively characterizing method of compact reservoir based on NMR and LTNA |
| CN109856176B (en) * | 2019-03-27 | 2022-03-08 | 中国石油大学(华东) | NMR and LTNA-based compact reservoir full-size pore quantitative characterization method |
| CN113670787A (en) * | 2020-05-14 | 2021-11-19 | 中国石油天然气股份有限公司 | Method for testing pore diameters of micropores and mesopores of organic matters and other minerals in shale |
| CN112304837A (en) * | 2020-06-24 | 2021-02-02 | 成都理工大学 | Method for judging shale oil reservoir organic matter microscopic occurrence structure |
| CN112304837B (en) * | 2020-06-24 | 2021-06-25 | 成都理工大学 | Method for judging shale oil reservoir organic matter microscopic occurrence structure |
| CN114428043A (en) * | 2020-09-18 | 2022-05-03 | 中国石油化工股份有限公司 | Porous medium pore size distribution characterization method and electronic equipment |
| CN113970512A (en) * | 2021-01-05 | 2022-01-25 | 中国石油天然气股份有限公司 | Method for determining enrichment pore size range of free hydrocarbon |
| CN113970512B (en) * | 2021-01-05 | 2024-05-28 | 中国石油天然气股份有限公司 | Method for determining free hydrocarbon enrichment pore size range |
| CN113504257A (en) * | 2021-08-06 | 2021-10-15 | 科正检测(苏州)有限公司 | Method for detecting oil content of shale |
| CN117571582A (en) * | 2024-01-16 | 2024-02-20 | 中国地质大学（武汉） | Method for determining porosity occupied by light hydrocarbon and heavy hydrocarbon in shale oil reservoir |
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