CN106323838A - Method for determining specific surface area of shale pore - Google Patents
Method for determining specific surface area of shale pore Download PDFInfo
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- CN106323838A CN106323838A CN201610790146.XA CN201610790146A CN106323838A CN 106323838 A CN106323838 A CN 106323838A CN 201610790146 A CN201610790146 A CN 201610790146A CN 106323838 A CN106323838 A CN 106323838A
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- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000011148 porous material Substances 0.000 title abstract description 14
- 238000001179 sorption measurement Methods 0.000 claims abstract description 87
- 239000002356 single layer Substances 0.000 claims abstract description 56
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 82
- 229920006395 saturated elastomer Polymers 0.000 claims description 50
- 229910052757 nitrogen Inorganic materials 0.000 claims description 41
- 238000002474 experimental method Methods 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 8
- 239000002156 adsorbate Substances 0.000 claims description 3
- 239000011435 rock Substances 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000011161 development Methods 0.000 abstract description 3
- 238000012512 characterization method Methods 0.000 abstract 2
- 239000000463 material Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 238000007872 degassing Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- 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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Abstract
The invention provides a method for determining the specific surface area of a shale pore and relates to the unconventional oil and gas exploration and development technologies. The method for determining the specific surface area of the shale pore comprises the following steps: acquiring total monolayer saturation adsorption capacity of the surface of a shale sample; determining the total specific surface area of shale according to the total monolayer saturation adsorption capacity; acquiring monolayer saturation adsorption capacity of the non-porous surface of the shale sample; determining the non-porous specific surface area according to the monolayer saturation adsorption capacity of the non-porous surface; determining the specific surface area of the pore according to the total specific surface area and the non-porous specific surface area. Shale pore development characteristics are considered sufficiently when the specific surface area of the pore is determined according to the total specific surface area and the non-porous specific surface area of the shale, larger errors caused by the fact that the specific surface area of the shale is evaluated with adoption of a conventional BET equation and a conventional instrument are avoided, the shale pore characterization is more precise, and more objective and more accurate data support is provided for characterization of a full-pore-diameter pore structure of the shale.
Description
Technical field
The present invention relates to unconventionaloil pool exploration and development technology, particularly relate to the specific area measuring side of a kind of shale micropore
Method.
Background technology
Shale gas is one of unconventional petroleum resources, before exploitation shale gas, in order to effectively open shale gas
Send out, be necessary for shale reservoir is evaluated, and the full aperture pore structure of shale characterizes the important ring being to evaluate shale reservoir
One of joint.Owing to shale micropore is grown, accurately calculate the specific surface area full aperture pore structure table for shale of shale micropore
Levy most important.
In prior art, the mensuration of the specific surface area of shale micropore is typically on existing determining instrument, selects phase
The model answered is to determine the pore-size distribution of shale, and then obtains the specific surface area at different pore size distribution.And micropore refers to aperture
Less than the hole of 2nm, when measuring the pore specific surface area of micropore, due to the restriction of the condition such as precision of existing instrument, cause gained
The deviation of result is relatively big, and accuracy is poor.
Summary of the invention
For drawbacks described above of the prior art, the present invention provides a kind of specific area measuring method of shale micropore, energy
Enough improve the accuracy of the specific surface area of the shale micropore obtained.
The present invention provides a kind of specific area measuring method of shale micropore, it is characterised in that including:
Obtain total monolayer saturated extent of adsorption on shale samples surface；
According to described total monolayer saturated extent of adsorption, determine the total specific surface area of shale；
Obtain the monolayer saturated extent of adsorption of the non-micropore surface of described shale samples；
According to the monolayer saturated extent of adsorption of described non-micropore surface, determine the non-micropore specific area of shale；
Micropore specific area is determined according to described total specific surface area and non-micropore specific area.
Further, total monolayer saturated extent of adsorption on described acquisition shale samples surface, including:
By shale samples being carried out low-pressure nitrogen adsorption experiment, obtain the nitrogen adsorption amount under different relative pressure；
According to the described nitrogen adsorption amount under different relative pressures, and the BET equation of classics determines described shale samples
Described total monolayer saturated extent of adsorption on surface.
Further, described according to the described nitrogen adsorption amount under different relative pressures, and the BET equation of classics determines
Described total monolayer saturated extent of adsorption on described shale samples surface, including:
According to following first formula, determine total monolayer saturated extent of adsorption V on described shale samples surfacem1,
Wherein, VadsFor nitrogen adsorption amount, Vm1For total monolayer saturated extent of adsorption, CBETFor constant, P/P0Relatively press for gas
Power.
Further, according to described total monolayer saturated extent of adsorption, determine the total specific surface area of shale, including:
The total specific surface area of shale is determined according to following second formula,
Wherein, S1For the total specific surface area of shale, Vm1For total monolayer saturated extent of adsorption, N is avogadros constant,For
Nitrogen molecular equivalence the maximum cross-section area.
Further, the monolayer saturated extent of adsorption of the non-micropore surface of the described shale samples of described acquisition, including:
By shale samples being carried out low-pressure nitrogen adsorption experiment, obtain the nitrogen adsorption amount under different relative pressure；
According to the described nitrogen adsorption amount under different relative pressures, and the BET equation revised determines described shale samples
The described monolayer saturated extent of adsorption of non-micropore surface.
Further, according to the described nitrogen adsorption amount under different relative pressures, and the BET equation revised determines described
The described monolayer saturated extent of adsorption of the non-micropore surface of shale samples, including:
Non-micropore surface monolayer saturated extent of adsorption V is determined according to following 3rd formulam2,
Wherein, VadsFor nitrogen adsorption amount, Vm2For non-micropore surface monolayer saturated extent of adsorption,For constant, VmicFor micro-
The volume of filling adsorbate, P/P in hole0For relative pressure.
Further, according to the monolayer saturated extent of adsorption of described non-micropore surface, determine the non-micropore specific area of shale,
Including:
The non-micropore specific area of shale is determined according to following 4th formula,
Wherein, S2For the non-micropore specific area of shale, Vm2For non-micropore surface monolayer saturated extent of adsorption, N is Avogadro
Sieve constant,For nitrogen molecular equivalence the maximum cross-section area.
Further, described determine micropore specific area according to described total specific surface area and non-micropore specific area, including:
Micropore specific area is determined according to following 5th formula,
S3=S1-S2
Wherein, S1For the total specific surface area of shale, S2For the non-micropore specific area of shale, S3For micropore specific area.
The specific area measuring method of the shale micropore that the present invention provides, during measuring, according to the total specific surface of shale
Long-pending determine micropore specific area with non-micropore specific area, taken into full account the feature that shale micropore is grown, it is to avoid utilization warp
Relatively large deviation produced by the specific surface area of shale evaluated by allusion quotation BET equation and existing instrument, makes the micropore of shale characterize more
Accurately, the full aperture pore structure for shale characterizes and provides more objective and accurate data support.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the specific area measuring method of embodiment of the present invention shale micropore.
Detailed description of the invention
For making the purpose of the embodiment of the present invention, technical scheme and advantage clearer, below in conjunction with the embodiment of the present invention
In accompanying drawing, the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is
The a part of embodiment of the present invention rather than whole embodiments.
Based on the embodiment in the present invention, those of ordinary skill in the art are obtained under not making creative work premise
The every other embodiment obtained, broadly falls into the scope of protection of the invention.In the case of not conflicting, following embodiment and enforcement
Feature in example can be mutually combined.
It should be noted that in describing the invention, term " first ", " second " are only used for conveniently describing different portions
Part, and it is not intended that indicate or hint ordering relation, relative importance or the implicit number indicating indicated technical characteristic
Amount.Thus, define " first ", the feature of " second " can express or implicitly include at least one this feature.
Fig. 1 is the schematic flow sheet of the specific area measuring method of embodiment of the present invention shale micropore；Refer to Fig. 1, this
Embodiment provides a kind of specific area measuring method of shale micropore, including:
S100, total monolayer saturated extent of adsorption on acquisition shale samples surface；
Specifically, the nitrogen under different relative pressure can be obtained by shale samples being carried out low-pressure nitrogen adsorption experiment
Gas adsorbance.Concrete experimental technique, can similarly to the prior art, and here is omitted.
Wherein, before shale samples is carried out low-pressure nitrogen adsorption experiment, need to be ground to shale samples 40～60
Mesh (425～250 microns), is dried 12h (hour, hour) at 110 DEG C of (degree Celsius) vacuum drying ovens, sloughs the water in shale samples
Divide and volatile material.Weigh about 1g shale samples, on instrument under the conditions of 383.15K (Kelvin), vacuum (< 10mm Hg)
Degassing 10h, sloughs the material of absorption in sample further.Set the relative pressure range P/P of nitrogen adsorption experiment0Value is
0.001～0.995, test under the conditions of liquid nitrogen temperature (77.35K), and record correspondence, actual measurement under different relative pressure
Nitrogen adsorption amount Vads；At least record nitrogen adsorption amount V under three groups of relative pressuresads。
And according to the nitrogen adsorption amount under different relative pressures, and the BET equation of classics determines shale samples surface
Total monolayer saturated extent of adsorption.Such as: according to following first formula, determine total monolayer saturated extent of adsorption V on shale samples surfacem1,
Wherein, VadsFor nitrogen adsorption amount, Vm1For total monolayer saturated extent of adsorption, CBETFor constant, P/P0Relatively press for gas
Power.P/P0Span be 0.05～0.35.
It is to be understood that during shale samples is carried out low-pressure nitrogen adsorption experiment, can record and organize nitrogen more
Gas adsorbance Vads, to improve the accuracy that micropore characterizes further.
S200, determine the total specific surface area of shale according to total monolayer saturated extent of adsorption；
Specifically, determine the total specific surface area of shale according to following second formula,
Wherein, S1For the total specific surface area of shale, Vm1For total monolayer saturated extent of adsorption, N is avogadros constant,For
Nitrogen molecular equivalence the maximum cross-section area；N is 6.023 × 1023,It is 16.2 × 10-20m2。
S300, the monolayer saturated extent of adsorption of the acquisition non-micropore surface of shale samples；
Specifically, by shale samples carries out low-pressure nitrogen adsorption experiment, the nitrogen obtained under different relative pressure is inhaled
Attached amount；
Non-micropore surface monolayer saturated extent of adsorption V is determined according to following 3rd formulam2,
Wherein, VadsFor nitrogen adsorption amount, Vm2For non-micropore surface monolayer saturated extent of adsorption,For constant, VmicFor micro-
The volume of filling adsorbate, P/P in hole0For relative pressure.
In the present embodiment, by the 3rd formula it may also be determined that shale micropore volume Vmic。
S400, monolayer saturated extent of adsorption according to non-micropore surface, determine the non-micropore specific area of shale；
Specifically, according to the monolayer saturated extent of adsorption of non-micropore surface, determine the non-micropore specific area of shale, including:
The non-micropore specific area of shale is determined according to following 4th formula,
Wherein, S2For the non-micropore specific area of shale, Vm2For the monolayer saturated extent of adsorption of non-micropore surface, N is that Avobenzene adds
Moral sieve constant,For nitrogen molecular equivalence the maximum cross-section area.
S500, determine micropore specific area according to total specific surface area and non-micropore specific area.
Specifically, determine micropore specific area according to following 5th formula,
S3=S1-S2
Wherein, S1For the total specific surface area of shale, S2For the non-micropore specific area of shale, S3For micropore specific area.
The specific area measuring method of the shale micropore that the present embodiment provides, during measuring, according to shale always than table
Area and non-micropore specific area determine micropore specific area, have taken into full account the feature that shale micropore is grown, it is to avoid utilization
Relatively large deviation produced by the specific surface area of shale evaluated by classical BET equation and existing instrument, makes the micropore of shale characterize more
Adding accurately, the full aperture pore structure sign for shale provides objective and accurate data support.
The specific area measuring method of shale micropore that the present embodiment provide be exemplified below:
1) shale samples is being carried out low pressure N2Before adsorption experiment, need to be ground to sample 40～60 mesh (425～
250 μm), it is dried 12h at 110 DEG C of vacuum drying ovens, sloughs moisture therein and volatile material.Weigh about 1g sample, at instrument
Deaerate under the conditions of upper 383.15K, vacuum (< 10mm Hg) 10h, sloughs the material of absorption in sample further；
2) experimental pressure scope P/P is set0Value is 0.001～0.995, carries out low under the conditions of liquid nitrogen temperature (77.35K)
Pressure N2Adsorption experiment, records 13 data points, as shown in table 1 between relative pressure 0.05～0.35:
Low pressure N of table 1 shale samples2Adsorption experiment
| P/P0 | Vads/cm3/g | |
| 1 | 0.0501511 | 2.7455 |
| 2 | 0.0752322 | 2.9385 |
| 3 | 0.0999558 | 3.1511 |
| 4 | 0.1258040 | 3.3070 |
| 5 | 0.1502580 | 3.4563 |
| 6 | 0.1752780 | 3.6085 |
| 7 | 0.2004310 | 3.7476 |
| 8 | 0.2252730 | 3.8937 |
| 9 | 0.2503720 | 4.0389 |
| 10 | 0.2753540 | 4.1901 |
| 11 | 0.3001900 | 4.3411 |
| 12 | 0.3249060 | 4.5114 |
| 13 | 0.3493110 | 4.6571 |
3) total monolayer saturated extent of adsorption V is obtained according to classical BET equation modelm1, then utilize specific surface area formula to ask
Go out total specific surface area.Such as, 13 groups of data in table 1 are substituted into the first formula and is fitted, then can determine that shale samples surface
Total monolayer saturated extent of adsorption Vm1=3.108cm3, and then total specific surface area S of shale is determined according to the second formula1=13.55m2/
g；
4) the monolayer saturated extent of adsorption V of non-micropore surface is obtained according to the BET equation model revisedm2, then utilize and compare table
Area formula obtains non-micropore specific area.Such as, 13 groups of data in table 1 are substituted into the 3rd formula and is fitted, then can be true
Determine the monolayer saturated extent of adsorption V of the non-micropore surface of shale samplesm2=2.104cm3, and then determine the non-of shale according to the 4th formula
Micropore specific area S2=9.17m2/g；
5) deduct non-micropore specific area by total specific surface area, such as, determine that according to the 5th formula the micropore of shale compares table
Area S3=4.38m2/g。
One of ordinary skill in the art will appreciate that: all or part of step realizing above-mentioned each method embodiment can be led to
The hardware crossing programmed instruction relevant completes.Aforesaid program can be stored in a computer read/write memory medium.This journey
Sequence upon execution, performs to include the step of above-mentioned each method embodiment；And aforesaid storage medium includes: ROM, RAM, magnetic disc or
The various media that can store program code such as person's CD.
Last it is noted that various embodiments above is only in order to illustrate technical scheme, it is not intended to limit；To the greatest extent
The present invention has been described in detail by pipe with reference to foregoing embodiments, it will be understood by those within the art that: it depends on
So the technical scheme described in foregoing embodiments can be modified, or the most some or all of technical characteristic is entered
Row equivalent；And these amendments or replacement, do not make the essence of appropriate technical solution depart from various embodiments of the present invention technology
The scope of scheme.
Claims (8)
1. the specific area measuring method of a shale micropore, it is characterised in that including:
Obtain total monolayer saturated extent of adsorption on shale samples surface；
According to described total monolayer saturated extent of adsorption, determine the total specific surface area of shale；
Obtain the monolayer saturated extent of adsorption of the non-micropore surface of described shale samples；
According to the monolayer saturated extent of adsorption of described non-micropore surface, determine the non-micropore specific area of shale；
Micropore specific area is determined according to described total specific surface area and non-micropore specific area.
The specific area measuring method of shale micropore the most according to claim 1, it is characterised in that described acquisition shale sample
Total monolayer saturated extent of adsorption on product surface, including:
By shale samples being carried out low-pressure nitrogen adsorption experiment, obtain the nitrogen adsorption amount under different relative pressure；
According to the described nitrogen adsorption amount under different relative pressures, and the BET equation of classics determines described shale samples surface
Described total monolayer saturated extent of adsorption.
The specific area measuring method of shale micropore the most according to claim 2, it is characterised in that described basis not homophase
To the described nitrogen adsorption amount under pressure, and the BET equation of classics determines that described total monolayer on described shale samples surface is satisfied
And adsorbance, including:
According to following first formula, determine total monolayer saturated extent of adsorption V on described shale samples surfacem1,
Wherein, VadsFor nitrogen adsorption amount, Vm1For total monolayer saturated extent of adsorption, CBETFor constant, P/P0For gas relative pressure.
4. according to the specific area measuring method of the shale micropore described in any one of claim 1-3, it is characterised in that according to institute
State total monolayer saturated extent of adsorption, determine the total specific surface area of shale, including:
The total specific surface area of shale is determined according to following second formula,
Wherein, S1For the total specific surface area of shale, Vm1For total monolayer saturated extent of adsorption, N is avogadros constant,Divide for nitrogen
Son equivalence the maximum cross-section area.
The specific area measuring method of shale micropore the most according to claim 1, it is characterised in that the described page of described acquisition
The monolayer saturated extent of adsorption of the non-micropore surface of rock sample product, including:
By shale samples being carried out low-pressure nitrogen adsorption experiment, obtain the nitrogen adsorption amount under different relative pressure；
According to the described nitrogen adsorption amount under different relative pressures, and the BET equation revised determines that described shale samples is non-micro-
The described monolayer saturated extent of adsorption of hole surface.
The specific area measuring method of shale micropore the most according to claim 5, it is characterised in that relatively press according to difference
Described nitrogen adsorption amount under power, and revise BET equation determine the non-micropore surface of described shale samples described monolayer satisfy
And adsorbance, including:
Non-micropore surface monolayer saturated extent of adsorption V is determined according to following 3rd formulam2,
Wherein, VadsFor nitrogen adsorption amount, Vm2For non-micropore surface monolayer saturated extent of adsorption,For constant, VmicFor in micropore
The volume of filling adsorbate, P/P0For relative pressure.
7. according to the specific area measuring method of the shale micropore described in claim 1,5 or 6, it is characterised in that according to described
The monolayer saturated extent of adsorption of non-micropore surface, determine the non-micropore specific area of shale, including:
The non-micropore specific area of shale is determined according to following 4th formula,
Wherein, S2For the non-micropore specific area of shale, Vm2For non-micropore surface monolayer saturated extent of adsorption, N is that Avogadro sieve is normal
Number,For nitrogen molecular equivalence the maximum cross-section area.
The specific area measuring method of shale micropore the most according to claim 1, it is characterised in that described according to described always
Specific surface area and non-micropore specific area determine micropore specific area, including:
Micropore specific area is determined according to following 5th formula,
S3=S1-S2
Wherein, S1For the total specific surface area of shale, S2For the non-micropore specific area of shale, S3For micropore specific area.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107991215A (en) * | 2017-11-23 | 2018-05-04 | 中南大学 | The natural aperture of the hypotonic rock sample of large scale and the test method of specific surface area |
| CN109269449A (en) * | 2018-10-12 | 2019-01-25 | 重庆大学 | Stockpile specific surface area test method |
| CN114136855A (en) * | 2020-09-03 | 2022-03-04 | 中国石油化工股份有限公司 | Method for judging shale pore connectivity, storage medium and computer equipment |
| CN114166723A (en) * | 2021-12-21 | 2022-03-11 | 中国石油大学(华东) | Method and system for predicting quantum physical adsorption behavior of gas in nano porous medium |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107991215A (en) * | 2017-11-23 | 2018-05-04 | 中南大学 | The natural aperture of the hypotonic rock sample of large scale and the test method of specific surface area |
| CN109269449A (en) * | 2018-10-12 | 2019-01-25 | 重庆大学 | Stockpile specific surface area test method |
| CN109269449B (en) * | 2018-10-12 | 2020-07-31 | 重庆大学 | Method for testing specific surface area of rockfill |
| CN114136855A (en) * | 2020-09-03 | 2022-03-04 | 中国石油化工股份有限公司 | Method for judging shale pore connectivity, storage medium and computer equipment |
| CN114136855B (en) * | 2020-09-03 | 2024-05-28 | 中国石油化工股份有限公司 | Method for judging shale pore connectivity, storage medium and computer equipment |
| CN114166723A (en) * | 2021-12-21 | 2022-03-11 | 中国石油大学(华东) | Method and system for predicting quantum physical adsorption behavior of gas in nano porous medium |
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Application publication date: 20170111 |