CN105043957A - Method for determining pore structure through classifying isothermal adsorption curve of mud shale - Google Patents

Method for determining pore structure through classifying isothermal adsorption curve of mud shale Download PDF

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CN105043957A
CN105043957A CN201510392207.2A CN201510392207A CN105043957A CN 105043957 A CN105043957 A CN 105043957A CN 201510392207 A CN201510392207 A CN 201510392207A CN 105043957 A CN105043957 A CN 105043957A
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mud shale
pore
sample
curve
adsorption
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CN105043957B (en
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闫长辉
李鹏
田园媛
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Chengdu Univeristy of Technology
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Abstract

The invention relates to the field of shale hydrocarbon reservoir exploration, and discloses a method for determining the pore structure through classifying the isothermal adsorption curve of mud shale. The method comprises the following steps: 1, collecting the bedrock standard column sample of mud shale; 2, crushing the bedrock standard column sample obtained in step 1, carrying out isothermal adsorption test, and drafting an isothermal adsorption curve; 3, sorting the pore form, the pore size and the pore throat to obtain a mud shale isothermal adsorption curve standard map; and 4, comparing the isothermal adsorption curve of the detected sample with the mud shale isothermal adsorption curve standard map to obtain the pore structure of the detected sample. The method for determining the pore structure through classifying the isothermal adsorption curve of mud shale realizes division of all types of isothermal adsorption curves of mud shale through the isothermal adsorption curve standard map standard map, and displays the difference of different isothermal adsorption curves; and the pore structure of the mud shale sample can be determined through the isothermal adsorption curve of the mud shale sample, and can be further associated with a shale gas exploitation apparatus.

Description

The method of pore texture is judged by the classification of mud shale adsorption isothermal curve
Technical field
The present invention relates to oil shale fuel gas reservoir exploration development field, particularly judged the method for pore texture by the classification of mud shale adsorption isothermal curve.
Background technology
Pore throat characteristic analysis is one of important content of shale evaluating reservoir., there is a large amount of micropore in mud shale Compacted rock, conventional hole research method has limitation in mud shale pore character describes in reservoir.The method adopting mercury intrusion method to combine with absorption method in the research of shale reservoir pore character more.Mud shale due to different shale samples pore character different, cause its absorption property variant, affect the form of its adsorption isothermal curve.To the classification that mud shale adsorption isothermal curve form is carried out, the pore structure characteristic of mud shale can be embodied.
And prior art is to the classification spininess effects on surface uniform properties material of adsorption isothermal curve form, Main Basis adsorption curve form or classify in conjunction with hysteresis loop form.But as special adsorbent, mud shale complicated, comprises multiple clay mineral, quartz, feldspar, landwaste and kerogen etc.Because the absorption property of different components differs, the adsorpting characteristic of mud shale is different from the uniform material of surface nature.Meanwhile, in mud shale, there is a large amount of micropore and mesoporous, adsorb potential energy distribution in hole and there is singularity, affect the form of its adsorption curve and hysteresis loop.
To the adsorption isothermal curve that the data of mud shale sample are made in experimentation, adsorption isothermal curve criteria for classification of the prior art is used to have very strong limitation to its classification.
Urgently there is a kind of method of specially mud shale adsorption curve form being classified.
Summary of the invention
The method being judged pore texture by the classification of mud shale adsorption isothermal curve disclosed by the invention, is solved prior art and cannot highlight otherness between different adsorption isothermal curve, and even effectively cannot judge the technical matters of mud shale pore texture.
Technical scheme of the present invention is achieved in that and judges to comprise the method for pore texture by the classification of mud shale adsorption isothermal curve: a, take the basement rock standard column sample of mud shale; B, the basement rock standard column sample in step a carried out to broken sample, isothermal adsorption test, obtain isothermal adsorption pressure, the adsorbance of basement rock standard sample post, draw adsorption isothermal curve and aperture frequency histogram; C, by pore morpholohy, pore size and pore throat sorting three factors, adsorption isothermal curve to be classified, obtain mud shale adsorption isothermal curve standard drawing, and the adsorption isothermal curve of basement rock standard column sample is described; The sample of e, mud shale, by broken sample, isothermal adsorption test, draws sample adsorption isothermal curve; By contrast sample adsorption isothermal curve and mud shale adsorption isothermal curve standard drawing, obtain the pore texture of sample, i.e. the form of sample hole, size and pore throat.
Preferably, also comprise steps d between described step c and e, by adsorption isothermal curve standard drawing in the frequency histogram verification step c of aperture to the analysis of pore throat sorting.
Further, the basement rock on what the basement rock of mud shale described in step a was concrete is mud shale drill cores and neighbouring analogous outcrop; Described standard column sample is the mud shale post sample of diameter 2.5cm, length 5cm.
Further, the isothermal adsorption test described in step b particularly under isothermal conditions, take liquid nitrogen as adsorbate, being instrument with full-automatic specific surface area and lacunarity analysis instrument, isothermal adsorption is tested.
Further, pore morpholohy described in step c is plate shaped, wedge shape and cylindrical; Described pore size is aperture, mesopore and macropore; Described pore throat sorting according to the degree of uniformity of throat for poor, in become reconciled.
Further, when described pore morpholohy is by cylindrical-wedge shape-plate shaped change, absorption-desorption curve changes to being parallel to transverse axis gradually by being parallel to the longitudinal axis, and hysteresis loop is larger to flat, transversely span big change by steep, longitudinal upper span.
Further, the descending impact on hysteresis loop form of described hole be hysteresis loop starting point to low-pressure area translation and hysteresis loop area reduce gradually, until disappear.
Further, described pore throat degree of sorting on the impact of desorption curve is: good, desorption curve declines fast; Difference, desorption curve declines in mild.
Further, described pore texture is corresponding with the quarrying apparatus of shale gas.
The method being judged pore texture by the classification of mud shale adsorption isothermal curve disclosed in this invention, by pore morpholohy, pore size and pore throat sorting, the adsorption isothermal curve of the basement rock standard sample post of mud shale is classified, i.e. adsorption isothermal curve standard drawing, achieve the division of whole mud shale sample adsorption isothermal curve type, described in curve, type is various, can embody the otherness of different adsorption isothermal curve; By can judge the gap structure of mud shale sample to mud shale sample adsorption isothermal curve, the development device of association shale gas further, while raising recovery ratio, avoids the improper high cost caused of recovery scheme; Technical scheme disclosed in this invention also effectively can promote the deduction of shale reservoir feature, provides new theoretical foundation for reserves calculate.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1: mud shale pore morpholohy is illustrated on the impact of adsorption isothermal curve;
Fig. 2: mud shale pore size affects schematic diagram to adsorption isothermal curve;
Fig. 3: the sorting of mud shale pore throat affects schematic diagram to adsorption isothermal curve;
Fig. 4: mud shale adsorption isothermal curve classification schematic diagram;
Fig. 5: cylindricality hole mud shale adsorption isothermal curve is classified;
Fig. 6: wedge shape hole mud shale adsorption isothermal curve is classified;
Fig. 7: plate shaped hole mud shale adsorption isothermal curve classification;
Fig. 8: Sichuan Basin mud shale sample adsorption isothermal curve;
The frequency histogram of sample in Fig. 9: Fig. 8;
Figure 10: Sichuan Basin mud shale sample adsorption isothermal curve;
The frequency histogram of sample in Figure 11: Figure 10.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Disclosed by the inventionly judge to comprise the method for pore texture by the classification of mud shale adsorption isothermal curve: a, take the basement rock standard column sample of mud shale; B, the basement rock standard column sample in step a carried out to broken sample, isothermal adsorption test, obtain isothermal adsorption pressure, the adsorbance of basement rock standard sample post, draw adsorption isothermal curve and aperture frequency histogram; C, by pore morpholohy, pore size and pore throat sorting three factors, adsorption isothermal curve to be classified, obtain mud shale adsorption isothermal curve standard drawing, and the adsorption isothermal curve of basement rock standard column sample is described; The sample of e, mud shale, by broken sample, isothermal adsorption test, draws sample adsorption isothermal curve; By contrast sample adsorption isothermal curve and mud shale adsorption isothermal curve standard drawing, obtain the pore texture of sample, i.e. the form of sample hole, size and pore throat.
Preferably, also comprise steps d between described step c and e, by adsorption isothermal curve standard drawing in the frequency histogram verification step c of aperture to the analysis of pore throat sorting.
Further, the basement rock on what the basement rock of mud shale described in step a was concrete is mud shale drill cores and neighbouring analogous outcrop; Described standard column sample is the mud shale post sample of diameter 2.5cm, length 5cm.Further, the isothermal adsorption test described in step b particularly under isothermal conditions, take liquid nitrogen as adsorbate, being instrument with full-automatic specific surface area and lacunarity analysis instrument, isothermal adsorption is tested.Further, pore morpholohy described in step c is plate shaped, wedge shape and cylindrical; Described pore size is aperture, mesopore and macropore; Described pore throat sorting according to the degree of uniformity of throat for poor, in become reconciled.
Further, as Fig. 1 mud shale pore morpholohy affects shown in schematic diagram on adsorption isothermal curve, when described pore morpholohy is by cylindrical-wedge shape-plate shaped change, absorption-desorption curve changes to being parallel to transverse axis gradually by being parallel to the longitudinal axis, and hysteresis loop is larger to flat, transversely span big change by steep, longitudinal upper span.Further, as Fig. 2 mud shale pore size affects shown in schematic diagram on adsorption isothermal curve, the descending impact on hysteresis loop form of described hole be hysteresis loop starting point to low-pressure area translation and hysteresis loop area reduce gradually, until disappear.Further, as the sorting of Fig. 3 mud shale pore throat affects shown in schematic diagram on adsorption isothermal curve, described pore throat degree of sorting on the impact of desorption curve is: good, desorption curve declines fast; Difference, desorption curve declines in mild.
In summary, mud shale pore morpholohy affects hysteresis loop width and ratio highly; Pore size affects the width of hysteresis loop and the relative pressure of starting point; Pore throat sorting affects desorption curve form, therefore selects this three aspect as mud shale adsorption isothermal curve classification foundation.
Particularly, in the pore morpholohy of mud shale, the adsorption isothermal curve of cylindrical pore, when reaching certain relative pressure, in all holes of radius corresponding to this pressure, capillary condensation occurs, hole is full of rapidly, adsorbance sharply increases, in like manner during desorb when reaching the desorption pressures corresponding to certain pore radius, the gas in these holes is discharged fast, so the longitudinal ratio of the adsorption isothermal curve of cylindrical pore and hysteresis loop parallel with desorb curve approximation is maximum; In the adsorption isothermal curve of plate shaped hole, the feature of hysteresis loop is that adsorption curve sharply rises when pressure is bordering on saturated vapor pressure, and desorption curve declines rapidly when medium relative pressure, causes hysteresis loop form to be flat, and longitudinal ratio is minimum; Hysteresis loop in the adsorption isothermal curve of wedge shape hole is mild, longitudinal ratio between cylindrical and plate shaped between.
Particularly, in the pore size of mud shale, the mud shale adsorption isothermal curve hysteresis loop closed area of aperture and grid scale little, and due to pressure condition required when gas condenses in fine porosity lower, therefore hysteresis loop starting point pressure is lower; In the mud shale adsorption isothermal curve of macropore, hysteresis loop closed area is large, and hysteresis loop starting point pressure is higher; The mud shale adsorption isothermal curve hysteresis loop closed area of mesopore and starting point pressure all medium, between fine porosity and macropore mud shale.
Particularly, divide and choose, nongraded mud shale at the pore throat of mud shale, its desorption curve is mild, without obvious adsorbance rapid drawdown spot pressure; Divide the mud shale chosen, its desorption curve has adsorbance rapid drawdown to show, but adsorbance reduction amplitude is little; Well-graded mud shale, in its desorption curve, adsorbance has obvious rapid drawdown, and adsorbance reduces amplitude comparatively greatly, and the desorption of reflection condensation product concentrates in less pressure limit.
In summary, actual mud shale sample is by pore morpholohy, pore size and pore throat sorting three kinds of factors.Due to effects such as deposition, diagenesis, mud shale sample hole shows abundant diversity.Therefore three kinds of factors are combined, form curve type in 27 altogether as shown in Fig. 4 mud shale adsorption isothermal curve classification schematic diagram, wherein cylindrical pore part, C1-C3, C4-C5, C7-C9, be namely counterclockwise respectively in sorting difference, sorting and good sorting.Different curve types represents different pore morpholohies, pore size and throat sorting feature.As Fig. 5,6,7 divides the three class plates made from pore morpholohy, particularly: the classification of cylindricality hole mud shale adsorption isothermal curve, the classification of wedge shape hole mud shale adsorption isothermal curve, the classification of plate shaped hole mud shale adsorption isothermal curve, every class plate contains the adsorption isothermal curve type of different aperture size and throat sorting in this kind of pore morpholohy.
And the pore texture of mud shale is judged by the classification of mud shale adsorption isothermal curve, the adsorption isothermal curve form of 23 actual mud shale samples and hysteresis loop form are classified: pore morpholohy has wedge shape hole peace plate shape hole, pore size is based on fine porosity, become reconciled two etc. during degree of sorting has, and the samples such as good sorting are more.As can be seen from classification results, adopt new criteria for classification to achieve division to whole mud shale sample adsorption isothermal curve type, and belonging to curve, type is various, embodies the otherness between different adsorption isothermal curve.
Further, described pore texture is corresponding with the quarrying apparatus of shale gas.Application mud shale adsorption isothermal curve sorting technique, namely the adsorption isothermal curve and the mud shale adsorption isothermal curve standard drawing that pass through mud shale sample contrast, tentatively can judge the pore structure characteristic of mud shale sample, i.e. pore morpholohy, pore size and pore throat sorting.According to the reservoir characteristic of the pore structure characteristic deducibility mud shale of mud shale sample, realize effectively being familiar with shale reservoir; Simultaneously when carrying out reserves and calculating, provide a new theoretical foundation.And then more reasonably development plan can be chosen, and be convenient to the exploitation of shale gas, both can the improper high cost brought of economy, also reach the effect improving recovery ratio simultaneously.
Specific embodiment 1: in composition graphs 8 Sichuan Basin mud shale sample adsorption isothermal curve and Fig. 9 Fig. 8 sample frequency histogram shown in, D11 sample, namely the result that mud shale sample in the Sichuan Basin is classified according to mud shale adsorption isothermal curve sorting technique is W8 type, is the medium wedge shape aperture of sorting.Shared by the hole can finding out D11 sample 10-20nm aperture from the histogram of aperture, volume of voids is maximum, tentatively can infer that sample is based on aperture; Sample aperture peak is obvious, but shared by aperture, peak value place, the percentage of cumulative volume is not high, only has about 16%, and peak value right-hand member aperture frequency declines successively and tends to be steady to about 6%, can find out point to choose.
Specific embodiment 2: in conjunction with sample in Figure 10 Sichuan Basin mud shale sample adsorption isothermal curve and Figure 11 Figure 10 frequency histogram shown in, the classification results of D10 sample and Sichuan Basin mud shale sample is W9 type, is well-graded wedge shape aperture.Shared by the hole that we can find out this sample 18-24nm aperture from the histogram of aperture, cumulative volume is maximum, and judgement sample is based on aperture; Sample peak value is obvious, and the percentage that aperture, peak value place accounts for cumulative volume is higher, and greatly about about 27%, on the right side of peak value, frequency is steady, greatly about about 5%, can find out that sorting is fine.
The method being judged pore texture by the classification of mud shale adsorption isothermal curve disclosed in this invention, by pore morpholohy, pore size and pore throat sorting, the adsorption isothermal curve of the basement rock standard sample post of mud shale is classified, i.e. adsorption isothermal curve standard drawing, achieve the division of whole mud shale sample adsorption isothermal curve type, described in curve, type is various, can embody the otherness of different adsorption isothermal curve; By can judge the gap structure of mud shale sample to mud shale sample adsorption isothermal curve, the development device of association shale gas further, while raising recovery ratio, avoids the improper high cost caused of recovery scheme; Technical scheme disclosed in this invention also effectively can promote the deduction of shale reservoir feature, provides new theoretical foundation for reserves calculate.
Certainly; when not deviating from the present invention's spirit and essence thereof; those of ordinary skill in the art should make various corresponding change and distortion according to the present invention, but these change accordingly and are out of shape the protection domain that all should belong to the claim appended by the present invention.

Claims (9)

1. judged the method for pore texture by the classification of mud shale adsorption isothermal curve, it is characterized in that, comprising:
A, take the basement rock standard column sample of mud shale;
B, the basement rock standard column sample in step a carried out to broken sample, isothermal adsorption test, obtain isothermal adsorption pressure, the adsorbance of basement rock standard sample post, draw adsorption isothermal curve and aperture frequency histogram;
C, by pore morpholohy, pore size and pore throat sorting three factors, adsorption isothermal curve to be classified, obtain mud shale adsorption isothermal curve standard drawing, and the adsorption isothermal curve of basement rock standard column sample is described;
The sample of e, mud shale, by broken sample, isothermal adsorption test, draws sample adsorption isothermal curve; By contrast sample adsorption isothermal curve and mud shale adsorption isothermal curve standard drawing, obtain the pore texture of sample, i.e. the form of sample hole, size and pore throat.
2. according to claim 1ly judge to it is characterized in that the method for pore texture by the classification of mud shale adsorption isothermal curve: also comprise steps d between described step c and e, by adsorption isothermal curve standard drawing in the frequency histogram verification step c of aperture to the analysis of pore throat sorting.
3. according to claim 2ly judge to it is characterized in that the method for pore texture by the classification of mud shale adsorption isothermal curve: the basement rock on what the basement rock of mud shale described in step a was concrete is mud shale drill cores and neighbouring analogous outcrop; Described standard column sample is the mud shale post sample of diameter 2.5cm, length 5cm.
4. judge to it is characterized in that the method for pore texture by the classification of mud shale adsorption isothermal curve according to Claims 2 or 3: the isothermal adsorption described in step b is tested particularly under isothermal conditions, take liquid nitrogen as adsorbate, being instrument with full-automatic specific surface area and lacunarity analysis instrument, isothermal adsorption is tested.
5. according to claim 4ly judge to it is characterized in that the method for pore texture by the classification of mud shale adsorption isothermal curve: pore morpholohy described in step c is plate shaped, wedge shape and cylindrical; Described pore size is aperture, mesopore and macropore; Described pore throat sorting according to the degree of uniformity of throat for poor, in become reconciled.
6. the method being judged pore texture by the classification of mud shale adsorption isothermal curve according to claim 5, it is characterized in that: when described pore morpholohy is by cylindrical-wedge shape-plate shaped change, absorption-desorption curve changes to being parallel to transverse axis gradually by being parallel to the longitudinal axis, and hysteresis loop is larger to flat, transversely span big change by steep, longitudinal upper span.
7. the method being judged pore texture by the classification of mud shale adsorption isothermal curve according to claim 5, it is characterized in that: the descending impact on hysteresis loop form of described hole be hysteresis loop starting point to low-pressure area translation and hysteresis loop area reduce gradually, until disappear.
8. the method being judged pore texture by the classification of mud shale adsorption isothermal curve according to claim 5, be is characterized in that: described pore throat degree of sorting on the impact of desorption curve is: good, desorption curve declines fast; Difference, desorption curve declines in mild.
9., according to the method being judged pore texture by the classification of mud shale adsorption isothermal curve in claim 6-8 described in any one, it is characterized in that: described pore texture is corresponding with the quarrying apparatus of shale gas.
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CN106526079A (en) * 2016-10-27 2017-03-22 中国石油大学(北京) Method used for studying tight sandstone pore-throat structure dynamic change
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CN106885755A (en) * 2017-01-10 2017-06-23 中国矿业大学 A kind of underground coal mine quickly determines the method and apparatus of coal-bed gas parameter
CN107194104A (en) * 2017-06-07 2017-09-22 成都理工大学 A kind of method that use log calculates inanimate matter porosity, total porosity and component in shale reservoir
CN107194104B (en) * 2017-06-07 2019-08-09 成都理工大学 The method for calculating inanimate matter porosity in shale reservoir
CN109540764A (en) * 2018-12-13 2019-03-29 中国石油大学(华东) A method of evaluation shale reservoir organic matter, clay and the contributed hole preservation ADSORPTION STATE methane thickness and density of other mineral
WO2021129315A1 (en) * 2019-12-26 2021-07-01 中国科学院广州能源研究所 Method for calculating pore distribution of marine sediment layer
WO2021203611A1 (en) * 2020-04-10 2021-10-14 中国地质大学(北京) Method for determining change in nanoscale pore structure, and use thereof
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