CN106501151A - A kind of shale aperture measurement device and method based on imbibition and ion diffusion property - Google Patents

A kind of shale aperture measurement device and method based on imbibition and ion diffusion property Download PDF

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Publication number
CN106501151A
CN106501151A CN201610937573.6A CN201610937573A CN106501151A CN 106501151 A CN106501151 A CN 106501151A CN 201610937573 A CN201610937573 A CN 201610937573A CN 106501151 A CN106501151 A CN 106501151A
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imbibition
water
shale
flask
jacking
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CN106501151B (en
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杨柳
张旭辉
鲁晓兵
李鹏
罗大双
刘庆杰
张祖波
葛洪魁
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Institute of Mechanics of CAS
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
    • G01N15/08Investigating permeability, pore-volume, or surface area of porous materials
    • G01N15/088Investigating volume, surface area, size or distribution of pores; Porosimetry
    • G01N15/0893Investigating volume, surface area, size or distribution of pores; Porosimetry by measuring weight or volume of sorbed fluid, e.g. B.E.T. method

Abstract

The invention discloses a kind of shale aperture measurement device and method based on imbibition and ion diffusion property, including:High accuracy analysis balance (1), support (2), flask (3), fishing line (4), magnetic stirring apparatus (5), jacking system (6), conductivity meter (7), climatic chamber (8).The present invention is by way of experiment is measured, make full use of the distinctive high capillary force imbibition of shale and strong ion diffusion property, devise high-precision shale imbibition and ion diffusion sync detection device, the average pore size evaluation method suitable for shale is proposed, the scientific and precision of shale inside diameter measurement is further increased;The features such as present invention has low little, testing cost simple to operate, affected by environment, reliable results.

Description

A kind of shale aperture measurement device and method based on imbibition and ion diffusion property
Technical field
The invention belongs to shale gas development technique field, more particularly to a kind of based on imbibition and the shale of ion diffusion property Aperture measurement device and method.
Background technology
South China marine facies shale gas aboundresources, used as important alternative energy source, which is commercialized exploitation to ensureing China Energy security, the domestic energy cost of reduction and environmental pressure have great importance.Shale gas are typical limit petroleum resourceses, It is in particular in that reservoir porosity and permeability are extremely low, hole is shouted in micro-nano rank, complex pore structure.Aperture is used as evaluation The important parameter of shale physical property characteristic is often difficult to accurately measurement.At present, pressure mercury, gas absorption and nuclear magnetic resonance etc. are relied primarily on Means are determining the pore size of shale, but often difference is larger in several method of testings aperture for obtaining, while testing cost Higher.
Content of the invention
The purpose of the present invention is:A kind of shale aperture measurement device and side based on imbibition and ion diffusion property is provided Method, further improves the certainty of measurement in shale aperture, reduces measurement cost, and the determination for shale physical property characteristic parameter provides science Foundation.
The technical scheme is that:A kind of shale aperture measurement device based on imbibition and ion diffusion property, it are wrapped Include:High accuracy analysis balance, support, flask, fishing line, magnetic stirring apparatus, jacking system, conductivity meter, climatic chamber;
The high accuracy analysis day is flat on above the support, is become for measuring the quality before and after shale samples absorb water Change;
Described is placed in the climatic chamber, for carrying the high accuracy analysis balance;In the middle of the support Aperture is provided with, for the shale samples being suspended on the high accuracy analysis balance are suspended vertically the internal stent;
The flask is placed in the magnetic stirring apparatus upper surface, for containing distilled water, hangs down in the high accuracy analysis Shale samples on balance can come in and go out from the flask oral area when rising or falling;
The fishing line is used for hanging down in the high accuracy balance shale samples;
The magnetic stirring apparatus is placed in the jacking system upper surface, for stirring the distilled water in the flask;
The jacking system is used for lifting the flask, realizes shale samples submergence or leaves distillation in the flask Water;
The conductivity meter hangs down in the flask in distilled water, and the ion for determining distilled water in the flask is dense Degree;
The climatic chamber is used for making the high accuracy analysis balance, the support, the flask, the fishing line, institute Magnetic stirring apparatus, the jacking system, the conductivity meter are stated in constant-temperature constant-humidity environment.
Further, the precision of the high accuracy analysis balance is 0.0001g.
Further, the flask is 250ml flasks.
Further, the fishing line is No. 0.6 fishing line.
Further, the conductivity meter precision is 0.1 μ S/cm.
A kind of shale bore diameter measuring method based on imbibition and ion diffusion property, comprises the following steps:
A. cylindrical shale samples are extracted, sectional area A is calculatedc, with epoxy resin by cylindrical shale samples cylinder sealing, It is placed in drying baker and dries, until cylindrical shale samples quality no longer changes;
B. high accuracy analysis day is flat on support, using fishing line by drying after cylindrical shale samples hang on height On precision analysis balance, high accuracy analysis balance reading M0 is recorded;
C. jacking system is placed in below support, flask is placed on magnetic stirring apparatus, and magnetic stirring apparatus is placed in jacking system On;
D. volume is added into flask for the distilled water of V, and determines electrical conductivity G0 in water;
E. magnetic stirring apparatus is opened, jacking system is increased, cylindrical shale samples is immersed in 20 seconds in distilled water;
F. decline jacking system so that cylindrical shale samples are completely exposed the water surface, recording balance reading M1, and determine Electrical conductivity G1 in water;
Theoretical, unit of account area water absorption V according to air water two phase fluid flowimbCause with the diffusion of imbibition process intermediate ion Electrical conductivity of solution G relations over time;The physical parameter x being directed to, kw,Pc,Swf,Swi, μw, B, C, n are not needed It is measured, B and C is obtained by the test curve in analysis later stage, and other parameters are disappeared by the means of the mathematic(al) manipulation in later stage Fall the impact of these parameters;
According to Handy imbibitions models, the position x of water phase imbibition leading edge with the variation relation of imbibition time t is:
K in formulawFor water penetration rate mD, PcFor capillary force Pa,For porosity, SwfFor leading edge water saturation, SwiFor first Beginning water saturation;
As cylindrical shale samples are fine and close, therefore leading edge water saturation is higher, and cylindrical shale samples have passed through Drying and processing, then difference between the two be approximately equal to 1;
During cylindrical shale samples imbibition, the volume change over time of unit area suction water is turned to:
In formula:Hold-ups g/cm of the B for unit area water2, μwViscosity for water
The electrical conductivity of solution change that then ion diffusion causes is turned to:
In formula:C is unit area ion adhesion amount mg/cm2, n is capillary number;
G. jacking system is made to increase again so that cylindrical shale samples are totally submerged 20 seconds in distilled water;
H. repeat step F and step G, obtain the change of M~M0 and G~G0 t over time, you can obtain water suction volume VimbChange with electrical conductivity of solution G t over time;
I. the water suction volume of drafting per surface area, electrical conductivity are with t0.5Change curve, ask for respectively the slope of curve, Imbibition speed A and ion diffusion rates D, the A and D of acquisition are calculated and can be obtained the ratio of A/D;
According to unit area water absorption VimbThe electrical conductivity of solution G caused with the diffusion of imbibition process intermediate ion becomes over time The theoretical formula of change, calculates the ratio that imbibition speed A and ion spread D, and process is as follows:
Imbibition speed with the ratio of ion diffusion rates is:
J. conductance profile extended line is C/V with the intercept of the longitudinal axis, obtains average pore size r of shale.
The present invention makes full use of the distinctive high capillary force imbibition of shale and the diffusion of strong ion by way of experiment is measured Characteristic, devises high-precision shale imbibition and ion diffusion sync detection device, and proposes the average hole suitable for shale Footpath evaluation method, can be used as effective supplement of conventional aperture means of testing.The present invention little, test simple to operate, affected by environment Low cost, reliable results, the also analysis for shale physical property characteristic provide a kind of brand-new thinking.
Description of the drawings
Fig. 1 is apparatus of the present invention schematic diagram;
Fig. 2 is the inventive method flow chart.
1-- high accuracy analysis balances, 2-- supports, 3-- sesame seed cakes, 4-- fishing lines, 5-- magnetic stirring apparatus, 6-- jacking systems, 7-- conductivity meters, 8-- climatic chambers
Specific embodiment
Embodiment 1:Referring to Fig. 1, a kind of shale aperture measurement device based on imbibition and ion diffusion property, its feature exist In it includes:High accuracy analysis balance 1, support 2, flask 3, fishing line 4, magnetic stirring apparatus 5, jacking system 6, conductivity meter 7, Climatic chamber 8;
The high accuracy analysis balance 1 is placed in above the support 2, is become for measuring the quality before and after shale samples absorb water Change;The precision of the high accuracy analysis balance 1 is 0.0001g;
The support 2 is placed in the climatic chamber 8, for carrying the high accuracy analysis balance 1;The support 2 Centre is provided with aperture, for the shale samples being suspended on the high accuracy analysis balance 1 are suspended vertically in the support 2 Portion;
The flask 3 is placed in 5 upper surface of the magnetic stirring apparatus, for containing distilled water, hangs down in the high accuracy point Shale samples on analysis balance 1 can come in and go out from 3 oral area of the flask when rising or falling;The flask 3 is 250ml flasks;
The fishing line 4 is used for hanging down in the high accuracy balance 1 shale samples;The fishing line 4 is No. 0.6 fishing line
The magnetic stirring apparatus 5 is placed in 6 upper surface of the jacking system, for stirring the distilled water in the flask 3;
The jacking system 6 is used for lifting the flask 3, realizes shale samples submergence or leaves steaming in the flask 3 Distilled water;
The conductivity meter 7 hangs down in the flask 3 in distilled water, for determine distilled water in the flask 3 from Sub- concentration;7 precision of the conductivity meter is 0.1 μ S/cm;
The climatic chamber 8 is used for making the high accuracy analysis balance 1, the support 2, the flask 3, the fishing line 4th, the magnetic stirring apparatus 5, the jacking system 6, the conductivity meter 7 are in constant-temperature constant-humidity environment.
Embodiment 2:Referring to Fig. 2, a kind of shale bore diameter measuring method based on imbibition and ion diffusion property, including following Step:
A. cylindrical shale samples are extracted, sectional area A is calculatedc, with epoxy resin by cylindrical shale samples cylinder sealing, It is placed in drying baker and dries, until cylindrical shale samples quality no longer changes;
B. high accuracy analysis day is flat on support, using fishing line by drying after cylindrical shale samples hang on height On precision analysis balance, high accuracy analysis balance reading M0 is recorded;
C. jacking system is placed in below support, flask is placed on magnetic stirring apparatus, and magnetic stirring apparatus is placed in jacking system On;
D. volume is added into flask for the distilled water of V, and determines electrical conductivity G0 in water;
E. magnetic stirring apparatus is opened, jacking system is increased, cylindrical shale samples is immersed in 20 seconds in distilled water;
F. decline jacking system so that cylindrical shale samples are completely exposed the water surface, recording balance reading M1, and determine Electrical conductivity G1 in water;
Theoretical, unit of account area water absorption V according to air water two phase fluid flowimbCause with the diffusion of imbibition process intermediate ion Electrical conductivity of solution G relations over time;The physical parameter x being directed to, kw,Pc,Swf,Swi, μw, B, C, n are not required to It is measured, B and C is obtained by the test curve in analysis later stage, means of the other parameters by the mathematic(al) manipulation in later stage The impact of these parameters that disappear;
According to Handy imbibitions models, the position x of water phase imbibition leading edge with the variation relation of imbibition time t is:
K in formulawFor water penetration rate mD, PcFor capillary force Pa,For porosity, SwfFor leading edge water saturation, SwiFor first Beginning water saturation;
As cylindrical shale samples are fine and close, therefore leading edge water saturation is higher, and cylindrical shale samples have passed through Drying and processing, then difference between the two be approximately equal to 1;
During cylindrical shale samples imbibition, the volume change over time of unit area suction water is turned to:
In formula:Hold-ups g/cm of the B for unit area water2, μwViscosity for water
The electrical conductivity of solution change that then ion diffusion causes is turned to:
In formula:C is unit area ion adhesion amount mg/cm2, n is capillary number;
G. jacking system is made to increase again so that cylindrical shale samples are totally submerged 20 seconds in distilled water;
H. repeat step F and step G, obtain the change of M~M0 and G~G0 t over time, you can obtain water suction volume VimbChange with electrical conductivity of solution G t over time;
I. the water suction volume of drafting per surface area, electrical conductivity are with t0.5Change curve, ask for respectively the slope of curve, Imbibition speed A and ion diffusion rates D, the A and D of acquisition are calculated and can be obtained the ratio of A/D;
According to unit area water absorption VimbThe electrical conductivity of solution G caused with the diffusion of imbibition process intermediate ion becomes over time The theoretical formula of change, calculates the ratio that imbibition speed A and ion spread D, and process is as follows:
Imbibition speed with the ratio of ion diffusion rates is:
J. conductance profile extended line is C/V with the intercept of the longitudinal axis, obtains average pore size r of shale.

Claims (6)

1. a kind of shale aperture measurement device based on imbibition and ion diffusion property, it is characterised in that it includes:High accuracy point Analysis balance (1), support (2), flask (3), fishing line (4), magnetic stirring apparatus (5), jacking system (6), conductivity meter (7), constant temperature Constant humidity cabinet (8);
High accuracy analysis balance (1) is placed in above the support (2), is become for measuring the quality before and after shale samples absorb water Change;
Support (2) are placed in the climatic chamber (8), for carrying high accuracy analysis balance (1);The support (2) aperture is provided with the middle of, for the shale samples being suspended on high accuracy analysis balance (1) are suspended vertically described Frame (2) is internal;
Flask (3) are placed in the magnetic stirring apparatus (5) upper surface, for containing distilled water, hang down in the high accuracy point Shale samples in analysis balance (1) can come in and go out from the flask (3) oral area when rising or falling;
Described fishing line (4) are used for hanging down in the high accuracy balance (1) shale samples;
Magnetic stirring apparatus (5) are placed in the jacking system (6) upper surface, for stirring the distilled water in the flask (3);
Described jacking system (6) are used for lifting the flask (3), realize shale samples submergence or leave in the flask (3) Distilled water;
Conductivity meter (7) hang down in the interior distilled water of the flask (3), for determining the interior distilled water of the flask (3) Ion concentration;
Described climatic chamber (8) are used for making high accuracy analysis balance (1), the support (2), the flask (3), described Fishing line (4), the magnetic stirring apparatus (5), the jacking system (6), the conductivity meter (7) are in constant-temperature constant-humidity environment.
2. a kind of shale aperture measurement device based on imbibition and ion diffusion property as claimed in claim 1, its feature exist In:The precision of high accuracy analysis balance (1) is 0.0001g.
3. a kind of shale aperture measurement device based on imbibition and ion diffusion property as claimed in claim 1, its feature exist In:Described flask (3) are 250ml flasks.
4. a kind of shale aperture measurement device based on imbibition and ion diffusion property as claimed in claim 1, its feature exist In:Described fishing line (4) are No. 0.6 fishing line.
5. a kind of shale aperture measurement device based on imbibition and ion diffusion property as claimed in claim 1, its feature exist In:Conductivity meter (7) precision is 0.1 μ S/cm.
6. a kind of shale bore diameter measuring method based on imbibition and ion diffusion property, it is characterised in that comprise the following steps:
A. cylindrical shale samples are extracted, sectional area A is calculatedc, with epoxy resin by cylindrical shale samples cylinder sealing, it is placed in Dry in drying baker, until cylindrical shale samples quality no longer changes;
B. high accuracy analysis day is flat on support, using fishing line by drying after cylindrical shale samples hang on high accuracy On assay balance, high accuracy analysis balance reading M0 is recorded;
C. jacking system is placed in below support, flask is placed on magnetic stirring apparatus, and magnetic stirring apparatus is placed on jacking system;
D. volume is added into flask for the distilled water of V, and determines electrical conductivity G0 in water;
E. magnetic stirring apparatus is opened, jacking system is increased, cylindrical shale samples is immersed in 20 seconds in distilled water;
F. decline jacking system so that cylindrical shale samples are completely exposed the water surface, recording balance reading M1, and determine in water Electrical conductivity G1;
Theoretical, unit of account area water absorption V according to air water two phase fluid flowimbThe solution caused with the diffusion of imbibition process intermediate ion Electrical conductivity G relation over time;The physical parameter x being directed to, kw, Pc,Swf,Swi, μw, B, C, n need not be carried out Determine, B and C is obtained by the test curve in analysis later stage, and other parameters disappear this by the means of the mathematic(al) manipulation in later stage The impact of a little parameters;
According to Handy imbibitions models, the position x of water phase imbibition leading edge with the variation relation of imbibition time t is:
x = 2 k w p c t φμ w ( S w f - S w i )
K in formulawFor water penetration rate mD;PcFor capillary force Pa,For porosity, SwfFor leading edge water saturation, SwiFor initially containing Water saturation;
As cylindrical shale samples are fine and close, therefore leading edge water saturation is higher, and cylindrical shale samples have passed through drying Process, then difference between the two is approximately equal to 1;
During cylindrical shale samples imbibition, the volume change over time of unit area suction water is turned to:
V i m b / A c = B + 2 k w p c φ ( S w f - S w i ) t μ w
In formula:Hold-ups g/cm of the B for unit area water2, μwViscosity for water
The electrical conductivity of solution change that then ion diffusion causes is turned to:
G / A c = 2 C V + 4 π r n C V 2 k w p c φμ w ( S w f - S w i ) · t
In formula:C is unit area ion adhesion amount mg/cm2, n is capillary number;
G. jacking system is made to increase again so that cylindrical shale samples are totally submerged 20 seconds in distilled water;
H. repeat step F and step G, obtain the change of M~M0 and G~G0 t over time, you can obtain water suction volume VimbWith The change of electrical conductivity of solution G t over time;
I. the water suction volume of drafting per surface area, electrical conductivity are with t0.5Change curve, ask for the slope of curve, imbibition respectively Speed A and ion diffusion rates D, the A and D of acquisition are calculated and can be obtained the ratio of A/D;
According to unit area water absorption VimbThe electrical conductivity of solution G caused with the diffusion of imbibition process intermediate ion changes over time Theoretical formula, calculates the ratio that imbibition speed A and ion spread D, and process is as follows:
V i m b / A c = B + A t
G / A c = 2 C V + D t
Imbibition speed with the ratio of ion diffusion rates is:
A D = V r ( S w f - S w i ) 4 C = V r 4 C
J. conductance profile extended line is C/V with the intercept of the longitudinal axis, obtains average pore size r of shale.
r = 4 · A D · C V
CN201610937573.6A 2016-10-25 2016-10-25 A kind of shale aperture measurement device and method based on imbibition and ion diffusion property Active CN106501151B (en)

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CN107402169A (en) * 2017-07-28 2017-11-28 中国科学院力学研究所 A kind of devices and methods therefor for distinguishing shale reservoir matrix pores and microcrack
CN107727549A (en) * 2017-09-27 2018-02-23 中国科学院力学研究所 A kind of shale microscopic void measuring method and equipment
CN109060627A (en) * 2018-08-27 2018-12-21 中国海洋石油集团有限公司 Improve the device and method of the volumetric method measurement spontaneous imbibition oil displacement efficiency of water-wet oil reservoir
CN109374490A (en) * 2018-08-27 2019-02-22 中国石油大学(北京) Imbibition extraction equipment and imbibition extraction experiments method
CN110470575A (en) * 2019-09-04 2019-11-19 西南石油大学 A kind of shale salt ion diffusivity experimental test procedures

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Publication number Priority date Publication date Assignee Title
CN107402169A (en) * 2017-07-28 2017-11-28 中国科学院力学研究所 A kind of devices and methods therefor for distinguishing shale reservoir matrix pores and microcrack
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CN109060627A (en) * 2018-08-27 2018-12-21 中国海洋石油集团有限公司 Improve the device and method of the volumetric method measurement spontaneous imbibition oil displacement efficiency of water-wet oil reservoir
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CN110470575A (en) * 2019-09-04 2019-11-19 西南石油大学 A kind of shale salt ion diffusivity experimental test procedures
CN110470575B (en) * 2019-09-04 2020-09-18 西南石油大学 Shale salt ion diffusion capacity experimental test method

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