CN105628575B - Shale property determination method and device and shale property determination instrument - Google Patents

Shale property determination method and device and shale property determination instrument Download PDF

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CN105628575B
CN105628575B CN201410598715.1A CN201410598715A CN105628575B CN 105628575 B CN105628575 B CN 105628575B CN 201410598715 A CN201410598715 A CN 201410598715A CN 105628575 B CN105628575 B CN 105628575B
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CN105628575A (en
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李武广
钟兵
杨洪志
杨学锋
冯曦
张小涛
任利明
刘光耀
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Petrochina Co Ltd
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Abstract

The invention discloses a shale property determination method, a shale property determination device and a shale property determination instrument, and belongs to the technical field of measurementt. The invention solves the problem that the measurement result is inaccurate because the influence of the nondazy flow characteristic and the adsorbed gas of the shale gas is not considered when the permeability of the shale is measured by the measurement method related to the background art; the accuracy of the measurement result is improved sufficiently.

Description

Shale property assay method, device and shale property analyzer
Technical field
The present invention relates to field of measuring technique, more particularly to a kind of shale property assay method, device and shale property are surveyed Determine instrument.
Background technology
Shale gas is a kind of unconventional gas resource being stored in rammell, has and has a very wide distribution, exploits the longevity The advantages that life length and long production cycle, there is good application prospect.
Fluid ability of the shale gas in rammell be evaluation shale gas can the economic exploitation an important factor for.Wherein, often Fluid ability evaluating is permeability.In the related art, generally use darcy steady flow method measures shale permeability. By measuring the flow of the gas under certain pressure by shale samples, law is then percolated according to darcy straight line and calculates shale The permeability of sample.
In addition, pertinent literature also proposed measures shale permeability using pulse attenuation method.Mainly include core column pulse Damped method, particle pulse attenuation method and degassing method these three assay methods.Wherein, core column pulse attenuation method to laboratory apparatus and The requirement of shale samples is more stringent, although possessing higher measure effect and precision, also needs further to grind in Mathematical treatment Study carefully;Shale samples are reduced to irregular figure by particle pulse attenuation method, destroy pore structure, have one to be fixed to measurement result It rings;Degassing method is only applicable to the test of live sealed coring, and related to the test of shale reservoir air content, precision is not high.
In the implementation of the present invention, inventor has found that above-mentioned technology has at least the following problems:Gas is in shale Seepage flow there are non-Darcy flow feature, calculating the permeability of shale using darcy straight line seepage flow law at this time necessarily causes to measure As a result the problem of inaccurate.In addition, the various assay methods that above-mentioned technology is related to, do not consider when measuring the permeability of shale The influence of adsorbed gas, the problem of causing measurement result inaccurate.
The content of the invention
The assay method being related to solve above-mentioned technology does not consider that the non-of shale gas reaches when measuring the permeability of shale The problem of influence of western flow behavior and adsorbed gas, caused measurement result is inaccurate, an embodiment of the present invention provides one Kind shale property assay method, device and shale property analyzer.The technical solution is as follows:
In a first aspect, a kind of shale property assay method is provided, the described method includes:
N group pressure values are obtained, during the n groups pressure value spreads for gas in shale samples, every pre- timing Between be spaced record the shale samples both ends pressure value, for each group of pressure value, the pressure value includes placing State the pressure value P of the input end of the rock core fastener of shale samplesinWith the pressure value P of the port of exportout, n >=2 and n are integer;
Corresponding n groups concentration value is calculated according to the n groups pressure value, for each group of concentration value, the concentration value bag Include the concentration value N of the input endinWith the concentration value N of the port of exportout
One-dimensional Diffusion Equation is solved according to the n groups concentration value and obtains the diffusion coefficient D of the shale samples, the diffusion Coefficient D is used to reflect diffusion of the gas in the shale samples;
The permeability k of the shale samples is calculated using following formula:
K=D μ φ βt
Wherein, the D represents the diffusion coefficient (m2/s);The μ represents fluid viscosity (Pas);The φ is represented The effecive porosity (%) of the shale samples;The βtRepresent the compressed coefficient (Pa under initial pore pressure-1)。
Optionally, the One-dimensional Diffusion Equation is:
Wherein, the L represents the length (m) of the shale samples;The N represents gas corresponding to position x and moment t Concentration value (kg/m3);
Alternatively,
The One-dimensional Diffusion Equation is:
Wherein, the L represents the length (m) of the shale samples;The N represents gas corresponding to position x and moment t Concentration value (kg/m3);Represent the incrementss of the adsorbed gas content corresponding to moment t;The ρ1Represent the shale Density (the kg/m of sample3);The ρ2Represent gas density (kg/m3)。
Optionally, before the permeability k that the shale samples are calculated using following formula, further include:
The effecive porosity φ of the shale samples is calculated using following formula:
Wherein, the S represents the sectional area (m of the shale samples2);The L represents the length of the shale samples (m);The P1Represent pulse (MPa);The P2Represent balance pressure (MPa);The Z1Represent gas in pressure P1Under Compressibility factor;The Z2Represent gas in pressure P2Under compressibility factor;The V1Represent the input end with the rock core fastener Connected upstream gas volume of a container (m3);The VxRepresent the upstream gas container, the upstream inlet valve, the rock Volume (the m of pipeline between core holder and the downstream inlet valve3)。
Optionally, the method further includes:
The adsorbed gas content Q of the shale samples is calculated using following formulan
Wherein, the QnIt represents in n-th of adsorption equilibrium pressure Pn *Under, what the shale samples of unit mass were adsorbed Gas volume (m3/kg);The m represents the quality (kg) of the shale samples;The VnIt represents in n-th of adsorption equilibrium pressure Pn *Under, gas volume (m that the shale samples are adsorbed3);The T0 Represent room temperature (DEG C), the T represents experimental temperature (DEG C), the P0Represent standard atmospheric pressure (MPa), the VhRepresent with it is described Upstream gas volume of a container (the m that the input end of rock core fastener is connected3), the VφRepresent the hole of the rock core fastener Volume (m3), the PnRepresent n-th of pulse (MPa), the Pn *Represent n-th of adsorption equilibrium pressure (MPa), the Zn Represent gas in pressure PnUnder compressibility factor, the Zn *Represent gas in pressure Pn *Under compressibility factor;As n=1,
Second aspect, provides a kind of shale property measurement device, and described device includes:
Pressure acquisition module, for obtaining n group pressure values, what the n groups pressure value spread for gas in shale samples In the process, the pressure value at the shale samples both ends of record is spaced at predetermined time intervals, for each group of pressure value, the pressure Force value includes the pressure value P for being placed with the input end of the rock core fastener of the shale samplesinWith the pressure value P of the port of exportout, n >=2 and n is integer;
Concentration calculation module is dense for each group for calculating corresponding n groups concentration value according to the n groups pressure value Angle value, the concentration value include the concentration value N of the input endinWith the concentration value N of the port of exportout
Diffusion coefficient computing module obtains the shale sample for solving One-dimensional Diffusion Equation according to the n groups concentration value The diffusion coefficient D of product, the diffusion coefficient D are used to reflect diffusion of the gas in the shale samples;
Computing permeability module, for following formula to be used to calculate the permeability k of the shale samples:
K=D μ φ βt
Wherein, the D represents the diffusion coefficient (m2/s);The μ represents fluid viscosity (Pas);The φ is represented The effecive porosity (%) of the shale samples;The βtRepresent the compressed coefficient (Pa under initial pore pressure-1)。
Optionally, the One-dimensional Diffusion Equation is:
Wherein, the L represents the length (m) of the shale samples;The N represents gas corresponding to position x and moment t Concentration value (kg/m3);
Alternatively,
The One-dimensional Diffusion Equation is:
Wherein, the L represents the length (m) of the shale samples;The N represents gas corresponding to position x and moment t Concentration value (kg/m3);Represent the incrementss of the adsorbed gas content corresponding to moment t;The ρ1Represent the shale Density (the kg/m of sample3);The ρ2Represent gas density (kg/m3)。
Optionally, described device further includes:
Porosity calculation module, for following formula to be used to calculate the effecive porosity φ of the shale samples:
Wherein, the S represents the sectional area (m of the shale samples2);The L represents the length of the shale samples (m);The P1Represent pulse (MPa);The P2Represent balance pressure (MPa);The Z1Represent gas in pressure P1Under Compressibility factor;The Z2Represent gas in pressure P2Under compressibility factor;The V1Represent the input end with the rock core fastener Connected upstream gas volume of a container (m3);The VxRepresent the upstream gas container, the upstream inlet valve, the rock Volume (the m of pipeline between core holder and the downstream inlet valve3)。
Optionally, described device further includes:
Adsorbed gas computing module, for following formula to be used to calculate the adsorbed gas content Q of the shale samplesn
Wherein, the QnIt represents in n-th of adsorption equilibrium pressure Pn *Under, what the shale samples of unit mass were adsorbed Gas volume (m3/kg);The m represents the quality (kg) of the shale samples;The VnIt represents in n-th of adsorption equilibrium pressure Pn *Under, gas volume (m that the shale samples are adsorbed3);The T0 Represent room temperature (DEG C), the T represents experimental temperature (DEG C), the P0Represent standard atmospheric pressure (MPa), the VhRepresent with it is described Upstream gas volume of a container (the m that the input end of rock core fastener is connected3), the VφRepresent the hole of the rock core fastener Volume (m3), the PnRepresent n-th of pulse (MPa), the Pn *Represent n-th of adsorption equilibrium pressure (MPa), the Zn Represent gas in pressure PnUnder compressibility factor, the Zn *Represent gas in pressure Pn *Under compressibility factor;As n=1,
The third aspect, provides a kind of shale property analyzer, and the shale property analyzer includes:Upstream gas is held Device, upstream inlet valve, for placing the rock core fastener of shale samples, downstream inlet valve, gas downstream container, upstream hydraulic pressure Pump, confining pressure hydraulic pump, downstream hydraulic pump, pressure sensor, differential pressure pickup, confining pressure intake valve, blow valve, insulating box, timing Device and computing device;
Wherein, the input end of the rock core fastener passes sequentially through the first valve of the upstream inlet valve, the upstream Second valve of intake valve is connected with the first end of the upstream gas container;The port of export of the rock core fastener passes sequentially through First valve of the downstream inlet valve, the downstream inlet valve the second valve and the gas downstream container first end phase Even;The rock core fastener, the upstream gas container and the gas downstream container are installed in the insulating box;On described Trip hydraulic pump is connected by the first pipeline with the 3rd valve of the upstream inlet valve, and the downstream hydraulic pump passes through the second pipeline It is connected with the 3rd valve of the downstream inlet valve;4th valve of the upstream inlet valve passes through the 3rd pipeline and the downstream 4th valve of intake valve is connected;5th valve of the upstream inlet valve is through the differential pressure pickup and the downstream inlet valve The 5th valve be connected;The confining pressure hydraulic pump is connected through the confining pressure intake valve with the side wall of the rock core fastener;It is described The second end of upstream gas container is connected with the pressure sensor, second end and the blow valve of the gas downstream container It is connected;The pressure sensor, the differential pressure pickup and the timer are connected respectively with the computing device;
The computing device, including the shale property measurement device as described in second aspect.
The advantageous effect that technical solution provided in an embodiment of the present invention is brought is:
The diffusion coefficient of shale samples is obtained by solving the One-dimensional Diffusion Equation pre-established, and then according to diffusion coefficient Acquire the permeability of shale samples;It solves the assay method that background technology is related to and does not consider page when measuring the permeability of shale The problem of Non-Darcy's flow dynamic characteristic of rock gas and influence of adsorbed gas, caused measurement result is inaccurate;It substantially increases The accuracy of measurement result.
Description of the drawings
To describe the technical solutions in the embodiments of the present invention more clearly, make required in being described below to embodiment Attached drawing is briefly described, it should be apparent that, the accompanying drawings in the following description is only some embodiments of the present invention, for For those of ordinary skill in the art, without creative efforts, other are can also be obtained according to these attached drawings Attached drawing.
Fig. 1 is the structure diagram of shale property analyzer provided by one embodiment of the present invention;
Fig. 2 is the method flow diagram of shale property assay method provided by one embodiment of the present invention;
Fig. 3 A are the method flow diagrams for the shale property assay method that another embodiment of the present invention provides;
Fig. 3 B are the schematic diagrames that the gas involved by another embodiment of the present invention is spread in shale samples;
Fig. 4 is the block diagram of shale property measurement device provided by one embodiment of the present invention;
Fig. 5 is the block diagram for the shale property measurement device that another embodiment of the present invention provides.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with attached drawing to embodiment party of the present invention Formula is described in further detail.
It please refers to Fig.1, it, should it illustrates the structure diagram of shale property analyzer provided by one embodiment of the present invention Shale property analyzer includes:Upstream gas container 101, upstream inlet valve 102, the rock core fastener for placing shale samples 103rd, downstream inlet valve 104, gas downstream container 105, upstream hydraulic pump 106, confining pressure hydraulic pump 107, downstream hydraulic pump 108, Pressure sensor 109, differential pressure pickup 110, confining pressure intake valve 111, blow valve 112, insulating box 113, timer 114 and calculating Equipment 115.Wherein:
The input end 103a of rock core fastener 103 passes sequentially through the first valve 102a, the upstream inlet of upstream inlet valve 102 Second valve 102b of valve 102 is connected with the first end of upstream gas container 101;The port of export 103b of rock core fastener 103 according to It is secondary to pass through the first valve 104a of downstream inlet valve 104, the second valve 104b of downstream inlet valve 104 and gas downstream container 105 first end is connected.
Rock core fastener 103 is used to place shale samples.Under normal conditions, shale samples are column, and diameter exists 2.5cm-10cm between, length is between 2cm-20cm.
Rock core fastener 103, upstream gas container 101 and gas downstream container 105 are installed in insulating box 113.Constant temperature The maximum temperature of case 113 may be set to 120 DEG C.
Upstream hydraulic pump 106 is connected by the first pipeline with the 3rd valve 102c of upstream inlet valve 102, downstream hydraulic pump 108 are connected by the second pipeline with the 3rd valve 104c of downstream inlet valve 104.Upstream hydraulic pump 106 and downstream hydraulic pump 108 For experimental gas to be respectively pressed into upstream gas container 101 and gas downstream container 105.Experimental gas can select purity For 99.9% CH4(methane), purity are 99.9% CO2(carbon dioxide), purity are 99.9% N2(nitrogen) or purity For 99.9% He (helium).Hydraulic pump generally selects distilled water with water.
4th valve 102d of upstream inlet valve 102 passes through the 3rd pipeline and the 4th valve 104d of downstream inlet valve 104 It is connected.Fiveth valve 104es of the 5th valve 102e of upstream inlet valve 102 through differential pressure pickup 110 Yu downstream inlet valve 104 It is connected.Differential pressure pickup 110 is used to gather the ports of export of the input end 103a with rock core fastener 103 of rock core fastener 103 Pressure differential between 103b.Upstream inlet valve 102 and downstream inlet valve 104 can select six-way valve.
Confining pressure hydraulic pump 107 is connected through confining pressure intake valve 111 with the side wall of rock core fastener 103.Confining pressure hydraulic pump 107 is used Certain confining pressure and axial compressive force is provided in giving shale samples.
The second end of upstream gas container 101 is connected with pressure sensor 109, the second end of gas downstream container 105 with Blow valve 112 is connected.Pressure sensor 109 is used to gather the pressure value of the input end 103a of rock core fastener 103.
Pressure sensor 109, differential pressure pickup 110 and timer 114 are connected respectively with computing device 115.For example, pressure Sensor 109, differential pressure pickup 110 and timer 114 can be connected by data cable with computing device 115 respectively.Computing device 115 be usually computer, can be desktop computer or portable computer on knee.Computing device 115 can be included such as The shale property measurement device that lower Fig. 4 or embodiment illustrated in fig. 5 provide, the shale property measurement device are configured as performing such as The shale property assay method that lower Fig. 2 Fig. 3 A illustrated embodiments provide.
In addition, in other possible embodiments, pressure sensor 109 or differential pressure pickup 110 can be by another Pressure sensor replaces, which is connected with gas downstream container 105, for gathering rock core fastener 103 Port of export 103b pressure value.
In technical solution provided in an embodiment of the present invention, shale can be measured by the analyzer of shale property shown in Fig. 1 The porosity of sample, permeability, the free parameters such as Gas content and adsorbed gas content.
Specifically, when measuring the porosity of shale samples, following several experimental procedures can be included:
(1) diameter d, length L and the quality m of shale samples are measured;
(2) dead volume V is measuredx, dead volume VxIncluding upstream gas container 101, upstream inlet valve 102, rock core fastener The volume of pipeline between 103 and downstream inlet valve 104;
(3) structure connects each instrument according to Fig. 1, and shale samples are put into rock core fastener 103;
(4) all valves are closed, certain confining pressure and axial compressive force are loaded to shale samples by confining pressure hydraulic pump 107;
(5) the second valve 102b and the 3rd valve 102c of upstream inlet valve 102 are opened, by upstream hydraulic pump 106 to Experimental gas is filled in upstream gas container 101, and reaches predetermined threshold P in the registration of pressure sensor 1091When, in closing Swim the 3rd valve 102c of intake valve 102;
(6) the first valve 102a of upstream inlet valve 102 is opened so that experimental gas is spread by shale samples, waits to press The registration of force snesor 109 is steady state value P2When, the registration P of record pressure sensor 1092
When measuring the permeability of shale samples, following several experimental procedures can be included:
(1) diameter d, length L and the quality m of shale samples are measured;
(2) dead volume V is measuredx, dead volume VxIncluding upstream gas container 101, upstream inlet valve 102, rock core fastener The volume of pipeline between 103 and downstream inlet valve 104;
(3) structure connects each instrument according to Fig. 1, and shale samples are put into rock core fastener 103;
(4) all valves are closed, certain confining pressure and axial compressive force are loaded to shale samples by confining pressure hydraulic pump 107;
(5) open upstream inlet valve 102 the second valve 102b and the 3rd valve 102c and downstream inlet valve 104 the Two valve 104b and the 3rd valve 104c pass through upstream hydraulic pump 106 and downstream hydraulic pump 108 upstream gas container respectively 101 and gas downstream container 105 in be filled with a certain amount of experimental gas;
(6) the 3rd valve 102c of upstream inlet valve 102 and the 3rd valve 104c of downstream inlet valve 104 are closed, and is beaten Open upstream inlet valve 102 the first valve 102a, the 4th valve 102d and the 5th valve 102e and downstream inlet valve 104 One valve 104a, the 4th valve 104d and the 5th valve 104e so that experimental gas is spread, in upstream gas container 101, downstream Balance is sufficiently achieved in gas container 105 and shale samples, when the registration of differential pressure pickup 110 is 0MPa, closes upstream The first valve 102a, the 4th valve 102d of intake valve 102 and the 4th valve 104d of downstream inlet valve 104;
(7) the 3rd valve 102c of upstream inlet valve 102 is opened, passes through upstream gas container 101 of upstream hydraulic pump 106 Apply a preset pulse, close the 3rd valve 102c of upstream inlet valve 102, and record pressure sensor 109 and the registration of differential pressure pickup 110;
(8) the first valve 102a of upstream inlet valve 102 is opened, under the action of concentration difference caused by pressure differential so that Experimental gas is spread by shale samples, and interval record pressure sensor 109 and differential pressure pickup 110 show at predetermined time intervals Number, until the registration of differential pressure pickup 110 is 0MPa.
When measuring the adsorbed gas content of shale samples, following several experimental procedures can be included:
(1) structure connects each instrument according to Fig. 1, and shale samples are put into rock core fastener 103;
(2) all valves are closed, certain confining pressure and axial compressive force are loaded to shale samples by confining pressure hydraulic pump 107;
(3) the second valve 102b and the 3rd valve 102c of upstream inlet valve 102 are opened, by upstream hydraulic pump 106 to A certain amount of experimental gas is filled in upstream gas container 101, and records the registration P1 of pressure sensor 109, close upstream into 3rd valve 102c of air valve 102;
(4) the first valve 102a of upstream inlet valve 102 is opened so that experimental gas is spread by shale samples, waits to press The registration of force snesor 109 is steady state value P1 *When, the registration P of record pressure sensor 1091 *, close upstream inlet valve 102 First valve 102a;
(5) repeat the above steps (3) and (4), records P2、P2 *、…、Pn、Pn *, until adsorption equilibrium pressure Pn *Reach advance The experiment maximum pressure of setting;
Optionally, following several desorption experiment steps are may also include after step (5):
(6) pressure in rock core fastener 103 is reduced, passes through pressure before the record balance of pressure sensor 109;
(7) when pressure balance, record desorption balance pressure, while above-mentioned pressure balance is recorded by timer 114 Time spent by journey;
(8) repeat the above steps (6) and (7), until desorption balance pressure reaches preset experiment minimum pressure.
It should be noted is that:In any of the above-described experiment, after structure according to Fig. 1 connects each instrument, Need the air-tightness of checking experiment device;It in addition, also needs to vacuumize entire experimental provision, it is ensured that without air in each instrument It is mixed into, reduces experimental error.
In the implementation of the present invention, inventor has found:Flowing of the gas in shale meets diffusion law, in pressure Under concentration difference caused by difference, one-dimensional diffusion occurs in shale for gas.It is therefore proposed that diffusion coefficient evaluates gas in shale Fluid ability.Diffusion coefficient is the physical quantity for representing gas diffusion degree, and diffusion coefficient refers to along dispersal direction, in unit Between under conditions of per unit concentration gradient, perpendicular through the quality of unit area institute diffusion gas, unit m2/ s or cm2/s.Into One step, the permeability of shale is solved according to diffusion coefficient, can so that measurement result is more accurate.
In the following, technical solution provided by the invention will be described in detail and be illustrated by several embodiments:
It please refers to Fig.2, it illustrates the method flow diagram of shale property assay method provided by one embodiment of the present invention, It is carried out in the computing device 115 that the present embodiment is applied to the shale property assay method in shale property analyzer shown in Fig. 1 It illustrates.The shale property assay method may include steps of:
Step 202, n group pressure values are obtained, during which spreads for gas in shale samples, every The pressure value at the shale samples both ends of predetermined time interval record, for each group of pressure value, this group of pressure value includes being placed with The pressure value P of the input end of the rock core fastener of shale samplesinWith the pressure value P of the port of exportout, n >=2 and n are integer.
Step 204, corresponding n groups concentration value is calculated according to above-mentioned n groups pressure value, for each group of concentration value, the group Concentration value includes the concentration value N of input endinWith the concentration value N of the port of exportout
Step 206, One-dimensional Diffusion Equation is solved according to above-mentioned n groups concentration value and obtains the diffusion coefficient D of shale samples, the expansion Coefficient D is dissipated for reflecting diffusion of the gas in shale samples.
Step 208, the permeability k of shale samples is calculated using following formula:
K=D μ φ βt
Wherein, D represents diffusion coefficient (m2/s);μ represents fluid viscosity (Pas);φ represents effective hole of shale samples Porosity (%);βtRepresent the compressed coefficient (Pa under initial pore pressure-1)。
In conclusion shale property assay method provided in this embodiment, by solving the one-dimensional diffused sheet pre-established Journey obtains the diffusion coefficient of shale samples, and then the permeability of shale samples is acquired according to diffusion coefficient;Solves background technology The assay method being related to does not consider the Non-Darcy's flow dynamic characteristic of shale gas and the shadow of adsorbed gas when measuring the permeability of shale The problem of sound, caused measurement result is inaccurate;Substantially increase the accuracy of measurement result.
A is please referred to Fig.3, it illustrates the method flows for the shale property assay method that another embodiment of the present invention provides Figure, the present embodiment with the shale property assay method be applied to shale property analyzer shown in Fig. 1 in computing device 115 in into Row illustrates.The shale property assay method may include steps of:
Step 301, the effecive porosity φ of shale samples is calculated:
Wherein, S represents the sectional area (m of shale samples2);L represents the length (m) of shale samples;P1Represent pulse (MPa);P2Represent balance pressure (MPa);Z1Represent gas in pressure P1Under compressibility factor;Z2Represent gas in pressure P2Under Compressibility factor;V1Represent the upstream gas volume of a container (m being connected with the input end of rock core fastener3);VxRepresent upstream gas Volume (the m of pipeline between container, upstream inlet valve, rock core fastener and downstream inlet valve3)。
First, the active porosity volume V of shale samples is calculated by Boyle's lawp
Z2P1V1=Z1P2(V1+Vx+Vp);
Wherein, P1Represent the experimental procedure (5) of pulse (MPa) namely the porosity in said determination shale samples The pressure value of middle record;P2Represent balance pressure (MPa) namely the experimental procedure of the porosity in said determination shale samples (6) pressure value of record in;Z1Represent gas in pressure P1Under compressibility factor;Z2Represent gas in pressure P2Under compression because Son;V1Represent the upstream gas volume of a container (m being connected with the input end of rock core fastener3);VxExpression upstream gas container, Volume (the m of pipeline between upstream inlet valve, rock core fastener and downstream inlet valve3), it is also referred to as dead volume;VpRepresent page Active porosity volume (the m of rock sample product3)。
It can be derived by above formula:Active porosity volume
The effecive porosity φ of shale samples is equal to the active porosity volume V of shale samplespWith the volume V's of shale samples Ratio namely:
Wherein, S represents the sectional area (m of shale samples2);L represents the length (m) of shale samples.
Optionally, when the cylindrical sample that shale samples are a diameter of d, length is L, due to the sectional area of shale samplesSo
Before the permeability k of shale samples is calculated, mathematical model is initially set up.As shown in Figure 3B, it illustrates gases The schematic diagram spread in shale samples.Incorporated by reference to the experimental procedure of the permeability with reference to said determination shale samples, in upstream When gas in gas container, gas downstream container and shale samples sufficiently achieves balance, a preset pressure arteries and veins Punching is acted in upstream gas container so that gas forms one-dimensional diffusion in shale samples, and Fig. 3 B arrows direction represents Gas diffusion direction.In entire diffusion process, the pressure in upstream gas container continuously decreases, the pressure in gas downstream container Power gradually rises, and the pressure differential at shale samples both ends is gradually reduced, and treats upstream gas container, gas downstream container and shale sample When gas in product reaches balance again, the pressure differential at shale samples both ends becomes 0MPa.
Object G is represented in position x and the concentration value of moment t with function N (x, t), which represents institute in unit volume The quality of diffusate.Since shale samples are placed in rock core fastener, there is certain confining pressure, shale samples are clamped with core Device is in close contact, it is believed that shale samples side surface part generates diffusion.Therefore, diffusion phenomena of the gas in shale samples meet One-dimensional diffusion derives that the mathematical modulo of one-dimensional diffusion occurs in shale samples for gas by imfinitesimal method and the principle of mass conservation Type.
Since shale has characterization of adsorption, in the case where considering adsorbed gas, flowing into a gas part for shale samples makes Concentration inside increases, and another part causes adsorbed gas content to increase, it is possible thereby to establish One-dimensional Diffusion Equation:
Wherein, L represents the length (m) of shale samples;N represents gas in the concentration value (kg/ corresponding to position x and moment t m3);Represent the incrementss of the adsorbed gas content corresponding to moment t;ρ1Represent the density (kg/m of shale samples3);ρ2 Represent gas density (kg/m3)。
In addition, if initial balance pressure design is sufficiently large, and under the action of pulse, the increasing of adsorbed gas content Dosage will be very small, can be ignored, then in the case of without considering adsorbed gas, One-dimensional Diffusion Equation is:
Wherein, L represents the length (m) of shale samples;N represents gas in the concentration value (kg/ corresponding to position x and moment t m3)。
After One-dimensional Diffusion Equation is established, the definite condition of the One-dimensional Diffusion Equation is determined.
Wherein, primary condition is:Represent initial time (namely t=0) In the concentration value of the gas of the different position x of shale samples.
Boundary condition is:N (0, t)=N1(t), N (L, t)=N2(t) (t >=0,0 < x < L);N1(t) represent in shale sample The concentration value of the x=0 positions of the product gas of t at different moments, N2(t) represent in the x=L positions of shale samples t at different moments The concentration value of gas.
In order to ensure the continuity of solution, above-mentioned primary condition and boundary condition must are fulfilled for compatibility condition, i.e.,:
It afterwards, can the number that is recorded in gas diffusion process of combination pressure sensor, differential pressure pickup and timer According to, and above-mentioned One-dimensional Diffusion Equation is solved using the separation of variable or calculus of finite differences, obtain the diffusion coefficient D of shale samples.Tool For body, following steps 302 to step 304:
Step 302, n group pressure values are obtained, during which spreads for gas in shale samples, every The pressure value at the shale samples both ends of predetermined time interval record.
For each group of pressure value, this group of pressure value includes the pressure for being placed with the input end of the rock core fastener of shale samples Force value PinWith the pressure value P of the port of exportout, n >=2 and n are integer.
Step 303, corresponding n groups concentration value is calculated according to above-mentioned n groups pressure value.
For each group of concentration value, this group of concentration value includes the concentration value N of input endinWith the concentration value N of the port of exportout.Its In, the concentration value N of input endinIt can be according to the pressure value P of input endinWith upstream gas volume of a container calculate and acquire; The concentration value N of the port of exportoutIt can be according to the pressure value P of the port of exportoutWith gas downstream volume of a container calculate and acquire.
Step 304, One-dimensional Diffusion Equation is solved according to above-mentioned n groups concentration value and obtains the diffusion coefficient D of shale samples.
Diffusion coefficient D is used to reflect diffusion of the gas in shale samples.
In the case where considering adsorbed gas, One-dimensional Diffusion Equation is:
Above-mentioned One-dimensional Diffusion Equation and definite condition are subjected to difference discrete, obtained difference scheme is:
NoteThen above-mentioned difference scheme can be changed to:
Solution calculating is carried out according to the boundary value of record and initial value (namely above-mentioned n groups concentration value), can be obtained arbitrary Moment t, any position x free gas concentration value N (x, t).When upstream gas container, gas downstream container and shale samples In gas when reaching balance again namely when concentration value is identical, solve α, and then solve diffusion coefficient D.It is specific to solve Process can establish Solving Linear, and the present embodiment does not introduce this specifically.
In the case of without considering adsorbed gas, One-dimensional Diffusion Equation is:
Likewise, above-mentioned One-dimensional Diffusion Equation and definite condition are carried out difference discrete, obtained difference scheme is:
NoteThen above-mentioned difference scheme can be changed to:
Solution calculating is carried out according to the boundary value of record and initial value (namely above-mentioned n groups concentration value), can be obtained arbitrary Moment t, any position x free gas concentration value N (x, t).When upstream gas container, gas downstream container and shale samples In gas when reaching balance again namely when concentration value is identical, solve α, and then solve diffusion coefficient D.It is specific to solve Process can establish Solving Linear, and the present embodiment does not introduce this specifically.
Step 305, the permeability k of shale samples is calculated:
K=D μ φ βt
After the above-mentioned One-dimensional Diffusion Equation on concentration is converted into the One-dimensional Diffusion Equation on pressure, it can be expanded Dissipate the relational expression of coefficient D and permeability k:
Wherein, D represents diffusion coefficient (m2/s);μ represents fluid viscosity (Pas);φ represents effective hole of shale samples Porosity (%);βtRepresent the compressed coefficient (Pa under initial pore pressure-1)。
Therefore, permeability k=D μ φ βt
It should be noted is that:The permeability k being calculated in the present embodiment is the apparent permeability based on diffusion. In calculating process, due to considering the influence of adsorbed gas so that result of calculation is relatively less than normal, and result of calculation is more accurate.
Optionally, it is provided in this embodiment with reference to the experimental procedure of the adsorbed gas content with reference to said determination shale samples Shale property assay method can also as follows 306 calculate shale samples adsorbed gas content.
Step 306, the adsorbed gas content Q of shale samples is calculatedn
Wherein, QnIt represents in n-th of adsorption equilibrium pressure Pn *Under, gas volume that the shale samples of unit mass are adsorbed (m3/kg);M represents the quality (kg) of shale samples;VnIt represents in n-th of adsorption equilibrium pressure Pn *Under, shale samples are adsorbed Gas volume (m3);T0Represent room temperature (DEG C), T represents experimental temperature (DEG C), P0Represent standard atmospheric pressure (MPa), VhRepresent the upstream gas volume of a container being connected with the input end of rock core fastener (m3), VφRepresent the pore volume (m of rock core fastener3), PnRepresent n-th of pulse (MPa), Pn *Represent that n-th of absorption is flat The pressure that weighs (MPa), ZnRepresent gas in pressure PnUnder compressibility factor, Zn *Represent gas in pressure Pn *Under compressibility factor;Work as n When=1,
Further, Lan Shi (Langmuir) equation is utilized:It can obtain the suction under arbitrary pressure Attached Gas content.Wherein, v represents adsorbance (cm of the gas in the case where balancing pressure p3/g);vmRepresent single molecular layer saturated absorption (cm3/g);P represents gas pressure (MPa);B represents the constant related with temperature and adsorbent;vLFor Langmuir volumes, represent Maximum adsorption ability, physical significance are:At a given temperature, adsorbed gas content when shale adsorbed methane reaches saturation (cm3/g);pLFor Langmuir pressure, the pressure corresponding to the half of Langmuir volumes, value is equivalent to 1/b (MPa).
In addition, in desorption process, the 1st desorption balance pressure p 'J(1) the stripping gas volume V corresponding toJ(1):
N-th of desorption balance pressure p 'J(n) the stripping gas volume V corresponding toJ(n):
It can obtain, under n-th of desorption balance pressure, the desorption quantity Q of shale samplesJ(n):
Desorption rate v (n):
Wherein, VJ(1) the 1st desorption balance pressure P is representedJStripping gas volume (m corresponding to ' (1)3);VJ(n) represent N-th of desorption balance pressure pJStripping gas volume (m corresponding to ' (n)3);PJ(1) represent to reduce in rock core fastener for the 1st time Balance the balance pressure (MPa) before pressure;PJ' (1) represents the 1st desorption balance pressure (MPa);PJ(n) represent that n-th reduces Balance pressure (MPa) before balance pressure in rock core fastener;pJ' (n) represents n-th of desorption balance pressure (MPa);ZJ(1) Represent gas in pressure PJ(1) compressibility factor under;ZJ' (1) represents gas in pressure PJCompressibility factor under ' (1);ZJ(n) table Show gas in pressure PJ(n) compressibility factor under;ZJ' (n) represents gas in pressure pJCompressibility factor under ' (n);M represents shale The quality (kg) of sample;T) n (represents the time (s) spent by n-th desorption process.
In conclusion shale property assay method provided in this embodiment, by solving the one-dimensional diffused sheet pre-established Journey obtains the diffusion coefficient of shale samples, and then the permeability of shale samples is acquired according to diffusion coefficient;Solves background technology The assay method being related to does not consider the Non-Darcy's flow dynamic characteristic of shale gas and the shadow of adsorbed gas when measuring the permeability of shale The problem of sound, caused measurement result is inaccurate;When solving the permeability of shale samples, non-Darcy flow spy had both been considered Property, it is contemplated that the influence of adsorbed gas, substantially increases the accuracy of measurement result.
In addition, shale property assay method provided in this embodiment, additionally provides the porosity of shale samples, free gas contains The computational methods of the related physical quantities such as amount, adsorbed gas content realize comprehensive, multi-angle synthesis measuring effect.
In the another embodiment provided on the basis of based on above-mentioned Fig. 2 and Fig. 3 A illustrated embodiments, pass through page shown in Fig. 1 Lithology matter analyzer can also measure shale slip flows and occurrence condition.Specifically, following several experimental procedures can be included:
(1) diameter d, length L and the quality m of shale samples are measured;
(2) shale samples porosity φ under formation conditions and permeability k are measured using the experimental procedure of above-mentioned introduction;
(3) a minimum pressure pulse is given so that upstream gas container 101, gas downstream container 105 and core folder Pressure in holder 103 reaches balance;
(4) give upstream gas container 101 several pressure pulses, until experiment maximum pressure;In the process, survey respectively Determine the permeability k of shale samplesi, treat the pressure in upstream gas container 101, gas downstream container 105 and rock core fastener 103 When power reaches balance, balance pressure p is measuredi, and this balance pressure is denoted as average pressure;Wherein, permeability kiCorresponding to average Pressure pi
(5) different average pressure p are usediUnder permeability kiValue and the ratio evaluation shale slip flows energy of permeability k Power.
, it is necessary to pay attention to the following in above-mentioned experiment:
1st, it is necessary to the air-tightness of checking experiment device after structure according to Fig. 1 connects each instrument;
2nd, before the experiments, entire experimental provision need to be vacuumized, it is ensured that no air is mixed into each instrument, is reduced real Test error;
3rd, experimental temperature control is in 90 DEG C or so of formation temperature;
4th, confining pressure simulated formation depth is the pressure at 2000m or so place, is approximately 50MPa;Wherein, confining pressure p=Zg ρ, Z table Show shale reservoir buried depth (m), g represents acceleration of gravity (N/kg), and ρ represents shale samples density (g/cm3);
5th, experimental design maximum average pore pressure is original formation pressure namely 50MPa;
6th, pressure pulse can be respectively set to 2MPa, 3MPa, 5MPa, 6MPa and 8MPa;When pressure pulse reaches 8MPa Afterwards, permeability determination is carried out with constant 8MPa pressure pulses, until average pore pressure reaches experimental design maximum averagely Pore pressure.
In the another embodiment provided on the basis of based on above-mentioned Fig. 2 and Fig. 3 A illustrated embodiments, pass through page shown in Fig. 1 Lithology matter analyzer can also measure permeability and porosity namely stress sensitivity of the shale under different confining pressures.Specific experiment Step can refer to said determination permeability and the experimental procedure of porosity, it is only necessary to adjust confining pressure during the experiment.
Following is apparatus of the present invention embodiment, can be used for performing the method for the present invention embodiment.It is real for apparatus of the present invention The details not disclosed in example is applied, refer to the method for the present invention embodiment.
It please refers to Fig.4, it illustrates the block diagram of shale property measurement device provided by one embodiment of the present invention, The shale property measurement device can be measured by the shale property shown in Fig. 1 that is implemented in combination with becoming of software, hardware or both Computing device in instrument it is some or all of.The shale property measurement device can include:Pressure acquisition module 410, concentration Computing module 420, diffusion coefficient computing module 430 and computing permeability module 440.
Pressure acquisition module 410, for obtaining n group pressure values, the n groups pressure value spreads for gas in shale samples During, the pressure value at the shale samples both ends of record is spaced at predetermined time intervals, it is described for each group of pressure value Pressure value includes the pressure value P for being placed with the input end of the rock core fastener of the shale samplesinWith the pressure value of the port of export Pout, n >=2 and n are integer.
Concentration calculation module 420, for calculating corresponding n groups concentration value according to the n groups pressure value, for each group Concentration value, the concentration value include the concentration value N of the input endinWith the concentration value N of the port of exportout
Diffusion coefficient computing module 430 obtains the shale for solving One-dimensional Diffusion Equation according to the n groups concentration value The diffusion coefficient D of sample, the diffusion coefficient D are used to reflect diffusion of the gas in the shale samples.
Computing permeability module 440, for following formula to be used to calculate the permeability k of the shale samples:
K=D μ φ βt
Wherein, the D represents the diffusion coefficient (m2/s);The μ represents fluid viscosity (Pas);The φ is represented The effecive porosity (%) of the shale samples;The βtRepresent the compressed coefficient (Pa under initial pore pressure-1)。
In conclusion shale property measurement device provided in this embodiment, by solving the one-dimensional diffused sheet pre-established Journey obtains the diffusion coefficient of shale samples, and then the permeability of shale samples is acquired according to diffusion coefficient;Solves background technology The assay method being related to does not consider the Non-Darcy's flow dynamic characteristic of shale gas and the shadow of adsorbed gas when measuring the permeability of shale The problem of sound, caused measurement result is inaccurate;Substantially increase the accuracy of measurement result.
Refer to Fig. 5, it illustrates another embodiment of the present invention provide shale property measurement device block diagram, The shale property measurement device can be measured by the shale property shown in Fig. 1 that is implemented in combination with becoming of software, hardware or both Computing device in instrument it is some or all of.The shale property measurement device can include:Pressure acquisition module 410, concentration Computing module 420, diffusion coefficient computing module 430 and computing permeability module 440.
Pressure acquisition module 410, for obtaining n group pressure values, the n groups pressure value spreads for gas in shale samples During, the pressure value at the shale samples both ends of record is spaced at predetermined time intervals, it is described for each group of pressure value Pressure value includes the pressure value P for being placed with the input end of the rock core fastener of the shale samplesinWith the pressure value of the port of export Pout, n >=2 and n are integer.
Concentration calculation module 420, for calculating corresponding n groups concentration value according to the n groups pressure value, for each group Concentration value, the concentration value include the concentration value N of the input endinWith the concentration value N of the port of exportout
Diffusion coefficient computing module 430 obtains the shale for solving One-dimensional Diffusion Equation according to the n groups concentration value The diffusion coefficient D of sample, the diffusion coefficient D are used to reflect diffusion of the gas in the shale samples.
Wherein, the One-dimensional Diffusion Equation is:
Wherein, the L represents the length (m) of the shale samples;The N represents gas corresponding to position x and moment t Concentration value (kg/m3)。
Alternatively, the One-dimensional Diffusion Equation is:
Wherein, the L represents the length (m) of the shale samples;The N represents gas corresponding to position x and moment t Concentration value (kg/m3);Represent the incrementss of the adsorbed gas content corresponding to moment t;The ρ1Represent the shale Density (the kg/m of sample3);The ρ2Represent gas density (kg/m3)。
Computing permeability module 440, for following formula to be used to calculate the permeability k of the shale samples:
K=D μ φ βt
Wherein, the D represents the diffusion coefficient (m2/s);The μ represents fluid viscosity (Pas);The φ is represented The effecive porosity (%) of the shale samples;The βtRepresent the compressed coefficient (Pa under initial pore pressure-1)。
Optionally, described device further includes:Porosity calculation module 402.
Porosity calculation module 402, for following formula to be used to calculate the effecive porosity φ of the shale samples:
Wherein, the S represents the sectional area (m of the shale samples2);The L represents the length of the shale samples (m);The P1Represent pulse (MPa);The P2Represent balance pressure (MPa);The Z1Represent gas in pressure P1Under Compressibility factor;The Z2Represent gas in pressure P2Under compressibility factor;The V1Represent the input end with the rock core fastener Connected upstream gas volume of a container (m3);The VxRepresent the upstream gas container, the upstream inlet valve, the rock Volume (the m of pipeline between core holder and the downstream inlet valve3)。
Optionally, described device further includes:Adsorbed gas computing module 442.
Adsorbed gas computing module 442, for following formula to be used to calculate the adsorbed gas content Q of the shale samplesn
Wherein, the QnIt represents in n-th of adsorption equilibrium pressure Pn *Under, what the shale samples of unit mass were adsorbed Gas volume (m3/kg);The m represents the quality (kg) of the shale samples;The VnIt represents in n-th of adsorption equilibrium pressure Pn *Under, gas volume (m that the shale samples are adsorbed3);The T0 Represent room temperature (DEG C), the T represents experimental temperature (DEG C), the P0Represent standard atmospheric pressure (MPa), the VhRepresent with it is described Upstream gas volume of a container (the m that the input end of rock core fastener is connected3), the VφRepresent the hole of the rock core fastener Volume (m3), the PnRepresent n-th of pulse (MPa), the Pn *Represent n-th of adsorption equilibrium pressure (MPa), the Zn Represent gas in pressure PnUnder compressibility factor, the Zn *Represent gas in pressure Pn *Under compressibility factor;As n=1,
In conclusion shale property measurement device provided in this embodiment, by solving the one-dimensional diffused sheet pre-established Journey obtains the diffusion coefficient of shale samples, and then the permeability of shale samples is acquired according to diffusion coefficient;Solves background technology The assay method being related to does not consider the Non-Darcy's flow dynamic characteristic of shale gas and the shadow of adsorbed gas when measuring the permeability of shale The problem of sound, caused measurement result is inaccurate;When solving the permeability of shale samples, non-Darcy flow spy had both been considered Property, it is contemplated that the influence of adsorbed gas, substantially increases the accuracy of measurement result.
In addition, shale property measurement device provided in this embodiment, additionally provides the porosity of shale samples, free gas contains The computing module of the related physical quantities such as amount, adsorbed gas content realizes comprehensive, multi-angle synthesis measuring effect.
It should be noted that:Above-described embodiment provide shale property measurement device when measuring shale property, only more than The division progress of each function module is stated for example, in practical application, it can be as needed and by above-mentioned function distribution by difference Function module complete, i.e., the internal structure of equipment is divided into different function modules, with complete it is described above whole or Person's partial function.In addition, shale property measurement device and the method for shale property assay method that above-described embodiment provides are implemented Example belongs to same design, and specific implementation process refers to embodiment of the method, and which is not described herein again.
It should be appreciated that it is used in the present context, unless context clearly supports exception, singulative " one It is a " (" a ", " an ", " the ") be intended to also include plural form.It is to be further understood that "and/or" used herein is Finger includes one or the arbitrary and all possible combinations of more than one project listed in association.
The embodiments of the present invention are for illustration only, do not represent the quality of embodiment.
One of ordinary skill in the art will appreciate that hardware can be passed through by realizing all or part of step of above-described embodiment It completes, relevant hardware can also be instructed to complete by program, the program can be stored in a kind of computer-readable In storage medium, storage medium mentioned above can be read-only memory, disk or CD etc..
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and Within principle, any modifications, equivalent replacements and improvements are made should all be included in the protection scope of the present invention.

Claims (7)

1. a kind of shale property assay method, which is characterized in that the described method includes:
Obtain n group pressure values, the n groups pressure value is during gas spreads in shale samples, at predetermined time intervals between Pressure value every the shale samples both ends of record, for each group of pressure value, the pressure value includes being placed with the page The pressure value P of the input end of the rock core fastener of rock sample productinWith the pressure value P of the port of exportout, n >=2 and n are integer;
Corresponding n groups concentration value is calculated according to the n groups pressure value, for each group of concentration value, the concentration value includes institute State the concentration value N of input endinWith the concentration value N of the port of exportout
One-dimensional Diffusion Equation is solved according to the n groups concentration value and obtains the diffusion coefficient D of the shale samples, the diffusion coefficient D is used to reflect diffusion of the gas in the shale samples;
The permeability k of the shale samples is calculated using following formula:
K=D μ φ βt
Wherein, the D represents the diffusion coefficient (m2/s);The μ represents fluid viscosity (Pas);The φ represents the page The effecive porosity (%) of rock sample product;The βtRepresent the compressed coefficient (Pa under initial pore pressure-1),
Before the permeability k for calculating the shale samples, further include:
The effecive porosity φ of the shale samples is calculated using following formula:
<mrow> <mi>&amp;phi;</mi> <mo>=</mo> <mfrac> <mrow> <mfrac> <mrow> <msub> <mi>Z</mi> <mn>2</mn> </msub> <msub> <mi>P</mi> <mn>1</mn> </msub> <msub> <mi>V</mi> <mn>1</mn> </msub> </mrow> <mrow> <msub> <mi>Z</mi> <mn>1</mn> </msub> <msub> <mi>P</mi> <mn>2</mn> </msub> </mrow> </mfrac> <mo>-</mo> <msub> <mi>V</mi> <mn>1</mn> </msub> <mo>-</mo> <msub> <mi>V</mi> <mi>x</mi> </msub> </mrow> <mrow> <mi>S</mi> <mi>L</mi> </mrow> </mfrac> <mo>;</mo> </mrow>
Wherein, the S represents the sectional area (m of the shale samples2);The L represents the length (m) of the shale samples;It is described P1Represent pulse (MPa);The P2Represent balance pressure (MPa);The Z1Represent gas in pressure P1Under compression because Son;The Z2Represent gas in pressure P2Under compressibility factor;The V1Represent what is be connected with the input end of the rock core fastener Upstream gas volume of a container (m3);The VxRepresent the upstream gas container, the upstream inlet valve, core clamping Volume (the m of pipeline between device and the downstream inlet valve3)。
2. according to the method described in claim 1, it is characterized in that,
The One-dimensional Diffusion Equation is:
<mrow> <mfrac> <mrow> <mo>&amp;part;</mo> <mi>N</mi> </mrow> <mrow> <mo>&amp;part;</mo> <mi>t</mi> </mrow> </mfrac> <mo>=</mo> <mi>D</mi> <mfrac> <mrow> <msup> <mo>&amp;part;</mo> <mn>2</mn> </msup> <mi>N</mi> </mrow> <mrow> <mo>&amp;part;</mo> <msup> <mi>x</mi> <mn>2</mn> </msup> </mrow> </mfrac> <mo>,</mo> <mrow> <mo>(</mo> <mi>t</mi> <mo>&amp;GreaterEqual;</mo> <mn>0</mn> <mo>,</mo> <mn>0</mn> <mo>&lt;</mo> <mi>x</mi> <mo>&lt;</mo> <mi>L</mi> <mo>)</mo> </mrow> <mo>;</mo> </mrow>
Wherein, the L represents the length (m) of the shale samples;The N represents gas dense corresponding to position x and moment t Angle value (kg/m3);
Alternatively,
The One-dimensional Diffusion Equation is:
<mrow> <mfrac> <mrow> <mo>&amp;part;</mo> <mi>N</mi> </mrow> <mrow> <mo>&amp;part;</mo> <mi>t</mi> </mrow> </mfrac> <mo>+</mo> <msub> <mi>&amp;rho;</mi> <mn>1</mn> </msub> <msub> <mi>&amp;rho;</mi> <mn>2</mn> </msub> <mfrac> <mrow> <mo>&amp;part;</mo> <mi>Q</mi> </mrow> <mrow> <mo>&amp;part;</mo> <mi>t</mi> </mrow> </mfrac> <mo>=</mo> <mi>D</mi> <mfrac> <mrow> <msup> <mo>&amp;part;</mo> <mn>2</mn> </msup> <mi>N</mi> </mrow> <mrow> <mo>&amp;part;</mo> <msup> <mi>x</mi> <mn>2</mn> </msup> </mrow> </mfrac> <mo>,</mo> <mrow> <mo>(</mo> <mi>t</mi> <mo>&amp;GreaterEqual;</mo> <mn>0</mn> <mo>,</mo> <mn>0</mn> <mo>&lt;</mo> <mi>x</mi> <mo>&lt;</mo> <mi>L</mi> <mo>)</mo> </mrow> <mo>;</mo> </mrow>
Wherein, the L represents the length (m) of the shale samples;The N represents gas dense corresponding to position x and moment t Angle value (kg/m3);Represent the incrementss of the adsorbed gas content corresponding to moment t;The ρ1Represent the shale samples Density (kg/m3);The ρ2Represent gas density (kg/m3)。
3. method according to claim 1 or 2, which is characterized in that the method further includes:
The adsorbed gas content Q of the shale samples is calculated using following formulan
<mrow> <msub> <mi>Q</mi> <mi>n</mi> </msub> <mo>=</mo> <mfrac> <msub> <mi>V</mi> <mi>n</mi> </msub> <mi>m</mi> </mfrac> <mo>;</mo> </mrow>
Wherein, the QnIt represents in n-th of adsorption equilibrium pressure Pn *Under, gas that the shale samples of unit mass are adsorbed Volume (m3/kg);The m represents the quality (kg) of the shale samples;The VnIt represents in n-th of adsorption equilibrium pressure Pn * Under, gas volume (m that the shale samples are adsorbed3);The T0Table Show room temperature (DEG C), the T represents experimental temperature (DEG C), the P0Represent standard atmospheric pressure (MPa), the VhIt represents and the rock Upstream gas volume of a container (the m that the input end of core holder is connected3), the VφRepresent the pore-body of the rock core fastener Product (m3), the PnRepresent n-th of pulse (MPa), the Pn *Represent n-th of adsorption equilibrium pressure (MPa), the ZnTable Show gas in pressure PnUnder compressibility factor, the Zn *Represent gas in pressure Pn *Under compressibility factor;As n=1,
4. a kind of shale property measurement device, which is characterized in that described device includes:
Pressure acquisition module, for obtaining n group pressure values, the n groups pressure value is the process that gas is spread in shale samples In, the pressure value at the shale samples both ends of record is spaced at predetermined time intervals, for each group of pressure value, the pressure value The pressure value P of input end including the rock core fastener that is placed with the shale samplesinWith the pressure value P of the port of exportout, n >=2 And n is integer;
Concentration calculation module, for calculating corresponding n groups concentration value according to the n groups pressure value, for each group of concentration value, The concentration value includes the concentration value N of the input endinWith the concentration value N of the port of exportout
Diffusion coefficient computing module obtains the shale samples for solving One-dimensional Diffusion Equation according to the n groups concentration value Diffusion coefficient D, the diffusion coefficient D are used to reflect diffusion of the gas in the shale samples;
Computing permeability module, for following formula to be used to calculate the permeability k of the shale samples:
K=D μ φ βt
Wherein, the D represents the diffusion coefficient (m2/s);The μ represents fluid viscosity (Pas);The φ represents the page The effecive porosity (%) of rock sample product;The βtRepresent the compressed coefficient (Pa under initial pore pressure-1),
Described device further includes:
Porosity calculation module, for following formula to be used to calculate the effecive porosity φ of the shale samples:
<mrow> <mi>&amp;phi;</mi> <mo>=</mo> <mfrac> <mrow> <mfrac> <mrow> <msub> <mi>Z</mi> <mn>2</mn> </msub> <msub> <mi>P</mi> <mn>1</mn> </msub> <msub> <mi>V</mi> <mn>1</mn> </msub> </mrow> <mrow> <msub> <mi>Z</mi> <mn>1</mn> </msub> <msub> <mi>P</mi> <mn>2</mn> </msub> </mrow> </mfrac> <mo>-</mo> <msub> <mi>V</mi> <mn>1</mn> </msub> <mo>-</mo> <msub> <mi>V</mi> <mi>x</mi> </msub> </mrow> <mrow> <mi>S</mi> <mi>L</mi> </mrow> </mfrac> <mo>;</mo> </mrow>
Wherein, the S represents the sectional area (m of the shale samples2);The L represents the length (m) of the shale samples;It is described P1Represent pulse (MPa);The P2Represent balance pressure (MPa);The Z1Represent gas in pressure P1Under compression because Son;The Z2Represent gas in pressure P2Under compressibility factor;The V1Represent what is be connected with the input end of the rock core fastener Upstream gas volume of a container (m3);The VxRepresent the upstream gas container, the upstream inlet valve, core clamping Volume (the m of pipeline between device and the downstream inlet valve3)。
5. device according to claim 4, which is characterized in that
The One-dimensional Diffusion Equation is:
<mrow> <mfrac> <mrow> <mo>&amp;part;</mo> <mi>N</mi> </mrow> <mrow> <mo>&amp;part;</mo> <mi>t</mi> </mrow> </mfrac> <mo>=</mo> <mi>D</mi> <mfrac> <mrow> <msup> <mo>&amp;part;</mo> <mn>2</mn> </msup> <mi>N</mi> </mrow> <mrow> <mo>&amp;part;</mo> <msup> <mi>x</mi> <mn>2</mn> </msup> </mrow> </mfrac> <mo>,</mo> <mrow> <mo>(</mo> <mi>t</mi> <mo>&amp;GreaterEqual;</mo> <mn>0</mn> <mo>,</mo> <mn>0</mn> <mo>&lt;</mo> <mi>x</mi> <mo>&lt;</mo> <mi>L</mi> <mo>)</mo> </mrow> <mo>;</mo> </mrow>
Wherein, the L represents the length (m) of the shale samples;The N represents gas dense corresponding to position x and moment t Angle value (kg/m3);
Alternatively,
The One-dimensional Diffusion Equation is:
<mrow> <mfrac> <mrow> <mo>&amp;part;</mo> <mi>N</mi> </mrow> <mrow> <mo>&amp;part;</mo> <mi>t</mi> </mrow> </mfrac> <mo>+</mo> <msub> <mi>&amp;rho;</mi> <mn>1</mn> </msub> <msub> <mi>&amp;rho;</mi> <mn>2</mn> </msub> <mfrac> <mrow> <mo>&amp;part;</mo> <mi>Q</mi> </mrow> <mrow> <mo>&amp;part;</mo> <mi>t</mi> </mrow> </mfrac> <mo>=</mo> <mi>D</mi> <mfrac> <mrow> <msup> <mo>&amp;part;</mo> <mn>2</mn> </msup> <mi>N</mi> </mrow> <mrow> <mo>&amp;part;</mo> <msup> <mi>x</mi> <mn>2</mn> </msup> </mrow> </mfrac> <mo>,</mo> <mrow> <mo>(</mo> <mi>t</mi> <mo>&amp;GreaterEqual;</mo> <mn>0</mn> <mo>,</mo> <mn>0</mn> <mo>&lt;</mo> <mi>x</mi> <mo>&lt;</mo> <mi>L</mi> <mo>)</mo> </mrow> <mo>;</mo> </mrow>
Wherein, the L represents the length (m) of the shale samples;The N represents gas dense corresponding to position x and moment t Angle value (kg/m3);Represent the incrementss of the adsorbed gas content corresponding to moment t;The ρ1Represent the shale samples Density (kg/m3);The ρ2Represent gas density (kg/m3)。
6. device according to claim 4 or 5, which is characterized in that described device further includes:
Adsorbed gas computing module, for following formula to be used to calculate the adsorbed gas content Q of the shale samplesn
<mrow> <msub> <mi>Q</mi> <mi>n</mi> </msub> <mo>=</mo> <mfrac> <msub> <mi>V</mi> <mi>n</mi> </msub> <mi>m</mi> </mfrac> <mo>;</mo> </mrow>
Wherein, the QnIt represents in n-th of adsorption equilibrium pressure Pn *Under, gas that the shale samples of unit mass are adsorbed Volume (m3/kg);The m represents the quality (kg) of the shale samples;The VnIt represents in n-th of adsorption equilibrium pressure Pn * Under, gas volume (m that the shale samples are adsorbed3);The T0Table Show room temperature (DEG C), the T represents experimental temperature (DEG C), the P0Represent standard atmospheric pressure (MPa), the VhIt represents and the rock Upstream gas volume of a container (the m that the input end of core holder is connected3), the VφRepresent the pore-body of the rock core fastener Product (m3), the PnRepresent n-th of pulse (MPa), the Pn *Represent n-th of adsorption equilibrium pressure (MPa), the ZnTable Show gas in pressure PnUnder compressibility factor, the Zn *Represent gas in pressure Pn *Under compressibility factor;As n=1,
7. a kind of shale property analyzer, which is characterized in that the shale property analyzer includes:Upstream gas container, upstream Intake valve, for placing the rock core fastener of shale samples, downstream inlet valve, gas downstream container, upstream hydraulic pump, confining pressure liquid Press pump, downstream hydraulic pump, pressure sensor, differential pressure pickup, confining pressure intake valve, blow valve, insulating box, timer and calculating are set It is standby;
Wherein, the input end of the rock core fastener passes sequentially through the first valve of the upstream inlet valve, the upstream inlet Second valve of valve is connected with the first end of the upstream gas container;The port of export of the rock core fastener passes sequentially through described First valve of downstream inlet valve, the second valve of the downstream inlet valve are connected with the first end of the gas downstream container; The rock core fastener, the upstream gas container and the gas downstream container are installed in the insulating box;The upstream Hydraulic pump is connected by the first pipeline with the 3rd valve of the upstream inlet valve, the downstream hydraulic pump by the second pipeline with 3rd valve of the downstream inlet valve is connected;4th valve of the upstream inlet valve by the 3rd pipeline and the downstream into 4th valve of air valve is connected;5th valve of the upstream inlet valve is through the differential pressure pickup and the downstream inlet valve 5th valve is connected;The confining pressure hydraulic pump is connected through the confining pressure intake valve with the side wall of the rock core fastener;On described The second end of trip gas container is connected with the pressure sensor, the second end of the gas downstream container and the blow valve phase Even;The pressure sensor, the differential pressure pickup and the timer are connected respectively with the computing device;
The computing device, including the shale property measurement device as described in claim 4 to 6 is any.
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