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 PDFInfo
- Publication number
- 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
- Authority
- CN
- China
- Prior art keywords
- mrow
- gas
- pressure
- msub
- represent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 238000000034 method Methods 0.000 title claims abstract description 33
- 230000035699 permeability Effects 0.000 claims abstract description 53
- 238000005259 measurement Methods 0.000 claims abstract description 36
- 238000011144 upstream manufacturing Methods 0.000 claims description 100
- 238000009792 diffusion process Methods 0.000 claims description 97
- 239000011435 rock Substances 0.000 claims description 67
- 238000003556 assay Methods 0.000 claims description 27
- 238000001179 sorption measurement Methods 0.000 claims description 20
- 239000011148 porous material Substances 0.000 claims description 13
- 239000012530 fluid Substances 0.000 claims description 11
- 238000004364 calculation method Methods 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 9
- 230000006835 compression Effects 0.000 claims description 3
- 238000007906 compression Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims 1
- 238000000691 measurement method Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 201
- 238000002474 experimental method Methods 0.000 description 21
- 238000003795 desorption Methods 0.000 description 14
- 238000010586 diagram Methods 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 6
- 230000006870 function Effects 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 238000007872 degassing Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000013401 experimental design Methods 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 210000001367 artery Anatomy 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000000205 computational method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 210000003127 knee Anatomy 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000013178 mathematical model Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002052 molecular layer Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 210000003462 vein Anatomy 0.000 description 1
Landscapes
- Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
- Investigation Of Foundation Soil And Reinforcement Of Foundation Soil By Compacting Or Drainage (AREA)
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
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>&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>&part;</mo>
<mi>N</mi>
</mrow>
<mrow>
<mo>&part;</mo>
<mi>t</mi>
</mrow>
</mfrac>
<mo>=</mo>
<mi>D</mi>
<mfrac>
<mrow>
<msup>
<mo>&part;</mo>
<mn>2</mn>
</msup>
<mi>N</mi>
</mrow>
<mrow>
<mo>&part;</mo>
<msup>
<mi>x</mi>
<mn>2</mn>
</msup>
</mrow>
</mfrac>
<mo>,</mo>
<mrow>
<mo>(</mo>
<mi>t</mi>
<mo>&GreaterEqual;</mo>
<mn>0</mn>
<mo>,</mo>
<mn>0</mn>
<mo><</mo>
<mi>x</mi>
<mo><</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>&part;</mo>
<mi>N</mi>
</mrow>
<mrow>
<mo>&part;</mo>
<mi>t</mi>
</mrow>
</mfrac>
<mo>+</mo>
<msub>
<mi>&rho;</mi>
<mn>1</mn>
</msub>
<msub>
<mi>&rho;</mi>
<mn>2</mn>
</msub>
<mfrac>
<mrow>
<mo>&part;</mo>
<mi>Q</mi>
</mrow>
<mrow>
<mo>&part;</mo>
<mi>t</mi>
</mrow>
</mfrac>
<mo>=</mo>
<mi>D</mi>
<mfrac>
<mrow>
<msup>
<mo>&part;</mo>
<mn>2</mn>
</msup>
<mi>N</mi>
</mrow>
<mrow>
<mo>&part;</mo>
<msup>
<mi>x</mi>
<mn>2</mn>
</msup>
</mrow>
</mfrac>
<mo>,</mo>
<mrow>
<mo>(</mo>
<mi>t</mi>
<mo>&GreaterEqual;</mo>
<mn>0</mn>
<mo>,</mo>
<mn>0</mn>
<mo><</mo>
<mi>x</mi>
<mo><</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>&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>&part;</mo>
<mi>N</mi>
</mrow>
<mrow>
<mo>&part;</mo>
<mi>t</mi>
</mrow>
</mfrac>
<mo>=</mo>
<mi>D</mi>
<mfrac>
<mrow>
<msup>
<mo>&part;</mo>
<mn>2</mn>
</msup>
<mi>N</mi>
</mrow>
<mrow>
<mo>&part;</mo>
<msup>
<mi>x</mi>
<mn>2</mn>
</msup>
</mrow>
</mfrac>
<mo>,</mo>
<mrow>
<mo>(</mo>
<mi>t</mi>
<mo>&GreaterEqual;</mo>
<mn>0</mn>
<mo>,</mo>
<mn>0</mn>
<mo><</mo>
<mi>x</mi>
<mo><</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>&part;</mo>
<mi>N</mi>
</mrow>
<mrow>
<mo>&part;</mo>
<mi>t</mi>
</mrow>
</mfrac>
<mo>+</mo>
<msub>
<mi>&rho;</mi>
<mn>1</mn>
</msub>
<msub>
<mi>&rho;</mi>
<mn>2</mn>
</msub>
<mfrac>
<mrow>
<mo>&part;</mo>
<mi>Q</mi>
</mrow>
<mrow>
<mo>&part;</mo>
<mi>t</mi>
</mrow>
</mfrac>
<mo>=</mo>
<mi>D</mi>
<mfrac>
<mrow>
<msup>
<mo>&part;</mo>
<mn>2</mn>
</msup>
<mi>N</mi>
</mrow>
<mrow>
<mo>&part;</mo>
<msup>
<mi>x</mi>
<mn>2</mn>
</msup>
</mrow>
</mfrac>
<mo>,</mo>
<mrow>
<mo>(</mo>
<mi>t</mi>
<mo>&GreaterEqual;</mo>
<mn>0</mn>
<mo>,</mo>
<mn>0</mn>
<mo><</mo>
<mi>x</mi>
<mo><</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.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201410598715.1A CN105628575B (en) | 2014-10-30 | 2014-10-30 | Shale property determination method and device and shale property determination instrument |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201410598715.1A CN105628575B (en) | 2014-10-30 | 2014-10-30 | Shale property determination method and device and shale property determination instrument |
Publications (2)
Publication Number | Publication Date |
---|---|
CN105628575A CN105628575A (en) | 2016-06-01 |
CN105628575B true CN105628575B (en) | 2018-06-01 |
Family
ID=56043712
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201410598715.1A Active CN105628575B (en) | 2014-10-30 | 2014-10-30 | Shale property determination method and device and shale property determination instrument |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN105628575B (en) |
Families Citing this family (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108267390B (en) * | 2016-12-30 | 2020-07-10 | 中国石油天然气股份有限公司 | Method for determining gas permeability of reservoir containing nanopores |
CN107220432B (en) * | 2017-05-24 | 2020-11-03 | 长江勘测规划设计研究有限责任公司 | Method for calculating diffusion concentration distribution of radioactive gas in underground rock mass |
CN109900614A (en) * | 2017-12-11 | 2019-06-18 | 中国石油化工股份有限公司 | The method for measuring Oil in Super-low Permeability core permeability |
WO2019236466A1 (en) * | 2018-06-05 | 2019-12-12 | Saudi Arabian Oil Company | Systems and methods for analyzing natural gas flow in subterranean reservoirs |
CN109085112B (en) * | 2018-10-08 | 2023-08-22 | 中国石油天然气股份有限公司 | Method and device for measuring permeability of compact rock sample |
CN112859945B (en) * | 2021-01-15 | 2022-06-17 | 四川大学 | Calibration platform pore pressure control system and control method thereof |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5696448A (en) * | 1995-06-26 | 1997-12-09 | Numar Corporation | NMR system and method for formation evaluation using diffusion and relaxation log measurements |
WO2014088756A1 (en) * | 2012-12-06 | 2014-06-12 | Exxonmobil Research And Engineering Company | Gas separation method using ddr type zeolites with stabilized adsorption activity |
FR2999716B1 (en) * | 2012-12-14 | 2015-01-02 | IFP Energies Nouvelles | PROCESS FOR THE PETROPHYSICAL CHARACTERIZATION OF CLAY SEDIMENTARY ROCKS OF NON-CONVENTIONAL RESERVOIRS |
CN103575631B (en) * | 2013-11-06 | 2015-10-07 | 河海大学 | Rock permeability test macro and method of testing |
-
2014
- 2014-10-30 CN CN201410598715.1A patent/CN105628575B/en active Active
Also Published As
Publication number | Publication date |
---|---|
CN105628575A (en) | 2016-06-01 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN105628575B (en) | Shale property determination method and device and shale property determination instrument | |
CN204177799U (en) | Shale property tester | |
CN105910971B (en) | The simultaneous measuring method of rich organic matter compact rock core gas permeability and diffusion coefficient | |
CN106970000B (en) | Shale gas adsorption method for evaluating coal/shale ultrahigh-pressure gas adsorption and seepage experiments | |
Civan et al. | Determining shale permeability to gas by simultaneous analysis of various pressure tests | |
CN106814018B (en) | Device and method for measuring gas-phase relative permeability of tight rock | |
Liu et al. | Compressibility of sorptive porous media: Part 2. Experimental study on coal | |
Robertson et al. | Modeling laboratory permeability in coal using sorption-induced-strain data | |
CN104502224B (en) | Saturation water Coal Under rock isothermal desorption curve determination device and method | |
CN104897525B (en) | The test system and method for diffusion coefficient and isothermal adsorption/desorption curve | |
CN102353625B (en) | Method for measuring overburden porosity with water in permeation fluid mechanics experiment | |
Alnoaimi et al. | Characterization and measurement of multiscale gas transport in shale-core samples | |
CN104237099B (en) | Measure the device and method of compact rock core radial penetration rate | |
CN106932323B (en) | A kind of shale gas reservoir gas effecive porosity inversion method | |
CN104897554B (en) | Hypotonic rock gas pervasion test device and method of testing under vapor heat mechanics coupling effect | |
Lin et al. | Gas sorption and the consequent volumetric and permeability change of coal I: experimental | |
CN204649538U (en) | Rock three axle acoustic emission experiment device under a kind of confined pressure, hole press strip part | |
CN106198338A (en) | Shale reservoir fracturing fracture stress sensitivity testing device and method using same | |
Zamirian et al. | New steady-state technique for measuring shale core plug permeability | |
CN206095886U (en) | Multi -functional high temperature high pressure rock core formation water damage experiment evaluation device | |
Al Ismail et al. | The effect of CO2 adsorption on permeability anisotropy in the Eagle Ford shale | |
Abba et al. | Experimental investigation on the impact of connate water salinity on dispersion coefficient in consolidated rocks cores during Enhanced Gas Recovery by CO2 injection | |
CN106769790A (en) | Shale permeability test device and method based on fluid pressure pulse under a kind of ul-trasonic irradiation | |
CN108801879B (en) | Shale matrix particle porosity and permeability integrated measurement system and method | |
Fan et al. | Laboratory investigation of coal deformation behavior and its influence on permeability evolution during methane displacement by CO 2 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |