CN106066291A - CO2displacement shale gas and shale are to shale gas or CO2absorption analytic simulation test System and method for - Google Patents
CO2displacement shale gas and shale are to shale gas or CO2absorption analytic simulation test System and method for Download PDFInfo
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- CN106066291A CN106066291A CN201610425861.3A CN201610425861A CN106066291A CN 106066291 A CN106066291 A CN 106066291A CN 201610425861 A CN201610425861 A CN 201610425861A CN 106066291 A CN106066291 A CN 106066291A
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- 238000012360 testing method Methods 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000004088 simulation Methods 0.000 title claims abstract description 20
- 238000006073 displacement reaction Methods 0.000 claims abstract description 41
- 239000004576 sand Substances 0.000 claims abstract description 33
- 238000010521 absorption reaction Methods 0.000 claims abstract description 31
- 238000002474 experimental method Methods 0.000 claims abstract description 18
- 230000006835 compression Effects 0.000 claims abstract description 16
- 238000007906 compression Methods 0.000 claims abstract description 16
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 18
- 230000008569 process Effects 0.000 claims description 14
- 239000011435 rock Substances 0.000 claims description 14
- 238000001179 sorption measurement Methods 0.000 claims description 14
- 238000007789 sealing Methods 0.000 claims description 12
- 239000000872 buffer Substances 0.000 claims description 10
- 230000000694 effects Effects 0.000 claims description 7
- 238000001514 detection method Methods 0.000 claims description 6
- 235000013312 flour Nutrition 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 229920006395 saturated elastomer Polymers 0.000 claims description 6
- 239000010454 slate Substances 0.000 claims description 6
- 230000007797 corrosion Effects 0.000 claims description 4
- 238000005260 corrosion Methods 0.000 claims description 4
- 238000010828 elution Methods 0.000 claims description 4
- 239000012774 insulation material Substances 0.000 claims description 4
- 230000036772 blood pressure Effects 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000012544 monitoring process Methods 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 2
- 238000002513 implantation Methods 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 230000003139 buffering effect Effects 0.000 claims 1
- 238000004364 calculation method Methods 0.000 claims 1
- 238000011160 research Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 126
- 238000005516 engineering process Methods 0.000 description 5
- 239000012530 fluid Substances 0.000 description 5
- 230000033228 biological regulation Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000006641 stabilisation Effects 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3504—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N7/02—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder
- G01N7/04—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder by absorption or adsorption alone
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Abstract
A kind of CO2Displacement shale gas and shale are to shale gas or CO2Absorption analytic simulation test system, including CO2Gas cylinder and CH4Gas cylinder, CO2Gas cylinder and CH4Gas cylinder connects first piston container and the input of the second piston container respectively, the power drive end of first piston container and the second piston container is connected with power-driven system, outfan is connected to the input of fill out sand tube, and it is provided with vacuum pump and calibration system connecting on pipeline, fill out sand tube is placed in calorstat, and being connected with axial compression pump, outfan is connected to tail gas recycle bottle, and arranges back pressure control system and infrared gas analyzer on pipeline；Present invention also offers method based on this system, can simulate and test the CO of different conditions2Replacement result to shale gas under different temperatures, pressure condition；This experimental provision can also be utilized to carry out shale to CH simultaneously4Or CO2Absorption, resolve experiment, research shale gas absorption under different temperatures, pressure condition, resolve rule.
Description
Technical field
The invention belongs to Oil-Gas Field Development Engineering technical field, particularly to a kind of CO2Displacement shale gas and shale are to page
Rock gas (main component CH4) or CO2Absorption analytic simulation test System and method for
Background technology
China's shale gas resource is the abundantest, and the Efficient Development of shale gas is to alleviating China's energy supply and demand contradiction meaning weight
Greatly, owing to shale gas has the feature of low porosity and low permeability, exploitation shale gas must carry out reservoir fracturing.Therefore, the selection of fracturing fluid
Most important.Successfully exploit the experience of shale gas according to the U.S., mainly use hydraulic fracturing technology, but this technology needs to consume greatly
Amount water resource and also seriously polluted.
Either CO2Pressure break shale reservoir, or CO2Displacement shale gas, all can have CO2Displacement this phenomenon of shale gas, because of
This, CO2Displacement shale gas is one of current study hotspot both domestic and external as a kind of new technique developing shale gas.CO2Displaced page
Rock gas has three advantage: CO in principle2Can displacement sorption CH on shale4；CO2It is higher than CH with the adsorption strength of shale4；
CO2Rammell will not be made to produce clay swell, meanwhile, it is possible to achieve part CO2Bury in underground, it is achieved greenhouse gases subtract
Row, minimizing hydraulic fracturing technology, to environment, contributes to environmental protection, and advantage technically and economically determines that it will become
The new technique of following shale gas Efficient Development.
But, at present about CO2The testing research of displacement methane has some deficiency following, first, simulation test CO2With rock
The device of masonry is mainly used in test adsorption isotherm or adsorption isotherm process more, tests CO2Displacement CH4Device pole
Few；Secondly, CO2Displacement CH4Technology is more for coal petrography, few for shale；Finally, only CO2Displacement CH4Device institute
The gas measurement device used can not realize the real-time monitoring to replacement result.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, it is an object of the invention to provide a kind of CO2Displacement shale gas and page
Rock is to shale gas (main component CH4) or CO2Absorption analytic simulation test System and method for, can with real-time Simulation and test not
CO with state2Replacement result to shale gas under different temperatures, pressure condition.This experimental provision can also be utilized to enter simultaneously
Row shale core is to shale gas or CO2Absorption, resolve experiment, study shale core gas under different temperatures, pressure condition
Body absorption, parsing rule.
To achieve these goals, the technical solution used in the present invention is:
A kind of CO2Displacement shale gas and shale are to shale gas or CO2Absorption analytic simulation test system, including CO2Gas cylinder
9 and CH4Gas cylinder 17, CO2The port of export of gas cylinder 9 is connected to first piston container 7, CH4The port of export of gas cylinder 17 is connected to second and lives
Plug container 15, the power drive end of first piston container 7 and the second piston container 15 is all connected with hydraulic pressure power-driven system 57, defeated
Go out the input of the fill out sand tube 41 that end is all connected with being placed in calorstat 40 and on connecting line, be provided with vacuum pump 25 and mark
Determining system 58, the outfan of fill out sand tube 41 connects tail gas recycle bottle 56, and is provided with infrared gas analyser on connecting line
54 and back pressure control system 59.
Described CO2Gas cylinder 9 is sequentially connected with first booster pump the 10, second relief valve the 11, second pressure transducer the 12, the 3rd valve
8, first piston container 7 and the 4th valve 13, the outlet of the 4th valve 13 connects the 7th valve 21 and first-class gauge 22；
Described CH4Gas cylinder 17 is sequentially connected with the second booster pump the 18, the 3rd relief valve the 19, the 3rd pressure transducer the 20, the 6th
Valve the 16, second piston container 15 and the 7th valve 21, the outlet of the 7th valve 21 connects the 4th valve 13 and first-class gauge 22；
It is provided with check valve 23 and the 8th valve on the described vacuum pump 25 input first-class gauge 22 of connection and connecting line
24, the outfan of vacuum pump 25 is connected with the 5th relief valve 33.
Described pressure power drive system 57 includes that first reservoir the 1, first valve 2 being sequentially connected with, constant-flux pump 3, first are pressed
Force transducer 4 and the first relief valve 5, pressure power drive system 57 connects the drive end of first piston container 7 by the second valve 6,
The drive end of the second piston container 15 is connected by the 5th valve 14.
Described calibration system 58 includes standard chamber 30 and calibrated bolck room 32, is placed with the page of known volume in calibrated bolck room 32
Rock core sample block, the entrance of standard chamber 30 connects the outlet of check valve 23, and is provided with the 9th valve 26, in high precision on pipeline
Temperature sensor the 27, the 4th pressure transducer 28 and the 4th relief valve 29, export through the tenth valve 31 connection standard block room 32, demarcate
System 58 utilizes the state equation law of gas to demarcate from the manifold volume between the 4th valve 13 and the 7th valve 21 to back-pressure valve 46
With instrument internal volume.
Described fill out sand tube 41 is connected with the hydraulically powered axial compression pump 38 of dependence, and axial compression pump 38 effect is to be compacted in sample room 43
On slate flour, the pressured state of shale under simulation stratum condition, the input of axial compression pump 38 connect the second reservoir 36 and
Being provided with the 11st valve 37 on pipeline, outfan connects the input of fill out sand tube 41 and is provided with the 12nd valve 39 on pipeline, fills out
The input of sandpipe 41 is connected with the outfan of check valve 23 and arranges the 6th relief valve 34 and the 5th pressure biography on pipeline
Sensor 35, outfan is sequentially connected with the 6th pressure transducer the 44 and the 13rd valve 45, and fill out sand tube 41 is internal includes sample room 43 He
Connecting the piston with groove 42 of sample room 43, piston 42 is designed with groove on shale side pressing close to, and its object is to increase
Gas and the contact area of shale so that it is more abundant that gas displacement and adsorption process are carried out.
Described back pressure control system 59 is used for controlling fill out sand tube outlet pressures, simulates stressor layer state truly, its bag
Including electronic backpressure pump 50, back pressure buffer container 52 and back-pressure valve 46, electronic backpressure pump 50 input connects the 7th relief valve 49, defeated
Go out to terminate back pressure buffer container 52 and the 14th valve 51 is set in its pipeline, between back pressure buffer container 52 and back-pressure valve 46
Connecting line is provided with the 7th pressure transducer 47 and the 6th relief valve 48, the input of back-pressure valve 46 and the 13rd valve 45
Outfan connects, and outfan is sequentially connected with second gauge 53, infrared gas analyzer the 54, the 15th valve 55 and tail gas recycle
Container 56.
Described second gauge 53 and infrared gas analyzer 54, survey in real time to gas component and each composition flow rate
Amount, overcomes the shortcoming that measurement result is delayed compared with gas chromatographicanalyzer.
All connecting lines all use 316L pipeline, in case CO2Sour corrosion to pipeline；And connect the 3rd valve 8 and the
Seven valves 16 arrive all pipelines between second gauge 53, are wound around parcel with insulation material.
Present invention also offers based on described a kind of CO2Displacement shale gas and shale are to shale gas or CO2Absorption resolve mould
The method intending test system, including CO2Displacement shale gas analog detection method and shale core are to shale gas or CO2Absorption, solution
Analysis experimental technique, it is characterised in that
CO2Displacement shale gas analog detection method comprises the steps:
Step 1, sets experimental temperature to calorstat 40；
Step 2, test experience device sealing, it is ensured that sealing effectiveness；
Step 3, demarcates from the manifold volume between the 4th valve 13 and the 7th valve 21 to back-pressure valve 46；
Step 4, carries out evacuation to device, arranges the pressure of back-pressure valve 46；
Step 5, injects CH in shale core4Gas is to saturated；
Step 6, notes CO2Displacement CH4；
Step 7, processes experimental data；
Step 8, changes temperature, pressure that experiment sets, repeats above step, can obtain between pressure gas production
Relation between relation, temperature gas production, thus study the CO of different conditions2To shale under different temperatures, pressure condition
The replacement result of gas；
Shale core is to shale gas or CO2Absorption, resolve experimental technique comprise the steps:
Step 1, sets experimental temperature to calorstat 40；
Step 2, test experience device sealing, it is ensured that sealing effectiveness；
Step 3, demarcates from the manifold volume between the 4th valve 13 and the 7th valve 21 to back-pressure valve 46；
Step 4, carries out evacuation to device, arranges the pressure of back-pressure valve 46；
Step 5, injects CH to shale core4/CO2To saturated；
Step 6, blood pressure lowering resolves, and processes experimental data；
Step 7, changes temperature, pressure that experiment sets, repeats above step, available time adsorbance/parsing amount
Between relation, the relation between pressure adsorption amount/parsing amount, the relation between temperature adsorption amount/parsing amount, thus grind
Study carefully shale core gas absorption under different temperatures, pressure condition, resolve rule.
Compared with prior art, the invention has the beneficial effects as follows:
(1) present invention is exclusively used in simulation and tests the CO of different conditions2To shale gas under different temperatures, pressure condition
Replacement result.This experimental provision can also be utilized to carry out shale core to shale gas or CO simultaneously2Absorption, resolve experiment, grind
Study carefully shale core gas absorption under different temperatures, pressure condition, resolve rule.
(2) first booster pumps 10 and the second booster pump 18 are possible not only to play the effect of supercharging for system pipeline, it is also possible to
As required, select suitable specifications and models, set discharge capacity, the flow of regulation pump.
(3) method that the present invention reduces test error: is the pipeline using suitable internal diameter；Two is to use calibration system 58
Demarcating volume, calibration system 58 includes standard chamber 30 and calibrated bolck room 32, and calibration system 58 utilizes the state equation of gas to demarcate
From the manifold volume between the 4th valve 13 and the 7th valve 21 to back-pressure valve 46 and container volume, the mistake of test can be effectively reduced
Difference.
(4) calorstat 40 of the present invention can control the temperature of slate flour in fill out sand tube as required, and axial compression pump 38 can
So that slate flour is carried out compaction, with the pressure in back pressure control system 57 co-controlling fill out sand tube, not equality of temperature can be carried out
Displacement experiment under degree, pressure.
(5) present invention uses material to be slate flour, it is impossible to enough simulate as straight as a die replacement process.
(6) present invention includes second gauge 53 and infrared gas analyzer 54, it is possible to quickly measure mixed gas
Total volumetric flow rate and the concentration of each component, it is achieved the function of the amount of the real time measure fill out sand tube output each composition of gas, intuitively reflect
CO2Displacement CH4Effect.
(7) in apparatus of the present invention, all connecting lines all use 316L pipeline, in case CO2Sour corrosion to pipeline；And
Connect all pipeline insulation materials between the 3rd valve 8 and the 6th valve the 16 to the second gas flowmeter 53 and be wound around parcel, it is simple to
The test error that prevent heat from transmitting, scatter and disappear etc. causes.
Accompanying drawing explanation
Fig. 1 is present configuration schematic diagram.
Detailed description of the invention
Embodiments of the present invention are described in detail below in conjunction with the accompanying drawings with embodiment.
As it is shown in figure 1, a kind of CO2Displacement shale gas simulating test device, including CO2Gas cylinder 9 and CH4Gas cylinder 17, described
CO2Gas cylinder 9 and CH4Gas cylinder 17 connects first piston container 7 and the input of the second piston container 15, first piston container 7 respectively
Connecting with the power drive end of the second piston container 15 and have hydraulic pressure power-driven system 57, outfan is connected to fill out sand tube 41
Input, and it is provided with vacuum pump 25, calibration system 58 connecting on pipeline, fill out sand tube 41 is placed in calorstat 40, and
Being connected with axial compression pump 38, outfan is connected to tail gas recycle container 56, and arranges outside line gas analyser 54 and back pressure on pipeline
Control system 59, wherein:
CO2Gas cylinder 9 can access gas as required, should deposit downward-sloping for bottle mouth of gas cylinder when depositing, it is simple to stable
Ground storage and output CO2。CO2Gas cylinder 9 be sequentially connected with first booster pump the 10, second relief valve the 11, second pressure transducer 12,
Three valves 8, first piston container 7 and the 4th valve 13.The effect of the first booster pump 10 is to increase CO2The pressure of gas makes its pressure
Reach desired value.First piston container 7 uses fluid pressure drive device, can will have certain pressure CO2The injection that gas is stable
In fill out sand tube.
CH4Gas cylinder 17 can access gas as required, should deposit downward-sloping for bottle mouth of gas cylinder when depositing, it is simple to stable
Ground storage and output CH4。CH4Gas cylinder 17 be sequentially connected with the second booster pump 18, the 3rd relief valve 19, the 3rd pressure transducer 20,
Six valve the 16, second piston container 15 and the 7th valves 21.The effect of the second booster pump 18 is to increase CH4The pressure of gas makes it press
Power reaches desired value.Second piston container 15 uses fluid pressure drive device, can will have certain pressure CH4The note that gas is stable
Enter in fill out sand tube.
First piston container 7 and the second piston container 15 connect dynamic drive system 57, and power-driven system 57 is successively
Connecting and include first reservoir the 1, first valve 2, constant-flux pump the 3, first pressure transducer 4 and the first relief valve 5, constant-flux pump 3 is permissible
As required, select suitable specifications and models, set discharge capacity, it is possible to the flow of regulation pump.This device passes through the second valve 6 and the 5th valve
14 are respectively connecting to first piston container 7 and the drive end of the second piston container 15.
Vacuum pump 25 is connected to first piston container 7 and the second piston container 15, respectively through its port of export the 4th valve 13 He
7th valve 21 imports first-class gauge 22, and pipeline passes sequentially through check valve the 23, the 8th valve 24, and vacuum pump 25 port of export arranges
Five relief valve 33.
Calibration system 58 includes standard chamber 30 and calibrated bolck room 32, and calibration system 58 utilizes the state equation law mark of gas
Fixed from the manifold volume between the 4th valve 13 and the 7th valve 21 to back-pressure valve 46 and container volume, the entrance of standard chamber 30 connects single
To the outlet of valve 23, and be provided with on pipeline the 9th valve 26, temperature sensors of high precision 27, the 4th pressure transducer 28,
Four relief valve 29, outlet connects core block room 32 through the tenth valve 31.
Fill out sand tube 41 is positioned at calorstat 40, connects and has axial compression pump 38, axial compression pump 38 to rely on hydraulic-driven, and input connects
Second fluid reservoir 36, and on pipeline, it is provided with the 11st valve 37, outfan connects the input of fill out sand tube 41, and on pipeline
Being provided with the 12nd valve 39, the input of fill out sand tube 41 and the outfan of the 9th valve 26 are connected, and arrange the 6th peace on pipeline
Full valve 34 and the 5th pressure transducer 35, outfan is sequentially connected with the 6th pressure transducer the 44 and the 13rd valve 45.Fill out sand tube 41
In squeeze piston 42 and sample room 43 are set, piston face is provided with cuboid groove, its role is to increase gas injection time gas
With the contact area of slate flour, improve conventional efficient；Calorstat 40 and axial compression pump 38 can control fill out sand tube 41 as required
Temperature and pressure, simulate specific temperature and pressure condition, CO2Displacement CH4Process, but experimental subject is only shale powder
End, therefore can not effectively simulate as straight as a die displacement replacement process.
Back pressure control system 59 includes electronic backpressure pump 50, back pressure buffer container 52 and back-pressure valve 46.Electronic backpressure pump 50
Suitable specifications and models can be selected as required, set discharge capacity, pressure, it is possible to the flow of regulation pump.Electronic backpressure pump input
Being connected to the 7th relief valve 49, outfan is connected to back pressure buffer container 52, and arranges the 14th valve 51 in its pipeline, and back pressure buffers
Connecting line between container 52 and back-pressure valve 46 is provided with the 7th pressure transducer 47 and the 6th relief valve 48, back-pressure valve 46
Input and the 13rd valve 45 outfan connect, outfan is provided with second gauge 53.
Infrared gas analyzer 54 input is connected to the outfan of fill out sand tube 41, and arranges second flow on pipeline
Meter 53.Second gauge 53 can with meter gaseous total flow, infrared gas analyzer 54 can measure in real time gas component with
And concentration, fast and easy, outfan is connected to tail gas recycle container 56, and is provided with the 15th valve 55 on pipeline, and tail gas recycle is held
Discarded gas after device recovery experiment, plays the effect of protection environment.
In the present invention, first-class gauge 22, second gauge 53, infrared gas analyzer the 54, first pressure transducer
4, the second pressure transducer the 11, the 3rd pressure transducer the 19, the 4th pressure transducer the 28, the 5th pressure transducer the 35, the 6th pressure
Force transducer the 44, the 7th pressure transducer 47 and calorstat 40 be all connected with digital collection control card, can by gather pressure,
Temperature and data on flows process and generate initial data form, and analytical statement and curve chart generate database file form simultaneously
So that user flexibility uses.
In the present invention, all connecting lines all use 316L pipeline, in case CO2Sour corrosion to pipeline；And connect the 3rd
Valve 8 and the 6th valve 16 arrive all pipelines between second gauge 53, are wound around parcel with insulation material, it is simple to prevent heat from passing
The test error that pass, scatter and disappear etc. causes.
The present invention provides according to aforementioned CO2Displacement shale gas analog detection method, comprises the following steps:
Step 1, assembles experimental facilities according to the Experimental equipment of Fig. 1, calorstat 40 is set experimental temperature.
Step 2, test experience device sealing.
All valves of shutoff device, open the second valve the 2, the 5th valve the 14, the 6th valve 16 and the 7th valve 21, by CH4Gas cylinder
The CH of 174Gas proceeds in the second piston container 15, is pressurized to set pressure to the second piston container 15 with constant-flux pump 3.Close
Second valve the 2, the 5th valve 14 and the 6th valve 16, after stable, slowly open check valve 23, makes high pressure CH4Gas slowly proceeds to fill out
In sandpipe 41, experimental system is carried out work pressure test, determine that its sealing is good.
Step 3, demarcates from the manifold volume between the 4th valve 13 and the 7th valve 21 to back-pressure valve 46.
Open the 11st valve the 37 and the 12nd valve 39, utilize axial compression pump 38 to add certain axial compression by sample room 43 to fill out sand tube 41
Interior shale rubble is compacted, and closes the 11st valve the 37 and the 12nd valve 39 after compacting.
Open the 4th valve the 13, the 7th valve 21, check valve the 23, the 8th valve the 24, the 9th valve the 26 and the 13rd valve 45, utilize vacuum
Pump 25 carries out evacuation to first piston container the 7, second piston container 15 and pipeline, closes the 4th valve the 13, the 7th valve 21 and list
To valve 23, open the first valve the 2, the 5th valve 14 and the 6th valve 16, by CH4The CH of gas cylinder 174Gas proceeds to the second piston container 15
In, it is pressurized to set pressure to the second piston container 15 with constant-flux pump 3, closes the second valve the 2, the 5th valve 14 and the 6th valve 16, treat
After Wen Ding, slowly open the 7th valve 21 and check valve 23, after pressure stabilisation, record temperature sensors of high precision 27 and the 4th pressure
Registration T of force transducer 281And P1, taking out the calibrated bolck 1 of calibrated bolck room 32, standard chamber volume is V1, the volume of calibrated bolck 1 is
V ', opens the tenth valve 31, after temperature, pressure is stable, records temperature sensors of high precision 27 and the 4th pressure transducer 28
Registration T2And P2, can calculate from the manifold volume between the 4th valve 13 and the 7th valve 21 to back-pressure valve 46 according to ripple horse law accordingly:
V=(P2T1V1+P2T1V’-P1T2V1)/(P2T1-P2T1), close the 9th valve 26 after demarcation.
Step 4, carries out evacuation to device, arranges the pressure of back-pressure valve.
After closing all valves, open the 4th valve the 13, the 7th valve 21, first-class gauge the 22, the 8th valve the 23, the 9th valve 26 and
13rd valve 45, utilizes vacuum pump 25 that first piston container the 7, second piston container 15 and pipeline are carried out evacuation, evacuation
Rear cut out the 8th valve the 24 and the 13rd valve 45, opens the 14th valve 51, utilizes electronic backpressure pump 50 to increase back pressure buffer container 52
It is pressed onto setting pressure.After waiting to stablize, slowly opening back-pressure valve 46, the pressure keeping back-pressure valve 46 is constant.
Step 5, injects CH in shale core4Gas is to saturated.
Close check valve 23 and the 4th valve 13, open the first valve the 2, the 5th valve 14 and the 6th valve 16, by CH4The CH of gas cylinder 174
Gas proceeds in the second piston container 15, is pressurized to set pressure to the second piston container 15 with constant-flux pump 3, sets pressure and is closing
It is slightly above back pressure pressure in the range of reason, closes the second valve the 2, the 5th valve 14 and the 6th valve 16, after stable, slowly open check valve
23 and the 13rd valve 45, makes high pressure CH4Gas slowly proceeds in fill out sand tube 41, allows gas sufficiently be spread and to adsorb.So
Rear closedown check valve 23, allows gas fully be spread in rock core and farthest adsorbs.
Step 6, notes CO2Displacement CH4。
Open the first valve the 2, second valve 6 and the 3rd valve 8, by CO2The CO of gas cylinder 92Gas proceeds in first piston container 7, uses
First piston container 7 is pressurized to set pressure by constant-flux pump 3, sets pressure and slightly above sets back pressure pressure in the reasonable scope,
Close the first valve the 2, second valve 6 and the 3rd valve 8, after stable, slowly open the 4th valve 13, check valve 23, make CO2Fluid is slow
Proceed to, in core chamber 41, inject appropriate CO2After, close check valve 23.Ensure CO2At the time long enough of rock core, to reach to fill
Split and change CH4Purpose.
After pressure stabilisation, open the first valve the 2, second valve the 6, the 3rd valve 8 and check valve 23, by CO2The CO of gas cylinder 92Gas
Proceed in first piston container 7, be pressurized to set pressure to first piston container 7 with constant-flux pump 3, set pressure at zone of reasonableness
Interior slightly above setting back pressure pressure, closes the first valve the 2, second valve 6 and the 3rd valve 8, after stable, slowly opens check valve, logical
CO2CO is no longer gone out to infrared gas analyzer 542Till.
Step 7, processes experimental data.
CH4Adsorbance calculates: gone out to be passed through CH by first-class gauge 22 is measurable4Cumulative volume VinCH4, the CH that is passed through4One
Dividing and adsorb on shale with ADSORPTION STATE, a part is full of pipeline and volume for demarcating volume V, by temperature pressure sensing with free state
The pressure and temp value that device records, can calculate the CH being passed through4Quality m1 is totalWith free state CH4Quality m1 trip, do difference and i.e. can get CH4Inhale
Attached amount m1 inhales。
CO2The calculating of displacement methane content: said process can be learnt according to first-class gauge 22 and be passed through CO2Cumulative volume, root
CO is measured according to second gauge 53 and infrared gas analyzer 542Accumulative elution volume, remaining CO in the duct2Volume,
The pressure and temp value recorded by temperature and pressure transmitter can be calculated result and is respectively m2 is total,m2 go out,m2 trips, then CO is obtained2Absorption
Amount m2 inhale=m2 is total-m2 go out-m2 trips, wherein CO2Accumulative elution volume calculates according to monitoring volume integral in real time.
CH4/CO2The calculating of rock core implantation quality: utilize the above results, can assess replacement result.
Step 8, changes temperature, pressure that experiment sets, repeats above step, can obtain between pressure gas production
Relation etc. between relation, temperature gas production, thus study the CO of different conditions2To page under different temperatures, pressure condition
The replacement result of rock gas.
The present invention provides and carries out shale core to shale gas or CO according to previous experiments device2Absorption, resolve experiment, bag
Include following experimental procedure:
Step 1, assembles experimental facilities according to the Experimental equipment of Fig. 1, calorstat 40 is set experimental temperature.
Step 2, test experience device sealing.
All valves of shutoff device, open the second valve the 2, the 5th valve the 14, the 6th valve 16 and the 7th valve 21, by CH4Gas cylinder
The CH of 174Gas proceeds in the second piston container 15, is pressurized to set pressure to the second piston container 15 with constant-flux pump 3.Close
Second valve the 2, the 5th valve 14 and the 6th valve 16, after stable, slowly open check valve 23, makes high pressure CH4Gas slowly proceeds to fill out
In sandpipe 41, experimental system is carried out work pressure test, determine that its sealing is good.
Step 3, demarcates from the manifold volume between the 4th valve 13 and the 7th valve 21 to back-pressure valve 46.
Open the 11st valve the 37 and the 12nd valve 39, utilize axial compression pump 38 to add certain axial compression by sample room 43 to fill out sand tube 41
Interior shale rubble is compacted, and closes the 11st valve the 37 and the 12nd valve 39 after compacting.
Open the 4th valve the 13, the 7th valve 21, check valve the 23, the 8th valve the 24, the 9th valve the 26 and the 13rd valve 45, utilize vacuum
Pump 25 carries out evacuation to first piston container the 7, second piston container 15 and pipeline, closes the 4th valve the 13, the 7th valve 21 and list
To valve 23, open the first valve the 2, the 5th valve 14 and the 6th valve 16, by CH4The CH of gas cylinder 174Gas proceeds to the second piston container 15
In, it is pressurized to set pressure to the second piston container 15 with constant-flux pump 3, closes the second valve the 2, the 5th valve 14 and the 6th valve 16, treat
After Wen Ding, slowly open the 7th valve 21 and check valve 23, after pressure stabilisation, record temperature sensors of high precision 27 and the 4th pressure
Registration T of force transducer 281And P1, taking out the calibrated bolck 1 of calibrated bolck room 32, standard chamber volume is V1, the volume of calibrated bolck 1 is
V ', opens the tenth valve 31, after temperature, pressure is stable, records temperature sensors of high precision 27 and the 4th pressure transducer 28
Registration T2And P2, can calculate from the manifold volume between the 4th valve 13 and the 7th valve 21 to back-pressure valve 46 according to ripple horse law accordingly:
V=(P2T1V1+P2T1V’-P1T2V1)/(P2T1-P2T1), close the 9th valve 26 after demarcation.
Step 4, carries out evacuation to device, arranges the pressure of back-pressure valve.
After closing all valves, open the 4th valve the 13, the 7th valve 21, first-class gauge the 22, the 8th valve the 23, the 9th valve 26 and
13rd valve 45, utilizes vacuum pump 25 that first piston container the 7, second piston container 15 and pipeline are carried out evacuation, evacuation
Rear cut out the 8th valve the 24 and the 13rd valve 45, opens the 14th valve 51, utilizes electronic backpressure pump 50 to increase back pressure buffer container 52
It is pressed onto setting pressure.After waiting to stablize, slowly opening back-pressure valve 46, the pressure keeping back-pressure valve 46 is constant.
Step 5, injects CH to shale core4/CO2To saturated.
Note CH4: close check valve 23 and the 4th valve 13, open the first valve the 2, the 5th valve 14 and the 6th valve 16, by CH4Gas cylinder
The CH of 174Gas proceeds in the second piston container 15, is pressurized to set pressure to the second piston container 15 with constant-flux pump 3, sets
Pressure is slightly above back pressure pressure in the reasonable scope, closes the second valve the 2, the 5th valve 14 and the 6th valve 16, after stable, slowly beats
Opening one-way valve the 23 and the 13rd valve 45, makes high pressure CH4Gas slowly proceeds in fill out sand tube 41, allow gas sufficiently be spread and
Absorption.It is then shut off check valve 23, allows gas fully be spread in rock core and farthest adsorb.
Note CO2: close check valve 23 and the 7th valve 21, open the first valve the 2, second valve 6 and the 3rd valve 8, by CO2Gas 9
CO2Gas proceeds in first piston container 7, is pressurized to set pressure to first piston container 7 with constant-flux pump 3, sets pressure and exists
It is slightly above back pressure pressure in zone of reasonableness, closes the first valve the 2, second valve 6 and the 3rd valve 8, after stable, slowly open check valve
23 and the 13rd valve 45, makes high pressure CO2Gas slowly proceeds in fill out sand tube 41, allows gas sufficiently be spread and to adsorb.So
Rear closedown check valve 23, allows gas fully be spread in rock core and farthest adsorbs.
Step 6, blood pressure lowering resolves, and processes experimental data.
Computer is utilized to carry out Treatment Analysis the data (temperature, pressure, flow) gathered, available CH4/CO2To shale
Absorption/analytic curve.
Step 7, changes temperature, pressure that experiment sets, repeats above step, available time adsorbance/parsing amount
Between relation, the relation between pressure adsorption amount/parsing amount, the relation etc. between temperature adsorption amount/parsing amount, thus
Study shale core gas absorption under different temperatures, pressure condition, resolve rule.
Claims (10)
1.CO2Displacement shale gas and shale are to shale gas or CO2Absorption analytic simulation test system, it is characterised in that include
CO2Gas cylinder (9) and CH4Gas cylinder (17), CO2The port of export of gas cylinder (9) is connected to first piston container (7), CH4Gas cylinder (17)
The port of export is connected to the second piston container (15), and the power drive end of first piston container (7) and the second piston container (15) is equal
Connecting hydraulic pressure power-driven system (57), outfan is all connected with the input of fill out sand tube (41) that is placed in calorstat (40) also
Being provided with vacuum pump (25) and calibration system (58) on connecting line, the outfan of fill out sand tube (41) connects tail gas recycle bottle
(56) infrared gas analyser (54) and back pressure control system (59), and it are provided with on connecting line.
CO the most according to claim 12Displacement shale gas and shale are to shale gas or CO2Absorption analytic simulation test system,
It is characterized in that,
Described CO2Gas cylinder (9) be sequentially connected with the first booster pump (10), the second relief valve (11), the second pressure transducer (12),
Three valves (8), first piston container (7) and the 4th valve (13), the outlet of the 4th valve (13) connects the 7th valve (21) and first flow
Meter (22)；
Described CH4Gas cylinder (17) be sequentially connected with the second booster pump (18), the 3rd relief valve (19), the 3rd pressure transducer (20),
Six valves (16), the second piston container (15) and the 7th valve (21), the outlet of the 7th valve (21) connects the 4th valve (13) and first-class
Gauge (22)；
It is provided with check valve (23) and the 8th on described vacuum pump (25) the input first-class gauge of connection (22) and connecting line
Valve (24), the outfan of vacuum pump (25) is connected with the 5th relief valve (33).
CO the most according to claim 12Displacement shale gas and shale are to shale gas or CO2Absorption analytic simulation test system,
It is characterized in that, the first reservoir (1) that described pressure power drive system (57) includes being sequentially connected with, the first valve (2), constant-flux pump
(3), the first pressure transducer (4) and the first relief valve (5), pressure power drive system (57) connects first by the second valve (6)
The drive end of piston container (7), connects the drive end of the second piston container (15) by the 5th valve (14).
CO the most according to claim 12Displacement shale gas and shale are to shale gas or CO2Absorption analytic simulation test system,
It is characterized in that, described calibration system (58) includes standard chamber (30) and calibrated bolck room (32), and calibrated bolck room is placed with in (32)
The shale core sample blocks of known volume, the entrance of standard chamber (30) connects the outlet of check valve (23), and arranges on pipeline
There are the 9th valve (26), temperature sensors of high precision (27), the 4th pressure transducer (28) and the 4th relief valve (29), export through the
Ten valves (31) connection standard block room (32), calibration system (58) utilize the state equation law of gas to demarcate from the 4th valve (13) and
7th valve (21) is to the manifold volume between back-pressure valve (46) and instrument internal volume.
CO the most according to claim 12Displacement shale gas and shale are to shale gas or CO2Absorption analytic simulation test system,
It is characterized in that, described fill out sand tube (41) is connected with the hydraulically powered axial compression pump (38) of dependence, and axial compression pump (38) effect is compacting
On sample room (43) interior slate flour, the pressured state of shale under simulation stratum condition, the input of axial compression pump (38) connects the
Two reservoirs (36) are also provided with the 11st valve (37) on pipeline, and outfan connects the input of fill out sand tube (41) and at pipeline
Being provided with the 12nd valve (39), the input of fill out sand tube (41) is connected with the outfan of check valve (23) and arranges on pipeline
6th relief valve (34) and the 5th pressure transducer (35), outfan is sequentially connected with the 6th pressure transducer (44) and the 13rd valve
(45), the internal piston with groove (42) including sample room (43) and connecting sample room (43) of fill out sand tube (41), piston (42)
Be designed with groove pressing close on shale side, its object is to increase the contact area of gas and shale so that gas displacement and
It is more abundant that adsorption process is carried out.
CO the most according to claim 12Displacement shale gas and shale are to shale gas or CO2Absorption analytic simulation test system,
It is characterized in that, described back pressure control system (59) is used for controlling fill out sand tube outlet pressures, simulates stressor layer state truly,
It includes electronic backpressure pump (50), back pressure buffer container (52) and back-pressure valve (46), and electronic backpressure pump (50) input connects the
Seven relief valve (49), outfan takes back pressure buffer container (52) and arranges the 14th valve (51) in its pipeline, and back pressure buffering is held
Connecting line between device (52) and back-pressure valve (46) is provided with the 7th pressure transducer (47) and the 6th relief valve (48), returns
The outfan of the input of pressure valve (46) and the 13rd valve (45) connects, and outfan is sequentially connected with second gauge (53), infrared
Line gas analyser (54), the 15th valve (55) and tail gas recycle container (56).
CO the most according to claim 62Displacement shale gas and shale are to shale gas or CO2Absorption analytic simulation test system,
It is characterized in that gas component and each composition flow rate are entered by described second gauge (53) and infrared gas analyzer (54)
Row is measured in real time.
CO the most according to claim 12Displacement shale gas and shale are to shale gas or CO2Absorption analytic simulation test system,
It is characterized in that, all connecting lines all use 316L pipeline, in case CO2Sour corrosion to pipeline；And connect the 3rd valve (8)
And the 7th valve (16) to all pipelines between second gauge (53), be wound around parcel with insulation material.
9. one kind based on CO described in claim 12Displacement shale gas and shale are to shale gas or CO2Absorption analytic simulation test
The method of system, including CO2Displacement shale gas analog detection method and shale core are to shale gas or CO2Absorption, resolve experiment
Method, it is characterised in that
CO2Displacement shale gas analog detection method comprises the steps:
Step 1, sets experimental temperature to calorstat (40)；
Step 2, test experience device sealing, it is ensured that sealing effectiveness；
Step 3, demarcates from the manifold volume between the 4th valve (13) and the 7th valve (21) to back-pressure valve (46)；
Step 4, carries out evacuation to device, arranges the pressure of back-pressure valve (46)；
Step 5, injects CH in shale core4Gas is to saturated；
Step 6, notes CO2Displacement CH4；
Step 7, processes experimental data；
Step 8, changes temperature, pressure that experiment sets, repeats above step, can obtain the pass between pressure gas production
Relation between system, temperature gas production, thus study the CO of different conditions2To shale gas under different temperatures, pressure condition
Replacement result；
Shale core is to shale gas or CO2Absorption, resolve experimental technique comprise the steps:
Step 1, sets experimental temperature to calorstat (40)；
Step 2, test experience device sealing, it is ensured that sealing effectiveness；
Step 3, demarcates from the manifold volume between the 4th valve (13) and the 7th valve (21) to back-pressure valve (46)；
Step 4, carries out evacuation to device, arranges the pressure of back-pressure valve (46)；
Step 5, injects CH to shale core4/CO2To saturated；
Step 6, blood pressure lowering resolves, and processes experimental data；
Step 7, changes temperature, pressure that experiment sets, repeats above step, between available time adsorbance/parsing amount
Relation, the relation between pressure adsorption amount/parsing amount, the relation between temperature adsorption amount/parsing amount, thus study page
Rock rock core gas absorption under different temperatures, pressure condition, resolve rule.
Method the most according to claim 1, it is characterised in that
Described CO2In displacement shale gas analog detection method, process experimental data and include:
CH4Adsorbance calculates: is measured by first-class gauge (22) and is passed through CH4Cumulative volume VinCH4, the CH that is passed through4A part with
ADSORPTION STATE adsorb on shale, a part with free state be full of pipeline and volume for demarcate volume V, temperature and pressure transmitter survey
The pressure and temp value obtained, calculates the CH being passed through4Quality m1 is totalWith free state CH4Quality m1 trip, do difference and obtain CH4Adsorbance m1 inhales；
CO2Displacement methane content calculates: learns according to first-class gauge (22) and is passed through CO2Cumulative volume, according to second gauge (53)
CO is measured with infrared gas analyzer (54)2Accumulative elution volume, remaining CO in the duct2Volume, is passed by temperature, pressure
The pressure and temp value that sensor records calculates result and is respectively m2 is total,m2 go out,m2 trips, then CO is obtained2Adsorbance m2 inhale=m2 is total-m2 go out-
m2 trips, wherein CO2Accumulative elution volume calculates according to monitoring volume integral in real time.
CH4/CO2The calculating of rock core implantation quality: according to above-mentioned CH4Adsorbance and CO2The result of calculation of displacement methane content, assessment is put
Change effect.
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