CN105651648B - It is a kind of to replace and adsorb analytic simulation test system and method - Google Patents

It is a kind of to replace and adsorb analytic simulation test system and method Download PDF

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Publication number
CN105651648B
CN105651648B CN201610161910.7A CN201610161910A CN105651648B CN 105651648 B CN105651648 B CN 105651648B CN 201610161910 A CN201610161910 A CN 201610161910A CN 105651648 B CN105651648 B CN 105651648B
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valve
pressure
gas
shale
gas cylinder
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CN105651648A (en
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张健
郜时旺
张国祥
荆铁亚
王金意
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Huaneng Clean Energy Research Institute
China Huaneng Group Co Ltd
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Huaneng Clean Energy Research Institute
China Huaneng Group Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N7/00Analysing materials by measuring the pressure or volume of a gas or vapour
    • G01N7/14Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N7/00Analysing materials by measuring the pressure or volume of a gas or vapour
    • G01N7/02Analysing 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
    • G01N7/04Analysing 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

Abstract

It is a kind of to replace and adsorb analytic simulation test system, including the first gas cylinder and the second gas cylinder, the outlet of first gas cylinder and the second gas cylinder is connected to the input terminal of core chamber, and calibrating tube is provided on connecting line, vacuum pump and piston container, the output end of core chamber is connected to gas sample collection device, and vacuum pump is provided on connecting line, calibrating tube and back pressure control system, wherein, piston container is provided with oil bath device, injection pump and pressure sensor, core chamber is located in insulating box, it is connected with confining pressure pump, the input of core chamber, output end is respectively arranged with pressure sensor, the present invention also provides its analog detection methods, it can simulate and test the CO of different conditions2To the replacement result of shale gas under different temperatures, pressure condition, while shale core is carried out to shale gas or CO using the experimental provision2Absorption, parsing experiment, gas absorption of the research shale core under different temperatures, pressure condition, parsing rule.

Description

It is a kind of to replace and adsorb analytic simulation test system and method
Technical field
The invention belongs to CO2Shale gas technical field is developed, more particularly to a kind of displacement and absorption analytic simulation test system System and method.
Background technology
As a kind of new shale gas development technique --- CO2Shale gas is replaced, is that shale gas exploitation is ground in the world at present Study carefully one of hot spot.CO2It replaces shale gas and mainly utilizes CO2It is higher than CH with the adsorption strength of shale4, CO2Energy displacement sorption is in page CH on rock4, while improving yield and throughput rate, rammell will not be made to generate the effects such as clay swell, water lock, realized CO2Part is buried, and greater advantage is technically and financially all had, will be as the new technology of the following shale gas Efficient Development.
However, at present about CO2Replace methane testing research mostly be directed to coal petrography, for shale research very It is few, for special simulation test CO2The system and equipment of shale gas are replaced, there are no the sale of ripe product currently on the market.
Invention content
In order to overcome the disadvantages of the above prior art, the purpose of the present invention is to provide a kind of displacement and absorption analytic simulations System and method is tested, the CO of different conditions can be simulated and test2To the displacement of shale gas under different temperatures, pressure condition Effect.Shale core can also be carried out using the experimental provision simultaneously to shale gas or CO2Absorption, parsing experiment, study page Gas absorption, parsing rule of the rock rock core under different temperatures, pressure condition.
To achieve the goals above, the technical solution adopted by the present invention is:
It is a kind of to replace and adsorb analytic simulation test system, including the first gas cylinder 1 and the second gas cylinder 7, first gas cylinder 1 It is connected to the input terminal of core chamber 24 with the outlet of the second gas cylinder 7, and is provided with the first calibrating tube 14, on connecting line The output end of one vacuum pump 17 and first piston container 19, core chamber 24 is connected to gas sample collection device 43, and in connecting tube Road is provided with the second vacuum pump 30, the second calibrating tube 32 and back pressure control system 44, wherein:
It is single that first gas cylinder 1 is sequentially connected the first valve 2, first filter 3, first flowmeter 4, the second valve 5 and first To valve 6, the outlet of the first check valve 6 connects the 5th valve 13 and the 6th valve 15.
Second gas cylinder 7 is sequentially connected the second valve 8, the second filter 9, second flowmeter 10, the 4th valve 11 and second The outlet of check valve 12, the second check valve 12 connects the 5th valve 13 and the 6th valve 15.
First calibrating tube 14 is used to demarcate the volume of first piston container 19, and from the second valve 5 and the 4th valve 11 Manifold volume to the 8th valve 22, entrance the first check valve 6 of connection of the first calibrating tube 14 and going out for the second check valve 12 Mouthful, and the 5th valve 13 is provided on connecting line, the 6th valve 15 of outlet connection.
First vacuum pump 17, which is connected on first piston container 19 and connecting line, is provided with the 7th valve 16 and first Pressure sensor 18.
The first piston container 19 is located in oil bath device 20 and is connected with the first injection pump 21, first piston container 19 It is connected between the 6th valve 15 and the 8th valve 22, and is provided with first pressure sensor 18 on connecting line.
The core chamber 24 is located in insulating box 25, is connected with confining pressure pump 26, and the input terminal of core chamber 24 is sequentially connected the Two pressure sensors 23 and the 8th valve 22, output end are sequentially connected third pressure sensor 27 and the 9th valve 28.
Second vacuum pump 30, which is connected in the outlet and connecting line of core chamber 24, is connected with the tenth valve 29, in turn Nine valves 28 and third pressure sensor 27.
Second calibrating tube 32 is for demarcating from the manifold volume between 28 to the 15th valve 41 of the 9th valve, the second calibration Pipe 32 is connected between the 9th valve 28 and back-pressure valve 33 and is provided with the 11st valve 31 on connecting line.
The back pressure control system 44 includes back-pressure valve 33, second piston container 36, the second injection pump 37 and third gas cylinder 40.The third gas cylinder 40, is sequentially connected the 14th valve 39, third flowmeter 38, the 13rd valve 35,36 and of second piston container The 37, the 13rd valve 35 of second injection pump connects and is provided with the 12nd valve 34 on back-pressure valve 33 and connecting line.
The gas sample collection device 43 is sequentially connected the 4th flowmeter 42, the 15th valve 41 and back-pressure valve 33.
All connecting lines are all made of 316L pipelines in apparatus of the present invention, to prevent CO2To the sour corrosion of pipeline;And it connects Second valve 5 and the 4th valve 11 are wound with thermal insulation material and are wrapped up to all pipelines between gas sample collection device 43.
The present invention also provides the CO based on the test system2Shale gas and shale are replaced to shale gas or CO2Absorption solution Analyse analog detection method, wherein CO2Displacement shale gas analog detection method includes the following steps:
Step 1, experimental facilities is assembled according to the Experimental equipment of Fig. 1, to insulating box 25 and the setting experiment of oil bath device 20 Temperature.
Step 2, test experience device leakproofness.
Step 3, the volume of first piston container 19 is demarcated and between 11 to the 8th valve 22 of the second valve 5 and the 4th valve Manifold volume.
Step 4, it demarcates from the manifold volume between 28 to the 15th valve 41 of the 9th valve.
Step 5, device is vacuumized, the pressure of back-pressure valve 33 is set.
Step 6, CH is injected into shale core4Gas is extremely saturated.
Step 7, device is vacuumized, notes CO2Replace CH4
Step 8, gaseous sample is collected, experimental data is handled.
Step 9, temperature, the pressure for changing experiment setting, repeat above step, can obtain between pressure-gas production Relationship etc. between relationship, temperature-gas production, to study the CO of different conditions2To page under different temperatures, pressure condition The replacement result of rock gas.
Shale core is to shale gas or CO2Absorption, parsing experiment, include the following steps:
Step 1, experimental facilities is assembled according to the Experimental equipment of Fig. 1, to insulating box 25 and the setting experiment of oil bath device 20 Temperature.
Step 2, test experience device leakproofness.
Step 3, the volume of first piston container 19 is demarcated and between 11 to the 8th valve 22 of the second valve 5 and the 4th valve Manifold volume.
Step 4, it demarcates from the manifold volume between 28 to the 15th valve 41 of the 9th valve.
Step 5, device is vacuumized, the pressure of back-pressure valve 33 is set.
Step 6, CH is injected to shale core4/CO2To saturation.
Step 7, decompression parsing handles experimental data.
Step 8, temperature, the pressure for changing experiment setting, repeat above step, time-adsorbance/parsing amount can be obtained Between relationship, the relationship between pressure-adsorbance/parsing amount, the relationship etc. between temperature-adsorbance/parsing amount, to Study gas absorption, parsing rule of the shale core under different temperatures, pressure condition.
Compared with prior art, the beneficial effects of the invention are as follows:
(1) present invention is exclusively used in simulating and testing the CO of different conditions2To shale gas under different temperatures, pressure condition Replacement result.Shale core can also be carried out using the experimental provision simultaneously to shale gas or CO2Absorption, parsing experiment, grind Study carefully gas absorption, parsing rule of the shale core under different temperatures, pressure condition.Furthermore it is also possible to utilize the experimental provision Simulate CO2Pressure break or CO2It handles up experiment.
(2) first injection pumps 22 and the second injection pump 37 can be not only that system pipeline play the role of supercharging, can be with As needed, appropriate specifications and models are selected, discharge capacity is set, adjusts the flow of pump.
(3) present invention reduces the method for measurement error:First, using the pipeline of appropriate internal diameter;Second is that being demarcated using calibrating tube Volume, the first calibrating tube 14 are used to demarcate the volume of first piston container 19 and from 11 to the 8th valves of the second valve 5 and the 4th valve Manifold volume between 22, the second calibrating tube 32, can for demarcating from the manifold volume between 28 to the 15th valve 41 of the 9th valve To effectively reduce the error of measurement.
(4) insulating box 25 of the invention and confining pressure pump 26 can control the temperature and pressure of core chamber 24, mould as needed The temperature and pressure condition of quasi- some depth of stratum.
(5) present invention is using rock core confining pressure in 26 control core chamber 24 of confining pressure pump.This confining pressure should be consistently greater than drive in experiment For pressure.When preventing confining pressure too low, true displacement replacement process cannot be effectively simulated.
(6) gas sample collection device 43 of the invention can conveniently collect gaseous sample at regular time and quantity, recycle chromatography point Analyzer analyzes the ingredient and ratio of gaseous sample.
(7) all connecting lines are all made of 316L pipelines in apparatus of the present invention, to prevent CO2To the sour corrosion of pipeline;And The second valve 5 and the 4th valve 11 are connected to all pipelines between gas sample collection device 43, is wound and is wrapped up with thermal insulation material, is convenient for Prevent test error caused by heat transfer, lost etc..
Description of the drawings
Fig. 1 is schematic structural view of the invention.
Specific implementation mode
The embodiment that the present invention will be described in detail with reference to the accompanying drawings and examples.
As shown in Figure 1, simulated testing system of the present invention, including the first gas cylinder 1 and the second gas cylinder 7, outlet are connected to The input terminal of core chamber 24, and the first calibrating tube 14, the first vacuum pump 17 and first piston container are provided on connecting line 19, the output end of core chamber 24 is connected to gas sample collection device 43, and the second vacuum pump 30, are provided on connecting line Two calibrating tubes 32 and back pressure control system 44, wherein:
First gas cylinder 1 can flexibly select gas cylinder to access quantity as needed, and when storage should tilt down bottle mouth of gas cylinder Storage, convenient for steadily storage and output methane.First gas cylinder 1 is sequentially connected the first valve 2, first filter 3, first flowmeter 4, the second valve 5 and the first check valve 6.The effect of first filter 3 is that vapor mixed in removing original methane gas etc. is miscellaneous Matter, purification obtain high-purity methane gas.First check valve 6 can prevent reverse flow of fluids, outlet the 5th valve 13 of connection and the Six valves 15.
Second gas cylinder 7 can flexibly select gas cylinder to access quantity as needed, and when storage should tilt down bottle mouth of gas cylinder Storage, convenient for steadily storage and output CO2.Second gas cylinder 7 is sequentially connected the second valve 8, the second filter 9, second flowmeter 10, the 4th valve 11 and the second check valve 12.The effect of second filter 9 is to remove original CO2The vapor etc. mixed in gas Impurity, purification obtain high-purity CO2Gas.Second check valve 12 can prevent reverse flow of fluids, outlet connection 13 He of the 5th valve 6th valve 15.
First calibrating tube 14 is used to demarcate the volume of first piston container 19 and from the second valve 5 and the 4th valve 11 to the 8th Manifold volume between valve 22, the outlet of entrance connection the first check valve 6 and the second check valve 12 of the first calibrating tube 14, and The 5th valve 13, the 6th valve 15 of outlet connection are provided on connecting line.
First vacuum pump 17, which is connected on first piston container 19 and connecting line, is connected with the 7th valve 16 and first in turn Pressure sensor 18.
First piston container 19 is located in oil bath device 20 and is connected with the first injection pump 21, and the first injection pump 21 can root According to needs, appropriate specifications and models are selected, discharge capacity is set, the flow of pump can be adjusted.First piston container 19 is connected to the 6th valve 15 and the 8th between valve 22, and first pressure sensor 18 is provided on connecting line.
Core chamber 24 is located in insulating box 25, is connected with confining pressure pump 26, the input terminal of core chamber 24 is sequentially connected the second pressure Force snesor 23 and the 8th valve 22, output end are sequentially connected third pressure sensor 27 and the 9th valve 28.Insulating box 25 and confining pressure Pump 26 can control the temperature and pressure of core chamber 24 as needed, and the temperature and pressure condition of some depth of simulated formation is real This confining pressure should be consistently greater than displacement pressure in testing, and when preventing confining pressure too low, cannot effectively simulate true displacement replacement process.
Second vacuum pump 30 is connected in the outlet and connecting line of core chamber 24 and is connected with the tenth valve 29, the 9th valve in turn 28 and third pressure sensor 27.
Second calibrating tube 32 is for demarcating from the manifold volume between 28 to the 15th valve 41 of the 9th valve, the second calibrating tube 32 It is connected between the 9th valve 28 and back-pressure valve 33 and is provided with the 11st valve 31 on connecting line.
Back pressure control system 44 includes back-pressure valve 33, second piston container 36, the second injection pump 37 and third gas cylinder 40.The Three gas cylinders 40 can flexibly select gas cylinder to access quantity as needed, and bottle mouth of gas cylinder should be tilted down storage by when storage, be convenient for Steadily storage and output helium.Third gas cylinder 40 is sequentially connected the 14th valve 39, third flowmeter 38, the 13rd valve 35, Two piston containers 36 and the second injection pump 37.Second injection pump 37 can be as needed, selects appropriate specifications and models, setting row Amount, can adjust the flow of pump.13rd valve 35 connects and is provided with the 12nd valve 34 on back-pressure valve 33 and connecting line.
Gas sample collection device 43 is sequentially connected the 4th flowmeter 42, the 15th valve 41 and back-pressure valve 33.Gaseous sample is received Storage 43 can conveniently collect gaseous sample at regular time and quantity, recycle the ingredient and ratio of chromatograph analysis gaseous sample.
In the present invention, first flowmeter 4, second flowmeter 10, third flowmeter 38, first pressure sensor 18, second Pressure sensor 23, third pressure sensor 27 and insulating box 25 are all connected with digital collection control card, can be by the pressure of acquisition Power, temperature and data on flows processing generate initial data report, analytical statement and curve graph, while generating database file lattice Formula uses so as to user flexibility.
All connecting lines are all made of 316L pipelines in the present invention, to prevent CO2To the sour corrosion of pipeline;And connection second Valve 5 and the 4th valve 11 are wound with thermal insulation material and are wrapped up, convenient for preventing heat to all pipelines between gas sample collection device 43 Test error caused by transmission, lost etc..
The present invention is provided according to aforementioned CO2Shale gas analog detection method is replaced, is included the following steps:
Step 1, experimental facilities is assembled according to the Experimental equipment of Fig. 1, to insulating box 25 and the setting experiment of oil bath device 20 Temperature.
Step 2, test experience device leakproofness.
All valves of device are closed, the first valve 2, the second valve 5 and the 6th valve 15 are opened, by the CH of the first gas cylinder 14Gas It is transferred in first piston container 19, setting pressure is pressurized to first piston container 19 with the first injection pump 21.Close the first valve 2, the second valve 5 and the 6th valve 15 slowly open the 8th valve 22, make high pressure CH after stablizing4Gas slowly is transferred to core chamber 24 In, work pressure test is carried out to experimental system, determines that its leakproofness is good.
Step 3, the volume of first piston container 19 is demarcated and between 11 to the 8th valve 22 of the second valve 5 and the 4th valve Manifold volume.
The 6th valve 15, the 7th valve 16 and the 8th valve 22 are opened, using the first vacuum pump 17 to first piston container 19 and pipe Road is vacuumized, and the 6th valve 15, the 7th valve 16 and the 8th valve 22 are closed, and reads liquid level elemental height in the first calibrating tube 14, The 5th valve 13 is opened, liquid level rises in the first calibrating tube 14, the liquid level rise volume volume V to be demarcated1.Close the 5th Valve 13.
Step 4, it demarcates from the manifold volume between 28 to the 15th valve 41 of the 9th valve.
The tenth valve 29 is opened, pipeline is vacuumized using the second vacuum pump 30, closes the tenth valve 29, reads the second mark Liquid level elemental height in fixed tube 32 opens the 11st valve 31, and liquid level rises in the second calibrating tube 32, and liquid level rise volume is The manifold volume V to be demarcated2.Close the 11st valve 31.
Step 5, device is vacuumized, the pressure of back-pressure valve is set.
Using confining pressure pump 26 plus certain low confining pressure, the 6th valve 15, the 8th valve 22 and the 9th valve 28 are opened, it is true using first 17 and second vacuum pump 30 of empty pump vacuumizes device, closes all valves, and confining pressure pump 26 is recycled to increase confining pressures in fact Test requirement.The 13rd valve 35, the 14th valve 39 are opened, the helium of third gas cylinder 40 is transferred in second piston container 36, with Two injection pumps 37 are pressurized to setting pressure to second piston container 36, wait after stablizing, and slowly open the 12nd valve 34, allow gas Slowly full of the cavity in back-pressure valve 33, keep the pressure of back-pressure valve 33 constant.
Step 6, CH is injected into shale core4Gas is extremely saturated.
The first valve 2, the second valve 5 and the 6th valve 15 are opened, by the CH of the first gas cylinder 14Gas is transferred to first piston container 19 In, setting pressure is pressurized to first piston container 19 with the first injection pump 21.Close the first valve 2, the second valve 5 and the 6th valve 15, after stablizing, the 8th valve 22 is slowly opened, high pressure CH is made4Gas slowly is transferred in core chamber 24, in order to allow gas to be filled The diffusion and absorption divided, can be relatively low by the setting of confining pressure value, and the time persistently injected is depending on rock core size.It is then shut off Eight valves 22, allow gas to obtain fully spreading and adsorbing to the greatest extent in rock core, increase confining pressure to experiment using confining pressure pump 26 It is required that.
Step 7, device is vacuumized, notes CO2Replace CH4
The temperature that oil bath device 20 is arranged reaches requirement of experiment, and (same step 5) is vacuumized to device.Open third valve 8, the 4th valve 11 and the 6th valve 15, by the CO of the second gas cylinder 72Gas is transferred in first piston container 19, with the first injection pump 21 Setting pressure is pressurized to first piston container 19.Third valve 8, the 4th valve 11 and the 6th valve 15 is closed slowly to beat after stablizing The 8th valve 22 is opened, CO is made2Fluid is slowly transferred in core chamber 24, injects suitable CO2Afterwards, the 8th valve 22 is closed.Ensure CO2? The time long enough of rock core, CH is sufficiently displaced to reach4Purpose.
Step 8, gaseous sample is collected, experimental data is handled.
The 9th valve 28 and the 15th valve 41 are opened, while adjusting the pressure of back-pressure valve 33, keeps the pressure of back-pressure valve 33 gradual It reduces, and back-pressure valve 33 is kept to have certain rate of pressure reduction.After replacement completion, CO is re-injected2Replace residue CH4, replace repeatedly Until CH in gaseous sample4Amount it is sufficiently small, and relatively stablize.Using gaseous sample collector 43 to extraction gas every identical A period of time, quantitative repeatedly sampling recycles the ingredient and ratio of chromatograph analysis gaseous sample, demarcated plus second The export pipeline volume V that pipe 32 is demarcated2, the accumulation gas production of different time can be obtained.
CH4/CO2The calculating of rock core implantation quality:In volume V1 and first piston container that first calibrating tube 14 is demarcated The volume V that piston advances3, CH is converted into according to the equation of gas state4/CO2Quality m1And m3, utilize first flowmeter 4/ second Flowmeter 10 obtains CH4/CO2Total implantation quality m, (m-m1+m3) it is CH4/CO2Rock core implantation quality.
Processing analysis is carried out using computer to the data (temperature, pressure, flow) of acquisition, time-extraction can be obtained CH4/CO2Relationship, time-CH between amount4Relationship etc. between recovery ratio, to Analysis for CO2Replace the effect of shale gas.
Step 9, temperature, the pressure for changing experiment setting, repeat above step, can obtain between pressure-gas production Relationship etc. between relationship, temperature-gas production, to study the CO of different conditions2To page under different temperatures, pressure condition The replacement result of rock gas.
The present invention is provided according to aforementioned shale core to shale gas or CO2Absorption, analytic simulation test method, including with Lower step:
Step 1, experimental facilities is assembled according to the Experimental equipment of Fig. 1, to insulating box 25 and the setting experiment of oil bath device 20 Temperature.
Step 2, test experience device leakproofness.
All valves of device are closed, the first valve 2, the second valve 5 and the 6th valve 15 are opened, by the CH of the first gas cylinder 14Gas It is transferred in first piston container 19, setting pressure is pressurized to first piston container 19 with the first injection pump 21.Close the first valve 2, the second valve 5 and the 6th valve 15 slowly open the 8th valve 22, make high pressure CH after stablizing4Gas slowly is transferred to core chamber 24 In, work pressure test is carried out to experimental system, determines that its leakproofness is good.
Step 3, the volume of first piston container 19 is demarcated and between 11 to the 8th valve 22 of the second valve 5 and the 4th valve Manifold volume.
The 6th valve 15, the 7th valve 16 and the 8th valve 22 are opened, using the first vacuum pump 17 to first piston container 19 and pipe Road is vacuumized, and the 6th valve 15, the 7th valve 16 and the 8th valve 22 are closed, and reads liquid level elemental height in the first calibrating tube 14, The 5th valve 13 is opened, liquid level rises in the first calibrating tube 14, the liquid level rise volume volume V to be demarcated1.Close the 5th Valve 13.
Step 4, it demarcates from the manifold volume between 28 to the 15th valve 41 of the 9th valve.
The tenth valve 29 is opened, pipeline is vacuumized using the second vacuum pump 30, closes the tenth valve 29, reads the second mark Liquid level elemental height in fixed tube 32 opens the 11st valve 31, and liquid level rises in the second calibrating tube 32, and liquid level rise volume is The manifold volume V to be demarcated2.Close the 11st valve 31.
Step 5, device is vacuumized, the pressure of back-pressure valve is set.
Using confining pressure pump 26 plus certain low confining pressure, the 6th valve 15, the 8th valve 22 and the 9th valve 28 are opened, it is true using first 17 and second vacuum pump 30 of empty pump vacuumizes device, closes all valves, and confining pressure pump 26 is recycled to increase confining pressures in fact Test requirement.The 13rd valve 35, the 14th valve 39 are opened, the helium of third gas cylinder 40 is transferred in second piston container 36, with Two injection pumps 37 are pressurized to setting pressure to second piston container 36, wait after stablizing, and slowly open the 12nd valve 34, allow gas Slowly full of the cavity in back-pressure valve 33, keep the pressure of back-pressure valve 33 constant.
Step 6, CH is injected to shale core4/CO2To saturation.
Note CH4:The first valve 2, the second valve 5 and the 6th valve 15 are opened, by the CH of the first gas cylinder 14Gas is transferred to first piston appearance In device 19, setting pressure is pressurized to first piston container 19 with the first injection pump 21.Close the first valve 2, the second valve 5 and the 6th Valve 15 slowly opens the 8th valve 22, makes high pressure CH after stablizing4Gas slowly is transferred in core chamber 24.
Note CO2:Third valve 8, the 4th valve 11 and the 6th valve 15 are opened, by the CO of the second gas cylinder 72Gas is transferred to first piston In container 19, setting pressure is pressurized to first piston container 19 with the first injection pump 21.Close third valve 8,11 and of the 4th valve 6th valve 15 slowly opens the 8th valve 22, makes CO after stablizing2Fluid is slowly transferred in core chamber 24.
In order to allow gas adequately to be spread and be adsorbed, relatively low, the time persistently injected can be arranged in confining pressure value Depending on rock core size.It is then shut off the 8th valve 22, allows gas to obtain fully spreading and adsorbing to the greatest extent in rock core, profit Increase confining pressure to requirement of experiment with confining pressure pump 26.
Step 7, decompression parsing handles experimental data.
The 9th valve 28 and the 15th valve 41 are opened, while adjusting the pressure of back-pressure valve 33, keeps the pressure of back-pressure valve 33 gradual It reduces, and back-pressure valve 33 is kept to have certain rate of pressure reduction.The gas solution of different time can be obtained using the 4th flowmeter 42 Analysis amount.Processing analysis is carried out using computer to the data (temperature, pressure, flow) of acquisition, CH can be obtained4/CO2To shale Absorption/analytic curve.
Step 8, temperature, the pressure for changing experiment setting, repeat above step, time-adsorbance/parsing amount can be obtained Between relationship, the relationship between pressure-adsorbance/parsing amount, the relationship etc. between temperature-adsorbance/parsing amount, to Study gas absorption, parsing rule of the shale core under different temperatures, pressure condition.

Claims (7)

1. a kind of displacement and absorption analytic simulation test system, including the first gas cylinder (1) and the second gas cylinder (7), the first gas cylinder (1) Outlet with the second gas cylinder (7) is connected to the input terminal of core chamber (24), and the first calibrating tube is provided on connecting line (14), the first vacuum pump (17) and first piston container (19), the output end of core chamber (24) are connected to gas sample collection device (43), it and on connecting line is provided with the second vacuum pump (30), the second calibrating tube (32) and back pressure control system (44), In:
The first piston container (19) is located in oil bath device (20) and is connected with the first injection pump (21), first piston container (19) it is connected between the 6th valve (15) and the 8th valve (22), and is provided with first pressure sensor (18) on connecting line;
The core chamber (24) is located in insulating box (25), is connected with confining pressure pump (26), and the input terminal of core chamber (24) connects successively Second pressure sensor (23) and the 8th valve (22) are connect, output end is sequentially connected third pressure sensor (27) and the 9th valve (28);
The back pressure control system (44) includes back-pressure valve (33), second piston container (36), the second injection pump (37) and third Gas cylinder (40);
It is characterized in that,
First gas cylinder (1) be sequentially connected the first valve (2), first filter (3), first flowmeter (4), the second valve (5) and The outlet of first check valve (6), the first check valve (6) connects the 5th valve (13) and the 6th valve (15);Second gas cylinder (7) according to Secondary connection third valve (8), the second filter (9), second flowmeter (10), the 4th valve (11) and the second check valve (12), second The outlet of check valve (12) connects the 5th valve (13) and the 6th valve (15);
First calibrating tube (14) is used to demarcate the volumes of first piston container (19), and from the second valve (5) and the 4th valve (11) to the manifold volume between the 8th valve (22), the entrance of the first calibrating tube (14) connects the first check valve (6) and the second list Outlet to valve (12), and the 5th valve (13) is provided on connecting line, the 6th valve (15) of outlet connection;
Second calibrating tube (32) is for demarcating from the 9th valve (28) to the manifold volume between the 15th valve (41), the second mark Fixed tube (32) is connected between the 9th valve (28) and back-pressure valve (33) and is provided with the 11st valve (31) on connecting line;
Third gas cylinder (40) bottleneck tilts down storage, convenient for steadily storage and output helium.
2. replacing and adsorb analytic simulation according to claim 1 tests system, which is characterized in that first vacuum pump (17) it is connected on first piston container (19) and connecting line and is connected with the 7th valve (16) and first pressure sensor in turn (18)。
3. replacing and adsorb analytic simulation according to claim 1 tests system, which is characterized in that second vacuum pump (30) it is connected on the outlet of core chamber (24) and connecting line and is connected with the tenth valve (29), the 9th valve (28) and third pressure in turn Force snesor (27).
4. replacing and adsorb analytic simulation according to claim 1 tests system, which is characterized in that the third gas cylinder (40) It is sequentially connected the 14th valve (39), third flowmeter (38), the 13rd valve (35), second piston container (36) and the second injection pump (37), it is provided with the 12nd valve (34) on the 13rd valve (35) connection back-pressure valve (33) and connecting line.
5. replacing and adsorb analytic simulation according to claim 1 tests system, which is characterized in that the gas sample collection Device (43) is sequentially connected the 4th flowmeter (42), the 15th valve (41) and back-pressure valve (33).
6. replacing and adsorb analytic simulation according to claim 1 tests system, which is characterized in that all connecting tubes in device Road is all made of 316L pipelines, to prevent CO2To the sour corrosion of pipeline;And the second valve of connection (5) and the 4th valve (11) arrive gas sample All pipelines between product collector (43) are wound with thermal insulation material and are wrapped up.
7. a kind of based on the test method that analytic simulation test system is replaced and adsorbed described in claim 1, including CO2Displaced page Rock gas analog detection method and shale core are to shale gas or CO2Absorption, parsing experimental method, which is characterized in that
CO2Displacement shale gas analog detection method includes the following steps:
Step 1, experimental temperature is set to insulating box (25) and oil bath device (20);
Step 2, test experience device leakproofness;
Step 3, the volume of calibration first piston container (19) and from the second valve (5) and the 4th valve (11) to the 8th valve (22) it Between manifold volume;
Step 4, calibration is from the 9th valve (28) to the manifold volume between the 15th valve (41);
Step 5, device is vacuumized, the pressure of setting back-pressure valve (33);
Step 6, CH is injected into shale core4Gas is extremely saturated;
Step 7, device is vacuumized, notes CO2Replace CH4
Step 8, gaseous sample is collected, experimental data is handled;
Step 9, temperature, the pressure for changing experiment setting, repeat above step, obtain relationship, the temperature between pressure-gas production Relationship between degree-gas production, to study the CO of different conditions2To the displacement of shale gas under different temperatures, pressure condition Effect;
Shale core is to shale gas or CO2Absorption, parsing experiment include the following steps:
Step 1, experimental temperature is set to insulating box (25) and oil bath device (20);
Step 2, test experience device leakproofness;
Step 3, the volume of calibration first piston container (19) and from the second valve (5) and the 4th valve (11) to the 8th valve (22) it Between manifold volume;
Step 4, calibration is from the 9th valve (28) to the manifold volume between the 15th valve (41);
Step 5, device is vacuumized, the pressure of setting back-pressure valve (33);
Step 6, CH is injected to shale core4/CO2To saturation;
Step 7, decompression parsing handles experimental data;
Step 8, temperature, the pressure for changing experiment setting, repeat above step, obtain between time-adsorbance/parsing amount Relationship, the relationship between relationship, temperature-adsorbance/parsing amount between pressure-adsorbance/parsing amount, to study shale Gas absorption, parsing rule of the rock core under different temperatures, pressure condition.
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CN106093345B (en) * 2016-06-16 2017-12-08 中国华能集团公司 One kind simulation CO2The method that the pneumatic state process of shale is replaced in displacement
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