CN106093345B - One kind simulation CO2The method that the pneumatic state process of shale is replaced in displacement - Google Patents

One kind simulation CO2The method that the pneumatic state process of shale is replaced in displacement Download PDF

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CN106093345B
CN106093345B CN201610425862.8A CN201610425862A CN106093345B CN 106093345 B CN106093345 B CN 106093345B CN 201610425862 A CN201610425862 A CN 201610425862A CN 106093345 B CN106093345 B CN 106093345B
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valve
pressure
gas
shale
displacement
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CN106093345A (en
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张健
张国祥
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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Abstract

The invention provides one kind to simulate CO2Slate flour sample, based on corresponding analogue means, is mainly placed in the sample room of fill out sand tube by the method that the pneumatic state process of shale is replaced in displacement, and the original state of sample is set according to actual formation condition, after calibration pipeline volume, is passed through appropriate CH4, then carry out CO2Displacement displacement shale gas experiment, according to the volume flowmeter of arrival end and the volume flowmeter and infrared ray gas analyzer determination experiment data of the port of export, displacement replacement result can be evaluated by calculating.The present invention can monitor the action effect of displacement replacement process in real time, obtain the factors such as temperature, pressure, injection discharge capacity to CO2CH is replaced in displacement4Dynamic process affecting laws.

Description

One kind simulation CO2 The method that the pneumatic state process of shale is replaced in displacement
Technical field
The invention belongs to Oil-Gas Field Development Engineering technical field, more particularly to a kind of simulation CO2Displacement displacement shale is pneumatic The method of state process.
Background technology
With being deepened continuously to shale gas resources exploration, related hydraulic fracturing technology is also gradually ripe, meanwhile, The technology needs to consume great lot of water resources and is also concerned by people the problems such as can producing pollution to stratum.CO2Displacement Displacement shale gas is one of current focus studied both at home and abroad as a kind of new technology for developing shale gas.Current research CO2 The method of displacement displacement is directed to coal seam more, less for shale;Secondly, on CO2Displacement displacement shale gas device mostly by It is limited to measurement apparatus, it is difficult to be monitored in real time to experiment process.Therefore, data result of calculation has necessarily with regard to experimentation Hysteresis quality, it is impossible in real time to replacement result carry out quantitative assessment.
The content of the invention
The shortcomings that in order to overcome above-mentioned prior art, it is an object of the invention to provide one kind to simulate CO2Displacement displaced page The method of rock gas dynamic process, can with real-time Simulation and test different temperatures, pressure, flow CO2In different temperatures, pressure strip To the replacement result of shale gas under part, and for a certain replacement result, the action rule of pressure and temperature can be analyzed.
To achieve these goals, the technical solution adopted by the present invention is:
One kind simulation CO2Displacement replace the pneumatic state process of shale method, based on analogue means include:
CO2Gas cylinder 9, be sequentially connected the first booster pump 10, the second safety valve 11, second pressure sensor 12, the 3rd valve 8, The valve 13 of first piston container 7 and the 4th, the outlet of the 4th valve 13 connect the 7th valve 21 and first flowmeter 22;
The CH4Gas cylinder 17, it is sequentially connected the second booster pump 18, the 3rd safety valve 19, the 3rd pressure sensor the 20, the 6th Valve 16, the valve 21 of second piston container 15 and the 7th, the outlet of the 7th valve 21 connect the 4th valve 13 and first flowmeter 22;
Hydraulic pressure power-driven system 57, including be sequentially connected the first reservoir 1, the first valve 2, constant-flux pump 3, first pressure The safety valve 5 of sensor 4 and first, the drive end that power-driven system 57 connects first piston container 7 by the second valve 6 is pressed, led to Cross the drive end of the 5th valve 14 connection second piston container 15;
Fill out sand tube 41, it is placed in insulating box 40, the output end of connection first piston container 7 and second piston container 15;
Vavuum pump 25, the input of vavuum pump 25 connects is provided with the He of check valve 23 on first flowmeter 22 and connecting line 8th valve 24, the output end of vavuum pump 25 are connected with the 5th safety valve 33;
The calibration system 58, including standard chamber 30 and calibrated bolck room 32, known volume is placed with calibrated bolck room 32 Shale core sample blocks, the outlet of the entrance connection check valve 23 of standard chamber 30, and it is provided with pipeline the 9th valve 26, high-precision Temperature sensor 27, the 4th pressure sensor 28 and the 4th safety valve 29 are spent, is exported through the tenth valve 31 connection calibrated bolck room 32;
Tail gas recycle bottle 56, connect the output end of fill out sand tube 41;
Back pressure control system 59, for controlling fill out sand tube outlet pressures, true strata pressure state is simulated, it includes electricity Dynamic backpressure pump 50, back pressure buffer container 52 and back-pressure valve 46, the electronic input of backpressure pump 50 connect the 7th safety valve 49, output end Take back pressure buffer container 52 and the 14th valve 51, the connection between back pressure buffer container 52 and back-pressure valve 46 are set in its pipeline The 7th pressure sensor 47 and the 6th safety valve 48, the output of the input of back-pressure valve 46 and the 13rd valve 45 are provided with pipeline End connection, output end are sequentially connected second flowmeter 53, infrared ray gas analyzer 54, the 15th valve 55 and tail gas recycle container 56;
Infrared gas analyser 54, it is arranged on the connecting line of fill out sand tube 41 and tail gas recycle bottle 56;
It is characterised in that it includes following steps:
Step 1, experimental temperature is set to insulating box 40;
Step 2, test experience device sealing;
Step 3, operate calibration system 58, using gas the demarcation of state equation law from the 4th valve 13 and the 7th valve 21 to Manifold volume between back-pressure valve 46;
Step 4, vavuum pump 25 is opened, device is vacuumized, the pressure of back-pressure valve 46 is set;
Step 5, CH is provided first4The CH of gas cylinder 174Gas boosting, by hydraulic pressure power-driven system 57 to fill out sand tube 41 Middle injection CH4Gas, the data of the arrival end first flowmeter 22 of fill out sand tube 41 are recorded, keep fill out sand tube 41 and relevant apparatus constant temperature Constant pressure certain time is to saturation;
Step 6, CO is continually fed into constant flow2, simulate CO2The dynamic process of shale gas is replaced, until fill out sand tube 41 CH is can't detect in the gas of port of export outflow4Untill, record first flowmeter 22, second flowmeter 53 and infrared in real time therebetween The data of line gas analyzer 54;
Step 7, CH is calculated according to experimental data4Adsorbance and CO2Shale tolerance is replaced, test and assess CO2Replace CH4Effect;
Step 8, change temperature, the pressure of experiment setting, repeat above step, obtain the pass between pressure-displacement tolerance System, the relation between temperature-displacement tolerance, so as to study different temperatures, pressure, flow velocity CO2In different temperatures, pressure strip To the replacement result of shale gas under part.
The fill out sand tube 41 is connected with the axle press pump 38 by hydraulic-driven, and the effect of axle press pump 38 is to be compacted in sample room 43 On slate flour, the pressured state of shale under simulation stratum condition, the input of axle press pump 38 connect the second reservoir 36 and The 11st valve 37 is provided with pipeline, the input of output end connection fill out sand tube 41 is simultaneously provided with the 12nd valve 39 on pipeline, filled out The input of sandpipe 41 is connected with the output end of check valve 23 and sets the 6th safety valve 34 and the 5th pressure to pass on pipeline Sensor 35, output end are sequentially connected the 6th pressure sensor 44 and the 13rd valve 45, and the inside of fill out sand tube 41 includes the He of sample room 43 The piston with groove 42 of sample room 43 is connected, piston 42 designs fluted on shale side is pressed close to, and its object is to increase The contact area of gas and shale so that gas displacement and adsorption process are carried out more abundant.
Demarcation is from the 4th valve 13 and the 7th valve 21 to the manifold volume between back-pressure valve 46 in the step 3, including following Step:
The 11st valve 37 and the 12nd valve 39 are opened, adds a dead axle pressure by sample room 43 to fill out sand tube 41 using axle press pump 38 Interior slate flour sample compacting, closes the 11st valve 37 and the 12nd valve 39 after compacting, open the 4th valve 13, the 7th valve 21, list To valve 23, the 8th valve 24, the 9th valve 26 and the 13rd valve 45, using vavuum pump 25 to first piston container 7, second piston container 15 and pipeline vacuumized, close the 4th valve 13, the 7th valve 21 and check valve 23, open the first valve 2, the 5th valve 14 and the Six valves 16, by CH4The CH of gas cylinder 174Gas is transferred in second piston container 15, and second piston container 15 is pressurized with constant-flux pump 3 To setting pressure, the second valve 2, the 5th valve 14 and the 6th valve 16 are closed, after stable, slowly opens the 7th valve 21 and check valve 23, it is after pressure stabilisation, record the registration T of the pressure sensor 28 of temperature sensors of high precision 27 and the 4th1And P1, take out standard The calibrated bolck one of block room 32, standard building volume are V1, the volume of calibrated bolck one is V, opens the tenth valve 31, treats that temperature, pressure is stable Afterwards, the registration T of the pressure sensor 28 of temperature sensors of high precision 27 and the 4th is recorded2And P2, accordingly according to the equation of gas state Law can be calculated from the 4th valve 13 and the 7th valve 21 to the manifold volume between back-pressure valve 46:
V '=(P2T1V1+P2T1V-P1T2V1)/(P2T1-P2T1), the 9th valve 26 is closed after demarcation.
CO is simulated in the step 62The dynamic process of shale gas is replaced, specifically includes following steps:
The first valve 2, the second valve 6 and the 3rd valve 8 are opened, by CO2The CO of gas cylinder 92Gas is transferred in first piston container 7, is used Constant-flux pump 3 is pressurized to setting pressure to first piston container 7, and setting pressure is slightly above back pressure pressure, closed in the reasonable scope First valve 2, the second valve 6 and the 3rd valve 8, after stable, the 4th valve 13, check valve 23 are slowly opened, makes CO2Fluid is slowly transferred to It is after pressure stabilisation in fill out sand tube 41, the first valve 2, the second valve 6, the 3rd valve 8 and check valve 23 are opened, by CO2The CO of gas cylinder 92 Gas is transferred in first piston container 7, setting pressure is pressurized to first piston container 7 with constant-flux pump 3, setting pressure is reasonable In the range of slightly above back pressure pressure, close the first valve 2, the second valve 6 and the 3rd valve 8, after stable, slowly open check valve, lead to CO2Until can't detect CH in the gas of port of export outflow4Untill.
CH is calculated in the step 74The method of adsorbance is as follows:
Go out to be passed through CH by first flowmeter 22 is measurable4Cumulative volume VinCH4, the CH that is passed through4A part is adsorbed with ADSORPTION STATE On shale samples, a part is full of pipeline using free state and volume is demarcation volume V, the pressure measured by temperature and pressure transmitter Power temperature value, the CH being passed through can be calculated4Quality m1 is totalWith free state CH4Quality m1 trip, make the difference and can obtain CH4Adsorbance m1 inhales
CO is calculated in the step 72The method for replacing shale tolerance is as follows:
Learnt according to first flowmeter 22 and be passed through CO2Cumulative volume, according to second flowmeter 53 and infrared ray gas analysis Instrument 54 measures CO2Accumulative elution volume, remaining CO in the duct2Volume, the pressure and temp measured by temperature and pressure transmitter Value, can calculate CO2Accumulative be passed through quality m2 is total, accumulative outflow quality m2 go outWith free state CO2Quality m2 trips, then CO is obtained2Absorption Measure m2 inhale=m2 is total-m2 go out-m2 trips, wherein CO2Accumulative elution volume is calculated according to real-time monitoring volume integral.
Compared with prior art, advantage of the invention is:
(1) present invention is exclusively used in simulating CO2The dynamic process of shale gas, the side of Real-Time Evaluation replacement result are replaced in displacement Method.
(2) present invention reduces the method for test error:First, the pipeline using appropriate internal diameter;Second, use calibration system 58 Volume is demarcated, calibration system 58 includes standard chamber 30 and calibrated bolck room 32, and calibration system 58 is demarcated using the state equation of gas From the 4th valve 13 and the 7th valve 21 to the manifold volume and container volume between back-pressure valve 46, the mistake of test can be effectively reduced Difference.
(4) insulating box 40 of the invention can control the temperature of slate flour sample in fill out sand tube, axle press pump as needed 38 can carry out the pressure in compaction, with the co- controlling fill out sand tube of back pressure control system 57 to slate flour sample, can enter Displacement experiment under row different temperatures, pressure.
(5) present invention using material is slate flour, being capable of more true simulation after compacting compared with shale particle The truth of layer, is easier to realize displacement replacement process compared with true core.
(6) present invention includes second flowmeter 53 and infrared ray gas analyzer 54, can quickly measure mixed gas The concentration of total volumetric flow rate and each component, the function of the amount of each composition of real time measure fill out sand tube output gas is realized, reflection directly perceived CO2Replace CH4Effect.
Brief description of the drawings
Fig. 1 is the structural representation for the analogue means that the present invention is based on.
Embodiment
Describe embodiments of the present invention in detail with reference to the accompanying drawings and examples.
A kind of simulation CO of the invention2The method that the pneumatic state process of shale is replaced in displacement, its principle are:
Slate flour sample is placed in fill out sand tube first, the original state of sample specimens is set according to actual formation condition (including temperature and pressure);The air-tightness of check device;Using calibration system, manifold volume is demarcated using calibrated bolck;Open true Empty pump vacuumizes device, and operation back pressure control system sets back pressure;Open CH4The booster pump and power-driven system of gas, By CH4Gas injects back-up sand guard system, is fully adsorbed under simulation stratum condition, and the volume for recording fill out sand tube arrival end adds up Flow;Open CO2The booster pump and power-driven system of gas, continue to be passed through CO into system2Until the gas of port of export outflow In can't detect CH4Untill, record in real time and handle volume flow and count data with infrared ray gas analyzer;Change is filled out Temperature, the pressure of sandpipe, study CO under different temperatures, pressure, flow condition2Replace CH4Effect, analyze inherent law.
Specifically, CO is included based on analogue means as shown in Figure 1, device2Gas cylinder 9 and CH4Gas cylinder 17, the CO2Gas cylinder 9 and CH4Gas cylinder 17 connects the input of first piston container 7 and second piston container 15, first piston container 7 and second respectively The power drive end of piston container 15 is connected with hydraulic pressure power-driven system 57, and output end is connected to the input of fill out sand tube 41 End, and vavuum pump 25, calibration system 58 are provided with connecting pipeline, fill out sand tube 41 is placed in insulating box 40, and is connected with Axle press pump 38, output end are connected to tail gas recycle container 56, and outside line gas analyzer 54 and back pressure control are set on pipeline System 59, wherein:
CO2Gas cylinder 9 can access gas as needed, and bottle mouth of gas cylinder should be tilted down to storage during storage, be easy to stabilization Ground stores and output CO2。CO2Gas cylinder 9 is sequentially connected the first booster pump 10, the second safety valve 11, second pressure sensor 12, Three valves 8, the valve 13 of first piston container 7 and the 4th.The effect of first booster pump 10 is 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 stable injection of gas In fill out sand tube.
CH4Gas cylinder 17 can access gas as needed, and bottle mouth of gas cylinder should be tilted down to storage during storage, be easy to stabilization Ground stores and output CH4。CH4Gas cylinder 17 is sequentially connected the second booster pump 18, the 3rd safety valve 19, the 3rd pressure sensor 20, Six valves 16, the valve 21 of second piston container 15 and the 7th.The effect of second booster pump 18 is increase CH4The pressure of gas makes its pressure Power reaches desired value.Second piston container 15 uses fluid pressure drive device, can will have certain pressure CH4The stable note of gas Enter in fill out sand tube.
First piston container 7 and second piston container 15 are connected with power-driven system 57, and power-driven system 57 is successively Connection includes the first reservoir 1, the first valve 2, constant-flux pump 3, the safety valve 5 of first pressure sensor 4 and first, and constant-flux pump 3 can be with As needed, appropriate specifications and models are selected, set discharge capacity, the flow of pump can be adjusted.The device passes through the second valve 6 and the 5th Valve 14 is respectively connecting to the drive end of first piston container 7 and second piston container 15.
Vavuum pump 25 is connected to first piston container 7 and second piston container 15, respectively through its He of the 4th valve of port of export 13 7th valve 21 imports first flowmeter 22, passes sequentially through check valve 23, the 8th valve 24 on pipeline, and the port of export of vavuum pump 25 sets the Five safety valves 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 It is fixed single from the 4th valve 13 and the 7th valve 21 to the manifold volume and container volume between back-pressure valve 46, the entrance connection of standard chamber 30 Outlet to valve 23, and the 9th valve 26, temperature sensors of high precision 27, the 4th pressure sensor 28, are provided with pipeline Four safety valves 29, export through the tenth valve 31 connection core block room 32.
Fill out sand tube 41 is located in insulating box 40, is connected with axle press pump 38, and axle press pump 38 relies on hydraulic-driven, input connection Second fluid reservoir 36, and the 11st valve 37 is provided with pipeline, output end connects the input of fill out sand tube 41, and on pipeline Provided with the 12nd valve 39, the input of fill out sand tube 41 is connected with the output end of the 9th valve 26, and the 6th peace is set on pipeline The pressure sensor 35 of full valve 34 and the 5th, output end are sequentially connected the 6th pressure sensor 44 and the 13rd valve 45.Fill out sand tube 41 Middle setting squeeze piston 42 and sample room 43, piston face are provided with cuboid groove, gas during its role is to increase gas injection With the contact area of slate flour, conventional efficient is improved;Insulating box 40 and axle press pump 38 can control fill out sand tube 41 as needed Temperature and pressure, simulate specific temperature and pressure condition, CO2Replace CH4Process.
Back pressure control system 59 includes electronic backpressure pump 50, back pressure buffer container 52 and back-pressure valve 46.Electronic backpressure pump 50 Can be as needed, select appropriate specifications and models, set discharge capacity, pressure, the flow of pump can be adjusted.Electronic backpressure pump input The 7th safety valve 49 is connected to, output is terminated with back pressure buffer container 52, and the 14th valve 51 is set in its pipeline, back pressure buffering The 7th pressure sensor 47 and the 6th safety valve 48, back-pressure valve 46 are provided with connecting line between container 52 and back-pressure valve 46 Input be connected with the output end of the 13rd valve 45, output end is provided with second flowmeter 53.
The input of infrared ray gas analyzer 54 is connected to the output end of fill out sand tube 41, and second flow is set on pipeline Meter 53.Second flowmeter 53 can with meter gaseous total flow, infrared ray gas analyzer 54 can measure in real time gas component with And concentration, fast and easy, output is terminated with tail gas recycle container 56, and the 15th valve 55 is provided with pipeline, and tail gas recycle is held Discarded gas after device recovery experiment, plays a part of environmental protection.
In the present invention, first flowmeter 22, second flowmeter 53, infrared ray gas analyzer 54, first pressure sensor 4th, second pressure sensor 11, the 3rd pressure sensor 19, the 4th pressure sensor 28, the 5th pressure sensor the 35, the 6th pressure Force snesor 44, the 7th pressure sensor 47 and insulating box 40 are all connected with digital collection control card, can by the pressure of collection, Temperature and data on flows processing generation initial data form, analytical statement and curve map, while generate database file form So that user flexibility uses.
All connecting lines use 316L pipelines in the present invention, to prevent CO2To the sour corrosion of pipeline;And connection the 3rd All pipelines that the valve 16 of valve 8 and the 6th is arrived between second flowmeter 53, wound and wrapped up with insulation material, be easy to prevent heat from passing Test error caused by passing, scatter and disappear etc..
Complete simulation process of the invention includes following arrangement:
Step 1, experimental facilities is assembled according to Fig. 1 installation drawing, experimental temperature is set to insulating box 40.
Step 2, test experience device sealing.
All valves of shutoff device, the second valve 2, the 5th valve 14, the 6th valve 16 and the 7th valve 21 are opened, by CH4Gas cylinder 17 CH4Gas is transferred in second piston container 15, and setting pressure is pressurized to second piston container 15 with constant-flux pump 3.Close Second valve 2, the 5th valve 14 and the 6th valve 16, after stable, check valve 23 is slowly opened, makes high pressure CH4Gas slowly, which is transferred to, to be filled out In sandpipe 41, work pressure test is carried out to experimental system, determines that its sealing is good.
Step 3, calibration system demarcation is operated from the 4th valve 13 and the 7th valve 21 to the manifold volume between back-pressure valve 46.
The 11st valve 37 and the 12nd valve 39 are opened, adds a dead axle pressure by sample room 43 to fill out sand tube 41 using axle press pump 38 Interior slate flour sample compacting, closes the 11st valve 37 and the 12nd valve 39 after compacting.Open the 4th valve 13, the 7th valve 21, list To valve 23, the 8th valve 24, the 9th valve 26 and the 13rd valve 45, using vavuum pump 25 to first piston container 7, second piston container 15 and pipeline vacuumized, close the 4th valve 13, the 7th valve 21 and check valve 23, open the first valve 2, the 5th valve 14 and the 6th Valve 16, by CH4The CH of gas cylinder 174Gas is transferred in second piston container 15, and second piston container 15 is pressurized to constant-flux pump 3 Pressure is set, closes the second valve 2, the 5th valve 14 and the 6th valve 16, after stable, slowly opens the 7th valve 21 and check valve 23, It is after pressure stabilisation, record the registration T of the pressure sensor 28 of temperature sensors of high precision 27 and the 4th1And P1, take out calibrated bolck room 32 calibrated bolck 1, standard building volume are V1, the volume of calibrated bolck 1 is V ', opens the tenth valve 31, after temperature, pressure is stable, note The registration T of the lower pressure sensor 28 of temperature sensors of high precision 27 and the 4th of record2And P2, accordingly according to equation of gas state law It can calculate from the 4th valve 13 and the 7th valve 21 to the manifold volume between back-pressure valve 46:
V=(P2T1V1+P2T1V’-P1T2V1)/(P2T1-P2T1), the 9th valve 26 is closed after demarcation.
Step 4, vavuum pump is opened, device is vacuumized, the pressure of back-pressure valve is set.
After closing all valves, the 4th valve 13, the 7th valve 21, first flowmeter 22, the 8th valve 23, the and of the 9th valve 26 are opened 13rd valve 45, first piston container 7, second piston container 15 and pipeline are vacuumized using vavuum pump 25, vacuumized The 8th valve 24 and the 13rd valve 45 are closed afterwards, open the 14th valve 51, back pressure buffer container 52 is increased using electronic backpressure pump 50 It is pressed onto setting pressure.After treating stabilization, back-pressure valve 46 is slowly opened, keeps the pressure of back-pressure valve 46 constant.
Step 5, to CH4Gas boosting, CH is injected into shale samples by power-driven system4Gas, record fill out sand tube The data of entrance volume flowmeter, kept for fill out sand tube and relevant apparatus constant temperature and pressure certain time to shale samples saturation.
The valve 13 of check valve 23 and the 4th is closed, the first valve 2, the 5th valve 14 and the 6th valve 16 are opened, by CH4The CH of gas cylinder 174 Gas is transferred in second piston container 15, setting pressure is pressurized to second piston container 15 with constant-flux pump 3, setting pressure is being closed It is slightly above back pressure pressure in the range of reason, closes the second valve 2, the 5th valve 14 and the 6th valve 16, after stable, slowly opens check valve 23 and the 13rd valve 45, makes high pressure CH4Gas slowly is transferred in fill out sand tube 41, is passed through CH4Cumulative volume VinCH1, allow gas to obtain Sufficiently diffusion and absorption.Be then shut off check valve 23, allow gas obtained in shale samples fully diffusion and farthest Absorption.
Step 6, CO is constantly passed through with constant flow2, simulate CO2The dynamic process of shale gas is replaced, until outlet Hold in the gas of outflow and can't detect CH4Untill, therebetween in real time record volume flowmeter and infrared gas analyser data.
The first valve 2, the second valve 6 and the 3rd valve 8 are opened, by CO2The CO of gas cylinder 92Gas is transferred in first piston container 7, is used Constant-flux pump 3 is pressurized to setting pressure to first piston container 7, and setting pressure slightly above sets back pressure pressure in the reasonable scope, The first valve 2, the second valve 6 and the 3rd valve 8 are closed, after stable, the 4th valve 13, check valve 23 slowly opened, makes CO2Fluid is slow It is transferred in fill out sand tube 41, it is after pressure stabilisation, the first valve 2, the second valve 6, the 3rd valve 8 and check valve 23 are opened, by CO2Gas cylinder 9 CO2Gas is transferred in first piston container 7, and setting pressure is pressurized to first piston container 7 with constant-flux pump 3, sets pressure Back pressure pressure is slightly above set in the reasonable scope, closes the first valve 2, the second valve 6 and the 3rd valve 8, after stable, is slowly opened Check valve, CO is continually fed into constant flow2Until can't detect CH in the gas of port of export outflow4Untill, record is passed through CO2Cumulative volume VinCO2, CO is calculated according to second flowmeter 53 and infrared ray gas analyzer 542Accumulative elution volume VoutCO2
Step 7, CH is calculated according to experimental data4Adsorbance and CO2Shale tolerance is replaced, test and assess CO2Replace CH4Effect.
CH4Adsorbance calculates:Go out to be passed through CH by first flowmeter 22 is measurable4Cumulative volume VinCH1, the CH that is passed through4One Divide with ADSORPTION STATE absorption on shale samples, a part is full of pipeline using free state and volume is demarcation volume V, by temperature, pressure The pressure and temp value that sensor measures, can calculate the CH being passed through4Quality m1 is totalWith free state CH4Quality m1 trip, make the difference i.e. available CH4Adsorbance m1 inhales
CO2The calculating of adsorbance:Above-mentioned experimentation can be learnt according to first flowmeter 22 is passed through CO2Cumulative volume VinCO2, CO measured according to second flowmeter 53 and infrared ray gas analyzer 542Accumulative elution volume VoutCO2, remain in pipe CO in road2Volume VCO2, it is respectively m that the pressure and temp value that is measured by temperature and pressure transmitter, which can be calculated result,2 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 is according to monitoring volume integral meter in real time Draw.
CH4The calculating of replacement amount:CH is measured according to second flowmeter 53 and infrared ray gas analyzer 544Accumulative outflow Volume VoutCH4, CH can be calculated4Accumulative discharge m1 goes out, then by CO2The CH displaced4Quality be m1 changes=m1 goes out-m1 trip
CH4/CO2The calculating of replacement result:Utilize the above results, you can according to displacing CH4Total amount and absorption CH4Total amount Ratio assess to obtain the Mathematics Proof of replacement result evaluation, according to CO2Adsorbance evaluates CO2Displacement replacement result.
Step 8 changes the temperature of experiment setting, pressure, repeats above step, can obtain between pressure-displacement tolerance Relation, relation between temperature-displacement tolerance etc., so as to study different temperatures, pressure, flow CO2Different temperatures, To the replacement result of shale gas under pressure condition.

Claims (4)

1. one kind simulation CO2Displacement replace the pneumatic state process of shale method, based on analogue means include:
CO2Gas cylinder (9), it is sequentially connected the first booster pump (10), the second safety valve (11), second pressure sensor (12), the 3rd valve (8), first piston container (7) and the 4th valve (13), the outlet of the 4th valve (13) connect the 7th valve (21) and first flowmeter (22);
CH4Gas cylinder (17), it is sequentially connected the second booster pump (18), the 3rd safety valve (19), the 3rd pressure sensor (20), the 6th Valve (16), second piston container (15) and the 7th valve (21), the outlet of the 7th valve (21) connect the 4th valve (13) and first flow Count (22);
Hydraulic pressure power-driven system (57), including be sequentially connected the first reservoir (1), the first valve (2), constant-flux pump (3), first Pressure sensor (4) and the first safety valve (5), press power-driven system (57) and first piston container is connected by the second valve (6) (7) drive end, the drive end of second piston container (15) is connected by the 5th valve (14);
Fill out sand tube (41), it is placed in insulating box (40), the output of connection first piston container (7) and second piston container (15) End;
Vavuum pump (25), the input of vavuum pump (25) connects is provided with check valve on first flowmeter (22) and connecting line (23) and the 8th valve (24), the output end of vavuum pump (25) are connected with the 5th safety valve (33);
Calibration system (58), including standard chamber (30) and calibrated bolck room (32), known volume is placed with calibrated bolck room (32) Shale core sample blocks, the outlet of the entrance connection check valve (23) of standard chamber (30), and the 9th is provided with connecting line Valve (26), temperature sensors of high precision (27), the 4th pressure sensor (28) and the 4th safety valve (29), are exported through the tenth valve (31) calibrated bolck room (32) are connected;
Tail gas recycle bottle (56), the output end of connection fill out sand tube (41);
Back pressure control system (59), for controlling fill out sand tube outlet pressures, true strata pressure state is simulated, it includes electronic Backpressure pump (50), back pressure buffer container (52) and back-pressure valve (46), electronic backpressure pump (50) input connect the 7th safety valve (49), output end connection back pressure buffer container (52) and the 14th valve (51) of setting in its connecting line, back pressure buffer container (52) the 7th pressure sensor (47) and the 6th safety valve (48), back pressure are provided with the connecting line between back-pressure valve (46) The input of valve (46) is connected with the output end of the 13rd valve (45), and output end is sequentially connected second flowmeter (53), infrared ray Gas analyzer (54), the 15th valve (55) and tail gas recycle bottle (56), the input connection fill out sand tube of the 13rd valve (45) (41) output end;
Infrared gas analyser (54), it is arranged on the connecting line of fill out sand tube (41) and tail gas recycle bottle (56);
It is characterised in that it includes following steps:
Step 1, experimental temperature is set to insulating box (40);
Step 2, test experience device sealing;
Step 3, calibration system (58) is operated, is demarcated using the state equation law of gas from the 4th valve (13) and the 7th valve (21) Manifold volume to back-pressure valve (46);
Step 4, vavuum pump (25) is opened, device is vacuumized, the pressure of back-pressure valve (46) is set;
Step 5, first to CH4The CH of gas cylinder (17)4Gas boosting, by hydraulic pressure power-driven system (57) to fill out sand tube (41) Middle injection CH4Gas, the data of record fill out sand tube (41) arrival end first flowmeter (22), keep fill out sand tube (41) and related dress Constant temperature and pressure certain time is put to saturation;
Step 6, CO is continually fed into constant flow2, simulate CO2The dynamic process of shale gas is replaced, until fill out sand tube (41) goes out CH is can't detect in the gas of mouth end outflow4Untill, record first flowmeter (22), second flowmeter (53) and red in real time therebetween The data of outside line gas analyzer (54);
Step 7, CH is calculated according to experimental data4Adsorbance and CO2Shale tolerance is replaced, test and assess CO2Replace CH4Effect;
Step 8, change temperature, the pressure of experiment setting, repeat above step, obtain relation between pressure-displacement tolerance, Relation between temperature-displacement tolerance, so as to study different temperatures, pressure, flow velocity CO2Under different temperatures, pressure condition To the replacement result of shale gas.
2. CO is simulated according to claim 12The method that the pneumatic state process of shale is replaced in displacement, it is characterised in that the back-up sand Pipe (41) is connected with the axle press pump (38) by hydraulic-driven, and axle press pump (38) acts on compacting sample room (43) interior slate flour On, the pressured state of shale under simulation stratum condition, the input of axle press pump (38) connects the second reservoir (36) and connected The 11st valve (37) is provided with pipeline, output end connects the input of fill out sand tube (41) and on connecting line provided with the 12nd Valve (39), the input of fill out sand tube (41) is connected with the output end of check valve (23) and the safety of setting the 6th on connecting line Valve (34) and the 5th pressure sensor (35), output end are sequentially connected the 6th pressure sensor (44) and the 13rd valve (45), filled out Include sample room (43) inside sandpipe (41) and connect the piston with groove (42) of sample room (43), piston (42) is pressing close to page Design fluted on rock side, its object is to increase the contact area of gas and shale so that gas displacement and adsorption process What is carried out is more abundant.
3. CO is simulated according to claim 22The method that the pneumatic state process of shale is replaced in displacement, it is characterised in that the step CH is calculated in 74The method of adsorbance is as follows:
Go out to be passed through CH by first flowmeter (22) is measurable4Cumulative volume VinCH4, the CH that is passed through4A part is existed with ADSORPTION STATE absorption On shale samples, a part is full of pipeline using free state and volume is demarcation volume V, is surveyed by pressure sensor and temperature sensor The pressure and temperature value obtained, can calculate the CH being passed through4Quality m1 is totalWith free state CH4Quality m1 trip, make the difference and can obtain CH4Absorption Measure m1 inhales
4. CO is simulated according to claim 22The method that the pneumatic state process of shale is replaced in displacement, it is characterised in that the step CO is calculated in 72The method for replacing shale tolerance is as follows:
Learnt according to first flowmeter (22) and be passed through CO2Cumulative volume, according to second flowmeter (53) and infrared ray gas analyzer (54) CO is measured2Accumulative elution volume, remaining CO in the duct2Volume, measured by pressure sensor and temperature sensor Pressure and temperature value, CO can be calculated2Accumulative be passed through quality m2 is total, accumulative outflow quality m2 go outWith free state CO2Quality m2 trips, then Obtain CO2Adsorbance m2 inhale=m2 is total-m2 go out-m2 trips, wherein CO2Accumulative elution volume is calculated according to real-time monitoring volume integral.
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