CN110057740A - High temperature and pressure coal petrography supercritical carbon dioxide pressure break-creep-seepage tests method - Google Patents

High temperature and pressure coal petrography supercritical carbon dioxide pressure break-creep-seepage tests method Download PDF

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CN110057740A
CN110057740A CN201910349188.3A CN201910349188A CN110057740A CN 110057740 A CN110057740 A CN 110057740A CN 201910349188 A CN201910349188 A CN 201910349188A CN 110057740 A CN110057740 A CN 110057740A
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pressure
coal petrography
axis
temperature
valve
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CN110057740B (en
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梁卫国
曹孟涛
武鹏飞
耿毅德
杨晓琴
高翔
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Taiyuan University of Technology
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    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/08Investigating permeability, pore-volume, or surface area of porous materials
    • G01N15/082Investigating permeability by forcing a fluid through a sample
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Abstract

High temperature and pressure coal petrography supercritical carbon dioxide pressure break-creep-seepage tests method, the supercritical carbon dioxide fluid crushing test of coal petrography at high temperature under high pressure, and the characteristic of the variation of the temperature, pressure of supercritical carbon dioxide and fracture initiation, extension in real-time monitoring, record supercritical carbon dioxide fracturing process, and the axially and radially deformation of real-time monitoring, record coal petrography sample, and can guarantee the CH of coal petrography before and after directly and efficiently measuring pressure break under conditions of not unloading coal petrography sample stress4Permeability, and post-fracturing coal petrography CH under creep effect may be implemented4Permeability measurement.Measurement method precision of the present invention is high, intuitive, and high degree of automation, equipment therefor structure are simple.

Description

High temperature and pressure coal petrography supercritical carbon dioxide pressure break-creep-seepage tests method
Technical field
The present invention is a kind of coal petrography supercritical carbon dioxide pressure break-creep-seepage tests method under high temperature and pressure, and pressure break is situated between Matter is supercritical carbon dioxide, belongs to rock mass mechanics and field of engineering technology scope.Specifically related to Deep Coalbed Methane exploitation in, Pressure break coal petrography sample, real-time monitoring, record supercritical carbon dioxide pressure are carried out as pressure break medium using supercritical carbon dioxide The characteristic of the variation of the temperature, pressure of supercritical carbon dioxide and fracture initiation, extension during splitting, and supervise in real time simultaneously It surveys, the axially and radially deformation of record coal petrography sample, and under the stress condition for not unloading coal petrography sample before and after measurement pressure break The gas permeability of coal petrography sample, and obtain the changing rule of post-fracturing coal petrography sample permeability under creep effect.
Technical background
Coal seam hydraulic pressure, which can be, realizes large-scale coal petrography release, increases the gas permeability of coal and rock, mentions to reach High coal bed gas extraction rate and the effect for discharging gas pressure, but since coal seam physico-mechanical properties are more complex and non-equal Matter is stronger, has water-sensitive, strong adsorption and hypotonic feature, therefore, fracturing effect is unsatisfactory.Water is carried out in coal seam In power fracturing activities, most common fracturing fluid is water, and in fracturing process, coal dust blocking high since there are leak-offs, water are larger The shortcomings that, influence pressing crack construction effect.Therefore, pressure break is carried out as fracturing fluid using gas, there is preferable development prospect.
Carbon dioxide can be used as fracturing fluid and carry out pressure break coal seam, advantageously reduce in atmosphere as a kind of greenhouse gases Carbon dioxide content, mitigate greenhouse effects.When the temperature and pressure of carbon dioxide is simultaneously greater than 31.10 °C and 7.38MPa, Carbon dioxide is up to supercriticality.Supercritical carbon dioxide has the similar diffusivity of gas and the solvability of liquid And density, while also there is the characteristic that surface tension is low, viscosity is small, permeability and mobility are preferable, therefore, can replace clear Water is as fracturing fluid.Supercritical carbon dioxide pressure break is a kind of new using the carbon dioxide of above-critical state as one kind of fracturing fluid Type fracturing technique, relative to conventional fracturing fluid, supercritical carbon dioxide is to reservoir fanout free region, and the row of returning is easy, therefore, non- There is very big advantage above the fracturing yield increasing of conventional reservoir.But at present for supercritical carbon dioxide pressure break coal and rock It is still unintelligible, and the experimental rig for being able to achieve supercritical carbon dioxide pressure break coal and rock is less.
In oil-gas mining field, fracturing device and method have been achieved for multinomial achievement, wherein are related to true triaxial pressure break The patent of invention of method and apparatus mainly has: CN 103821487 A, CN 102621000 B, CN 103883301 A, CN 104655495 A of 103728184 A, CN 103993867 A, CN 103592186 A, CN.Existing true triaxial pressure break mould Quasi- experimental rig and method may be implemented to simulate hydraulic fracturing and the examination of other gas pressure breaks under buried formation temperature, stress condition It tests, but true triaxial fracturing device is difficult to realize the gas permeability of square coupons after directly measuring pressure break.And to existing three axis Fracturing device (cylindrical sample), such as 105510142 A of CN, it is difficult to overcome under the stress condition for not unloading sample accurately The permeability of sample directly before and after measurement pressure break, and be difficult to realize under the conditions of high temperature (300 °C), high pressure (70MPa), using sound Lift-off technology accurately and reliably monitors the crack initiation in the crack of sample, extended attribute in fracturing process, observation, analysis and grasp The formation in crack and extension mechanism.Therefore, it is the occurrence condition of preferably real simulation deep subsurface rock, carries out overcritical two Carbonoxide crushing test research, while coal petrography sample before and after pressure break can be directly measured under the stress condition for not unloading sample Gas permeability, and measure gas permeability of the post-fracturing coal petrography sample under long duration of action, need to experimental rig and Method carries out important innovation.
Summary of the invention
The present invention provides a kind of coal petrography supercritical carbon dioxide pressure break-creep-seepage tests method under high temperature and pressure, mesh The supercritical carbon dioxide fluid fracturing experiments for being that by coal petrography under high temperature and pressure, and real-time monitoring, record it is overcritical The characteristic of the variation of the temperature, pressure of supercritical carbon dioxide and fracture initiation, extension during carbon dioxide pressure break, and it is same When real-time monitoring, record the axially and radially deformation of coal petrography sample, and can guarantee in the condition for not unloading coal petrography sample stress The CH of coal petrography sample before and after lower measurement pressure break4Permeability, and can be carried out CH of the coal petrography sample under creep effect after pressure break4Infiltration The measurement of rate.
A kind of high temperature and pressure coal petrography supercritical carbon dioxide pressure break-creep-seepage flow test device, it is characterised in that the examination Experiment device can load high stress, hot conditions to coal petrography sample, and the size of coal petrography sample is 50 × 100mm of Ф, coal petrography sample Axis pressure and confining pressure reach 70MPa, up to 300 °C, analog mineral buried depth reaches the geology ring of 2500m for the temperature of coal petrography sample Border.
The experimental rig is by triaxial cell, axis pressure and confining pressure loading system, heating temperature-controlling system, overcritical titanium dioxide Carbon generator system, acoustic emission monitoring system, pressure-deformation monitoring system, totally seven parts form permeability measurement systems.
Triaxial cell is to provide the environment of a simulated formation stress state and temperature to coal petrography sample.
The triaxial cell includes triaxial cell's cylinder (16), porous plate b(3), porous plate a(2), left pressure head (4), Right pressure head (5), axial hydraulic piston (10), axis pressure cavity (9), axis pressure cavity fixed device (8), rubber sleeve (22), coning sleeve b (18), coning sleeve a(23), first fixed device (24), second fixed device (25).
Triaxial cell's cylinder (16) have axially through triaxial cell's cavity (21), axis pressure cavity fix Device (8) and triaxial cell's cavity (21) coaxial placement, the side wall of triaxial cell's cylinder (16) are disposed with confining pressure and enter Mouth (20), confining pressure outlet (15) and thermometric entrance (19).
Coning sleeve a(23) and coning sleeve b(18) it is separately positioned on two pressure head peripheries.
Cavity between rubber sleeve (22) and triaxial cell's cylinder (16) forms triaxial cell's cavity (21).
Coning sleeve a(23) and coning sleeve b(18) front end is tapered, it can guarantee between coning sleeve a, b and rubber sleeve in this way Reach good sealing effect, is realized and sealed by O-ring between triaxial cell's cylinder (16);First fixed device (24) It is connect with triaxial cell's cylinder (16), axis pressure cavity fixed device (8) is connect with triaxial cell's cylinder (16), and is realized solid Determine coning sleeve a(23) and coning sleeve b(18) purpose;
Second fixed device (25) are connected to first fixed device (24), are gently against left pressure head (4) left side, and squeeze porous Plate a(2), guarantee porous plate a(2) with the left end face contact of coal petrography sample (1).Place one in the left end of axial hydraulic piston (10) End face diameter is the right pressure head (5) of 50mm, then passes through porous plate b(3), it offsets with the right end of coal petrography sample;It is pressed by axis permanent Stream constant pressure pump (34) is filled to axis and presses cavity (9) inner, so that axial hydraulic piston (10) be pushed to be loaded.
The surface of the left pressure head (4) and right pressure head (5) be provided with three acoustic emission probe preformed holes (7) (see Fig. 5, Fig. 6), it should allow the spatial distribution of probe straggly different as much as possible when installation, guarantee any four probe not in the same space In plane, Lai Shixian acoustic emission monitor(ing) acquires breakdown point spatial position accurate, reliable.
Left pressure head (4), right pressure head (5) are both provided with circulating water cooling device water inlet (44) and circulating water cooling device goes out The mouth of a river (45) realizes the cooling of left and right pressure head under the conditions of hot test, guarantees the operating temperature of acoustic emission probe.
Left pressure head (4) is equipped with centre bore (46), and stainless steel high pressure line can pass through centre bore and enter coal petrography sample (1), It realizes supercritical carbon dioxide crushing test, while stainless steel high pressure line is sealed by cutting ferrule and left pressure head, guarantees pressure When splitting test and permeability survey test, gas is not flowed out from the gap location of stainless steel high pressure line and centre bore.
The lower part of left pressure head (4) is equipped with circular hole (6), is connected by valve V8 with graduated cylinder (28), guarantees the survey in permeability In amount, after closing valve V1, gas is only flowed out from the left side of coal petrography sample, and is passed into graduated cylinder by circular hole (6), to prevent Result of the gas from centre bore or stainless steel high pressure line outflow interference permeability survey.
Axis pressure and confining pressure loading system, including axis pressure constant current constant voltage pump (34), confining pressure constant current constant voltage pump (36) and Valve V9, valve V10 and axis pressure cooling device (42) and confining pressure cooling device (41), the axis pressure, confining pressure cooling device are adopted Stainless steel high pressure line is cooled down with recirculated water mode, it is ensured that the normal work pumped under hot conditions (60 °C or more).
Axis presses constant current constant voltage pump (34), is linked into axis pressure cooling device (42) by valve V10, is connected to axis pressure cavity (9) axis pressure load is realized in;Confining pressure constant current constant voltage pumps (36) and is connected to confining pressure cooling device (41), finally by valve V9 It accesses in triaxial cell's cavity (21), realizes the load of confining pressure;Axis pressure, confining pressure loading system use constant current constant voltage water pump, and By pressure sensor monitoring pressure value, and the size of automatic control flow, to meet constant-pressure conditions.
It further illustrates, above-mentioned axis pressure, confining pressure loading system may insure that in fracturing process, axis pressure, confining pressure are always It keeps constant.
The heating temperature-controlling system, including heating mantle (17) and thermometric entrance (19) and heating device (35).
Heating mantle (17) is wrapped in outside triaxial cell's cylinder, is connected to heating device (35), realizes heating coal petrography sample (1) purpose, and pass through the temperature that thermometric entrance (19) carry out detection coal petrography sample (1), temperature is carried out by heating device (35) Real-time monitoring and control.
The supercritical carbon dioxide generator system, by CO2Gas cylinder (39), fracturing pump (38), preheater (37), valve V2, valve V4, valve V5, four-way valve (30), the first temperature sensor (31), first pressure sensor (29) and heat preservation are not Become rusty steel high pressure line composition.
CH4Gas cylinder is used to provide gas source, and fracturing pump (38) is increased the pressure of carbon dioxide, be injected into the mode of constant current The inside of coal petrography sample (1), until crushing test success;
Preheater (37) is to CO2Gas is heated, and CO is made2Supercriticality is always maintained in fracturing process;Heat preservation is not Steel high pressure line become rusty primarily to guaranteeing the constant of the supercritical carbon dioxide temperature come out from preheater.
It further illustrates, connects a four-way valve (30) in preheater (37) front end, four-way valve (30) is separately connected first Temperature sensor (31) and first pressure sensor (29) are connected by valve V1 with pressure break entrance (26);It is required that four-way valve (30) as far as possible close to pressure break entrance (26), it is ensured that the pressure, temperature for being accurately monitored carbon dioxide in fracturing process become Change.
The acoustic emission monitoring system monitors supercritical carbon dioxide pressure break coal petrography specimen using Acoustic radiating instrument In, positioning and the real-time tracking of crackle are realized in the crack initiation in crack, extended attribute, left pressure head (4) and right pressure in triaxial cell The thinner thickness of head (5), and three acoustic emission probe preformed holes are respectively provided in the right side of the left side of left pressure head, right pressure head (see Fig. 5 and Fig. 6) guarantees accurate, the stable detection and transmission of acoustic emission signal;Pay attention to allowing probe when installation as far as possible Spatial distribution is straggly different, guarantees that any four are popped one's head in not in the same space plane, Lai Shixian acoustic emission monitor(ing) is to destruction Space of points station acquisition it is accurate, reliable.
Pressure-deformation monitoring system (43) mainly includes pressure-temperature acquisition device, axial deformation acquisition device And radial displacement acquisition device, by first pressure sensor (29) described above, second pressure sensor (32), One temperature sensor (31), second temperature sensor (33), LVDT displacement sensor (13) and axis pressure constant current constant voltage pump (34), Confining pressure constant current constant voltage pump (36) and fracturing pump (38) are connected with multi-channel data acquisition board, and are linked into computer, realize pressure Power, flow, temperature and the real-time acquisition of deformation.
The pressure-temperature acquisition device is by fracturing pump (38), first pressure sensor (29), the second pressure Force snesor (32) and the first temperature sensor (31), second temperature sensor (33) are connect with multi-channel data acquisition board, It is linked into computer, the temperature and pressure surveyed for each temperature and pressure sensor in automatic measurement, record experimentation Numerical value, and record the flow and pressure of fracturing pump.
The axial deformation acquisition device includes LVDT displacement transducer fixed support (11) and LVDT displacement sensor (13) (see figure 1) and multi-channel data acquisition board, LVDT displacement transducer fixed support (11) are fixed on axis pressure cavity and fix On device (8), LVDT displacement sensor (13) is symmetrically mounted at the two sides of axis pressure hydraulic piston (10), LVDT displacement sensing Device bottom end is against axis pressure hydraulic piston (10) right side respectively, and guarantees LVDT displacement sensor (13), axis pressure hydraulic piston (10) and the axis of triaxial cell's cylinder (16) is parallel to each other.
As further explanation, under hot conditions, LVDT displacement sensor is by unsuitable work, therefore, in axis hydraulic fluid pressure The outside of piston (10) adds circulating water cooling device (12) Lai Jiangwen, guarantees the temperature of LVDT displacement sensor position Degree maintains room temperature.
The radial deformation acquisition device includes multi-channel data acquisition board, by acquiring, recording confining pressure constant current constant voltage The volume change of fluid measures the radial deformation of coal petrography sample in fracturing process in pump, and the specific method is as follows: assuming that coal petrography The length of sample isL 0Mm, diameter ared 0 Mm,t 0When=0, the integrated flux of confining pressure constant current constant voltage pump isV 0Ml, LVDT displacement The reading of sensor isa 0 mm;?t 1When, the integrated flux of confining pressure constant current constant voltage pump isV 1Ml, LVDT displacement sensor reading Fora 1 Mm, the decrement of coal petrography specimen lengthL(axial deflection) is
The then radial diameter d of coal petrography sample1For
The momentt 1The radial strain of coal petrography sample is
As further explanation, under hot conditions, axis pressure cooling device is respectively set before axis pressure, confining pressure constant current constant voltage pump (42), confining pressure cooling device (41) (see figure 1), it is ensured that axis pressure, the temperature of confining pressure constant current constant voltage pump substantially remain in room temperature, it is ensured that The two can work normally.
As further explanation, at normal temperature, water can be selected as the loaded medium of axis pressure, confining pressure, and in high temperature item Under part, loaded medium of the silicone oil as axis pressure, confining pressure can be used.
Permeability measurement systems are by CH4Gas cylinder (40), fracturing pump (38), preheater (37), graduated cylinder (28), second pressure pass Sensor (32) valve V3, V4, V7, V8 and heat preservation stainless steel high pressure line composition.CH4The CH of gas cylinder (40)4By valve V3 into Enter fracturing pump (38), fracturing pump (38) injects CH with constant current mode4Gas is connected to preheater (38) by valve V4, leads to Valve V7 is crossed to osmotic pressure entrance (14);The effect of preheater (38) is to heat CH4Gas guarantees that it reaches and coal petrography sample Identical temperature can accurately measure different temperatures and act on lower CH4Permeability;In the left end of coal petrography sample, valve is closed V1, so that CH4It is only flowed out from circular hole (6), completes CH by graduated cylinder (28)4The collection of gas can obtain the temperature, answer by calculating The CH of coal petrography sample under the conditions of power4Permeability accurately measures pressure break so as to realize under conditions of not unloading coal petrography sample The CH of front and back coal petrography sample4Permeability.
As further explanation, the permeability of coal petrography sample before and after pressure break is measured, gas used is not limited to CH4, It can be nitrogen, supercritical carbon dioxide or inert gas.
As further embodiment of the invention:
Compared with prior art, the beneficial effects of the present invention are: simulation deep may be implemented in the present invention (under high temperature, condition of high voltage) Crushing test of the coal petrography under supercritical carbon dioxide effect, and monitor supercritical carbon dioxide in fracturing process (fracturing fluid) The crack initiation in crack and extended attribute in pressure, temperature change and fracturing process, while being also able to achieve coal in monitoring fracturing process Axial direction, the radial deformation mechanism of rock, so as to the crack initiation more fully hereinafter to supercritical carbon dioxide pressure break coal petrography, striking machine Reason and deformation mechanism carry out research and analysis.
Compared with prior art, the beneficial effects of the present invention are: the present invention can also realize supercritical carbon dioxide pressure break After coal petrography sample, CH directly is carried out to coal petrography under conditions of not unloading coal petrography sample4Seepage Experiment can unload in this way to avoid adding Carry damage of the history to coal petrography sample, can also to avoid caused by artificial during unloading and reloading to coal petrography sample not Evitable destruction, after crushing test, the CH of the coal petrography sample before and after available pressure break4Permeability, and after pressure break can be obtained Coal petrography sample under long duration of action CH4The Evolution of permeability more realistically evaluates super face from the actual angle of engineering Beneficial effect of boundary's carbon dioxide pressure break coal petrography to coal bed gas extraction.
Compared with prior art, the sealing device rubber sleeve of coal petrography sample can be with high temperature resistant (300 °C), and corrosion-resistant, energy Enough effects for realizing the long-term ground sealing carbon dioxide in fracturing process, avoid partial CO 2 from penetrating into three by rubber sleeve In axis pressure chamber cavity, experimental result is influenced.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of experimental rig in the present invention;
Fig. 2 is the cross-sectional view of the structure of porous plate a;
Fig. 3 is the cross-sectional view of the structure of left pressure head;
Fig. 4 is the structural schematic diagram of the coal petrography sample of processing;
Fig. 5 is the left side structural schematic diagram of left pressure head;
Fig. 6 is the right side structural schematic diagram of right pressure head;
Figure label: 1 --- coal petrography sample;2 --- porous plate a;3 --- porous plate b;4 --- left pressure head;5 --- right pressure head; 6 --- circular hole;7 --- acoustic emission probe preformed hole;8 --- axis presses the fixed device of cavity;9 --- axis presses cavity;10 --- axis To hydraulic piston;11 --- LVDT displacement transducer fixed support;12 --- circulating water cooling device;13 --- LVDT displacement passes Sensor;14 --- osmotic pressure entrance;15 --- confining pressure outlet;16 --- triaxial cell's cylinder;17 --- heating mantle;18—— Coning sleeve b;19 --- thermometric entrance;20 --- confining pressure entrance;21 --- triaxial cell's cavity;22 --- rubber sleeve; 23 --- coning sleeve a;24 --- the first fixed device;25 --- the second fixed device;26 --- pressure break entrance;27 --- infiltration Extrude mouth;28 --- graduated cylinder;29 --- first pressure sensor;30 --- four-way valve;31 --- the first temperature sensor; 32 --- second pressure sensor;33 --- second temperature sensor;34 --- axis presses constant current constant voltage pump;35 --- heating dress It sets;36 --- confining pressure constant current constant voltage pump;37 --- preheater;38 --- fracturing pump;39-——CO2Gas cylinder;40——CH4Gas Bottle;41 --- confining pressure cooling device;42 --- axis presses cooling device;43 --- pressure-deformation monitors system;44 --- recirculated water Cooling device water inlet;45 --- circulating water cooling device water outlet;46 --- centre bore.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described, Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all Belong to the scope of protection of the invention.
Embodiment: coal petrography supercritical carbon dioxide pressure break-creep-seepage flow test device, feature exist under high temperature and pressure High stress and hot conditions can be loaded to coal petrography sample in the device, the size of coal petrography sample can be 50 × 100mm of Ф, coal The axis pressure and confining pressure of rock sample reach 70MPa, and the temperature of coal petrography sample is up to 300 °C, and analog mineral buried depth is up to 2500m's Geological environment.
Experimental rig is sent out by triaxial cell, axis pressure and confining pressure loading system, heating temperature-controlling system, supercritical carbon dioxide Raw device system, acoustic emission monitoring system, pressure-deformation monitoring system, totally seven parts form permeability measurement systems;
Triaxial cell is the important component of the present apparatus, is to provide the ring of a reservoir stress and temperature for coal petrography sample Border.
The triaxial cell includes triaxial cell's cylinder (16), porous plate b(3), porous plate a(2), left pressure head (4), Right pressure head (5), axial hydraulic piston (10), axis pressure cavity (9), axis pressure cavity fixed device (8), rubber sleeve (22), coning sleeve b (18), coning sleeve a(23), first fixed device (24), second fixed device (25).
Triaxial cell's cylinder (16) have axially through triaxial cell's cavity (21), axis pressure cavity fix Coaxially, the side wall of triaxial cell's cylinder (16) is disposed with confining pressure entrance for device (8) and triaxial cell's cavity (21) (20), thermometric entrance (19) and confining pressure outlet (15).
Coning sleeve a(23) and coning sleeve b(18) it is separately positioned on two pressure head peripheries.
Cavity between rubber sleeve (22) and triaxial cell's cylinder (16) forms triaxial cell's cavity (21).
Coning sleeve a(23) and coning sleeve b(18) front end is tapered, it can guarantee between coning sleeve a, b and rubber sleeve in this way Reach good sealing effect, coning sleeve a(23) and coning sleeve b(18) between triaxial cell's cylinder (16) by O-shaped Circle realizes sealing;First fixed device (24) are connect with triaxial cell's cylinder (16), and axis presses cavity fixed device (8) and three axis Pressure chamber's cylinder (16) connection, and realize fixed coning sleeve a(23) and coning sleeve b(18) purpose;
Second fixed device (25) are connected to first fixed device (24), are gently against left pressure head (4) left side, and squeeze porous Plate a(2), guarantee porous plate a(2) with the left end face contact of coal petrography sample (1).Place one in the left end of axial hydraulic piston (10) End face diameter is the right pressure head (5) of 50mm, then passes through porous plate b(3), it offsets with the right end of coal petrography sample;It is pressed by axis permanent Stream constant pressure pump is filled to axis and presses cavity (9) inner, so that axial hydraulic piston (10) be pushed to be loaded.
The axis pressure and confining pressure loading system include axis pressure constant current constant voltage pump (34), confining pressure constant current constant voltage pump (36), valve Door V9, valve V10, axis press cooling device (42), confining pressure cooling device (41), and the axis pressure, confining pressure cooling device are used and followed Ring water mode cools down pipeline, it is ensured that the normal work pumped under 60 °C or more of hot conditions;Axis presses constant current constant voltage pump (34), axis pressure cooling device (42) is linked by valve V10, and is connected in axis pressure cavity (9) and realizes axis pressure load;Confining pressure Constant current constant voltage pumps (36) and is connected to confining pressure cooling device (41) by valve V9, finally accesses triaxial cell's cavity (21) It is interior, realize the load of confining pressure.
The heating temperature-controlling system, including heating mantle (17), temperature sensor, (19), heating device (35), heating mantle (17) it is wrapped in outside the cavity of triaxial cell, heating mantle (17) connects heating device (35), heats the mesh of coal petrography sample (1) , and pass through the temperature that thermometric entrance (19) carry out detection coal petrography sample (1), the real-time prison of temperature is carried out by heating device (35) It surveys and controls.
The supercritical carbon dioxide generator system, by CO2Gas cylinder (39), fracturing pump (38) and preheater (37) and The stainless steel high pressure line of heat preservation forms.CH4Gas cylinder is used to provide gas source;Fracturing pump (38) increases CO with the mode of constant current2's Pressure is injected into the inside of coal petrography sample (1), until crushing test success;Preheater (37) adds carbon dioxide gas Heat makes carbon dioxide be always maintained at supercriticality in fracturing process;The stainless steel high pressure line of heat preservation is primarily to protect Demonstrate,prove the constant of the supercritical carbon dioxide temperature come out from preheater.
The acoustic emission monitoring system uses Acoustic radiating instrument, and acoustic emission monitoring system effect is the overcritical titanium dioxide of monitoring Carbon pressure is split in coal petrography specimen, the crack initiation in crack, extended attribute, realizes positioning and the real-time tracking of crackle, triaxial cell In left pressure head (4) and right pressure head (5) thinner thickness, and be respectively set in the right side of the left side of left pressure head, right pressure head Three acoustic emission probes (see Fig. 5 and Fig. 6) guarantee accurate, the stable detection and transmission of acoustic emission signal;Pay attention to when installation to the greatest extent It is possible to make the spatial distribution of probe straggly different, guarantee that any four are popped one's head in not in the same space plane, Lai Shixian sound Launch monitor acquires breakdown point spatial position accurate, reliable.
The pressure-deformation monitoring system includes pressure-temperature acquisition device, axial deformation acquisition device and radial direction Displacement acquisition device, first pressure sensor (29), second pressure sensor (32), the first temperature sensor (31), the second temperature Spend sensor (33), LVDT displacement sensor (13), axis pressure constant current constant voltage pump (36), confining pressure constant current constant voltage pump (34), fracturing pump (38) it is connected with multichannel collecting box, and is linked into computer, realizes pressure, flow, temperature and the real-time acquisition of deformation.
Permeability measurement systems are by CH4Gas cylinder (40), fracturing pump (38), preheater (37), graduated cylinder (28), valve V3, valve Door V4, valve V7, valve V8 and heat preservation stainless steel high pressure line composition.
CH4The CH of gas cylinder (40)4Entered fracturing pump (38) by valve V3, fracturing pump (38) injects CH with constant current mode4Gas Body;CH4Preheater (38) are connected to by valve V4;CH4Pass through valve V7 to osmotic pressure entrance (14);The work of preheater (38) Be heat CH4Gas guarantees CH4Gas reaches temperature identical with coal petrography sample, accurately measures under different temperatures effect CH4Permeability;In the left end of coal petrography sample, valve V1 is closed, CH is made4It is flowed out from circular hole (6), completes CH by graduated cylinder (28)4 The collection of gas.By calculating, the CH of coal petrography sample under temperature, stress condition at this time can be obtained4Permeability is not being unloaded to realize Under conditions of carrying coal petrography sample, the accurate CH for measuring pressure break front and back coal petrography sample4Permeability.
High temperature and pressure coal petrography supercritical carbon dioxide pressure break-creep-seepage flow test device of the present invention may be implemented do not unloading Under conditions of carrying coal petrography sample stress, the accurate CH for measuring supercritical carbon dioxide pressure break front and back coal petrography sample4Permeability.
Supercritical carbon dioxide pressure break measurement method, specific steps are as follows:
1. it is 50 mm that coal petrography sample, which is processed into diameter, length is the cylindrical body coal petrography sample of 100mm;In the axis of coal petrography sample Heart drilling, the diameter of drilling are 5mm, depth 60mm;The drilling for cleaning coal petrography sample, after to be dried, by stainless steel high-voltage tube In line insertion drilling, and the gap of stainless steel high pressure line and the wall of a borehole is poured using epoxide-resin glue;It is small to place 24 When;
2. stainless steel high pressure line to be passed through to the porous plate a(2 of experimental rig), the centre bore of left pressure head (4), and stainless steel High pressure line and left pressure head (4) are tightly fixed by cutting ferrule;Later, it is put into triaxial cell's cavity together, installation second is solid Determine device (25), it is made gently to resist left pressure head (4);Then, porous plate b(3 is successively installed on the right side of the triaxial cell), it is right Pressure head (5) and axis pressure cavity are fixed device (8), screw axis pressure cavity fixed device (8), second fixed device (25), so that Left pressure head (4), left porous plate (2), coal petrography sample (1), porous plate b(3) and right pressure head (5) tightly contact;
3. opening heating temperature-controlling system, temperature is set as given temperature (25 °C -300 °C), certain rate of heat addition is set (5 °C/min-40 °C/min), after reaching given temperature, after heat preservation 4 hours, i.e., it is believed that the temperature of coal petrography sample reaches given Temperature;
4. opening axis pressure, confining pressure constant current constant voltage pump, and valve V10, V9 are opened, and cooling device (42) are pressed by axis respectively, are enclosed It presses cooling device (41), loaded medium (water or silicone oil) is each led into axis and presses cavity, in triaxial cell's cavity, make axis Pressure, confining pressure respectively reach setting value σ1、σ3MPa, and keep constant.
5. coal petrography sample CH4 permeability k before pressure break1Measurement, the specific steps are as follows: CH4Gas in gas cylinder (40) is logical Valve V3 is crossed, is passed into fracturing pump (38), setting osmotic pressure is given pressureP 0MPa, and keepP 0MPa is constant, opens Valve V4, gas is passed into preheater, and temperature (25 °C -300 °C) identical with coal petrography sample is arranged, then opens valve V7, CH4Gas is passed into osmotic pressure entrance (14) by second pressure sensor (32);Valve V1 is closed, in left pressure head (4) Position on the lower side be equipped with a circular hole (6), stainless steel high pressure line and circular hole (6) connection, open valve V8, be passed into graduated cylinder (28) in, using draining water gathering of gas law, the gas volume in cooling water of units of measurement time in graduated cylinder passes through after gas volume is stablized The value calculates CH of the coal petrography sample under the conditions of temperature, axis pressure, confining pressure4Permeability is denoted as k1
6. closing valve V3 and V7, and the gas in preheater and fracturing pump is emptied, by the way of vacuumizing, empties coal petrography CH inside sample4Gas;
7. opening pressure-deformation monitors system, the deformation of coal petrography sample axial direction is acquired by axial deformation acquisition device;Pass through Radial displacement acquisition device acquires radial deformation in fracturing process, is become by the volume of fluid in the confining pressure constant current constant voltage pump of acquisition Change the radial deformation for measuring coal petrography sample;
Measuring radial deformation, the specific method is as follows: assuming that the original length of coal petrography sample isL 0Mm, diameter ared 0mm;?t 0= When 0, the integrated flux of confining pressure constant current constant voltage pump isV 0The reading of ml, LVDT displacement sensor isa 0 mm;?t 1When, confining pressure constant current The integrated flux of constant pressure pump isV 1Ml, LVDT displacement sensor are reada 1 Mm, the decrement of coal petrography specimen lengthL(axis To deflection) be
The diameter of rock coal petrography sample after then deformingd 1For
The then radial strain of the coal petrography sample at the moment is
As further explanation, under hot conditions, constant current constant voltage pump can not work well, therefore, can be in constant current constant voltage Add a cooling device before pump, cooled down by the way of water circulation, so that the temperature of constant current constant voltage pump is maintained at permanent Fixed temperature (see figure 1);As further explanation, under the high temperature conditions, Jie of the silicone oil as loading axis pressure, confining pressure can be used Matter;As further explanation, under hot conditions, LVDT displacement sensor is by unsuitable work.Therefore, work is pressed using in axis hydraulic fluid The outside of plug adds cooling water circulating device (12) Lai Jiangwen, guarantees that the temperature of LVDT displacement sensor position maintains Temperature indoors;
8. acoustic emission monitoring system is opened, for monitoring the crack initiation, extension of coal petrography and closing characteristics in fracturing process;
9. opening dioxide bottle, valve V2 is opened, and start fracturing pump, valve V4 is opened, using constant current mode, with perseverance Fixed flow carbon dioxide injection into preheater, and sets preheater temperature, heats to carbon dioxide, reaches it To supercriticality, then by valve V5, a four-way valve (30), four way valve are connected to by keeping the temperature stainless steel high-voltage tube It is separately connected temperature sensor (31) and pressure sensor (29), and accesses valve V1, passes through pressure break entrance (26), is linked into examination Inside sample, then, using the mode of constant current, fracturing pump constantly toward injecting supercritical carbon dioxide inside coal petrography sample, until Pressure break success;
Further illustrate, above-mentioned four-way valve can guarantee to accurately measure the temperature of supercritical carbon dioxide in fracturing process, Pressure change, so as to preferably judge the postcritical phase-state change of supercritical carbon dioxide in fracturing process;
10. closing valve V2, valve V3, the supercritical carbon dioxide gas being vented in preheater and fracturing pump repeats step (5), the CH of coal petrography sample after pressure break is obtained4Gas permeability k2
11. keeping axis pressure set by coal petrography sample, confining pressure, temperature-resistant, setting 6 hours are time gradient, repeat step 5, Post-fracturing coal petrography sample is measured in the CH of different moments4Permeability so just obtains coal petrography after supercritical carbon dioxide pressure break CH of the sample under creep effect4The Evolution of permeability;Meanwhile it being acquired by axial deformation acquisition device and radial deformation The Evolution of axial deformation and radial deformation of the post-fracturing coal petrography sample under creep effect also can be obtained in device;
12. closing power supply, and all devices are put back to as former state after testing.
The preferred embodiment of the present invention has shown and described in above description, as previously described, it should be understood that the present invention is not office Be limited to form disclosed herein, should not be regarded as an exclusion of other examples, and can be used for various other combinations, modification and Environment, and can be changed within that scope of the inventive concept describe herein by the above teachings or related fields of technology or knowledge It is dynamic.And changes and modifications made by those skilled in the art do not depart from the spirit and scope of the present invention, then it all should be appended by the present invention In scope of protection of the claims.

Claims (7)

1. coal petrography supercritical carbon dioxide pressure break-creep-seepage tests method under high temperature and pressure, it is characterized in that including following steps It is rapid:
(1) coal petrography sample is processed into diameter is 50 mm, and length is the cylindrical body coal petrography sample of 100mm;In the axis of coal petrography sample Heart drilling, the diameter of drilling are 5mm, depth 60mm;The drilling for cleaning coal petrography sample, after to be dried, by stainless steel high-voltage tube In line insertion drilling, and the gap of stainless steel high pressure line and the wall of a borehole is poured using epoxide-resin glue;It is small to place 24 When;
(2) stainless steel high pressure line is passed through to the porous plate a(2 of experimental rig), the centre bore of left pressure head (4), and stainless steel High pressure line and left pressure head (4) are tightly fixed by cutting ferrule;Later, it is put into triaxial cell's cavity together, installation second is solid Determine device (25), it is made gently to resist left pressure head (4);Then, porous plate b(3 is successively installed on the right side of the triaxial cell), it is right Pressure head (5) and axis pressure cavity are fixed device (8), screw axis pressure cavity fixed device (8), second fixed device (25), so that Left pressure head (4), left porous plate (2), coal petrography sample (1), porous plate b(3) and right pressure head (5) tightly contact;
(3) heating temperature-controlling system to be opened, and temperature is set as 25 °C -300 °C, the setting rate of heat addition is 5 °C/min-40 °C/ Min, after reaching given temperature, after heat preservation 4 hours;
(4) axis pressure, confining pressure constant current constant voltage pump are opened, and opens valve V10, V9, and cooling device (42) are pressed by axis respectively, are enclosed It presses cooling device (41), loaded medium is each led into axis pressure cavity, in triaxial cell's cavity, makes axis pressure, confining pressure difference Reach setting value σ1、σ3MPa, and keep constant;
(5) coal petrography sample CH before pressure break4Permeability k1Measuring process it is as follows: CH4Gas in gas cylinder (40) passes through valve V3, lead to Enter in fracturing pump (38), setting osmotic pressure is given pressureP 0 MPa, and keepP 0MPa is constant, valve V4 is opened, gas Body is passed into preheater, and it is 25 °C -300 °C that temperature identical with coal petrography sample, which is arranged, then opens valve V7, CH4Gas It is passed into osmotic pressure entrance (14) by pressure sensor 2(32);Valve V1 is closed, is set in the position on the lower side of left pressure head (4) There are a circular hole (6), stainless steel high pressure line and circular hole (6) connection, opens valve V8, be passed into graduated cylinder (28), using row Water gas collection method, the gas volume in cooling water of units of measurement time in graduated cylinder calculate the coal by the value after gas volume is stablized CH of the rock sample under the conditions of temperature, axis pressure, confining pressure4Permeability is denoted as k1
(6) valve V3 and V7 are closed, and empties the gas in preheater and fracturing pump, by the way of vacuumizing, empties coal petrography CH inside sample4Gas;
(7) it opens pressure-deformation and monitors system, the deformation of coal petrography sample axial direction is acquired by axial deformation acquisition device;Pass through Radial displacement acquisition device acquires radial deformation in fracturing process, is become by the volume of fluid in the confining pressure constant current constant voltage pump of acquisition Change the radial deformation for measuring coal petrography sample;
Measuring radial deformation, the specific method is as follows: assuming that the original length of coal petrography sample isL 0Mm, diameter ared 0mm;?t 0= When 0, the integrated flux of confining pressure constant current constant voltage pump isV 0The reading of ml, LVDT displacement sensor isa 0 mm;?t 1When, confining pressure constant current The integrated flux of constant pressure pump isV 1Ml, LVDT displacement sensor are reada 1 Mm, the decrement of coal petrography specimen lengthLFor
The diameter of coal petrography sample after then deformingd 1For
The then radial strain of the coal petrography sample at the moment is
(8) acoustic emission monitoring system is opened, crack initiation, extension and the closing characteristics of coal petrography sample in fracturing process are monitored;
(9) dioxide bottle is opened, opens valve V2, and start fracturing pump, valve V4 is opened, with constant flow dioxy Change carbon to be injected into preheater, and set preheater temperature, carbon dioxide is heated, carbon dioxide is made to reach supercritical state State, carbon dioxide are passed through temperature sensor (31) and pressure sensing by valve V5, heat preservation stainless steel high-voltage tube, four-way valve (30) Device (29), and it is passed through valve V1, it passes through pressure break entrance (26), is passed into inside coal petrography sample, fracturing pump is constantly by constant current Supercritical carbon dioxide injects inside coal petrography sample, until pressure break success;
(10) valve V2, V3 are closed, the supercritical carbon dioxide gas being vented in preheater and fracturing pump is repeated step (5), obtained The CH of coal petrography sample after to pressure break4Gas permeability k2
(11) axis pressure set by coal petrography sample, confining pressure, temperature-resistant is kept, setting 6 hours are time gradient, step 5 is repeated, Post-fracturing coal petrography sample is measured in the CH of different moments4Permeability so just obtains coal petrography after supercritical carbon dioxide pressure break CH of the sample under creep effect4The Evolution of permeability;Meanwhile it being acquired by axial deformation acquisition device and radial deformation The Evolution of axial deformation and radial deformation of the post-fracturing coal petrography sample under creep effect also can be obtained in device.
2. high temperature and pressure coal petrography supercritical carbon dioxide pressure break-creep-seepage tests method according to claim 1, It is characterized in that test temperature can achieve 300 °C, axis pressure, confining pressure can achieve 70MPa.
3. coal petrography supercritical carbon dioxide pressure break-creep-seepage tests method under high temperature and pressure according to claim 1, It is characterized in the experimental rig, it is characterized in that by triaxial cell, axis pressure and confining pressure loading system, heating temperature-controlling system, surpassing and facing Boundary's carbon-dioxide generator system, acoustic emission monitoring system, pressure-deformation monitoring system, permeability measurement systems composition;It is described Triaxial cell includes triaxial cell's cylinder (16), porous plate b(3), porous plate a(2), left pressure head (4), right pressure head (5), axis To hydraulic piston (10), axis pressure cavity (9), axis pressure cavity fixed device (8), rubber sleeve (22), coning sleeve b(18), coning sleeve a (23), first fixed device (24), second fixed device (25);Triaxial cell's cylinder (16) have axially through Triaxial cell's cavity (21), axis press cavity fixed device (8) and triaxial cell's cavity (21) coaxially, triaxial cell's cylinder (16) side wall is disposed with confining pressure entrance (20), confining pressure outlet (15) and thermometric entrance (19);Coning sleeve a(23) and taper Set b(18) it is separately positioned on two pressure head peripheries;Cavity between rubber sleeve (22) and triaxial cell's cylinder (16) forms three Axis pressure chamber cavity (21);Coning sleeve a(23) and coning sleeve b(18) front end is tapered, guarantee coning sleeve a, coning sleeve b and rubber Sealed between set, coning sleeve a(23) and coning sleeve b(18) sealed between triaxial cell's cylinder (16) by O-ring;The One fixed device (24) are connect with triaxial cell's cylinder (16), and axis presses cavity fixed device (8) and triaxial cell's cylinder (16) connect, to realize fixed coning sleeve a(23) and coning sleeve b(18) purpose;Second fixed device (25) connection first is solid Determine device (24), second fixed device (25) are against left pressure head (4) left side and squeeze porous plate a(2), guarantee porous plate a(2) With the left end face contact of coal petrography sample (1);Place the right pressure that an end face diameter is 50mm in the left end of axial hydraulic piston (10) Porous plate b(3 is arranged on the left of right pressure head (5) in head (5)), porous plate b(3) it offsets with the right end of coal petrography sample;Constant current is pressed by axis Constant pressure pump is filled to axis and presses cavity (9) inner, so that axial hydraulic piston (10) be pushed to be loaded;
The described axis pressure and confining pressure loading system include axis pressure constant current constant voltage pump (34), confining pressure constant current constant voltage pump (36), valve V9, Valve V10, axis press cooling device (42), confining pressure cooling device (41), and axis pressure constant current constant voltage pump (34) is linked by valve V10 Axis presses cooling device (42), and is connected in axis pressure cavity (9) and realizes axis pressure load;Confining pressure constant current constant voltage pump (36) passes through valve V9 is connected to confining pressure cooling device (41), and accesses in triaxial cell's cavity (21), realizes the load of confining pressure;
The heating temperature-controlling system includes heating mantle (17), heating device (35), the first temperature sensor (33), heating mantle (17) It is wrapped in outside the cavity of triaxial cell and connects heating device (35), the first temperature sensor (33) is inserted into thermometric entrance (19) The temperature for carrying out detection coal petrography sample (1) carries out the real-time control of temperature by heating device (35);
The supercritical carbon dioxide generator system, by CO2Gas cylinder (39), fracturing pump (38), preheater (37) and heat preservation Stainless steel high pressure line composition, is connected with valve V4, fracturing pump (38) and CO between preheater (37) and fracturing pump (38)2Gas cylinder (39) valve V2 is connected between;
Pressure-deformation monitoring system (43) includes pressure-temperature acquisition device, axial deformation acquisition device, radial position Move acquisition device;
The pressure-temperature acquisition device includes computer, first pressure sensor (29), second pressure sensor (32), and One pressure sensor (29), second pressure sensor (32), the first temperature sensor (31), second temperature sensor (33), LVDT displacement sensor (13), axis pressure constant current constant voltage pump (34), confining pressure constant current constant voltage pump (36), fracturing pump (38) pass through multichannel Data collecting card is connected in computer, is surveyed for each temperature and pressure sensor in automatic measurement, record experimentation Temperature and pressure value, and record the flow and pressure of fracturing pump;
The axial deformation acquisition device includes LVDT displacement transducer fixed support (11) and LVDT displacement sensor (13) And multi-channel data acquisition board, LVDT displacement transducer fixed support (11) are fixed on axis pressure cavity fixed device (8), LVDT displacement sensor (13) is symmetrically mounted at the two sides of axis pressure hydraulic piston (10), and LVDT displacement sensor bottom end is supported respectively Hydraulic piston (10) right side is pressed in axis, and guarantees LVDT displacement sensor (13), axis pressure hydraulic piston (10) and three axis pressures The axis of power room cylinder (16) is parallel to each other;
The radial displacement acquisition device, pressure-temperature acquisition device include first pressure sensor (29), second pressure sensing Device (32), the first temperature sensor (31), second temperature sensor (33), LVDT displacement sensor (13), axis press constant current constant voltage Pump (36), confining pressure constant current constant voltage pump (34), fracturing pump (38) are connected with multichannel collecting box, and are linked into computer, realize pressure Power, flow, temperature and the real-time acquisition of deformation;Permeability measurement systems are by CH4Gas cylinder (40), fracturing pump (38), preheater (37), graduated cylinder (28), valve V3, valve V4, valve V7, valve V8 and heat preservation stainless steel high pressure line composition;
CH4Gas cylinder (40) passes through valve V3 connection fracturing pump (38), CH4Gas cylinder (40) passes through valve V4 connection preheater (38); CH4Gas cylinder (40) passes through valve V7 to osmotic pressure entrance (14).
4. high temperature and pressure coal petrography supercritical carbon dioxide pressure break-creep-seepage tests method according to claim 2, The left pressure head (4) in triaxial cell described in being characterized in that is equipped with centre bore (46), and stainless steel high pressure line passes through centre bore Into coal petrography sample (1), supercritical carbon dioxide crushing test is realized, while stainless steel high pressure line passes through cutting ferrule and left pressure head It is sealed, when guaranteeing that crushing test and permeability survey are tested, gas is not from the gap of stainless steel high pressure line and centre bore Place's outflow.
5. high temperature and pressure coal petrography supercritical carbon dioxide pressure break-creep-seepage tests method according to claim 3, The lower part of the left pressure head (4) in triaxial cell described in being characterized in that is equipped with circular hole (6), passes through valve V8 and graduated cylinder (28) phase Even, it is ensured that in the measurement of coal petrography sample permeability, after closing valve V1, gas is flowed out from the left side of coal petrography sample, is passed through Circular hole (6) is passed into graduated cylinder.
6. high temperature and pressure coal petrography supercritical carbon dioxide pressure break-creep-seepage tests method according to claim 3, It is characterized in that three acoustic emission probe preformed holes, left pressure head is respectively set in the left side of left pressure head, the right side of right pressure head (4), right pressure head (5) is provided with circulating water cooling device water inlet (44) and circulating water cooling device water outlet (45), realizes The cooling of left and right pressure head under the conditions of hot test, guarantees the operating temperature of acoustic emission probe.
7. high temperature and pressure coal petrography supercritical carbon dioxide pressure break-creep-seepage tests method according to claim 3, It is characterized in that four-way valve (30) is respectively connected to the first temperature sensor (31) and first pressure sensor (29), with pressure break entrance phase Even, it is ensured that temperature, the pressure change of the supercritical carbon dioxide in fracturing process at the same position are accurately measured, with Just more accurately judge the phase-state change of supercritical carbon dioxide in fracturing process.
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