CN103018132B - Dynamic deformation characteristic testing method in coal absorption and desorption process - Google Patents
Dynamic deformation characteristic testing method in coal absorption and desorption process Download PDFInfo
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- CN103018132B CN103018132B CN201210558897.0A CN201210558897A CN103018132B CN 103018132 B CN103018132 B CN 103018132B CN 201210558897 A CN201210558897 A CN 201210558897A CN 103018132 B CN103018132 B CN 103018132B
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- 238000010521 absorption reaction Methods 0.000 title claims abstract description 175
- 239000003245 coal Substances 0.000 title claims abstract description 122
- 238000000034 method Methods 0.000 title claims abstract description 67
- 238000012360 testing method Methods 0.000 title claims abstract description 58
- 230000008569 process Effects 0.000 title claims abstract description 55
- 238000003795 desorption Methods 0.000 title claims abstract description 32
- 230000002860 competitive effect Effects 0.000 claims abstract description 8
- 238000001179 sorption measurement Methods 0.000 claims description 58
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 32
- 239000000523 sample Substances 0.000 claims description 24
- 230000008859 change Effects 0.000 claims description 18
- 238000002336 sorption--desorption measurement Methods 0.000 claims description 18
- 238000011144 upstream manufacturing Methods 0.000 claims description 12
- 239000003034 coal gas Substances 0.000 claims description 10
- 238000005259 measurement Methods 0.000 claims description 10
- 230000006641 stabilisation Effects 0.000 claims description 7
- 230000004083 survival effect Effects 0.000 claims description 6
- 238000010998 test method Methods 0.000 claims description 6
- 239000004576 sand Substances 0.000 claims description 4
- 230000000274 adsorptive effect Effects 0.000 claims description 3
- 239000003818 cinder Substances 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 230000010429 evolutionary process Effects 0.000 abstract 4
- 238000009825 accumulation Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 167
- 239000000243 solution Substances 0.000 description 101
- 238000009434 installation Methods 0.000 description 14
- 239000011435 rock Substances 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 9
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 8
- 238000012545 processing Methods 0.000 description 6
- 230000009467 reduction Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 230000007246 mechanism Effects 0.000 description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 description 4
- 239000001569 carbon dioxide Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000001307 helium Substances 0.000 description 4
- 229910052734 helium Inorganic materials 0.000 description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 4
- 210000000867 larynx Anatomy 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000013508 migration Methods 0.000 description 3
- 230000005012 migration Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
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- 239000003638 chemical reducing agent Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000005538 encapsulation Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 241001442654 Percnon planissimum Species 0.000 description 1
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- Filling Or Discharging Of Gas Storage Vessels (AREA)
- Separation Of Gases By Adsorption (AREA)
Abstract
The invention discloses a dynamic deformation characteristic testing method in a coal absorption and desorption process. The method comprises the following steps: (1) measuring empty volumes of a high-pressure air accumulation bottle and a high-pressure absorption and desorption tank; (2) mounting samples; (3) measuring the free space volume of the absorption and desorption tank; (4) implementing the dynamic coal evolutionary process test in a gas isothermal constant-volume absorption process; (5) implementing the dynamic coal evolutionary process test in a gas isothermal constant-pressure absorption process; (6) implementing the absorption-desorption dynamic evolution process test under the gas constant-volume and variable-temperature condition; (7) implementing the dynamic coal evolutionary process test in a gas competitive absorption process; and (8) implementing the dynamic coal evolutionary process test in a gas desorption process. The method is easy to operate; and the accuracy of test results is high.
Description
Technical field
The present invention relates to a kind of experiment test device and method of testing, particularly relating to a kind of proving installation for measuring coal deformation amount in coal body Adsorption and desorption methane gas process and method.
Background technology
Coal and non-coal interaction mechanism is the Basic Science Problem of Gas Disaster prevention and control field research, it not only has important directive function to probing into mine coal rock gas dynamic disaster mechanism, simultaneously also for the extraction of coal-bed gas or cbm development provide important technical support.Mine gas is created on the metamorphic episode of coal, mainly deposits to be adsorbed in the state tax that microporosity is surperficial and pressure-bearing is in coal petrography body opening, crack.Coal body-country rock system is in the equilibrium state of geo-stationary under gas pressure and rock mass stress acting in conjunction.When well work mining activity enters in coal seam and country rock thereof, this equilibrium state is disturbed, and causes coal and rock stress field to redistribute the migration again with gas in coal rock layer.In equilibrium state change process, micro-microscopical structure change of coal body, except the effect being subject to surrouding rock stress, is also also subject to the impact of the pore gas pressure of free state gas generation and the coal body dilatational strain of ADSORPTION STATE gas generation to a great extent.A large amount of actual phenomenons and test findings show, the change of this coal body condition caused due to gas absorption, desorb plays an important role in gas dynamical disaster generating process.Therefore, the evolution mechanism of dynamic evolution mechanism to deep understanding coal rock gas dynamic disaster studying the distortion of coal body Adsorption and desorption gas has vital role.Adsorption and desorption distortion is the inherent characteristic of coal body, and its deformation values reflects coal mass strength, metamorphic grade, coal seam temperature, pore characteristic and cranny development degree and the power containing gas ability.Under same external condition, the deformation values of outstanding coal is much larger than non-protruding coal.Therefore, the Adsorption and desorption deformation characteristic of coal body also measures Coal Seam Outburst Hazard booster action.In addition, in the migration process of coal-bed gas, the Adsorption and desorption of gas can make coal body produce expansion, drawdown deformation, the mechanical property of coal body is changed, thus causes the pore texture of coal petrography to change, and then cause the infiltrative change of coal petrography.Meanwhile, the pore texture of coal petrography and infiltration coefficient change affect again the tax of gas in coal body conversely and deposit and flowing.Therefore, the true migration rule of coal-bed gas be obtained, then must consider the impact that coal body Adsorption and desorption is out of shape.
The method measuring coal gas adsorbance has a lot, and conventional mainly contains gravimetric method and volumetric method.Volumetric method is placed in the closed system of known volume by coal body, under a series of methane gas pressure, according to equation of gaseous state, i.e. gaseous mass and relation between temperature, pressure and volume, calculate methane gas by adsorbance.It is reasonable that volumetric method measuring technology has assay method, the features such as determinator is simple, easy to operate, and the data of test are reliable, directly perceived, is universities and colleges of China, the Research Center method that mainly adopts of office in one's power.But current volumetric method proving installation, has certain limitation when measuring Adsorption and desorption distortion, such as, the sample of these proving installations is all adopt graininess coal sample, and coal sample size, between 0.25 ~ 0.18mm, is difficult to obtain Adsorption and desorption deflection; The structure of High Pressure Absorption solution cucurbitula is the design of particle coal sample specially, process applicable lump coal sample very difficult; In addition High Pressure Absorption solution cucurbitula does not generally arrange deformation measurement interface yet.
In recent years, along with people are to coal rock gas dynamic disaster mechanism, coal-bed gas exploitation and CO
2the improving constantly of technical concerns degree such as to be sealed up for safekeeping in coal seam, and many researchers start the research of coal petrography absorption, absorption distortion and perviousness measurement aspect, and in succession develop technology and the device of test coal petrography adsorbance and Adsorption and desorption distortion.Although these devices are developed by the Adsorption and desorption distortion of measuring coal body specially, experiment condition often can not meet the demands.As shorter in existing equipment time of equilibrium adsorption, the equilibration time of most experiment is all within 60 hours, and adsorb the block coal sample of deformation test and be different from graininess coal sample, especially when testing with raw coal, the time of equilibrium adsorption of coal body is much longer, the hundreds of of wanting had just can reach balance in individual hour, and existing equipment is subject to the restriction of stability, can not reach this requirement; The Adsorption and desorption deformation test gaseous tension great majority utilizing existing equipment to carry out are within 5.0MPa, and coal body under high pressure, often show characteristic when being different from low pressure, therefore need the proving installation (0 ~ 10.0MPa) that can realize High Pressure Absorption distortion; When carrying out desorb deformation test, according to Practical Project situation, needing to test the deformation values of coal sample under different pressures gradient, therefore, needing the desorb for coal containing methane gas to provide a controlled environmental pressure.Equally, gas with various and CH is being utilized
4between competitive Adsorption effect carry out CO
2during the tests such as coal seam is sealed up for safekeeping, coal-seam gas gas injection increasing is adopted, also need the pressure environment providing a gas and vapor permeation and displacement, these are all that existing test unit is irrealizable; In addition, existing volumetric method testing apparatus, when calculating adsorbance, all have ignored the impact of Adsorption and desorption distortion on free space volumes of coal body, there is certain error between the adsorbance thus recorded and true adsorbance.
Therefore, those skilled in the art are devoted to develop and a kind ofly make proving installation that in coal body Adsorption and desorption methane gas process, the Deformation Analysis result reliability is higher and method of testing.
Summary of the invention
Because the above-mentioned defect of prior art, technical matters to be solved by this invention is to provide and a kind ofly makes proving installation that in coal body Adsorption and desorption methane gas process, the Deformation Analysis result reliability is higher and method of testing.
For realizing the object of the first level of the present invention, the invention provides a kind of coal body adsorption-desorption methane gas process deformation test device, comprising deformation test system, the gentle body control system of High Pressure Absorption solution cucurbitula; Described deformation test system comprises the resistance strain gage and electric wire strain gauge that are connected to each other; Described electric wire strain gauge is connected with integrated processing terminal; Described integrated processing terminal is connected with pressure acquisition card;
Described High Pressure Absorption solution cucurbitula comprises tank body and is arranged on the top cover above described tank body; Sealing gasket is provided with between described tank body and described top cover; The top of described tank body is provided with radial flange; Described tank body and top cover are fastened by fastening clamp; Described fastening clamp comprises the first clip portion and the second clip portion of separated from one another, structural symmetry; The larynx hoop that described first clip portion and the second clip portion are arranged by cylindrical is held tightly; The lower end of described fastening clamp is provided with the snap ring of convex; Described snap ring can snap in the bottom surface of described radial flange; The upper end of described fastening clamp is provided with the pressure ring of convex; Described pressure ring and clip head clearance are arranged; Described clip top and described pressure ring are evenly equipped with housing screw at circumferencial direction;
Described top cover comprises base portion and the interface installation portion of one; Described interface installation portion passes described fastening clamp; Described interface installation portion is provided with the gas interface, gas pressure sensor interface and the stress-strain measurement interface that are communicated with tank inner chamber;
Described stress-strain measurement interface comprises the first through hole stud; The lower end of described first through hole stud and described top cover threaded engagement, upper end coordinates with the first check nut; Perforated baffle is provided with between the top of described first through hole stud and described first check nut; The first wire is had by epoxy encapsulation in described first through hole stud; The upper end of described first wire is connected with described electric wire strain gauge with after the first check nut through described perforated baffle; The lower end of described first wire is stretched in described tank body, and can be connected with described resistance strain gage;
Described gas pressure sensor interface is connected with the first gas pressure sensor;
Described gas control system comprises high pressure air bottle; The endpiece of described high pressure air bottle is connected with the second gas pressure sensor; Described second gas pressure sensor is connected with the first needle valve; Described first needle valve is connected with described gas interface; The entrance point of described high pressure air bottle is connected with the first four-way connection;
First gas circuit of described first four-way connection is connected with gas diffusion mouth, vacuum pump, the first retaining valve and the first needle valve in turn; Second gas circuit of described first four-way connection is connected with flowmeter, the second retaining valve, the second needle valve in turn; 3rd gas circuit of described first four-way connection is connected with the second four-way connection;
First gas circuit of described second four-way connection is connected with high pressure methane bottle, methane pressure reducer valve, the 3rd needle valve in turn; Second gas circuit of described second four-way connection is connected with high pressure helium gas cylinder, helium reduction valve and the 4th needle valve in turn; 3rd gas circuit of described second four-way connection is connected with high-pressure carbon dioxide bottle, carbon dioxide reduction valve and the 5th needle valve in turn.
For improving sealing effectiveness further, described top cover surface is provided with annular groove to described tank body side; Described tank body is provided with the axial ledge coordinated with described annular groove; Described sealing gasket arranges the top of described axial ledge.
For the temperature conditions of accurate Control experiment, described tank body is outside equipped with the first heating jacket; Described high pressure air bottle is outside equipped with the second heating jacket; Described second heating jacket is provided with thermopair; Described integrated processing terminal is connected with temperature controller.
Preferably, described larynx hoop is T-shaped bolt larynx hoop.
For realizing the object of the present invention second aspect, the invention provides a kind of method to dynamic deformation characteristic test in coal body Adsorption and desorption gas process, concrete steps are as follows:
A () measures the volume of high pressure air bottle and High Pressure Absorption solution cucurbitula
First, when High Pressure Absorption desorb ullage is put, vacuum tightness is evacuated to high pressure air bottle and High Pressure Absorption solution cucurbitula and reaches below 4.0Pa;
Secondly, the He gas of 0.2MPa is poured in high pressure air bottle; Inflation is stopped after pressure stability; Measure the force value p in high pressure air bottle
rwith the force value p in High Pressure Absorption solution cucurbitula
s;
Again, He is filled with in High Pressure Absorption solution cucurbitula, the equilibrium pressure force value p in measurement high pressure air bottle after pressure stabilisation and High Pressure Absorption solution cucurbitula
e0; He gas in release High Pressure Absorption solution cucurbitula, high pressure air bottle and pipeline, makes the pressure in High Pressure Absorption solution cucurbitula, high pressure air bottle and pipeline equal with ambient pressure;
Finally, be that High Pressure Absorption solution cucurbitula is put in the solid metal reference block of Vn by known volume, repeat aforesaid operations, and read the force value p in High Pressure Absorption solution cucurbitula before inflation in high pressure air bottle respectively
r', the force value p in High Pressure Absorption solution cucurbitula
s' with the equalized pressure p after inflation in High Pressure Absorption solution cucurbitula
e0';
If the pressure p before twice pressure equilibrium in High Pressure Absorption solution cucurbitula
sand p
s' be all less than 4Pa, then ignore the survival gas in High Pressure Absorption solution cucurbitula, think that it is vacuum state, then calculate high pressure air bottle and pipeline thereof according to following system of equations, the volume of High Pressure Absorption solution cucurbitula and pipeline thereof:
V
r, V
s, V
n---be respectively high pressure air bottle and manifold volume, High Pressure Absorption solution cucurbitula and manifold volume thereof and reference block volume, unit is cm
3;
P
r, p
s, p
e0---be respectively the pressure of high pressure air bottle and High Pressure Absorption solution cucurbitula after the pressure of high pressure air bottle under High Pressure Absorption desorb ullage configuration state, the pressure of High Pressure Absorption solution cucurbitula and balance, unit is MPa;
P
r', p
s', p
e0'---be respectively the pressure that High Pressure Absorption solution cucurbitula inserts high pressure air bottle and High Pressure Absorption solution cucurbitula after the pressure of high pressure air bottle under reference block state, the pressure of High Pressure Absorption solution cucurbitula and balance, unit is MPa;
Z
r0, Z
r0'---be respectively High Pressure Absorption solution cucurbitula under blank state and under inserting reference block state, the compressibility factor of high pressure air bottle initial gas, dimensionless;
Z
e0, Z
e0'---be respectively High Pressure Absorption solution cucurbitula under blank state and under inserting reference block state, the compressibility factor of gas under high pressure air bottle and High Pressure Absorption solution cucurbitula equilibrium condition, dimensionless;
B () sample is installed:
The coal cinder fetched from coal seam is made rectangular parallelepiped or right cylinder coal sample according to the volume of tank body; At specimen surface, resistance strain gage is installed, and sample is placed in High Pressure Absorption solution cucurbitula;
C () measures the free space volumes of High Pressure Absorption solution cucurbitula:
First, system is vacuumized; When vacuum tightness reaches below 4.0Pa, still keep the state that vacuumizes 1 hour;
Secondly, the He gas of 0.2MPa is poured in high pressure air bottle; Inflation is stopped after pressure stability; Read the force value p in high pressure air bottle
1with the force value p in High Pressure Absorption solution cucurbitula
2;
Finally, He is filled with in High Pressure Absorption solution cucurbitula, reading high pressure air bottle force value p after pressure stabilisation
e1; He gas in release High Pressure Absorption solution cucurbitula, high pressure air bottle and pipeline, makes the pressure in High Pressure Absorption solution cucurbitula, high pressure air bottle and pipeline equal with ambient pressure;
If the pressure p before pressure equilibrium in High Pressure Absorption solution cucurbitula
2be less than 4Pa, then ignore the survival gas in High Pressure Absorption solution cucurbitula, think that it is vacuum state.Free space volumes is calculated according to Boyle's law:
V
f---High Pressure Absorption tank free space volumes, unit is cm
3;
V
r---be high pressure air bottle and manifold volume thereof, unit is cm
3;
P
1, p
e1---be respectively the original pressure of He gas in high pressure air bottle and the pressure after balancing, unit is MPa;
Z
r1---for High Pressure Absorption solution cucurbitula under vacuum conditions, the compressibility factor in high pressure air bottle under He gas original pressure, dimensionless;
Z
e1---for High Pressure Absorption solution cucurbitula is after being filled with He gas, the compressibility factor of gas under high pressure air bottle and High Pressure Absorption solution cucurbitula equilibrium condition, dimensionless;
D () carries out coal body Dynamic Evolution test in gas isothermal constant volume adsorption process:
First, again system is vacuumized, make vacuum tightness reach 4.0Pa;
Secondly, in high pressure air bottle, the CH of 1.0MPa ~ 10.0MPa is filled with
4; Stop inflation after pressure stability, and read the force value p in now high pressure air bottle
3with the force value in High Pressure Absorption solution cucurbitula; If the force value in High Pressure Absorption solution cucurbitula is less than 4Pa, then continue next step, otherwise repeat above step;
Finally, by CH
4be filled with in High Pressure Absorption solution cucurbitula, read the pressure value P a in adsorption process mesohigh air bottle
i; The gas adsorption amount of coal body is calculated according to following equation:
Q
t1---coal gas adsorbance (STP), unit is cm
3;
V
f---High Pressure Absorption solution cucurbitula free space volumes, unit is cm
3;
V
r---the volume of high pressure air bottle and pipeline thereof, unit is cm
3;
V
ai---due to the cubic deformation amount that coal body adsorption gas causes, unit is cm
3;
Z
r3---for High Pressure Absorption solution cucurbitula under vacuum conditions, high pressure air bottle is filled with CH
4compressibility factor under rear original pressure, dimensionless;
P
ai---the force value in adsorption process mesohigh air bottle, unit is MPa;
Z
ai---CH in adsorption process
4pressure is p
aitime compressibility factor, dimensionless;
T
c---thermostat temperature, unit is K;
T
0---mark condition temperature, unit is K;
P
0---mark condition pressure, unit is MPa;
E () carries out coal body Dynamic Evolution test in gas isothermal level pressure adsorption process:
First, again 4.0Pa is evacuated to system;
Secondly, in high pressure air bottle, CH is filled with
4, CH
4force value be greater than test set pressure 2.0MPa ~ 3.0MPa; Stop inflation after pressure stability, and read the force value p in now high pressure air bottle
4; And the top hole pressure of high pressure air bottle is set as experimental test pressure p
5, make CH
4gas is filled with in the tank body of High Pressure Absorption solution cucurbitula; Keep pressure stability in High Pressure Absorption solution cucurbitula;
Finally, in 30 minutes, when the pressure change in high pressure air bottle is no more than 0.02MPa, thinks and reach adsorption equilibrium, record the force value p in now high pressure air bottle
6;
The gas adsorption amount of coal body is obtained by following equation:
Q
t2---coal gas adsorbance (STP), unit is cm
3;
V
f---High Pressure Absorption solution cucurbitula free space volumes, unit is cm
3;
V
r---the volume of high pressure air bottle and pipeline thereof, unit is cm
3;
V
ai---due to the cubic deformation amount that coal body adsorption gas causes, unit is cm
3;
Z
r4---for High Pressure Absorption solution cucurbitula under vacuum conditions, high pressure air bottle is filled with CH
4compressibility factor under rear original pressure, dimensionless;
Z
r5---for High Pressure Absorption solution cucurbitula is at CH
4pressure is p
5under compressibility factor, dimensionless;
Z
r6---for high pressure air bottle is at CH
4pressure is p
6under compressibility factor, dimensionless;
T
c---thermostat temperature, unit is K;
T
0---mark condition temperature, unit is K;
P
0---mark condition pressure, unit is MPa;
F () carries out gas constant volume temperature match curing conditions under, absorption-desorption Dynamic Evolution is tested:
First, according to the step of (d), make the coal sample in High Pressure Absorption solution cucurbitula reach adsorption-desorption balance, read high pressure air bottle force value p now
7;
Secondly, High Pressure Absorption solution cucurbitula is made to reach probe temperature T
i;
Finally, in temperature changing process, keep the gas gross in High Pressure Absorption solution cucurbitula not change, reaching under new temperature conditions, the adsorption-desorption balance making coal body reach new, reads high pressure air bottle force value p now
bi;
Then in temperature changing process, the change of coal body adsorbance is calculated by following formula:
Q
t3---coal gas adsorbance (STP), unit is cm
3;
V
a1, V
aj---the cubic deformation amount of coal body in initial equilibrium conditions and alternating temperature process, unit is cm
3;
P
bi---after temperature variation, coal body reaches the force value of high pressure air bottle when new adsorption-desorption balances, and unit is MPa;
Z
r7, Z
bi---be p at pressure respectively
7, p
bi, temperature T
1, T
ithe compressibility factor of lower methane, dimensionless;
T
1, T
i---be respectively the temperature after initial equilibrium temperature and change, unit is K;
V
f---High Pressure Absorption solution cucurbitula free space volumes, unit is cm
3
V
r---the volume of high pressure air bottle and pipeline thereof, unit is cm
3;
T
0---mark condition temperature, unit is K;
P
0---mark condition pressure, unit is MPa;
G () carries out coal body Dynamic Evolution test in gas competitive adsorption process:
First, isolated high-voltage air bottle and High Pressure Absorption solution cucurbitula; Pressure in high pressure air bottle and upstream is reduced to standard atmospheric pressure; Vacuum tightness is evacuated to high pressure air bottle and upstream and is less than 4.0Pa;
Secondly, in high pressure air bottle, CO is filled with
2gas, CO
2the pressure of gas is according to CO
2the adsorptive pressure of relatively different coal body is determined;
Finally, by CO
2gas is filled with in High Pressure Absorption solution cucurbitula, makes CO
2and CH
4being at war with property is adsorbed, until when the pressure in high pressure air bottle reaches stationary value, then show CO
2and CH
4reach adsorption-desorption balance;
Coal body Dynamic Evolution test in (h) desorption of mash gas process:
When measuring solution and being drawn onto standard atmospheric pressure, record gas flow;
When measuring (4Pa ~ standard atmospheric pressure) when solution is drawn onto negative pressure state, first isolated high-voltage air bottle and High Pressure Absorption solution cucurbitula, be reduced to standard atmospheric pressure by the pressure in high pressure air bottle and upstream thereof; Then high pressure air bottle and upstream thereof are vacuumized, after predetermined negative pressure to be achieved (4Pa ~ standard atmospheric pressure), stop vacuumizing, be communicated with high pressure air bottle and High Pressure Absorption solution cucurbitula, carry out the desorb under negative pressure;
When measuring solution and being drawn onto fixation pressure, carry out according to the following steps:
First isolated high-voltage air bottle and High Pressure Absorption solution cucurbitula, be reduced to standard atmospheric pressure by the pressure in high pressure air bottle and upstream thereof; Then high pressure air bottle and upstream thereof are vacuumized, after predetermined negative pressure to be achieved (4Pa ~ standard atmospheric pressure), stop vacuumizing; CH is filled with in high pressure air bottle
4, CH
4pressure be default desorption pressures; Finally, be communicated with high pressure air bottle and High Pressure Absorption solution cucurbitula, be fixed the desorb under pressure, when the pressure in high pressure air bottle reaches stationary value, reach desorb balance;
I () carries out in process above (d)-(g) step, except step (f), and can by Systematical control in stationary temperature; And by the pressure of pressure acquisition card and gas pressure sensor real time record and each measuring point of display; Shown in real time by electric wire strain gauge and record the stress and strain on coal body surface.
In other embodiments, also dioxide bottle can be replaced by other gas cylinders, thus test the competitive Adsorption of methane and other gases in making step (g).
The invention has the beneficial effects as follows:
(1) the present invention solves the problem of gas adsorption-desorption process and coal deformation synchro measure preferably, by custom-designed gas control system, achieve the gas adsorption-desorb Dynamic Evolution test under isothermal constant volume, isothermal level pressure, constant volume temperature match curing conditions, and the desorption of mash gas deformation test under different pressures gradient and the test under the effect of gas with various competitive Adsorption, the fields such as exploitation of oil-gas field, shale gas exploitation, nuclear waste disposal are also with a wide range of applications.
(2) this device High Pressure Absorption, desorb test macro stability is high, good seal performance, intensity are high, can meet the requirement of higher gas absorption pressure and longer adsorption time.
(3) this device is when calculating gas adsorption amount, and efficiently solve adsorption-desorption and be out of shape the free space volumes error caused, make the adsorbance calculated closer to actual value, test findings reliability is high; On the other hand, in computation process, have ignored the small quantity that may have an impact to test findings, thus simplify experiment calculation process.
(4) this experimental technique is simple, widely applicable, can simulate the evolution of mine coal rock gas dynamic disaster, coal bed gas extraction (or cbm development) and CO more truly
2the field condition of gas absorption desorb problem such as to be sealed up for safekeeping in coal seam, for more in depth research provides shop experiment study condition.
Accompanying drawing explanation
Fig. 1 is the structural representation of the embodiment of the invention.
Fig. 2 is the structural representation of embodiment of the invention mesohigh adsorption-desorption tank.
Fig. 3 is the partial enlarged drawing at I place in Fig. 2.
Fig. 4 is the A direction view of Fig. 3.
Fig. 5 is the structural representation of stress-strain measurement interface in the embodiment of the invention.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described:
As shown in Figures 1 to 5, a kind of coal body absorption desorbs proving installation, comprises High Pressure Absorption solution cucurbitula, deformation test system and gas control system.
Deformation test system comprises the resistance strain gage 32 and electric wire strain gauge 35 that are connected to each other.Electric wire strain gauge 35 is connected with integrated processing terminal 36, and integrated processing terminal 36 is connected with pressure acquisition card 38.
The top cover 27 that High Pressure Absorption solution cucurbitula comprises tank body 28 and is arranged on above tank body 28, top cover 27 is provided with annular groove 27c towards tank body 28 side, and tank body 28 is provided with the axial ledge 28b coordinated with annular groove 27c, and sealing gasket 39 arranges the top of axial ledge 28b.The top of tank body 28 is provided with radial flange 28a.
Tank body 28 and top cover 27 are fastened by fastening clamp 30.Fastening clamp 30 comprises the tommyhead bolt larynx hoop 44 that the first clip portion 30a of separated from one another, structural symmetry and the second clip portion 30b, the first clip portion 30a and the second clip portion 30b arranged by cylindrical and holds tightly.The lower end of fastening clamp 30 is provided with the snap ring 30c of convex, and snap ring 30c can snap in the bottom surface of radial flange 28a.The upper end of fastening clamp 30 is provided with the pressure ring 30d of convex, and pressure ring 30d and 30e interval, clip top are arranged, and clip top 30e and pressure ring 30d is evenly equipped with housing screw 30f at circumferencial direction.
Top cover 27 comprises base portion 27a and the interface installation portion 27b of one, and interface installation portion 27b passes fastening clamp 30.Interface installation portion 27b is provided with the gas interface 24, gas pressure sensor interface 25 and the stress-strain measurement interface 26 that are communicated with tank inner chamber.
Stress-strain measurement interface 26 comprises lower end and top cover 27 threaded engagement of the first through hole stud 40, first through hole stud 40, and upper end coordinates with the first check nut 41.Perforated baffle 42 is provided with between the top of the first through hole stud 40 and the first check nut 49, the upper end of the first wire 43, first wire 43 is had to be connected with electric wire strain gauge 35 through perforated baffle 42 and the first check nut 49 are rear by epoxy encapsulation in first through hole stud 40.The lower end of the first wire 43 is stretched in tank body 28, and can be connected with resistance strain gage 32.
Gas pressure sensor interface 25 is connected with the first gas pressure sensor 31.
Gas control system comprises high pressure air bottle 21, the endpiece of high pressure air bottle 21 is connected with the second gas pressure sensor 22, second gas pressure sensor 22 is connected with the 6th needle valve 23,6th needle valve 23 is connected with gas interface 24, and the entrance point of high pressure air bottle 21 is connected with the first four-way connection 8.
First gas circuit of the first four-way connection 8 is connected with gas diffusion mouth 1, vacuum pump 2, first retaining valve 3 and the first needle valve 4 in turn; Second gas circuit of the first four-way connection 8 is connected with flowmeter 5, second retaining valve 6, second needle valve 7 in turn; 3rd gas circuit of the first four-way connection 8 is connected with the second four-way connection 15.
First gas circuit of the second four-way connection 15 is connected with high pressure methane bottle 19, methane pressure reducer valve 10, the 3rd needle valve 11 in turn; Second gas circuit of the second four-way connection 15 is connected with high pressure helium gas cylinder 12, helium reduction valve 13 and the 4th needle valve 14 in turn; 3rd gas circuit of the second four-way connection 15 is connected with high-pressure carbon dioxide bottle 19, carbon dioxide reduction valve 17 and the 5th needle valve 16 in turn.
Tank body 28 is outside equipped with the first heating jacket 34; High pressure air bottle 21 is outside equipped with the second heating jacket 20; Second heating jacket 20 is provided with thermopair 19; Integrated processing terminal 36 is connected with temperature controller 37.
During proving installation work, first carry out test preliminary work, comprise making sample: the coal cinder fetched from coal seam is made rectangular parallelepiped or right cylinder coal sample according to the volume of tank body 28; At specimen surface, resistance strain gage 32 is installed, resistance strain gage 32 is connected with the first wire 43.
As follows to the concrete steps of dynamic deformation characteristic test in coal body Adsorption and desorption gas process:
A () measures the volume of high pressure air bottle and High Pressure Absorption solution cucurbitula
First, when High Pressure Absorption desorb ullage is put, top cover 27 and fastening clamp 30 are installed, tighten housing screw 30f in order, heating jacket 34 is rolled in the outside of tank body 28, connects the gas interface 24 on tank body 28, gas pressure sensor interface 25 and each surveying instrument; Open the first needle valve 4 and the 6th needle valve 23, determine that other needle valve is in closed condition, start vacuum pump 2, system is vacuumized; When vacuum tightness reaches below 4.0Pa, close the first needle valve 4 and the 6th needle valve 23;
Secondly, open high pressure He gas cylinder 12, regulate He reduction valve 13, after making it reach 0.2MPa, open the 4th needle valve 14, make He gas pour high pressure air bottle 21; Close the 4th needle valve 14 after pressure stability, read the indicating value p of now the second gas pressure sensor 22
rwith the indicating value p of the first gas pressure sensor 31
s;
Again, open the 6th needle valve 23, make He be filled with in tank body 28, the indicating value p of reading second gas pressure sensor 22 after pressure stabilisation
e, now it is equal with the indicating value of the first pressure transducer 31; After record, open the second needle valve 7, the He gas in release High Pressure Absorption solution cucurbitula, high pressure air bottle and pipeline, after pressure is equal with ambient pressure, closes the second needle valve 7;
Finally, be that High Pressure Absorption solution cucurbitula is put in the solid metal reference block of Vn by known volume, repeat aforesaid operations, and read the indicating value p that the 6th needle valve 23 opens front second gas pressure sensor respectively
r', the indicating value p of the first gas pressure sensor 31
s' the equalized pressure p after opening with the 6th needle valve 23
e'.
If the pressure p before twice pressure equilibrium in High Pressure Absorption solution cucurbitula
sand p
s' be all less than 4Pa, then ignore the survival gas in High Pressure Absorption solution cucurbitula, think that it is vacuum state.High pressure air bottle and pipeline thereof is calculated, the volume of High Pressure Absorption solution cucurbitula and pipeline thereof according to following system of equations:
V
r, V
s, V
n---be respectively high pressure air bottle and manifold volume, High Pressure Absorption solution cucurbitula and manifold volume thereof and reference block volume, unit is cm
3;
P
r, p
s, p
e0---be respectively the pressure of high pressure air bottle and High Pressure Absorption solution cucurbitula after the pressure of high pressure air bottle under High Pressure Absorption desorb ullage configuration state, the pressure of High Pressure Absorption solution cucurbitula and balance, unit is MPa;
P
r', p
s', p
e0'---be respectively the pressure that High Pressure Absorption solution cucurbitula inserts high pressure air bottle and High Pressure Absorption solution cucurbitula after the pressure of high pressure air bottle under reference block state, the pressure of High Pressure Absorption solution cucurbitula and balance, unit is MPa;
Z
r0, Z
r0'---be respectively High Pressure Absorption solution cucurbitula under blank state and under inserting reference block state, the compressibility factor of high pressure air bottle initial gas, dimensionless;
Z
e0, Z
e0'---be respectively High Pressure Absorption solution cucurbitula under blank state and under inserting reference block state, the compressibility factor of gas under high pressure air bottle and High Pressure Absorption solution cucurbitula equilibrium condition, dimensionless.
PaPa (b) sample is installed:
At specimen surface, resistance strain gage 32 is installed, resistance strain gage 32 is connected with the first wire 43; Sample is put into tank body 28, top cover 27 and fastening clamp 30 are installed, tighten housing screw 30f in order, heating jacket 34 is rolled in the outside of tank body 28, connect the gas interface 24 on tank body 28, gas pressure sensor interface 25 and stress-strain measurement interface 26, and each surveying instrument; Check each valve, determine all to be in closed condition; Open temp controller 37, and temperature is set as test temperature.
C () measures the free space volumes of High Pressure Absorption solution cucurbitula:
First, open the first needle valve 4 and the 6th needle valve 23, start vacuum pump 2, system is vacuumized; When vacuum tightness reaches below 4.0Pa, vacuum pump 2 continuous service, after 1 hour, closes the first needle valve 4 and the 6th needle valve 23;
Secondly, open high pressure He gas cylinder 12, regulate He reduction valve 13, after making it reach 0.2MPa, open the 4th needle valve 14, make He gas pour high pressure air bottle 21; Close the 4th needle valve 14 after pressure stability, read the indicating value p of now the second gas pressure sensor 22
1, the indicating value p of the first pressure transducer 31
2.
Finally, open the 6th needle valve 23, make He be filled with in tank body 28, the indicating value p of reading after pressure stabilisation now the second gas pressure sensor 22
e; After record, open the second needle valve 7, the He gas in release High Pressure Absorption solution cucurbitula, high pressure air bottle and pipeline, after pressure is equal with ambient pressure, closes the second needle valve 7.
Equally, if the pressure p before pressure equilibrium in High Pressure Absorption solution cucurbitula
2be less than 4Pa, then ignore the survival gas in High Pressure Absorption solution cucurbitula, think that it is vacuum state.Free space volumes is calculated according to Boyle's law:
V
f---High Pressure Absorption solution cucurbitula free space volumes, unit is cm
3;
V
r---be high pressure air bottle and manifold volume thereof, unit is cm
3;
P
1, p
e1---be respectively the original pressure of He gas in high pressure air bottle and the pressure after balancing, unit is MPa;
Z
r1---for High Pressure Absorption solution cucurbitula under vacuum conditions, the compressibility factor in high pressure air bottle under He gas original pressure, dimensionless;
Z
e1---for High Pressure Absorption solution cucurbitula is after being filled with He gas, the compressibility factor of gas under high pressure air bottle and High Pressure Absorption solution cucurbitula equilibrium condition, dimensionless.
Pa (d) carries out coal body Dynamic Evolution test in gas isothermal constant volume adsorption process:
First, open the first needle valve 4 and vacuum pump 2 successively, again vacuumize system, vacuum tightness closes the first needle valve 4 after reaching 4.0Pa;
Secondly, high pressure CH is opened
4gas cylinder 9, regulates CH
4reduction valve 10, reaches (this predetermined pressure is determined according to test pressure, generally at 1.0MPa ~ 10.0MPa) after predetermined pressure, opens the 3rd needle valve 11, make CH
4gas is filled with high pressure air bottle 21; Close the 3rd needle valve 11 after pressure stability, read the indicating value p of now the second gas pressure sensor 22
3with the indicating value p of the first pressure transducer 31
3; If the indicating value of the first gas pressure sensor 31 is less than 4Pa, then continue next step, otherwise repeat above step;
Finally, open the 6th needle valve 23, make CH
4be filled with in High Pressure Absorption desorb tank 28, read the indicating value p of the second gas pressure sensor 22 in adsorption process
i.The gas adsorption amount of coal body is calculated according to following equation:
Q
t1---coal gas adsorbance (STP), unit is cm
3;
V
f---High Pressure Absorption solution cucurbitula free space volumes, unit is cm
3; V
r---the volume of high pressure air bottle and pipeline thereof, unit is cm
3;
V
ai---due to the cubic deformation amount that coal body adsorption gas causes, unit is cm
3;
Z
r3---for High Pressure Absorption solution cucurbitula under vacuum conditions, high pressure air bottle is filled with CH
4compressibility factor under rear original pressure, dimensionless;
P
ai---the force value in adsorption process mesohigh air bottle, unit is MPa;
Z
ai---CH in adsorption process
4pressure is p
aitime compressibility factor, dimensionless;
T
c---thermostat temperature, unit is K;
T
0---mark condition temperature, unit is K;
P
0---mark condition pressure, unit is MPa;
Pa (e) carries out coal body Dynamic Evolution test in gas isothermal level pressure adsorption process:
When carrying out isothermal constant-pressure test, need the 6th needle valve 23 to be replaced by the adjustable variable valve of top hole pressure, then operate according to the following steps:
First, open the first needle valve 4 and vacuum pump 2 successively, again system is vacuumized, after reaching 4.0Pa, close the first needle valve 4;
Secondly, high pressure CH is opened
4gas cylinder 9, regulates CH
4reduction valve 10, reaches (this predetermined pressure is determined according to test pressure, is generally greater than test pressure 2.0MPa ~ 3.0MPa) after predetermined pressure, opens the 3rd needle valve 11, make CH
4gas is filled with high pressure air bottle 21, closedown after pressure stabilisation 3rd needle valve 11; Read the indicating value p of now the second gas pressure sensor 22
4;
Open variable valve, and to set top hole pressure be experimental test pressure p
5, make CH
4gas is filled with in the tank body 28 of High Pressure Absorption solution cucurbitula; Keep variable valve to be in opening always, with reference to the indicating value of the first gas sensor 31, supplement source of the gas, keep pressure stability in High Pressure Absorption solution cucurbitula; Finally, in 30 minutes, when the pressure change in high pressure air bottle is no more than 0.02MPa, thinks and reach adsorption equilibrium, record the indicating value p of now the second pressure transducer
6.
The gas adsorption amount of coal body can be obtained by following equation:
Q
t2---coal gas adsorbance (STP), unit is cm
3;
V
f---High Pressure Absorption solution cucurbitula free space volumes, unit is cm
3;
V
r---the volume of high pressure air bottle and pipeline thereof, unit is cm
3;
V
ai---due to the cubic deformation amount that coal body adsorption gas causes, unit is cm
3;
Z
r4---for High Pressure Absorption solution cucurbitula under vacuum conditions, high pressure air bottle is filled with CH
4compressibility factor under rear original pressure, dimensionless;
Z
r5---for High Pressure Absorption solution cucurbitula is at CH
4pressure is p
5under compressibility factor, dimensionless;
Z
r6---for high pressure air bottle is at CH
4pressure is p
6under compressibility factor, dimensionless;
T
c---thermostat temperature, unit is K;
T
0---mark condition temperature, unit is K;
P
0---mark condition pressure, unit is MPa;
Under Pa (f) carries out gas constant volume temperature match curing conditions, absorption-desorption Dynamic Evolution is tested:
First, according to the step of (d), make the coal sample in High Pressure Absorption solution cucurbitula reach adsorption-desorption balance, read the indicating value p of the second gas pressure sensor
7;
Secondly, by regulating temperature controller 37, thermopair 19 and the first heating jacket 34 being had an effect, makes High Pressure Absorption solution cucurbitula reach probe temperature T
i;
Finally, in temperature changing process, keep the gas gross in High Pressure Absorption solution cucurbitula not change, reaching under new temperature conditions, the adsorption-desorption balance making coal body reach new, reads the indicating value p of the second gas pressure sensor
i
Then in temperature changing process, the change of coal body adsorbance is calculated by following formula:
Q
t3---coal gas adsorbance (STP), unit is cm
3;
V
a1, V
aj---the cubic deformation amount of coal body in initial equilibrium conditions and alternating temperature process, unit is cm
3;
P
bi---after temperature variation, coal body reaches the force value of high pressure air bottle when new adsorption-desorption balances, and unit is MPa;
Z
r7, Z
bi---be p at pressure respectively
7, p
bi, temperature T
1, T
ithe compressibility factor of lower methane, dimensionless;
T
1, T
i---be respectively the temperature after initial equilibrium temperature and change, unit is K;
V
f---High Pressure Absorption solution cucurbitula free space volumes, unit is cm
3
V
r---the volume of high pressure air bottle and pipeline thereof, unit is cm
3;
T
0---mark condition temperature, unit is K;
P
0---mark condition pressure, unit is MPa;
Pa (g) carries out coal body Dynamic Evolution test in gas competitive adsorption process:
First, the 6th needle valve 23 is closed, then open the second needle valve 7, the pressure in pipeline and high pressure air bottle 21 is reduced to standard atmospheric pressure; Close the second needle valve 7, open the first needle valve 4, start vacuum pump, high pressure air bottle 21 and pipeline are vacuumized, is less than after 4.0Pa until vacuum tightness, close the first needle valve 4;
Secondly, by CO
2gas cylinder 18 is opened, and regulates CO
2reduction valve 17, opens the 5th needle valve 16, by certain pressure (according to CO
2the adsorptive pressure of relatively different coal body is determined) CO
2gas inject high pressure air bottle 21, and close the 5th needle valve 16;
Finally, open the 6th needle valve 23, make CO
2and CH
4being at war with property is adsorbed, until when the second gas pressure sensor 22 reaches stationary value, then show CO
2and CH
4reach adsorption-desorption balance;
Coal body Dynamic Evolution test in (h) desorption of mash gas process:
When measuring solution and being drawn onto standard atmospheric pressure, only the second needle valve 7 need be opened, record gas flow by flowmeter 5;
When measuring (4Pa ~ standard atmospheric pressure) when solution is drawn onto negative pressure state, first the 6th needle valve 23 being closed, then opening the second needle valve 7, the pressure in pipeline and high pressure air bottle 21 is reduced to standard atmospheric pressure; Close the second needle valve 7, open the first needle valve 4, start vacuum pump 2, high pressure air bottle 21 and pipeline are vacuumized, after predetermined negative pressure to be achieved (4Pa ~ standard atmospheric pressure), closes the first needle valve 4; Finally, open the 6th needle valve 23, carry out the desorb under negative pressure;
When measuring solution and being drawn onto fixation pressure, carry out according to the following steps: first, then the second needle valve 7 is opened, pressure in pipeline and high pressure air bottle 21 is reduced to standard atmospheric pressure, closes the second needle valve 7, open the first needle valve 4, start vacuum pump 2, high pressure air bottle 21 and pipeline are vacuumized, after predetermined vacuum tightness to be achieved, closes the first needle valve 4; Secondly, by CH
4gas cylinder 9 is opened, and regulates CH
4reduction valve 10, opens the 3rd needle valve 11, by the CH of certain pressure (predetermined desorption pressures, its value is 0MPa-adsorption equilibrium pressure)
4after gas inject high pressure air bottle 21, close the 3rd needle valve 11; Finally, open the 6th needle valve 23, the coal seam with gas in High Pressure Absorption solution cucurbitula is at the CH of certain pressure
4under carry out desorb, when the second gas pressure sensor 22 reaches stationary value, reach desorb balance;
I () carries out in process above (d)-(g) step, except step (f), temperature controller 37 and thermopair 19 by Systematical control in stationary temperature; The pressure of pressure acquisition card 38 and the second gas pressure sensor 22 real time record and each measuring point of display; By electric wire strain gauge 35 display in real time and the stress and strain recording coal body surface.
In other embodiments, also dioxide bottle can be replaced by other gas cylinders, thus test the competitive Adsorption of methane and other gases in making step (g).
The order of step (d) (e) (f) can be omitted, and also can sequentially exchange.
More than describe preferred embodiment of the present invention in detail.Should be appreciated that those of ordinary skill in the art just design according to the present invention can make many modifications and variations without the need to creative work.Therefore, all technician in the art, all should by the determined protection domain of claims under this invention's idea on the basis of existing technology by the available technical scheme of logical analysis, reasoning, or a limited experiment.
Claims (2)
1. a dynamic deformation characteristics test method in coal body adsorption-desorption process, is characterized in that: comprise the following steps:
(1) empty volume of high pressure air bottle and High Pressure Absorption solution cucurbitula is measured:
11) when High Pressure Absorption desorb ullage is put, vacuum tightness is evacuated to high pressure air bottle and High Pressure Absorption solution cucurbitula and reaches below 4.0Pa;
12) the He gas of 0.2MPa is poured in high pressure air bottle; Inflation is stopped after pressure stability; Measure the force value p in high pressure air bottle
rwith the force value p in High Pressure Absorption solution cucurbitula
s;
13) He is filled with in High Pressure Absorption solution cucurbitula, the equilibrium pressure force value p in measurement high pressure air bottle after pressure stabilisation and High Pressure Absorption solution cucurbitula
e0; He gas in release High Pressure Absorption solution cucurbitula, high pressure air bottle and pipeline, makes the pressure in High Pressure Absorption solution cucurbitula, high pressure air bottle and pipeline equal with ambient pressure;
14) be that High Pressure Absorption solution cucurbitula is put in the solid metal reference block of Vn by known volume, repeat above-mentioned 11) to 13) operation, and read the force value p in High Pressure Absorption solution cucurbitula before inflation in high pressure air bottle respectively
r', the force value p in High Pressure Absorption solution cucurbitula
s' and High Pressure Absorption solution cucurbitula in inflation after equalized pressure p
e0';
If the pressure p before twice pressure equilibrium in High Pressure Absorption solution cucurbitula
sand p
s' be all greater than 4Pa, then repeat step 11) to 14); If the pressure p before twice pressure equilibrium in High Pressure Absorption solution cucurbitula
sand p
s' be all less than 4Pa, then ignore the survival gas in High Pressure Absorption solution cucurbitula, think that it is vacuum state, then calculate high pressure air bottle and pipeline thereof according to following system of equations, the volume of High Pressure Absorption solution cucurbitula and pipeline thereof:
V
r, V
s, V
n---be respectively high pressure air bottle and manifold volume, High Pressure Absorption solution cucurbitula and manifold volume thereof and reference block volume, unit is cm
3;
P
r, p
s, p
e0---be respectively the pressure of high pressure air bottle and High Pressure Absorption solution cucurbitula after the pressure of high pressure air bottle under High Pressure Absorption desorb ullage configuration state, the pressure of High Pressure Absorption solution cucurbitula and balance, unit is MPa;
P
r', p
s', p
e0'---be respectively the pressure that High Pressure Absorption solution cucurbitula inserts high pressure air bottle and High Pressure Absorption solution cucurbitula after the pressure of high pressure air bottle under reference block state, the pressure of High Pressure Absorption solution cucurbitula and balance, unit is MPa;
Z
r0, Z
r0'---be respectively High Pressure Absorption solution cucurbitula under blank state and under inserting reference block state, the compressibility factor of high pressure air bottle initial gas, dimensionless;
Z
e0, Z
e0'---be respectively High Pressure Absorption solution cucurbitula under blank state and under inserting reference block state, the compressibility factor of gas under high pressure air bottle and High Pressure Absorption solution cucurbitula equilibrium condition, dimensionless;
(2) sample is installed:
The coal cinder fetched from coal seam is made rectangular parallelepiped or right cylinder coal sample according to the volume of tank body; At specimen surface, resistance strain gage is installed, and sample is placed in High Pressure Absorption solution cucurbitula;
(3) free space volumes of High Pressure Absorption solution cucurbitula is measured:
31) vacuumize with high pressure air bottle and the tank connected gas charging system of High Pressure Absorption desorb; When vacuum tightness reaches below 4.0Pa, still keep the state that vacuumizes 1 hour;
32) the He gas of 0.2MPa is poured in high pressure air bottle; Inflation is stopped after pressure stability; Read the force value p in high pressure air bottle
1with the force value p in High Pressure Absorption solution cucurbitula
2;
33) He is filled with in High Pressure Absorption solution cucurbitula, reading high pressure air bottle force value p after pressure stabilisation
e1; He gas in release High Pressure Absorption solution cucurbitula, high pressure air bottle and pipeline, makes the pressure in High Pressure Absorption solution cucurbitula, high pressure air bottle and pipeline equal with ambient pressure;
If the pressure p before pressure equilibrium in High Pressure Absorption solution cucurbitula
2be greater than 4Pa, then repeat step 31) to 33); If p
2be less than 4Pa, then ignore the survival gas in High Pressure Absorption solution cucurbitula, think that it is vacuum state; Free space volumes is calculated according to Boyle's law:
V
f---High Pressure Absorption solution cucurbitula free space volumes, unit is cm
3;
V
r---be high pressure air bottle and manifold volume thereof, unit is cm
3;
P
1, p
e1---be respectively the original pressure of He gas in high pressure air bottle and the pressure after balancing, unit is MPa;
Z
r1---for High Pressure Absorption solution cucurbitula under vacuum conditions, the compressibility factor in high pressure air bottle under He gas original pressure, dimensionless;
Z
e1---for High Pressure Absorption solution cucurbitula is after being filled with He gas, the compressibility factor of gas under high pressure air bottle and High Pressure Absorption solution cucurbitula equilibrium condition, dimensionless;
(4) coal body Dynamic Evolution test in gas isothermal constant volume adsorption process is carried out:
41) again system is vacuumized, make vacuum tightness reach 4.0Pa;
42) in high pressure air bottle, be filled with the CH of 1.0MPa ~ 10.0MPa
4; Stop inflation after pressure stability, and read the force value p in now high pressure air bottle
3with the force value in High Pressure Absorption solution cucurbitula; If the force value in High Pressure Absorption solution cucurbitula is less than 4Pa, then continues next step, otherwise enter step 41);
43) by CH
4be filled with in High Pressure Absorption solution cucurbitula, read the pressure value P a in adsorption process mesohigh air bottle
i; The gas adsorption amount of coal body is calculated according to following equation:
Q
t1---coal gas adsorbance (STP), unit is cm
3;
V
f---High Pressure Absorption solution cucurbitula free space volumes, unit is cm
3; V
r---the volume of high pressure air bottle and pipeline thereof, unit is cm
3;
V
ai---due to the cubic deformation amount that coal body adsorption gas causes, unit is cm
3;
Z
r3---for High Pressure Absorption solution cucurbitula under vacuum conditions, high pressure air bottle is filled with CH
4compressibility factor under rear original pressure, dimensionless;
Z
ai---CH in adsorption process
4pressure is p
aitime compressibility factor, dimensionless;
T
c---thermostat temperature, unit is K;
T
0---mark condition temperature, unit is K;
P
0---mark condition pressure, unit is MPa;
(5) coal body Dynamic Evolution test in gas isothermal level pressure adsorption process is carried out:
51) again 4.0Pa is evacuated to system;
52) in high pressure air bottle, CH is filled with
4, CH
4force value be greater than test set pressure 2.0MPa ~ 3.0MPa; Stop inflation after pressure stability, and read the force value p in now high pressure air bottle
4; And the top hole pressure of high pressure air bottle is set as experimental test pressure p
5, make CH
4gas is filled with in the tank body of High Pressure Absorption solution cucurbitula; Keep pressure stability in High Pressure Absorption solution cucurbitula;
53) in 30 minutes, when the pressure change in high pressure air bottle is no more than 0.02MPa, thinks and reach adsorption equilibrium, record the force value p in now high pressure air bottle
6;
The gas adsorption amount of coal body is obtained by following equation:
Q
t2---coal gas adsorbance (STP), unit is cm
3;
V
f---High Pressure Absorption solution cucurbitula free space volumes, unit is cm
3;
V
r---the volume of high pressure air bottle and pipeline thereof, unit is cm
3;
V
ai---due to the cubic deformation amount that coal body adsorption gas causes, unit is cm
3;
Z
r4---for High Pressure Absorption solution cucurbitula under vacuum conditions, high pressure air bottle is filled with CH
4compressibility factor under rear original pressure, dimensionless;
Z
r5---for High Pressure Absorption solution cucurbitula is at CH
4pressure is p
5under compressibility factor, dimensionless;
Z
r6---for high pressure air bottle is at CH
4pressure is p
6under compressibility factor, dimensionless;
T
c---thermostat temperature, unit is K;
T
0---mark condition temperature, unit is K;
P
0---mark condition pressure, unit is MPa;
(6) under carrying out gas constant volume temperature match curing conditions, absorption-desorption Dynamic Evolution is tested:
61) according to the step of (4), make the coal sample in High Pressure Absorption solution cucurbitula reach adsorption-desorption balance, read high pressure air bottle force value p now
7;
62) High Pressure Absorption solution cucurbitula is made to reach probe temperature T
i;
63) in temperature changing process, keep the gas gross in High Pressure Absorption solution cucurbitula not change, reaching under new temperature conditions, the adsorption-desorption balance making coal body reach new, reads high pressure air bottle force value p now
bi;
Then in temperature changing process, the change of coal body adsorbance is calculated by following formula:
Q
t3---coal gas adsorbance (STP), unit is cm
3;
V
a1, V
aj---the cubic deformation amount of coal body in initial equilibrium conditions and alternating temperature process, unit is cm
3;
Z
r7, Z
bi---be p at pressure respectively
7, p
bi, temperature T
1, T
ithe compressibility factor of lower methane, dimensionless;
T
1, T
i---be respectively the temperature after initial equilibrium temperature and change, unit is K;
V
f---High Pressure Absorption solution cucurbitula free space volumes, unit is cm
3
V
r---the volume of high pressure air bottle and pipeline thereof, unit is cm
3;
T
0---mark condition temperature, unit is K;
P
0---mark condition pressure, unit is MPa;
(7) coal body Dynamic Evolution test in gas competitive adsorption process is carried out:
71) isolated high-voltage air bottle and High Pressure Absorption solution cucurbitula; Pressure in high pressure air bottle and upstream is reduced to standard atmospheric pressure; Vacuum tightness is evacuated to high pressure air bottle and upstream and is less than 4.0Pa;
72) in high pressure air bottle, CO is filled with
2gas, CO
2the pressure of gas is according to CO
2the adsorptive pressure of relatively different coal body is determined;
73) by CO
2gas is filled with in High Pressure Absorption solution cucurbitula, makes CO
2and CH
4being at war with property is adsorbed, until when the pressure in high pressure air bottle reaches stationary value, then show CO
2and CH
4reach adsorption-desorption balance;
(8) coal body Dynamic Evolution test in desorption of mash gas process:
When measuring solution and being drawn onto standard atmospheric pressure, record gas flow;
When measuring solution and being drawn onto negative pressure state, namely during 4Pa ~ standard atmospheric pressure, first isolated high-voltage air bottle and High Pressure Absorption solution cucurbitula, be reduced to standard atmospheric pressure by the pressure in high pressure air bottle and upstream thereof; Then high pressure air bottle and upstream thereof are vacuumized, after predetermined negative pressure to be achieved, namely reach Pa after 4Pa ~ standard atmospheric pressure, stop vacuumizing, be communicated with high pressure air bottle and High Pressure Absorption solution cucurbitula, carry out the desorb under negative pressure;
When measuring solution and being drawn onto fixation pressure, carry out according to the following steps:
First isolated high-voltage air bottle and High Pressure Absorption solution cucurbitula, be reduced to standard atmospheric pressure by the pressure in high pressure air bottle and upstream thereof; Then high pressure air bottle and upstream thereof are vacuumized, after predetermined negative pressure to be achieved, namely reach Pa after 4Pa ~ standard atmospheric pressure, stop vacuumizing; CH is filled with in high pressure air bottle
4, CH
4pressure be default desorption pressures; Finally, be communicated with high pressure air bottle and High Pressure Absorption solution cucurbitula, be fixed the desorb under pressure, when the pressure in high pressure air bottle reaches stationary value, reach desorb balance.
2. dynamic deformation characteristics test method in coal body adsorption-desorption process as claimed in claim 1, it is characterized in that: in above (4), (5), (7) step carry out in process, by Systematical control in stationary temperature, and by the pressure of pressure acquisition card and gas pressure sensor real time record and each measuring point of display; Shown in real time by electric wire strain gauge and record the stress and strain on coal body surface.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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| CN109540733A (en) * | 2019-01-10 | 2019-03-29 | 中国矿业大学(北京) | Changes of heat flux experimental apparatus for testing and method during a kind of coal adsorption-desorption gas |
| CN109946215B (en) * | 2019-04-22 | 2024-05-24 | 洛阳理工学院 | In-situ coal gas adsorption capacity test simulation device |
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| US4758408A (en) * | 1985-02-27 | 1988-07-19 | The United States Of America As Represented By The Secretary Of The Air Force | Automatic oxygen measuring system |
| CN201778806U (en) * | 2010-07-26 | 2011-03-30 | 长江大学 | Full-automatic multifunctional isothermal line adsorption and desorption and pollution evaluation experimental instrument |
| CN101936861A (en) * | 2010-07-30 | 2011-01-05 | 中国矿业大学 | Test method of supercritical carbon dioxide content in coal |
| CN201965069U (en) * | 2010-08-13 | 2011-09-07 | 中国科学院山西煤炭化学研究所 | Instrument for simultaneously and automatically measuring adsorption capacity and adsorption swelling capacity of coal petrography in high pressure gas |
| CN101975718B (en) * | 2010-08-13 | 2012-11-14 | 中国科学院山西煤炭化学研究所 | Method for simultaneously measuring high-pressure gas adsorption capacity and adsorption swell capacity of coal petrography and measuring equipment |
| CN202502025U (en) * | 2012-02-29 | 2012-10-24 | 中国矿业大学(北京) | Device for high pressure isothermal absorption experiment of coal |
| CN102636424B (en) * | 2012-04-24 | 2013-12-18 | 中煤科工集团重庆研究院 | Method and device for measuring coal rock adsorption gas quantity and permeability |
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