CN104792644A - Test method of coal and rock sample free volume expansion amount in competitive adsorption process - Google Patents
Test method of coal and rock sample free volume expansion amount in competitive adsorption process Download PDFInfo
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- 239000003245 coal Substances 0.000 title claims abstract description 78
- 238000000034 method Methods 0.000 title claims abstract description 35
- 230000008569 process Effects 0.000 title claims abstract description 30
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 19
- 230000002860 competitive effect Effects 0.000 title claims abstract description 17
- 238000010998 test method Methods 0.000 title claims abstract description 15
- 239000011435 rock Substances 0.000 title abstract description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 88
- 238000012360 testing method Methods 0.000 claims abstract description 72
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 44
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 43
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- 239000007788 liquid Substances 0.000 claims description 26
- 238000013461 design Methods 0.000 claims description 19
- 239000001307 helium Substances 0.000 claims description 19
- 229910052734 helium Inorganic materials 0.000 claims description 19
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 19
- 230000006835 compression Effects 0.000 claims description 18
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- 230000000630 rising effect Effects 0.000 claims description 3
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- 238000002347 injection Methods 0.000 abstract description 11
- 239000007924 injection Substances 0.000 abstract description 11
- 238000012544 monitoring process Methods 0.000 abstract description 5
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Abstract
The invention discloses a test method of coal and rock sample free volume expansion amount in a competitive adsorption process and belongs to the field of coal-bed methane exploitation. The test method is characterized in that a deep coal bed high temperature, high pressure and sealed environment is stimulated in a sample room (3) and a reference cylinder (4), pressure, an air source and temperature are provided by a pressurization system (2) and a constant temperature system, supercritical carbon dioxide is generated by an injection system (1), the CO2 in a normal state or a super-critical state is provided, confining pressure is provided by a confining pressure tracking and measuring system, the coal and rock expansion amount is measured, and test processes are monitored by an electrical control and monitoring system. The method comprises the following specific steps: test sample canning, air-tightness inspection, coal and rock free expansion amount measurement and test system cleaning. According to the method, the coal and rock sample free volume expansion amount in the competitive adsorption process can be accurately measured in a test room, the temperature control precision is high, the temperature fluctuation is small, and safety and reliability are achieved.
Description
Technical field
The present invention relates to a kind of test method measuring coal petrography free volume swell increment, particularly relate to a kind of test method of coal petrography sample free volume swell increment in experiment Indoor measurement competitive Adsorption process, belong to coal-bed gas exploitation field.
Background technology
China has abundant coal bed gas resource, cbm development to the nervous present situation of alleviation China hydrocarbon resources, alleviate mine disaster degree, to reduce greenhouse gas emission etc. significant.Coal and rock is a kind of porous medium containing a large amount of absorption coal-seam gas, and its mechanical property has material impact to coal-bed gas exploitation.Large quantity research proves, matrix of coal absorption N
2, CH
4, CO
2deng gas time will produce dilatational strain, gas desorption can make Coal matrix shrinkage, thus changes coal seam permeability, storage capacity, and the dilatational strain after research coal petrography adsorbed gas is most important to cbm development, particularly coal seam CO
2geological storage and CH
4enhanced recovery, N
2inject and CH
4in enhanced recovery process, supercritical CO
2, N
2can with ADSORPTION STATE CH in coal
4there is competitive Adsorption, cause ADSORPTION STATE CH
4out, meanwhile, in coal, in multicomponent gas competitive Adsorption process, the dilatational strain of matrix of coal changes, and coal seam permeability, storage capacity change further for replaced and displacement, particularly important to the validity of coal-seam gas strengthening well stimulation.And the CH of coal absorption at present
4, CO
2, N
2deng multicomponent gas competitive Adsorption in gas or coal expanding volume or pass through indirect method, measure stress changes and then be converted to dependent variable, or directly monitor the strain of certain several point in sample, and calculate overall deformation, true, comprehensive, the accurate free expansion volume of coal petrography sample and expansion coefficient cannot be obtained.
Summary of the invention
In order to solve the problem, the invention provides the test method of coal petrography sample free volume swell increment in a kind of competitive Adsorption process, the method can obtain true, comprehensive, the accurate free expansion volume of coal petrography sample and expansion coefficient.The measuring accuracy of the method is high, simple to operate, easily realizes, and data are accurate.
In order to achieve the above object, in this competitive Adsorption process, the test method of coal petrography sample free volume swell increment simulates deep fractures high temperature in sample chamber with reference in cylinder, high pressure, sealed environment, pressure and source of the gas is provided to sample chamber with reference to cylinder by compression system, temperature is provided to sample chamber with reference to cylinder by constant temperature system, generated by supercritical carbon dioxide and produce with injected system and provide supercritical carbon dioxide to sample chamber, press Tracking and Measurment system to provide ring to press for sample chamber by ring and measure the free volume swell increment of coal petrography sample in competitive Adsorption process, the supervisory control and data acquisition (SCADA) of whole process of the test is carried out by electrical control and supervisory system, display, store, concrete steps are as follows:
(a) sample tinning: pre-service is carried out to coal sample; Switch on power, connect supercritical carbon dioxide and generate and injected system and compression system; Coal sample is put into heat-shrink tube, often puts into one section of coal sample, add a moulded coal pad, during placement, the axis of moulded coal pad and the dead in line of heat-shrink tube; Heat-shrink tube is enclosed within and cushion block carries out sealing and pyrocondensation is carried out to heat-shrink tube, be finally enclosed within respectively on the heat-shrink tube outside two cushion blocks with two O type circles, seal heat-shrink tube further; Heat-shrink tube is put into clamper and is placed in constant temperature air bath;
B () airtight test: open the valve between pumped vacuum systems intermediate pump and vacuum tank on pipeline and the valve between vacuum tank and sample chamber on pipeline, utilizes pumped vacuum systems to vacuumize device; Close all valves, tracking pump is pressed to add confined pressure to 2MPa to annular space by ring, high-purity helium is injected to reference to cylinder and sample chamber, open the valve near bottom place on valve in pumped vacuum systems between vacuum tank and sample chamber on pipeline and vacuum tank, the valve near bottom place on vacuum tank is closed after device inner air is replaced away, open the valve between vacuum pump and vacuum tank on pipeline, process is vacuumized to device; Close all valves, make constant temperature air bath be heated to require temperature to reference to cylinder and sample chamber; High-purity helium is injected to reference to cylinder by gas boosting pump, make with reference to in-cylinder pressure higher than test top pressure 1MPa, valve on the main pipe rail that closedown compression system is connected with sample chamber and reference cylinder, open with reference to the valve on the pipeline of cylinder porch and the valve on the pipeline of porch, sample chamber, increase the confined pressure in the annular space outside heat-shrink tube simultaneously, ensure that the pressure in heat-shrink tube and the confined pressure in annular space are increased to the pressure after with reference to cylinder and sample chamber balance simultaneously, close with reference to the valve on the pipeline of cylinder porch and the valve on the pipeline of porch, sample chamber; Whether steady system acquisition, with reference to the pressure data in cylinder and sample chamber, observed pressure, if pressure is not steady, then repeated step (a); If steady with reference to the pressure in cylinder and sample chamber, open the valve near bottom place on valve in pumped vacuum systems between vacuum tank and sample chamber on pipeline and vacuum tank, gas in heat-shrink tube is slowly released, meanwhile, is laid down the confined pressure in annular space by ring pressure tracking pump;
C () measures the free expansion volume of coal petrography: press tracking pump to add confined pressure to 2MPa to annular space by ring, open the valve between pumped vacuum systems intermediate pump and vacuum tank on pipeline and the valve between vacuum tank and sample chamber on pipeline, pumped vacuum systems is utilized to vacuumize device, high-purity methane is injected to reference to cylinder and sample chamber, vacuumize again, repeat 3-5 time;
Close all valves, arrange and regulating system temperature, make the temperature stabilization of reference cylinder and sample chamber in test temperature, the original pressure of record reference cylinder and reaction chamber;
Methane or carbon dioxide or mixed gas is injected to reference to cylinder with regime flow, its pressure is made to reach test design pressure, valve on the main pipe rail that closedown compression system is connected with sample chamber and reference cylinder, open with reference to the valve on the pipeline of cylinder porch and the valve on the pipeline of porch, sample chamber, receive pyrocondensation overpressure by pressure transducer I simultaneously, the confined pressure of following the tracks of in pump control increase annular space is pressed by ring, make the confined pressure in annular space and pyrocondensation overpressure moment keep identical, and rise to test design pressure simultaneously;
Confined pressure in annular space stops pressurization after rising to test design pressure, the opening pressure of following the tracks of pump control check valve is pressed to be test design pressure by ring, with the liquid that beaker access is flowed out from annular space, utilize the liquid weight at normal temperatures and pressures in high Accuracy Electronic Balance weighing beaker;
Once pressure drop in heat-shrink tube, then continue to inject methane or carbon dioxide or mixed gas, pyrocondensation overpressure is made to remain on test design pressure, until in heat-shrink tube pressure stability at test design pressure, test stops, according to discharged liquid weight, the free expansion volume of conversion coal and free expansion coefficient;
D () pilot system is cleared up: after off-test, opens the valve near bottom place on valve in pumped vacuum systems between vacuum tank and sample chamber on pipeline and vacuum tank, is slowly released by the gas in heat-shrink tube; Meanwhile, the confined pressure in annular space is laid down by ring pressure tracking pump; Releasing gas circuit connects, and cools; Take out the heat-shrink tube on clamper, take out seal, take out coal sample and moulded coal pad;
Further, described test pressure is 0.1MPa ~ 25MPa, and test temperature is room temperature ~ 150 DEG C;
Further, sample chamber and with reference in cylinder pressure maintaining period, when pipeline and Sealing ring for container No leakage, range of pressure fluctuations is at below 0.05MPa, and temperature fluctuation is within 0.5 DEG C;
Further, when pyrocondensation is carried out to heat-shrink tube, first that the pyrocondensation of heat-shrink tube two incline is extremely level and smooth, then adopt the path of the spiral escalation that passes through to carry out overall pyrocondensation to heat-shrink tube.
The present invention is generated by supercritical carbon dioxide and can be injected into reference in cylinder and sample chamber by carbon dioxide with injected system, can also supercritical carbon dioxide be generated when needs and be injected into reference in cylinder and sample chamber, compression system pressurization and constant temperature system heating keep constant temperature that the pressure and temperature in sample chamber can be made can to reach the pressure and temperature of deep fractures, by referring to cylinder can calibration sample room volume to obtain measurement data accurately, pumped vacuum systems can air before on-test in emptying whole device, make the state reaching vacuum in test unit as far as possible, the reliability of warranty test data, the free volume swell increment of coal petrography in the process of adsorbed gas can be measured accurately by ring pressure Tracking and Measurment system, electrical control and supervisory system can make the remote service test device of testing crew and Control experiment flow process, video monitoring is carried out to the outer state of pressure vessel, and can take, record process of the test, can safeguards system safety.This test method temperature-controlled precision is high, and heat balance time is short, and temperature fluctuation is little, and homogeneity is good, and data display is accurate, directly perceived, compact conformation.The present invention is convenient to control, simple to operate, safe and reliable, can obtain coal petrography sample true, comprehensively, accurate free expansion volume and expansion coefficient.
Accompanying drawing explanation
Fig. 1 is the structural representation of device used in the present invention.
In figure: 1, supercritical carbon dioxide generates and injected system, 1-1, high-pressure carbon dioxide cylinder, 1-2, refrigeration system, 1-3, carbon dioxide pump, 1-4, injection pump, 1-5, piston container, 1-6, heating system, 1-7, pressure transducer VI, 1-8a ~ 1-8h, valve; 2, compression system, 2-1a, helium gas cylinder, 2-1b, methane gas cylinder, 2-1c, mixed gas gas cylinder, 2-2, air compressor machine, 2-3, gas boosting pump, 2-4, solenoid valve, 2-5a, pressure regulator valve I, 2-5b, pressure regulator valve II, 2-5c, pressure regulator valve III, 2-6a, gas meter I, 2-6b, gas meter II, 2-6c, gas meter III, 2-7a, retaining valve I, 2-7b, retaining valve II, 2-7c, retaining valve III, 2-8a ~ 2-8i, valve; 3, sample chamber, 3-1, heat-shrink tube, 3-2a, 3-2b, cushion block and O type circle, 3-3, moulded coal pad, 3-4, pressure transducer I, 3-5, clamper, 3-6, annular space; 4, with reference to cylinder, 4-1, pressure transducer II; 5, constant temperature air bath; 6, pumped vacuum systems, 6-1, vacuum pump, 6-2, vacuum tank, 6-3, vacuum meter, 6-4a ~ 6-4c, valve; 7, gaseous sample acquisition system, 7-1, gas chromatograph, 7-2, gas-liquid separation container, 7-3, pressure regulator valve IV, 7-4a ~ 7-4c, valve, 7-5, gas meter IV; 8, ring pressure Tracking and Measurment system, 8-1, ring pressure follows the tracks of pump, 8-2, back pressure buffer container, 8-3, check valve, 8-4, high Accuracy Electronic Balance, 8-5, beaker, 8-6a, pressure transducer III, 8-6b, pressure transducer IV, 8-6c, pressure transducer V, 8-7a, two-way valve I, 8-7b, two-way valve II, 8-8a, 8-8b, valve.
Embodiment
Below in conjunction with accompanying drawing, the invention will be further described.
Be illustrated in figure 1 the structural representation of test unit used in the present invention, test unit comprises:
Sample chamber 3, the reaction chamber of this device, for loading sample and simulated formation high temperature, high pressure, sealed environment, heat radially can go up free deformation, does not hinder coal petrography deformation;
With reference to cylinder 4, for calibration sample room volume, accurately to be detected data;
Supercritical carbon dioxide generates and injected system 1, for generating supercritical carbon dioxide, and is injected into by supercritical carbon dioxide in sample chamber 3 and reference cylinder 4;
Compression system 2, for sample chamber 3 with reference to injection test gas in cylinder 4, and adjustable sample chamber 3 and with reference to the pressure in cylinder 4;
Constant temperature system, for providing hot environment and keep constant temperature in process of the test for sample chamber 3 with reference to cylinder 4, its temperature adjustable;
Pumped vacuum systems 6, is connected with sample chamber 3, for emptying sample chamber 3 with reference to the gas in cylinder 4;
Gaseous sample acquisition system 7, is connected with sample chamber 3, can be used for collect test in test after gas, carry out the operations such as condensation, step-down, gas-liquid separation, gas composition measurement;
Ring pressure Tracking and Measurment system 8, for measuring coal petrography sample free volume swell increment in competitive Adsorption process;
Electrical control and supervisory system, for monitoring process of the test, Real-time Collection, display and storage data.
Described sample chamber 3 comprises heat-shrink tube 3-1, cushion block 3-2a, O type circle 3-2b, moulded coal pad 3-3, pressure transducer I3-4 and clamper 3-5, sample chamber 3 is fixed in constant temperature system by clamper 3-5, heat-shrink tube 3-1 two ends adopt cushion block 3-2a and O type circle 3-2b to seal, moulded coal pad 3-3 has the hole of certain order number, be positioned over two sections of coal samples of space between adjacent in heat-shrink tube 3-1, during placement, the axis of moulded coal pad 3-3 and the dead in line of heat-shrink tube 3-1, pressure transducer I3-4 is connected with heat-shrink tube 3-1, is provided with annular space 3-6 outside heat-shrink tube 3-1; Maximum working pressure (MOP) in sample chamber 3 can reach 25MPa, and maximum operating temperature can reach 150 DEG C, makes sample chamber 3 in process of the test can meet the needs of the pressure and temperature of simulating different deep fractures; Heat-shrink tube 3-1 is used for putting coal petrography sample, can free deformation be there is in radial direction and not hinder coal petrography deformation in heat, the internal diameter of the heat-shrink tube 3-1 that this test uses is 50mm, length is 1000 ± 10mm, axial is 20:1 with the length ratio of radial direction, during test, the axial deformation of coal petrography can be ignored, only measure the whole distortion of radial deformation as coal petrography; The moulded coal pad 3-3 placed between adjacent two sections of coal samples can make gas be full of whole heat-shrink tube 3-1 space fast, cushion block 3-2a and O type circle 3-2b is used for sealing heat-shrink tube 3-1, pressure transducer I3-4 is for measuring pressure in heat-shrink tube 3-1 for analysis of experimental data, and can inject silicone oil in the annular space 3-6 outside heat-shrink tube 3-1 increases confined pressure to heat-shrink tube 3-1;
Described is connected with pressure transducer II4-1 with reference on cylinder 4, is communicated with between sample chamber 3; With reference to cylinder 4 for calibration sample room volume, accurately to be detected data; Adopt high pressure resistant stainless cylinder of steel as with reference to cylinder 4, to ensure still have good sealing at the large temperature range of testing requirements, superelevation pressure conditions lower cylinder body; Sample chamber 3 and with reference in cylinder 4 pressure maintaining period, when pipeline and Sealing ring for container No leakage, range of pressure fluctuations is at below 0.05MPa, and temperature fluctuation, within 0.5 DEG C, makes the pressure and temperature ambient stable of sample chamber 3, the precision of warranty test;
Described constant temperature system is constant temperature air bath 5, and constant temperature air bath 5 wraps up whole sample chamber 3 and reference cylinder 4; In process of the test, constant temperature air bath 5 keeps constant temperature by sample chamber 3 with after being heated to design temperature with reference to cylinder 4, after off-test, relies on cross-ventilation to realize cooling;
Described supercritical carbon dioxide generates and comprises high-pressure carbon dioxide cylinder 1-1 with injected system 1, refrigeration system 1-2, carbon dioxide pump 1-3, injection pump 1-4, piston container 1-5, valve 1-8a ~ the 1-8c of heating system 1-6 and the turnover of multiple control gas, 1-8e, 1-8f, 1-8h, high-pressure carbon dioxide cylinder 1-1 is connected with the air intake opening of refrigeration system 1-2, the gas outlet of refrigeration system 1-2 is connected with the air intake opening of carbon dioxide pump 1-3, one end of piston container 1-5 and the gas outlet of carbon dioxide pump 1-3, the air intake opening of sample chamber 3 is connected with the air intake opening with reference to cylinder 4, the other end is connected with injection pump 1-4, heating system 1-6 is wrapped in outside piston container 1-5, high-pressure carbon dioxide cylinder 1-1 provide gaseous carbon dioxide to device, control gas by valve 1-8a to supply, through the cooled liquid carbon dioxide of refrigeration system 1-2 by carbon dioxide pump 1-3 infusion in the piston container 1-5 be attached thereto, control liquid carbon dioxide by valve 1-8b and valve 1-8e to supply, heating system 1-6 adds thermosetting supercritical carbon dioxide to the liquid carbon dioxide in piston container 1-5, valve 1-8c controls the connection of injection pump 1-4 and piston container 1-5, injection pump 1-4 provides power for piston container 1-5, supercritical carbon dioxide is injected in sample chamber 3 and reference cylinder 4, valve 1-8f on filling line and valve 1-8h controls carbon dioxide supply,
Described compression system 2 comprises valve 2-8a ~ 2-8i that helium gas cylinder 2-1a, methane gas cylinder 2-1b, mixed gas gas cylinder 2-1c, air compressor machine 2-2, gas boosting pump 2-3, solenoid valve 2-4 and multiple control gas pass in and out, helium gas cylinder 2-1a, methane gas cylinder 2-1b are connected with gas boosting pump 2-3 with mixed gas gas cylinder 2-1c, be provided with solenoid valve 2-4 between gas boosting pump 2-3 and air compressor machine 2-2, gas boosting pump 2-3 gas outlet is connected with sample chamber 3 with reference to cylinder 4 by pipeline, helium gas cylinder 2-1a, methane gas cylinder 2-1b and mixed gas gas cylinder 2-1c provides helium respectively to device, methane and mixed gas, control gas by the valve 2-8a ~ 2-8c being located at gas cylinder exit to supply, pipeline between valve 2-8a ~ 2-8c and gas supercharge pump 2-3 there is valve 2-8e, control gas supplies, ensure security of system, gas boosting pump 2-3 is gas boosting, and provide gases at high pressure to sample chamber 3 with reference to cylinder 4, solenoid valve 2-4 controls air compressor machine 2-2 and provides power to gas boosting pump 2-3, by the 2-8f in pipeline, 2-8g, 2-8h, 2-8i controls gas boosting pump 2-3 to sample chamber 3 and the air feed with reference to cylinder 4, wherein, valve 2-8f is located on the pipeline in gas boosting pump 2-3 exit, valve 2-8h is located on the pipeline with reference to cylinder 4 porch, valve 2-8i is located on the valve of porch, sample chamber 3, valve 2-8g is located at compression system 2 and sample chamber 3 and on the main pipe rail that is connected with reference to cylinder 4, if valve-off 2-8g, then helium gas cylinder 2-1a, gas in methane gas cylinder 2-1b and mixed gas gas cylinder 2-1c all can not be injected in sample chamber 3 and reference cylinder 4, valve 2-8d is located at helium gas cylinder 2-1a, methane gas cylinder 2-1b, on the main pipe rail that mixed gas gas cylinder 2-1c is connected with sample chamber 3 and reference cylinder 4, if valve-off 2-8d, then without the helium gas cylinder 2-1a that gas boosting pump 2-3 boosts, gas in methane gas cylinder 2-1b and mixed gas gas cylinder 2-1c all can not be injected in sample chamber 3 and reference cylinder 4,
Described pumped vacuum systems 6 comprises vacuum pump 6-1, vacuum pump 6-1 is connected with sample chamber 3 and its connecting line is provided with the valve 6-4c that pilot piping closes and opens, vacuum pump 6-1 is used for the air in emptying whole test unit, make the state reaching vacuum in test unit as far as possible, the reliability of warranty test data;
Described gaseous sample acquisition system 7 comprises gas chromatograph 7-1, gas-liquid separation container 7-2 and pressure regulator valve IV7-3, gas chromatograph 7-1 is connected with gas-liquid separation container 7-2 and connecting line is provided with valve 7-4c, pressure regulator valve IV7-3 one end is connected with sample chamber 3, the other end is connected with gas-liquid separation container 7-2 and connecting line is provided with valve 7-4a, and gas-liquid separation container 7-2 is also provided with valve 7-4b; Reduce after pressure from sample chamber 3 effluent air sample through pressure regulator valve IV7-3, enter after the valve 7-4a that pilot piping closes and opens in gas-liquid separation container 7-2 and carry out gas-liquid separation, liquid after gas-liquid separation stays gas-liquid separation container 7-2, gas both can be flowed out by the valve 7-4b on gas-liquid separation container 7-2 top, flow in gas chromatograph 7-1 and carry out gas componant detection after the valve 7-4c that also can close through pilot piping and open;
Described ring pressure Tracking and Measurment system 8 comprises ring pressure and follows the tracks of pump 8-1, back pressure buffer container 8-2, check valve 8-3, high Accuracy Electronic Balance 8-4, beaker 8-5 and pressure transducer III8-6a, ring pressure is followed the tracks of pump 8-1 and to be connected with the annular space 3-6 of sample chamber 3 by pipeline and connecting line is provided with pressure transducer III8-6a, pipeline between ring pressure tracking pump 8-1 and pressure transducer III8-6a is provided with two-way valve I8-7a, back pressure buffer container 8-2 and ring are pressed and are followed the tracks of pump 8-1 and to be connected and connecting line is provided with two-way valve II8-7b, check valve 8-3 one end is connected with annular space 3-6 and connecting line is provided with valve 8-8b, the other end is connected with back pressure buffer container 8-2 and connecting line is provided with branch road, high Accuracy Electronic Balance 8-4 and beaker 8-5 is positioned over branch circuit outlet, valve 8-8a is located at the exit with annular space 3-6 connecting line, ring pressure is followed the tracks of pump 8-1 and is closed for injecting silicone oil and control check valve 8-3 in annular space 3-6 and open, pressure in pressure transducer III8-6a feedback ring space 3-6, closed and the unlatching following the tracks of pipeline between pump 8-1 and annular space 3-6 is pressed by two-way valve I8-7a control loop, back pressure buffer container 8-2 can guarantee that the fluid in annular space 3-6 steadily flows out, closed and the unlatching following the tracks of pipeline between pump 8-1 is pressed by two-way valve II8-7b control back pressure buffer container 8-2 and ring, during back pressure, the liquid flowed out through check valve 8-3 flows into beaker 8-5 by the road, the quality under its normal temperature and pressure can be measured by high Accuracy Electronic Balance 8-4 so can converse coal sample absorption free expansion amount, when needing, silicone oil in annular space 3-6 directly flows out by valve 8-8a, realize annular space 3-6 release, to guarantee security of system, this ring pressure Tracking and Measurment system 8 can realize pressure in annular space 3-6 and sample gas pressure inside and synchronously rise, with prevent heat-shrink tube 3-1 due to inside and outside differential pressure excessive and break,
Described electrical control and supervisory system, be made up of industrial computer, display and transmission device table, high-speed camera, relay protection and warning circuit and the electrical equipment such as electric control circuit, power distribution circuit and control software design, major function is: to the distribution of electrical equipment, the functions such as the safeguard protection of system and warning; The pressure, temperature etc. of whole experiment simulator are gathered, process and shown; Video monitoring is carried out, with safeguards system safety to the outer state of pressure vessel.
Described piston container 1-5 upper and lower is respectively equipped with valve 1-8d, 1-8g, is used for respectively to piston container 1-5 and injection pump 1-4 release to guarantee security of system.
Described supercritical carbon dioxide generates and also comprises pressure transducer VI1-7 with injected system 1, and pressure transducer VI1-7 is located between valve 1-8f and valve 1-8h, is used for feeding back to sample chamber 3 and the pressure injecting the pipeline of supercritical carbon dioxide with reference to cylinder 4.
Described compression system 2 also comprises gas meter I2-6a, gas meter II2-6b and gas meter III2-6c, gas meter I2-6a, gas meter II2-6b and gas meter III2-6c is located at helium gas cylinder 2-1a respectively, methane gas cylinder 2-1b, on the pipeline that mixed gas gas cylinder 2-1c is connected with gas boosting pump 2-3, at gas meter I2-6a, connecting line between gas meter II2-6b and gas meter III2-6c and gas boosting pump 2-3 is respectively equipped with retaining valve I2-7a, retaining valve II2-7b and retaining valve III2-7c, at helium gas cylinder 2-1a, methane gas cylinder 2-1b, mixed gas gas cylinder 2-1c and gas meter I2-6a, gas meter II2-6b, connecting line between gas meter III2-6c is respectively equipped with pressure regulator valve I2-5a, pressure regulator valve II2-5b, pressure regulator valve III2-5c, gas meter I2-6a, gas meter II2-6b and gas meter III2-6c monitors helium respectively, the flow of methane and mixed gas, because the gas flow controller used in device is all high-precision, so range is shorter and sensitiveer, pressure regulator valve I2-5a, pressure regulator valve II2-5b and pressure regulator valve III2-5c, for reducing the pressure of effluent air in gas cylinder, prevents due to gas coming through flowmeter I2-6a, the gaseous tension of gas meter II2-6b and gas meter III2-6c is excessive and make gas meter I2-6a, gas meter II2-6b and gas meter III2-6c damages, retaining valve retaining valve I2-7a, retaining valve II2-7b and retaining valve III2-7c, for controlling gas unidirectional flowing, prevents gas backstreaming and affects gas meter I2-6a, gas meter II2-6b and gas meter III2-6c records the degree of accuracy of data.
Described pumped vacuum systems 6 also comprises the vacuum tank 6-2 be connected with vacuum pump 6-1 and sample chamber 3, and the connecting line between vacuum tank 6-2 and vacuum pump 6-1 is provided with valve 6-4a, and vacuum tank 6-2 is provided with valve 6-4b near bottom place; When vacuumizing, the water be mixed with in the gas extracted out from whole device is deposited in vacuum tank 6-2, when opening valve 6-4b rear-inclined vacuum tank 6-2, condensate water remaining in vacuum tank 6-2 can be made to flow out, valve 6-4a is used for the closed of control linkage pipeline and opens.
Described pumped vacuum systems 6 also comprises the vacuum meter 6-3 be located between vacuum tank 6-2 and valve 6-4a on connecting line, for measure and whether pressure in display device reaches vacuum with judgment means, convenient test.
Described gaseous sample acquisition system 7 also comprises the gas meter IV7-5 be located between pressure regulator valve IV7-3 and gas-liquid separation container 7-2 on connecting line, be used for monitoring the flow of gas, if broken down with reference to cylinder 4, the amount of coal petrography adsorbed gas can be analyzed by the data of gas meter record.
Described ring pressure Tracking and Measurment system 8 also comprises pressure transducer IV8-6b and pressure transducer V8-6c, pressure transducer IV8-6b is located on the connecting line of check valve 8-3 and annular space 3-6, and pressure transducer V8-6c is located on the connecting line of check valve 8-3 and back pressure buffer container 8-2; Two pressure transducers are used for feeding back to the pressure in pressure valve 8-3 two lateral line respectively, can regulate test process according to pressure, ensure the safety of system.
This device also comprises demolition set, and demolition set is connected with sample chamber 3, during superpressure, can releasing pressure automatically, and ensure safety.
When there is power failure and burst accident, also can, manually to device pressure release, avoid having an accident.
Pipeline in whole device adopts 316L pipeline.
The present invention, for guaranteeing safety, is divided into control zone, test site, and control zone and test site isolate, and guarantee that human users is in safety zone.Whole operation control system is in an independent room, sample chamber, reference cylinder and air compressor machine etc. are observed in pulpit by camera, the present invention adopts the running program of pressurizeing afterwards that first heats up, in the force value that control system setting needs, when force value reaches desired value, compression system stops automatically, boost process is controlled, guarantees experimental safe.
The test method of coal petrography sample free volume swell increment in competitive Adsorption process of the present invention, step is as follows:
(a) sample tinning: equilibrium moisture or other pre-service are carried out to coal sample; Switch on power, connect supercritical carbon dioxide to generate and helium gas cylinder 2-1a, the methane gas cylinder 2-1b in injected system 1 and compression system 2, mixed gas gas cylinder 2-1c, high-pressure carbon dioxide cylinder 1-1, air compressor machine 2-2 and gas supercharge pump 2-3, refrigeration system 1-2, carbon dioxide pump 1-3, injection pump 1-4, piston container 1-5, heating system 1-6; Coal sample is put into heat-shrink tube 3-1, often put into one section of coal sample, add a moulded coal pad 3-3; Heat-shrink tube 3-1 is enclosed within cushion block 3-2a and seals, pass through the pyrocondensation of heat-shrink tube 3-1 two incline to level and smooth, then overall pyrocondensation, pyrocondensation path is the spiral escalation that passes through, make heat-shrink tube 3-1 pyrocondensation even, thus heat-shrink tube 3-1 and coal sample are fitted completely, be finally enclosed within the heat-shrink tube outside two cushion block 3-2a respectively with two O type circle 3-2b, further sealing heat-shrink tube 3-1; Heat-shrink tube 3-1 is put into clamper 3-5 and is placed in constant temperature air bath 5;
B () airtight test: open the valve 6-4a between pumped vacuum systems 6 intermediate pump 6-1 and vacuum tank 6-2 on pipeline and the valve 6-4c between vacuum tank 6-2 and sample chamber 3 on pipeline, utilizes pumped vacuum systems 6 pairs of devices to vacuumize, close all valves, running control software, press tracking pump 8-1 to inject silicone oil to annular space 3-6 by ring and add confined pressure to about 2MPa, high-purity helium that purity is 99.99% is injected to reference to cylinder 4 and sample chamber 3, open the valve 6-4b near bottom place on valve 6-4c in pumped vacuum systems 6 between vacuum tank 6-2 and sample chamber 3 on pipeline and vacuum tank 6-2, device inner air is replaced away, then the valve 6-4b near bottom place on vacuum tank 6-2 is closed, open the valve 6-4a between vacuum pump 6-1 and vacuum tank 6-2 on pipeline, process is vacuumized to device, close all valves, running control software, make constant temperature air bath 5 be heated to require temperature to reference to cylinder 4 and sample chamber 3, high-purity helium is injected to reference to cylinder 4 by gas boosting pump 2-3, make with reference to pressure in cylinder 4 higher than test top pressure 1MPa, valve 2-8g on the main pipe rail that closedown compression system 2 is connected with sample chamber 3 and reference cylinder 4, open with reference to the valve 2-8h on the pipeline of cylinder 4 porch and the valve 2-8i on the pipeline of porch, sample chamber 3, make with reference to cylinder 4 and sample chamber 3 pressure equilibrium, in the annular space 3-6 outside heat-shrink tube 3-1, inject silicone oil simultaneously increase confined pressure, ensure that the pressure in heat-shrink tube 3-1 and the confined pressure in annular space 3-6 are increased to the pressure after balancing with reference to cylinder 4 and sample chamber 3 simultaneously, close with reference to the valve 2-8h on the pipeline of cylinder 4 porch and the valve 2-8i on the pipeline of porch, sample chamber 3, system acquisition is with reference to the pressure data in cylinder 4 and sample chamber 3, and it is good that pressure is steadily then considered as system impermeability, if any gas leak phenomenon, repeat step (a), if steady with reference to the pressure in cylinder 4 and sample chamber 3, open the valve 6-4b near bottom place on valve 6-4c in pumped vacuum systems 6 between vacuum tank 6-2 and sample chamber 3 on pipeline and vacuum tank 6-2, gas in heat-shrink tube 3-1 is slowly released, meanwhile, the confined pressure in annular space 3-6 is laid down by ring pressure tracking pump 8-1,
C () measures the free expansion volume of coal petrography: pressed by ring and follow the tracks of pump 8-1 to annular space 3-6 injection silicone oil increase confined pressure to about 2MPa, open the valve 6-4a between pumped vacuum systems 6 intermediate pump 6-1 and vacuum tank 6-2 on pipeline and the valve 6-4c between vacuum tank 6-2 and sample chamber 3 on pipeline, device is vacuumized, running control software, perform manual operation program, the high-purity methane that a small amount of purity is 99.99% is injected to reference to cylinder 4 and sample chamber 3, detergent line, vacuumize again, repeat 3-5 time, guarantee that in pipeline, helium cleans up;
Close all valves, running control software, arrange and regulating system temperature, make the temperature stabilization of reference cylinder 4 and sample chamber 3 in test temperature, the original pressure of record reference cylinder 4 and reaction chamber 3;
Methane or carbon dioxide or mixed gas is injected to reference to cylinder 4 with regime flow, its pressure is made to reach test design pressure, valve 2-8g on the main pipe rail that closedown compression system 2 is connected with sample chamber 3 and reference cylinder 4, open with reference to the valve 2-8h on the pipeline of cylinder 4 porch and the valve 2-8i on the pipeline of porch, sample chamber 3, utilize the gap between heat-shrink tube and coal sample, make with reference to cylinder 4 and sample chamber 3 rapid pressure equalisation, receive pressure in heat-shrink tube 3-1 by pressure transducer I3-4 simultaneously, and be transferred to ring pressure tracking pump 8-1, pressed by ring and follow the tracks of pump 8-1 control to annular space 3-6 injection silicone oil increase confined pressure, the confined pressure in annular space 3-6 is made to keep identical with the pressure moment in heat-shrink tube 3-1, and rapidly increase to test design pressure simultaneously,
Confined pressure in annular space 3-6 stops pressurization after rising to test design pressure, namely the opening pressure of following the tracks of pump 8-1 control check valve 8-3 is pressed to be test design pressure by ring, now, dilatational strain after coal sample adsorbed methane or carbon dioxide or mixed gas, heat-shrink tube 3-1 will be promoted and extrude annular space 3-6, confined pressure is caused to increase, because in confined pressure and heat-shrink tube 3-1, pressure pressure reduction is 0, by the pressure that check valve 8-3 sets, the pressure exceeding part will discharge, discharging by the liquid in annular space 3-6 flows in beaker 8-5, utilize the liquid weight at normal temperatures and pressures in high Accuracy Electronic Balance 8-4 weighing beaker 8-5,
Once pressure drop in heat-shrink tube 3-1, then continue to inject methane or carbon dioxide or mixed gas, pressure in heat-shrink tube 3-1 is made to remain on test design pressure, until in heat-shrink tube 3-1 pressure stability at test design pressure (in 30min pressure change be less than 0.05MPa), test stops, according to discharged liquid weight, the free expansion volume of conversion coal and free expansion coefficient;
D () pilot system is cleared up: after off-test, opens the valve 6-4b at the upper close bottom place of valve 6-4c in pumped vacuum systems 6 between vacuum tank 6-2 and sample chamber 3 on pipeline and vacuum tank 6-2, is slowly released by the gas in heat-shrink tube 3-1; Meanwhile, follow the tracks of pump 8-1 by ring pressure the confined pressure in annular space 3-6 is laid down; Releasing gas circuit connects, and cools; Take out the heat-shrink tube 3-1 on clamper 3-5, take out cushion block 3-2a and O type circle 3-2b, take out sample and moulded coal pad 3-3.
The test pressure of this test method is 0.1MPa ~ 25MPa, and test temperature is room temperature ~ 150 DEG C, can simulate the pressure and temperature in different depth coal seam.
Claims (4)
1. the test method of coal petrography sample free volume swell increment in a competitive Adsorption process, it is characterized in that: in sample chamber (3) with reference to cylinder (4) middle simulation deep fractures high temperature, high pressure, sealed environment, pressure and source of the gas is provided to sample chamber (3) with reference to cylinder (4) by compression system (2), temperature is provided to sample chamber (3) with reference to cylinder (4) by constant temperature system, generated by supercritical carbon dioxide and produce with injected system (1) and provide supercritical carbon dioxide to sample chamber (3), Tracking and Measurment system (8) is pressed to provide ring pressure for sample chamber (3) by ring, the supervisory control and data acquisition (SCADA) of whole process of the test is carried out by electrical control and supervisory system, display, store, concrete steps are as follows:
(a) sample tinning: pre-service is carried out to coal sample; Switch on power, connect supercritical carbon dioxide and generate and injected system (1) and compression system (2); Coal sample is put into heat-shrink tube (3-1), often put into one section of coal sample, add a moulded coal pad (3-3), during placement, the axis of moulded coal pad (3-3) and the dead in line of heat-shrink tube (3-1); Heat-shrink tube (3-1) is enclosed within and cushion block (3-2a) carries out sealing and pyrocondensation is carried out to heat-shrink tube (3-1), finally use two O type circles (3-2b) to be enclosed within respectively on two cushion blocks (3-2a) heat-shrink tube outward, seal heat-shrink tube (3-1) further; Heat-shrink tube (3-1) is put into clamper (3-5) and is placed in constant temperature air bath (5);
B () airtight test: open the valve (6-4a) between pumped vacuum systems (6) intermediate pump (6-1) and vacuum tank (6-2) on pipeline and the valve (6-4c) between vacuum tank (6-2) and sample chamber (3) on pipeline, utilizes pumped vacuum systems (6) to vacuumize device, close all valves, tracking pump (8-1) is pressed to add confined pressure to 2MPa to annular space (3-6) by ring, high-purity helium is injected to reference to cylinder (4) and sample chamber (3), open the valve (6-4c) in pumped vacuum systems (6) between vacuum tank (6-2) and sample chamber (3) on pipeline and the upper valve (6-4b) near bottom place of vacuum tank (6-2), the upper valve (6-4b) near bottom place of vacuum tank (6-2) is closed after device inner air is replaced away, open the valve (6-4a) between vacuum pump (6-1) and vacuum tank (6-2) on pipeline, process is vacuumized to device, close all valves, make constant temperature air bath (5) be heated to require temperature to reference to cylinder (4) and sample chamber (3), high-purity helium is injected to reference to cylinder (4) by gas boosting pump (2-3), make with reference to cylinder (4) interior pressure higher than test top pressure 1MPa, valve (2-8g) on the main pipe rail that closedown compression system (2) is connected with sample chamber (3) and reference cylinder (4), open with reference to the valve (2-8h) on the pipeline of cylinder (4) porch and the valve (2-8i) on the pipeline of sample chamber (3) porch, increase the confined pressure in heat-shrink tube (3-1) annular space outward (3-6) simultaneously, ensure that the pressure in heat-shrink tube (3-1) and the confined pressure in annular space (3-6) are increased to the pressure after with reference to cylinder (4) and sample chamber (3) balance simultaneously, close with reference to the valve (2-8h) on the pipeline of cylinder (4) porch and the valve (2-8i) on the pipeline of sample chamber (3) porch, whether steady system acquisition, with reference to the pressure data in cylinder (4) and sample chamber (3), observed pressure, if pressure is not steady, then repeated step (a), if steady with reference to the pressure in cylinder (4) and sample chamber (3), open the valve (6-4c) in pumped vacuum systems (6) between vacuum tank (6-2) and sample chamber (3) on pipeline and the upper valve (6-4b) near bottom place of vacuum tank (6-2), gas in heat-shrink tube (3-1) is slowly released, meanwhile, the confined pressure in annular space (3-6) is laid down by ring pressure tracking pump (8-1),
C () measures the free expansion volume of coal petrography: press tracking pump (8-1) to add confined pressure to 2MPa to annular space (3-6) by ring, open the valve (6-4a) between pumped vacuum systems (6) intermediate pump (6-1) and vacuum tank (6-2) on pipeline and the valve (6-4c) between vacuum tank (6-2) and sample chamber (3) on pipeline, pumped vacuum systems (6) is utilized to vacuumize device, high-purity methane is injected to reference to cylinder (4) and sample chamber (3), vacuumize again, repeat 3-5 time;
Close all valves, arrange and regulating system temperature, make the temperature stabilization of reference cylinder (4) and sample chamber (3) in test temperature, the original pressure of record reference cylinder (4) and reaction chamber (3);
Methane or carbon dioxide or mixed gas is injected to reference to cylinder (4) with regime flow, its pressure is made to reach test design pressure, valve (2-8g) on the main pipe rail that closedown compression system (2) is connected with sample chamber (3) and reference cylinder (4), open with reference to the valve (2-8h) on the pipeline of cylinder (4) porch and the valve (2-8i) on the pipeline of sample chamber (3) porch, receive heat-shrink tube (3-1) interior pressure by pressure transducer I (3-4) simultaneously, the confined pressure of following the tracks of in pump (8-1) control increase annular space (3-6) is pressed by ring, the confined pressure in annular space (3-6) is made to keep identical with heat-shrink tube (3-1) the interior pressure moment, and rise to test design pressure simultaneously,
Confined pressure in annular space (3-6) stops pressurization after rising to test design pressure, the opening pressure of pressing tracking pump (8-1) to control check valve (8-3) by ring is test design pressure, with the liquid that beaker (8-5) access is flowed out from annular space (3-6), high Accuracy Electronic Balance (8-4) is utilized to weigh liquid weight at normal temperatures and pressures in beaker (8-5);
Once heat-shrink tube (3-1) interior pressure drop, then continue to inject methane or carbon dioxide or mixed gas, heat-shrink tube (3-1) interior pressure is made to remain on test design pressure, until heat-shrink tube (3-1) interior pressure stability is at test design pressure, test stops, according to discharged liquid weight, the free expansion volume of conversion coal and free expansion coefficient;
D () pilot system is cleared up: after off-test, open the valve (6-4c) in pumped vacuum systems (6) between vacuum tank (6-2) and sample chamber (3) on pipeline and the upper valve (6-4b) near bottom place of vacuum tank (6-2), the gas in heat-shrink tube (3-1) is slowly released; Meanwhile, the confined pressure in annular space (3-6) is laid down by ring pressure tracking pump (8-1); Releasing gas circuit connects, and cools; Take out the heat-shrink tube (3-1) on clamper (3-5), take out seal, take out coal sample and moulded coal pad (3-3).
2. the test method of coal petrography sample free volume swell increment in a kind of competitive Adsorption process according to claim 1, it is characterized in that: described test pressure is 0.1MPa ~ 25MPa, test temperature is room temperature ~ 150 DEG C.
3. the test method of coal petrography sample free volume swell increment in a kind of competitive Adsorption process according to claim 2, it is characterized in that: in sample chamber (3) and reference cylinder (4) pressure maintaining period, when pipeline and Sealing ring for container No leakage, range of pressure fluctuations is at below 0.05MPa, and temperature fluctuation is within 0.5 DEG C.
4. the test method of coal petrography sample free volume swell increment in a kind of competitive Adsorption process according to claim 1, it is characterized in that: when pyrocondensation is carried out to heat-shrink tube (3-1), first that heat-shrink tube (3-1) two incline pyrocondensation is extremely level and smooth, then adopt the path of the spiral escalation that passes through to carry out overall pyrocondensation to heat-shrink tube (3-1).
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