CN103344537A - Test method for high-temperature high-pressure pyrolysis reaction - Google Patents
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Abstract
A test method for a high-temperature high-pressure pyrolysis reaction belongs to the category of the pyrolysis reaction technology field. The test method is characterized in that an adopted device is a device which can seal a test specimen under high temperature and high pressure conditions, wherein the specimen dimension is phi 25*50 mm or phi 50*100 mm, the axial pressure and the confining pressure of the specimen are both up to 20 MPa, and the environment temperature of the specimen is up to 600 DEG C; and can simulate geological environment conditions in a mineral burial depth of 800 m. The test device adopted by the test method consists of four systems: a pyrolysis reaction system, a gas pressure injection system, a fluid product discharging system and a test control system. The new developed test device for the high-temperature high-pressure pyrolysis reaction is utilized, stress conditions are fully considered, the geological environmental conditions of deep mineral burial depth are simulated, so the shortcomings and the defects that the specimen is in an unconstrained state and is not loaded in a conventional test device are overcome, and feasibility test researches on oil shale and low metamorphic coal in hundreds of meters deep underground can be carried out.
Description
Technical field:
The test method of a kind of High Temperature High Pressure pyrolytic reaction of the present invention belongs to pyrolytic reaction technical field category.Be mainly used in resinous shale and low-disintegration coal etc. is carried out pyrolytic reaction experimental study under high-temperature and high-pressure conditions, and by the test specimen after the pyrolysis being carried out the component content analysis of dynamic characteristic test, permeability test, product, for original position heat injection exploitation provides theoretical foundation.
Background technology:
Original position heat injection exploitation belongs to the category of original position solution mining, it is to arrange well pattern by covering the face of land at exploitation target ore bed, pyrolyzation fluid is injected the target ore bed, coupling principles such as the physics that takes place between utilization injection fluid and the ore bed useful constituent, chemistry, heat, power, to ore bed carry out pyrolysis and will be wherein useful constituent change fluid into, flowing transfers to the target well, and then row adopts a kind of mining methods to ground.Compare with strip mining transformation or pit mining, huge advantage with aspects such as safety, efficient, energy-saving and environmental protection, owing to do not destroy the face of land, free from environmental pollution, exploit, especially have very wide development and application prospect in the mining mineral resource of deep at underground mineral resources, therefore, theoretical research is carried out in original position heat injection exploitation, had very important meaning and value.
Existing thermal decomposition test studies show that, all there are the critical temperature value that influences the mineral pyrolysis and generate product speed in resinous shale and low-disintegration coal etc., gas yield reached maximum when the meager lean coal heating surpassed 310 ℃, and long-flame coal is aerogenesis optimum temperature section at 450～500 ℃, and the critical temperature value of resinous shale is between 400～600 ℃.But these results all obtain under no restrained condition, be simple consideration structural change and the product analysis of mineral under the variation of temperature effect, the true occurrence condition of its test condition and subsurface mineral is far apart, can not embody the deep mineral and compose the terrestrial stress condition of depositing.Be the occurrence condition of real simulation deep subsurface mineral more, carry out the research of High Temperature High Pressure pyrolytic reaction, need carry out important innovation to test method and test unit.
Summary of the invention:
The purpose of the test method of a kind of High Temperature High Pressure pyrolytic reaction of the present invention is, overcome the shortcomings and deficiencies of traditional experiment method, according to the terrestrial stress condition under the mineral geology occurrence condition, provide a kind of can satisfy in testing laboratory underground deep mineral are carried out the advanced person of High Temperature High Pressure pyrolytic reaction, efficient, directly perceived, test method and related device reliably.
The test method of a kind of High Temperature High Pressure pyrolytic reaction of the present invention, it is characterized in that the device that adopts can load axial compression and confined pressure to test specimen under hot conditions, sample dimensions is respectively Ф 25 * 50mm and Ф 50 * 100mm, test specimen axial compression and confined pressure reach 20MPa, the test specimen environment temperature reaches 600 ℃, can simulate the geologic media condition that the mineral depth of burial reaches 800m, this test unit is by the pyrolytic reaction system, the gaseous tension injected system, fluid product discharges system and test control system four big systems form, the pyrolytic reaction system is the important component part of system, the test specimen that is respectively Ф 25 * 50mm and Ф 50 * 100mm around two kinds of sample dimensions heats respectively, the highlyest be heated to 600 ℃, fully to carry out pyrolytic reaction; The gaseous tension injected system mainly is injected into gases at high pressure in the kettle, loads axial compression and the confined pressure reach as high as 20MPa to test specimen, truly buries geologic media with the simulation mineral; Fluid product is discharged system, and mainly the fluid of the free state that test specimen is generated after the High Temperature High Pressure pyrolytic reaction discharges the discharge kettle naturally and collects; Test control system is mainly accurately measured and is controlled process of the test by all temps and pressure transducer, with the reliability of warranty test condition and test structure, and directly shows total system working condition and test result after the computer computational analysis; Adopt the method for this device: at first test specimen is placed sample tube 16, and sample tube 16 put into kettle inner chamber 17, covering kettle inner chamber lid 14 also seals with fastening bolt 13, set heating-up temperature, opening 18 pairs of test specimens of heating rod heats, by control temperature sensor 10 control temperature, after temperature reaches setting value and stablizes 30 minutes, open the gaseous tension injected system test specimen is applied axial compression and confined pressure, by electro connecting pressure gauge 7 controlled pressures to setup pressure value, make test specimen remain on constant temperature and pressure state under the simulation stratum condition fully to carry out pyrolytic reaction by regulating test control system, reaction time is 24～48 hours, then, open fluid product and discharge system, the fluid of the free state that test specimen is generated after the High Temperature High Pressure pyrolytic reaction discharges naturally discharges kettle, and respectively by vent port 21, vent valve 22 and outage 24, tapping valve 25 enters into gas gathering system 23 and fluid collection systems 26; By the composition and the analysis on Content that generate product are injected input output analysis, and test specimen carried out permeability test and rock mechanics attribute testing, under this test condition, the pyrolysis benefit of resinous shale or low-disintegration coal is carried out evaluation analysis, change sample and respective action temperature, pressure geologic media condition, the repetition above-mentioned steps can be carried out resinous shale or the analysis of low-disintegration coal pyrolysis benefit evaluation under the different condition, and its concrete step of implementing is:
1) is that the test specimen of Ф 25 * 50mm or Ф 50 * 100mm places sample tube 16 with sample dimensions, and puts it into kettle inner chamber 17, cover kettle inner chamber lid 14 and seal with 13 pairs of kettlies of fastening bolt;
2) set heating-up temperature, open 18 pairs of test specimens of heating rod and heat, after temperature reaches 20～600 ℃ of setting values and stablizes 30 minutes, open the gaseous tension injected system test specimen is applied axial compression and confined pressure, to setup pressure value 0～20MPa;
3) make test specimen remain on constant temperature and pressure state under the simulation stratum condition fully to carry out pyrolytic reaction by regulating test control system, the reaction time is 24～48 hours;
4) open fluid product and discharge system, the fluid of the free state that test specimen is generated after the High Temperature High Pressure pyrolytic reaction discharges naturally discharges kettle, and enters into gas gathering system 23 and fluid collection systems 26 by vent port 21, vent valve 22 and outage 24, tapping valve 25 respectively;
5) utilize temperature sensor 10,11 and pressure transducer 7,9 detection of dynamic test figures, and with data transmission to computing machine, by the composition and the analysis on Content that generate product are injected input output analysis, and test specimen carried out permeability test and rock mechanics attribute testing, under this test condition, the pyrolysis benefit of resinous shale or low-disintegration coal is carried out evaluation analysis, and this High Temperature High Pressure pyrolytic reaction test is finished.
The advantage of the test method of a kind of High Temperature High Pressure pyrolytic reaction of the present invention is: compare with related device with existing High Temperature High Pressure thermal decomposition test method, this detection method takes into full account the terrestrial stress condition under the mineral geology occurrence condition, utilize its device to load axial compression and the confined pressure that reaches 20MPa respectively to test specimen, the test specimen environment temperature reaches 600 ℃, can simulate the geologic media condition that the mineral depth of burial reaches 800m.The present invention is not only the test method of High Temperature High Pressure pyrolytic reaction and the important innovation of test unit, and the original position solution mining that more big buried depth can not be exploited mineral provides feasible test method.
Description of drawings:
Fig. 1: the test unit synoptic diagram of High Temperature High Pressure pyrolytic reaction
Label among the figure: 1---gas; 2---filtrator; 3---pressure regulator valve; 4---the gas boosting pump; 5---gas admittance valve; 6---air admission hole; 7---electro connecting pressure gauge; 8---safety valve; 9---pressure transducer; 10---the control temperature sensor; 11---the thermometric temperature sensor; 12---go up insulation cover; 13---fastening bolt; 14---kettle inner chamber lid; 15---the kettle bracing frame; 16---the sample tube; 17---the kettle inner chamber; 18---heating rod; 19---orifice plate; 20---following insulation cover; 21---vent port; 22---vent valve; 23---gas gathering system; 24---outage; 25---tapping valve; 26---fluid collection systems.
Embodiment:
Embodiment 1:The test unit that this test method adopts discharges system by pyrolytic reaction system, gaseous tension injected system, fluid product and test control system four big systems form.Wherein, the pyrolytic reaction system is the important component part of system, mainly test specimen is heated, to carry out pyrolytic reaction; The gaseous tension injected system mainly is injected into gases at high pressure in the kettle, loads different axial compression and confined pressure to test specimen, truly buries geologic media with the simulation mineral; Fluid product is discharged system, and mainly the fluid of the free state that test specimen is generated after the High Temperature High Pressure pyrolytic reaction discharges the discharge kettle naturally and collects; Test control system is mainly accurately measured and is controlled process of the test by all temps and pressure transducer, with the reliability of warranty test condition and test structure, and directly shows total system working condition and test result after the computer computational analysis.
The test unit that this test method adopts can satisfy the testing requirements that simulation mineral depth of burial reaches the geologic media condition of 400m, by heating rod test specimen is heated to 600 ℃, axial compression and the confined pressure of 10MPa are provided to test specimen by the gaseous tension injected system, kept the abundant pyrolytic reaction of constant temperature and pressure state 24 hours, by the composition and the analysis on Content that generate product are injected input output analysis, and test specimen carried out permeability test and rock mechanics attribute testing, under this test condition, the pyrolysis benefit of resinous shale or low-disintegration coal is carried out evaluation analysis.The concrete operations step is as follows:
I. be that the test specimen of Ф 50 * 100mm places sample tube 16 with sample dimensions, and put it into kettle inner chamber 17, cover kettle inner chamber lid 14 and seal with 13 pairs of kettlies of fastening bolt;
II. setting heating-up temperature is 600 ℃, opens 18 pairs of test specimens of heating rod and heats, and after temperature reaches setting value and stablizes 30 minutes, opens the gaseous tension injected system test specimen is applied axial compression and confined pressure, to setup pressure value 10MPa;
III. make test specimen remain on constant temperature and pressure state under the simulation stratum condition to carry out pyrolytic reaction by regulation and control system, the reaction time is 24 hours;
IV. open fluid product and discharge system, the fluid of the free state that test specimen is generated after the High Temperature High Pressure pyrolytic reaction discharges naturally discharges kettle, and enters into gas gathering system 23 and fluid collection systems 26 by vent port 21, vent valve 22 and outage 24, tapping valve 25 respectively;
V. by the composition and the analysis on Content that generate product are injected input output analysis, and test specimen carried out permeability test and rock mechanics attribute testing, under this test condition, the pyrolysis benefit of resinous shale or low-disintegration coal is carried out evaluation analysis, and this High Temperature High Pressure pyrolytic reaction test is finished.
Embodiment 2:The test unit that this test method adopts can satisfy the testing requirements that simulation mineral depth of burial reaches the geologic media condition of 600m, by heating rod test specimen is heated to 600 ℃, axial compression and the confined pressure of 15MPa are provided to test specimen by the gaseous tension injected system, kept the abundant pyrolytic reaction of constant temperature and pressure state 36 hours, by the composition and the analysis on Content that generate product are injected input output analysis, and test specimen carried out permeability test and rock mechanics attribute testing, under this test condition, the pyrolysis benefit of resinous shale or low-disintegration coal is carried out evaluation analysis.Other is with embodiment 1.
Embodiment 3:The test unit that this test method adopts can satisfy the testing requirements that simulation mineral depth of burial reaches the geologic media condition of 800m, by heating rod test specimen is heated to 600 ℃, axial compression and the confined pressure of 20MPa are provided to test specimen by the gaseous tension injected system, kept the abundant pyrolytic reaction of constant temperature and pressure state 48 hours, by the composition and the analysis on Content that generate product are injected input output analysis, and test specimen carried out permeability test and rock mechanics attribute testing, under this test condition, the pyrolysis benefit of resinous shale or low-disintegration coal is carried out evaluation analysis.Other is with embodiment 1.
Claims (1)
1. the test method of a High Temperature High Pressure pyrolytic reaction, it is characterized in that the device that adopts can load axial compression and confined pressure to test specimen under hot conditions, sample dimensions is respectively Ф 25 * 50mm and Ф 50 * 100mm, test specimen axial compression and confined pressure reach 20MPa, the test specimen environment temperature reaches 600 ℃, can simulate the geologic media condition that the mineral depth of burial reaches 800m, this test unit is by the pyrolytic reaction system, the gaseous tension injected system, fluid product discharges system and test control system four big systems form, the pyrolytic reaction system is the important component part of system, the test specimen that is respectively Ф 25 * 50mm and Ф 50 * 100mm around two kinds of sample dimensions heats respectively, the highlyest be heated to 600 ℃, fully to carry out pyrolytic reaction; The gaseous tension injected system mainly is injected into gases at high pressure in the kettle, loads axial compression and the confined pressure reach as high as 20MPa to test specimen, truly buries geologic media with the simulation mineral; Fluid product is discharged system, and mainly the fluid of the free state that test specimen is generated after the High Temperature High Pressure pyrolytic reaction discharges the discharge kettle naturally and collects; Test control system is mainly accurately measured and is controlled process of the test by all temps and pressure transducer, with the reliability of warranty test condition and test structure, and directly shows total system working condition and test result after the computer computational analysis; Adopt the method for this device: at first test specimen is placed sample tube (16), and sample tube (16) put into kettle inner chamber (17), covering kettle inner chamber lid (14) also seals with fastening bolt (13), set heating-up temperature, opening heating rod (18) heats test specimen, by control temperature sensor (10) control temperature, after temperature reaches setting value and stablizes 30 minutes, open the gaseous tension injected system test specimen is applied axial compression and confined pressure, by electro connecting pressure gauge (7) controlled pressure to setup pressure value, make test specimen remain on constant temperature and pressure state under the simulation stratum condition fully to carry out pyrolytic reaction by regulating test control system, reaction time is 24～48 hours, then, open fluid product and discharge system, the fluid of the free state that test specimen is generated after the High Temperature High Pressure pyrolytic reaction discharges naturally discharges kettle, and respectively by vent port (21), vent valve (22) and outage (24), tapping valve (25) enters into gas gathering system (23) and fluid collection systems (26), by the composition and the analysis on Content that generate product are injected input output analysis, and test specimen carried out permeability test and rock mechanics attribute testing, under this test condition, the pyrolysis benefit of resinous shale or low-disintegration coal is carried out evaluation analysis, change sample and respective action temperature, pressure geologic media condition, the repetition above-mentioned steps can be carried out resinous shale or the analysis of low-disintegration coal pyrolysis benefit evaluation under the different condition, and its concrete step of implementing is:
1) is that the test specimen of Ф 25 * 50mm or Ф 50 * 100mm places sample tube (16) with sample dimensions, and puts it into kettle inner chamber (17), cover kettle inner chamber lid (14) and with fastening bolt (13) kettle is sealed;
2) set heating-up temperature, open heating rod (18) test specimen is heated, after temperature reaches 20～600 ℃ of setting values and stablizes 30 minutes, open the gaseous tension injected system test specimen is applied axial compression and confined pressure, to setup pressure value 0～20MPa;
3) make test specimen remain on constant temperature and pressure state under the simulation stratum condition fully to carry out pyrolytic reaction by regulating test control system, the reaction time is 24～48 hours;
4) open fluid product and discharge system, the fluid of the free state that test specimen is generated after the High Temperature High Pressure pyrolytic reaction discharges naturally discharges kettle, and enters into gas gathering system (23) and fluid collection systems (26) by vent port (21), vent valve (22) and outage (24), tapping valve (25) respectively;
5) utilize temperature sensor (10), (11) and pressure transducer (7), (9) detection of dynamic test figure, and with data transmission to computing machine, by the composition and the analysis on Content that generate product are injected input output analysis, and test specimen carried out permeability test and rock mechanics attribute testing, under this test condition, the pyrolysis benefit of resinous shale or low-disintegration coal is carried out evaluation analysis, and this High Temperature High Pressure pyrolytic reaction test is finished.
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| CN105203583A (en) * | 2014-05-30 | 2015-12-30 | 宝山钢铁股份有限公司 | Device and method for testing coal pyrolysis coking process |
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| CN107064450A (en) * | 2017-03-14 | 2017-08-18 | 中国矿业大学 | The experimental method of the solid thermalization multi- scenarios method of coal body stream under a kind of simulation Thermal-mechanical Coupling |
| CN109632868A (en) * | 2019-01-14 | 2019-04-16 | 中南大学 | A kind of closed system hydrocarbon thermal simulation experiment device and its application method |
| CN112730503A (en) * | 2021-01-20 | 2021-04-30 | 太原理工大学 | Operation method of simulation device for extracting oil shale from high-temperature fluid |
| CN112782209A (en) * | 2020-12-17 | 2021-05-11 | 中国石油大学(华东) | Diagenetic simulation experiment device and method capable of researching underground in-situ conversion process |
| CN113092279A (en) * | 2021-04-02 | 2021-07-09 | 太原理工大学 | Triaxial fracturing seepage device under coal rock thermo-hydro-mechanical coupling effect and test method |
| CN114509378A (en) * | 2022-04-13 | 2022-05-17 | 太原理工大学 | Simulation device and experiment method for seepage and pyrolysis in-situ mining of organic rock |
| CN114527255A (en) * | 2022-02-18 | 2022-05-24 | 中国矿业大学 | Method for quantitatively evaluating element mobility in coal in high-temperature simulation process |
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| CN103822842B (en) * | 2014-02-13 | 2019-02-26 | 中国科学院过程工程研究所 | Sampling and quantitative analysis method in a kind of solid fuel pyrolysis production process |
| CN104849172A (en) * | 2014-02-18 | 2015-08-19 | 中国石油化工股份有限公司 | Oil shale oil content test experiment apparatus and test method thereof |
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| CN107064450B (en) * | 2017-03-14 | 2019-04-26 | 中国矿业大学 | Coal body stream consolidates the experimental method of thermalization multi- scenarios method under a kind of simulation Thermal-mechanical Coupling |
| CN109632868A (en) * | 2019-01-14 | 2019-04-16 | 中南大学 | A kind of closed system hydrocarbon thermal simulation experiment device and its application method |
| CN109632868B (en) * | 2019-01-14 | 2021-05-28 | 中南大学 | Closed system hydrocarbon generation thermal simulation experiment device and using method thereof |
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| CN112782209A (en) * | 2020-12-17 | 2021-05-11 | 中国石油大学(华东) | Diagenetic simulation experiment device and method capable of researching underground in-situ conversion process |
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