CN109540734A - Coal seam with gas High Pressure Absorption/the test device for desorption and method of controllable moisture - Google Patents
Coal seam with gas High Pressure Absorption/the test device for desorption and method of controllable moisture Download PDFInfo
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- CN109540734A CN109540734A CN201910020382.7A CN201910020382A CN109540734A CN 109540734 A CN109540734 A CN 109540734A CN 201910020382 A CN201910020382 A CN 201910020382A CN 109540734 A CN109540734 A CN 109540734A
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- 238000012360 testing method Methods 0.000 title claims abstract description 115
- 239000003245 coal Substances 0.000 title claims abstract description 106
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 title claims abstract description 14
- 238000003795 desorption Methods 0.000 title claims abstract description 11
- 238000005259 measurement Methods 0.000 claims abstract description 53
- 239000012266 salt solution Substances 0.000 claims abstract description 39
- 238000002336 sorption--desorption measurement Methods 0.000 claims abstract description 21
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 20
- 239000007789 gas Substances 0.000 claims description 133
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 90
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 56
- 239000001307 helium Substances 0.000 claims description 39
- 229910052734 helium Inorganic materials 0.000 claims description 39
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 39
- 229920006395 saturated elastomer Chemical class 0.000 claims description 34
- 238000007789 sealing Methods 0.000 claims description 33
- 238000001179 sorption measurement Methods 0.000 claims description 30
- 239000002245 particle Substances 0.000 claims description 14
- 238000005192 partition Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000002817 coal dust Substances 0.000 claims description 9
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical class C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- 238000011161 development Methods 0.000 claims description 6
- 238000010998 test method Methods 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 4
- 238000009938 salting Methods 0.000 claims description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 3
- 238000003556 assay Methods 0.000 claims description 3
- 238000009434 installation Methods 0.000 claims description 3
- 238000012544 monitoring process Methods 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- 238000005660 chlorination reaction Methods 0.000 claims description 2
- 238000002474 experimental method Methods 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 206010003497 Asphyxia Diseases 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003034 coal gas Substances 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N7/02—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder
- G01N7/04—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder by absorption or adsorption alone
Abstract
The present invention relates to the coal seam with gas High Pressure Absorption/test device for desorption and method of a kind of controllable moisture, belong to coal seam with gas test field.The device includes pumped vacuum systems, inflation system, constant temperature system and the gas adsorption/desorption test macro for controlling moisture;Controllable moisture measurement tank of the invention keeps confined space humidity principle using saturation inorganic salt solution, successfully solves the problems, such as since test period is too long or the change of experimental condition etc. causes moisture in coal body to change.The present invention includes pumped vacuum systems, inflation system, constant temperature system, the gas adsorption/desorption test macro for controlling moisture, and overall structure is simple, and easy to operate, using effect is obvious, and cost is relatively low.
Description
Technical field
The invention belongs to coal seam with gas to test field, be related to a kind of coal seam with gas High Pressure Absorption/solution of controllable moisture
Inhale experimental rig and method.
Background technique
Gas (coal bed gas) is the accompaniment in coal generating process, is that rotten plant type organic matter generates simultaneously in coalification course
Preservation is methane in coal seam and a kind of natural-gas of coal measure strata, main ingredient.Gas is to cause coal mine production safety thing
Therefore important hidden danger.Gas in the form of free state and two kinds of adsorbed state preservation in coal seam.In seam mining, by well
Under adopt movement industry influence, cause coal-bed gas constantly to discharge, to cause coal and gas prominent, gas explosion, gas asphyxiation
Deng harm, the sound development of coal in China industrial security is seriously threatened.From the perspective of the energy, gas is a kind of clean
Only, conveniently, efficient new energy.Therefore, the gas adsorption/desorption properties for accurately grasping coal seam are to prevent mine safety accidents
The key point that generation and coal bed gas Efficient Development utilize.
It is well known that coal body is a kind of hole and a kind of simultaneous porous media in crack.The preservation ring of primitive coalbed
Border be by coal body, gas, moisture three-phase coexistence organic system.Water in coal is mainly deposited in the form of Free water and inherent two kinds of water
?.Free water is primarily present in coalmass crevasse, inherent water mainly by polymolecular layer physical absorption and cohesion etc. in a manner of preservation in
In coal body hole, hole is more flourishing, and inherent water content is also bigger.
Currently, related moisture to the impact analysis of coal seam with gas adsorption/desorption feature mainly based on laboratory research, close
Mainly include following water flood in the production of moisture content coal sample and is saturated external saturated salt solution method.
The water flood.Such method invades liquid water in coal sample, controls coal by the quality of the liquid water of injection
Moisture content in sample, to complete the production of different water cut coal sample.As Chinese patent literature CN201010580065 is authorized
" test device and method of the additional moisture to coal seam with gas desorption properties ".
The external saturated salt solution method.Such Method And Principle is to utilize coal sample moisture in saturated salt solution Control experiment tank
Content.Such as a kind of " gas adsorption desorption properties test of pre- adsorption moisture coal sample of Chinese patent CN201711091105 publicity
Device and its test method ", the patent is mixed by the distilled water of certain temperature (60 DEG C) and a certain amount of salt (K2SO4) particle first
It closes, is configured to saturated solution under the conditions of certain temperature, then saturated salt solution pours into glass evacuated ware and restores to room temperature, most again
Then vacuum ware equipped with saturated salt solution is connected to by the end form environment certain at relative humidity with the test tank equipped with coal sample,
It allows coal sample adsorption moisture, and then obtains the test coal sample of different water cut.
In conclusion the coal sample that the production method of two kinds of moisture content coal samples can be obtained accurately when test just starts is aqueous
Rate, but they all have ignored the change with experimental condition, the moisture content of coal sample can also change.Such as in test tank
The moisture of coal sample changes with the increase of adsorption/desorption time and the variation of adsorption/desorption temperature, especially hot conditions
Under, liquid water molecules will be vaporized gradually in coal sample, cause coal gas to measure test result error larger.Therefore, above-mentioned two
Kind method not can guarantee a certain fixed value of water tariff collection in coal sample during the whole test process.
Summary of the invention
In view of this, that the purpose of the present invention is to provide a kind of structures is simple, test method is easy, suction can be efficiently controlled
Attached water divides the gas adsorption/desorption properties test device and its test method of coal sample.
In order to achieve the above objectives, the invention provides the following technical scheme:
Coal seam with gas High Pressure Absorption/test device for desorption of controllable moisture, including pumped vacuum systems, inflation system, perseverance
Gas adsorption/desorption test macro of warm system and control moisture;
The pumped vacuum systems includes vacuum pump, the vacuum meter and vacuum line that are connected with vacuum pump, and described in connection
The first valve on vacuum line;Vacuum meter is installed on the vacuum pump;The vacuum pump side is connect with vacuum line, described
Vacuum line end is installed by the first valve;First valve one end is connect with vacuum line, the other end and the 4th Highpressure Tee
Connection;
The inflation system includes high-pressure helium inflation system and high pressure methane inflation system;The helium inflation system
Including high pressure helium gas cylinder, the first pressure reducing valve and the first high-precision pressure sensor;The high pressure helium gas cylinder, the first pressure reducing valve and
It is successively attached using pressure duct between first high-precision pressure sensor, and is finally reached the first Highpressure Tee;It is described
Methane inflation system include high pressure methane gas cylinder, pressure reducing valve and the second high-precision pressure sensor;The high pressure methane gas
It is successively attached using pressure duct between bottle, the second pressure reducing valve and the second high-precision pressure sensor, and is finally reached the
One Highpressure Tee;The first air circuit connection of first Highpressure Tee helium inflation system;Second air circuit connection methane inflation system;
The second Highpressure Tee of third air circuit connection;First Highpressure Tee described in second Highpressure Tee, first air circuit connection;Second gas
Road connects the second valve, and is eventually leading to control moisture with reference in tank;Third air circuit connection third high-precision pressure sensor;Institute
State third high-precision pressure sensor connection third Highpressure Tee;Third described in first air circuit connection of third Highpressure Tee
High-precision pressure sensor;Second air circuit connection third valve, and it is eventually leading to control moisture measurement tank;Third air circuit connection
Four Highpressure Tees;The first gas circuit of 4th Highpressure Tee is connect with the third Highpressure Tee, the second gas circuit and described first
Valve connection, into vacuum system;Third gas circuit is connect with the 4th valve, and is eventually leading to atmosphere;
The water bath with thermostatic control system includes thermostatic water bath and circulation;The thermostatic water bath includes slot, heating tube, temperature
Spend sensor, humidostat and partition composition;The humidostat is arranged in outside groove body, by conducting wire and heating tube and
Temperature sensor connection, and then control temperature;The baffle arrangement separates groove body in the lower part of groove body, for managing, described
Heating tube, temperature sensor are arranged in below partition, aspect placement control moisture reference can and control moisture on the partition
Test tank;The circulation is made of water-circulating pump and circulation line;2 are separately included in the water bath with thermostatic control system
Water-circulating pump and circulation line are arranged in groove body two sides deep and superficial part, form uniform and stable bath temperature;
Gas adsorption/desorption test macro of the control moisture includes that two structures are identical, the equal control of volume size
Moisture processed is with reference to tank, control moisture measurement tank, the second valve, third valve, the 5th valve, the 5th Highpressure Tee, high temperature and pressure
Hygrometer, graduated cylinder and conical flask, third high-precision pressure sensor;The control moisture is placed on the clamping plate with reference to tank,
The control moisture connects the second valve, the second valve connection second Highpressure Tee with reference to tank top;The control
Moisture measurement tank processed is also positioned on the clamping plate, the control moisture measurement tank and the first gas of the 5th Highpressure Tee
Road connection, the second gas circuit of the 5th Highpressure Tee are connect with third valve, the third valve and the third Highpressure Tee
Second air circuit connection;The 5th Highpressure Tee third gas circuit is connect with high pressure-temperature hygrometer, the high pressure-temperature hygrometer
It is connect with the 5th valve, the 5th valve is connect with the graduated cylinder, and the graduated cylinder is connect with the conical flask;
The control moisture is that two structures are identical with control moisture measurement tank with reference to tank, volume size comparable assay tank
Body;Structure composition about the tank body is analyzed, and is analyzed for controlling moisture measurement tank;The control moisture measurement tank
Including pedestal, saturated salt solution stores cavity, limiting device, screen device, coal sample and tests cavity, tank body sealing cover body, high pressure
Air inlet/outlet, the first sealing ring, the second sealing ring composition;The bottom of the control moisture measurement tank is the pedestal, is placed on
On the clamping plate;The pedestal top is arranged the saturated salt solution and stores cavity;The saturated salt solution stores cavity top
Inwardly projecting limiting device is set, removable filter device is installed above the limiting slot;The saturated salt solution storage
Cavity top is installed by the first sealing ring;Installation coal sample tests cavity above first sealing ring;The saturated salt solution is deposited
It puts and is connected by screw bolts between cavity top and coal sample test cavity;The second sealing of installation at the top of the coal sample test cavity
Circle, second sealing ring upper end install tank body sealing cover body, install high pressure air inlet/outlet in the middle part of the tank body sealing cover body;Institute
Coal sample test cavity top is stated to be connected by screw bolts with tank body sealing cover body.
Test method based on described device, comprising the following steps:
(a) sample making;Raw coal is crushed first, then test coal dust is screened using sieve;Especially need to infuse
Meaning, since control moisture measurement tank installs sieve, the mesh number of test coal powder has to be larger than in control moisture measurement tank and sieves
The mesh number of net avoids coal dust during test from falling into salting liquid, influences test accuracy;
(2) saturated salt solution is prepared and is placed;According to the experimental condition of quasi- development, suitable inorganic salt particle is selected, it will
The distilled water of certain temperature and a certain amount of a certain inorganic salt particle mixing, prepare saturation inorganic salt solution, then will saturation
Inorganic salt solution pours into control moisture and stores in cavity with reference to the saturated salt solution in tank and control moisture measurement tank, and will filtering
Device is placed in the top of the tank body, finally tightens between the saturated salt solution storage cavity of test tank and coal sample test cavity
Bolt;
(3) test sample is placed;The coal dust of certain mass is put into control moisture measurement tank coal sample test cavity, control
Moisture refers in tank and does not add test coal sample, and tightens bolt;Then it allows and is placed into water bath with thermostatic control clamping plate with reference to tank and test tank
On, finally connect each gas piping;
(4) air-leakage test;All test associated pipes are connected, and the tank body is placed into the clamping plate of thermostatic water bath
On;The first valve, the 4th valve and the 5th valve are closed, the second valve and third valve are opened, then opens high pressure helium gas cylinder
And first pressure reducing valve 7MPa or so high-pressure helium is filled with into test macro;The first pressure reducing valve is closed after a period of time, is observed
The situation of change of high-precision pressure meter pressure;After the completion of gas air tight test, closes high pressure helium gas cylinder and the first pressure reducing valve and beat
The 4th valve is opened, the helium in system is discharged;
(5) water bath with thermostatic control;Add water in the sink for laying tank body, it is necessary to which flooding test tank completely could stop adding water;
Bath temperature is set, and starts water circulating pump;
(6) vacuum outgas;Set temperature is reached after a certain period of time to bath temperature, closes the 4th valve, opens the first valve
Door is opened vacuum pump, is vacuumized to system;When vacuum degree reaches 4.0Pa or less, one timing of evacuated state is still kept
Between;
(7) high pressure helium gas cylinder and the first pressure reducing valve are opened, closes high pressure after the helium of about 3MPa is slowly filled with to reference tank
Helium tank and the first pressure reducing valve record the reading of third high-precision pressure gauge, then slowly open third valve, enter gas
Coal sample tank records after the stable reading of high-precision pressure gauge again, calculates the free volume of coal sample tank;
(8) the 4th valve is opened, the helium in pilot system is released;It is then shut off the 4th valve, opens the first valve, the
Two valves and third valve, and vacuum pump is opened, operation is vacuumized to pilot system for the second time, is reached to vacuum degree
When 4.0Pa or less, still keep evacuated state 3 hours or more;
(9) the first valve and vacuum pump are successively closed, is then surveyed using high temperature and pressure humidity sensor monitoring control moisture
Humidity in tank is tried, the time for controlling coal sample adsorption moisture in moisture measurement tank must not be lower than 5 days, ensure that coal sample sufficiently adsorbs water
Point;
(10) close third valve, open high pressure methane gas cylinder and the second pressure reducing valve, make the methane gas of certain pressure into
Enter moisture control with reference to tank, is then shut off high pressure methane gas cylinder and the second pressure reducing valve, and record third high-precision pressure sensor
Data;
(11) third valve is slowly opened, moisture control is allowed to enter control moisture measurement tank with reference to the methane gas in tank,
Adsorb methane gas with certain moisture coal sample, after adsorption equilibrium 12 hours and third high-precision pressure sensor data not
When change, related pressure data are recorded, are then calculated in turn according to absorption front and back change value of pressure and the volume test value
Methane adsorption amount under the adsorption equilibrium pressure condition, is then shut off third valve;
(12) high pressure methane gas cylinder and the second pressure reducing valve are opened, increases adsorbed gas pressure step by step, and be repeated in step
Suddenly the coal body adsorption gas curve under certain temperature and moisture condition is drawn in (10)~(11);
(13) after completing adsorption test, the second valve is closed, the 5th valve is opened, releases a certain amount of methane gas
The 5th valve is closed afterwards, utilizes the volume of graduated cylinder and conical flask measurement release methane gas;Then moisture control is allowed to be adsorbed simultaneously
Coal sample in tank is adsorbed again with gas, and adsorption time is not less than 12 hours, and utilizes the record absorption of third high-precision pressure gauge
Pressure value after balance;
(14) step (13) are repeated, discharges methane gas in moisture control test tank step by step, obtains certain temperature and humidity
Under the conditions of coal body desorb gas curve;
(15) when carrying out the test of next temperature grade, above-mentioned steps (9)~(14) are repeated in, and then are obtained certain
Coal body adsorption/desorption gas curve under moisture and condition of different temperatures;
(16) when carrying out the test of next moisture levels, according to required moisture condition, suitable inorganic salt particle is selected, so
After repeat the above steps (2)~(15).
Further, the suitable inorganic salt particle meets: when testing moisture is 20%, selective chlorination sodium inorganic salts
Grain.
The beneficial effects of the present invention are: controllable moisture measurement tank of the invention keeps closed using saturation inorganic salt solution
Space humidity principle is successfully solved since test period is too long or the change of experimental condition etc. causes moisture in coal body to occur
The problem of variation.The present invention includes pumped vacuum systems, inflation system, constant temperature system, the gas adsorption/desorption test for controlling moisture
System, overall structure is simple, easy to operate, and using effect is obvious, and cost is relatively low.
Detailed description of the invention
In order to keep the purpose of the present invention, technical scheme and beneficial effects clearer, the present invention provides following attached drawing and carries out
Illustrate:
Fig. 1 is a kind of coal seam with gas High Pressure Absorption/test device for desorption structural schematic diagram of controllable moisture;
Fig. 2 is that a kind of control moisture refers to tank arrangement structural schematic diagram;
Appended drawing reference: 1- vacuum pump;2- vacuum meter;3- vacuum line;4- high pressure helium gas cylinder;5- high pressure methane gas cylinder;6-
First pressure reducing valve;The second pressure reducing valve of 7-;8- pressure duct;The first high-precision pressure sensor of 9-;The second high-precision pressure of 10- passes
Sensor;The first Highpressure Tee of 11-;The second Highpressure Tee of 12-;13- third Highpressure Tee;The 4th Highpressure Tee of 14-;15- the 5th
Highpressure Tee;16- groove body;17- heating tube;18- temperature sensor;19- humidostat;20- partition;21- water-circulating pump;
22- circulation line;23- controls moisture and refers to tank;24- controls moisture measurement tank;25- high temperature and pressure hygrometer;26- graduated cylinder;27-
Conical flask;28- third high-precision pressure sensor;The first valve of F1-;The second valve of F2-;F3- third valve;The 4th valve of F4-
Door;The 5th valve of F5-;231- pedestal;232- saturated salt solution stores cavity;233- limiting device;234- screen device;235-
Coal sample tests cavity;236- tank body sealing cover body;237- high pressure air inlet/outlet;The first sealing ring of 238-;The second sealing ring of 239-.
Specific embodiment
Below in conjunction with attached drawing, a preferred embodiment of the present invention will be described in detail.
As shown in Figure 1, a kind of coal seam with gas High Pressure Absorption/test device for desorption under controllable moisture condition it include taking out
Vacuum system, inflation system, constant temperature system, the gas adsorption/desorption test macro for controlling moisture.
Pumped vacuum systems includes vacuum pump 1, the vacuum meter being connected with vacuum pump 2 and vacuum line 3, and connection vacuum tube
The first valve F1 on road 3.Vacuum meter 2 is mounted on vacuum pump 1;Vacuum pump side is connect with vacuum line 3, vacuum line end
End is mounted with the first valve F1;First one end valve F1 is connect with vacuum line 3, and the other end is connect with the 4th Highpressure Tee 14.
Pumped vacuum systems is for carrying out whole system to vacuumize degassing process.
Inflation system includes high-pressure helium inflation system and high pressure methane inflation system.Helium inflation system mainly includes height
Press helium tank 4, the first pressure reducing valve 6 and the first high-precision pressure sensor 9.High pressure helium gas cylinder 4, the first pressure reducing valve 6 and first are high
It is successively attached using pressure duct 8 between accuracy pressure sensor 9, and is finally reached the first Highpressure Tee 11.Methane fills
Gas system mainly includes high pressure methane gas cylinder 5, pressure reducing valve 7 and the second high-precision pressure sensor 10.High pressure methane gas cylinder 5,
It is successively attached using pressure duct 8 between two pressure reducing valves 7 and the second high-precision pressure sensor 10, and is finally reached first
Highpressure Tee 11.First Highpressure Tee, 11 first air circuit connection helium inflation system;Second air circuit connection methane inflation system;The
Three the second Highpressure Tees of air circuit connection 12.First Highpressure Tee 11 described in second Highpressure Tee, 12 first air circuit connection;Second gas
Road connects the second valve F2, and is eventually leading to control moisture with reference in tank 23;Third air circuit connection third high-precision pressure sensing
Device 28.Third high-precision pressure sensor 28 connects third Highpressure Tee 13.13 first air circuit connection third of third Highpressure Tee
High-precision pressure sensor 28;Second air circuit connection third valve F3, and it is eventually leading to control moisture measurement tank 24;Third gas circuit
Connect the 4th Highpressure Tee 14.4th Highpressure Tee, 14 first gas circuit is connect with the third Highpressure Tee 13, the second gas circuit with
The first valve F1 connection, into vacuum system;Third gas circuit is connect with the 4th valve F4, and is eventually leading to atmosphere.Inflation
System is for providing the test gas of different pressures.
Water bath with thermostatic control system includes thermostatic water bath and circulation.Thermostatic water bath mainly include groove body 16, heating tube 17,
Temperature sensor 18, humidostat 19 and partition 20 form.Humidostat 19 is arranged in outside groove body 16, by conducting wire with
Heating tube 17 and temperature sensor 19 connect, and then control temperature;Partition 20 is arranged in the lower part of groove body 16, separates for managing
Groove body 16, heating tube 17, temperature sensor 18 are arranged in 20 lower section of partition, placement control moisture reference can 23 above partition 20
With control moisture measurement tank 24.Circulation is mainly made of water-circulating pump 21 and circulation line 22.In water bath with thermostatic control system
2 water-circulating pumps 21 and circulation line 22 have been separately included, 16 two sides deep of groove body and superficial part are arranged in, has been formed uniformly steady
Fixed bath temperature.Water bath with thermostatic control system is for providing different test simulation temperature.
Gas adsorption/desorption the test macro for controlling moisture mainly includes that two structures are identical, the equal control of volume size
Moisture processed is with reference to tank 23, control moisture measurement tank 24, the second valve F2, third valve F3, the 5th valve F5, the 5th Highpressure Tee
15, high temperature and pressure hygrometer 25, graduated cylinder 26 and conical flask 27, third high-precision pressure sensor 28.It controls moisture and refers to tank 23
It is placed on the clamping plate 20, control moisture connects the second valve F2, second valve F2 the second high pressure of connection with reference to 23 top of tank
Threeway 12.Control moisture measurement tank 24 is also positioned on clamping plate 20, controls moisture measurement tank 24 and the 5th Highpressure Tee 15
First air circuit connection, 15 second gas circuit of the 5th Highpressure Tee are connect with third valve F3, third valve F3 and third Highpressure Tee
13 second air circuit connections;5th Highpressure Tee, 15 third gas circuit is connect with high temperature and pressure hygrometer 26, high temperature and pressure hygrometer 26
It is connect with the 5th valve F5, the 5th valve F5 is connect with graduated cylinder 26, and graduated cylinder 26 is connect with conical flask 27.The gas for controlling moisture is inhaled
It is attached/desorption test macro using saturated salt solution adjust confined space moisture principle, by select different saturated salt solutions for
Test provides different damp conditions.
It is that two structures are identical with control moisture measurement tank 24 that moisture, which is controlled, with reference to tank 23, volume size comparable assay tank
Body.Structure composition about tank body is analyzed, and is described for controlling moisture measurement tank 23.It is main to control moisture measurement tank 23
Including pedestal 231, saturated salt solution stores cavity 232, limiting device 233, screen device 234, coal sample and tests cavity 235, tank
Body sealing cover body 236, high pressure air inlet/outlet 237, the first sealing ring 238, the second sealing ring 239 composition.Control moisture measurement tank
23 bottom is pedestal 231, is placed on clamping plate 20;231 top of pedestal is arranged saturated salt solution and stores cavity 232;Saturated salt
Solution stores 232 top of cavity and is provided with inwardly projecting limiting device 233, is mounted with removably mistake above limiting slot 233
Filter device 234;Saturated salt solution storage 232 top of cavity is mounted with the first sealing ring 238;It is installed above first sealing ring 238
Coal sample tests cavity 235;It is connected by screw bolts between saturated salt solution storage 232 top of cavity and coal sample test cavity 235;
The second sealing ring 239 is mounted at the top of coal sample test cavity 235, and 239 upper end of the second sealing ring is mounted with tank body sealing cover body
236, high pressure air inlet/outlet 237 is mounted in the middle part of tank body sealing cover body 236;Coal sample tests 234 top of cavity and tank body sealing cover
Body 235 is connected by screw bolts.
Coal seam with gas High Pressure Absorption/test device for desorption test method of above-mentioned controllable moisture includes the following steps:
(a) sample making.Raw coal is crushed first, then test coal dust is screened using sieve.Especially need to infuse
Meaning, since control moisture measurement tank is mounted with sieve, the mesh number of test coal powder is had to be larger than in control moisture measurement tank
The mesh number of sieve avoids coal dust during test from falling into salting liquid, influences test accuracy.
(2) saturated salt solution is prepared and is placed.According to the experimental condition of quasi- development, suitable inorganic salt particle (example is selected
Such as, test moisture 20% or so when, may be selected sodium chloride inorganic salt particle), by the distilled water of certain temperature and it is a certain amount of certain
A kind of inorganic salt particle mixing, prepares saturation inorganic salt solution, and saturation inorganic salt solution is then poured into control moisture with reference to tank
23 store in cavity with the saturated salt solution in control moisture measurement tank 24, and screen device is placed in the top of tank body, most
After tighten bolt.
(3) test sample is placed.The coal dust of certain mass is put into control 24 coal sample of moisture measurement tank test cavity, control
Moisture processed refers in tank 23 and does not add test coal sample, and tightens bolt.Then it allows and is placed into water bath with thermostatic control with reference to tank and test tank
On partition 20, each gas piping is finally connected.
(4) air-leakage test.All test associated pipes are connected, the first valve F1, the 4th valve F4 and the 5th valve are closed
Door F5, opens the second valve F2 and third valve F3, then opens high pressure helium gas cylinder 4 and the first pressure reducing valve 6 to test macro
In be filled with 7MPa or so high-pressure helium.The first pressure reducing valve 6 is closed after a period of time, the first high-precision pressure sensor 9 of observation
Pressure changing.After the completion of air tight test, the 4th valve F4 is opened, the helium in system is discharged.
(5) temperature controls.In the sink 16 for laying tank body 23 and 24 plus water, water must be flooded completely with reference to 23 He of tank
Test tank 24 could stop plus water;Bath temperature is set using humidostat 19, and starts water circulating pump 21.
(6) vacuum outgas.Set temperature is reached after a certain period of time to bath temperature, closes the 4th valve F4, opens first
Valve F1 opens vacuum pump 1, vacuumizes to system;When vacuum degree reaches 4.0Pa or less, evacuated state is still kept
Certain time.
(7) free volume calculates.High pressure helium gas cylinder 4 and the first pressure reducing valve 6 are opened, is slowly filled with about 3MPa to reference tank 23
Helium after close high pressure helium gas cylinder 4 and the first pressure reducing valve 6, record the reading of third high-precision pressure sensor 28, it is then slow
It is slow to open third valve F3, so that gas is entered control moisture measurement tank 24, the stable reading of third high-precision pressure sensor 28
It records again afterwards, the free volume of control moisture measurement tank 24 can be calculated.
(8) secondary vacuum pumping.The 4th valve F4 is opened, the helium in pilot system is released;It is then shut off the 4th valve F4,
The first valve F1, the second valve F2 and third valve F3 are opened, and opens vacuum pump 1, second is carried out to pilot system and is taken out very
Idle job is still kept evacuated state 3 hours or more when vacuum degree reaches 4.0Pa or less.
(9) water adsorption.The first valve F1 and vacuum pump 1 are successively closed, high temperature and pressure humidity sensor 25 is then utilized
Humidity in monitoring control moisture measurement tank, the time for controlling coal sample adsorption moisture in moisture measurement tank 24 must not be lower than 5 days, ensure
The abundant adsorption moisture of coal sample.
(10) third valve F3 is closed, high pressure methane gas cylinder 5 and the second pressure reducing valve 7 is opened, makes the methane gas of certain pressure
Body enters moisture control with reference to tank 23, is then shut off high pressure methane gas cylinder 5 and the second pressure reducing valve 7, and records third high-precision and press
The data of force snesor 28.
(11) third valve F3 is slowly opened, moisture control is allowed to enter control moisture measurement with reference to the methane gas in tank 23
In tank 24, adsorb methane gas with certain moisture coal sample, after adsorption equilibrium 12 hours and third high-precision pressure senses
When 28 pressure data of device is constant, related pressure data are recorded, are then surveyed according to absorption front and back change value of pressure and the volume
Examination value calculates the methane adsorption amount under the adsorption equilibrium pressure condition in turn, is then shut off third valve F3.
(12) high pressure methane gas cylinder 5 and the second pressure reducing valve 7 are opened, increases adsorbed gas pressure step by step, and be repeated in
Step (10)~(11) can draw the coal body adsorption gas curve under certain temperature and moisture condition.
(13) after completing adsorption test, the second valve F2 is closed, the 5th valve F5 is opened, releases out a certain amount of first
The 5th valve F5 is closed after alkane gas, utilizes the volume of graduated cylinder 26 and the measurement release methane gas of conical flask 27.Then it allows simultaneously
Coal sample in moisture control adsorption tanks 24 is adsorbed again with gas, and adsorption time is not less than 12 hours, and utilizes third high-precision
Pressure sensor 28 records pressure value after adsorption equilibrium.
(14) step (13) are repeated, discharges methane gas in moisture control test tank 24 step by step, obtains certain temperature and wet
Coal body under the conditions of degree desorbs gas curve.
(15) when carrying out the test of next temperature grade, above-mentioned steps (9)~(14) are repeated in, and then are obtained certain
Coal body adsorption/desorption gas curve under moisture and condition of different temperatures.
(16) when carrying out the test of next moisture levels, according to required moisture condition, suitable inorganic salt particle is selected, so
After repeat the above steps (2)~(15).
The present invention is changed aqueous in coal sample by the different saturated salt solution of the adsorption/desorption Systematic selection of control moisture
Amount;And can guarantee one timing of experimental condition, the moisture of coal sample remains steady state value during test, successfully avoids due to examination
The extension for testing the time causes the volatilization of moisture to the influence of test result.The invention can study coal sample in different in moisture content pair
Gas adsorption/desorption properties influence, the gas adsorption/desorption that can preferably react primitive coalbed especially High water cut coal seam drills
Law not only contributes to effectively preventing for coal-bed gas disaster, is also beneficial to the development and utilization of coal bed gas resource, overall structure
Simply, easy to operate, using effect is obvious, and cost is relatively low.
Finally, it is stated that preferred embodiment above is only used to illustrate the technical scheme of the present invention and not to limit it, although logical
It crosses above preferred embodiment the present invention is described in detail, however, those skilled in the art should understand that, can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Claims (3)
1. coal seam with gas High Pressure Absorption/test device for desorption of controllable moisture, it is characterised in that: including pumped vacuum systems, fill
Gas system, constant temperature system and the gas adsorption/desorption test macro for controlling moisture;
The pumped vacuum systems includes vacuum pump, the vacuum meter and vacuum line that are connected with vacuum pump, and the connection vacuum
The first valve on pipeline;Vacuum meter is installed on the vacuum pump;The vacuum pump side is connect with vacuum line, the vacuum
Line end installs the first valve;First valve one end is connect with vacuum line, and the other end is connect with the 4th Highpressure Tee;
The inflation system includes high-pressure helium inflation system and high pressure methane inflation system;The helium inflation system includes
High pressure helium gas cylinder, the first pressure reducing valve and the first high-precision pressure sensor;The high pressure helium gas cylinder, the first pressure reducing valve and first
It is successively attached using pressure duct between high-precision pressure sensor, and is finally reached the first Highpressure Tee;The first
Alkane inflation system includes high pressure methane gas cylinder, pressure reducing valve and the second high-precision pressure sensor;The high pressure methane gas cylinder,
It is successively attached using pressure duct between two pressure reducing valves and the second high-precision pressure sensor, and is finally reached the first high pressure
Threeway;The first air circuit connection of first Highpressure Tee helium inflation system;Second air circuit connection methane inflation system;Third gas
Road connects the second Highpressure Tee;First Highpressure Tee described in second Highpressure Tee, first air circuit connection;Second air circuit connection
Second valve, and control moisture is eventually leading to reference in tank;Third air circuit connection third high-precision pressure sensor;The third
High-precision pressure sensor connects third Highpressure Tee;The high-precision of third described in first air circuit connection of third Highpressure Tee
Pressure sensor;Second air circuit connection third valve, and it is eventually leading to control moisture measurement tank;The 4th high pressure of third air circuit connection
Threeway;The first gas circuit of 4th Highpressure Tee is connect with the third Highpressure Tee, and the second gas circuit and first valve connect
It connects, into vacuum system;Third gas circuit is connect with the 4th valve, and is eventually leading to atmosphere;
The water bath with thermostatic control system includes thermostatic water bath and circulation;The thermostatic water bath includes slot, heating tube, temperature biography
Sensor, humidostat and partition composition;The humidostat is arranged in outside groove body, passes through conducting wire and heating tube and temperature
Sensor connection, and then control temperature;The baffle arrangement separates groove body, the heating in the lower part of groove body, for managing
Pipe, temperature sensor are arranged in below partition, aspect placement control moisture reference can and control moisture measurement on the partition
Tank;The circulation is made of water-circulating pump and circulation line;2 water are separately included in the water bath with thermostatic control system to follow
Ring pump and circulation line, are arranged in groove body two sides deep and superficial part, form uniform and stable bath temperature;
Gas adsorption/desorption test macro of the control moisture includes that two structures are identical, the equal control water of volume size
Divide with reference to tank, control moisture measurement tank, the second valve, third valve, the 5th valve, the 5th Highpressure Tee, high temperature and pressure humidity
Meter, graduated cylinder and conical flask, third high-precision pressure sensor;The control moisture is placed on the clamping plate with reference to tank, described
It controls moisture and connects the second valve, the second valve connection second Highpressure Tee with reference to tank top;The control water
Point test tank is also positioned on the clamping plate, and the control moisture measurement tank and the first gas circuit of the 5th Highpressure Tee connect
It connects, the second gas circuit of the 5th Highpressure Tee is connect with third valve, the third valve and the third Highpressure Tee second
Air circuit connection;The 5th Highpressure Tee third gas circuit is connect with high pressure-temperature hygrometer, the high pressure-temperature hygrometer and institute
The connection of the 5th valve is stated, the 5th valve is connect with the graduated cylinder, and the graduated cylinder is connect with the conical flask;
The control moisture is that two structures are identical with control moisture measurement tank with reference to tank, volume size comparable assay tank body;It closes
It analyzes in the structure composition of the tank body, is analyzed for controlling moisture measurement tank;The control moisture measurement tank includes
Pedestal, saturated salt solution store cavity, limiting device, screen device, coal sample test cavity, tank body sealing cover body, high pressure disengaging
Port, the first sealing ring, the second sealing ring composition;The bottom of the control moisture measurement tank is the pedestal, is placed on described
On clamping plate;The pedestal top is arranged the saturated salt solution and stores cavity;Saturated salt solution storage cavity top setting
Removable filter device is installed in inwardly projecting limiting device, the limiting slot top;The saturated salt solution stores cavity
Top is installed by the first sealing ring;Installation coal sample tests cavity above first sealing ring;The saturated salt solution storage chamber
It is connected by screw bolts between body top and coal sample test cavity;The second sealing ring is installed at the top of the coal sample test cavity,
Tank body sealing cover body is installed in second sealing ring upper end, installs high pressure air inlet/outlet in the middle part of the tank body sealing cover body;It is described
Coal sample test cavity top is connected by screw bolts with tank body sealing cover body.
2. the test method based on claim 1 described device, it is characterised in that: the following steps are included:
(a) sample making;Raw coal is crushed first, then test coal dust is screened using sieve;Especially it shall be noted that by
Sieve is installed in control moisture measurement tank, therefore the mesh number of test coal powder has to be larger than the mesh of sieve in control moisture measurement tank
Number avoids coal dust during test from falling into salting liquid, influences test accuracy;
(2) saturated salt solution is prepared and is placed;According to the experimental condition of quasi- development, suitable inorganic salt particle is selected, it will be certain
The distilled water of temperature and a certain amount of a certain inorganic salt particle mixing, prepare saturation inorganic salt solution, then will be saturated inorganic
Salting liquid pours into control moisture with reference to tank and controls in saturated salt solution storage cavity in moisture measurement tank, and by filter device
It is placed in the top of the tank body, finally tightens the spiral shell between the saturated salt solution storage cavity of test tank and coal sample test cavity
Bolt;
(3) test sample is placed;The coal dust of certain mass is put into control moisture measurement tank coal sample test cavity, moisture is controlled
With reference to not adding test coal sample in tank, and tighten bolt;Then it allows and is placed on water bath with thermostatic control clamping plate with reference to tank and test tank, most
After connect each gas piping;
(4) air-leakage test;All test associated pipes are connected, and the tank body is placed on the clamping plate of thermostatic water bath;It closes
It closes the first valve, the 4th valve and the 5th valve, opens the second valve and third valve, then open high pressure helium gas cylinder and the
One pressure reducing valve is filled with 7MPa or so high-pressure helium into test macro;The first pressure reducing valve, observation high-precision are closed after a period of time
The situation of change of gage pressure;After the completion of gas air tight test, closes high pressure helium gas cylinder and the first pressure reducing valve and open the 4th
Helium in system is discharged valve;
(5) water bath with thermostatic control;Add water in the sink for laying tank body, it is necessary to which flooding test tank completely could stop adding water;Setting
Good bath temperature, and start water circulating pump;
(6) vacuum outgas;Set temperature is reached after a certain period of time to bath temperature, closes the 4th valve, is opened the first valve, is opened
Vacuum pump is opened, system is vacuumized;When vacuum degree reaches 4.0Pa or less, evacuated state certain time is still kept;
(7) high pressure helium gas cylinder and the first pressure reducing valve are opened, closes high-pressure helium after the helium of about 3MPa is slowly filled with to reference tank
Bottle and the first pressure reducing valve record the reading of third high-precision pressure gauge, then slowly open third valve, gas is made to enter coal sample
Tank records after the stable reading of high-precision pressure gauge again, calculates the free volume of coal sample tank;
(8) the 4th valve is opened, the helium in pilot system is released;It is then shut off the 4th valve, opens the first valve, the second valve
Door and third valve, and open vacuum pump, are vacuumized operation for the second time to pilot system, to vacuum degree reach 4.0Pa with
When lower, still keep evacuated state 3 hours or more;
(9) the first valve and vacuum pump are successively closed, high temperature and pressure humidity sensor monitoring control moisture measurement tank is then utilized
Middle humidity, the time for controlling coal sample adsorption moisture in moisture measurement tank must not be lower than 5 days, ensure the abundant adsorption moisture of coal sample;
(10) third valve is closed, high pressure methane gas cylinder and the second pressure reducing valve is opened, the methane gas of certain pressure is made to enter water
Sub-control system refers to tank, is then shut off high pressure methane gas cylinder and the second pressure reducing valve, and record the number of third high-precision pressure sensor
According to;
(11) third valve is slowly opened, allows moisture control to enter control moisture measurement tank with reference to the methane gas in tank, makes first
Alkane gas is adsorbed with certain moisture coal sample, and after adsorption equilibrium 12 hours and third high-precision pressure sensor data are constant
When, related pressure data are recorded, this is then calculated in turn according to absorption front and back change value of pressure and the volume test value
Methane adsorption amount under adsorption equilibrium pressure condition, is then shut off third valve;
(12) high pressure methane gas cylinder and the second pressure reducing valve are opened, increases adsorbed gas pressure step by step, and be repeated in step
(10) the coal body adsorption gas curve under certain temperature and moisture condition is drawn in~(11);
(13) after completing adsorption test, the second valve is closed, the 5th valve is opened, is closed after releasing a certain amount of methane gas
The 5th valve is closed, the volume of graduated cylinder and conical flask measurement release methane gas is utilized;Then moisture is allowed to control in adsorption tanks simultaneously
Coal sample adsorbed again with gas, adsorption time be not less than 12 hours, and using third high-precision pressure gauge record adsorption equilibrium
Pressure value afterwards;
(14) step (13) are repeated, discharges methane gas in moisture control test tank step by step, obtains certain temperature and damp condition
Under coal body desorb gas curve;
(15) when carrying out the test of next temperature grade, above-mentioned steps (9)~(14) are repeated in, and then obtain certain moisture
With the coal body adsorption/desorption gas curve under condition of different temperatures;
(16) when carrying out the test of next moisture levels, according to required moisture condition, suitable inorganic salt particle is selected, is then weighed
Multiple above-mentioned steps (2)~(15).
3. coal seam with gas High Pressure Absorption/desorption experiment method of controllable moisture according to claim 2, feature exist
In: the suitable inorganic salt particle meets: when testing moisture is 20%, selective chlorination sodium inorganic salt particle.
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