CN103033442B - A kind of gas adsorption test device for desorption - Google Patents

A kind of gas adsorption test device for desorption Download PDF

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Publication number
CN103033442B
CN103033442B CN201210557924.2A CN201210557924A CN103033442B CN 103033442 B CN103033442 B CN 103033442B CN 201210557924 A CN201210557924 A CN 201210557924A CN 103033442 B CN103033442 B CN 103033442B
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valve
coal sample
desorption
gas
sample tank
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CN201210557924.2A
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CN103033442A (en
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魏建平
王云刚
李波
鄢桂云
吴松刚
秦恒洁
李盟
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河南理工大学
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Abstract

A kind of gas adsorption test device for desorption, comprises gas charging system, degas system, gas adsorption desorption system and temperature control system.Structure of the present invention is simple, for the absorption constant of coal, the mensuration of limit desorption of mash gas amount, the parameters such as loss tolerance, Desorption Index for Drill Cuttings and the coefficient of diffusion under different temperatures, different pressures, different rank and different grain size condition can be determined, be applicable to the test of particulate coal gas adsorption adsorption law; Can reservoir environment under simulation well, gas adsorption, the desorption experiment of four groups of different grain size chip coal samples in condition of different temperatures can be carried out simultaneously, isothermal adsorption test, Methane Diffusion test can be carried out, and directly can measure desorption of mash gas loss amount and gas limit solution pipette; Can do many group gas adsorptions simultaneously and diffuse experiment, effectively can improve conventional efficient, estimating precision is high.

Description

A kind of gas adsorption test device for desorption

Technical field

The invention belongs to Experiments on Gas device technique field, particularly a kind of gas adsorption test device for desorption.

Background technology

Coal seam gas-bearing capacity and gas pressure are the crucial reservoir parameters characterizing coalbed methane reservoir feature, Obtaining Accurate coal seam gas-bearing capacity and gas pressure for coal bed gas resource exploratory development and coal-mine gas diaster prevention and control significant.According to coal seam gas-bearing capacity down-hole Direct Determination (GBT23250-2009) and survey coal seam gas-bearing capacity assay method in period (GB/T23249-2009), coal seam gas-bearing capacity equals stripping gas content, residual gas content and loss Gas content three sum.Stripping gas content and residual gas content are directly surveyed by desorption experiment; Loss Gas content is the gas amount lost during coal sample measures desorption of mash gas amount from being exposed to, directly cannot record, can only be estimated by coal sample desorption of mash gas rule experimental formula.Due to the restriction of field condition, coal-bed gas pressure often cannot directly measure, and generally adopts Langmuir equation by surveying gas bearing capacity Inversion Calculation coal-bed gas pressure, and two absorption constants a, b in Langmuir equation must draw from isothermal adsorption test.Therefore, gas adsorption and desorption experiment have realistic meaning.But, also there is not the test unit that can carry out isothermal adsorption and Methane Diffusion at present.

Summary of the invention

The invention provides a kind of structure simple, isothermal gas adsorption-diffuse experiment, experimental data is accurate and conventional efficient is high gas adsorption test device for desorption can be carried out.

For achieving the above object, technical scheme of the present invention is: a kind of gas adsorption test device for desorption, comprises gas charging system, degas system, gas adsorption desorption system and temperature control system, gas charging system comprises the gas pressure reducer in high-pressure air source and high-pressure air source, degas system comprises vacuum pump, compound vacuum gauge, vacuum gauge and vacuum piping, and vacuum tube is fastened and is provided with operation valve and vacuum suction operation valve, and compound vacuum gauge and vacuum gauge are connected on vacuum tube and fasten, and vacuum pump is connected with vacuum piping by operation valve, gas adsorption desorption system comprises absorbing unit and desorption unit, absorbing unit comprises gasing tank, coal sample tank and data collecting instrument, gasing tank is provided with gasing tank operation valve, gauge valve and pressure transducer, gasing tank operation valve is provided with gasing tank stop valve, coal sample tank is provided with coal sample tank operation valve, gauge valve and pressure transducer, coal sample tank operation valve is provided with coal sample tank stop valve, coal sample tank stop valve is connected with gasing tank operation valve, pressure transducer is connected with data collecting instrument, desorption unit comprises desorption of mash gas speed determinator, high precision gas desorption rate tester and the T-valve being communicated with desorption of mash gas speed determinator and high precision gas desorption rate tester, the T-valve other end is connected with coal sample tank operation valve, gasing tank stop valve is connected with vacuum suction operation valve with gas pressure reducer by T-valve, temperature control system comprises water bath with thermostatic control and the coconnected thermostat of water bath with thermostatic control, and absorbing unit is positioned at water bath with thermostatic control.

Described coal sample tank is four, be respectively the first coal sample tank, the second coal sample tank, the 3rd coal sample tank and the 4th coal sample tank, each coal sample tank is equipped with coal sample tank operation valve, gauge valve and pressure transducer, coal sample tank operation valve is provided with coal sample tank stop valve, pressure transducer is connected with data collecting instrument, it is one group that first coal sample tank is connected by respective coal sample tank operation valve with the second coal sample tank, and it is one group that the 3rd coal sample tank is connected by respective coal sample tank operation valve with the 4th coal sample tank; Be provided with absorption T-valve between the coal sample tank stop valve of the first coal sample tank and gasing tank operation valve, the 3rd coal sample tank is connected with absorption T-valve by coal sample tank stop valve; The coal sample tank stop valve of the second coal sample tank is provided with the first T-valve, the coal sample tank stop valve of the 4th coal sample tank is provided with the second T-valve, the other two ends of the first T-valve are connected with high precision gas desorption rate tester with desorption of mash gas speed determinator respectively, and the other two ends of the second T-valve are connected with high precision gas desorption rate tester with desorption of mash gas speed determinator respectively.

Described desorption of mash gas speed determinator comprises the high range desorption instrument that 2 are of a size of Φ 150mm × 1000mm, and high precision gas desorption rate tester comprises the down scale desorption instrument that 6 minimum scales are 2ml.

Compared with prior art, advantage of the present invention is:

1, the present invention includes gas charging system, degas system, gas adsorption desorption system and temperature control system, its structure is simple, for the absorption constant of coal, the mensuration of limit desorption of mash gas amount, the parameters such as loss tolerance, Desorption Index for Drill Cuttings and the coefficient of diffusion under different temperatures, different pressures, different rank and different grain size condition can be determined, be applicable to the test of particulate coal gas adsorption adsorption law; Can reservoir environment under simulation well, gas adsorption, the desorption experiment of four groups of different grain size chip coal samples in condition of different temperatures can be carried out simultaneously, isothermal adsorption test, Methane Diffusion test can be carried out, and directly can measure desorption of mash gas loss amount and gas limit solution pipette; Can do many group gas adsorptions simultaneously and diffuse experiment, effectively can improve conventional efficient, estimating precision is high.

2, water bath with thermostatic control of the present invention and thermostat can make system temperature constant, get rid of the interference that gas source temperature is different, coal sample gas adsorption desorption process is carried out at the same temperature, can realize integrality and the continuity of experiment.

3, the present invention's pressure-bearing pipeline is everywhere high-pressure rubber pipe, can strict pilot piping length, as much as possible reduces the free space of pipeline, makes experimental data more accurate.When carrying out test chamber volume calibration, accuracy requirement must could be met for below 10Pa according to prior art specification specified vacuum degree, but general degas system is difficult to reach this requirement, degas system of the present invention when vacuum tightness is not more than 100Pa, also can carry out accurate calibration to system free space with the use of new method.

4, desorption unit comprises the desorption of mash gas speed determinator of high range and the high precision gas desorption rate tester of down scale, when doing desorb and measuring, gas pressure Fast-Balance measures to the gas flow desorption of mash gas speed determinator in atmospheric pressure period, gas pressure equilibrates to atmospheric pressure and measures with high precision gas desorption rate tester later period, dead space free gas can be avoided to discharge the enormous impact brought to high precision gas desorption rate tester fast in the desorb starting stage, the impact of dead space free gas can be eliminated again, conveniently determine desorb initial time, passing through of desorption data is processed, set up corresponding adsorption law model, calculate gas loss amount more accurately.

5, the data of data collecting instrument of the present invention to required collection are computer-automatic collection except desorption quantity, and can reduce the error of artificial reading, acquisition precision is high, can improve experiment accuracy rate and efficiency.

Accompanying drawing explanation

Fig. 1 is structural representation of the present invention.

Embodiment

Gas adsorption test device for desorption as shown in Figure 1, it comprises the gas charging system, degas system, gas adsorption desorption system and the temperature control system that are connected by pipeline.

Gas charging system comprises the gas pressure reducer 22 in high-pressure air source 19 and high-pressure air source 19.High-pressure air source 19 is high-purity methane gas cylinders that the concentration of being produced by the general gas companies of Beijing helium is 99.999%, pressure is 13.6Mpa, and gas regulation to the pressure needed for testing, thus is provided constant voltage source of the gas for gas adsorption desorption system by gas pressure reducer 22.

Degas system comprises vacuum pump 15, compound vacuum gauge 8, vacuum gauge 12 and vacuum piping 13, be provided with vacuum suction operation valve 14 on the top of vacuum piping 13, bottom is provided with operation valve 23, compound vacuum gauge 8 and vacuum gauge 12 are connected to vacuum piping 13 top after connecting, and vacuum pump 15 is connected with vacuum piping 13 by operation valve 23.The measurement range of compound vacuum gauge 8 is 1.0 × 10 5~ 1.0 × 10 -5pa, control accuracy be≤± 1%.Vacuum pump 15 is Double-stage rotary vane vacuum pump.

Gas adsorption desorption system comprises absorbing unit and desorption unit, and absorbing unit comprises gasing tank 18, first coal sample tank 9, second coal sample tank 92, the 3rd coal sample tank 93, the 4th coal sample tank 94 and data collecting instrument 6.Gasing tank 18 is provided with gasing tank operation valve 17, gauge valve 16 and pressure transducer 21, and gasing tank operation valve 17 right-hand member is provided with gasing tank stop valve 24, and gasing tank stop valve 24 is connected with vacuum suction operation valve 14 with gas pressure reducer 22 by T-valve 28.Coal sample tank 9 is provided with coal sample tank operation valve 5, gauge valve 25 and pressure transducer 26, and coal sample tank operation valve 5 one end is provided with coal sample tank stop valve 11; Coal sample tank 92 is provided with coal sample tank operation valve 52, gauge valve 252 and pressure transducer 262, and coal sample tank operation valve 52 left end is provided with coal sample tank stop valve 112; Coal sample tank 93 is provided with coal sample tank operation valve 53, gauge valve 253 and pressure transducer 263, and coal sample tank operation valve 53 right-hand member is provided with coal sample tank stop valve 113; Coal sample tank 94 is provided with coal sample tank operation valve 54, gauge valve 254 and pressure transducer 264, and coal sample tank operation valve 54 left end is provided with coal sample tank stop valve 114.Pressure transducer 21, pressure transducer 26, pressure transducer 262, pressure transducer 263 and pressure transducer 264 are all connected on data collecting instrument 6, can read the gaseous tension numerical value in each tank body in real time.It is one group that first coal sample tank 9 is connected by coal sample tank operation valve 5 and coal sample tank operation valve 52 with the second coal sample tank 92, and it is one group that the 3rd coal sample tank 93 is connected by coal sample tank operation valve 53 and coal sample tank operation valve 54 with the 4th coal sample tank 94.Be provided with between the coal sample tank stop valve 11 of the first coal sample tank 9 and gasing tank operation valve 17 and adsorb T-valve 20, the 3rd coal sample tank 93 is connected with this absorption T-valve 20 by coal sample tank stop valve 113.The coal sample tank stop valve 114 coal sample tank stop valve 112 of the second coal sample tank 92 being connected with the first T-valve 27, the 4th coal sample tank 94 is connected with the second T-valve 3, first T-valve 27 and the second T-valve 3 is glass three-way valve.Desorption unit comprises desorption of mash gas speed determinator 2 and high precision gas desorption rate tester 1, desorption of mash gas speed determinator 2 comprises the high range desorption instrument that 2 are of a size of Φ 150mm × 1000mm, high precision gas desorption rate tester 1 comprises the down scale desorption instrument that 6 minimum scales are 2ml, gas pressure Fast-Balance measures to the gas flow desorption of mash gas speed determinator 2 in atmospheric pressure period, and gas pressure equilibrates to atmospheric pressure and measures with high precision gas desorption rate tester 1 later period.First all the other two ends of T-valve 27 are connected with high precision gas desorption rate tester 1 from left end with desorption of mash gas speed determinator 2 respectively, second all the other two ends of T-valve 3 are connected with high precision gas desorption rate tester 1 from right-hand member with desorption of mash gas speed determinator 2 respectively, are used by the switching regulating the first T-valve 27 and the second T-valve 3 to realize desorption unit.

Temperature control system comprises water bath with thermostatic control 7 and the coconnected thermostat 4 of water bath with thermostatic control 7, absorbing unit is positioned at water bath with thermostatic control 7, namely gasing tank 18 and on gasing tank operation valve 17, gauge valve 16 and pressure transducer 21,4 coal sample tanks 9 and on coal sample tank operation valve 5, gauge valve 25 be positioned at water bath with thermostatic control 7 with pressure transducer 26, data collecting instrument 6 and gasing tank stop valve 24, T-valve 20 and T-valve 28.Water bath with thermostatic control 7 is a large-scale automatic constant-temperature water-bath, and water bath with thermostatic control 7 put into by experimental provision, controls whole experimental situation temperature by regulating water temperature.The temperature regulating range of temperature control system is-10 DEG C ~ 90 DEG C, temperature changing speed is 2min/ DEG C, temperature control precision is ± 0.05 DEG C.

In the present invention, data collecting instrument 6 is mainly by gaseous tension and atmospheric pressure in the temperature of computer-automatic collection water bath with thermostatic control 7, environment temperature, vacuum tightness, tank body.

In the present embodiment, coal sample tank 9 is of a size of Φ 50mm × 100mm, and the volume of gasing tank 18 is 2000ml, and coal sample tank 9 and gasing tank 18 all set two-layer O-ring seal to ensure tank body sealing; Pressure-bearing pipeline is everywhere high-pressure rubber pipe, and high-pressure rubber pipe internal diameter is 4mm, the gaseous tension of resistance to 64MPa, can reduce the volume of free space and improve the security of experiment; Stop valve and operation valve all gaseous tensions of resistance to 16MPa.

The step that the present invention carries out the experiment of gas adsorption adsorption law is as follows:

(1) prepare before experiment

Deliver to laboratory after the fresh coal sample choosing getting working face tightly encapsulates, fresh coal sample pulverized, be sieved into required granularity, the coal sample choosing corresponding granularity respectively carries out the isoparametric mensuration of technical analysis, real density and pseudodensity.

(2) experimental provision detects debugging

Testing fixture is reliable to guarantee that system connects, and uses N 2the impermeability of testing fixture; Coal sample dried, the oven dry coal sample taking certain mass loads in coal sample tank 9; Then, opening coal sample tank operation valve 5, coal sample tank stop valve 11, vacuum suction operation valve 14 and gasing tank operation valve 17, vacuum gauge pressure display 20Pa closes gauge valve 16 and gauge valve 25, opens vacuum pump 15 degassed, until can close vacuum pump 15 in more than tri-hours; The stereometry and the residual volume that carry out coal sample tank 9 measure; System and desorption of mash gas speed determinator 2 are connected, reads graduated cylinder initial liquid height h 1; Finally, open vacuum valve and air is entered in tested coal sample tank 9 and pipeline thereof, now in graduated cylinder, liquid level rises to h 2, h 2-h 1volume be the volume of tested coal sample tank 9 and pipeline thereof, atmospheric pressure, indoor temperature, water temperature in recording room simultaneously, so that correction data.

(3) adsorption experiment

The temperature of water bath with thermostatic control 7 is transferred to predetermined value, is filled with a certain amount of gas to gasing tank 18, the force value after record is stable; Then, successively coal sample tank 9 is inflated, when force value is lower than predetermined value, tonifying Qi need be carried out to coal sample tank 9, when force value is higher than predetermined value, then need to exit to coal sample tank 9, repeatable operation like this, until tensimeter continuous 3 hours readings are constant and adsorption time is greater than 8h, then think that absorption reaches balance, record related data; Repeat above-mentioned steps, at least obtain the data under eight groups of different pressures conditions, can be calculated absorption constant a, b value by Data Management Analysis.

(4) desorption experiment

In adsorption test, after each adsorption equilibrium, carry out Methane Diffusion test.After being connected with high precision gas desorption rate tester 1 by coal sample tank 9 after adsorption equilibrium, measure the Changing Pattern changing desorption rate and accumulative gas desorption amount in time.Measure when just starting, read a number every 1min, prolongation in time after 20min, gas desorption amount reduces, reading time interval proper extension, and the total test duration is 120min; Meanwhile, recording laboratory atmospheric temperature, desorption instrument tank temperature and atmospheric pressure are so that Data correction.Under different temperatures, pressure condition, the gas limit solution pipette adsorbance equaled under this temperature and pressure condition deducts the adsorbance under desorption temperature and pressure condition.Large owing to just starting desorption quantity, measure with desorption of mash gas speed determinator 2; When gas desorption amount reduces, then use high precision gas desorption rate tester 1 instead and measure.

(5) experiment terminates

Arrange experimental record, analytical calculation experimental data.

In step (2), in order to ensure the accuracy of experimental apparatus volume calibration, repeated test 5 times, gets its mean value.

Be not limited to above-mentioned embodiment, the present invention can be fixed on support, the present invention be positioned in water bath with thermostatic control 7 together with support, and support is connected with jacking gear.

Claims (2)

1. a gas adsorption test device for desorption, is characterized in that, comprises gas charging system, degas system, gas adsorption desorption system and temperature control system, gas charging system comprises the gas pressure reducer in high-pressure air source and high-pressure air source, degas system comprises vacuum pump, compound vacuum gauge, vacuum gauge and vacuum piping, and vacuum tube is fastened and is provided with operation valve and vacuum suction operation valve, and compound vacuum gauge and vacuum gauge are connected on vacuum tube and fasten, and vacuum pump is connected with vacuum piping by operation valve, gas adsorption desorption system comprises absorbing unit and desorption unit, absorbing unit comprises gasing tank, coal sample tank and data collecting instrument, gasing tank is provided with gasing tank operation valve, gauge valve and pressure transducer, gasing tank operation valve is provided with gasing tank stop valve, coal sample tank is provided with coal sample tank operation valve, gauge valve and pressure transducer, coal sample tank operation valve is provided with coal sample tank stop valve, coal sample tank stop valve is connected with gasing tank operation valve, pressure transducer is connected with data collecting instrument, desorption unit comprises desorption of mash gas speed determinator, high precision gas desorption rate tester and the T-valve being communicated with desorption of mash gas speed determinator and high precision gas desorption rate tester, the T-valve other end is connected with coal sample tank operation valve, gasing tank stop valve is connected with vacuum suction operation valve with gas pressure reducer by T-valve, temperature control system comprises water bath with thermostatic control and the coconnected thermostat of water bath with thermostatic control, and absorbing unit is positioned at water bath with thermostatic control,
described coal sample tank is fourbe respectively the first coal sample tank, the second coal sample tank, the 3rd coal sample tank and the 4th coal sample tank, each coal sample tank is equipped with coal sample tank operation valve, gauge valve and pressure transducer, coal sample tank operation valve is provided with coal sample tank stop valve, pressure transducer is connected with data collecting instrument, it is one group that first coal sample tank is connected by respective coal sample tank operation valve with the second coal sample tank, and it is one group that the 3rd coal sample tank is connected by respective coal sample tank operation valve with the 4th coal sample tank; Be provided with absorption T-valve between the coal sample tank stop valve of the first coal sample tank and gasing tank operation valve, the 3rd coal sample tank is connected with absorption T-valve by coal sample tank stop valve; The coal sample tank stop valve of the second coal sample tank is provided with the first T-valve, the coal sample tank stop valve of the 4th coal sample tank is provided with the second T-valve, the other two ends of the first T-valve are connected with high precision gas desorption rate tester with desorption of mash gas speed determinator respectively, and the other two ends of the second T-valve are connected with high precision gas desorption rate tester with desorption of mash gas speed determinator respectively.
2. gas adsorption test device for desorption as claimed in claim 1, it is characterized in that, described desorption of mash gas speed determinator comprises the high range desorption instrument that 2 are of a size of Φ 150mm × 1000mm, and high precision gas desorption rate tester comprises the down scale desorption instrument that 6 minimum scales are 2ml.
CN201210557924.2A 2012-12-20 2012-12-20 A kind of gas adsorption test device for desorption CN103033442B (en)

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