CN103033442A - Gas adsorption and desorption test apparatus - Google Patents

Gas adsorption and desorption test apparatus Download PDF

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Publication number
CN103033442A
CN103033442A CN2012105579242A CN201210557924A CN103033442A CN 103033442 A CN103033442 A CN 103033442A CN 2012105579242 A CN2012105579242 A CN 2012105579242A CN 201210557924 A CN201210557924 A CN 201210557924A CN 103033442 A CN103033442 A CN 103033442A
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valve
coal sample
desorption
sample tank
gas
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CN2012105579242A
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CN103033442B (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

The invention relates to a gas adsorption and desorption test apparatus, which comprises an inflation system, a degassing system, a gas adsorption and desorption system and a temperature control system. The gas adsorption and desorption test apparatus with a simple structure is used for determining the adsorption constant and the ultimate gas desorption quantity of coal, can determine the parameters such as the quantity of lost gas, the drilling cuttings desorption index, the diffusion coefficient and the like under the conditions of different temperature, different pressure, different degree of metamorphism and different particle sizes, and is suitable for a test of particles of coal gas adsorption and desorption laws. The gas adsorption and desorption test apparatus can simulate the underground reservoir environment, can simultaneously conduct gas adsorption and desorption tests of four groups of different particle sizes of cuttings coal samples at different temperatures, can conduct isothermal adsorption tests and gas diffusion tests, and can directly determine the gas adsorption loss amount and the ultimate gas desorption quantity. The gas adsorption and desorption test apparatus can simultaneously conduct multiple groups of gas adsorption and diffusion tests and effectively increase the test efficiency, and the determining 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 that characterizes the coalbed methane reservoir feature, and Obtaining Accurate coal seam gas-bearing capacity and gas pressure are significant for coal bed gas resource exploratory development and coal-mine gas diaster prevention and control.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 that coal sample begins to measure the gas amount of losing during the desorption of mash gas amount from being exposed to, and can't directly record, and can only estimate by coal sample desorption of mash gas rule experimental formula.Because the restriction of field condition, coal-bed gas pressure often can't directly be measured, and generally adopts the Langmuir equation by actual measurement gas bearing capacity Inversion Calculation coal-bed gas pressure, and two absorption constant a, b in the Langmuir equation must draw from the isothermal adsorption test.Therefore, gas adsorption and desorption experiment have realistic meaning.But, also do not have the test unit that can carry out isothermal adsorption and Methane Diffusion at present.

Summary of the invention

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

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 on high-pressure air source and the 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 the vacuum piping by operation valve; The gas adsorption desorption system comprises absorbing unit and desorb unit, absorbing unit comprises gasing tank, coal sample tank and data collecting instrument, gasing tank is provided with the gasing tank operation valve, gauge valve and pressure transducer, the gasing tank operation valve is provided with the gasing tank stop valve, the 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 links to each other with the gasing tank operation valve, pressure transducer links to each other with data collecting instrument, the desorb unit comprises desorption of mash gas velocity determination instrument, the T-valve of high precision gas desorption rate tester and connection desorption of mash gas velocity determination instrument and high precision gas desorption rate tester, the T-valve other end links to each other with coal sample tank operation valve; The gasing tank stop valve links to each other with the 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, be equipped with coal sample tank operation valve, gauge valve and pressure transducer on each coal sample tank, coal sample tank operation valve is provided with coal sample tank stop valve, pressure transducer links to each other with data collecting instrument, it is one group that the first coal sample tank is connected by coal sample tank operation valve separately with the second coal sample tank, and it is one group that the 3rd coal sample tank is connected by coal sample tank operation valve separately with the 4th coal sample tank; Be provided with the absorption T-valve between the coal sample tank stop valve of the first coal sample tank and the gasing tank operation valve, the 3rd coal sample tank links to each other with the 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 link to each other with the high precision gas desorption rate tester with desorption of mash gas velocity determination instrument respectively, and the other two ends of the second T-valve link to each other with the high precision gas desorption rate tester with desorption of mash gas velocity determination instrument respectively.

Described desorption of mash gas velocity determination instrument comprises 2 high range desorption instruments that are of a size of Φ 150mm * 1000mm, and the 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, it is simple in structure, be used for the absorption constant of coal, the mensuration of limit desorption of mash gas amount, can determine the parameters such as loss tolerance, Desorption Index for Drill Cuttings and coefficient of diffusion under different temperatures, different pressures, different rank and the different grain size condition, be fit to the test of particulate coal gas adsorption adsorption law; Can simulate the downhole in reservoir environment, can carry out simultaneously four groups of different grain size chip coal samples in gas adsorption, the desorption experiment of condition of different temperatures, isothermal adsorption test, Methane Diffusion test can be carried out, and desorption of mash gas loss amount and gas limit solution pipette can be directly measured; Can do simultaneously many group gas adsorptions and diffuse experiment, but the Effective Raise conventional efficient is measured precision high.

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

3, the present invention's pressure-bearing pipeline everywhere is high-pressure rubber pipe, can strict pilot piping length, as much as possible reduce the free space of pipeline, and make experimental data more accurate.When carrying out the test chamber volume calibration, must be for satisfying accuracy requirement below the 10Pa according to prior art regulation and stipulation vacuum tightness, yet general degas system is difficult to reach this requirement, degas system of the present invention is used in conjunction with new method when vacuum tightness is not more than 100Pa, also can carry out accurate calibration to system's free space.

4, the desorb unit comprises the desorption of mash gas velocity determination instrument of high range and the high precision gas desorption rate tester of down scale, when doing desorb mensuration, the gas pressure Fast-Balance is measured with desorption of mash gas velocity determination instrument to the gas flow in atmospheric pressure period, gas pressure equilibrates to atmospheric pressure and measures with the high precision gas desorption rate tester later period, can avoid the dead space free gas to discharge fast the enormous impact that brings to the high precision gas desorption rate tester in the desorb starting stage, can eliminate again the impact of dead space free gas, convenient definite desorb zero-time, process for desorption data is processed, set up corresponding adsorption law model, calculate more accurately the gas loss amount.

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

Description of drawings

Fig. 1 is structural representation of the present invention.

Embodiment

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

Gas charging system comprises the gas pressure reducer 22 on high-pressure air source 19 and the high-pressure air source 19.High-pressure air source 19 be by the concentration that helium general gas companies in Beijing is produced be 99.999%, pressure is the high-purity methane gas cylinder of 13.6Mpa, gas pressure reducer 22 with gas regulation to the required pressure of experiment, thereby provide the constant voltage source of the gas for the gas adsorption desorption system.

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, the bottom is provided with operation valve 23, be connected to vacuum piping 13 tops after compound vacuum gauge 8 and vacuum gauge 12 series connection, 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.

The gas adsorption desorption system comprises absorbing unit and desorb unit, and absorbing unit comprises gasing tank 18, the first coal sample tank 9, the second coal sample tank 92, the 3rd coal sample tank 93, the 4th coal sample tank 94 and data collecting instrument 6.Be provided with gasing tank operation valve 17, gauge valve 16 and pressure transducer 21 at gasing tank 18, gasing tank operation valve 17 right-hand members are provided with gasing tank stop valve 24, and gasing tank stop valve 24 links to each other 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 ends are 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 ends are 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 members are 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 ends are provided with coal sample tank stop valve 114.Pressure transducer 21, pressure transducer 26, pressure transducer 262, pressure transducer 263 and pressure transducer 264 all are connected on the data collecting instrument 6, can read in real time the gaseous tension numerical value in each tank body.It is one group that the 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.Being provided with absorption T-valve 20, the three coal sample tanks 93 between the coal sample tank stop valve 11 of the first coal sample tank 9 and the gasing tank operation valve 17 links to each other with this absorption T-valve 20 by coal sample tank stop valve 113.Be connected with on the coal sample tank stop valve 112 of the second coal sample tank 92 and be connected with the second T-valve 3, the first T-valve 27 on the coal sample tank stop valve 114 of the first T-valve 27, the 4th coal sample tank 94 and the second T-valve 3 is the glass three-way valve.The desorb unit comprises desorption of mash gas velocity determination instrument 2 and high precision gas desorption rate tester 1, desorption of mash gas velocity determination instrument 2 comprises 2 high range desorption instruments that 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, the gas pressure Fast-Balance is measured with desorption of mash gas velocity determination instrument 2 to the gas flow in atmospheric pressure period, and gas pressure equilibrates to atmospheric pressure and measures with high precision gas desorption rate tester 1 later period.The first T-valve 27 all the other two ends link to each other with high precision gas desorption rate tester 1 with desorption of mash gas velocity determination instrument 2 from left end respectively, the second T-valve 3 all the other two ends link to each other with high precision gas desorption rate tester 1 with desorption of mash gas velocity determination instrument 2 from right-hand member respectively, realize that by regulating the first T-valve 27 and the second T-valve 3 switching of desorb unit is used.

Temperature control system comprises water bath with thermostatic control 7 and water bath with thermostatic control 7 coconnected thermostats 4, 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 experimental provision is put into water bath with thermostatic control 7, controls whole experimental situation temperature by regulating water temperature.The temperature regulating range of temperature control system is that-10 ℃～90 ℃, temperature changing speed are that 2min/ ℃, temperature control precision are ± 0.05 ℃.

In the present invention, data collecting instrument 6 mainly is by gaseous tension and atmospheric pressure in the temperature of computer-automatic collection water bath with thermostatic control 7, environment temperature, vacuum tightness, the 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 is all set two-layer O-ring seal to guarantee the tank body sealing with gasing tank 18; Pressure-bearing pipeline everywhere is high-pressure rubber pipe, and the high-pressure rubber pipe internal diameter is 4mm, the gaseous tension of anti-64MPa, can reduce the volume of free space and improve the security of testing; Stop valve and operation valve be the gaseous tension of anti-16MPa all.

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

(1) prepares before the experiment

Deliver to the laboratory after the fresh coal sample of choosing getting working face tightly encapsulates, fresh coal sample is pulverized, is sieved into required granularity, choose respectively the coal sample of corresponding granularity and carry 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; With coal sample oven dry, the oven dry coal sample that takes by weighing certain mass is packed in the 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, close gauge valve 16 and gauge valve 25, open vacuum pump 15 degassed, until vacuum gauge pressure shows that 20Pa can close vacuum pump 15 more than three hours; Carrying out stereometry and the residual volume of coal sample tank 9 measures; System and desorption of mash gas velocity determination instrument 2 are connected, read the initial liquid level h of graduated cylinder 1At last, open vacuum valve air is entered in tested coal sample tank 9 and the pipeline thereof, the interior liquid level of graduated cylinder this moment rises to h 2, h 2-h 1Volume be the volume of tested coal sample tank 9 and pipeline thereof, simultaneously atmospheric pressure, indoor temperature, water temperature in the recording room are 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, need coal sample tank 9 is carried out tonifying Qi, when force value is higher than predetermined value, then need coal sample tank 9 is exitted, repeatable operation like this, until continuous 3 hours readings of tensimeter are constant and adsorption time greater than 8h, think that then absorption has reached balance, the record related data; Repeat above-mentioned steps, obtain at least eight groups of data under the different pressures condition, can be calculated absorption constant a, b value by Data Management Analysis.

(4) desorption experiment

In adsorption test, after each adsorption equilibrium, carry out the Methane Diffusion test.After the coal sample tank 9 after the adsorption equilibrium and 1 connection of high precision gas desorption rate tester, measure the Changing Pattern of temporal evolution desorption rate and accumulative total gas desorption amount.Measure when just having begun, read number one time every 1min, in time prolongation behind the 20min, the gas desorption amount reduces, reading interval proper extension, the total test duration is 120min; Simultaneously, recording laboratory atmospheric temperature, desorption instrument tank temperature and atmospheric pressure are so that Data correction.Gas limit solution pipette equals adsorbance under this temperature and the pressure condition and deducts adsorbance under desorption temperature and the pressure condition under different temperatures, the pressure condition.Because it is large just to have begun desorption quantity, measure with desorption of mash gas velocity determination instrument 2; When the gas desorption amount reduces, then use high precision gas desorption rate tester 1 instead and measure.

(5) experiment finishes

The arrangement experimental record, the analytical calculation experimental data.

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

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

Claims (3)

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 on high-pressure air source and the 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 the vacuum piping by operation valve; The gas adsorption desorption system comprises absorbing unit and desorb unit, absorbing unit comprises gasing tank, coal sample tank and data collecting instrument, gasing tank is provided with the gasing tank operation valve, gauge valve and pressure transducer, the gasing tank operation valve is provided with the gasing tank stop valve, the 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 links to each other with the gasing tank operation valve, pressure transducer links to each other with data collecting instrument, the desorb unit comprises desorption of mash gas velocity determination instrument, the T-valve of high precision gas desorption rate tester and connection desorption of mash gas velocity determination instrument and high precision gas desorption rate tester, the T-valve other end links to each other with coal sample tank operation valve; The gasing tank stop valve links to each other with the 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.
2. gas adsorption test device for desorption as claimed in claim 1, it is characterized in that, 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, be equipped with coal sample tank operation valve, gauge valve and pressure transducer on each coal sample tank, coal sample tank operation valve is provided with coal sample tank stop valve, pressure transducer links to each other with data collecting instrument, it is one group that the first coal sample tank is connected by coal sample tank operation valve separately with the second coal sample tank, and it is one group that the 3rd coal sample tank is connected by coal sample tank operation valve separately with the 4th coal sample tank; Be provided with the absorption T-valve between the coal sample tank stop valve of the first coal sample tank and the gasing tank operation valve, the 3rd coal sample tank links to each other with the 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 link to each other with the high precision gas desorption rate tester with desorption of mash gas velocity determination instrument respectively, and the other two ends of the second T-valve link to each other with the high precision gas desorption rate tester with desorption of mash gas velocity determination instrument respectively.
3. gas adsorption test device for desorption as claimed in claim 1 or 2, it is characterized in that, described desorption of mash gas velocity determination instrument comprises 2 high range desorption instruments that are of a size of Φ 150mm * 1000mm, and the high precision gas desorption rate tester comprises the down scale desorption instrument that 6 minimum scales are 2ml.
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