CN103439226A - Device and method for measuring diffusion coefficient of adsorbent gas in coal shale in magnetic suspension manner - Google Patents

Device and method for measuring diffusion coefficient of adsorbent gas in coal shale in magnetic suspension manner Download PDF

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CN103439226A
CN103439226A CN2013103941676A CN201310394167A CN103439226A CN 103439226 A CN103439226 A CN 103439226A CN 2013103941676 A CN2013103941676 A CN 2013103941676A CN 201310394167 A CN201310394167 A CN 201310394167A CN 103439226 A CN103439226 A CN 103439226A
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gas
danks
sample
diffusion
laboratory module
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蔡益栋
刘大锰
姚艳斌
陈杨
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China University of Geosciences
China University of Geosciences Beijing
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Abstract

The invention discloses a device and a method for measuring a diffusion coefficient of adsorbent gas in coal shale in a magnetic suspension manner. The device comprises a cabin body and a computer control system arranged outside the cabin body, wherein the cabin body is divided through a baffle into a microbalance measurement system and an experiment cabin which are independent from each other; the microbalance measurement system is arranged above the experiment cabin; the experiment cabin and the microbalance measurement system are independent from each other, and a sample can be suspended in the experiment cabin, so that the gas in the experiment cabin can be in full contact with a coal shale substrate and then effectively diffuses. Therefore, according to the technical scheme disclosed by the invention, a coal shale block which is completely the same as an underground rock stratum can be used as the sample for detection; the original characteristic of the sample is retained, and the phenomenon of an inaccurate experiment result caused by an experiment apparatus can be avoided. A diffusion coefficient detection result obtained by the method disclosed by the invention is closer to the diffusion coefficient of the gas under the underground rock stratum state. According to the device disclosed by the invention, the diffusion coefficient of the gas in the coal shale substrate can be precisely obtained.

Description

The device and method of absorbing gas coefficient of diffusion in danks is measured in magnetic levitation
Technical field
The present invention relates to a kind of device and method of measuring adsorbed gas coefficient of diffusion in danks.Belong to gas development technique field in danks.
Background technology
Coal-seam gas (or shale gas), refer to compose exist in coal (page) rock take methane as principal ingredient, take be adsorbed on the matrix granule surface as main, partly be free in hole or be dissolved in the hydrocarbon gas in the water of rock stratum.
Coal-seam gas (or shale gas) has following characteristics: 1., substantially not containing the heavy hydrocarbon more than C2, there is no inorganic impurity during output; If 2., in Main Underground is present in danks with the adsorbed state of macromolecular mass, possess production capacity basis preferably; 3. coal-bed gas exploitation is to reduce reservoir pressure by draining, makes coal-seam gas desorb-diffusion in the coal seam-extraction of flowing, and conventional gas is the pressure output by self; 4. the coal-seam gas initial production yields poorly, but the cycle is long, can reach many decades, and the rock gas initial potential is high, and the production cycle often is less than 10 years; 4. coal-seam gas claims again coal-mine gas, is the chief threat of coal mine production safety, and the greenhouse effect of its generation simultaneously are than CO 2by force.
Therefore, exploiting coal bed methane is conducive to: at first, reduce mine safety accidents; Secondly, can play environmental protection effect; Again, can produce good economic benefit.
Before coal-seam gas (or shale gas) is exploited, need to first see clearly its migration rule in danks, diffusion is the link that must experience in the coal bed gas product process.The output of coal-seam gas certainly will be through the process of desorb-diffusion-seepage flow, and the height of methane output is subject to the co-controlling of these three links.After reservoir pressure drops to critical desorption pressures, coal-seam gas just desorbs from the coal internal pore surface.Because microporosity that diameter is less than 10nm be take as main in the matrix of coal mesoporosity, permeability is extremely low, and at first coal-seam gas is diffused into could the seepage flow output in perviousness crack or hugger.Gas is deferred to Darcy's law seepage flow after entering the perviousness crack, and gas yield is the function of pressure and permeability.As can be seen here, diffusion plays important linking effect in the desorb output process of coal-seam gas.The motion that the essence of diffusion is gas from macromolecule density region (matrix of coal) to low molecular density district (perviousness crack), rate of propagation and gas molecule diffusion length are the inverse ratio that square is of fracture spacing.The early yield of diffusion major effect coal bed gas well and the stable production period in later stage thereof.
Actual coal-seam gas (or shale gas) diffusion process can be described by Fick's second law, as equation (1):
(1)
Figure 2013103941676100002DEST_PATH_IMAGE002
In formula (1), the concentration that C is coal-seam gas (or shale gas); T is the time; X, y, z is volume coordinate, and D is coal-seam gas (or shale gas) coefficient of diffusion, and it shows the gas diffusivity.The degree of accuracy of coefficient of diffusion reflects the awareness of the mankind to coal-seam gas (or shale gas) migration process, has also reflected the development ability of coal-seam gas (or shale gas).Therefore, need effectively accurately to determine coal-seam gas (or shale gas) diffusion coefficient D.
Prior art is determined coal-seam gas (or shale gas) coefficient of diffusion in matrix, that the pulverized particles sample is placed in to sealing diffusion vessel, inject wherein coal-seam gas (or shale gas), when gas starts to diffuse in sample, the atmospheric pressure value in the diffusion vessel descends again.Utilize monitoring instrument to record its air pressure dynamic change value, when saturated (adsorb) can be calculated by Fick's second law the coefficient of diffusion of gas when diffusion during in equilibrium state.
But this technology has been destroyed the distinctive space structure of danks itself, cause the result of detection and the coefficient of diffusion of actual danks matrix to differ larger; A kind of technology is separately arranged, and it has preserved danks primary sample space structure, but the space leakproofness of its instrument is unstable, is difficult to reach the requirement of the diffusion of Accurate Measurement.
Summary of the invention
The technical issues that need to address of the present invention just are to overcome the defect of prior art, provide a kind of magnetic levitation to measure the device and method of absorbing gas coefficient of diffusion in danks, utilize device of the present invention can accurately obtain the coefficient of diffusion of gas in danks matrix, it is more more effective than existing apparatus; Can obtain the coefficient of diffusion of coal-seam gas/shale gas in danks by method of the present invention, than art methods, more approach actual value.
For addressing the above problem, the present invention adopts following technical scheme:
The invention provides a kind of magnetic levitation and measure the device of absorbing gas coefficient of diffusion in danks, described device comprises a cabin body, the external computer control system with being installed on cabin, described cabin body is separate micro-balance measurement system and Laboratory Module by a baffle for separating, and micro-balance measurement system is arranged at the Laboratory Module top;
Described micro-balance measurement system comprises the electromagnet be arranged in the body of micro-balance measurement system cabin, and is connected, is installed on micro-balance of body top, cabin with electromagnet; Electromagnet is connected with computer control system respectively with micro-balance;
Described Laboratory Module comprises the measurement charger that is installed on the Laboratory Module middle part and is hung on the sample bin of measuring the charger below, in described sample bin, sample is installed, measure the charger top and be provided with permanent magnet, permanent magnet is connected with the measurement charger by a location sensitive core, Laboratory Module bulkhead corresponding to the location sensitive core is provided with the location sensitive coil, the Laboratory Module upper and lower is respectively arranged with and the extraneous pipeline communicated, be respectively arranged with gas control valve on pipeline, the pipeline Bonding pressure control system of below; Be provided with pressure inductor in Laboratory Module, pressure inductor and location sensitive coil are connected with computer control system respectively.
The whole cabin body of described device is installed in a calibration cell, and described calibration cell is provided with temperature inductor, and described temperature inductor is connected with computer control system.
Described measurement charger comprises the support be installed on the Laboratory Module bulkhead, and a draw-in groove is installed on support, and a snap ring is installed in draw-in groove, and by snap ring link position induction core, the draw-in groove below is equipped with a card pendant, by card, falls and hangs sample bin.
Micro-balance described in the present invention is connected with controlled electromagnet, for obtaining the suffered power of electromagnet; Described measurement charger is connected with sample bin, makes sample be suspended from airtight Laboratory Module inside; Described calibration cell and Laboratory Module are fitted fully, can control experimental temperature; Described control pressurer system is connected with Laboratory Module, can control experimental gas pressure; Described computer control system is connected with temperature, pressure and position sensor, obtains temperature, pressure and position data.
The present invention provides a kind of magnetic levitation to measure the method for absorbing gas coefficient of diffusion in danks simultaneously, and described method comprises the following steps:
Step 1: Laboratory Module is vacuumized, make the temperature in the sealing experiment cabin remain rated temperature simultaneously; By measuring charger, sample is suspended from sample bin, makes the sample in sample bin fully contact with filled gas;
Step 2: open computer control system, carry out the temperature and pressure data calibration; Record position inductor numerical value; Obtain position and gaseous tension initial value;
Step 3: by the gaseous tension control system, to Laboratory Module injection experiments pressed gas, each micro-balance weight of moment of record, gaseous tension and rated temperature, calculate coal-seam gas or the coefficient of diffusion of shale gas in danks matrix.
In the inventive method, each that utilizes record is injected into gaseous tension in the sealing experiment cabin and the weight change of micro-balance constantly, produce the time dependent curve of weight that micro-balance is measured, the time dependent curve of the gas flow adsorbed in sample, then by the formula (1) of each boundary condition substitution Fick's second law, thereby calculate the coefficient of diffusion of gas in danks matrix.
Particularly, in the inventive method, utilize the method for the coefficient of diffusion of Fick's second law calculating gas in danks matrix as follows:
For finite time t, the diffusion process of gas in danks matrix obey suc as formula
Figure 2013103941676100002DEST_PATH_IMAGE003
(1)
Shown Fick's second law:
(2)
In formula (2), D efor effective diffusion cofficient; T is the time; M tthe adsorbance of danks matrix to gas during for moment t; M for the maximal absorptive capacity of danks to gas.
According to M t/ M with t 1/2relation, can matching draw the slope K (constant) of this straight line; K=6 (D e/ π) 1/2,
Figure 2013103941676100002DEST_PATH_IMAGE007
i.e. (3)
Like this, according to detection method provided by the invention, can obtain exactly gas diffusing capacity curve in time, thereby and then utilize formula (3) accurately to calculate the effective diffusion cofficient of gas in danks matrix.
In the inventive method, utilize water bath with thermostatic control to make the Laboratory Module temperature remain steady temperature; Described rated temperature is the temperature between 20 ℃-80 ℃;
In the inventive method, before the danks sample is suspended to inside, sealing experiment cabin, bulk sample is no more than 40 mm * 40 mm * 40 mm, pulverizes sample and is no more than 300g;
In the inventive method, the real-time gas pressure value of described Laboratory Module is 0-15MPa.
In the present invention, due to Laboratory Module and micro-balance measurement system is separate, and sample can be suspended from Laboratory Module inside, make the gas in Laboratory Module can fully contact with danks matrix, and then effectively spread, therefore, technical scheme provided by the invention can be utilized with the identical danks piece of subterranean strata and use sample as detecting, the experimental result that keeps the sample primary characteristic and can avoid experimental apparatus to cause is inaccurate, and in the present invention, coefficient of diffusion testing result and the gas coefficient of diffusion under the subterranean strata state is more approaching.
The accompanying drawing explanation
Fig. 1 is for detecting the apparatus structure schematic diagram of the coefficient of diffusion of gas in danks matrix.
Wherein, the micro-balance of 1-; The 2-gas control valve; The 3-electromagnet; The 4-permanent magnet; 5-location sensitive core; 6-location sensitive coil; 7-measures charger; The 8-sample bin; The 9-computer control system; The 10-control pressurer system; The 11-sample; The 12-calibration cell; The 13-temperature inductor; The 14-pressure inductor; The 15-Laboratory Module.
Fig. 2 is for measuring charger loading structure schematic diagram.
Wherein, 16-draw-in groove; The 17-support; 18-card pendant.
Fig. 3 is the schematic flow sheet that the present invention detects the coefficient of diffusion of gas in danks matrix.
Embodiment
In order to make the purpose, technical solutions and advantages of the present invention clearer, below in conjunction with the drawings and specific embodiments, describe the present invention.
The apparatus structure schematic diagram that Fig. 1 is the coefficient of diffusion of detection gas provided by the invention in danks matrix.As shown in Figure 1, this device comprises micro-balance 1; Gas control valve 2; Electromagnet 3; Permanent magnet 4; Location sensitive core 5; Location sensitive coil 6; Measure charger 7; Sample bin 8; Computer control system 9; Control pressurer system 10; Sample 11; Calibration cell 12; Temperature inductor 13; Pressure inductor 14; Laboratory Module 15.
Concrete structure is: described device comprises a cabin body, and is installed on the external computer control system in cabin, and described cabin body is separate micro-balance measurement system and Laboratory Module by a baffle for separating, and micro-balance measurement system is arranged at the Laboratory Module top;
Described micro-balance measurement system comprises the electromagnet be arranged in the body of micro-balance measurement system cabin, and is connected, is installed on micro-balance of body top, cabin with electromagnet; Electromagnet is connected with computer control system respectively with micro-balance;
Described Laboratory Module comprises the measurement charger that is installed on the Laboratory Module middle part and is hung on the sample bin of measuring the charger below, in described sample bin, sample is installed, measure the charger top and be provided with permanent magnet, permanent magnet is connected with the measurement charger by a location sensitive core, Laboratory Module bulkhead corresponding to the location sensitive core is provided with the location sensitive coil, the Laboratory Module upper and lower is respectively arranged with and the extraneous pipeline communicated, be respectively arranged with gas control valve on pipeline, the pipeline Bonding pressure control system of below; Be provided with pressure inductor in Laboratory Module, pressure inductor and location sensitive coil are connected with computer control system respectively.
The whole cabin body of described device is installed in a calibration cell, and described calibration cell is provided with temperature inductor, and described temperature inductor is connected with computer control system.
As shown in Figure 2, for measuring the charger structural representation, comprise draw-in groove 16; Support 17; Card pendant 18, for the sample bin that suspends.
Described measurement charger comprises the support be installed on the Laboratory Module bulkhead, and a draw-in groove is installed on support, and a snap ring is installed in draw-in groove, and by snap ring link position induction core, the draw-in groove below is equipped with a card pendant, by card, falls and hangs sample bin.
The micro-balance of the present invention is connected with electromagnet, for obtaining the weight change of Laboratory Module; Whole cabin body is placed in calibration cell, for the temperature in Laboratory Module, keeps rated temperature, and sample bin is also the same nominal temperature; Permanent magnet is connected with location sensitive core and measurement charger, for measuring the example weight of loading; The measurement charger is placed on support and is connected with sample bin, can change different laboratory samples; Sample is placed in sample bin, is suspended from Laboratory Module, can fully contact with the gas injected, thereby and then effectively spread, in the present invention, coefficient of diffusion testing result and the gas coefficient of diffusion under the subterranean strata state is more approaching; Control pressurer system can be used for filling gas and start before experiment, Laboratory Module to be vacuumized in Laboratory Module; Computer control system comprises the real time record of temperature, pressure and position numerical value, the calculating of coefficient of diffusion.
Fig. 2 comprises draw-in groove 16 for measuring charger; Support 17; Card pendant 18, for the sample bin that suspends.
The method figure that Fig. 3 is the coefficient of diffusion of detection gas provided by the invention in danks matrix.As shown in Figure 3, the method comprises:
Step 301: Laboratory Module is vacuumized, make the temperature in the sealing experiment cabin remain rated temperature simultaneously; Sample is suspended from sample bin, can realizes by measuring charger, like this can be so that the sample in sample bin fully fully contacts with filled gas;
Step 302: open computer control system, carry out the temperature and pressure data calibration; Record position inductor numerical value; Obtain position and gaseous tension initial value;
Step 303: by the gaseous tension control system, to Laboratory Module injection experiments pressed gas, each micro-balance weight of moment of record, gaseous tension and rated temperature, calculate the coefficient of diffusion of coal-seam gas/shale gas in danks matrix.
Each that utilizes record is injected into gaseous tension in the sealing experiment cabin and the weight change of micro-balance constantly, can produce the time dependent curve of weight that micro-balance is measured, the time dependent curve of the gas flow adsorbed in sample, then by the formula of each boundary condition substitution Fick's second law
Figure 975827DEST_PATH_IMAGE002
(1),
Thereby calculate the coefficient of diffusion of gas in danks matrix.
Utilize the method for the coefficient of diffusion of Fick's second law calculating gas in danks matrix as follows:
For finite time t=3600s, the diffusion process of gas in danks matrix obey suc as formula
Figure 727882DEST_PATH_IMAGE003
(1)
Shown Fick's second law:
Figure DEST_PATH_IMAGE009
(2)
In formula (2), D efor effective diffusion cofficient; T is the time; M tthe adsorbance of danks matrix to gas during for moment t; M for the maximal absorptive capacity of danks to gas.
According to M t/ M with t 1/2relation, can matching draw the slope K of this straight line=0.006(constant); K=6 (D e/ π) 1/2,
Figure 488027DEST_PATH_IMAGE007
(3)
Like this, according to detection method provided by the invention, can obtain exactly gas diffusing capacity curve in time, thereby and then utilize formula (3) accurately to calculate the effective diffusion cofficient D of gas in this coal petrography matrix e=3.19 * 10 -6(S -1).
Core of the present invention is: utilize magnetic levitation that Laboratory Module and micro-balance measurement system is separate, and sample can be suspended from Laboratory Module inside fully, make the gas in Laboratory Module can fully contact with danks matrix, thereby effectively spread, therefore, technical scheme provided by the invention can be utilized with the identical danks piece of subterranean strata and use sample as detecting, and the experimental result that keeps the sample primary characteristic and can avoid experimental apparatus to cause is inaccurate; Utilize pressure control device by experimental gas injection experiments cabin, and record each gaseous tension and micro-balance weight constantly in Laboratory Module by computer control system, calculate the coefficient of diffusion of gas in danks matrix.
Finally it should be noted that: obviously, above-described embodiment is only for example of the present invention clearly is described, and is not the restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without also giving all embodiments.And the apparent variation of being amplified out thus or change are still among protection scope of the present invention.

Claims (7)

1. the device of absorbing gas coefficient of diffusion in danks is measured in a magnetic levitation, it is characterized in that: described device comprises a cabin body, the external computer control system with being installed on cabin, described cabin body is separate micro-balance measurement system and Laboratory Module by a baffle for separating, and micro-balance measurement system is arranged at the Laboratory Module top;
Described micro-balance measurement system comprises the electromagnet be arranged in the body of micro-balance measurement system cabin, and is connected, is installed on micro-balance of body top, cabin with electromagnet; Electromagnet is connected with computer control system respectively with micro-balance;
Described Laboratory Module comprises the measurement charger that is installed on the Laboratory Module middle part and is hung on the sample bin of measuring the charger below, in described sample bin, sample is installed, measure the charger top and be provided with permanent magnet, permanent magnet is connected with the measurement charger by a location sensitive core, Laboratory Module bulkhead corresponding to the location sensitive core is provided with the location sensitive coil, the Laboratory Module upper and lower is respectively arranged with and the extraneous pipeline communicated, be respectively arranged with gas control valve on pipeline, the pipeline Bonding pressure control system of below; Be provided with pressure inductor in Laboratory Module, pressure inductor and location sensitive coil are connected with computer control system respectively.
2. the device of absorbing gas coefficient of diffusion in danks is measured in magnetic levitation as claimed in claim 1, it is characterized in that: the whole cabin body of described device is installed in a calibration cell, described calibration cell is provided with temperature inductor, and described temperature inductor is connected with computer control system.
3. the device of absorbing gas coefficient of diffusion in danks is measured in magnetic levitation as claimed in claim 2, it is characterized in that: described measurement charger comprises the support be installed on the Laboratory Module bulkhead, a draw-in groove is installed on support, a snap ring is installed in draw-in groove, by snap ring link position induction core, the draw-in groove below is equipped with a card pendant, by card, falls and hangs sample bin.
4. the method for absorbing gas coefficient of diffusion in danks is measured in a magnetic levitation, it is characterized in that, described method comprises the following steps:
Step 1: Laboratory Module is vacuumized, make the temperature in the sealing experiment cabin remain rated temperature simultaneously; By measuring charger, sample is suspended from sample bin, makes the sample in sample bin fully contact with filled gas;
Step 2: open computer control system, carry out the temperature and pressure data calibration; Record position inductor numerical value; Obtain position and gaseous tension initial value;
Step 3: by the gaseous tension control system, to Laboratory Module injection experiments pressed gas, each micro-balance weight of moment of record, gaseous tension and rated temperature, calculate coal-seam gas or the coefficient of diffusion of shale gas in danks matrix.
5. method as claimed in claim 4, it is characterized in that: each that utilizes record is injected into gaseous tension in the sealing experiment cabin and the weight change of micro-balance constantly, produce the time dependent curve of weight that micro-balance is measured, the time dependent curve of the gas flow adsorbed in sample, then by the formula (1) of each boundary condition substitution Fick's second law, thereby calculate the coefficient of diffusion of gas in danks matrix.
6. method as claimed in claim 5 is characterized in that: utilize Fick's second law to calculate the method for the coefficient of diffusion of gas in danks matrix as follows:
Figure 998654DEST_PATH_IMAGE002
for finite time t, the diffusion process of gas in danks matrix obey suc as formula
(1)
Shown Fick's second law:
(2)
In formula (2), D efor effective diffusion cofficient; T is the time; M tthe adsorbance of danks matrix to gas during for moment t; M for the maximal absorptive capacity of danks to gas;
According to M t/ M with t 1/2relation, can matching draw the slope K (constant) of this straight line; K=6 (D e/ π) 1/2,
Figure 633214DEST_PATH_IMAGE006
(3)
Like this, according to detection method provided by the invention, can obtain exactly gas diffusing capacity curve in time, thereby and then utilize formula (3) accurately to calculate the effective diffusion cofficient of gas in danks matrix.
7. as the arbitrary described method of claim 5-6, it is characterized in that, utilize water bath with thermostatic control to make the Laboratory Module temperature remain steady temperature; Described rated temperature is the temperature between 20 ℃-80 ℃;
Before the danks sample is suspended to inside, sealing experiment cabin, bulk sample is no more than 40 mm * 40 mm * 40 mm, pulverizes sample and is no more than 300g;
The real-time gas pressure value of described Laboratory Module is 0-15MPa.
CN2013103941676A 2013-09-03 2013-09-03 Device and method for measuring diffusion coefficient of adsorbent gas in coal shale in magnetic suspension manner Pending CN103439226A (en)

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CN104502239A (en) * 2014-12-30 2015-04-08 中国石油天然气集团公司 Method for measuring wettability of coal and rock
CN105136603A (en) * 2015-09-18 2015-12-09 武汉理工大学 Method for detecting diffusion coefficient of water vapor in bituminous mixture
CN108387485A (en) * 2018-03-29 2018-08-10 安徽理工大学 Solute molecule diffusion coefficients experimental provision based on layering porous media
CN108387485B (en) * 2018-03-29 2023-09-22 安徽理工大学 Experimental device for determining diffusion coefficient of solute molecules based on layered porous medium
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CN109238905B (en) * 2018-09-16 2024-02-09 金华职业技术学院 Gas adsorption testing device
CN110455665A (en) * 2019-08-16 2019-11-15 武汉理工大学 Asphalt accumulation type aqueous vapor movement parameter detection apparatus and method
CN113670777A (en) * 2021-08-26 2021-11-19 中国石油大学(华东) Imbibition experimental method
CN113670777B (en) * 2021-08-26 2023-08-15 中国石油大学(华东) Shale imbibition experimental method for simulating formation temperature and pressure conditions

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