CN107202744B - Device and method for synchronously measuring coal rock adsorption deformation and porosity - Google Patents

Device and method for synchronously measuring coal rock adsorption deformation and porosity Download PDF

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CN107202744B
CN107202744B CN201710395432.0A CN201710395432A CN107202744B CN 107202744 B CN107202744 B CN 107202744B CN 201710395432 A CN201710395432 A CN 201710395432A CN 107202744 B CN107202744 B CN 107202744B
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gas
coal sample
adsorption
coal
porosity
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CN107202744A (en
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程波
邹银辉
张志刚
向衍斌
李文哲
李大勇
程建圣
孙炳兴
张林良
王建
龚选平
冀超辉
杜文波
黄光利
刘俊
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CCTEG Chongqing Research Institute Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N7/00Analysing materials by measuring the pressure or volume of a gas or vapour
    • G01N7/02Analysing 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
    • G01N7/04Analysing 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
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01BMEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B7/00Measuring arrangements characterised by the use of electric or magnetic techniques
    • G01B7/16Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge
    • G01B7/18Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge using change in resistance
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/08Investigating permeability, pore-volume, or surface area of porous materials
    • G01N15/088Investigating volume, surface area, size or distribution of pores; Porosimetry
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N7/00Analysing materials by measuring the pressure or volume of a gas or vapour
    • G01N7/10Analysing materials by measuring the pressure or volume of a gas or vapour by allowing diffusion of components through a porous wall and measuring a pressure or volume difference

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Abstract

The invention belongs to the technical field of coal mine safety, and relates to a device and a method for synchronously measuring coal rock adsorption deformation and porosity, wherein a strain sensor and a first solid gas pressure sensor at the upper end of an adsorption tank are connected on a multi-path signal conditioner through leads, a gas pressure reducing valve and a second solid gas pressure sensor which are connected on the multi-path signal conditioner through leads are fixedly arranged on a high-pressure gas cylinder, a pipeline on the high-pressure gas cylinder is connected with a standard tank and is provided with a second mass flowmeter, a rotary platform is arranged below the adsorption tank, an X-ray source and a ray detector which are opposite to the adsorption tank are fixedly arranged in a constant-temperature air bath arranged outside the adsorption tank, a data acquisition and analysis system is arranged on the ray detector, a first mass flowmeter and a vacuum degassing pump are connected on the adsorption tank through a pipeline, a degassing control valve and a vacuum thermocouple meter are, the problem of in the coal petrography adsorbed gas volume survey process, can't survey coal sample adsorption deformation and porosity in step is solved.

Description

A kind of coal petrography absorption deformation and porosity synchronous measurement device and method
Technical field
The invention belongs to technical field of mine safety, be related to a kind of coal petrography absorption deformation and porosity synchronous measurement device and Method.
Background technique
Coal mine gas (also known as " coal bed gas ") is preservation in coal seam and its country rock, is existed with absorption or free state , with methane Unconventional gas as main component.China's coal bed gas resource is abundant, according to known to new round of resources evaluation: I 2000 meters of state is about 36.81 tcms with shallow Coal bed gas project, is equivalent to 49,000,000,000 tons of standard coals, arranges third place in the world Position.But it is that coal bed gas gas output per well is too low that current China's cbm development industry development, which has the reality that can not ignore, economical Benefit is lower, and industry faces in straitened circumstances.Therefore, during " 13 ", further to push China's CBM exploration and development industry Development is bound to that essence breakthrough should be obtained in terms of basic theory and technical matters.Coal itself belongs to a kind of special porous media, It makes it be different from other rocks the strong characterization of adsorption of methane gas.It is existing a large number of studies show that after coal adsorption gas, will Different degrees of dilatancy occurs, further will affect the porosity of coal.The porosity of coal is evaluation Reservoir Characteristics of Coal Important indicator, and calculate the basis of coal seam gas-bearing capacity.Currently, China generallys use, " coal and physical-mechanical properties of rock are surveyed Determine method " in the block density of the Sealing Method enumerated or volumetric method measurement coal, using bottle method or gas expansion method real density The real density of analysis-e/or determining coal, and then calculate the porosity of coal.This kind of method can accurately measure coal sample without gas item Porosity under part, but there are strong suction-operated between coal and methane gas, different gas pressures will lead to coal sample Different deformations.It is existing practice have shown that: even if under the conditions of lower gas pressure, coal adsorption gas cause deformation cause The opposite variation of its porosity is maximum up to 17.98%.Therefore, by the mapping principle of gas pressure and coal porosity, as Basis is modified the calculation method of porosity, can be the evaluation of reservoir coal bed gas resource or Mine Gas Emission Prediction Accurate foundation is provided.
In view of this, the invention discloses the synchronous measurement device of a kind of coal petrography adsorbed gas scale of construction, deformation and porosity and Method, solve the measurement coal petrography adsorbed gas of high pressure content method measure it is fixed during, can not Simultaneous Determination coal sample absorption deformation with The problem of porosity, can provide accurate section for the solution formulation of coalbed gas in coal mine area development project and the evaluation of reservoir coal bed gas resource Learn foundation.
Summary of the invention
In view of this, during the present invention is in order to solve coal petrography adsorbed gas measurement calmly, it can not the absorption of Simultaneous Determination coal sample The problem of deformation is with porosity provides a kind of coal petrography absorption deformation and porosity synchronous measurement device and method.
In order to achieve the above objectives, the invention provides the following technical scheme: including adsorption tanks, multi-channel signal conditioning device and high pressure Gas gas cylinder, adsorption tanks upper end lead are connected with strain transducer and the first solid state gas pressure sensor, strain transducer and First solid state gas pressure sensor conducting wire is connected on multi-channel signal conditioning device, and gas is fixedly installed in high pressure gas gas cylinder Pressure reducing valve and the second solid state gas pressure sensor, the second solid state gas pressure sensor conducting wire are connected to multi-channel signal conditioning device On, the second mass flowmenter, standard can and adsorption tanks are installed on pipeline connection standard can and the pipeline in high pressure gas gas cylinder Pipeline connection, adsorption tanks are equipped with constant temperature air bath outside, and rotating platform, fixed peace in constant temperature air bath are equipped with below adsorption tanks X-ray source and ray detector equipped with face adsorption tanks are equipped with data acquisition and analysis system, absorption on ray detector Pipeline is connected with the first mass flowmenter and vacuum outgas pump on tank, is fixedly installed with flow control on the first mass flowmenter Valve, vacuum outgas, which pumps, is fixedly installed with degassing control valve, is equipped with vacuum thermocouple meter on vacuum outgas pump.
Further, the first control valve and the second control valve are fixedly installed on adsorption tanks, the first control valve is mounted on absorption On the pipeline that tank is communicated with the first mass flowmenter and vacuum outgas pump, the second control valve is mounted on standard can and adsorption tanks connect On the pipeline connect.
Further, vacuum piping is installed on vacuum outgas pump, vacuum thermocouple meter is connected to vacuum tube by conducting wire and fastens.
Further, rotating platform includes the column spinner being fixedly mounted in the middle part of constant temperature air bath and is rotatably connected on column spinner On rotating disk, adsorption tanks are fixedly mounted on the middle part of rotating disk, are fixedly installed with rotating electric machine in rotating disk.
Further, x-ray source and ray detector are fixedly mounted on the rotating platform in constant temperature air bath by telescopic rod Surrounding, x-ray source are connect with ray detector conducting wire.
Further, it is provided with resistance strain gage conducting wire outlet at the top of adsorption tanks, pacified on resistance strain gage conducting wire outlet Equipped with interface, the first solid state gas pressure sensing and strain transducer are installed on interface.
A kind of coal petrography absorption deformation and porosity Simultaneous Determination method, specifically includes the following steps:
S1: by the mold of the coal grain prepared indentation loop column type, it is cold-pressed one-pass molding, will be prepared using coring device Good circular ring type coal sample is taken out, and is polished using sand paper coal sample surface, makes its surfacing;
S2: the coal sample prepared being placed in vacuum oven and is dried, and the time controls more than for 24 hours, finally The size of coal sample is measured, the volume for recording coal sample is Vm, and be put into the hermetic bag marked;
S3: slightly wearing down coal sample surface with crosus cloth and wipe dedusting with alcohol after oxide layer to remove, then with quick colloid Resistance strain gage is pasted on coal sample surface, and is compacted resistance strain gage to eliminate bubble, then with adhesive tape by resistance strain gage Resistance strain gage is finally connect by conducting wire with strain transducer by tightly paste on coal sample surface;
S4: the coal sample that surface is stained with resistance strain gage is placed in adsorption tanks, opens vacuum outgas pump and degassing control valve Adsorption tanks are de-gassed, influence of the air to test result is adsorbed under normal pressure to eliminate, shows numerical value to vacuum thermocouple meter Lower than 5 × 10-1After Pa, stop deaerating to adsorption tanks;While opening vacuum outgas pump and degassing control valve, the strain to coal sample It is monitored, axial direction at this time and hoop strain ε is recorded after degassingz0、εr0;Bulk strain after coal sample degassing is εv0z0+2εr0, the volume after coal sample degassing is Vm0=(1+ εv0)Vm;Rotating platform, x-ray source and ray detector are opened to coal The porosity of sample different layers position is scanned, and the hole rate score of different layers position is averaged to obtain when adsorbance is 0 Mean porosities Φ0;Adsorption tanks demarcate coal sample volume before testing, and recording its volume is Vx;Mean porosities Φ0By Data acquisition and analysis system output;
S5: gas pressure reducer is opened, makes the methane gas in high pressure gas gas cylinder, is entered to via the second mass flowmenter In standard can, the pressure p of gas in standard can is filled with by the second solid state gas pressure sensor record1, pass through the second mass Cmf record is filled with the device in Gas scale of construction in standard can, standard can and is connected thereto to the pipeline of adsorption tanks and the second mass The total volume of the pipeline of flowmeter connection, is demarcated in experiment, and recording its volume is Vb
S6: the second control valve is opened, the high pressure gas in standard can is made to enter to the adsorption tanks equipped with coal sample via pipeline In, after coal sample adsorption gas balance, record gas pressure p at this time1p;Open rotating platform, x-ray source and ray detector The porosity of coal sample different layers position is scanned, the hole rate score of different layers position is averaged to obtain adsorption equilibrium Pressure p1pWhen mean porosities Φ1;Adsorption equilibrium pressure p is recorded simultaneously1pWhen axial direction and hoop strain εz1、εr1, calculate phase The coal sample bulk strain answered is εv1z1+2εr1, the volume after coal sample adsorption equilibrium is Vml=(1+ εv1)Vm, then adsorption tanks at this time The mole of middle coal sample adsorption gas are as follows:
In formula: Z1、Z1pRespectively p1、p1pWhen, the compressibility factor of methane gas;n1For adsorption equilibrium pressure p1pWhen, coal sample The mole of adsorption gas;
Adsorption equilibrium pressure p1pWhen, the adsorption gas amount V of coal samplexp1=22.4 × n1×1000。
S7: closing the second control valve, opens gas pressure reducer, continues to be filled with standard can high pressure gas gas, record this When standard can gas pressure p2
S8: opening the second control valve, enter to the high pressure gas in standard can in adsorption tanks, flat to coal sample adsorption gas After weighing apparatus, adsorption equilibrium gas pressure p at this time is recorded2p;It is different to coal sample from ray detector to open rotating platform, x-ray source The porosity of layer position is scanned, and the hole rate score of different layers position is averaged to obtain adsorption equilibrium pressure p2pWhen Mean porosities Φ2;And adsorption equilibrium pressure p is recorded simultaneously2pWhen axial direction and hoop strain εz2、εr2, calculate corresponding coal sample Bulk strain is εv2z2+2εr2, the volume after coal sample adsorption equilibrium is Vm2=(1+ εv2)Vm, then coal sample is inhaled in adsorption tanks at this time The mole of attached gas are as follows:
In formula: Z2、Z2pRespectively p2、p2pWhen, the compressibility factor of methane gas;n2For adsorption equilibrium pressure p2pWhen, coal sample The mole of adsorption gas.
Adsorption equilibrium pressure p2pWhen, the adsorption gas amount V of coal samplexp2=22.4 × n2×1000。
S9: S7, S8 are repeated, the gas pressure p of standard can is accordingly filled withiAnd adsorption equilibrium gas pressure pip, average hole Gap rate Φi, adsorption equilibrium pressure pipWhen axial direction and hoop strain εzi、εri, corresponding coal sample bulk strain is εvizi +2εri, the volume after coal sample adsorption equilibrium is Vmi=(1+ εvi)Vm, then at this time in adsorption tanks coal sample adsorption gas mole ni Are as follows:
In formula: Zi、ZipRespectively pi、pipWhen, the compressibility factor of methane gas;niFor adsorption equilibrium pressure pipWhen, coal sample The mole of adsorption gas.
Adsorption equilibrium pressure pipWhen, the adsorption gas amount V of coal samplexpi=22.4 × ni×1000;
S10: after the test under predetermined maximum adsorption balanced pressure condition to be done, the second control valve is closed, opens first Control valve, flow control valve and the first mass flowmenter, make the high pressure gas in adsorption tanks, via the first mass flowmenter stream Out;After high pressure gas outflow a part in tank to be adsorbed, the first mass flowmenter can accurately record the gas amount of outflow part, Free gas in adsorption tanks is calculated, into one according to the porosity and coal sample bulk strain after balance in conjunction with balance pressure Step obtains the adsorbance under corresponding balance gas pressure;
S11: repeating S10, obtains coal sample during diffusing gas, any adsorbance balanced under pressure, porosity, directly It is emptied to by the high pressure gas in adsorption tanks.
Further, the preparation of the experiment coal sample in step S1 the specific steps are crushing coal sample to be measured, and screens out 0.2 The coal dust of~0.25mm partial size, a certain amount of coal dust is put into moulded coal grinding tool, and moulded coal grinding tool is cylindrical.
Further, the resistance strain gage conducting wire in step S3 is connected with strain transducer, specifically includes the following steps:
S31: after resistance strain gage conducting wire is drawn by the resistance strain gage conducting wire outlet at the top of adsorption tanks, using epoxy Resin is sealed outlet, prevents high pressure gas from flowing out;
S32: the interface on adsorption tanks top resistive foil gauge conducting wire outlet connects the first solid state gas pressure sensor, Measure the methane gas pressure value in adsorption tanks.
Further, the specific step of rotating platform, x-ray source and ray detector to coal sample different layers bit scan in step S4 Suddenly are as follows:
While S41:X radiographic source emits signal, rotating platform slowly rotates, by data after ray detector reception signal Data acquisition and analysis system is passed to carry out data after data acquisition and analysis system receive the data of ray detector Analysis, and then obtain the porosity of coal sample;
S42: the porosity of coal sample is averaged and obtains according to the porosity of coal sample upper surface, middle part cross section, lower end surface It takes.
The test philosophy of coal petrography absorption deformation and porosity synchronous measurement device of the present invention:
The coal petrography adsorbed gas scale of construction, deformation and the synchronous measurement device of porosity of the invention and the purpose of test method are To obtain the adsorbed gas scale of construction, deformation and porosity of the coal sample under different adsorption gas balanced pressure conditions.Its principle is will be electric Strain gauge adhesion is hindered after testing coal sample surface, is put into adsorption tanks, resistance strain gage conducting wire is drawn via adsorption tanks upper end, Pass through the first solid state gas pressure sensor and strain transducer and multi-channel signal conditioning on resistance strain gage conducting wire outlet Device connection, to measure the pressure of methane gas in adsorption tanks.By high pressure gas gas cylinder, gas pressure reducer makes high pressure gas gas Methane gas in bottle passes through the second mass flowmenter first, then enters in standard can, the second mass flowmenter is to entrance The gas flow of standard can is measured.The second control valve being arranged on adsorption tanks is then opened, the gas in standard can is entered Adsorption tanks equipped with coal sample, and x-ray source, ray detector, rotating platform and the first solid state gas pressure sensing are opened simultaneously Device is respectively monitored the gas pressure in the porosity of coal sample, deformation and adsorption tanks.After coal sample adsorption equilibrium, read It is flat in corresponding absorption to calculate coal sample using the equation of gas state for gas pressure parameter in the strain parameter of coal sample, adsorption tanks Adsorption gas amount under the conditions of the gas pressure that weighs.
The coal petrography adsorbed gas scale of construction proposed by the present invention, deformation and porosity synchronous measurement device and method, can be accurately real The adsorbed gas scale of construction of existing coal sample during absorption, release gas, deformation and porosity Simultaneous Determination, coal petrography of the invention inhales Attached gas flow, deformation have the advantage that compared with previous test method with the synchronous measurement device of porosity and method
1, the distinctive coal petrography adsorbed gas scale of construction of the present invention, deformation and porosity synchronous measurement device and method, can be real-time The variation characteristic of deformation of coal sample during adsorption gas, porosity is monitored, can be mentioned for the physical characteristic of research coal containing methane gas For technical support, and data acquisition is reliable, as a result accurate credible.
2, the coal petrography adsorbed gas scale of construction provided by the invention, deformation and porosity synchronous measurement device and method, can be accurate Porosity and adsorbance of the measurement coal sample test specimen under the conditions of different adsorption equilibrium gas pressures, obtained experimental data can Further progress numerical analysis, fitting obtain adsorption equilibrium gas pressure and being associated between porosity, adsorbance, not only can be right Langmuir equation is modified, while can be also modified to the porosity under the conditions of different gas pressures, final to can be achieved The amendment that coal seam gas-bearing capacity calculates, for accurate evaluation reservoir coal bed gas resource and coal and gas prominent danger provide it is scientific according to According to.
3, the coal petrography adsorbed gas scale of construction provided by the invention, deformation and porosity synchronous measurement device and method, carrying out Porosity, adsorbed gas under the conditions of different adsorption equilibrium gas pressures measure timing, from low to high using gas pressure, gradually Raised method is de-gassed before only testing under minimum adsorption equilibrium gas pressure, easy to operate, and completes difference After the adsorbed gas scale of construction, deformation and porosity measurement under adsorption gas balanced pressure condition, the first of openable outlet end setting Mass flowmenter carries out the measurement of coal sample release gas amount, provides reliable technical support for research coal-bed gas diffusion mechanism.
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 the structural schematic diagram of coal petrography of the present invention absorption deformation and porosity synchronous measurement device.
Specific embodiment
Below in conjunction with attached drawing, a preferred embodiment of the present invention will be described in detail.
Appended drawing reference in Figure of description includes:
First mass flowmenter 1, degassing control valve 2, vacuum piping 3, strain transducer 4, the first solid state gas pressure pass It is sensor 5, vacuum outgas pump 6, x-ray source 7, standard can 8, rotating platform 9, ray detector 10, adsorption tanks 11, conducting wire 12, true Empty thermocouple meter 13, constant temperature air bath 14, the first control valve 15, the second control valve 16, gas pressure reducer 17, the second mass flowmenter 18, the second solid state gas pressure sensor 19, high pressure gas gas cylinder 20, multi-channel signal conditioning device 21, data acquisition and analysis system System 22, flow control valve 23.
Coal petrography absorption deformation and porosity synchronous measurement device, including adsorption tanks 11, multi-channel signal conditioning as shown in Figure 1 12 outlet of resistance strain gage conducting wire, resistance strain gage conducting wire 12 are arranged at the top of adsorption tanks 11 for device 21 and high pressure gas gas cylinder 20 Interface is installed on outlet, the first solid state gas pressure sensing and strain transducer 4 are installed on interface.Strain transducer 4 and One solid state gas pressure sensor, 5 conducting wire 12 is connected on multi-channel signal conditioning device 21, is fixedly mounted in high pressure gas gas cylinder 20 Gas pressure reducer 17 and the second solid state gas pressure sensor 19,19 conducting wire 12 of the second solid state gas pressure sensor are connected to more On road signal conditioner 21.
It is connected in high pressure gas gas cylinder 20 by pipeline and the second mass flowmenter 18 is installed in standard can 8 and the pipeline, marked The second control valve 16 is installed on quasi- tank 8 and the pipeline that 11 pipeline of adsorption tanks is connect and standard can 8 is connect with 11 pipeline of adsorption tanks, is inhaled Constant temperature air bath 14 is installed outside attached tank 11, rotating platform 9 is installed below adsorption tanks 11, rotating platform 9 includes being fixedly mounted on perseverance The column spinner at 14 middle part of warm air bath and the rotating disk being rotatably connected on column spinner, adsorption tanks 11 are fixedly mounted on rotating disk Middle part is fixedly installed with rotating electric machine in rotating disk.
Be fixedly mounted the x-ray source 7 and ray detector 10 of face adsorption tanks 11 in constant temperature air bath 14, x-ray source 7 with Ray detector 10 is fixedly mounted on 9 surrounding of rotating platform in constant temperature air bath 14, x-ray source 7 and ray by telescopic rod The connection of 10 conducting wire 12 of detector.Installation data acquisition and analysis system 22 on ray detector 10.
Pipeline connects the first mass flowmenter 1 and vacuum outgas pump 6, adsorption tanks 11 and the first mass flow on adsorption tanks 11 The first control valve 15 is installed on the pipeline that meter 1 and vacuum outgas pump 6 communicate, flow is fixedly mounted on the first mass flowmenter 1 Control valve 23, vacuum outgas pump and degassing control valve 2 and vacuum piping 3 are fixedly mounted on 6, and vacuum thermocouple meter 13 is connected by conducting wire 12 It connects on vacuum piping 3.
A kind of coal petrography absorption deformation and porosity Simultaneous Determination method, specifically includes the following steps:
S1: coal sample to be measured is crushed, and screens out the coal dust of 0.2~0.25mm partial size, and a certain amount of coal dust is pressed into and is justified In the mold of annulated column type, it is cold-pressed one-pass molding, is taken out the circular ring type coal sample prepared using coring device, using sand paper to coal Sample surface is polished, its surfacing is made.
S2: the coal sample prepared being placed in vacuum oven and is dried, and the time controls more than for 24 hours, finally The size of coal sample is measured, the volume for recording coal sample is Vm, and be put into the hermetic bag marked.
S3: slightly wearing down coal sample surface with crosus cloth and wipe dedusting with alcohol after oxide layer to remove, then with quick colloid Resistance strain gage is pasted on coal sample surface, and is compacted resistance strain gage to eliminate bubble, then with adhesive tape by resistance strain gage Resistance strain gage is finally connect by conducting wire 12 with strain transducer 4 by tightly paste on coal sample surface;Wherein, resistance-strain After piece conducting wire 12 is drawn by 12 outlet of resistance strain gage conducting wire at the top of adsorption tanks 11, using epoxy resin to outlet into Row sealing, prevents high pressure gas from flowing out;Interface connection first on 11 top resistive foil gauge conducting wire of adsorption tanks, 12 outlet is solid State gas pressure sensor 5 measures the methane gas pressure value in adsorption tanks 11.
S4: the coal sample that surface is stained with resistance strain gage is placed in adsorption tanks 11, opens vacuum outgas pump 6 and degassing control Valve 2 is de-gassed adsorption tanks 11, and influence of the air to test result is adsorbed under normal pressure to eliminate, aobvious to vacuum thermocouple meter 13 After registration value is lower than 5 × 10-1Pa, stop deaerating to adsorption tanks 11;While opening vacuum outgas pump 6 and degassing control valve 2, The strain of coal sample is monitored, axial direction at this time and hoop strain ε are recorded after degassingz0、εr0;After coal sample degassing Bulk strain is εv0z0+2εr0, the volume after coal sample degassing is Vm0=(1+ εv0)Vm;Open rotating platform 9, x-ray source 7 with Ray detector 10 is scanned the porosity of coal sample different layers position, by the hole rate score of different layers position, be averaged with Obtain mean porosities Φ when adsorbance is 00;Adsorption tanks 11 demarcate coal sample volume before testing, and record its volume For Vx;Mean porosities Φ0It is exported by data acquisition and analysis system 22;Wherein, while x-ray source 7 emits signal, rotation Platform 9 slowly rotates, and ray detector 10 passes data to data acquisition and analysis system 22, data acquisition after receiving signal And after the data of the reception ray detector 10 of analysis system 22, data are analyzed, and then obtain the porosity of coal sample;Coal sample Porosity according to the porosity of coal sample upper surface, middle part cross section, lower end surface, be averaged acquisition.
S5: gas pressure reducer 17 is opened, makes the methane gas in high pressure gas gas cylinder 20, via the second mass flowmenter 18 It enters in standard can 8, the pressure p of gas in standard can 8 is filled with by the second solid state gas pressure sensor 19 record1, lead to The second mass flowmenter 18 record is crossed to be filled with the device in Gas scale of construction in standard can 8, standard can 8 and be connected thereto to adsorption tanks 11 The total volume of pipeline, the pipeline connecting with the second mass flowmenter 18, is demarcated in experiment, and recording its volume is Vb
S6: the second control valve 16 is opened, the high pressure gas in standard can 8 is made to enter to the absorption equipped with coal sample via pipeline In tank 11, after coal sample adsorption gas balance, gas pressure p at this time is recorded1p;Open rotating platform 9, x-ray source 7 and ray Detector 10 is scanned the porosity of coal sample different layers position, and the hole rate score of different layers position is averaged to obtain Adsorption equilibrium pressure p1p;When mean porosities Φ1;Adsorption equilibrium pressure p is recorded simultaneously1pWhen axial direction and hoop strain εz1、 εr1, calculating corresponding coal sample bulk strain is εv1z1+2εr1, the volume after coal sample adsorption equilibrium is Vm1=(1+ εv1)Vm, then At this time in adsorption tanks 11 coal sample adsorption gas mole are as follows:
In formula: Z1、Z1pRespectively p1、p1pWhen, the compressibility factor of methane gas;n1For adsorption equilibrium pressure p1pWhen, coal sample The mole of adsorption gas.
Adsorption equilibrium pressure p1pWhen, the adsorption gas amount V of coal samplexp1=22.4 × n1×1000。
S7: closing the second control valve 16, opens gas pressure reducer 17, continues to be filled with standard can 8 high pressure gas gas, remembers Record the gas pressure p of standard can 8 at this time2
S8: opening the second control valve 16, enter to the high pressure gas in standard can 8 in adsorption tanks 11, adsorbs to coal sample After mash gas balancing, adsorption equilibrium gas pressure p at this time is recorded2p;Open rotating platform 9, x-ray source 7 and ray detector 10 The porosity of coal sample different layers position is scanned, the hole rate score of different layers position is averaged to obtain adsorption equilibrium Pressure p2pWhen mean porosities Φ2;And adsorption equilibrium pressure p is recorded simultaneously2pWhen axial direction and hoop strain εz2、εr2, calculate Corresponding coal sample bulk strain is εv2z2+2εr2, the volume after coal sample adsorption equilibrium is Vm2=(1+ εv2)Vm, then adsorb at this time The mole of coal sample adsorption gas in tank 11 are as follows:
In formula: Z2、Z2pRespectively p2、p2pWhen, the compressibility factor of methane gas;n2For adsorption equilibrium pressure p2pWhen, coal sample The mole of adsorption gas.
Adsorption equilibrium pressure p2pWhen, the adsorption gas amount V of coal samplexp2=22.4 × n2×1000。
S9: S7, S8 are repeated, the gas pressure p of standard can 8 is accordingly filled withiAnd adsorption equilibrium gas pressure pip, average Porosity Φi, adsorption equilibrium pressure pipWhen axial direction and hoop strain εzi、εri, corresponding coal sample bulk strain is εvi= εzi+2εri, the volume after coal sample adsorption equilibrium is Vmi=(1+ εvi)Vm, then at this time in adsorption tanks 11 coal sample adsorption gas mole Measure niAre as follows:
In formula: Zi、ZipRespectively pi、pipWhen, the compressibility factor of methane gas;niFor adsorption equilibrium pressure pipWhen, coal sample The mole of adsorption gas.
Adsorption equilibrium pressure pipWhen, the adsorption gas amount V of coal samplexpi=22.4 × ni×1000。
S10: after the test under predetermined maximum adsorption balanced pressure condition to be done, the second control valve 16 is closed, opens the One control valve 15, flow control valve 23 and the first mass flowmenter 1, make the high pressure gas in adsorption tanks 11, via the first mass Flowmeter 1 flows out;After high pressure gas outflow a part in tank 11 to be adsorbed, the first mass flowmenter 1 can accurately record outflow Partial gas amount, the free gas in adsorption tanks 11 is according to the porosity and coal sample bulk strain after balance, in conjunction with balance pressure Power is calculated, and the adsorbance under corresponding balance gas pressure is further obtained;
S11: repeating S10, obtains coal sample during diffusing gas, any adsorbance balanced under pressure, porosity, directly It is emptied to by the high pressure gas in adsorption tanks 11.
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 (8)

1. a kind of coal petrography absorption deformation and porosity synchronous measurement device, which is characterized in that including adsorption tanks, multi-channel signal conditioning Device and high pressure gas gas cylinder, the adsorption tanks upper end lead are connected with strain transducer and the first solid state gas pressure sensor, The strain transducer and the first solid state gas pressure sensor conducting wire are connected on multi-channel signal conditioning device, the high pressure gas Gas pressure reducer and the second solid state gas pressure sensor, the second solid state gas pressure sensor are fixedly installed on gas cylinder Conducting wire is connected on multi-channel signal conditioning device, is equipped with the on pipeline connection standard can and the pipeline in the high pressure gas gas cylinder Two mass flowmenters, the standard can are connect with adsorption tanks pipeline, and constant temperature air bath, the absorption are equipped with outside the adsorption tanks Rotating platform is installed below tank, the x-ray source and X-ray detection X of face adsorption tanks are fixedly installed in the constant temperature air bath Device is equipped with data acquisition and analysis system on the ray detector, and pipeline is connected with the first quality stream on the adsorption tanks Meter and vacuum outgas pump, and flow control valve is fixedly installed on first mass flowmenter, and the vacuum outgas pumps solid Dingan County is equipped with vacuum thermocouple meter on vacuum outgas pump equipped with degassing control valve, and the is fixedly installed on the adsorption tanks One control valve and the second control valve, first control valve is mounted on adsorption tanks and the first mass flowmenter and vacuum outgas pump is equal On the pipeline communicated, second control valve is mounted on standard can and adsorbs on tank connected pipeline, the coal in the adsorption tanks Resistance strain gage is pasted on sample, resistance-strain on piece is connected with resistance strain gage conducting wire, and setting is useful at the top of the adsorption tanks It is equipped on the resistance strain gage conducting wire outlet for drawing resistance strain gage conducting wire, the resistance strain gage conducting wire outlet Interface installs the first solid state gas pressure sensing and strain transducer on the interface.
2. coal petrography absorption deformation as described in claim 1 and porosity synchronous measurement device, which is characterized in that the vacuum is de- Vacuum piping is installed, the vacuum thermocouple meter is connected to vacuum tube by conducting wire and fastens on air pump.
3. coal petrography absorption deformation as claimed in claim 2 and porosity synchronous measurement device, which is characterized in that the rotary flat Platform includes the column spinner being fixedly mounted in the middle part of constant temperature air bath and the rotating disk being rotatably connected on column spinner, the adsorption tanks It is fixedly mounted on the middle part of rotating disk, is fixedly installed with rotating electric machine in the rotating disk.
4. coal petrography absorption deformation as claimed in claim 3 and porosity synchronous measurement device, which is characterized in that the X-ray Source and ray detector are fixedly mounted on the rotating platform surrounding in constant temperature air bath by telescopic rod, the x-ray source with penetrate The connection of line detector conducting wire.
5. a kind of coal petrography absorption deformation and porosity Simultaneous Determination method, are adsorbed using any coal petrography of Claims 1 to 4 Deformation and porosity synchronous measurement device, which is characterized in that specifically includes the following steps:
S1: by the mold of the coal grain for preparing indentation loop column type, it is cold-pressed one-pass molding, will be prepared using coring device Circular ring type coal sample is taken out, and is polished using sand paper coal sample surface, makes its surfacing;
S2: the coal sample prepared being placed in vacuum oven and is dried, and the time controls more than for 24 hours, finally to coal The size of sample measures, and the volume for recording coal sample is Vm, and be put into the hermetic bag marked;
S3: slightly wear down coal sample surface with crosus cloth and wipe dedusting with alcohol after oxide layer to remove, then will be electric with quick colloid Hinder strain gauge adhesion in coal sample surface, and be compacted resistance strain gage to eliminate bubble, then with adhesive tape by resistance strain gage tightly It is pasted onto coal sample surface, finally connect resistance strain gage with strain transducer by conducting wire;
S4: the coal sample that surface is stained with resistance strain gage is placed in adsorption tanks, opens vacuum outgas pump and degassing control valve to suction Attached tank is de-gassed, and influence of the air to test result is adsorbed under normal pressure to eliminate, and shows that numerical value is lower than 5 to vacuum thermocouple meter ×10-1After pa, stop deaerating to adsorption tanks;While opening vacuum outgas pump and degassing control valve, the strain of coal sample is carried out Axial direction at this time and hoop strain ε are recorded in monitoring after degassingz0、εr0;Bulk strain after coal sample degassing is εv0z0+ 2εr0, the volume after coal sample degassing is Vm0=(1+ εv0)Vm;Rotating platform, x-ray source and ray detector are opened to coal sample not The porosity of same layer position is scanned, and the hole rate score of different layers position is averaged to obtain being averaged when adsorbance is 0 Porosity Φ0;Adsorption tanks demarcate coal sample volume before testing, and recording its volume is Vx;Mean porosities Φ0By data Acquisition and analysis system output;
S5: gas pressure reducer is opened, makes the methane gas in high pressure gas gas cylinder, enters to standard via the second mass flowmenter In tank, the pressure p of gas in standard can is filled with by the second solid state gas pressure sensor record1, pass through the second mass flow Meter record is filled with the device in Gas scale of construction in standard can, standard can and is connected thereto to the pipeline of adsorption tanks and the second mass flow The total volume for counting the pipeline of connection, is demarcated in experiment, and recording its volume is Vb
S6: opening the second control valve, enter to the high pressure gas in standard can in the adsorption tanks equipped with coal sample via pipeline, to After coal sample adsorption gas balance, gas pressure p at this time is recorded1p;Rotating platform, x-ray source and ray detector are opened to coal The porosity of sample different layers position is scanned, and the hole rate score of different layers position is averaged to obtain adsorption equilibrium pressure p1pWhen mean porosities Φ1;Adsorption equilibrium pressure p is recorded simultaneously1pWhen axial direction and hoop strain εz1、εr1, calculate corresponding Coal sample bulk strain is εv1z1+2εr1, the volume after coal sample adsorption equilibrium is Vm1=(1+ εv1)Vm, then coal in adsorption tanks at this time The mole of sample adsorption gas are as follows:
In formula: Z1、Z1pRespectively p1、p1pWhen, the compressibility factor of methane gas;n1For adsorption equilibrium pressure p1pWhen, coal sample absorption The mole of gas;
Adsorption equilibrium pressure p1pWhen, the adsorption gas amount V of coal samplexp1=22.4 × n1×1000;
S7: closing the second control valve, opens gas pressure reducer, continues to be filled with standard can high pressure gas gas, record this markers The gas pressure p of quasi- tank2
S8: opening the second control valve, enter to the high pressure gas in standard can in adsorption tanks, balances to coal sample adsorption gas Afterwards, adsorption equilibrium gas pressure p at this time is recorded2p;Rotating platform, x-ray source and ray detector are opened to coal sample different layers The porosity of position is scanned, and the hole rate score of different layers position is averaged to obtain adsorption equilibrium pressure p2pWhen it is flat Equal porosity Φ2;And adsorption equilibrium pressure p is recorded simultaneously2pWhen axial direction and hoop strain εz2、εr2, calculate corresponding coal sample body Product strain is εv2z2+2εr2, the volume after coal sample adsorption equilibrium is Vm2=(1+ εv2)Vm, then coal sample is adsorbed in adsorption tanks at this time The mole of gas are as follows:
In formula: Z2、Z2pRespectively p2、p2pWhen, the compressibility factor of methane gas;n2For adsorption equilibrium pressure p2pWhen, coal sample absorption The mole of gas;
Adsorption equilibrium pressure p2pWhen, the adsorption gas amount V of coal samplexp2=22.4 × n2×1000;
S9: S7, S8 are repeated, the gas pressure p of standard can is accordingly filled withiAnd adsorption equilibrium gas pressure pip, mean porosities Φi, adsorption equilibrium pressure pipWhen axial direction and hoop strain εzi、εri, corresponding coal sample bulk strain is εvizi+2 εri, the volume after coal sample adsorption equilibrium is Vmi=(1+ εvi)Vm, then at this time in adsorption tanks coal sample adsorption gas mole niAre as follows:
In formula: Zi、ZipRespectively pi、pipWhen, the compressibility factor of methane gas;niFor adsorption equilibrium pressure pipWhen, coal sample absorption The mole of gas;
Adsorption equilibrium pressure pipWhen, the adsorption gas amount V of coal samplexpi=22.4 × ni×1000;
S10: after the test under predetermined maximum adsorption balanced pressure condition to be done, closing the second control valve, opens the first control Valve, flow control valve and the first mass flowmenter, make the high pressure gas in adsorption tanks, flow out via the first mass flowmenter;To After high pressure gas outflow a part in adsorption tanks, the first mass flowmenter can accurately record the gas amount of outflow part, absorption Free gas in tank is calculated in conjunction with balance pressure, is further obtained according to the porosity and coal sample bulk strain after balance The adsorbance under balance gas pressure must be corresponded to;
S11: repeating S10, obtains coal sample during diffusing gas, any adsorbance balanced under pressure, porosity, until will High pressure gas emptying in adsorption tanks.
6. coal petrography absorption deformation as claimed in claim 5 and porosity Simultaneous Determination method, which is characterized in that in step S1 The preparation for testing coal sample the specific steps are crushing coal sample to be measured, and screens out the coal dust of 0.2~0.25mm partial size, will be certain The coal dust of amount is put into moulded coal grinding tool, and moulded coal grinding tool is cylindrical.
7. coal petrography absorption deformation as claimed in claim 6 and porosity Simultaneous Determination method, which is characterized in that in step S3 Resistance strain gage conducting wire is connected with strain transducer, specifically includes the following steps:
S31: after resistance strain gage conducting wire is drawn by the resistance strain gage conducting wire outlet at the top of adsorption tanks, using epoxy resin Outlet is sealed, prevents high pressure gas from flowing out;
S32: the interface on adsorption tanks top resistive foil gauge conducting wire outlet connects the first solid state gas pressure sensor, measurement Methane gas pressure value in adsorption tanks.
8. coal petrography absorption deformation as claimed in claim 7 and porosity Simultaneous Determination method, which is characterized in that revolved in step S4 Turn platform, x-ray source and ray detector to the specific steps of coal sample different layers bit scan are as follows:
While S41:X radiographic source emits signal, rotating platform slowly rotates, and ray detector transmits data after receiving signal To data acquisition and analysis system, after the data of data acquisition and analysis system reception ray detector, data are analyzed, And then obtain the porosity of coal sample;
S42: the porosity of coal sample is averaged acquisition according to the porosity of coal sample upper surface, middle part cross section, lower end surface.
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