CN105300849B - The test device and method of gas diffusivity in a kind of porous media - Google Patents
The test device and method of gas diffusivity in a kind of porous media Download PDFInfo
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Abstract
The invention discloses the test device and method of gas diffusivity in a kind of porous media, the device it is main by clamper, gas sampling system, confined pressure pump, pressure balancing system, gas supply system, gas chromatographic analysis instrument and vacuum pump group into, the clamper two ends are all connected with the entrance point of gas sampling system, the port of export connection gas chromatographic analysis instrument and vavuum pump of gas sampling system, clamper two ends connect gas supply system respectively, are also connected with confined pressure pump and pressure balancing system；Clamper is made up of housing, sample bridge, sample chambers, plug, has confined pressure chamber in housing, sample bridge location is in clamper center, sample chambers storage porous media sample.Influence of the pressure oscillation to test result when the process eliminate osmotic flow in porous media of gas in test process and gas sample, effectively interference of the gas residue to test result in reduction sampling line.The principle of the invention is reliable, easy to operate, the degree of accuracy of surveyed diffusion coefficient is improved, with wide market prospects.
Description
Technical field
The present invention relates to the test device and method of gas diffusivity in molecular mass-transfer analysis field porous media, especially
Suitable for the measure device and method of gas-gas bi-component diffusion coefficient porous media.
Background technology
Molecule diffusion (referred to as spreading) is a phenomenon of nature generally existing, and it specifically refers to dense by material in system
Molecule is macroscopically showing the phenomenon of orientation transmission caused by degree difference.Coefficient of molecular diffusion (abbreviation diffusion coefficient) is reflection
The physical quantity of material diffusivity, the power for quantitatively portraying molecule diffusion under certain condition.Diffusion coefficient is in oil
And oil-gas migration research, the analysis of underground oil and gas reserve capacity, capability forecasting, Eor By Gas Injection and core in field of environmental engineering
Waste material and carbon dioxide all many-sides such as are buried and are all widely used.Therefore, diffusion coefficient is determined at grinding for above-mentioned each category
Study carefully work and actual production is all significant.
Now, the method for gas diffusivity can be divided into direct method and indirect method in test porous media.Wherein, direct method
By direct measurement different diffusion times or after the material concentration in lower diffusion system, expanded based on diffusion mathematical modeling
Dissipate the calculating of coefficient；Indirect method is by measuring diffusion system pressure, density etc. and concentration dependent indirect amount, and being converted
The determination of diffusion coefficient is realized based on diffusion mathematical modeling after concentration.Two class methods are both needed to the direct or indirect base of experiment collection
Plinth data, therefore the quality of relevant data acquisition device and flow and method will directly affect the test result of diffusion coefficient.
Although prior art has made certain work in terms of the diffusion coefficient measurement error in reducing gas porosity medium,
Still suffer from following deficiency：
(1) influence of osmosis of the gas in porous media to test result is not overcome
In terms of oil-gas migration research, gas injection improve gas deposit recovery efficiency and carbon dioxide is buried, elevated pressures are typically needed
Simulation underground actual conditions are diffused the measure of coefficient.It is logical to the porous media originally evacuated that the experiment starting stage opens valve
During gas, the unlatching of porous media two ends valve is difficult to true synchronization, and this asynchronism will drive gas pressure difference
Anisotonic flow is produced in porous media sample, the phenomenon does not need saturated liquid in Hi-pot test or some porous medias
In the case of will be apparent from.Because seepage flow speed is typically much higher than diffusion rate, therefore, this seepage discharge will mix with diffusing capacity
Together, test result is caused to significantly affect (the methods of professional standard SY/T 6129-1995；Qu Xiuying diffusion coefficients test skill
Art research [J] grand celebrations petroleum geology and exploitation, 2012,31 (4):46-49).
(2) in indirect method test process, existing sampling method brings error to test result
Need repeatedly to carry out chromatography concentration of component to gas sample in the air chamber at porous media two ends when indirect method is tested
Change, but such device announced at present can generally cause the air chamber pressure disturbance of porous media two ends when being sampled, from
And bring error to diffusion coefficient measurement.In addition, in multiple sampling analysis, in the pipeline being connected with gas composition analysis system
The last gas sampled remained analysis result next time can also be impacted (Chinese patent CN1773246A,
CN102980837B)。
To overcome the deficiency of existing device for testing diffusion coefficient and method, the present invention is proposed in a set of new porous media
The test device and method of gas diffusivity, belong to direct method class, available for more accurately measurement gas-gas bi-component many
Diffusion coefficient in the medium of hole.
The content of the invention
An object of the present invention is the test device for providing gas diffusivity in a kind of porous media, can exclude survey
Osmotic flow of the gas in porous media and influence of the pressure oscillation to test result during gas sample during examination, and can have
Interference of the gas residue to test result in effect reduction sampling line, with wide market prospects.
Another object of the present invention is also resided in offer and gas diffusivity in porous media is surveyed using said apparatus
The method of examination, this method principle is reliable, easy to operate, can effectively improve the degree of accuracy of surveyed diffusion coefficient, overcome existing skill
The defect and deficiency of art.
To reach above technical purpose, the present invention provides following technical scheme.
The test device of gas diffusivity in a kind of porous media, mainly by clamper, gas sampling system, constant temperature
Case, confined pressure pump, pressure balancing system, gas supply system, gas chromatographic analysis instrument and vacuum pump group into.
The clamper two ends are all connected with the entrance point of gas sampling system, and each gas sampling system is by pressure gauge, many
Pass joint and at least three gas sampling cells composition, the port of export connection gas chromatographic analysis instrument and vacuum of gas sampling system
Pump；Clamper two ends connect gas supply system respectively, and the gas supply system includes source of the gas and supercharger；Clamper also connects
Connect confined pressure pump and pressure balancing system.
The clamper is made up of housing, sample bridge, sample chambers, plug.There is confined pressure chamber in housing, confined pressure chamber connection
Confined pressure pump, can produce confined pressure, and sample bridge location is in the center of clamper, and its both sides is hollow on sample chambers, sample bridge
Passage has valve, and the break-make between sample chambers can be achieved；Sample chambers are used to deposit porous media sample, and sample chambers connection is stifled
Head, is realized by plug and blocked, and has diffuser casing and hollow channel in plug, hollow channel connects diffuser casing with plug two ends.
The clamper and gas sampling system are positioned in insulating box.
The insulating box is used to provide the temperature environment to be simulated of experiment, can need its constant inner space according to temperature
Temperature.
The confined pressure pump is used to produce the constant confining pressure needed for clamping sample.
The pressure balancing system is used for the balance for realizing gas pressure, can make its pressure at two ends balance in set pressure
Force value.
The gas supply system is used to provide the single-component gas needed for test, has supercharger to ensure to confess inside it
Gas has higher molar concentration (i.e. elevated pressures).
The gas chromatographic analysis instrument is connected with the gas sampling cell port of export, is transmitted for analyzing gas sampling cell
The component of gas sample.
The vavuum pump is used to vacuumize pipeline and space in communication, implements two functions：One is
Before ensureing that test starts, gas diffusion space in porous media sample internal void and device (including diffuser casing, gas sampling system
System and pipeline between them) it is vacuum state；The second is when reduction carries out gas composition analysis every time, last gas sample analysis
Afterwards, influence of the gas residue in pipeline to analysis result.
The method tested using said apparatus gas diffusivity in porous media, is comprised the following steps successively：
(1) two block size identicals porous media sample to be measured is chosen, its length and cross-sectional area are respectively l and s, Xiang Jia
Respectively load one piece of porous media sample in holder sample chambers；
(2) confined pressure is applied to clamper using confined pressure pump, using vavuum pump to the gas in porous media sample and device
Diffusion space is thoroughly evacuated；
(3) calorstat temperature temperature for needed for experiment is set, and it is constant to temperature to preheat each part；
(4) into porous media sample, supply is required to testing respectively for the source of the gas and supercharger connected using clamper two ends
Pressure, two ends gas is designated as X and Y respectively, and the pressure for making clamper two ends sample chambers with pressure balancing system reaches balance；
(5) open sample bridge valve and start diffusion process, and using the moment as diffusion initial time t0；
(6) clamper two ends gas is sampled simultaneously at regular intervals, respectively taken per sub-sampling two ends using a gas
Sample unit, the note ith sampling moment is ti；
(7) using the gas sample component in the sampling unit of gas chromatographic analysis instrument analysis clamper two ends, divide every time per one end
It is both needed to thoroughly evacuate the pipeline between gas sampling cell and gas chromatographic analysis instrument with vavuum pump before analysis component, X in note gas sample
It is c with Y component molar percentages one endLXiAnd cLYi, the other end is cRXiAnd cRYi, above step is repeated several times and reaches sampling analysis
Number of times requirement；
(8) according to the one-dimensional spread condition of Fick second laws, with reference to professional standard SY/T 6129-1995, following formula is utilized
Calculate the diffusion coefficient of gas X and Y in porous media：
In formula：DX、DY- it is respectively the diffusion coefficient of gas X and Y in porous media, m2/ s,
ΔcXi、ΔcYi- when being respectively ith sampling, X gas molar percentage differences is absolute in the sampling unit of two ends
The absolute value of value and Y gas molar percentage differences, %,
tiAt the time of-ith is sampled, s,
cLXi、cLYi- when being respectively ith sampling, gas X and Y molar percentage in the sampling unit of one end, %,
cRXi、cRYi- when being respectively ith sampling, gas X and Y molar percentage in other end sampling unit, %,
S-porous media specimen cross sectional area, m2,
L-porous media specimen length, m,
N-sampling number of times, dimensionless,
V0- single diffuser casing volume, m3,
Vu- single gas sampling cell volume, m3；
(9) with Mi(ti-t0) it is abscissa, with-ln (Δ cXi) it is ordinate, in rectangular coordinate system described point and use Linear Quasi
Close, the slope of gained straight line is DX, with Mi(ti-t0) it is abscissa, with-ln (Δ cYi) it is ordinate, retouched in rectangular coordinate system
Put and use linear fit, the slope of gained straight line is DY。
Compared with prior art, the beneficial effects of the present invention are：Surveyed present invention effectively prevents existing apparatus and method
When measuring diffusion coefficient of the gas in porous media, the influence that porous media osmosis is brought to measurement result, due to diffusion
General very little is measured, therefore the degree of accuracy of surveyed diffusion coefficient can be greatly improved on the exclusion that osmosis influences；In addition, of the invention
The pressure oscillation problem generally having when can also effectively overcome existing larger installations to sample, can further improve the standard of measurement result
True property；Meanwhile, relative to similar technique, some operations of the invention (such as test the ventilation at two ends and each gas color when starting
Analysis of spectrum etc.) need not synchronously it carry out, while experimenter's artificial disturbance is mitigated, also reduce the operation difficulty of experimenter.
The present invention can be used for oil-gas migration research, the analysis of underground oil and gas reserve capacity, capability forecasting, Eor By Gas Injection and
Carbon dioxide such as buries at the measure of oil and the diffusion coefficient involved by many research fields of environment-friendly engineering, and its measurement result is more
Accurately and reliably, with higher practical value.
Brief description of the drawings
Fig. 1 is a kind of structural representation of the test device of gas diffusivity in porous media.
Fig. 2 is the structural representation of clamper in Fig. 1.
Fig. 3 is that embodiment 1 is drawn on rectangular coordinate system-ln (Δ cXi) and Mi(ti-t0) data point and fitting a straight line.
Embodiment
The invention will be further described with reference to the accompanying drawings and examples.It should be pointed out that illustrating that the present embodiment is intended to pair
The present invention is further explained explanation, and is not intended to limit the present invention.
Referring to Fig. 1, Fig. 2.
The test device of gas diffusivity in a kind of porous media, mainly by clamper 1, gas sampling system, gas
Supply system, insulating box 10, confined pressure pump 2, pressure balancing system 11, gas chromatographic analysis instrument 14 and vavuum pump 15 are constituted, described
The two ends of clamper 1 are all connected with the entrance point of gas sampling system, each gas sampling system by gas sampling cell (5,6,7,8,
9), pressure gauge 4 and multiple-pass joint 3 are constituted, the port of export connection gas chromatographic analysis instrument 14 and vavuum pump 15 of gas sampling system；
Clamper two ends connect gas supply system respectively, and the gas supply system includes source of the gas 13 and supercharger 12；Clamper is also
Connect confined pressure pump 2 and pressure balancing system 11.
The clamper 1 is made up of housing 21, sample bridge 16, sample chambers 17, plug 19, there is confined pressure chamber 20 in housing,
Confined pressure chamber connection confined pressure pump 2, can produce confined pressure, sample bridge location is in the center of clamper, and its both sides is sample chambers 17,
Hollow channel on sample bridge has valve, and the break-make between sample chambers can be achieved；Sample chambers 17 connect plug 19, real by plug
Now block, there is diffuser casing 18 and hollow channel in plug, hollow channel connects diffuser casing with plug two ends.
The clamper and gas sampling system are positioned in insulating box 10.
Embodiment 1
Using the test device of gas diffusivity in the porous media, CO is tested2With CH4Spread in formation rock
When CH4Diffusion coefficient, be to note CO in certain gas field DAMAGE OF TIGHT SAND GAS RESERVOIRS2Improve gas reservoir natural gas (CH4) recovery ratio research offer base
Plinth parameter, the gas reservoir purpose stratum temperature and pressure is respectively 77 DEG C and 21.6MPa.Detailed step is as follows：
A) (including diffuser casing, the gas of gas diffusion space in attachment means and porous media sample interior hole and device
Sampling system and pipeline between them) evacuation process：
(A1) it is respectively that (i.e. cross-sectional area s is 5.07cm to 5cm and 2.54cm to choose two block length l and diameter d2) roundlet
Post rock sample, loads clamper 1 and assembles clamper 1；
(A2) 10 gas sampling cells are chosen, two gas sampling systems, and even good pipeline is assembled into；
(A3) 25MPa confined pressures are added to sample in clamper 1 by confined pressure pump 2；
(A4) using 15 pair of two gas sampling system of vavuum pump, porous media sample and between pipeline vacuumize 2 hours.
B) gas diffusion process in porous media, gas sampling and component analysis from different diffusion times：
(B1) it is 77 DEG C to set insulating box 10 temperature, and it is completely constant to temperature to preheat each part 2 hours；
(B2) by supercharger 12 to being maintained 1 hour after gas boosting in source of the gas 13 to 21.6MPa；
(B3) power supply of cut-in pressure bascule 11, balances the pressure of two ends diffusion space；
(B4) after after pressure at two ends balance, valve starts diffusion of the gas in rock core on opening valve sample bridge 16, remembers
The moment is recorded for initial time t0；
(B5) start after diffusion, gas was sampled and component analysis every 8 hours or so, specific method is：Every time
Two ends are sampled respectively using a gas sampling cell, and it is t to remember each sub-sampling momenti, subscript i is sampling ordinal number, during sampling simultaneously
Close this pair of gas sampling cell entrance point valves；Gas sampling cell outlet valve is successively opened after sampling (to beat each time
When opening outlet valve, the residue gas between gas sampling cell and gas chromatographic analysis instrument in pipeline need to be evacuated with vavuum pump 15
Body)；Then two ends gas sample component is analyzed one by one with gas chromatographic analysis instrument 14, when ith is sampled, CH in the gas sample of two ends4Component
Percentage is respectively cLYiAnd cRYi；
(B6) it is completed to 5 sub-samplings to test with analysis, test data record is shown in Table 1：
Table 1
C) gas diffusion coefficient in porous media is asked for, and method is as follows：
(C1) the equal sign left side is calculated based on the first formula in formula (1) and formula (2) and formula (3) to be respectively worth；
(C2) with Mi(ti-t0) it is abscissa, with-ln (Δ cXi) it is ordinate, according to calculated value in rectangular coordinate system described point
And with linear fit (such as Fig. 3), it is 2.042 × 10 to draw fitting a straight line slope-9, therefore CH4Diffusion coefficient in surveyed rock core
For 2.042 × 10-9m2·s-1。
Fit correlation is found out from Fig. 3, matching correlation R2For 99.87%, illustrate the test value and related reason of the device
It is fine by coincideing, further demonstrate the reliability and accuracy of method of testing of the present invention.
Claims (1)
1. the method tested using device gas diffusivity in porous media, the device is main by clamper (1), gas
Sampler body system, gas supply system, insulating box (10), confined pressure pump (2), pressure balancing system (11), gas chromatographic analysis instrument
(14) constituted with vavuum pump (15), clamper (1) two ends are all connected with the entrance point of gas sampling system, each gas sampling
System is made up of at least three gas sampling cells, pressure gauge (4) and multiple-pass joint (3), and the port of export of gas sampling system connects
Connect gas chromatographic analysis instrument (14) and vavuum pump (15)；Clamper two ends connect gas supply system, the gas supply respectively
System includes source of the gas (13) and supercharger (12)；Clamper is also connected with confined pressure pump (2) and pressure balancing system (11)；The clamping
Device (1) is made up of housing (21), sample bridge (16), sample chambers (17), plug (19), has confined pressure chamber (20) in housing, this encloses
Chamber connection confined pressure pump (2) is pressed, sample bridge location is in the center of clamper, and its both sides is on sample chambers (17), sample bridge
Hollow channel has valve；There are diffuser casing (18) and hollow channel in sample chambers (17) connection plug (19), plug；The clamping
Device and gas sampling system are positioned in insulating box (10)；This method comprises the following steps successively：
(1) two block size identicals porous media sample to be measured is chosen, its length and cross-sectional area are respectively l and s, to clamper
Respectively load one piece of porous media sample in sample chambers；
(2) confined pressure is applied to clamper using confined pressure pump, using vavuum pump to the gas diffusion in porous media sample and device
Space is thoroughly evacuated；
(3) calorstat temperature temperature for needed for experiment is set, and it is constant to temperature to preheat each part；
(4) source of the gas and supercharger connected using clamper two ends respectively into porous media sample, to needed for testing press by supply
Power, two ends gas is designated as X and Y respectively, and the pressure for making clamper two ends sample chambers with pressure balancing system reaches balance；
(5) open sample bridge valve and start diffusion process, and using the moment as diffusion initial time t0；
(6) clamper two ends gas is sampled simultaneously at regular intervals, per sub-sampling two ends respectively using a gas sample list
Member, the note ith sampling moment is ti；
(7) using the gas sample component in the sampling unit of gas chromatographic analysis instrument analysis clamper two ends, every time per one end analysis group
It is both needed to thoroughly evacuate the pipeline between gas sampling cell and gas chromatographic analysis instrument with vavuum pump before point, X and Y groups in note gas sample
It is c to divide molar percentage one endLXiAnd cLYi, the other end is cRXiAnd cRYi, above step is repeated several times and reaches sampling analysis number of times
It is required that；
(8) diffusion coefficient of gas X and Y in porous media is calculated using following formula：
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In formula：DX、DY- it is respectively the diffusion coefficient of gas X and Y in porous media, m2/ s,
cLXi、cLYi- when being respectively ith sampling, gas X and Y molar percentage in the sampling unit of one end, %,
cRXi、cRYi- when being respectively ith sampling, gas X and Y molar percentage in other end sampling unit, %,
S-porous media specimen cross sectional area, m2,
L-porous media specimen length, m,
N-sampling number of times, dimensionless,
V0- single diffuser casing volume, m3,
Vu- single gas sampling cell volume, m3；
(9) with Mi(ti-t0) it is abscissa, with-ln (Δ cXi) it is ordinate, in rectangular coordinate system described point and linear fit is used, institute
The slope for obtaining straight line is DX, with Mi(ti-t0) it is abscissa, with-ln (Δ cYi) it is ordinate, in rectangular coordinate system described point simultaneously
With linear fit, the slope of gained straight line is DY。
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| CN105300849A (en) | 2016-02-03 |
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