CN105259080A - Shale gas reservoir gas diffusion coefficient experiment test method - Google Patents

Shale gas reservoir gas diffusion coefficient experiment test method Download PDF

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CN105259080A
CN105259080A CN201510767852.8A CN201510767852A CN105259080A CN 105259080 A CN105259080 A CN 105259080A CN 201510767852 A CN201510767852 A CN 201510767852A CN 105259080 A CN105259080 A CN 105259080A
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gas
pressure
shale
rock sample
methane
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CN201510767852.8A
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康毅力
杨斌
游利军
李相臣
陈一健
陈明君
梁李
陈强
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西南石油大学
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Abstract

The invention discloses a shale gas reservoir gas diffusion coefficient experiment test method. According to a method, a one-dimensional diffusion mathematic model is built by monitoring pressure attenuation data in a shale plunger rock sample under effective stress conditions of methane gas with a certain initial pressure in a constant-temperature closed system with the micro-pore structure and the gas existence state of a shale reservoir as bases, the diffusion coefficient of the gas (methane) in shale is calculated, and the diffusion mass-transfer capacity of the gas (methane) in the shale is quantitatively assessed. In the experiment testing process, the diffusion process of gas in the shale gas reservoir can be effectively simulated, and influences of effective stress, gas adsorption/desorption and other factors on the diffusion coefficient are reflected. Besides, the method can overcome influences of gas free expansion stage data in a traditional adsorption/desorption method on the diffusion coefficient. The method can assess the diffusion mass-transfer capacity of the gas in the shale and provide experiment support for researches in the aspects of shale gas reservoir productivity models, productivity prediction and the like.

Description

A kind of shale gas reservoir gas diffusivity experimental test procedures
Technical field
The present invention relates to unconventionaloil pool reservoir gas mass transfer capacity experimental evaluation method technical field, is a kind of simulation shale gas reservoir gas (methane) diffusion process, the experimental technique of test coefficient of diffusion.
Background technology
Shale gas is typical Unconventional forage, originates from extremely low hole and oozes, and preserves in series of rocks based on rich organic shale, belongs to hydrocarbon source rock gas reservoir.China's shale gas mining resources amount is about 25.08 × 10 12m 3, suitable with conventional gas stock number.In shale gas reservoir, shale gas is mainly composed with free state and ADSORPTION STATE and is deposited.After gas well opening well and making production, free gas is output first; Simultaneously along with the transmission of pressure wave, the adsorbed gas in the organic hole of shale can desorb gradually, and forms a concentration gradient; Under the effect of concentration gradient, the adsorbed gas of pore interior can carry out diffusion mass transfer to the low concentration region starting desorb gradually.Thus, the output process of shale gas is a multiple dimensioned mass transport process containing desorb, diffusion and seepage flow.Shale gas not only controls the output speed of adsorbed gas in organic inner diffusion process, and also appreciable impact adsorbed gas is to the contribution proportion of whole gas well deliverability.Gas diffusibility in research shale matrix, contributes to the multiple dimensioned output mechanism of clear and definite shale gas, sets up and be applicable to shale gas well capacity model.
The key parameter evaluating gas diffusivity power in rock is gas diffusivity.But the current acquisition about gas diffusivity in shale mainly fits the method for theoretical calculation by computer mould, also lack test support accordingly in productivity model for the value of coefficient of diffusion.Cause the reason of this predicament mainly not clear to the understanding of gas diffusion process in shale, existing coefficient of diffusion experimental test procedures is difficult to effectively reflect the diffusion process of shale gas in reservoir, and obtains reliable experimental result.
Existing measurement gas mainly contains time lag method, hydrocarbon concentration method and adsorption/desorption method in the method for diffusion coefficient of rock.Time lag method and hydrocarbon concentration method are often applied to Gas diffusion migration in reservoir rock and the closure research of supracrustal rocks.What time lag method was tested is under rock saturation water condition, and in unit rock under water-soluble hydrocarbon concentration gradient, rock gas is by the coefficient of diffusion of rock.But the water saturation of shale gas reservoir is extremely low or not moisture under it has been generally acknowledged that original place condition, thus the method inapplicable.The test of hydrocarbon concentration method be the coefficient of diffusion of certain component in the relative diffusion process of the lower pair component gases of pressure-balanced condition, the method adopts dry rock sample usually, but needs repeatedly to sample in test process, very easily causes larger experimental implementation error.Meanwhile, time lag method and hydrocarbon concentration method all do not consider the impact of adsorbed gas, and in experimental simulation process and shale gas output, the diffusion process of gas differs greatly, and is difficult to be applied to the experiment test of gas diffusivity in shale.
Adsorption/desorption method test coefficient of diffusion is applied comparatively wide in coal-seam gas, and the method calculates coefficient of diffusion by the response curve analyzing adsorbance and concentration or pressure change, can fully demonstrate the adsorption/desorption-diffusion process of gas at rock interior.But adsorption/desorption method also has the following disadvantages: first, adopt pulverized specimen (60 ~ 80 order) to test, characterize yardstick minimum, and the coefficient of diffusion recorded is by the size impact of sample; Secondly, pulverized specimen sample preparation is loaded down with trivial details, and cannot reflect that effective stress changes the impact on pore texture and diffusion process.
In addition, in the research of the porosints such as molecular sieve, the methods such as distance of zero mark post (ZLC) chromatography, frequency response method, Pulsed-field gradient NMR and the scattering of pseudo-elastic approximation seed are also applied to the test of coefficient of diffusion.But they or experiment condition and engineer applied very different, or instrument and equipment complex and expensive, be difficult to popularize.
To sum up, the coefficient of diffusion size of shale gas in reservoir evaluates gas diffusion mass transfer ability power in shale, optimize the key parameter of productivity model and prediction adsorbed gas output degree, in the face of the deficiency that existing experimental test procedures exists, need badly and explore a kind of coefficient of diffusion method of testing that shale gas actual dispersion process and being easy in reservoir operates that can reflect.
Summary of the invention
For the deficiency of existing coefficient of diffusion experiment test means, provide a kind of newly can simulate effective stress condition, the coefficient of diffusion experimental test procedures of gas actual dispersion process in reflection shale gas reservoir.Under first the method needs monitoring constant temperature constant volume condition, gas (methane) is to the decline of pressure process in effective stress state lower plunger shale, extract and wherein reflect the data of gas in the organic concentration inside diffusion of shale, coefficient of diffusion asked for by the one dimension diffusion model according to setting up.
The present invention has following advantage compared with existing method:
(1) experimental test procedures is the inverse process of shale gas reservoir gas output, can to greatest extent reduction adsorption gas output time in the organic inner desorb-diffusion process of shale;
(2) compare pulverized specimen test, this method adopts plunger rock sample, not only can be applied with efficacy, can also reflect the impact of microcellular structure on diffusion process more all sidedly;
(3) compare existing adsorption/desorption method, this method eliminates the decline of pressure data in gas free expansion stage based on rock sample parameter, eliminates the impact that it calculates coefficient of diffusion.
Object of the present invention is achieved through the following technical solutions:
First drill through, cut shale rock sample, fully dry (60 DEG C) to constant weight, measure its length, diameter and factor of porosity; First pick-up unit impermeability before experiment, calibrates the dead volume of pipeline again; Then experiment rock sample is put into clamper, default temperature and confined pressure are applied to system; After temperature, pressure is stable, more than 72h is vacuumized to rock sample and pipeline; Then pass into methane gas to small intermediate receptacle, treat that methane gas is preheated to system temperature, and pressure stability is after preset value, opens corresponding operation valve, methane starts to flow in rock core, starts the decline of pressure data gathering whole chamber simultaneously; Treat that system pressure 24h internal drop is less than 2KPa, think that the decline of pressure process of gas reaches approximate equilibrium (more than 100h), data acquisition terminates.
After obtaining decline of pressure curve, first the methane mass that can store in rock sample hole under experimental temperature pressure condition should be asked for according to the size of rock sample and factor of porosity, and as reference, reject in decline of pressure curve and reflect the data of premature gas to the free expansion stage in rock sample.After this stage, the methane entering rock sample is mainly deposited with the tax of the form of ADSORPTION STATE, and by concentration diffusion to organic inner migration.The decline of pressure data of this process are substituted into one dimension coefficient of diffusion computation model, gas (methane) coefficient of diffusion in shale can be tried to achieve.
Accompanying drawing explanation
Fig. 1 coefficient of diffusion experiment test device schematic diagram.
In figure: 1-6. operation valve, 7. gas cylinder, 8. small intermediate receptacle, 9. vacuum pump, 10. core holding unit, 11. confined pressure pumps, 12. pressure transducers, 13. constant temperature temperature control systems, 14. data acquisition system (DAS)s.
The decline of pressure curve of Fig. 2 experimental test procedures gas (methane).
The decline of pressure data linear regression of Fig. 3 gas (methane) diffusion process.
Embodiment
The present invention is further illustrated below according to example.
Choose 1 piece, Sichuan Basin Longma small stream group shale plunger rock sample, adopt the inventive method test gas (methane) coefficient of diffusion in shale.Concrete steps are as follows:
Step 1, prepare plunger shale rock sample (LMX-1) according to SYT5358-2010 rock sample preparation method; First adopting nitrogen to drill through also cutting diameter is 2.52cm, and length is the shale rock sample of 3.93cm, then puts into the baking oven of 60 DEG C, weighs once every 24h, and change of weighing for twice until adjacent is less than 1.0% of sample quality, thinks that rock sample is fully dried; It is 4.06% that rock sample after oven dry adopts CMS300 to test rock sample factor of porosity;
Step 2, steel rock sample (factor of porosity is zero) to be loaded in core holding unit, and apply certain confined pressure, open constant temperature temperature control system, after system temperature is heated to design temperature T, demarcate steel rock sample end face to the whole spatial volume (V between operation valve 1 and operation valve 3 d), scaling method is: closed control valve 1, opens operation valve 2-4, starts vacuum pump and vacuumizes more than 2h to internal system, then closed control valve 3, and close down vacuum pump; By the volumetric standard that injects certain pressure helium, (known volume is V r) be connected to operation valve 1, after pressure stability in volumetric standard, record pressure P 1; Open operation valve 1, after internal system pressure stability, record pressure P now 2; Rock sample end face can be tried to achieve to the whole spatial volume V between operation valve 1 and operation valve 3 according to equation (1) dfor 58.8362cm 3;
V D = ( P 1 Z 2 P 2 Z 1 - 1 ) V R - - - ( 1 )
V in formula d-rock sample end face to the whole spatial volumes between operation valve 1 and operation valve 3, cm 3;
V r-volumetric standard volume, cm 3;
Z 1, Z 2-be respectively pressure P 1, P 2the deviation factors of lower helium, zero dimension;
Step 3, by steel rock sample load core holding unit, and apply preset confined pressure 10MPa and temperature 82 DEG C; In system, pass into the helium (air-leakage test pressure is higher than experimental pressure) that certain pressure is 3MPa, in closed control valve 1 and operation valve 3,24h, pressure system pressure drop is less than 0.5KPa, illustrates that impermeability well reaches requirement of experiment;
After step 4, air-leakage test, take out steel rock sample, load shale plunger rock sample to be analyzed, again apply default confined pressure 10MPa and temperature 82 DEG C by confined pressure pump 11 and constant temperature temperature control system 13, and keep confined pressure and temperature constant; Then closed control valve 1, opens operation valve 2-4, and unlatching vacuum pump 9 pairs of rock samples and pipeline system vacuumize 72h; Then closed control valve 2-4, opens operation valve 1, passes into a certain amount of gas (methane) to small intermediate receptacle 8, rises to after preset pressure, closed control valve 1 until pressure of methane; When the methane gas passed into is preheated to system temperature, and after pressure remained steady, now gaseous tension is 1420KPa, opens operation valve 2, records the gaseous tension attenuation data of methane to rock sample flow process by pressure transducer 12 and data acquisition system (DAS) 14 simultaneously; Treat that system pressure 24h internal drop is less than 2KPa, think that gaseous tension reaches balance; As shown in Figure 2, pressure balance time is got in this experiment is 100h;
Step 5, methane flow in the rock sample fully vacuumized, and first gas can be full of hole in shale and microfracture system by free expansion, and then methane can be adsorbed on the organic nano-pore wall in shale further; Adsorbed gas, under the effect of concentration gradient, spreads to organic inside gradually; In view of the Analysis On Multi-scale Features of gas flowing in shale, the decline of pressure packet of monitoring contains early stage methane to the free expansion stage in rock sample hole, and in the computation process of coefficient of diffusion, need to remove this phase data; Concrete processing procedure is as follows, and the quality that t free expansion enters the methane of rock sample can be tried to achieve by equation (2):
m e x ( t ) = V D M w R ( P i n i Z i n i T i n i - P ( t ) Z ( t ) T ( t ) ) - - - ( 2 )
M in formula ext the free expansion of ()-t enters the quality of the methane of rock sample, i.e. accumulative gas-storing capacity this moment, g;
M w-gas molar quality, g/mol;
R-mol gas constant, J/ (molK);
P ini, P (t)-system initial time and t pressure, MPa;
T ini, T (t)-test macro temperature, keep constant temperature, T iniequal with T (t), K;
Z ini, the deviation factor for gas of Z (t)-initial time and t, dimensionless;
Under step 6, same temperature pressure condition, the quality required for volume of voids that methane is full of experiment rock sample can be calculated by following formula:
m P = V P M w R P Z P T - - - ( 3 )
M in formula pthe gas-storing capacity of rock sample volume of voids under-a certain temperature, pressure, g;
V p-rock sample volume of voids (by rock sample size and porosity calculation), cm 3;
(because in experiment, gaseous tension attenuation amplitude is less than 10%, it is initial for being similar to and getting P to P-methane gas pressure
The mean pressure of moment and t), MPa;
T-test macro temperature, K;
Z pdeviation factor for gas under-temperature T, pressure P, dimensionless;
Step 7, according to the rock sample parameter of this experiment and temperature, pressure parameter etc., when the methane mass entering rock sample meets equation (4), the i.e. decline of pressure process initial stage, methane gas has been filled with the moment t=11.92h of rock sample hole, think that methane starts, at hole wall adsorption with under concentration gradient effect, to carry out gas diffusion (Fig. 2) to organic inside after carving at this moment;
m ex(t)=m P(4)
Step 8, occurrence status according to adsorbed gas in shale, be reduced to one-dimensional linear diffusion by adsorbed gas in shale to organic inner diffusion process; Obtain according to Fick's second law and the principle of mass conservation:
∂ 2 c g ∂ z 2 = 1 D ∂ c g ∂ t - - - ( 5 )
Starting condition: c g(z, t=0)=0 (6)
Boundary condition: ∂ c g ∂ z | z = h = 0 - - - ( 7 )
c g ( z = 0 , t ) = c g *
Above-mentioned mathematical model is solved, following analytic expression can be obtained:
M t M ∞ = 8 π 2 [ 1 - exp ( - Dπ 2 4 h 2 t ) ] - - - ( 8 )
M in formula t, M -t and balance moment diffuse into organic inner methane mass, g;
D-methane to organic inner effective diffusion cofficient, cm 2/ s;
H-gas can diffuse into the mean depth in kerogen, nm;
C * g-hole wall adsorbed gas concentration (assuming that concentration value keeps constant), mol/cm 3;
Equation (8) is out of shape and gets natural logarithm, can obtain following expression:
l n ( 1 - π 2 8 M t M ∞ ) = - Dπ 2 4 h 2 t - - - ( 9 )
Equation (9) is the linear function about time t, according to test philosophy, after getting the t=11.92h moment, the pressure before equilibration time and time data make the graph of a relation of the equation left side and t, then the slope l that linear regression obtains fitting a straight line is-0.00000521 (Fig. 3); Under can trying to achieve confined pressure 10MPa, gas original pressure (methane) 1420KPa, temperature 82 DEG C of conditions according to equation (10), the diffusion coefficient D of methane methane in shale is 2.89 × 10 -17cm 2/ s.
- Dπ 2 4 h 2 = l - - - ( 10 )
Above embodiment has carried out concrete description to method of the present invention, but content of the present invention is not restricted to above case study on implementation, as long as not exceeding in main scope of the present invention, can change flexibly experiment condition and method.

Claims (3)

1. a shale gas reservoir gas diffusivity experimental test procedures, it comprises the following steps:
Step 1, prepare plunger shale rock sample according to SYT5358-2010 rock sample preparation method; First adopting nitrogen to drill through also cutting diameter is 2.54cm, and length is the shale rock sample of 3 ~ 4cm, then puts into the baking oven of 60 DEG C, weighs once every 24h, and change of weighing for twice until adjacent is less than 1.0% of sample quality, thinks that rock sample is fully dried; Rock sample after oven dry adopts CMS300 instrument connection porosity;
Step 2, steel rock sample (factor of porosity is zero) to be loaded in core holding unit, and apply certain confined pressure, open constant temperature temperature control system, after system temperature is heated to design temperature T, demarcate steel rock sample end face to the whole spatial volume (V between operation valve 1 and operation valve 3 d), scaling method is: closed control valve 1, opens operation valve 2-4, starts vacuum pump and vacuumizes more than 2h to internal system, then closed control valve 3, and close down vacuum pump; By the volumetric standard that injects certain pressure helium, (known volume is V r) be connected to operation valve 1, after pressure stability in volumetric standard, record pressure P 1; Open operation valve 1, after internal system pressure stability, record pressure P now 2; Rock sample end face can be tried to achieve to the whole spatial volume V between operation valve 1 and operation valve 3 according to following formula d:
V in formula d-rock sample end face to the whole spatial volumes between operation valve 1 and operation valve 3, cm 3;
V r-volumetric standard volume, cm 3;
Z 1, Z 2-be respectively pressure P 1, P 2the deviation factors of lower helium, zero dimension;
Step 3, by steel rock sample load core holding unit, and apply preset confined pressure and temperature; In system, pass into the helium of certain pressure, closed control valve 1 and operation valve 3, if system pressure pressure drop amplitude in 24h is less than 0.5KPa, then illustrate that impermeability well reaches requirement of experiment; Air-leakage test pressure is higher than experimental pressure;
After step 4, air-leakage test, take out steel rock sample, load shale plunger rock sample to be analyzed, again apply default confined pressure and temperature by confined pressure pump 11 and constant temperature temperature control system 13; Then closed control valve 1, opens operation valve 2-4, and unlatching vacuum pump 9 pairs of rock samples and pipeline system vacuumize more than 72h; Then closed control valve 2-4, opens operation valve 1, passes into a certain amount of gas (methane) to small intermediate receptacle 8, rises to after preset pressure, closed control valve 1 until pressure of methane; When the methane gas passed into is preheated to system temperature, and after pressure remained steady, open operation valve 2, record the gaseous tension attenuation data of methane to rock sample flow process by pressure transducer 12 and data acquisition system (DAS) 14 simultaneously; Treat that system pressure 24h internal drop is less than 2KPa, think that gaseous tension reaches balance (more than 100h);
Step 5, methane flow in the rock sample fully vacuumized, and first gas can be full of hole in shale and microfracture system by free expansion, and then methane can be adsorbed on the organic nano-pore wall in shale further; Adsorbed gas, under the effect of concentration gradient, spreads to organic inside gradually; In view of the Analysis On Multi-scale Features of gas flowing in shale, the decline of pressure packet of monitoring contains early stage methane to the free expansion stage in rock sample hole, and in the computation process of coefficient of diffusion, need to remove this phase data; Concrete processing procedure is as follows, and the quality that t free expansion enters the methane of rock sample can be tried to achieve by equation (2):
M in formula ext the free expansion of ()-t enters the quality of the methane of rock sample, i.e. accumulative gas-storing capacity this moment, g;
M w-gas molar quality, g/mol;
R-mol gas constant, J/ (molK);
P ini, P (t)-system initial time and t pressure, MPa;
T ini, T (t)-test macro temperature, keep constant temperature, T iniequal with T (t), K;
Z ini, the deviation factor for gas of Z (t)-initial time and t, dimensionless;
Under step 6, same temperature pressure condition, the quality required for volume of voids that methane is full of experiment rock sample can be calculated by following formula:
M in formula pthe gas-storing capacity of rock sample volume of voids under-a certain temperature, pressure, g;
V p-rock sample volume of voids (by rock sample size and porosity calculation), cm 3;
(because in experiment, gaseous tension attenuation amplitude is less than 10%, it is initial for being similar to and getting P to P-methane gas pressure
The mean pressure of moment and t), MPa;
T-test macro temperature, K;
Z pdeviation factor for gas under-temperature T, pressure P, dimensionless;
Step 7, at a time t, when the methane mass entering rock sample meets equation (4), namely think that, at the decline of pressure process initial stage, methane gas has been filled with rock sample hole; After t, methane starts with hole wall adsorption with under concentration gradient effect, is main to organic inner diffusion process;
m ex(t)=m P(4)
Step 8, occurrence status according to adsorbed gas in shale, be reduced to one-dimensional linear diffusion by adsorbed gas in shale to organic inner diffusion process; Obtain according to Fick's second law and the principle of mass conservation:
Starting condition: c g(z, t=0)=0 (6)
Boundary condition:
Above-mentioned mathematical model is solved, following analytic expression can be obtained:
M in formula t, M -t and balance moment diffuse into organic inner methane mass, g;
D-methane to organic inner effective diffusion cofficient, cm 2/ s;
H-gas can diffuse into the mean depth in kerogen, nm;
C * g-hole wall adsorbed gas concentration (assuming that concentration value keeps constant), mol/cm 3;
Equation (8) is out of shape and gets natural logarithm, can obtain following expression:
Equation (9) is the linear function about time t, and experimentally data make the graph of a relation of the equation left side and t, then linear regression obtains the slope l of fitting a straight line; The diffusion coefficient D of methane methane in shale under a certain temperature, pressure condition can be tried to achieve according to equation (10).
2. a kind of shale gas reservoir gas diffusivity experimental test procedures according to claim 1, it is characterized in that: laboratory sample is plunger rock sample, under effective stress effect can being simulated in comparatively large scale, in shale gas reservoir during adsorbed gas output in organic inner desorb-diffusion process.
3. a kind of shale gas reservoir gas diffusivity experimental test procedures according to claim 1, it is characterized in that: the decline of pressure data eliminating the gas free expansion stage based on rock sample parameter, eliminate the impact that non-diffusing phase data calculates organic internal gas coefficient of diffusion.
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CN108663186A (en) * 2017-03-28 2018-10-16 中国石油化工股份有限公司 The device and method of gas transfer between test sheets cleft and matrix
CN108663186B (en) * 2017-03-28 2020-09-01 中国石油化工股份有限公司 Device and method for testing gas mass transfer between shale fracture and matrix
CN108801860A (en) * 2017-05-02 2018-11-13 中国石油化工股份有限公司 A method of measuring diffusion coefficient of the carbon dioxide in crude oil
CN108801860B (en) * 2017-05-02 2021-01-01 中国石油化工股份有限公司 Method for measuring diffusion coefficient of carbon dioxide in crude oil
CN107461192A (en) * 2017-06-01 2017-12-12 西南石油大学 Shale dynamic table sees the computational methods of permeability under reservoir conditions
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CN107144625A (en) * 2017-06-23 2017-09-08 国家地质实验测试中心 Gas hydrates drill core light hydrocarbon gas content parses test system and method
CN107702999A (en) * 2017-11-13 2018-02-16 中国科学院地质与地球物理研究所 Miniature hydraulic pressure-break net quantitative testing device and method
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Application publication date: 20160120