CN102980837B - Hydro carbons diffusion coefficients equipment and assay method in rock under High Temperature High Pressure - Google Patents
Hydro carbons diffusion coefficients equipment and assay method in rock under High Temperature High Pressure Download PDFInfo
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- CN102980837B CN102980837B CN201210465895.7A CN201210465895A CN102980837B CN 102980837 B CN102980837 B CN 102980837B CN 201210465895 A CN201210465895 A CN 201210465895A CN 102980837 B CN102980837 B CN 102980837B
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Abstract
To the invention provides under High Temperature High Pressure hydro carbons diffusion coefficients equipment and assay method in rock.This equipment mainly comprises rock diffusion coefficient analyzer, vacuum pump, confined pressure force (forcing) pump, hydro carbons source of the gas, N
2source of the gas, left piston container, right piston container, Self-pressurizing agri pump, chromatogram detector, computing machine, drying unit, rock saturation water device etc.The gas injection equalized pressure that this equipment and assay method can realize core holding unit two ends diffuser casing remains accurately consistent, guarantee not exist in whole experimentation the driving of pressure gradient and only there is concentration gradient and drive lower hydro carbons to spread, the gas injection equalized pressure simultaneously solving source of the gas equalized pressure opertaing device in conventional diffusion coefficients is less, the relatively low problem that there are differences with actual formation condition of experimental temperature.
Description
Technical field
The present invention relates to hydro carbons diffusion coefficients experimental facilities and assay method in a kind of rock, to particularly relate under a kind of high-temperature and high-pressure conditions hydro carbons diffusion coefficients experimental facilities and assay method in rock, belong to the Natural Gas Geology analysis technical field in technical field of petroleum extraction.
Background technology
Diffusion refers to that hydrocarbon gas is under concentration gradient effect, and gas molecule reaches a kind of physical process of balance to low concentration region free migration by various medium from high concentration region.Diffusion is one of important mechanism of oil-gas migration, it is for oil gas, and particularly rock gas is (because molecule is little, lightweight, activity is strong, so have stronger diffusivity in underground) migration, assemble poly-, become to hide, preserve and destroyed most important effect.For the gas reservoir assembled, except the impact of cap rock Self-Closing ability, tomography, supracrustal rocks are the most important factor affecting gas reservoir Late reformation, destruction for the diffusivity of hydro carbons; But, except as the traditional destructive factor of routine, be diffused in gas migration, gathering and Filling process and also may produce positive role and contribution, especially in fields such as unconventional tight sand, shale gas.Coefficient of diffusion, as describing the important evaluating of rock gas by rock rate of propagation speed, is that Gas diffusion charging amount and windage calculate requisite important parameter.At present, experimental determination coefficient of diffusion adopts indirect method, namely passes through diffusing capacity or the concentration of sample in measuring certain hour, then by these measured values by determining someway or trying to achieve diffusion coefficient value.The coefficient of diffusion that routine records is owing to limiting by experiment Temperature-pressure Conditions and Geologic Time, deviation is there is with the real diffusivity of rock under actual geologic condition, and along with buried depth increase, compacting diagenesis's effect strengthen in the geologic epoch, diffusion coefficient of natural gas is also different in the different geologic epoch.As can be seen here, at utmost measure rock hydro carbons coefficient of diffusion close to actual geology high-temperature and high-pressure conditions, for hydro carbons diffusivity in accurate evaluation rock, assessment Gas diffusion charging amount and diffusion loss amount, carry out the migration of routine, very rock gas, gathering, one-tenth hides and preservation is studied and resource evaluation all has effect of crucial importance.
Domestic and international laboratory rock hydro carbons diffusion coefficients is mainly at normal temperature, normal pressure (room temperature 22 DEG C, 0.2MPa gas injection equalized pressure at present, 3MPa confined pressure) carry out under condition, and existing diffusion coefficients device many employings precision pressure gauges etc. control two ends diffuser casing gas injection equalized pressure, can not ensure that two ends diffuser casing gas injection equalized pressure remains identical well, the small pressure reduction of easy generation, thus can not ensure that whole experimentation only has concentration gradient drive and do not have pressure gradient completely; In addition, under general less and the relatively low and actual geologic condition of experimental temperature of the gas injection equalized pressure controlled due to the bleed pressure opertaing device of routine rock be in the earth formation saturated local water, high temperature, high pressure state there is larger difference, the diffusivity that rock hydro carbons is real under geologic condition can not be reflected preferably.Therefore, be necessary to transform existing equipment and provide a kind of High Temperature High Pressure rock hydro carbons diffusion coefficients experimental facilities to overcome above-mentioned technical matters.
Summary of the invention
For solving the problems of the technologies described above, to the object of the present invention is to provide under a kind of high-temperature and high-pressure conditions hydro carbons diffusion coefficients experimental facilities and assay method in rock.This experimental facilities and assay method can to measure under high-temperature and high-pressure conditions hydro carbons coefficient of diffusion in rock convenient, fast, accurately and efficiently, for carrying out Gas diffusion charging amount, windage evaluation and carrying out routine or Unconventional forage fortune is poly-, become to hide, preserve and resource evaluation research provides the Data support of science.
For reaching above-mentioned purpose, to the invention provides under a kind of high-temperature and high-pressure conditions hydro carbons diffusion coefficients experimental facilities in rock, it is characterized in that, this equipment comprises rock diffusion coefficient analyzer, vacuum pump, confined pressure force (forcing) pump, hydro carbons source of the gas, N
2source of the gas, left piston container, right piston container, Self-pressurizing agri pump, chromatogram detector, computing machine, drying unit, rock saturation water device;
Wherein, described rock diffusion coefficient analyzer comprises constant temperature oven, core holding unit and temperature controller;
Described core holding unit is positioned at described constant temperature oven, for placing sample, and is separated into left diffuser casing and right diffuser casing by sample;
Described temperature controller is connected with described constant temperature oven;
Described confined pressure force (forcing) pump is connected with described core holding unit, adopts the mode of hydraulic pressure to the confined pressure under core holding unit loading simulation formation condition;
Described chromatogram detector is connected with described right diffuser casing with described left diffuser casing respectively by pipeline, the pipeline that described left diffuser casing is connected with chromatogram detector is provided with left sample valve, the pipeline that described right diffuser casing is connected with chromatogram detector is provided with right sample valve, and described chromatogram detector is for detecting hydro carbons in the left diffuser casing of rock diffusion coefficient analyzer and N
2concentration change situation, and hydro carbons and N in right diffuser casing
2concentration change situation;
Described computing machine is connected with described chromatogram detector, runs for controlling chromatogram detector and records and store raw data;
Described vacuum pump is connected with two ends, described rock diffusion coefficient analyzer left and right respectively by pipeline, described pipeline is provided with vacuum pump operation valve, for vacuumizing pipeline, being single, pure hydro carbons to ensure in the left diffuser casing of diffusion coefficients initial time, is single, pure N in right diffuser casing
2gas;
Described left piston container and described right piston container dimensional size be connected identical, two-piston container includes piston, fluid pressurization cylinder and cylinder;
The cylinder of described left piston container is connected with described left diffuser casing by pipeline, described pipeline is provided with left piston container operation valve and left diffuser casing operation valve, wherein, described left piston container operation valve is arranged on the pipeline of left piston container, and described left diffuser casing operation valve is arranged on the pipeline of left diffuser casing; The cylinder of described right piston container is connected with right diffuser casing by pipeline, described pipeline is provided with right piston container operation valve and right loose room operation valve, wherein, described right piston container operation valve is arranged on the pipeline of right piston container, and described right diffuser casing operation valve is arranged on the pipeline of right diffuser casing;
Described hydro carbons source of the gas is connected by the side of pipeline with the cylinder of described left piston container, and described pipeline is provided with left air source control valve; Described N
2source of the gas is connected by the side of pipeline with the cylinder of described right piston container, and described pipeline is provided with right air source control valve;
Described Self-pressurizing agri pump is connected with the fluid pressurization cylinder of described left piston container and described right piston container respectively by pipeline.
In above-mentioned experimental facilities, described hydro carbons source of the gas can be the one-component gas source of the gas hydro carbons such as methane gas source, ethane source of the gas, propane source of the gas, butane source of the gas or pentane source of the gas.
In above-mentioned experimental facilities, left piston container and right piston container can be stainless steel, and volume is 20L, maximum working pressure (MOP) 30MPa.
In above-mentioned experimental facilities, described core holding unit can be conventional high temperature high voltage resistant core holding unit, and its bearing capacity is not less than 50MPa, and temperature tolerance is not less than 150 DEG C.Each pipeline is conventional high temperature high voltage resistant pipeline, is stainless steel.Described drying unit can be conventional baking apparatus, and be preferably baking oven, it is for the oven dry of sample.Described rock saturation water device can be conventional saturation water device, and it is mainly used in the saturated local water carried out according to actual geologic condition the sample after drying under simulation stratum condition.
In above-mentioned experimental facilities, described Self-pressurizing agri pump built with pressurized liquid, and is provided with the setting device of gas injection equalized pressure and constant supercharging flow velocity; Pressurized liquid promotion piston compression gas boosting is injected by the fluid pressurization cylinder constant speed of mode to left piston container and right piston container of setting gas injection equalized pressure and constant supercharging flow velocity, and finally realize left piston container, gas injection equalized pressure that right piston container reaches identical setting, thus ensure that rock core accommodates the left diffuser casing in device, right diffuser casing all has identical gas injection equalized pressure, ensure that hydro carbons only exists the diffusion under concentration gradient effect and there is not the diffusion under pressure gradient effect.
The direction term mentioned in the present invention such as: left and right etc., is only the direction with reference to accompanying drawing.Therefore, the direction term of use is used to illustrate and is not used for limiting the present invention.
The present invention also to provide under a kind of high-temperature and high-pressure conditions hydro carbons diffusion coefficients method in rock, and it comprises the following steps:
A. rock sample is made that diameter is 2.5cm, length is the small cylinder of 0.5-0.6cm, and conventional orifices porosity is carried out to sample, permeability detects;
B. described sample is put into drying unit, dry more than 8h, until constant weight, wherein, bake out temperature can carry out routine by persons skilled in the art according to different types of rock sample and select, and the bake out temperature of such as sandstone is at 80 ± 2 DEG C;
C. actual formation water data prepares simulated formation aqueous solution per sample, utilizes rock saturation water device to vacuumize then abundant saturated local water more than 8 hours to sample, until bubble-free is overflowed, has taken out the sample of saturation water completely;
D. saturation water sample is put into the core holding unit of rock diffusion coefficient analyzer, utilize confined pressure force (forcing) pump to load the confined pressure under the simulation stratum condition of setting to core holding unit;
E. the pipeline that the pipeline utilizing vacuum pump to be connected with right piston container to left diffuser casing, right diffuser casing, its two ends and left piston container and its two ends are connected with chromatogram detector vacuumizes, after close left diffuser casing operation valve, right diffuser casing operation valve, left piston container operation valve, right piston container operation valve, left sample valve, right sample valve, vacuum pump operation valve successively;
F. utilize leak detection liquid to carry out vacuum leak hunting to pipeline junction and each valve, find that seepage carries out tightening in time and leak detection guarantees that pipeline does not exist seepage repeatedly;
G. the actual ground temperature data of sampling horizon per sample, is set as actual ground temperature, as experimental temperature by the temperature controller of rock diffusion coefficient analyzer;
H., when the pipeline of rock diffusion coefficient analyzer and valve do not leak gas, open left air source control valve, right air source control valve, left piston container operation valve, right piston container operation valve respectively, utilize hydro carbons source of the gas, N
2source of the gas fills quantitative hydro carbons and N respectively to left piston container, right piston container
2serve as balanced gas, start Self-pressurizing agri pump, required gas injection equalized pressure and constant supercharging flow velocity are carried out in setting experiment, pressurized liquid promotion piston compression gas boosting is injected by the fluid pressurization cylinder constant speed of Self-pressurizing agri pump to left piston container and right piston container, when the cylinder of final left piston container and right piston container reaches the gas injection equalized pressure of setting, Self-pressurizing agri pump stops supercharging, in this, as experiment start time, thus accurate control realization left piston container cylinder, right piston container cylinder, rock core accommodates the left diffuser casing in device two ends, in right diffuser casing and associated line thereof, all there is identical gas injection equalized pressure, then close left piston container operation valve, right piston container operation valve, left diffuser casing operation valve, right diffuser casing operation valve, only there is concentration gradient and there is not the gas diffusion of pressure gradient in gas in identical gas injection equalized pressure bottom left diffuser casing, right diffuser casing, ,
I. experiment opened left sample valve every 0.5-2 hour after starting, right sample valve makes the gas of a small amount of left diffuser casing, right diffuser casing send into chromatogram detector to measure and record hydro carbons and N in left diffuser casing respectively
2concentration, hydro carbons and N in right diffuser casing
2concentration, utilize Computer Storage and record the gas concentration data of each two diffuser casings;
J. reduce when being checked through hydro carbons concentration in left diffuser casing, in right diffuser casing, the increase of hydro carbons concentration then can judge that hydrocarbon gas diffuses into right diffuser casing by sample from left diffuser casing, and using these data as the 1st group of left diffuser casing, right diffuser casing hydro carbons concentration change data, then the left diffuser casing of more than 8 groups is recorded continuously, after right diffuser casing hydro carbons concentration change data, experiment terminates, close left piston container operation valve, right piston container operation valve, left diffuser casing operation valve, right diffuser casing operation valve, left sample valve, right sample valve etc., sample is taken out from core holding unit,
K. bring all raw data that computer recording is preserved into Fick's second law, to utilize under following formulae discovery high-temperature and high-pressure conditions hydro carbons coefficient of diffusion in rock:
D＝ln(ΔC
0/ΔC
i)/[E(t
i-t
0)]，
Wherein E=A (1/V
1+ 1/V
2)/L, t
0for initial time, t
ifor the i moment, Δ C
ifor i moment hydro carbons concentration difference in two diffuser casings, Δ C
0for initial time hydro carbons concentration difference in two diffuser casings, A is the sectional area of rock sample, and L is the length of rock sample, V
1, V
2be respectively the volume of left diffuser casing, right diffuser casing, analyze the relation between itself and gas injection equalized pressure, experimental temperature.
In the above-mentioned methods, preferably, described rock sample is mud shale, sandstone or gypsum-salt rock.
In the above-mentioned methods, when rock sample actual formation water data is unknown, the normal saline solution of every premium on currency sodium chloride-containing 70g, anhydrous calcium chloride 6g and 4g magnesium chloride hexahydrate can be utilized to replace.
In the above-mentioned methods, preferably, in step D, described confined pressure is up to 3-50MPa.
In the above-mentioned methods, preferably, in step G, described actual ground temperature is palaeogeothermal or Present temperature, and described experimental temperature is room temperature-150 DEG C.
In the above-mentioned methods, preferably, in steph, described gas injection equalized pressure is 0.2-10MPa; Described constant supercharging flow velocity is 0.5mL/min-20mL/min.More preferably, described gas injection equalized pressure is 3MPa; Described constant supercharging flow velocity is 5mL/min.
In the above-mentioned methods, preferably, it also comprises and detecting multiple sample according to described steps A-K, calculates their High Temperature High Pressure rock hydro carbons coefficient of diffusion respectively, analyzes the relation between itself and gas injection equalized pressure, experimental temperature respectively.
Under high-temperature and high-pressure conditions provided by the invention, in rock, hydro carbons diffusion coefficients experimental facilities utilizes two piston containers and Self-pressurizing agri pump, ensure that the gas injection equalized pressure of core holding unit two ends diffuser casings remains accurately consistent, guarantee not exist in whole experimentation the driving of pressure gradient and only there is concentration gradient and drive lower hydro carbons to spread; Meanwhile, the gas injection equalized pressure solving source of the gas equalized pressure opertaing device in conventional diffusion coefficients is less, the relatively low problem that there are differences with actual formation condition of experimental temperature.The direct mensuration of the assay method of hydro carbons coefficient of diffusion saturated local water rock sample hydro carbons coefficient of diffusion under achieving high temperature, condition of high voltage in rock under high-temperature and high-pressure conditions provided by the invention, for rock hydro carbons coefficient of diffusion under obtaining actual geology high temperature, condition of high voltage provides technological means, for carrying out Gas diffusion charging amount, windage evaluation and carrying out routine or Unconventional forage fortune is poly-, become to hide, preserve and resource evaluation research provides the Data support of science.
Accompanying drawing explanation
Fig. 1 is hydro carbons diffusion coefficients experimental facilities structural drawing in rock under the high-temperature and high-pressure conditions of embodiment 1.
Fig. 2 is rock hydro carbons coefficient of diffusion and the gas injection equalized pressure graph of a relation of the sandstone that hydro carbons diffusion coefficients method records in rock under the high-temperature and high-pressure conditions of embodiment 2.
Fig. 3 is rock hydro carbons coefficient of diffusion and the temperature relation figure of the mud stone that hydro carbons diffusion coefficients method records in rock under the high-temperature and high-pressure conditions of embodiment 2.
Primary clustering symbol description:
The rock diffusion coefficient analyzer 1 constant temperature oven 101 high temperature high voltage resistant left diffuser casing 103 of the core holding unit 102 left diffuser casing operation valve 105 of the right diffuser casing 104 right diffuser casing left sample valve 107 of operation valve 106 right sample valve 108 temperature controller 109
Sample 2 vacuum pump 3 confined pressure force (forcing) pump 4 methane source of the gas 5 N
2the left air source control valve of the right piston container 8 of source of the gas 6 left piston container 79 right air source control valve 10 left piston container operation valve 11 right piston container operation valve 12 Self-pressurizing agri pump 13 vacuum pump operation valve 14 chromatogram detector 15 computing machine 16
Embodiment
Embodiment 1
To present embodiments provide under a kind of high-temperature and high-pressure conditions hydro carbons diffusion coefficients equipment in rock, as shown in Figure 1, this experimental facilities mainly comprises rock diffusion coefficient analyzer 1, vacuum pump 3, confined pressure force (forcing) pump 4, methane source of the gas 5, N
2source of the gas 6, left piston container 7, right piston container 8, left air source control valve 9, right air source control valve 10, left piston container operation valve 11, right piston container operation valve 12, Self-pressurizing agri pump 13, vacuum pump operation valve 14, chromatogram detector 15, computing machine 16, baking oven (not marking in figure), rock saturation water device (not marking in figure) and pipeline etc.;
Wherein, described rock diffusion coefficient analyzer 1 comprises constant temperature oven 101, high temperature high voltage resistant core holding unit 102, left diffuser casing 103, right diffuser casing 104, left diffuser casing operation valve 105, right diffuser casing operation valve 106, left sample valve 107, right sample valve 108 and temperature controller 109;
Described high temperature high voltage resistant core holding unit position 102, in described constant temperature oven 101, for placing sample 2, and is separated into left diffuser casing 103 and right diffuser casing 104 by sample 2;
Described temperature controller 109 is connected with described constant temperature oven 101;
Described confined pressure force (forcing) pump 4 is connected with described high temperature high voltage resistant core holding unit 102;
Described chromatogram detector 15 is connected with described left diffuser casing 103 and described right diffuser casing 104 respectively by pipeline, the pipeline that described left diffuser casing 103 is connected with chromatogram detector 15 is provided with left sample valve 107, and the pipeline that described right diffuser casing 104 is connected with chromatogram detector 15 is provided with right sample valve 108;
Described computing machine 16 is connected with described chromatogram detector 15;
Described vacuum pump 3 is connected with described rock diffusion coefficient analyzer about 1 two ends respectively by pipeline, and described pipeline is provided with vacuum pump operation valve 14;
Described left piston container 7 and described right piston container 8 size be connected identical, two-piston container includes piston, fluid pressurization cylinder and cylinder;
The cylinder of described left piston container 7 is connected with described left diffuser casing 103 by pipeline, and described pipeline is provided with left piston container operation valve 11 and left diffuser casing operation valve 105; The cylinder of described right piston container 8 is connected with right diffuser casing 104 by pipeline, and described pipeline is provided with right piston container operation valve 12 and right loose room operation valve 105;
Described methane source of the gas 5 is connected by the side of pipeline with the cylinder of described left piston container 7, and described pipeline is provided with left air source control valve 9; Described N
2source of the gas 6 is connected by the side of pipeline with the cylinder of described right piston container 8, and described pipeline is provided with right air source control valve 10;
Described Self-pressurizing agri pump 13 is connected with the fluid pressurization cylinder of described left piston container 7 with described right piston container 8 respectively by pipeline.
In the present embodiment, the bearing capacity of described high temperature high voltage resistant core holding unit is not less than 50MPa, and temperature tolerance is not less than 150 DEG C.Each pipeline is conventional high temperature high voltage resistant pipeline, is stainless steel.Described baking oven is mainly used in drying rock sample, and described rock saturation water device is mainly used in the saturated local water carried out according to actual geologic condition the sample after drying under simulation stratum condition.Described left piston container and right piston container can be stainless steel, and volume is 20L, maximum working pressure (MOP) 30MPa.
Embodiment 2
The present embodiment to provide under a kind of high-temperature and high-pressure conditions hydro carbons diffusion coefficients method in rock, and it is that the experimental facilities using embodiment 1 to provide carries out testing, and this assay method comprises the following steps:
A. make that diameter is 2.5cm, length is the small cylinder of 0.5-0.6cm by taking from each one piece of the mud stone of different regions, sample of sandstone, and conventional orifices porosity is carried out to sample, permeability detects;
B. above-mentioned 2 rock samples are put into drying unit, dry more than 8h, until constant weight at 100 DEG C;
C. according to described mud stone, sandstone separately local water data utilize sodium chloride, lime chloride, magnesium chloride to prepare simulated formation aqueous solution (described mudstone sample reservoir water salinity is about 40g/l, water type is chloride-calcium type, configures the simulated formation aqueous solution of every premium on currency chloride containing calcium 40g; Described sample of sandstone reservoir water salinity is about 80g/l, water type is chloride-calcium type, configure the simulated formation aqueous solution of every premium on currency chloride containing calcium 80g), rock saturation water device is utilized to vacuumize then abundant saturated local water more than 8 hours to described 2 rock samples respectively, until bubble-free is overflowed, take out the sample of saturation water completely;
D. respectively 2 of described saturation water rock samples are put into the high temperature high voltage resistant core holding unit 102 of rock diffusion coefficient analyzer 1, utilize confined pressure force (forcing) pump 4 to the confined pressure under described high temperature high voltage resistant core holding unit 102 loading simulation formation condition, wherein, 32Mpa confined pressure under described mudstone sample loading simulation formation condition, 28MPa confined pressure under described sample of sandstone loading simulation formation condition;
E. the pipeline that the pipeline utilizing vacuum pump 3 to be connected with right piston container 8 to left diffuser casing 103, right diffuser casing 104, its two ends and left piston container 7 and its two ends are connected with chromatogram detector 15 vacuumizes, after close left diffuser casing operation valve 105, right diffuser casing operation valve 106, left piston container operation valve 11, right piston container operation valve 12, left sample valve 107, right sample valve 108, vacuum pump operation valve 14 successively;
F. utilize leak detection liquid to carry out vacuum leak hunting to pipeline junction and each valve, find that seepage carries out tightening in time and leak detection guarantees that pipeline does not exist seepage repeatedly;
G. the actual ground temperature data of sampling horizon per sample, the temperature controller 109 of rock diffusion coefficient analyzer 1 is set as actual ground temperature, as experimental temperature, wherein, the simulated formation experimental temperature of described mud stone rock sample is 90 DEG C, also investigate the rock diffusion coefficient of mud stone rock sample at 70 DEG C, 50 DEG C, 30 DEG C respectively, the simulated formation experimental temperature of described sandstone rock sample is 70 DEG C simultaneously;
H., when the pipeline of rock diffusion coefficient analyzer 1 and valve do not leak gas, open left air source control valve 9, right air source control valve 10, left piston container operation valve 11, right piston container operation valve 12 respectively, utilize methane source of the gas 5, N
2source of the gas 6 fills quantitative methane and N respectively to left piston container 7, right piston container 8
2serve as balanced gas, start Self-pressurizing agri pump 13, setting experiment carries out required final gas injection equalized pressure and constant supercharging flow velocity 5mL/min, by Self-pressurizing agri pump 13 pairs of left piston containers 7, the lower liquid pressurized cylinder constant speed of right piston container 8 is injected pressurized liquid and is promoted piston compression gas boosting, final left piston container 7, the upper cylinder of right piston container 8 reaches Self-pressurizing agri pump 13 when setting gas injection equalized pressure and stops supercharging, in this, as experiment start time, thus accurate control realization left piston container 7 cylinder, right piston container 8 cylinder, high temperature high voltage resistant rock core accommodates the left diffuser casing 103 in device 102 two ends, in right diffuser casing 104 and associated line thereof, all there is identical gas injection equalized pressure, then can close left piston container operation valve 11, right piston container operation valve 12, left diffuser casing operation valve 105, right diffuser casing operation valve 106, at identical gas injection equalized pressure bottom left diffuser casing 103, in right diffuser casing 104 only there is concentration gradient and there is not the gas diffusion of pressure gradient in gas, and wherein, the gas injection equalized pressure of described mud rock sample is 3MPa, and the gas injection equalized pressure of described sandstone rock sample is respectively 0.2MPa, 0.5MPa, 1MPa, 1.5MPa, 2MPa, 2.5MPa, 3MPa,
I. experiment opened left sample valve 107 every 2 hours after starting, right sample valve 108 makes the gas of a small amount of left diffuser casing 103, right diffuser casing 104 send into chromatogram detector 15 to measure and record methane and N in left diffuser casing 103 respectively
2concentration, methane and N in right diffuser casing 104
2concentration, utilize computing machine 16 to store and record the gas concentration data of each two diffuser casings;
J. reduce when being checked through methane concentration in left diffuser casing 103, in right diffuser casing 104, methane concentration increase then can judge that methane gas diffuses into right diffuser casing by sample from left diffuser casing, and using these data as the 1st group of left diffuser casing 103, right diffuser casing 104 methane concentration delta data, then the left diffuser casing 103 of 8 groups is recorded continuously, after right diffuser casing 104 methane concentration delta data, experiment terminates, close left piston container operation valve 11, right piston container operation valve 12, left diffuser casing operation valve 105, right diffuser casing operation valve 106, left sample valve 107, right sample valve 108 etc., sample is taken out from high temperature high voltage resistant core holding unit 102,
K. computing machine 16 is recorded 8 groups of hydrocarbon concentration datas of preservation, calculate the 1st group of two diffuser casing initial time t
0initial hydrocarbon concentration difference Δ C
0, and other 7 group of two diffuser casing moment t
ihydrocarbon concentration difference Δ C
i.Fick's second law is followed in the diffusion of hydro carbons in rock, can obtain computing formula D=ln (Δ C according to definition
0/ Δ C
i)/[E (t
i-t
0)], wherein E=A (1/V
1+ 1/V
2)/L, t
0-initial time, t
i-i the moment, Δ C
i-i moment hydro carbons concentration difference in two diffuser casings, Δ C
0-initial time hydro carbons is concentration difference in two diffuser casings, the sectional area of A-rock sample, the length of L-rock sample, V
1, V
2-be respectively the volume of left diffuser casing 103, right diffuser casing 104; Formula distortion is obtained ln (Δ C
0/ Δ C
i)=DE*t
i-DE*t
0, initial concentration difference Δ C in formula
0, rock diffusion coefficient D, E=A (1/V
1+ 1/V
2)/L is all constants, ln (Δ C
0/ Δ C
i) and t
ilinear, application least square method carries out matching, utilizes 8 groups of data to obtain ln (Δ C
0/ Δ C
i) and t
islope K, according to slope K, diffusion coefficient D=K/E can be tried to achieve; The relation between itself and gas injection equalized pressure, experimental temperature can be analyzed on this basis further.
In the present embodiment, when different experiments temperature or the investigation of different gas injection equalized pressure are carried out to same sample, after carrying out the diffusion coefficients under each experimental temperature or gas injection equalized pressure, need again to dry sample and saturated local water, and then carry out the diffusion coefficients under next experimental temperature or gas injection equalized pressure.
In the present embodiment, the coefficient of diffusion of described sandstone rock sample under different gas injection equalized pressure 0.2MPa, 0.5MPa, 1MPa, 1.5MPa, 2MPa, 2.5MPa, 3MPa is respectively 9.67 × 10
-7cm
2/ s, 6.01 × 10
-7cm
2/ s, 2.85 × 10
-7cm
2/ s, 2.38 × 10
-7cm
2/ s, 1.64 × 10
-7cm
2/ s, 9.47 × 10
-7cm
2/ s, 9.66 × 10
-8cm
2/ s, as shown in Figure 2, along with the increase of gas injection equalized pressure, coefficient of diffusion reduces the relation of its coefficient of diffusion and gas injection equalized pressure gradually.The coefficient of diffusion of described mud stone rock sample at different experiments temperature 90 DEG C, 70 DEG C, 50 DEG C, 30 DEG C is respectively 2.42 × 10
-8cm
2/ s, 1.26 × 10
-8cm
2/ s, 1.0 × 10
-8cm
2/ s, 9.37 × 10
-9cm
2/ s, as shown in Figure 3, along with the rising of experimental temperature, coefficient of diffusion increases the relation of its coefficient of diffusion and experimental temperature gradually.
Claims (3)
1. a hydro carbons diffusion coefficients method in rock under high-temperature and high-pressure conditions, the equipment that the method adopts comprises rock diffusion coefficient analyzer, vacuum pump, confined pressure force (forcing) pump, hydro carbons source of the gas, N
2source of the gas, left piston container, right piston container, Self-pressurizing agri pump, chromatogram detector, computing machine, drying unit and rock saturation water device;
Described rock diffusion coefficient analyzer comprises constant temperature oven, core holding unit and temperature controller;
Described core holding unit is positioned at described constant temperature oven, for placing sample, and is separated into left diffuser casing and right diffuser casing by sample;
Described temperature controller is connected with described constant temperature oven;
Described confined pressure force (forcing) pump is connected with described core holding unit;
Described chromatogram detector is connected with described right diffuser casing with described left diffuser casing respectively by pipeline, and the pipeline that described left diffuser casing is connected with chromatogram detector is provided with left sample valve, and the pipeline that described right diffuser casing is connected with chromatogram detector is provided with right sample valve;
Described computing machine is connected with described chromatogram detector;
Described vacuum pump is connected with two ends, described rock diffusion coefficient analyzer left and right respectively by pipeline, and described pipeline is provided with vacuum pump operation valve;
Described left piston container and described right piston container dimensional size be connected identical, two-piston container includes piston, fluid pressurization cylinder and cylinder;
The cylinder of described left piston container is connected with described left diffuser casing by pipeline, and described pipeline is provided with left piston container operation valve and left diffuser casing operation valve; The cylinder of described right piston container is connected with right diffuser casing by pipeline, and described pipeline is provided with right piston container operation valve and right loose room operation valve;
Described hydro carbons source of the gas is connected by the side of pipeline with the cylinder of described left piston container, and described pipeline is provided with left air source control valve; Described N
2source of the gas is connected by the side of pipeline with the cylinder of described right piston container, and described pipeline is provided with right air source control valve;
Described Self-pressurizing agri pump is connected with the fluid pressurization cylinder of described left piston container with described right piston container respectively by pipeline;
The method comprises the following steps:
A. rock sample is made that diameter is 2.5cm, length is the small cylinder of 0.5-0.6cm, and conventional orifices porosity is carried out to sample, permeability detects; Described rock sample is mud shale, sandstone or gypsum-salt rock;
B. described sample is put into drying unit, dry more than 8h, until constant weight;
C. actual formation water data prepares simulated formation aqueous solution per sample, utilizes rock saturation water device to vacuumize then abundant saturated local water more than 8 hours to sample, until bubble-free is overflowed, has taken out the sample of saturation water completely;
D. saturation water sample is put into the core holding unit of rock diffusion coefficient analyzer, utilize confined pressure force (forcing) pump to load the confined pressure 3-50MPa under the simulation stratum condition of setting to core holding unit;
E. the pipeline that the pipeline utilizing vacuum pump to be connected with right piston container to left diffuser casing, right diffuser casing, its two ends and left piston container and its two ends are connected with chromatogram detector vacuumizes, after close left diffuser casing operation valve, right diffuser casing operation valve, left piston container operation valve, right piston container operation valve, left sample valve, right sample valve, vacuum pump operation valve successively;
F. utilize leak detection liquid to carry out vacuum leak hunting to pipeline junction and each valve, find that seepage carries out tightening in time and leak detection guarantees that pipeline does not exist seepage repeatedly;
G. the actual ground temperature data of sampling horizon per sample, is set as actual ground temperature, as experimental temperature by the temperature controller of rock diffusion coefficient analyzer; Described actual ground temperature is palaeogeothermal or Present temperature, and described experimental temperature is room temperature-150 DEG C;
H., when the pipeline of rock diffusion coefficient analyzer and valve do not leak gas, open left air source control valve, right air source control valve, left piston container operation valve, right piston container operation valve respectively, utilize hydro carbons source of the gas, N
2source of the gas fills quantitative hydro carbons and N respectively to left piston container, right piston container
2serve as balanced gas, start Self-pressurizing agri pump, required final gas injection equalized pressure and constant supercharging flow velocity are carried out in setting experiment, by Self-pressurizing agri pump to left piston container, the fluid pressurization cylinder constant speed of right piston container is injected pressurized liquid and is promoted piston compression gas boosting, when the cylinder of final left piston container and right piston container reaches the gas injection equalized pressure of setting, Self-pressurizing agri pump stops supercharging, in this, as experiment start time, then left piston container operation valve is closed, right piston container operation valve, left diffuser casing operation valve, right diffuser casing operation valve, at identical gas injection equalized pressure bottom left diffuser casing, in right diffuser casing only there is concentration gradient and there is not the gas diffusion of pressure gradient in gas, wherein, described gas injection equalized pressure is 0.2-10MPa, and described constant supercharging flow velocity is 0.5mL/min-20mL/min,
I. experiment opened left sample valve every 0.5-2 hour after starting, right sample valve makes the gas of a small amount of left diffuser casing, right diffuser casing send into chromatogram detector to measure and record hydro carbons and N in left diffuser casing respectively
2concentration, hydro carbons and N in right diffuser casing
2concentration, utilize Computer Storage and record the gas concentration data of each two diffuser casings;
J. reduce when being checked through hydro carbons concentration in left diffuser casing, in right diffuser casing, the increase of hydro carbons concentration then can judge that hydrocarbon gas diffuses into right diffuser casing by sample from left diffuser casing, and using these data as the 1st group of left diffuser casing, right diffuser casing hydro carbons concentration change data, then the left diffuser casing of more than 8 groups is recorded continuously, after right diffuser casing hydro carbons concentration change data, experiment terminates, close left piston container operation valve, right piston container operation valve, and left diffuser casing operation valve, right diffuser casing operation valve, left sample valve, right sample valve etc., sample is taken out from core holding unit,
K. bring all raw data that computer recording is preserved into Fick's second law, utilize hydro carbons coefficient of diffusion in following formulae discovery High Temperature High Pressure rock:
D＝ln(ΔC
0/ΔC
i)/[E(t
i-t
0)]，
Wherein E=A (1/V
1+ 1/V
2)/L, t
0for initial time, t
ifor the i moment, Δ C
ifor i moment hydro carbons concentration difference in two diffuser casings, Δ C
0for initial time hydro carbons concentration difference in two diffuser casings, A is the sectional area of rock sample, and L is the length of rock sample, V
1, V
2be respectively the volume of left diffuser casing, right diffuser casing, analyze the relation between itself and gas injection equalized pressure, experimental temperature.
2. the method for claim 1, wherein in steph, described gas injection equalized pressure is 3MPa; Described constant supercharging flow velocity is 5mL/min.
3. method as claimed in claim 1 or 2, it also comprises and detecting multiple sample according to described steps A-K, calculates hydro carbons coefficient of diffusion in their High Temperature High Pressure rock respectively, analyzes the relation between itself and gas injection equalized pressure, experimental temperature respectively.
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