CN102980837A - Device and measuring method for hydrocarbon diffusion coefficient in rocks under high temperature and high pressure - Google Patents

Device and measuring method for hydrocarbon diffusion coefficient in rocks under high temperature and high pressure Download PDF

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Publication number
CN102980837A
CN102980837A CN2012104658957A CN201210465895A CN102980837A CN 102980837 A CN102980837 A CN 102980837A CN 2012104658957 A CN2012104658957 A CN 2012104658957A CN 201210465895 A CN201210465895 A CN 201210465895A CN 102980837 A CN102980837 A CN 102980837A
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diffuser casing
piston container
sample
rock
pipeline
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CN102980837B (en
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李志生
王晓波
王东良
李剑
杨春霞
严启团
王义凤
王蓉
马卫
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China National Petroleum Corp
China Petroleum and Natural Gas Co Ltd
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China Petroleum and Natural Gas Co Ltd
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Abstract

The invention provides a device and measuring method for the hydrocarbon diffusion coefficient in rocks under high temperature and high pressure. The device mainly comprises a rock diffusion coefficient tester, a vacuum pump, a confining pressure pump, hydrocarbon gas source, nitrogen (N2) gas source, a left piston container, a right piston container, an automatic pressure pump, a chromatographic detector, a computer, a drying device and a rock saturated water device and the like. According to the device and method, the consistent accurate accordance of the gas injection balance pressure in the diffusion chambers respectively arranged at two ends of a core holder can be achieved and the existence of the hydrocarbon diffusion driven by the concentration gradient not by the pressure gradient in the whole process of experiment is ensured. Meanwhile, according to the device and method, the problem of low gas injection balance pressure, relatively low experimental temperature and having difference with the actual formation condition of the gas source balance pressure control device in the measuring of normal diffusion coefficient is resolved.

Description

Under the High Temperature High Pressure in the rock hydro carbons coefficient of diffusion measure with equipment and assay method
Technical field
The present invention relates in a kind of rock the hydro carbons coefficient of diffusion measures with experimental facilities and assay method, relate in particular under a kind of high-temperature and high-pressure conditions in the rock hydro carbons coefficient of diffusion and measure with experimental facilities and assay method, belong to the Natural Gas Geology analysis technical field in the technical field of petroleum extraction.
Background technology
Diffusion refers to hydrocarbon gas under the concentration gradient effect, and gas molecule reaches a kind of physical process of balance to the low concentration region free migration by various media 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 a stronger diffusivity underground) migration, assemble poly-, become to hide, preserve and destroyed most important effect.For the gas reservoir of having assembled, except the impact of cap rock Self-Closing ability, tomography, supracrustal rocks are the greatest factor that affects gas reservoir Late reformation, destruction for the diffusivity of hydro carbons; Yet, except as conventional traditional destructive factor, be diffused in gas migration, gathering and become the Tibetan process also may produce positive role and contribution, especially in fields such as unconventional tight sand, shale gas.Coefficient of diffusion is that rock gas diffusion charging amount and windage calculate requisite important parameter as describing the important evaluating of rock gas by rock rate of propagation speed.At present, the experimental determination coefficient of diffusion adopts indirect method, i.e. diffusing capacity or concentration by sample in the measuring certain hour, again by these measured values by determining someway or trying to achieve the coefficient of diffusion value.The coefficient of diffusion that routine records is owing to tested Temperature-pressure Conditions and Geologic Time limits, exist deviation with the real diffusivity of rock under the actual geologic condition, and along with buried depth increases, compacting diagenesis's effect strengthens, diffusion coefficient of natural gas also is different in the different geologic epochs in the geologic epoch.This shows, at utmost measure rock hydro carbons coefficient of diffusion near actual geology high-temperature and high-pressure conditions, for hydro carbons diffusivity in the accurate evaluation rock, assessment rock gas diffusion charging amount and diffusion loss amount are carried out routine, very migration, gathering, the one-tenth of rock gas are hidden and preserved research and resource evaluation all has effect of crucial importance.
Laboratory rock hydro carbons coefficient of diffusion is measured mainly at normal temperature, normal pressure (22 ℃ of room temperatures, 0.2MPa gas injection equalized pressure both at home and abroad at present, the 3MPa confined pressure) carries out under the condition, and existing coefficient of diffusion determinator adopts the control two ends diffuser casing gas injection equalized pressures such as precision pressure gauge more, can not guarantee well that two ends diffuser casing gas injection equalized pressure remains identical, produce easily small pressure reduction, thereby can not guarantee fully that whole experimentation only has the concentration gradient driving and do not have pressure gradient to exist; In addition, since the gas injection equalized pressure of conventional bleed pressure opertaing device control general less and experimental temperature is relatively low and actual geologic condition under the rock state that in the stratum, is in saturated local water, high temperature, high pressure have larger difference, can not reflect preferably the real diffusivity of rock hydro carbons under the geologic condition.Therefore, be necessary existing equipment transformed and provide a kind of High Temperature High Pressure rock hydro carbons coefficient of diffusion to measure to overcome above-mentioned technical matters with experimental facilities.
Summary of the invention
For solving the problems of the technologies described above, the object of the present invention is to provide under a kind of high-temperature and high-pressure conditions in the rock hydro carbons coefficient of diffusion to measure with experimental facilities and assay method.This experimental facilities and assay method can be measured under the high-temperature and high-pressure conditions hydro carbons coefficient of diffusion in the rock convenient, fast, accurately and efficiently, for carrying out rock gas diffusion charging amount, windage evaluation and carrying out the Data support that conventional or unconventional Natural Gas Migration And Accumulation, Cheng Zang, preservation and resource evaluation research provide science.
For reaching above-mentioned purpose, the invention provides under a kind of high-temperature and high-pressure conditions in the rock hydro carbons coefficient of diffusion and measure and use experimental facilities, 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, is used 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 the 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 the chromatogram detector is provided with left sample valve, the pipeline that described right diffuser casing is connected with the chromatogram detector is provided with right sample valve, and described chromatogram detector is for detection of hydro carbons and N in the left diffuser casing of rock diffusion coefficient analyzer 2Concentration change situation, and hydro carbons and N in the right diffuser casing 2The concentration change situation;
Described computing machine is connected with described chromatogram detector, is used for the detector operation of control chromatogram and record and storage raw data;
Described vacuum pump links to each other with two ends, the described rock diffusion coefficient analyzer left and right sides respectively by pipeline, be provided with the vacuum pump operation valve at described pipeline, be used for pipeline is vacuumized, to guarantee that coefficient of diffusion measures in the left diffuser casing of initial time as single, pure hydro carbons, be single, pure N in the right diffuser casing 2Gas;
Described left piston container and described right piston container dimensional size be connected identically, the two-piston container includes piston, liquid pressurized cylinder and cylinder;
The cylinder of described left piston container is connected with described left diffuser casing by pipeline, be provided with left piston container operation valve and left diffuser casing operation valve at described pipeline, wherein, described left piston container operation valve is arranged near on the pipeline of left piston container, and described left diffuser casing operation valve is arranged near on the pipeline of left diffuser casing; The cylinder of described right piston container is connected with right diffuser casing by pipeline, be provided with right piston container operation valve and right loose chamber operation valve at described pipeline, wherein, described right piston container operation valve is arranged near on the pipeline of right piston container, and described right diffuser casing operation valve is arranged near 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, is provided with left air source control valve at described pipeline; Described N 2Source of the gas is connected by the side of pipeline with the cylinder of described right piston container, is provided with right air source control valve at described pipeline;
Described Self-pressurizing agri pump is connected with the liquid pressurized 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 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 the high temperature high voltage resistant core holding unit of routine, and its bearing capacity is not less than 50MPa, and temperature tolerance is not less than 150 ℃.Each pipeline is conventional high temperature high voltage resistant pipeline, is stainless steel.Described drying unit can be conventional baking apparatus, is preferably baking oven, and it is used for the oven dry of sample.Described rock saturation water device can be conventional saturation water device, and it is mainly used in the sample after the oven dry is carried out saturated local water under the simulation stratum condition according to actual geologic condition.
In above-mentioned experimental facilities, in the described Self-pressurizing agri pump pressurized liquid is housed, and is provided with the setting device of gas injection equalized pressure and constant supercharging flow velocity; By the mode of setting gas injection equalized pressure and constant supercharging flow velocity the liquid pressurized cylinder constant speed of left piston container and right piston container is injected the supercharging of pressurized liquid pushing piston pressure gas, and realize that finally left piston container, right piston container reach the gas injection equalized pressure of identical setting, thereby guarantee that rock core adds the left diffuser casing of holding in the device, right diffuser casing all has identical gas injection equalized pressure, guarantee that only there is the diffusion under the concentration gradient effect in hydro carbons and does not have diffusion under the pressure gradient effect.
The direction term of mentioning among the present invention, such as: left and right etc., only be direction with reference to the accompanying drawings.Therefore, the direction term of use is to illustrate not to be to limit the present invention.
The present invention also provides under a kind of high-temperature and high-pressure conditions hydro carbons coefficient of diffusion assay method in the rock, and it may further comprise the steps:
A. rock sample being made diameter is that 2.5cm, length are the small cylinder of 0.5-0.6cm, and sample is carried out conventional factor of porosity, permeability detection;
B. described sample is put into drying unit, more than the oven dry 8h, until constant weight, wherein, bake out temperature can carry out routine selection according to different types of rock sample by persons skilled in the art, such as the bake out temperature of sandstone at 80 ± 2 ℃;
C. actual formation water data is prepared the simulated formation aqueous solution per sample, and abundant saturated local water until overflow without bubble, took out the fully sample of saturation water more than 8 hours to utilize rock saturation water device to vacuumize then to sample;
D. the saturation water sample is put into the core holding unit of rock diffusion coefficient analyzer, utilized the confined pressure under the confined pressure force (forcing) pump simulation stratum condition that loading is set to core holding unit;
E. utilize pipeline that vacuum pump links to each other with right piston container to left diffuser casing, right diffuser casing, its two ends and left piston container, with and two ends vacuumize with the pipeline that the chromatogram detector is connected, close successively 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 after complete;
F. utilize leak detection liquid that vacuum leak hunting is carried out in pipeline junction and each valve, the discovery seepage is in time tightened and is repeatedly hunted leak and guarantee that there is not seepage in pipeline;
G. the actual ground temperature data of sampling horizon per sample is set as actual ground temperature with the temperature controller of rock diffusion coefficient analyzer, as experimental temperature;
H. when the pipeline of rock diffusion coefficient analyzer and valve do not leak gas, open respectively left air source control valve, right air source control valve, left piston container operation valve, right piston container operation valve, utilize hydro carbons source of the gas, N 2Source of the gas fills respectively quantitative hydro carbons and N to left piston container, right piston container 2Serve as balanced gas; Start the Self-pressurizing agri pump, set experiment and carry out required gas injection equalized pressure and constant supercharging flow velocity, by the Self-pressurizing agri pump liquid pressurized cylinder constant speed of left piston container and right piston container is injected the supercharging of pressurized liquid pushing piston pressure gas, the Self-pressurizing agri pump stopped supercharging when the cylinder of final left piston container and right piston container reached the gas injection equalized pressure of setting, as testing the zero hour, realize left piston container cylinder thereby accurately control with this, right piston container cylinder, rock core adds holds the left diffuser casing in device two ends, all has identical gas injection equalized pressure in right diffuser casing and the associated line thereof; 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 in gas and does not exist the gas of pressure gradient to spread in identical gas injection equalized pressure bottom left diffuser casing, right diffuser casing;
I. opened left sample valve, right sample valve after the experiment beginning made respectively the gas of a small amount of left diffuser casing, right diffuser casing send into the chromatogram detector to measure and record hydro carbons and N in the left diffuser casing every 0.5-2 hour 2Concentration, right diffuser casing in hydro carbons and N 2Concentration, utilize Computer Storage and record the gas concentration data of each two diffuser casings;
J. ought be checked through hydro carbons concentration reduction in the left diffuser casing, the increase of hydro carbons concentration can judge that then hydrocarbon gas diffuses into right diffuser casing by sample from left diffuser casing in the right diffuser casing, and with these data as the 1st group of left diffuser casing, right diffuser casing hydro carbons concentration change data, then above left diffuser casings of 8 groups of continuous recordings, after the right diffuser casing hydro carbons concentration change data, experiment finishes, 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 valves etc. take out sample from core holding unit;
All raw data of K. computer recording being preserved are brought Fick's second law into, utilize following formula to calculate under the high-temperature and high-pressure conditions hydro carbons coefficient of diffusion in the rock:
D=ln(ΔC 0/ΔC i)/[E(t i-t 0)],
E=A (1/V wherein 1+ 1/V 2)/L, t 0Be initial time, t iBe the i moment, Δ C iBe i moment hydro carbons concentration difference in two diffuser casings, Δ C 0Be 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, the experimental temperature.
In said method, preferably, described rock sample is mud shale, sandstone or gypsum-salt rock.
In said method, when rock sample actual formation water data is unknown, can utilize the normal saline solution of every premium on currency sodium chloride-containing 70g, anhydrous calcium chloride 6g and 4g magnesium chloride hexahydrate to replace.
In said method, preferably, in step D, described confined pressure is up to 3-50MPa.
In said method, preferably, in step G, described actual ground temperature is palaeogeothermal or ground temperature now, and described experimental temperature is room temperature-150 ℃.
In said method, preferably, in step H, 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 said method, preferably, it also comprises according to described steps A-K a plurality of samples is detected, and calculates respectively their High Temperature High Pressure rock hydro carbons coefficient of diffusion, analyzes respectively the relation between itself and gas injection equalized pressure, the experimental temperature.
Under the high-temperature and high-pressure conditions provided by the invention in the rock hydro carbons coefficient of diffusion measure and to utilize two piston containers and Self-pressurizing agri pump with experimental facilities, the gas injection equalized pressure that guarantees core holding unit two ends diffuser casing remains accurately consistent, guarantees not have the driving of pressure gradient in the whole experimentation and only exists concentration gradient to drive lower hydro carbons to spread; Simultaneously, solved the problem that the gas injection equalized pressure is less, experimental temperature is relatively low and the actual formation condition there are differences of source of the gas equalized pressure opertaing device in the conventional coefficient of diffusion mensuration.Under the high-temperature and high-pressure conditions provided by the invention in the rock assay method of hydro carbons coefficient of diffusion realized the direct mensuration of saturated local water rock sample hydro carbons coefficient of diffusion under high temperature, the condition of high voltage, rock hydro carbons coefficient of diffusion provides technological means under actual geology high temperature, the condition of high voltage in order to obtain, for carrying out rock gas diffusion charging amount, windage evaluation and carrying out the Data support that conventional or unconventional Natural Gas Migration And Accumulation, Cheng Zang, preservation and resource evaluation research provide science.
Description of drawings
Fig. 1 be under the high-temperature and high-pressure conditions of embodiment 1 in the rock hydro carbons coefficient of diffusion measure and use the experimental facilities structural drawing.
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 coefficient of diffusion assay method records in the 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 coefficient of diffusion assay method records in the rock under the high-temperature and high-pressure conditions of embodiment 2.
The primary clustering symbol description:
Rock diffusion coefficient analyzer 1 constant temperature oven 101 high temperature high voltage resistant core holding units 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 temperature controllers 109
Sample 2 vacuum pumps 3 confined pressure force (forcing) pumps 4 methane sources of the gas 5 N 2Source of the gas 6 left piston containers 7 right piston container 8 left air source control valve 9 right air source control valve 10 left piston container operation valves 11 right piston container operation valve 12 Self-pressurizing agri pumps 13 vacuum pump operation valves 14 chromatogram detectors 15 computing machines 16
Embodiment
Embodiment 1
Present embodiment provides under a kind of high-temperature and high-pressure conditions in the rock hydro carbons coefficient of diffusion to measure and has used equipment, and 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 (marking among the figure), rock saturation water device (marking among the 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 is used for placing sample 2, and is separated into left diffuser casing 103 and right diffuser casing 104 by sample 2 in described constant temperature oven 101;
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 links to each other with two ends, described rock diffusion coefficient analyzer 1 left and right sides respectively by pipeline, is provided with vacuum pump operation valve 14 at described pipeline;
Described left piston container 7 and described right piston container 8 sizes be connected identically, the two-piston container includes piston, liquid pressurized cylinder and cylinder;
The cylinder of described left piston container 7 is connected with described left diffuser casing 103 by pipeline, is provided with left piston container operation valve 11 and left diffuser casing operation valve 105 at described pipeline; The cylinder of described right piston container 8 is connected with right diffuser casing 104 by pipeline, is provided with right piston container operation valve 12 and right loose chamber operation valve 105 at described pipeline;
Described methane source of the gas 5 is connected by the side of pipeline with the cylinder of described left piston container 7, is provided with left air source control valve 9 at described pipeline; Described N 2Source of the gas 6 is connected by the side of pipeline with the cylinder of described right piston container 8, is provided with right air source control valve 10 at described pipeline;
Described Self-pressurizing agri pump 13 is connected with the liquid pressurized cylinder of described right piston container 8 with described left piston container 7 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 ℃.Each pipeline is conventional high temperature high voltage resistant pipeline, is stainless steel.Described baking oven is mainly used in rock sample is dried, and described rock saturation water device is mainly used in the sample after the oven dry is carried out saturated local water under the simulation stratum condition according to actual geologic condition.Described left piston container and right piston container can be stainless steel, and volume is 20L, maximum working pressure (MOP) 30MPa.
Embodiment 2
Present embodiment provides under a kind of high-temperature and high-pressure conditions hydro carbons coefficient of diffusion assay method in the rock, and it is that the experimental facilities that uses embodiment 1 to provide is tested, and this assay method may further comprise the steps:
A. it is that 2.5cm, length are the small cylinder of 0.5-0.6cm that each on mud stone, sample of sandstone will taking from different regions made diameter, and to sample carry out conventional factor of porosity, permeability detects;
B. above-mentioned 2 rock samples are put into drying unit, more than 100 ℃ of oven dry 8h, until constant weight;
C. the local water data is utilized sodium chloride, lime chloride separately, (described mudstone sample reservoir water salinity is about 40g/l to magnesium chloride preparation simulated formation aqueous solution according to described mud stone, sandstone, the water type is chloride-calcium type, disposes the simulated formation aqueous solution of every premium on currency chloride containing calcium 40g; The about 80g/l of described sample of sandstone reservoir water salinity, the water type is chloride-calcium type, dispose the simulated formation aqueous solution of every premium on currency chloride containing calcium 80g), utilize rock saturation water device respectively then described 2 rock samples to be vacuumized abundant saturated local water more than 8 hours, until overflow without bubble, taken out the fully sample of saturation water;
D. respectively 2 rock samples of described saturation water 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 the described high temperature high voltage resistant core holding unit 102 loading simulation formation conditions, wherein, 32Mpa confined pressure under the described mudstone sample loading simulation formation condition, 28MPa confined pressure under the described sample of sandstone loading simulation formation condition;
E. utilize pipeline that 3 pairs of left diffuser casings 103 of vacuum pump, right diffuser casing 104, its two ends and left piston container 7 link to each other with right piston container 8, with and two ends vacuumize with the pipeline that chromatogram detector 15 is connected, close successively 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 after complete;
F. utilize leak detection liquid that vacuum leak hunting is carried out in pipeline junction and each valve, the discovery seepage is in time tightened and is repeatedly hunted leak and guarantee that there is not seepage in pipeline;
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 ℃, simultaneously also investigate respectively the rock diffusion coefficient of mud stone rock sample under 70 ℃, 50 ℃, 30 ℃, the simulated formation experimental temperature of described sandstone rock sample is 70 ℃;
H. when the pipeline of rock diffusion coefficient analyzer 1 and valve do not leak gas, open respectively left air source control valve 9, right air source control valve 10, left piston container operation valve 11, right piston container operation valve 12, utilize methane source of the gas 5, N 2Source of the gas 6 fills respectively quantitative methane and N to left piston container 7, right piston container 8 2Serve as balanced gas; Start Self-pressurizing agri pump 13, set experiment and carry out required final gas injection equalized pressure and constant supercharging flow velocity 5mL/min, by 13 pairs of left piston containers 7 of Self-pressurizing agri pump, the lower liquid pressurized cylinder constant speed of right piston container 8 is injected the supercharging of pressurized liquid pushing piston pressure gas, final left piston container 7, Self-pressurizing agri pump 13 stopped supercharging when the upper cylinder of right piston container 8 reached setting gas injection equalized pressure, with this as the experiment zero hour, thereby accurately control realizes left piston container 7 cylinders, right piston container 8 cylinders, the high temperature high voltage resistant rock core adds holds the left diffuser casing 103 in device 102 two ends, all has identical gas injection equalized pressure in right diffuser casing 104 and the associated line thereof, 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, only there is concentration gradient in gas and does not exist the gas of pressure gradient to spread in the right diffuser casing 104, wherein, the gas injection equalized pressure of described mud stone stone 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. opened left sample valve 107, right sample valve 108 after the experiment beginning made respectively 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 the left diffuser casing 103 every 2 hours 2Concentration, right diffuser casing 104 in methane and N 2Concentration, utilize computing machine 16 storage and record the gas concentration data of each two diffuser casings;
J. ought be checked through methane concentration reduction in the left diffuser casing 103, the methane concentration increase can judge that then methane gas diffuses into right diffuser casing by sample from left diffuser casing in the right diffuser casing 104, and with these data as the 1st group of left diffuser casing 103, right diffuser casing 104 methane concentration delta datas, then the left diffuser casing 103 of 8 groups of continuous recordings, behind the right diffuser casing 104 methane concentration delta datas, experiment finishes, 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 valves 108 etc. take out sample from high temperature high voltage resistant core holding unit 102;
K. 8 groups of hydrocarbon concentration datas computing machine 16 records being preserved calculate the 1st group of two diffuser casing initial time t 0The poor Δ C of initial hydrocarbon concentration 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 get computing formula D=ln (Δ C according to definition 0/ Δ C i)/[E (t i-t 0)], E=A (1/V wherein 1+ 1/V 2)/L, t 0-initial time, t i-i the moment, Δ C i-i is hydro carbons concentration difference in two diffuser casings constantly, 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; The formula distortion is obtained ln (Δ C 0/ Δ C i)=DE*t i-DE*t 0, the poor Δ C of initial concentration in the formula 0, rock diffusion coefficient D, E=A (1/V 1+ 1/V 2)/L all is constants, ln (Δ C 0/ Δ C i) and t iLinear, use least square method and carry out match, utilize 8 groups of data to obtain ln (Δ C 0/ Δ C i) and t iSlope K, according to slope K, can try to achieve diffusion coefficient D=K/E; Can further analyze on this basis the relation between itself and gas injection equalized pressure, the experimental temperature.
In the present embodiment, when same sample is carried out different experiments temperature or the investigation of different gas injection equalized pressure, after the coefficient of diffusion mensuration of carrying out under each experimental temperature or the gas injection equalized pressure, need to again dry sample and saturated local water, and then the coefficient of diffusion that carries out under next experimental temperature or the gas injection equalized pressure is measured.
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, the relation of its coefficient of diffusion and gas injection equalized pressure as shown in Figure 2, along with the increase of gas injection equalized pressure, coefficient of diffusion reduces gradually.The coefficient of diffusion of described mud stone rock sample under 90 ℃, 70 ℃, 50 ℃, 30 ℃ of different experiments temperature 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, the relation of its coefficient of diffusion and experimental temperature as shown in Figure 3, along with the rising of experimental temperature, coefficient of diffusion increases gradually.

Claims (8)

  1. Under the high-temperature and high-pressure conditions in the rock hydro carbons coefficient of diffusion measure and use experimental facilities, 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 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, is used 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 the chromatogram detector is provided with left sample valve, and the pipeline that described right diffuser casing is connected with the chromatogram detector is provided with right sample valve;
    Described computing machine is connected with described chromatogram detector;
    Described vacuum pump links to each other with two ends, the described rock diffusion coefficient analyzer left and right sides respectively by pipeline, is provided with the vacuum pump operation valve at described pipeline;
    Described left piston container and described right piston container dimensional size be connected identically, the two-piston container includes piston, liquid pressurized cylinder and cylinder;
    The cylinder of described left piston container is connected with described left diffuser casing by pipeline, is provided with left piston container operation valve and left diffuser casing operation valve at described pipeline; The cylinder of described right piston container is connected with right diffuser casing by pipeline, is provided with right piston container operation valve and right loose chamber operation valve at described pipeline;
    Described hydro carbons source of the gas is connected by the side of pipeline with the cylinder of described left piston container, is provided with left air source control valve at described pipeline; Described N 2Source of the gas is connected by the side of pipeline with the cylinder of described right piston container, is provided with right air source control valve at described pipeline;
    Described Self-pressurizing agri pump is connected with the liquid pressurized cylinder of described right piston container with described left piston container respectively by pipeline.
  2. 2. hydro carbons coefficient of diffusion assay method in the rock under the high-temperature and high-pressure conditions, it may further comprise the steps:
    A. rock sample being made diameter is that 2.5cm, length are the small cylinder of 0.5-0.6cm, and sample is carried out conventional factor of porosity, permeability detection;
    B. described sample is put into drying unit, more than the oven dry 8h, until constant weight;
    C. actual formation water data is prepared the simulated formation aqueous solution per sample, and abundant saturated local water until overflow without bubble, took out the fully sample of saturation water more than 8 hours to utilize rock saturation water device to vacuumize then to sample;
    D. the saturation water sample is put into the core holding unit of rock diffusion coefficient analyzer, utilized the confined pressure under the confined pressure force (forcing) pump simulation stratum condition that loading is set to core holding unit;
    E. utilize pipeline that vacuum pump links to each other with right piston container to left diffuser casing, right diffuser casing, its two ends and left piston container, with and two ends vacuumize with the pipeline that the chromatogram detector is connected, close successively 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 after complete;
    F. utilize leak detection liquid that vacuum leak hunting is carried out in pipeline junction and each valve, the discovery seepage is in time tightened and is repeatedly hunted leak and guarantee that there is not seepage in pipeline;
    G. the actual ground temperature data of sampling horizon per sample is set as actual ground temperature with the temperature controller of rock diffusion coefficient analyzer, as experimental temperature;
    H. when the pipeline of rock diffusion coefficient analyzer and valve do not leak gas, open respectively left air source control valve, right air source control valve, left piston container operation valve, right piston container operation valve, utilize hydro carbons source of the gas, N 2Source of the gas fills respectively quantitative hydro carbons and N to left piston container, right piston container 2Serve as balanced gas, start the Self-pressurizing agri pump, set experiment and carry out required final gas injection equalized pressure and constant supercharging flow velocity, by the Self-pressurizing agri pump to the left piston container, the liquid pressurized cylinder constant speed of right piston container is injected the supercharging of pressurized liquid pushing piston pressure gas, when the cylinder of final left piston container and right piston container reaches the gas injection equalized pressure of setting, the Self-pressurizing agri pump stops supercharging, with this as the experiment zero hour, then close left piston container operation valve, right piston container operation valve, left diffuser casing operation valve, right diffuser casing operation valve is at identical gas injection equalized pressure bottom left diffuser casing, only there is concentration gradient in gas and does not exist the gas of pressure gradient to spread in the right diffuser casing;
    I. opened left sample valve, right sample valve after the experiment beginning made respectively the gas of a small amount of left diffuser casing, right diffuser casing send into the chromatogram detector to measure and record hydro carbons and N in the left diffuser casing every 0.5-2 hour 2Concentration, right diffuser casing in hydro carbons and N 2Concentration, utilize Computer Storage and record the gas concentration data of each two diffuser casings;
    J. ought be checked through hydro carbons concentration reduction in the left diffuser casing, the increase of hydro carbons concentration can judge that then hydrocarbon gas diffuses into right diffuser casing by sample from left diffuser casing in the right diffuser casing, and with these data as the 1st group of left diffuser casing, right diffuser casing hydro carbons concentration change data, then above left diffuser casings of 8 groups of continuous recordings, after the right diffuser casing hydro carbons concentration change data, experiment finishes, 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 valves etc. take out sample from core holding unit;
    All raw data of K. computer recording being preserved are brought Fick's second law into, utilize following formula to calculate hydro carbons coefficient of diffusion in the High Temperature High Pressure rock:
    D=ln(ΔC 0/ΔC i)/[E(t i-t 0)],
    E=A (1/V wherein 1+ 1/V 2)/L, t 0Be initial time, t iBe the i moment, Δ C iBe i moment hydro carbons concentration difference in two diffuser casings, Δ C 0Be 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, the experimental temperature.
  3. 3. method as claimed in claim 2, wherein, described rock sample is mud shale, sandstone or gypsum-salt rock.
  4. 4. method as claimed in claim 2, wherein, in step D, described confined pressure is 3-50MPa.
  5. 5. method as claimed in claim 2, wherein, in step G, described actual ground temperature is palaeogeothermal or ground temperature now, described experimental temperature is room temperature-150 ℃.
  6. 6. method as claimed in claim 2, wherein, in step H, described gas injection equalized pressure is 0.2-10MPa; Described constant supercharging flow velocity is 0.5mL/min-20mL/min.
  7. 7. method as claimed in claim 2, wherein, in step H, described gas injection equalized pressure is 3MPa; Described constant supercharging flow velocity is 5mL/min.
  8. 8. such as each described method of claim 2-7, it also comprises according to described steps A-K a plurality of samples is detected, calculate respectively hydro carbons coefficient of diffusion in their the High Temperature High Pressure rock, analyze respectively the relation between itself and gas injection equalized pressure, the experimental temperature.
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CN103616317A (en) * 2013-12-16 2014-03-05 南京工业大学 Full-automatic equipment and method for testing helium diffusion coefficient of reactor material
CN104237078A (en) * 2014-09-29 2014-12-24 清华大学 Method and device for measuring molecular diffusion coefficient of voluminous powder
CN104502237A (en) * 2014-12-15 2015-04-08 中国石油大学(华东) Device for measuring diffusion coefficient of CO2 diffusing from aqueous phase to oil phase and operating method thereof
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