CN105628811A - Testing device for competitive adsorption of supercritical CO2 and CH4 in shale and testing method of device - Google Patents
Testing device for competitive adsorption of supercritical CO2 and CH4 in shale and testing method of device Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/088—Investigating volume, surface area, size or distribution of pores; Porosimetry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
Abstract
The invention provides a testing device for competitive adsorption of supercritical CO2 and CH4 in shale and a testing method of the device. The device comprises an injection pump system, a long core holder, a back-pressure valve, a differential pressure gauge, a temperature control system, a liquid fraction collector, a gas meter and a gas chromatograph instrument. The testing method comprises an evaluation method of CH4 single component gas in a shale core and an evaluation method of CH4 gas, converted by the supercritical CO2, in the shale core. According to the device and method, the detection conditions of a laboratory test that the supercritical CO2 displaces CH4 adsorbed in the shale under the high temperature and high pressure conditions of a stratum are met through a multifunctional long core displacement method, and then the purpose of evaluating the efficiency that the supercritical CO2 displaces the adsorbed CH4 is achieved; by using the combined long core, the gas injection volume is large, the errors are decreased, and the formation condition is truly restored; the cracked long core can simulate the competitive adsorption process of the fractured supercritical CO2 and the CH4 under the true shale reservoir condition; the injected CO2 is in the supercritical state, and an experiment is performed in a step-by-step depressurizing mode, and the depletion exploitation process of a stratum can be truly simulated.
Description
Technical field
The invention belongs to analog detection experimental technique field, particularly relate at high temperature under high pressure, supercritical co, to the simulation of the desorb metathesis of adsorbed methane gas in shale and detection technique, is used to guide the raising of the reasonable high efficient mining technology of shale gas.
Background technology
World's shale gas stock number is huge, and with breakthrough and the output fast growth of North America shale gas exploratory development technology, shale gas has been considered as having the Unconventional forage of extraction value. Understand shale gas reservoir development features and development scheme, it is contemplated that how to realize improving shale gas recovery ratio very important. In shale gas reservoir, it is considered that the occurrence form of Sweet natural gas has three kinds, adsorbed gas, free gas and solution gas. Adding up according to some scholars, adsorbed gas content occupies 20%��85%, and the exploitation strengthening adsorbed gas is particularly important to shale gas volume increase.
According to CO2CH in displacement coal seam4Successful experience, CO2Can success displacement coal seam in CH4Mainly have benefited from CO2Adsorptive power be greater than CH4, part scholar is to shale CO absorption2��CH4Characteristic carried out primary work, result all shows that shale is to CO2Adsorptive power be significantly better than CH4. But at present both at home and abroad to CO2Displacement shale adsorbs CH4Laboratory Evaluation also considerably less, the experiment carried out can not meet the conditions such as stratum high-temperature high pressure mostly, particularly can't simulation shale virtual condition more complete, comprehensive, thus cannot reduce practical condition, instruct the reasonable high-efficiency mining of shale gas better, it is to increase efficiency.
Summary of the invention
The object of the invention is to provide a kind of the shop experiment detection device and the research method thereof that are applicable to actual production conditions. The present invention passes through supercritical CO2With CH in shale4Competitive adsorption experimental evaluation CO2To the replacement result of adsorbed gas in shale. Experiment completes in multi-functional long-core test device, and this principle of device is reliable, rational in infrastructure.
The present invention is achieved through the following technical solutions:
The present invention realizes disclosing a kind of supercritical CO2With CH in shale4Competitive adsorption test set, comprising: injection pump system, long rock core holder, check valve, pressure reduction table, temperature controlling system, liquid distillate collector, gasometer flask and gas chromatograph; Wherein:
Long rock core holder is made up of the axial connector at long cores urceolus, rubber cover and two ends; Long cores urceolus is arranged in rubber cover, two ends are connected with axial connector, and rubber cover forms airtight reactive system with axial connector;
Injection pump system comprises entrance displacement pump, back pressure regulates pump and confined pressure control pump;
Described entrance displacement pump is by intermediate receptacle in parallel, valve and inlet end axial connector UNICOM, and described back pressure regulates pump by check valve and exit end axial connector UNICOM, and described confined pressure controls pump and overlaps UNICOM by valve and rubber; Check valve one branch road is also by gasometer flask and gas chromatograph UNICOM.
Described device each UNICOM pipeline is provided with pressure reduction table.
Described long rock core holder inlet end and exit end are provided with pressure reduction table.
Present invention also offers a kind of supercritical CO2With CH in shale4Competitive adsorption testing method,
Testing method adopts above-mentioned disclosed test set;
Testing method comprises CH in shale core4Supercritical CO in single-component gas evaluation method and shale core2Displacement CH4Gas evaluation method:
CH4Single-component gas evaluation method comprises:
(1) choose length 4��6cm, the little rock pillar of diameter 2.5cm shale, carry out basis physical property measurement, by the selected short rock core of the shale pressing crack in order permutation and combination become long cores, load core holding unit and also vacuumize;
(2) rear long rock core holder will be vacuumized and put into baking oven, setting oven temperature is formation temperature belonging to shale, setting clamper confined pressure is the overlying formation pressure value on stratum belonging to shale, and lead to into methane gas to airtight clamper system, fully absorption is saturated in shale to make methane gas, saturation time is 72 hours, and methane saturation pressure is the Pore Pressure force value on stratum belonging to shale;
(3) clamper system entry end is closed, open exit end, to methane gas step pressure reducing in system, and record step-down time, exit end output tolerance, and exit end closes 12 hours after step-down, make the abundant desorb of adsorbed methane gas in shale, and then open exit end, repeat step-down above, time and output tolerance record, close/open exit end step, till methane gas pressure is reduced to the exploitation abandonment pressure of gas reservoir belonging to shale in system, calculate accumulative output tolerance;
Described supercritical CO2Displacement CH4Gas evaluation method comprises:
(4) CH is continued to use4Single-component gas evaluation method experiment rock sample, vacuumizes system, and repeats above-mentioned experimental implementation;
(5) open clamper inlet end and exit end valve, inject supercritical CO with the injection pressure of 35MPa to long cores2, and this procedure exit end gas is carried out stratographic analysis;
(6) when the gas that exit end detects out is all carbon dioxide content, close clamper system entry end and exit end valve 72 hours, make CO2Fully absorption, and replace ADSORPTION STATE CH4Gas;
(7) close clamper system entry end, open exit end, make mixed gas step-down 2MPa in system, the record step-down time, and by stratographic analysis record output CH4Tolerance; After step-down, exit end closes 12 hours, makes the CO in shale2Fully absorption displacement CH4Gas, and then open exit end, repeat above-mentioned step-down, time and output tolerance record, close/open exit end step, till gaseous tension is reduced to the exploitation abandonment pressure of gas reservoir belonging to shale in system, calculate accumulative output methane tolerance;
(8) contrast the methane yield that two groups are tested same pressure drop point, evaluate supercritical CO2CH in competitive adsorption shale4Effect.
In test set of the present invention, the three axial length core holding units of about 1 meter long are the crucial parts in long-core test device, primarily of long cores urceolus, rubber cover and axial connector composition. In this covering device, the condensate gas exhaustion speed in rock core is controlled by exit end pressure drop rate, and exit end pressure drop rate is controlled by the pressure drop rate of check valve.
This valve testing method is completed by two groups of Experimental comparison.
By short rock core in certain sequence permutation and combination become long cores, load core holding unit, clean and blow dry vacuumizing, more saturated CH4To formation condition, and stablize at this pressure and within 72 hours, carry out two groups of experiments. First group of experiment exhaustion from formation condition, the abundant desorb in 12 hours of every one-level exhaustion pressure-stabilisation, each exhaustion terminates to record corresponding experimental data; Contrast experiment mainly considers CO2To CH4Competitive adsorption effect, first by quick displacement, by the CH in matrix4Displacement is clean, afterwards under the experiment condition same with first group, measures the component concentration of output gas, and test point corresponding to first group carries out experiment effect comparative analysis.
The present invention has following useful effect compared with the conventional method:
1) when finding there is no Reality simulation shale reservoir fracturing at present through investigation, supercritical CO in analog development process2With CH4Competitive adsorption experiment test is studied;
2) with the use of combination long cores so that gas injection volume amount is big, error reduces, and truly reduces formation condition;
3) crack long cores can under Reality simulation shale reservoir conditions after supercritical CO 2 pressure break with CH4 competitive adsorption process;
4) CO is injected2For above-critical state, and experiment take step pressure reducing mode to carry out, it is possible to real simulation stratum exhaustion recovery process.
Accompanying drawing explanation
Fig. 1 is that apparatus of the present invention connect structural representation.
In figure, 11 is entrance displacement pump, and 12 is that back pressure regulates pump, 13 is confined pressure control pump, 2 long rock core holder, and 21 is long cores urceolus, 22 is rubber cover, and 23 is axial connector, and 31 is intermediate receptacle 1,32 is intermediate receptacle 2,4 is pressure reduction table, and 5 is valve, and 6 is check valve, 7 is gasometer flask, and 8 is gas chromatograph.
Embodiment
Below by embodiment, the present invention is specifically described; embodiment is only for being further detailed the present invention; can not being interpreted as limiting the scope of the invention, improvement and the adjustment of some non-intrinsically safes that the technician of this area makes according to the content of the present invention also belong to the scope of protection of the invention.
Composition graphs 1.
Test set
As shown in Figure 1, apparatus of the present invention comprise injection pump system, long rock core holder 2, check valve 6, pressure reduction table 4, temperature controlling system, liquid distillate collector, gasometer flask 7 and gas chromatograph 8; Temperature controlling system and liquid distillate collector do not indicate in the drawings; Wherein:
Long rock core holder 2 is made up of the axial connector 23 at long cores urceolus 21, rubber cover 22 and two ends; Long cores urceolus 21 is arranged in rubber cover 22, two ends are connected with axial connector 23, and rubber cover 22 forms airtight reactive system with axial connector 23;
Injection pump system comprises entrance displacement pump 11, back pressure regulates pump 12 and confined pressure control pump 13;
Entrance displacement pump 11 by intermediate receptacle in parallel 31,32, valve 5 and inlet end axial connector 23 UNICOM, back pressure regulates pump 12 by check valve 6 and exit end axial connector 23 UNICOM, and confined pressure control pump 13 overlaps 22 UNICOMs by valve 5 and rubber; Check valve 6 one branch road is also by gasometer flask 7 and gas chromatograph 8 UNICOM.
Apparatus of the present invention are provided with pressure reduction table 4 in each UNICOM pipeline; It is provided with pressure reduction table 4 at long rock core holder 2 inlet end and exit end.
Test experiments
This experiment will be divided into two groups to carry out, by the feasibility of this evaluation method of comparative analysis.
First group: CH in shale core4The output process evaluation of single-component gas
1. choose the shale cylindrical sample of length 4��6cm, diameter 2.5cm, utilize Brazil's split the law that selected rock sample is manually made seam, and test and make seam rear rock sample porosity, Permeability Parameters;
2. according to making seam rear rock sample rate of permeation, length parameter, ask for the harmonic mean rate of permeation of all core column, and choose the core column the most close with harmonic mean rate of permeation, be recorded as No. 1 core column;
3. with reference to step 2. middle method, new harmonic mean rate of permeation is obtained by residue core column, and by all residue core column number consecutivelies;
4. by step 2., 3. in rock core by number successively series connection load thermoplastic tube, and heat moulds wrapping and encapsulating core column, thus is spliced to form long core experiment sample, is loaded long rock core holder 2 system, and guarantees the gas-tight property of system, then it vacuumizes 24 hours;
5. will vacuumize rear long rock core holder 2 and put into baking oven, setting oven temperature is 80 DEG C, setting long rock core holder 2 confined pressure is 60MPa, and lead to into intermediate receptacle 31 methane gas to airtight long rock core holder 2 system, fully absorption is saturated in shale to make methane gas, saturation time is 72 hours, and methane saturation pressure is 35MPa;
6. long rock core holder 2 system entry end valve door 5 is closed, open exit end valve 5, make methane gas step-down 2MPa in system, and record step-down time, exit end output tolerance, and exit end closes 12 hours after step-down, make the abundant desorb of adsorbed methane gas in shale, and then open exit end valve 5, repeat step-down above, time and output tolerance record, close/open exit end step, till methane gas pressure is reduced to the exploitation abandonment pressure of gas reservoir belonging to shale in system, calculate accumulative output tolerance;
2nd group: shale core exists supercritical CO2CH during metathesis4The output process evaluation of gas
1. continue to use first group of experiment rock sample and experimental installation, system is vacuumized, and repeats first group of step experimental implementation 5.;
2. open long rock core holder 2 system entry end and exit end valve 5, inject supercritical CO with the injection pressure of 35MPa to long cores2, because fracture permeability is much larger than matrix permeability, it will be recognized that the contribution amount of the methane displaced in displacement process fast all comes from crack, and exit end gas need to be carried out stratographic analysis by this process;
3. thinking when the exit end complexion gas that detects out of spectrum be all carbon dioxide content that the methane in crack is all by displacement out, this end of processing, closedown clamper system entry end and exit end valve 72 hours, make CO2Fully absorption, and replace ADSORPTION STATE CH4Gas;
4. close clamper system entry end valve door 5, open exit end valve 5, make mixed gas step-down 2MPa in system, the record step-down time, and record output methane tolerance by gas chromatograph 8, and after step-down, exit end closes 12 hours, makes the CO in shale2Fully absorption displacement CH4Gas, and then open exit end valve 5, repeat above-mentioned step-down, time and output tolerance record, close/open exit end step, till gaseous tension is reduced to the exploitation abandonment pressure of gas reservoir belonging to shale in system, calculate accumulative output methane tolerance;
5. contrast the methane yield that two groups are tested same pressure drop point, evaluate supercritical CO2CH in competitive adsorption shale4Effect.
Claims (4)
1. a supercritical CO2With CH in shale4Competitive adsorption test set, it is characterised in that: comprise injection pump system, long rock core holder, check valve, pressure reduction table, temperature controlling system, liquid distillate collector, gasometer flask and gas chromatograph; Wherein:
Long rock core holder is made up of the axial connector at long cores urceolus, rubber cover and two ends; Long cores urceolus is arranged in rubber cover, two ends are connected with axial connector, and rubber cover forms airtight reactive system with axial connector;
Injection pump system comprises entrance displacement pump, back pressure regulates pump and confined pressure control pump;
Described entrance displacement pump is by intermediate receptacle in parallel, valve and inlet end axial connector UNICOM, and described back pressure regulates pump by check valve and exit end axial connector UNICOM, and described confined pressure controls pump and overlaps UNICOM by valve and rubber; Check valve one branch road is also by gasometer flask and gas chromatograph UNICOM.
2. supercritical CO according to claim 12With CH in shale4Competitive adsorption test set, it is characterised in that: described device each UNICOM pipeline is provided with pressure reduction table.
3. supercritical CO according to claim 12With CH in shale4Competitive adsorption test set, it is characterised in that: described long rock core holder inlet end and exit end are provided with pressure reduction table.
4. a supercritical CO2With CH in shale4Competitive adsorption testing method, it is characterised in that:
Described test adopts the test set described in the arbitrary item of claims 1 to 3;
Described testing method comprises CH in shale core4Supercritical CO in single-component gas evaluation method and shale core2Displacement CH4Gas evaluation method:
CH4Single-component gas evaluation method comprises:
(1) choose length 4��6cm, the little rock pillar of diameter 2.5cm shale, carry out basis physical property measurement, by the selected short rock core of the shale pressing crack in order permutation and combination become long cores, load core holding unit and also vacuumize;
(2) rear long rock core holder will be vacuumized and put into baking oven, setting oven temperature is formation temperature belonging to shale, setting clamper confined pressure is the overlying formation pressure value on stratum belonging to shale, and lead to into methane gas to airtight clamper system, fully absorption is saturated in shale to make methane gas, saturation time is 72 hours, and methane saturation pressure is the Pore Pressure force value on stratum belonging to shale;
(3) clamper system entry end is closed, open exit end, to methane gas step pressure reducing in system, and record step-down time, exit end output tolerance, and exit end closes 12 hours after step-down, make the abundant desorb of adsorbed methane gas in shale, and then open exit end, repeat step-down above, time and output tolerance record, close/open exit end step, till methane gas pressure is reduced to the exploitation abandonment pressure of gas reservoir belonging to shale in system, calculate accumulative output tolerance;
Described supercritical CO2Displacement CH4Gas evaluation method comprises:
(4) CH is continued to use4Single-component gas evaluation method experiment rock sample, vacuumizes system, and repeats above-mentioned experimental implementation;
(5) open clamper inlet end and exit end valve, inject supercritical CO with the injection pressure of 35MPa to long cores2, and this procedure exit end gas is carried out stratographic analysis;
(6) when the gas that exit end detects out is all carbon dioxide content, close clamper system entry end and exit end valve 72 hours, make CO2Fully absorption, and replace ADSORPTION STATE CH4Gas;
(7) close clamper system entry end, open exit end, make mixed gas step-down 2MPa in system, the record step-down time, and by stratographic analysis record output methane tolerance; After step-down, exit end closes 12 hours, makes the CO in shale2Fully absorption displacement CH4Gas, and then open exit end, repeat above-mentioned step-down, time and output tolerance record, close/open exit end step, till gaseous tension is reduced to the exploitation abandonment pressure of gas reservoir belonging to shale in system, calculate accumulative output methane tolerance;
(8) contrast the methane yield that two groups are tested same pressure drop point, evaluate supercritical CO2CH in competitive adsorption shale4Effect.
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