CN103115844B - Measuring method for isothermal adsorption/desorption curve of coaly shale - Google Patents

Measuring method for isothermal adsorption/desorption curve of coaly shale Download PDF

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CN103115844B
CN103115844B CN201310030953.8A CN201310030953A CN103115844B CN 103115844 B CN103115844 B CN 103115844B CN 201310030953 A CN201310030953 A CN 201310030953A CN 103115844 B CN103115844 B CN 103115844B
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pressure
gas
desorption
measured
experimentation
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CN103115844A (en
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冯其红
张先敏
张纪远
李晓东
王建强
赵希春
李加祥
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中国石油大学(华东)
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Abstract

The invention provides a measuring method for an isothermal adsorption/desorption curve of coaly shale. The measuring method mainly comprises the following steps of: placing a coaly shale specimen into a true triaxial core clamping system; setting an initial measuring state of the specimen according to the actual stratigraphic condition; carrying out an adsorption/desorption experiment on the specimen after the volume of a free pore is calibrated; respectively measuring and recording a cumulative flow value of gas at an inlet end or outlet end and a balanced system pressure value according to a high-precise gas mass flow meter at the inlet end or outlet end and a system pressure sensor; calculating to obtain the volume of the absorbed gas; and then, drawing the isothermal adsorption/desorption curve of the coaly shale specimen. By using the measuring method, influences of a strain field, a temperature field and the like to the adsorption/desorption of gas on the surface of the coaly shale can be truly reflected, experiments carried out under the influence of single factor and experiments carried out under the coupled action of multiple factors can be achieved, and the measured adsorption/desorption curve can be used for truly representing the adsorption/desorption characteristic for gas in an actual coaly shale reservoir.

Description

A kind of assay method of danks isothermal adsorption/desorption curve
Technical field:
The present invention relates to a kind of method of measuring danks surface gas adsorption/desorption amount and isothermal adsorption/desorption curve, espespecially measure the method for coal petrography or shale surface gas adsorption/desorption amount and isothermal adsorption/desorption curve under layer state truly such as differently stress, different temperatures etc.
Background technology:
The experimental technique of mensurated gas composition isothermal adsorption/desorption curve in danks mainly contains pressure application, volumetric method and gravitational method at present.Pressure application is current the most conventional method, and its experimental provision is mainly by gas cylinder, vacuum pump, form with reference to cylinder, sample cylinder, pressure gauge and constant temperature oil bath (or constant temperature oven).In experimentation, first to reference to being filled with gas in cylinder, after pressure stability, measure and record with reference to cylinder pressure; Then by sample cylinder with reference to cylinder, be communicated with, after pressure equilibrium, working sample cylinder pressure; By the equation of gas state, calculate the volume of adsorbed gas.Repeat above-mentioned steps, can obtain the adsorbed gas scale of construction under different pressures.Pressure application is to measure at present the method that gas-solid adsorption curve is most widely used, but its operating process complexity; In addition, the data processing in later stage and the computation process of adsorbance are comparatively loaded down with trivial details.Volumetric method device mainly by vacuum pump, piston pump, with reference to cylinder, sample cylinder, pressure gauge, constant temperature oil bath (or constant temperature oven), its principle is similar to pressure application, difference is that the volume that is filled with gas is to record by the volume change of piston pump.There is larger difference in the experimental provision that gravitational method adopts and principle and said two devices, its main device is comprised of electromagnetic suspension system balance, high-pressure sealed cylinder and constant temperature oven.Wherein, airtight cylinder is separated into two confined chambers, and coal sample to be measured and gases at high pressure are placed in respectively in two confined chambers.In experimentation, first record the quality reading of sample; Progressively in sample chamber, be filled with gas to be measured, after charged magnetic suspention balance stable reading, record the sample quality after adsorption equilibrium, the difference of two inferior qualities is the quality of adsorbed gas.And under true formation condition, fluid in coal petrography or shale is subject to the coupling in many, stress field, temperature field etc., and the adsorption/desorption of actual coal-seam gas or shale gas is one and has the very long geochronic continuous physical mechanical process that is subject to many couplings.The effect in stress field and temperature field must cause the adsorption/desorption of actual coal-seam gas or shale gas and Diffusion Law to have the characteristic differing under unstressed condition.And domestic existing method of testing is measured the isothermal adsorption/desorption curve under the true danks reservoir conditions under many couplings such as stress field, temperature field, and then affect the credibility of experimental result.
Summary of the invention:
The object of the present invention is to provide a kind of assay method of danks isothermal adsorption/desorption curve, for measuring differently danks gas absorption/desorption quantity and the isothermal adsorption/desorption curve under layer state truly such as stress, different temperatures.
Object of the present invention realizes according to the following steps: first danks sample test specimen to be measured is placed in to true triaxial core grasping system, sets the initial measured state of sample test specimen according to actual formation condition; In system, inject helium, after system pressure is stable, by inlet end mass flowmeter and pressure transducer, record the gas flow and the system pressure that are filled with respectively, and then demarcate free pore space volume; Again device is vacuumized, according to the system pressure of experimental design, in system, be filled with gas to be measured, according to inlet end high-precision gas mass flowmeter and system pressure sensor, measure respectively the system pressure after inlet end gas integrated flow and balance, calculate adsorbed gas volume, improve successively experimental pressure, repeat above-mentioned steps, until reach the highest experimental pressure; For desorption process, the maximum equalized pressure from isothermal adsorption experiment starts, and successively reduces system experimentation pressure, until minimum experimental pressure; According to endpiece high-precision gas mass flowmeter and system pressure sensor, measure respectively the system pressure after endpiece gas integrated flow and balance, can calculate adsorbed gas volume, according to the system balancing pressure of isothermal adsorption/desorption experiment process record with and corresponding adsorbed gas volume, can obtain isothermal adsorption/desorption curve, specifically be achieved through the following technical solutions:
S1: coal petrography or shale sample test specimen are packed in true triaxial core grasping system;
S2: connect constant temperature oven power supply, set the initial measured state of sample test specimen according to actual formation condition;
S3: be filled with helium (purity > 99.999%) to system, after system pressure is stable, the gas flow and the system pressure that by inlet end high-precision gas mass flowmeter and system pressure sensor record, are filled with respectively, can be by the free space volumes of following formula computing system, repeat to test three times, average as free space volumes:
V free = ZmRT pM - - - ( 1 )
In formula: V freefor free space volumes, m 3; P is the system pressure after balance, Pa; M is the quality that is filled with helium in clamper, g; M is gas relative molecular mass, g/mol; Z is Gas Compression Factor, dimensionless; R is universal gas constant, 8.314J/ (molK); T is system temperature, K.
S4: open vacuum pump, open vacuum pump valve, system is vacuumized, the duration is 6h left and right;
S5: isothermal adsorption experimentation: according to the system pressure of experimental design, be filled with gas to be measured in system, improve successively experimental pressure, until reach the highest experimental pressure of design; By inlet end high-precision gas mass flowmeter and system pressure sensor, measure respectively the system pressure after inlet end gas integrated flow and balance, calculate as follows adsorbed gas volume:
V ad = Z 0 m i RT 0 p 0 M - 0.0224 p V free ZRT - - - ( 2 )
In formula: m ifor inlet end gas integrated flow, g; V adfor the adsorbance of gas to be measured, m 3; Subscript 0 represents standard state.
S6: isothermal desorption experimentation: the maximum equalized pressure from isothermal adsorption experiment starts, and successively reduces system experimentation pressure, until the minimum experimental pressure of design; By endpiece high-precision gas mass flowmeter and system pressure sensor, measure respectively the system pressure after endpiece gas integrated flow and balance, calculate as follows adsorbed gas volume:
V ad = Z 0 ( m t - m o ) RT 0 p 0 M - 0.0224 p V free ZRT - - - ( 3 )
In formula: m tfor accumulative total is filled with the gaseous mass to be measured in system, g; m ofor endpiece gas integrated flow to be measured, g.
S7: according to the system balancing pressure of isothermal adsorption/desorption experiment record with and corresponding adsorbed gas volume, draw isothermal adsorption/desorption curve.
Further, the initial measured state of described setting sample test specimen, specifically comprises the following steps:
S21: connect constant temperature oven power supply, reserve experimental temperature according to actual formation temperature setting, and to the emptying oiling in triaxial cell of true triaxial core grasping system, check whether each system normally works;
S22: checking experiment device impermeability, open vacuum pump, open vacuum pump valve, sample test specimen to be carried out degassed, the degassed time is 3-6h;
S23: true triaxial core grasping system entirety is put into constant temperature oven or thermostatical oil bath cabinet, and according to the axial compression of actual formation condition setting and confined pressure.
Further, described isothermal adsorption experimentation, specifically comprises the following steps:
S51: open inlet end high-precision gas mass flowmeter power switch and high pressure gas cylinder reduction valve to be measured, regulate the high pressure gas cylinder to be measured valve of giving vent to anger, in system, be filled with gas to be measured to experimental design pressure, close the high pressure gas cylinder to be measured valve of giving vent to anger, by inlet end high-precision gas mass flowmeter record, be filled with the quality of gas;
S52: keep 24-48h, make sample test specimen fully adsorb gas to be measured, treat that system pressure sensor institute measuring pressure value tends towards stability, by system pressure sensor, determine the system pressure after balance, according to formula (2), calculate and record the adsorbed gas volume that this equalized pressure is corresponding;
S53: according to experiment needs, improve successively system experimentation pressure, repeating step S51-S52, until reach the highest system experimentation pressure.
Further, described isothermal desorption experimentation, specifically comprises the following steps:
S61: close inlet end high-precision gas mass flowmeter power switch, open endpiece high-precision gas mass flowmeter power switch, open endpiece venting valve, emit part gas to be measured to experimental design pressure, close venting valve, by endpiece high-precision gas mass flowmeter record, emit the quality of gas;
S62: keep 24-48h, make sample test specimen fully adsorb gas to be measured, treat that system pressure sensor institute measuring pressure value tends towards stability, by system pressure sensor, determine the system pressure after balance, according to formula (3), calculate and record the adsorbed gas volume that this equalized pressure is corresponding;
S63: according to experiment needs, successively reduce system experimentation pressure, repeating step S61-S62, until reach minimum experimental pressure.
Beneficial effect of the present invention:
1, concentrated expression of the present invention the impacts on danks gas absorption/desorb such as stress, pore pressure, temperature, both can carry out the test under single-factor influence, also can carry out the test under multifactor coupling, the test of carrying out can be reproduced the residing environment of actual danks gas absorption/desorb more realistically;
2, higher sensor and the mass-flow gas meter of data acquisition system adopted sensitivity of the present invention and degree of accuracy, comprises system pressure sensor, system temperature sensor, mass-flow gas meter etc., has guaranteed the reliability of data acquisition;
3, stress loading servo apply hydraulic pressure system of the present invention, loading procedure is stable, and can guarantee loading accuracy, can realize circulation and add the testing programs such as unloaded;
4, the present invention adopts high-precision gas mass flow meter measurement danks to adsorb gas flow to be measured, has not only simplified experimental provision, and also simplification greatly of experiment process, and late time data processing and amount of calculation are relatively less.
Accompanying drawing explanation:
Fig. 1 is the schematic diagram of one embodiment of the invention.
Wherein: 1-vacuum pump; 2-vacuum pump valve; 3-high pressure helium gas cylinder; 4-high pressure gas cylinder to be measured; 5-high pressure helium gas cylinder air outlet valve door; 6-high pressure helium gas cylinder reduction valve; The 7-high pressure gas cylinder to be measured valve of giving vent to anger; 8-high pressure gas cylinder reduction valve to be measured; 9-inlet end high-grade pressure gauge; 10-inlet end high-precision gas mass flowmeter; 11-system pressure sensor; The true triaxial core clamping of 12-and compression system; 13-constant temperature oven; 14-system temperature sensor; 15-endpiece venting valve; 16-endpiece high-precision gas mass flowmeter.
Embodiment:
Below in conjunction with drawings and Examples, the invention will be further described, but do not limit practical range of the present invention.
Take methane (purity >99.99%), the isothermal adsorption/desorption experiment in Southern Qinshui Basin coal sample is example explaination the present invention below.
Referring to Fig. 1, first the raw coal coal sample of the Φ 50 × 100mm drilling through is placed in to saturation water in climatic chamber and uses in order to test.Coal petrography or shale sample test specimen are packed in true triaxial core clamping and compression system 12; Connect constant temperature oven 13 power supplys, according to 23 ℃ of actual formation Temperature Setting experimental temperatures, by system temperature sensor 14, monitor temperature in core holding unit; And to the emptying oiling in triaxial cell of the clamping of true triaxial core and compression system 12, check whether each system normally works; After arrangement, close vacuum pump valve 2, high pressure gas cylinder to be measured give vent to anger valve 7 and endpiece venting valve 15, open high pressure helium gas cylinder air outlet valve door 5, after being filled with a certain amount of helium in system, close the valve 5 of giving vent to anger, after pressure stability, every 1h register system pressure, change, if system pressure, without significant change, illustrates that impermeability is good in 6h; If system pressure changes obviously, illustrate that impermeability is poor, need reexamine and assemble experimental provision.If impermeability is good, open vacuum pump 1, open vacuum pump valve 2, sample test specimen is carried out degassed, in order to eliminate the impact of coal sample absorbed air on test findings, the degassed time is 3-6h, until system pressure without significant change, is closed vacuum pump 1 and vacuum pump valve 2; True triaxial core grasping system 12 entirety are put into constant temperature oven 13, and according to actual formation condition setting confined pressure 8.21MPa; Open high pressure helium gas cylinder air outlet valve door 5, to true triaxial core grasping system 12, be filled with after a certain amount of helium (purity > 99.999%), close the valve 5 of giving vent to anger, after system pressure is stable, by inlet end high-precision gas mass flowmeter 10 and system pressure sensor 11, measure and record the methane gas quality and the system pressure that are filled with respectively, according to the free space volumes of formula (1) computing system; Repeat to test three times, average as free space volumes; Open vacuum pump 1, open vacuum pump valve 2, system is vacuumized, the duration is 6h left and right, until pressure without significant change, is closed vacuum pump 1 and vacuum pump valve 2; Open inlet end high-precision gas mass flowmeter 10 power switches and high pressure methane gas cylinder reduction valve 8, regulate the high pressure methane gas cylinder valve 7 of giving vent to anger, in system, be filled with methane gas (purity >99.99%) to experimental design pressure, close the valve 7 of giving vent to anger, according to inlet end high-precision gas mass flowmeter 10 records, be filled with the quality of gas; After system pressure balance (time is generally 24-48h), by system pressure sensor 11, record the system pressure after balance, according to formula (2), calculate and record the adsorbed gas volume that this equalized pressure is corresponding; Improve successively system experimentation pressure, to true triaxial core clamping and compression system 12, be filled with methane gas, adsorption equilibrium pressure is increased gradually, can record the isothermal adsorption curve of methane in coal petrography.By the experiment of isothermal adsorption repeatedly, until reach after the highest contrived experiment force value, carry out desorption experiment process.Close inlet end high-precision gas mass flowmeter 10 power switches, open endpiece high-precision gas mass flowmeter 16 power switches, slowly open endpiece venting valve 15, emit part methane gas to experimental design pressure, close venting valve 15, according to endpiece high-precision gas mass flowmeter 16 records, emit the quality of gas, after system pressure balance (time is generally 24-48h), by system pressure sensor 11, record the system pressure after balance, according to formula (3), calculate the adsorbed gas scale of construction in desorption process.Repeat to discharge the operation of methane gas, and calculate and record methane adsorbance corresponding under this equalized pressure according to formula (3), successively reduce system experimentation pressure and test, until reach minimum experimental pressure, can draw desorption process methane isothermal adsorption curve.
In sum; these are only preferred embodiment of the present invention, but protection scope of the present invention is not limited to this, any be familiar with those skilled in the art the present invention disclose technical scope in; the variation that can expect easily or conversion, within all should being encompassed in protection scope of the present invention.

Claims (4)

1. the assay method of a danks isothermal adsorption/desorption curve, comprise that setting initial measured state, demarcation free space volumes, isothermal adsorption experimentation, isothermal desorption experimentation and isothermal adsorption/desorption curve draws, it is characterized in that, comprise the following steps:
S1: coal petrography or shale test specimen are inserted in true triaxial core grasping system, set the initial measured state of test specimen according to actual formation condition;
S2: the helium that is filled with purity > 99.999% to system, after system pressure is stable, by fill gas weight and the system pressure of inlet end high-precision gas mass flowmeter and system pressure sensor record, by the free space volumes of following formula computing system: get the mean value of three replications as calibration value, in formula, V freefor free space volumes, m 3; P is the system pressure after balance, Pa; M is the quality that system is filled with helium, g; M is gas relative molecular mass, g/mol; Z is Gas Compression Factor, dimensionless; R is universal gas constant, 8.314J/ (molK); T is system temperature, K;
S3: open vacuum pump valve, system is vacuumized, the duration is 3-6h;
S4: test specimen isothermal adsorption experimentation: according to the system pressure of experimental design, be filled with gas to be measured in system, improve successively experimental pressure, until reach the highest experimental pressure; By the system pressure after system entry end high-precision gas mass flowmeter and system pressure sensor difference record entry end gas buildup influx and balance, be calculated as follows adsorbed gas volume: in formula, m ifor inlet end gas buildup flow, g; V adfor the adsorbance of gas to be measured, m 3; Subscript 0 represents standard state;
S5: test specimen isothermal desorption experimentation: the maximum equalized pressure from isothermal adsorption experiment starts, and successively reduces system experimentation pressure, until minimum experimental pressure; By system outlet end high-precision gas mass flowmeter and system pressure sensor, record respectively the system pressure after endpiece gas buildup discharge and balance, be calculated as follows adsorbed gas volume: in formula, m tfor accumulative total is filled with the gaseous mass to be measured in system, g; m ofor endpiece gas buildup discharge to be measured, g,
S6: according to the system balancing pressure of isothermal adsorption/desorption experiment record with and corresponding adsorbed gas volume data, draw the isothermal adsorption/desorption curve of test specimen.
2. the assay method of danks isothermal adsorption/desorption curve as claimed in claim 1, is characterized in that, the initial measured state of the setting test specimen in described step S1 is further comprising the steps:
S11: connect constant temperature oven or thermostatical oil bath cabinet power supply, reserve experimental temperature according to actual formation temperature setting, and by emptying the triaxial cell of system oiling, check whether each system normally works;
S12: check system impermeability, open vacuum pump valve, to the degassed 3-6h of sample test specimen;
S13: true triaxial core grasping system entirety is put into constant temperature oven or thermostatical oil bath cabinet, and according to the axial compression of actual formation condition setting and confined pressure.
3. the assay method of danks isothermal adsorption/desorption curve as claimed in claim 1, is characterized in that, the test specimen isothermal adsorption experimentation of described step S4 is further comprising the steps:
S41: regulate the high pressure gas cylinder to be measured valve of giving vent to anger, be filled with gas to be measured to experimental design pressure in system, close the gas cylinder valve of giving vent to anger, be filled with the quality of gas by inlet end high-precision gas mass flowmeter record;
S42: keep 24-48h, make sample test specimen fully adsorb gas to be measured, treat that system pressure sensor institute measuring pressure value tends towards stability, and determines the system pressure after balance by system pressure sensor, according to formula calculate and record the adsorbed gas volume that this equalized pressure is corresponding;
S43: according to experiment needs, improve successively system experimentation pressure, repeating step S41-S42, until reach the highest system experimentation pressure.
4. the assay method of danks isothermal adsorption/desorption curve as claimed in claim 1, is characterized in that, the test specimen isothermal desorption experimentation of described step S5 is further comprising the steps:
S51: open endpiece venting valve, emit part gas to be measured to experimental design pressure, close venting valve, emit the quality of gas by endpiece high-precision gas mass flowmeter record;
S52: keep 24-48h, make sample test specimen fully adsorb gas to be measured, treat that system pressure sensor institute measuring pressure value tends towards stability, and determines the system pressure after balance by system pressure sensor, according to formula calculate and record the adsorbed gas volume that this equalized pressure is corresponding;
S53: according to experiment needs, successively reduce system experimentation pressure, repeating step S51-S52, until reach minimum experimental pressure.
CN201310030953.8A 2013-01-28 2013-01-28 Measuring method for isothermal adsorption/desorption curve of coaly shale CN103115844B (en)

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