CN103115844A - 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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CN103115844A
CN103115844A CN2013100309538A CN201310030953A CN103115844A CN 103115844 A CN103115844 A CN 103115844A CN 2013100309538 A CN2013100309538 A CN 2013100309538A CN 201310030953 A CN201310030953 A CN 201310030953A CN 103115844 A CN103115844 A CN 103115844A
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pressure
gas
measured
desorption
test specimen
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CN103115844B (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 method at present commonly used, 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, at first be filled with gas in the reference cylinder, after pressure stability, measure and record with reference to cylinder pressure; Then with sample cylinder be communicated with reference to cylinder, after pressure equilibrium, working sample cylinder pressure; Calculate the volume of adsorbed gas by the equation of gas state.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 the gas-solid adsorption curve is most widely used, but its operating process is complicated; In addition, the computation process of the processing of the data in later stage and adsorbance is comparatively loaded down with trivial details.The 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, the volume that is filled with gas is that the volume change by piston pump records.There are larger difference in the experimental provision that gravitational method adopts and principle and said two devices, and 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, at first record the quality reading of sample; Progressively be filled with gas to be measured in the sample chamber, record the sample quality after adsorption equilibrium after charged magnetic suspention balance stable reading, 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 subjected 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 that the characteristic that differs under unstressed condition is arranged.And domestic existing method of testing is measured the isothermal adsorption/desorption curve under true danks reservoir conditions under many couplings such as stress field, temperature field, and then affects 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, be used for measuring differently danks gas absorption/desorption quantity and the isothermal adsorption/desorption curve under layer state truly such as stress, different temperatures.

Purpose of the present invention realizes according to the following steps: at first danks sample test specimen to be measured is placed in true triaxial core grasping system, sets the initial measured state of sample test specimen according to the actual formation condition; Inject helium in system, after system pressure is stable, the gas flow and the system pressure that are filled with by inlet end mass flowmeter and pressure transducer record respectively, and then demarcate the free pore space volume; Again device is vacuumized, system pressure according to experimental design, be filled with gas to be measured in system, measure respectively system pressure after inlet end gas integrated flow and balance according to inlet end high-precision gas mass flowmeter and system pressure sensor, calculate the adsorbed gas volume, improve successively experimental pressure, repeat above-mentioned steps, until reach the highest experimental pressure; For desorption process, from the maximum equalized pressure after the isothermal adsorption experiment, successively reduce system experimentation pressure, until minimum experimental pressure; Measure respectively system pressure after endpiece gas integrated flow and balance according to endpiece high-precision gas mass flowmeter and system pressure sensor, can calculate the 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 the constant temperature oven power supply, set the initial measured state of sample test specimen according to the 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 are filled with by inlet end high-precision gas mass flowmeter and system pressure sensor record respectively, can be by the free space volumes of following formula computing system, repeated experiments three times, average as free space volumes:

V free = ZmRT pM - - - ( 1 )

In formula: V FreeBe free space volumes, m 3P is the system pressure after balance, Pa; M is the quality that is filled with helium in clamper, g; M is the 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 the vacuum pump valve, system is vacuumized, the duration is the 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; Measure respectively system pressure after inlet end gas integrated flow and balance by inlet end high-precision gas mass flowmeter and system pressure sensor, calculate as follows the adsorbed gas volume:

V ad = Z 0 m i RT 0 p 0 M - 0.0224 p V free ZRT - - - ( 2 )

In formula: m iBe inlet end gas integrated flow, g; V adBe the adsorbance of gas to be measured, m 3Subscript 0 represents standard state.

S6: isothermal desorption experimentation: from the maximum equalized pressure after the isothermal adsorption experiment, successively reduce system experimentation pressure, until the minimum experimental pressure of design; Measure respectively system pressure after endpiece gas integrated flow and balance by endpiece high-precision gas mass flowmeter and system pressure sensor, calculate as follows the 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 adding up to be filled with the gaseous mass to be measured in system, g; m oBe 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 the constant temperature oven power supply, reserve experimental temperature according to the actual formation temperature setting, and to the emptying oiling in the triaxial cell of true triaxial core grasping system, check whether each system works;

S22: checking experiment device impermeability, open vacuum pump, open the vacuum pump valve, the sample test specimen to be carried out degassed, the degassed time is 3-6h;

S23: true triaxial core grasping system integral body 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, be filled with gas to be measured to experimental design pressure in system, close the high pressure gas cylinder to be measured valve of giving vent to anger, be filled with the quality of gas by inlet end high-precision gas mass flowmeter record;

S52: keep 24-48h, make the sample test specimen fully adsorb gas to be measured, treat that system pressure sensor institute measuring pressure value tends towards stability, determine system pressure after balance to calculate and record adsorbed gas volume corresponding to this equalized pressure according to formula (2) by the system pressure sensor;

S53: according to the experiment needs, improve successively system experimentation pressure, repeating step S51-S52 is 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 the venting valve, emit the quality of gas by endpiece high-precision gas mass flowmeter record;

S62: keep 24-48h, make the sample test specimen fully adsorb gas to be measured, treat that system pressure sensor institute measuring pressure value tends towards stability, determine system pressure after balance to calculate and record adsorbed gas volume corresponding to this equalized pressure according to formula (3) by the system pressure sensor;

S63: according to the experiment needs, successively reduce system experimentation pressure, repeating step S61-S62 is 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, comprise system pressure sensor, system temperature sensor, mass-flow gas meter etc., guaranteed the reliability of data acquisition;

3, stress loading servo apply hydraulic pressure of the present invention system, loading procedure is stable, and can guarantee loading accuracy, can realize that circulation adds the testing programs such as unloaded;

4, the present invention adopts high-precision gas mass flow meter measurement danks absorption 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.

Description of drawings:

Fig. 1 is the schematic diagram of one embodiment of the invention.

Wherein: the 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; The 13-constant temperature oven; 14-system temperature sensor; 15-endpiece venting valve; 16-endpiece high-precision gas mass flowmeter.

Embodiment:

The invention will be further described below in conjunction with drawings and Examples, but do not limit practical range of the present invention.

Below take the isothermal adsorption/desorption experiment of methane (purity〉99.99%) in the Southern Qinshui Basin coal sample as example explaination the present invention.

Referring to Fig. 1, at first the raw coal coal sample of Φ 50 * 100mm of drilling through is placed in climatic chamber saturation water 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 temperature in system temperature sensor 14 monitoring core holding units; And to the emptying oiling in triaxial cell of true triaxial core clamping and compression system 12, check whether each system works; Settle complete after, close vacuum pump valve 2, high pressure gas cylinder to be measured give vent to anger valve 7 and endpiece venting valve 15, the opening high pressure helium tank valve 5 of giving vent to anger, close the valve 5 of giving vent to anger after being filled with a certain amount of helium in the system, change every 1h register system pressure after pressure stability, if in 6h, system pressure without significant change, illustrates that impermeability is good; If system pressure changes obviously, illustrate that impermeability is relatively poor, need reexamine and assemble experimental provision.If impermeability is good, open vacuum pump 1, open vacuum pump valve 2, the sample test specimen is carried out degassed, in order to eliminate the coal sample absorbed air to the impact of 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 integral body are put into constant temperature oven 13, and according to actual formation condition setting confined pressure 8.21MPa; The opening high pressure helium tank valve 5 of giving vent to anger, after being filled with a certain amount of helium (purity>99.999%) to true triaxial core grasping system 12, close the valve 5 of giving vent to anger, after system pressure is stable, measure and record by inlet end high-precision gas mass flowmeter 10 and system pressure sensor 11 methane gas quality and the system pressure that is filled with respectively, according to the free space volumes of formula (1) computing system; Repeated experiments three times is averaged as free space volumes; Open vacuum pump 1, open vacuum pump valve 2, system is vacuumized, the duration is the 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, be filled with methane gas (purity〉99.99%) in the system to experimental design pressure, close the valve 7 of giving vent to anger, be filled with the quality of gas according to inlet end high-precision gas mass flowmeter 10 records; After the system pressure balance (time is generally 24-48h), record system pressure after balance by system pressure sensor 11, calculate and record adsorbed gas volume corresponding to this equalized pressure according to formula (2); Improve successively system experimentation pressure, be filled with methane gas to true triaxial core clamping and compression system 12, 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 after reaching the highest contrived experiment force value, carry out the 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 the part methane gas to experimental design pressure, close venting valve 15, emit the quality of gas according to endpiece high-precision gas mass flowmeter 16 records, after the system pressure balance (time is generally 24-48h), record system pressure after balance by system pressure sensor 11, calculate the adsorbed gas scale of construction in desorption process according to formula (3).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, anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or conversion are 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, is characterized in that, comprises the following steps:
S1: coal petrography or shale sample test specimen are packed in true triaxial core grasping system;
S2: connect the constant temperature oven power supply, set the initial measured state of sample test specimen according to the actual formation condition;
S3: the helium that is filled with purity>99.999% to system, after system pressure is stable, the gas flow and the system pressure that are filled with by inlet end high-precision gas mass flowmeter and system pressure sensor record respectively, free space volumes by the following formula computing system, repeated experiments three times, average as free space volumes: In formula, V FreeBe free space volumes, m 3P is the system pressure after balance, Pa; M is the quality that is filled with helium in clamper, g; M HeBe gas relative molecular mass, g/mol; Z is Gas Compression Factor, dimensionless; R is universal gas constant, 8.314J/ (mol*K); T is system temperature, K;
S4: open vacuum pump, open the vacuum pump valve, system is vacuumized, the duration is 3-6h;
S5: sample 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; Measure respectively system pressure after inlet end gas integrated flow and balance by inlet end high-precision gas mass flowmeter and system pressure sensor, calculate as follows the adsorbed gas volume: In formula, m iBe inlet end gas integrated flow, g; V adBe the adsorbance of gas to be measured, m 3Subscript 0 represents standard state;
S6: sample test specimen isothermal desorption experimentation: from the maximum equalized pressure after the isothermal adsorption experiment, successively reduce system experimentation pressure, until minimum experimental pressure; Measure respectively system pressure after endpiece gas integrated flow and balance by endpiece high-precision gas mass flowmeter and system pressure sensor, calculate as follows the adsorbed gas volume: In formula, m tFor adding up to be filled with the gaseous mass to be measured in system, g; m oBe 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.
2. the assay method of danks isothermal adsorption/desorption curve as claimed in claim 1, is characterized in that, sets the initial measured state of sample test specimen in described step S2, and is further comprising the steps:
S21: connect the constant temperature oven power supply, reserve experimental temperature according to the actual formation temperature setting, and to the emptying oiling in the triaxial cell of true triaxial core grasping system, check whether each system works;
S22: checking experiment device impermeability, open vacuum pump, open the vacuum pump valve, the sample test specimen to be carried out degassed, the degassed time is 3-6h;
S23: true triaxial core grasping system integral body 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, sample test specimen isothermal adsorption experimentation in described step S5 is further comprising the 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, be filled with gas to be measured to experimental design pressure in system, close the valve of giving vent to anger, be filled with the quality of gas by inlet end high-precision gas mass flowmeter record;
S52: keep 24-48h, make the sample test specimen fully adsorb gas to be measured, treat that system pressure sensor institute measuring pressure value tends towards stability, determine system pressure after balance by the system pressure sensor, according to formula Calculate and record adsorbed gas volume corresponding to this equalized pressure;
S53: according to the experiment needs, improve successively system experimentation pressure, repeating step S51-S52 is 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, sample test specimen isothermal desorption experimentation in described step S6 is further comprising the 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 the venting valve, emit the quality of gas by endpiece high-precision gas mass flowmeter record;
S62: keep 24-48h, make the sample test specimen fully adsorb gas to be measured, treat that system pressure sensor institute measuring pressure value tends towards stability, determine system pressure after balance by the system pressure sensor, according to formula Calculate and record adsorbed gas volume corresponding to this equalized pressure;
S63: according to the experiment needs, successively reduce system experimentation pressure, repeating step S61-S62 is 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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CN103439238A (en) * 2013-09-03 2013-12-11 中国地质大学(北京) Measurement method of storage porosity in coal shale
CN103776713A (en) * 2014-01-09 2014-05-07 中国石油天然气股份有限公司 Dense rock gas desorption rate testing device
CN103885496A (en) * 2014-03-28 2014-06-25 黄斌 High and low temperature triaxial test temperature control device
CN104502224A (en) * 2014-08-14 2015-04-08 中国石油大学(华东) Device and method for determination of coal rock isothermal desorption curve under saturated water condition
CN104713802A (en) * 2015-04-01 2015-06-17 中国石油化工股份有限公司江汉油田分公司勘探开发研究院 Method and device for testing gas content of shale gas reservoir
CN104713803A (en) * 2015-03-16 2015-06-17 中国石油大学(华东) Method for accurately measuring absorbed phase density of methane on shale
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CN103439238B (en) * 2013-09-03 2015-07-08 中国地质大学(北京) Measurement method of storage porosity in coal shale
CN103776713A (en) * 2014-01-09 2014-05-07 中国石油天然气股份有限公司 Dense rock gas desorption rate testing device
CN104897525B (en) * 2014-03-03 2017-08-04 中国石油化工股份有限公司 The test system and method for diffusion coefficient and isothermal adsorption/desorption curve
CN104897525A (en) * 2014-03-03 2015-09-09 中国石油化工股份有限公司 Diffusion coefficient and isothermal adsorption/desorption curve test system and method
CN103885496A (en) * 2014-03-28 2014-06-25 黄斌 High and low temperature triaxial test temperature control device
CN104502224A (en) * 2014-08-14 2015-04-08 中国石油大学(华东) Device and method for determination of coal rock isothermal desorption curve under saturated water condition
CN104502224B (en) * 2014-08-14 2016-04-20 中国石油大学(华东) Saturation water Coal Under rock isothermal desorption curve determination device and method
CN104713803A (en) * 2015-03-16 2015-06-17 中国石油大学(华东) Method for accurately measuring absorbed phase density of methane on shale
CN104713803B (en) * 2015-03-16 2017-05-17 中国石油大学(华东) Method for accurately measuring absorbed phase density of methane on shale
CN104713802B (en) * 2015-04-01 2018-12-04 中国石油化工股份有限公司江汉油田分公司勘探开发研究院 A kind of shale gas reservoir gassiness weight testing method
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CN106323833A (en) * 2015-07-08 2017-01-11 中国石油天然气股份有限公司 Core porosity measurement method and device
CN106370576A (en) * 2015-07-20 2017-02-01 中国石油化工股份有限公司 Simulation apparatus and method for researching permeability of coal rock
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