CN103149118A - Carbonaceous shale isothermal adsorption/desorption experimental device - Google Patents

Carbonaceous shale isothermal adsorption/desorption experimental device Download PDF

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Publication number
CN103149118A
CN103149118A CN2013100326389A CN201310032638A CN103149118A CN 103149118 A CN103149118 A CN 103149118A CN 2013100326389 A CN2013100326389 A CN 2013100326389A CN 201310032638 A CN201310032638 A CN 201310032638A CN 103149118 A CN103149118 A CN 103149118A
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CN
China
Prior art keywords
pressure
inlet
gas
triaxial core
desorption
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CN2013100326389A
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Chinese (zh)
Inventor
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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Priority to CN2013100326389A priority Critical patent/CN103149118A/en
Publication of CN103149118A publication Critical patent/CN103149118A/en

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Abstract

The invention provides an experimental device for testing adsorption/desorption amounts of gas on carbonaceous shale and adsorption/desorption curves. The device is mainly composed of real triaxial core clamping and compression system, a system pressure sensor, a system temperature sensor, an inlet end high-grade pressure gauge, an inlet end high-precision gas mass flow meter, an outlet high-precision gas mass flow meter, a vacuum pump, a high pressure helium tank, a high pressure to-be-measured gas cylinder, a thermostat, a corresponding pipeline and a valve. A carbonaceous shale test piece is placed in the real triaxial core clamping and compression system. An initial measuring condition of the test piece is set according to a real formation condition. After free pore volume is set, an adsorption/desorption test of the test piece is performed. According to a gas cumulative discharge value and a balanced system pressure value which are measured and recorded by the inlet end high-precision gas mass flow meter or the outlet end high-precision gas mass flow meter end and the system pressure sensor, adsorbed gas volume is calculated so that the isothermal adsorption/desorption curve of the carbonaceous shale test piece is drawn.

Description

A kind of danks isothermal adsorption/desorption experimental apparatus
Technical field:
The present invention relates to a kind of experimental provision of measuring danks surface gas adsorption/desorption amount and adsorption/desorption curve, espespecially measure the experimental provision of danks surface gas adsorption/desorption amount and 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).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, and higher to manometric accuracy requirement.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.But volumetric method is high to the pressure precision requirement of piston pump, and operating process is complicated.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.Gravitational method experimental provision cost used is relatively costly, uses at present few.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 experimental provision can't be realized the real simulation to formation condition, namely can't measure the isothermal adsorption/desorption curve under the 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 danks isothermal adsorption/desorption experimental apparatus, be used for measuring differently danks surface gas adsorption/desorption amount and the isothermal adsorption/desorption curve under layer state truly such as stress, different temperatures.
Purpose of the present invention realizes according to following design: described experimental provision mainly is comprised of vacuum pump, high pressure helium gas cylinder, high pressure gas cylinder to be measured, inlet end high-grade pressure gauge, inlet end high-precision gas mass flowmeter, endpiece high-precision gas mass flowmeter, true triaxial core clamping and compression system, system pressure sensor, system temperature sensor, constant temperature oven and respective lines, valve.Described inlet end high-precision gas mass flowmeter interface and true triaxial core grasping system air intake opening, inlet end high-grade pressure gauge interface are connected in series by pipeline; Inlet end is equipped with four-way piece, and four interfaces of described four-way piece are connected with vacuum pump with inlet end high-grade pressure gauge interface, high pressure gas cylinder reduction valve outlet to be measured, the outlet of high pressure helium gas cylinder reduction valve respectively; Described vacuum pump interface arranges a valve; Described endpiece high-precision gas mass flowmeter interface be connected triaxial core grasping system gas outlet and connect by pipeline, the centre arranges the venting valve.Described true triaxial core grasping system is packed in constant temperature oven, and described constant temperature oven is used for arranging and keeping the real formation temperature conditions of sample test specimen.
described true triaxial core clamping and compression system adds by true triaxial core the system of holding and hydraulic servo control system forms, the supporting Z axis automatic pressure oil pump of described hydraulic servo control system and two X, the Y-axis automatic pressure oil pump, described Z axis automatic pressure oil pump links by the Z axis oil-in of pipeline and described true triaxial core grasping system, to Z axis piston cylinder infusion liquid, described X, the Y-axis automatic pressure oil pump respectively with the X of described true triaxial core grasping system, the Y-axis oil-in links, directly to described X, infusion liquid in Y confined pressure packing element, realize that axial compression loading and confined pressure load.
Further, described automatic pressure oil pump can be realized automatic value-added tax function by computer control, possesses constant current and pressure-keeping functions.
Described true triaxial core grasping system is comprised of clamp body, X, Y confined pressure packing element, rock core packing element, Z axis plunger, Z axis pressure chamber, upper cover, sealing platen, packing element grommet, stop grommet, stop plug, stop plunger.Be processed with vertically cross special-shaped hole in the middle of described clamp body, spatially form four relative grooves, groove is used for placing X, Y confined pressure packing element and rock core packing element; Described X, Y confined pressure packing element are four prolate square hollow cylinders, quality of rubber materials, and an end sealing, an end be the opening with flange, is used for the insert-seal platen to seal the pressure of X, Y-direction; Described rock core packing element center has the column type through hole, quality of rubber materials, and the heart cylindrical rock core of can packing into therein, two ends are pressed into respectively the packing element grommet, the stop grommet plays and supports and the auxiliary seal effect, insert described Z axis plunger and described stop plunger; The end face of described stop plunger and described Z axis plunger offers the waterline groove of the mutual communications and liaison of ring-type, and warranty test medium and rock core have larger contact area.
Beneficial effect of the present invention:
1, concentrated expression the impacts on danks surface gas adsorption/desorption 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 surface gas adsorption/desorption more realistically.
2, data acquisition system adopted sensitivity and degree of accuracy are higher sensor and mass-flow gas meter comprise system pressure sensor, system temperature sensor, mass-flow gas meter etc., have guaranteed the reliability of data acquisition.
3, stress loading servo apply hydraulic pressure system, loading procedure is stable, and can guarantee loading accuracy, can realize that circulation adds the testing programs such as unloaded.
4, adopt high-precision gas mass flow meter measurement danks absorption gas flow to be measured, not only simplified experimental provision, and also simplification greatly of experiment process, 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.
In figure, 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 present invention is described in further detail below in conjunction with drawings and Examples, but do not limit practical range of the present invention.
The below is take the isothermal adsorption/desorption experiment of methane (purity〉99.99%) in the Southern Qinshui Basin coal sample as example explaination operating process of 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.Therefore, protection scope of the present invention should be as the criterion with the protection domain that claim was defined.

Claims (3)

1. danks isothermal adsorption/desorption experimental apparatus, comprise true triaxial core clamping and compression system, system pressure sensor, system temperature sensor, inlet end high-grade pressure gauge, inlet end high-precision gas mass flowmeter, endpiece high-precision gas mass flowmeter, vacuum pump, high pressure helium gas cylinder, high pressure gas cylinder to be measured, constant temperature oven, pipeline and valve, it is characterized in that, described inlet end high-precision gas mass flowmeter interface be connected triaxial core grasping system air intake opening, inlet end high-grade pressure gauge interface and connect by pipeline; Described inlet end high-grade pressure gauge interface is connected with the four-way piece of inlet end; Four interfaces of described four-way piece are connected with vacuum pump with inlet end high-grade pressure gauge interface, high pressure gas cylinder reduction valve outlet to be measured, the outlet of high pressure helium gas cylinder reduction valve respectively; Described vacuum pump interface arranges a valve; Described endpiece high-precision gas mass flowmeter interface be connected triaxial core grasping system gas outlet and connect by pipeline, the centre arranges the venting valve.
2. danks isothermal adsorption/desorption experimental apparatus as claimed in claim 1, it is characterized in that, described true triaxial core clamping and compression system adds by true triaxial core the system of holding and hydraulic servo control system forms, the supporting Z axis automatic pressure oil pump of described hydraulic servo control system and two X, the Y-axis automatic pressure oil pump, described Z axis automatic pressure oil pump links by the Z axis oil-in of pipeline and described true triaxial core grasping system, to Z axis piston cylinder infusion liquid, described X, the Y-axis automatic pressure oil pump respectively with the X of described true triaxial core grasping system, the Y-axis oil-in links, directly to described X, infusion liquid in Y confined pressure packing element, realize that axial compression loading and confined pressure load.
3. danks isothermal adsorption/desorption experimental apparatus as claimed in claim 1, is characterized in that, described true triaxial core grasping system is packed in constant temperature oven.
CN2013100326389A 2013-01-28 2013-01-28 Carbonaceous shale isothermal adsorption/desorption experimental device CN103149118A (en)

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Cited By (12)

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Publication number Priority date Publication date Assignee Title
CN103822856A (en) * 2014-03-14 2014-05-28 中国矿业大学(北京) Coal gas adsorption/desorption diffusion simulation experiment device under different stress constraint conditions
CN104048982A (en) * 2014-06-30 2014-09-17 中国科学院武汉岩土力学研究所 Multifunctional rock core holder for rock core scale nuclear magnetic resonance test
CN104897514A (en) * 2015-06-12 2015-09-09 徐春碧 Device for measuring danks surface gas adsorption and danks desorption curves
CN105484713A (en) * 2015-12-25 2016-04-13 中国石油天然气股份有限公司 Experimental method and device for simulating shale gas pool exploitation
CN106066291A (en) * 2016-06-16 2016-11-02 中国华能集团公司 CO2displacement shale gas and shale are to shale gas or CO2absorption analytic simulation test System and method for
CN106093345A (en) * 2016-06-16 2016-11-09 中国华能集团公司 A kind of simulation CO2the method of displacement displacement shale pneumatic state process
CN106168565A (en) * 2015-07-17 2016-11-30 中国石油天然气股份有限公司 A kind of device and method measuring shale substrate air content
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
CN107462472A (en) * 2017-07-26 2017-12-12 太原理工大学 A kind of experimental simulation device and analogy method of the compound fracturing coal body of temperature and pressure pulse
CN107478559A (en) * 2017-07-26 2017-12-15 太原理工大学 A kind of device and method simulated gas and migrated in different-grain diameter size coal sample
CN107976351A (en) * 2017-11-27 2018-05-01 大连理工大学 A kind of ocean gas hydrate core remodeling device and method
CN108663498A (en) * 2017-03-27 2018-10-16 中国石油化工股份有限公司 The shale gas site desorption experimental provision and method of high temperature decompression and pressure break

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Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103822856B (en) * 2014-03-14 2016-08-31 中国矿业大学(北京) Coal body gas adsorption desorbing diffusion modeling experiments device under the conditions of different stress constraints
CN103822856A (en) * 2014-03-14 2014-05-28 中国矿业大学(北京) Coal gas adsorption/desorption diffusion simulation experiment device under different stress constraint conditions
CN104048982A (en) * 2014-06-30 2014-09-17 中国科学院武汉岩土力学研究所 Multifunctional rock core holder for rock core scale nuclear magnetic resonance test
CN104897514A (en) * 2015-06-12 2015-09-09 徐春碧 Device for measuring danks surface gas adsorption and danks desorption curves
CN106168565A (en) * 2015-07-17 2016-11-30 中国石油天然气股份有限公司 A kind of device and method measuring shale substrate air content
CN106370576B (en) * 2015-07-20 2019-04-02 中国石油化工股份有限公司 For studying the simulator and method of Permeability Oe Coal And Porous Rock And Fractured Rock
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
CN105484713A (en) * 2015-12-25 2016-04-13 中国石油天然气股份有限公司 Experimental method and device for simulating shale gas pool exploitation
CN106093345A (en) * 2016-06-16 2016-11-09 中国华能集团公司 A kind of simulation CO2the method of displacement displacement shale pneumatic state process
CN106066291B (en) * 2016-06-16 2018-11-09 中国华能集团公司 CO2 replaces shale gas and shale and tests System and method for the absorption analytic simulation of shale gas or CO2
CN106066291A (en) * 2016-06-16 2016-11-02 中国华能集团公司 CO2displacement shale gas and shale are to shale gas or CO2absorption analytic simulation test System and method for
CN108663498A (en) * 2017-03-27 2018-10-16 中国石油化工股份有限公司 The shale gas site desorption experimental provision and method of high temperature decompression and pressure break
CN107462472A (en) * 2017-07-26 2017-12-12 太原理工大学 A kind of experimental simulation device and analogy method of the compound fracturing coal body of temperature and pressure pulse
CN107478559A (en) * 2017-07-26 2017-12-15 太原理工大学 A kind of device and method simulated gas and migrated in different-grain diameter size coal sample
CN107462472B (en) * 2017-07-26 2019-12-31 太原理工大学 Experimental simulation device and simulation method for temperature-pressure pulse composite fracturing coal body
CN107478559B (en) * 2017-07-26 2020-11-24 太原理工大学 Device and method for simulating migration of gas in coal samples with different particle sizes
CN107976351A (en) * 2017-11-27 2018-05-01 大连理工大学 A kind of ocean gas hydrate core remodeling device and method

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