CN110426311A - Shale is measured to CO2And CH4The method of mixed gas sorption ability - Google Patents
Shale is measured to CO2And CH4The method of mixed gas sorption ability Download PDFInfo
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- CN110426311A CN110426311A CN201910692583.1A CN201910692583A CN110426311A CN 110426311 A CN110426311 A CN 110426311A CN 201910692583 A CN201910692583 A CN 201910692583A CN 110426311 A CN110426311 A CN 110426311A
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- shale
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N24/00—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
- G01N24/08—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
- G01N24/081—Making measurements of geologic samples, e.g. measurements of moisture, pH, porosity, permeability, tortuosity or viscosity
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N7/02—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder
- G01N7/04—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder by absorption or adsorption alone
Abstract
Shale is measured to CO2And CH4The method of mixed gas sorption ability, includes the following steps: A) check device air-tightness；B) cavity free space volumes are tested；C) it is based on Nuclear Magnetic Resonance Measurement CO2And CH4In mixed gas, shale is to CH4Adsorption capacity；D) based on volumetric method and Nuclear Magnetic Resonance Measurement as a result, in CO2And CH4In mixed-gas environment, the accurate shale that calculates is to CO2Adsorption capacity；The invention has the benefit that the present invention is with nuclear magnetic resonance to CH in shale4Based on the research of adsorption capacity, by building experiment porch, in conjunction with volumetric method, while the advantages of play nuclear magnetic resonance and volumetric method, innovatively realize to CO in shale2And CH4While mixed gas each component adsorption capacity, direct quantitative characterization.
Description
Technical field
The present invention relates to one kind for shale to CO2And CH4The side of mixed gas each component adsorption capacity simultaneous quantitative measurement
Method belongs to shale to gas sorption ability field of measuring technique.
Background technique
Use CO2Strengthen the hot issue that shale gas exploitation is current Unconventional gas research.The mechanism of action of this method
It is CO2It is adsorbed to replace CH by shale4Adsorption site so that ADSORPTION STATE CH4It is desorbed from shale particle surface, to improve
Shale gas recovery ratio.That is, CO2Strengthen shale gas exploitation, is substantially CO2And CH4Competitive Adsorption result in shale.
So quantitative determination shale is to CO2And CH4Mixed gas each component adsorption capacity, for CO2Strengthen the research of shale gas exploitation
It is particularly significant.Then, routine experiment method (such as volumetric method, gravitational method) is only capable of individually measuring shale to CO2Or CH4Absorption
Ability, can not quantitative judge shale to CO2And CH4The adsorption capacity of each component in mixed gas.In consideration of it, needing to develop one kind
Can Accurate Determining shale to CO2And CH4The experimental method of mixed gas each component adsorption capacity.
Summary of the invention
To achieve the goals above, the present invention provides one kind for shale to CO2And CH4Mixed gas each component adsorption energy
The method of power simultaneous quantitative measurement.
Particular content of the invention are as follows: measurement shale is to CO2And CH4The method of mixed gas sorption ability, including walk as follows
It is rapid:
A) check device air-tightness；
B) cavity free space volumes are tested；
C) it is based on Nuclear Magnetic Resonance Measurement CO2And CH4In mixed gas, shale is to CH4Adsorption capacity；
D) based on volumetric method and Nuclear Magnetic Resonance Measurement as a result, in CO2And CH4It is accurate to calculate shale pair in mixed-gas environment
CO2Adsorption capacity.
Further, the slate flour sample after drying is packed into sample cavity, using vacuum pump to reference cavity and sample
Chamber carries out vacuumize process；
To helium is injected in reference cavity, pressure P is recordedaiMPa；
After reference cavity is connected to sample cavity, after pressure balance, P is recordedaiiMpa；
After repeating repeatedly, it is averaged,
Cavity free space is
ZaiAnd ZaiiRespectively PaiAnd PaiiWhen compressibility factor, VrcIt is the volume of reference cavity；
Record different PaiCorresponding Paii；
According to the different P of inquiryaiCorresponding Zai, according to the different P of inquiryaiiCorresponding Zaii；Calculate Vfree。
Further, the step C) in, it is specific to use:
It is packed into the slate flour sample after drying in sample cavity, vacuumize process, place are carried out to reference cavity and sample cavity
Reason is using booster pump to injecting CH in reference cavity4, CO is then injected into reference cavity again2, recording manometer is shown as 10MPa；
By CO2And CH4Mixed gas enters in sample cavity, after reference cavity and sample cavity pressure balance, according to nuclear magnetic resonance
Test result records ADSORPTION STATE methane nuclear magnetic resonance amplitude；
It is calculated using following formula:
Based on nuclear magnetic resonance amplitude and shale to CH4The linear relationship V of adsorption capacityad=0.4207 × T2A；
Wherein VadIt is shale to CH4 adsorbance；
T2AFor the corresponding nuclear magnetic resonance amplitude of ADSORPTION STATE methane；
Based on molar volume of gas, above formula can be converted into nad=1.878 × 10-5×T2A, wherein nadIt is shale to CH4It inhales
Attached amount.
Further, according to formula:
Wherein, nCO2It is shale to be calculated to CO2Adsorbance, R are ideal gas constant 8.31441J/ (molK), T
For temperature, ZbiAnd ZbiiRespectively pressure PbiAnd PbiiWhen Gas Compression Factor；
It is calculated according to inquiry.
The invention has the benefit that the present invention is with nuclear magnetic resonance to CH in shale4Based on the research of adsorption capacity, lead to
It crosses and builds experiment porch, in conjunction with volumetric method, while the advantages of play nuclear magnetic resonance and volumetric method, innovatively realize to shale
Middle CO2And CH4While mixed gas each component adsorption capacity, direct quantitative characterization.
Detailed description of the invention
Fig. 1 is equipment schematic applied by measuring method provided by the present invention.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is explained in further detail.It should be appreciated that specific embodiment described herein is used only for explaining the present invention, and
It is not used in the restriction present invention.
On the contrary, the present invention covers any substitution done on the essence and scope of the present invention being defined by the claims, repairs
Change, equivalent method and scheme.Further, in order to make the public have a better understanding the present invention, below to of the invention thin
It is detailed to describe some specific detail sections in section description.Part without these details for a person skilled in the art
The present invention can also be understood completely in description.
As shown in Figure 1, being the shale provided by the present invention that is directed to CO2And CH4Mixed gas each component adsorption capacity is simultaneously
Equipment applied by the method for quantitative measurment, the equipment include CH4Gas cylinder 1, CO2Gas cylinder 2, helium (He) gas cylinder 3, booster pump
4, heated at constant temperature chamber 5, nuclear-magnetism coil 6, vacuum pump 7, waste gas recovery pond 8, reference cavity 9, sample cavity 10, temperature sensors of high precision
11 and check valve 12, multiple air valve switch (A1-A11), high-precision pressure gauge (P1, P2)；
The wherein CH4Gas cylinder 1, CO2Gas cylinder 2, helium (He) gas cylinder 3, booster pump 4 pass through corresponding air valve switch respectively
It is connected on the reference cavity 9, and the reference cavity 9 is placed in the heated at constant temperature chamber 5, the reference cavity 9 is again by high-precision
Degree temperature sensor 11 connects on the sample cavity 10, and is provided at the top of the reference cavity 9 and the sample cavity 10
Corresponding high-precision pressure gauge, the sample cavity 10 are arranged in the nuclear-magnetism coil 6；The sample cavity 10 passes through pipe again simultaneously
Road connects the waste gas recovery pond 8, connects the vacuum pump 7 between the sample cavity 10 and the waste gas recovery pond 8, and
Corresponding air valve switch is provided at corresponding node on pipeline；
The specific steps of measurement method of the present invention are as follows:
1) check device air-tightness
This is tested all testing process and completes in 30 DEG C of conditions, and 5 temperature of heating chamber is regulated to 30 DEG C.
First close all air valve switch.Sample is not filled in sample cavity, then opens valve A3, A4, A5, A6, A7, A8, A9,
The helium for being higher than experiment maximum pressure 1.5MPa is injected into reference cavity 9, sample cavity 10 by booster pump 4, is then shut off valve
A3, A4, A5, A6,10 minutes after pressure stabilisation, and observation pressure gauge P1, pressure gauge P2 do not change then two chambers within 8 hours
Air-tightness reaches requirement.
2) cavity free space volumes are tested
It is packed into the slate flour sample (80 mesh, 31.58 grams) after drying into sample cavity 9, closes all air valve switch.It beats
Valve opening door A7, A8, A9, A10, A11 and check valve 12 carry out vacuumizing place using vacuum pump 7 to reference cavity 9, sample cavity 10
Reason, after close all gas valve.
Then valve A3, A4, A5, A6, A8 are opened, injects helium into reference cavity 9, until pressure gauge P1 is shown as
PaiMPa, it is rear to close valve A3, A4, A5, A6, and Open valve A7, A9, after pressure balance in reference cavity 9 and sample cavity 10
(i.e. pressure gauge P1 and P2 show value is identical and no longer changes), record balance pressure is PaiiMpa。
Repeat three groups of experiments, PaiRespectively 2,4 and 6MPa.This test sample free space includes the body of reference cavity 9
Between product, reference cavity 9 and sample cavity 10 in the volume of connectivity trachea and sample cavity between shale particle and inside shale particle
The volume in free gas preservation space.Then, the average value tested three times, cavity free space (V are takenfree, cm3) beWherein, ZaiAnd ZaiiRespectively PaiAnd PaiiWhen compressibility factor, VrcIt is the volume of reference cavity 9
(62.78cm3).In this test, work as PaiFor 2,4 and 6Mpa, PaiiRespectively 1.243,2.478 and 3.708MPa.
PaiWhen equal to 2,4,6MPa, Z is inquiredaiRespectively 1.00972,1.02058,1.03248；PaiiEqual to 1.243,
When 2.478,3.708MPa, Z is inquiredaiiRespectively 1.0059,1.01221,1.01893.To sum up, V under this condition is measuredfreeFor
100.46cm3。
3) it is based on Nuclear Magnetic Resonance Measurement CO2And CH4In mixed gas, shale is to CH4Adsorption capacity
Based on nuclear magnetic resonance basic principle, using lateral relaxation time, forefathers establish nuclear magnetic resonance amplitude and shale pair
CH4The linear relationship of adsorption capacity, Vad=0.4207 × T2A, wherein VadIt is shale to CH4Adsorbance (cm3), T2AFor ADSORPTION STATE
The corresponding nuclear magnetic resonance amplitude of methane.Based on molar volume of gas (22.4mol/L), above formula can be converted into nad=1.878 × 10-5×T2A(formula 1), wherein nadIt is shale to CH4Adsorbance (unit: mol).
Open valve A7, A8, A9, A10, A11 and check valve 12, using vacuum pump 7 to reference cavity 9, sample cavity 10 into
Row vacuumize process, after close all gas valve.Valve A1, A4, A5, A6, A8 are opened, using booster pump 4 to reference
The CH of 5MPa (being labeled as Pb) pressure is injected in chamber 94, it is then shut off valve A1, A2 is opened, is continued using vacuum pump 4 to reference
CO is injected in chamber 92, until pressure gauge P1 is shown as 10MPa (labeled as Pbi)。
Valve A1, A4, A5, A6 are closed, A7, A9 is opened, makes CO2And CH4Mixed gas enters in sample cavity 10.Wait refer to
(i.e. pressure gauge P1 and P2 show value is identical and no longer changes), record balance pressure are after pressure balance in chamber 9 and sample cavity 10
6.858MPa (is labeled as Pbii).
According to nuclear magnetic resonance test result, ADSORPTION STATE methane nuclear magnetic resonance amplitude is 47.44a.u., then is obtained by formula 1
Shale CH4Adsorbance be 0.000891mol (be labeled as nCH4), by unit conversion can obtain under this condition shale to CH4Absorption
Ability is 0.63cm3/g。
4) based on volumetric method and Nuclear Magnetic Resonance Measurement as a result, in CO2And CH4In mixed gas hybird environment, page is accurately calculated
Rock is to CO2Adsorption capacity
On the basis of 3) step, shale is established to CO2Calculation formula.Integral Thought are as follows: CO2Adsorbance=CO2And CH4
Gas gross-ADSORPTION STATE CH in gas gross-cavity free space4Amount.The formula isWherein, nCO2It is shale to be calculated to CO2Adsorbance (unit: mol),
R is ideal gas constant (8.31441J/ (molK)), and T is temperature (30 DEG C, i.e. 303.15K), ZbiAnd ZbiiRespectively pressure
PbiAnd PbiiWhen Gas Compression Factor.Inquiry can obtain, PbiWhen equal to 10MPa, Zbi 0.72841；Pbii is equal to 6.858MPa
When, Zbii 0.8107.
Shale is calculated to CO2Adsorbance is 0.001109mol, by unit conversion can obtain under this condition shale to CO2
Adsorption capacity is 2.70cm3/g。
5) according to above-mentioned experimental method process, under the conditions of can measuring different pressures, various concentration ratio, shale is to CO2With
CH4The adsorption capacity of mixed gas each component.
Claims (4)
1. measuring shale to CO2And CH4The method of mixed gas sorption ability, which comprises the steps of:
A) check device air-tightness；
B) cavity free space volumes are tested；
C) it is based on Nuclear Magnetic Resonance Measurement CO2And CH4In mixed gas, shale is to CH4Adsorption capacity；
D) based on volumetric method and Nuclear Magnetic Resonance Measurement as a result, in CO2And CH4In mixed-gas environment, the accurate shale that calculates is to CO2
Adsorption capacity.
2. measurement shale according to claim 1 is to CO2And CH4The method of mixed gas sorption ability, which is characterized in that
It is packed into the slate flour sample after drying in sample cavity, vacuumize process is carried out to reference cavity and sample cavity using vacuum pump；
To helium is injected in reference cavity, pressure P is recordedaiMPa；
After reference cavity is connected to sample cavity, after pressure balance, P is recordedaiiMpa；
After repeating repeatedly, it is averaged,
Cavity free space is
ZaiAnd ZaiiRespectively PaiAnd PaiiWhen compressibility factor, VrcIt is the volume of reference cavity；
Record different PaiCorresponding Paii；
According to the different P of inquiryaiCorresponding Zai, according to the different P of inquiryaiiCorresponding Zaii；Calculate Vfree。
3. measurement shale according to claim 2 is to CO2And CH4The method of mixed gas sorption ability, which is characterized in that
The step C) in, it is specific to use:
It is packed into the slate flour sample after drying in sample cavity, vacuumize process, processing benefit are carried out to reference cavity and sample cavity
With booster pump to injecting CH in reference cavity4, CO is then injected into reference cavity again2, recording manometer is shown as 10MPa；
By CO2And CH4Mixed gas enters in sample cavity, after reference cavity and sample cavity pressure balance, is tested according to nuclear magnetic resonance
As a result, record ADSORPTION STATE methane nuclear magnetic resonance amplitude；
It is calculated using following formula:
Based on nuclear magnetic resonance amplitude and shale to CH4The linear relationship V of adsorption capacityad=0.4207 × T2A；
Wherein VadIt is shale to CH4 adsorbance；
T2AFor the corresponding nuclear magnetic resonance amplitude of ADSORPTION STATE methane；
Based on molar volume of gas, above formula can be converted into nad=1.878 × 10-5×T2A, wherein nadIt is shale to CH4Adsorbance.
4. measurement shale according to claim 3 is to CO2And CH4The method of mixed gas sorption ability, which is characterized in that
According to formula:
Wherein, nCO2It is shale to be calculated to CO2Adsorbance, R are ideal gas constant 8.31441J/ (molK), and T is temperature
Degree, ZbiAnd ZbiiRespectively pressure PbiAnd PbiiWhen Gas Compression Factor；
It is calculated according to inquiry.
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| CN115931949A (en) * | 2022-10-11 | 2023-04-07 | 中国矿业大学 | Method for improving coal bed gas recovery ratio by quantitatively evaluating gas injection |
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