CN106770413A - A kind of method for measuring coal adsorbed methane or the equal number of molecule layers of level - Google Patents
A kind of method for measuring coal adsorbed methane or the equal number of molecule layers of level Download PDFInfo
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Abstract
The invention discloses a kind of method for measuring coal adsorbed methane or the equal number of molecule layers of level, methods described measures the nuclear magnetic resonance T2 (T of the coal sample of saturation methane or water with low-field nuclear magnetic resonance2) spectrum, the resultant signal amount of adsorption peak is obtained, under equal measuring condition, measure the pure methane of certain mass or the nuclear magnetic resonance T of pure water2Spectrum, obtain the resultant signal amount of unit mass methane or water, then the average adsorption number of plies of methane molecule or hydrone on coal surface is finally drawn, then by changing pressure and temperature condition, realize the quantitatively characterizing of the coal surface adsorbed molecules number of plies under different pressures and temperature conditionss by conversion.
Description
Technical field
The present invention relates to a kind of method for measuring coal adsorbed methane or the equal number of molecule layers of level, belong to the binding molecule layer of coal
Number field of measuring technique.
Background technology
Mainly with ADSORPTION STATE preservation in coal body surface, the water in reservoir has material impact to coal bed gas to coal bed gas product.
The absorption number of plies of the methane molecule on coal surface is the important evidence for calculating coal bed gas adsorbance, and conventional Adsorption Model is base at present
In the Langmuir models of mono layer adsorption, actual conditions, methane coal surface the multi-molecular absorption that is adsorbed as, methane and
Water coal surface the absorption number of plies can indirect reaction coal to methane and the adsorption capacity of water.During cbm development, contribute to
How by the water discharge in coal seam, the absorption number of plies of methane molecule and hydrone on coal surface is constantly in hypothesis state for research,
It is basic without can method for quantitative measuring, for this reason, it may be necessary to study a kind of method of measurable methane and water in the coal adsorption number of plies.
The content of the invention
It is existing problem more than solving, the invention discloses a kind of side for measuring coal adsorbed methane or the equal number of molecule layers of level
Method.
A kind of method for measuring coal adsorbed methane or the equal number of molecule layers of level, it is characterised in that utilize low-field nuclear magnetic resonance
Nuclear magnetic resonance T2 (the T of the coal sample of measurement saturation methane or water2) spectrum, the resultant signal amount of adsorption peak is obtained, same
Etc. under measuring condition, the pure methane of certain mass or the nuclear magnetic resonance T of pure water are measured2Spectrum, acquisition unit mass methane or water
Resultant signal amount, then finally draws the average adsorption number of plies of methane molecule or hydrone on coal surface by conversion.
The method of a kind of measurement coal adsorbed methane of the present invention or the equal number of molecule layers of level is comprised the following steps：
1) saturated sample and measurement：In pressure P (units：MPa under), coal sample is vacuumized into saturation methane or water 12 hours,
The T of methane or water in measurement coal sample2Spectrum, then vacuum saturation methane or water 4 hours again, measure the T of coal sample2Spectrum, until adjacent two
The T of methane or water in the coal sample of secondary measurement2Spectrum signal no longer changes, and illustrates that coal sample is fully saturated, by the T after saturation2Inhaled in spectrum
The signal of attached state methane or water is integrated resultant signal amount W (dimensionless) for drawing ADSORPTION STATE methane or water；
2) standard specimen measurement：It is m to take pure methane or pure water quality0(unit：G), the condition and parameter for being measured using sample, are surveyed
The T of amount pure methane or pure water2Spectrum, by T2In spectrum the signal of pure methane or pure water be integrated mass be m0Pure methane or
The resultant signal amount W of pure water0(dimensionless)；
3) adsorbed methane or water quality are calculated：If the quality of adsorbed methane or water is m (units：G), according to the sample of measurement
The resultant signal amount and unit mass pure methane or the resultant signal amount of pure water of middle adsorbed methane or water, absorption is tried to achieve by formula (1)
The quality m of methane or water：
4) sample adsorption methane or moisture subnumber are calculated：Sample adsorption molecular number N (units are tried to achieve according to formula (2)：It is individual)：
M is the molal weight of methane or water in formula, and unit is g/mol；NAIt is Avogadro's number, take 6.02 ×
1023mol-1；
5) specific surface area measurement：Surveyed by specific surface area measuring method (pressure mercury, liquid nitrogen are adsorbed, liquid carbon dioxide is adsorbed)
The specific surface area for trying out the interconnected pore of below sample 100nm is S (units：m2/g)；
6) methane molecule or the Water Molecular Adsorption number of plies are calculated：Methane molecule or hydrone are tried to achieve in coal table according to formula (3)
The absorption number of plies L (units in face：Layer)：
R is the radius of a methane molecule or hydrone in formula, and unit is m；π is pi, takes 3.14；
7) by changing different pressure and temperatures, repeat step 1)~6), it can be deduced that different pressures are with a temperature of
The average adsorption number of plies.
The invention provides a kind of method for measuring coal adsorbed methane or the equal number of molecule layers of level, methods described utilizes low field
Nuclear magnetic resonance technique and specific surface area measuring technology (pressure mercury, low temperature liquid nitrogen absorption and low-temperature carbon dioxide absorption) are combined, profit
With methane in coal sample or the nuclear magnetic resonance T of water2First total amount of spectral peak (adsorption peak) signal in left side in spectrum, according to same survey
Under the conditions of examination, the pure methane or pure water nuclear magnetic resonance T of unit mass2Signal total amount in spectrum, calculate absorption methane molecule or
The gross mass of hydrone, then by calculating the surface area shared by total binding molecule number and total binding molecule, finally
According to the sample specific surface area data of test, the absorption number of plies of methane molecule or hydrone on coal surface can be drawn.
Principle of the invention is：
It is of the invention mainly to pass through nuclear magnetic resonance T2 T2Compose to measure the methane of absorption in coal column or containing for water
Amount, is then contrasted with the pure methane of unit mass or the semaphore of pure water, is mean molecule by certain formula scales
Count layer by layer.What nuclear magnetic resonance technique was detected is the hydrogen nuclei in methane in the present invention, in its signal amplitude and investigative range
The quality of methane or water is directly proportional.The methane or water of ADSORPTION STATE have different nuclear-magnetisms from the methane or water of other states in coal sample
Resonance characteristics；In T2In spectrum, T2Time is shorter, and corresponding hole is smaller.In theory, the nuclear magnetic resonance of methane laterally relaxes in coal column
Henan time T2Substantially there are three spectral peaks in spectrum, and the methane in ADSORPTION STATE methane or water, limited porous dehiscence gap is from left to right represented respectively
Or water and free state methane or water.In practice, due to experiment coal column small volume, coal column porous dehiscence gap agensis, institute again in itself
May not observed with free state methane or water.
Thus the present invention has advantages below：
Compared with prior art, the average adsorption number of plies of methane or water on coal surface can quickly be determined using the present invention.
Brief description of the drawings
Fig. 1 is saturation water coal sample nuclear magnetic resonance T2Spectrogram.
Specific embodiment
The method of the present invention is mainly the content by ADSORPTION STATE methane or water in low-field nuclear magnetic resonance commercial measurement coal, so
Contrasted with the pure methane of unit mass or the semaphore of pure water afterwards, by the mean molecule that certain formula scales are absorption
Count layer by layer.Because measurement and computational methods are completely the same, so only by taking water as an example.In Fig. 1, peak P1(0.43~4.04ms) is suction
The signal of attached state water, P2It is the signal of hole bound state water.As can be seen here, low-field nuclear magnetic resonance T2Spectrum can be very good to distinguish
The signal of different conditions water.
The invention will be further described with reference to the accompanying drawings and detailed description.
The method of the present invention needs first to measure the T of saturation coal sample reclaimed water2Spectrum, integration obtains total letter of ADSORPTION STATE methane or water
Number amount, then contrasted with the pure methane of unit mass or the semaphore of pure water, by certain formula scales be average mark
The sublayer number of plies.Comprise the following steps that：
1) saturated sample and measurement：In pressure P (units：MPa under), coal sample is vacuumized into saturation methane or water 12 hours,
The T of methane or water in measurement coal sample2Spectrum, then vacuum saturation methane or water 4 hours again, measure the T of coal sample2Spectrum, until adjacent two
The T of methane or water in the coal sample of secondary measurement2Spectrum signal no longer changes, and illustrates that coal sample is fully saturated, by the T after saturation2Inhaled in spectrum
The signal of attached state methane or water is integrated resultant signal amount W (dimensionless) for drawing ADSORPTION STATE methane or water；
2) standard specimen measurement：It is m to take pure methane or pure water quality0(unit：G), the condition and parameter for being measured using sample, are surveyed
The T of amount pure methane or pure water2Spectrum, by T2In spectrum the signal of pure methane or pure water be integrated mass be m0Pure methane or
The resultant signal amount W of pure water0(dimensionless)；
3) adsorbed methane or water quality are calculated：If the quality of adsorbed methane or water is m (units：G), according to the sample of measurement
The resultant signal amount and unit mass pure methane or the resultant signal amount of pure water of middle ADSORPTION STATE methane or water, suction is tried to achieve by formula (1)
The quality m of attached methane or water：
4) sample adsorption methane molecule or moisture subnumber are calculated：Sample adsorption molecular number N (units are tried to achieve according to formula (2)：
It is individual)：
M is the molal weight of methane or water in formula, and unit is g/mol；NAIt is Avogadro's number, take 6.02 ×
1023mol-1；
5) specific surface area measurement：Surveyed by specific surface area measuring method (pressure mercury, liquid nitrogen are adsorbed, liquid carbon dioxide is adsorbed)
The specific surface area for trying out the interconnected pore of below sample 100nm is S (units：m2/g)；
6) methane molecule or the Water Molecular Adsorption number of plies are calculated：Methane molecule or hydrone are tried to achieve in coal table according to formula (3)
The absorption number of plies L (units in face：Layer)：
R is the radius of a methane molecule or hydrone in formula, and unit is m；π is pi, takes 3.14；
7) by changing different pressure and temperatures, repeat step 1)~6), it can be deduced that different pressures are with a temperature of
The average adsorption number of plies.
Embodiment：
Under 25 DEG C of normal temperature and normal pressure 0.1MPa states, by taking water as an example, the method for measuring the equal number of molecule layers of coal adsorption levels, profit
Nuclear magnetic resonance T2 (the T of the coal sample of saturation water is measured with low-field nuclear magnetic resonance2) spectrum, obtain the resultant signal of adsorption peak
Amount, under equal measuring condition, measures the nuclear magnetic resonance T of the pure water of certain mass2Spectrum, obtains the resultant signal of unit mass water
Amount, then finally draws the average adsorption number of plies of the hydrone on coal surface by conversion.
A kind of method for measuring the equal number of molecule layers of coal adsorption levels of the present invention is comprised the following steps：
1) saturated sample and measurement：In pressure P (units：MPa under), sample is vacuumized into saturation water 12 hours, measures coal
The T of sample reclaimed water2Spectrum, then vacuum saturation 4 hours again, measure the T of coal sample reclaimed water2Spectrum, until the adjacent coal sample reclaimed water for measuring twice
T2Spectrum signal no longer changes, and illustrates that coal sample is fully saturated, by the T after saturation2The signal of ADSORPTION STATE water is integrated in spectrum
Go out the resultant signal amount W=11059.9155 of ADSORPTION STATE water；
2) standard specimen measurement：Pure water quality is taken for m0=10g, the condition and parameter measured using sample measures the T of pure water2
Spectrum, by T2In spectrum the signal of pure water be integrated mass be m0Pure water resultant signal amount W0=159146.12；
3) absorption water quality is calculated：If the quality for adsorbing water is m (units：G), ADSORPTION STATE water in the sample according to measurement
The resultant signal amount of resultant signal amount and unit mass pure water, the quality m=0.695g of absorption water is tried to achieve by formula (1)：
4) sample adsorption moisture subnumber is calculated：Sample adsorption molecular number N=2.32439 × 10 are tried to achieve according to formula (2)22It is individual
M is the molal weight of water in formula, and unit is g/mol, M=18g/mol；NAIt is Avogadro's number, takes 6.02
×1023mol-1；
5) specific surface area measurement：Surveyed by specific surface area measuring method (pressure mercury, liquid nitrogen are adsorbed, liquid carbon dioxide is adsorbed)
The specific surface area for trying out the interconnected pore of below sample 100nm is S=350.97m2/g；
6) the Water Molecular Adsorption number of plies is calculated：Absorption number of plies L=8.32 of the hydrone on coal surface is tried to achieve according to formula (3)
Layer：
R is a radius for hydrone in formula, and unit is m, r=2 × 10-10m；π is pi, takes 3.14；
7) by changing different pressure and temperatures, repeat step 1)~6), it can be deduced that different pressures are with a temperature of
The average adsorption number of plies.
When measuring and calculating the coal adsorbed methane mean molecule number of plies, measurement and computational methods are completely the same, so
Only the parameters of water need to be changed to the parameter of methane with methane as measurement object, you can draw the number of molecule layers of methane.
General principle of the invention and principal character and advantages of the present invention, the technology of the industry has been shown and described above
Personnel it should be appreciated that the present invention is not limited to the above embodiments, simply explanation described in above-described embodiment and specification this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes
Change and improvement all fall within the protetion scope of the claimed invention, invention is claimed, and scope is by appending claims and its waits
Effect thing is defined.
Claims (2)
1. a kind of method for measuring coal adsorbed methane or the equal number of molecule layers of level, it is characterised in that surveyed using low-field nuclear magnetic resonance
Nuclear magnetic resonance T2 (the T of the coal sample of amount saturation methane or water2) spectrum, the resultant signal amount of adsorption peak is obtained, equal
Under measuring condition, the pure methane of certain mass or the nuclear magnetic resonance T of pure water are measured2Spectrum, obtains the total of unit mass methane or water
Semaphore, then finally draws the average adsorption number of plies of methane molecule or hydrone on coal surface by conversion.
2. a kind of method for measuring coal adsorbed methane or the equal number of molecule layers of level according to claim 1, it is characterised in that
Comprise the following steps：
1) saturated sample and measurement：In pressure P (units：MPa under), coal sample is vacuumized into saturation methane or water 12 hours, measurement
The T of methane or water in coal sample2Spectrum, then vacuum saturation methane or water 4 hours again, measure the T of coal sample2Spectrum, surveys twice until adjacent
The T of methane or water in the coal sample of amount2Spectrum signal no longer changes, and illustrates that coal sample is fully saturated, by the T after saturation2ADSORPTION STATE in spectrum
The signal of methane or water is integrated resultant signal amount W (dimensionless) for drawing ADSORPTION STATE methane or water；
2) standard specimen measurement：It is m to take pure methane or pure water quality0(unit：G), the condition and parameter for being measured using sample, are measured pure
The T of methane or pure water2Spectrum, by T2In spectrum the signal of pure methane or pure water be integrated mass be m0Pure methane or pure water
Resultant signal amount W0(dimensionless)；
3) adsorbed methane or water quality are calculated：If the quality of adsorbed methane or water is m (units：G), inhaled in the sample according to measurement
The resultant signal amount and unit mass pure methane or the resultant signal amount of pure water of attached state methane or water, absorption first is tried to achieve by formula (1)
The quality m of alkane or water：
4) sample adsorption methane molecule or moisture subnumber are calculated：Sample adsorption molecular number N (units are tried to achieve according to formula (2)：It is individual)：
M is the molal weight of methane or water in formula, and unit is g/mol；NAIt is Avogadro's number, takes 6.02 × 1023mol-1；
5) specific surface area measurement：Tested out by specific surface area measuring method (pressure mercury, liquid nitrogen are adsorbed, liquid carbon dioxide is adsorbed)
The specific surface area of the interconnected pore of below sample 100nm is S (units：m2/g)；
6) methane molecule or the Water Molecular Adsorption number of plies are calculated：Methane molecule or hydrone are tried to achieve on coal surface according to formula (3)
Absorption number of plies L (units：Layer)：
R is the radius of a methane molecule or hydrone in formula, and unit is m；π is pi, takes 3.14；
7) by changing different pressure and temperatures, repeat step 1)~6), it can be deduced that different pressures are average with a temperature of
The absorption number of plies.
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Cited By (1)
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| CN109696451A (en) * | 2019-03-03 | 2019-04-30 | 中国科学院山西煤炭化学研究所 | A kind of NMR measuring method of PAMAM to guest molecules adsorbance |
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| CN109696451B (en) * | 2019-03-03 | 2020-08-28 | 中国科学院山西煤炭化学研究所 | NMR determination method of PAMAM (polyamidoamine) on guest small molecule adsorption quantity |
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