CN113008927A - Conversion method of nuclear magnetic resonance T2 spectrum and pore distribution of coal seam - Google Patents
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Abstract
The invention relates to a method for converting a nuclear magnetic resonance T2 spectrum and pore distribution of a coal seam, which is characterized by comprising the following steps: a, performing nuclear magnetic resonance measurement on a saturated water coal crushed sample to obtain a nuclear magnetic resonance T2 spectrum; b, carrying out low-temperature nitrogen adsorption experiment measurement on the saturated water coal crushed sample to obtain a pore distribution curve; c, comparing the nuclear magnetic resonance T2 spectrum with a pore distribution curve, picking up the transverse relaxation time T2 and the pore diameter R value of the corresponding extreme point, and obtaining a conversion relation of the transverse relaxation time T2 and the pore diameter R value; d, converting the nuclear magnetic resonance porosity component in the nuclear magnetic resonance T2 spectrum into the pore volume of the sample with unit mass; e, converting the nuclear magnetic resonance T2 spectrum into a pore distribution curve by using a conversion relation of the transverse relaxation time T2 and the pore diameter R value and a conversion relation of nuclear magnetic resonance porosity components and the pore volume of a unit mass sample. The method of the invention only needs to be carried out under the condition of normal temperature, and the analysis cost is lower.
Description
Technical Field
The invention relates to a conversion method of a nuclear magnetic resonance T2 spectrum and pore distribution of a coal seam, belonging to the technical field of energy exploitation.
Background
The coal bed pore distribution and the size thereof have important significance for evaluating the development potential of the coal bed gas. The pore size of coal seams can be generally classified into 3 grades: macropores (pore radius larger than 30 nm), mesopores (pore radius 1.2-30 nm) and micropores (pore radius 0.4-1.2 nm). The content of methane gas present in the coal bed is related to both pore volume and pore distribution. The small pores contribute most to the specific surface area of the coal, and more than 90 percent of methane gas exists in the small pores; methane gas exists as free gas or dissolves in water in large pores (cleats) or mesopores. Although coal bed macropores and mesopores contribute little to methane gas storage space, permeability and diffusivity are determined. Successful coal bed gas mining requires a balanced distribution of macropores, mesopores and micropores. At present, the pore distribution of a coal sample can be measured by several different methods such as a mercury intrusion method, a nitrogen adsorption method, a nuclear magnetic resonance method and the like, and each method has respective advantages and limitations.
Mercury intrusion methods, also known as mercury porosimetry, rely on the application of pressure to force mercury into the pores against surface tension to determine pore size and distribution. The increased applied pressure allows mercury to enter the smaller pores, corresponding to smaller pore radii. According to the principle that the surface tension of mercury in pores is balanced with the applied pressure, a calculation method of the pore diameter can be obtained, and the pore volume of the corresponding pore radius can be known by measuring the amount of mercury entering the pores under different pressures. Currently, mercury intrusion gauges are used that use pressures up to about 200MPa and can measure pore diameters in the range of about 0.0064 to 950 microns. Since mercury is highly volatile and toxic, it is likely to cause environmental pollution.
The nitrogen adsorption method is also called as low temperature liquid nitrogen adsorption method, and the method adopts the principle of volume equivalent substitution, namely, the liquid nitrogen filled in the holes is equivalent to the volume of the holes. From the capillary condensation phenomenon, it is known that pore diameters within which the capillary condensation phenomenon can occur are different at different relative pressures. When the relative pressure value is increased, the pore radius capable of generating the condensation phenomenon is increased, a critical pore radius value exists corresponding to a certain relative pressure value, all pores with pore radii smaller than the corresponding relative pressure critical value are subjected to capillary condensation, and liquid nitrogen is filled in the pores; the pores with the pore radius larger than the corresponding critical value of the relative pressure can not generate capillary condensation, liquid nitrogen can not be filled in the pores, and the critical pore radius value can be calculated by the Kelvin equation. Due to the limitation of the relative pressure measurement precision, the method can measure the diameter of the pore in the range of about 0.35-500 nanometers.
The nuclear magnetic resonance method is also called a low-magnetic-field nuclear magnetic resonance method, and parameters such as the volume of fluid in a pore space are obtained by measuring the nuclear magnetic resonance characteristics of the hydrogen nuclei of the fluid contained in the rock sample in a low-frequency magnetic field. Generally, when the fluid is confined in the rock pores, the nuclear magnetic resonance relaxation time of the hydrogen nuclei is greatly shortened due to the interaction between the fluid and the pores. The nuclear magnetic resonance relaxation time in rock is determined by the size of the pores, the larger the pores the longer the relaxation time. By using a mathematical inversion method, the portion of the fluid in pores with different sizes, namely a transverse relaxation time spectrum (T2 spectrum) can be calculated. The integral area of the transverse relaxation time spectrum is in direct proportion to the volume of the fluid contained in the rock, and the pore volume occupied by the fluid containing hydrogen atomic nuclei can be obtained only by properly scaling the transverse relaxation time spectrum. The nuclear magnetic resonance method can be used for rapidly and nondestructively measuring the pore size distribution of the rock sample, the measurement range is wider than 0.002-1000 microns, but the nuclear magnetic resonance method can be used for obtaining the pore distribution of the measured sample only by converting the transverse relaxation time T2 spectrum obtained by measurement.
Disclosure of Invention
Aiming at the outstanding problems, the invention provides a method for converting a coal bed nuclear magnetic resonance T2 spectrum and pore distribution, and the method can make up the defect that the pore distribution of a low-temperature nitrogen adsorption experiment lacks of nano-scale pores by converting the coal bed nuclear magnetic resonance T2 spectrum into the pore distribution.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for converting a nuclear magnetic resonance T2 spectrum and pore distribution of a coal seam comprises the following steps:
a, performing nuclear magnetic resonance measurement on a saturated water coal crushed sample to obtain a nuclear magnetic resonance T2 spectrum;
b, carrying out low-temperature nitrogen adsorption experiment measurement on the saturated water coal crushed sample in the step a to obtain a pore distribution curve;
c, comparing the nuclear magnetic resonance T2 spectrum in the step a with the pore distribution curve in the step b, picking up the transverse relaxation time T2 and the pore diameter R value of the corresponding extreme point, and obtaining a conversion relation of the transverse relaxation time T2 and the pore diameter R value;
d, converting the nuclear magnetic resonance porosity component in the nuclear magnetic resonance T2 spectrum obtained in the step a into the pore volume of the sample with unit mass by using a nuclear magnetic resonance porosity component and pore volume conversion relation of the sample with unit mass;
e converting the nuclear magnetic resonance T2 spectrum in the step a into a pore distribution curve by using the conversion relation of the transverse relaxation time T2 and the pore diameter R value in the step c and the conversion relation of the nuclear magnetic resonance porosity component and the pore volume of the sample per unit mass in the step d.
The conversion method, preferably, in the step c, the conversion relation between the transverse relaxation time T2 and the pore diameter R value is shown as formula (1):
R＝a×T2b (1)
in the formula: r is the pore diameter; t2 is the transverse relaxation time; a. b is a conversion coefficient.
In the conversion method, preferably, in the step d, the conversion relation between the nuclear magnetic resonance porosity component and the pore volume of the unit mass of the sample is as follows:
in the formula: PV is the pore volume per mass of the sample; POR is the nuclear magnetic resonance porosity component; rhobIs the bulk density of the sample.
In the switching method, preferably, in the step a, the echo interval time TE of the nmr experiment apparatus is set to be equal to or less than 0.2 ms, and the polarization waiting time TW is set to be greater than or equal to 6 seconds.
In the conversion method, preferably, in the step a, the preparation process of the saturated water coal crushed sample comprises the following steps:
a1 collecting a sample of the coal seam drilling debris to be measured;
a2, drying the coal bed drilling rock debris sample in the step a1 to constant weight, and cooling to room temperature to obtain a dried coal bed drilling rock debris sample;
a3, crushing the dried coal bed drilling rock debris sample obtained in the step a2 by using crushing equipment to obtain a coal fragment sample, and weighing the coal fragment sample;
a4, adding water according to the weight of the crushed coal sample in the step a3, completely immersing the crushed coal sample in the water, and filtering to obtain a saturated water crushed coal sample;
a5, placing the drying agent and the saturated water coal crushed sample in the step a4 in a closed container until the weight of the saturated water coal crushed sample is unchanged, and obtaining the saturated water coal crushed sample with surface moisture removed.
The conversion method preferably further comprises a step a6, wherein the coal fragment sample in the step a4 is firstly stirred or ultrasonically treated by a stirring device or an ultrasonic device so as to ensure that water completely enters the pores of the coal, and then the filtration is carried out.
The conversion method preferably, the weight of the coal bed drilling debris sample collected in the step a1 is not less than 100 g.
In the conversion method, preferably, the drying temperature of the coal bed drilling rock debris sample in the step a2 is 80-150 ℃, and the drying time is 3-6 hours.
In the conversion method, preferably, the crushing equipment in the step a3 is a vibrating screen, the mesh number of the vibrating screen is 80-100 meshes, and the diameter of the obtained coal crushed sample particles is 0.15-0.18 mm.
In the conversion method, preferably, in the step a5, the drying agent is a supersaturated potassium sulfate solution.
Due to the adoption of the technical scheme, the invention has the following advantages:
1. the invention provides a new method for realizing the interconversion between the nuclear magnetic resonance T2 spectrum of the coal bed and the pore distribution curve of the low-temperature nitrogen adsorption experiment based on extreme points; according to the method, the nuclear magnetic resonance T2 spectrum of the coal seam is converted into pore distribution, so that the defect that the pore distribution of a low-temperature nitrogen adsorption experiment lacks of nano-scale pores can be overcome.
2. The method adopts the nuclear magnetic resonance experiment to replace the low-temperature nitrogen adsorption experiment to measure the pore distribution of the coal bed, and only needs to be carried out under the normal temperature condition, so that the analysis cost is lower.
Drawings
FIG. 1 is a nuclear magnetic resonance T2 spectrum extreme point diagram of a coal seam sample according to an embodiment of the present invention;
FIG. 2 is a graph of an extreme point of pore distribution measured for a corresponding cryogenic nitrogen adsorption experiment using the coal seam sample of FIG. 1;
FIG. 3 is a graph of the transition of the transverse relaxation time T2 of nuclear magnetic resonance to the pore diameter R for the extreme points of FIGS. 1 and 2;
FIG. 4 is a comparison graph of the nuclear magnetic resonance T2 spectrum conversion realized by the conversion method of the present invention into a pore distribution curve and a pore distribution curve of a low-temperature nitrogen adsorption experiment.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention are described clearly and completely below, and it is obvious that the described embodiments are some, not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The invention discloses a method for converting a nuclear magnetic resonance T2 spectrum and pore distribution of a coal seam, which comprises the following steps:
a, performing nuclear magnetic resonance measurement on a saturated water coal crushed sample to obtain a nuclear magnetic resonance T2 spectrum;
b, carrying out low-temperature nitrogen adsorption experiment measurement on the saturated water coal crushed sample in the step a to obtain a pore distribution curve;
c, because the sizes of the rock pores have the characteristic of centralized distribution, the nuclear magnetic resonance T2 spectrum measured by the same rock sample and a low-temperature nitrogen adsorption experiment pore distribution curve have the same extreme points (maximum points or minimum points), through the statistical analysis of the extreme points of a plurality of blocks of rock samples, the transverse relaxation time T2 corresponding to the extreme point of the same block and the corresponding pore diameter R have the same conversion relation, the conversion relation of the transverse relaxation time T2 of the same block into the pore diameter R can be realized by establishing the linear relation, and the conversion relation of the transverse relaxation time T2 and the pore diameter R is as follows:
R＝a×T2b (1)
in the formula: r is the pore diameter, nanometer; t2 is the transverse relaxation time, in milliseconds; a and b are conversion coefficients which are obtained by actual data statistics and are dimensionless;
d, since the porosity component in the nuclear magnetic resonance T2 spectrum reflects the pore volume of the rock sample in unit volume, and the pore distribution curve measured by the low-temperature nitrogen adsorption experiment reflects the pore volume of the rock sample in unit mass, the porosity component in the nuclear magnetic resonance T2 spectrum needs to be converted into the pore volume of the sample in unit mass by dividing the volume density of the sample, and the conversion formula is as follows:
in the formula: PV is the pore volume per unit mass of the sample, cubic centimeters per gram; POR is the porosity component of nuclear magnetic resonance T2 spectrum, dimensionless; rhobIs the bulk density of the sample, grams per cubic centimeter;
e converting the nuclear magnetic resonance T2 spectrum in the step a into a pore distribution curve by using the formulas (1) and (2).
In this embodiment, in step a, the echo interval time TE of the nmr experiment apparatus is preferably set to 0.2 ms or less, and the polarization waiting time TW is preferably set to 6 seconds or more.
In this embodiment, in step c, the relationship of the transverse relaxation time T2 converted into the pore diameter R is obtained from the actual data statistics of the same block.
In this embodiment, preferably, in the step a, the preparation process of the saturated water coal crushed sample includes the following steps:
a1 collecting a sample of the coal seam drilling debris to be measured;
a2, drying the coal bed drilling rock debris sample in the step a1 to constant weight, and cooling to room temperature to obtain a dried coal bed drilling rock debris sample;
a3, crushing the dried coal bed drilling rock debris sample obtained in the step a2 by using crushing equipment to obtain a coal fragment sample, and weighing the coal fragment sample;
a4, adding water according to the weight of the crushed coal sample in the step a3, completely immersing the crushed coal sample in the water, and filtering to obtain a saturated water crushed coal sample;
a5, placing the drying agent and the saturated water coal crushed sample in the step a4 in a closed container until the weight of the saturated water coal crushed sample is unchanged, and obtaining the saturated water coal crushed sample with surface moisture removed.
In this embodiment, it is preferable that step a6 is further included, in which the crushed coal sample in step a4 is first stirred or sonicated by a stirring device or a sonicating device to ensure that water completely enters into the pores of the coal, and then is filtered.
In this embodiment, it is preferable that the weight of the sample of coal bed drilling cuttings collected in step a1 is not less than 100 g.
In this embodiment, preferably, the drying temperature of the coal bed drilling rock debris sample in the step a2 is 80-150 ℃, and the drying time is 3-6 hours; more preferably, the drying temperature is 110 ℃ and the drying time is 4 h.
In this embodiment, preferably, the pulverizing equipment in the step a3 is a vibrating screen, the mesh number of the vibrating screen is 70-110 meshes, and the diameter of the obtained coal crushed sample particles is 0.12-0.20 mm; more preferably, the mesh number of the vibrating screen is 90 mesh, and the diameter of the resulting coal dust sample particles is 0.16 mm.
In this embodiment, preferably, in step a5, the drying agent is a supersaturated potassium sulfate solution, and more preferably, the supersaturated potassium sulfate solution and the saturated water-coal crushed sample are placed in a closed container and left standing until the weight of the saturated water-coal crushed sample is constant.
In this embodiment, the water in step a4 is preferably deionized water or distilled water, and more preferably, distilled water is used.
In this embodiment, in step a5, the interval between weighing the saturated water coal crushed sample is preferably 3-6 hours, and more preferably 4 hours.
In this embodiment, preferably, in the step a6, the stirring or ultrasonic treatment time is 15-20 min.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A method for converting a nuclear magnetic resonance T2 spectrum and pore distribution of a coal seam is characterized by comprising the following steps:
a, performing nuclear magnetic resonance measurement on a saturated water coal crushed sample to obtain a nuclear magnetic resonance T2 spectrum;
b, carrying out low-temperature nitrogen adsorption experiment measurement on the saturated water coal crushed sample in the step a to obtain a pore distribution curve;
c, comparing the nuclear magnetic resonance T2 spectrum in the step a with the pore distribution curve in the step b, picking up the transverse relaxation time T2 and the pore diameter R value of the corresponding extreme point, and obtaining a conversion relation of the transverse relaxation time T2 and the pore diameter R value;
d, converting the nuclear magnetic resonance porosity component in the nuclear magnetic resonance T2 spectrum obtained in the step a into the pore volume of the sample with unit mass by using a nuclear magnetic resonance porosity component and pore volume conversion relation of the sample with unit mass;
e converting the nuclear magnetic resonance T2 spectrum in the step a into a pore distribution curve by using the conversion relation of the transverse relaxation time T2 and the pore diameter R value in the step c and the conversion relation of the nuclear magnetic resonance porosity component and the pore volume of the sample per unit mass in the step d.
2. The conversion method according to claim 1, wherein in step c, the conversion relationship between the transverse relaxation time T2 and the pore diameter R value is shown in formula (1):
R＝a×T2b (1)
in the formula: r is the pore diameter; t2 is the transverse relaxation time; a. b is a conversion coefficient.
3. The conversion method according to claim 1, wherein in step d, the nmr porosity component is converted to the pore volume per unit mass of the sample by the following equation:
in the formula: PV is the pore volume per mass of the sample; POR is the nuclear magnetic resonance porosity component; rhobIs the bulk density of the sample.
4. The transformation method according to claim 1, wherein in step a, the echo interval time TE of the nmr experiment apparatus is set to 0.2 ms or less, and the polarization waiting time TW is set to 6 seconds or more.
5. The conversion method according to claim 1, wherein in the step a, the preparation process of the saturated water coal crushed sample comprises the following steps:
a1 collecting a sample of the coal seam drilling debris to be measured;
a2, drying the coal bed drilling rock debris sample in the step a1 to constant weight, and cooling to room temperature to obtain a dried coal bed drilling rock debris sample;
a3, crushing the dried coal bed drilling rock debris sample obtained in the step a2 by using crushing equipment to obtain a coal fragment sample, and weighing the coal fragment sample;
a4, adding water according to the weight of the crushed coal sample in the step a3, completely immersing the crushed coal sample in the water, and filtering to obtain a saturated water crushed coal sample;
a5, placing the drying agent and the saturated water coal crushed sample in the step a4 in a closed container until the weight of the saturated water coal crushed sample is unchanged, and obtaining the saturated water coal crushed sample with surface moisture removed.
6. The conversion method according to claim 5, further comprising a step a6, wherein the crushed coal sample obtained in the step a4 is first stirred or sonicated by a stirring device or a sonicating device to ensure that water is completely introduced into the pores of the coal, and then filtered.
7. The conversion method according to claim 5, wherein the weight of the coal bed drilling debris sample collected in the step a1 is not less than 100 g.
8. The conversion method according to claim 5, wherein the drying temperature of the coal bed drilling debris sample in the step a2 is 80-150 ℃ and the drying time is 3-6 h.
9. The conversion method according to claim 5, wherein the crushing device in the step a3 is a vibrating screen, the mesh number of the vibrating screen is 80-100 meshes, and the diameter of the obtained coal crushed sample particles is 0.15-0.18 mm.
10. The conversion process of claim 5, wherein in step a5, the desiccant is a supersaturated solution of potassium sulfate.
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Cited By (1)
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| CN114577673B (en) * | 2022-01-18 | 2024-02-02 | 重庆大学 | Pore wettability NMR characterization method of equal-particle-size pulverized coal |
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