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CN112613174B - Shale methane adsorption capacity evaluation method considering multiple adsorption mechanisms - Google Patents

Shale methane adsorption capacity evaluation method considering multiple adsorption mechanisms Download PDF

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CN112613174B
CN112613174B CN202011506504.2A CN202011506504A CN112613174B CN 112613174 B CN112613174 B CN 112613174B CN 202011506504 A CN202011506504 A CN 202011506504A CN 112613174 B CN112613174 B CN 112613174B
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赵玉龙
刘香禺
张烈辉
张芮菡
唐慧莹
郭晶晶
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Abstract

The invention discloses a shale methane adsorption capacity evaluation method considering multiple adsorption mechanisms, based on the difference of adsorption mechanisms in nanopores with different sizes and the difference of adsorption phase methane densities under different adsorption mechanisms, the combined characterization is carried out on micropore filling type adsorption and polymolecular layer type adsorption, an established DA-TBET isothermal adsorption model has a clear physical background, the defects of the current adsorption model are overcome, and the evaluation result of the shale methane adsorption capacity is more reasonable and accurate. In addition, the method can be used for evaluating the methane adsorption capacity of the shale and the methane adsorption capacity of the coal bed sample, and has important application value in unconventional natural gas exploration and development.

Description

Shale methane adsorption capacity evaluation method considering multiple adsorption mechanisms
Technical Field
The invention relates to the technical field of unconventional natural gas exploration and development, in particular to a shale methane adsorption capacity evaluation method considering multiple adsorption mechanisms.
Background
The reasonable and accurate evaluation of the methane adsorption capacity of the shale is an important basis for realizing economic and efficient development of the shale gas reservoir, and plays a significant role in gas reservoir development. Through reasonably and accurately evaluating the methane adsorption capacity of the shale, the gas reservoir geological reserve can be calculated, and the method has important guiding significance for making and adjusting a shale gas reservoir development scheme, and related researches are widely concerned.
The indoor isothermal adsorption experiment is an important method for researching the methane adsorption capacity of the shale, and researchers develop a large amount of experimental improvement innovation and theoretical derivation work based on the experiment, wherein the research on the isothermal adsorption model representation of the methane adsorption capacity of the shale is particularly hot. According to different assumed adsorption mechanisms, the isothermal adsorption model mainly comprises a monolayer model, a polymolecular layer model and a micropore filling model. At present, although there are many isothermal adsorption models for methane in shale, no model considers the difference of adsorption phase methane density in pore channels with different sizes, and the adsorption phase methane density in different isothermal adsorption models is considered to be the same. According to the conclusion of molecular dynamics simulation research, methane molecules in micropores are influenced by the adsorption potential of the wall surface of a pore passage in an overlapping manner, so that the adsorption phase molecules are arranged more closely and the density of the adsorption phase molecules is higher, which is not distinguished in the conventional research on an isothermal adsorption model. In addition, although researchers consider microporous adsorption mode as filling adsorption mode and monolayer adsorption mode in mesopores and macropores and provide corresponding combined models (such as DA-Langmuir model and DA-LF model), the researchers find that methane is actually adsorbed in the mesopores as a polymolecular layer based on molecular dynamics simulation. Therefore, corresponding research work is necessary to be carried out, an isothermal adsorption model for effectively representing multiple adsorption mechanisms of shale gas is established, and support is provided for reasonably and accurately evaluating methane adsorption capacity of shale.
Disclosure of Invention
The invention mainly overcomes the defects in the prior art, and aims to provide the shale methane adsorption capacity evaluation method considering multiple adsorption mechanisms.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
an evaluation method for methane adsorption capacity of shale considering multiple adsorption mechanisms is characterized in that the calculation method comprises the following steps:
s1: drilling a shale core, crushing the core into powder in a laboratory, and screening out shale fine particles with the size of 60-80 meshes by using a screen;
s2: drying the shale sample prepared in the step in a thermostat at 80 ℃, and performing mass weighing record once by using a micro electronic balance every 12 hours until the mass change of the sample obtained by two adjacent times of weighing is less than or equal to 2%;
s3: loading the sample into a sample cylinder of a volumetric or gravimetric isothermal adsorption instrument, continuously vacuumizing for 24 hours, and further removing impurity adsorption gas and water vapor in the sample;
s4: carrying out isothermal adsorption experiments on the shale samples by using a volumetric method or gravimetric method isothermal adsorption instrument at least 3 different temperatures, and recording the change data of the excess adsorption quantity along with the pressure;
s5: fitting the experimental data by adopting a DA-TBET isothermal adsorption model considering a multiple adsorption mechanism to obtain isothermal adsorption model parameters at different temperatures;
s6: and calculating the adsorption capacity curve of the shale to the methane at different temperatures and pressures by using the isothermal adsorption model parameters at different temperatures obtained in the steps.
Further, the method for crushing the shale sample in the step S1 can refer to GB/T19560-2008 standard.
Further, the DA-TBET isothermal adsorption model expression considering the multiple adsorption mechanism established in step S5 is as follows:
Figure BDA0002845080240000031
in the formula, VexFor actually measuring the excess adsorption capacity, cm3/g；ρad1Adsorption phase methane density in cm in micropore filling mode3/g；ρad2Adsorption phase methane density in cm in the form of medium-large pore polymolecular layer3/g；ρgIs free phase methane density, cm3/g；VwThe volume of the adsorption space in cm is filled in the form of micropores in the sample3(ii)/g; r is a general gas constant, and the value here is 8.314J/(mol.K); t is adsorption experiment test temperature, K; e is the adsorption characteristic energy, J/mol; p is the experimental test pressure, MPa; p is a radical of0Is the methane virtual saturated vapor pressure, MPa; q is a parameter for representing the heterogeneity of the shale adsorption pores; vmIs the maximum adsorption capacity of the first molecular layer in the mesopores and macropores, cm3(ii)/g; c is a constant related to the heat of adsorption; n represents the number of adsorption layers; free phase methane density ρgCan be directly obtained by searching in chemical databases of national institute of standards and technology.
Further, the key parameters in the DA-TBET isothermal adsorption model considering the multiple adsorption mechanism established in step S5 are selected as follows:
adsorption phase methane density rho for micropore filling formad1Because of the superposition of adsorption potentials in narrow pore canals, methane molecules are closely arranged, and the density of the methane molecules is considered to be equal to the density of a boiling point, and the value is 0.425g/cm3；
Adsorption phase methane density rho for multi-molecular layer form in mesopore and macroporead2Using an adsorbed phase methane densitometer as proposed by Ozawa et al (1976)Calculating an empirical formula, wherein the expression is as follows:
ρad2＝ρbexp[-0.0025(T-Tb)]
in the formula, ρad2Adsorption phase methane density in cm in the form of medium-large pore polymolecular layer3/g；ρbThe boiling point density of methane is 0.425g/cm3(ii) a T is adsorption experiment test temperature, K; t isbThe boiling point temperature of methane under the standard atmospheric pressure is 111.7K;
for the number n of adsorbed layers of the polymolecular layer in the mesopores and macropores, the study conclusion of Zhongshang et al (shale gas adsorption mechanism study based on modified BET model, 2018) and the study conclusion of the applicant based on molecular dynamics simulation should be combined, and the number of adsorbed layers of the polymolecular layer in the shale should be 2.
Further, the virtual saturated vapor pressure calculation formula in the DA-TBET isothermal adsorption model considering the multiple adsorption mechanism established in step S5 is as follows:
Figure BDA0002845080240000041
in the formula, p0Is the methane virtual saturated vapor pressure, MPa; p is a radical ofcThe critical pressure of methane is 4.5992 MPa; t iscThe critical temperature of methane is 190.564K; t is adsorption experiment test temperature, K; k is a parameter characterizing the adsorption system.
Further, when the DA-TBET isothermal adsorption model is adopted to fit the experimental data at different temperatures in step S5, it is required to satisfy the parameter V in the DA-TBET modelwE, k and q remain the same.
Further, the adsorption capacity curve expression of the shale to methane at different temperatures and pressures in the step S6 is as follows:
Figure BDA0002845080240000042
in the formula, VabIs the real adsorption capacity of the shale to the methane, cm3(ii)/g; the remaining parameters are the values fitted in step S5.
According to the shale methane adsorption capacity evaluation method considering multiple adsorption mechanisms, based on the difference of adsorption mechanisms in nanopores with different sizes and the difference of adsorption phase methane densities under different adsorption mechanisms, the combined characterization is carried out on the adsorption in the micropore filling form and the adsorption in the multi-molecular-layer form, the established DA-TBET isothermal adsorption model has a clear physical background, the defects of the current adsorption model are overcome, and the evaluation result of the shale methane adsorption capacity is more reasonable and accurate. In addition, the method can be used for evaluating the methane adsorption capacity of the shale and the methane adsorption capacity of the coal bed sample, and has important application value in unconventional natural gas exploration and development.
Has the advantages that:
compared with the prior art, the invention has the following beneficial effects:
based on the difference of adsorption mechanisms in nanopores with different sizes and the difference of adsorption phase methane densities under different adsorption mechanisms, the combined characterization of micropore filling type adsorption and multi-molecular-layer type adsorption is carried out, the established DA-TBET isothermal adsorption model has a clear physical background, the defects of the current adsorption model are overcome, and the evaluation result of the methane adsorption capacity of the shale is more reasonable and accurate. In addition, the method can be used for evaluating the methane adsorption capacity of the shale and the methane adsorption capacity of the coal bed sample, and has important application value in unconventional natural gas exploration and development.
Drawings
FIG. 1 is measured isothermal adsorption data for shale samples 4-08 at different temperatures;
FIG. 2 is a comparison graph of measured isothermal adsorption data of shale samples 4-08 at different temperatures and fitting results of a DA-TBET model;
FIG. 3 is a graph of the methane adsorption capacity of shale samples 4-08 evaluated at different temperatures based on the DA-TBET model.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example (b):
a shale methane adsorption capacity evaluation method considering multiple adsorption mechanisms comprises the following specific calculation methods:
s1: drilling a shale core, crushing the core into powder according to GB/T19560-;
s2: drying the shale sample prepared in the step in a thermostat at 80 ℃, and performing mass weighing record once by using a micro electronic balance every 12 hours until the mass change of the sample obtained by two adjacent times of weighing is less than or equal to 2%;
s3: loading the sample into a sample cylinder of a volumetric or gravimetric isothermal adsorption instrument, continuously vacuumizing for 24 hours, and further removing impurity adsorption gas and water vapor in the sample;
s4: carrying out isothermal adsorption experiments on the shale samples by using a volumetric method or gravimetric method isothermal adsorption instrument at least 3 different temperatures, and recording the change data of the excess adsorption quantity along with the pressure;
s5: fitting the experimental data by adopting a DA-TBET isothermal adsorption model considering a multiple adsorption mechanism to obtain isothermal adsorption model parameters at different temperatures;
the DA-TBET isothermal adsorption model expression taking the multiple adsorption mechanism into consideration established in the step S5 is as follows:
Figure BDA0002845080240000061
in the formula, VexFor actually measuring the excess adsorption capacity, cm3/g；ρad1Adsorption phase methane density in cm in micropore filling mode3/g；ρad2Adsorption phase methane density in cm in the form of medium-large pore polymolecular layer3/g；ρgIs a free phaseDensity of methane in cm3/g；VwThe volume of the adsorption space in cm is filled in the form of micropores in the sample3(ii)/g; r is a general gas constant, and the value here is 8.314J/(mol.K); t is adsorption experiment test temperature, K; e is the adsorption characteristic energy, J/mol; p is the experimental test pressure, MPa; p is a radical of0Is the methane virtual saturated vapor pressure, MPa; q is a parameter for representing the heterogeneity of the shale adsorption pores; vmIs the maximum adsorption capacity of the first molecular layer in the mesopores and macropores, cm3(ii)/g; c is a constant related to the heat of adsorption; n represents the number of adsorption layers; free phase methane density ρgCan be directly obtained by searching in chemical databases of national institute of standards and technology.
The key parameters in the DA-TBET isothermal adsorption model considering the multiple adsorption mechanism established in the step S5 are selected as follows:
adsorption phase methane density rho for micropore filling formad1Because of the superposition of adsorption potentials in narrow pore canals, methane molecules are closely arranged, and the density of the methane molecules is considered to be equal to the density of a boiling point, and the value is 0.425g/cm3；
Adsorption phase methane density rho for multi-molecular layer form in mesopore and macroporead2An empirical formula was calculated using the adsorption phase methane density proposed by Ozawa et al (1976) and expressed as:
ρad2＝ρbexp[-0.0025(T-Tb)]
in the formula, ρad2Adsorption phase methane density in cm in the form of medium-large pore polymolecular layer3/g；ρbThe boiling point density of methane is 0.425g/cm3(ii) a T is adsorption experiment test temperature, K; t isbThe boiling point temperature of methane under the standard atmospheric pressure is 111.7K;
for the number n of adsorbed layers of the polymolecular layer in the mesopores and macropores, the study conclusion of Zhongshang et al (shale gas adsorption mechanism study based on modified BET model, 2018) and the study conclusion of the applicant based on molecular dynamics simulation should be combined, and the number of adsorbed layers of the polymolecular layer in the shale should be 2.
The virtual saturated vapor pressure calculation formula in the DA-TBET isothermal adsorption model considering the multiple adsorption mechanism established in step S5 is as follows:
Figure BDA0002845080240000071
in the formula, p0Is the methane virtual saturated vapor pressure, MPa; p is a radical ofcThe critical pressure of methane is 4.5992 MPa; t iscThe critical temperature of methane is 190.564K; t is adsorption experiment test temperature, K; k is a parameter characterizing the adsorption system.
When the DA-TBET isothermal adsorption model is adopted to fit the experimental data at different temperatures in the step S5, the parameter V in the DA-TBET model needs to be satisfiedwE, k and q remain the same.
S6: calculating the adsorption capacity curve of the shale to the methane at different temperatures and pressures by using the isothermal adsorption model parameters at different temperatures obtained in the step;
the expression of the adsorption capacity curve of the shale to methane at different temperatures and pressures in the step S6 is as follows:
Figure BDA0002845080240000081
in the formula, VabIs the real adsorption capacity of the shale to the methane, cm3(ii)/g; the remaining parameters are the values fitted in step S5.
Example 1:
the data used in this example are from 4-08 adsorption data for shale samples taken from the Shirai reef dam in the open literature (Tian et al, 2016) and the isothermal adsorption data obtained using a volumetric instrumentation at 35.4 deg.C, 50.4 deg.C and 65.4 deg.C, respectively, are shown in FIG. 1 and Table 1.
Free phase methane densities at different temperature and pressure conditions were obtained from queries in the national institute of standards and technology chemical database, as shown in table 1.
Adopting the established DA-TBET isothermal adsorption model to perform isothermal adsorption experiments on the samples measured at different temperaturesFitting data, calculating model parameters at different temperatures and fitting R2As shown in table 2. And substituting the parameters obtained by fitting into a DA-TBET model, and comparing the calculation result with the actually measured experimental data, as shown in figure 2. As can be seen from Table 2, the fitting R at different temperatures2All exceed 0.999, which shows that the DA-TBET model has good fitting effect. It can also be seen from FIG. 2 that the model fitting results are in good agreement with the measured isothermal adsorption experimental data. Based on the fitted model parameters, the methane adsorption capacity curve of the shale sample at different temperatures can be calculated, as shown in fig. 3.
In addition, by the established DA-TBET isothermal adsorption model, the total adsorption capacity of the shale to methane can be evaluated, and the methane gas quantity adsorbed by different adsorption modes in the shale pore canal can be respectively calculated by the first half part (micropore filling adsorption) and the second half part (multi-molecular layer adsorption) of the model, so that the method has important significance for further clarifying the adsorption capacity of the shale in different pore canals.
TABLE 1 measured isothermal adsorption data and free phase methane Density at different temperatures and pressures
Figure BDA0002845080240000091
TABLE 2 model parameters and fitting R calculated at different temperatures2
T Vw E k q Vm C n ρad1 ρad2 R2
308.55 0.00114 13721.5 4.71078 3.3193 2.10586 9.49687 2.0 0.425 0.25822 0.99926
323.55 0.00114 13721.5 4.71078 3.3193 1.98224 11.11999 2.0 0.425 0.24872 0.99968
338.55 0.00114 13721.5 4.71078 3.3193 1.96559 11.34600 2.0 0.425 0.23957 0.99903
According to the shale methane adsorption capacity evaluation method considering multiple adsorption mechanisms, based on the difference of adsorption mechanisms in nanopores with different sizes and the difference of adsorption phase methane densities under different adsorption mechanisms, the combined characterization is carried out on the adsorption in the micropore filling form and the adsorption in the multi-molecular-layer form, the established DA-TBET isothermal adsorption model has a clear physical background, the defects of the current adsorption model are overcome, and the evaluation result of the shale methane adsorption capacity is more reasonable and accurate. In addition, the method can be used for evaluating the methane adsorption capacity of the shale and the methane adsorption capacity of the coal bed sample, and has important application value in unconventional natural gas exploration and development.
Although the present invention has been described with reference to the above embodiments, it should be understood that the present invention is not limited to the above embodiments, and those skilled in the art can make various changes and modifications without departing from the scope of the present invention.

Claims (5)

1. A shale methane adsorption capacity evaluation method considering multiple adsorption mechanisms is characterized by comprising the following steps:
s1: drilling a shale core, crushing the core into powder in a laboratory, and screening out shale fine particles with the size of 60-80 meshes by using a screen;
s2: drying the shale sample prepared in the step in a thermostat at 80 ℃, and performing mass weighing record once by using a micro electronic balance every 12 hours until the mass change of the sample obtained by two adjacent times of weighing is less than or equal to 2%;
s3: loading the sample into a sample cylinder of a volumetric or gravimetric isothermal adsorption instrument, continuously vacuumizing for 24 hours, and further removing impurity adsorption gas and water vapor in the sample;
s4: carrying out isothermal adsorption experiments on the shale samples by using a volumetric method or gravimetric method isothermal adsorption instrument at least 3 different temperatures, and recording the change data of the excess adsorption quantity along with the pressure;
s5: fitting the experimental data by adopting a DA-TBET isothermal adsorption model considering a multiple adsorption mechanism to obtain isothermal adsorption model parameters at different temperatures; the DA-TBET isothermal adsorption model expression taking the multiple adsorption mechanism into consideration established in the step S5 is as follows:
Figure FDA0003458126680000011
in the formula, VexFor actually measuring the excess adsorption capacity, cm3/g；ρad1Adsorption phase methane density in cm in micropore filling mode3/g；ρad2Adsorption phase methane density in cm in the form of medium-large pore polymolecular layer3/g；ρgIs free phase methane density, cm3/g；VwThe volume of the adsorption space in cm is filled in the form of micropores in the sample3(ii)/g; r is a general gas constant, and the value here is 8.314J/(mol.K); t is adsorption experiment test temperature, K; e is adsorptionCharacteristic energy, J/mol; p is the experimental test pressure, MPa; p is a radical of0Is the methane virtual saturated vapor pressure, MPa; q is a parameter for representing the heterogeneity of the shale adsorption pores; vmIs the maximum adsorption capacity of the first molecular layer in the mesopores and macropores, cm3(ii)/g; c is a constant related to the heat of adsorption; n represents the number of adsorption layers; free phase methane density ρgCan be directly obtained by inquiring in a chemical database of the national institute of standards and technology;
s6: calculating the adsorption capacity curve of the shale to the methane at different temperatures and pressures by using the isothermal adsorption model parameters at different temperatures obtained in the step;
the expression of the adsorption capacity curve of the shale to methane at different temperatures and pressures in the step S6 is as follows:
Figure FDA0003458126680000012
in the formula, VabIs the real adsorption capacity of the shale to the methane, cm3(ii)/g; the remaining parameters are the values fitted in step S5.
2. The method for evaluating the methane adsorption capacity of shale considering multiple adsorption mechanisms as claimed in claim 1, wherein the method for crushing the shale sample in step S1 is according to GB/T19560-2008 standard.
3. The method for evaluating the methane adsorption capacity of shale considering multiple adsorption mechanisms according to claim 1, wherein the key parameters in the DA-TBET isothermal adsorption model considering multiple adsorption mechanisms established in step S5 are selected as follows:
adsorption phase methane density rho for micropore filling formad1Because of the superposition of adsorption potentials in narrow pore canals, methane molecules are closely arranged, and the density of the methane molecules is considered to be equal to the density of a boiling point, and the value is 0.425g/cm3；
Adsorption phase methane density rho for multi-molecular layer form in mesopore and macroporead2Which isThe expression is as follows:
ρad2＝ρbexp[-0.0025(T-Tb)]
in the formula, ρad2Adsorption phase methane density in cm in the form of medium-large pore polymolecular layer3/g；ρbThe boiling point density of methane is 0.425g/cm3(ii) a T is adsorption experiment test temperature, K; t isbThe boiling point temperature of methane under the standard atmospheric pressure is 111.7K;
and for the number n of the adsorption layers of the polymolecular layers in the mesopores and the macropores, the number of the adsorption layers of the polymolecular layers in the shale is 2.
4. The method for evaluating the methane adsorption capacity of shale in consideration of multiple adsorption mechanisms according to claim 1, wherein the virtual saturated vapor pressure calculation formula in the DA-TBET isothermal adsorption model in consideration of multiple adsorption mechanisms established in the step S5 is as follows:
Figure FDA0003458126680000021
in the formula, p0Is the methane virtual saturated vapor pressure, MPa; p is a radical ofcThe critical pressure of methane is 4.5992 MPa; t iscThe critical temperature of methane is 190.564K; t is adsorption experiment test temperature, K; k is a parameter characterizing the adsorption system.
5. The method for evaluating the methane adsorption capacity of shale considering multiple adsorption mechanisms as claimed in claim 1, wherein the parameter V in the DA-TBET model is satisfied when the DA-TBET isothermal adsorption model is used to fit experimental data at different temperatures in step S5wE, k and q remain the same.
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