CN112946005B - Shale microcrack evaluation method and application thereof - Google Patents
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- G01N24/00—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention relates to the technical field of petrochemical industry, and particularly discloses a shale microcrack evaluation method and application thereof. According to the shale microcrack evaluation method, the size of a micro-pore is represented by combining low-temperature nitrogen adsorption and nuclear magnetic resonance to judge the shale microcracks, quantitative representation is performed by using Gaussian fitting, and microcrack factor control analysis is performed at the same time; because the method adopts the nuclear magnetic resonance technology and the Gaussian fitting method, the experimental result is not only qualitative, but also the size and the proportion of the fractures are visually represented by further quantitatively analyzing the microcracks, the operability is strong, the repeatability degree is high, the method has important significance for quantitatively evaluating the microcracks of the shale reservoir, the problem that most of the conventional shale microcrack evaluation methods cannot be accurately evaluated is solved, and the method has wide application prospect.
Description
Technical Field
The invention relates to the technical field of petrochemical industry, in particular to a shale microcrack evaluation method and application thereof.
Background
Shale oil is a petroleum resource contained in shale layer systems dominated by shale. With the development of industrial economy, the demand of oil and gas resources is increasing day by day, and by 2020, the dependence of oil resources in China on the outside is as high as more than 60%, so that the energy crisis is urgent and needs to be solved as soon as possible. Shale oil gas is used as a main unconventional oil gas resource type, has huge resource potential and large recoverable resource amount, and is expected to solve the huge gap existing in the current energy demand.
Microcracks are an important pore type of shales. The microcracks are classified according to the sizes of the fractures, generally, the fractures with the widths of 100 micrometers or less than 150 micrometers are called microcracks, a good seepage network can be formed, so that the reservoir quality is improved, and quantitative research on the microcracks is beneficial to understanding the shale reservoir type and exploration potential evaluation. In addition, the microcracks are widely developed in various reservoirs, and a large number of students have verified that the microcracks have the capacity of storing oil and gas and providing seepage channels, so that the microcracks have important significance for oil and gas development, and can help to determine information of crack development and reveal some problems of crack-related mechanisms which are difficult to discuss. Therefore, how to judge the shale microcracks, and carry out quantitative characterization and cause control analysis on the shale microcracks has great significance.
At present, shale microcrack evaluation has important significance for the exploration and development of shale oil. However, most shale microcrack evaluation methods in the prior art cannot perform accurate evaluation, so that shale reservoir type cannot be effectively known and exploration potential evaluation cannot be performed.
Disclosure of Invention
The embodiment of the invention aims to provide a shale microcrack evaluation method to solve the problem that most of the existing shale microcrack evaluation methods in the background art cannot be accurately evaluated.
In order to achieve the above purpose, the embodiments of the present invention provide the following technical solutions:
a shale microcrack evaluation method, particularly a method for researching shale microcracks by using nuclear magnetic resonance technology, which is characterized in that shale to be evaluated (also can be shale) is washed with oil and dried to obtain a dry sample, the dry sample is subjected to a nuclear magnetic resonance experiment in the process of vacuumizing and pressurizing saturated oil, the size of a micro aperture is represented in combination with low-temperature nitrogen adsorption to judge the shale microcracks, quantitative representation is carried out by using Gaussian fitting, and microcrack control factor analysis is carried out at the same time.
The embodiment of the invention also aims to provide application of the shale microcrack evaluation method in shale oil exploration and development.
Compared with the prior art, the invention has the beneficial effects that:
the shale microcrack evaluation method provided by the embodiment of the invention can be used for researching shale and/or shale microcracks, the size of the micro-pore diameter is represented by the combination of low-temperature nitrogen adsorption and nuclear magnetic resonance to judge the shale microcracks, the quantitative representation is carried out by using Gaussian fitting, and the microcrack factor control analysis is carried out at the same time; because the method adopts the nuclear magnetic resonance technology and the Gaussian fitting method, the experimental result is not only qualitative, but also the size and the proportion of the fractures are visually represented by further quantitatively analyzing the microcracks, the operability is strong, the repeatability degree is high, the method has important significance for quantitatively evaluating the microcracks of the shale reservoir, the problem that most of the conventional shale microcrack evaluation methods cannot be accurately evaluated is solved, and the method has wide application prospect.
Drawings
Fig. 1 is a schematic flow chart of a shale microcrack evaluation method according to an embodiment of the present invention.
Fig. 2 is a nuclear magnetic resonance T2 spectrum of saturated oil shale according to an embodiment of the present invention.
Fig. 3 is a crack image of a sample provided in an embodiment of the present invention.
FIG. 4 is a scanning electron microscope image of microcracks of a sample provided in an embodiment of the invention.
Fig. 5 is a graph of a combined characterization result of low-temperature nitrogen adsorption and nuclear magnetic resonance provided in an embodiment of the present invention.
FIG. 6 is a graph of the results of a Gaussian fit characterization of microcracks provided in an embodiment of the invention.
FIG. 7 is a plot of a fit of a graticule equation between fluid volumes of n-dodecane and nuclear magnetic semaphores in an embodiment of the present invention.
FIG. 8 is a linear relationship graph of the total quartz and feldspar content and microcracks in an embodiment of the invention.
FIG. 9 is a graph of the linear relationship of total calcite and dolomite content to microcracks in an example of the invention.
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples. The following examples will aid those skilled in the art in further understanding the present invention, but are not intended to limit the invention in any manner. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
First, it should be noted that microcracks can help to determine information about crack development and reveal some mechanistic issues related to cracks that are difficult to explore. The length of the microcracks can be used for predicting the development scale of the microcracks, for example, in the prior art, the macroscopic high-angle microcracks in the shale reservoir are successfully predicted by using the microcracks in the bedding pulses, the influence of the geometric characteristics of the fracture walls of the tension-type microcracks in the shale reservoir on the permeability is discussed, and the mechanism of the influence of the shape of the fracture walls on the seepage is disclosed; the microcracks can be applied to the research of information such as ancient structural stress fields, ancient ground temperature, ancient pressure, ancient salinity and the like; the micro-cracks and diagenesis can be mutually influenced and can be applied to the research of diagenesis evolution history. The Zhao help Sheng and the like consider that geological conditions of shale gas reservoirs in Shangdos basin Shanxi groups are general, but the microcracks can be gathered into reservoirs, the microcracks can improve the permeability of the reservoirs, and the shale gas reservoir has better shale gas exploration potential in a microcrack development area. Yangji et al indicate that microcracks are important reservoir spaces and percolation channels in shale reservoirs, and the development degree of microcracks is directly related to the reserve volume and capacity of shale gas. Therefore, how to judge the shale microcracks, quantitatively characterize the shale microcracks and perform factor control analysis has great significance.
Secondly, in the prior art, various shale microcrack evaluation schemes exist, but most evaluation results are not accurate enough. For example:
the technical scheme is as follows: according to outcrop section and well core observation, Wangyuman et al observes the Wufeng-Longmaxi group shale of a certain landmark well in the south of Chuan, and totally observes 66 micro-cracks in 8 core sections with the length of 79.86 m. The technical scheme has the following disadvantages: the method directly observes the crack scale (length and width) of the rock sample, is only suitable for describing macro cracks with crack width of more than 0.1mm, and cannot judge the micro cracks and the filling condition thereof.
The second technical scheme is as follows: the nanometer-scale micro-cracks can be described conveniently through a rock slice/high-precision SEM, the crack scale (length and width) and the filling condition are directly observed, the crack density is estimated, and the method is suitable for fine description of the cracks. The technical scheme has the following disadvantages: the technology is greatly influenced by a sample observation point, is limited to qualitative observation of the microcracks, and cannot quantitatively characterize the microcracks.
The third technical scheme is as follows: a double-pore medium porosity mathematical model is applied to Wangyuiman, golden light and the like, and a rock physical model is formed according to experiment test data such as a helium method and the like and pore volume to respectively calculate the porosity of the developed cracks in the Fuling gas field and the Changning gas area, and the result shows that the depth section below 2540m is a crack pore concentrated development section. The technical scheme has the following disadvantages: the dual-pore medium model method of the scheme quantitatively calculates the porosity of the matrix and the porosity of the crack, but the representation of the ratio of the size to the volume of the microcrack is not clear, and the influence of an experimental test method is large.
Aiming at the prior technical scheme, the shale microcrack evaluation method provided by the embodiment of the invention is a method for researching shale microcracks by using a nuclear magnetic resonance technology, and the method is characterized in that oil washing and drying are carried out on shale (or shale) to be evaluated to obtain a dry sample, the dry sample is subjected to a nuclear magnetic resonance experiment in the process of vacuumizing and pressurizing saturated oil, the size of a microscopic aperture is represented in combination with low-temperature nitrogen adsorption to judge the shale microcracks, quantitative representation is carried out by using Gaussian fitting, and microcrack control factor analysis is carried out at the same time.
The embodiment of the invention aims at the problems of improving the reservoir quality through the microcracks, knowing the shale reservoir type and exploring potential evaluation, and distinguishing the shale microcracks on the basis of representing the size of the micro-pore size through the combination of low-temperature nitrogen adsorption and nuclear magnetic resonance by taking the nuclear magnetic resonance technology as a technical means. And performing quantitative characterization on the micro-crack by using Gaussian fitting, and simultaneously performing micro-crack factor control analysis.
In another preferred embodiment of the invention, the oil washing and drying is to wash the shale to be evaluated by using a soxhlet extraction method or an ultrasonic method to remove residual oil in pores, then carry out vacuum drying on the sample after oil washing, set the temperature to be 60-70 ℃, and the drying time to be 6-12h, and place the dried sample in a drying dish for later use.
Preferably, in the oil washing drying, after oil washing, a sample subjected to oil washing is placed in a vacuum oven for drying, the temperature is set to 65 ℃, the drying time is 9 hours, and the dried sample is placed in a drying dish as a dry sample for later use.
As another preferred embodiment of the invention, the solvent of the wash oil is a mixed organic solvent of dichloromethane and acetone with a volume ratio of 1.5: 1.
Preferably, the solvent of the wash oil is a mixed organic solvent of dichloromethane and acetone in a volume ratio of 3: 1.
As another preferred embodiment of the present invention, the characterization of the micro pore size by the combination of low-temperature nitrogen adsorption and nuclear magnetic resonance of the dry sample in the process of vacuumizing and pressurizing saturated oil specifically comprises: and carrying out a nuclear magnetic resonance test on the dry sample before vacuumizing and pressurizing the saturated oil, and carrying out a nuclear magnetic resonance test on the dry sample after vacuumizing and pressurizing the saturated oil. Specifically, the transverse relaxation time T2 of the sample is measured by selecting a CPMG pulse sequence for the dry sample, and after the parameters of the measurement system are set, the measurement is started after the current parameters are confirmed to be accurate; after the saturated oil is vacuumized and pressurized, taking out the saturated sample from the sample chamber, wiping the surface free fluid, measuring the nuclear magnetic signal characteristics of the sample, and performing corresponding dry sample inversion.
As another preferred embodiment of the invention, in the characterization of the microscopic pore size by the combination of the low-temperature nitrogen adsorption and the nuclear magnetic resonance of the dry sample in the process of vacuumizing and pressurizing saturated oil, the dry sample is vacuumized and discharged from the air in the pore throat, and then saturated oil (preferably n-dodecane) is injected, the pressure is kept between 12 and 17MPa (preferably about 15 MPa), and the saturation time is 24h to 48 h.
As another preferred embodiment of the invention, the dry sample is vacuumized to exhaust the air in the pore throat, and the relative vacuum degree reaches 75kPa for 12h-24 h.
As another preferred embodiment of the present invention, the shale microcracks are determined according to a result of a nuclear magnetic resonance test performed on a dry sample after the dry sample is vacuumized and pressurized with saturated oil (to obtain saturated oil shale or mud shale), and the specific determination process is as follows:
in the nuclear magnetic resonance T2 spectrum of saturated oil shale or mud shale, the nuclear magnetic resonance spectrum T2 shows a unimodal or multimodal morphology and can be regarded as being composed of a plurality of normal distributions which are superposed. The nuclear magnetic resonance T2 spectrum of the saturated shale shows that the relaxation time is mainly distributed between 0.01ms and 1000ms, the saturated shale shows a 'double peak' state, and the amplitude of a post-peak signal is low. The residual signal after the gaussian fit indicates the amount of fluid signal present in the microfractures. The existence of cracks can be found through the observation of the sample, the existence of micro cracks can be observed according to a scanning electron microscope, and the relaxation time is prolonged due to the existence of the micro cracks.
As another preferred embodiment of the present invention, the quantitative characterization by using gaussian fitting specifically includes calibrating the nuclear magnetic resonance relaxation-pore size conversion coefficient C according to the result of the low-temperature nitrogen adsorption and nuclear magnetic resonance combined characterization performed on the dry sample in the process of vacuum-pumping and pressurizing saturated oil, and performing gaussian fitting on the main peak in nuclear magnetic resonance, where the initial signal amount of the free fluid in the main peak in the nuclear magnetic resonance test is denoted as a0, and the signal amount after gaussian fitting is denoted as a1, and then the signal amount Af of the free fluid in the microcrack is denoted as a0-a 1.
As another preferred embodiment of the present invention, the gaussian fitting process is performed according to the following formula: x is a × EXP (- (((log (C × M) -a)/b)2))
Wherein A is a nuclear magnetic resonance T2 spectrum semaphore peak; c is the NMR relaxation-pore diameter conversion coefficient; a is a peak value of a central axis corresponding to a main peak of a nuclear magnetic resonance T2 spectrum; b is the nuclear magnetic resonance main peak T2 spectral width; m is the nuclear magnetic resonance T2 spectral semaphore at different times.
As another preferred embodiment of the present invention, the nmr relaxation-pore size conversion coefficient C is calculated according to the following formula: c is Amax/Bmax; wherein Amax is the maximum value corresponding to the main peak in the nuclear magnetic resonance T2 spectrum, Bmax is the maximum value corresponding to the adsorption capacity in nitrogen adsorption, and C is the nuclear magnetic resonance relaxation-aperture conversion coefficient.
The embodiment of the invention also provides application of the shale microcrack evaluation method in shale oil exploration and development.
The technical effects of the shale microcrack evaluation method of the present invention will be further described below by referring to specific examples.
Example 1
A shale microcrack evaluation method takes a nuclear magnetic resonance technology as a technical means, and shale microcracks are judged on the basis of representing the size of a micro pore size by the combination of low-temperature nitrogen adsorption and nuclear magnetic resonance. And performing quantitative characterization on the micro-crack by using Gaussian fitting, and simultaneously performing micro-crack factor control analysis.
In the embodiment of the invention, the shale microcrack evaluation method specifically comprises the following steps:
judging microcracks;
step two, representing the size of the microcracks;
step three, the micro-cracks account for the ratio;
and step four, controlling the micro-crack.
Example 2
A shale microcrack evaluation method is specifically shown in figure 1, and specifically comprises the following steps:
1) preparing a shale dry sample: washing oil and drying the shale to be evaluated to obtain a dry sample;
2) preparing saturated oil shale: the method comprises the steps of vacuumizing and pressurizing saturated oil on a dry sample, performing a nuclear magnetic resonance experiment on the dry sample in the vacuumizing and pressurizing saturated oil process, jointly representing the size of a micro-pore in combination with low-temperature nitrogen adsorption so as to judge shale microcracks, quantitatively representing the shale microcracks by using Gaussian fitting, and simultaneously performing microcrack factor control analysis.
Example 3
Compared with the embodiment 1, the specific process for the step one is as follows:
(1) the laboratory temperature was adjusted to 25 ℃ and ferrous metal ware around the nmr magnet box was removed. The instrument power is turned on, the magnet control temperature is set to 35 ℃ according to the instrument requirements, and the probe and the magnet are kept at constant temperature. The instrument is preheated for more than 16 h.
(2) And entering measurement control analysis software, and checking whether the communication between the software and the instrument is normal or not.
(3) And sequentially numbering the obtained original shale samples, removing residual oil in pores by a Soxhlet extraction method or an ultrasonic method, and adopting a mixed organic solvent of dichloromethane and acetone with a volume ratio of 3:1 as a solvent. And (3) placing the sample after oil washing in a vacuum oven for drying, setting the temperature to be 65 ℃, setting the drying time to be 9h, and placing the dried sample in a drying dish for later use.
(4) Setting nuclear magnetic resonance parameters: according to SY/T6490-2014 (rock sample nuclear magnetic resonance parameter laboratory measurement specification) and in combination with the properties of the sample, the acquisition parameters of nuclear magnetic resonance measurement transverse relaxation time T2 of the shale are set as follows: the waiting Time (TW) is 3000ms, the echo interval (TE) is 0.07ms, the Number of Echoes (NECH) is 3000, and the Number of Superpositions (NS) is 32; and measuring the NMR spin echo train of the sample by using a spin echo pulse sequence (CPMG), and inverting the nuclear magnetic resonance relaxation signal by using a SIRT method.
(5) Nuclear magnetic resonance testing: firstly, standard sample preparation: a standard (25mL-30mL) containing a 0.05 wt% solution of CuSO4 was placed in a glass test tube (non-magnetic container) at the center of the magnetic field. Measuring a dry sample signal of the shale sample: and (3) well loading the prepared rock sample (dry sample) to be measured by using a glass test tube, and putting the rock sample into the measurement cavity. And selecting a CPMG pulse sequence to measure the transverse relaxation time T2 of the sample, setting the parameters of the measurement system, and starting measurement after confirming that the current parameters are accurate. ③ saturated oil of the sample: and (5) placing the dry sample after the test is finished in a vacuumizing saturation device, and saturating the oil. Firstly, opening a vacuumizing switch, and vacuumizing air in a sample chamber and the pore throat of the rock sample until the relative vacuum degree reaches 75kPa for 12-24 h. And then closing the vacuum pump, opening a switch of the fluid saturation device, and injecting n-dodecane into the sample chamber, wherein the pressure is kept at about 15MPa, and the saturation time is 24-48 h. And taking out the saturated sample from the sample chamber, wiping the surface free fluid, measuring the nuclear magnetic signal characteristics of the sample, and performing corresponding dry sample inversion.
Example 4
Compared with the embodiment 3, the method further comprises a micro-crack specific judging process in the step one: in a saturated oil shale nuclear magnetic resonance T2 spectrum, a T2 nuclear magnetic spectrum shows a unimodal or multimodal morphology and can be regarded as consisting of superposition of multiple normal distributions. The nuclear magnetic T2 spectrum of the saturated shale shows that the relaxation time is mainly distributed between 0.01ms and 1000ms, the saturated shale shows a 'double peak' state, and the amplitude of a post-peak signal is low. The residual signal after the gaussian fit indicates the amount of fluid signal present in the microfractures. The existence of cracks can be found through the observation of the sample, the existence of micro cracks can be observed according to a scanning electron microscope, and the relaxation time is prolonged due to the existence of the micro cracks.
Example 5
Compared with the embodiment 1, the specific process is as follows when the second step is carried out:
(ii) Joint characterization of pore diameter
The pore size span range of the shale is large, the full pore size structure of the shale cannot be effectively represented by a single experiment from nanometer to micrometer (a millimeter level for part of sample development), different experimental means are only suitable for detection in a certain pore size (pore diameter) range, and each method also has respective advantages and disadvantages.
The pore diameter characterization of the invention integrates a low-temperature nitrogen adsorption experiment and a nuclear magnetic resonance experiment, and effectively and comprehensively obtains the pore structure information of the shale. And calibrating the nuclear magnetic resonance relaxation-aperture conversion coefficient by combining the nuclear magnetic resonance T2 spectrum with the low-temperature nitrogen adsorption curve. And carrying out pore diameter joint characterization on the sample to obtain the obtained pore diameter distribution curve.
Wherein the nuclear magnetic resonance relaxation-pore diameter conversion coefficient is calculated according to the following formula:
C＝Amax/Bmax
in the formula, Amax is the maximum value corresponding to the main peak in a nuclear magnetic resonance T2 spectrum, Bmax is the maximum value corresponding to the adsorption capacity in nitrogen adsorption, and C is the nuclear magnetic resonance relaxation-aperture conversion coefficient.
Indication of microcracks
The data processing adopts a Gaussian fitting method, the main peak in nuclear magnetic resonance is subjected to Gaussian fitting, the initial signal quantity of the free fluid in the main peak in nuclear magnetic resonance testing is recorded as A0, the signal quantity after the Gaussian fitting is recorded as A1, and the signal quantity Af of the free fluid in the microcrack is recorded as A0-A1.
Wherein, the Gaussian fitting process is carried out according to the following formula:
X＝A×EXP(-(((log(C×M)-a)/b)2))
wherein A is a nuclear magnetic resonance T2 spectrum semaphore peak; c is the NMR relaxation-pore diameter conversion coefficient; a is a peak value of a central axis corresponding to a main peak of a nuclear magnetic resonance T2 spectrum; b is the nuclear magnetic resonance main peak T2 spectral width; m is the nuclear magnetic resonance T2 spectral semaphore at different times.
Example 6
Compared with the embodiment 1, the specific process when the third step is carried out is as follows:
fluid calibration experimental process
1) Taking out five small bottles with the volume of about 1.2mL and matched bottle caps, and weighing the mass of 5 empty bottles respectively after screwing the bottle caps; after weighing, respectively placing the bottles in a nuclear magnetic resonance apparatus to measure T2 spectrums of the bottles as empty bottle bases; in view of the pore volume of the sample of the experiment, the pipette was removed and n-dodecane of different mass (0.1g to 1.35g at intervals of about 0.1 g) was measured separately as a standard in 5 empty bottles.
2) Respectively weighing and placing the weighed materials into a glass test tube for nuclear magnetic resonance testing; after the test is finished, respectively removing the corresponding empty bottle bases for inversion; after the inversion is finished, respectively accumulating the free fluid signal amplitude of the T2 spectrum corresponding to each volume; fitting the linear relation between the n-dodecane volume of the standard sample and the corresponding signal amplitude by using a statistical linear regression method; because the magnitude order difference between the fluid volume and the signal amplitude is large, in order to ensure the accuracy of the coefficient as much as possible, the signal amplitude is reduced by 10000 times and then is fitted with the fluid volume; the following set of graticule equations was obtained:
Voil＝k×K×10-5
Where K is the slope of the plot equation and K is the total nuclear magnetic signal of n-dodecane.
Secondly, converting the fluid volume of the signal quantity Af of the free fluid in the microcrack to obtain the fluid volume Vf. Then the volume ratio of the microcracks is as follows:
V＝Vf/Vrock*100
In the formula, VRockIs the volume of rock, V is the volume of microcracks, VfIs the volume of fluid.
Example 7
Compared with the example 1, when the fourth step is carried out, the specific process is as follows:
the analysis of the main control factors of the micro-crack development is helpful for understanding the distribution of the micro-cracks, and a great deal of research is carried out on the main control factors of the micro-crack development by the predecessors. The development of tectonic microcracks in shale is primarily controlled by two major factors, intrinsic and extrinsic. The internal factors can be subdivided into rock components and structures, and the rock components mainly refer to the content of brittle minerals (mainly the content of siliceous minerals and the content of brittle minerals such as feldspar) and the content of clay minerals. The external factors are mainly related to the construction position and the construction stress magnitude.
The invention analyzes the micro-crack and rock component-mineral content (internal cause) to obtain the leading factor which influences the micro-crack development.
Example 8
A shale microcrack evaluation method, in particular to a method for researching microcracks on shale by utilizing a nuclear magnetic resonance technology. As shown in figure 1, a nuclear magnetic resonance T2 spectrum test is carried out after a sample is washed with oil, dried at low temperature and saturated with oil, pore size characterization is carried out by combining low-temperature nitrogen adsorption, and the microcrack size ratio is characterized by adopting a Gaussian fitting method. The specific experimental procedures are as follows:
(1) the laboratory temperature was adjusted to 25 ℃ and ferrous metal ware around the nmr magnet box was removed. The instrument power is turned on, the magnet control temperature is set to 35 ℃ according to the instrument requirements, and the probe and the magnet are kept at constant temperature. The instrument is preheated for more than 16 h.
(2) And entering measurement control analysis software, and checking whether the communication between the software and the instrument is normal or not.
(3) And sequentially numbering the obtained original shale samples, removing residual oil in pores by a Soxhlet extraction method or an ultrasonic method, and adopting a mixed organic solvent of dichloromethane and acetone with a volume ratio of 3:1 as a solvent. And (3) placing the sample after oil washing in a vacuum oven for drying, setting the temperature to be 65 ℃, setting the drying time to be 9h, and placing the dried sample in a drying dish for later use.
(4) Setting nuclear magnetic resonance parameters: according to SY/T6490-2014 (rock sample nuclear magnetic resonance parameter laboratory measurement specification) and in combination with the properties of the sample, the acquisition parameters of nuclear magnetic resonance measurement transverse relaxation time T2 of the shale are set as follows: the waiting Time (TW) is 3000ms, the echo interval (TE) is 0.07ms, the Number of Echoes (NECH) is 3000, and the Number of Superpositions (NS) is 32; and (3) measuring the NMR spin echo train of the sample by using a spin echo pulse sequence (CPMG), and inverting the nuclear magnetic resonance relaxation signal by using a SIRT method.
(5) Nuclear magnetic resonance testing: firstly, standard sample preparation: a standard (25mL-30mL) containing 0.05% CuSO4 solution was placed in a glass tube (non-magnetic container) at the center of the magnetic field. Measuring a dry sample signal of the shale sample: and (3) loading the prepared rock sample (dry sample) to be measured by using a glass test tube, and putting the rock sample into a measurement cavity. And selecting a CPMG pulse sequence to measure the transverse relaxation time T2 of the sample, setting the parameters of the measurement system, and starting measurement after confirming that the current parameters are accurate. ③ saturated oil of the sample: and (4) placing the dry sample after the test is finished in a vacuumizing saturation device, and saturating the oil. Firstly, opening a vacuumizing switch, and vacuumizing air in a sample chamber and the pore throat of the rock sample until the relative vacuum degree reaches 75kPa for 12-24 h. And then closing the vacuum pump, opening a switch of the fluid saturation device, and injecting n-dodecane into the sample chamber, wherein the pressure is kept at about 15MPa, and the saturation time is 24-48 h. And taking out the saturated sample from the sample chamber, wiping the surface free fluid, measuring the nuclear magnetic signal characteristics of the sample, and performing corresponding dry sample inversion.
Example 9
Compared with the embodiment 8, the method further comprises a micro-crack specific judging process:
in a saturated oil shale nuclear magnetic resonance T2 spectrum, a T2 nuclear magnetic spectrum shows a unimodal or multimodal morphology and can be regarded as consisting of superposition of multiple normal distributions. The nuclear magnetic T2 spectrum of the saturated shale shows that the relaxation time is mainly distributed between 0.01ms and 1000ms, the saturated shale shows a 'double peak' state, and the amplitude of a post-peak signal is low. The residual signal after the gaussian fitting indicates the fluid signal existing in the microcracks, specifically referring to fig. 2, fig. 2 is a nuclear magnetic resonance T2 spectrum of the saturated oil shale, and the microcrack proportion can be calculated through the region marked by the microcracks in the graph.
By observing and characterizing the sample, the specific crack image of the sample is shown in fig. 3, and the existence of the crack can be found according to the observation of the sample in fig. 3.
By performing scanning electron microscope characterization on a sample, a specific microcrack scanning electron microscope image is shown in fig. 4, the existence of microcracks can be observed according to the scanning electron microscope image shown in fig. 4, and the relaxation time is prolonged due to the existence of microcracks.
Example 10
In comparison to example 9, a microcrack size characterization was also included:
(ii) Joint characterization of pore diameter
The pore size span range of the shale is large, the full pore size structure of the shale cannot be effectively represented by a single experiment from nanometer to micrometer (a millimeter level for part of sample development), different experimental means are only suitable for detection in a certain pore size (pore diameter) range, and each method also has respective advantages and disadvantages.
The pore diameter characterization method integrates a low-temperature nitrogen experiment and a nuclear magnetic resonance experiment, and effectively and comprehensively obtains the pore structure information of the shale. And calibrating the nuclear magnetic resonance relaxation-aperture conversion coefficient C by combining the nuclear magnetic resonance T2 spectrum with the low-temperature nitrogen adsorption curve. The pore diameter joint characterization is carried out on the sample, and the obtained pore diameter distribution curve result is shown in figure 5, in particular to a low-temperature nitrogen adsorption and nuclear magnetic resonance joint characterization result graph.
B’＝B*25.03
B' is the corresponding value after nitrogen adsorption conversion, and B is the nitrogen adsorption value.
Indication of microcracks
The data processing adopts a Gaussian fitting method, the pre-peak in the double peak is subjected to Gaussian fitting when the nuclear magnetic resonance is in a double peak type, the specific result is shown in FIG. 6, FIG. 6 is a result graph of representing the microcracks through Gaussian fitting, the initial signal quantity A0 is recorded as 5894.57a.u., the fitted signal quantity A1 is recorded as 4157.19a.u., and then the signal quantity A of the free fluid in the microcracksf1737.38a.u., the gaussian fit equation is as follows: x ═ 99.7 × EXP (((LOG (25.03 × T2) -0.936)/0.71)2))。
Example 11
Compared with the embodiment 10, the method also comprises the following calculation of the micro-crack ratio:
fluid calibration experimental process
(1) Taking out five small bottles with the volume of about 1.2mL and matched bottle caps, and weighing the mass of 5 empty bottles respectively after screwing the bottle caps; after weighing, respectively placing the bottles in a nuclear magnetic resonance apparatus to measure T2 spectrums of the bottles as empty bottle bases; in view of the pore volume of the sample of this experiment, the pipette was removed and n-dodecane of different masses (0.1g to 1.35g at intervals of about 0.1 g) was metered into 5 empty bottles as standard samples.
(2) Respectively weighing and placing the weighed materials into a glass test tube for nuclear magnetic resonance testing; after the test is finished, respectively removing the corresponding empty bottle bases to carry out inversion; after the inversion is finished, respectively accumulating the free fluid signal amplitude of the T2 spectrum corresponding to each volume; fitting the linear relation between the n-dodecane volume of the standard sample and the corresponding signal amplitude by using a statistical linear regression method; because the magnitude order difference between the fluid volume and the signal amplitude is large, in order to ensure the accuracy of the coefficient as much as possible, the signal amplitude is reduced by 10000 times and then is fitted with the fluid volume, and the obtained graticule equation fitting graph between the n-dodecane fluid volume and the nuclear magnetic semaphore is shown in FIG. 7, so that a graticule equation set is obtained as follows:
Voil＝0.6921*K*10-5
Where 0.6921 is the slope of the plot equation and K is the total nuclear magnetic signal of n-dodecane.
② signal quantity A of free fluid in the above-mentioned microfracturesfCarrying out fluid volume conversion to obtain a fluid volume Vf＝0.12cm3. The microcrack volume fraction V is 0.12/19.31 x 100 is 0.62%.
Example 12
Compared to example 11, a microcrack control factor analysis was also included:
the micro-cracks and rock components (internal factors) are analyzed at this time, and the leading factors influencing the micro-crack development are obtained. The mineral content, lithology and the like of the micro-cracks are analyzed, and specific results are shown in fig. 8 and fig. 9, wherein fig. 8 is a linear relation graph of the total content of quartz and feldspar and the micro-cracks, and fig. 9 is a linear relation graph of the total content of calcite and dolomite and the micro-cracks. Fig. 8 shows that the signal quantity in the fracture is positively correlated with quartz and feldspar, and fig. 9 shows that the signal quantity in the fracture is negatively correlated with calcite and dolomite, because the filling of the calcite and the dolomite in the fracture causes the signal quantity to be weakened.
Example 13
The procedure of example 8 was repeated except that the temperature at which the oil-washed sample was placed in a vacuum oven and dried was set to 60 ℃ and the drying time was set to 12 hours, as compared with example 8.
Example 14
The procedure of example 8 was repeated except that the temperature at which the oil-washed sample was placed in a vacuum oven and dried was set to 70 ℃ and the drying time was set to 6 hours, as compared with example 8.
Example 15
The same procedure as in example 8 was repeated, except that the solvent for washing the oil was a mixed organic solvent of methylene chloride and acetone at a volume ratio of 1:1 as compared with example 8.
Example 16
The method is the same as example 8 except that the solvent for washing the oil is a mixed organic solvent of dichloromethane and acetone in a volume ratio of 5:1 compared with example 8.
Example 17
The procedure of example 8 was repeated, except that the sample chamber and the throat of the rock sample were evacuated to a relative vacuum of 70kPa for 24 hours, as compared with example 8.
Example 18
The procedure of example 8 was repeated, except that the sample chamber and the throat of the rock sample were evacuated to a relative vacuum of 80kPa for 12 hours, as compared with example 8.
Example 19
The procedure was carried out in the same manner as in example 8 except that the pressure was kept at about 12MPa and the saturation time was 48 hours when n-dodecane was injected into the sample chamber, as compared with example 8.
Example 20
The procedure was carried out in the same manner as in example 8 except that the pressure was kept at about 17MPa and the saturation time was 24 hours when n-dodecane was injected into the sample chamber, as compared with example 8.
The invention researches shale microcracks by using a nuclear magnetic resonance technology, wherein the microcracks are important pore types of shale, a good seepage network can be formed so as to improve the reservoir quality, and quantitative research on the microcracks is beneficial to understanding the shale reservoir type and exploration potential evaluation. The shale reservoir type and exploration potential evaluation problem is known aiming at improving the reservoir quality through the microcracks. The method takes a nuclear magnetic resonance technology as a technical means, and judges the shale microcracks on the basis of representing the size of the micro pore size by the combination of low-temperature nitrogen adsorption and nuclear magnetic resonance. And the quantitative characterization is carried out by applying Gaussian fitting, and the microcrack factor control analysis is carried out at the same time, so that the method has important significance for the exploration and development of the shale oil.
While the preferred embodiments of the present invention have been described in detail, the present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the scope of the invention.
Claims (7)
1. The shale microcrack evaluation method is characterized in that the shale microcrack evaluation method comprises the steps of washing oil and drying shale to be evaluated to obtain a dry sample, performing a nuclear magnetic resonance experiment on the dry sample in the process of vacuumizing and pressurizing saturated oil, jointly representing the size of a microscopic aperture by combining low-temperature nitrogen adsorption to judge shale microcracks, quantitatively representing by applying Gaussian fitting, and simultaneously performing microcrack control factor analysis;
in the shale microcrack evaluation method, the quantitative characterization by using Gaussian fitting specifically comprises the steps of performing nuclear magnetic resonance test according to a dry sample after a process of vacuumizing and pressurizing saturated oil, calibrating a nuclear magnetic resonance relaxation-pore diameter conversion coefficient according to a result of low-temperature nitrogen adsorption joint characterization, and performing Gaussian fitting on a main peak in nuclear magnetic resonance, wherein an initial signal quantity of free fluid in the main peak in the nuclear magnetic resonance test is recorded as A0, and a signal quantity after the Gaussian fitting is recorded as A1, so that the signal quantity Af of the free fluid in the microcrack is = A0-A1;
the gaussian fitting process is performed according to the following formula:
X=A×EXP(-(((log(C×M)-a)/b)2))
wherein A is a nuclear magnetic resonance T2 spectrum semaphore peak; c is the NMR relaxation-pore diameter conversion coefficient; a is a peak value of a central axis corresponding to a main peak of a nuclear magnetic resonance T2 spectrum; b is the nuclear magnetic resonance main peak T2 spectral width; m is the nuclear magnetic resonance T2 spectral semaphore at different times;
the nuclear magnetic resonance relaxation-aperture conversion coefficient is performed according to the following formula:
C=Amax/Bmax
wherein Amax is the maximum value corresponding to the main peak in the nuclear magnetic resonance T2 spectrum, Bmax is the maximum value corresponding to the adsorption capacity in low-temperature nitrogen adsorption, and C is the nuclear magnetic resonance relaxation-aperture conversion coefficient.
2. The shale microcrack evaluation method according to claim 1, wherein in the shale microcrack evaluation method, the oil washing and drying is to wash the shale to be evaluated by a Soxhlet extraction method or an ultrasonic method so as to remove residual oil in pores, and then the sample after oil washing is subjected to vacuum drying at the temperature of 60-70 ℃ for 6-12 h.
3. The shale microcrack evaluation method of claim 2, wherein the solvent of the wash oil is a mixed organic solvent of dichloromethane and acetone, wherein the volume ratio of dichloromethane to acetone is 3: 1.
4. The shale microcrack evaluation method according to claim 1, wherein in the shale microcrack evaluation method, the dry sample is subjected to a nuclear magnetic resonance experiment in a vacuumizing and pressurizing saturated oil process, and the characterization of the microscopic pore size by combining with low-temperature nitrogen adsorption specifically comprises the following steps: and performing nuclear magnetic resonance test on the dry sample before vacuumizing and pressurizing the saturated oil, and performing nuclear magnetic resonance test on the dry sample after vacuumizing and pressurizing the saturated oil.
5. The shale microcrack evaluation method according to claim 1, wherein in the shale microcrack evaluation method, the step of vacuumizing and pressurizing the dry sample to saturate oil is to vacuumize the dry sample and exhaust air in a pore throat, and then inject the saturated oil, wherein the pressure is kept between 12 and 17MPa, and the saturation time is between 24 and 48 hours.
6. The shale microcrack evaluation method according to claim 5, wherein in the shale microcrack evaluation method, the dry sample is vacuumized to exhaust air in the pore throat, and the relative vacuum degree is particularly vacuumized to 70-80kPa for 12-24 h.
7. Use of the shale microcrack evaluation method according to any one of claims 1 to 6 in shale oil exploration and development.
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