CN115856267B - Method for analyzing properties of shale oil in different connectivity pores of shale and application - Google Patents

Method for analyzing properties of shale oil in different connectivity pores of shale and application Download PDF

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CN115856267B
CN115856267B CN202310155501.6A CN202310155501A CN115856267B CN 115856267 B CN115856267 B CN 115856267B CN 202310155501 A CN202310155501 A CN 202310155501A CN 115856267 B CN115856267 B CN 115856267B
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shale
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crushed particles
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oil
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CN115856267A (en
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窦立荣
张婧雅
朱如凯
刘畅
白斌
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Petrochina Co Ltd
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Abstract

The invention discloses a property analysis method and application of shale oil in different connectivity pores of shale, wherein the method can comprise the following steps: sequentially preparing shale crushed particles with different particle sizes; extracting the shale crushed particles step by step, and performing geochemical analysis on the extract to obtain geochemical analysis results of the shale crushed particles with different connectivity pores; and analyzing shale oil properties in different connectivity pores of the shale based on the geochemical analysis result. The method utilizes macroscopic geologic samples to explore the property difference of microfluidics in a shale pore system, can provide an effective technical means for finely representing the microscopic occurrence state of shale oil and clarifying the microscopic occurrence mechanism of the shale oil, and provides a reliable basis for optimizing subsequent shale oil reservoir desserts and selecting favorable targets.

Description

Method for analyzing properties of shale oil in different connectivity pores of shale and application
Technical Field
The invention relates to the technical field of unconventional oil and gas exploration and reservoir evaluation, in particular to a shale oil property analysis method and application in different connectivity pores of shale.
Background
Shale oil layer has high organic carbon content and strong reservoir heterogeneity, and generally presents enrichment characteristics of autogenous and source storage. The shale reservoir has smaller pore throats, taking the shale with a Qingshan group as an example, the effective porosity is mainly 3.0% -11.0%, the median value is 5.7%, the permeability is more smaller than 0.1mD, the pore structure is complex, the pore space is mainly composed of nano micropores-micropores, more than 80%, most of the pore space is smaller than 50nm, the average pore throats are 6.7-13.5 nm, and the coordination number of the pore throats is generally smaller than 0.1, so that the connectivity among the pores is poor. The microscopic occurrence characteristic difference of petroleum in the shale reservoir is obvious, under the actions of shale hydrocarbon generation and discharge and petroleum micro-migration, strong polar hydrocarbon is preferentially adsorbed by kerogen and occupies in-situ pores, and weak polar hydrocarbon (saturated hydrocarbon and aromatic hydrocarbon) can be more easily discharged into shale inorganic pores, so that shale oil components and properties in pores with different types, pore sizes and connectivity inside the shale reservoir are different. However, since the shale has very small micro-pore space, the property differences of crude oil in the micro-nano pores cannot be observed by conventional means.
Disclosure of Invention
The inventor finds that partial scholars can characterize the contents of shale oil (such as free oil, adsorbed oil and residual oil) in different occurrence states by carrying out step-by-step extraction on shale samples with different particle sizes, but the step-by-step relay extraction is not carried out on the shale samples before, and the geochemical characteristics of soluble organic matters of the shale samples are not comprehensively analyzed, so that the differences of shale oil components and maturity in pores with different connectivity cannot be judged, and finally the shale pores cannot be effectively related to the shale oil components and the shale oil maturity, and the differences of shale oil properties in the pores with different connectivity cannot be accurately evaluated. In view of the above, the present invention has been made to provide a method and application of analyzing properties of shale oil in shale different connectivity pores which overcomes or at least partially solves the above-mentioned problems.
In a first aspect, an embodiment of the present invention provides a method for analyzing shale oil properties in pores with different connectivity of shale, which may include:
sequentially preparing shale crushed particles with different particle sizes;
extracting the shale crushed particles step by step, and performing geochemical analysis on the extract to obtain geochemical analysis results of the shale crushed particles with different connectivity pores;
and analyzing shale oil properties in different connectivity pores of the shale based on the geochemical analysis result.
Optionally, the method specifically includes:
crushing the obtained internal shale sample which is not polluted by the drilling fluid, and sieving the crushed internal shale sample by using a 2.5-5 mesh sieve to obtain 2.5-5 mesh shale crushed particles; extracting the 2.5-5-mesh shale crushed particles by using a polar organic solvent, and carrying out joint geochemical analysis on the extract to obtain a first geochemical analysis result;
intermittently crushing the extracted shale crushed particles, and sieving the crushed shale particles by using a 10-20 mesh sieve to obtain 10-20 mesh shale crushed particles; extracting the 10-20-mesh shale crushed particles by using a polar organic solvent, and carrying out combined geochemical analysis on the extract to obtain a second geochemical analysis result;
intermittently crushing the extracted shale crushed particles, and sieving the crushed shale particles by using a 60-100 mesh sieve to obtain 60-100 mesh shale crushed particles; extracting the 60-100 mesh shale crushed particles by using a polar organic solvent, and carrying out combined geochemical analysis on the extract to obtain a third geochemical analysis result;
intermittently crushing the extracted shale crushed particles, and sieving the crushed shale crushed particles by using a sieve with a mesh size larger than 150 meshes to obtain shale crushed particles with a particle size smaller than 150 meshes; extracting the shale crushed particles smaller than 150 meshes by using a polar organic solvent, and carrying out combined geochemical analysis on the extract to obtain a fourth geochemical analysis result;
and comparing and analyzing the first geochemical analysis result, the second geochemical analysis result, the third geochemical analysis result and the fourth geochemical analysis result to obtain shale oil components and maturity differences in different connectivity pores.
Optionally, the polar organic solvent includes: n-hexane solvent, dichloromethane solvent, chloroform solvent or a mixed solvent of dichloromethane and methanol.
Optionally, the polar organic solvent is a dichloromethane solvent.
Alternatively, the combined geochemical analysis may comprise: quantitative analysis of soluble organic components, full hydrocarbon gas chromatography, adamantane dual mass spectrometry, saturated hydrocarbon chromatography mass spectrometry, and aromatic hydrocarbon chromatography mass spectrometry.
Alternatively, the extraction time is 72 hours.
Optionally, the weight of the prepared shale crushed particles with the size of 2.5-5 meshes is not less than 100g.
Optionally, before crushing the obtained shale sample, the method may further include: the skin of the acquired shale sample is stripped to obtain a core part which is not polluted by drilling fluid.
In a second aspect, the embodiment of the invention provides an application of the shale oil composition and maturity difference in the pores with different connectivity obtained by the shale oil property analysis method in the pores with different connectivity in the shale according to the first aspect in shale oil reservoir dessert optimization.
In a third aspect, embodiments of the present invention provide a shale oil reservoir sweet spot optimization method, which may include:
the composition and maturity differences of shale oil in the pores of different connectivity obtained by the method for analyzing the properties of shale oil in the pores of different connectivity according to the first aspect are taken as the basis for reservoir dessert preference.
The technical scheme provided by the embodiment of the invention has the beneficial effects that at least:
the embodiment of the invention provides a method for analyzing the properties of shale oil in different connectivity pores of shale and application thereof, wherein the method utilizes a macroscopic geological sample to explore the property difference of microfluidics in a shale pore system, can provide an effective technical means for finely representing the microscopic occurrence state of the shale oil and clarifying the microscopic occurrence mechanism of the shale oil, and provides a reliable basis for optimizing and selecting favorable targets of subsequent shale oil reservoir desserts.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention may be realized and attained by the structure particularly pointed out in the written description and drawings.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate the invention and together with the embodiments of the invention, serve to explain the invention. In the drawings:
FIG. 1 is a flow chart of a method for analyzing properties of shale oil in different connectivity pores of shale provided in an embodiment of the invention;
FIG. 2 is a detailed flow chart of a method for analyzing properties of shale oil in different connectivity pores of shale provided in an embodiment of the invention;
FIG. 3 is a detailed flow chart of a method for analyzing properties of shale oil in different connectivity pores of another shale provided in an embodiment of the invention;
FIG. 4 is a graph of saturated hydrocarbon chromatograms of shale extracts of different particle sizes provided in an embodiment of the present invention;
fig. 5 is a graph of the methyl diamantane dual mass spectrum of shale extracts of different particle sizes provided in an embodiment of the present invention.
Detailed Description
Exemplary embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings. While exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the present disclosure may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.
The embodiment of the invention provides a method for analyzing properties of shale oil in pores with different connectivity of shale, and referring to fig. 1, the method can comprise the following steps:
and S11, sequentially preparing shale crushed particles with different connectivity pores.
The method comprises the steps of sequentially and gradually crushing the obtained fresh shale samples, and extracting crushed shale particles in the step S12, wherein the crushed shale particles are continuously crushed again after the extraction is finished, so that the shale crushed particles with different connectivity pores are sequentially prepared. In the embodiment of the invention, the prepared shale crushing particles are crushed step by step and step-relay extracted step by step aiming at the same shale sample, so as to realize the judgment of the shale oil components and maturity differences in different connectivity pores. According to the embodiment of the invention, the inventors can represent the contribution of different connectivity pores aiming at shale particles with different particle sizes, and the finer the shale is crushed, the smaller the particle size of the shale particles is, so that more pores with poor connectivity are exposed, and therefore the extract can represent the property of shale oil in the pores with poor connectivity more.
Step S12, extracting the shale crushed particles step by step, and performing geochemical analysis on the extract to obtain geochemical analysis results of the shale crushed particles with different connectivity pores.
In the step, the shale crushed particles are extracted by using a polar organic solvent to extract shale oil in different connectivity pores, and then the shale oil in the different connectivity pores is subjected to geochemical analysis, so that shale oil components and maturity in the different connectivity pores are obtained, and a foundation is laid for subsequent comparative analysis.
And S13, analyzing shale oil properties in different connectivity pores of the shale based on a geochemistry analysis result.
The method comprises the steps of comparing and analyzing shale oil components and maturity in different connectivity pores, further determining shale oil composition characteristic differences and maturity changes in pore spaces with different connectivity, and providing support for fine characterization of shale oil microscopic occurrence states and/or shale oil reservoir microscopic hydrocarbon difference enrichment mechanisms.
According to the method for analyzing the shale oil properties in the pores with different connectivity of the shale, provided by the embodiment of the invention, the micro-fluid property difference in the shale pore system is explored by utilizing the macroscopic geological sample, so that an effective technical means can be provided for finely representing the micro occurrence state of the shale oil and clarifying the micro occurrence mechanism of the shale oil, and a reliable basis is provided for optimizing subsequent shale oil reservoir desserts and selecting favorable targets.
The embodiment of the invention provides a detailed method for analyzing the properties of shale oil in different connectivity pores of shale, which is shown by referring to fig. 2 and 3, and specifically comprises the following steps:
and S20, stripping the skin of the acquired shale sample to obtain a core part which is not polluted by the drilling fluid.
In the step, the epidermis of the obtained shale sample is stripped, and a core part which is not polluted by the drilling fluid is taken, so that the influence of the drilling fluid on the geochemical analysis result is avoided.
And S21, crushing the obtained internal shale sample which is not polluted by the drilling fluid, and sieving the crushed shale sample by using a 2.5-5 mesh sieve to obtain shale crushed particles with the size of 2.5-5 meshes.
In the step, a core sample which is not polluted by drilling fluid is crushed, and in the concrete implementation, a geological hammer is used for crushing the core sample into particles with 2.5-5 meshes, and then a screen with 2.5-5 meshes is used for sieving, so that shale crushed particles with 2.5-5 meshes (4-8 mm) are obtained. In the embodiment of the invention, the same shale sample is crushed step by step and subjected to step-relay extraction, so that the weight of crushed particles of the shale with the particle size of 2.5-5 meshes prepared in the application is not less than 100g, and the problem that the error of a geochemical analysis result is overlarge because the total amount of the particles meeting the required particle size range in the subsequent crushing process is reduced step by step is avoided.
And S22, extracting the shale crushed particles with the particle size of 2.5-5 meshes by using a polar organic solvent, and carrying out joint geochemical analysis on the extract to obtain a first geochemical analysis result.
The polar organic solvent in the embodiment of the present invention may include: n-hexane solvent, dichloromethane solvent, chloroform solvent or a mixed solvent of dichloromethane and methanol. Wherein, in the mixed solvent of dichloromethane and methanol, dichloromethane is methanol=93:7, or dichloromethane is methanol=9:1. The inventor finds that the extraction requirement can be met because the dichloromethane solvent is nontoxic and because the polarity of the dichloromethane is relatively strong, and the polar organic solvent in the embodiment of the invention is preferably the dichloromethane solvent. In the embodiment, the extraction time of the inventor during extraction is 72 hours, so that the extraction requirement can be met, and shale oil in shale particles with different particle sizes can be fully extracted.
The above-described combined geochemical analysis in embodiments of the present invention may include: quantitative analysis of soluble organic components, full hydrocarbon gas chromatography, adamantane dual mass spectrometry, saturated hydrocarbon chromatography mass spectrometry, and aromatic hydrocarbon chromatography mass spectrometry.
And S23, intermittently crushing the extracted shale crushed particles, and sieving the crushed shale particles by using a 10-20-mesh screen to obtain the shale crushed particles with the mesh size of 10-20 (0.85-1.7 mm).
In the step and the subsequent steps, the extracted shale crushed particles are required to be crushed intermittently, and a crushing machine is used in crushing. The purpose of intermittent crushing firstly avoids volatilization of shale oil components (hydrocarbon is lost) caused by long-time crushing temperature rise, and secondly avoids direct crushing of shale samples into particles with smaller particle sizes, and too small total amount of the shale crushed particles with the required particle sizes can cause overlarge error of geochemical analysis results of the extract. Before intermittent crushing, the polar organic solvent used in extraction needs to be volatilized and crushed, so that errors caused by the organic solvent to the subsequent extraction result and geochemical analysis result are avoided.
And S24, extracting the shale crushed particles with the particle size of 10-20 meshes by using a polar organic solvent, and carrying out joint geochemical analysis on the extract to obtain a second geochemical analysis result.
And S25, intermittently crushing the extracted shale crushed particles, and sieving the crushed shale particles by using a 60-100-mesh screen to obtain 60-100-mesh (0.18-0.25 mm) shale crushed particles.
And S26, extracting the shale crushed particles with 60-100 meshes by using a polar organic solvent, and carrying out joint geochemical analysis on the extract to obtain a third geochemical analysis result.
And step S27, crushing the extracted shale crushed particles, and sieving the crushed shale particles by using a 150-mesh sieve to obtain shale crushed particles with the particle size smaller than 150 meshes (< 0.106 mm).
And S28, extracting the shale crushed particles with the particle size smaller than 150 meshes by using a polar organic solvent, and carrying out combined geochemical analysis on the extract to obtain a fourth geochemical analysis result.
The crushing conditions in the present step S25 and step S27 are intermittent crushing, and the purpose is the same as in the step S23. The polar organic solvents in the steps S24, S26 and S28 are the same as those in the step S22, the extraction conditions and the extraction time are the same as those in the step S22, and the means for the combined geochemical analysis of the extracts are the same.
And S29, comparing and analyzing the first geochemical analysis result, the second geochemical analysis result, the third geochemical analysis result and the fourth geochemical analysis result to obtain shale oil components and maturity differences in different connectivity pores.
In the step, the analysis of group component quantification, full hydrocarbon gas chromatography and saturated hydrocarbon gas chromatography mass spectrum is carried out on the extracted soluble organic matters, the relative contents of saturated hydrocarbon, aromatic hydrocarbon, non-hydrocarbon and asphaltene of shale extracts with different particle sizes, the spectrogram characteristics of full hydrocarbon gas chromatography and the main peak carbon shift phenomenon are compared, and the component difference of shale oil in pores with different connectivity is analyzed. By subjecting the extracted soluble organic matter to saturated hydrocarbon gas chromatography mass spectrometry, aromatic hydrocarbon gas chromatography mass spectrometry and adamantane dual mass spectrometry, the maturity parameters (such as Ts/Tm and Ts/C) of biomarker compounds of extracts with different particle diameters are compared 30 17 alpha-hopanadine) and adamantane maturity parameters (e.g., methyl Diamantane Index (MDI), 4-methyl diamantane/3-methyl diamantane (4-MD/3-MD) and 4, 9-dimethyl diamantane/3, 4-dimethyl diamantane (4, 9-DMD/3, 4-DMD)), define their rules of variation, thereby elucidating the differences in maturity of shale oil in different connectivity pores.
It should be noted that the quantitative analysis of the group components in the embodiment of the invention can be performed according to the standard SY/T5119-2008 "analysis of soluble organic matters in rock and crude oil group components"; the full hydrocarbon gas chromatographic analysis can be carried out by adopting an Agilent 7890A gas chromatograph, and the specific operation and flow are carried out according to the standard SY/T5779-2008 Petroleum and deposited organic hydrocarbon gas chromatographic analysis method; the analysis of adamantane double mass spectrum can be carried out by adopting a TSQ8000Evo gas chromatography triple quadrupole mass spectrometer, and specific operation and flow are carried out according to the standard SY/T7470-2020 quantitative analysis method of adamantane compounds in crude oil; the analysis of saturated hydrocarbon and aromatic hydrocarbon gas chromatography mass spectrum adopts an Agilent 7890-5975C gas chromatography mass spectrometer for analysis, and specific operation and flow are carried out according to the standard GB/T18606-2017 gas chromatography mass spectrometry for determining sediment and biomarkers in crude oil.
According to the method for analyzing the shale oil properties in the pores with different connectivity in the shale, provided by the embodiment of the invention, the micro-fluid property difference in the shale pore system is explored by utilizing the macroscopic geological sample, so that an effective technical means can be provided for finely representing the micro occurrence state of the shale oil and clarifying the micro occurrence mechanism of the shale oil, and a reliable basis is provided for optimizing and selecting favorable targets of subsequent shale oil reservoirs.
In order to more clearly and in detail describe the method for analyzing the shale oil properties in the pores with different connectivity in the shale provided by the embodiment of the invention, so as to analyze the shale oil components and the maturity difference in the micropores with different connectivity in the shale reservoir, the embodiment of the invention is further described in detail below with reference to an application example.
The application example is Qingshan kou group shale, and the development of pure shale type medium and high-grade shale oil is an important shale oil production layer. The specific implementation method is as follows:
the experimental procedure is presented as follows:
(1) Selecting a blocky shale sample of a Qingshan mouth group, removing the outer surface of the blocky shale sample, taking a part of the interior of the blocky shale sample which is not polluted by drilling fluid, knocking the blocky shale sample into more than 100g of 2.5-5-mesh particle samples by using a geological hammer, continuously extracting the 2.5-5-mesh particle samples for 72 hours by using a dichloromethane organic solvent, and collecting soluble organic matters for geochemical analysis such as group component quantification, full hydrocarbon gas chromatography, adamantane dual-mass spectrometry, saturated hydrocarbon gas chromatography mass spectrometry, aromatic hydrocarbon gas chromatography mass spectrometry and the like;
(2) Continuously crushing the 2.5-5-mesh particle sample obtained after the extraction of the dichloromethane in the step (1) into 10-20-mesh shale particles, continuously extracting for 72 hours by using the dichloromethane, and collecting soluble organic matters for carrying out geochemical analysis such as group component quantification, full hydrocarbon gas chromatography, adamantane dual-mass spectrometry, saturated hydrocarbon gas chromatography mass spectrometry, aromatic hydrocarbon gas chromatography mass spectrometry and the like;
(3) Continuously crushing the 10-20-mesh particle sample obtained after the extraction of the dichloromethane in the step (2) into 60-80-mesh shale particles, continuously extracting for 72 hours by using the dichloromethane, and collecting soluble organic matters for geochemical analysis such as group component quantification, full hydrocarbon gas chromatography, adamantane dual-mass spectrometry, saturated hydrocarbon gas chromatography mass spectrometry, aromatic hydrocarbon gas chromatography mass spectrometry and the like;
(4) Continuously crushing the 60-80-mesh particle sample obtained after the extraction of the dichloromethane in the step (3) into shale particles with the particle size of less than 150 meshes, continuously extracting for 72 hours by using the dichloromethane, and collecting soluble organic matters for geochemical analysis such as group component quantification, full hydrocarbon gas chromatography, adamantane dual-mass spectrometry, saturated hydrocarbon gas chromatography mass spectrometry, aromatic hydrocarbon gas chromatography mass spectrometry and the like.
The shale oil composition differential analysis in the different connectivity pores is as follows:
group component quantification and full hydrocarbon chromatographic analysis are carried out on the stepwise-relay extracts of the different-particle-size particles of the two shale samples in the Qingshan kou group, and the test results are shown in the petroleum group component characteristic tables of the different-particle-size extracts of the shale samples in the figure 4 and the table 1.
TABLE 1 Petroleum family Components characterization Table of extracts of shale samples of different particle sizes
Figure SMS_1
Note that: * Representing a small sample size, data for reference, representing undetected or invalid data
The analysis showed that the percentage of saturated hydrocarbons in the extract gradually decreased and the percentage of aromatic hydrocarbons, non-hydrocarbons and asphaltenes gradually increased as the particle size of the sample was gradually reduced. Taking a 129 # sample as an example, when the particle size of the sample is 2.5-5 meshes, the percentage contents of saturated hydrocarbon, aromatic hydrocarbon, non-hydrocarbon and asphaltene are 76.47%, 4.33%, 3.25% and 1.44% respectively; when (when)When the particle size of the sample is 10-20 meshes, the percentage contents of saturated hydrocarbon, aromatic hydrocarbon, non-hydrocarbon and asphaltene are 43.11%, 7.56%, 25.33% and 16.44% respectively; when the particle size of the sample is 60-100 meshes, the percentage contents of saturated hydrocarbon, aromatic hydrocarbon, non-hydrocarbon and asphaltene are 26.83%, 15.85%, 32.93% and 20.73% respectively; when the particle size of the sample<At 150 mesh, the sample quantity (extracted chloroform asphalt A content) is too small, and the sample quality is even smaller than the systematic error during weighing, so the data has no reference value. From the quantitative results of the group components, shale oil components in different connectivity pores have certain difference, the components of weak polar hydrocarbon in the pores with poor connectivity are relatively less, and the content of the polar hydrocarbon is relatively increased; the total ion flow diagrams of the full hydrocarbon gas chromatograph and the saturated hydrocarbon chromatin also show the component difference of the extracts with different particle diameters, and fig. 4 shows that the main peak carbon of the shale extract with 2.5-5 meshes is C 17 The main peak carbon of the shale extract with 10-20 meshes is C 20 The main peak carbon of the shale extract with 60-100 meshes is C 23 ,>The main peak carbon of the 150-mesh shale extract is C 26 That is, as the particle size of the shale sample gradually decreases, the main peak carbon of the extract gradually shifts to higher carbon numbers, indicating that the shale oil components in the pores with poor connectivity are relatively heavier.
The shale oil maturity differential analysis in the different connectivity pores is as follows:
biomarker compound and adamantane dual mass spectrometry analysis was performed on stepwise extracts of different particle sizes of two shale samples. The prior art studies show that, in the postnatal stage, C 27 17 alpha-trinitroalane (Tm) stability ratio C 27 18 alpha-trinexaold II (Ts) is inferior and validated by calculation of the molecular mechanisms of formation of different hopanes (including Ts and Tm) (Kolaczkowska et al, 1990), so that as the degree of thermal evolution of shale increases, the ratio of Ts/Tm increases accordingly; furthermore, volkman et al (1983) propose Ts/C 30 17 alpha-hopane can be used as a maturity parameter for high maturity crude oil and condensate because of C during high thermal evolution 29 Or C 30 Side chain cleavage of 17α -hopanane can produce Ts, thus as maturity increases, ts/C 30 17 alpha-hopananeAnd the ratio of (c) will increase accordingly. Saturated hydrocarbon chromatographic mass spectrometry analysis results of the Qingshan kou shale show (Table 1) that as the particle size of the sample is gradually reduced, the ratio of Ts/Tm and Ts/C 30 The 17 alpha-hopane ratio has a tendency to become progressively greater, indicating that the shale oil in the poorly connected pores is of relatively higher maturity.
Because the shale oil has overall higher maturity, some common biomarker parameters indicative of maturity, such as C 29 Stanes 20S/(20S+20R) and C 29 The stanes beta/(alpha + beta) have failed. Besides the biomarker compound index can be used for researching the maturity of raw oil rock and petroleum, adamantane is more stable than other hydrocarbons in the geological evolution process, has strong heat resistance and biodegradability resistance, and can be used as an important index of the maturity. The adamantane compounds at different methyl substituent positions have different thermal stability, and the substituent is transferred from a relatively unstable position to a relatively stable position under the action of heat. The fractional extractives of the two shale samples with different particle sizes in the Qingshan oral group are subjected to adamantane dual mass spectrometry, and the result is shown in the maturity parameter characteristic table of the shale samples with different particle sizes in fig. 5 and table 2, wherein the ratio of the Methyl Diamantane Index (MDI), 4-methyl diamantane/3-methyl diamantane (4-MD/3-MD) and 4, 9-dimethyl diamantane/3, 4-dimethyl diamantane (4, 9-DMD/3, 4-DMD) of the extractives shows a gradually increasing trend along with the gradual decrease of the particle sizes of the shale particles, and the fact that the maturity of shale oil in pores with poor connectivity is relatively higher is also proved.
TABLE 2 maturity parameter characterization of extracts of shale samples of different particle sizes
Figure SMS_2
Note that: representing undetected or data invalidation
Wherein, parameters such as Methyl Diamantane Index (MDI), 4-MD/3-MD, 4,9-DMD/3,4-DMD and the like are calculated from adamantane dual mass spectrum, and Ts/Tm and Ts/17 alpha-H are calculated from saturated hydrocarbon gas chromatography mass spectrum.
Based on the same inventive concept, the embodiment of the invention also provides an application of the shale oil composition and maturity difference in different connectivity pores obtained by the shale oil property analysis method in different connectivity pores in shale oil reservoir dessert optimization.
Based on the same inventive concept, the embodiment of the invention also provides a shale oil reservoir dessert optimization method, which can comprise the following steps:
the shale oil components and maturity differences in different connectivity pores obtained according to the shale oil property analysis method in different connectivity pores of the shale are used as the basis for reservoir dessert optimization.
The above application and the preferred method of shale oil reservoir dessert in the embodiment of the present invention may refer to the above method for analyzing properties of shale oil in different connectivity pores of shale, and the embodiment of the present invention is not described herein again.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.

Claims (7)

1. A method for analyzing properties of shale oil in different connectivity pores of shale, comprising:
step-by-step crushing and step-by-step relay extraction are carried out on the same shale sample, so that shale crushed particles with different particle sizes are sequentially prepared, and dichloromethane solvent is used for extracting the shale crushed particles with different particle sizes step by step; wherein, the particle diameter of shale crushing particulate matters with different particle diameters is as follows: 2.5-5 mesh, 10-20 mesh, 60-100 mesh and less than 150 mesh;
respectively carrying out quantitative analysis of group components and/or gas chromatography analysis of all hydrocarbon on the extract to obtain components of shale oil in different connectivity pores of shale;
performing adamantane dual-mass spectrometry, saturated hydrocarbon chromatography-mass spectrometry and/or aromatic hydrocarbon chromatography-mass spectrometry on the extract respectively to obtain the maturity of shale oil in different connectivity pores of shale;
the differences in properties of shale oil in its different connectivity pores are analyzed based on their composition and maturity.
2. The method according to claim 1, characterized in that it comprises in particular:
crushing the obtained internal shale sample which is not polluted by the drilling fluid, and sieving the crushed internal shale sample by using a 2.5-5 mesh sieve to obtain 2.5-5 mesh shale crushed particles; extracting the 2.5-5-mesh shale crushed particles by using a polar organic solvent, and carrying out joint geochemical analysis on the extract to obtain a first geochemical analysis result;
intermittently crushing the extracted shale crushed particles, and sieving the crushed shale particles by using a 10-20 mesh sieve to obtain 10-20 mesh shale crushed particles; extracting the 10-20-mesh shale crushed particles by using a polar organic solvent, and carrying out combined geochemical analysis on the extract to obtain a second geochemical analysis result;
intermittently crushing the extracted shale crushed particles, and sieving the crushed shale particles by using a 60-100 mesh sieve to obtain 60-100 mesh shale crushed particles; extracting the 60-100 mesh shale crushed particles by using a polar organic solvent, and carrying out combined geochemical analysis on the extract to obtain a third geochemical analysis result;
crushing the extracted shale crushed particles, and sieving the crushed shale crushed particles by using a 150-mesh sieve to obtain shale crushed particles with the particle size smaller than 150 meshes; extracting the shale crushed particles smaller than 150 meshes by using a polar organic solvent, and carrying out combined geochemical analysis on the extract to obtain a fourth geochemical analysis result;
comparing and analyzing the first geochemical analysis result, the second geochemical analysis result, the third geochemical analysis result and the fourth geochemical analysis result to obtain shale oil components and maturity differences in different connectivity pores;
wherein the joint geochemical analysis comprises: quantitative analysis of group components, gas chromatography of whole hydrocarbons, dual mass spectrometry of adamantane, mass spectrometry of saturated hydrocarbons and mass spectrometry of aromatic hydrocarbons.
3. The method according to claim 2, wherein the extraction time is 72 hours.
4. The method of claim 2, wherein the weight of the prepared shale crushed particles with the size of 2.5-5 meshes is not less than 100g.
5. The method of any one of claims 2-4, further comprising, prior to comminuting the acquired shale sample: the skin of the acquired shale sample is stripped to obtain a core part which is not polluted by drilling fluid.
6. Use of shale oil composition and maturity differences in different connectivity pores obtained by the shale oil property analysis method in shale different connectivity pores according to any one of claims 1-5 in shale oil reservoir dessert optimization.
7. A shale oil reservoir dessert optimization method, comprising:
the method for analyzing the properties of shale oil in different connectivity pores of shale according to any one of claims 1-5, wherein the difference in shale oil components and maturity in different connectivity pores is obtained as a basis for reservoir dessert optimization.
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