Rapid detection method and device for multiple features of mud shale movable oil
Through laser confocal microscopy and gas chromatography analysis technology, the problem of long detection cycle and insufficient information in mud shale is solved, and fast and accurate detection of movable oil characteristics is achieved, supporting drilling tracking and development plan preparation.
Patent Information
- Application Number
- CN202310745698.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2023-06-21
- Publication Date
- 2024-12-24
AI Technical Summary
The prior art is difficult to quickly and accurately detect the presence status, carbon number distribution range and content of each component of movable oil in mud shale, resulting in low exploration and development efficiency and long detection cycles.
The rock sheet was scanned twice by laser confocal microscope, combined with organic solvent flushing and gas chromatography analysis, and obtained the movable oil content, carbon number range and component content, and generated a submicron-level high-resolution movable oil distribution image. .
It achieves rapid and accurate acquisition of movable oil content and carbon number range, shortens the detection cycle, and provides technical support for drilling tracking, mud shale quality evaluation and development plan preparation.
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Figure CN119178763A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of petroleum exploration and development, and in particular relates to a method and a device for quickly detecting multiple characteristics of movable oil in shale. Background Art
[0002] Shale oil is a non-gaseous hydrocarbon that exists in the effective hydrocarbon-generating shale formation in various forms such as free, adsorbed and dissolved, and has exploration and development significance. Research on shale reservoir evaluation mostly focuses on the acquisition of parameters such as porosity, permeability, and oil saturation. However, the density of shale reservoirs limits the flow of oil in them. Even if the parameters such as porosity and oil saturation are clarified, only reserve data can be obtained, and further recoverable reserve data cannot be obtained. Therefore, for shale, it is more important to determine the movable oil content, which is the bottleneck factor restricting its exploration and development results. At the same time, it is also necessary to clarify the occurrence state of movable oil, the carbon number distribution range, and the content of each carbon number group component, so that a targeted development plan can be established and the expected economic benefits can be evaluated. The main methods for detecting the oil content of shale oil are geochemical methods, including organic solvent extraction, pyrolysis, and the drilling site step-by-step thermal hydrocarbon release method developed in recent years. These methods can obtain the movable oil content, but cannot characterize the occurrence state of the movable oil; and the detection cycle of the geochemical method is relatively long. The prior art also discloses a method for detecting the components and content of organic matter in mudstone. This method scans the sample through a two-photon laser confocal microscope, distinguishes light, heavy and kerogen components through the spectral characteristics of organic matter of different components, and characterizes their spatial distribution. This method clarifies the fluorescence characteristics of organic components under a two-photon laser confocal microscope, and can quantify and characterize the occurrence state of light, heavy and kerogen components, but cannot determine the mobility, movable amount and movable oil carbon number range of crude oil. Summary of the invention
[0003] In order to overcome the defects of the above-mentioned prior art, the purpose of the present invention is to provide a rapid detection method for multiple characteristics of movable oil in mud shale, using the core or well wall coring obtained from the mud shale reservoir coring well to analyze its movable oil occurrence state, and obtain the movable oil content and movable oil carbon number range. This method can effectively shorten the movable oil content detection cycle, and at the same time can obtain submicron high-resolution movable oil distribution three-dimensional image, movable oil pore number distribution map, movable oil pore volume distribution map, and evaluate the movable oil carbon number range and the content of each component. It can provide technical support for drilling tracking, real-time evaluation of mud shale quality, development plan preparation, economic benefit evaluation, etc.
[0004] To achieve the above object, the present invention provides the following technical solutions:
[0005] A rapid detection method for multiple characteristics of movable oil in shale, including:
[0006] sampling and preparing thin sections of rocks;
[0007] Select the test area of the rock thin section and take microscopic photos;
[0008] Performing a first scan of the detection area using a laser confocal microscope to obtain a first crude oil three-dimensional distribution image data volume;
[0009] The rock thin section after the first scan is rinsed with an organic solvent and the rinse liquid is collected;
[0010] A laser confocal microscope is used to scan the detection area of the washed rock slice for a second time to obtain a second crude oil three-dimensional distribution image data volume;
[0011] Obtaining movable oil content through the first crude oil three-dimensional distribution image data volume and the second crude oil three-dimensional distribution image data volume;
[0012] The flushing liquid was analyzed by gas chromatography to obtain the movable oil carbon number range and the content of each component.
[0013] Further, sampling and preparation of rock thin sections include:
[0014] When the core is out of the barrel, samples are taken and sealed for storage.
[0015] The samples were sliced and polished to obtain rock thin sections.
[0016] Furthermore, the sample is a block core, and the sample mass is 20-50g.
[0017] Furthermore, the rock thin sections were polished on both sides without cover glass.
[0018] Furthermore, the detection area of the rock slice is selected and microscopic photos are taken, including:
[0019] The rock thin section is placed under a fluorescence microscope and excited with ultraviolet light to observe the fluorescence characteristics of the rock and record the observation characteristics of the rock thin section, including fluorescence color, luminous intensity and crude oil distribution characteristics.
[0020] Further, a first scan of the detection area is performed using a laser confocal microscope, comprising:
[0021] The laser confocal microscope uses 488nm laser as excitation light and receives excitation fluorescence in the range of 489nm-700nm as crude oil signal.
[0022] Further, a laser confocal microscope is used to perform a first scan on the detection area, comprising:
[0023] The scanning resolution and scanning speed of the laser confocal microscope are adjusted according to the requirements of the scanning effect, and other parameters required for scanning are adjusted according to the observation characteristics of the rock thin section.
[0024] Further, a first scan of the detection area is performed using a laser confocal microscope, comprising:
[0025] The three-dimensional scanning range of the laser confocal microscope takes the absence of excitation light upward and downward from the objective lens as the scanning start and end points, and the scanning step length is 0.1-1 μm.
[0026] Further, the rock slice after the first scan is washed with an organic solvent and the washing liquid is collected, including:
[0027] The rock slices after the first scan are spot-washed with organic solvent to wash out the movable oil.
[0028] Furthermore, the amount of the organic solvent used is 2-10 ml.
[0029] Further, after washing the rock slice after the first scan with an organic solvent and collecting the washing liquid, the following steps are performed:
[0030] The washed rock slices were dried and scanned a second time.
[0031] Furthermore, the scanning parameters of the second scanning are the same as those of the first scanning.
[0032] Further, obtaining the movable oil content through the first crude oil three-dimensional distribution image data volume and the second crude oil three-dimensional distribution image data volume includes:
[0033] subtracting the second crude oil three-dimensional distribution image data volume from the first crude oil three-dimensional distribution image data volume to obtain a movable oil three-dimensional distribution image data volume;
[0034] The volume percentage of the movable oil signal of the movable oil three-dimensional distribution image data volume is calculated, wherein the volume percentage of the movable oil signal is the movable oil content.
[0035] On the other hand, the present invention also discloses a rapid detection device for multiple characteristics of movable oil in shale, comprising:
[0036] A rock thin section preparation unit, used for preparing rock thin sections;
[0037] A detection area selection unit is used to select the detection area of the rock slice and take a microscopic photograph;
[0038] A scanning unit, used for performing a first scan and a second scan on the rock slice to obtain a first crude oil three-dimensional distribution image data volume and a second crude oil three-dimensional distribution image data volume;
[0039] A flushing unit, used to flush the rock slice after the first scan and collect the flushing fluid;
[0040] A data processing unit, used for obtaining movable oil content through the first crude oil three-dimensional distribution image data volume and the second crude oil three-dimensional distribution image data volume;
[0041] The movable oil carbon number detection unit is used to perform gas chromatography analysis on the flushing liquid to obtain the movable oil carbon number range and the content of each component.
[0042] Furthermore, the rock thin sections were polished on both sides without cover glass.
[0043] Furthermore, the detection area selection unit includes an ultraviolet microscope, which uses ultraviolet light to excite rock slices. The ultraviolet microscope is used to observe rock fluorescence characteristics of the rock slices and record their observation characteristics, and the observation characteristics include fluorescence color, luminous intensity and crude oil distribution characteristics.
[0044] Furthermore, the scanning unit includes a laser confocal microscope, which uses a 488nm laser as excitation light and receives excitation fluorescence in the range of 489nm-700nm as a crude oil signal.
[0045] Furthermore, the scanning resolution and scanning speed of the laser confocal microscope are adjusted according to the requirements of the scanning effect, and other parameters required for scanning are adjusted according to the fluorescence color, luminescence intensity, and crude oil distribution characteristics of the rock slice;
[0046] The three-dimensional scanning range of the laser confocal microscope takes the absence of excitation light upward and downward from the objective lens as the scanning start and end points, and the scanning step length is 0.1-1 μm.
[0047] Furthermore, the washing unit uses an organic solvent to wash the rock slice after the first scan, and the amount of the organic solvent used is 2-10 ml.
[0048] Furthermore, the data processing unit includes digital core analysis software for opening the first crude oil three-dimensional distribution image data volume and the second crude oil three-dimensional distribution image data volume.
[0049] Technical effects and advantages of the present invention:
[0050] 1. The present invention can use the cores or well wall cores obtained from the core wells of the shale reservoir to analyze the occurrence state of movable oil, determine the volume content of movable oil in the shale reservoir, the range of movable oil carbon numbers and the content of each component, obtain submicron-level high-resolution movable oil distribution three-dimensional images, movable oil pore quantity distribution maps, and movable oil pore volume distribution maps, and provide technical support for drilling tracking, real-time evaluation of shale quality, development plan preparation, economic benefit evaluation, etc.
[0051] 2. The whole process of sampling, film making and detection in the method of the present invention only takes a few hours, which effectively shortens the detection cycle of movable oil content and greatly improves the detection speed.
[0052] Other features and advantages of the present invention will be described in the following description, and partly become apparent from the description, or understood by practicing the present invention. The purpose and other advantages of the present invention can be realized and obtained by the structures pointed out in the description, claims and drawings. BRIEF DESCRIPTION OF THE DRAWINGS
[0053] Figure 1 This is a flow chart of a method for rapid detection of multiple characteristics of movable oil in shale according to the present invention;
[0054] Figure 2 A top view of a first crude oil three-dimensional distribution image data volume;
[0055] Figure 3 A top view of a second crude oil three-dimensional distribution image data volume;
[0056] Figure 4 It is the top view of the movable oil three-dimensional distribution image data volume;
[0057] Figure 5 It is a side view of the movable oil three-dimensional distribution image data volume;
[0058] Figure 6 is the pore quantity distribution diagram;
[0059] Figure 7 is the movable oil pore volume distribution diagram;
[0060] Figure 8 This is the gas chromatography analysis spectrum of the flushing liquid. DETAILED DESCRIPTION
[0061] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0062] like Figure 1 As shown, the present invention provides a method for rapid detection of multiple characteristics of movable oil in shale, including:
[0063] sampling and preparing thin sections of rocks;
[0064] Select the test area of the rock thin section and take microscopic photos;
[0065] Performing a first scan of the detection area using a laser confocal microscope to obtain a first crude oil three-dimensional distribution image data volume;
[0066] Washing the rock slice after the first scan with an organic solvent and collecting the washing liquid, wherein the organic solvent includes dichloromethane;
[0067] A laser confocal microscope is used to scan the detection area of the washed rock slice for a second time to obtain a second crude oil three-dimensional distribution image data volume;
[0068] Obtaining movable oil content through the first crude oil three-dimensional distribution image data volume and the second crude oil three-dimensional distribution image data volume;
[0069] The flushing liquid was analyzed by gas chromatography to obtain the movable oil carbon number range and the content of each component.
[0070] In some embodiments of the present invention, sampling and preparing rock thin sections includes:
[0071] When the core comes out of the barrel, samples are taken and sealed for storage. It is worth mentioning that samples need to be taken as soon as the core comes out of the barrel and rock thin sections need to be prepared as soon as possible.
[0072] In some embodiments of the present invention, the sample obtained by sampling is a block core, and the sample mass is 20-50g.
[0073] In some embodiments of the present invention, the rock slice is double-sided polished without a cover glass, and the thickness of the rock slice is adjusted according to the detection needs, for example, 0.05 mm.
[0074] In some embodiments of the present invention, selecting a detection area of a rock slice and taking a microscopic photograph comprises:
[0075] The rock thin section is placed under a fluorescence microscope and excited with ultraviolet light to observe the fluorescence characteristics of the rock and record the observation characteristics of the rock thin section, where the observation characteristics include fluorescence color, luminous intensity and crude oil distribution characteristics.
[0076] In some embodiments of the present invention, a first scan of the detection area is performed using a laser confocal microscope, comprising:
[0077] The laser confocal microscope uses 488nm laser as excitation light and receives excitation fluorescence in the range of 489nm-700nm as crude oil signal.
[0078] In some embodiments of the present invention, a first scan of the detection area is performed using a laser confocal microscope, comprising:
[0079] The scanning resolution and scanning speed of the laser confocal microscope were adjusted according to the requirements of the scanning effect. In view of the extremely small pores in the shale reservoir and the extremely small crude oil particles, the scanning resolution of the laser confocal microscope was set to the highest and the scanning speed to slow. Other parameters required for scanning were adjusted according to the observation characteristics of the rock thin sections to obtain the best scanning effect.
[0080] In some embodiments of the present invention, a first scan of the detection area is performed using a laser confocal microscope, comprising:
[0081] The three-dimensional scanning range of the laser confocal microscope takes the absence of excitation light upward and downward from the objective lens as the scanning start and end points, and the scanning step length is 0.1-1 μm.
[0082] In some embodiments of the present invention, washing the rock slice after the first scan with an organic solvent and collecting the washing liquid comprises:
[0083] The rock slices after the first scan are spot-washed with organic solvent to wash out the movable oil.
[0084] In some embodiments of the present invention, the amount of organic solvent used is 2-10 ml, and the amount of organic solvent used is based on completely washing out the movable oil in the rock slice.
[0085] In some embodiments of the present invention, after washing the rock slice after the first scan with an organic solvent and collecting the washing liquid, the method includes:
[0086] The washed rock slices were dried and scanned a second time.
[0087] In some embodiments of the present invention, the scanning parameters of the second scan are the same as those of the first scan.
[0088] In some embodiments of the present invention, obtaining the movable oil content through the first crude oil three-dimensional distribution image data volume and the second crude oil three-dimensional distribution image data volume includes:
[0089] Subtracting the second crude oil three-dimensional distribution image data volume from the first crude oil three-dimensional distribution image data volume to obtain a movable oil three-dimensional distribution image data volume;
[0090] The volume percentage of the movable oil signal of the movable oil three-dimensional distribution image data volume is calculated, wherein the volume percentage of the movable oil signal is the movable oil content.
[0091] On the other hand, the present invention also discloses a rapid detection device for multiple characteristics of movable oil in shale, comprising:
[0092] A rock thin section preparation unit, used for preparing rock thin sections;
[0093] A detection area selection unit is used to select the detection area of the rock slice and take a microscopic photograph;
[0094] A scanning unit, used for performing a first scan and a second scan on the rock slice to obtain a first crude oil three-dimensional distribution image data volume and a second crude oil three-dimensional distribution image data volume;
[0095] A flushing unit, used to flush the rock slice after the first scan and collect the flushing fluid;
[0096] A data processing unit, used for obtaining movable oil content through the first crude oil three-dimensional distribution image data volume and the second crude oil three-dimensional distribution image data volume;
[0097] The movable oil carbon number detection unit is used to perform gas chromatography analysis on the flushing liquid to obtain the movable oil carbon number range and the content of each component.
[0098] In some embodiments of the present invention, the rock slice is double-sided polished without a cover glass, and the thickness of the rock slice is adjusted according to the detection requirements, for example, 0.05 mm.
[0099] In some embodiments of the present invention, the detection area selection unit includes an ultraviolet microscope, which uses ultraviolet light to excite rock slices. The ultraviolet microscope is used to observe rock fluorescence characteristics of the rock slices and record their observation characteristics, and the observation characteristics include fluorescence color, luminous intensity and crude oil distribution characteristics.
[0100] In some embodiments of the present invention, the scanning unit includes a laser confocal microscope, which uses a 488nm laser as excitation light and receives excitation fluorescence in the range of 489nm-700nm as a crude oil signal.
[0101] In some embodiments of the present invention, the scanning resolution setting and scanning speed of the laser confocal microscope are adjusted according to the requirements of the scanning effect, and other parameter settings required for scanning are adjusted according to the observation characteristics of the rock slice;
[0102] The three-dimensional scanning range of the laser confocal microscope takes the absence of excitation light upward and downward from the objective lens as the scanning start and end points, and the scanning step length is 0.1-1 μm.
[0103] In some embodiments of the present invention, the flushing unit uses an organic solvent to flush the rock slice after the first scan, and the amount of the organic solvent used is 2-10 ml.
[0104] In some embodiments of the present invention, the data processing unit includes digital core analysis software for opening the first crude oil three-dimensional distribution image data volume and the second crude oil three-dimensional distribution image data volume.
[0105] In order to better illustrate the solution of the present invention, the present invention provides the following embodiments:
[0106] S1: The shale was cored in Well A of Block J of Liaohe Oilfield. 30g of block samples were selected as soon as the core came out of the barrel, and immediately wrapped with plastic wrap and sealed in a glass bottle for storage. It was immediately sent to the rock thin section preparation unit to be made into double-sided polished, uncapped, 0.05mm thick rock thin sections.
[0107] S2: Place the rock slice prepared in S1 under a fluorescence microscope, use ultraviolet light excitation to observe the rock fluorescence characteristics, and record the sample's fluorescence color, luminous intensity, crude oil distribution characteristics and other information. The sample's fluorescence characteristics are: diffuse dots, laminar dark yellow-white, yellow-brown, mainly containing oily asphalt and asphaltene asphalt. Select the test area and take a microscopic photo.
[0108] S3: Use a laser confocal microscope to perform a first scan on the detection area selected in S2 to obtain the first crude oil three-dimensional distribution image data volume. The top view of the image data volume is as follows: Figure 2 As shown by Figure 2 It can be seen that the crude oil in the sample detection area is mostly enriched in the bedding fractures and distributed in the matrix in a dotted manner. The specific scanning settings are as follows: use 488nm laser as the excitation light, and receive the excitation fluorescence in the range of 489nm-700nm as the crude oil signal. The scanning resolution should be set to 2048×2048, and the scanning speed should be set to 2; adjust the five parameters of excitation light intensity, pinhole, main gain, digital compensation, and digital gain to make the laser confocal image brightness, crude oil distribution characteristics, etc. meet the characteristics of fluorescence luminescence intensity and crude oil distribution characteristics obtained in step 2. Adjust the objective lens to have no excitation light upward and no excitation light downward, determine the scanning start and end points respectively, and set the scanning step length to 1μm.
[0109] S4: Use 2 ml of organic solvent to rinse the rock slice that has been scanned for the first time in S3, wash out the movable oil, collect the rinse liquid during the rinse process, and dry the rock slice after the rinse is completed. During the operation, qualified labor protection equipment must be worn and completed in a fume hood.
[0110] S5: Place the rock slice processed by S4 under a laser confocal microscope, find the scanning area of S3, and perform a second scan using the same scanning parameter settings as S3 to obtain the second crude oil three-dimensional distribution image data volume after washing away the movable oil. The top view of the image data volume is shown in Figure 3 As shown by Figure 3 It can be seen that after washing with organic solvents, the fluorescence intensity of the sample detection area decreases, and the crude oil content in the bedding fractures is relatively high.
[0111] S6: In the digital core analysis software, open the first crude oil 3D distribution image data volume and the second crude oil 3D distribution image data volume. The movable oil 3D distribution image data volume can be obtained by subtracting the second crude oil 3D distribution image data volume from the first crude oil 3D distribution image data volume. The top view of the movable oil 3D distribution image data volume is shown in FIG. Figure 4 As shown by Figure 4 It can be seen that the movable oil is mainly distributed in the bedding fractures, and the movable oil content in the matrix is relatively low. The side view of the movable oil three-dimensional distribution image data body is shown in Figure 5 As shown, Figure 5 The side view can more clearly show the characteristics that the movable oil is mainly stored in the bedding fractures. Further, the volume percentage of the movable oil signal in the movable oil three-dimensional distribution image data volume is calculated to be 1.757%, that is, the movable oil content of the sample is 1.757%. Data extraction and analysis of the movable oil pores were performed, and a total of 123,362 pores were extracted. According to the statistics of pore radius, the movable oil of the sample is mainly stored in pores of 0.46μm-13.23μm. The number of pores is distributed as follows Figure 6 As shown by Figure 6 It can be seen that the smaller the pore radius of the movable oil, the more pores there are. Among the 123,362 pores, more than 120,000 pores with a radius of 1-3 μm for movable oil are distributed as follows: Figure 7 As shown by Figure 7 It can be seen that the radius of the pores where movable oil is stored is less than 14μm, mainly 1-5μm. Among the 123,362 pores, the volume fraction of pores with a radius of about 1μm, 3μm, and 4μm where movable oil is stored is the largest, all above 15%, and the volume fraction of pores with a radius of about 2μm and 5μm is all above 10%.
[0112] S7: The washing liquid collected in S4 is subjected to gas chromatography analysis. The gas chromatography analysis spectrum is as follows: Figure 8 The gas chromatography analysis data are shown in Table 1. Figure 8 It can be seen that the movable oil of the sample is distributed in a single peak. Figure 8 As can be seen from Table 1, the carbon number range is C8-C34, the main peak carbon is C19, and the content of each carbon number component can also be obtained at the same time.
[0113] Table 1
[0114]
[0115]
[0116] In summary, the present invention utilizes the cores or wellbore coring obtained from the shale reservoir coring well to analyze the movable oil occurrence state, obtains the movable oil content and the movable oil carbon number range, can effectively shorten the movable oil content detection cycle, and at the same time can obtain submicron high-resolution movable oil distribution three-dimensional images, movable oil pore number distribution maps, movable oil pore volume distribution maps, and evaluate the movable oil carbon number range and the content of each component, which can provide technical support for drilling tracking, real-time evaluation of shale quality, development plan preparation, economic benefit evaluation, etc.
[0117] Finally, it should be noted that the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.
Claims
1. A rapid detection method for multiple characteristics of movable oil in shale, characterized in that: include: sampling and preparing thin sections of rocks; Selecting a detection area of the rock slice and taking a microscopic photograph; Scanning the detection area for the first time using a laser confocal microscope to obtain a first crude oil three-dimensional distribution image data volume; Washing the rock slice after the first scan with an organic solvent and collecting the washing liquid; Scanning the detection area of the washed rock slice for a second time using a laser confocal microscope to obtain a second crude oil three-dimensional distribution image data volume; Acquiring movable oil content through the first crude oil three-dimensional distribution image data volume and the second crude oil three-dimensional distribution image data volume; The flushing liquid is subjected to gas chromatography analysis to obtain the movable oil carbon number range and the content of each component.
2. A rapid detection method for multiple characteristics of movable oil in shale according to claim 1, characterized in that: The sampling and preparation of rock slices comprises: When the core is out of the barrel, samples are taken and sealed for storage. The samples were sliced and polished to obtain rock thin sections.
3. A rapid detection method for multiple characteristics of movable oil in shale according to claim 2, characterized in that: The sample is a block core, and the sample mass is 20-50g.
4. A rapid detection method for multiple characteristics of movable oil in shale according to claim 2, characterized in that: The rock slices were double-sided polished and not covered with a cover glass.
5. The method for rapid detection of multiple characteristics of movable oil in shale according to claim 1, characterized in that: The step of selecting the detection area of the rock slice and taking a microscopic photograph comprises: The rock slice is placed under a fluorescence microscope and excited by ultraviolet light to observe the fluorescence characteristics of the rock, and the observation characteristics of the rock slice are recorded, wherein the observation characteristics include fluorescence color, luminous intensity and crude oil distribution characteristics.
6. The method for rapid detection of multiple characteristics of movable oil in shale according to claim 1, characterized in that: The first scanning of the detection area using a laser confocal microscope comprises: The laser confocal microscope uses 488nm laser as excitation light and receives excitation fluorescence in the range of 489nm-700nm as crude oil signal.
7. A method for rapid detection of multiple characteristics of movable oil in shale according to claim 5, characterized in that: The first scanning of the detection area using a laser confocal microscope includes: The scanning resolution and scanning speed of the laser confocal microscope are adjusted according to the requirements of the scanning effect, and other parameters required for scanning are adjusted according to the observation characteristics of the rock slice.
8. The method for rapid detection of multiple characteristics of movable oil in shale according to claim 1, characterized in that: The first scanning of the detection area using a laser confocal microscope comprises: The three-dimensional scanning range of the laser confocal microscope is based on the fact that there is no excitation light upward and downward from the objective lens as the scanning start and end points, and the scanning step length is 0.1-1 μm.
9. A rapid detection method for multiple characteristics of movable oil in shale according to claim 1, characterized in that: The method of washing the rock slice after the first scan with an organic solvent and collecting the washing liquid comprises: The rock slice after the first scan is spot-washed with an organic solvent to wash out the movable oil.
10. A rapid detection method for multiple characteristics of movable oil in shale according to claim 9, characterized in that: The amount of the organic solvent used is 2-10 ml.
11. A method for rapid detection of multiple characteristics of movable oil in shale according to claim 9, characterized in that: After the rock slice is washed with an organic solvent after the first scan and the washing liquid is collected, the method comprises: The washed rock slice is air-dried, and the air-dried rock slice is scanned for the second time.
12. A rapid detection method for multiple characteristics of movable oil in shale according to claim 1, characterized in that: The scanning parameters of the second scanning are the same as those of the first scanning.
13. The method for rapid detection of multiple characteristics of movable oil in shale according to claim 1, characterized in that: The method of obtaining the movable oil content through the first crude oil three-dimensional distribution image data volume and the second crude oil three-dimensional distribution image data volume includes: subtracting the second crude oil three-dimensional distribution image data volume from the first crude oil three-dimensional distribution image data volume to obtain a movable oil three-dimensional distribution image data volume; The volume percentage of the movable oil signal of the movable oil three-dimensional distribution image data volume is calculated, wherein the volume percentage of the movable oil signal is the movable oil content.
14. A rapid detection device for multiple characteristics of movable oil in shale, characterized in that: include: A rock thin section preparation unit, used for preparing rock thin sections; A detection area selection unit, used to select the detection area of the rock slice and take a microscopic photograph; A scanning unit, used for performing a first scan and a second scan on the rock slice to obtain a first crude oil three-dimensional distribution image data volume and a second crude oil three-dimensional distribution image data volume; A flushing unit, used to flush the rock slice after the first scan and collect the flushing fluid; A data processing unit, configured to obtain movable oil content through the first crude oil three-dimensional distribution image data volume and the second crude oil three-dimensional distribution image data volume; The movable oil carbon number detection unit is used to perform gas chromatography analysis on the flushing liquid to obtain the movable oil carbon number range and the content of each component.
15. A rapid detection device for multiple characteristics of movable oil in shale according to claim 14, characterized in that: The rock slices were double-sided polished and not covered with a cover glass.
16. A rapid detection device for multiple characteristics of movable oil in shale according to claim 14, characterized in that: The detection area selection unit includes an ultraviolet microscope, which uses ultraviolet light to excite the rock slice, and is used to observe the rock fluorescence characteristics of the rock slice and record its observation characteristics. The observed characteristics include fluorescence color, luminescence intensity and crude oil distribution characteristics.
17. A rapid detection device for multiple characteristics of movable oil in shale according to claim 14, characterized in that: The scanning unit comprises a laser confocal microscope, which uses 488nm laser as excitation light and receives excitation fluorescence in the range of 489nm-700nm as crude oil signal.
18. A rapid detection device for multiple characteristics of movable oil in shale according to claim 17, characterized in that: The scanning resolution and scanning speed of the laser confocal microscope are adjusted according to the requirements of the scanning effect, and other parameters required for scanning are adjusted according to the fluorescence color, luminescence intensity and crude oil distribution characteristics of the rock slice; The three-dimensional scanning range of the laser confocal microscope is based on the fact that there is no excitation light upward and downward from the objective lens as the scanning start and end points, and the scanning step length is 0.1-1 μm.
19. A rapid detection device for multiple characteristics of movable oil in shale according to claim 14, characterized in that: The washing unit uses an organic solvent to wash the rock slice after the first scan, and the amount of the organic solvent used is 2-10 ml.
20. A rapid detection device for multiple characteristics of movable oil in shale according to claim 14, characterized in that: The data processing unit includes digital core analysis software for opening the first crude oil three-dimensional distribution image data volume and the second crude oil three-dimensional distribution image data volume.
Citation Information
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