CN103439302A - Method for three-dimensionally detecting distribution and content of organic matter components in mudstone and tight sandstone by utilizing two-photon laser scanning confocal microscopy - Google Patents

Method for three-dimensionally detecting distribution and content of organic matter components in mudstone and tight sandstone by utilizing two-photon laser scanning confocal microscopy Download PDF

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CN103439302A
CN103439302A CN2013104225264A CN201310422526A CN103439302A CN 103439302 A CN103439302 A CN 103439302A CN 2013104225264 A CN2013104225264 A CN 2013104225264A CN 201310422526 A CN201310422526 A CN 201310422526A CN 103439302 A CN103439302 A CN 103439302A
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data volume
kerogen
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CN103439302B (en
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索丽敏
孙先达
李舰
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Northeast Petroleum University
Heilongjiang Bayi Agricultural University
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Abstract

The invention relates to a detection method of the distribution and content of organic matter components in mudstone and tight sandstone and particularly relates to a detection method of the distribution and content of the organic matter components in unconventional reservoirs mainly including the mudstone and the tight sandstone during exploration and development processes of an oil field. According to the method, a two-photon laser scanning confocal microscope is utilized for scanning and analyzing the organic matter components in the mudstone and the tight sandstone, and organic matters with the different components can be subjected to classified three-dimensional space exhibition by utilizing a spectrum separation technique under a situation that a sample is not broken; characteristics of the organic matters in the mudstone and the tight sandstone are researched when a primary structure state of the sample is maintained.

Description

The method of organic composite distribution and content in the burnt three-dimensional detection mud stone of a kind of two-photon laser copolymerization and tight sand
Technical field
The present invention relates to the detection method of machine matter composite distribution and content in a kind of mud stone and tight sand, be specifically related to a kind of in the In Oil Field Exploration And Development process to take the detection method of mud stone and tight sand machine matter composite distribution and content in main unconventional reservoir.
Background technology
Under the prerequisite that at present international energy is in short supply, take mud stone and tight sand is that main unconventional reservoir is the new direction of crude oil reserve of taping the latent power.So it is extremely important to analyze content, component, distribution organic in mud stone and tight sand.Adopt in the past organic component in liquid chromatography and fluorescence thin section methods analyst sandstone, but chromatogram need to pulverize sample to extract again, the structure of having destroyed sample can't be reduced the virgin state of crude oil each component; And the fluorescence thin section method can only be differentiated the organic matter on mudstone sample surface because resolution is relatively low and the fluorescence penetrability is more weak, the None-identified sample interior, and light source is very large on the accuracy impact of result during by the organic component of color differentiating.
Summary of the invention
The object of the present invention is to provide a kind of burnt three-dimensional method that detects organic composite distribution and content in mud stone and tight sand of two-photon laser copolymerization, utilize this effective detection method to come observation and analysis that certain thickness mud stone or tight sand sample are arranged, and can keep under the prerequisite of real blowhole network structure, analyze the method for content organic in mud stone and tight sand, component, distribution.
Microscopic remaining oil laser co-focusing analytical approach is basis by the freezing film-making of rock core, and all band fluorescence microscopy and laser confocal microscope profit rock detect analytical technology and form.
The technical solution adopted in the present invention is: this two-photon laser copolymerization burnt three-dimensional detect in mud stone and tight sand the method for organic composite distribution and content comprise the following steps into:
1) carry out sample preparation under freezing conditions: before section, sample is inserted freezing preservation in liquid nitrogen, and it is air-dry that the rear sample of section need to be placed on environment below 5 ℃.While making sample, with T-2 or T-2 type 502 glue, carry out cementing.During abrasive disc, roughly grind to 2mm, the analytical table mirror polish is processed.
2) adopt two-photon laser copolymerization Jiao method, the two-photon laser Laser Scanning Confocal Microscope is analyzed mud stone or tight sand: sample is placed on objective table, and polished surface upwards.The camera lens of laser scanning co-focusing microscope is adjusted to and observed the sample top, select suitable excitation source scanning samples, use long-focal length lens, select suitable multiple object lens to be observed, image observed in record;
Concrete application and the result of the copolymerization of two-photon laser step 2) Jiao method:
A) spectra collection of lightweight component standard model, select the laser of 710nm wavelength as excitation source, and lightweight component standard model is scanned, and selects XY λ scan pattern, receives the lightweight component characteristic spectrum data volume of 400nm-700nm scope, and preserve;
B) spectra collection of heavy component standard model, select the laser of 710nm wavelength as excitation source, and heavy component standard model is scanned, and selects XY λ scan pattern, receives the heavy component characteristic spectrum data volume of 400nm-700nm scope, and preserve;
C) spectra collection of kerogen component standard model, select the laser of 710nm wavelength as excitation source, kerogen component standard model is scanned, select XY λ scan pattern, receive the kerogen component characteristic spectrum data volume of 400nm-700nm scope, and preserve;
D) spectra collection of detected sample, select the laser of 710nm wavelength as excitation source, and detected sample is scanned, select XY λ Z scan pattern, thickness of sample 50um, interlamellar spacing 1um, receive the detected sample characteristic spectrum data volume of 400nm-700nm scope, and preserve;
E) in detected sample, the lightweight component separates, lightweight component characteristic spectrum data volume in opening a) with spectral separation software, adopt the method for spectral separation to separate d) middle detected sample characteristic spectrum data volume, preserve the lightweight component 3-D data volume of separating.
F) in detected sample, the heavy component separates, open b with spectral separation software) in heavy component characteristic spectrum data volume, adopt the method for spectral separation to separate d) middle detected sample characteristic spectrum data volume, preserve the heavy component 3-D data volume of separating.
G) in detected sample, the kerogen component separates, open c with spectral separation software) in kerogen component characteristic spectrum data volume, adopt the method for spectral separation to separate d) middle detected sample characteristic spectrum data volume, preserve the kerogen component 3-D data volume of separating.
3) organic component three-dimensional reconstruction, e), f), g) in lightweight, heavy and kerogen 3-D data volume carry out three-dimensional reconstruction by computer technology, show lightweight, heavy and space distribution position and the form of kerogen in sample.
4) organic component quantitative analysis, utilize software 3) in data after three-dimensional reconstruction carry out respectively lightweight, heavy and kerogen cubage, obtain lightweight, heavy and kerogen content value.
Effect of the present invention and advantage are: in fine and close oil research, tight sand and Oil source rock often are close to, and mutual deposition, when formation testing, dense sand layer and shale layer concurrent fracturing are fuel-displaced, but the crude oil major storage is at dense sand layer or shale layer, existence what, be the problem that the scientific research personnel studies always.The method is in the situation that keep mud stone and tight sand prototype structure, the content of Accurate Analysis sample interior crude oil, component and distributed in three dimensions state, two-photon has very strong penetrability, detect the weak sample of mud stone and tight sand printing opacity and there is good effect, and spectral unmixing technology can not destroy in the situation of sample, the organic matter of the different components three dimensions of being classified is showed.
The accompanying drawing explanation
Fig. 1 is lightweight component spectrogram;
Fig. 2 heavy component spectrogram;
Fig. 3 kerogen component spectrogram;
Fig. 4 lightweight component three-dimensional reconstruction figure;
Fig. 5 heavy component three-dimensional reconstruction figure;
The superimposed three-dimensional reconstruction figure of Fig. 6 weight component;
Fig. 7 weight component, the superimposed three-dimensional reconstruction figure of kerogen.
Embodiment
Below the just step of the method for a kind of real-time observing mother oil displacement process of true core of the present invention and the effect that can produce, cooperation accompanying drawing, embodiment are described in detail as follows:
This experiment gathers crude oil, stable hydrocarbon, aromatic hydrocarbons, nonhydrocarbon, bituminous matter, the kerogen sample, utilize the laser co-focusing three-dimensional reconstruction, study its laser spectrum feature, find that the wavelength that former light oil constituents produces under Ear Mucosa Treated by He Ne Laser Irradiation is short, near 488nm, the wavelength of heavy component is long, between 600nm~700nm, the mixed composition wavelength of kerogen and adsorbed hydrocarbons thereof is relatively wide, utilize each component peak position and peak type feature to study the space distribution of organic component in tight sand and mudstone sample, the crude oil occurrence status, light components and heavy component (free oil), the blending ingredients relative volume degree of kerogen and adsorbed hydrocarbons thereof.
Laboratory sample, from the distant basin of pine, flushes 1 well location in the western nosing structure of central depression Qijia sag apricot, and formation testing in 2012 obtains the commercial oil of 10.2t/d, is the important breakthrough on the unconventional fine and close exploration activity in loose distant basin.Continuous coring section at the high estrade oil reservoir 20m that flushes 1 well, sample 45, and wherein mud stone is 16,15 of silties, 14 of siltstones.The factor of porosity distribution range of mud stone, silty, siltstone is similar, and between 3.1-11.3%, but siltstone factor of porosity mean value is lower slightly, may be with siltstone containing calcareous relevant; Siltstone is close with the mud stone quartz content, all in 35% left and right; The siltstone feldspar content is high, calcareous content is high, clay mineral content is low, is respectively 40%, 15%, 25%, and mud stone is just in time contrary; On porosity type, siltstone is that intergranular pore, dissolution pore, molten seam, Jie are considered endoporus, microfracture to be worth doing, mud stone be microstructural fracture, laminated structure of shale seam, corrosion seam, matrix micropores, organic cracking Kong,Hou road diameter main peak between 20-40nm, pure shale Hou road diameter main peak is less than 5nm; Mud stone is ripe, rich organic, and TOC is average 2.67%, siltpelite, and abundance of organic matter is also higher, and TOC average 1.89%.Utilize the occurrence status of laser co-focusing research oil in different lithology, find that dissimilar reservoir oiliness there are differences.
Concrete operation step is:
1) carry out sample preparation under freezing conditions: before section, sample is inserted freezing preservation in liquid nitrogen, and it is air-dry that the rear sample of section need to be placed on (0~5 ℃) below 5 ℃ environment.While making sample, with T-2 or T-2 type 502 glue, carry out cementing.During abrasive disc, roughly grind to 2mm, the analytical table mirror polish is processed.
2) adopt two-photon laser copolymerization Jiao method, the two-photon laser Laser Scanning Confocal Microscope is analyzed mud stone or tight sand: sample is placed on objective table, and polished surface upwards.The camera lens of laser scanning co-focusing microscope is adjusted to and observed the sample top, select 710nm excitation source scanning samples, use long-focal length lens, select 10 multiple object lens to be observed, image observed in record;
Concrete application and the result of the copolymerization of two-photon laser step 2) Jiao method:
A) spectra collection of lightweight component standard model: select the laser of 710nm wavelength as excitation source, lightweight component standard model is scanned, select XY λ scan pattern, receive the lightweight component characteristic spectrum data volume (as Fig. 1) of 400nm-700nm scope, and preserve;
B) spectra collection of heavy component standard model: select the laser of 710nm wavelength as excitation source, heavy component standard model is scanned, select XY λ scan pattern, receive the heavy component characteristic spectrum data volume (as Fig. 2) of 400nm-700nm scope, and preserve;
C) spectra collection of kerogen component standard model: select the laser of 710nm wavelength as excitation source, kerogen component standard model is scanned, select XY λ scan pattern, receive the kerogen component characteristic spectrum data volume (as Fig. 3) of 400nm-700nm scope, and preserve;
D) spectra collection of detected sample: select the laser of 710nm wavelength as excitation source, detected sample is scanned, select XY λ Z scan pattern, thickness of sample 50um, interlamellar spacing 1um, receive the detected sample characteristic spectrum data volume of 400nm-700nm scope, and preserve;
E) in detected sample, the lightweight component separates: the lightweight component characteristic spectrum data volume in opening a) with spectral separation software, adopt the method for spectral separation to separate d) middle detected sample characteristic spectrum data volume, preserve the lightweight component 3-D data volume of separating.
F) the heavy component characteristic spectrum data volume heavy component separation in detected sample: with spectral separation software, open b), adopt the method for spectral separation to separate d) middle detected sample characteristic spectrum data volume, preserve the heavy component 3-D data volume of separating.
G) the kerogen component characteristic spectrum data volume kerogen component separation in detected sample: with spectral separation software, open c), adopt the method for spectral separation to separate d) middle detected sample characteristic spectrum data volume, preserve the kerogen component 3-D data volume of separating.
3) organic component three-dimensional reconstruction: e), f), g) in lightweight, heavy and kerogen 3-D data volume carry out three-dimensional reconstruction by computer software, obtain lightweight, heavy and kerogen space distribution position and the form (as Fig. 4, Fig. 5, Fig. 6 and Fig. 7) in sample.
4) data organic component quantitative analysis: utilize software 3) after three-dimensional reconstruction are carried out respectively lightweight, heavy and kerogen cubage, result is as follows: light components content is 3.5%, heavy constituent content 5%, kerogen content is 8.5%, and in mud stone light components content 2.3%, heavy constituent content 4.7%, kerogen content is 6.5%, silty light components content is 1.2%, heavy constituent content 2.8%, and kerogen content is 4%.
As Fig. 4, Fig. 5, Fig. 6 and Fig. 7, from space distribution, the blending ingredients of the light components of mud stone and silty, heavy component and kerogen and adsorbed hydrocarbons thereof, overlap each other together, and three kinds of components of siltstone stagger, particularly between the blending ingredients of light, heavy component and kerogen and adsorbed hydrocarbons thereof, be in staggered distribution more obvious;
Quantitative from component, in siltstone, light components and heavy components content are high, and these explanation siltstones are many containing free oil, and mud stone, silty free oil content are minimum.This is consistent with the result that the petrographic thin section observation is seen, the general oil-containing of siltstone, be free state, and mud stone, few or substantially do not contain containing siltpelite free oil content, this is adsorbed the mud stone oil base by kerogen, the most oil-containings of burning into sand bar reservoir in mud stone are one of fine and close oil and mud stone oil Main Reservoirs.
Utilize laser co-focusing Study In Reservoir oiliness, its advantage can be observed at three dimensions the space distribution of different organic components in reservoir, the content between can also each component of quantitative examination.

Claims (1)

1. the burnt three-dimensional method that detects organic composite distribution and content in mud stone and tight sand of a two-photon laser copolymerization, comprise the following steps:
1) carry out sample preparation under freezing conditions: before section, sample is inserted freezing preservation in liquid nitrogen, and it is air-dry that the rear sample of section need to be placed on 0 ℃ of environment below-5 ℃, while making sample, with T-2 or T-2 type 502 glue, carry out cementing, during abrasive disc, roughly grind to 2mm, the analytical table mirror polish is processed;
2) adopt two-photon laser copolymerization Jiao method, the two-photon laser Laser Scanning Confocal Microscope is analyzed mud stone or tight sand: sample is placed on objective table, polished surface upwards, the camera lens of laser scanning co-focusing microscope is adjusted to and observed the sample top, select 710nm excitation source scanning samples, use long-focal length lens, select 10 multiple object lens to be observed, image observed in record;
Concrete application and the result of the copolymerization of two-photon laser step 2) Jiao method:
A) spectra collection of lightweight component standard model: select the laser of 710nm wavelength as excitation source, lightweight component standard model is scanned, select XY λ scan pattern, receive the lightweight component characteristic spectrum data volume of 400nm-700nm scope, and preserve;
B) spectra collection of heavy component standard model, select the laser of 710nm wavelength as excitation source, and heavy component standard model is scanned, and selects XY λ scan pattern, receives the heavy component characteristic spectrum data volume of 400nm-700nm scope, and preserve;
C) spectra collection of kerogen component standard model, select the laser of 710nm wavelength as excitation source, kerogen component standard model is scanned, select XY λ scan pattern, receive the kerogen component characteristic spectrum data volume of 400nm-700nm scope, and preserve;
D) spectra collection of detected sample, select the laser of 710nm wavelength as excitation source, and detected sample is scanned, select XY λ Z scan pattern, thickness of sample 50um, interlamellar spacing 1um, receive the detected sample characteristic spectrum data volume of 400nm-700nm scope, and preserve;
E) in detected sample, the lightweight component separates, lightweight component characteristic spectrum data volume in opening a) with spectral separation software, adopt the method for spectral separation to separate d) middle detected sample characteristic spectrum data volume, preserve the lightweight component 3-D data volume of separating;
F) in detected sample, the heavy component separates, open b with spectral separation software) in heavy component characteristic spectrum data volume, adopt the method for spectral separation to separate d) middle detected sample characteristic spectrum data volume, preserve the heavy component 3-D data volume of separating;
G) in detected sample, the kerogen component separates, open c with spectral separation software) in kerogen component characteristic spectrum data volume, adopt the method for spectral separation to separate d) middle detected sample characteristic spectrum data volume, preserve the kerogen component 3-D data volume of separating;
3) organic component three-dimensional reconstruction: step e), f), g) in lightweight, heavy and kerogen 3-D data volume carry out three-dimensional reconstruction by computer technology, obtain lightweight, heavy and kerogen space distribution position and the form in sample;
4) organic component quantitative analysis, utilize software 3) in data after three-dimensional reconstruction carry out respectively lightweight, heavy and kerogen cubage, obtain lightweight, heavy and kerogen content value.
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CN113884420A (en) * 2020-07-02 2022-01-04 中国石油化工股份有限公司 Method for accurately acquiring fluorescence oil-containing porosity in clastic rock reservoir

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CN103630669A (en) * 2013-12-16 2014-03-12 中国石油天然气股份有限公司 Experimental method for evaluating oiliness of unconventionally-compacted shale reservoir stratums
CN103630669B (en) * 2013-12-16 2016-03-30 中国石油天然气股份有限公司 Unconventional densification and shale reservoir oil bearing evaluation experimental technique
CN106826405A (en) * 2016-12-27 2017-06-13 中国石油天然气股份有限公司 Rock is ground method
CN107167400B (en) * 2017-05-03 2021-11-09 黑龙江八一农垦大学 Method for detecting crude oil density in petroleum inclusion
CN107167400A (en) * 2017-05-03 2017-09-15 黑龙江八农垦大学 A kind of detection method of petroleum inclusion Central Plains oil density
CN108931497A (en) * 2018-04-20 2018-12-04 中国石油天然气股份有限公司 The method and apparatus that laser co-focusing three-dimensionalreconstruction evaluates hydrocarbon source rock
CN108931497B (en) * 2018-04-20 2021-06-01 中国石油天然气股份有限公司 Method and device for evaluating hydrocarbon source rock through laser confocal three-dimensional reconstruction
CN111175207A (en) * 2018-11-12 2020-05-19 中石化石油工程技术服务有限公司 Method for detecting effective porosity of rock
CN111175207B (en) * 2018-11-12 2023-04-18 中石化石油工程技术服务有限公司 Method for detecting effective porosity of rock
CN110794173A (en) * 2019-11-10 2020-02-14 东北石油大学 Detection method for occurrence states of shale movable fluid and solid organic matter
CN110794173B (en) * 2019-11-10 2022-05-31 东北石油大学 Detection method for occurrence states of shale movable fluid and solid organic matter
CN113884420A (en) * 2020-07-02 2022-01-04 中国石油化工股份有限公司 Method for accurately acquiring fluorescence oil-containing porosity in clastic rock reservoir
CN112362594A (en) * 2020-10-14 2021-02-12 华南理工大学 Direct detection method for mixed gel component distribution based on confocal microscopic hyperspectral imaging
CN112362594B (en) * 2020-10-14 2022-04-22 华南理工大学 Direct detection method for mixed gel component distribution based on confocal microscopic hyperspectral imaging

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