CN110726778A - Method and system for judging lower limit of flowing croup of shale oil - Google Patents
Method and system for judging lower limit of flowing croup of shale oil Download PDFInfo
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Abstract
The invention discloses a method for judging the lower limit of flowing croup of shale oil, which comprises the following steps: (1) obtaining a plurality of shale raw material samples of an area to be researched; (2) analyzing hydrocarbon substances in each shale raw material sample to obtain a sigma nC 20-sigma nC21+ ratio of each shale raw material sample; (3) carrying out mercury-nitrogen adsorption combined measurement on each shale raw material sample to obtain a pore throat median radius value of each shale raw material sample; (4) carrying out correlation analysis on the sigma nC 20-sigma nC21+ ratio and the pore throat median radius value of different shale raw material samples to obtain a relation graph of the sigma nC 20-sigma nC21+ ratio and the pore throat median radius value of the shale raw materials; the inflection point of the relational graph is the shale oil flowable throat lower limit of the region to be researched. The method has scientific principle, widely used experimental technology, strong judgment and indication operability and easy popularization, and can meet the requirements of exploration, development and research of shale oil.
Description
Technical Field
The invention relates to a method and a system for judging the lower limit of the flowing throat of shale oil, in particular to a method-level system for judging the lower limit of the flowing throat of shale oil by utilizing molecular geochemical parameters, belonging to the technical field of petroleum and natural gas exploration and development research.
Background
The shale oil is retention oil which is left in matrix pores and natural cracks of a mud shale layer series rich in organic matters and carbonate rock, sandstone and siltstone interlayers, is basically liquid hydrocarbon which is retained in situ or is gathered nearby after being adjusted and transported only by short distance in the mud shale layer series, and the mud shale is not only a hydrocarbon source rock but also a reservoir layer. The shale oil has three occurrence states, including a free state, an adsorption state and a kerogen mutual solubility state, wherein the free state shale oil is an effective target resource, the combination of shale organic matter type, abundance, evolution stage and rock physical property plays a crucial role in controlling the occurrence form of the shale oil, and the matching relation between the shale oil content, the shale oil molecular composition and a storage space is the most direct main control factor of the shale oil mobility. Research reveals that the mobility of oil and gas in a conventional reservoir can be well characterized by Darcy's law, but micro-nano-scale pores of a shale reservoir are relatively developed, the shale reservoir has the characteristics of ultra-low pore/ultra-low permeability and rich organic matters, the liquid-solid action is complex, and some factors (such as velocity slip, surface force and electrostatic force) which can be ignored in the conventional macro-meso scale flow gradually begin to occupy a dominant position in the flow, so that a plurality of relatively special micro-nano scale flow phenomena are caused. The phenomena are difficult to explain by using a conventional fluid mechanics theory, so that the research on the fluid flow rule in the shale nano-scale pore structure is mostly limited, and an effective description and characterization method is still lacked so far, for example, aiming at a research target area, the lower limit of the pore throat where shale oil can flow is obtained, so that the method has very important guiding significance for evaluating the shale oil effective resources and making a development scheme, but related mature technical methods are basically not available. Zhangpengfei et al (lower limit of shale oil reservoir physical property, petroleum and natural gas geology 2016, 37 (1): P93-100) in New channel mouth group of Jianghan basin, etc.) use Wall method to obtain minimum flow pore throat radius of reservoir, capillary pressure curve used by it is directly obtained by high pressure mercury pressing experiment, but the seepage mechanism of mercury substance is obviously different from the molecular diffusion mechanism of shale oil complex component, therefore its result is not very practical. In addition, some scholars also make researches on other methods, such as yaoxinping (internal data: report of accumulation space and development mode achievement of shale oil in continental facies, which is subject to 02 topic of enrichment mechanism and distribution rule of shale oil in the east department of China in the national 973 project, 2014CB239102) through microscopic observation, the random value of the width of a shale oil overflow point is measured to be distributed between 8.9 nm and 20.1nm, the average width value is 13.7nm, from the fracture width distribution characteristic, 10nm is considered as the minimum pore diameter of shale oil capable of realizing migration in shale pores, and for pores smaller than 10nm, shale oil is not easy to displace, but can be accumulated in an adsorption state and is difficult to exist in a free state form; crepe (Nano-sized Pore-throats and Hydrocarbon Accumulation feedstocks in ShaleSystem.2012, Wuxi International shale oil conference) studies suggest that the throat lower radius of shale oil flow is 54nm, where 50nm is the throat waterfilm thickness, but waterfilms do not necessarily exist where wettability changes; the statistical median pore throat radius of the oil well in the depressed saline space of the Yangtze river and Han oil field is generally more than 50nm (internal data). As a result of the progress of the prior art, the study of the lower limit of shale oil flowable throats, both from theoretical and from technical approaches, has been inadequate.
Shale oil is a complex mixture comprising saturated hydrocarbons, aromatic hydrocarbons, non-hydrocarbons and the like, wherein saturated hydrocarbons are the predominant components. In the nanometer confined space, the flow of shale oil neither satisfies darcy seepage nor differs from the flow mechanism of a single substance. Shale oil sub-components including long and short paraffins, naphthenesThe macromolecular compounds of hydrocarbon, aromatic hydrocarbon and condensed ring, etc. have different molecular sizes and different diffusion capacities in nanometer space. The method for accurately calculating the characteristic molecular size of heavy oil in Panyuqiu et al (a method for accurately calculating the characteristic molecular size of heavy oil, Petroleum institute (Petroleum processing) 2007, 23 (4): P63-67) accurately calculates the characteristic molecular size of heavy oil, and the volume and the minimum cross-sectional diameter of a residual oil molecule (DQ-fcut) of a first fraction of the molecular size of Daqing heavy oil narrow fraction characteristic molecule are 4.1427nm3And 1.8703 nm; and the residual oil molecules (DQ-mcut) of the second fraction are 14.6209nm respectively3And 3.0080 nm; the residual oil molecules (DQ-endcut) of the residue were 25.249nm, respectively3And 3.4929 nm. From the molecular composition of the shale oil that has been mined, the pore throat diameters of the shale of 5nm that have been wetted are sufficient for the passage of the paraffin, naphthene, aromatic and fused ring macromolecules of different molecular carbon numbers, as long as the driving force is sufficient. However, as mentioned above, the molecular flow in the nanometer space is mainly a diffusion mode, and is limited by various factors such as velocity slip, surface force, electrostatic force and the like, and a diffusion energy barrier exists. Research shows that in a nanometer restricted space, the diffusion of molecules has a diffusion energy barrier, the larger the molecular size is, the larger the diffusion energy barrier is, the smaller the throat radius of the same molecule is (Yuansai, and the like. the molecular simulation of the diffusion behavior of aromatic hydrocarbon and naphthenic hydrocarbon molecules in MFI and FAU molecular sieves. Petroleum institute, 2011, 27 (4): P508-515.). The shale oil is a complex mixture and is in a homogeneous state in a general space, and when the radius of pore throats is small to a certain level, the shale oil is influenced by a diffusion energy barrier, the molecular composition of the shale oil can generate component differentiation in a nanometer restricted pore canal, the pore throats are smaller, macromolecular components are relatively less in occurrence, and the micromolecular components are opposite, so that the shale oil can select the dominant components, and the differentiation condition of the shale oil in the nanometer pore throats can be represented by utilizing the content ratio of the micromolecular compounds to the macromolecular compounds, such as the parameter ratio of n-alkanes below C20 to n-alkanes above C21. When the molecular parameter ratio is unchanged, the molecular components of the shale oil are unchanged, the shale oil is homogeneous, and the fluidity of the shale oil is not affected; when the molecular parameter ratio just begins to change, the shale oil components are differentiated, and the shale oil components are differentiated at the momentThe mobility is affected, and the corresponding shale pore throat radius is the lower pore throat limit where shale oil can flow. This is the theoretical basis for using geochemical analysis parameters to judge the lower limit of the flowable pore throat of shale oil.
Disclosure of Invention
The invention aims to solve the defects of the prior art and the actual requirements of shale oil exploration, development and research, and develops a method for judging the lower limit of the flowable pore throat of shale oil by using molecular geochemical parameters by applying the prior analysis technology and the molecular diffusion theory in a nanometer limited space.
According to one aspect of the invention, there is provided a method of indicating the lower roar limit of shale oil flowable, comprising:
(1) obtaining a plurality of shale raw material samples of an area to be researched;
(2) analyzing hydrocarbon substances in each shale raw material sample to obtain a sigma nC 20-sigma nC21+ ratio of each shale raw material sample;
(3) carrying out mercury-nitrogen adsorption combined measurement on each shale raw material sample to obtain a pore throat median radius value of each shale raw material sample;
(4) carrying out correlation analysis on the sigma nC 20-sigma nC21+ ratio and the pore throat median radius value of different shale raw material samples to obtain a relational graph of the sigma nC 20-sigma nC21+ ratio and the pore throat median radius value of the shale raw material in a region to be researched; the inflection point of the relational graph is the shale oil flowable throat lower limit of the region to be researched.
According to some embodiments of the present invention, the shale feedstock samples should comprise at least 20 samples of different TOC values, different oil contents in the study area.
According to a preferred embodiment of the present invention, the step (2) comprises:
(2A) crushing a shale raw material sample into sample particles/blocks with diameters of 6mm-8 mm;
(2B) adding dichloromethane and 1-C18 alkene standard samples into the crushed samples, carrying out ultrasonic treatment, and carrying out solid-liquid separation to obtain extract liquor and solid particles;
(2C) and performing mass spectrometry on the extract to obtain a sigma nC 20-/. SIGMA nC21+ ratio of the shale raw material sample, wherein SIGMA nC 20-is the sum of the contents of normal alkanes of C13-C20, and SIGMA nC21+ is the sum of the contents of normal alkanes above C21.
Wherein, the 1-C18 alkene standard sample is prepared according to 1ug/ul, the solvent is dichloromethane, and the adding amount of each sample standard sample is 5ul-10 ul.
According to some embodiments of the invention, the power density of the sonication is 0.3W/cm2-0.4W/cm2The ultrasonic frequency is 2KHz-3KHz, and the time interval is 8-12 min.
According to a preferred embodiment of the present invention, the step (3) comprises:
(3A) drying the solid particles in the step (2B);
(3B) and (4) carrying out mercury-nitrogen adsorption joint measurement on the dried solid particle sample to obtain the pore throat median radius value of the sample.
According to some embodiments of the invention, the step (4) comprises:
and (3) plotting the sigma nC 20-sigma nC21+ ratio values of different shale raw material samples on the pore throat median radius value to obtain a relation graph of the sigma nC 20-sigma nC21+ ratio value and the pore throat median radius value of the shale raw material, carrying out correlation analysis, and fitting to obtain a relation graph of the sigma nC 20-sigma nC21+ ratio value and the pore throat median radius value of the shale raw material.
According to another aspect of the present invention there is provided a system for indicating the lower roar limit of shale oil flowable, comprising:
a feed system for obtaining a plurality of shale feed samples for an area to be studied;
the hydrocarbon substance analysis system is used for analyzing the hydrocarbon substances in each shale raw material sample to obtain a sigma nC 20-sigma nC21+ ratio of each shale raw material sample, and the input of the sigma nC 20-sigma nC21+ ratio is connected with the output of the raw material system;
the mercury-nitrogen adsorption combined measurement system is used for carrying out mercury-nitrogen adsorption combined measurement on each shale raw material sample to obtain a pore throat median radius value of each shale raw material sample, and the input of the pore throat median radius value is connected with the output of the hydrocarbon substance analysis system;
the correlation analysis system is used for carrying out correlation analysis on the sigma nC 20-/-sigma nC21+ ratio and the pore throat median radius value of different shale raw material samples to obtain a relation graph of the sigma nC 20-/-sigma nC21+ ratio and the pore throat median radius value of the shale raw materials, and the input of the relation graph is connected with the output of the hydrocarbon substance analysis system and the mercury-nitrogen absorption combined determination system respectively;
the inflection point of the relational graph is the shale oil flowable throat lower limit of the region to be researched.
According to some embodiments of the present invention, the shale feedstock samples should comprise at least 20 samples of different TOC values, different oil contents in the study area.
According to some embodiments of the invention, the hydrocarbon material analysis system comprises:
crushing a shale raw material sample into sample particles/blocks with diameters of 6mm-8 mm;
adding dichloromethane and 1-C18 alkene standard samples into the crushed samples, carrying out ultrasonic treatment, and carrying out solid-liquid separation to obtain extract liquor and solid particles;
and performing mass spectrometry on the extract to obtain a sigma nC 20-/. SIGMA nC21+ ratio of the shale raw material sample, wherein SIGMA nC 20-is the sum of the n-alkane contents of C13-C20, and SIGMA nC21+ is the sum of the n-alkane contents of C21.
According to a preferred embodiment of the present invention, the mercury-nitrogen adsorption combined measurement system comprises:
drying the extracted solid particles;
and (4) carrying out mercury-nitrogen adsorption joint measurement on the dried solid particle sample to obtain the pore throat median radius value of the sample.
According to some preferred embodiments of the present invention, the correlation analysis system comprises:
and (3) plotting the sigma nC 20-sigma nC21+ ratio values of different shale raw material samples on the pore throat median radius value to obtain a relation graph of the sigma nC 20-sigma nC21+ ratio value and the pore throat median radius value of the shale raw material, carrying out correlation analysis on the relation graph, and determining the corresponding pore throat median radius value when the sigma nC 20-sigma nC21+ ratio value is mutated.
Drawings
FIG. 1 is a graph of sigma nC 20-/. sigma nC21+ ratio versus pore throat median radius value for a shale feedstock in accordance with an embodiment of the present invention.
Detailed Description
The invention is further illustrated by the following figures and examples.
The depression of Jiyang is located in southeast part of Bohai Bay basin and consists of 4 depressions of east camp, Huimin, Zhanhua and town and a plurality of protrusions for separating the depressions, and the area is 25510km2Is an important component of the breaking-setback composite basin for the middle and new generations. The depression mainly develops the sand four superior sub-section, the sand three inferior sub-section and the sand one shale layer system of the ancient near series of the sand river street, and the accumulated thickness can reach more than one thousand meters. The shale of the upper sub-section of sand four and the shale of the first sub-section of sand are deposited in a saline water-brackish water lake phase, and the shale of the lower sub-section of sand three is deposited in a fresh water-brackish water lake phase. The organic matter type of the shale oil pool is I-II 1, the TOC content is generally more than 2%, the Ro is distributed between 0.5% and 1.3%, and the shale oil pool has a material basis for forming the shale oil pool. By 2012, the shale interval in the Jiyang depression exploration well has 38 wells for industrial oil and gas flow or low-yield oil and gas flow, 26 wells for mud shale segments only produce oil, and 12 wells for mud shale segments both produce oil and gas. The density of the produced shale oil is generally 0.745-0.93g/cm3The viscosity of the crude oil is between 0.74 and 208 mPa.s, and the density and viscosity of the crude oil are reduced and the gas-oil ratio is increased along with the increase of the burial depth. The system coring well is designed in a shale oil exploration well and comprises a fan-leaf 1 well (FY1), a Li-leaf 1 well (LY1), a ox-leaf 1 well (NY1) and a Ro 69 well (L69), wherein the fan-leaf 1 well, the Li-leaf 1 well and the ox-leaf 1 well belong to an eastern valley, and the Ro 69 well belongs to a staining valley.
The method is used for carrying out experimental analysis on the rock core sample of the oil part of the economical-yang depressed shale, the rock core sample is crushed into particles of 6mm-8mm, a quantitative particle sample is weighed and placed into a sample bottle with a plug, a dichloromethane solvent and an internal standard C18 are added, and the power density is 0.3W/cm2-0.4W/cm2The ultrasonic extraction is carried out for 8-12min under the condition that the ultrasonic frequency is 2KHz-3KHzAnd then performing liquid-solid separation. Performing chromatographic mass spectrum quantitative analysis on the extract to obtain a ratio of sigma nC 20-/' sigma nC21 +; and (4) drying the solid particles, and then carrying out mercury-nitrogen adsorption combined measurement to obtain the median pore throat radius of the rock. The rock sigma nC20-/∑ nC21+ ratio and the corresponding pore throat median radius are plotted (as shown in figure 1), and correlation analysis of the rock sigma nC20-/∑ nC21+ ratio and the corresponding median pore throat radius shows that when the shale pore throat radius is larger than 20nm, the sigma nC20-/∑ nC21+ ratio is basically unchanged, at the moment, the shale oil is in a homogeneous state, the molecular composition of the shale oil is not influenced by the molecular diffusion energy barrier of a nanometer restricted space, and the flow of the shale oil is not influenced and the mobility of the shale oil is good; when the pore throat of the shale is smaller than 20nm, the ratio of sigma nC 20-sigma nC21+ is rapidly increased along with the reduction of the radius of the pore throat of the shale, which indicates that the molecular composition of shale oil movable in the pore throat of the shale begins to change, the flow of macromolecular hydrocarbon substances in the pore canal of the shale is influenced by a diffusion energy barrier, and the molecular composition of the shale oil is differentiated, so that the mobility of the shale oil is limited, and the turning point is the lower limit of the pore throat of the shale oil in the research area, which is about 20 nm.
Any numerical value mentioned in this specification, if there is only a two unit interval between any lowest value and any highest value, includes all values from the lowest value to the highest value incremented by one unit at a time. For example, if it is stated that the amount of a component, or a value of a process variable such as temperature, pressure, time, etc., is 50 to 90, it is meant in this specification that values of 51 to 89, 52 to 88 … …, and 69 to 71, and 70 to 71, etc., are specifically enumerated. For non-integer values, units of 0.1, 0.01, 0.001, or 0.0001 may be considered as appropriate. These are only some specifically named examples. In a similar manner, all possible combinations of numerical values between the lowest value and the highest value enumerated are to be considered to be disclosed in this application.
It should be noted that the above-mentioned embodiments are only for explaining the present invention, and do not constitute any limitation to the present invention. The present invention has been described with reference to exemplary embodiments, but the words which have been used herein are words of description and illustration, rather than words of limitation. The invention can be modified, as prescribed, within the scope of the claims and without departing from the scope and spirit of the invention. Although the invention has been described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, but rather extends to all other methods and applications having the same functionality.
Claims (10)
1. A method of indicating the lower croup limit upon which shale oil may flow, comprising:
(1) obtaining a plurality of shale raw material samples of an area to be researched;
(2) analyzing hydrocarbon substances in each shale raw material sample to obtain a sigma nC 20-sigma nC21+ ratio of each shale raw material sample;
(3) carrying out mercury-nitrogen adsorption combined measurement on each shale raw material sample to obtain a pore throat median radius value of each shale raw material sample;
(4) carrying out correlation analysis on the sigma nC 20-sigma nC21+ ratio and the pore throat median radius value of different shale raw material samples to obtain a relational graph of the sigma nC 20-sigma nC21+ ratio and the pore throat median radius value of the shale raw material in a region to be researched; the inflection point of the relational graph is the shale oil flowable throat lower limit of the region to be researched.
2. The method of claim 1, wherein the number of shale feedstock samples is at least 20.
3. The method of claim 1 or 2, wherein the step (2) comprises:
(2A) crushing a shale raw material sample into sample particles/blocks with diameters of 6mm-8 mm;
(2B) adding dichloromethane and 1-C18 alkene standard samples into the crushed sample particles, carrying out ultrasonic treatment, and carrying out solid-liquid separation to obtain an extraction liquid and solid particles;
(2C) and performing mass spectrometry on the extract to obtain a sigma nC 20-/. SIGMA nC21+ ratio of the shale raw material sample, wherein SIGMA nC 20-is the sum of the contents of normal alkanes of C13-C20, and SIGMA nC21+ is the sum of the contents of normal alkanes above C21.
4. The method of claim 3, wherein the power density of the sonication is 0.3-0.4W/cm2The ultrasonic frequency is 2-3KHz, and the time is 8-12 min.
5. The method according to any one of claims 1-4, wherein the step (3) comprises:
(3A) drying the solid particles in the step (2B);
(3B) and (4) carrying out mercury-nitrogen adsorption joint measurement on the dried solid particle sample to obtain the pore throat median radius value of the sample.
6. The apparatus according to any one of claims 1-5, wherein the step (4) comprises:
and (3) plotting the sigma nC 20-sigma nC21+ ratio of different shale raw material samples on the pore throat median radius value, carrying out correlation analysis, and fitting to obtain a relation graph of the sigma nC 20-sigma nC21+ ratio of the shale raw materials and the pore throat median radius value.
7. A shale oil flowable croup lower threshold interpretation system comprising:
a feed system for obtaining a plurality of shale feed samples for an area to be studied;
the hydrocarbon substance analysis system is used for analyzing the hydrocarbon substances in each shale raw material sample to obtain a sigma nC 20-sigma nC21+ ratio of each shale raw material sample, and the input of the sigma nC 20-sigma nC21+ ratio is connected with the output of the raw material system;
the mercury-nitrogen adsorption combined measurement system is used for carrying out mercury-nitrogen adsorption combined measurement on each shale raw material sample to obtain a pore throat median radius value of each shale raw material sample, and the input of the pore throat median radius value is connected with the output of the hydrocarbon substance analysis system;
the correlation analysis system is used for carrying out correlation analysis on the sigma nC 20-/-sigma nC21+ ratio and the pore throat median radius value of different shale raw material samples to obtain a relation graph of the sigma nC 20-/-sigma nC21+ ratio and the pore throat median radius value of the shale raw material in a region to be researched, and the input of the correlation analysis system is connected with the output of the hydrocarbon substance analysis system and the mercury-nitrogen absorption combined determination system respectively;
the inflection point of the relational graph is the shale oil flowable throat lower limit of the region to be researched.
8. The system of claim 7, wherein the hydrocarbon material analysis system comprises:
crushing a shale raw material sample into sample particles/blocks with diameters of 6mm-8 mm;
adding dichloromethane and 1-C18 alkene standard samples into the crushed sample particles, carrying out ultrasonic treatment, and carrying out solid-liquid separation to obtain an extraction liquid and solid particles;
and performing mass spectrometry on the extract to obtain a sigma nC 20-/. SIGMA nC21+ ratio of the shale raw material sample, wherein SIGMA nC 20-is the sum of the n-alkane contents of C13-C20, and SIGMA nC21+ is the sum of the n-alkane contents of C21.
9. The system of claim 7 or 8, wherein the mercury-nitrogen adsorption combined assay system comprises:
drying the extracted solid particles;
and (4) carrying out mercury-nitrogen adsorption joint measurement on the dried solid particle sample to obtain the pore throat median radius value of the sample.
10. The system according to any one of claims 7-9, wherein the correlation analysis system comprises:
and (3) plotting the sigma nC 20-sigma nC21+ ratio of different shale raw material samples on the pore throat median radius value, carrying out correlation analysis, and fitting to obtain a relation graph of the sigma nC 20-sigma nC21+ ratio of the shale raw materials and the pore throat median radius value.
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