CN111912958A - Method for detecting adsorption and free oil amount in shale inorganic mineral enriched oil - Google Patents

Method for detecting adsorption and free oil amount in shale inorganic mineral enriched oil Download PDF

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CN111912958A
CN111912958A CN202010856524.6A CN202010856524A CN111912958A CN 111912958 A CN111912958 A CN 111912958A CN 202010856524 A CN202010856524 A CN 202010856524A CN 111912958 A CN111912958 A CN 111912958A
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shale
oil
kaolinite
pore
pores
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CN111912958B (en
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柳波
田善思
付晓飞
曾芳
迟亚奥
周晨阳
单翀
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Northeast Petroleum University
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Abstract

The invention discloses a method for detecting the adsorption and free oil amount in shale inorganic mineral enriched oil. The method comprises the following steps: loading the shale oil compound component into the kaolinite pores to obtain a kaolinite pore-shale oil model; performing molecular dynamics simulation on the model to obtain a shale oil density curve in the kaolinite pores; determining the oil adsorption capacity of the kaolinite surface per unit area according to the shale oil density curve in the kaolinite pores and the surface area of the model; determining the specific surface area of inorganic minerals in the shale sample according to the number of the inorganic pores in 1g of the shale sample and the surface area of the inorganic pores in the shale sample; and determining the product of the oil adsorption capacity of the kaolinite surface per unit area and the specific surface area of the inorganic minerals in the shale sample as the oil adsorption amount in the shale inorganic mineral enriched oil. By adopting the method and the system, the accuracy of the detection results of the adsorption and free oil quantity can be improved.

Description

Method for detecting adsorption and free oil amount in shale inorganic mineral enriched oil
Technical Field
The invention relates to the technical field of petroleum geological exploration, in particular to a method for detecting the adsorption and free oil amount in shale inorganic mineral enriched oil.
Background
Shale has the potential to be an oil reservoir, but whether oil can effectively flow and how much oil can flow in shale is related to liquid-solid phase interaction and occurrence states and mechanisms (such as adsorption, dissociation, dissolution and the like) of oil in the reservoir besides pore throat size, structure, distribution and connectivity of shale, which is further related to composition, type and physical properties (such as viscosity, density) of shale oil.
The occurrence state of shale oil in shale, the proportion of different occurrence states (dissolution, swelling, adsorption and dissociation), the occurrence pore size and the interconversion condition, namely the shale oil occurrence mechanism are closely related to the shale oil flowability. Because the water content in shale is low, and the oil solubility in water is extremely low, the dissolved shale oil can be ignored in shale oil occurrence research. The swollen shale oil is present in an organic matrix, the shale oil molecules are "surrounded" by kerogen molecules, and the swollen shale oil is most difficult to flow. The adsorbed petroleum is adsorbed on the surface of organic matter and mineral particles in a 'quasi-solid state', and the flowability is inferior. The free shale oil is not adsorbed by kerogen and mineral particles and flows most easily. The shale organic matter occurrence oil comprises three parts of a swelling state, an adsorption state and a free state, wherein the proportion of the swelling state to the adsorption state is large, so that the mobility of the organic matter occurrence oil is poor, and the shale inorganic mineral occurrence oil only comprises two parts of the adsorption state and the free state, wherein the proportion of the free state is high, so that the mobility of the inorganic mineral occurrence oil is high, and the accuracy of shale oil mobility evaluation can be improved through quantitative evaluation of the shale inorganic mineral occurrence oil. However, the shale oil-inorganic mineral system simulated by molecular dynamics is small, so that the shale oil-inorganic mineral system is difficult to be applied to geological conditions of shale oil adsorption, and the adsorbed and free oil amount in the shale inorganic mineral occurrence oil amount at different evolution stages cannot be detected.
Disclosure of Invention
The invention aims to provide a method for detecting the amount of adsorbed and free oil in shale inorganic mineral enriched oil, which can improve the accuracy of the detection result of the amount of adsorbed and free oil.
In order to achieve the purpose, the invention provides the following scheme:
a method for detecting the amount of oil adsorbed in shale inorganic mineral enriched oil comprises the following steps:
obtaining a shale sample and shale oil compound components, and loading the shale oil compound components into kaolinite pores to obtain a kaolinite pore-shale oil model;
performing molecular dynamics simulation on the kaolinite pore-shale oil model to obtain a shale oil density curve in the kaolinite pores;
determining the oil adsorption capacity of the kaolinite surface per unit area according to the kaolinite pore inner shale oil density curve and the surface area of the kaolinite pore-shale oil model;
determining the specific surface area of the inorganic minerals in the shale sample according to the number of the inorganic pores in the shale sample and the surface area of the inorganic pores in the shale sample;
and determining the product of the oil adsorption capacity of the kaolinite per unit area on the surface and the specific surface area of the inorganic mineral in the shale sample as the oil adsorption amount in the shale inorganic mineral enriched oil.
Optionally, performing molecular dynamics simulation on the kaolinite pore-shale oil model to obtain a shale oil density curve in the kaolinite pore, specifically including:
performing energy minimization and relaxation treatment on the kaolinite pore-shale oil model;
and (3) performing molecular dynamics simulation on the relaxed kaolinite pore-shale oil model under the NPT (non-uniform pressure) ensemble under the condition of preset temperature and pressure to obtain a shale oil density curve in the kaolinite pores.
Optionally, determining the oil adsorption capacity of the kaolinite per unit area according to the kaolinite pore inner shale oil density curve and the surface area of the kaolinite pore-shale oil model specifically includes:
determining the oil adsorption capacity of the kaolinite pore-shale oil model surface unit area according to the following formula:
c＝(cada-a+cads-a)/2
Figure BDA0002646553620000021
Figure BDA0002646553620000022
wherein C represents the oil-adsorbing capacity per unit area of the surface of kaolinite, Cada-aRepresents the oil-adsorbing capacity per unit area of the aluminum octahedral surface, Cads-aM represents the oil-adsorbing ability per unit area of the surface of the silicone-oxygen tetrahedronadaRepresents the aluminum octahedral surface adsorption mass madsRepresents the surface adsorption quality of the silicon-oxygen tetrahedron, AadaRepresenting the surface area of the aluminum oxygen octahedral surface in the kaolinite pore-shale oil model; a. theadsRepresenting the surface area, s, of the surface of the silicon-oxygen tetrahedron in the kaolinite pore-shale oil modelmodelRepresenting the cross-sectional area, rho, of the kaolinite pore-shale oil modeloilDenotes the shale oil density curve in the kaolinite pores, L1Denotes the starting position of the shale oil density curve within the kaolinite pores, L2Represents the cut-off position of the aluminum oxy octahedral surface adsorption layer, L3Denotes the position where the octahedral surface adsorption phase is separated from the free phase, L4Represents the cut-off position of the shale oil density curve within the kaolinite pores.
Optionally, the determining the specific surface area of the inorganic mineral in the shale sample according to the number of the inorganic pores in the shale sample and the surface area of the inorganic pores in the shale sample specifically includes:
determining the specific surface area of the inorganic minerals in the shale sample according to the following formula:
Figure BDA0002646553620000031
wherein the content of the first and second substances,
SMn＝NMDn·sMDn
Figure BDA0002646553620000032
Figure BDA0002646553620000033
Figure BDA0002646553620000034
Figure BDA0002646553620000035
Figure BDA0002646553620000036
Figure BDA0002646553620000037
in the formula, SM represents the specific surface area of inorganic minerals in the shale sample, n represents the sectional statistical number of the pore diameter of the shale sample, and SMnIs the nth section aperture ratio surface area, NMDnRepresents the number of pores with the nth section of pore diameter in 1g of shale, sMDnDenotes a single diameter of DnSurface area of pores of (2), VMnRepresents the inorganic pore volume vM in the shale sample in the n section of pore diameterDnDenotes a diameter DnOf individual pore volume, VshaleIs the volume of a 1g shale sample,. phi. represents the porosity of the shale sample,. TOC represents the total organic carbon content, VφRepresents the organic pore volume, P, per unit mass of organic carbonnIndicating that the nth segment of the pore diameter is in the nucleusRatio in magnetic resonance aperture distribution, FMnThe proportion of the pore diameter of the inorganic mineral in the nth section, DnDenotes the cut-off diameter of the n-th stage pore, Dn-1Denotes the starting diameter of the n-th pore, PNMRRepresents the pore size distribution ratio, Pk, based on the nuclear magnetic resonance experimentnRepresents the proportion of the n-th section of organic aperture in the aperture distribution of the scanning electron microscope, PmnRepresents the proportion of the n-th inorganic aperture on the aperture distribution of the scanning electron microscope, PkSEMRepresents the pore size distribution, Pm, of the organic pores obtained by a scanning electron microscope experimentSEMShowing the pore size distribution of the inorganic pores obtained by a scanning electron microscope experiment.
The invention also provides a method for detecting the free oil amount in the shale inorganic mineral occurrence oil, which comprises the following steps:
obtaining a shale sample and shale oil compound components, and loading the shale oil compound components into kaolinite pores to obtain a kaolinite pore-shale oil model;
performing molecular dynamics simulation on the kaolinite pore-shale oil model to obtain a shale oil density curve in the kaolinite pores;
determining the oil adsorption capacity of the kaolinite surface per unit area according to the kaolinite pore inner shale oil density curve and the surface area of the kaolinite pore-shale oil model;
determining the specific surface area of the inorganic minerals in the shale sample according to the number of the inorganic pores in the shale sample and the surface area of the inorganic pores in the shale sample;
determining the product of the oil adsorption capacity of the kaolinite surface per unit area and the specific surface area of the inorganic minerals in the shale sample as the oil adsorption amount in the shale inorganic mineral enriched oil;
obtaining the amount of the shale inorganic mineral oil;
and determining the difference value of the shale inorganic mineral occurrence oil quantity and the oil adsorption quantity in the shale inorganic mineral occurrence oil as the free oil quantity in the shale inorganic mineral occurrence oil.
Optionally, performing molecular dynamics simulation on the kaolinite pore-shale oil model to obtain a shale oil density curve in the kaolinite pore, specifically including:
performing energy minimization and relaxation treatment on the kaolinite pore-shale oil model;
and (3) performing molecular dynamics simulation on the relaxed kaolinite pore-shale oil model under the NPT (non-uniform pressure) ensemble under the condition of preset temperature and pressure to obtain a shale oil density curve in the kaolinite pores.
Optionally, determining the oil adsorption capacity of the kaolinite per unit area according to the kaolinite pore inner shale oil density curve and the surface area of the kaolinite pore-shale oil model specifically includes:
determining the oil adsorption capacity of the kaolinite pore-shale oil model surface unit area according to the following formula:
c＝(cada-a+cads-a)/2
Figure BDA0002646553620000041
Figure BDA0002646553620000042
wherein C represents the oil-adsorbing capacity per unit area of the surface of kaolinite, Cada-aRepresents the oil-adsorbing capacity per unit area of the aluminum octahedral surface, Cads-aM represents the oil-adsorbing ability per unit area of the surface of the silicone-oxygen tetrahedronadaRepresents the aluminum octahedral surface adsorption mass madsRepresents the surface adsorption quality of the silicon-oxygen tetrahedron, AadaRepresenting the surface area of the aluminum oxygen octahedral surface in the kaolinite pore-shale oil model; a. theadsRepresenting the surface area, s, of the surface of the silicon-oxygen tetrahedron in the kaolinite pore-shale oil modelmodelRepresenting the cross-sectional area, rho, of the kaolinite pore-shale oil modeloilDenotes the shale oil density curve in the kaolinite pores, L1Denotes the starting position of the shale oil density curve within the kaolinite pores, L2Represents the cut-off position of the aluminum oxy octahedral surface adsorption layer, L3Represents aluminum oxidePosition of octahedral surface adsorption phase separated from free phase, L4Represents the cut-off position of the shale oil density curve within the kaolinite pores.
Optionally, the determining the specific surface area of the inorganic mineral in the shale sample according to the number of the inorganic pores in the shale sample and the surface area of the inorganic pores in the shale sample specifically includes:
determining the specific surface area of the inorganic minerals in the shale sample according to the following formula:
Figure BDA0002646553620000051
wherein the content of the first and second substances,
SMn＝NMDn·sMDn
Figure BDA0002646553620000052
Figure BDA0002646553620000053
Figure BDA0002646553620000054
Figure BDA0002646553620000055
Figure BDA0002646553620000056
Figure BDA0002646553620000057
in the formula, SM represents the specific surface area of inorganic minerals in the shale sample, n represents the pore size segmentation system of the shale sampleCounting, SMnIs the nth section aperture ratio surface area, NMDnRepresents the number of pores with the nth section of pore diameter in 1g of shale, sMDnDenotes a single diameter of DnSurface area of pores of (2), VMnRepresents the inorganic pore volume vM in the shale sample in the n section of pore diameterDnDenotes a diameter DnOf individual pore volume, VshaleIs the volume of a 1g shale sample,. phi. represents the porosity of the shale sample,. TOC represents the total organic carbon content, VφRepresents the organic pore volume, P, per unit mass of organic carbonnDenotes the ratio of the n-th section of the pore diameter to the nuclear magnetic resonance pore size distribution, FMnThe proportion of the pore diameter of the inorganic mineral in the nth section, DnDenotes the cut-off diameter of the n-th stage pore, Dn-1Denotes the starting diameter of the n-th pore, PNMRRepresents the pore size distribution ratio, Pk, based on the nuclear magnetic resonance experimentnRepresents the proportion of the n-th section of organic aperture in the aperture distribution of the scanning electron microscope, PmnRepresents the proportion of the n-th inorganic aperture on the aperture distribution of the scanning electron microscope, PkSEMRepresents the pore size distribution, Pm, of the organic pores obtained by a scanning electron microscope experimentSEMShowing the pore size distribution of the inorganic pores obtained by a scanning electron microscope experiment.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a method for detecting adsorption and free oil amount in shale inorganic mineral enriched oil, which comprises the steps of loading shale oil compound components into kaolinite pores to obtain a kaolinite pore-shale oil model; performing molecular dynamics simulation on the kaolinite pore-shale oil model to obtain a shale oil density curve in the kaolinite pores; determining the oil adsorption capacity of the kaolinite surface per unit area according to the density curve of the shale oil in the kaolinite pores and the surface area of the kaolinite pore-shale oil model; determining the specific surface area of inorganic minerals in the shale sample according to the number of the inorganic pores in 1g of the shale sample and the surface area of the inorganic pores in the shale sample; determining the product of the oil adsorption capacity of the kaolinite surface per unit area and the specific surface area of the inorganic minerals in the shale sample as the oil adsorption capacity in the shale inorganic mineral enriched oil; the difference value of the shale inorganic mineral occurrence oil quantity and the oil adsorption quantity in the shale inorganic mineral occurrence oil is determined as the free oil quantity in the shale inorganic mineral occurrence oil, the problem that a shale oil model is replaced by a single component in the past is solved, the accuracy of the adsorption and free oil quantity detection results is improved, important parameters are provided for shale oil mobility evaluation, and the accuracy of shale oil mobility evaluation is improved conveniently.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
FIG. 1 is a flowchart of a method for detecting an amount of oil adsorbed in shale inorganic mineral enriched oil according to an embodiment of the present invention;
FIG. 2 is a schematic illustration of shale oil compound composition in an example of the present invention;
FIG. 3 is a schematic view of a kaolinite pore-shale oil model according to an embodiment of the present invention;
FIG. 4 is a diagram of the last frame of the adsorption simulation of shale oil in a kaolinite slit hole and a schematic diagram of a shale oil density curve in a kaolinite pore space in the embodiment of the invention;
FIG. 5 is a graph of the evolution of the specific surface area of inorganic minerals with Ro in the example of the present invention;
FIG. 6 is a graph showing the evolution trend of the amount of oil adsorbed by inorganic minerals with Ro in the example of the present invention;
FIG. 7 is a graph showing the evolution trend of the amount of the inorganic mineral oil along with Ro in the embodiment of the present invention;
FIG. 8 is a graph showing the evolution trend of the amount of free oil in inorganic pores with Ro in the example of the present invention;
FIG. 9 is a flowchart of a method for detecting the amount of free oil in shale inorganic mineral-bearing oil in the embodiment of the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention aims to provide a method for detecting the amount of adsorbed and free oil in shale inorganic mineral enriched oil, which can improve the accuracy of the detection result of the amount of adsorbed and free oil.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Examples
Fig. 1 is a flowchart of a method for detecting an amount of oil adsorbed in shale inorganic mineral existing oil in an embodiment of the present invention, and as shown in fig. 1, the method for detecting an amount of free oil in shale inorganic mineral existing oil includes:
step 101: and obtaining a shale sample and shale oil compound components, and loading the shale oil compound components into kaolinite pores to obtain a kaolinite pore-shale oil model.
According to the shale oil family composition in the northern part of the Songliao basin: the proportions of saturated hydrocarbons, aromatic hydrocarbons, non-hydrocarbon compounds, colloids and asphaltenes and the hue chromatogram of saturated hydrocarbons are modeled to approximate the molecular dynamics of geologically realistic shale oil, as shown in FIG. 2, C of FIG. 2(a)8H18～C30H62These 23 normal paraffins represent the saturated hydrocarbon components, dimethyldodecylamine (C) of FIGS. 2(b) and 2(C)14H31N) and N-octadecanoic acid (C)18H36O2) Benzene (C) of FIG. 2(d) and FIG. 2(e) representing a non-hydrocarbon compound component6H6) And naphthalene (C)10H8) Asphaltene (C) of FIG. 2(f), representing an aromatic hydrocarbon component60H81NS) represents the colloidal and asphaltene components. Because the kaolinite sheet layer has unique physical properties, the silicon-oxygen tetrahedron is a non-polar surface, the aluminum octahedron is a polar surface,the adsorption characteristics of shale oil molecules on polar and nonpolar surfaces can be known simultaneously by researching the adsorption of the shale oil in the kaolinite, so the kaolinite is selected as an adsorbent to research the adsorption characteristics of the shale oil on the surfaces of inorganic minerals. The 28 compounds in the shale oil compound component were loaded into 13nm wide kaolinite pores using PackMol software, the kaolinite pore-shale oil model is shown in figure 3.
Step 102: and (4) performing molecular dynamics simulation on the kaolinite pore-shale oil model to obtain a shale oil density curve in the kaolinite pore.
Respectively attaching force fields to kaolinite and shale oil molecules by using a ClayFF force field and a Charmm 36/Cgofff force field, respectively using a Lorentz-Bertholt mixing rule for the interaction force between oil mixture molecules and clay minerals, using a Particle-Mesh-Ewald (PME) model for an electrostatic force, and setting the Van der Waals radius to be 1.4 nm; performing energy minimization and relaxation on the kaolinite pore-shale oil model obtained in the step 101 by using Gromacs software, and performing molecular dynamics simulation on the relaxed kaolinite pore-shale oil model under an NPT (non-point-of-care) system under the actual formation temperature and pressure condition (348K and 200bar) in the northern part of the Songliaowan, wherein the simulation time is 200ns, and the simulation last frame is shown in FIG. 4 (a); the simulation result is processed by using a g _ dense module to obtain a density curve of the shale oil in the kaolinite pores, as shown in fig. 4(b), fig. 4(a) is a last frame of adsorption simulation of the shale oil in the kaolinite slit holes, fig. 4(b) is a schematic diagram of the density curve of the shale oil in the kaolinite pores, the abscissa in fig. 4(b) represents the length of the kaolinite pores, and the ordinate represents the density.
Step 103: and determining the oil adsorption capacity of the kaolinite surface per unit area according to the density curve of the shale oil in the kaolinite pores and the surface area of the kaolinite pore-shale oil model.
c＝(cada-a+cads-a)/2
Figure BDA0002646553620000081
Figure BDA0002646553620000082
In the formula: c represents the oil adsorption capacity per unit area of the surface of the kaolinite, Cada-aThe unit area of the aluminum octahedron surface is the oil adsorption capacity in mg/m2；Cads-aThe surface unit area of the silicon-oxygen tetrahedron is provided with the capacity of absorbing oil in mg/m2；madaThe aluminum octahedron surface adsorption mass is mg; m isadsThe adsorption mass of the surface of the silica tetrahedron, mg; smodelIs the cross-sectional area of kaolinite pore-shale oil model, m2；ρoilIs shale oil density curve, kg/m3；AadaIs the surface area of the aluminum oxygen octahedral surface in the kaolinite pore-shale oil model, m2；AadsIs the surface area of the surface of the silicon-oxygen tetrahedron in the kaolinite pore-shale oil model, m2，L1Denotes the starting position of the shale oil density curve within the kaolinite pores, L2Represents the cut-off position of the aluminum oxy octahedral surface adsorption layer, L3Denotes the position where the octahedral surface adsorption phase is separated from the free phase, L4Represents the cut-off position of the shale oil density curve within the kaolinite pores.
The amount of adsorption per unit area of the kaolinite aluminoxy octahedral surface to the mixed component shale oil was found to be 1.93mg/m according to the above formula2And the amount of adsorption of the surface of the silicone-oxygen tetrahedron to the unit area thereof is 2.17mg/m2. It can also be seen that the shale oil with mixed components has different adsorption characteristics on the surfaces of different kaolinite ore sheets, and the adsorption capacity of the surface of the silica tetrahedron is stronger. The result is that in the mixed component shale oil model, the proportion of non-polar components such as saturated hydrocarbon, aromatic hydrocarbon and the like is large, and the proportion of polar components such as non-hydrocarbon, asphaltene and the like is small. The surface of the kaolinite aluminum-oxygen octahedron is a polar surface, polar components with small proportion are easy to adsorb, and non-polar components with large proportion are adsorbed by the surface of the kaolinite silicon-oxygen tetrahedron.
Step 104: and determining the specific surface area of the inorganic mineral in the shale sample according to the number of the inorganic pores in the shale sample and the surface area of the inorganic pores in the shale sample with the unit mass (1 g).
Making kaolinite microporous (<10nm), small holes (10 nm-50 nm), medium holes (50 nm-150 nm), and large holes (150 nm-1000 nm, 1000 nm-10000 nm) are divided according to logarithmic coordinates, each segment is divided into 10 parts on average, and the nth segment (D) is countedn-1～Dn) The surface area of the organic pores within the pore size.
Determining the specific surface area of the inorganic minerals in the shale sample according to the following formula:
Figure BDA0002646553620000091
wherein the content of the first and second substances,
SMn＝NMDn·sMDn
Figure BDA0002646553620000092
Figure BDA0002646553620000093
Figure BDA0002646553620000094
Figure BDA0002646553620000095
Figure BDA0002646553620000096
Figure BDA0002646553620000097
in the formula, SM represents the specific surface area of the inorganic mineral in the shale sample, n represents the sectional statistical number of the pore diameter of the shale sample, n is 50, and SMnIs the nth segment (D)n-1～Dn) Specific surface area of pore diameter, m2，NMDnRepresents the nth stage (D) of 1g of shalen-1～Dn) Number of pores in the pore diameter, sMDnDenotes a single diameter of DnSurface area of pores, m2，VMnRepresents the inorganic pore volume vM in the shale sample in the n section of pore diameterDnDenotes a diameter DnIndividual pore volume of m3，VshaleIs the volume of a 1g shale sample,. phi. represents the porosity of the shale sample,. TOC represents the total organic carbon content, VφRepresents the volume of organic pores per unit mass of organic carbon, cm3/g TOC，PnRepresents the nth segment (D)n-1～Dn) Ratio of pore size in nuclear magnetic resonance pore size distribution, FMnIndicating the inorganic mineral pores of the shale sample in the nth stage (D)n-1～Dn) Ratio of pore diameters, DnDenotes the cut-off diameter of the n-th stage pore, Dn-1Denotes the starting diameter of the n-th pore, PNMRRepresents the pore size distribution ratio, Pk, based on the nuclear magnetic resonance experimentnRepresents the proportion of the n-th section of organic aperture in the aperture distribution of the scanning electron microscope, PmnRepresents the proportion of the n-th inorganic aperture on the aperture distribution of the scanning electron microscope, PkSEMRepresents the pore size distribution, Pm, of the organic pores obtained by a scanning electron microscope experimentSEMShowing the pore size distribution of the inorganic pores obtained by a scanning electron microscope experiment.
After obtaining the specific surface area of the inorganic mineral pores in 1g of shale, it is necessary to normalize it to the TOC. Through calculation, a graph of the evolution trend of the specific surface area of the inorganic mineral along with Ro is obtained, as shown in FIG. 5, and as can be seen from FIG. 5, the specific surface area of the inorganic mineral tends to decrease first and then increase along with the increase of Ro. At the stage of Ro being 0.6-1.2%, the proportion of macropores in inorganic pores of the shale is increased, so that the specific surface area of inorganic minerals is continuously reduced; in the Ro > 1.2% stage, the proportion of macropores in the shale is reduced, and the proportion of micropores and mesopores is increased, so that the specific surface area of the inorganic mineral is increased.
Step 105: and determining the product of the oil adsorption capacity of the kaolinite surface per unit area and the specific surface area of the inorganic minerals in the shale sample as the oil adsorption amount in the shale inorganic mineral enriched oil. The evolution trend graph of the oil adsorption amount of the inorganic minerals along with Ro is shown in figure 6.
FIG. 9 is a flowchart of a method for detecting the amount of free oil in shale inorganic mineral-bearing oil in the embodiment of the invention. As shown in fig. 9, a method for detecting the amount of free oil in shale inorganic mineral-enriched oil includes:
step 201: and obtaining a shale sample and shale oil compound components, and loading the shale oil compound components into kaolinite pores to obtain a kaolinite pore-shale oil model.
Step 202: and (4) performing molecular dynamics simulation on the kaolinite pore-shale oil model to obtain a shale oil density curve in the kaolinite pore.
Step 202, specifically comprising:
performing energy minimization and relaxation treatment on the kaolinite pore-shale oil model;
and (3) performing molecular dynamics simulation on the relaxed kaolinite pore-shale oil model under the NPT (non-uniform pressure) ensemble under the condition of preset temperature and pressure to obtain a shale oil density curve in the kaolinite pores.
Step 203: and determining the oil adsorption capacity of the kaolinite surface per unit area according to the density curve of the shale oil in the kaolinite pores and the surface area of the kaolinite pore-shale oil model.
Step 203, specifically comprising:
determining the oil adsorption capacity of the kaolinite pore-shale oil model surface unit area according to the following formula:
c＝(cada-a+cads-a)/2
Figure BDA0002646553620000111
Figure BDA0002646553620000112
wherein C represents the oil-adsorbing capacity per unit area of the surface of kaolinite, Cada-aRepresents the oil-adsorbing capacity per unit area of the aluminum octahedral surface, Cads-aM represents the oil-adsorbing ability per unit area of the surface of the silicone-oxygen tetrahedronadaRepresents the aluminum octahedral surface adsorption mass madsRepresents the surface adsorption quality of the silicon-oxygen tetrahedron, AadaDenotes the surface area of the aluminum-oxygen octahedral surface in the Kaolin pore-shale oil model, m2；AadsRepresenting the surface area, s, of the surface of the silicon-oxygen tetrahedron in the kaolinite pore-shale oil modelmodelRepresenting the cross-sectional area, rho, of the kaolinite pore-shale oil modeloilDenotes the shale oil density curve in the kaolinite pores, L1Denotes the starting position of the shale oil density curve within the kaolinite pores, L2Represents the cut-off position of the aluminum oxy octahedral surface adsorption layer, L3Denotes the position where the octahedral surface adsorption phase is separated from the free phase, L4Represents the cut-off position of the shale oil density curve within the kaolinite pores.
Step 204: and determining the specific surface area of the inorganic mineral in the shale sample according to the number of the inorganic pores in the shale sample and the surface area of the inorganic pores in the shale sample with the unit mass (1 g).
Step 204, specifically comprising:
determining the specific surface area of the inorganic minerals in the shale sample according to the following formula:
Figure BDA0002646553620000113
wherein the content of the first and second substances,
SMn＝NMDn·sMDn
Figure BDA0002646553620000114
Figure BDA0002646553620000121
Figure BDA0002646553620000122
Figure BDA0002646553620000123
Figure BDA0002646553620000124
Figure BDA0002646553620000125
in the formula, SM represents the specific surface area of inorganic minerals in the shale sample, n represents the sectional statistical number of the pore diameter of the shale sample, and SMnIs the nth section aperture ratio surface area, NMDnRepresents the number of pores with the nth section of pore diameter in 1g of shale, sMDnDenotes a single diameter of DnSurface area of pores of (2), VMnRepresents the inorganic pore volume vM in the shale sample in the n section of pore diameterDnDenotes a diameter DnOf individual pore volume, VshaleIs the volume of a 1g shale sample,. phi. represents the porosity of the shale sample,. TOC represents the total organic carbon content, VφRepresents the organic pore volume, P, per unit mass of organic carbonnDenotes the ratio of the n-th section of the pore diameter to the nuclear magnetic resonance pore size distribution, FMnThe proportion of the pore diameter of the inorganic mineral in the nth section, DnDenotes the cut-off diameter of the n-th stage pore, Dn-1Denotes the starting diameter of the n-th pore, PNMRRepresents the pore size distribution ratio, Pk, based on the nuclear magnetic resonance experimentnRepresents the proportion of the n-th section of organic aperture in the aperture distribution of the scanning electron microscope, PmnRepresents the proportion of the n-th inorganic aperture on the aperture distribution of the scanning electron microscope, PkSEMRepresents the pore size distribution, Pm, of the organic pores obtained by a scanning electron microscope experimentSEMShowing the pore size distribution of the inorganic pores obtained by a scanning electron microscope experiment.
Step 205: and determining the product of the oil adsorption capacity of the kaolinite surface per unit area and the specific surface area of the inorganic minerals in the shale sample as the oil adsorption amount in the shale inorganic mineral enriched oil.
Step 206: obtaining the amount of the shale inorganic mineral oil.
Step 207: and determining the difference value of the shale inorganic mineral occurrence oil mass and the oil mass adsorbed in the shale inorganic mineral occurrence oil as the free oil mass in the shale inorganic mineral occurrence oil.
The amount of oil formed in the shale inorganic minerals is shown in fig. 7, and the amount of free oil in the inorganic pores is shown in fig. 8. The amount of oil adsorbed by the inorganic minerals showed a tendency to increase rapidly first, then to remain substantially unchanged and finally to increase slowly as Ro increases (fig. 6). Shale oil enters inorganic pores after meeting the requirements of kerogen swelling oil, kerogen adsorption oil and organic pore free oil, and is firstly adsorbed on the surface of inorganic minerals, so that the oil adsorption capacity of the inorganic minerals is rapidly increased at the stage of Ro being 0.72-0.75%, and the evolution trend of the oil adsorption capacity of the inorganic minerals is mainly controlled by the specific surface area of the inorganic minerals at the stage of Ro being more than 0.75%. The amount of free oil in the inorganic pores tends to increase and decrease with the increase of Ro, and the maximum value is 131.13mg/g TOC. Because the adsorbed mineral oil amount is far less than the inorganic pore free oil amount, in the inorganic pores, the shale oil is mainly in a free state, and the evolution trend of the inorganic pore free oil amount is mainly controlled by the inorganic part of the shale oil amount.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In summary, this summary should not be construed to limit the present invention.

Claims (8)

1. A method for detecting the amount of oil adsorbed in shale inorganic mineral enriched oil is characterized by comprising the following steps:
obtaining a shale sample and shale oil compound components, and loading the shale oil compound components into kaolinite pores to obtain a kaolinite pore-shale oil model;
performing molecular dynamics simulation on the kaolinite pore-shale oil model to obtain a shale oil density curve in the kaolinite pores;
determining the oil adsorption capacity of the kaolinite surface per unit area according to the kaolinite pore inner shale oil density curve and the surface area of the kaolinite pore-shale oil model;
determining the specific surface area of the inorganic minerals in the shale sample according to the number of the inorganic pores in the shale sample and the surface area of the inorganic pores in the shale sample;
and determining the product of the oil adsorption capacity of the kaolinite per unit area on the surface and the specific surface area of the inorganic mineral in the shale sample as the oil adsorption amount in the shale inorganic mineral enriched oil.
2. The method for detecting the amount of oil adsorbed in shale inorganic mineral inventory oil according to claim 1, wherein the molecular dynamics simulation of the kaolinite pore-shale oil model is performed to obtain a density curve of the shale oil in the kaolinite pores, and specifically comprises:
performing energy minimization and relaxation treatment on the kaolinite pore-shale oil model;
and (3) performing molecular dynamics simulation on the relaxed kaolinite pore-shale oil model under the NPT (non-uniform pressure) ensemble under the condition of preset temperature and pressure to obtain a shale oil density curve in the kaolinite pores.
3. The method for detecting the amount of oil adsorbed in shale inorganic mineral oil according to claim 2, wherein the determining of the oil adsorption capacity per unit area of the kaolinite surface according to the kaolinite pore internal shale oil density curve and the surface area of the kaolinite pore-shale oil model specifically comprises:
determining the oil adsorption capacity of the kaolinite pore-shale oil model surface unit area according to the following formula:
c＝(cada-a+cads-a)/2
Figure FDA0002646553610000011
Figure FDA0002646553610000012
wherein C represents the oil-adsorbing capacity per unit area of the surface of kaolinite, Cada-aRepresents the oil-adsorbing capacity per unit area of the aluminum octahedral surface, Cads-aM represents the oil-adsorbing ability per unit area of the surface of the silicone-oxygen tetrahedronadaRepresents the aluminum octahedral surface adsorption mass madsRepresents the surface adsorption quality of the silicon-oxygen tetrahedron, AadaRepresenting the surface area of the aluminum oxygen octahedral surface in the kaolinite pore-shale oil model; a. theadsRepresenting the surface area, s, of the surface of the silicon-oxygen tetrahedron in the kaolinite pore-shale oil modelmodelRepresenting the cross-sectional area, rho, of the kaolinite pore-shale oil modeloilDenotes the shale oil density curve in the kaolinite pores, L1Denotes the starting position of the shale oil density curve within the kaolinite pores, L2Represents the cut-off position of the aluminum oxy octahedral surface adsorption layer, L3Denotes the position where the octahedral surface adsorption phase is separated from the free phase, L4Represents the cut-off position of the shale oil density curve within the kaolinite pores.
4. The method for detecting the amount of oil adsorbed in the shale inorganic mineral enriched oil according to claim 3, wherein the determining the specific surface area of the inorganic mineral in the shale sample according to the number of the inorganic pores in the shale sample and the surface area of the inorganic pores in the shale sample specifically comprises:
determining the specific surface area of the inorganic minerals in the shale sample according to the following formula:
Figure FDA0002646553610000021
wherein the content of the first and second substances,
SMn＝NMDn·sMDn
Figure FDA0002646553610000022
Figure FDA0002646553610000023
Figure FDA0002646553610000024
Figure FDA0002646553610000025
Figure FDA0002646553610000026
Figure FDA0002646553610000027
in the formula, SM represents the specific surface area of inorganic minerals in the shale sample, n represents the sectional statistical number of the pore diameter of the shale sample, and SMnIs the nth section aperture ratio surface area, NMDnRepresents the number of pores with the nth section of pore diameter in 1g of shale, sMDnDenotes a single diameter of DnSurface area of pores of (2), VMnRepresents the inorganic pore volume vM in the shale sample in the n section of pore diameterDnDenotes a diameter DnOf individual pore volume, VshaleIs the volume of a 1g shale sample,. phi. represents the porosity of the shale sample,. TOC represents the total organic carbon content, VφRepresents the organic pore volume, P, per unit mass of organic carbonnThe ratio of the nth section aperture on the nuclear magnetic resonance aperture distribution is shown,FMnthe proportion of the pore diameter of the inorganic mineral in the nth section, DnDenotes the cut-off diameter of the n-th stage pore, Dn-1Denotes the starting diameter of the n-th pore, PNMRRepresents the pore size distribution ratio, Pk, based on the nuclear magnetic resonance experimentnRepresents the proportion of the n-th section of organic aperture in the aperture distribution of the scanning electron microscope, PmnRepresents the proportion of the n-th inorganic aperture on the aperture distribution of the scanning electron microscope, PkSEMRepresents the pore size distribution, Pm, of the organic pores obtained by a scanning electron microscope experimentSEMShowing the pore size distribution of the inorganic pores obtained by a scanning electron microscope experiment.
5. A method for detecting the amount of free oil in shale inorganic mineral occurrence oil is characterized by comprising the following steps:
obtaining a shale sample and shale oil compound components, and loading the shale oil compound components into kaolinite pores to obtain a kaolinite pore-shale oil model;
performing molecular dynamics simulation on the kaolinite pore-shale oil model to obtain a shale oil density curve in the kaolinite pores;
determining the oil adsorption capacity of the kaolinite surface per unit area according to the kaolinite pore inner shale oil density curve and the surface area of the kaolinite pore-shale oil model;
determining the specific surface area of the inorganic minerals in the shale sample according to the number of the inorganic pores in the shale sample and the surface area of the inorganic pores in the shale sample;
determining the product of the oil adsorption capacity of the kaolinite surface per unit area and the specific surface area of the inorganic minerals in the shale sample as the oil adsorption amount in the shale inorganic mineral enriched oil;
obtaining the amount of the shale inorganic mineral oil;
and determining the difference value of the shale inorganic mineral occurrence oil quantity and the oil adsorption quantity in the shale inorganic mineral occurrence oil as the free oil quantity in the shale inorganic mineral occurrence oil.
6. The method for detecting the amount of free oil in shale inorganic mineral residual oil according to claim 5, wherein the molecular dynamics simulation of the kaolinite pore-shale oil model is performed to obtain a density curve of the shale oil in the kaolinite pores, and the method specifically comprises the following steps:
performing energy minimization and relaxation treatment on the kaolinite pore-shale oil model;
and (3) performing molecular dynamics simulation on the relaxed kaolinite pore-shale oil model under the NPT (non-uniform pressure) ensemble under the condition of preset temperature and pressure to obtain a shale oil density curve in the kaolinite pores.
7. The method for detecting the amount of free oil in shale inorganic mineral occurrence oil according to claim 6, wherein the determining of the oil adsorption capacity per unit area of the kaolinite surface according to the kaolinite pore internal shale oil density curve and the surface area of the kaolinite pore-shale oil model specifically comprises:
determining the oil adsorption capacity of the kaolinite pore-shale oil model surface unit area according to the following formula:
c＝(cada-a+cads-a)/2
Figure FDA0002646553610000041
Figure FDA0002646553610000042
wherein C represents the oil-adsorbing capacity per unit area of the surface of kaolinite, Cada-aRepresents the oil-adsorbing capacity per unit area of the aluminum octahedral surface, Cads-aM represents the oil-adsorbing ability per unit area of the surface of the silicone-oxygen tetrahedronadaRepresents the aluminum octahedral surface adsorption mass madsRepresents the surface adsorption quality of the silicon-oxygen tetrahedron, AadaRepresenting the surface area of the aluminum oxygen octahedral surface in the kaolinite pore-shale oil model; a. theadsRepresenting silicon-oxygen tetrahedrons in kaolinite pore-shale oil modelSurface area of the surface, smodelRepresenting the cross-sectional area, rho, of the kaolinite pore-shale oil modeloilDenotes the shale oil density curve in the kaolinite pores, L1Denotes the starting position of the shale oil density curve within the kaolinite pores, L2Represents the cut-off position of the aluminum oxy octahedral surface adsorption layer, L3Denotes the position where the octahedral surface adsorption phase is separated from the free phase, L4Represents the cut-off position of the shale oil density curve within the kaolinite pores.
8. The method for detecting the amount of free oil in shale inorganic mineral-bearing oil according to claim 7, wherein the determining the specific surface area of the inorganic mineral in the shale sample according to the number of the inorganic pores in the shale sample and the surface area of the inorganic pores in the shale sample specifically comprises:
determining the specific surface area of the inorganic minerals in the shale sample according to the following formula:
Figure FDA0002646553610000043
wherein the content of the first and second substances,
SMn＝NMDn·sMDn
Figure FDA0002646553610000044
Figure FDA0002646553610000045
Figure FDA0002646553610000046
Figure FDA0002646553610000047
Figure FDA0002646553610000048
Figure FDA0002646553610000049
in the formula, SM represents the specific surface area of inorganic minerals in the shale sample, n represents the sectional statistical number of the pore diameter of the shale sample, and SMnIs the nth section aperture ratio surface area, NMDnRepresents the number of pores with the nth section of pore diameter in 1g of shale, sMDnDenotes a single diameter of DnSurface area of pores of (2), VMnRepresents the inorganic pore volume vM in the shale sample in the n section of pore diameterDnDenotes a diameter DnOf individual pore volume, VshaleIs the volume of a 1g shale sample,. phi. represents the porosity of the shale sample,. TOC represents the total organic carbon content, VφRepresents the organic pore volume, P, per unit mass of organic carbonnDenotes the ratio of the n-th section of the pore diameter to the nuclear magnetic resonance pore size distribution, FMnThe proportion of the pore diameter of the inorganic mineral in the nth section, DnDenotes the cut-off diameter of the n-th stage pore, Dn-1Denotes the starting diameter of the n-th pore, PNMRRepresents the pore size distribution ratio, Pk, based on the nuclear magnetic resonance experimentnRepresents the proportion of the n-th section of organic aperture in the aperture distribution of the scanning electron microscope, PmnRepresents the proportion of the n-th inorganic aperture on the aperture distribution of the scanning electron microscope, PkSEMRepresents the pore size distribution, Pm, of the organic pores obtained by a scanning electron microscope experimentSEMShowing the pore size distribution of the inorganic pores obtained by a scanning electron microscope experiment.
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