CN112414913B - Visual carbonate rock microscopic seepage model and preparation method and application thereof - Google Patents
Visual carbonate rock microscopic seepage model and preparation method and application thereof Download PDFInfo
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- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 title claims abstract description 56
- 239000011435 rock Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 230000000007 visual effect Effects 0.000 title claims abstract description 22
- 239000011148 porous material Substances 0.000 claims abstract description 93
- 239000004575 stone Substances 0.000 claims abstract description 35
- 239000003292 glue Substances 0.000 claims abstract description 24
- 238000005530 etching Methods 0.000 claims abstract description 13
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- 239000011248 coating agent Substances 0.000 claims abstract description 7
- 238000000576 coating method Methods 0.000 claims abstract description 7
- 238000004026 adhesive bonding Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 8
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- 238000005325 percolation Methods 0.000 claims description 6
- 238000003776 cleavage reaction Methods 0.000 claims description 5
- 238000011161 development Methods 0.000 claims description 5
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
- G01N13/04—Investigating osmotic effects
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Abstract
The invention provides a visual carbonate rock micro seepage model and a preparation method and application thereof. The preparation method of the model comprises the following steps: preparing a pore structure pattern of an actual carbonate rock core; cutting ice winter stones to obtain two ice winter stone sheets with the same size, wherein the two ice winter stone sheets are respectively used as a bottom plate and a panel; marking a gluing area and a pore network area on the surface of the bottom plate; etching the pore structure pattern to the pore network area on the surface of the bottom plate and etching the pore channel structure; etching a sample inlet and a sample outlet communicated with the pore passage on the surface of the bottom plate, and reserving channels of the sample inlet and the sample outlet on the corresponding panel; and after the glue coating area on the surface of the bottom plate is coated with glue, covering the bottom plate through the panel, and curing to obtain the visual carbonate rock micro seepage model. The model has the mineral properties and good light transmittance of natural carbonate rocks, can simulate the geometric shape and pore size of real carbonate rock pores, and reduces the mineral composition on the inner surfaces of the real carbonate rock pores to the maximum extent.
Description
Technical Field
The invention belongs to the technical field of oil and gas field development, and relates to a visual carbonate rock microscopic seepage model and a preparation method and application thereof.
Background
The microscopic seepage model and the manufacturing technology thereof are the basis of the microscopic seepage experiment. In order to meet the requirements of different research contents, people develop various physical models for simulating a pore system of a porous medium and performing various micro seepage experiments to obtain detailed and exact research results which are as close to the real situation of the interior of the actual porous medium as possible. Therefore, the micro-seepage physical model must have the following two properties. Firstly, simulating the pore size, the geometric form, the surface mineral components and the like of a porous medium pore system, wherein the more vivid the simulation is, the closer to the actual porous medium is, the better the model is; secondly, the model has good light transmission so as to observe and study the distribution and flow condition of the multiphase fluid in the pore passage by means of an optical instrument, the better the light transmission is, the clearer the image can be obtained, and the model has practical research value. The real core of the oil layer has a real pore system, and can completely and truly simulate the internal seepage state of a real porous medium; however, the actual core is opaque and cannot be used to observe the distribution and flow of fluid inside the pore canal by means of optical instruments. Therefore, on the premise of meeting the light transmission, people simulate the pore system of the porous medium from different angles according to the requirements of research contents, so that different types of microscopic seepage physical models are developed to perform a simulation experiment of microscopic seepage mechanics and research various problems of microscopic seepage. These models can be roughly classified into four categories: a bead clamping model, a capillary network model, a pore network model and a sandstone pore model.
The process for making the bead-sandwiched model is to use two pieces of glass to densely clamp a layer of sorted glass beads, seal the periphery and only leave the inlet and the outlet, thus making a layered porous medium model. The model can better realize the three-dimensional structure of the pore medium, has light transmittance and can display certain characteristic details of flow. However, the bead-filled model does not easily control the pore size of the pore system precisely, and it is very difficult to observe the phase-to-phase motion and the interaction of each phase completely inside the three-dimensional model.
The capillary network model is a capillary network etched on a glass plate. A capillary network model is developed in the 20 th century and the 80 th century in which the seepage mechanics of Chinese academy of sciences is located, and is matched with a pore inner surface wettability control technology, a pore inner surface roughness control technology, a model regeneration and modification technology and the like, so that the micro seepage simulation technology is greatly developed. The advantage of such a model is that the pore size and the morphology distribution of the pore system can be exactly set, but certain morphology distribution characteristics of a three-dimensional pore system, in particular the characteristics of pore throat variations, cannot be simulated.
The pore network model is made by making porous medium pore system pattern on glass by photoetching technology and sintering. In conjunction with the aforementioned supporting techniques, such models have been able to largely mimic the pore size and geometric distribution of the pore system within a real porous media. It can reproduce the characteristics of the pore structure of the porous medium, particularly the characteristics of pore throat variation. The two-dimensional transparent model is very suitable for the experiment of observing and researching the distribution and the flow of the fluid in the pore channel, and is suitable for researching the interface phenomenon and the interaction mechanism among the fluids in various phases. However, since the model is made of glass (the main component is silicon dioxide), the mineral composition of some special lithology (such as carbonate rock) and the complex properties of the inner surface of the pore canal cannot be simulated. Although there are some documents which adopt the aim of coating mineral powder on the inner wall of a glass pore canal so as to simulate the mineral composition of the inner wall of the pore canal, the technology is high in cost and the model is not reproducible.
The sandstone pore model is a microscopic model of a real oil layer pore structure, and is manufactured by adhering an actual rock core between two optical glass plates after being subjected to oil washing and flaking, and sealing and connecting an inlet and an outlet. The advantages are that: because the core is made of a real core, the pore structure, the shape and the mineral composition of the real core are basically maintained. But the disadvantages are also evident: the light transmission of the real sandstone core is poor, and the display of a partial flow field is easy to be unclear.
The main problem of the existing microcosmic seepage physical model is that the geometric form and surface minerals of a real oil reservoir pore system are difficult to simulate, and meanwhile, the microcosmic seepage physical model has good light transmittance so as to be convenient for observation and research.
Disclosure of Invention
Based on the problems in the prior art, the first purpose of the invention is to provide a visual carbonate rock micro-seepage model; the second purpose of the invention is to provide a preparation method of the visualized carbonate rock micro-seepage model, which is prepared by adopting ice winter stone as a raw material and combining a photoetching technology and a model sealing technology; the third purpose of the invention is to provide the application of the visual carbonate rock micro-seepage model in researching the carbonate rock reservoir water injection development micro-seepage rule; the model can simulate real carbonate reservoir pore networks and surface minerals and can realize visualization.
The purpose of the invention is realized by the following technical means:
in one aspect, the invention provides a preparation method of a visual carbonate rock micro-seepage model, which comprises the following steps:
preparing a pore structure pattern of an actual carbonate rock core;
cutting ice winter stones to obtain two ice winter stone sheets with the same size, wherein the two ice winter stone sheets are respectively used as a bottom plate and a panel;
marking a gluing area and a pore network area on the surface of the bottom plate;
etching the pore structure pattern to the pore network area on the surface of the bottom plate and etching the pore channel structure;
etching a sample inlet and a sample outlet communicated with the pore passage on the surface of the bottom plate, and reserving channels of the sample inlet and the sample outlet on the corresponding panel;
and after the glue coating area on the surface of the bottom plate is coated with glue, covering the bottom plate through the panel, and curing to obtain the visual carbonate rock micro seepage model.
Compared with the prior art that the quartz stone is adopted to manufacture the model, the model obtained by the invention has the mineral properties and good light transmittance of the natural carbonate rock, can simulate the geometric form and pore size of the real carbonate rock pore, can reduce the mineral composition on the inner surface of the real carbonate rock pore to the maximum extent, and can directly observe the seepage rule, seepage characteristics and oil displacement mechanism in the pore. Compared with a glass sand filling model and a real sandstone model, the model has the advantages of low manufacturing cost and repeated use.
In the above-mentioned preparation method, preferably, the direction of cleavage of the ice is perpendicular to the cleavage plane of the ice.
In the above preparation method, preferably, the thickness of the obtained ice winter stone sheet is 1.5-2 mm.
The crystal structure of the natural ice winter stone belongs to a trigonal system, a rhombohedral crystal cell belongs to a completely cleaved mineral, a cleavage plane is smooth and fragile, and the ice winter stone is difficult to process into slices of 1.5-2 mm.
In the above preparation method, preferably, the pore structure pattern is repeatedly etched to the pore network region on the surface of the base plate by using a photolithography technique. The photolithographic techniques employed are conventional in the art.
In the above preparation method, preferably, the method for etching the pore structure includes:
taking the bottom plate after the pore structure pattern is repeatedly engraved, performing wax sealing on the surface of the bottom plate except the pore structure pattern, then soaking the bottom plate in acid liquor to etch pore channels, then taking out the bottom plate, removing wax, and performing ultrasonic cleaning and drying. The wax sealing part is the part for bonding the bottom plate and the panel.
In the preparation method, preferably, the acid solution is obtained by compounding hydrochloric acid, sulfuric acid and water, and the volume ratio of the hydrochloric acid to the sulfuric acid to the water is 1:1 (34.5-40).
The acid liquor of the invention adopts a specific formula and a specific proportion, and the pore channel structure close to the real carbonate rock can be obtained by etching the acid liquor.
In the preparation method, the soaking time is preferably 15-20 h.
In the above preparation method, preferably, the glue used for gluing the gluing area on the surface of the base plate is optical UV glue. It has oil resistance and water resistance; the bonding strength is larger than the strength of the ice winter stone; the viscosity is easy to blend; the setting time is longer than the time required for the bonding operation.
In the preparation method, the thickness of the glue layer after gluing and curing is preferably controlled to be 3-5 μm.
In the above preparation method, preferably, the UV lamp is used for irradiation curing, and the curing operation is completed after the glue solution is completely solidified.
In the above preparation method, it is preferable that the curing time is not less than 30 min.
On the other hand, the invention also provides a visual carbonate rock micro seepage model prepared by the preparation method.
On the other hand, the invention also provides application of the visual carbonate rock micro-seepage model in researching the carbonate rock reservoir water injection development micro-seepage rule.
The visualized carbonate rock microscopic seepage model disclosed by the invention can solve the problems that the existing microscopic seepage model cannot simultaneously simulate surface minerals and visualize the rock core of a real carbonate rock, has the mineral properties and good light transmittance of a natural carbonate rock, can simulate the geometric form and the pore size of a real carbonate rock pore, can also reduce the mineral composition on the inner surface of the real carbonate rock pore to the maximum extent, and can directly observe the seepage rule, the seepage characteristic and the oil displacement mechanism in the pore; fills the blank in the aspect of the visual microscopic seepage simulation technology of the carbonate reservoir. The visualized carbonate rock microscopic seepage model is not only suitable for the field of development and research of oil fields, but also can be used and referred to in other research fields related to seepage phenomena.
Drawings
Fig. 1 is a template of the pore structure pattern of an actual carbonate core used in example 1 of the present invention.
FIG. 2 is a picture of the natural ice winter stone used for modeling in example 1 of the present invention.
FIG. 3 is a drawing of two sheets of ice winter stone obtained by cutting natural ice winter stone according to example 1 of the present invention as a floor and a panel, respectively.
FIG. 4 is a diagram of a visualized carbonate rock micro-seepage model prepared in example 1 of the present invention.
Fig. 5 is an oil-containing distribution diagram of an initial state in a water flooding micro seepage experiment process by using a visual carbonate rock micro seepage model diagram in embodiment 2 of the present invention.
Fig. 6 is an oil-containing distribution diagram of water flooding in the water flooding micro-seepage experiment process by using a visual carbonate rock micro-seepage model diagram in embodiment 2 of the present invention.
Fig. 7 is an oil-containing distribution diagram after water flooding is finished in a water flooding micro seepage experiment process by using a visual carbonate rock micro seepage model diagram in embodiment 2 of the present invention.
FIG. 8 is a graph of the contact angle of crude oil on the surface of ice and winter stones in a contact angle comparison experiment of the invention.
FIG. 9 is a graph showing the contact angle of crude oil on the surface of quartz stone in the contact angle comparison experiment of the present invention.
Detailed Description
The technical solutions of the present invention will be described in detail below in order to clearly understand the technical features, objects, and advantages of the present invention, but the present invention is not limited to the practical scope of the present invention.
Example 1:
the embodiment provides a visual carbonate rock micro seepage model and a preparation method thereof, and the specific preparation method of the visual carbonate rock micro seepage model comprises the following steps:
(1) preparing a pore template: depending on the subject, a template of the pore structure pattern of the actual carbonate core was prepared, as shown in fig. 1.
(2) Cutting the bottom plate and the panel: according to the design size (76X 1.5 mm)3) Cutting natural ice stone (as shown in figure 2), wherein the cutting direction is perpendicular to the cleavage plane of the ice stone, and obtaining two ice stone sheets with the same size as a bottom plate and a panel (as shown in figure 3).
(3) And (3) re-engraving a pore pattern: the pattern of pore structures is replicated to the pore network regions of the backplane surface using photolithography techniques (conventional in the art).
(4) Etching the pore channel structure: taking the bottom plate which is subjected to the pore structure pattern regrooving in the step (3), performing wax sealing on the surface of the bottom plate except the pore structure pattern, then soaking the bottom plate in acid liquor to etch pore channels, then taking out the bottom plate, and removing wax; the acid solution is obtained by compounding hydrochloric acid, sulfuric acid and water, wherein the volume ratio of the hydrochloric acid to the sulfuric acid to the water is 1:1: 34.5.
(5) Cleaning the bottom plate: and (3) placing the dewaxed bottom plate into an ultrasonic cleaning machine, adding ultrapure water, cleaning for 2-3 times under ultrasonic waves, and drying.
(6) Sealing the model: and (5) coating optical UV glue on the glue coating area on the surface of the base plate dried in the step (5), slowly covering the panel on the base plate, and uniformly spreading the glue in the glue coating area of the base plate by means of the pressure of the panel.
(7) Curing the model: and (3) placing the model with the glued glue under a UV lamp for curing for at least 30min, finishing the curing operation after the glue is completely solidified, wherein the thickness of the cured glue layer is 3-5 mu m, and curing to obtain the visual carbonate rock micro seepage model (as shown in figure 4).
Example 2:
the water flooding micro seepage experiment is carried out by adopting the visual carbonate rock micro seepage model prepared in the embodiment 1. Due to the birefringent properties of naturally occurring ice stones, ghosting phenomena occur when the percolation law inside the ice stone model is directly observed. Therefore, in the course of the experiment, the directly taken photograph was subjected to the deghosting process, and the experimental results are shown in fig. 5, 6, and 7.
As can be seen from fig. 5: in the initial state of the water flooding experiment, crude oil (brown) is filled in the pores and occupies the whole pore space; as can be seen from fig. 6: after the oil displacement process, injected water occupies the pore space occupied by the original crude oil, and the crude oil is gradually produced; as can be seen from fig. 7: and (5) continuing the oil-water displacement experiment, wherein the injected water further occupies the pore space, and the oil phase is further reduced. The residual oil after water flooding exists in pores in the form of oil films and oil drops.
The water flooding microscopic seepage experiment result of the visualized carbonate rock microscopic seepage model shows that the model can truly and effectively simulate the real seepage characteristics of fluid in the carbonate rock core.
Contact angle comparison experiment:
for the micro-percolation model, the mineral composition of the pore interior surfaces can influence the micro-percolation mechanism by changing the surface wettability. Particularly, capillary force in oleophylic pores is resistance of water flooding, and a water phase is difficult to enter smaller pores; and capillary force in the hydrophilic pores is the power of water flooding, so that the recovery rate of the water flooding is higher. To verify that the ice winter stone of the present invention can better simulate the wettability and seepage laws of actual carbonate rocks, the following contact angle comparison experiment was designed.
The contact angle experiment is the most direct research means of rock surface wettability, and the contact angle on an oil-water-rock interface can be measured through an optical contact angle device, so that the wettability of the rock surface under a specific physical environment can be obtained. On the oil-water rock three-phase surface, if the contact range is between 0 and 90 degrees, the rock surface is wet; if the contact angle is in the range of 90-180 degrees, the surface of the rock is oil wet.
The comparative experiment was conducted on quartz (SiO as the main component)2) And ice winter stone (CaCO as main ingredient)3) Experimental investigation of the contact angle of two materials that can be modeled as micro-scale percolation in aqueous phase against crude oil, the experimental results are shown in fig. 8 and 9.
As can be seen from fig. 8 and 9: in aqueous phase conditions, quartz and ice winter stone have different wettabilities. In a simulated formation water (the degree of mineralization is 20000ppm) environment, the contact angle of crude oil on the surface of quartz is 50 degrees, and the surface is hydrophilic; and the contact angle of crude oil on the surface of the ice winter stone is 140 degrees, and the ice winter stone is an oleophilic surface. The carbonate reservoir is oil-wet, and the quartz glass is water-wet, so the glass model cannot simulate the wettability of the carbonate reservoir, and the seepage rule made by the glass model is difficult to conform to the seepage rule of the carbonate reservoir. According to a contact angle comparison experiment, the ice winter stone is oil-wet and consistent with the mineral composition and wettability of a carbonate reservoir, and the visual carbonate microcosmic seepage model prepared by the ice winter stone can truly simulate the wettability of an actual carbonate reservoir, so that the made seepage rule is closer to the real seepage rule of the carbonate reservoir.
Claims (11)
1. A preparation method of a visual carbonate rock micro seepage model comprises the following steps:
preparing a pore structure pattern of an actual carbonate rock core;
cutting ice winter stones to obtain two ice winter stone sheets with the same size, wherein the two ice winter stone sheets are respectively used as a bottom plate and a panel; the cutting direction of cutting the ice winter stone is perpendicular to the direction of a cleavage plane of the ice winter stone, and the thickness of the ice winter stone slice obtained by cutting is 1.5-2 mm;
marking a gluing area and a pore network area on the surface of the bottom plate;
etching the pore structure pattern to the pore network area on the surface of the bottom plate and etching the pore channel structure;
etching a sample inlet and a sample outlet communicated with the pore passage on the surface of the bottom plate, and reserving channels of the sample inlet and the sample outlet on the corresponding panel;
and after the glue coating area on the surface of the bottom plate is coated with glue, covering the bottom plate through the panel, and curing to obtain the visual carbonate rock micro seepage model.
2. A method of manufacturing as claimed in claim 1, wherein the pattern of pore structures is replicated to the pore network region of the backplane surface using photolithography techniques.
3. The method of claim 1, wherein the step of etching the channel structure comprises:
taking the bottom plate after the pore structure pattern is repeatedly engraved, performing wax sealing on the surface of the bottom plate except the pore structure pattern, then soaking the bottom plate in acid liquor to etch pore channels, then taking out the bottom plate, removing wax, and performing ultrasonic cleaning and drying.
4. The preparation method according to claim 3, wherein the acid solution is obtained by compounding hydrochloric acid, sulfuric acid and water, and the volume ratio of the hydrochloric acid to the sulfuric acid to the water is 1:1 (34.5-40).
5. The method according to claim 4, wherein the time for immersion is 15 to 20 hours.
6. The manufacturing method according to claim 1, wherein the glue used for applying the glue to the glue application area on the surface of the base plate is an optical UV glue.
7. The preparation method according to claim 6, wherein the thickness of the glue layer after the glue is cured is controlled to be 3-5 μm.
8. The preparation method according to claim 1, wherein the curing is performed by irradiation of a UV lamp, and the curing operation is completed after the glue solution is completely solidified.
9. The method according to claim 8, wherein the curing time is not less than 30 min.
10. The visualized carbonate rock micro seepage model prepared by the preparation method of any one of claims 1 to 9.
11. The use of the visualized carbonate micro-percolation model of claim 10 in studying carbonate reservoir waterflood development micro-percolation laws.
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