CN115753521A - Preparation method of microscopic seepage model - Google Patents
Preparation method of microscopic seepage model Download PDFInfo
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Abstract
The invention provides a preparation method of a microscopic seepage model, which comprises the following steps: a) Sequentially carrying out surface cleaning, laser engraving and pore cleaning on the PMMA substrate to obtain a microcosmic seepage model base plate; b) Carrying out pore surface mineral cementation on the microcosmic seepage model base plate obtained in the step a) by adopting a mineral cementing agent, and finally carrying out model encapsulation by using an encapsulation adhesive to obtain a microcosmic seepage model; the mineral cementing agent is prepared from the following raw materials: 8-15 parts of MMA powder; 3-10 parts of alpha-ethyl cyanoacrylate; 50-80 parts by weight of dichloromethane; 3 to 10 parts of p-toluenesulfonic acid. Compared with the prior art, the preparation method provided by the invention has the advantages that the acrylic seepage model is cemented by the combined action of the physical process and the chemical process, the high-strength integrated cementation between the bottom plate and the cover plate can be realized, the complete transparency and the visibility are strong, the leakage influence is avoided, and the influence of the preparation method on the geometric form of the pore space is small.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a preparation method of a microcosmic seepage model.
Background
The microcosmic seepage model technology is a technology which etches pre-designed pores and flow channels on a base material, is used for environmental monitoring, biopharmaceutical and medical detection after operations such as cementation, packaging and the like, and is very important to be applied in the field of oil and gas field development. In order to better know the characteristics of reservoirs of oil reservoirs and fluid flow characteristics, students at home and abroad propose various microscopic physical seepage models for indoor experimental research, wherein the microscopic physical seepage models comprise real core slices, glass etching models, acrylic etching models and the like. (1) The real core model is mainly packaged by a real core sheet through epoxy resin pouring or through glass, organic polymer and other materials as a splint, and can simulate seepage rules and an oil-water-rock reaction mechanism; the core slice is usually bonded with a base material, an upper cover plate, the core slice and a lower cover plate are sequentially bonded, and then the periphery of the core slice is encapsulated by an adhesive; the adhesive in the manufacturing method is easy to permeate into the pores, so that the pores of the rock core are blocked, and the research on the seepage rule in the pores is influenced; meanwhile, in a displacement experiment, water and oil are generally dyed by using a dyeing agent, but due to poor light transmittance of a real core, even though the fluid distribution and migration states in the pore passage are still difficult to observe through the auxiliary operation. (2) The glass etching model usually uses acid carving or photoetching, and the glass with the etching channel and the glass cover plate are properly bonded together in a sintering mode and a liquid glue bonding mode by heating or coating the liquid glue; the glass etching model is generally used for simulating the seepage rule and mechanism in a sandstone reservoir and is difficult to simulate the seepage rule of a carbonate reservoir; although the glass etching model has better observability, the sintering mode has high control requirement, the pore channel is melted and blocked due to high temperature, and the controllable width of the pore channel is lower; the liquid glue bonding mode is influenced by the gluing thickness, and the gluing effect is influenced by the phenomenon that the upper part is thin and the lower part is thick; meanwhile, the liquid glue is easy to block an etching pore channel, so that the seepage rule research is influenced. (3) The acrylic etching model takes an organic polymer acrylic material as a base material, a pre-designed simulation pore channel is etched on the surface of the base material through laser, and then packaging and cementing are carried out through a cover plate, and the common methods comprise hot-press packaging, cementing agent packaging and the like; the hot-pressing packaging needs to be carried out at high temperature and under larger pressure, so that the seepage channel is easy to deform and block; in the process of packaging the cementing agent, the cementing agent is easy to be embedded into the micro-channel, the chemical heat resistance is poor, the cementing agent is easy to be dissolved in oil, the pore channel is blocked, the packaging failure of the etching model is caused, and the leakage occurs; meanwhile, the surface of the acrylic material is oleophilic, and although the wettability of a carbonate reservoir can be simulated, the reaction mechanism of the acrylic material cannot be researched.
Chinese patent publication No. CN106338889A discloses a method for preparing a microscopic visual etching low-permeability model, which mainly comprises the steps of performing an exposure experiment on a glass sheet coated with a photoresist, transferring a designed pattern onto the glass sheet coated with the photoresist, and then performing the procedures of development, corrosion, photoresist removal and the like to obtain the microscopic pore model. The method comprises the following specific steps of (1) cleaning process. By mass ratio of H 2 O 2 ：H 2 SO 4 =2.5:7.5 boiling the mixture, and cleaning surface impurities with tap water, alcohol and distilled water; and then dried. And (2) a photoetching process. Adsorbing a glass sheet on a rotating table, coating a basement membrane solution on the glass sheet, uniformly dispersing, baking, coating a photoresist in a rotating manner, and then baking again to fix the glue solution; and transferring the drawn pattern onto a glass sheet coated with photoresist by exposure, placing the glass sheet in a developing solution after the exposure is finished, and developing for 5min to dissolve the glue solution in the exposure area and display the photoetching part. And (3) acid etching process. Placing the photoetched glass sheet on a glue baking plate to fix glue solution; sealing wax on the part without glue coating, and carrying out acid etching by using a buffer solution of 40% hydrofluoric acid and ammonium fluoride; scraping off wax on the surface of the glass sheet by using a blade, placing the glass sheet in a degumming solution for degumming, and repeatedly cleaning the glass sheet by using alcohol and distilled water; is prepared by. However, in the technology, a pore channel is etched on the surface of the glass by using a buffer solution of 40% hydrofluoric acid and ammonium fluoride, and the longer the time in the acid etching process is, the larger the pore is, the shorter the time is, the smaller the pore is, so that the depth and the width of the pore cannot be accurately controlled, and the repeatability of an experiment and the result of a real seepage rule in a rock core are influenced; in the displacement experiment process, particularly when the multiphase fluid flows, the multiphase fluid is difficult to distinguish under a microscope, so that the flow characteristics of the fluid cannot be really observed; in addition, the technology is researched by taking glass as a base material, and because the main component of the glass is silicon dioxide and has water-wettability, the technology can only simulate sandstone reservoirs but cannot simulate oil-wettability carbonate reservoirs.
Chinese patent publication No. CN 109827822A discloses a high-temperature high-pressure visual real rock seepage model and a manufacturing method thereof, the manufacturing process is mainly divided into four parts, i.e. bonding one face of a rock slice, stacking a lead groove dam, bonding the other face of the rock slice and glue pouring molding. And (1) sticking one surface of the rock slice. And grinding the processed rock slice to be flat, then uniformly adhering the flat surface to the glass slice by using an adhesive, and arranging a fluid inlet and a fluid outlet. And (2) stacking the guide groove dam. And (3) utilizing an adhesive to stack inlet guide grooves on the two short edges of the rock slices and the periphery of the rock slices, and simultaneously polishing the rock slices and the box dam. And (3) sticking the other surface of the rock slice. The other side of the rock laminate was glued to the center of the second glass laminate. And (4) pouring glue and forming. And filling the space between the two glass sheets and the areas at the two ends of the rock slice with the adhesive, and curing to finish the preparation. However, the technology adopts a glue-pouring forming method for packaging, and glue is easy to permeate into pores in the glue-pouring process, so that the pores are blocked, and the oil-water seepage process in the pores is influenced; meanwhile, the technology utilizes the core slice for simulation, although the core slice has visibility, the experimental phenomenon is inconvenient to observe due to the fact that the inner pore channel is disordered and the light transmittance is poor.
In summary, in the prior art, there is no preparation method for effectively realizing a microscopic seepage model for simulating the seepage rule and mechanism of an oil reservoir without affecting the structure and function of a micro-flow channel.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing a microscopic seepage model, in which an acrylic seepage model is cemented by a physical process and a chemical process, so that a high-strength integrated cementation between a bottom plate and a cover plate can be realized, the transparency and visibility are strong, no leakage effect is caused, and the influence of the preparation method on the geometrical shape of a pore is small.
The invention provides a preparation method of a microscopic seepage model, which comprises the following steps:
a) Sequentially carrying out surface cleaning, laser engraving and pore cleaning on the PMMA substrate to obtain a microcosmic seepage model base plate;
b) Carrying out pore surface mineral cementation on the microcosmic seepage model base plate obtained in the step a) by adopting a mineral cementing agent, and finally carrying out model encapsulation by using an encapsulation adhesive to obtain a microcosmic seepage model;
the mineral cementing agent is prepared from the following raw materials:
8-15 parts of MMA powder;
3-10 parts of alpha-ethyl cyanoacrylate;
50-80 parts by weight of dichloromethane;
3 to 10 parts of p-toluenesulfonic acid.
The invention provides a novel preparation and application method of a microcosmic seepage model, which comprises the design of the microcosmic seepage model capable of simulating an oil-water-rock coupling action mechanism and the technical content of the formula design of a surface mineral cementing agent and an encapsulation adhesive used in the microcosmic seepage model.
In the present invention, the process of surface cleaning in step a) is preferably embodied as follows:
sequentially using alcohol and deionized water to ultrasonically clean the PMMA substrate for 2-4 times respectively, and each time lasts for 4-6 min; and then dried at normal temperature.
In the present invention, the laser engraving process in step a) is preferably specifically:
a1 Wax sealing: placing the dried substrate sheet on a rotating table of a glue homogenizing machine, setting the temperature to be 60-70 ℃, taking molten paraffin by using a glue dropper to coat the molten paraffin on the surface of the substrate so as to completely cover the surface of the substrate, starting the glue homogenizing machine to uniformly disperse the paraffin, then taking down the substrate, and cooling at normal temperature so as to make the paraffin adhere to the substrate sheet to form a smooth thin wax film with the thickness of less than 1 mu m;
a2 Preparation of a pattern of micro-pore structures: the pore pattern is taken from a real core section scanning picture, and the porosity range of the core scanning picture is 10-30%;
a3 Processing of microscopic model: and (3) processing the PMMA substrate by using a laser engraving machine according to the prepared geometric pattern of the pore canal of the real rock core to obtain the engraved microcosmic seepage model base plate.
In the invention, the laser power of the laser engraving machine in the step a 3) is preferably 35-40%, and the moving speed is preferably 250-300 mm/min.
In the present invention, the cleaning process of the pore channel in the step a) is preferably specifically:
firstly, cleaning the surface of a pore channel for 2 to 4 times by using alcohol and a brush, wherein each time lasts for 4 to 6min; then, ultrasonically cleaning the PMMA bottom plate by using alcohol and deionized water for 2-4 times respectively, wherein each time lasts for 4-6 min; and drying at normal temperature to obtain the microcosmic seepage model base plate.
In the invention, the mineral cementing agent in the step b) is prepared from the following raw materials:
8-15 parts of MMA powder;
3-10 parts of alpha-ethyl cyanoacrylate;
50-80 parts of dichloromethane;
3-10 parts of p-toluenesulfonic acid;
preferably prepared from the following components:
8-12 parts of MMA powder;
3-5 parts of alpha-ethyl cyanoacrylate;
60-70 parts by weight of dichloromethane;
3 to 7 parts of p-toluenesulfonic acid.
In the invention, the preparation method of the mineral cementing agent is preferably as follows:
MMA powder, alpha-ethyl cyanoacrylate, dichloromethane and p-toluenesulfonic acid are mixed, the mixture is continuously stirred for 1min to 5min at the rotating speed of 150r/min to 250r/min by using a stirrer under the condition of air isolation, and the mixture is kept stand to obtain the mineral cementing agent.
In the present invention, the mineral cementation process on the surface of the pores in the step b) is preferably embodied as follows:
taking 0.5-1 ml of mineral cementing agent, uniformly coating the mineral cementing agent on the pore surface of the microcosmic seepage model base plate, and waiting for 1-3 min; purging surface pores by using nitrogen, and cleaning residual mineral cementing agent; then taking nano CaCO 3 Powder or nano SiO 2 Powder is evenly sprayed on the surface of the bottom plate, and the thickness of the powder exceeds the depth of the pores of the bottom plate by 0.5-1.5 mm; placing the sprayed base material into a tabletting machine for pressing, wherein the pressure is set to be 0.5-1 MPa, the temperature is 20-30 ℃, and the pressing time is 5-15 min; after taking out the base material, cleaning the residual mineral powder on the surface of the base material and in the pores by using alcohol and deionized water in sequence, wherein the cleaning is carried out for 2-4 times and 4-6 min each time; and then drying at normal temperature to complete the surface cementation of minerals.
In the present invention, the packaging adhesive in step b) is preferably prepared from raw materials comprising the following components:
0.75 to 4 weight portions of MMA powder;
2-4 parts of formic acid;
2-4 parts of methanol;
3-10 parts of dichloromethane;
more preferably prepared from the following components:
0.75 to 1.25 parts by weight of MMA powder;
2-4 parts of formic acid;
2-4 parts of methanol;
3-7 parts of dichloromethane.
In the present invention, the preparation method of the packaging adhesive is preferably as follows:
mixing MMA powder, formic acid, methanol and dichloromethane, continuously stirring for 1-5 min at the rotating speed of 150-250 r/min by using a stirrer under the condition of isolating air, and standing to obtain the mineral cementing agent.
In the present invention, the process of encapsulating the model in step b) is preferably as follows:
wiping off the residual wax thin layer on the surface of the carved base plate by alcohol at the temperature of 40-60 ℃ for 2-4 times, and each time is 4-6 min; 2-3 ml of packaging adhesive is uniformly smeared on the surfaces of the cover plate and the bottom plate, and is kept stand for 2-5 min, so that the packaging adhesive is fully reacted with the surfaces of the cover plate and the bottom plate respectively; aligning and fixing the cover plate and the bottom plate, putting the cover plate and the bottom plate into a tabletting machine, and uniformly applying pressure with the pressure of 0.2-0.7 MPa; the tablet press is then immediately placed in a vacuum oven at 10 -1 Pa～10 -5 And discharging the packaging adhesive remained in the pores out of the seepage model under the vacuum condition of Pa, wherein the setting temperature of the vacuum environment is 50-80 ℃, and the time is 10-20 min, so as to obtain the microscopic seepage model.
The invention provides a novel PMMA cementing agent and a cementing method, which are used for cementing an acrylic seepage model under the combined action of a physical process and a chemical process; the high-strength integrated cementation between the bottom plate and the cover plate can be realized, the transparent and visible performance is high, the leakage influence is avoided, and the cementation method has small influence on the geometric shape of the pore. Wherein:
(1) The chemical process comprises the following steps: the cementing agent promotes and inhibits hydrolysis reaction by adding and reducing reactants so as to control cementing effect. Formula (1) is the MMA monomer esterification equation, usually in concentrated H 2 SO 4 The reaction speed is accelerated by heating and catalyzing, and the reaction process is reversible. MMA monomer, i.e. CH 2 C(CH 3 )COOCH 3 Is easy to be hydrolyzed into CH when meeting strong acid 2 C(CH 3 ) COOH and CH 3 And (5) OH. Therefore, in view of this reversible reaction, the reaction product methanol and the volatile acid (formic acid) are added to the solution to accelerate the hydrolysis reaction. In the cementing process, formic acid, methanol and dichloromethane are gradually volatilized, and the MMA esterification reaction is regenerated, so that the integrated cementing is completed.
(2) Physical process: because dichloromethane has stronger solubility to MMA monomer, MMA is dissolved in dichloromethane, methanol and formic acid mixed solution, and after dichloromethane, methanol and formic acid volatilize, the dissolved MMA is solidified, and the micro seepage model cementation is completed.
At present, most seepage models can only research the fluid migration rule in a rock pore system, and the invention provides a novel PMMA surface mineral (nano SiO) 2 Or CaCO 3 Powder) cementing agent and cementing method, which can solve the problem that the micro-seepage model can not research the oil-water-rock coupling mechanism.
The cementing agent takes alpha-ethyl cyanoacrylate and MMA as main active ingredients, wherein the alpha-ethyl cyanoacrylate is used for H 2 O is very sensitive and can be in H 2 And O is catalyzed to rapidly polymerize. P-toluenesulfonic acid is generally used as a stabilizer for polymerization, a catalyst for organic synthesis (esters and the like), and a stabilizer curing agent, and has strong water-extraction property. By adding p-toluenesulfonic acid into the solution, the polymerization reaction speed of alpha-ethyl cyanoacrylate can be reduced, the cementing time with minerals is prolonged, the cementing effect on mineral powder is enhanced, and the influence of the mineral cementing process on the depth of pores can be reduced.
Aiming at the defects of high research threshold, high cost of related equipment and processing environment and the like of the existing microcosmic seepage model technology, the invention utilizes the PMMA material with low cost to carry out carving and packaging, and compared with the traditional microfluidic technology, the invention is expected to obviously reduce the processing cost of a chip and the requirements of the processing process on precise equipment and environment.
Drawings
FIG. 1 is a technical route diagram of a method for preparing a micro-seepage model according to an embodiment of the present invention;
FIG. 2 is a schematic representation of a pore pattern of a micro-seepage model in an embodiment of the present invention, wherein (a) a base plate, (b) a cover plate;
FIG. 3 is a schematic diagram of a carved PMMA substrate base plate in the example of the present invention;
FIG. 4 is a pictorial view of a backing plate in an embodiment of the invention in which (a) the backing plate is unconsolidated with a surface mineral, (b) the backing plate is in the process of consolidating a mineral, and (c) the backing plate is after consolidating a mineral;
FIG. 5 is a cross-sectional micrograph of a microscopic seepage pattern after encapsulation according to an embodiment of the present invention;
FIG. 6 is a schematic illustration of mineral cementation at the surface of the pores;
FIG. 7 is a view of a micro seepage model after saturating crude oil and an application example.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood 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.
Examples
(1) Cleaning the surface of PMMA:
the surface of the PMMA substrate is clean, and organic pollutants remained on the surface of the PMMA substrate are removed to the maximum extent. Ultrasonic cleaning PMMA substrate with alcohol and deionized water for 5min each 3 times; and then dried at normal temperature.
(2) Laser engraving:
(1) wax sealing:
and (2) placing the dried substrate sheet on a rotating table of a glue homogenizing machine, setting the temperature to 65 ℃, taking molten paraffin by using a glue dropper to coat the molten paraffin on the surface of the substrate so as to completely cover the surface of the substrate, starting the glue homogenizing machine to uniformly disperse the paraffin, then taking down the substrate, and cooling at normal temperature so as to adhere the paraffin on the substrate sheet to form a smooth thin wax film with the thickness of less than 1 mu m.
(2) Preparation of the pattern of the microscopic pore structure:
the porosity pattern is obtained from a real core section scanning picture, the porosity range of the core scanning picture can be 10% -30%, and the porosity of the core scanning picture in the experiment is about 20.37%, as shown in fig. 2.
(3) Processing of the microscopic model:
and (3) processing the PMMA base material according to the designed geometric pattern of the duct of the real core by using a laser engraving machine. The laser power and the engraving rate were adjusted and set as shown in table 1, and the effect of etching the channels was determined by both the laser power and the moving rate. According to different schemes, the moving speed is 250mm/min, the laser power is 35% and 40%, the basic hole depth requirement can be met, and the optimal carving effect is selected according to the final effect comparison. Therefore, the laser power of 35% and the moving speed of 250mm/min are preferably set as the engraving parameters of the PMMA plate. Fig. 3 shows the pore channel with the carved surface, which is seen from the carved microcosmic seepage model base plate of the PMMA material under the parameter, the flow channel is distributed uniformly, the base material is smooth and has no melting and burning through, and the depth of the pore channel is about 100 μm.
TABLE 1 laser power and engraving Rate Effect
(3) Cleaning a pore channel:
the etched pore surfaces are left with debris as the surfaces are engraved by the laser. Cleaning the surface of the pore channel with alcohol and a brush for 5min for 3 times; then, ultrasonically cleaning the PMMA bottom plate by using alcohol and deionized water for 3 times respectively, and 5min each time; drying at normal temperature to remove the PMMA particles remained on the surface to the maximum extent.
(4) Mineral cementation on the surface of pores:
(1) preparing a mineral cementing agent:
MMA powder, ethyl α -cyanoacrylate, methylene chloride, p-toluenesulfonic acid were mixed in the proportions shown in Table 2 below, continuously stirred for 3min at 200r/min with air excluded, allowed to dissolve sufficiently, and left to stand for use. The larger the MMA is, the less the dichloromethane is, the larger the viscosity of the mineral cementing agent is, and the poorer the fluidity is; the larger the mass part of the alpha-ethyl cyanoacrylate is, the faster the cementation speed is; the larger the mass fraction of p-toluenesulfonic acid, the lower the bonding strength. Preferably, the mass parts of MMA, alpha-ethyl cyanoacrylate, dichloromethane and p-toluenesulfonic acid are 8-15, 3-10, 50-80 and 3-10 respectively, wherein the optimal proportion is 10, 5, 65 and 5, and the optimal mineral cementation effect can be achieved.
TABLE 2 proportioning of mineral cementing agent solution by weight parts
(2) And (3) surface mineral cementation:
taking 0.8ml of the mineral cementing agent solution prepared in the step (1), uniformly coating the solution on the surface of the etched substrate pores, and waiting for 2min; and (4) purging the surface pores by using nitrogen, and cleaning the residual mineral cementing agent. Taking nano CaCO 3 Powder is evenly sprayed on the surface of the bottom plate, and the thickness of the powder exceeds the depth of the pores of the bottom plate by about 0.5mm to 1.5mm; placing the sprayed base material into a tabletting machine, setting the pressure at 0.5-1 MPa and the pressure at 25 ℃ for 5-15 min; after taking out the substrate, cleaning the residual mineral powder on the surface of the substrate and in the pores by using alcohol and deionized water in sequence, wherein the cleaning is carried out for 5min each time for 3 times; and then drying at normal temperature to complete the surface cementation of the minerals. Nano CaCO 3 When the thickness of the powder is too large or too small, the powder cannot be effectively embedded into the surface of the pore channel under the pressure action of a tablet press to complete cementation, and the effect is worse; when the pressure of the tablet press is lower, the embedding effect is poorer, and the base material is easily deformed and damaged when the pressure is higher. Preference is therefore given to using nano-CaCO 3 The powder is uniformly sprayed to a thickness exceeding the thickness of the pores by about 1mm, the pressing pressure is 0.7MPa, the pressing time is 10min, and the optimal effect can be achieved.
(5) Preparing an encapsulating adhesive:
MMA powder, formic acid, methanol, and methylene chloride were mixed in the proportions shown in Table 3 below; keeping stirring for 3min at 200r/min with a stirrer in the absence of air to dissolve completely, and standing for use. The methanol can reduce the corrosion and the solubility of methylene dichloride to PMMA, is volatile in the bonding process, reduces the influence on the bonding effect, and can promote the esterification reaction when being used as a reactant; formic acid may promote hydrolysis of MMA. The less the mass part of the dichloromethane is, the poorer the physical dissolving effect on the PMMA substrate is; the more the dichloromethane is in parts by mass, the stronger the physical dissolution effect on the PMMA substrate is, and the greater the influence on the pore depth is; too much or too little methanol or formic acid content directly affects the chemical solubility of MMA. Therefore, the optimal proportion of the MMA powder, the formic acid, the methanol and the dichloromethane in parts by mass is 0.75-4, 2-4 and 3-10, wherein the optimal proportion is 1, 3 and 5, and the optimal effect can be achieved after the components are mixed, and the depth of pores is hardly influenced.
TABLE 3 mixture ratio of adhesives in parts by weight
(6) Packaging a microscopic seepage model:
table 4 shows the effect on the pore depth for different bonding conditions. The main factors influencing the bonding effect of the micro seepage model comprise bonding time, bonding temperature and applied pressure. The longer the bonding time is, the better the bonding effect is; too high or too low a bonding temperature can lead to adhesive failure; the higher the bonding pressure is, the larger the influence on the hole depth of the pore channel is, and the microscopic model with too small pressure cannot be bonded completely, so that the leakage phenomenon is easy to occur.
And (3) wiping off the residual wax thin layer on the surface of the carved base plate by using alcohol at 50 ℃ for 5min each time, and ensuring that the wax thin layer on the surface is completely removed. Uniformly coating 2.5ml of adhesive on the surfaces of the cover plate and the bottom plate, and standing for 3min to ensure that the adhesive is fully reacted with the surfaces of the cover plate and the bottom plate; aligning and fixing the cover plate and the bottom plate, putting the cover plate and the bottom plate into a tabletting machine, and uniformly applying pressure with the pressure of 0.2-0.7 MPa; the tablet press is then immediately placed in a vacuum oven at 10 -3 The packaging adhesive remained in the pores can be discharged out of the seepage model under the vacuum condition of Pa, and the setting temperature of the vacuum environment is 50-80 ℃ for 10-20 min. The preferable bonding pressure is 0.5MPa, the bonding temperature is 70 ℃, the bonding time is 15min, the bonded micro seepage model has no swelling cracking, and the influence on the aperture is small and is about 1 mu m; a cross-sectional micrograph of the microscopic seepage pattern after encapsulation in an embodiment of the invention is shown in fig. 5.
TABLE 4 reduction in pore thickness under different bonding conditions
The technical scheme provided by the invention has the following beneficial effects:
(1) According to the formula of the packaging cementing agent provided by the invention, the acrylic base plate and the cover plate are cemented by the optimized packaging cementing agent to form a seepage model, and the cementing agent can avoid strong corrosion on the base plate and the cover plate to influence the geometric form of a pore channel.
(2) According to the micro seepage model prepared by the pore surface mineral cementing agent and the cementing method, oil-water-rock interaction simulation which is difficult to realize in the existing method can be realized, a coupling mechanism between oil-water-rock can be analyzed directly through the micro seepage model, and fig. 6 is a schematic diagram of surface mineral cementing.
(3) According to the packaging technical process provided by the invention, the influence of the packaging process on the depth of the pore can be reduced to the minimum degree by controlling the pressure, the temperature and the duration of the tablet press, and meanwhile, the packaged microcosmic seepage model is free from swelling, cracking and whitening, and an application effect diagram is shown in FIG. 7.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A preparation method of a micro seepage model comprises the following steps:
a) Sequentially carrying out surface cleaning, laser engraving and pore cleaning on the PMMA substrate to obtain a microcosmic seepage model base plate;
b) Carrying out pore surface mineral cementation on the microcosmic seepage model base plate obtained in the step a) by adopting a mineral cementing agent, and finally carrying out model encapsulation by using an encapsulation adhesive to obtain a microcosmic seepage model;
the mineral cementing agent is prepared from the following raw materials:
8-15 parts of MMA powder;
3-10 parts of alpha-ethyl cyanoacrylate;
50-80 parts by weight of dichloromethane;
3 to 10 parts of p-toluenesulfonic acid.
2. The method for preparing the nano-particles according to claim 1, wherein the surface cleaning process in the step a) is specifically as follows:
sequentially using alcohol and deionized water to ultrasonically clean the PMMA substrate for 2-4 times respectively, and each time lasts for 4-6 min; and then dried at normal temperature.
3. The preparation method according to claim 1, wherein the laser engraving process in step a) is specifically:
a1 Wax sealing: placing the dried substrate sheet on a rotating table of a spin coater, setting the temperature to be 60-70 ℃, using a rubber head dropper to take molten paraffin to be smeared on the surface of the substrate so as to completely cover the surface of the substrate, starting the spin coater to uniformly disperse the paraffin, then taking down the substrate, and cooling at normal temperature so as to enable the paraffin to be adhered on the substrate sheet to form a smooth thin wax film with the thickness of less than 1 mu m;
a2 Preparation of a pattern of micro-pore structures: the pore pattern is taken from a real core section scanning picture, and the porosity range of the core scanning picture is 10-30%;
a3 Processing of microscopic model: and (3) processing the PMMA substrate by using a laser engraving machine according to the prepared geometric pattern of the pore canal of the real rock core to obtain the engraved microcosmic seepage model base plate.
4. The preparation method according to claim 3, wherein the laser power of the laser engraving machine in the step a 3) is 35-40%, and the moving speed is 250-300 mm/min.
5. The method according to claim 1, wherein the cleaning of the pore channels in step a) is performed by:
firstly, cleaning the surface of a pore channel for 2 to 4 times by using alcohol and a brush, wherein each time lasts for 4 to 6min; then, ultrasonically cleaning the PMMA bottom plate by using alcohol and deionized water for 2-4 times respectively, wherein each time lasts for 4-6 min; and drying at normal temperature to obtain the microcosmic seepage model base plate.
6. The method of claim 1, wherein the method of preparing the mineral binder in step b) is specifically:
MMA powder, alpha-ethyl cyanoacrylate, dichloromethane and p-toluenesulfonic acid are mixed, the mixture is continuously stirred for 1min to 5min at the rotating speed of 150r/min to 250r/min by using a stirrer under the condition of air isolation, and the mixture is kept stand to obtain the mineral cementing agent.
7. The preparation method according to claim 1, wherein the pore surface mineral cementation in the step b) is specifically carried out by:
taking 0.5-1 ml of mineral cementing agent, uniformly coating the mineral cementing agent on the pore surface of the microcosmic seepage model base plate, and waiting for 1-3 min; purging surface pores by using nitrogen, and cleaning residual mineral cementing agent; then taking nano CaCO 3 Powder or nano SiO 2 Powder is evenly sprayed on the surface of the bottom plate, and the thickness of the powder exceeds the depth of the pores of the bottom plate by 0.5 mm-1.5 mm; placing the sprayed base material into a tabletting machine for pressing, wherein the pressure is set to be 0.5-1 MPa, the temperature is 20-30 ℃, and the pressing time is 5-15 min; after the base material is taken out, sequentially cleaning the mineral powder remained on the surface and in the pores of the base material by using alcohol and deionized water for 2-4 times, and 5min each time; and then drying at normal temperature to complete the surface cementation of minerals.
8. The method of claim 1, wherein the packaging adhesive in step b) is prepared from raw materials comprising the following components:
0.75 to 4 weight portions of MMA powder;
2-4 parts of formic acid;
2-4 parts of methanol;
3-10 parts of dichloromethane.
9. The method according to claim 8, wherein the method for preparing the packaging adhesive comprises:
mixing MMA powder, formic acid, methanol and dichloromethane, continuously stirring for 1-5 min at the rotating speed of 150-250 r/min by using a stirrer under the condition of air isolation, and standing to obtain the mineral cementing agent.
10. The method according to claim 1, wherein the step b) of encapsulating the mold comprises:
wiping off the residual wax thin layer on the surface of the carved base plate by alcohol at 40-60 ℃ for 2-4 times, and each time is 4-6 min; 2-3 ml of packaging adhesive is uniformly smeared on the surfaces of the cover plate and the bottom plate, and is kept stand for 2-5 min, so that the packaging adhesive is fully reacted with the surfaces of the cover plate and the bottom plate respectively; aligning and fixing the cover plate and the bottom plate, putting the cover plate and the bottom plate into a tabletting machine, and uniformly applying pressure with the pressure of 0.2-0.7 MPa; the tablet press is then immediately placed in a vacuum oven at 10 -1 Pa～10 -5 And discharging the packaging adhesive remained in the pores out of the seepage model under the vacuum condition of Pa, wherein the setting temperature of the vacuum environment is 50-80 ℃, and the time is 10-20 min, so as to obtain the microscopic seepage model.
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