CN114906855B - Preparation method of visual artificial rock core for displaying fingering phenomenon - Google Patents
Preparation method of visual artificial rock core for displaying fingering phenomenon Download PDFInfo
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- CN114906855B CN114906855B CN202210519973.0A CN202210519973A CN114906855B CN 114906855 B CN114906855 B CN 114906855B CN 202210519973 A CN202210519973 A CN 202210519973A CN 114906855 B CN114906855 B CN 114906855B
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- 239000011435 rock Substances 0.000 title claims abstract description 52
- 230000000007 visual effect Effects 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000499 gel Substances 0.000 claims abstract description 102
- HWYHZTIRURJOHG-UHFFFAOYSA-N luminol Chemical class O=C1NNC(=O)C2=C1C(N)=CC=C2 HWYHZTIRURJOHG-UHFFFAOYSA-N 0.000 claims abstract description 71
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 53
- 229960002413 ferric citrate Drugs 0.000 claims abstract description 22
- NPFOYSMITVOQOS-UHFFFAOYSA-K iron(III) citrate Chemical compound [Fe+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NPFOYSMITVOQOS-UHFFFAOYSA-K 0.000 claims abstract description 22
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 21
- 239000000126 substance Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000012986 modification Methods 0.000 claims abstract description 11
- 230000004048 modification Effects 0.000 claims abstract description 11
- 239000000741 silica gel Substances 0.000 claims abstract description 9
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 9
- 238000000465 moulding Methods 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 84
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 57
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims description 48
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 43
- 239000002904 solvent Substances 0.000 claims description 39
- 238000003756 stirring Methods 0.000 claims description 32
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 24
- 239000005051 trimethylchlorosilane Substances 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000007864 aqueous solution Substances 0.000 claims description 17
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 13
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 13
- 238000001723 curing Methods 0.000 claims description 12
- 230000002209 hydrophobic effect Effects 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 11
- 238000007789 sealing Methods 0.000 claims description 9
- 238000002791 soaking Methods 0.000 claims description 9
- UMULKNIDVSBBLE-UHFFFAOYSA-N 3-aminobenzene-1,2-dicarbohydrazide Chemical compound NNC(=O)C1=CC=CC(N)=C1C(=O)NN UMULKNIDVSBBLE-UHFFFAOYSA-N 0.000 claims description 5
- YDROOKPRUYAZGR-UHFFFAOYSA-N 5-amino-2-(hydrazinecarbonyl)benzoic acid Chemical compound NC=1C=C(C(C(=O)NN)=CC1)C(=O)O YDROOKPRUYAZGR-UHFFFAOYSA-N 0.000 claims description 4
- LEOJISUPFSWNMA-UHFFFAOYSA-N ABEI Chemical compound O=C1NNC(=O)C=2C1=CC(N(CCCCN)CC)=CC=2 LEOJISUPFSWNMA-UHFFFAOYSA-N 0.000 claims description 4
- 239000012530 fluid Substances 0.000 abstract description 19
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 abstract description 16
- 239000000377 silicon dioxide Substances 0.000 abstract description 16
- 230000008569 process Effects 0.000 abstract description 14
- 238000004088 simulation Methods 0.000 abstract description 13
- 239000011148 porous material Substances 0.000 abstract description 11
- 230000009471 action Effects 0.000 abstract description 5
- 230000037396 body weight Effects 0.000 abstract 1
- 238000011049 filling Methods 0.000 description 8
- 239000000443 aerosol Substances 0.000 description 6
- 238000004020 luminiscence type Methods 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- HRFDKUFUQJBSOW-UHFFFAOYSA-N 3-hydrazinylaniline Chemical compound NNC1=CC=CC(N)=C1 HRFDKUFUQJBSOW-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000010779 crude oil Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000012800 visualization Methods 0.000 description 2
- 239000011800 void material Substances 0.000 description 2
- 239000004965 Silica aerogel Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- 238000004391 petroleum recovery Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/157—After-treatment of gels
- C01B33/158—Purification; Drying; Dehydrating
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/157—After-treatment of gels
-
- G—PHYSICS
- G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
- G09B—EDUCATIONAL OR DEMONSTRATION APPLIANCES; APPLIANCES FOR TEACHING, OR COMMUNICATING WITH, THE BLIND, DEAF OR MUTE; MODELS; PLANETARIA; GLOBES; MAPS; DIAGRAMS
- G09B25/00—Models for purposes not provided for in G09B23/00, e.g. full-sized devices for demonstration purposes
Abstract
The invention discloses a preparation method of a visual artificial core for displaying a fingering phenomenon, which is implemented according to the following steps: step 1, preparing KH560 modified luminol; step 2, preparing gel; step 3, carrying out gel modification on the gel prepared in the step 2; and 4, curing and molding the gel prepared in the step 3 to form the artificial rock core. According to the invention, the visual artificial rock core with high simulation degree and simple process is obtained by introducing the substance with the chemiluminescence potential into the silicon dioxide gel and forming the pore throat structure of the porous structure simulation rock core by using the silicon dioxide gel in the curing and forming process. The chemiluminescence phenomenon of the rock core is that the alkaline fluid containing hydrogen peroxide contacts with the modified luminol on the surface of the rock core pore channel in the advancing process of the rock core in the pore space environment, and the chemiluminescence phenomenon is displayed under the action of the ferric citrate which is the silica gel body weight, so that the three-dimensional fingering phenomenon of the fluid is clearly displayed.
Description
Technical Field
The invention belongs to the technical field of oil and gas reservoir development, and relates to a preparation method of a visual artificial core for displaying fingering phenomenon.
Background
Viscous fingering is a phenomenon of interfacial instability that occurs when a fluid of greater viscosity is displaced by a fluid of lesser viscosity, and is called fingering because the interface between the two phases advances non-uniformly like a "finger". In the process of oil field development, other fluids are required to be injected to displace crude oil, and the viscous fingering phenomenon enables a large amount of crude oil to remain underground due to unswept, so that the displacement efficiency is reduced, and further the petroleum recovery efficiency is reduced. Therefore, the method utilizes the micro model to simulate and research the viscous fingering phenomenon and has important significance for deepening the understanding of the chemical flooding micro seepage mechanism and improving the development effect of the oil and gas field.
At present, chemical flooding theory and technology are usually researched through physical simulation experiments, and compared with field experiments, the model has the advantages of low cost, short time, repeatability and the like. The selection of the artificial rock core in the physical simulation experiment is very important, and particularly, the selection of the visual artificial rock core is beneficial to the deep research of the chemical flooding seepage theory. At present, a common visual artificial core is mainly a glass simulation core, the glass simulation core reflects a real pore structure by carving a pore canal on a glass model, but the throat diameter of the structure of the glass simulation core is large, the physicochemical property of the pore surface of a real stratum is difficult to reflect, the visual degree is limited, and the application and research of the visual artificial core are severely limited. Therefore, the development of a visual artificial core with high simulation degree, high visualization degree, simple preparation process and low cost is urgently needed.
Disclosure of Invention
The invention aims to provide a preparation method of a visual artificial rock core for displaying a finger advance phenomenon, and solves the problems of low simulation degree and difficult manufacturing process of the visual artificial rock core prepared by the prior art.
The technical scheme adopted by the invention is that the preparation method of the visual artificial core for displaying the fingering phenomenon is implemented according to the following steps:
step 1, preparing KH560 modified luminol;
step 2, preparing gel;
step 3, carrying out gel modification on the gel prepared in the step 2;
and 4, curing and molding the gel prepared in the step 3 to form the artificial rock core.
The present invention is also characterized in that,
the step 1 is implemented according to the following steps: dissolving luminol in 0.001mol/L aqueous solution of sodium hydroxide, and adding ethanol solution of gamma-glycidoxypropyltrimethoxysilane, wherein the molar ratio of the gamma-glycidoxypropyltrimethoxysilane to the luminol is 1:1.0 to 1.1, reacting for 2 hours at the temperature of 25 ℃, and distilling under reduced pressure to remove the solvent to obtain the KH560 modified luminol.
The step 2 is implemented according to the following steps: adding tetraethoxysilane, ethanol and water into a flask provided with a stirring device, uniformly mixing, then dropwise adding 0.5mol/L acetic acid aqueous solution, adjusting the pH of the system to 2-3, continuously stirring for 60min to obtain silicic acid sol, adding ferric citrate into the silicic acid sol, uniformly stirring, adding 0.01mol/L sodium hydroxide aqueous solution, adjusting the pH of the system to 6-7, and stirring for 30min to obtain gel.
Step 3 is specifically implemented according to the following steps: mixing the KH560 modified luminol prepared in the step 1 with trimethylchlorosilane/n-hexane, soaking the gel obtained in the step 2 in trimethylchlorosilane/n-hexane and KH560 modified luminol/ethanol, sealing, placing in an oven, reacting at 20-40 ℃ for 24-48 h to obtain hydrophobic modified silica gel carrying luminescent substances, and pouring a gel system containing a solvent to remove a large amount of the solvent to obtain the silica gel.
And 4, filling the silicon dioxide gel prepared in the step 3 into a rock core mould, then placing the rock core mould into a constant-temperature oven for gradual drying, and forming the artificial rock core framework structure through drying, curing and molding the silicon dioxide gel.
In the step 1, luminol adopts any one of 3-amino-phenylhydrazine, N- (4-aminobutyl) -N-ethyl isoluminol and 4-aminophthalic hydrazide.
In the step 2, the molar ratio of ethyl orthosilicate, ethanol and water is 1.
In the step 2, the addition amount of ferric citrate accounts for 0.2-0.4 wt% of the amount of ethyl orthosilicate in the silicic acid sol;
in the step 3, the addition amount of the trimethylchlorosilane accounts for 1-15 wt% of the amount of the ethyl orthosilicate in the gel.
In the step 3, the addition amount of the KH560 modified luminol accounts for 0.2-0.5 wt% of the amount of the ethyl orthosilicate in the gel.
The invention has the beneficial effects that: the invention relates to a preparation method of a visual artificial rock core for displaying fingering phenomena, which is characterized in that alkaline fluid containing hydrogen peroxide contacts modified luminol on the surface of a rock core pore channel in the advancing process of an artificial rock core in a gap environment, and shows chemiluminescence phenomena under the action of ferric citrate of silica gel, so that the three-dimensional fingering phenomena of the fluid can be displayed clearly, and the three-dimensional visual display of the fingering phenomena of the fluid in the advancing process of the gap environment is realized by utilizing the chemiluminescence potential of the artificial rock core. The artificial rock core surface layer provided by the invention can simulate the rock core wetting degree under different conditions through modification treatment of trimethylchlorosilane with different contents, and through the artificial rock core simulation of preparing the silica aerogel with luminous potential, the three-dimensional shape of the water-driving front appears according to light rays to show an obvious fingering phenomenon so as to adjust the oil deposit injection and production, and the artificial rock core with lower price, simple manufacturing process and high simulation degree can be prepared.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The invention relates to a preparation method of a visual artificial core for displaying finger advance phenomenon, which is implemented according to the following steps:
step 1, preparing KH560 modified luminol;
the specific process of the step 1 is as follows:
dissolving luminol in 0.001mol/L aqueous solution of sodium hydroxide, and adding ethanol solution of gamma-glycidoxypropyltrimethoxysilane, wherein the molar ratio of the gamma-glycidoxypropyltrimethoxysilane to the luminol is 1: 1.0-1.1, reacting for 2h at 25 ℃, and distilling under reduced pressure to remove the solvent to obtain the KH560 modified luminol.
The luminol is any one of 3-amino-phenylhydrazine, N- (4-aminobutyl) -N-ethyl isoluminol and 4-aminophthalic hydrazide.
KH560 modified luminol is prepared by reacting gamma-glycidoxypropyltrimethoxysilane (KH 560) with luminol in the presence of alkaline catalyst sodium hydroxide, wherein the molar ratio of KH560 to luminol is 1: (1-1.1) and the reaction temperature is 25 ℃, thus obtaining the KH560 modified luminol.
Step 2, preparing gel;
adding tetraethoxysilane, ethanol and water into a flask provided with a stirring device, uniformly mixing, then dropwise adding 0.5mol/L acetic acid aqueous solution, adjusting the pH of the system to 2-3, continuously stirring for 60min to obtain silicic acid sol, adding ferric citrate into the silicic acid sol, uniformly stirring, adding 0.01mol/L sodium hydroxide aqueous solution, adjusting the pH of the system to 6-7, and stirring for 30min to obtain gel.
Wherein the molar ratio of ethyl orthosilicate, ethanol and water is 1;
step 3, carrying out gel modification on the gel prepared in the step 2;
mixing the KH 560-modified luminol/ethanol prepared in the step 1 with trimethylchlorosilane/n-hexane, soaking the gel obtained in the step 2 in the trimethylchlorosilane/n-hexane and the KH 560-modified luminol/ethanol, sealing, placing in an oven, reacting for 24-48 h at 20-40 ℃ to obtain hydrophobic modified silica gel carrying luminescent substances, and pouring a gel system containing a solvent to remove a large amount of the solvent to obtain the silica gel.
The hydrophobic modified silica gel is formed by the reaction of trimethylchlorosilane and gel, the using amount of the trimethylchlorosilane determines the hydrophilicity and hydrophobicity of the artificial rock core, wherein the adding amount of the trimethylchlorosilane accounts for 1-15 wt% of the amount of ethyl orthosilicate in the gel, the silica gel has luminous potential due to the introduction of the modified luminol, and the adding amount of the KH560 modified luminol accounts for 0.2-0.5 wt% of the amount of the ethyl orthosilicate in the gel.
Step 4, solidifying and molding the gel prepared in the step 3 to form an artificial rock core;
and (3) filling the silicon dioxide gel prepared in the step (3) into a rock core mould, then placing the rock core mould into a constant-temperature oven for gradual drying, and forming the skeleton structure of the artificial rock core in drying, curing and molding of the silicon dioxide gel.
The visual artificial rock core for displaying the fluid fingering phenomenon is prepared, a substance with chemiluminescence potential is introduced into the silicon dioxide gel, and the silicon dioxide gel is utilized to form a pore throat structure of the porous structure simulation rock core in the curing and forming process, so that the visual artificial rock core with high simulation degree and simple process is obtained.
The chemical luminescence phenomenon of the visual artificial rock core for displaying the fluid fingering phenomenon is that the alkaline fluid containing hydrogen peroxide contacts the modified luminol on the surface of a rock core pore channel in the advancing process of the alkaline fluid in the rock core void environment, and the chemical luminescence phenomenon is displayed under the action of ferric citrate which is silicon dioxide gel weight, and the phenomenon can clearly display the three-dimensional fingering phenomenon of the fluid.
Example 1
The preparation method of the visual artificial core for displaying the fingering phenomenon is implemented according to the following steps:
step 1, preparing KH560 modified luminol, dissolving 3-amino-benzenedicarboxhydrazide in 0.001mol/L aqueous sodium hydroxide solution, and adding an ethanol solution of gamma-glycidoxypropyltrimethoxysilane (KH 560), wherein the molar ratio of KH560 to luminol is 1:1.0, reacting for 2h at 25 ℃, and distilling under reduced pressure to remove the solvent to obtain KH560 modified luminol.
Step 2, preparing gel, namely adding tetraethoxysilane, ethanol and water into a flask provided with a stirring device, wherein the molar ratio of tetraethoxysilane to ethanol to water is 1; adding ferric citrate into the silicic acid sol, and uniformly stirring, wherein the addition amount of the ferric citrate accounts for 0.2wt% of the amount of the ethyl orthosilicate; and adding 0.01mol/L sodium hydroxide aqueous solution, adjusting the pH value of the system to 6, and stirring for 30min to obtain gel.
Step 3, carrying out gel modification on the gel prepared in the step 2; and (3) soaking the gel formed in the step (2) in trimethylchlorosilane/n-hexane and KH560 modified luminol/ethanol, sealing, and then placing in an oven to react for 24 hours at 20 ℃, wherein the adding amounts of the trimethylchlorosilane and the KH560 modified luminol respectively account for 1wt% and 0.2wt% of the ethyl orthosilicate, so as to obtain the hydrophobic modified silica gel carrying the luminescent substance. The gel system containing the solvent was poured to remove a large amount of the solvent, and then the gel was gradually dried in a constant temperature oven to obtain a silica aerosol.
And 4, curing and forming to form the artificial rock core:
removing a large amount of solvent from the gel system containing the solvent, filling the gel system into a core mold, and then gradually drying the gel system in a constant-temperature oven to obtain the visual artificial core for displaying the fingering phenomenon.
Example 2
The preparation method of the visual artificial core for displaying the fingering phenomenon is implemented according to the following steps:
step 1, preparing KH560 modified luminol, dissolving 3-amino-benzenedicarboxhydrazide (luminol) in 0.001mol/L aqueous sodium hydroxide solution, and adding an ethanol solution of gamma-glycidoxypropyltrimethoxysilane (KH 560), wherein the molar ratio of KH560 to luminol is 1:1.0, reacting for 2h at 25 ℃, and distilling under reduced pressure to remove the solvent to obtain KH560 modified luminol.
Step 2, preparing gel, namely adding tetraethoxysilane, ethanol and water into a flask provided with a stirring device, uniformly mixing the tetraethoxysilane, the ethanol and the water, wherein the molar ratio of the tetraethoxysilane to the ethanol to the water is 1; adding ferric citrate into the system, and uniformly stirring, wherein the addition amount of the ferric citrate accounts for 0.3wt% of the amount of the ethyl orthosilicate; and adding 0.01mol/L sodium hydroxide aqueous solution, adjusting the pH value of the system to 6, and stirring for 30min to obtain gel.
Step 3, carrying out gel modification on the gel prepared in the step 2; and (3) soaking the gel formed in the step (2) in trimethylchlorosilane/n-hexane and KH560 modified luminol/ethanol, sealing, and then placing in an oven to react for 48 hours at 30 ℃, wherein the adding amounts of the trimethylchlorosilane and the KH560 modified luminol respectively account for 5wt% and 0.3wt% of the ethyl orthosilicate, so as to obtain the hydrophobic modified silica gel carrying the luminescent substance. The gel system containing the solvent was poured to remove a large amount of the solvent, and then the gel was gradually dried in a constant temperature oven to obtain a silica aerosol.
And 4, curing and forming to form the artificial rock core:
removing a large amount of solvent from the gel system containing the solvent, filling the gel system into a core mold, and then gradually drying the gel system in a constant-temperature oven to obtain the visual artificial core for displaying the fingering phenomenon.
Example 3
The preparation method of the visual artificial core for displaying the fingering phenomenon is implemented according to the following steps:
step 1, preparing KH560 modified luminol, dissolving 3-amino-benzenedicarboxhydrazide (luminol) in 0.001mol/L aqueous sodium hydroxide solution, and adding an ethanol solution of gamma-glycidoxypropyltrimethoxysilane (KH 560), wherein the molar ratio of KH560 to luminol is 1:1.0, reacting for 2h at 25 ℃, and distilling under reduced pressure to remove the solvent to obtain KH560 modified luminol.
Step 2, preparing gel, namely adding tetraethoxysilane, ethanol and water into a flask provided with a stirring device, uniformly mixing the tetraethoxysilane, the ethanol and the water, dropwise adding 0.5mol/L acetic acid aqueous solution into the system, adjusting the pH of the system to 2, and continuously stirring for 60min to obtain silicic acid sol, wherein the molar ratio of the tetraethoxysilane, the ethanol and the water is 1; adding ferric citrate into the system, and uniformly stirring, wherein the addition amount of the ferric citrate accounts for 0.4wt% of the amount of the ethyl orthosilicate; and adding 0.01mol/L sodium hydroxide aqueous solution, adjusting the pH value of the system to 6, and stirring for 30min to obtain gel.
Step 3, carrying out gel modification on the gel prepared in the step 2; and (3) soaking the gel formed in the step (2) in trimethylchlorosilane/n-hexane and KH560 modified luminol/ethanol, sealing, and then placing in an oven to react for 48 hours at 40 ℃, wherein the adding amounts of the trimethylchlorosilane and the KH560 modified luminol respectively account for 10wt% and 0.4wt% of the ethyl orthosilicate, so as to obtain the hydrophobic modified silica gel carrying the luminescent substance. The gel system containing the solvent was poured to remove a large amount of the solvent, and then the gel was gradually dried in a constant temperature oven to obtain a silica aerosol.
And 4, curing and forming to form the artificial rock core:
removing a large amount of solvent from the gel system containing the solvent, filling the gel system into a core mold, and then gradually drying the gel system in a constant-temperature oven to obtain the visual artificial core for displaying the fingering phenomenon.
Example 4
The preparation method of the visual artificial core for displaying the fingering phenomenon is implemented according to the following steps:
step 1, preparing KH560 modified luminol, dissolving 3-amino-benzenedicarboxhydrazide (luminol) in 0.001mol/L aqueous sodium hydroxide solution, and adding an ethanol solution of gamma-glycidoxypropyltrimethoxysilane (KH 560), wherein the molar ratio of KH560 to luminol is 1:1.0, reacting for 2h at 25 ℃, and distilling under reduced pressure to remove the solvent to obtain KH560 modified luminol.
Step 2, preparing gel, namely adding tetraethoxysilane, ethanol and water into a flask provided with a stirring device, uniformly mixing the tetraethoxysilane, the ethanol and the water, wherein the molar ratio of the tetraethoxysilane to the ethanol to the water is 1; adding ferric citrate into the system, and uniformly stirring, wherein the addition amount of the ferric citrate accounts for 0.4wt% of the amount of the ethyl orthosilicate; and adding 0.01mol/L sodium hydroxide aqueous solution, adjusting the pH value of the system to 7, and stirring for 30min to obtain gel.
Step 3, carrying out gel modification on the gel prepared in the step 2; and (3) soaking the gel formed in the step (2) in trimethylchlorosilane/n-hexane and KH560 modified luminol/ethanol, sealing, and then placing in an oven to react for 36h at 40 ℃, wherein the adding amounts of the trimethylchlorosilane and the KH560 modified luminol respectively account for 15wt% and 0.5wt% of the ethyl orthosilicate, so as to obtain the hydrophobic modified silica gel carrying the luminescent substance. The gel system containing the solvent was poured to remove a large amount of the solvent, and then the gel was gradually dried in a constant temperature oven to obtain a silica aerosol.
And 4, curing and forming to form the artificial rock core:
removing a large amount of solvent from the gel system containing the solvent, filling the gel system into a core mold, and then gradually drying the gel system in a constant-temperature oven to obtain the visual artificial core for displaying the fingering phenomenon.
Example 5
The preparation method of the visual artificial core for displaying the fingering phenomenon is implemented according to the following steps:
step 1, preparing KH560 modified luminol, dissolving 4-aminophthalic hydrazide (luminol) in 0.001mol/L aqueous sodium hydroxide solution, and adding an ethanol solution of gamma-glycidoxypropyltrimethoxysilane (KH 560), wherein the molar ratio of KH560 to luminol is 1:1.1, reacting for 2h at 25 ℃, and distilling under reduced pressure to remove the solvent to obtain KH560 modified luminol.
Step 2, preparing gel, namely adding tetraethoxysilane, ethanol and water into a flask provided with a stirring device, uniformly mixing the tetraethoxysilane, the ethanol and the water, wherein the molar ratio of the tetraethoxysilane to the ethanol to the water is 1; adding ferric citrate into the system, and uniformly stirring, wherein the addition amount of the ferric citrate accounts for 0.2wt% of the amount of the ethyl orthosilicate; and adding 0.01mol/L sodium hydroxide aqueous solution, adjusting the pH value of the system to 6, and stirring for 30min to obtain gel.
Step 3, carrying out gel modification on the gel prepared in the step 2; and (3) soaking the gel formed in the step (2) in trimethylchlorosilane/n-hexane and KH560 modified luminol/ethanol, sealing, and then placing in an oven to react for 24 hours at 20 ℃, wherein the adding amounts of the trimethylchlorosilane and the KH560 modified luminol respectively account for 1wt% and 0.2wt% of the ethyl orthosilicate, so as to obtain the hydrophobic modified silica gel carrying luminescent substances. The gel system containing the solvent was poured to remove a large amount of the solvent, and then the gel was gradually dried in a constant temperature oven to obtain a silica aerosol.
And 4, curing and forming to form the artificial rock core:
removing a large amount of solvent from the gel system containing the solvent, filling the gel system into a core mold, and then gradually drying the gel system in a constant-temperature oven to obtain the visual artificial core for displaying the fingering phenomenon.
Example 6
The preparation method of the visual artificial core for displaying the fingering phenomenon is implemented according to the following steps:
step 1, preparing KH560 modified luminol, dissolving N- (4-aminobutyl) -N-ethyl isoluminol (luminol) in 0.001mol/L aqueous sodium hydroxide solution, adding ethanol solution of gamma-glycidoxypropyltrimethoxysilane (KH 560), wherein the molar ratio of KH560 to luminol is 1:1.1, reacting for 2h at 25 ℃, and distilling under reduced pressure to remove the solvent to obtain KH560 modified luminol.
Step 2, preparing gel, namely adding tetraethoxysilane, ethanol and water into a flask provided with a stirring device, uniformly mixing the tetraethoxysilane, the ethanol and the water, dropwise adding 0.5mol/L acetic acid aqueous solution into the system, adjusting the pH of the system to 2, and continuously stirring for 60min to obtain silicic acid sol, wherein the molar ratio of the tetraethoxysilane, the ethanol and the water is 1; adding ferric citrate into the system, and uniformly stirring, wherein the addition amount of the ferric citrate accounts for 0.4wt% of the amount of the ethyl orthosilicate; and adding 0.01mol/L sodium hydroxide aqueous solution, adjusting the pH value of the system to 7, and stirring for 30min to obtain gel.
Step 3, carrying out gel modification on the gel prepared in the step 2; and (3) soaking the gel formed in the step (2) in trimethylchlorosilane/n-hexane and KH560 modified luminol/ethanol, sealing, and then placing in an oven to react for 48 hours at 40 ℃, wherein the adding amounts of the trimethylchlorosilane and the KH560 modified luminol respectively account for 15wt% and 0.5wt% of the ethyl orthosilicate, so as to obtain the hydrophobic modified silica gel carrying the luminescent substance. The gel system containing the solvent was poured to remove a large amount of the solvent, and then the gel was gradually dried in a constant temperature oven to obtain a silica aerosol.
And 4, solidifying and forming to form the artificial rock core:
removing a large amount of solvent from the gel system containing the solvent, filling the gel system into a core mold, and then placing the core mold into a constant-temperature oven for gradual drying to obtain a visual artificial core for displaying the fingering phenomenon.
The visual artificial rock cores prepared in the above examples 1 to 6 utilize the chemiluminescence potential of the artificial rock core to realize three-dimensional visual display of the fingering phenomenon of the fluid to be measured in the advancing process of the void environment. When the fingering phenomenon is displayed, the modified luminol is contacted with the alkaline hydrogen peroxide fluid under the action of ferric citrate to generate a luminescence phenomenon. Wherein the pH value of the alkaline hydrogen peroxide system is 8-9, and the addition of 10 percent hydrogen peroxide accounts for 0.5-5.0 wt percent of the fluid. The process of displaying the fingering phenomenon is to inject the fluid to be detected containing the alkaline hydrogen peroxide into the pore throat of the rock core after the prepared silicon dioxide gel carrying the luminescent substance is dried, cured and molded, so that the three-dimensional visualization of the fluid fingering phenomenon can be realized.
The invention discloses a preparation method of a visual artificial rock core for displaying finger advance phenomenon, wherein the artificial rock core with chemiluminescence potential is hydrophobic modified silica gel, and the surface of the silica gel carries a modified luminol chemiluminescence substance. The porous structure formed by water evaporation in the gel drying, curing and forming process is similar to the pore throat structure in the core. The chemical luminescence phenomenon of the visual artificial rock core is that alkaline fluid containing hydrogen peroxide contacts with the surface modified luminol of the rock core in the advancing process of the artificial rock core in the gap environment, and the chemical luminescence phenomenon is displayed under the action of ferric citrate.
Claims (7)
1. The preparation method of the visual artificial core for displaying the fingering phenomenon is characterized by comprising the following steps:
step 1, preparing KH560 modified luminol;
the step 1 is specifically implemented according to the following steps: dissolving luminol in 0.001mol/L aqueous solution of sodium hydroxide, and adding ethanol solution of gamma-glycidoxypropyltrimethoxysilane, wherein the molar ratio of the gamma-glycidoxypropyltrimethoxysilane to the luminol is 1:1.0 to 1.1, reacting for 2 hours at the temperature of 25 ℃, and distilling under reduced pressure to remove the solvent to obtain KH560 modified luminol;
step 2, preparing gel;
the step 2 is specifically implemented according to the following steps: adding tetraethoxysilane, ethanol and water into a flask provided with a stirring device, uniformly mixing, then dropwise adding 0.5mol/L acetic acid aqueous solution, adjusting the pH of the system to 2 to 3, continuously stirring for 60min to obtain silicic acid sol, adding ferric citrate into the silicic acid sol, uniformly stirring, adding 0.01mol/L sodium hydroxide aqueous solution, adjusting the pH of the system to 6 to 7, and stirring for 30min to obtain gel;
step 3, carrying out gel modification on the gel prepared in the step 2;
the step 3 is specifically implemented according to the following steps: mixing the KH560 modified luminol prepared in the step 1 with trimethylchlorosilane/n-hexane, soaking the gel in the step 2 in the trimethylchlorosilane/n-hexane and the KH560 modified luminol/ethanol, sealing, placing in an oven, and reacting at 20-40 ℃ for 24-48h to obtain hydrophobic modified silica gel carrying luminescent substances, and pouring a gel system containing a solvent to remove a large amount of the solvent to obtain silica gel;
and 4, curing and molding the gel prepared in the step 3 to form the artificial rock core.
2. The method for preparing the artificial core for displaying the fingering phenomenon according to claim 1, wherein the silica gel prepared in step 3 is filled into a core mold, and then is placed in a constant temperature oven for gradual drying, and the silica gel is formed into a skeleton structure of the artificial core during drying, curing and molding.
3. The method for preparing a visual artificial core for displaying fingering phenomenon according to claim 1, wherein the luminol in step 1 is any one of 3-amino-benzenedicarboxhydrazide, N- (4-aminobutyl) -N-ethyl isoluminol, and 4-aminophthalic hydrazide.
4. The method for preparing a visual artificial core for displaying fingering phenomenon according to claim 1, wherein the molar ratio of ethyl orthosilicate, ethanol and water in the step 2 is 1.
5. The preparation method of the visual artificial core for displaying fingering phenomenon according to claim 1, wherein the addition amount of ferric citrate in the step 2 is 0.2-0.4 wt% of the amount of ethyl orthosilicate in the silicic acid sol.
6. The preparation method of the visual artificial rock core for displaying the fingering phenomenon in the claim 1, characterized in that the addition amount of the trimethylchlorosilane in the step 3 is 1-15wt% of the amount of the ethyl orthosilicate in the gel.
7. The preparation method of the visual artificial rock core for displaying the fingering phenomenon, according to the claim 1, is characterized in that the addition amount of the KH560 modified luminol in the step 3 is 0.2 to 0.5wt% of the amount of ethyl orthosilicate in the gel.
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