CN117143578A - Active crude oil plugging system and preparation method and application thereof - Google Patents
Active crude oil plugging system and preparation method and application thereof Download PDFInfo
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- 239000010779 crude oil Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000000839 emulsion Substances 0.000 claims abstract description 80
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 58
- 239000002135 nanosheet Substances 0.000 claims abstract description 51
- 239000003921 oil Substances 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 29
- 239000002736 nonionic surfactant Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 12
- 150000003839 salts Chemical class 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 4
- MTNDZQHUAFNZQY-UHFFFAOYSA-N imidazoline Chemical compound C1CN=CN1 MTNDZQHUAFNZQY-UHFFFAOYSA-N 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 13
- -1 silicate ester Chemical class 0.000 claims description 12
- 239000002064 nanoplatelet Substances 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000003995 emulsifying agent Substances 0.000 claims description 10
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 9
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 7
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 7
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 7
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000005642 Oleic acid Substances 0.000 claims description 7
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 7
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 7
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid group Chemical group C(CCCCCCC\C=C/CCCCCCCC)(=O)O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 7
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 claims description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical group CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 5
- 230000002378 acidificating effect Effects 0.000 claims description 5
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 3
- 230000001804 emulsifying effect Effects 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 230000002194 synthesizing effect Effects 0.000 claims description 3
- FZMJEGJVKFTGMU-UHFFFAOYSA-N triethoxy(octadecyl)silane Chemical group CCCCCCCCCCCCCCCCCC[Si](OCC)(OCC)OCC FZMJEGJVKFTGMU-UHFFFAOYSA-N 0.000 claims description 3
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 230000002209 hydrophobic effect Effects 0.000 claims description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000011084 recovery Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 16
- 150000001875 compounds Chemical class 0.000 abstract description 5
- 239000007762 w/o emulsion Substances 0.000 abstract description 5
- 230000007774 longterm Effects 0.000 abstract description 3
- 238000013329 compounding Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 239000004094 surface-active agent Substances 0.000 description 21
- 239000012071 phase Substances 0.000 description 16
- 230000000694 effects Effects 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- 230000035699 permeability Effects 0.000 description 5
- 239000008398 formation water Substances 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 238000009826 distribution Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000011435 rock Substances 0.000 description 3
- 239000013543 active substance Substances 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000033558 biomineral tissue development Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- 238000004088 simulation Methods 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000037361 pathway Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Classifications
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- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B33/00—Sealing or packing boreholes or wells
- E21B33/10—Sealing or packing boreholes or wells in the borehole
- E21B33/13—Methods or devices for cementing, for plugging holes, crevices or the like
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/502—Oil-based compositions
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- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Mining & Mineral Resources (AREA)
- Geology (AREA)
- Physics & Mathematics (AREA)
- Fluid Mechanics (AREA)
- Geochemistry & Mineralogy (AREA)
- Environmental & Geological Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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Abstract
The application discloses an active crude oil plugging system, a preparation method and application thereof. The method comprises the steps of compounding a nonionic surfactant and a silica-based amphiphilic Janus nano sheet, and dispersing the compound in crude oil to form active crude oil; mixing the water phase with active crude oil under a certain shear strength to prepare Pickering emulsion; the active crude oil plugging system can obviously reduce the oil-water interfacial tension, and the constructed high-viscosity water-in-oil emulsion has strong stability and excellent rheological property; the system can be stably dispersed for more than 3 days under the condition of high salt (35000 ppm) at high temperature (80 ℃). The material is used as a plugging agent, can meet the requirement of long-term efficient stable plugging in a high-temperature high-salt oil reservoir, is environment-friendly, has low economic cost and has wide application prospect.
Description
Technical Field
The application belongs to the technical field of oil extraction in oil fields, relates to an active crude oil plugging system, a preparation method and application thereof, and in particular relates to an amphiphilic nano-sheet reinforced active crude oil plugging agent composition, and a preparation method and application thereof.
Background
After the oil field exploitation enters the middle and later stages, the water flooding problem is more and more complex, and finding a chemical profile control water shutoff agent with stronger adaptability and better performance becomes a key for improving the oil reservoir residual oil mining. The active crude oil plugging agent enters a high-oil-content layer to be compatible, and is discharged in a return way in normal production; upon entering the high water-bearing layer, a water-in-oil emulsion is formed to thicken and form a plug. The active crude oil water shutoff not only has high selectivity and no damage to an oil layer, but also can obtain higher benefit from both technical and economic aspects. However, conventional active substances used in active crude oil are agglomerated under the high-temperature and high-salt conditions of an oil reservoir, so that emulsion demulsification is caused, and long-term effective plugging cannot be realized.
In recent years, silica nanomaterials have received high attention due to their good surface modification pathways as well as rich resources and good environmental acceptance. The amphiphilic Janus nano sheet is different from particles with uniform surface wettability, has a non-centrosymmetric structure, has two completely different characteristics of hydrophilicity and hydrophobicity on two sides, and has high adsorption energy at an interface. And its rigid structure has been shown to significantly enhance emulsion performance.
However, there is no research on the application of Janus nanoplatelets to the performance improvement of active crude plugging systems.
Disclosure of Invention
Based on the problems of the prior art, the application aims to provide an emulsifier composition and a preparation method thereof.
According to the application, the silica-based amphiphilic Janus nano-sheet and the nonionic surfactant are compounded for use, so that the prepared Janus nano-sheet enhanced active crude oil emulsion can be stabilized for more than 3 days under the high-temperature (80 ℃) high-salt (35000 ppm) condition.
The second object of the application is to provide an active crude oil plugging system, wherein the compounded nano-sheets and surfactant can reduce interfacial tension, improve rheological behavior of emulsion and enhance emulsion stability.
The third purpose of the application is to provide the application of Janus nanosheet reinforced active crude oil plugging agent in oil extraction in an oil field, which has better plugging effect, higher plugging rate and better scouring resistance.
The aim of the application is achieved by the following technical means:
in one aspect, the present application provides an emulsifier composition comprising a silica-based amphiphilic Janus nanoplatelet and a nonionic surfactant;
wherein the mass ratio of the silica-based amphiphilic Janus nano sheet to the nonionic surfactant is 1:2-6;
the silica-based amphiphilic Janus nano-sheet is modified with an amino hydrophilic side and C 10 -C 18 Long chain alkyl hydrophobic side.
The silica-based amphiphilic Janus nanoplatelets are prepared according to the method described in the literature (Janus hollow spheres by emulsion interfacial self-assembled sol-gel process, fuxin Liang, jiguang Liu, chengliang Zhang, xiaozhong Qu, jiaoli Li and Zhenzhong Yang, chem. Commun.,2011,47,1231-1233) by a method comprising the steps of:
preparing an emulsion of an O/W emulsion for synthesizing the nano-sheets; dispersing the emulsion in water according to a certain concentration to serve as a water phase of the O/W emulsion, and regulating the pH value of the solution to be acidic; adding a silane coupling agent and silicate ester into n-decane to serve as an oil phase of the O/W emulsion; heating the water phase and the oil phase respectively, mixing and emulsifying to obtain O/W emulsion; the silane coupling agent and silicate self-assemble on the interface of emulsion under the catalysis of acid, and sol-gel reaction is carried out; and removing the oil core in the obtained nano spherical shell, and breaking the spherical shell structure to obtain the silica-based amphiphilic Janus nano sheet.
Wherein the O/W emulsion is a reaction vessel for synthesizing nano sheets, the emulsion is polystyrene-maleic anhydride (HSMA), and the concentration of the emulsion in water can be 10wt%;
the silane coupling agent comprises aminopropyl triethoxysilane (APTES) and C 10 -C 18 Long chain alkyl triethoxysilanes;
the silicate may specifically be tetraethyl orthosilicate (TEOS);
wherein, aminopropyl triethoxysilane and C 10 -C 18 The molar ratio of the long-chain alkyl triethoxysilane and the silicate ester is as follows: 0.8-1.2:1.0-1.4:4.8-5.2;
the concentration of aminopropyl triethoxysilane in the oil phase may be (2.5-3.5) x 10 -4 mol/mL；
The volume ratio of the water phase to the oil phase is 7-8:3, a step of;
the reaction temperature of the sol-gel reaction is 70 ℃ and the pH value is 2.5; the reaction time may be 6 to 12 hours.
Specifically, the C 10 -C 18 The long-chain alkyl triethoxysilane is octadecyl triethoxysilane; the prepared silica-based amphiphilic Janus nano-sheet is silica-based amphiphilic Janus nano-sheet Janus-L18.
The nonionic surfactant may specifically be an oleic acid Imidazoline (IMO).
On the other hand, the application also provides an active crude oil plugging system, and the emulsion formed by the emulsifier composition has excellent interfacial properties and rheological behavior and can be kept stable under the conditions of a high-temperature and high-salt oil reservoir.
The active crude oil plugging system comprises a silica-based amphiphilic Janus nano sheet, a nonionic surfactant and crude oil;
wherein the mass ratio of the silica-based amphiphilic Janus nano sheet to the nonionic surfactant is 1:2-6;
the mass sum of the silica-based amphiphilic Janus nano sheet and the nonionic surfactant accounts for 1.5-3.0wt% of the total mass of the active crude oil plugging system.
The silica-based amphiphilic Janus nanosheet can be specifically a silica-based amphiphilic Janus nanosheet Janus-L18;
the nonionic surfactant may specifically be an oleic acid Imidazoline (IMO).
The active crude oil plugging system is prepared by a method comprising the following steps:
and (3) dissolving the nonionic surfactant and the silica-based amphiphilic Janus nano sheet in crude oil according to a proportion, and performing ultrasonic dispersion to obtain an active crude oil plugging system.
In yet another aspect, the present application also provides the use of the above-described emulsifier composition and an active crude oil plugging system in oil recovery in an oilfield.
Specifically, the application is: the active crude oil plugging system is applied to plugging of high-temperature high-salt oil reservoirs, wherein the highest temperature can reach 80 ℃, and the highest salt content can reach 35000ppm.
The application adopts the amphiphilic Janus nanosheets to enhance the performance of the active crude oil emulsion and is used for improving the plugging performance of the active crude oil emulsion system under the high-temperature and high-salt environment.
The application has the following advantages:
(1) In the active crude oil plugging agent, the formed emulsion can be stabilized for more than 3 days under the condition of high temperature (80 ℃) and high salt (35000 ppm) by compounding the amphiphilic Janus nanosheets and the surfactant, so that the active crude oil enhanced by the amphiphilic Janus nanosheets has the potential of being applied to plugging of high-temperature and high-salt oil reservoirs.
(2) The compound system of the amphiphilic Janus nano-sheet and the surfactant obviously reduces the interfacial tension of oil and water, improves the rheological behavior of the formed emulsion and enhances the stability of the formed emulsion.
(3) The active crude oil plugging agent disclosed by the application has good physical simulation plugging effect and flushing resistance under the condition of a high-temperature high-salt oil reservoir, can form high-viscosity emulsion to efficiently plug a stratum when a rock core is physically simulated for subsequent water flooding, and keeps certain plugging aging.
Drawings
FIG. 1 is a schematic structural diagram of a silica-based amphiphilic Janu nanoplatelet used in the present application and a synthetic route.
In fig. 2, (a) and (b) are viscosity-temperature curves and oil-out amounts of the compound system of amphiphilic Janus nanosheets and surfactant, respectively, and the emulsion formed when either component is used alone, (b) a represents oil-out amount when surfactant and nanosheets are added to the emulsion, b represents oil-out amount when only surfactant is added to the emulsion, and c represents oil-out amount when only nanosheets are added to the emulsion.
FIG. 3 is a graph showing the dynamic interfacial tension of oil and water when the amphiphilic Janus nanosheets and surfactant are combined and either component is used alone.
FIG. 4 is a graph of the viscoelastic modulus of an amphiphilic Janus nanosheets with surfactant and emulsion formed when either component is used alone as a function of shear rate.
Fig. 5 is a core physical simulation experiment result of the active crude oil plugging system of the present application.
Detailed Description
The following detailed description of the application is provided in connection with the accompanying drawings that are presented to illustrate the application and not to limit the scope thereof. The examples provided below are intended as guidelines for further modifications by one of ordinary skill in the art and are not to be construed as limiting the application in any way.
The experimental methods in the following examples, unless otherwise specified, are conventional methods, and are carried out according to techniques or conditions described in the literature in the field or according to the product specifications. Materials, reagents and the like used in the examples described below are commercially available unless otherwise specified.
The silica-based amphiphilic Janus nanoplatelets used in the examples below were prepared by the method described in the literature (Janus hollow spheres by emulsion interfacial self-assembled sol-gel process, fuxin Liang, jiguang Liu, chengliang Zhang, xiaozhong Qu, jiaoli Li and ZhenzhongYang, chem.Commun.,2011,47,1231-1233), and the schematic structure and synthetic routes are shown in FIG. 1. The specific operation is as follows:
dispersing the emulsion (HSMA) in water at a concentration of 10wt% as an aqueous phase of an O/W emulsion and adjusting the pH of the solution to be acidic (ph=2.5); aminopropyl triethoxysilane (APTES) 0.005mol, octadecyl triethoxysilane 0.006mol and tetraethyl orthosilicate (TEOS) 0.025mol were added to 14ml n-decane as the oil phase of the O/W emulsion; heating the water phase and the oil phase respectively, mixing and emulsifying to obtain O/W emulsion; self-assembling the silane coupling agent and silicate ester on the interface of the emulsion under the acidic condition, and performing sol-gel reaction (70 ℃ for 12 h); and removing the oil core in the obtained nano spherical shell, and breaking the spherical shell structure to obtain the silicon dioxide-based amphiphilic Janus nano sheet Janus-L18.
Example 1,
The embodiment provides a preparation method of an active crude oil plugging system with high temperature resistance and high salt resistance, which comprises the following steps:
Janus-L18 and IMO are compounded according to the mass ratio of 1:4, the total concentration is 1.5wt% relative to the oil phase, namely 0.3wt% of nano-sheets and 1.2wt% of surfactant are taken to be dissolved in crude oil, and ultrasonic dispersion is carried out for more than 30 minutes until each component is completely dispersed in the crude oil. And (3) preparing stratum water with the mineralization degree of 35000ppm by imitating the high-salt environment of the stratum. And (3) adding formation water into the active crude oil slowly for a small amount for a plurality of times according to the volume ratio of oil to water of 3:7 at the rotating speed of 500rpm, stirring for 3min until a water-in-oil emulsion is formed, transferring the emulsion to a cylinder with a plug, placing the cylinder into an oven at 80 ℃, and observing emulsion breaking condition of the emulsion.
In order to evaluate the improvement degree of the compound system on the emulsion performance and stability of the active crude oil emulsion, janus-L18 (0.3 wt%) and IMO (1.2 wt%) are respectively added into the oil phase as single active substances, the emulsion (oil-water volume ratio 3:7) is prepared according to the same means as the steps, an Olympus optical microscope is used for observing the size and distribution condition of emulsion liquid drops, the curve of the viscosity of the emulsion along with the change of temperature is tested, and the change of the oil precipitation of the emulsion after three days is recorded. The higher the viscosity of the formed emulsion, the smaller the emulsion droplets, the more uniform the distribution, indicating that the better the emulsification effect. Meanwhile, the smaller the oil precipitation amount of the emulsion, the higher the stability of the emulsion.
The results of the experimental tests are shown in fig. 2. In this example, it can be observed that the viscosity-temperature curves of the three emulsions have the same tendency to decrease with increasing temperature. When the oleic acid imidazoline or the nano-sheet is used independently, the viscosity of the stabilized emulsion is smaller than that when the oleic acid imidazoline or the nano-sheet is added simultaneously, and the emulsion emulsification effect reflected from the viscosity is also proved from the emulsion particle size and the droplet distribution condition. In addition, when the oleic acid imidazoline or the nano-sheet is singly used, the oil precipitation of the stabilized emulsion is larger than that when the oleic acid imidazoline or the nano-sheet is added at the same time, which shows that after the surfactant and the nano-sheet are compounded for use, the emulsion effect of the emulsion is improved, and the long-term stability of the emulsion under a high-temperature and high-salt environment is enhanced.
Wherein simulated formation water having a mineralization of 35000ppm was prepared, and the specific ion composition thereof is shown in Table 1.
Table 1:
EXAMPLE 2,
The interfacial tension between active crude oil containing individual amphiphilic Janus nanoplatelets, containing individual surfactants, containing nanoplatelets and surfactant complex systems and simulated formation water was measured at 80 ℃ using an SVT20 (SVT 20, germany) spin drop interfacial tensiometer, and the results are shown in FIG. 3. The interfacial tension of crude oil/mineralized water was about 15.3mN/m, and after 0.3wt% Janus-L18 was added to the crude oil alone, the interfacial tension was reduced to about 8.6mN/m, and after 1.2wt% IMO was added to the crude oil alone, the interfacial tension was reduced to 1.2mN/m, and when 1.2wt% IMO and 0.3wt% Janus-L18 were added to the crude oil simultaneously, the oil-water interfacial tension was further reduced to 0.55mN/m. The interfacial tension can be obviously reduced by using the nano-sheet and the surfactant independently, but the surfactant plays a larger role in reducing the interfacial tension of active crude oil and formation water, and the interfacial tension can be further reduced after the nano-sheet and the surfactant are used cooperatively.
Three sets of emulsions were prepared according to the emulsion formulation method described in example 1, wherein amphiphilic Janus nanoplatelets, surfactant, nanoplatelet and surfactant complex systems (mass ratio 1:4) were added to the active crude oil as the emulsion oil phase, respectively. The bulk viscoelastic properties of emulsions are macroscopic manifestations of the rheological properties of oil-water interfaces, emulsion formation and migration and plugging of emulsions at the pore canal and pore throats of the formation, bulk viscoelasticity being an important characterization of their plugging capability. Thus, the change in the viscoelastic modulus of the emulsion with shear frequency was measured using a haak rheometer, and the rheological behavior of the emulsion was evaluated. As shown in the results shown in fig. 4, the elastic modulus and viscous modulus of the emulsion with the surfactant and the nanoplatelets added simultaneously were both higher than those with either one alone, which corresponds to the results of the viscosity test. The elastic modulus and viscous modulus of the three groups of emulsions both increased with increasing shear frequency. The elastic modulus of each set of emulsions was greater than the viscous modulus, which indicated that the emulsions exhibited more solid-like properties. The degree of the increase of the elastic modulus along with the shearing frequency is larger than that of the viscous modulus, the molecular diffusion relaxation process of the general phase and the interface is shortened along with the increase of the shearing frequency, the acceleration of the viscous modulus is small, but the interface deformation is accelerated, the intermolecular action on the interface is aggravated, the elastic modulus of the interface is greatly increased, and the bulk modulus of the emulsion is generally increased along with the increase of the oscillating frequency. Compared with the emulsion formed by the single surfactant or the nano-sheet, after the synergistic effect of the surfactant and the nano-sheet, the viscoelasticity of the emulsion is obviously improved, and the plugging capability of an active crude oil plugging system can be greatly improved theoretically.
EXAMPLE 3,
Core plugging and scour resistance experiments:
core displacement experiments were performed using cores of different permeability (core parameters are shown in table 2). And (3) carrying out aging treatment on the core after saturated water and saturated oil to simulate the state of a reservoir, then carrying out primary water flooding, reverse injection of active crude oil and subsequent water flooding according to the flow rate of 1mL/min, recording the oil-water liquid output and pressure change in the process, and evaluating the plugging effect through the plugging rate, the breakthrough pressure, the resistance coefficient and the residual resistance coefficient, wherein the experimental result is shown in Table 3. After entering the core to undergo a crosslinking reaction, the viscosity of the plugging agent is increased, so that rock pores and roar channels are blocked. The breakthrough pressure represents the maximum pressure of the porous medium when the water drive breaks through, and reflects the plugging capability of the temporary plugging agent in the porous medium to the aqueous phase fluid, so that the strength of the plugging agent can be better reflected. Besides the plugging effect of the plugging agent is evaluated by using the plugging rate, the residual resistance coefficient is also commonly used for reflecting the capacity of the plugging agent for reducing the permeability of the porous medium, is an important index for measuring the plugging capacity of the plugging agent on the porous medium, and shows that the retention of the plugging agent in the core is the ratio of the permeability of the plugging agent before and after the core is plugged. The results of plugging experiments prove that the plugging rate of the active crude oil plugging agent on three cores with different permeabilities is higher than 95%, the residual resistance coefficient is higher, and particularly on a core of 913.58mD, the residual resistance coefficient is highest, and the plugging rate reaches 98.55%. And (5) continuously injecting water after the subsequent water flooding, and observing pressure change to evaluate the plugging strength and durability of the plugging system. Figure 5 records the injection pressure at the inlet end after the start of the subsequent water flooding up to the time of continuous injection for 5h when cores of different permeability are plugged. The injected water phase meets active crude oil in the core to form high-viscosity water-in-oil emulsion to block the throat channel, so that pressure is suddenly increased, residual oil in the small throat is forced to be driven out, the pressure is gradually reduced to reach a more stable state, along with continuous injection of the water phase, the pressure has a descending trend, the process is slower, and the erosion resistance experiment proves the timeliness of the emulsion blocking. The experiment fully reflects the capability of the nano-sheet and surfactant compound system to form stable water-in-oil emulsion in the rock core to effectively block the stratum, and has good application prospect in high-temperature and high-salt oil reservoirs.
Table 2:
table 3:
the present application is described in detail above. It will be apparent to those skilled in the art that the present application can be practiced in a wide range of equivalent parameters, concentrations, and conditions without departing from the spirit and scope of the application and without undue experimentation. While the application has been described with respect to specific embodiments, it will be appreciated that the application may be further modified. In general, this application is intended to cover any variations, uses, or adaptations of the application following, in general, the principles of the application and including such departures from the present disclosure as come within known or customary practice within the art to which the application pertains.
Claims (8)
1. An emulsifier composition comprising silica-based amphiphilic Janus nanoplatelets and a nonionic surfactant; the silica-based amphiphilic Janus nano-sheet is modified with an amino hydrophilic side and C 10 -C 18 A long chain alkyl hydrophobic side;
the mass ratio of the silica-based amphiphilic Janus nano sheet to the nonionic surfactant is 1:2-6.
2. The emulsifier composition of claim 1 wherein: the nonionic surfactant is oleic acid imidazoline;
the silica-based amphiphilic Janus nano sheet is prepared by a method comprising the following steps:
dispersing the emulsion in water according to a certain concentration to serve as a water phase of the O/W emulsion, and regulating the pH value of the solution to be acidic; adding a silane coupling agent and silicate ester into n-decane to serve as an oil phase of the O/W emulsion; heating the water phase and the oil phase respectively, mixing and emulsifying to obtain O/W emulsion; self-assembling the silane coupling agent and silicate ester on the interface of the emulsion under an acidic condition, and performing sol-gel reaction; and removing the oil core in the obtained nano spherical shell, and breaking the spherical shell structure to obtain the silica-based amphiphilic Janus nano sheet.
3. An emulsifier composition according to claim 2, characterized in that: the O/W emulsion is a reaction vessel for synthesizing the nano-sheets, the emulsion is HSMA, and the concentration of the emulsion in water is 10wt%;
the silane coupling agent comprises aminopropyl triethoxy silane and C 10 -C 18 Long chain alkyl triethoxysilanes;
the silicate is ethyl orthosilicate;
wherein, aminopropyl triethoxysilane and C 10 -C 18 The molar ratio of the long-chain alkyl triethoxysilane and the silicate ester is as follows: 0.8-1.2:1.0-1.4:4.8-5.2;
the concentration of aminopropyl triethoxysilane in the oil phase is (2.5-3.5) x 10 -4 mol/mL；
The volume ratio of the water phase to the oil phase is 7-8:3, a step of;
the reaction temperature of the sol-gel reaction is 70 ℃ and the pH value is 2.5; the reaction time is 6-12h.
4. An emulsifier composition according to claim 3, characterized in that: the C is 10 -C 18 The long-chain alkyl triethoxysilane is octadecyl triethoxysilane; the prepared silica-based amphiphilic Janus nano-sheet is silica-based amphiphilic Janus nano-sheet Janus-L18.
5. An active crude oil plugging system comprises a silica-based amphiphilic Janus nano-sheet, a nonionic surfactant and crude oil;
wherein the mass sum of the silica-based amphiphilic Janus nano sheet and the nonionic surfactant accounts for 1.5-3.0wt% of the total mass of the active crude oil plugging system.
6. A method of preparing the active crude oil plugging system of claim 5 comprising the steps of:
and (3) dissolving the nonionic surfactant and the silica-based amphiphilic Janus nano sheet in crude oil according to a proportion, and performing ultrasonic dispersion to obtain an active crude oil plugging system.
7. Use of the emulsifier composition of any one of claims 1-4 or the active crude oil plugging system of claim 5 in oil recovery in an oilfield.
8. The use according to claim 7, characterized in that: the application is as follows: the emulsifier composition is made into an active crude oil plugging system or the active crude oil plugging system is applied to plugging of high-temperature high-salt oil reservoirs, wherein the high temperature is up to 80 ℃, and the high salt is up to 35000ppm.
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