CN117050227A - Core-shell structure microsphere profile control agent capable of improving recovery ratio and preparation method thereof - Google Patents

Core-shell structure microsphere profile control agent capable of improving recovery ratio and preparation method thereof Download PDF

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Publication number
CN117050227A
CN117050227A CN202311024277.3A CN202311024277A CN117050227A CN 117050227 A CN117050227 A CN 117050227A CN 202311024277 A CN202311024277 A CN 202311024277A CN 117050227 A CN117050227 A CN 117050227A
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core
shell
solution
profile control
control agent
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马国艳
杨延哲
田童木
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Xian Shiyou University
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Xian Shiyou University
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/04—Acids; Metal salts or ammonium salts thereof
    • C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/52—Amides or imides
    • 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
    • C09K8/504—Compositions based on water or polar solvents
    • C09K8/506—Compositions based on water or polar solvents containing organic compounds
    • C09K8/508—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
    • C09K8/5083—Compositions based on water or polar solvents containing organic compounds macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • 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
    • C09K8/516—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls characterised by their form or by the form of their components, e.g. encapsulated material
    • 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
    • C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
    • C09K8/588—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids characterised by the use of specific polymers
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A20/00—Water conservation; Efficient water supply; Efficient water use
    • Y02A20/20—Controlling water pollution; Waste water treatment
    • Y02A20/204—Keeping clear the surface of open water from oil spills

Abstract

The invention discloses a core-shell structure microsphere profile control agent capable of improving recovery ratio: the weight portions of the oil phase solution are 45 to 60 portions, 35 to 45 portions of core layer solution, 35 to 70 portions of shell layer solution, 0.03 to 0.5 portion of initiator, 15 to 30 portions of auxiliary agent and proper amount of deionized water. According to the core-shell structure microsphere profile control agent capable of improving the recovery ratio and the preparation method thereof, the prepared core-shell polymer microsphere has good core blocking capability, and compared with a water flooding stage, the core-shell structure microsphere profile control agent can effectively improve the oil displacement recovery ratio.

Description

Core-shell structure microsphere profile control agent capable of improving recovery ratio and preparation method thereof
Technical Field
The invention relates to the technical field of polymer microsphere oil displacement, in particular to a core-shell structure microsphere oil displacement agent capable of improving recovery ratio and a preparation method thereof.
Background
After the oil field enters a high water content or ultra-high water content period, the water flooding problem of the oil field is more and more complicated, and how to improve the recovery ratio of the high water content period is a problem of general concern in the petroleum industry. In the water flooding process, the water flooding oil washing efficiency is low due to high oil-water interfacial tension, poor rock surface wettability and the like. The polymer flooding is the oil extraction technology that uses water-soluble high molecular polymer to increase the viscosity of water and uses it as the oil field developing injection agent to increase the oil recovery ratio. The oil-water fluidity ratio in the oil displacement process can be greatly improved, so that the rising speed of the water content in the produced liquid is delayed, the actual oil displacement efficiency is closer to the limit oil displacement efficiency, and even the limit oil displacement efficiency is reached.
The core-shell polymer sphere belongs to one of polymer microsphere profile control agents, and has higher stability due to the fact that the special core-shell structure provides strong compression resistance and cracking prevention, and the shape and the function of the core-shell polymer sphere can be maintained under the harsher stratum environment condition to form effective blocking profile control. How to develop new technology to further improve the recovery ratio of the water-flooding crude oil has research value.
Disclosure of Invention
The invention aims to provide a core-shell microsphere profile control agent capable of improving recovery ratio and a preparation method thereof, and the prepared core-shell microsphere can effectively improve the recovery ratio and has excellent plugging performance.
In order to achieve the aim, the invention provides the microsphere profile control agent with the core-shell structure, which can improve the recovery ratio, and the microsphere profile control agent comprises, by mass, 45-60 parts of oil phase solution, 35-45 parts of core layer solution, 35-70 parts of shell layer solution, 0.03-0.5 part of initiator, 15-30 parts of auxiliary agent and a proper amount of deionized water.
Preferably, the oil phase solution comprises castor oil polyoxyethylene ether, lipopeptides and vegetable oil.
Preferably, the core layer solution comprises cationic monomer, N-dimethylacrylamide and deionized water.
Preferably, the shell solution comprises sodium hydroxide, 3-acrylamido-3-methylbutanoic acid, methacrylic acid, and deionized water.
Preferably, the initiator is one or more of potassium persulfate, sodium persulfate, ammonium persulfate, sodium sulfite, sodium thiosulfate, azobisisobutyronitrile, triethylamine and beta-dimethylaminopropionitrile.
Preferably, the auxiliary agent is one of an acrylamide auxiliary agent and an acrylic cellulose nanofibril.
Preferably, the cationic monomer is one or more of dimethyldiallylammonium halide, methacryloxyethyl diethylbenzyl ammonium halide, acryloxyethyl trimethylammonium chloride, and methacryloxyethyl trimethylammonium chloride.
The preparation method of the microsphere profile control agent with the core-shell structure, which can improve the recovery ratio, comprises the following steps:
s1, preparing an oil phase solution: mixing castor oil polyoxyethylene ether and vegetable oil, and stirring to obtain an oil phase solution;
s2, preparing a nuclear layer solution: mixing a cationic monomer, N-dimethylacrylamide and deionized water, and stirring until the mixture is dissolved to obtain a nuclear layer solution;
s3, preparing a shell solution: mixing methacrylic acid, 3-acryloimido-3-methylbutyric acid and deionized water, stirring to obtain a mixed solution, preparing a sodium hydroxide solution, dripping the sodium hydroxide solution into the mixed solution, adding an auxiliary agent, and regulating the pH to 5.5-7 to obtain a shell layer solution;
s4, mixing the oil phase solution in the S1 with the core layer solution in the S2, stirring at 1200-1400r/min, introducing nitrogen to emulsify for 25-35min to obtain an emulsion, adding an initiator, and polymerizing at 65-85 ℃;
s5, adding the shell layer solution in the step S3 into the solution in the step S4, stirring at 250-350r/min, adding an initiator, and reacting at 45-60 ℃ for 2-3h in a heat preservation way;
s6, cooling the reaction system in the step S5 to 35 ℃, adding an auxiliary agent, stirring, filtering, and performing suction filtration and drying to obtain the microsphere with the core-shell structure.
The core-shell structure microsphere prepared by the preparation method of the core-shell structure microsphere profile control agent capable of improving the recovery ratio can be compounded with other chemicals or directly used for oil displacement and recovery ratio improvement.
Therefore, the core-shell structure microsphere profile control agent with the formula and the preparation method thereof have the beneficial effects that:
1. under the action of shearing force, the core-shell structure microsphere presents a layered structure which is orderly arranged and clear in structure, and most of the microspheres only move at the positions of the microspheres in layers, and the aggregation and dissociation of the shearing stress on the microsphere particles can reach an equilibrium state due to the crosslinking action in the microspheres, so that the shearing viscosity of a polymer microsphere system is basically stable;
2. the core-shell polymer microsphere has better core plugging capability, and can effectively improve oil displacement recovery ratio compared with the water displacement stage.
The technical scheme of the invention is further described in detail through examples.
Detailed Description
The technical scheme of the invention is further described below by examples.
The present invention will be explained in more detail by the following examples, and the purpose of the present invention is to protect all changes and modifications within the scope of the present invention, and the present invention is not limited to the following examples.
Example 1
S1, preparing an oil phase solution: mixing and stirring castor oil polyoxyethylene ether, lipopeptide and vegetable oil to obtain an oil phase solution.
S2, preparing a nuclear layer solution: and mixing dimethyl diallyl ammonium chloride, N-dimethyl acrylamide and deionized water, and stirring until the mixture is dissolved to obtain a nuclear layer solution.
S3, preparing a shell solution: mixing methacrylic acid, 3-acryloimido-3-methyl butyric acid and deionized water, stirring to obtain a mixed solution, preparing a sodium hydroxide solution, dripping the sodium hydroxide solution into the mixed solution, adding cellulose acrylate nanofibrils, and regulating the pH to 6 to obtain a shell layer solution.
S4, mixing 50 parts of the oil phase solution in the S1 with 40 parts of the core layer solution in the S2, stirring at 1300r/min, introducing nitrogen, emulsifying for 30min, reducing the rotating speed to 300r/min, stirring for 30min, fully emulsifying to obtain emulsion, adding the sodium thiosulfate solution, and polymerizing at 75 ℃.
S5, adding 60 parts of the shell layer solution in S3 into the solution in S4, stirring at 300r/min, adding the sodium thiosulfate solution, and reacting at 60 ℃ for 3 hours.
S6, cooling the reaction system in the step S5 to 35 ℃, adding an acrylamide auxiliary agent, stirring, filtering, and performing suction filtration and drying to obtain the core-shell structure microsphere.
Example 2
S1, preparing an oil phase solution: mixing and stirring castor oil polyoxyethylene ether, lipopeptide and vegetable oil to obtain an oil phase solution.
S2, preparing a nuclear layer solution: and mixing dimethyl diallyl ammonium chloride, N-dimethyl acrylamide and deionized water, and stirring until the mixture is dissolved to obtain a nuclear layer solution.
S3, preparing a shell solution: mixing methacrylic acid, 3-acryloimido-3-methyl butyric acid and deionized water, stirring to obtain a mixed solution, preparing a sodium hydroxide solution, dripping the sodium hydroxide solution into the mixed solution, adding an acrylamide auxiliary agent, and regulating the pH to 6 to obtain a shell layer solution.
S4, mixing 45 parts of the oil phase solution in the S1 with 35 parts of the core layer solution in the S2, stirring at 1300r/min, introducing nitrogen, emulsifying for 30min, reducing the rotating speed to 300r/min, stirring for 30min, fully emulsifying to obtain emulsion, adding the sodium thiosulfate solution, and polymerizing at 75 ℃.
S5, adding 53 parts of the shell layer solution in S3 into the solution in S4, stirring at 300r/min, adding the sodium thiosulfate solution, and reacting at 60 ℃ for 2 hours.
S6, cooling the reaction system in the step S5 to 35 ℃, adding an acrylamide auxiliary agent, stirring, filtering, and performing suction filtration and drying to obtain the core-shell structure microsphere.
Example 3
S1, preparing an oil phase solution: mixing and stirring castor oil polyoxyethylene ether, lipopeptide and vegetable oil to obtain an oil phase solution.
S2, preparing a nuclear layer solution: and mixing dimethyl diallyl ammonium chloride, N-dimethyl acrylamide and deionized water, and stirring until the mixture is dissolved to obtain a nuclear layer solution.
S3, preparing a shell solution: mixing methacrylic acid, 3-acryloimido-3-methyl butyric acid and deionized water, stirring to obtain a mixed solution, preparing a sodium hydroxide solution, dripping the sodium hydroxide solution into the mixed solution, adding an acrylamide auxiliary agent, and regulating the pH to 6 to obtain a shell layer solution.
S4, mixing 60 parts of the oil phase solution in the S1 with 45 parts of the core layer solution in the S2, stirring at 1300r/min, introducing nitrogen, emulsifying for 30min, reducing the rotating speed to 300r/min, stirring for 30min, fully emulsifying to obtain emulsion, adding the sodium thiosulfate solution, and polymerizing at 75 ℃.
S5, adding 70 parts of the shell layer solution in S3 into the solution in S4, stirring at 300r/min, adding the sodium thiosulfate solution, and reacting at 60 ℃ for 3h under heat preservation.
S6, cooling the reaction system in the step S5 to 35 ℃, adding an acrylamide auxiliary agent, stirring, filtering, and performing suction filtration and drying to obtain the core-shell structure microsphere.
Example 4
S1, preparing an oil phase solution: mixing and stirring castor oil polyoxyethylene ether, lipopeptide and vegetable oil to obtain an oil phase solution.
S2, preparing a nuclear layer solution: and mixing dimethyl diallyl ammonium chloride, N-dimethyl acrylamide and deionized water, and stirring until the mixture is dissolved to obtain a nuclear layer solution.
S3, preparing a shell solution: mixing methacrylic acid, 3-acryloimido-3-methyl butyric acid and deionized water, stirring to obtain a mixed solution, preparing a sodium hydroxide solution, dripping the sodium hydroxide solution into the mixed solution, adding an acrylamide auxiliary agent, and regulating the pH to 6 to obtain a shell layer solution.
And S4, mixing 55 parts of the oil phase solution in the S1 with 42 parts of the core layer solution in the S2, stirring at 1300r/min, introducing nitrogen, emulsifying for 30min, reducing the rotating speed to 300r/min, stirring for 30min, fully emulsifying to obtain an emulsion, adding the sodium thiosulfate solution, and polymerizing at 75 ℃.
S5, adding 63 parts of the shell layer solution in S3 into the solution in S4, stirring at 300r/min, adding the sodium thiosulfate solution, and reacting at 60 ℃ for 3h under heat preservation.
S6, cooling the reaction system in the step S5 to 35 ℃, adding an acrylamide auxiliary agent, stirring, filtering, and performing suction filtration and drying to obtain the core-shell structure microsphere.
Example 5
Performance test of core-shell microspheres prepared in examples 1 to 4
a. Testing the shearing resistance;
the core is circularly displaced by adopting the artificial core to the core-shell structure microsphere mother liquor in the examples 1-4, and the core-shell structure microsphere has certain shearing deformation when being transported and sheared in the core, but can still keep a relatively complete sphere under the shearing action, and has better shearing resistance.
b. Testing plugging property;
the blocking rates of the core-shell microspheres of examples 1-4 at the end of injection and at the end of water flooding at different pressures are shown in table 1.
Blocking Rate of core-shell microspheres in Table 1, examples 1-4
c. Oil displacement efficiency test
The recovery enhancement for core-shell microspheres in examples 1-4 is shown in Table 2.
Table 2, table 1-4 shows the recovery ratio enhancement of core-shell microspheres with respect to water flooding
Example 1 Example 2 Example 3 Example 4
Enhanced recovery% 15.4 16.7 15.9 16.2
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting it, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that: the technical scheme of the invention can be modified or replaced by the same, and the modified technical scheme cannot deviate from the spirit and scope of the technical scheme of the invention.

Claims (9)

1. The microsphere profile control agent with the core-shell structure capable of improving recovery ratio is characterized in that: the weight portions of the oil phase solution are 45 to 60 portions, 35 to 45 portions of core layer solution, 35 to 70 portions of shell layer solution, 0.03 to 0.5 portion of initiator, 15 to 30 portions of auxiliary agent and proper amount of deionized water.
2. The core-shell microsphere profile control agent capable of improving recovery ratio according to claim 1, wherein the core-shell microsphere profile control agent is characterized in that: the oil phase solution comprises castor oil polyoxyethylene ether, lipopeptid and vegetable oil.
3. The core-shell microsphere profile control agent capable of improving recovery ratio according to claim 1, wherein the core-shell microsphere profile control agent is characterized in that: the core layer solution comprises cationic monomer, N-dimethylacrylamide and deionized water.
4. The core-shell microsphere profile control agent capable of improving recovery ratio according to claim 1, wherein the core-shell microsphere profile control agent is characterized in that: the shell solution comprises sodium hydroxide, 3-acrylimido-3-methylbutanoic acid, methacrylic acid and deionized water.
5. The core-shell microsphere profile control agent capable of improving recovery ratio according to claim 1, wherein the core-shell microsphere profile control agent is characterized in that: the initiator is one or more of potassium persulfate, sodium persulfate, ammonium persulfate, sodium sulfite, sodium thiosulfate, azodiisobutyronitrile, triethylamine and beta-dimethylaminopropionitrile.
6. The core-shell microsphere profile control agent capable of improving recovery ratio according to claim 1, wherein the core-shell microsphere profile control agent is characterized in that: the auxiliary agent is one of an acrylamide auxiliary agent and an acrylic cellulose nano-filament.
7. The core-shell microsphere profile control agent capable of improving recovery ratio according to claim 1, wherein the core-shell microsphere profile control agent is characterized in that: the cationic monomer is one or more of dimethyl diallyl ammonium halide, methacryloxyethyl diethyl benzyl ammonium halide, acryloxyethyl trimethyl ammonium chloride and methacryloxyethyl trimethyl ammonium chloride.
8. The method for preparing the microsphere profile control agent with the enhanced oil recovery ratio and a core-shell structure according to any one of claims 1 to 7, which is characterized in that: s1, preparing an oil phase solution: mixing castor oil polyoxyethylene ether and vegetable oil, and stirring to obtain an oil phase solution;
s2, preparing a nuclear layer solution: mixing a cationic monomer, N-dimethylacrylamide and deionized water, and stirring until the mixture is dissolved to obtain a nuclear layer solution;
s3, preparing a shell solution: mixing methacrylic acid, 3-acryloimido-3-methylbutyric acid and deionized water, stirring to obtain a mixed solution, preparing a sodium hydroxide solution, dripping the sodium hydroxide solution into the mixed solution, adding an auxiliary agent, and regulating the pH to 5.5-7 to obtain a shell layer solution;
s4, mixing the oil phase solution in the S1 with the core layer solution in the S2, stirring at 1200-1400r/min, introducing nitrogen to emulsify for 25-35min to obtain an emulsion, adding an initiator, and polymerizing at 65-85 ℃;
s5, adding the shell layer solution in the step S3 into the solution in the step S4, stirring at 250-350r/min, adding an initiator, and reacting at 45-60 ℃ for 2-3h in a heat preservation way;
s6, cooling the reaction system in the step S5 to 35 ℃, adding an auxiliary agent, stirring, filtering, and performing suction filtration and drying to obtain the microsphere with the core-shell structure.
9. The core-shell structure microsphere prepared by the preparation method of the core-shell structure microsphere profile control agent capable of improving recovery ratio according to claim 8, which is characterized in that: can be compounded with other chemicals or directly used for oil displacement and recovery efficiency improvement.
CN202311024277.3A 2023-08-15 2023-08-15 Core-shell structure microsphere profile control agent capable of improving recovery ratio and preparation method thereof Pending CN117050227A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102399345A (en) * 2010-09-14 2012-04-04 中国科学院理化技术研究所 Emulsion deep profile/displacement control agent and preparation method of emulsion deep profile/displacement control agent containing gel microspheres of core shell structure
CN108315003A (en) * 2017-01-17 2018-07-24 中国石油化工股份有限公司 Polyacrylamide microballoon in-depth profile control and its preparation method and application

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102399345A (en) * 2010-09-14 2012-04-04 中国科学院理化技术研究所 Emulsion deep profile/displacement control agent and preparation method of emulsion deep profile/displacement control agent containing gel microspheres of core shell structure
CN108315003A (en) * 2017-01-17 2018-07-24 中国石油化工股份有限公司 Polyacrylamide microballoon in-depth profile control and its preparation method and application

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
代刚: "热致缔合聚合物的合成及其溶液性能研究", 中国优秀博硕士学位论文全文数据库（硕士）工程科技I辑, 15 February 2019 (2019-02-15), pages 1 - 3 *

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