CN116333700B - Double-control phase-change self-repairing toughness gel plugging agent and preparation method thereof - Google Patents
Double-control phase-change self-repairing toughness gel plugging agent and preparation method thereof Download PDFInfo
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- CN116333700B CN116333700B CN202310295800.XA CN202310295800A CN116333700B CN 116333700 B CN116333700 B CN 116333700B CN 202310295800 A CN202310295800 A CN 202310295800A CN 116333700 B CN116333700 B CN 116333700B
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- 238000002360 preparation method Methods 0.000 title abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 65
- 229920000642 polymer Polymers 0.000 claims abstract description 58
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 24
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 23
- 239000003899 bactericide agent Substances 0.000 claims abstract description 23
- 230000009977 dual effect Effects 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 43
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 239000003921 oil Substances 0.000 claims description 21
- 239000002245 particle Substances 0.000 claims description 18
- 239000003995 emulsifying agent Substances 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 238000006116 polymerization reaction Methods 0.000 claims description 12
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 9
- SJIXRGNQPBQWMK-UHFFFAOYSA-N 2-(diethylamino)ethyl 2-methylprop-2-enoate Chemical compound CCN(CC)CCOC(=O)C(C)=C SJIXRGNQPBQWMK-UHFFFAOYSA-N 0.000 claims description 9
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 9
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- OMNKZBIFPJNNIO-UHFFFAOYSA-N n-(2-methyl-4-oxopentan-2-yl)prop-2-enamide Chemical compound CC(=O)CC(C)(C)NC(=O)C=C OMNKZBIFPJNNIO-UHFFFAOYSA-N 0.000 claims description 9
- 230000001105 regulatory effect Effects 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical class O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 6
- 239000000084 colloidal system Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000003999 initiator Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- YIKWKLYQRFRGPM-UHFFFAOYSA-N 1-dodecylguanidine acetate Chemical compound CC(O)=O.CCCCCCCCCCCCN=C(N)N YIKWKLYQRFRGPM-UHFFFAOYSA-N 0.000 claims description 5
- IBVAQQYNSHJXBV-UHFFFAOYSA-N adipic acid dihydrazide Chemical compound NNC(=O)CCCCC(=O)NN IBVAQQYNSHJXBV-UHFFFAOYSA-N 0.000 claims description 5
- KHSLHYAUZSPBIU-UHFFFAOYSA-M benzododecinium bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 KHSLHYAUZSPBIU-UHFFFAOYSA-M 0.000 claims description 5
- JBIROUFYLSSYDX-UHFFFAOYSA-M benzododecinium chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 JBIROUFYLSSYDX-UHFFFAOYSA-M 0.000 claims description 5
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 5
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 5
- QOHMWDJIBGVPIF-UHFFFAOYSA-N n',n'-diethylpropane-1,3-diamine Chemical compound CCN(CC)CCCN QOHMWDJIBGVPIF-UHFFFAOYSA-N 0.000 claims description 5
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 4
- 241000195493 Cryptophyta Species 0.000 claims description 4
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 4
- ZZTCPWRAHWXWCH-UHFFFAOYSA-N diphenylmethanediamine Chemical compound C=1C=CC=CC=1C(N)(N)C1=CC=CC=C1 ZZTCPWRAHWXWCH-UHFFFAOYSA-N 0.000 claims description 4
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 claims description 4
- QUSNBJAOOMFDIB-UHFFFAOYSA-O ethylaminium Chemical compound CC[NH3+] QUSNBJAOOMFDIB-UHFFFAOYSA-O 0.000 claims description 4
- 229910052744 lithium Inorganic materials 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 239000005543 nano-size silicon particle Substances 0.000 claims description 4
- 229920000191 poly(N-vinyl pyrrolidone) Polymers 0.000 claims description 4
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 4
- 229920000053 polysorbate 80 Polymers 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- 239000002689 soil Substances 0.000 claims description 4
- 229920001213 Polysorbate 20 Polymers 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 3
- ONCZQWJXONKSMM-UHFFFAOYSA-N dialuminum;disodium;oxygen(2-);silicon(4+);hydrate Chemical compound O.[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Na+].[Na+].[Al+3].[Al+3].[Si+4].[Si+4].[Si+4].[Si+4] ONCZQWJXONKSMM-UHFFFAOYSA-N 0.000 claims description 3
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims description 3
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims description 3
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 claims description 3
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 claims description 3
- 229940080314 sodium bentonite Drugs 0.000 claims description 3
- 229910000280 sodium bentonite Inorganic materials 0.000 claims description 3
- -1 tween-40 Polymers 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 2
- 238000007664 blowing Methods 0.000 claims 1
- 238000003786 synthesis reaction Methods 0.000 claims 1
- 230000007704 transition Effects 0.000 claims 1
- 239000003292 glue Substances 0.000 abstract description 7
- 239000007788 liquid Substances 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 3
- 230000009471 action Effects 0.000 abstract description 2
- 238000007789 sealing Methods 0.000 abstract description 2
- 238000005086 pumping Methods 0.000 abstract 1
- 239000000499 gel Substances 0.000 description 64
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 12
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 6
- 238000009472 formulation Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 235000010265 sodium sulphite Nutrition 0.000 description 4
- 239000000178 monomer Substances 0.000 description 3
- 229960001124 trientine Drugs 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000020477 pH reduction Effects 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000008439 repair process Effects 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000009545 invasion Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000003129 oil well Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000002464 physical blending Methods 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000004043 responsiveness Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- ANOBYBYXJXCGBS-UHFFFAOYSA-L stannous fluoride Chemical compound F[Sn]F ANOBYBYXJXCGBS-UHFFFAOYSA-L 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 235000020681 well water Nutrition 0.000 description 1
Classifications
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- 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
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/426—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells for plugging
-
- 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
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/44—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing organic binders only
-
- 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
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- 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
- C09K8/512—Compositions based on water or polar solvents containing organic compounds macromolecular compounds containing cross-linking agents
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- 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
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a double-control phase-change self-repairing toughness gel plugging agent and a preparation method thereof, and relates to the technical field of temporary gel plugging. The formula of the double-control gel comprises the following components in percentage by mass: 8-15% of polymer main agent, 0.1-2% of cross-linking agent, 0.01-0.08% of bactericide and the balance of water. The temperature is changed to control the glue speed, the pH is adjusted to control the glue strength, so that the glue is used as a temporary plugging agent for cracks or a shaft rubber plug, and the purposes of soft sealing and soft layering are achieved. The invention realizes the dual control of the gel forming speed and the strength, thereby being applicable to different stratum environments. The gel temporary plugging agent is liquid at normal temperature, can be rapidly crosslinked into gel under the action of temperature after entering a stratum, and has the advantages of simple preparation, good pumping performance, good plugging effect, easiness in flowback after gel breaking and the like.
Description
Technical Field
The invention relates to the technical field of temporary gel plugging of oil and gas fields, and discloses a double-control phase-change self-repairing tough gel plugging agent and a preparation method thereof.
Background
Polymer gels are now widely used in various fields of oil and gas field development.
In the fracturing and acidizing operation, polymer gel is generally used as a temporary plugging agent for diversion, and the principle is that after the gel is injected into a stratum, the gel preferentially enters an existing high-diversion channel for plugging, so that fluid is forced to divert, a target layer generates new cracks, and the oil gas seepage area is increased.
Because oil gas seepage is easy to be blocked by water phase, the water content of most of oilfield produced liquid in China rises rapidly, and some oilfield produced liquid is even in a production stopping state, so that the oil well water invasion is prevented by gel water shutoff operation, and the continuous stable production of the oilfield is maintained.
In workover operations, polymer gel is often used as a "liquid rubber plug" to prevent well control fluid from penetrating into the formation, blocking formation cracks, and blocking oil-gas diversion channels.
However, most polymer gels have a single effect and cannot be used for multifunctional operations. Therefore, a multifunctional gel temporary plugging system with controllable gel forming strength and gel forming time, certain permeability and easy gel breaking needs to be developed.
Disclosure of Invention
The invention aims to provide a double-control gel temporary plugging agent which has the advantages of controllable gel forming time and gel forming strength.
The second object of the present invention is to provide a method for preparing the double-control gel temporary plugging agent, which can flexibly change the gel formulation to be suitable for different stratum environments.
The third object of the invention is to provide the application of the double-control gel temporary plugging agent in well repair leakage prevention and steering fracturing acidification.
In order to achieve the above purpose, the present invention adopts the following technical scheme.
1. The double-control phase-change self-repairing toughness gel comprises the following main components in percentage by mass: 8-15% of polymer main agent, 0.1-2% of cross-linking agent, 0.01-0.08% of bactericide and the balance of water.
The polymer main agent comprises the following components in percentage by mass: 48% of polymer particles, 3% of inorganic toughening materials, 2% of emulsifying agents and 47% of white oil.
The polymer particles are prepared by copolymerizing 30-50 parts of acrylamide, 15-30 parts of diacetone acrylamide, 20-30 parts of acrylic acid and 10-20 parts of diethylaminoethyl methacrylate, wherein the weight parts are all.
The inorganic toughening material comprises one or more of lithium algae soil, hydroxyapatite, montmorillonite, organic modified bentonite, sodium bentonite and nano silicon dioxide.
The emulsifier comprises one or more of Tween-20, tween-40, tween-80, peregal, OP-10, and OP-20.
The cross-linking agent comprises one or more of adipic acid dihydrazide, diethylenetriamine, triethylenetetramine, diaminodiphenylmethane, diethylaminopropylamine and hexamethylenediamine.
The bactericide comprises one or more of dodecyl dimethyl benzyl ammonium chloride, dodecyl trimethyl ammonium chloride, dodecyl dimethyl benzyl ammonium bromide, dodecyl guanidine acetate and hexadecyl dimethyl (2-sulfurous acid) ethyl ammonium.
The invention also provides a preparation method of the polymer main agent, which comprises the following steps:
(1) Adding acrylamide, diacetone acrylamide, acrylic acid and diethylaminoethyl methacrylate with certain mass into pure water, stirring and dissolving, and regulating the pH value to be neutral by using a sodium hydroxide solution with the concentration of 2 mol/L.
(2) The reaction temperature was adjusted to 40℃and nitrogen was continuously blown in for 20min, after which an initiator was added to initiate polymerization.
(3) And (3) taking out the colloid after polymerization for 8 hours, granulating, drying and crushing to obtain the polymer particles.
(4) Placing the white oil into a stirring cup, regulating the rotating speed of a stirrer to 2000r/min, adding an emulsifying agent, and stirring for 20min; adding the inorganic toughening material, stirring for 20min, adding the polymer particles, and continuously stirring for 40min to obtain the polymer main agent.
The embodiment of the invention provides a double-control phase-change self-repairing tough gel, which has the beneficial effects that: adding the cross-linking agent and the bactericide into water, stirring and dissolving, dripping 2mol/L sodium hydroxide solution to regulate the pH value, and finally adding the polymer main agent into the mixture, and stirring the mixture uniformly to obtain the gel temporary plugging agent. The gel forming process can be carried out at 65-140 deg.C, and the gel forming time can be controlled at 15-120min.
The temperature is changed to control the glue speed, the pH is adjusted to control the glue strength, so that the glue is used as a temporary plugging agent for cracks or a shaft rubber plug, and the purposes of soft sealing and soft layering are achieved. The invention realizes the dual control of the glue forming speed and the strength, so that the invention is suitable for different stratum environments; the gel is liquid at normal temperature, can be rapidly crosslinked into gel under the action of temperature after entering a stratum, and has the advantages of simple preparation, good pumpability, good plugging effect, easiness in flowback after gel breaking and the like.
Drawings
FIG. 1 shows the gel morphology of a dual-control phase-change self-healing ductile gel according to an embodiment of the present invention;
FIG. 2 is a graph showing the rheological profile of a dual control phase change self-healing ductile gel forming process according to an embodiment of the present invention;
FIG. 3 is a graph showing the morphology after breaking with ammonium persulfate;
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent.
The double-control phase-change self-repairing ductile gel temporary plugging agent provided by the embodiment of the invention is prepared by simply stirring and mixing a polymer main agent, a cross-linking agent, a bactericide and water, and has the advantages of simple preparation process and convenience for site construction. The gel forming strength can be controlled under the condition of the gel forming temperature of 65-140 ℃. The stronger the gel strength, the more difficult the corresponding gel breaking. For the low-pressure stratum environment with low requirement on gel strength, the gel is easier to break in the later period, and a low-strength gel system can be adopted.
In order to improve the performance of the gel temporary plugging agent, after a large number of experiments are carried out, a better formula proportion is obtained, and the gel temporary plugging agent comprises the following components in percentage by mass: 8-15% of polymer main agent, 0.1-2% of cross-linking agent, 0.01-0.08% of bactericide and the balance of water.
Specifically, the polymer main agent consists of polymer particles, inorganic toughening materials, emulsifying agents and white oil
Further, the polymer particles are prepared by polymerizing four monomers of acrylamide, diacetone acrylamide, acrylic acid and diethylaminoethyl methacrylate through aqueous solution. The monomers are all commercial raw materials, and the characteristic functional groups on the monomers endow the gel with temperature and pH responsiveness, self-repairing property and toughness, so that the gel is suitable for application in well repair leakage prevention and steering fracturing acidification.
Further, the inorganic toughening material is selected from one or more of lithium algae soil, hydroxyapatite, montmorillonite, organic modified bentonite, sodium bentonite and nano silicon dioxide. The inorganic toughening material not only forms a gel structure in a simple physical blending mode, but also can be used as a functional cross-linking agent to form a special inorganic/organic network structure, so that the strength and toughness of the gel are greatly improved.
Further, the emulsifier is selected from one or more of Tween-20, tween-40, tween-80, peregal, OP-10, and OP-20. The emulsifier can improve the stability of the polymer main agent, and is favorable for long-term storage and long-distance transportation.
Specifically, the cross-linking agent is selected from one or more of adipic acid dihydrazide, diethylenetriamine, triethylenetetramine, diaminodiphenylmethane, diethylaminopropylamine and hexamethylenediamine. Crosslinking agents are necessary agents for forming a three-dimensional network structure from a gel, creating chemical bonds between linear polymer molecules, interconnecting the linear molecules together, and changing from a liquid state to a solid state.
Specifically, the bactericide is one or more selected from dodecyl dimethyl benzyl ammonium chloride, dodecyl trimethyl ammonium chloride, dodecyl dimethyl benzyl ammonium bromide, dodecyl guanidine acetate and hexadecyl dimethyl (2-sulfurous acid) ethyl ammonium. The bactericide can effectively control the growth and propagation of stratum bacteria, and avoid the influence of metabolites generated by bacteria on the gel forming strength.
The features and capabilities of the present invention are described in further detail below in connection with the examples.
Example 1
The preparation of the polymer main agent comprises the following steps:
(1) 35 parts of acrylamide, 15 parts of diacetone acrylamide, 30 parts of acrylic acid and 20 parts of diethylaminoethyl methacrylate are added to a certain mass of pure water and dissolved by stirring.
(2) The reaction temperature was adjusted to 40℃and nitrogen was continuously blown in for 20 minutes, followed by the addition of 0.02 part of ammonium persulfate and 0.02 part of sodium sulfite initiator to initiate polymerization.
(3) And (3) taking out the colloid after polymerization for 8 hours, granulating, drying and crushing to obtain polymer particles.
(4) Placing 47 parts of white oil into a stirring cup, regulating the rotating speed of a stirrer to 2000r/min, adding 2 parts of emulsifier Tween-40, and stirring for 20min; and adding 3 parts of lithium algae soil, stirring for 20min, adding 48 parts of polymer particles, and continuously stirring for 40min to obtain the polymer main agent.
The preparation method of the gel temporary plugging agent comprises the following steps:
(1) Adding the cross-linking agent and the bactericide into water, stirring and dissolving, dripping 2mol/L sodium hydroxide solution to adjust the pH value to 8, and finally adding the polymer main agent into the mixture, and stirring uniformly to obtain the gel temporary plugging agent. Wherein, the formula of the system is as follows: 9% of polymer main agent, 0.3% of cross-linking agent adipic dihydrazide, 0.03% of bactericide dodecyl dimethyl benzyl ammonium chloride and the balance of water.
(2) Placing the prepared gel temporary plugging agent into an oil bath pot at 90 ℃ to examine the gelling condition.
Example 2
The preparation of the polymer main agent comprises the following steps:
(1) 40 parts of acrylamide, 20 parts of diacetone acrylamide, 20 parts of acrylic acid and 20 parts of diethylaminoethyl methacrylate are added to a certain mass of pure water and dissolved by stirring.
(2) The reaction temperature was adjusted to 40℃and nitrogen was continuously blown in for 20 minutes, followed by the addition of 0.02 part of ammonium persulfate and 0.02 part of sodium sulfite initiator to initiate polymerization.
(3) And (3) taking out the colloid after polymerization for 8 hours, granulating, drying and crushing to obtain polymer particles.
(4) Placing 47 parts of white oil into a stirring cup, regulating the rotating speed of a stirrer to 2000r/min, adding 2 parts of emulsifier Tween-80, and stirring for 20min; then adding 2 parts of montmorillonite and 1 part of mechanically modified bentonite, stirring for 20min, adding 48 parts of polymer particles, and continuously stirring for 40min to obtain the polymer main agent.
The preparation method of the gel temporary plugging agent comprises the following steps:
(1) Adding the cross-linking agent and the bactericide into water, stirring and dissolving, dripping 2mol/L sodium hydroxide solution to adjust the pH value to 9, and finally adding the polymer main agent into the mixture, and stirring uniformly to obtain the gel temporary plugging agent. Wherein, the formula of the system is as follows: 11% of polymer main agent, 0.5% of cross-linking agent diethylenetriamine, 0.04% of bactericide dodecylguanidine acetate and the balance of water.
(2) Placing the prepared gel temporary plugging agent into an oil bath pot at 90 ℃ to examine the gelling condition.
Example 3
The preparation of the polymer main agent comprises the following steps:
(1) 30 parts of acrylamide, 25 parts of diacetone acrylamide, 30 parts of acrylic acid and 15 parts of diethylaminoethyl methacrylate are added to a certain mass of pure water and dissolved by stirring.
(2) The reaction temperature was adjusted to 40℃and nitrogen was continuously blown in for 20 minutes, followed by the addition of 0.02 part of ammonium persulfate and 0.02 part of sodium sulfite initiator to initiate polymerization.
(3) And (3) taking out the colloid after polymerization for 8 hours, granulating, drying and crushing to obtain polymer particles.
(4) Placing 47 parts of white oil into a stirring cup, regulating the rotation speed of a stirrer to 2000r/min, adding 1 part of emulsifier OP-10 and 1 part of OP-20, and stirring for 20min; then adding 1 part of organic modified bentonite and 2 parts of montmorillonite, stirring for 20min, adding 48 parts of polymer particles, and continuously stirring for 40min to obtain the polymer main agent.
The preparation method of the gel temporary plugging agent comprises the following steps:
(1) Adding the cross-linking agent and the bactericide into water, stirring and dissolving, dripping 2mol/L sodium hydroxide solution to adjust the pH value to 10, and finally adding the polymer main agent into the mixture, and stirring uniformly to obtain the gel temporary plugging agent. Wherein, the formula of the system is as follows: 13% of polymer main agent, 0.9% of cross-linking agent diethylaminopropylamine, 0.05% of bactericide dodecyl trimethyl ammonium chloride and the balance of water.
(2) Placing the prepared gel temporary plugging agent into an oil bath pot at 90 ℃ to examine the gelling condition.
Example 4
The preparation of the polymer main agent comprises the following steps:
(1) 45 parts of acrylamide, 20 parts of diacetone acrylamide, 20 parts of acrylic acid and 15 parts of diethylaminoethyl methacrylate are added to a certain mass of pure water and dissolved by stirring.
(2) The reaction temperature was adjusted to 40℃and nitrogen was continuously blown in for 20 minutes, followed by the addition of 0.02 part of ammonium persulfate and 0.02 part of sodium sulfite initiator to initiate polymerization.
(3) And (3) taking out the colloid after polymerization for 8 hours, granulating, drying and crushing to obtain polymer particles.
(4) Placing 47 parts of white oil into a stirring cup, regulating the rotating speed of a stirrer to 2000r/min, adding 2 parts of emulsifier peregal, and stirring for 20min; adding 1 part of organic modified bentonite and 2 parts of nano silicon dioxide, stirring for 20min, adding 48 parts of polymer particles, and stirring for 40min to obtain a polymer main agent
The preparation method of the gel temporary plugging agent comprises the following steps:
(1) Adding the cross-linking agent and the bactericide into water, stirring and dissolving, dripping 2mol/L sodium hydroxide solution to adjust the pH value to 10, and finally adding the polymer main agent into the mixture, and stirring uniformly to obtain the gel temporary plugging agent. Wherein, the formula of the system is as follows: 12% of polymer main agent, 0.8% of cross-linking agent diamino diphenyl methane, 0.04% of bactericide dodecyl dimethyl benzyl ammonium bromide and the balance of water.
(2) Placing the prepared gel temporary plugging agent into an oil bath pot at 90 ℃ to examine the gelling condition.
Example 5
This example is largely identical to example 2, except that the system formulation is: 10% of polymer main agent, 1% of cross-linking agent triethylene tetramine, 0.05% of bactericide hexadecyldimethyl (2-sulfurous acid) ethyl ammonium and the balance of water. The oil bath temperature was 65 ℃.
Example 6
This example is largely identical to example 2, except that the system formulation is: 13% of polymer main agent, 0.7% of cross-linking agent hexamethylenediamine, 0.05% of bactericide dodecyl dimethyl benzyl ammonium chloride and the balance of water. The temperature of the oil bath pot is 100 ℃.
Example 7
This example is largely identical to example 3, except that the system formulation is: 12% of polymer main agent, 0.8% of cross-linking agent adipic dihydrazide, 0.06% of bactericide dodecyl dimethyl benzyl ammonium bromide and the balance of water. The temperature of the oil bath pot was 120 ℃.
Example 8
This example is largely identical to example 3, except that the system formulation is: 13% of polymer main agent, 0.8% of cross-linking agent diethylaminopropylamine, 0.06% of bactericide dodecylguanidine acetate and the balance of water. The oil bath temperature was 140 ℃.
Test example 1
The gel temporary plugging agent in the embodiment 2 has a gel forming morphology shown in fig. 1 after 60min of reaction, has higher toughness and mechanical strength as a whole, and shows certain self-repairing property.
Test example 2
The rheological curve of the gel temporary plugging agent prepared in the example 2 is tested, and the result is shown in fig. 2. From the figure, it can be seen that 90℃170S -1 In the following, there is a shear thickening phenomenon. Especially after 20min, the viscosity rise rate is accelerated, the strength is obviously increased, and the adhesive is basically and completely formed within 60 min.
Test example 3
The gel temporary plugging agent prepared in the example 2 is tested for gel breaking property, and a physical diagram after gel breaking is shown in fig. 3. The addition amount of the breaker ammonium persulfate is 1%, the breaking temperature is 90 ℃, and the breaking time is 120min. From the figure, the broken liquid has low viscosity and less residue, is easy to flow back in the stratum and can not cause damage to the stratum.
Claims (3)
1. A dual-control phase-change self-healing malleable gel, comprising: 8-15% of polymer main agent, 0.1-2% of cross-linking agent, 0.01-0.08% of bactericide and the balance of water;
the polymer main agent comprises the following components in percentage by mass: 48% of polymer particles, 3% of inorganic toughening materials, 2% of emulsifying agents and 47% of white oil;
the polymer particles are formed by copolymerizing 30-50 parts of acrylamide, 15-30 parts of diacetone acrylamide, 20-30 parts of acrylic acid and 10-20 parts of diethylaminoethyl methacrylate, wherein the weight parts are respectively;
the inorganic toughening material comprises one or more of lithium algae soil, hydroxyapatite, montmorillonite, organic modified bentonite, sodium bentonite and nano silicon dioxide;
the emulsifier comprises one or more of Tween-20, tween-40, tween-80, peregal, OP-10 and OP-20;
the cross-linking agent comprises one or more of adipic acid dihydrazide, diethylenetriamine, triethylenetetramine, diaminodiphenylmethane, diethylaminopropylamine and hexamethylenediamine;
the bactericide comprises one or more of dodecyl dimethyl benzyl ammonium chloride, dodecyl trimethyl ammonium chloride, dodecyl dimethyl benzyl ammonium bromide, dodecyl guanidine acetate and hexadecyl dimethyl (2-sulfurous acid) ethyl ammonium.
2. The dual control phase change self-healing malleable gel of claim 1, wherein the polymer base synthesis comprises the steps of:
(1) Adding acrylamide, diacetone acrylamide, acrylic acid and diethylaminoethyl methacrylate with certain mass into pure water, stirring and dissolving, and regulating the pH value to be neutral by using a sodium hydroxide solution with the concentration of 2 mol/L;
(2) Regulating the reaction temperature to 40 ℃, continuously blowing nitrogen for 20min, and then adding an initiator to initiate polymerization;
(3) Taking out colloid after polymerization for 8 hours, granulating, drying and crushing to obtain polymer particles;
(4) Placing white oil into a stirring cup, regulating the rotation speed of a stirrer to 2000r/min, adding an emulsifying agent, stirring for 20min, adding an inorganic toughening material, stirring for 20min, adding polymer particles, and continuously stirring for 40min to obtain a polymer main agent.
3. The dual control phase transition self-healing malleable gel according to claim 1, wherein the gel is obtained by the following method: adding a cross-linking agent and a bactericide into water, stirring and dissolving, dropwise adding a sodium hydroxide solution with the concentration of 2mol/L to adjust the pH value, and finally adding a polymer main agent into the mixture, and stirring uniformly to obtain a gel temporary plugging agent; wherein the gel forming temperature is 65-140 ℃, and the gel forming time is 15-120min.
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