CN114426652B - High-temperature-resistant nano-micron plugging agent for drilling fluid and preparation method thereof - Google Patents
High-temperature-resistant nano-micron plugging agent for drilling fluid and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 122
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 61
- 239000000178 monomer Substances 0.000 claims abstract description 43
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- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 6
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- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 8
- ZORQXIQZAOLNGE-UHFFFAOYSA-N 1,1-difluorocyclohexane Chemical compound FC1(F)CCCCC1 ZORQXIQZAOLNGE-UHFFFAOYSA-N 0.000 claims description 7
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- -1 pH regulator Substances 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
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- DZSVIVLGBJKQAP-UHFFFAOYSA-N 1-(2-methyl-5-propan-2-ylcyclohex-2-en-1-yl)propan-1-one Chemical compound CCC(=O)C1CC(C(C)C)CC=C1C DZSVIVLGBJKQAP-UHFFFAOYSA-N 0.000 claims description 4
- XLPJNCYCZORXHG-UHFFFAOYSA-N 1-morpholin-4-ylprop-2-en-1-one Chemical compound C=CC(=O)N1CCOCC1 XLPJNCYCZORXHG-UHFFFAOYSA-N 0.000 claims description 4
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 4
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- PQUXFUBNSYCQAL-UHFFFAOYSA-N 1-(2,3-difluorophenyl)ethanone Chemical compound CC(=O)C1=CC=CC(F)=C1F PQUXFUBNSYCQAL-UHFFFAOYSA-N 0.000 claims description 3
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 3
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 3
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 3
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 3
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- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 229940047670 sodium acrylate Drugs 0.000 claims description 3
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 3
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 3
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 3
- MNCGMVDMOKPCSQ-UHFFFAOYSA-M sodium;2-phenylethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=CC1=CC=CC=C1 MNCGMVDMOKPCSQ-UHFFFAOYSA-M 0.000 claims description 3
- MTNDZQHUAFNZQY-UHFFFAOYSA-N imidazoline Chemical compound C1CN=CN1 MTNDZQHUAFNZQY-UHFFFAOYSA-N 0.000 claims description 2
- 239000004289 sodium hydrogen sulphite Substances 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 15
- 239000000377 silicon dioxide Substances 0.000 abstract description 11
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 6
- 239000011148 porous material Substances 0.000 abstract description 4
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 abstract description 3
- 239000003345 natural gas Substances 0.000 abstract description 3
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- 239000002002 slurry Substances 0.000 description 25
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- 238000010526 radical polymerization reaction Methods 0.000 description 4
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 230000000903 blocking effect Effects 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
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- 230000036571 hydration Effects 0.000 description 3
- 238000006703 hydration reaction Methods 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- UWNADWZGEHDQAB-UHFFFAOYSA-N 2,5-dimethylhexane Chemical group CC(C)CCC(C)C UWNADWZGEHDQAB-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 239000000440 bentonite Substances 0.000 description 2
- 229910000278 bentonite Inorganic materials 0.000 description 2
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical group O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 2
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- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 2
- 229920000536 2-Acrylamido-2-methylpropane sulfonic acid Polymers 0.000 description 1
- XHZPRMZZQOIPDS-UHFFFAOYSA-N 2-Methyl-2-[(1-oxo-2-propenyl)amino]-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(C)(C)NC(=O)C=C XHZPRMZZQOIPDS-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
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- 239000008186 active pharmaceutical agent Substances 0.000 description 1
- 150000001409 amidines Chemical class 0.000 description 1
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 1
- 239000010428 baryte Substances 0.000 description 1
- 229910052601 baryte Inorganic materials 0.000 description 1
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- 125000000524 functional group Chemical group 0.000 description 1
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- 229920001477 hydrophilic polymer Polymers 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
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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
- C08F285/00—Macromolecular compounds obtained by polymerising monomers on to preformed graft polymers
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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
- C08F292/00—Macromolecular compounds obtained by polymerising monomers on to inorganic materials
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- 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
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
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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
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
- C09K8/035—Organic additives
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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
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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
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/10—Nanoparticle-containing well treatment fluids
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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The application provides a high-temperature-resistant nano-micron plugging agent for drilling fluid applicable to a fractured stratum and a preparation method thereof, and belongs to the technical field of petroleum and natural gas drilling engineering. The high-temperature-resistant nano-micron plugging agent comprises the following raw materials: the hydrophilic nano silica comprises 1-20 parts by weight of hydrophilic nano silica, 10-40 parts by weight of hydrophilic nano silica, 0.5-5 parts by weight of emulsifier, 0.05-5 parts by weight of sodium bicarbonate, 0.01-5 parts by weight of tetraethyl orthosilicate, 0.05-3.5 parts by weight of initiator and 50-200 parts by weight of tap water relative to 100 parts by weight of hydrophobic alkenyl monomer. The high-temperature-resistant nano-micron plugging agent provided by the application has good high-temperature-resistant deformable plugging performance on deep fractured formations, and can obviously reduce the pore pressure transmission effect of the fractured formations.
Description
Technical Field
The invention belongs to the technical field of petroleum and natural gas drilling engineering, and particularly relates to an anti-high-temperature nano-micron plugging agent for drilling fluid applicable to a fractured stratum and a preparation method thereof.
Background
The drilling fluid strong plugging technology is one of key technologies in deep well and ultra-deep well drilling engineering. Along with the development of petroleum and natural gas exploration in China, the deep oil and gas resource is gradually expanded, and the high-temperature plugging technology for drilling fluid is more and more severely required. The deep stratum has large ground temperature gradient, high bottom hole temperature and large stratum pressure coefficient, and is influenced by the movement of an extrusion structure, and micro cracks, micro holes and the like of the deep stratum rock are relatively developed, so that drilling fluid filtrate, even the leakage of the drilling fluid into a fractured stratum, easily occurs in the actual drilling process, thereby causing the erosion and collapse of the well wall of the open hole stratum, frequent jamming of a downhole drilling tool is often caused, and downhole jamming faults even the scrapping of a borehole are caused in severe cases. However, the deformable plugging agent, especially the deformable nano-micron plugging agent, is added into the drilling fluid, so that the nano-micron fracture pores of the deep fractured stratum can be effectively plugged, and the leakage of the drilling fluid and filtrate thereof in the deep micro-fractured stratum can be effectively reduced, so that the complex drilling accidents caused by the leakage can be reduced and even effectively avoided.
At present, aiming at the plugging of deep fractured formations, a traditional asphalt high-temperature-resistant deformable plugging agent (such as modified asphalt or sulfonated asphalt) and the like are added into a drilling fluid, and ultrafine solid particles such as ultrafine calcium carbonate and the like are added into the drilling fluid at the same time so as to enhance the plugging performance of the drilling fluid. As disclosed in chinese patent application 201811039787.7, a pressure-bearing plugging agent for high temperature resistant oil-based drilling fluid, comprising, based on 100 parts by weight of the pressure-bearing plugging agent, 5-15 parts by weight of oxidized asphalt, 5-20 parts by weight of hydrophobically modified sulfonated asphalt, 3-5 parts by weight of hard asphalt, 2-5 parts by weight of asphalt resin, 5-20 parts by weight of hydrophobically modified nano-or micro-scale graphite oxide, 5-30 parts by weight of substituted styrene acrylate copolymer and the balance hydrophobically modified nano-or micro-scale rigid solid particulate material. However, drilling construction practice shows that on-site drilling fluid has limited plugging capability by adopting single traditional asphalt deformable plugging agents, and is difficult to form strong plugging compact mud cakes aiming at finer nano-micro cracks, and drilling fluid and filtrate thereof still can leak in the nano-micro hole seams under the action of pressure difference, so that effective plugging of a fractured stratum (especially the condition of developing the nano-micro hole seams in the fractured stratum) is difficult to realize, repeated backfill sidetracking is still often caused in the drilling construction process, the safe well formation and the well drilling aging are seriously influenced, and the existing nano-micro plugging agent for the drilling fluid is more suitable for plugging the nano-micro hole seams in shale gas stratum or shale stratum, and generally has good plugging performance.
At present, researches on nano-micron plugging agents are more, such as documents (Mao Hui. Development and action mechanism of hydrophobic association polymer/nano-silica filtrate reducer [ J ]. Petroleum report, 2015,35 (4): 771-778), report that a polymer matrix composite material formed by modifying a polymer material with nano-silica particles has a core-shell structure, and the inorganic property of nano-silica is utilized to obtain the high-temperature-resistant filtrate reducer taking the hydrophobic association polymer as a main body, and experimental results show that the polymer matrix composite material has certain nano-micron plugging performance, but the novel material belongs to the polymer viscosity-increasing filtrate reducer for the high-temperature-resistant drilling fluid, is mainly used for reducing the filtrate loss of the drilling fluid, and is not mainly used for enhancing the nano-micron plugging performance of the drilling fluid.
The Chinese patent application CN 105884954A discloses a temperature-resistant and salt-resistant latex plugging agent and a preparation method thereof, wherein the latex plugging agent with a core-shell structure is prepared by optimizing the structure of the nano-micron latex plugging agent and utilizing hydrophobic monomers, hydrophilic monomers, emulsifying agents, buffering agents, molecular weight regulators, protective agents, initiators and water, the latex plugging agent with a core-shell structure is resistant to high temperature of 170 ℃, and is difficult to break emulsion and high in stability in a high-temperature and high-salt drilling environment when being used for drilling fluid.
The Chinese patent application CN 105199688A discloses an intelligent nano-micron plugging agent for water-based drilling fluid, which is prepared by selecting magnetic nano particles modified by intelligent polymers, polyethylene glycol, polytetrahydrofuran glycol and other raw materials, wherein the hydrophilic performance and the hydrophobic performance of the intelligent nano-micron plugging agent can be correspondingly changed along with the difference of formation temperature and pH value of the drilling fluid, so that the functions of physical plugging and the like can be carried out on tiny pores of a well wall in the drilling process of a shale stratum, and finally the water blocking performance of the drilling fluid is improved to a certain extent.
However, in practical application, the plugging agents have certain deformability, the inner cores of some plugging agents also have certain elasticity and deformability, the plugging agents are easy to deform and escape under the action of external pressure in microcracks, the nano-micron plugging effect is poor, and especially the microcrack plugging effect aiming at deep high Wen Liefeng stratum still needs to be improved; meanwhile, the existing nano-micron plugging agents are insufficient in high-temperature resistance and can resist high temperature of more than 180 ℃ and few in nano-micron plugging agents, so that when the nano-micron plugging agents are applied to deep high Wen Liefeng complex stratum, phenomena such as thermal degradation, coalescence and sedimentation are easy to occur, and finally the nano-micron plugging performance of drilling fluid added with the nano-micron plugging agents is reduced, and the plugging effect of nano-micron microcracks is not ideal.
Disclosure of Invention
Based on the defects and shortcomings in the prior art, the application aims to provide the high-temperature-resistant nano-micron plugging agent for the drilling fluid applicable to the fractured stratum and the preparation method thereof, wherein the high-temperature-resistant nano-micron plugging agent is not easy to escape due to external pressure in the drilling environment of the high-temperature fractured stratum when being used for the drilling fluid of a deep well due to the core-mantle-shell structure, has high-temperature stability and high salt resistance, and can obviously improve the nano-micron plugging performance of the drilling fluid.
In particular, on the one hand, the invention provides a high-temperature-resistant nano-micron plugging agent for drilling fluid applicable to a fractured stratum, wherein the high-temperature-resistant nano-micron plugging agent comprises the following raw materials: hydrophilic nano silicon dioxide, hydrophobic alkenyl monomer, hydrophilic alkenyl monomer, emulsifier, pH regulator, silane coupling agent, initiator and tap water;
The high temperature resistant nano-micron plugging agent comprises, by weight, relative to 100 parts of the hydrophobic alkenyl monomer, 1-20 parts of hydrophilic nano-silica, 10-40 parts of hydrophilic alkenyl monomer, 0.5-5 parts of emulsifier, 0.05-5 parts of pH regulator, 0.01-5 parts of silane coupling agent, 0.05-3.5 parts of initiator and 50-200 parts of tap water.
In some preferred embodiments, the particles of the high temperature resistant nano-micron blocking agent have a "core-veil-shell" structure, wherein the "core" of the high temperature resistant nano-micron blocking agent particles comprises hydrophilic nano-silica modified with a silane coupling agent; the "veil" of the high temperature resistant nano-micron plugging agent particles comprises a poorly soluble hydrophobically associating polymer formed by free radical polymerization of a relatively large amount of hydrophobic alkenyl monomer and a very small amount of hydrophilic monomer; the "shell" of the high temperature resistant nano-micron blocking agent particles comprises a water-soluble hydrophobic association polymer formed by free radical polymerization of a relatively small amount of hydrophobic alkenyl monomer and a relatively large amount of hydrophilic monomer.
In other preferred embodiments, the hydrophobic alkenyl monomer is selected from one or more of the group consisting of acryloylmorpholine, styrene, methyl acrylate, methyl methacrylate, butyl acrylate, and butyl methacrylate.
In other preferred embodiments, the hydrophilic alkenyl monomer is selected from one or more of acrylamide, 2-acrylamido-2-methylpropanesulfonic acid, sodium acrylate, maleic anhydride, N-vinylpyrrolidone, and sodium styrene sulfonate.
In other preferred embodiments, the hydrophilic nanosilica is selected from nanosilicas having a particle size of from 10nm to 100 nm.
In other preferred embodiments, the emulsifier is one or more of sorbitan monooleate, alkylphenol ethoxylates, and sodium dodecyl sulfate.
In other preferred embodiments, the initiator is selected from one or two of azobisiso Ding hydrochloride, azobisisobutylamidine hydrochloride, azobiscyano valeric acid or azobisisopropyl imidazoline, ammonium persulfate, and sodium bisulfite.
In other preferred embodiments, the nano-sized blocking agent has an average particle size of 50nm to 400nm and the average particle size range is adjustable.
In other preferred embodiments, the silane coupling agent is tetraethyl orthosilicate.
In other preferred embodiments, the pH adjuster is sodium bicarbonate.
On the other hand, the invention also provides a preparation method of the high-temperature-resistant nano-micron plugging agent for the drilling fluid applicable to the deep well fractured formation, which comprises the following steps:
(1) Mixing 90 parts by weight of hydrophobic alkenyl monomer, 0-10 parts by weight of hydrophilic alkenyl monomer, 0.5-3.5 parts by weight of emulsifier and 45-50 parts by weight of tap water, and stirring to prepare a first mixed solution;
(2) Mixing and stirring the rest weight parts of hydrophobic alkenyl monomer, the rest weight parts of hydrophilic alkenyl monomer, 0.5-2 weight parts of emulsifier and 50-110 weight parts of tap water to prepare a second mixed solution;
(3) Mixing 10-15 parts by weight of tap water and all the initiator to prepare a third mixed solution;
(4) Mixing and stirring the pH regulator, the silane coupling agent, the nano silicon dioxide and the rest tap water, and performing ultrasonic treatment for 20min to prepare a fourth mixed solution;
(5) Adding the fourth mixed solution into a container, stirring and mixing uniformly, heating to 68-72 ℃ and stirring for 30min under the protection of inert gas; then, dripping the first mixed solution obtained in the step (1) and simultaneously dripping the third mixed solution obtained in the step (3) to keep the temperature of the reaction container unchanged; after the first mixed liquid is dripped, preserving heat for 50-70min, and then starting to add the second mixed liquid obtained in the step (2) and simultaneously starting to drip the rest third mixed liquid; after the second mixed liquid is dripped, the high temperature resistant nano-micron plugging agent is obtained after heat preservation for 4 hours at 80-85 ℃.
The weight ratio of the third mixed solution added dropwise in the step (5) to the third mixed solution added dropwise in the second step is 3:2, and the two times of adding are controlled to be 40-50min and 30min respectively.
Compared with the common polymer latex or polymer-based nano-micron plugging agent, the high-temperature-resistant nano-micron plugging agent provided by the embodiment of the application has better nano-micron plugging performance and temperature-resistant and salt-resistant capabilities in deep fractured formations, and the temperature-resistant capabilities are more than 180 ℃. This is mainly due to: the rechecking material composed of the rigid nano silicon dioxide particles and the polymer can combine the characteristics of the rigid particles and the polymer, so that the rechecking material has more excellent thermal stability; the hard core composed of the rigid nano silicon dioxide, the curtain composed of the hydrophobic polymer and the outer shell composed of the hydrophilic polymer enable the inner core of the nano plugging agent to be clamped and kept unchanged in the nano cracks under the existence of external pressure, the holes and the cracks can be plugged spatially in the nano cracks, and the outer structure curtain and the shell can be extruded into the nano cracks through deformation under the action of the external pressure; the hydrophobic association polymer formed by polymerizing the hydrophobic alkenyl monomer and the hydrophilic alkenyl monomer has better temperature resistance and salt resistance; in addition, the outer layer shell of the core-mantle-shell structure of the high-temperature resistant nano-micron plugging agent is a strong hydrophilic shell, contains more strong hydration groups and adsorption groups, and contains strong hydrophilic high-temperature resistant salt groups, so that nano-micron particles can be strongly adsorbed on the wall surface of a microcrack to ensure that the nano-micron particles are not easy to escape in the microcrack, and the compatibility of the nano-micron plugging agent in drilling fluid can be improved, and meanwhile, the surface hydration film thickness and the temperature resistant salt resistance of the high-temperature resistant nano-micron plugging agent are improved.
Compared with the prior art, the invention has the beneficial effects that:
(1) In the deep well complex fracture stratum drilling construction process, the high temperature resistant nano-micron plugging agent provided by the invention presents nano-micron particles with a certain particle size range distribution, wherein the inner rigid core has an inflexibility characteristic, and the outer veil and the shell have a certain deformability characteristic. In the drilling construction process, under the action of the pressure of a drilling fluid column at the bottom of a well, the deformable part in the high-temperature-resistant nano-micron plugging agent is easy to squeeze into micro cracks and holes in nano-micron scale units, so that the effects of plugging the nano-micron cracks and reducing the leakage amount of the drilling fluid are achieved;
(2) The high temperature resistant nano-micron plugging agent provided by the invention is an inorganic/organic composite material nano-micron plugging agent with a 'core-shell' structure, wherein the inner core is a modified nano-silica rigid 'hard core', the middle layer is a deformable elastic layer formed by hydrophobic polymers, the outer layer is a hydrophobic association polymer, the shell contains specific functional groups, and the carried hydration groups and adsorption groups can form stronger interaction with rock minerals and the like in micro cracks, so that the stagnation effect of the deformable nano-micron plugging agent in the micro cracks is enhanced, the nano-micron cracks can be greatly plugged by combining the blocking effect of the micro cracks on nano-micron particles, and the leakage amount of deep fractured stratum drilling fluid is reduced, thereby reducing or eliminating the underground complex conditions such as borehole wall instability and the like caused by the leakage of the drilling fluid.
Drawings
FIG. 1 is a TEM image of a high temperature resistant nano-micro plugging agent for drilling fluids suitable for deep well fractured formations prepared in example 1;
FIG. 2 is an SEM image of the high temperature resistant nano-micron plugging agent on the surface of mud cake for drilling fluid suitable for deep well fractured formations prepared in example 1;
FIG. 3 is a particle size distribution of the high temperature resistant nano-micron plugging agent for drilling fluids suitable for deep well fractured formations prepared in example 1;
FIG. 4 is the PPA test results of each of the experimental slurries prepared in example 1 after aging for 16 hours at 150 ℃ in the experimental slurries of the high temperature resistant nano-micron plugging agent for drilling fluid suitable for deep well fractured formations;
FIG. 5 is a plot of filtrate volume versus square root of time for each of the experimental slurries prepared in example 1 after 150 ℃ aging for 16 hours of the high temperature resistant nano-micron plugging agent for drilling fluids suitable for deep well fractured formations;
FIG. 6 is a plot of filtrate volume versus square root of time for each of the experimental slurries prepared in example 1 after 180℃aging for 16 hours in the experimental slurries for a high temperature resistant nano-micron plugging agent for drilling fluids suitable for deep well fractured formations;
FIG. 7 is a plot of filtrate volume versus square root of time for each comparative experimental slurry prepared in example 1 after 180℃aging for 16 hours in the experimental slurry for a high temperature resistant nano-micron plugging agent for drilling fluids suitable for deep well fractured formations;
FIG. 8 is the PPA test results of comparative test slurries prepared in example 1 after 180℃aging for 16 hours in the test slurries of the high temperature resistant nano-micron plugging agent for drilling fluids suitable for deep well fractured formations;
Fig. 9 is a result of an experiment for evaluating the pressure transmission effect of the high temperature resistant nano-micron plugging agent for drilling fluid applicable to deep well fractured formations prepared in example 1 in a shale sample.
Detailed Description
Embodiments of the present application will now be described by way of specific examples, which are chosen to illustrate the objects of the present application and not to limit the scope of the application.
Basic example high temperature resistant nano-micron plugging agent for drilling fluid
The high temperature resistant nano-micron plugging agent is prepared from the following raw materials including hydrophilic nano-silica, hydrophobic alkenyl monomer, hydrophilic alkenyl monomer, emulsifier, pH regulator, silane coupling agent, initiator and tap water.
Wherein the content of the hydrophilic nano silica is 1-20 parts by weight, the content of the hydrophilic alkenyl monomer is 10-40 parts by weight, the content of the emulsifier is 0.5-5 parts by weight, the content of the pH regulator is 0.05-5 parts by weight, the content of the silane coupling agent is 0.01-5 parts by weight, the content of the initiator is 0.05-3.5 parts by weight, and the content of tap water is 50-200 parts by weight, relative to 100 parts by weight of the hydrophobic alkenyl monomer.
The particles of the high temperature resistant nano-micron plugging agent have a 'core-veil-shell' structure, wherein the 'core' of the high temperature resistant nano-micron plugging agent particles comprises hydrophilic nano-silica 'hard core' modified by a silane coupling agent.
The "veil" of the high temperature resistant nano-micron plugging agent particles comprises a poorly soluble hydrophobically associating polymer formed by free radical polymerization of a relatively large amount of hydrophobic alkenyl monomer and a very small amount of hydrophilic monomer.
The "shell" of the high temperature resistant nano-micron blocking agent particles comprises a water-soluble hydrophobic association polymer formed by free radical polymerization of a relatively small amount of hydrophobic alkenyl monomer and a relatively large amount of hydrophilic monomer.
The high temperature resistant nano-micron plugging agent, wherein the hydrophobic alkenyl monomer is selected from one or more of acryloylmorpholine, styrene, methyl acrylate, methyl methacrylate, butyl acrylate and butyl methacrylate.
The hydrophilic alkenyl monomer is selected from one or more of acrylamide, 2-acrylamide-2-methylpropanesulfonic acid, sodium acrylate, maleic anhydride, N-vinyl pyrrolidone and sodium styrenesulfonate heavy metal.
The hydrophilic nano silicon dioxide is selected from hydrophilic nano silicon dioxide with the particle size of 10nm-100 nm.
The high temperature resistant nano-micron plugging agent is characterized in that the emulsifying agent is one or more of sorbitan monooleate, alkylphenol ethoxylates and sodium dodecyl sulfate.
The high temperature resistant nano-micron plugging agent is characterized in that the initiator is selected from one or two of azo diiso Ding hydrochloride, azo diisobutyl amidine hydrochloride, azo dicyanovaleric acid or azo diisopropyl imidazoline, ammonium persulfate and sodium bisulphite.
The average particle size of the nano-micron plugging agent is 50nm-400nm, and the average particle size range is adjustable.
The silane coupling agent is tetraethyl orthosilicate.
In an embodiment of the application, the pH adjuster is sodium bicarbonate.
The preparation method of the high-temperature-resistant nano-micron plugging agent for the drilling fluid applicable to the deep well fractured stratum comprises the following steps:
(1) Mixing 90 parts by weight of hydrophobic alkenyl monomer, 0-10 parts by weight of hydrophilic alkenyl monomer, 0.5-3.5 parts by weight of emulsifier and 45-50 parts by weight of tap water, and stirring to prepare a first mixed solution;
(2) Mixing and stirring the rest weight parts of hydrophobic alkenyl monomer, the rest weight parts of hydrophilic alkenyl monomer, 0.5-2 weight parts of emulsifier and 50-110 weight parts of tap water to prepare a second mixed solution;
(3) Mixing 10-15 parts by weight of tap water and all the initiator to prepare a third mixed solution;
(4) Mixing and stirring the pH regulator, the silane coupling agent, the nano silicon dioxide and the rest tap water, and performing ultrasonic treatment for 20min to prepare a fourth mixed solution;
(5) Adding the fourth mixed solution into a container, stirring and mixing uniformly, heating to 68-72 ℃ and stirring for 30min under the protection of inert gas; then, dripping the first mixed solution obtained in the step (1) and simultaneously dripping the third mixed solution obtained in the step (3) to keep the temperature of the reaction container unchanged; after the first mixed liquid is dripped, preserving heat for 50-70min, and then starting to add the second mixed liquid obtained in the step (2) and simultaneously starting to drip the rest third mixed liquid; after the second mixed liquid is dripped, the high temperature resistant nano-micron plugging agent is obtained after heat preservation for 4 hours at 80-85 ℃.
The weight ratio of the third mixed solution added dropwise in the step (5) to the third mixed solution added dropwise in the second step is 3:2, and the two times of adding are controlled to be 40-50min and 30min respectively.
Example 1 high temperature resistant nano-micron blocking agent for drilling fluid
The preparation method comprises the following steps:
(1) The following raw materials were added to beaker one: 70g of methyl methacrylate, 20g of acryloylmorpholine, 45g of tap water and 2.3g of sorbitan monooleate, and then stirring at a high speed to prepare a first mixed solution;
(2) Adding the following raw materials into a beaker II: 10g of methyl acrylate, 6g of 2-acrylamide-2-methylpropanesulfonic acid, 2g of acrylamide, 1g of sorbitan monooleate, 0.5g of alkylphenol ethoxylates and 50g of tap water, and then stirring at a high speed to prepare a second mixed solution;
(3) The following raw materials were added to beaker three: 15g of tap water and 0.2744g of azo diiso Ding-hydrochloride, and then uniformly stirring to prepare a third mixed solution;
(4) The following materials were added to beaker four: 0.3g of sodium bicarbonate, 4.2g of tetraethyl orthosilicate, 1.2g of hydrophilic nano silicon dioxide with the particle size of 12nm and 30g of tap water, and then performing ultrasonic treatment for 20min after high-speed stirring to prepare a fourth mixed solution;
(5) Pouring the fourth mixed solution into a 500mL three-neck reaction flask, stirring, heating the three-neck flask to 70 ℃, and stirring for 30min under the protection of nitrogen atmosphere;
simultaneously dropwise adding the first mixed solution and 9mL of the third mixed solution into the three-rear flask under the protection of stirring and nitrogen atmosphere, after the dropwise addition is completed within 40min, preserving heat for 50min at 70 ℃;
And (3) dropwise adding the second mixed solution and the rest of the third mixed solution into the three-neck flask, after dropwise adding is completed within 30min, then raising the temperature of the three-neck flask to 80 ℃, preserving heat for 4h, then cooling to room temperature, and discharging.
Example 2 high temperature resistant nano-micron blocking agent for drilling fluid
The preparation method comprises the following steps:
(1) The following raw materials were added to beaker one: 90g of styrene, 50g of tap water and 3g of sorbitan monooleate, and then stirring at a high speed to prepare a first mixed solution;
(2) Adding the following raw materials into a beaker II: 10g of methyl acrylate, 9g of 2-acrylamide-2-methylpropanesulfonic acid, 1g of sorbitan monooleate, 0.5g of alkylphenol ethoxylates and 70g of tap water, and then stirring at a high speed to prepare a second mixed solution;
(3) The following raw materials were added to beaker three: 30g of tap water, 0.14g of ammonium persulfate and 0.1325g of azo diiso Ding-hydrochloride, and then uniformly stirring to prepare a third mixed solution;
(4) The following materials were added to beaker four: 0.3g of sodium bicarbonate, 5g of tetraethyl orthosilicate, 1.2g of hydrophilic nano silicon dioxide with the particle size of 12nm and 30g of tap water, and then performing ultrasonic treatment for 20min after high-speed stirring to prepare a fourth mixed solution;
(5) Pouring the fourth mixed solution into a 500mL three-neck reaction flask, stirring, heating the three-neck flask to 70-75 ℃, and stirring for 30min under the protection of nitrogen atmosphere;
Simultaneously dropwise adding the first mixed solution and 20mL of the third mixed solution into the three-rear flask under the protection of stirring and nitrogen atmosphere, after the dropwise addition is completed within 40min, preserving heat at 75 ℃ for 50min;
And (3) dropwise adding the second mixed solution and the rest of the third mixed solution into the three-neck flask, after dropwise adding is completed within 30min, then raising the temperature of the three-neck flask to 85 ℃, preserving heat for 4h, then cooling to room temperature, and discharging.
Effect test
Test example 1, transmission Electron microscope detection
Microscopic morphology of the 0.2% concentration nano-micrometer blocking agent prepared in example 1 was observed by Transmission Electron Microscopy (TEM), as shown in fig. 1. As can be seen from FIG. 1, the prepared nano-micron plugging agent is spherical and has a particle size of about 300nm.
Test example 2, field emission scanning electron microscope detection
The microscopic morphology of the nano-micron plugging agent prepared in example 1 on the mud cake was observed by using a field emission Scanning Electron Microscope (SEM), as shown in fig. 2. As can be seen from fig. 2, the prepared nano-micron plugging agent is accumulated on the surface of the mud cake, which shows that the nano-micron plugging agent is suitable for plugging microcracks.
Test example 3 Malvern particle size distribution Instrument detection
The nano-micron plugging agent prepared in example 1 was tested for particle size distribution using a Malvern particle size distribution apparatus, and the results are shown in fig. 3. As can be seen from FIG. 3, the particle size distribution of the prepared nano-micron plugging agent is 185-422nm, and the average particle size is about 300nm, which shows that the nano-micron plugging agent is suitable for plugging nano-micron microcracks.
Test example 4, test sand tray blocking ability evaluation:
With the help of a plugging performance evaluation instrument of a hypotonic sand disk (PPA sand disk), adopting a basic formula under the evaluation conditions of filter element number 12114301d (400 mD hypotonic sand disk), 7MPa and 180 ℃ and a plugging performance of the formula with the high-temperature resistant nano plugging agent on the 400mD hypotonic sand disk after 180 ℃/16h aging.
Preparing a prehydration dilute aqueous slurry: 400mL of tap water is added into a high stirring cup, 0.8g of anhydrous sodium carbonate and 16g of secondary bentonite for drilling fluid are sequentially added at the stirring speed of 8000 revolutions per minute, the mixture is stirred for 2 hours, and the mixture is sealed and kept stand for 24 hours to obtain prehydrated dilute water-based slurry.
The testing method comprises the following steps: 400mL of pre-hydrated fresh water base slurry are respectively taken, the serial numbers of the pre-hydrated fresh water base slurry are respectively marked as No. 1, no. 2, no. 3, no. 4 and No. 5, 5 test slurries are uniformly stirred at high speed at a stirring speed of 8000 revolutions per minute, then 0%, 1%, 2%, 3% and 4% of the nano-micron plugging agent sample prepared in example 1 by weight are respectively added, the mixture is stirred at high speed for 20 minutes, and then rheological properties (apparent viscosity AV, plastic viscosity PV and dynamic shear force YP), medium pressure fluid loss characteristics (FL API) and sand disc plugging fluid loss (FL Sand disk ) of the test slurries after aging at 180 ℃ for 16 hours are respectively measured. The test and evaluation method is carried out according to GB/T16783.1-2014. The test results are shown in table 1:
Table 1 test results in pre-hydrated fresh water-based slurries
Note that: FL Sand disk is the sand tray plugging fluid loss tested under the condition of 30min/7 MPa.
Test results show that after the high-temperature-resistant nano-micron plugging agent for drilling fluid is added into pre-hydrated fresh water base slurry, the viscosity is gradually increased along with the increase of the addition amount, and a certain weak tackifying effect is achieved; with the gradual increase of the addition, the medium-pressure filtration loss is gradually reduced, and after the nano-micron plugging agent is added for 4 percent, the medium-pressure filtration loss is reduced by 27.8 percent; with the gradual increase of the addition, the plugging performance of the sand disc of the test slurry is obviously improved, and when 4% of the nano-micron plugging agent is added, the plugging performance of the sand disc is reduced from 39mL to 9.6mL, and the plugging filtration loss of the sand disc is reduced by about 75.4%, so that the sample of the embodiment has excellent microcrack and micropore plugging performance and can resist the high temperature of 180 ℃.
To further understand the nano-micron plugging effect of the high temperature resistant nano-micron plugging agent in the drilling fluid in example 1, the nano-micron plugging performance of the sample in example 1 in the following drilling fluid formulation was tested and evaluated by using a sand tray plugging experimental device.
The experimental slurry formula is as follows: 4.0% bentonite slurry +0.15% fas367 +0.25%80a51+4% smp-3+3% sphh +4% sy-a01+1.5% sy-a07+0.3% polyamine (barite weighting to 1.4g/cm 3).
0#: Experimental pulp+0% nano-micron plugging agent CLG-Seal
1#: Experimental pulp +1% nano-micron plugging agent CLG-Seal
2#: Experimental pulp +2% nano-micron plugging agent CLG-Seal
3#: Experimental pulp +3% nano-micron plugging agent CLG-Seal
As shown in fig. 4 and 5, it can be seen from fig. 4 that the sand disc plugging fluid loss of each experimental slurry after aging at a high temperature of 150 ℃ gradually decreases with the gradual increase of the addition amount of the nano-micron plugging agent in example 1, the sand disc plugging fluid loss of the experimental slurry without the nano-micron plugging agent is 8.4mL, and the sand disc plugging fluid loss of the sand disc plugging fluid loss with the nano-micron plugging agent added by 3% is only about 1.8mL, which indicates that the nano-micron plugging agent in example 1 can significantly reduce the leakage of drilling fluid in low-permeability microcracks and microcracks, and the nano-micron plugging agent can show stronger nano-micron plugging performance when the addition amount is 3%.
The drilling fluid formulation with 3% of nano plugging agent has plugging performance to 400mD hypotonic sand plate after aging at 180 ℃/16h, and the experimental result is shown in figure 6.
Under 180 ℃ test conditions, the relationship curve between the filtrate volume and the square root of time of the drilling fluid and the drilling fluid after the 3% nano-micron plugging agent CLG-Seal is added is y=1.95+0.58 x and y=2.04+0.20 x, respectively, so that the instantaneous fluid loss of the drilling fluid without the nano-micron plugging agent and the drilling fluid with the nano-micron plugging agent is 1.95mL and 2.04mL respectively, which are almost the same, but the static fluid loss rates of the drilling fluid without the nano-micron plugging agent and the drilling fluid with the nano-micron plugging agent are 0.58mL/min 1/2 and 0.20mL/min 1/2 respectively, therefore, the static fluid loss rate of the drilling fluid with the nano-micron plugging agent is obviously lower than that of the drilling fluid without the nano-micron plugging agent, which is about 0.38mL/min 1/2, further indicates that the nano-micron plugging agent in example 1 can remarkably reduce the fluid leakage loss in low-permeability cracks and micro-gaps under a relatively high temperature environment (180 ℃).
Similarly, to further understand the comparison of the plugging effect of the nano-micron plugging agent CLG-Seal in example 1 with the existing nano-micron plugging agent, the plugging performance of the basic formulation and the three formulations with 3% of nano-plugging agent, 3% of n-Seal (abroad) and 3% of sd-Seal (domestic) on 400mD hypotonic sand plates after 180 ℃/16h aging was evaluated under the evaluation conditions of filter element number 12114301d (400 mD hypotonic sand plates), 7MPa and 180 ℃. The test results are shown in fig. 7 and 8.
From the experimental results in fig. 7, the relationship between the volume of the filtrate and the square root of time after adding 3% of the nano-micrometer plugging agent, 3% of the n-Seal and 3% of the sd-Seal to the drilling fluid is y=2.05+0.20x, y=1.71+0.33x and y=2.35+0.34x, respectively, and it is known that after adding 3% of the nano-micrometer plugging agent CLG-Seal, 3% of the n-Seal and 3% of the sd-Seal to the drilling fluid:
the instantaneous fluid loss of the drilling fluid is respectively 4.1mL, 3.42mL and 4.7mL, and the order of the instantaneous fluid loss is respectively as follows: N-Seal > example 1 sample > SD-Seal;
The static filtration stall rates of the drilling fluid are respectively 0.2mL/min 1/2、0.33mL/min1/2 and 0.34mL/min 1/2, and the good and bad sequences of the static filtration rates are respectively: example 1 samples > N-Seal > SD-Seal;
As can be seen from fig. 8, PPA fluid loss of the drilling fluid is: the PPA fluid loss is respectively in the following order of 6.2mL, 6.9mL and 8.3 mL: example 1 samples > N-Seal > SD-Seal.
In conclusion, the PPA plugging performance of the nano-micron plugging agent of the embodiment 1 is better, the performance of the nano-micron plugging agent is close to that of foreign products, and the capability of plugging sand trays is better than that of the domestic existing products.
In order to further understand the pressure transmission inhibition effect of the nano-micron plugging agent of the embodiment 1 and the existing nano-micron plugging agent at home and abroad, a SHM-3 type high-temperature high-pressure well wall stability simulation experiment device is adopted to carry out a pressure transmission (PPT) experiment, and the pressure transmission inhibition effect of the nano-micron plugging agent of the embodiment 1, the existing nano-micron plugging agent N-Seal at home and the existing nano-micron plugging agent SD-Seal at home and abroad on shale is respectively evaluated.
In the pressure transmission process, the downstream test solution adopts 4wt% NaCl aqueous solution, the upstream test solution adopts 4wt% NaCl aqueous solution or 4wt% NaCl aqueous solution+3 wt% sample of example 1, the upstream pressure is maintained at 2.1MPa, the downstream pressure is maintained at 1MPa, and the experimental temperature is 135 ℃. The experimental results are shown in FIG. 9
As can be seen from the pressure transfer curve of fig. 9, the pressure transfer rate of the 4wt% aqueous nacl solution is fast, and after 1h, the downstream pressure is substantially level with the upstream pressure, and the upstream pressure penetrates the core; the next 4% base slurry, after 2.5 hours the downstream pressure was substantially level with the upstream pressure, which penetrated the core. However, under the condition of the test temperature of 135 ℃, the time for the pressure transmission can be obviously delayed by adding the experimental slurry of the sample of the embodiment 1, and the time for the upstream pressure to penetrate the rock core is obviously delayed, so that the required time is greatly increased; the time for the upstream pressure of experimental slurry of the sample of the embodiment 1 to penetrate through the rock core is about 8.3h, 12.5h and 19.5h respectively after the SD-Seal of the similar nano-micron plugging agent in China, the N-Seal of the similar nano-micron plugging agent in foreign countries are added, which shows that the sample of the embodiment 1 can be effectively pressed into micropores and microcracks on the surface of rock to form a physical plugging layer under the action of pressure difference, and the nano-micron plugging agent can resist the pressure transmission rate. From the comparison test results, the sample of the embodiment 1 has the most obvious effect of reducing the shale permeability, and can obviously improve the stability of the well wall of the shale stratum; the other is the foreign similar product N-Seal, and finally the domestic similar product SD-Seal. The comprehensive experimental result shows that the nano-micron plugging performance of the embodiment 1 is superior to that of similar products at home and abroad.
In conclusion, the high-temperature-resistant nano-micron plugging agent for drilling fluid provided by the application has good high-temperature-resistant deformable plugging performance on deep fractured formations, can obviously reduce the leakage of microcracks, and can effectively slow the pore pressure transmission effect of the fractured formations.
Claims (6)
1. The high temperature resistant nano-micron plugging agent for drilling fluid suitable for fractured formations is characterized in that: the high-temperature-resistant nano-micron plugging agent comprises the following raw materials: hydrophilic nano silicon dioxide, hydrophobic alkenyl monomer, hydrophilic alkenyl monomer, emulsifier, pH regulator, silane coupling agent, initiator and tap water;
in the raw materials of the high temperature resistant nano-micron plugging agent for the drilling fluid applicable to the fractured stratum, relative to 100 parts by weight of the hydrophobic alkenyl monomer, the content of the hydrophilic nano-silicon dioxide is 1-20 parts by weight, the content of the hydrophilic alkenyl monomer is 10-40 parts by weight, the content of the emulsifier is 0.5-5 parts by weight, the content of the pH regulator is 0.05-5 parts by weight, the content of the silane coupling agent is 0.01-5 parts by weight, the content of the initiator is 0.05-3.5 parts by weight, and the content of tap water is 50-200 parts by weight;
The hydrophobic alkenyl monomer is one or more of acryloylmorpholine, styrene, methyl acrylate, methyl methacrylate, butyl acrylate and butyl methacrylate;
The hydrophilic alkenyl monomer is one or more of acrylamide, 2-acrylamide-2-methylpropanesulfonic acid, sodium acrylate, maleic anhydride, N-vinyl pyrrolidone and sodium styrene sulfonate;
The preparation method of the high-temperature-resistant nano-micron plugging agent for the drilling fluid applicable to the fractured stratum comprises the following steps of:
(1) Mixing 90 parts by weight of hydrophobic alkenyl monomer, 0-10 parts by weight of hydrophilic alkenyl monomer, 0.5-3.5 parts by weight of emulsifier and 45-50 parts by weight of tap water, and stirring to prepare a first mixed solution;
(2) Mixing and stirring the rest weight parts of hydrophobic alkenyl monomer, the rest weight parts of hydrophilic alkenyl monomer, 0.5-2 weight parts of emulsifier and 50-110 weight parts of tap water to prepare a second mixed solution;
(3) Mixing 10-15 parts by weight of tap water and all the initiator to prepare a third mixed solution;
(4) Mixing and stirring the pH regulator, the silane coupling agent, the nano silicon dioxide and the rest tap water, and performing ultrasonic treatment for 20min to prepare a fourth mixed solution;
(5) Adding the fourth mixed solution into a container, stirring and mixing uniformly, heating to 68-72 ℃ and stirring for 30min under the protection of inert gas; then, dripping the first mixed solution obtained in the step (1) and simultaneously dripping the third mixed solution obtained in the step (3) to keep the temperature of the reaction container unchanged; after the first mixed liquid is dripped, preserving heat for 50-70min, and then starting to add the second mixed liquid obtained in the step (2) and simultaneously starting to drip the rest third mixed liquid; after the second mixed liquid is dripped, the high temperature resistant nano-micron plugging agent is obtained after heat preservation for 4 hours at 80-85 ℃.
2. The high temperature resistant nano-micron plugging agent for drilling fluids suitable for fractured formations of claim 1, wherein: the hydrophilic nano silicon dioxide is selected from nano silicon dioxide with the particle size of 10nm-100 nm.
3. The high temperature resistant nano-micron plugging agent for drilling fluids suitable for fractured formations of claim 1, wherein: the emulsifier is one or more of sorbitan monooleate, alkylphenol ethoxylates and sodium dodecyl sulfate.
4. The high temperature resistant nano-micron plugging agent for drilling fluids suitable for fractured formations of claim 1, wherein: the initiator is one or two selected from azodiiso Ding hydrochloride, azodiisobutyl amidine hydrochloride, azodicyanovaleric acid or azodiisopropyl imidazoline, ammonium persulfate and sodium bisulphite.
5. The high temperature resistant nano-micron plugging agent for drilling fluids suitable for fractured formations of claim 1, wherein: the silane coupling agent is tetraethyl orthosilicate; the pH regulator is sodium bicarbonate.
6. The high temperature resistant nano-micron plugging agent for drilling fluids suitable for fractured formations of claim 1, wherein: the weight ratio of the third mixed solution added dropwise in the step (5) to the third mixed solution added dropwise in the second time is 3:2, and the time of the two drops is controlled to be 40-50min and 30min respectively.
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