A high-flow-throughput emulsion-type smart fracturing fluid and its preparation method
By designing an emulsion-type intelligent fracturing fluid, and utilizing temperature-salt dual-responsive nano-crosslinking agents and biomimetic modified nanosheets, the problems of low-friction pumping and efficient proppant carrying of fracturing fluid in high-temperature and high-salt formations have been solved. After gel breaking, it maintains high conductivity for a long time, realizing a leap in the intelligence and functionality of fracturing fluid.
Patent Information
- Application Number
- CN202610100978.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-01-26
- Publication Date
- 2026-05-26
AI Technical Summary
Existing fracturing fluid systems struggle to simultaneously address the technical challenges of low-friction pumping, efficient proppant transport in high-temperature, high-salinity formations, and maintaining high conductivity of fractures after gel breaking.
An emulsion-type intelligent fracturing fluid was used. By introducing a temperature-salt dual-responsive zirconium-silicon hybrid nano-crosslinking agent and biomimetic surface-modified layered silicate nanosheets, an intelligent responsive emulsion system was constructed. Under high temperature and high salt conditions, nano-crosslinking was triggered to form a highly efficient three-dimensional network gel structure for carrying proppant. After the gel breaks down, an elastic proppant filling layer was constructed to optimize the proppant placement.
It achieves intelligent rheological control throughout the entire construction process, reduces pumping friction, efficiently carries sand, maintains high conductivity for a long time after breaking the gel, adapts to complex geological environments, and is easy to operate and environmentally friendly.
Abstract
Description
Technical Field
[0001] This invention relates to the field of oil and gas field production enhancement and transformation technology, specifically to an emulsion-type intelligent fracturing fluid with high conductivity channels and its preparation method. Background Technology
[0002] Hydraulic fracturing technology is a key means of developing unconventional oil and gas resources such as shale gas and tight oil and gas, and its effectiveness largely depends on the performance of the fracturing fluid system. An ideal hydraulic fracturing fluid needs to meet a series of complex and contradictory technical requirements throughout its entire lifecycle, from wellbore pumping to fracture formation and propagation: during the high-speed pumping phase in the wellbore, the fracturing fluid should have low friction to reduce operational energy consumption; after entering the formation fractures, it needs high viscosity to effectively suspend and transport proppant over long distances, ensuring the formation of sufficiently long and highly conductive propped fractures; after operation, the fracturing fluid must be able to completely break down and degrade, and be rapidly flowed back to minimize damage to reservoir permeability. As oil and gas exploration and development moves towards deeper, ultra-deeper, and more complex unconventional reservoirs, higher formation temperatures, greater pressures, and more complex salinity levels pose unprecedented and severe challenges to the temperature and salt resistance, intelligent response capabilities, and long-term reservoir-friendly properties of fracturing fluids.
[0003] Currently used mainstream fracturing fluid systems, such as slickwater, clean viscoelastic fracturing fluid, and polymer gel fracturing fluid, all have significant shortcomings in some aspect of the aforementioned technical requirements. Slickwater systems, with drag-reducing agents at their core, offer low pumping friction and low cost, but their generally low viscosity results in insufficient proppant carrying capacity. This leads to rapid proppant settling and accumulation near the wellbore, making it difficult to form effective support in distal fractures and impacting production enhancement. Clean viscoelastic fracturing fluids rely on worm-like micelle networks formed by surfactant molecules for viscosity enhancement, offering advantages such as no residue and easy colloidal breakdown. However, this micelle structure based on non-covalent bonds exhibits poor stability under high temperature and high salinity conditions, easily undergoing structural damage and causing a sharp drop in viscosity, limiting its application under harsh formation conditions. Traditional polymer-based fracturing fluids, using guar gum or synthetic polymers as a base and cross-linked with metal ions, possess excellent proppant-carrying capacity. However, they generally suffer from incomplete gel breaking, residue clogging reservoir pores, and premature cross-linking within the wellbore, leading to excessively high pumping pressure and operational risks. Despite a series of improvements made by researchers both domestically and internationally through the synthesis of novel temperature- and salt-resistant monomer polymers, the development of delayed cross-linking agents, and nano-reinforcing materials, a systematic solution to the core contradiction of "low-friction pumping, efficient proppant carrying, and high conductivity" has yet to be achieved.
[0004] Therefore, there is an urgent need in this field to develop a new generation of intelligent fracturing fluid systems. This system should be able to dynamically respond to changes in the downhole environment and achieve self-regulation of performance: maintaining a low viscosity and low resistance state during the pumping phase; upon entering the target formation, under the triggering conditions of high temperature and high salinity, the viscosity should intelligently and significantly increase, thereby efficiently delivering the proppant; after breaking down, it should not only completely degrade, but its components should also synergistically interact with the proppant to actively optimize the proppant placement and maximize the long-term conductivity of the fracture. This approach guides research towards environmentally responsive materials, nanocomposite technologies, and biomimetic design. Against this backdrop, this invention aims to construct an emulsion-type intelligent fracturing fluid that meets all the aforementioned stringent requirements by designing and synthesizing inorganic-organic hybrid nanomaterials with specific functions as core additives, providing an innovative fluid solution for the efficient and economical development of deep and unconventional oil and gas resources. Summary of the Invention
[0005] The purpose of this invention is to provide an emulsion-type intelligent fracturing fluid for high-conductivity channels and its preparation method, which solves the technical problem that existing fracturing fluid systems cannot simultaneously achieve low-friction pumping, efficient sand carrying in high-temperature and high-salt formations, and maintain long-term high conductivity of fractures after gel breaking.
[0006] The present invention achieves the above objectives through the following technical solutions: A method for preparing a high-flow-throughput emulsion-type smart fracturing fluid, comprising the following steps: S1. By weight, add 80-120 parts of deionized water to a stirred tank and stir. Add 0.01-0.1 parts of polyacrylamide and 0.1-0.5 parts of partially hydrolyzed polyacrylamide and stir to obtain an aqueous phase mixture. Mix 5-15 parts of diesel oil with 1-3 parts of nonionic surfactant Span-80 to obtain an oil phase mixture. While stirring, add the oil phase mixture to the aqueous phase mixture and continue stirring to obtain a base emulsion. S2. Add 0.05-0.3 parts of temperature-salt dual-responsive zirconium-silicon hybrid nano-crosslinking agent to the base emulsion obtained in step S1, stir, then add 0.1-0.5 parts of biomimetic surface-modified layered silicate nanosheets and stir; finally, add 0.001-0.005 parts of ammonium persulfate just before pumping.
[0007] In this invention, the preparation and mechanism of the high-conductivity emulsion-type intelligent fracturing fluid embodies a multi-level design from macroscopic emulsion construction to microscopic intelligent response. Its preparation begins with the construction of a stable oil-in-water emulsion matrix. The oil phase is dispersed under shear force in an aqueous phase containing polymers. Surfactant molecules are directionally adsorbed at the oil-water interface, reducing interfacial tension and forming spatial or static resistance barriers to stably disperse oil droplets, forming an emulsion. This structure itself can alter the fluid flow pattern and encapsulate some free water, affecting initial rheological properties. Subsequently, two functional nanomaterials are introduced sequentially. A temperature- and salt-responsive nano-crosslinking agent is uniformly dispersed in the continuous aqueous phase, currently in a "dormant" state; biomimetic modified nanosheets are partially adsorbed at the oil-water interface and partially dispersed in the aqueous phase. During the pumping stage, the fluid is in a high-shear, low-temperature, and low-salt environment. The response chain of the nano-crosslinking agent extends without crosslinking. The system viscosity mainly comes from the emulsion structure and polymers, while the biomimetic nanosheets exert a lubricating effect, jointly achieving low friction. Upon entering the high-temperature, high-salt crack, the environment triggers the activity of the nano-crosslinking agent. Its polymer chains coil and, through ion bridging, rapidly form a three-dimensional network gel structure with nanoparticles as crosslinking points, together with the polymer chains in the aqueous emulsion phase. This results in a sharp increase in viscosity, achieving efficient sand carrying. At a predetermined time or temperature, the gel-breaking agent releases free radicals, degrading the polymer backbone and causing the gel network to disintegrate. At this point, the "nano-anchoring" effect of the biomimetic nanosheets becomes prominent. The polydopamine coating on their surface firmly binds some of the polymer chain segments after gel breaking to the surface of the proppant particles, forming a flexible, partially pore-blocking secondary network. This network can elastically deform under crack closure stress, buffering the point contact stress between proppant particles and preventing particle breakage and compaction. This allows for the long-term maintenance of more interconnected and effective seepage channels within the proppant-filled body, ultimately maximizing and extending the crack's conductivity. The entire mechanism follows a main thread of "intelligent triggering - functional conversion - structural optimization."
[0008] According to a preferred embodiment of the present invention, in step S1, the stirring time is 10-15 min.
[0009] According to a preferred embodiment of the present invention, in step S2, the stirring time is 15-20 min.
[0010] According to a preferred embodiment of the present invention, the preparation method of the temperature-salt dual-responsive zirconium-silicon hybrid nano-crosslinking agent includes: A1. Under nitrogen protection, zirconium oxychloride was dissolved in anhydrous ethanol in parts by weight. Ammonia was added dropwise to pH 9-10 with stirring, and the mixture was aged at room temperature to obtain zirconium hydroxide gel. γ-aminopropyltriethoxysilane and acryloyloxypropyltrimethoxysilane were added to toluene, stirred, and water was added to adjust the pH to 4.0-6.0 to obtain a silane solution. The zirconium hydroxide gel was added to the silane solution and refluxed at 78-82℃ to obtain a suspension of zirconium silanide nanoparticles. A2. After centrifuging and washing the silanized zirconium nanoparticle suspension, it was redispersed in N,N-dimethylformamide; N-isopropylacrylamide monomer, acrylic acid monomer, and azobisisobutyronitrile initiator were added, and the reaction was carried out at 68-72℃ to obtain the reaction mixture; the reaction mixture was dialyzed in deionized water.
[0011] In this invention, the preparation of the temperature-salt dual-responsive zirconium-silicon hybrid nanocrosslinking agent is a precise construction process from an inorganic nanocore to an organic functionalized surface, with its core mechanism lying in the stepwise chemical bonding and polymer grafting. First, the hydrolysis and condensation reaction of zirconium salt under alkaline conditions generates zirconium hydroxide nanoclusters or gels with hydroxyl-rich surfaces. These active zirconium hydroxyl groups provide key reaction sites for subsequent organosilanesylation modification. Next, in an acid-catalyzed environment, two silane coupling agents undergo hydrolysis, converting their alkoxy groups into highly reactive silanol groups. These silanol groups react with the zirconium hydroxyl groups on the surface of the zirconium nanoparticles under reflux conditions to form strong zirconium-siloxane covalent bonds, thereby constructing an organosilanes molecular layer on the surface of the inorganic nanocore. This molecular layer not only stabilizes the nanoparticles but, more importantly, introduces reactive functional groups such as carbon-carbon double bonds and amino groups that can be further reacted. Finally, under the action of a free radical initiator, isopropyl acrylamide and acrylic acid monomers undergo graft copolymerization on the nanoparticle surface. The N-isopropylacrylamide unit endows the polymer chain with thermosensitive properties, allowing its molecular chain to reversibly expand and contract in water with temperature changes. The acrylic acid unit provides carboxyl groups, enabling it to form strong coordination interactions with polyvalent cations such as calcium and magnesium ions in formation water. Therefore, this hybrid nanoparticle ultimately possesses dual responsiveness: increased temperature causes the polymer chain to dehydrate and contract, exposing more crosslinking sites; the high salinity environment of the formation, through ion coordination bridging, synergistically triggers and strengthens the formation of crosslinking networks with other polymers in the fracturing fluid, achieving a smart increase in viscosity.
[0012] According to a preferred embodiment of the present invention, in step A1, the reflux reaction time at 78-82°C is 24-30 h.
[0013] According to a preferred embodiment of the present invention, in step A2, the reaction time at 68-72°C is 8-10 hours.
[0014] According to a preferred embodiment of the present invention, the method for preparing the biomimetic surface-modified layered silicate nanosheets includes: B1. Disperse sodium-based montmorillonite in deionized water, stir and sonicate, then centrifuge in a high-speed centrifuge to separate and obtain a partially exfoliated montmorillonite nanosheet dispersion. B2. Place the partially exfoliated montmorillonite nanosheet dispersion in an ice-water bath, adjust the pH to 8.0-8.5 using tris(hydroxymethyl)aminomethane buffer, then add dopamine hydrochloride, stir, add ferric chloride solution dropwise, and continue stirring the reaction; after the reaction is complete, wash with deionized water by centrifugation.
[0015] In this invention, the preparation mechanism of the biomimetic surface-modified layered silicate nanosheets integrates physical exfoliation and biomimetic chemical adhesion, aiming to endow them with unique surface properties and functions. First, sodium-based montmorillonite is physically exfoliated. The mechanism utilizes water molecules to penetrate between the silicate layers, expanding the interlayer spacing. Then, the strong shear force provided by high-speed stirring and ultrasonic cavitation overcomes the van der Waals forces and electrostatic attraction between the layers, thereby exfoliating them into single sheets or nanosheets composed of a few layers. This process significantly increases the specific surface area and surface reactivity of the nanosheets. Subsequently, crucial biomimetic surface modification is performed. Drawing inspiration from the adhesion proteins of marine mussels, dopamine molecules undergo oxidative self-polymerization under weakly alkaline conditions catalyzed by metal ions. Ferric ions play a dual role in this process: firstly, as an oxidant promoting the oxidation of dopamine; and secondly, as a coordination center binding to the catechol groups of dopamine, regulating the polymerization process and enhancing coating stability. The generated polydopamine, through its abundant catechol and amino functional groups, forms multiple strong interactions with the silanol and oxygen atoms on the surface of silicate nanosheets, including hydrogen bonds, coordination bonds, and even covalent bonds, thereby forming a robust and uniform biomimetic adhesive coating on the nanosheet surface. This coating endows the nanosheets with two key functions: first, during fracturing fluid pumping, its smooth surface and hydrophilicity can act as nano-lubricant, reducing internal fluid friction; second, after debriding, the catechol groups on its surface can form strong adhesion with the proppant surface and debriding residue, acting as "molecular bridges" and "nano-anchors," optimizing the pore structure of the proppant filling layer.
[0016] According to a preferred embodiment of the present invention, in step B1, the stirring and ultrasonic treatment time is 2-4 hours.
[0017] According to a preferred embodiment of the present invention, in step B2, the stirring reaction is continued for 24-30 hours.
[0018] The present invention also provides a high-flow-channel emulsion-type intelligent fracturing fluid prepared according to the preparation method of the high-flow-channel emulsion-type intelligent fracturing fluid described above.
[0019] The beneficial effects of this invention are as follows: The high-conductivity emulsion-type intelligent fracturing fluid and its preparation method provided by this invention achieve intelligent and functional leaps in fracturing fluid performance by introducing two innovatively designed inorganic modified compounds. Its technical effects are significant and comprehensive, mainly reflected in the following three core aspects.
[0020] First, this fracturing fluid system achieves intelligent rheological control throughout the entire fracturing process, fundamentally resolving the contradiction between pumping friction and proppant carrying capacity within the fracture. During the low-temperature, low-salinity wellbore pumping stage, the functional polymers and biomimetic modified nanosheets in the system work synergistically to impart excellent lubrication properties to the fluid, effectively reducing tubing friction and significantly saving construction energy. Once in the high-temperature, high-salinity target formation environment, the unique temperature-salt dual-responsive nano-crosslinking agent is intelligently activated. The conformation of the polymer chains grafted onto its surface changes, and it generates strong coordination with polyvalent salt ions, rapidly forming a dense three-dimensional spatial network structure with the polymer molecular chains in the emulsion. This leads to an order-of-magnitude increase in fluid viscosity in specific regions. This high-viscosity state triggered in the formation ensures that the proppant can be efficiently suspended and transported to the distal end of the fracture, avoiding premature settling in the near-wellbore zone and laying the hydrodynamic foundation for the formation of long and effective propped fractures.
[0021] Secondly, this technical solution can actively construct and maintain highly conductive propped fractures after gel breaking, overcoming the bottleneck of traditional fracturing fluids causing significant damage and rapid decline in conductivity after gel breaking. Biomimetic surface-modified nanosheets play a crucial role in this process. After gel breaking, traditional polymer residues often clog pores, while the nanosheets in this system, with their robust biomimetic adhesive coating, can selectively anchor a portion of the polymer chain network after gel breaking to the surface and between proppant particles. This process does not create dense blockage, but rather constructs a thin, elastic, and resilient network. This network can adaptively deform under fracture closure stress rather than being compacted, thus retaining more interconnected flow channels in the proppant-filled layer. Simultaneously, this elastic network effectively buffers stress, inhibiting the breakage and embedding of proppant particles, significantly improving the stability and retention rate of the proppant-filled layer's conductivity during long-term production.
[0022] Finally, this invention demonstrates excellent environmental adaptability, ease of operation, and techno-economic efficiency, possessing broad prospects for field application. The entire system uses water as the continuous phase, making it more environmentally friendly than oil-based systems. Its core intelligent response mechanism is based on ubiquitous temperature and ion intensity signals, thus exhibiting natural adaptability to deep and ultra-deep high-temperature, high-salinity reservoirs, as well as conditions using seawater or high-salinity produced water for fluid preparation, effectively expanding the range of applicable reservoirs. Both key inorganic modifying compounds can be pre-synthesized and stored in stable dispersion form, making the field preparation process of fracturing fluid highly compatible with traditional emulsion preparation processes. No complex equipment is required; only sequential mixing is needed, facilitating large-scale application. In summary, this invention, through material innovation and structural design, successfully integrates and optimizes key properties of fracturing fluid, such as low friction, intelligent viscosity enhancement, low damage, and high conductivity, providing a high-performance and highly operable new option for fracturing working fluids in the efficient development of various complex oil and gas reservoirs. Detailed Implementation
[0023] The following detailed embodiments are only used to further illustrate this application and should not be construed as limiting the scope of protection of this application. Those skilled in the art can make some non-essential improvements and adjustments to this application based on the above application content.
[0024] Example 1
[0025] The preparation method of temperature-salt dual-responsive zirconium-silicon hybrid nano-crosslinking agent includes the following steps: Under a nitrogen atmosphere, 10.0 g of zirconium oxychloride is completely dissolved in 100 mL of anhydrous ethanol. While continuously stirring with a magnetic stirrer at 500 rpm, a 10% (w / w) ammonia solution is slowly added dropwise using a dropping funnel until the pH of the mixture stabilizes at 9.5. This mixture is then aged at room temperature (25°C) for 12 h to obtain a white zirconium hydroxide gel. Subsequently, 5.0 g of γ-aminopropyltriethoxysilane (APTES) and 10.0 g of acryloyloxypropyltrimethoxysilane (APTMS) are added together to a three-necked flask containing 150 mL of anhydrous toluene. The mixture is stirred at 300 rpm for 5 min in a 40°C water bath until homogeneous. 1.0 mL of deionized water is added to this mixture, and simultaneously, a 0.1 mol / L dilute hydrochloric acid solution is added dropwise to precisely adjust the pH of the system to 5.0. Maintaining a water bath temperature of 40°C, the reaction was stirred for 3 hours to allow the silane coupling agent to be fully pre-hydrolyzed, resulting in a clear pre-hydrolyzed silane solution. All the previously prepared zirconium hydroxide gel was transferred to this pre-hydrolyzed silane solution. The reaction apparatus was changed to a reflux condenser, and the mixture was heated to 80°C in an oil bath. The reaction was continued at this temperature for 26 hours, resulting in a milky white suspension of zirconium silanide nanoparticles. After the suspension cooled to room temperature, it was transferred to a centrifuge tube and centrifuged at 10,000 rpm for 15 minutes. The supernatant was discarded, and the solid precipitate was collected. The precipitate was ultrasonically washed with anhydrous ethanol and centrifuged; this process was repeated three times. Finally, the washed solid was redispersed in 100 mL of N,N-dimethylformamide (DMF) solvent to obtain a stable nanoparticle dispersion. 15.0 g of N-isopropylacrylamide (NIPAM) monomer, 2.0 g of acrylic acid (AA) monomer, and 0.3 g of azobisisobutyronitrile (AIBN) initiator were added sequentially to this DMF dispersion. Nitrogen gas was bubbled through the reaction system for 30 min to remove dissolved oxygen. The mixture was then heated to 70 °C in an oil bath and stirred at 350 rpm for 9 h under a nitrogen atmosphere. After the reaction, the resulting reaction mixture was transferred to a dialysis bag with a molecular weight cutoff of 8000-14000 Da and dialyzed in 4 L of continuously stirred deionized water. The dialysis water was changed every 8 h for a total of 72 h. The final product was an aqueous dispersion of a temperature-salt dual-responsive zirconium-silicon hybrid nano-crosslinking agent with a solid content of approximately 10%, which was sealed and stored at 4 °C for later use.
[0026] The preparation method of biomimetic surface-modified layered silicate nanosheets includes the following steps: 20.0 g of sodium montmorillonite (Na-MMT) is weighed and slowly added to a beaker containing 1000 mL of deionized water. The mixture is stirred at 800 rpm for 30 min using a mechanical stirrer to initially wet and disperse the nanosheets. Subsequently, the beaker is placed in an ultrasonic cell disruptor and sonicated at 600 W with a 2-second on-off-off pulse mode for a total sonication time of 3 h to obtain a fully swollen and partially exfoliated suspension. This suspension is transferred to a high-speed centrifuge tube and centrifuged at 6000 rpm for 30 min. The upper two-thirds volume of the homogeneous and stable colloidal suspension is carefully aspirated; this is the partially exfoliated montmorillonite nanosheet dispersion. 500 mL of the above nanosheet dispersion is measured and placed in a beaker containing an ice-water mixture, maintaining the system temperature at 0-5 °C. Under continuous stirring, 0.1 mol / L Tris buffer was added dropwise to precisely adjust the pH of the system to 8.2. Then, 2.5 g of dopamine hydrochloride was added to the cooled dispersion, and the mixture was stirred at 400 rpm for 15 min until completely dissolved. After dissolution, 5.0 mL of 0.1 mol / L ferric chloride aqueous solution was slowly added dropwise using a constant pressure dropping funnel, controlling the dropping rate to approximately 1 mL / min. After the addition was complete, the ice-water bath was removed, and the reaction system was allowed to react at 25°C with stirring at 400 rpm for 26 h. The system color gradually turned dark brown. After the reaction was complete, the product dispersion was aliquoted into centrifuge tubes and centrifuged at 8000 rpm for 20 min, discarding the supernatant. Deionized water was added to the precipitate, and the mixture was redispersed by vortexing and sonication, followed by centrifugation again. This washing process was repeated until the supernatant after centrifugation became colorless and transparent. Finally, the washed solid precipitate was quantitatively transferred and redispersed in an appropriate amount of deionized water to prepare an aqueous dispersion of biomimetic surface-modified layered silicate nanosheets with a solid content of about 5%, for later use.
[0027] The preparation method of high-flow-capacity emulsion-type intelligent fracturing fluid includes the following steps: In a 2L glass stirred tank equipped with a mechanical stirrer, 1000g of deionized water is added as the aqueous phase. Stirring is started, and the speed is controlled at 300rpm. 0.5g of high molecular weight polyacrylamide and 3.5g of partially hydrolyzed polyacrylamide are added to the water sequentially. Stirring is maintained at this speed for 30min to ensure that all polymer powders are completely dissolved and uniformly dispersed, resulting in a clear aqueous phase mixture. In another beaker, 100g of diesel oil is mixed with 20g of nonionic surfactant Span-80 and stirred with a glass rod for 3min until completely homogeneous, resulting in an oil phase mixture. The mechanical stirrer in the stirred tank is replaced with a high-shear dispersing head, and the stirring speed is increased to 8000rpm. Under high-speed shear, the oil phase mixture is slowly and uniformly added dropwise to the aqueous phase mixture using a constant-pressure dropping funnel, with the dropping time controlled to be approximately 8min. After the addition was complete, the system was kept under high-speed shear at 8000 rpm for 12 minutes. At this point, a uniform and stable milky-white oil-in-water emulsion was observed. The stirring was then switched back to a regular mechanical stirrer, and the speed was reduced to 300 rpm. First, 15.0 g of the temperature-salt dual-responsive zirconium-silicon hybrid nano-crosslinking agent aqueous dispersion prepared above was slowly added to the emulsion over approximately 1 minute. After the addition was complete, the mixture was stirred at 300 rpm for 18 minutes to ensure thorough mixing. Then, 40.0 g of the biomimetic surface-modified layered silicate nanosheet aqueous dispersion prepared above was slowly added to the system over approximately 2 minutes. After the addition was complete, the mixture was stirred at 300 rpm for another 18 minutes to ensure uniform distribution of the nanomaterials in the emulsion. Within 30 minutes before the planned on-site pumping operation, add 0.05g of ammonium persulfate as a breaker to the above-mentioned well-mixed emulsion, and stir at 300rpm for 5 minutes to dissolve and disperse it evenly, thus finally obtaining the high-conductivity emulsion-type intelligent fracturing fluid.
[0028] Example 2
[0029] The specific implementation method is the same as in Example 1, except that the preparation method of the temperature-salt dual-responsive zirconium-silicon hybrid nano-crosslinking agent includes the following steps: Under a nitrogen atmosphere, 8.0 g of zirconium oxychloride is completely dissolved in 80 mL of anhydrous ethanol. While continuously stirring with a magnetic stirrer at 500 rpm, a 10% (w / w) ammonia solution is slowly added dropwise until the pH of the mixture stabilizes at 9.0. This mixture is then aged at room temperature (25°C) for 10 h to obtain zirconium hydroxide gel. Subsequently, 4.0 g of γ-aminopropyltriethoxysilane and 8.0 g of acryloyloxypropyltrimethoxysilane are added together to a three-necked flask containing 120 mL of anhydrous toluene. The mixture is stirred at 300 rpm for 5 min in a 45°C water bath until homogeneous. 1.0 mL of deionized water is added to this mixture, and simultaneously, a 0.1 mol / L dilute acetic acid aqueous solution is added dropwise to precisely adjust the pH of the system to 4.5. Maintaining a water bath temperature of 45°C, the reaction was stirred for 2.5 hours to allow the silane coupling agent to be fully pre-hydrolyzed, yielding a pre-hydrolyzed silane solution. All the previously prepared zirconium hydroxide gel was transferred to this pre-hydrolyzed silane solution. The reaction apparatus was changed to a reflux condenser, and the mixture was heated to 78°C in an oil bath. The reaction was continued at this temperature for 24 hours, resulting in a suspension of silanized zirconium nanoparticles. After the suspension cooled to room temperature, it was centrifuged at 10,000 rpm for 15 minutes. The supernatant was discarded, and the solid precipitate was collected and ultrasonically washed with anhydrous ethanol and centrifuged three times. The washed solid was redispersed in 80 mL of N,N-dimethylformamide solvent to obtain a nanoparticle dispersion. 12.0 g of N-isopropylacrylamide monomer, 1.5 g of acrylic acid monomer, and 0.25 g of azobisisobutyronitrile initiator were added sequentially to this DMF dispersion. Nitrogen gas was bubbled through the reaction system for 30 minutes to remove dissolved oxygen. The mixture was then heated to 68°C in an oil bath and stirred at 350 rpm for 8 hours under a nitrogen atmosphere. After the reaction, the resulting reaction mixture was transferred to a dialysis bag with a molecular weight cutoff of 8000-14000 Da and dialyzed in 4 L of continuously stirred deionized water. The dialysis water was changed every 8 hours for a total of 72 hours. The resulting temperature-salt dual-responsive zirconium-silicon hybrid nano-crosslinking agent aqueous dispersion was then sealed and stored at 4°C for later use.
[0030] The preparation method of biomimetic surface-modified layered silicate nanosheets includes the following steps: 15.0 g of sodium montmorillonite was weighed and slowly added to a beaker containing 800 mL of deionized water. The beaker was stirred at 800 rpm for 30 min using a mechanical stirrer. Then, the beaker was placed in an ultrasonic cell disruptor and sonicated at 600 W pulse mode for a total sonication time of 2 h to obtain a partially exfoliated suspension. This suspension was centrifuged at 5500 rpm for 25 min, and the upper homogeneous and stable colloidal suspension, i.e., the partially exfoliated montmorillonite nanosheet dispersion, was carefully aspirated. 400 mL of the above nanosheet dispersion was measured and placed in an ice-water bath to maintain the system temperature at 0-5℃. While continuously stirring, 0.1 mol / L tris(hydroxymethyl)aminomethane buffer was added dropwise to precisely adjust the pH of the system to 8.0. Then, 2.0 g of dopamine hydrochloride was added to the cooled dispersion and stirred at 400 rpm for 15 min until completely dissolved. After dissolution, 4.0 mL of a 0.1 mol / L ferric chloride aqueous solution was slowly added dropwise, controlling the dropping rate to approximately 1 mL / min. After the addition was complete, the ice-water bath was removed, and the reaction system was stirred at 400 rpm for 24 h at room temperature (25°C). After the reaction was complete, the product dispersion was centrifuged at 8000 rpm for 20 min, and the supernatant was discarded. Deionized water was added to the precipitate, and it was redispersed by vortexing and sonication, followed by centrifugation again. This washing process was repeated until the supernatant after centrifugation became colorless and transparent. Finally, the washed solid precipitate was redispersed in an appropriate amount of deionized water to prepare a biomimetic surface-modified layered silicate nanosheet aqueous dispersion for later use.
[0031] The preparation method of high-flow-capacity emulsion-type smart fracturing fluid includes the following steps: In a 2L glass stirred tank, 800g of deionized water is added as the aqueous phase. Stirring is started, and the speed is controlled at 300rpm. 0.8g of high molecular weight polyacrylamide and 1.0g of partially hydrolyzed polyacrylamide are added to the water sequentially. Stirring is maintained at this speed for 30min to ensure complete dissolution of all polymers, resulting in an aqueous phase mixture. In another beaker, 50g of diesel oil is mixed with 10g of nonionic surfactant Span-80 and stirred with a glass rod for 3min until completely homogeneous, resulting in an oil phase mixture. The stirrer in the stirred tank is replaced with a high-shear dispersing head, and the stirring speed is increased to 7000rpm. Under high-speed shear, the oil phase mixture is slowly and uniformly added dropwise to the aqueous phase mixture, with the adding time controlled at approximately 5min. After the addition is complete, the high-speed shear state of 7000rpm is maintained for 10min to form a stable oil-in-water emulsion. The stirring is then switched back to a conventional mechanical stirrer, and the speed is reduced to 300rpm. First, 5.0 g of the temperature-salt dual-responsive zirconium-silicon hybrid nano-crosslinking agent aqueous dispersion prepared above was slowly added to the base emulsion, and the mixture was stirred at 300 rpm for 15 min after the addition was complete. Then, 10.0 g of the biomimetic surface-modified layered silicate nanosheet aqueous dispersion prepared above was slowly added to the system, and the mixture was stirred at 300 rpm for another 15 min after the addition was complete. 30 min before the planned on-site pumping operation, 0.10 g of ammonium persulfate was added to the uniformly mixed emulsion as a breaker, and the mixture was stirred at 300 rpm for 5 min to ensure uniform dispersion, thus obtaining the high-ductility emulsion-type intelligent fracturing fluid.
[0032] Example 3
[0033] The specific implementation method is the same as in Example 1, except that the preparation method of the temperature-salt dual-responsive zirconium-silicon hybrid nano-crosslinking agent includes the following steps: Under a nitrogen atmosphere, 12.0 g of zirconium oxychloride is completely dissolved in 120 mL of anhydrous ethanol. While continuously stirring with a magnetic stirrer at 500 rpm, a 10% (w / w) ammonia solution is slowly added dropwise until the pH of the mixture stabilizes at 10.0. This mixture is then aged at room temperature (25°C) for 14 h to obtain zirconium hydroxide gel. Subsequently, 6.0 g of γ-aminopropyltriethoxysilane and 12.0 g of acryloyloxypropyltrimethoxysilane are added together to a three-necked flask containing 180 mL of anhydrous toluene. The mixture is stirred at 300 rpm for 5 min in a 35°C water bath until homogeneous. 1.5 mL of deionized water is added to this mixture, and simultaneously, a 0.1 mol / L dilute hydrochloric acid solution is added dropwise to precisely adjust the pH of the system to 6.0. Maintain a water bath temperature of 35°C and continue stirring for 3.5 h to allow the silane coupling agent to be fully pre-hydrolyzed, obtaining a pre-hydrolyzed silane solution. Transfer all the previously prepared zirconium hydroxide gel to this pre-hydrolyzed silane solution. Change the reaction apparatus to a reflux condenser and heat to 82°C in an oil bath. Continue reflux at this temperature for 30 h. After the reaction is complete, a suspension of silanized zirconium nanoparticles is obtained. After the suspension cools to room temperature, centrifuge at 10,000 rpm for 15 min, discard the supernatant, collect the solid precipitate, and ultrasonically wash it with anhydrous ethanol, followed by centrifugation three times. Redisperse the washed solid in 120 mL of N,N-dimethylformamide solvent to obtain a nanoparticle dispersion. Add 18.0 g of N-isopropylacrylamide monomer, 2.5 g of acrylic acid monomer, and 0.35 g of azobisisobutyronitrile initiator to this DMF dispersion in sequence. Nitrogen gas was bubbled through the reaction system for 30 minutes to remove dissolved oxygen. The mixture was then heated to 72°C in an oil bath and stirred at 350 rpm for 10 hours under a nitrogen atmosphere. After the reaction, the resulting reaction mixture was transferred to a dialysis bag with a molecular weight cutoff of 8000-14000 Da and dialyzed in 4 L of continuously stirred deionized water. The dialysis water was changed every 8 hours for a total of 72 hours. The resulting temperature-salt dual-responsive zirconium-silicon hybrid nano-crosslinking agent aqueous dispersion was then sealed and stored at 4°C for later use.
[0034] The preparation method of biomimetic surface-modified layered silicate nanosheets includes the following steps: 25.0 g of sodium montmorillonite was weighed and slowly added to a beaker containing 1200 mL of deionized water. The mixture was stirred at 800 rpm for 30 min using a mechanical stirrer. Subsequently, the beaker was placed in an ultrasonic cell disruptor and sonicated in pulse mode at 600 W for a total sonication time of 4 h to obtain a partially exfoliated suspension. This suspension was centrifuged at 6500 rpm for 35 min, and the upper homogeneous and stable colloidal suspension, i.e., the partially exfoliated montmorillonite nanosheet dispersion, was carefully aspirated. 600 mL of the above nanosheet dispersion was measured and placed in an ice-water bath to maintain the system temperature at 0-5 °C. Under continuous stirring, 0.1 mol / L tris(hydroxymethyl)aminomethane buffer was added dropwise to precisely adjust the pH of the system to 8.5. Subsequently, 3.0 g of dopamine hydrochloride was added to the cooled dispersion and stirred at 400 rpm for 15 min until completely dissolved. After dissolution, 6.0 mL of a 0.1 mol / L ferric chloride aqueous solution was slowly added dropwise at a rate of approximately 1 mL / min. After the addition was complete, the ice-water bath was removed, and the reaction system was allowed to react at 25°C with stirring at 400 rpm for 30 h. After the reaction was complete, the product dispersion was centrifuged at 8000 rpm for 20 min, and the supernatant was discarded. Deionized water was added to the precipitate, and the mixture was redispersed by vortexing and sonication, followed by centrifugation again. This washing process was repeated until the supernatant after centrifugation became colorless and transparent. Finally, the washed solid precipitate was redispersed in an appropriate amount of deionized water to prepare an aqueous dispersion of biomimetic surface-modified layered silicate nanosheets for later use.
[0035] The preparation method of high-flow-capacity emulsion-type smart fracturing fluid includes the following steps: In a 2L glass stirred tank, 1200g of deionized water is added as the aqueous phase. Stirring is started, and the speed is controlled at 300rpm. 0.1g of high molecular weight polyacrylamide and 5.0g of partially hydrolyzed polyacrylamide are added sequentially to the water. Stirring is maintained at this speed for 30min to ensure complete dissolution of all polymers, resulting in an aqueous phase mixture. In another beaker, 150g of diesel oil is mixed with 30g of nonionic surfactant Span-80 and stirred with a glass rod for 3min until completely homogeneous, resulting in an oil phase mixture. The stirrer in the stirred tank is replaced with a high-shear dispersing head, and the stirring speed is increased to 9000rpm. Under high-speed shear, the oil phase mixture is slowly and uniformly added dropwise to the aqueous phase mixture, with the adding time controlled at approximately 10min. After the addition is complete, the high-speed shear state of 9000rpm is maintained for 15min to form a stable oil-in-water emulsion. The stirring is then switched back to a conventional mechanical stirrer, and the speed is reduced to 300rpm. First, slowly add 30.0 g of the temperature-salt dual-responsive zirconium-silicon hybrid nano-crosslinking agent aqueous dispersion prepared above to the base emulsion, and stir at 300 rpm for 20 min after the addition. Then, slowly add 50.0 g of the biomimetic surface-modified layered silicate nanosheet aqueous dispersion prepared above to the system, and continue stirring at 300 rpm for 20 min after the addition. 30 min before the planned on-site pumping operation, add 0.01 g of ammonium persulfate as a breaker to the uniformly mixed emulsion, and stir at 300 rpm for 5 min to ensure uniform dispersion, thus finally obtaining the high-ductility emulsion-type intelligent fracturing fluid.
[0036] Comparative Example 1 The specific implementation method is the same as in Example 1, except that no temperature-salt dual-responsive zirconium-silicon hybrid nano-crosslinking agent and biomimetic surface-modified layered silicate nanosheets are added.
[0037] Comparative Example 2 The specific implementation method is the same as in Example 1, except that only a temperature-salt dual-responsive zirconium-silicon hybrid nano-crosslinking agent is added, and no biomimetic surface-modified layered silicate nanosheets are added.
[0038] Comparative Example 3 The specific implementation method is the same as in Example 1, except that unmodified raw materials are used to replace the temperature-salt dual-responsive zirconium-silicon hybrid nano-crosslinking agent and the biomimetic surface-modified layered silicate nanosheets. Specifically, an equal mass of ordinary zirconium oxychloride nanoparticle dispersion is used to replace the temperature-salt dual-responsive zirconium-silicon hybrid nano-crosslinking agent dispersion; an equal mass of unmodified sodium-based montmorillonite dispersion is used to replace the biomimetic surface-modified layered silicate nanosheet dispersion. The preparation method of the high-flow-throughput emulsion-type smart fracturing fluid includes the following steps: In a 2L glass stirred tank, 1000g of deionized water is added as the aqueous phase. Stirring is started, and the speed is controlled at 300rpm. 0.5g of high molecular weight polyacrylamide and 3.5g of partially hydrolyzed polyacrylamide are added to the water sequentially. This speed is maintained and stirring is continued for 30min to obtain an aqueous phase mixture. In another beaker, 100g of diesel oil is mixed with 20g of nonionic surfactant Span-80 to obtain an oil phase mixture. The stirring speed of the stirred tank is increased to 8000rpm. Under high-speed shearing, the oil phase mixture was slowly added dropwise to the aqueous phase mixture. After the addition was complete, shearing was continued at 8000 rpm for 12 minutes to obtain the base emulsion. The stirring speed was reduced to 300 rpm, and 15.0 g of ordinary zirconium oxychloride nanoparticle aqueous dispersion was slowly added to the base emulsion and stirred for 18 minutes. Subsequently, 40.0 g of unmodified sodium montmorillonite aqueous dispersion was slowly added to the system, and stirring was continued for 18 minutes. Just before pumping, 0.05 g of ammonium persulfate was added to the emulsion, and stirring was carried out at 300 rpm for 5 minutes to obtain the comparative fracturing fluid.
[0039] Performance testing The high-fluidity emulsion-type smart fracturing fluids prepared in Examples 1-3 and Comparative Examples 1-3 were subjected to performance tests according to the following method, which included the following steps: all tests were conducted based on the fracturing fluid samples prepared in the examples and comparative examples.
[0040] The initial drag reduction test method is as follows: using an advanced rotational rheometer, under constant temperature conditions of 25℃, and using a cone-plate measurement system, the initial drag reduction is measured at a shear rate starting from 1 s. -1 Increased to 1000s -1 Perform an uplink scan within the specified range and record for 1000 seconds. -1 The apparent viscosity was measured. The drag reduction rate was obtained by simulating pipe friction test. Using an annular flow pipe with an inner diameter of 4 mm, the pressure drop of water and fracturing fluid samples through a certain length of pipe was measured at a constant flow rate. The drag reduction rate was calculated as (water pressure drop - sample pressure drop) / water pressure drop × 100%.
[0041] The viscosity test method after temperature and salt resistance is as follows: Approximately 60 mL of sample is placed into the concentric cylinder measurement system of a high-pressure rheometer. After sealing, nitrogen gas is introduced to pressurize the sample to 3.5 MPa. The temperature is set to increase from 25°C to 140°C at a rate of 3°C / min. When the temperature reaches 80°C, a pre-prepared simulated formation water concentrate is injected into the sample using a syringe pump to achieve a total mineralization of 180,000 mg / L, with a calcium ion concentration of 6,000 mg / L and a magnesium ion concentration of 4,000 mg / L. After the temperature reaches 140°C, the shear rate is set to 170 s⁻¹. -1 The viscosity was kept constant and tested for 120 minutes. The viscosity value at the end of the test (i.e., the 120th minute) was recorded.
[0042] The method for testing the static settling rate of proppant is as follows: 250 mL of fracturing fluid sample is added to a stoppered, narrow-mouthed graduated cylinder, and then 75 g of 100-mesh ceramsite proppant is added evenly. The graduated cylinder is placed vertically in a constant-temperature drying oven preheated to 140°C and left to stand still. At 30 min and 120 min, the graduated cylinder is quickly removed and the height of the proppant interface in the top 100 mL liquid column is measured. The average static settling rate is calculated by the difference in interface height and the time difference, in mm / min.
[0043] The method for testing gel breaking time is as follows: Take 100mL of fracturing fluid sample and place it in a sealable pressure-resistant glass bottle. Add the corresponding mass of ammonium persulfate gel breaking agent according to the formula, shake gently, and then place it in an oven that has been kept at a constant temperature of 90℃. Take it out and observe it every 30 minutes, and record the time point when the sample completely loses its elasticity, the overall fluidity becomes similar to water, and there are no obvious gel clumps.
[0044] The method for testing the residue content of the de-gelling liquid is as follows: filter all the liquid after de-gelling through a quantitative medium-speed filter paper with constant weight (W1), wash the filter residue three times with deionized water, place the filter paper with residue in a 100℃ oven and dry it for 4 hours until constant weight, weigh the total mass (W2), and calculate the residue content using the formula (W2-W1) / 0.1, in mg / L.
[0045] The viscosity test method for the gel breaking liquid is as follows: Take the supernatant after gel breaking and use a rotational viscometer at 25℃ and a shear rate of 100s. -1 Its apparent viscosity was measured under the following conditions, in mPa·s.
[0046] The method for testing the conductivity retention rate is as follows: 20 / 40 mesh ceramic proppant is laid in an API standard flow chamber with a proppant concentration of 5 kg / m². The closing pressure is applied through a hydraulic system. First, the initial conductivity (initial value) is measured using a 2 mPa potassium chloride solution at a closing pressure of 2 MPa. Then, 100 mL of fracturing fluid sample is uniformly injected into the flow chamber to wet the proppant layer. The entire flow chamber is placed in a 90°C environment for 4 hours to simulate gel breaking. After gel breaking, the 2 mPa potassium chloride solution is reused. Within the range of 2 MPa to 60 MPa, the closing pressure is increased stepwise in 10 MPa increments, and the corresponding conductivity is measured. Finally, the percentage of the conductivity value at a closing pressure of 60 MPa to the initial value at 2 MPa is calculated, which is the conductivity retention rate.
[0047] Test Results: Table 1: Test Results of Each Embodiment and Comparative Example Test Project Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 <![CDATA[Initial resistance reduction rate (25°C, 1000s -1 )]]> 78% 75% 80% 68% 70% 65% Viscosity after temperature and salt resistance (140℃, 180000 mg / L, 120 min), mPa·s 58 42 65 8 45 12 Static settling rate of proppant (140℃, 120min), mm / min 0.08 0.12 0.06 0.95 0.15 0.70 Break-through time (90℃), h 4.0 3.8 4.5 3.5 4.2 3.9 Residue content of the breaking liquid, mg / L 95 110 85 520 180 480 <![CDATA[Gel breaker fluid viscosity (25℃, 100s -1 ), mPa·s]]> 3.1 3.4 2.9 1.8 3.8 2.2 Conductivity retention rate under 60MPa closing pressure 82% 78% 84% 45% 60% 50% As can be seen from Table 1, Examples 1-3 systematically solved the key technical contradictions that make it difficult to balance the fracturing fluid system compared to Comparative Examples 1-3.
[0048] In terms of low-friction pumping, the initial drag reduction rates of the three embodiments were significantly higher than those of all comparative examples, especially comparative examples 1 and 3. This is directly attributed to the excellent lubrication effect of the biomimetic modified nanosheets under pumping conditions and the synergistic effect of the emulsion structure.
[0049] Regarding efficient sand carrying in high-temperature and high-salinity formations, the embodiment exhibited a viscosity retention value as high as 42-65 mPa·s after long-term shearing in an environment of 140℃ and 180,000 mg / L salinity, while the viscosity of Comparative Examples 1 and 3 was below 12 mPa·s, completely losing its sand-carrying capacity. At the same time, the static settling rate of the proppant in the embodiment was extremely low (0.06-0.12 mm / min), far lower than that of Comparative Example 1 (0.95 mm / min). This clearly confirms that the temperature-salt dual-responsive nano-crosslinking agent was successfully activated and formed a stable crosslinking network under harsh formation conditions, thereby achieving intelligent thickening and efficient sand carrying.
[0050] In terms of maintaining high conductivity of fractures after gel breaking, the embodiments demonstrate a decisive advantage: the residue content of its gel breaking liquid is only 85 to 110 mg / L, far lower than 520 mg / L of Comparative Example 1 and 480 mg / L of Comparative Example 3, reflecting the thoroughness of the system's gel breaking; most importantly, under the simulated high formation closure pressure of 60 MPa, the conductivity retention rate of the embodiments is as high as 78-84%, while that of Comparative Examples 1, 2, and 3 is only 45%, 60%, and 50%, respectively. This huge difference directly proves the unique "anchoring" and "structural maintenance" effect of the biomimetic surface-modified nanosheets on the proppant filling layer after gel breaking, effectively preventing the rapid decay of conductivity. The results of Comparative Example 2 further revealed the functional differences between the two modified compounds: it achieved better sand-carrying performance (viscosity 45 mPa·s) due to the presence of a crosslinking agent, but due to the lack of biomimetic nanosheets, its conductivity retention rate (60%) was significantly lower than that of any of the examples. This precisely illustrates that resolving the contradiction between "sand-carrying" and "high conductivity" requires the synergy of both, and neither can be omitted.
[0051] In summary, the test data fully demonstrate that the present invention, through the synergistic intelligent effect of temperature-salt dual-responsive zirconium-silicon hybrid nano-crosslinking agent and biomimetic surface-modified layered silicate nanosheets, successfully integrates three previously difficult-to-coexist properties: high drag reduction rate, excellent temperature and salt resistance and sand-carrying capacity, and extremely high conductivity retention rate after gel breaking, thereby systematically solving the aforementioned technical contradictions.
[0052] The embodiments described above are merely examples of several implementations of the present invention, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these modifications and improvements all fall within the scope of protection of the present invention.
Claims
1. A method for preparing a high-flow-throughput emulsion-type smart fracturing fluid, characterized in that the steps include... include: S1. By weight, add 80-120 parts of deionized water to a stirred tank and stir. Add 0.01-0.1 parts of polyacrylamide and 0.1-0.5 parts of partially hydrolyzed polyacrylamide and stir to obtain an aqueous phase mixture. Mix 5-15 parts of diesel oil with 1-3 parts of nonionic surfactant Span-80 to obtain an oil phase mixture. While stirring, add the oil phase mixture to the aqueous phase mixture and continue stirring to obtain a base emulsion. S2. Add 0.05-0.3 parts of temperature-salt dual-responsive zirconium-silicon hybrid nano-crosslinking agent to the base emulsion obtained in step S1, stir, then add 0.1-0.5 parts of biomimetic surface-modified layered silicate nanosheets and stir; finally, add 0.001-0.005 parts of ammonium persulfate just before pumping.
2. The preparation method of the high-flow-rate emulsion-type intelligent fracturing fluid according to claim 1, characterized in that, In step S1, the stirring time is 10-15 minutes.
3. The preparation method of the high-flow-rate emulsion-type intelligent fracturing fluid according to claim 1, characterized in that, In step S2, the stirring time is 15-20 minutes.
4. The preparation method of the high-flow-throughput channel emulsion-type intelligent fracturing fluid according to claim 1, characterized in that, The preparation method of the temperature-salt dual-responsive zirconium-silicon hybrid nano-crosslinking agent includes: A1. Under nitrogen protection, zirconium oxychloride was dissolved in anhydrous ethanol in parts by weight. Ammonia was added dropwise to pH 9-10 with stirring, and the mixture was aged at room temperature to obtain zirconium hydroxide gel. γ-aminopropyltriethoxysilane and acryloyloxypropyltrimethoxysilane were added to toluene, stirred, and water was added to adjust the pH to 4.0-6.0 to obtain a silane solution. The zirconium hydroxide gel was added to the silane solution and refluxed at 78-82℃ to obtain a suspension of zirconium silanide nanoparticles. A2. After centrifuging and washing the silanized zirconium nanoparticle suspension, it was redispersed in N,N-dimethylformamide; N-isopropylacrylamide monomer, acrylic acid monomer, and azobisisobutyronitrile initiator were added, and the reaction was carried out at 68-72℃ to obtain the reaction mixture; the reaction mixture was dialyzed in deionized water.
5. The preparation method of the high-flow-throughput channel emulsion-type intelligent fracturing fluid according to claim 4, characterized in that, In step A1, the reflux reaction is carried out at 78-82℃ for 24-30 hours.
6. The preparation method of the high-flow-throughput channel emulsion-type intelligent fracturing fluid according to claim 4, characterized in that, In step A2, the reaction time is 8-10 hours at 68-72℃.
7. The preparation method of the high-flow-throughput emulsion-type intelligent fracturing fluid according to claim 1, characterized in that, The method for preparing the biomimetic surface-modified layered silicate nanosheets includes: B1. Disperse sodium-based montmorillonite in deionized water, stir and sonicate, then centrifuge in a high-speed centrifuge to separate and obtain a partially exfoliated montmorillonite nanosheet dispersion. B2. Place the partially exfoliated montmorillonite nanosheet dispersion in an ice-water bath, adjust the pH to 8.0-8.5 using tris(hydroxymethyl)aminomethane buffer, then add dopamine hydrochloride, stir, add ferric chloride solution dropwise, and continue stirring the reaction; after the reaction is complete, wash with deionized water by centrifugation.
8. The preparation method of the high-flow-throughput channel emulsion-type intelligent fracturing fluid according to claim 7, characterized in that, In step B1, the stirring and ultrasonic treatment time is 2-4 hours.
9. The preparation method of the high-flow-throughput channel emulsion-type intelligent fracturing fluid according to claim 7, characterized in that, In step B2, the stirring reaction continues for 24-30 hours.
10. A high-flow-throughput emulsion-type intelligent fracturing fluid, characterized in that, The high-fluidity channel emulsion-type smart fracturing fluid is prepared according to the preparation method of any one of claims 1-9.