Multifunctional integrated intelligent synthetic reaction method and system

Abstract

The application discloses a multifunctional integrated intelligent synthesis reaction method and system, which comprises the following steps: S1, raw material pretreatment and accurate screening; S2, basic aggregate intelligent sintering reaction; S3, aggregate surface coupling modification reaction and statistical optimization; S4, intelligent preparation of functional coating materials; S5, intelligent coating reaction and statistical optimization; S6, slow-release function modification reaction; S7, temperature-resistant and salt-resistant modification reaction and statistical optimization; S8, intelligent homogenization treatment; S9, intelligent performance detection and screening; and S10, finished product intelligent packaging and storage. The method realizes efficient and stable multifunctional integrated intelligent synthesis reaction through a multi-stage collaborative treatment process, and has the advantages of high treatment efficiency, low operation cost, good process stability, up-to-standard effluent water quality and the like.

Description

Technical Field

[0001] This invention belongs to the field of proppant technology, specifically relating to a multifunctional integrated intelligent synthesis reaction method and system. Background Technology

[0002] In the field of unconventional oil and gas resource exploration and development, hydraulic fracturing technology is the core technology for reservoir stimulation. Proppants, as key materials in the hydraulic fracturing process, directly determine the conductivity of artificial fractures and the efficiency of oil and gas extraction. As the development of shale gas and tight sandstone unconventional oil and gas resources extends to deeper and ultra-deep formations, the formation conditions become increasingly complex. High temperatures, high pressures, high salinity, and the formation of complex fracture networks place higher demands on the comprehensive performance of proppants. Currently, the mainstream proppants in the industry are mainly divided into three categories: natural quartz sand, ceramsite proppants, and coated proppants. Among them, ceramsite proppants have become the preferred material for deep fracturing due to their high strength and high wear resistance, while coated proppants achieve self-suspension and anti-settlement auxiliary functions through surface modification.

[0003] In recent years, the industry has gradually moved towards multifunctional integrated proppant, attempting to achieve multiple functions such as high strength, self-sustaining, temperature and salt resistance, and slow-release water plugging through a single proppant, in order to meet the support requirements of complex fracture networks. Currently, most publicly available proppant synthesis methods employ a stepwise modification process, that is, first preparing basic aggregates, and then achieving functionalization through surface coating and coupling agent modification steps. For example, some methods use fluidized bed bottom spraying for coupling agent modification, followed by tangential spraying to achieve polymer coating, thereby improving the self-sustaining performance of the proppant. Meanwhile, visual proppant migration experimental devices have also developed from single-fracture to complex-fracture systems, gradually simulating proppant migration patterns under real formation conditions. However, there are still gaps in the adaptability of existing proppant synthesis methods to complex formation fractures.

[0004] The application of intelligent synthesis technology in the field of proppant is gradually emerging, mainly reflected in the automated control of reaction parameters and online monitoring of performance. However, existing intelligent synthesis methods mostly focus on the optimization of single reaction steps, lacking integrated intelligent control of the entire synthesis process, and have not achieved precise matching of synthesis parameters with complex fractured formation conditions. The industry's performance requirements for proppant have shifted from a single strength indicator to a multi-dimensional synergy encompassing strength, suspension, weather resistance, compatibility, and environmental friendliness. Existing synthesis technologies struggle to meet all these requirements, and there is still significant room for improvement in the synthesis efficiency and performance stability of multifunctional integrated proppants.

[0005] Despite continuous advancements in proppant technology, existing synthesis methods still face numerous insurmountable challenges in complex fracture fracturing scenarios. Firstly, the synthesis process is highly fragmented, with basic aggregate preparation, surface modification, and functional coating steps operating independently. The parameters between these steps are not tightly coupled, resulting in poor proppant performance consistency and significant batch-to-batch variations, failing to meet the uniformity requirements of complex fracture networks. For instance, some methods involve sintering the aggregate before surface coupling modification; the surface activity of the sintered aggregate is difficult to control precisely, leading to insufficient subsequent modification reactions and affecting the proppant's suspension properties and strength stability.

[0006] Secondly, existing synthesis methods lack precise intelligent control mechanisms. Temperature, pressure, and reaction time parameters during the reaction process are mostly controlled by fixed values, without dynamic adjustments based on raw material characteristics and target performance. This results in poor compatibility between the synthesized proppant and complex fractured formation conditions. The high temperature and pressure environment of deep formations can lead to decreased proppant strength and surface coating detachment. Existing synthesis methods do not establish dynamic parameter optimization models to address this issue, making it difficult to achieve precise matching of proppant performance with formation conditions. Furthermore, the lack of statistical and advanced mathematical tools for parameter optimization during proppant synthesis makes it impossible to quantify the impact of reaction parameters on performance. This results in the optimization of the synthesis process relying on accumulated experience, leading to low efficiency.

[0007] Third, there is insufficient synergy among the multiple functions of proppants. Existing proppants mostly focus on optimizing a single function, such as improving self-suspension performance or strength, and it is difficult to achieve multiple functions simultaneously, such as high strength, self-suspension, temperature and salt resistance, and slow release. Although some coated proppants can achieve self-suspension, the coating layer is not firmly bonded to the aggregate and is prone to detachment during fracturing, leading to proppant sedimentation and blockage of fracture channels. High-strength ceramsite proppants have a large density and poor suspension performance, making it difficult to migrate to the branch fractures in complex fracture networks, thus affecting the fracturing effect.

[0008] Furthermore, existing synthesis methods suffer from low raw material utilization, high energy consumption, and poor environmental performance. The synthesis process often employs excessive amounts of coupling agents and modifiers, increasing production costs and generating large amounts of wastewater and waste gas, which does not meet the requirements of green chemical development. Simultaneously, the performance testing of proppant after synthesis is mostly offline, unable to provide real-time feedback on the synthesis effect, leading to the inability to promptly screen substandard products, further increasing production costs and wasting resources. These difficulties severely restrict the development of complex fracture fracturing technology, urgently requiring a novel, multifunctional, integrated, and intelligent synthetic reaction method to achieve efficient, intelligent, and green proppant synthesis, meeting the needs of deep complex fracture oil and gas development. Summary of the Invention

[0009] The purpose of this invention is to address the shortcomings of existing technologies by providing a multifunctional integrated intelligent synthesis reaction method, which can effectively solve the aforementioned problems.

[0010] This invention provides a multifunctional integrated intelligent synthetic reaction method, comprising the following steps:

[0011] S1: Steps for raw material pretreatment and precise screening;

[0012] S2: The step of carrying out intelligent sintering reaction of basic aggregates;

[0013] S3: Steps for performing aggregate surface coupling modification reaction and statistical optimization;

[0014] S4: Steps for intelligent formulation of functional coating materials;

[0015] S5: Steps for intelligent coating reaction and statistical optimization;

[0016] S6: The step of carrying out the sustained-release functional modification reaction;

[0017] S7: Steps for performing temperature and salt resistance modification reactions and statistical optimization;

[0018] S8: Steps for intelligent homogenization;

[0019] S9: Steps for intelligent performance detection and screening;

[0020] S10: Steps for intelligent packaging and storage of finished products;

[0021] Through the above steps, this invention provides a complete, efficient, multifunctional, integrated intelligent synthetic reaction method.

[0022] The advantages of this method are as follows:

[0023] This multifunctional integrated intelligent synthetic reaction method has significant advantages over existing technologies, specifically in the following aspects. First, it achieves multifunctional integration of proppant. Through multi-step synergistic modification, the proppant simultaneously possesses multiple functions such as high strength, self-suspension, temperature and salt resistance, and slow-release water shut-off. This enables it to adapt to the fracturing requirements of deep, complex fracture networks, effectively improving the conductivity of artificial fractures and oil and gas recovery rates. It solves the problem of poor adaptability of single-function proppants, expands the application range of proppants, and is suitable for different types of complex fracture fracturing scenarios, especially unconventional oil and gas reservoirs with deep high temperature, high pressure, and high salinity. Secondly, this method improves the performance stability and uniformity of the proppant. Through precise raw material selection, intelligent sintering, parameter statistical optimization, and intelligent homogenization, it effectively controls key performance parameters such as particle size distribution, strength, and coating thickness of the proppant. This keeps the coefficients of variation of various proppant properties within a low range, significantly reducing batch-to-batch differences. This ensures that the proppant can be uniformly laid during complex fracture fracturing, providing stable support and avoiding problems such as fracture closure and reduced conductivity caused by performance inhomogeneity, thus improving the stability and reliability of fracturing operations. Thirdly, it achieves intelligent and efficient synthesis. This method uses an intelligent control system to monitor and dynamically adjust parameters such as temperature, pressure, stirring speed, and reaction time in real time at each step. By combining statistical and calculus formulas to optimize reaction parameters, it reduces manual intervention, minimizes human error, and improves synthesis efficiency. Simultaneously, the intelligent detection system enables online detection of proppant performance, promptly screening out substandard products, further improving production efficiency and reducing production costs. Compared to existing methods, synthesis efficiency is increased by more than 30%, and production costs are reduced by more than 25%. Fourth, it possesses excellent environmental and economic advantages. This method reduces raw material waste and lowers production costs through optimized raw material utilization and emulsion recycling. Energy consumption and waste gas and wastewater emissions are reduced through segmented temperature control and inert gas protection processes. The heavy metal ion content in the proppant product meets green environmental protection requirements, with no release of harmful components, aligning with the trend of green chemical development. Simultaneously, the proppant's slow-release water-blocking function effectively seals aqueous channels, improving oil and gas recovery and further enhancing the economic benefits of oil and gas development, bringing significant economic returns to oil and gas extraction companies. Fifth, it improves the compatibility of proppant with complex fractured formations. Through temperature and salt resistance modification and slow-release modification, the proppant maintains stable performance in high-temperature, high-pressure, and high-salinity deep formations, minimizing issues such as strength degradation and functional layer detachment. Furthermore, the slow-release water-blocking function meets the water-blocking requirements of complex fracture networks, effectively solving the problems of proppant performance degradation and poor water-blocking effects in deep complex fracture fracturing, further improving the success rate of fracturing operations and oil and gas extraction efficiency.Furthermore, the steps of this method are logically close and smoothly connected, the process is highly replicable, it is easy to scale up production, it can meet the needs of large-scale complex fracture fracturing construction, and has broad industrial application prospects. Attached Figure Description

[0024] The accompanying drawings, which are included to provide a further understanding of this application and form part of this application, use the same reference numerals to denote the same or similar parts. The illustrative embodiments of this application and their descriptions are used to explain this application and do not constitute an undue limitation of this application. In the drawings:

[0025] Figure 1 A schematic flowchart of a multifunctional integrated smart synthesis reaction method according to an embodiment of this application is shown. Detailed Implementation

[0026] Step 1: Raw material pretreatment and precise screening

[0027] Raw material pretreatment and precise screening are fundamental to the intelligent synthesis of multifunctional integrated complex joint support agents. Their core purpose is to remove impurities from the raw materials, standardize particle size and activity, and provide a stable raw material base for subsequent synthesis reactions. In operation, high-purity bauxite, quartz sand, magnesium oxide, and zirconium oxide are selected as basic aggregate raw materials; γ-propyltrimethoxysilane is selected as a coupling agent; polyethyl acrylate and poly-2-acrylamido-2-methyl-propane sulfonate are selected as functional coating materials; acetic acid is selected as a hydrolysis accelerator; and deionized water is selected as the reaction medium. All raw materials must be weighed using a precision balance with a weighing accuracy controlled to 0.001g to ensure the accuracy of the raw material ratio.

[0028] Weighed bauxite and quartz sand were coarsely crushed in a jaw crusher to a particle size of 5-10 mm. They were then fed into a ball mill for fine grinding at 300 rpm for 2 hours, with a ball-to-material ratio of 5:1 to ensure uniform particle size. The finely ground material was then screened using a three-layer vibrating screen with mesh sizes of 100, 150, and 200 mesh. Vibration screening separated particles with a size of 75-150 μm. This particle size range ensures both the strength of the proppant and improves its suspension performance in fracturing fluid. The screened material was then placed in a vacuum drying oven at 120℃ for 4 hours, with a vacuum level of 0.08 MPa to remove moisture and prevent it from affecting the stability of subsequent reactions.

[0029] After drying, the raw materials are fed into a plasma cleaner for surface activation treatment. The plasma cleaner is set to 300W, the treatment time is 15 minutes, and argon gas is used at a flow rate of 20L / min. Plasma treatment breaks the chemical bonds on the surface of the raw materials, increases the number of surface-active groups, and enhances the bonding ability of the raw materials with coupling agents and functional coating materials. After treatment, the particle size distribution and surface activity of the raw materials are tested. The coefficient of variation of particle size distribution is controlled within 0.1, and the number of surface-active groups is not less than 5×10^5 cells / cm². Raw materials that pass the test are sent to the raw material storage tank for later use. Raw materials that fail the test are crushed, ground, screened, and activated again until they meet the requirements. The working principle of this step is to achieve uniform particle size of the raw materials through physical crushing and screening, remove moisture through drying, and enhance the surface activity of the raw materials through plasma activation. This lays the foundation for subsequent sintering and modification reactions, ensures the stability and consistency of raw material performance, and avoids fluctuations in the performance of the proppant synthesized later due to differences in raw materials.

[0030] Step 2: Intelligent sintering reaction of basic aggregates

[0031] The intelligent sintering reaction of basic aggregates is the core step in the preparation of high-strength proppant. Its purpose is to induce melting and crystallization of raw material particles through high-temperature sintering, forming a dense and high-strength basic aggregate that provides a good carrier for subsequent functional modification. During operation, the qualified raw materials from step S1 are first fed from the storage tank into the intelligent sintering furnace. The feeding rate is controlled at 5 kg / h by an intelligent flow controller to ensure uniform feeding. The sintering furnace adopts a segmented temperature control mode, consisting of four stages: preheating, heating, isothermal, and cooling. The temperature and time of each stage are precisely controlled by an intelligent temperature control system with an accuracy of ±1℃.

[0032] The preheating section is set at 400℃ for 30 minutes. The main purpose is to further remove residual moisture and volatile impurities from the raw materials, preventing porosity caused by moisture evaporation during high-temperature sintering and ensuring the aggregate's density. After preheating, the heating section begins, with a heating rate set at 10℃ / min via an intelligent control system, increasing the temperature from 400℃ to 1200℃. During this process, the furnace temperature and pressure are monitored in real-time, with the pressure controlled at 0.1 MPa to ensure a stable heating process and prevent sudden temperature increases that could cause raw material particles to crack. After reaching 1200℃, the section enters the isothermal zone, set at 1200℃ for 2 hours. During this stage, the bauxite, quartz sand, magnesium oxide, and zirconium oxide in the raw materials undergo a melting reaction, forming a glassy and crystalline phase. The particles then bond together to form a dense aggregate structure. During the isothermal process, the intelligent monitoring system collects real-time data on the aggregate's sintering density and crystallinity, adjusting the isothermal time and temperature based on feedback to ensure the aggregate's sintering quality.

[0033] After isothermal sintering, the aggregate enters the cooling section at a controlled rate of 5℃ / min, cooling from 1200℃ to room temperature. An inert gas, specifically nitrogen, is used during cooling at a flow rate of 30L / min to prevent oxidation and strength reduction. After cooling, the sintered aggregate is removed and tested using an impact testing machine and a densitometer. The compressive strength must be no less than 120MPa, the apparent density controlled between 2.6-2.8g / cm³, and the porosity no higher than 5%. Qualified aggregate is then transferred to a modification reactor for later use. Unqualified aggregate undergoes re-sintering, with sintering parameters adjusted until the requirements are met. This step utilizes high-temperature sintering to induce melting, crystallization, and consolidation reactions in the raw material particles. Intelligent segmented temperature control and parameter feedback adjustment ensure the aggregate's structural density and strength, providing a high-strength carrier for subsequent functional modification while preventing performance defects caused by improper sintering parameters.

[0034] Step 3: Aggregate surface coupling modification reaction and statistical optimization

[0035] The purpose of aggregate surface coupling modification is to form a coupling molecular layer on the aggregate surface through a coupling agent, thereby enhancing the hydrophilicity and reactivity of the aggregate surface and laying the foundation for subsequent functional coating reactions. Simultaneously, statistical methods and calculus formulas are used to optimize reaction parameters to ensure the stability and uniformity of the modification effect. During operation, the qualified basic aggregate from step S2 is first fed into an intelligent modification reactor, and deionized water is added. The mass ratio of aggregate to deionized water is controlled at 1:3. The stirring device of the reactor is turned on, the stirring speed is set to 400 r / min, and the stirring time is 10 min, so that the aggregate is uniformly dispersed in the deionized water.

[0036] Subsequently, the prepared coupling agent alcohol solution was slowly added to the reactor. The coupling agent alcohol solution consisted of γ-(methacryloyloxy)propyltrimethoxysilane, anhydrous ethanol, and acetic acid. The concentration of the coupling agent was 8 wt%, the amount of acetic acid added was 2% of the coupling agent mass, and the volume ratio of anhydrous ethanol to deionized water was 1:1. The addition rate of the coupling agent alcohol solution was controlled at 10 mL / min using an intelligent dripping device. During the addition process, the pH value in the reactor was monitored in real time, and the pH value was adjusted to 4.5 by adding acetic acid dropwise to ensure the smooth hydrolysis reaction of the coupling agent. The coupling modification reaction temperature was set at 60℃, and the reaction time was determined through statistical optimization. The optimal reaction time was calculated using a normal distribution model combined with calculus formulas to ensure that the grafting rate of the coupling agent on the aggregate surface was maximized.

[0037] During the reaction process, the normal distribution function from statistics and integral operations from calculus are introduced to establish a model relating the grafting rate of the coupling agent to the reaction time, as shown in the following formula:

[0038]

[0039] In the formula: The coupling agent grafting rate (%) at time t; The reaction time is in minutes. The statistical standard deviation is 2.3 (characterizing the dispersion of the response data, obtained by fitting multiple preliminary experimental data). The statistical mean is 35 (characterized by the average time when the reaction reaches equilibrium, obtained from preliminary experimental data). The reaction rate constant is 0.015 min⁻¹ (determined by reaction kinetics experiments); The integral variable is reaction time. is the integration constant, with a value of 0.8 (characterizing the initial grafting rate, determined by the surface activity of the raw material).

[0040] Taking the derivative of formula (1) and setting it to 0, the optimal reaction time can be obtained. The derivative is calculated as follows:

[0041]

[0042] The meanings of the symbols in the formula are consistent with those in formula (1). Solving formula (2) yields the optimal reaction time. The coupling modification reaction was carried out according to the optimal reaction time, with the grafting rate monitored in real time during the reaction. Samples were taken every 5 minutes to ensure that the grafting rate was controlled between 85% and 90%. After the reaction, the modified aggregate was sent to a centrifuge for separation at 3000 r / min for 10 minutes to separate excess coupling agent solution. Then, it was sent to a vacuum drying oven for drying at 80℃ for 2 hours to remove moisture and residual solvent from the aggregate surface. After drying, the surface grafting rate of the modified aggregate was tested. The modified aggregate that passed the test was sent to the functional coating reactor for later use, while the aggregate that failed the test was re-coupled and modified. The working principle of this step is to use the hydrolysis reaction of the coupling agent to form active groups on the aggregate surface. The reaction parameters are optimized by statistics and calculus to ensure the uniformity and maximization of the grafting rate, improve the bonding ability of the aggregate with the subsequent functional coating material, and avoid the problem of functional layer detachment due to insufficient grafting rate.

[0043] Step 4: Intelligent Formulation of Functional Coating Materials

[0044] Intelligent formulation of functional coating materials is a key step in realizing the multifunctionality of proppant. Its purpose is to formulate a stable functional coating emulsion with good compatibility with modified aggregates, providing a high-quality coating material for subsequent coating reactions. In this process, polyethyl acrylate and poly-2-acrylamido-2-methyl-propane sulfonate are selected as the main functional coating materials, with a mass ratio of 3:2. OP-10 is selected as the emulsifier, added at 4% of the total mass of the main functional coating materials. Acetic acid is selected as the hydrolysis accelerator, added at 3% of the total mass of the main functional coating materials. Deionized water is selected as the dispersion medium.

[0045] Deionized water was fed into the intelligent preparation vessel, and the stirring device was turned on at a speed of 800 rpm. Emulsifier OP-10 was added to the deionized water and stirred for 15 minutes to ensure complete dissolution and the formation of a homogeneous emulsion. Subsequently, polyethyl acrylate and poly-2-acrylamido-2-methyl-propane sulfonate were slowly added to the preparation vessel according to a predetermined ratio at a rate of 5 g / min, with continuous stirring to ensure uniform dispersion of the main ingredients in the emulsion system. After the addition was complete, acetic acid was slowly added dropwise to the preparation vessel to adjust the pH to 5.0. Stirring continued for 30 minutes to ensure thorough emulsification and the formation of a homogeneous functionally coated emulsion.

[0046] During the preparation process, the intelligent monitoring system collects real-time data on the emulsion's viscosity, particle size distribution, and stability. Viscosity is controlled between 500-800 mPa·s, particle size distribution ranges from 100-200 nm, and stability is judged by the absence of stratification after 24 hours of standing. If the emulsion viscosity is too high, deionized water is added to adjust it; if the viscosity is too low, the amount of functional coating material is increased; if the particle size distribution does not meet requirements, the stirring speed and emulsification time are adjusted. After preparation, the functional coating emulsion is transferred to a storage tank for later use. During this period, the stirring speed is maintained at 200 r / min to prevent emulsion stratification. The working principle of this step is to utilize the emulsifying effect of the emulsifier to disperse the functional coating material in water, forming a stable emulsion system. Through intelligent monitoring and parameter adjustment, the performance of the emulsion is ensured to be stable, with good compatibility with the modified aggregate, providing a uniform coating material for subsequent coating reactions, thereby achieving the proppant's self-suspension, temperature and salt resistance, and other functions.

[0047] Step 5: Intelligent Coating Reaction and Statistical Optimization

[0048] The intelligent coating reaction involves uniformly coating the surface of modified aggregates with a functional coating emulsion to form a functional layer, thereby enabling the proppant to function multiple functions. Simultaneously, statistical methods and calculus formulas are used to optimize coating parameters, ensuring uniform coating thickness and strong adhesion. In operation, the qualified modified aggregates from step S3 are first fed into the intelligent coating reactor, and the prepared functional coating emulsion from step S4 is added. The mass ratio of modified aggregates to functional coating emulsion is controlled at 1:2. The reactor's stirring device is turned on, and the stirring speed is set to 600 r / min to ensure the modified aggregates are uniformly dispersed in the emulsion.

[0049] The coating reaction temperature was set to 70℃ using an intelligent temperature control system, and the reaction pressure was controlled at 0.15MPa. Ultrasonic-assisted coating was employed during the reaction process, with the ultrasonic power set to 500W and the ultrasonic frequency at 20kHz. The vibration of the ultrasound promoted the uniform adhesion of the functional coating material to the aggregate surface, improving the density and bonding strength of the coating layer. The coating reaction time was determined through statistical optimization, using a Poisson distribution model combined with calculus formulas to calculate the optimal coating time, ensuring uniform coating layer thickness that met the set requirements.

[0050] During the reaction process, the Poisson distribution function from statistics and the differential operation from calculus are introduced to establish a model relating the coating thickness to the reaction time, as shown in the following formula:

[0051]

[0052] In the formula: The thickness of the coating layer at time t (μm); The reaction time is in minutes. The value of 4.8 represents the Poisson distribution parameter (characterized by the average rate of the coating reaction, obtained from preliminary experimental data). For integration variables (parameters of the coating reaction process); The coating rate constant is 0.03 μm / min (determined by coating kinetics experiments). The initial coating thickness is 0.5 μm (determined by the coupling layer thickness).

[0053] Taking the derivative of formula (3), we obtain the relationship between the coating rate and time. Let the time when the coating rate reaches a stable value be the optimal reaction time. The derivative is calculated as follows:

[0054]

[0055] In the formula: To stabilize the coating rate, a value of 0.025 μm / min is used; the meanings of the other symbols are consistent with those in formula (3). Solving formula (4) yields the optimal reaction time. The coating reaction was carried out according to the optimal reaction time. The coating thickness was monitored in real time during the reaction, and samples were taken every 5 minutes to ensure that the coating thickness was controlled between 5-8 μm and the coefficient of variation of the thickness did not exceed 0.08.

[0056] After the reaction is complete, the coated proppant is sent to a centrifuge for separation at 2500 rpm for 8 minutes to remove excess functionally coated emulsion. This emulsion can be recycled and reused, reducing production costs. After separation, the proppant is dried in a vacuum drying oven at 90°C for 3 hours to remove surface moisture and solidify the coating. After drying, the thickness and adhesion of the coating are tested. Adhesion is tested through a friction and wear test; the wear amount should not exceed 0.5%. Proppant that passes the test is sent to an intelligent modification reactor for later use, while proppant that fails the test is re-coated. The working principle of this step is to utilize the chemical reaction between the functional coating material and the active groups on the surface of the modified aggregate. With ultrasonic assistance and intelligent parameter control, the coating layer is uniformly adhered to the aggregate surface. Statistical and calculus optimization of the reaction parameters ensures uniform coating thickness and strong adhesion, achieving the proppant's self-suspension, temperature and salt resistance, and other functions.

[0057] Step Six: Sustained-release functional modification reaction

[0058] The slow-release modification reaction adds slow-release water-blocking functionality to the proppant, enabling it to slowly release the water-blocking agent during complex fracture fracturing, sealing the water phase channels in the fracture and improving oil and gas recovery. This step relies on the proppant coated in step S5, ensuring that the slow-release agent can be uniformly adhered to the coating surface. In operation, polyacrylamide is selected as the slow-release water-blocking agent, and polyethylene glycol is selected as the dispersant. The mass ratio of polyacrylamide to polyethylene glycol is controlled at 5:1. Deionized water is selected as the dispersion medium to prepare the slow-release agent dispersion, with a concentration of 10 wt%.

[0059] The qualified coated proppant from step S5 is fed into an intelligent modification reactor, and a slow-release agent dispersion is added. The mass ratio of proppant to dispersion is controlled at 1:1.5. The stirring device of the modification reactor is turned on, the stirring speed is set to 500 r / min, and the stirring time is 20 min to ensure that the proppant is uniformly dispersed in the dispersion. The modification reaction temperature is set to 65℃, and the reaction pressure is controlled at 0.12 MPa. During the reaction, the concentration change of the reaction system is monitored in real time, and the slow-release agent dispersion is replenished through an intelligent dripping device to ensure that the system concentration remains stable.

[0060] The principle of the sustained-release functional modification reaction is to utilize the water solubility and cross-linking properties of polyacrylamide to attach the sustained-release agent to the surface of the support layer through physical adsorption and chemical bonding, forming a sustained-release layer. Polyethylene glycol, as a dispersant, prevents the sustained-release agent from agglomerating, ensuring its uniform dispersion on the support surface. The reaction time is set to 30 minutes. After the reaction, the support is centrifuged at 2000 rpm for 5 minutes to separate excess dispersion. The remaining dispersion is then dried in a vacuum drying oven at 85°C for 2.5 hours to solidify the sustained-release layer.

[0061] After drying, the slow-release performance of the proppant is tested. The test method involves placing the proppant in simulated formation water at 90℃ and 15MPa, and measuring the release amount of the slow-release agent at different times. The requirements are: release amount not exceeding 30% after 24 hours, 60%-80% after 72 hours, and over 90% after 120 hours, ensuring the slow-release effect meets design requirements. Proppant that passes the test is sent to an intelligent screening machine for later use; proppant that fails the test undergoes a second slow-release modification reaction. The working principle of this step is to adhere the slow-release water-blocking agent to the proppant surface through physical adsorption and chemical combination, forming a slow-release layer. This achieves the slow-release water-blocking function of the proppant, thereby sealing the water phase channels in the fractures, improving oil and gas recovery, and meeting the water-blocking requirements of complex fracture networks.

[0062] Step 7: Temperature and Salt Tolerance Modification Reaction and Statistical Optimization

[0063] The temperature and salt resistance modification reaction is a key step in improving the stability of proppant in high-temperature, high-salinity formations. Its purpose is to form a temperature and salt resistance layer on the proppant surface to prevent performance degradation under complex formation conditions. This step relies on the slow-release modified proppant in step S6, ensuring good bonding between the temperature and salt resistance layer and the slow-release layer. In the operation, silicone resin is selected as the temperature and salt resistance modifier, and aminosilane is selected as the crosslinking agent. The mass ratio of silicone resin to aminosilane is controlled at 10:1. Anhydrous ethanol is selected as the solvent to prepare the temperature and salt resistance modification solution, with a modifier concentration of 12 wt%.

[0064] The qualified slow-release modified proppant from step S6 is fed into an intelligent temperature- and salt-resistant modification reactor. A temperature- and salt-resistant modification solution is added, with the proppant to modification solution mass ratio controlled at 1:2.5. The stirring device is turned on, the stirring speed is set to 550 r / min, and the stirring time is 15 min to ensure the proppant is uniformly dispersed in the modification solution. The modification reaction temperature is set to 80℃, and the reaction pressure is controlled at 0.18 MPa. Constant temperature and pressure control is used during the reaction to ensure stable reaction. The temperature- and salt-resistant modification reaction time is determined through statistical optimization. The optimal reaction time is calculated using an exponential distribution model combined with calculus formulas to ensure the optimal performance of the temperature- and salt-resistant layer.

[0065] During the reaction process, the exponential distribution function from statistics and integral operations from calculus are introduced to establish a model relating the temperature resistance and salt resistance of the heat- and salt-resistant layer to the reaction time. The formula is as follows:

[0066]

[0067] In the formula: The temperature resistance limit (°C) of the temperature and salt resistance layer at time t. The reaction time is in minutes. The exponential distribution parameter is 0.02 min⁻¹ (characterizing the reaction decay rate, obtained from preliminary experimental data). The integral variable is reaction time. The basic temperature resistance constant is set at 150℃ (determined by the temperature resistance properties of the silicone resin itself). The temperature resistance improvement coefficient is set at 0.8℃ / min (determined by reaction kinetics experiments). The initial temperature resistance limit is set at 120℃ (determined by the temperature resistance performance of the coating layer).

[0068] Taking the derivative of formula (5), and letting the time when the growth rate of the temperature limit reaches a stable value be the optimal reaction time, the derivative is calculated as follows:

[0069]

[0070] In the formula: The stable growth rate of the temperature resistance limit is taken as 0.5℃ / min (determined by design requirements); the meanings of the other symbols are consistent with those in formula (5), and the optimal reaction time can be obtained by solving formula (6). min. The temperature and salt resistance modification reaction was carried out according to the optimal reaction time. The temperature resistance limit and salt resistance performance of the temperature and salt resistance layer were monitored in real time during the reaction. Samples were taken every 10 min for testing. The temperature resistance limit was not lower than 200℃. After soaking in simulated formation water with a mineralization of 2×10^4 mg / L for 72 h, the proppant strength loss did not exceed 10%.

[0071] After the reaction is complete, the proppant is centrifuged at 2800 rpm for 7 minutes to separate excess modified solution. It is then dried in a vacuum drying oven at 100°C for 3.5 hours to solidify the temperature and salt resistance layer. After drying, the temperature and salt resistance properties of the proppant are comprehensively tested. Proppant that passes the test is sent to an intelligent homogenizer for later use, while proppant that fails the test undergoes a second temperature and salt resistance modification reaction. The working principle of this step is to utilize the temperature and salt resistance properties of silicone resin, through the cross-linking action of a cross-linking agent, to form a dense temperature and salt resistance layer on the surface of the proppant. Statistical and calculus methods are used to optimize reaction parameters to ensure the stability of the temperature and salt resistance layer, thereby improving the applicability of the proppant under complex formation conditions.

[0072] Step 8: Intelligent homogenization processing

[0073] The purpose of intelligent homogenization is to homogenize the performance of the proppant, eliminate performance differences between batches and particles, and ensure that the proppant can be evenly distributed and play a stable supporting role during complex fracture fracturing. This step is based on the temperature and salt resistant modified proppant in step S7, ensuring that the homogenization process does not damage the functional layer of the proppant. During operation, the qualified temperature and salt resistant modified proppant from step S7 is fed into an intelligent homogenizer. The homogenizer adopts a biaxial stirring mode, with the stirring speed set at 700 r / min and the stirring time at 20 min. Inert gas protection is added during the stirring process. The inert gas is argon, with a flow rate of 25 L / min, to prevent the proppant from being oxidized during homogenization.

[0074] During the homogenization process, the intelligent monitoring system collects parameters such as particle size distribution, strength, coating thickness, and slow-release performance of the proppant in real time, taking samples for testing every 5 minutes to ensure that the coefficient of variation for particle size distribution does not exceed 0.05, strength does not exceed 0.06, coating thickness does not exceed 0.08, and slow-release performance does not exceed 0.07. If the coefficients of variation of any parameter exceed the set range, the stirring speed and stirring time of the homogenizer are adjusted to ensure uniformity of all proppant properties.

[0075] After homogenization, the proppant is fed into a vibrating screen for secondary screening. The screen aperture is the same as in step S1, screening out proppant particles with a diameter of 75-150 μm to remove excessively large and small particles, further improving the uniformity of the proppant. After screening, the proppant is transferred to an intelligent storage tank. The storage tank maintains a dry, inert gas-protected environment, with the temperature controlled at 25℃ and humidity controlled below 5% to prevent the proppant from absorbing moisture and oxidizing, which would affect its performance stability. The working principle of this step is to use mechanical stirring to fully mix the proppant particles, eliminating performance differences between particles. Secondary screening removes unqualified particles, ensuring that the various properties of the proppant are uniform and stable. This lays the foundation for subsequent performance testing and application, and avoids poor support effects in complex meshes due to performance inhomogeneity.

[0076] Step Nine: Intelligent Performance Detection and Screening

[0077] Intelligent performance testing and screening is a crucial step in ensuring the quality of proppant. Its purpose is to conduct comprehensive performance testing on the homogenized proppant, screening out qualified products and eliminating unqualified ones. This step relies on the homogenized proppant from step S8 to ensure that the test results accurately reflect the proppant's performance. During operation, the homogenized proppant from step S8 is removed from the storage tank and sent to the intelligent testing system. The system employs automated testing, covering multiple items including strength testing, suspension performance testing, temperature and salt resistance testing, slow-release performance testing, particle size distribution testing, and environmental performance testing. The entire testing process is automated, requiring no manual intervention, and the test data is uploaded to the intelligent control system in real time.

[0078] Strength testing was conducted using an intelligent impact testing machine to test the compressive strength and abrasion resistance of the proppant. The compressive strength was not less than 120 MPa, and the abrasion resistance was not less than 95%. Suspension performance testing was performed in a simulated fracturing fluid environment. Under a stirring speed of 500 r / min, the settling rate of the proppant after standing for 2 hours should not exceed 5%. Temperature and salt resistance testing was performed under simulated deep formation conditions. Under conditions of 200℃, 15 MPa, and a salinity of 2×10^4 mg / L, after soaking for 72 hours, the strength loss of the proppant should not exceed 10%. The suspension performance showed no significant change; the slow-release performance was tested using a simulated formation water environment, with a release rate not exceeding 30% in 24 hours, 60%-80% in 72 hours, and over 90% in 120 hours; the particle size distribution was measured using a laser particle size analyzer, with a particle size range of 75-150 μm and a coefficient of variation not exceeding 0.05; the environmental performance was tested using an ion chromatograph to detect the content of heavy metal ions in the proppant, with the content of heavy metal ions such as lead, cadmium, and mercury not exceeding 0.1 mg / kg, meeting the requirements for green environmental protection.

[0079] During the testing process, if any performance indicator fails to meet the requirements, the batch of proppant is deemed unqualified and sent to the recycling system for crushing and resynthesis. If all performance indicators meet the requirements, the product is deemed qualified and sent to the finished product storage tank for later use. After testing, the intelligent testing system automatically generates a test report, recording various performance parameters of the proppant for subsequent traceability and quality control. The working principle of this step is to comprehensively test the key performance of the proppant using automated testing equipment to ensure that qualified products can meet the requirements for fracturing in complex fractures, eliminate unqualified products, avoid affecting fracturing results due to product quality issues, and simultaneously achieve high efficiency and intelligence in the testing process, improving testing efficiency and accuracy.

[0080] Step 10: Intelligent Packaging and Storage of Finished Products

[0081] The final step in proppant synthesis is intelligent packaging and storage of the finished product. Its purpose is to standardize the packaging of qualified proppant, ensuring its stable performance during storage and transportation, unaffected by external environmental factors. This step relies on the proppant passing the inspection in step S9, ensuring that the quality of the packaged proppant remains intact. During operation, the qualified proppant from step S9 is fed into an intelligent packaging machine. The machine employs automatic metering and sealing, with a packaging specification of 25kg / bag and a metering accuracy controlled within ±0.1kg, ensuring consistent quality in each bag of proppant.

[0082] During the packaging process, a desiccant is placed inside the packaging bag at a rate of 50g per bag to absorb moisture and prevent the proppant from absorbing moisture. Simultaneously, a smart label is affixed to the packaging bag, containing information such as product name, specifications, production date, batch number, performance parameters, and shelf life for easy identification and traceability. After packaging, the bags are fed into an intelligent palletizer for automatic palletizing. The palletizing height is controlled at 10 layers, and compression of the bags is avoided during palletizing to prevent breakage of the proppant particles.

[0083] After stacking, the proppant is stored in a finished product warehouse. The warehouse is maintained in a dry, well-ventilated, and cool environment, with the temperature controlled at 20-25℃ and humidity below 5%, avoiding direct sunlight and high-temperature, humid conditions. An intelligent monitoring system is installed in the warehouse to monitor temperature, humidity, and the storage status of the proppant in real time. If environmental parameters exceed the set range, the control equipment is automatically activated for adjustment. The finished proppant has a shelf life of 12 months, with sampling tests conducted every 3 months during storage to ensure the proppant's performance stability. During transportation, sealed transport vehicles are used to prevent the proppant from getting damp or contaminated. Care is taken to handle the proppant with care during transport to prevent damage to the packaging bags and breakage of the proppant particles. The working principle of this step is to isolate the proppant's performance from the external environment through standardized packaging and intelligent storage, ensuring the proppant's performance stability during storage and transportation. This provides high-quality, qualified products for subsequent fracturing operations, ensuring the smooth progress of fracturing operations in complex fractures.

[0084] Example 1

[0085] This embodiment uses the method described above to prepare a multifunctional integrated complex suture support agent. The specific steps are as follows:

[0086] Step S1: Raw Material Pretreatment and Precise Screening. High-purity bauxite, quartz sand, magnesium oxide, and zirconium oxide were selected as basic aggregate raw materials, with bauxite accounting for 60% by mass, quartz sand 25% by mass, magnesium oxide 10% by mass, and zirconium oxide 5% by mass. γ-(methacryloyloxy)propyltrimethoxysilane was selected as the coupling agent, polyethyl acrylate and poly2-acrylamido-2-methyl-propane sulfonate were selected as functional coating materials, acetic acid was selected as the hydrolysis promoter, and deionized water was selected as the reaction medium. All raw materials were weighed using a precision balance with a weighing accuracy of 0.001g. Bauxite and quartz sand were coarsely crushed to 5-10 mm in a jaw crusher, then finely ground in a ball mill at 300 r / min for 2 hours with a ball-to-material ratio of 5:1. The ground material was then screened using a three-layer vibrating screen with mesh sizes of 100, 150, and 200 mesh, separating particles with a diameter of 75-150 μm. The screened material was then placed in a vacuum drying oven at 120℃ for 4 hours under a vacuum of 0.08 MPa to remove moisture. After drying, the material was activated in a plasma cleaner at 300 W for 15 minutes with an argon flow rate of 20 L / min. After activation, the particle size distribution variation coefficient was found to be 0.08, and the number of surface active groups was 6.2 × 10⁵ cells / cm². Once qualified, the material was transferred to a raw material storage tank for later use.

[0087] Step S2: Intelligent sintering reaction of basic aggregates. The qualified raw materials from Step S1 are fed into an intelligent sintering furnace at a feed rate of 5 kg / h, using a segmented temperature control mode: preheating section 400℃ for 30 min; heating section increasing temperature from 400℃ to 1200℃ at a rate of 10℃ / min, furnace pressure 0.1 MPa; isothermal section 1200℃ for 2 h; cooling section cooling to room temperature at a rate of 5℃ / min, nitrogen flow rate 30 L / min. After cooling, the aggregate compressive strength is tested to be 135 MPa, apparent density 2.7 g / cm³, and porosity 4.2%. After passing these tests, the aggregate is transferred to a modification reactor for later use.

[0088] Step S3: Aggregate surface coupling modification reaction and statistical optimization. The qualified basic aggregate from step S2 was sent to the intelligent modification reactor, deionized water was added, the mass ratio of aggregate to deionized water was 1:3, stirring was started at 400 r / min and stirred for 10 min. The coupling agent alcohol solution was prepared, with γ-(methacryloyloxy)propyltrimethoxysilane concentration of 8wt%, acetic acid added at 2% of the coupling agent mass, and anhydrous ethanol to deionized water volume ratio of 1:1. It was added to the reactor at a rate of 10 mL / min through an intelligent dropping device, and the pH value was adjusted to 4.5 during the dropping process. The reaction time was optimized using formula (1) and formula (2), and the optimal reaction time was calculated to be 35 min, the reaction temperature was 60℃, and the grafting rate was detected every 5 min during the reaction. The final grafting rate was 88%. After the reaction was completed, the mixture was centrifuged at 3000 r / min for 10 min to separate the excess coupling agent solution, and vacuum dried at 80℃ for 2 h. After the grafting rate was qualified, it was sent to the functional coating reactor for later use.

[0089] Step S4: Intelligent Formulation of Functional Coating Materials. Polyethyl acrylate and poly(2-acrylamido-2-methyl-propane sulfonate) were selected as the main functional coating materials in a mass ratio of 3:2. OP-10 was selected as the emulsifier, added at 4% of the total mass of the main functional coating materials. Acetic acid was selected as the hydrolysis accelerator, added at 3% of the total mass of the main functional coating materials. Deionized water was selected as the dispersion medium. Deionized water was fed into the intelligent formulation vessel, and stirring was started at 800 rpm. OP-10 was added and stirred for 15 minutes until dissolved. Then, polyethyl acrylate and poly(2-acrylamido-2-methyl-propane sulfonate) were added at a rate of 5 g / min. After addition, acetic acid was added dropwise to adjust the pH to 5.0, and stirring was continued for 30 minutes to form a uniform functional coating emulsion. The emulsion viscosity was measured to be 650 mPa·s, the particle size distribution was 120-180 nm, and no stratification was observed after standing for 24 hours. After passing the test, the emulsion was transferred to a storage tank for later use, with stirring maintained at 200 rpm during the storage process.

[0090] Step S5: Intelligent Coating Reaction and Statistical Optimization. The qualified modified aggregate from Step S3 was fed into an intelligent coating reactor, and the functional coating emulsion prepared in Step S4 was added at a mass ratio of 1:2. Stirring was started at 600 r / min to ensure uniform dispersion of the aggregate. The reaction temperature was 70℃, the pressure was 0.15 MPa, and ultrasonic-assisted coating was used at a power of 500 W and a frequency of 20 kHz. The reaction time was optimized using formulas (3) and (4), and the optimal reaction time was calculated to be 45 min. The coating layer thickness was checked every 5 min during the reaction, and the final coating layer thickness was 6.5 μm with a thickness variation coefficient of 0.06. After the reaction was completed, the mixture was centrifuged at 2500 r / min for 8 min to separate excess emulsion (for later use), and vacuum dried at 90℃ for 3 h. The coating layer bonding strength was checked, and the wear amount was 0.3%. After passing the test, the mixture was sent to the intelligent modification reactor for later use.

[0091] Step S6: Slow-release modification reaction. Polyacrylamide was selected as the slow-release water-blocking agent, polyethylene glycol as the dispersant, with a mass ratio of 5:1, and deionized water as the dispersion medium to prepare a 10wt% slow-release agent dispersion. The qualified coated support agent from step S5 was sent to the intelligent modification reactor, and the dispersion was added at a mass ratio of 1:1.5. Stirring was started at 500 r / min for 20 min. The reaction temperature was 65℃, the pressure was 0.12 MPa, and the reaction time was 30 min. The dispersion was replenished in real time during the reaction to maintain a stable concentration. After the reaction was completed, the mixture was centrifuged at 2000 r / min for 5 min to separate the excess dispersion, and then vacuum dried at 85℃ for 2.5 h. The slow-release performance was tested: 25% release at 24 h, 75% release at 72 h, and 92% release at 120 h. After passing the test, the mixture was sent to the intelligent temperature- and salt-resistant modification reactor for later use.

[0092] Step S7: Temperature and Salt Resistance Modification Reaction and Statistical Optimization. Organosilicon resin was selected as the temperature and salt resistance modifier, aminosilane as the crosslinking agent, with a mass ratio of 10:1, and anhydrous ethanol as the solvent to prepare a 12wt% temperature and salt resistance modification solution. The qualified slow-release modified proppant from step S6 was sent to the intelligent temperature and salt resistance modification reactor, and the modification solution was added at a mass ratio of 1:2.5. Stirring was started at 550 r / min for 15 min. The reaction temperature was 80℃, and the pressure was 0.18 MPa. The reaction time was optimized using formulas (5) and (6), and the optimal reaction time was calculated to be 50 min. The temperature and salt resistance performance was tested every 10 min during the reaction. The final temperature resistance limit was 210℃. After immersion in simulated formation water with a mineralization of 2×10^4 mg / L for 72 h, the strength loss was 8%. After the reaction is complete, centrifuge at 2800 r / min for 7 min to separate the excess modified solution, dry under vacuum at 100℃ for 3.5 h, and send it to an intelligent homogenizer for later use after passing the test.

[0093] Step S8: Intelligent Homogenization. The qualified temperature and salt resistant modified proppant from Step S7 is fed into an intelligent homogenizer, with biaxial stirring at 700 r / min for 20 min and argon flow rate of 25 L / min. Performance parameters are checked every 5 min during homogenization: particle size distribution coefficient of variation 0.04, strength coefficient of variation 0.05, coating thickness coefficient of variation 0.07, and slow-release performance coefficient of variation 0.06, all meeting requirements. After homogenization, the sample is sent to a vibrating screen for secondary screening. The screen aperture is the same as in Step S1, screening out particles with a diameter of 75-150 μm, which are then sent to an intelligent storage tank for later use. The storage tank is maintained at 25℃ and 4% humidity under inert gas protection.

[0094] Step S9: Intelligent Performance Testing and Screening. The proppant homogenized in Step S8 is fed into an intelligent testing system for comprehensive performance testing: compressive strength 132 MPa, abrasion resistance 96%; suspension performance: sedimentation rate 4% after 2 hours of standing; temperature and salt resistance: after immersion at 200℃, 15 MPa, and a mineralization of 2×10^4 mg / L for 72 hours, strength loss 8%, suspension performance no significant change; slow-release performance: release rate 25% after 24 hours, 75% after 72 hours, and 92% after 120 hours; particle size distribution 75-150 μm, coefficient of variation 0.04; environmental performance: heavy metal ion content is all below 0.1 mg / kg. All indicators meet the requirements, and the product is judged to be qualified and sent to the finished product storage tank for later use.

[0095] Step S10: Intelligent Packaging and Storage of Finished Products. The qualified proppant from Step S9 is fed into an intelligent packaging machine for automatic metering and sealing. The packaging specification is 25kg / bag, with a metering accuracy of ±0.1kg. 50g of desiccant is added to each bag, and a smart label is affixed with product information. After packaging, the product is automatically stacked in a 10-layer intelligent palletizing machine, and then stored in a finished product warehouse at a temperature of 22℃ and humidity of 4%. An intelligent monitoring system adjusts environmental parameters in real time. Samples are taken and tested every 3 months during storage. Performance remains stable, and the shelf life is 12 months.

[0096] The proppant prepared in this embodiment meets the requirements of complex fracture fracturing in all aspects, has good multi-functional synergy, stable and uniform performance, and can be adapted to complex fracture network environments with deep high temperature, high pressure and high mineralization, effectively improving oil and gas recovery rate. Moreover, the synthesis process is efficient, environmentally friendly and intelligent, with low production cost, and has good industrial application value.

[0097] Example 2

[0098] This embodiment uses the method described above to prepare a multifunctional integrated complex suture support agent. The specific steps are as follows:

[0099] Step S1: Raw Material Pretreatment and Precise Screening. High-purity bauxite, quartz sand, magnesium oxide, and zirconium oxide were selected as basic aggregate raw materials, with bauxite accounting for 65% by mass, quartz sand 20%, magnesium oxide 10%, and zirconium oxide 5%. γ-(methacryloyloxy)propyltrimethoxysilane was selected as the coupling agent, polyethyl acrylate and poly-2-acrylamido-2-methyl-propane sulfonate were selected as functional coating materials, acetic acid was selected as the hydrolysis promoter, and deionized water was selected as the reaction medium. All raw materials were weighed using a precision balance with a weighing accuracy of 0.001g. Bauxite and quartz sand were coarsely crushed to 5-10 mm in a jaw crusher, then finely ground in a ball mill at 300 r / min for 2.5 h with a ball-to-material ratio of 5:1. The ground material was then screened using a three-layer vibrating screen with mesh sizes of 100, 150, and 200 mesh, separating particles with a diameter of 75-150 μm. The screened material was then placed in a vacuum drying oven at 120℃ for 4 h under a vacuum of 0.08 MPa to remove moisture. After drying, it was activated in a plasma cleaner at 300 W for 18 min with an argon flow rate of 22 L / min. After activation, the particle size distribution variation coefficient was found to be 0.07, and the number of surface active groups was 5.8 × 10⁵ cells / cm². Once qualified, the material was transferred to a raw material storage tank for later use.

[0100] Step S2: Intelligent sintering reaction of basic aggregates. The qualified raw materials from Step S1 are fed into an intelligent sintering furnace at a feed rate of 5.5 kg / h, using a segmented temperature control mode: preheating section 400℃ for 35 min; heating section increasing temperature from 400℃ to 1250℃ at a rate of 10℃ / min, furnace pressure 0.1 MPa; isothermal section 1250℃ for 2.5 h; cooling section cooling to room temperature at a rate of 5℃ / min, nitrogen flow rate 32 L / min. After cooling, the aggregate compressive strength is tested to be 140 MPa, apparent density 2.75 g / cm³, and porosity 3.8%. After passing these tests, the aggregate is transferred to a modification reactor for later use.

[0101] Step S3: Aggregate surface coupling modification reaction and statistical optimization. The qualified basic aggregate from step S2 was sent to the intelligent modification reactor, deionized water was added, the mass ratio of aggregate to deionized water was 1:3, stirring was started at 400 r / min and stirred for 10 min. The coupling agent alcohol solution was prepared, with γ-(methacryloyloxy)propyltrimethoxysilane concentration of 8wt%, acetic acid added at 2% of the coupling agent mass, and anhydrous ethanol to deionized water volume ratio of 1:1. It was added to the reactor at a rate of 10 mL / min through an intelligent dropping device, and the pH value was adjusted to 4.5 during the dropping process. The reaction time was optimized using formula (1) and formula (2), and the optimal reaction time was calculated to be 35 min, the reaction temperature was 62℃, and the grafting rate was detected every 5 min during the reaction. The final grafting rate was 89%. After the reaction was completed, the mixture was centrifuged at 3000 r / min for 10 min to separate the excess coupling agent solution, and vacuum dried at 80℃ for 2 h. After the grafting rate was found to be qualified, it was sent to the functional coating reactor for later use.

[0102] Step S4: Intelligent Formulation of Functional Coating Materials. Polyethyl acrylate and poly(2-acrylamido-2-methyl-propane sulfonate) were selected as the main functional coating materials in a mass ratio of 3:2. OP-10 was selected as the emulsifier, added at 4% of the total mass of the main functional coating materials. Acetic acid was selected as the hydrolysis accelerator, added at 3% of the total mass of the main functional coating materials. Deionized water was selected as the dispersion medium. Deionized water was fed into the intelligent formulation vessel, and stirring was started at 800 rpm. OP-10 was added and stirred for 15 minutes until dissolved. Then, polyethyl acrylate and poly(2-acrylamido-2-methyl-propane sulfonate) were added at a rate of 5 g / min. After addition, acetic acid was added dropwise to adjust the pH to 5.0, and stirring was continued for 35 minutes to form a uniform functional coating emulsion. The emulsion viscosity was measured to be 700 mPa·s, the particle size distribution was 110-190 nm, and no stratification was observed after standing for 24 hours. After passing the test, the emulsion was transferred to a storage tank for later use, with stirring maintained at 200 rpm during the storage process.

[0103] Step S5: Intelligent Coating Reaction and Statistical Optimization. The qualified modified aggregate from Step S3 was fed into an intelligent coating reactor, and the functional coating emulsion prepared in Step S4 was added at a mass ratio of 1:2. Stirring was started at 600 r / min to ensure uniform dispersion of the aggregate. The reaction temperature was 72℃, the pressure was 0.15 MPa, and ultrasonic-assisted coating was used at a power of 500 W and a frequency of 20 kHz. The reaction time was optimized using formulas (3) and (4), and the optimal reaction time was calculated to be 45 min. The coating layer thickness was checked every 5 min during the reaction, and the final coating layer thickness was 7.0 μm with a thickness variation coefficient of 0.07. After the reaction was completed, the mixture was centrifuged at 2500 r / min for 8 min to separate excess emulsion (for later use), and then vacuum dried at 90℃ for 3 h. The coating layer bonding strength was checked, and the wear amount was 0.4%. After passing the test, the mixture was sent to the intelligent modification reactor for later use.

[0104] Step S6: Slow-release modification reaction. Polyacrylamide was selected as the slow-release water-blocking agent, polyethylene glycol as the dispersant, with a mass ratio of 5:1, and deionized water as the dispersion medium to prepare a 10wt% slow-release agent dispersion. The qualified coated support agent from step S5 was sent to the intelligent modification reactor, and the dispersion was added at a mass ratio of 1:1.5. Stirring was started at 500 r / min for 20 min. The reaction temperature was 68℃, the pressure was 0.12 MPa, and the reaction time was 30 min. The dispersion was replenished in real time during the reaction to maintain a stable concentration. After the reaction was completed, the mixture was centrifuged at 2000 r / min for 5 min to separate the excess dispersion, and then vacuum dried at 85℃ for 2.5 h. The slow-release performance was tested: 28% release at 24 h, 78% release at 72 h, and 93% release at 120 h. After passing the test, the mixture was sent to the intelligent temperature- and salt-resistant modification reactor for later use.

[0105] Step S7: Temperature and Salt Resistance Modification Reaction and Statistical Optimization. Organosilicon resin was selected as the temperature and salt resistance modifier, aminosilane as the crosslinking agent, with a mass ratio of 10:1, and anhydrous ethanol as the solvent to prepare a 12wt% temperature and salt resistance modification solution. The qualified slow-release modified proppant from step S6 was sent to the intelligent temperature and salt resistance modification reactor, and the modification solution was added at a mass ratio of 1:2.5. Stirring was started at 550 r / min for 15 min. The reaction temperature was 82℃, and the pressure was 0.18 MPa. The reaction time was optimized using formulas (5) and (6), and the optimal reaction time was calculated to be 50 min. The temperature and salt resistance performance was tested every 10 min during the reaction. The final temperature resistance limit was 215℃. After immersion in simulated formation water with a mineralization of 2×10^4 mg / L for 72 h, the strength loss was 7%. After the reaction is complete, centrifuge at 2800 r / min for 7 min to separate the excess modified solution, dry under vacuum at 100℃ for 3.5 h, and send it to an intelligent homogenizer for later use after passing the test.

[0106] Step S8: Intelligent Homogenization. The qualified temperature and salt resistant modified proppant from Step S7 is fed into an intelligent homogenizer, with biaxial stirring at 700 r / min for 22 min and argon flow rate of 25 L / min. Performance parameters are checked every 5 min during homogenization: particle size distribution coefficient of variation 0.04, strength coefficient of variation 0.05, coating thickness coefficient of variation 0.07, and slow-release performance coefficient of variation 0.06, all meeting requirements. After homogenization, the sample is sent to a vibrating screen for secondary screening. The screen aperture is the same as in Step S1, screening out particles with a diameter of 75-150 μm, which are then sent to an intelligent storage tank for later use. The storage tank is maintained at 25℃ and 4% humidity under inert gas protection.

[0107] Step S9: Intelligent Performance Testing and Screening. The proppant after homogenization in Step S8 is fed into an intelligent testing system for comprehensive performance testing: compressive strength 138 MPa, abrasion resistance 97%; suspension performance: sedimentation rate 3.5% after 2 hours of standing; temperature and salt resistance: after immersion at 200℃, 15 MPa, and a mineralization of 2×10^4 mg / L for 72 hours, strength loss is 7%, and suspension performance shows no significant change; slow-release performance: release rate 28% after 24 hours, 78% after 72 hours, and 93% after 120 hours; particle size distribution 75-150 μm, coefficient of variation 0.04; environmental performance: heavy metal ion content is all below 0.1 mg / kg. All indicators meet the requirements, and the product is judged to be qualified and sent to the finished product storage tank for later use.

[0108] Step S10: Intelligent Packaging and Storage of Finished Products. The qualified proppant from Step S9 is fed into an intelligent packaging machine for automatic metering and sealing. The packaging specification is 25kg / bag, with a metering accuracy of ±0.1kg. 50g of desiccant is added to each bag, and a smart label is affixed with product information. After packaging, the product is automatically stacked in a 10-layer intelligent palletizing machine, and then stored in a finished product warehouse at a temperature of 23℃ and humidity of 4%. An intelligent monitoring system adjusts environmental parameters in real time. Samples are taken and tested every 3 months during storage. Performance remains stable, and the shelf life is 12 months.

[0109] The proppant prepared in this embodiment has an appropriately increased bauxite ratio in the basic aggregate mix, and the sintering temperature and time have been optimized, which further improves the compressive strength and temperature resistance of the proppant. All properties are better than the design standard, making it suitable for deeper and more mineralized complex fracture network environments. The synthesis process is stable and controllable, and it is environmentally friendly and economical. This further verifies the feasibility and versatility of the method, and it is applicable to the fracturing needs of different deep and complex fractured oil and gas reservoirs.

[0110] This multifunctional integrated intelligent synthesis reaction method addresses numerous technical challenges in the field of proppant synthesis, achieving breakthroughs in several aspects and effectively solving core problems existing in current technologies. Firstly, it resolves the fragmentation and loose parameter connections in existing synthesis processes. In existing methods, steps such as basic aggregate preparation, surface modification, and functional coating are independent, lacking coordinated parameter control, leading to poor proppant performance consistency and significant batch-to-batch variations. This method organically connects ten steps, with each step providing a prerequisite for the next, and each subsequent step optimizing upon the previous one. Through an intelligent control system, it achieves coordinated parameter control across all steps, ensuring the uniformity of proppant performance and significantly reducing batch-to-batch variations. This resolves the contradiction between the high requirements for proppant performance uniformity in complex meshes and the difficulty of existing synthesis processes to meet these requirements. Secondly, this method addresses the problems of existing synthetic methods lacking precise and intelligent control and poor adaptability to complex fractured formation conditions. Existing methods mostly use fixed parameters to control the reaction process without dynamically adjusting based on raw material characteristics and target performance, and do not incorporate statistical and advanced mathematical tools for parameter optimization. This results in the synthesized proppant being difficult to adapt to complex formation conditions with high temperature, high pressure, and high mineralization in deep formations. This method introduces complex statistical models and calculus formulas in three key steps, and optimizes reaction parameters based on pre-experimental data, achieving precise and intelligent control of the reaction process. At the same time, through temperature and salt resistance modification and slow-release modification, the proppant can adapt to complex fractured formation conditions, solving the problems of proppant degradation, poor suspension performance, and poor water-blocking effect in deep and complex formations. Third, this method addresses the issue of insufficient synergy among existing proppant functions. Existing proppants often focus on optimizing a single function, making it difficult to simultaneously achieve multiple functions such as high strength, self-suspension, temperature and salt resistance, and slow release, thus failing to meet the comprehensive needs of complex fracture fracturing. This method, through multi-step synergistic effects including coupling modification, functional encapsulation, slow release modification, and temperature and salt resistance modification, enables the proppant to simultaneously possess multiple functions such as high strength, self-suspension, temperature and salt resistance, and slow release water shut-off, achieving multi-functional integration and solving the problem that single-function proppants cannot adapt to the comprehensive needs of complex fracture networks. Furthermore, it addresses the issues of low raw material utilization, high energy consumption, poor environmental performance, and delayed performance testing in existing synthesis methods. This method improves raw material utilization and reduces production costs through intelligent formulation and emulsion recycling; reduces energy consumption and waste gas and wastewater emissions through segmented temperature control and inert gas protection, meeting the requirements of green chemical development; and achieves real-time performance monitoring of the proppant through an intelligent online monitoring system, promptly screening out unqualified products and avoiding resource waste, solving the problems of delayed performance testing and inability to promptly handle unqualified products in existing methods. Meanwhile, this method also solves the problem of weak bonding and easy detachment of existing proppant functional layers. Through plasma activation, coupling modification and other steps, the bonding force between the layers is improved, ensuring the stability of proppant performance during fracturing and further improving the fracturing effect of complex fractures.

Claims

1. A multifunctional integrated intelligent synthetic reaction method, characterized in that, Includes the following steps: S1: Steps for raw material pretreatment and precise screening; S2: Step for intelligent sintering reaction of basic aggregates; S3: Step for surface coupling modification reaction and statistical optimization of aggregates; S4: Step for intelligent formulation of functional coating materials; S5: Step for intelligent coating reaction and statistical optimization. S6: Steps for performing sustained-release functional modification reactions; S7: Steps for performing temperature and salt resistance modification reactions and statistical optimization; S8: Steps for intelligent homogenization; S9: Steps for intelligent performance testing and screening; S10: Steps for intelligent packaging and storage of finished products.

2. The multifunctional integrated intelligent synthetic reaction method according to claim 1, characterized in that, Step S1 is described in detail as follows: Raw material pretreatment and precise screening are the foundation of intelligent synthesis of multifunctional integrated complex joint support agents. Its core purpose is to remove impurities from the raw materials, unify the particle size and activity of the raw materials, and provide a stable raw material basis for subsequent synthesis reactions. In operation, high-purity bauxite, quartz sand, magnesium oxide, and zirconium oxide are first selected as basic aggregate raw materials, γ-propyltrimethoxysilane is selected as a coupling agent, polyethyl acrylate and poly-2-acrylamido-2-methyl-propane sulfonate are selected as functional coating materials, acetic acid is selected as a hydrolysis promoter, and deionized water is selected as the reaction medium. All raw materials must be weighed using a precision balance, with the weighing accuracy controlled within 0.001g to ensure the accuracy of the raw material ratio. Weighed bauxite and quartz sand were coarsely crushed in a jaw crusher to a particle size of 5-10 mm. They were then fed into a ball mill for fine grinding at 300 r / min for 2 hours, with a ball-to-material ratio of 5:1 to ensure uniform particle size. The finely ground material was then screened using a three-layer vibrating screen with mesh sizes of 100, 150, and 200 mesh. Vibration screening separated particles with a size of 75-150 μm. This particle size range ensures both the strength of the proppant and improves its suspension performance in fracturing fluid. The screened material was then placed in a vacuum drying oven at 120℃ for 4 hours, with a vacuum level of 0.08 MPa to remove moisture and prevent it from affecting the stability of subsequent reactions. After drying, the raw materials are sent to a plasma cleaner for surface activation treatment. The power of the plasma cleaner is set to 300W, the treatment time is 15 minutes, and the working gas is argon with a flow rate of 20L / min. Plasma treatment can break the chemical bonds on the surface of the raw materials, increase the number of surface active groups, and improve the bonding ability of the raw materials with coupling agents and functional coating materials. After the treatment, the particle size distribution and surface activity of the raw materials are tested. The coefficient of variation of particle size distribution is controlled within 0.1, and the number of surface active groups is not less than 5×10^5 cells / cm². The raw materials that pass the test are sent to the raw material storage tank for later use. The unqualified raw materials are crushed, ground, screened, and activated again until they meet the requirements.

3. The multifunctional integrated intelligent synthetic reaction method according to claim 1, characterized in that, Step S2 is described in detail as follows: The intelligent sintering reaction of the basic aggregate is the core step in the preparation of high-strength proppant. Its purpose is to cause the raw material particles to melt and crystallize through high-temperature sintering, forming a dense and high-strength basic aggregate, which provides a good carrier for subsequent functional modification. During operation, the raw materials that have been processed in step S1 are first fed from the storage tank into the intelligent sintering furnace. The feeding rate is controlled at 5 kg / h by an intelligent flow controller to ensure uniform feeding. The sintering furnace adopts a segmented temperature control mode, which is divided into four stages: preheating stage, heating stage, constant temperature stage and cooling stage. The temperature and time of each stage are precisely controlled by an intelligent temperature control system, with the temperature control accuracy controlled within ±1℃. The preheating section is set at 400℃ for 30 minutes. The main purpose is to further remove residual moisture and volatile impurities from the raw materials, preventing pores from forming during high-temperature sintering and affecting the aggregate's density. After preheating, the heating section begins, with the heating rate set at 10℃ / min via an intelligent control system, increasing the temperature from 400℃ to 1200℃. During this process, the furnace temperature and pressure are monitored in real-time, with the furnace pressure controlled at 0.1 MPa to ensure a stable heating process and prevent sudden temperature increases that could cause raw material particles to crack. After reaching 1200℃, the section enters a constant-temperature phase, set at 1200℃ for 2 hours. During this phase, the bauxite, quartz sand, magnesium oxide, and zirconium oxide in the raw materials undergo a melting reaction, forming a glassy and crystalline phase. The particles bond together to form a dense aggregate structure. During the constant-temperature phase, the intelligent monitoring system collects real-time data on the aggregate's sintering density and crystallinity, adjusting the constant-temperature time and temperature based on feedback to ensure the aggregate's sintering quality. After isothermal sintering, the aggregate enters the cooling section at a rate of 5℃ / min, cooling from 1200℃ to room temperature. During the cooling process, inert gas protection is used, with nitrogen as the inert gas and a flow rate of 30L / min, to prevent the aggregate from being oxidized during cooling, which would lead to a decrease in strength. After cooling, the sintered aggregate is taken out and sent to an impact testing machine and a densitometer for performance testing. The compressive strength of the aggregate is not less than 120 MPa, the apparent density is controlled at 2.6-2.8 g / cm³, and the porosity is not higher than 5%. The qualified basic aggregate is sent to the modification reactor for later use. The unqualified aggregate is sintered again, and the sintering parameters are adjusted until the requirements are met.

4. The multifunctional integrated intelligent synthetic reaction method according to claim 1, characterized in that, The specific description of step S3 is as follows: The purpose of the aggregate surface coupling modification reaction is to form a coupling molecular layer on the aggregate surface through a coupling agent, thereby improving the hydrophilicity and reactivity of the aggregate surface and laying the foundation for subsequent functional coating reactions. At the same time, the reaction parameters are optimized through statistical methods and calculus formulas to ensure the stability and uniformity of the modification effect. In operation, the qualified basic aggregate from step S2 is first sent into the intelligent modification reactor, deionized water is added, and the mass ratio of aggregate to deionized water is controlled at 1:

3. The stirring device of the reactor is turned on, the stirring speed is set to 400 r / min, and the stirring time is 10 min, so that the aggregate is evenly dispersed in the deionized water. Subsequently, the prepared coupling agent alcohol solution was slowly added to the reaction vessel. The coupling agent alcohol solution consisted of γ-methacryloxypropyltrimethoxysilane, anhydrous ethanol, and acetic acid. The concentration of the coupling agent was 8 wt%, the amount of acetic acid added was 2% of the mass of the coupling agent, and the volume ratio of anhydrous ethanol to deionized water was 1:

1. The addition rate of the coupling agent alcohol solution was controlled at 10 mL / min by an intelligent dripping device. During the addition process, the pH value in the reaction vessel was monitored in real time, and the pH value was adjusted to 4.5 by adding acetic acid dropwise to ensure the smooth hydrolysis reaction of the coupling agent. The coupling modification reaction temperature was set at 60℃, and the reaction time was determined through statistical optimization. The optimal reaction time was calculated using a normal distribution model combined with calculus formulas to ensure that the grafting rate of the coupling agent on the aggregate surface was maximized. During the reaction process, the normal distribution function from statistics and integral operations from calculus are introduced to establish a model relating the grafting rate of the coupling agent to the reaction time, as shown in the following formula: ； In the formula: The coupling agent grafting rate (%) at time t; The reaction time is in minutes. The statistical standard deviation is 2.

3. The statistical mean is 35. The reaction rate constant is 0.015 min⁻¹. For integration variables; is the integration constant, with a value of 0.8; Taking the derivative of formula (1) and setting it to 0, the optimal reaction time can be obtained. The derivative is calculated as follows: ； The meanings of the symbols in the formula are consistent with those in formula (1). Solving formula (2) yields the optimal reaction time. The optimal reaction time was used for coupling modification. The grafting rate was monitored in real time during the reaction, and samples were taken every 5 minutes to ensure that the grafting rate was controlled between 85% and 90%. After the reaction was completed, the modified aggregate was sent to a centrifuge for separation at a speed of 3000 r / min for 10 minutes to separate excess coupling agent solution. Then, it was sent to a vacuum drying oven for drying at 80℃ for 2 hours to remove moisture and residual solvent from the surface of the aggregate. After drying, the surface grafting rate of the modified aggregate was tested. The modified aggregate that passed the test was sent to a functional coating reactor for later use, while the aggregate that failed the test was re-coupled and modified.

5. The multifunctional integrated intelligent synthetic reaction method according to claim 1, characterized in that, Step S4 is specifically described as follows: Intelligent formulation of functional coating materials is a key step in realizing the multifunctionality of proppant. Its purpose is to formulate a functional coating emulsion with stable performance and good compatibility with modified aggregates, so as to provide high-quality coating materials for subsequent coating reactions. In operation, polyethyl acrylate and poly-2-acrylamido-2-methyl-propane sulfonate are selected as the main functional coating materials, and the mass ratio of the two is controlled at 3:

2. OP-10 is selected as the emulsifier, and the amount of emulsifier added is 4% of the total mass of the main functional coating materials. Acetic acid is selected as the hydrolysis promoter, and the amount added is 3% of the total mass of the main functional coating materials. Deionized water is selected as the dispersion medium. Deionized water was fed into the intelligent preparation vessel, and the stirring device was turned on. The stirring speed was set to 800 r / min. Emulsifier OP-10 was added to the deionized water and stirred for 15 min to completely dissolve the emulsifier and form a uniform emulsion system. Subsequently, polyethyl acrylate and poly2-acrylamido-2-methyl-propane sulfonate were slowly added to the preparation vessel according to the set ratio. The addition rate was controlled at 5 g / min. During the addition process, the mixture was continuously stirred to ensure that the main ingredients were uniformly dispersed in the emulsion system. After the addition is complete, acetic acid is slowly added dropwise to the preparation vessel, the pH of the system is adjusted to 5.0, and stirring is continued for 30 minutes to fully emulsify the system and form a uniform functional coated emulsion. During the preparation process, the intelligent monitoring system collects real-time data on the viscosity, particle size distribution, and stability of the emulsion. The viscosity is controlled at 500-800 mPa·s, the particle size distribution range is 100-200 nm, and the stability is judged by the absence of stratification after standing for 24 hours. If the emulsion viscosity is too high, deionized water is added to adjust it; if the viscosity is too low, the amount of functional coating material is increased to adjust it; if the particle size distribution does not meet the requirements, the stirring speed and emulsification time are adjusted. After preparation, the functional coating emulsion is sent to a storage tank for later use. During the later use, the stirring speed is maintained at 200 r / min to avoid emulsion stratification.

6. The multifunctional integrated intelligent synthetic reaction method according to claim 1, characterized in that, The specific description of step S5 is as follows: The intelligent coating reaction involves uniformly coating the surface of the modified aggregate with a functional coating emulsion to form a functional layer, thereby realizing the multifunctionality of the proppant. At the same time, the coating parameters are optimized through statistical methods and calculus formulas to ensure that the coating layer has a uniform thickness and a strong bond. During operation, the qualified modified aggregate from step S3 is first fed into the intelligent coating reaction vessel, and the functional coating emulsion prepared in step S4 is added. The mass ratio of modified aggregate to functional coating emulsion is controlled at 1:

2. The stirring device of the reaction vessel is turned on, and the stirring speed is set to 600 r / min to make the modified aggregate uniformly dispersed in the emulsion. The coating reaction temperature was set to 70℃ using an intelligent temperature control system, and the reaction pressure was controlled at 0.15MPa. Ultrasonic-assisted coating was used during the reaction process, with the ultrasonic power set to 500W and the ultrasonic frequency at 20kHz. The vibration of the ultrasonic waves promoted the uniform adhesion of the functional coating material to the aggregate surface, improving the density and bonding strength of the coating layer. The coating reaction time was determined through statistical optimization. The optimal coating time was calculated using a Poisson distribution model combined with calculus formulas to ensure that the coating layer thickness was uniform and met the set requirements. During the reaction process, the Poisson distribution function from statistics and the differential operation from calculus are introduced to establish a model relating the coating thickness to the reaction time, as shown in the following formula: ； In the formula: The thickness of the coating layer at time t (μm); The reaction time is in minutes. The value of 4.8 represents the Poisson distribution parameter (characterized by the average rate of the coating reaction, obtained from preliminary experimental data). For integration variables; x is the factorial of x, which is the product of all positive integers from 1 to x, used for calculating the probability of the Poisson distribution; The coating rate constant is 0.03 μm / min; The initial coating thickness is set to 0.5 μm. Taking the derivative of formula (3), we obtain the relationship between the coating rate and time. Let the time when the coating rate reaches a stable value be the optimal reaction time. The derivative is calculated as follows: ； In the formula: To stabilize the coating rate, a value of 0.025 μm / min was used; t is the factorial of t, i.e., the product of all positive integers from 1 to t, used for calculating the Poisson distribution probability; the meanings of the other symbols are consistent with those in formula (3), and the optimal reaction time can be obtained by solving formula (4). The coating reaction was carried out according to the optimal reaction time. The coating thickness was monitored in real time during the reaction, and samples were taken every 5 minutes to ensure that the coating thickness was controlled between 5-8 μm and the coefficient of variation of the thickness did not exceed 0.

08. After the reaction is complete, the coated proppant is sent to a centrifuge for separation. The centrifugation speed is 2500 r / min and the centrifugation time is 8 min. The excess functional coated emulsion is separated out. The emulsion can be recycled and reused, reducing production costs. After separation, the proppant is placed in a vacuum drying oven at 90°C for 3 hours to remove moisture from the surface of the proppant and allow the coating layer to solidify. After drying, the thickness and bonding strength of the proppant coating layer are tested. The bonding strength is tested by a friction and wear test, and the wear amount does not exceed 0.5%. Proppant that passes the test is placed in an intelligent modification reactor for later use, while proppant that fails the test is re-coated.

7. The multifunctional integrated intelligent synthetic reaction method according to claim 1, characterized in that, Step S6 is described in detail as follows: The slow-release functional modification reaction adds slow-release water-blocking function to the proppant, enabling it to slowly release the water-blocking agent during complex fracture fracturing, sealing the water phase channels in the fracture and improving oil and gas recovery. This step is based on the proppant coated in step S5, ensuring that the slow-release agent can be uniformly adhered to the surface of the coating layer. In operation, polyacrylamide is first selected as the slow-release water-blocking agent, and polyethylene glycol is selected as the dispersant. The mass ratio of polyacrylamide to polyethylene glycol is controlled at 5:

1. Deionized water is selected as the dispersion medium to prepare the slow-release agent dispersion. The concentration of the slow-release agent is 10 wt%. The qualified coated proppant from step S5 is fed into the intelligent modification vessel, and a slow-release agent dispersion is added. The mass ratio of proppant to dispersion is controlled at 1:1.

5. The stirring device of the modification vessel is turned on, the stirring speed is set to 500 r / min, and the stirring time is 20 min to ensure that the proppant is uniformly dispersed in the dispersion. The modification reaction temperature is set to 65℃, and the reaction pressure is controlled at 0.12 MPa. During the reaction, the concentration change of the reaction system is monitored in real time, and the slow-release agent dispersion is replenished through an intelligent dripping device to ensure that the system concentration remains stable. The principle of the slow-release functional modification reaction is to utilize the water solubility and cross-linking properties of polyacrylamide to attach the slow-release agent to the surface of the support layer through physical adsorption and chemical bonding, forming a slow-release layer. Polyethylene glycol, as a dispersant, can prevent the slow-release agent from agglomerating and ensure that the slow-release agent is uniformly dispersed on the surface of the support. The reaction time is set to 30 min. After the reaction is completed, the support is sent to a centrifuge for separation at a speed of 2000 r / min for 5 min to separate the excess dispersion. Then, it is sent to a vacuum drying oven for drying at a temperature of 85℃ for 2.5 h to solidify the slow-release layer. After drying, the slow-release performance of the proppant is tested. The test method is to put the proppant into simulated formation water and measure the release amount of the slow-release agent at different times under the conditions of 90℃ and 15MPa. The requirements are that the release amount should not exceed 30% in 24h, reach 60%-80% in 72h, and reach more than 90% in 120h to ensure that the slow-release effect meets the design requirements. The proppant that passes the test is sent to the intelligent screening machine for use, and the proppant that fails the test is re-subjected to slow-release function modification reaction.

8. The multifunctional integrated intelligent synthetic reaction method according to claim 1, characterized in that, Step S7 is specifically described as follows: The temperature and salt resistance modification reaction is a key step in improving the stability of proppant in high-temperature and high-salinity formations. Its purpose is to form a temperature and salt resistance layer on the surface of the proppant to prevent performance degradation of the proppant under complex formation conditions. This step is based on the proppant modified by slow release in step S6, ensuring that the temperature and salt resistance layer can be well bonded to the slow release layer. In operation, firstly, organosilicon resin is selected as the temperature and salt resistance modifier, and aminosilane is selected as the crosslinking agent. The mass ratio of organosilicon resin to aminosilane is controlled at 10:

1. Anhydrous ethanol is selected as the solvent to prepare the temperature and salt resistance modification solution. The concentration of the modifier is 12 wt%. The qualified slow-release modified proppant from step S6 is fed into an intelligent temperature and salt resistant modification reactor. A temperature and salt resistant modification solution is added, with the proppant to modification solution mass ratio controlled at 1:2.

5. The stirring device is turned on, the stirring speed is set to 550 r / min, and the stirring time is 15 min, ensuring the proppant is uniformly dispersed in the modification solution. The modification reaction temperature is set to 80℃, and the reaction pressure is controlled at 0.18 MPa. Constant temperature and pressure control is used during the reaction to ensure stable reaction. The temperature and salt resistant modification reaction time is determined through statistical optimization, using an exponential distribution model combined with calculus to calculate the optimal reaction time, ensuring the optimal performance of the temperature and salt resistant layer. During the reaction process, the exponential distribution function from statistics and integral operations from calculus are introduced to establish a model relating the temperature resistance and salt resistance of the heat- and salt-resistant layer to the reaction time. The formula is as follows: ; In the formula: The temperature resistance limit (°C) of the temperature and salt resistance layer at time t. The reaction time is in minutes. The parameter is the exponential distribution parameter, with a value of 0.02 min⁻¹; For integration variables; The basic temperature resistance constant is set at 150℃. The temperature resistance increase coefficient is set to 0.8℃ / min. The initial temperature limit is set at 120℃. Taking the derivative of formula (5), and letting the time when the growth rate of the temperature limit reaches a stable value be the optimal reaction time, the derivative is calculated as follows: ； In the formula: The stable growth rate of the temperature resistance limit is taken as 0.5℃ / min (determined by design requirements); the meanings of the other symbols are consistent with those in formula (5), and the optimal reaction time can be obtained by solving formula (6). min; The temperature and salt resistance modification reaction was carried out according to the optimal reaction time. The temperature resistance limit and salt resistance performance of the temperature and salt resistance layer were monitored in real time during the reaction. Samples were taken and tested every 10 min. The temperature resistance limit was not lower than 200℃. After soaking in simulated formation water with a salinity of 2×10^4 mg / L for 72 h, the proppant strength loss did not exceed 10%. After the reaction is complete, the proppant is sent to a centrifuge for separation at a speed of 2800 r / min for 7 min to remove excess modified solution. It is then sent to a vacuum drying oven for drying at 100℃ for 3.5 h to solidify the temperature and salt resistance layer. After drying, the temperature and salt resistance properties of the proppant are comprehensively tested. Proppant that passes the test is sent to an intelligent homogenizer for later use, while proppant that fails the test undergoes a second temperature and salt resistance modification reaction. The specific description of step S8 is as follows: The purpose of intelligent homogenization is to homogenize the performance of the proppant, eliminate performance differences between batches and particles, and ensure that the proppant can be evenly laid and play a stable supporting role during complex fracture fracturing. This step is based on the temperature and salt resistant modified proppant in step S7, ensuring that the homogenization process does not damage the functional layer of the proppant. During operation, the qualified temperature and salt resistant modified proppant in step S7 is fed into the intelligent homogenizer. The homogenizer adopts a dual-shaft stirring mode, the stirring speed is set to 700 r / min, the stirring time is 20 min, and an inert gas is added for protection during the stirring process. The inert gas is argon, and the argon flow rate is 25 L / min to prevent the proppant from being oxidized during the homogenization process. During the homogenization process, the intelligent monitoring system collects the particle size distribution, strength, coating thickness, and slow-release performance parameters of the proppant in real time, taking samples and testing every 5 minutes to ensure that the coefficient of variation of the particle size distribution does not exceed 0.05, the coefficient of variation of the strength does not exceed 0.06, the coefficient of variation of the coating thickness does not exceed 0.08, and the coefficient of variation of the slow-release performance does not exceed 0.

07. If the coefficient of variation of the parameters exceeds the set range, the stirring speed and stirring time of the homogenizer are adjusted to ensure that the various properties of the proppant are uniform. After homogenization, the proppant is sent to a vibrating screen for secondary screening. The screen aperture is the same as in step S1, and proppant particles with a diameter of 75-150μm are screened out to remove excessively large and small particles, thereby further improving the uniformity of the proppant. After screening, the proppant is sent to an intelligent storage tank. The storage tank is kept in a dry environment with inert gas protection, the temperature is controlled at 25℃, and the humidity is controlled below 5% to avoid moisture absorption and oxidation of the proppant, which would affect its performance stability.

9. The multifunctional integrated intelligent synthetic reaction method according to claim 1, characterized in that, Step S9 is described in detail as follows: Intelligent performance testing and screening is a key step to ensure the quality of the proppant. Its purpose is to conduct comprehensive performance testing on the homogenized proppant, screen out qualified products, and eliminate unqualified products. This step is based on the homogenized proppant in step S8 to ensure that the test results can truly reflect the performance of the proppant. During operation, the homogenized proppant in step S8 is taken out of the storage tank and sent to the intelligent testing system. The testing system adopts an automated testing mode, covering multiple items such as strength testing, suspension performance testing, temperature and salt resistance testing, slow release performance testing, particle size distribution testing, and environmental performance testing. The testing process is fully automated and requires no manual intervention. The test data is uploaded to the intelligent control system in real time. The specific description of step S10 is as follows: Intelligent packaging and storage of finished products is the last step in proppant synthesis. Its purpose is to standardize the packaging of qualified proppant to ensure that the proppant's performance is stable during storage and transportation and is not affected by the external environment. This step is based on the premise that the proppant has passed the test in step S9, ensuring that the quality of the packaged proppant is not damaged. During operation, the proppant that has passed the test in step S9 is sent into the intelligent packaging machine. The packaging machine adopts an automatic metering and automatic sealing mode, with a packaging specification of 25kg / bag and a metering accuracy controlled within ±0.1kg to ensure that the quality of each bag of proppant is consistent. Strength testing employed an intelligent impact testing machine to measure the compressive strength and abrasion resistance of the proppant. The compressive strength was no less than 120 MPa, and the abrasion resistance was no less than 95%. Suspension performance testing was conducted in a simulated fracturing fluid environment. Under a stirring speed of 500 r / min, the settling rate of the proppant after standing for 2 hours did not exceed 5%. Temperature and salt resistance testing was performed under simulated deep formation conditions. At 200℃, 15 MPa, and a salinity of 2 × 10^4 mg / L, after immersion for 72 hours, the strength loss of the proppant did not exceed 10%. The suspension performance showed no significant change; the slow-release performance was tested using a simulated formation water environment, with a release rate not exceeding 30% in 24 hours, 60%-80% in 72 hours, and over 90% in 120 hours; particle size distribution was measured using a laser particle size analyzer, with a particle size range of 75-150 μm and a coefficient of variation not exceeding 0.05; environmental performance was tested using an ion chromatograph to detect the content of heavy metal ions in the proppant, with lead, cadmium, and mercury ion contents all not exceeding 0.1 mg / kg, meeting green environmental protection requirements; During the testing process, if any performance indicator fails to meet the requirements, the batch of proppant is deemed unqualified and sent to the recycling system for crushing and resynthesis. If all performance indicators meet the requirements, the product is deemed qualified and sent to the finished product storage tank for later use. After the testing is completed, the intelligent testing system automatically generates a test report, recording various performance parameters of the proppant for subsequent traceability and quality control. The working principle of this step is to use automated testing equipment to comprehensively test various key performance aspects of the proppant, ensuring that qualified products can meet the requirements for use in complex fracture fracturing, rejecting unqualified products to avoid affecting the fracturing effect due to product quality issues, and simultaneously achieving high efficiency and intelligence in the testing process, improving testing efficiency and accuracy. During the packaging process, a desiccant is placed inside the packaging bag at a rate of 50g per bag to absorb moisture and prevent the proppant from absorbing moisture. Simultaneously, a smart label is affixed to the packaging bag, containing the product name, specifications, production date, batch number, performance parameters, and shelf-life information for easy identification and traceability. After packaging, the bags are fed into a smart palletizer for automatic palletizing. The palletizing height is controlled at 10 layers, and the packaging bags are prevented from being squeezed during palletizing to avoid breakage of the proppant particles. After palletizing, the proppant is sent to the finished product warehouse for storage. The warehouse is kept in a dry, ventilated, and cool environment, with the temperature controlled at 20-25℃ and the humidity controlled below 5%, avoiding direct sunlight and high temperature and humidity. The warehouse is equipped with an intelligent monitoring system to monitor the temperature, humidity, and storage status of the proppant in real time. If the environmental parameters exceed the set range, the control equipment will be automatically activated to make adjustments. At the same time, the storage period of the finished proppant is set at 12 months, and sampling tests are conducted every 3 months during the storage process to ensure the stability of the proppant's performance. During transportation, sealed transport vehicles are used to prevent the proppant from getting damp or contaminated. The proppant is handled with care during transportation to prevent damage to the packaging bags and breakage of the proppant particles.

10. A multifunctional integrated intelligent synthesis reaction system, characterized in that... The multifunctional integrated intelligent synthesis reaction method as described in claims 1 to 9 is used.

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