Production system for preparing two-dimensional aromatic polyamide based on liquid phase loop tube

Abstract

The invention provides a production system for preparing two-dimensional aromatic polyamide based on a liquid-phase loop tube, and relates to the technical field of two-dimensional aromatic polyamide production, and the production system comprises a loop tube core reaction module used for carrying out a two-dimensional aromatic polyamide polycondensation reaction through a loop tube reactor; the intelligent regulation and control module is used for monitoring operation parameters of the ring pipe core reaction module in real time and generating a reaction parameter regulation and control instruction and a heat dissipation optimization strategy. Strong turbulent flow is generated in the loop reactor through high-speed circulating flow of the axial flow pump, continuous and uniform shearing and mixing are provided for reaction materials, a retention area possibly formed by high-viscosity fluid can be effectively broken, full contact of monomers, oligomers and growing two-dimensional lamellas is ensured, the mass transfer efficiency is improved, and the mass transfer efficiency is improved. Non-uniform local concentration and a reaction dead zone are avoided; dynamic optimization and safety interlocking protection of reaction parameters are realized by combining a kinetic model, so that the reaction controllability is improved, the production risk is reduced, and the product conversion rate and the molecular weight stability are guaranteed.

Description

Technical Field

[0001] This invention relates to the field of two-dimensional polyarylamide production technology, and in particular to a production system for preparing two-dimensional polyarylamide based on a liquid-phase loop. Background Technology

[0002] Two-dimensional polyarylamides (2DPAs), as an emerging two-dimensional polymer material, exhibit great application potential in fields such as flexible electronics, high-performance separation membranes, and advanced composite materials due to their unique two-dimensional planar topology, ultra-high mechanical strength, excellent gas barrier properties, and good chemical stability. Their synthesis typically involves interfacial or solution polycondensation reactions of multifunctional aromatic monomers.

[0003] However, like all two-dimensional polymers, the synthesis of 2DPA faces a core challenge: as the polymerization reaction proceeds, the formation of the two-dimensional network structure leads to an exponential increase in the system viscosity, rapidly transitioning from a low-viscosity solution to a high-viscosity state or even a gel state. This characteristic poses a severe challenge to traditional reactors.

[0004] In laboratory settings, batch reactors are typically used for small-batch synthesis. However, as the reaction scales up, the "scale-up effect" of traditional batch reactors becomes apparent: reactor volume (V∝r) increases significantly. 3 The increase in mass and heat transfer surface area (A∝r) is much faster than that in mass and heat transfer surface area (A∝r). 2 The increase in viscosity leads to a sharp decrease in specific surface area (A / V). For a system like 2DPA, which may lose its fluidity due to a viscosity spike in the middle of the reaction, the mechanical stirring of the batch reactor becomes completely ineffective after scale-up, resulting in uneven mixing, deteriorated heat transfer, local overheating, and exacerbated side reactions, ultimately causing the reaction to terminate prematurely, resulting in low molecular weight products and poor batch stability.

[0005] Microfluidic reactor technology, due to its extremely high specific surface area, provides excellent mass and heat transfer efficiency and is theoretically suitable for rapid mixing and strongly exothermic reactions. However, its direct application to the entire synthesis of 2DPA has inherent drawbacks: the extremely high viscosity in the later stages of the reaction leads to extremely high pressure drops in the micron-scale channels, easily causing blockage, and the pressure head requirements of the feed pump are extremely stringent, making continuous and stable industrial production difficult to achieve. A simple microreactor approach lacks the necessary operational flexibility and engineering feasibility to handle the viscosity changes throughout the entire 2DPA synthesis process.

[0006] Loop reactors, as a mature and widely used device in the chemical industry, have advantages such as simple structure, large production capacity per unit volume, good heat transfer, and internal flow close to plug flow. Its core component—the axial flow pump—provides continuous circulation power for the reaction fluid, enhancing mixing and mass transfer. Computational fluid dynamics (CFD) studies show that in loop reactors, high circulation velocities contribute to uniform particle distribution in straight sections, although some non-uniformity may occur in curved sections due to centrifugal force.

[0007] The synthesis of two-dimensional polyarylamide materials in the existing technology faces difficulties in mass and heat transfer due to the dramatic increase in viscosity, long reaction cycle, low molecular weight of product, poor batch stability, and difficulty in large-scale scale-up. Summary of the Invention

[0008] This invention provides a production system for preparing two-dimensional polyarylamides based on a liquid-phase loop, which solves the problem of drastic viscosity increase in the synthesis of two-dimensional polyarylamide materials in the prior art.

[0009] On one hand, this invention provides a production system for preparing two-dimensional polyarylamides based on a liquid-phase loop reactor, comprising: a raw material processing module, a loop reactor core reaction module, an intelligent control module, a product separation module, a product purification module, and a product drying module; the raw material processing module is used to process the aromatic monomers and feed liquid required for the synthesis of two-dimensional polyarylamides; the loop reactor core reaction module is used to carry out the polycondensation reaction of two-dimensional polyarylamides through the loop reactor, outputting a primary two-dimensional polyarylamide mixture; the intelligent control module is used to monitor the operating parameters of the loop reactor core reaction module in real time, and generate reaction parameter control instructions and heat dissipation optimization strategies; the product separation module is used to perform solid-liquid separation on the primary two-dimensional polyarylamide mixture, outputting a solid two-dimensional polyarylamide mixture; the product purification module is used to purify the solid two-dimensional polyarylamide mixture and recover the solvent, obtaining high-purity two-dimensional polyarylamides and recovered solvent; the product drying module is used to remove residual moisture and solvent from the high-purity two-dimensional polyarylamides, outputting dried two-dimensional polyarylamides.

[0010] According to the present invention, a production system for preparing two-dimensional polyaromatic amides based on a liquid-phase loop reactor is provided. The core reaction module of the loop reactor includes a feeding unit, a loop reactor, an axial flow pump, a temperature control unit, and a discharge unit. The feeding unit is used to receive aromatic monomers and feed liquid and output a mixture. The loop reactor is used for the polycondensation reaction of the mixture. The axial flow pump is used to continuously circulate the mixture in the loop reactor. The temperature control unit is used to regulate the internal temperature of the loop reactor. The discharge unit is used to continuously or intermittently extract the primary two-dimensional polyaromatic amide mixture.

[0011] According to the present invention, a production system for preparing two-dimensional polyarylamide based on a liquid-phase loop reactor is provided. The steps of the two-dimensional polyarylamide polycondensation reaction in the loop reactor core reaction module include:

[0012] Prepare the first feed solution and the second feed solution.

[0013] Close the discharge valve of the discharge unit, pressurize the loop reactor with nitrogen to 0.2 MPa, maintain the pressure and then release the pressure. Repeat this process three times to remove oxygen from the loop reactor.

[0014] Dry N-methylpyrrolidone solvent is injected into the loop reactor, the initial speed of the axial flow pump is set, and the temperature inside the loop reactor is preheated to the preset temperature through the temperature control unit.

[0015] Start the metering pump to pump the first and second feed liquids into the loop reactor at a constant flow rate, and control the total residence time of the mixture.

[0016] The mixture is circulated at high speed in the loop reactor under the drive of an axial flow pump to carry out a polycondensation reaction.

[0017] After the system is running stably, open the discharge valve to continuously draw out the primary two-dimensional polyaramid mixture at a flow rate that is the same as the total volumetric flow rate of the feed.

[0018] According to the present invention, a production system for preparing two-dimensional polyarylamide based on a liquid-phase loop reactor is provided. The intelligent control module includes an online monitoring unit, a central control unit, and a safety interlock unit. The online monitoring unit is used to monitor the key operating parameters of the core reaction module of the loop reactor in real time. The central control unit is used to analyze the data based on the key operating parameters through a preset two-dimensional polyarylamide polycondensation reaction kinetic model, and dynamically generate reaction parameter control instructions and heat dissipation optimization strategies. The safety interlock unit is used to verify the reaction parameter control instructions and simultaneously monitor the key operating parameters. When the preset safety threshold is exceeded, the interlock protection action is automatically triggered.

[0019] According to the production system for preparing two-dimensional polyarylamide based on a liquid-phase loop provided by the present invention, the steps for constructing the kinetic model of the polycondensation reaction of two-dimensional polyarylamide in the central control unit include:

[0020] Design multiple orthogonal experiments, using the temperature inside the loop reactor, the molar ratio of aromatic monomers, the residence time of the mixture, and the circulation flow rate as variables, to conduct two-dimensional polyaramid polycondensation reaction experiments within the preset variable range, and output experimental datasets.

[0021] Based on experimental datasets and the stepwise polymerization characteristics of polycondensation reactions, assuming that the reaction system is a homogeneous reaction and neglecting interfacial mass transfer resistance, the key reaction steps in the formation of two-dimensional polyarylamides are identified, and the reaction mechanism hypothesis is output.

[0022] Based on the reaction mechanism assumption, and with the law of conservation of mass and the basic principles of reaction kinetics as the core, an initial kinetic equation is established.

[0023] Based on the experimental dataset and the initial dynamic equation, the unknown parameters are fitted using the least squares method to obtain the initial parameter values. The reliability of the fit is verified by residual analysis. If the residual exceeds the preset range, the model assumptions are adjusted or the fitting algorithm is optimized and the fitting is repeated until the residual meets the requirements. Finally, the corrected dynamic equation is output.

[0024] Based on the experimental dataset, the experimental conditions are substituted into the modified kinetic equation to calculate the theoretical values ​​of monomer conversion and polymer molecular weight distribution. The deviation between the theoretical values ​​and the experimentally measured values ​​is compared to output the static reaction kinetic equation.

[0025] By combining the static reaction kinetic equations with the flow model of the loop reactor, and adapting to the continuous operation characteristics of the liquid-phase loop reactor based on the circulation flow rate, a two-dimensional polyaramid polycondensation reaction kinetic model is output.

[0026] According to the present invention, a production system for preparing two-dimensional polyarylamide based on a liquid-phase loop tube includes the following steps for verifying the reliability of the fit through residual analysis:

[0027] Based on the key response values ​​of the prototype experimental points in the experimental dataset and the corresponding predicted values ​​obtained by fitting the initial dynamic equation, the residual of each experimental point is calculated, and the original residual dataset is output.

[0028] Perform statistical calculations on the original residual dataset to obtain the residual mean. Determine whether the residual mean is close to 0. If the residual mean deviates from 0 and exceeds a preset threshold, it is preliminarily determined that there is a systematic bias in the fitting results. Output the statistical analysis results and the preliminary bias determination conclusion.

[0029] Based on the original residual dataset, a residual frequency histogram and a normal probability plot are drawn. The residuals at the experimental points are analyzed to determine whether they conform to an approximate normal distribution. The results of the distribution pattern analysis and the conclusion of the distribution conformity judgment are output.

[0030] Based on the original residual dataset, corresponding predicted values, and experimental dataset, we analyze whether there is a significant linear or periodic trend in the residuals at the experimental points, and output a trend conformity judgment conclusion.

[0031] Based on the original residual dataset and residual standard deviation as input, the 3σ criterion is used to identify abnormal residuals. For the experimental points corresponding to abnormal residuals, the standardization of experimental operation, the accuracy of detection instruments and the accuracy of data recording are checked, and the corrected residual dataset and the conclusion of abnormality handling are output.

[0032] Using the preliminary deviation judgment conclusion, distribution conformity judgment conclusion, trend conformity judgment conclusion, and anomaly handling conclusion as joint inputs, if the four conditions are met—the residual mean is close to 0, the residual conforms to a normal distribution, the residual has no significant trend, and the proportion of abnormal residuals is <5%—then the fit is considered reliable. If any condition is not met, the residual is considered to exceed the preset range, the final conclusion of the fit reliability is output, and the model optimization instruction is triggered simultaneously.

[0033] According to the production system for preparing two-dimensional polyarylamide based on a liquid-phase loop tube provided by the present invention, the step of verifying the reaction parameter control command of the safety interlock unit includes:

[0034] Based on the safe operating boundary of the two-dimensional polyarylamide condensation reaction and the rated operating parameters of the equipment, a standardized verification checklist is formed by presetting the safe threshold range, upper limit of the control amplitude, and parameter linkage rules for each control parameter.

[0035] Based on the reaction parameter control instructions and the classification criteria of the control objects in the standardized verification list, the control objects, target control parameter values ​​and control rates in the instructions are analyzed, classified and entered into the verification module, and the parsed parameter set is output.

[0036] Using the parsed parameter set as the verification object, the target value of each parameter is compared with the safety threshold range one by one. At the same time, it is determined whether the control range exceeds the limit in the standardized verification list, and the single parameter verification result set is output.

[0037] Extract the associated parameters from the parsed parameter set, verify the rationality of the control logic between the associated parameters based on the parameter linkage rules, and output the linkage verification results.

[0038] Based on the single-parameter verification result set and the linkage verification result, the control command execution signal is sent to the corresponding actuator or abnormal information is fed back to the central control unit and triggered hierarchical alarm, and the control command execution signal is output.

[0039] According to the present invention, a production system for preparing two-dimensional polyarylamide based on a liquid-phase loop tube is provided. The product separation module includes a feed buffer unit, a continuous centrifugal separation unit, a filtrate collection unit, and a solid conveying unit. The feed buffer unit is used to temporarily store the primary two-dimensional polyarylamide mixture and output a primary mixture with a stable flow rate. The continuous centrifugal separation unit is used to perform solid-liquid centrifugal separation on the primary mixture with a stable flow rate and output a solid two-dimensional polyarylamide mixture and a solvent-containing filtrate. The filtrate collection unit is used to collect the solvent-containing filtrate. The solid conveying unit is used to convey the solid two-dimensional polyarylamide mixture and output it to the product purification module.

[0040] According to the present invention, a production system for preparing two-dimensional polyarylamide based on a liquid-phase loop is provided. The product purification module includes a multi-stage washing unit, a washing liquid separation unit, a vacuum distillation recovery unit, and a solvent storage unit. The multi-stage washing unit is used to perform gradient washing on the solid two-dimensional polyarylamide mixture to remove residual monomers and impurities, and outputs high-purity two-dimensional polyarylamide and washing waste liquid. The washing liquid separation unit is used to perform solid-liquid secondary separation on the washing waste liquid, and outputs a solvent-containing clarified washing liquid. The vacuum distillation recovery unit is used to perform vacuum distillation on the solvent-containing clarified washing liquid, and outputs recovered solvent and distillation residue. The solvent storage unit is used to store the recovered solvent and outputs recyclable recovered solvent.

[0041] According to the present invention, a production system for preparing two-dimensional polyarylamide based on a liquid-phase loop tube is provided. The product drying module includes a vacuum drying unit, a temperature and pressure control unit, and a tail gas treatment unit. The vacuum drying unit is used to perform vacuum drying treatment on high-purity two-dimensional polyarylamide, and outputs dried two-dimensional polyarylamide and tail gas containing residual solvent. The temperature and pressure control unit is used to adjust the temperature and pressure parameters in the vacuum drying unit in real time to obtain a stable vacuum drying environment. The tail gas treatment unit is used to purify the tail gas containing residual solvent and output tail gas that meets emission standards.

[0042] This invention provides a production system for preparing two-dimensional polyaramids based on a liquid-phase loop reactor. High-speed circulation via an axial flow pump generates intense turbulence within the loop reactor, providing continuous and uniform shearing and mixing of the reactants. This effectively breaks down stagnant zones that may form in high-viscosity fluids, ensuring full contact between monomers, oligomers, and growing two-dimensional sheets. This significantly improves mass transfer efficiency and avoids localized concentration inhomogeneities and reaction dead zones. An intelligent control module combined with a kinetic model enables dynamic optimization of reaction parameters and safety interlock protection, enhancing reaction controllability, reducing production risks, and ensuring product conversion and molecular weight stability. Attached Figure Description

[0043] To more clearly illustrate the technical solutions in this invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this invention. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0044] Figure 1 This is a schematic diagram of a production system for preparing two-dimensional polyarylamide based on a liquid-phase loop tube, provided by an embodiment of the present invention.

[0045] Figure 2 This is a flowchart of the two-dimensional polyaramid polycondensation reaction carried out by the loop core reaction module provided in this embodiment of the invention;

[0046] Figure 3 This is a flowchart illustrating the construction of a two-dimensional polyarylamide polycondensation reaction kinetic model in the central control unit provided in this embodiment of the invention;

[0047] Figure 4 These are one-dimensional polycondensation reaction and two-dimensional polycondensation reaction mechanism diagrams provided in the embodiments of the present invention;

[0048] Figure 5 This is a schematic diagram of the loop reactor provided in an embodiment of the present invention. Detailed Implementation

[0049] To make the objectives, technical solutions, and advantages of this invention clearer, the technical solutions of this invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of this invention. All other embodiments obtained by those skilled in the art based on the embodiments of this invention without creative effort are within the scope of protection of this invention.

[0050] The following is combined Figures 1-5 This invention describes a production system for preparing two-dimensional polyarylamides based on a liquid-phase loop.

[0051] like Figures 1-5 As shown in the embodiment of the present invention, a production system for preparing two-dimensional polyarylamides based on a liquid-phase loop reactor includes: a raw material processing module, a loop reactor core reaction module, an intelligent control module, a product separation module, a product purification module, and a product drying module. The raw material processing module is used to process the aromatic monomers and feed liquid required for the synthesis of two-dimensional polyarylamides. The first monomer is 1,3,5-benzenetricarboxylic acid chloride (TMC), the second monomer is melamine, the solvent is N-methylpyrrolidone (NMP), and the acid-binding agent is pyridine.

[0052] The loop reactor core reaction module is used to carry out the polycondensation reaction of two-dimensional polyaramids in a loop reactor, outputting a primary two-dimensional polyaramid mixture. The intelligent control module monitors the operating parameters of the loop reactor core reaction module in real time, generating reaction parameter control commands and heat dissipation optimization strategies. The product separation module performs solid-liquid separation on the primary two-dimensional polyaramid mixture, outputting a solid two-dimensional polyaramid mixture. The product purification module purifies the solid two-dimensional polyaramid mixture and recovers the solvent, obtaining high-purity two-dimensional polyaramid and recovered solvent. The product drying module removes residual moisture and solvent from the high-purity two-dimensional polyaramid, outputting dried two-dimensional polyaramid.

[0053] Two-dimensional polyarylamides are polyarylamide materials with a planar two-dimensional sheet structure formed by the condensation reaction of aromatic monomers. The molecular chains are arranged in a periodic planar manner, and they have high specific surface area, excellent mechanical properties and chemical stability. They are widely used in filter membranes, composite material reinforcing phases, electronic device packaging and other fields.

[0054] A loop reactor is a continuous reaction system that uses a loop pipe as the core reaction zone and drives the reactants to flow continuously within the loop to complete the reaction. It features high mass and heat transfer efficiency, uniform reaction conditions, and ease of large-scale scaling.

[0055] The core reaction module of the loop reactor includes a feed unit, a loop reactor, an axial flow pump, a temperature control unit, and a discharge unit. The feed unit receives aromatic monomers and feed liquid, and outputs a mixture. The loop reactor is used for the polycondensation reaction of the mixture, and the axial flow pump ensures continuous circulation of the mixture within the loop reactor. By adjusting the speed of the axial flow pump, the material circulation rate is controlled to ensure that the Reynolds number Re ≥ 10000 within the loop, creating a turbulent flow state and improving mass transfer efficiency.

[0056] The temperature control unit is used to regulate the internal temperature of the loop reactor. A temperature sensor collects the material temperature inside the loop reactor in real time and transmits the data to the temperature controller. The temperature controller adjusts the heating / cooling power of the constant-temperature circulating water bath based on the deviation between the set temperature and the actual temperature. Through a jacketed heat exchanger, precise temperature control of the material inside the loop reactor is achieved, with a control accuracy of ±0.5℃.

[0057] The discharge unit is used to continuously or intermittently extract the primary two-dimensional polyaramid mixture. The discharge flow rate is adjusted by the opening of the electromagnetic diaphragm valve, and the flow sensor monitors the discharge flow rate in real time to ensure that the discharge flow rate is balanced with the total feed volume flow rate, thus maintaining the stability of the material volume in the loop reactor.

[0058] The steps of the two-dimensional polyaramid polycondensation reaction in the loop core reaction module include:

[0059] A first feed solution and a second feed solution were prepared separately. The first feed solution was a solution of 1,3,5-benzenetricarboxylic chloride (TMC) dissolved in N-methylpyrrolidone (NMP) with a concentration of 0.15 g / mL. The second feed solution was a solution of melamine dissolved in a mixed solvent of NMP and pyridine with a volume ratio of NMP to pyridine of 4:1 and a concentration of 0.09 g / mL. The molar ratio of TMC to melamine was controlled to be 1:1.05.

[0060] Close the discharge valve of the discharge unit, and purge the loop reactor with nitrogen to 0.2 MPa. Hold the pressure for 30 seconds, then release the pressure to atmospheric pressure. Repeat this process three times to remove oxygen from the loop reactor and ensure that the system is oxygen-free. Using nitrogen to replace the air in the reactor reduces the oxygen content and prevents oxygen from inhibiting the polycondensation reaction, as oxygen reacts with the active groups of the monomers, terminating the polymerization chain growth. The nitrogen purging pressure is monitored in real time by a pressure sensor on the loop reactor, and the holding time is monitored by a timer.

[0061] Dry NMP solvent is injected into the loop reactor, filling 80% of the loop's effective volume. The initial speed of the axial flow pump is set, typically 300 rpm, and read via a frequency converter. The temperature inside the loop is acquired in real time by a temperature sensor. The temperature inside the loop reactor is preheated to a preset temperature by a temperature control unit, which is a jacketed temperature control system, typically maintaining a temperature of 60 ± 2℃.

[0062] The metering pump is started to pump the first and second feed solutions into the loop reactor at a constant flow rate, controlling the total residence time of the mixture to approximately 45 minutes. Driven by an axial flow pump, the mixture circulates at a preset circulation rate (typically 5 m / s) within the loop reactor for polycondensation. Temperature and pressure changes within the loop are monitored in real time. If an abnormal temperature rise occurs, the feed flow rate is immediately reduced or the cooling system is activated. Polycondensation refers to the reaction in which 1,3,5-benzenetricarboxylic chloride (TMC) and melamine are linked through amide bonds to form a two-dimensional polyarylamide. The feed flow rate is collected by the flow sensor integrated into the metering pump, the circulation velocity is monitored by a flow rate sensor, and temperature and pressure are collected in real time by corresponding sensors.

[0063] The preset circulation velocity is determined as follows:

[0064] The axial flow pump speeds were set to 150 rpm, 300 rpm, and 450 rpm, respectively, corresponding to circulation velocities of approximately 2.5 m / s, 5 m / s, and 7.5 m / s.

[0065] When the circulation flow rate was 2.5 m / s, the system was slightly thickened in the later stage of the reaction, the discharge was slightly obstructed, and the molecular weight of the product was about 120,000.

[0066] The system operated stably at circulation flow rates of 5 m / s and 7.5 m / s, and the molecular weights of the products reached 150,000 and 155,000, respectively.

[0067] This indicates that a higher circulation flow rate is beneficial for mass transfer and obtaining products with higher molecular weights, but an excessively high flow rate may lead to increased energy consumption. Taking all factors into consideration, 5 m / s is the optimal choice.

[0068] After the system stabilizes, open the discharge valve to continuously discharge the primary two-dimensional polyaramid mixture at the same flow rate as the total feed volume flow rate. Stable operation is judged by fluctuations in temperature and pressure within the loop pipe ≤ ±0.5℃ and ±0.01MPa, respectively, for 10 minutes. Flow balance control uses a flow sensor to provide real-time feedback on the discharge flow rate and adjusts the discharge valve opening to ensure the deviation between the discharge flow rate and the total feed volume flow rate is ≤ ±2%. Parameters such as feed flow rate, discharge flow rate, loop pipe temperature, and pressure are recorded in real-time, with data recorded every 5 minutes.

[0069] The resulting primary two-dimensional polyarylamide mixture was immediately introduced into a quenching vessel containing isopropanol and stirred for quenching. Subsequently, after centrifugation, washing (with ethanol and deionized water sequentially), and freeze-drying, a pale yellow 2DPA powder was obtained.

[0070] The intelligent control module includes an online monitoring unit, a central control unit, and a safety interlock unit. The online monitoring unit monitors key operating parameters of the core reaction module in real time. The central control unit, based on these key operating parameters, analyzes the data using a preset two-dimensional polyarylamide polycondensation reaction kinetic model to dynamically generate reaction parameter control commands and heat dissipation optimization strategies. The safety interlock unit verifies the reaction parameter control commands and simultaneously monitors key operating parameters, automatically triggering interlock protection actions when preset safety thresholds are exceeded.

[0071] The steps for constructing the kinetic model of the two-dimensional polyaramid polycondensation reaction in the central control unit include:

[0072] Multiple orthogonal experiments were designed, with the temperature inside the loop reactor, the molar ratio of aromatic monomers, the residence time of the mixture, and the circulation flow rate as variables. Each variable was set with 3-4 levels, and L... 16 (4 5 Orthogonal experimental design table for arranging experiments. 16 (4 5 In the orthogonal experiment table, L is the general code for orthogonal table, representing orthogonality; 16 indicates that the orthogonal table requires 16 sets of experiments; 4 indicates that each experimental factor is set with 4 levels, that is, 3-4 levels of variables such as loop temperature and monomer molar ratio. Selecting 4 levels can accommodate the needs of multiple variable levels; 5 indicates that the orthogonal table can arrange a maximum of 5 experimental factors, namely temperature, monomer molar ratio, residence time, and circulation flow rate. The remaining column is a blank column, which is used to estimate experimental error.

[0073] Two-dimensional polyarylamide condensation reaction experiments were conducted within a preset variable range. The monomer conversion rate, number-average molecular weight, and weight-average molecular weight of each experimental group were measured, and the experimental dataset was output. The monomer conversion rate was calculated by measuring the monomer concentration before and after the reaction using high-performance liquid chromatography (HPLC); the polymer molecular weight was determined by gel permeation chromatography (GPC).

[0074] Based on experimental data and considering the stepwise polymerization characteristics of condensation reactions, assuming a homogeneous reaction and neglecting interfacial mass transfer resistance, the key reaction steps in the formation of two-dimensional polyarylamides are identified, and a reaction mechanism hypothesis is derived. The acyl chloride groups (-COCl) in TMC molecules undergo a nucleophilic substitution reaction with the amino groups (-NH2) in melamine molecules, removing HCl molecules and forming amide bonds (-CONH-). Each TMC molecule contains 3 acyl chloride groups, and each melamine molecule contains 6 amino groups; the two are linked by amide bonds to form a two-dimensional planar network structure. The reaction can be divided into three stages: the acyl chloride groups initially react with the amino groups to form oligomers; further reactions occur between oligomer molecules, leading to rapid chain growth and the formation of a two-dimensional sheet-like structure; the reaction rate gradually decreases, and the monomer conversion rate tends to stabilize.

[0075] Based on the reaction mechanism assumptions, and with the law of conservation of mass and the fundamental principles of reaction kinetics as the core, an initial kinetic equation is established. The reaction rate is directly proportional to the first power of the reactant concentration, indicating a second-order reaction; the reaction rate constant follows the Arrhenius equation. Let the initial concentration of TMC be c. A0 The initial concentration of melamine was c. B0 If the reaction time is t and the monomer conversion rate is x, then the concentration c of TMC during the reaction is... A Represented as:

[0076]

[0077] melamine concentration c B Represented as:

[0078]

[0079] Polycondensation reaction rate r p Defined as the decrease in monomer concentration per unit time, for a second-order reaction, its expression is:

[0080]

[0081] Where k is the reaction rate constant and t is the reaction time. In a continuous reaction system in a loop, the reaction time is equal to the residence time of the mixture. This indicates the rate of change of TMC concentration over time. The negative sign indicates that TMC, as a reactant, gradually decreases in concentration over time during the reaction. The reaction rate is indirectly quantified by the rate of concentration change.

[0082] Combining the relationship between the residence time τ of the mixture and the reaction time t, i.e., in a continuous reaction system, τ=t, we can simplify to obtain:

[0083]

[0084] After integration, the initial dynamic equation is expressed as:

[0085]

[0086] The reaction rate constant k follows the Arrhenius equation:

[0087]

[0088] Where A is the pre-exponential factor, E a The activation energy is given by R, the gas constant is given by R = 8.314 J / (mol·K), and T is the absolute temperature.

[0089] Based on the experimental dataset and the initial dynamic equations, the least squares method is used to fit the unknown parameters to obtain the initial parameter values. Let the predicted value of the i-th experiment be... The experimental value is y i The residual of the i-th experiment Then the objective function is expressed as:

[0090]

[0091] Where S is the sum of the squares of the residuals at all experimental points, and it is the core indicator for measuring the model's fit. The smaller the S value, the higher the degree of agreement between the model's predicted values ​​and the experimentally measured values, and the better the fit. n is the total number of trials, that is, the number of orthogonal experimental groups designed when constructing the dynamic model, representing the total number of samples participating in the fitting. The size of n directly affects the reliability of the fitting results. i is the experimental point index, used to distinguish experimental data from different groups.

[0092] Substituting k from the initial dynamic equations into the Arrhenius equations, we obtain the equations containing A and E. a The expression is then substituted into the objective function for A and E. a Taking the partial derivatives and setting them to zero, we obtain the system of equations as follows:

[0093]

[0094] Solving the system of equations yields the initial pre-exponential factor and the initial activation energies A0 and E. a0 .

[0095] The reliability of the fit is verified through residual analysis. If the residuals exceed the preset range, the model assumptions are adjusted or the fitting algorithm is optimized, and the fitting is repeated until the residuals meet the requirements. The corrected dynamic equation is then output, expressed as:

[0096]

[0097] Where, k d is the flow rate influencing factor, and v is the circulation velocity.

[0098] Based on the experimental dataset, the experimental conditions were substituted into the modified kinetic equation to calculate the theoretical values ​​of monomer conversion and polymer molecular weight distribution. The deviations between the theoretical and experimental values ​​were compared. If the deviation was <5%, the model validation was successful. If the deviation was ≥5%, the reaction mechanism assumptions were re-optimized, corrected, and validated again, outputting the static reaction kinetic equation. The formula for calculating the deviation between the theoretical and experimental values ​​is as follows:

[0099]

[0100] Where δ is the deviation between the theoretical value and the experimentally measured value, x cal x is the theoretically calculated value of monomer conversion rate. exp These are the experimentally measured values ​​for monomer conversion rate.

[0101] Combining static reaction kinetics equations with a loop reactor flow model, and adapting to the continuous operation characteristics of the liquid-phase loop reactor based on the circulation velocity, a two-dimensional polyaramid polycondensation reaction kinetic model is derived. An axial dispersion model (ADM) is used to describe the flow state of the material within the loop. The axial dispersion coefficient is experimentally determined, typically using a tracer pulse injection method. By coupling the axial dispersion model with the static kinetic equations and introducing a term incorporating the influence of flow parameters on the reaction rate, the final two-dimensional polyaramid polycondensation reaction kinetic model is expressed as follows:

[0102]

[0103] Where z is the axial position coordinate of the annular pipe, and D z is the axial dispersion coefficient.

[0104] The steps to verify the reliability of the fit through residual analysis include:

[0105] Based on the key response values ​​of the prototype experimental points in the experimental dataset and the corresponding predicted values ​​obtained by fitting the initial dynamic equation, the residual of each experimental point is calculated, and the original residual dataset is output.

[0106] Statistical calculations were performed on the original residual dataset to obtain the residual mean. The system determines whether the mean residual is close to 0. If the mean residual deviates from 0 and exceeds the preset threshold of 0.01, it is preliminarily determined that there is a systematic bias in the fitting result, and outputs the statistical analysis results and the preliminary bias determination conclusion.

[0107] Based on the original residual dataset, Origin software was used to plot the residual frequency histogram and normal probability plot. The graphical features were analyzed to determine whether the experimental point residuals conformed to an approximate normal distribution. If the frequency histogram exhibited a symmetrical bell-shaped distribution, and the data points in the normal probability plot were approximately distributed along a straight line, then the residuals were determined to conform to a normal distribution; otherwise, they were determined not to. Finally, the distribution pattern analysis results and the distribution conformity determination conclusion were output.

[0108] Based on the original residual dataset, corresponding predicted values, and experimental datasets, residual-predicted value relationship graphs and residual-experimental variable relationship graphs are plotted respectively. The analysis examines whether the residuals at experimental points exhibit significant trends such as linearity or periodicity, and outputs a trend conformity judgment conclusion. If the residuals are randomly distributed in the graphs without obvious patterns, it is determined that the residuals have no significant trend; if the residuals show obvious linear increases / decreases or periodic fluctuations with the predicted values ​​or experimental variables, it is determined that a significant trend exists.

[0109] Based on the original residual dataset and the residual standard deviation as input, the residual standard deviation is expressed as:

[0110]

[0111] Where σ is the standard deviation of the residuals. The 3σ criterion is used to identify outlier residuals; if |e i If |> 3σ, then the residual is determined to be an abnormal residual. For the experimental points corresponding to the abnormal residuals, check the standardization of experimental operation, the accuracy of the testing instruments, and the accuracy of data recording. If it is an operational or recording error, correct the data and recalculate the residual; if it is an experimental random error, remove the abnormal data point, output the corrected residual dataset and the abnormality handling conclusion.

[0112] Using the preliminary deviation judgment conclusion, distribution conformity judgment conclusion, trend conformity judgment conclusion, and anomaly handling conclusion as joint inputs, if the following four conditions are met: the residual mean approaches 0, the residuals conform to a normal distribution, the residuals have no significant trend, and the proportion of abnormal residuals is <5%, then the fit is considered reliable. If any condition is not met, then the residuals are considered to exceed the preset range, the final conclusion on the fit reliability is output, and the model optimization command is triggered simultaneously.

[0113] The steps for verifying the response parameter control instructions of the safety interlock unit include:

[0114] Based on the safe operating boundaries of the two-dimensional polyaramid polycondensation reaction and the rated operating parameters of the equipment, a standardized verification checklist is formed by presetting the safe threshold range, upper limit of the control amplitude, and parameter linkage rules for each control parameter. The parameter linkage rule is that when the temperature rises, if it is necessary to lower the temperature, the cooling medium flow rate can be increased (control amplitude ≤ 20%) and the feed flow rate can be decreased (control amplitude ≤ 5%) at the same time, and the control ratio of cooling medium flow rate to feed flow rate is ≥ 4:1.

[0115] Based on the reaction parameter control instructions and the classification criteria of the control objects in the standardized verification list, the control objects, target control parameter values, and control rates in the instructions are analyzed, classified and entered into the verification module, and the parsed parameter set is output, including the control object, target value, control rate, and control direction.

[0116] Using the parsed parameter set as the verification object, each parameter's target value is compared with the safety threshold range. Simultaneously, it is determined whether the adjustment range exceeds the limits in the standardized verification checklist, and a single-parameter verification result set is output. The verification method is: adjustment range α = |(target value - current value) / current value| × 100%. If α ≤ the upper limit of the adjustment range and the target value is within the safety threshold range, then the single-parameter verification passes; otherwise, the verification fails.

[0117] The associated parameters in the parsed parameter set are extracted. Based on the parameter linkage rules, the rationality of the control logic between the associated parameters is verified, and the linkage verification result is output. For example, if the control command is "increase the temperature by 5°C" while "decrease the cooling medium flow rate by 20%", according to the linkage rule "when the temperature increases, the cooling medium flow rate should increase or remain unchanged", then the control logic is determined to be conflicting, and the linkage verification is abnormal. If the control command is "decrease the temperature by 2°C" while "increase the cooling medium flow rate by 10%", then the linkage verification is reasonable.

[0118] The system summarizes the single-parameter verification results and the linkage verification results. If both are "pass / reasonable," a control command execution signal is issued to the corresponding actuator. If an "abnormal / conflict" occurs, the issuance of the control command is immediately blocked, abnormal information is reported to the central control unit, a tiered alarm is triggered, and a control command execution signal is output. Tiered alarms include:

[0119] Level 1 alarm: Audible and visual alarm to alert operators;

[0120] Level 2 alarm: Automatically activates the emergency cooling system and cuts off the feed.

[0121] Level 3 alarm: Emergency shutdown, inert gas protection.

[0122] The product separation module includes a feed buffer unit, a continuous centrifugal separation unit, a filtrate collection unit, and a solids conveying unit. The feed buffer unit temporarily stores the primary two-dimensional polyaramid mixture, outputting a stable flow rate of the primary mixture. The primary mixture enters the buffer tank, and a level sensor continuously monitors the liquid level. When the liquid level is below 30%, the feed flow rate is reduced; when the liquid level is above 70%, the discharge flow rate is increased to ensure stable liquid level and provide a stable feed flow rate for subsequent centrifugal separation.

[0123] The continuous centrifugal separation unit is used for solid-liquid centrifugal separation of a stable flow rate of primary mixture, outputting a solid two-dimensional polyaramid mixture and a solvent-containing filtrate. The stable flow rate of the primary mixture enters the centrifuge drum. Under the centrifugal force generated by high-speed rotation, the solid two-dimensional polyaramid particles settle to the inner wall of the drum. A screw conveyor pushes the solid particles to the discharge port, while the solvent-containing filtrate is discharged through the overflow port on the drum. The drum speed is read by a frequency converter, the separation factor is calculated, the filtrate turbidity is monitored by an online turbidity meter, and the solid recovery rate is calculated by weighing the solids before and after separation.

[0124] The filtrate collection unit is used to collect solvent-containing filtrate. The solids conveying unit is used to convey the solid two-dimensional polyaramid mixture using a screw conveyor. The conveying speed is matched with the solid discharge speed of the centrifuge, and the output is sent to the product purification module. The conveying speed is read by the screw conveyor's frequency converter.

[0125] The product purification module includes a multi-stage washing unit, a washing liquid separation unit, a vacuum distillation recovery unit, and a solvent storage unit. The multi-stage washing unit is used to perform gradient washing on the solid two-dimensional polyarylamide mixture to remove residual monomers and impurities, outputting high-purity two-dimensional polyarylamide and washing waste liquid. The first-stage washing medium is deionized water, used to remove soluble impurities; the second stage is a dilute hydrochloric acid solution (0.1 mol / L) used to remove unreacted melamine; and the third stage is deionized water used to remove residual hydrochloric acid and salts. The solid material enters the first-stage washing vessel, where deionized water is added, and the mixture is stirred and washed for 30 minutes at 40℃ and 200 rpm, then enters the washing liquid separation unit. The separated solid enters the second-stage washing vessel, where dilute hydrochloric acid solution is added for washing under the same conditions; then it enters the third-stage washing vessel, where deionized water is added for washing, completing the multi-stage washing process. The washing temperature is monitored by a temperature sensor, the stirring rate is read by a frequency converter, and the product purity and residual monomer content are determined by high-performance liquid chromatography (HPLC).

[0126] The washing liquid separation unit is used for secondary solid-liquid separation of the washing waste liquid. A plate and frame filter press is used for this secondary separation, with a filtration pressure of 0.3-0.5 MPa and a filtration temperature of 40℃. The output is a clear washing liquid containing solvent and a small amount of solid residue. The small amount of solid residue is returned to the multi-stage washing unit for rewashing.

[0127] The vacuum distillation recovery unit is used to treat solvent-containing clarified washing liquid by vacuum distillation, outputting recovered solvent and distillation residue. Under reduced pressure, the boiling point of the solvent decreases. The solvent is vaporized by heating, and the recovered solvent is obtained after condensation. The distillation residue consists of a small amount of high-boiling-point impurities.

[0128] The solvent storage unit is used to store recycled solvents. Once the recycled solvents pass inspection and have a purity of ≥99.0%, they can be recycled for use in the preparation of the feed liquid, and the recycled solvents can be output as recyclable products.

[0129] The product drying module includes a vacuum drying unit, a temperature and pressure control unit, and a tail gas treatment unit. The vacuum drying unit is used to vacuum dry high-purity two-dimensional polyarylamide, outputting dried two-dimensional polyarylamide and tail gas containing residual solvent. The specific operation is as follows: high-purity two-dimensional polyarylamide enters the dryer, the feed inlet is closed, the vacuum pump is started to reduce the pressure inside the dryer to -0.09 MPa, the heating device is started to raise the temperature to the preset drying temperature, and simultaneously the rake agitator is started to stir the material to prevent agglomeration and improve drying uniformity. After drying for the preset time, heating and stirring are stopped, and after the temperature drops to room temperature, the vacuum is broken and the dried two-dimensional polyarylamide is output.

[0130] The temperature and pressure control unit is used to adjust the temperature and pressure parameters within the vacuum drying unit in real time to obtain a stable vacuum drying environment. When the drying temperature is lower than the preset value, the heating power is increased; when the temperature is higher than the preset value, the heating power is decreased; when the drying pressure is higher than the preset value, the vacuum pump's pumping speed is increased; when the pressure is lower than the preset value, the pumping speed is decreased.

[0131] The exhaust gas treatment unit is used to purify exhaust gas containing residual solvents and output exhaust gas that meets emission standards. The exhaust gas containing residual solvents (NMP, pyridine) generated during the drying process first enters the condenser to recover most of the solvent; the uncondensed exhaust gas enters the activated carbon adsorption tower to remove the residual solvent through activated carbon adsorption; the exhaust gas after adsorption is tested and qualified, and then discharged through the exhaust pipe.

[0132] In summary, this invention provides a production system for preparing two-dimensional polyaramids based on a liquid-phase loop reactor. High-speed circulation driven by an axial flow pump generates intense turbulence within the loop, providing continuous and uniform shearing and mixing of the reactants. This effectively breaks down stagnant zones that may form in high-viscosity fluids, ensuring full contact between monomers, oligomers, and growing two-dimensional sheets, significantly improving mass transfer efficiency and avoiding localized concentration inhomogeneities and reaction dead zones. Furthermore, the loop reactor is particularly suitable for systems where viscosity changes drastically with the reaction process. The axial flow pump, as the power source, overcomes the flow resistance caused by high viscosity, maintaining stable system operation. Compared to the sharp drop in efficiency of traditional stirred tank reactors at high viscosity and the clogging risk faced by microreactors, the loop system exhibits a wider viscosity operating window and better engineering robustness. The loop reactor has a large specific surface area; combined with the high-speed internal material flow and external jacket temperature control, it can efficiently remove the heat generated by the polycondensation reaction, precisely control the reaction temperature, and prevent side reactions and product structural defects caused by localized overheating. This technology enables continuous or semi-continuous production of 2DPA, breaking the limitations of traditional batch production and significantly improving production efficiency. The loop reactor has a simple structure and relatively clear scale-up characteristics. CFD simulations can help optimize the hydrodynamic behavior during scale-up, effectively reducing the "scale-up effect" and providing a reliable path for large-scale industrial production. Due to uniform mixing and precise temperature control during the reaction process, the prepared 2DPA materials typically exhibit higher molecular weights, more regular two-dimensional lamellar structures, and better batch-to-batch consistency. The products exhibit stable performance, meeting the demands of high-performance applications.

[0133] Through the above description of the embodiments, those skilled in the art can clearly understand that each embodiment can be implemented by means of software plus necessary general-purpose hardware platforms, and of course, it can also be implemented by hardware. Based on this understanding, the above technical solutions, in essence or the part that contributes to the prior art, can be embodied in the form of a software product. This computer software product can be stored in a computer-readable storage medium, such as ROM / RAM, magnetic disk, optical disk, etc., including several instructions to cause a computer device (which may be a personal computer, server, or network device, etc.) to execute the methods of various embodiments or some parts of embodiments.

[0134] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A production system for preparing two-dimensional polyarylamides based on a liquid-phase loop, characterized in that, include: The raw material processing module is used to process the aromatic monomers and feed liquid required for the synthesis of two-dimensional polyarylamides. The loop core reaction module is used to carry out the two-dimensional polyaramid polycondensation reaction through the loop reactor and output a primary two-dimensional polyaramid mixture. The intelligent control module is used to monitor the operating parameters of the core reaction module of the loop in real time and generate reaction parameter control commands and heat dissipation optimization strategies. The product separation module is used to perform solid-liquid separation on the primary two-dimensional polyaramid mixture and output a solid two-dimensional polyaramid mixture. The product purification module is used to purify the solid two-dimensional polyarylamide mixture and recover the solvent to obtain high-purity two-dimensional polyarylamide and recovered solvent. The product drying module is used to remove residual moisture and solvent from the high-purity two-dimensional polyarylamide and output dried two-dimensional polyarylamide.

2. The production system for preparing two-dimensional polyarylamide based on a liquid-phase loop according to claim 1, characterized in that, The loop core reaction module includes a feeding unit, a loop reactor, an axial flow pump, a temperature control unit, and a discharge unit. The feeding unit receives the aromatic monomers and feed liquid and outputs a mixture. The loop reactor is used for the polycondensation reaction of the mixture. The axial flow pump continuously circulates the mixture within the loop reactor. The temperature control unit regulates the internal temperature of the loop reactor. The discharge unit continuously or intermittently extracts the primary two-dimensional polyaramid mixture.

3. The production system for preparing two-dimensional polyarylamide based on a liquid-phase loop according to claim 2, characterized in that, The steps of the two-dimensional polyaramid polycondensation reaction in the loop core reaction module include: Prepare the first and second feed solutions; Close the discharge valve of the discharge unit, and fill the loop reactor with nitrogen to 0.2 MPa. After maintaining the pressure, release the pressure and repeat three times to remove the oxygen in the loop reactor. Dry N-methylpyrrolidone solvent is injected into the loop reactor, the initial speed of the axial flow pump is set, and the temperature inside the loop reactor is preheated to a preset temperature by the temperature control unit. Start the metering pump to pump the first feed liquid and the second feed liquid into the loop reactor at a constant flow rate, and control the total residence time of the mixture. The mixture undergoes a polycondensation reaction in the loop reactor at a preset circulation rate driven by an axial flow pump. After the system is running stably, the discharge valve is opened to continuously draw out the primary two-dimensional polyaramid mixture at a flow rate that is the same as the total feed volume flow rate.

4. The production system for preparing two-dimensional polyarylamide based on a liquid-phase loop according to claim 1, characterized in that, The intelligent control module includes an online monitoring unit, a central control unit, and a safety interlock unit; the online monitoring unit is used to monitor the key operating parameters of the core reaction module of the loop in real time; the central control unit is used to analyze the data based on the key operating parameters through a preset two-dimensional polyarylamide polycondensation reaction kinetic model, and dynamically generate the reaction parameter control instructions and heat dissipation optimization strategies. The safety interlock unit is used to verify the reaction parameter control command and simultaneously monitor the key operating parameters. When the parameters exceed the preset safety threshold, the interlock protection action is automatically triggered.

5. The production system for preparing two-dimensional polyarylamide based on a liquid-phase loop according to claim 4, characterized in that, The steps for constructing the kinetic model of the two-dimensional polyaramid polycondensation reaction in the central control unit include: Design multiple orthogonal experiments, using the temperature inside the loop reactor, the molar ratio of aromatic monomers, the residence time of the mixture, and the circulation flow rate as variables, to conduct two-dimensional polyarylamide polycondensation reaction experiments within the preset variable range, and output experimental datasets; Based on the experimental dataset and the stepwise polymerization characteristics of polycondensation reaction, assuming that the reaction system is a homogeneous reaction and ignoring interfacial mass transfer resistance, the key reaction steps in the formation of two-dimensional polyarylamide are identified, and the reaction mechanism hypothesis is output. Based on the aforementioned reaction mechanism assumptions, and with the law of conservation of mass and the basic principles of reaction kinetics as the core, an initial kinetic equation is established. Based on the experimental dataset and the initial dynamic equation, the unknown parameters are fitted using the least squares method to obtain the initial parameter values. The reliability of the fit is verified by residual analysis. If the residual exceeds the preset range, the model assumptions are adjusted or the fitting algorithm is optimized and the fitting is repeated until the residual meets the requirements. The corrected dynamic equation is then output. Based on the experimental dataset, the experimental conditions are substituted into the modified kinetic equation to calculate the theoretical values ​​of monomer conversion and polymer molecular weight distribution; the deviation between the theoretical values ​​and the experimentally measured values ​​is compared to output the static reaction kinetic equation. Combining the static reaction kinetic equations with the loop reactor flow model, and adapting the continuous operation characteristics of the liquid-phase loop reactor based on the circulating flow rate, the two-dimensional polyaramid polycondensation reaction kinetic model is output.

6. The production system for preparing two-dimensional polyarylamide based on a liquid-phase loop according to claim 5, characterized in that, The steps to verify the reliability of the fit through residual analysis include: Based on the key response values ​​of the prototype experimental points in the experimental dataset and the corresponding predicted values ​​obtained by fitting the initial dynamic equation, the residual of each experimental point is calculated, and the original residual dataset is output. Statistical calculations are performed on the original residual dataset to obtain the residual mean. It is then determined whether the residual mean is close to 0. If the residual mean deviates from 0 and exceeds a preset threshold, it is preliminarily determined that there is a systematic bias in the fitting result. Statistical analysis results and preliminary bias determination conclusions are output. Based on the original residual dataset, a residual frequency histogram and a normal probability plot are drawn. The graphical features are used to analyze whether the residuals of the experimental points conform to an approximate normal distribution. The distribution pattern analysis results and distribution conformity judgment conclusions are output. Based on the original residual dataset, the corresponding predicted values, and the experimental dataset, analyze whether there is a significant linear or periodic trend in the residuals of the experimental points, and output a trend conformity judgment conclusion. Based on the original residual dataset and residual standard deviation as input, the 3σ criterion is used to identify abnormal residuals. For the experimental points corresponding to the abnormal residuals, the standardization of experimental operation, the accuracy of detection instruments and the accuracy of data recording are checked, and the corrected residual dataset and the conclusion of abnormality handling are output. Using the preliminary deviation judgment conclusion, the distribution conformity judgment conclusion, the trend conformity judgment conclusion, and the anomaly handling conclusion as joint inputs, if the following four conditions are met: the mean residual is close to 0, the residual conforms to a normal distribution, the residual has no significant trend, and the proportion of abnormal residuals is <5%, then the fit is determined to be reliable; if any condition is not met, then the residual is determined to exceed the preset range, the final conclusion of the fit reliability is output, and the model optimization instruction is triggered simultaneously.

7. The production system for preparing two-dimensional polyarylamide based on a liquid-phase loop according to claim 5, characterized in that, The steps for the safety interlock unit to verify the reaction parameter control command include: Based on the safe operating boundary of the two-dimensional polyarylamide condensation reaction and the rated operating parameters of the equipment, a standardized verification checklist is formed by presetting the safe threshold range, upper limit of the control amplitude and parameter linkage rules of each control parameter. According to the reaction parameter control instruction, based on the control object classification criteria in the standardized verification list, the control object, target control parameter value and control rate in the instruction are analyzed, classified and entered into the verification module, and the parsed parameter set is output. Using the parsed parameter set as the verification object, compare the target value of each parameter with the safety threshold range one by one, and at the same time determine whether the control range exceeds the limit in the standardized verification list, and output a single parameter verification result set. Extract the associated parameters from the parsed parameter set, verify the rationality of the control logic between the associated parameters based on the parameter linkage rules, and output the linkage verification result; Based on the single-parameter verification result set and the linkage verification result, a control command execution signal is issued to the corresponding actuator or abnormal information is fed back to the central control unit and a graded alarm is triggered, and a control command execution signal is output.

8. The production system for preparing two-dimensional polyarylamide based on a liquid-phase loop according to claim 1, characterized in that, The product separation module includes a feed buffer unit, a continuous centrifugal separation unit, a filtrate collection unit, and a solid conveying unit. The feed buffer unit is used to temporarily store the primary two-dimensional polyaramid mixture and output a stable flow rate of the primary mixture. The continuous centrifugal separation unit is used to perform solid-liquid centrifugal separation on the stable flow rate of the primary mixture and output a solid two-dimensional polyaramid mixture and a solvent-containing filtrate. The filtrate collection unit is used to collect the solvent-containing filtrate. The solid conveying unit is used to convey the solid two-dimensional polyaramid mixture and output it to the product purification module.

9. A production system for preparing two-dimensional polyarylamide based on a liquid-phase loop according to claim 1, characterized in that, The product purification module includes a multi-stage washing unit, a washing liquid separation unit, a vacuum distillation recovery unit, and a solvent storage unit; the multi-stage washing unit is used to perform gradient washing on the solid two-dimensional polyarylamide mixture to remove residual monomers and impurities, and output high-purity two-dimensional polyarylamide and washing waste liquid. The washing liquid separation unit is used to perform solid-liquid secondary separation on the washing waste liquid and output a clear washing liquid containing solvent; the vacuum distillation recovery unit is used to perform vacuum distillation on the clear washing liquid containing solvent and output a recovered solvent and distillation residue; the solvent storage unit is used to store the recovered solvent and output a recyclable recovered solvent.

10. A production system for preparing two-dimensional polyarylamide based on a liquid-phase loop according to claim 1, characterized in that, The product drying module includes a vacuum drying unit, a temperature and pressure control unit, and a tail gas treatment unit. The vacuum drying unit is used to perform vacuum drying on the high-purity two-dimensional polyarylamide, outputting dried two-dimensional polyarylamide and tail gas containing residual solvent. The temperature and pressure control unit is used to adjust the temperature and pressure parameters within the vacuum drying unit in real time to obtain a stable vacuum drying environment. The tail gas treatment unit is used to purify the tail gas containing residual solvent, outputting tail gas that meets emission standards.

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