A method and system for detecting catalytic activity of a polyester titanium catalyst

Abstract

The application discloses a polyester titanium catalyst catalytic activity detection method and system, belongs to the polyester catalyst detection technical field, and aims to solve the problems of working condition simulation distortion, serious non-catalytic factor interference, uncoupling of activity and selectivity, and disconnection of detection results and industrial application of an existing detection method; a complete process is provided, which comprises uniformly configuring a standardization detection group of effective titanium concentration, simulating industrial continuous working conditions through parallel multistage series connection of reaction kettles, monitoring and access control in stages, obtaining pure catalytic parameters through three-layer baseline correction, and decoupling and quantifying catalytic performance in different dimensions. The application realizes rapid, accurate and repeatable detection of the catalytic performance of a titanium catalyst, and provides a reliable basis for industrial screening.

Description

Technical Field

[0001] This invention relates to the field of polyester catalyst detection technology, and more specifically to a method and system for detecting the catalytic activity of polyester titanium catalysts. Background Technology

[0002] Polyester is one of the world's largest-volume and most widely used polymer materials, widely applied in textiles, packaging, engineering plastics, and other fields. With increasingly stringent environmental requirements and continuous improvements in product performance, titanium-based catalysts, with their advantages of being non-toxic, highly active, and highly selective, are gradually replacing traditional antimony-based catalysts and becoming the mainstream in the polyester industry. The catalytic activity and selectivity of a catalyst are core indicators determining its industrial application value, and rapid, accurate, and reliable evaluation and detection technologies are crucial for the research, screening, and industrial promotion of titanium-based catalysts. However, current industry-standard catalyst detection methods differ significantly from actual industrial production conditions, making it difficult to effectively eliminate interference from various external factors, accurately separate the performance contribution of the catalyst at different reaction stages, and independently quantify activity and selectivity. This results in poor repeatability and comparability of detection results, and a disconnect from the actual industrial performance of the catalyst, severely prolonging the research and development cycle of titanium-based catalysts and increasing the risks and costs of industrial applications. Therefore, to overcome these limitations, this invention proposes a method and system for detecting the catalytic activity of titanium-based polyester catalysts. Summary of the Invention

[0003] To address the shortcomings of existing technologies, the present invention aims to provide a method and system for detecting the catalytic activity of polyester titanium catalysts, which solves the technical problems of distorted operating condition simulation, severe interference from non-catalytic factors, inability to decouple activity and selectivity, and disconnect between detection results and industrial applications in the detection of the catalytic activity of polyester titanium catalysts.

[0004] To achieve the above objectives, the present invention provides the following technical solution: A system for detecting the catalytic activity of a polyester titanium catalyst, comprising: The detection group construction module is used to determine the effective titanium mass fraction of the titanium-based catalyst to be tested after homogenization pretreatment, and then configure the composition ratio of the basic common components and the differentiated catalyst components of each detection group. The reaction simulation module, based on the component ratio of the detection group, configures the homogenized materials prepared by each detection group and puts them into the corresponding multi-stage series micro reactor group to start the reaction synchronously under the same control conditions. The process monitoring module collects the characteristic process parameters of each reaction stage of the multi-stage series micro reactor group corresponding to each detection group, executes the access control of each micro reactor group reaction stage, and obtains the effective reaction time and conversion characteristic parameters of each reaction stage. The data processing module collects product performance data for each reaction stage after each reaction stage is completed. Based on the type of each detection group and the effective reaction time of each reaction stage, it classifies and organizes the characteristic process parameters and converted characteristic parameters of each reaction stage, performs time series standardization and stratified baseline correction, and obtains pure catalytic contribution parameters. The decoupled quantification module performs multidimensional and multi-stage decoupled calculations on the pure catalytic contribution parameters, and quantifies the catalytic activity, catalytic selectivity and comprehensive catalytic performance of the titanium catalyst under test.

[0005] Specifically, the multi-stage series-connected micro reactor groups are arranged in parallel. Each multi-stage series-connected micro reactor group contains a number of micro reactors connected in series in sequence, corresponding to the number of reaction stages. Each micro reactor is used to correspond to a reaction stage in the simulated industrial polyester production process.

[0006] Specifically, the steps for implementing access control for each microreactor group's reaction stage include: For each stage of the micro reactor, a reasonable fluctuation range of characteristic process parameters and a fixed reaction time are pre-set for all detection groups to be consistent; After the testing team starts the multi-stage series micro reactor group, the online monitoring unit in each stage of the micro reactor collects the characteristic process parameters of the reaction stage in real time at a preset acquisition frequency. Based on the quantification of characteristic process parameters, the corresponding reaction process conversion characteristic parameters are obtained to determine whether the corresponding reaction process has been completed, and combined with a reasonable fluctuation range, it is determined whether the corresponding reaction process has abnormal operating conditions. When the cumulative reaction time of a certain micro-reactor reaches the preset fixed reaction time, all detection groups simultaneously determine that the reaction stage has ended, open the material conveying valve between the current micro-reactor and the next level micro-reactor in all detection groups, and convey all the material in the current micro-reactor to the next level micro-reactor. After the conveying is completed, the material conveying valve is automatically closed and the start command of the next level micro-reactor is triggered. The effective reaction time, characteristic process parameters and converted characteristic parameters of the reaction stage are recorded.

[0007] Specifically, the steps of obtaining the converted characteristic parameters of the corresponding reaction process based on the quantification of characteristic process parameters, determining whether the corresponding reaction process has been completed, and determining whether there are abnormal operating conditions in the corresponding reaction process in combination with a reasonable fluctuation range include: The system continuously compares the real-time collected characteristic process parameters with the preset reasonable fluctuation range of the corresponding reaction stage. If any characteristic process parameter exceeds the reasonable fluctuation range and the duration reaches the preset abnormal judgment time, it is determined that there is an abnormal working condition in the detection group, and the reaction process corresponding to the detection group is automatically terminated. If all characteristic process parameters are within a reasonable range of fluctuation, then the current reaction stage should be maintained and the reaction should continue. Based on the real-time acquired characteristic process parameters, the corresponding conversion characteristic parameters of the reaction process are extracted; If the converted characteristic parameters of a certain detection group reach the standard threshold of the reaction degree of the corresponding reaction stage and the fluctuation range does not exceed the preset allowable deviation for a preset stable judgment time, then the reaction of this reaction stage of the detection group is determined to be completed, and the steady state maintenance mode is automatically triggered.

[0008] Specifically, the detection group refers to a set of standardized reaction systems used to compare and detect the catalytic activity of titanium-based catalysts. It includes an experimental group and a control group. The experimental group is a reaction system with the titanium-based catalyst to be tested added. The control group is a pre-set multi-level benchmark detection group system, which consists of multiple benchmark detection groups with the same group composition ratio as the experimental group but different only in catalyst components. The multi-level benchmark detection group system contains at least three levels. The first level benchmark detection group is a benchmark system without added catalytically active components. The second level benchmark detection group is a benchmark system with added known universal benchmark catalysts. The third level benchmark detection group is a benchmark system with added target type benchmark catalysts.

[0009] Specifically, based on each detection group type and the effective reaction time of each reaction stage, the steps for classifying, organizing, time-series standardizing, and stratified baseline correction of the characteristic process parameters and converted characteristic parameters of each reaction stage to obtain the pure catalytic contribution parameters include: The effective reaction time, characteristic process parameters and converted characteristic parameters of each reaction stage of each detection group were extracted, as well as the product performance data after the reaction stage. According to the collection time, the characteristic process parameter sequence and the converted characteristic parameter sequence were constructed respectively. Calculate the average and range of the effective reaction time for the same reaction stage for all detection groups, and determine whether the ratio of the range to the average is less than a preset deviation threshold; if so, perform simple time series standardization; otherwise, perform dual-mode time series standardization. Based on the time-series standardized characteristic process parameter sequences and converted characteristic parameter sequences of each reaction stage in each detection group, the characteristic process parameter sequences, converted characteristic parameter sequences, and product performance data of the detection group to which the titanium catalyst under test belongs are subjected to stratified baseline correction to obtain pure catalytic contribution parameters.

[0010] Specifically, performing simple time series standardization includes: Using the average effective reaction time of all test groups in this reaction stage as the baseline time, the characteristic process parameter sequence and the converted characteristic parameter sequence of each test group in this reaction stage are resampled using a linear interpolation method to generate a standardized time series of characteristic process parameter sequence and converted characteristic parameter sequence with the same length as the baseline time and the same number of sampling points, and then the timestamps are aligned.

[0011] Specifically, performing dual-mode time series standardization includes: The characteristic process parameter sequence and the converted characteristic parameter sequence of each detection group for this reaction stage are retained. At the same time, the time axis of the characteristic process parameter sequence and the converted characteristic parameter sequence of each detection group for this reaction stage are normalized to the interval [0,1], where 0 corresponds to the start time of the reaction stage and 1 corresponds to the completion time of the reaction stage of this detection group. Normalized time points are selected at equal intervals within the interval [0,1], and the characteristic process parameter value and the converted characteristic parameter value corresponding to each normalized time point are calculated using a linear interpolation method to generate the normalized time series of the characteristic process parameter sequence and the converted characteristic parameter sequence.

[0012] Specifically, the characteristic process parameter sequence, converted characteristic parameter sequence, and product performance data of the detection group containing the titanium-based catalyst under test are subjected to stratified baseline correction to obtain pure catalytic contribution parameters, including: The first-level baseline correction is performed by comparing the characteristic process parameter values, converted characteristic parameter values, and single-point values ​​of product performance data of each reaction stage in the detection group of the titanium catalyst to be tested with the corresponding data of the corresponding reaction stage and the same time point in the first-level benchmark detection group to obtain the first-level correction parameters. To perform the second-level system error correction, the first-level correction characteristic process parameter value, the first-level correction converted characteristic parameter value, and the first-level correction product performance data value after the first-level background baseline correction are compared with the corresponding data of the second-level benchmark detection group at the same time point in the corresponding reaction stage to obtain the second-level correction parameters. The third-level benchmark correction is performed by comparing the relative coefficients of the second-level corrected characteristic process parameters, the relative coefficients of the second-level corrected converted characteristic parameters, and the relative coefficients of the second-level corrected product performance data with the corresponding data at the same time point in the corresponding reaction stage of the third-level benchmark detection group. The resulting third-level correction parameters are used as pure catalytic contribution parameters.

[0013] Specifically, the stratified baseline correction for the characteristic process parameter sequence, converted characteristic parameter sequence, and product performance data of the detection group containing the titanium catalyst to be tested also includes: While performing baseline correction at each level, the average value of characteristic process parameters, the average value of converted characteristic parameters, the average value of product performance data, and the correction coefficient of the corresponding level are recorded simultaneously at each time point of the corresponding level benchmark detection group. The correction coefficient of the first level is the parameter value corresponding to the first level benchmark detection group, the correction coefficient of the second level is the reciprocal of the correction parameter value of the second level benchmark detection group corresponding to the first level, and the correction coefficient of the third level is the reciprocal of the correction parameter value of the third level benchmark detection group corresponding to the second level.

[0014] Specifically, the pure catalytic contribution parameters include the benchmarking factor of the third-level corrected characteristic process parameters, the benchmarking factor of the third-level corrected converted characteristic parameters, and the benchmarking factor of the third-level corrected product performance data. Specifically, the pure catalytic contribution parameters are decoupled and calculated in a multi-dimensional and multi-stage manner to quantify the catalytic activity, catalytic selectivity, and overall catalytic performance of the titanium-based catalyst under test, including: The third-level correction conversion characteristic parameter benchmarking factor was extracted from the pure catalytic contribution parameters of each reaction stage. The independent catalytic activity index of each reaction stage was obtained by kinetic weighting calculation in combination with the effective reaction time of each reaction stage. The independent catalytic activity index of all reaction stages was weighted and summed according to the process weight of each reaction stage to obtain the total catalytic activity index of the titanium catalyst to be tested. The performance data of the third-level modified product in the pure catalytic contribution parameters of each reaction stage were extracted and compared with the benchmark ratio. The side reaction inhibition index of each reaction stage was obtained by reciprocal conversion. The side reaction inhibition index of all reaction stages was weighted and summed according to the quality control weight to obtain the total catalytic selectivity index of the titanium catalyst to be tested. Based on the calculated total catalytic activity index and total catalytic selectivity index, weighted calculations and normalization conversions are performed according to preset application requirement weights to obtain the comprehensive catalytic performance score of the titanium catalyst under test.

[0015] A method for detecting the catalytic activity of a polyester titanium-based catalyst includes: The effective titanium mass fraction of the titanium-based catalyst to be tested after homogenization pretreatment was determined, and then the composition ratio of the basic common components and the differentiated catalyst components of each test group was configured. Based on the component ratio of the detection group, the homogenized materials prepared by each detection group are configured and put into the corresponding multi-stage series micro reactor group, and the reaction is started synchronously under the same control conditions. Collect characteristic process parameters of each reaction stage of the multi-stage series micro reactor group corresponding to each detection group, execute access control of each micro reactor group reaction stage, and obtain the effective reaction time and conversion characteristic parameters of each reaction stage. After each reaction stage, product performance data for each detection group corresponding to the reaction stage are collected. Based on each detection group type and the effective reaction time of each reaction stage, the characteristic process parameters and converted characteristic parameters of each reaction stage are classified, time series standardized and stratified baseline corrected to obtain pure catalytic contribution parameters. The pure catalytic contribution parameters were decoupled and calculated in a multidimensional and staged manner to quantify the catalytic activity, catalytic selectivity and comprehensive catalytic performance of the titanium-based catalyst under test.

[0016] The beneficial effects of this invention are: This invention eliminates interference from non-catalyst variables and establishes a unified detection benchmark by determining the effective titanium mass fraction and standardizing the effective titanium concentration of the titanium-based catalyst under test, configuring an experimental group with completely identical basic components and a three-layer reference control group; it employs a parallel multi-stage series micro-reactor group, with each reactor independently controlled, to synchronously start the entire continuous reaction simulation under the same conditions, which not only highly replicates the steady-state conditions of industrial polyester production, but also enables parallel synchronous detection of multiple samples, significantly improving detection efficiency and operating condition matching; through staged process monitoring and access control, it automatically and synchronously switches reaction stages and intercepts unqualified materials, avoiding the downward propagation of errors, while accurately... The study records the effective reaction time and characteristic parameters at each stage; it addresses the challenge of cross-sectional comparison caused by different reaction times through differentiated time series standardization; and systematically eliminates all non-catalytic interference factors through a three-layer progressive baseline correction system to obtain pure catalytic contribution parameters that reflect only the intrinsic performance of the catalyst. Finally, it performs multi-dimensional and multi-stage decoupled calculations on the pure catalytic contribution parameters to quantify catalytic activity, selectivity, and overall performance, achieving complete separation of activity and selectivity and independent characterization of the performance of each reaction stage. This makes the test results objective, repeatable, and highly consistent with industrial applications, providing accurate and reliable decision-making basis for the rapid screening, formulation optimization, and industrial substitution of titanium-based catalysts. Attached Figure Description

[0017] Figure 1 This is a schematic diagram of a polyester titanium catalyst catalytic activity detection system according to the present invention; Figure 2 This is a flowchart illustrating the access control process for each microreactor group during the reaction stage of this invention. Figure 3 This is a flowchart of step A3 of the present invention; Figure 4 The flowchart illustrates how to obtain pure catalytic contribution parameters and generate standardized performance parameters for this invention. Detailed Implementation

[0018] Example 1 Please see Figure 1This embodiment introduces a catalytic activity detection system for polyester titanium catalysts, including a detection group construction module, a reaction simulation module, a process monitoring module, a data processing module, and a decoupling quantification module; The detection group construction module is used to determine the effective titanium mass fraction of the titanium catalyst to be tested after homogenization pretreatment, and then configure the composition ratio of the basic common components and the differentiated catalyst components of each detection group; The basic common components refer to the reaction raw materials and auxiliaries that are completely consistent in type, ratio, and amount in all test groups. Specifically, they include: the basic reaction raw materials are terephthalic acid (PTA) and ethylene glycol (EG), with a molar ratio controlled at 1:(1.10–1.25), and an industrial standard ratio of 1:1.15 is used as an example; the auxiliaries are phosphorus-based stabilizers, selected from one of trimethyl phosphate, triphenyl phosphate, or triphenyl phosphite, with trimethyl phosphate used as an example, and the amount added is 15 ppm; the initial amount of PTA is consistent in all test groups, with an example single group amount of 200 g, and the amount of EG is calculated according to the above fixed molar ratio.

[0019] The effective titanium mass fraction refers to the proportion of catalytically active chelated titanium in the total mass of the titanium-based catalyst being tested. Based on this effective titanium mass fraction, the actual addition amount of each titanium-based catalyst sample is determined to ensure that the effective titanium concentration remains consistent across all test groups containing titanium-based catalysts.

[0020] The test group refers to a standardized reaction system that operates synchronously and in parallel under identical component ratios, initial operating conditions, and operational conditions. It is used to compare and test the catalytic activity of titanium-based catalysts. The system includes an experimental group and a control group, with differences between groups only in the catalyst composition. The experimental group consists of a reaction system with the titanium-based catalyst to be tested added, used to reflect the true catalytic activity, selectivity, and overall performance of the catalyst under simulated continuous industrial operating conditions. The control group is a pre-designed multi-level benchmark detection system, consisting of multiple benchmark detection groups with the same group proportions as the experimental group but differing only in catalyst composition. Different levels of benchmark detection groups correspond to correction benchmarks for different types of non-catalytic factors, used to establish a unified detection benchmark, eliminate interference from non-catalytic factors layer by layer, and complete industrial-scale calibration. The multi-level benchmark detection system contains at least three levels: the first level is a benchmark system without added catalytically active components, used to deduct the background contribution of the reaction system itself; the second level is a benchmark system with added general-purpose benchmark catalysts of known stability, used to correct systematic errors in the experimental process; and the third level is a benchmark system with added target-type benchmark catalysts with industry-recognized stable performance, used to achieve direct quantitative benchmarking between the tested catalyst and similar mature industrial products.

[0021] For example, the first-level benchmark detection group is a blank control group, without any catalyst added, used to subtract baseline interference from the thermal reaction and side reactions of the raw materials themselves; the second-level benchmark detection group is an industrial benchmark catalyst control group, with standard antimony glycol added, used to correct systematic errors such as operating condition fluctuations and equipment drift; the third-level benchmark detection group is a benchmark titanium catalyst control group, with industry-recognized stable standard titanium catalyst added, whose effective titanium concentration is consistent with the experimental group, used to achieve direct benchmarking between the test sample and mature industrial titanium catalysts.

[0022] Specifically, the detection group construction module is designed to address the shortcomings of existing polyester titanium catalyst activity testing processes, such as inconsistent component ratios, inaccurate effective titanium measurement, incomplete control systems, and susceptibility to non-catalytic interference. This module aims to accurately characterize the true catalytic activity of the catalyst under test. It adopts a method of first standardizing the basic components and then differentiating the catalyst configurations, completely fixing the ratios of all non-catalytically related raw materials and additives, thus eliminating interference from non-catalytic variables at the source. By quantitatively measuring the effective titanium mass fraction and standardizing the effective titanium concentration, it achieves equal activity comparison of the true catalytic capabilities between different titanium catalyst samples, eliminating detection bias caused by ineffective titanium components. By simultaneously constructing a complete control system including a blank control, an industrial benchmark catalyst control, and a benchmark titanium catalyst control, it layers and solidifies background interference, systematic errors, and industrial benchmarks, replacing the traditional single-control or no-control detection mode. By clarifying the rules for component ratios and feed calculation methods, it achieves standardized and reproducible detection group configuration, providing a unified, comparable, and reliable experimental benchmark system for subsequent multi-stage series reaction simulation, phased process monitoring, and multi-dimensional catalytic performance testing.

[0023] The reaction simulation module configures the homogenized materials prepared by each detection group based on the component ratio of the detection group, and puts them into the corresponding multi-stage series micro reactor group to start the reaction synchronously under the same control conditions.

[0024] The multi-stage series-connected microreactor groups are arranged in parallel. Each group consists of multiple microreactors connected in series and can independently simulate the steady-state conditions of each stage of continuous industrial polyester production. Each group contains a number of microreactors connected in series, corresponding to the number of reaction stages in the continuous industrial polyester production process. The number of microreactors is at least 3, preferably 5. For example, they correspond to the esterification I, esterification II, pre-condensation I, pre-condensation II, and final condensation reaction stages in the five-reactor continuous industrial production process. Each group also supports one detection unit. All materials in the test group independently complete the continuous reaction simulation of the entire process from esterification to final polycondensation. Each micro reactor corresponds to a reaction stage in the simulated industrial polyester production process, independently maintaining the preset steady-state conditions of that stage, realizing decoupled control of each reaction stage. Each micro reactor is equipped with an independent temperature control unit, pressure and vacuum adjustment unit, magnetic stirring unit, and staged devolatilization and reflux pipeline. Its operating parameters are not directly affected by the material state of the reactors before and after it. Structurally, it avoids the problems of mutual interference between stages and large deviations between operating conditions and industrial production in traditional single-reactor batch reactions.

[0025] The homogenized material refers to a uniformly dispersed system obtained by mixing the basic general components of the detection group with the differentiated catalyst components according to the component ratio, and then stirring and ultrasonically dispersing them. The catalyst components are uniformly dispersed in the raw material system as molecules or nano-sized particles, without agglomeration or sedimentation, ensuring that the catalytic active centers are evenly distributed during the reaction process, and avoiding uneven reaction rates and distortion of detection results caused by local concentration differences.

[0026] The same control conditions refer to the consistent initial operating conditions, process control conditions, and operating sequence conditions of all multi-stage series micro reactor groups in each reaction stage. Specifically, this includes: the same initial temperature, initial pressure, and initial stirring speed; the same heating rate, cooling rate, and vacuum extraction rate; the same reaction stage switching logic, material delivery sequence, and devolatilization reflux parameters; ensuring that the catalyst type is the only variable in all test groups, eliminating interference from non-catalytic factors from the reaction start-up stage, and guaranteeing the comparability and repeatability of test results.

[0027] Specifically, the reaction simulation module is designed to address the shortcomings of existing polyester titanium catalyst activity detection methods, such as distorted simulation of operating conditions, low detection efficiency, severe coupling of reaction stages, and poor consistency of parallel experiments. Industrial polyester production adopts a continuous steady-state process, with each reaction stage operating under fixed temperature, pressure, and residence time. The material flows continuously, and the operating conditions of each stage are independent. In contrast, traditional single-reactor batch reactions are non-steady-state processes with varying temperature, pressure, and concentration, which cannot reproduce the steady-state reaction environment of each stage in industrial production, resulting in large deviations between the detection results and actual industrial applications. Existing multi-reactor devices mostly use a shared control system, which cannot achieve independent steady-state control of each reaction stage. Fluctuations in the material state of the previous stage are directly transmitted to the next stage, making it impossible to decouple the differences in catalytic activity between different stages. This module aims to highly replicate continuous steady-state industrial operating conditions and achieve parallel and synchronous detection of multiple samples. It employs a multi-stage, parallel, series-connected micro-reactor architecture, with each reactor group independently corresponding to a detection group, enabling the simultaneous detection of multiple samples. By configuring independent control units and piping systems for each stage of the micro-reactor, complete decoupling control of each reaction stage is achieved, allowing each reactor to independently maintain preset steady-state conditions unaffected by the material states of preceding and following stages. Unified control of the initial conditions, process parameters, and operating sequence of all reactor groups ensures that all detection groups operate synchronously under identical conditions. An automated material conveying system enables automatic switching between reaction stages, eliminating timing errors caused by manual operation. This fundamentally solves the problems of distortion and poor parallelism in traditional single-reactor batch reaction simulations, providing a realistic, stable, and comparable reaction basis for subsequent staged process monitoring, data acquisition, and precise catalytic performance detection.

[0028] The process monitoring module collects characteristic process parameters of each reaction stage of the multi-stage series micro reactor group corresponding to each detection group, executes access control for each reaction stage of the micro reactor group, and obtains the effective reaction time and conversion characteristic parameters of each reaction stage to prevent unqualified materials from entering the next stage and causing chain deviations, while automatically terminating invalid experiments.

[0029] Please see Figure 2 Furthermore, the specific steps for implementing access control for each microreactor group's reaction stage include: A1: For each stage of the micro reactor, pre-set a reasonable fluctuation range and a fixed reaction time for the characteristic process parameters that are consistent across all detection groups; The reasonable fluctuation range of the characteristic process parameters is set according to the process control points of the corresponding stage of continuous industrial polyester production. It is the allowable deviation range of each measurable parameter under normal catalytic reaction and is used to judge whether the equipment operating status is stable in real time. If the characteristic process parameters exceed the reasonable fluctuation range, the equipment warning will be triggered. The fixed reaction time is set based on the average residence time of the corresponding stage in the continuous production of industrial polyester, and is 1.1–1.2 times the time required for the benchmark titanium catalyst control group to complete the reaction of this stage. This ensures that all catalysts with industrial application value can reach the industrial required reaction level within this time, and also ensures that low-activity systems such as blank control groups can complete the entire process reaction. For example, the parameters for each stage are set as follows: Esterification Stage 1: Fixed reaction time 60 min; reasonable fluctuation range of characteristic process parameters: reaction temperature 255±1℃, internal pressure 0.25±0.02MPa, condensate output 18–30 mL; Esterification Stage 2: Fixed reaction time 40 min; reasonable fluctuation range of characteristic process parameters: reaction temperature 260±1℃, internal pressure 0.10±0.01MPa, cumulative condensate output 32–35 mL; Pre-condensation Stage 1: Fixed reaction time 30 min; reasonable fluctuation range of characteristic process parameters... The reaction temperature was 265±1℃, the system vacuum degree was 50±5kPa, and the stirring torque was 0.8–1.5N・m; the pre-condensation stage was fixed at a reaction time of 40min; the reasonable fluctuation range of characteristic process parameters was a reaction temperature of 270±1℃, a system vacuum degree of 5±1kPa, and a stirring torque of 1.8–2.8N・m; the final condensation stage was fixed at a reaction time of 90min; the reasonable fluctuation range of characteristic process parameters was a reaction temperature of 275±1℃, a system vacuum degree of <100Pa, and a stirring torque of 3.5–5.0N・m.

[0030] A2: After the testing team starts the multi-stage series-connected microreactor group, the online monitoring unit in each stage of the microreactor collects the characteristic process parameters of that reaction stage in real time at a preset acquisition frequency. These characteristic process parameters refer to physical parameters that can be directly and quantitatively acquired online and have a linear correlation with the reaction progress and product quality, including: reaction temperature, pressure inside the reactor, system vacuum, stirring torque, condensate output during the esterification stage, and stirring power during the pre-condensation and final condensation stages. The online monitoring unit refers to an industrial-grade standard sensing device integrated into the body of each stage of the microreactor and its supporting pipelines, capable of simultaneous acquisition of multiple parameters and real-time data upload, providing continuous and reliable data for process monitoring and subsequent performance testing. The data support includes: a temperature sensor installed in the jacket and material layer inside the microreactor; a pressure sensor installed on the top of the microreactor; a vacuum sensor installed in the gas phase pipeline of the microreactor; a weighing-type water output monitoring device installed below the condensate collection bottle; a non-invasive torque sensor installed on the output shaft of the stirring motor; and an online Fourier transform infrared spectrometer installed in the liquid phase pipeline of the microreactor to assist in verifying the esterification rate and terminal carboxyl content. The preset acquisition frequency is set to ensure data continuity to accurately capture the reaction kinetic curve while avoiding redundant data that would increase the system's computational load. For example, the preset acquisition frequency is 1–10 seconds / time, preferably 5 seconds / time.

[0031] A3: Based on the quantification of characteristic process parameters, the corresponding reaction process conversion characteristic parameters are obtained to determine whether the corresponding reaction process has been completed, and combined with a reasonable fluctuation range, it is determined whether the corresponding reaction process has abnormal operating conditions. Please see Figure 3 Furthermore, A3 includes: A31: Continuously compare the real-time collected characteristic process parameters with the preset reasonable fluctuation range of the corresponding reaction stage. If any characteristic process parameter exceeds the reasonable fluctuation range and the duration reaches the preset anomaly judgment time, it is determined that the detection group has an abnormal condition. The reaction process corresponding to the detection group is automatically terminated, the group is marked as an abnormal condition group, and no more materials are supplied to the next level micro-reactor. The preset anomaly judgment time refers to the shortest duration used to eliminate instantaneous interference from sensors and ensure the accuracy of anomaly judgment. Its setting is based on the response time of industrial-grade sensing devices and the parameter fluctuation characteristics of the polyester reaction system. For example, the preset anomaly judgment time is 5 minutes. If all characteristic process parameters are within the reasonable fluctuation range, the current reaction stage continues to react. A32: Based on real-time acquired characteristic process parameters, the corresponding conversion characteristic parameters of the reaction process are extracted; the conversion characteristic parameters refer to derived parameters that can directly characterize the reaction completion degree and product quality, including the esterification rate in the esterification stage and the melt intrinsic viscosity in the pre-condensation and final condensation stages; based on the parameter conversion relationship calibrated and solidified in advance through offline standard detection methods, the corresponding conversion characteristic parameters of the reaction process are quantified through real-time acquired characteristic process parameters; the parameter conversion relationship calibrated and solidified by offline standard detection methods refers to a pre-established function or curve model that maps the real-time acquired process parameters to the reaction process characteristic parameters, wherein the esterification rate is calculated by the ratio of the condensate output to the theoretical output of PTA after complete esterification, and the melt intrinsic viscosity is converted by the stirring torque and the pre-established torque-viscosity calibration curve; The process of establishing the torque-viscosity calibration curve includes: selecting multiple sets of standard samples with the same formulation and process conditions as the target polymerization reaction system, collecting the corresponding stirring torque values ​​at different reaction stages, and simultaneously measuring the melt intrinsic viscosity of each standard sample using the offline Ubbelohde viscometer standard method. Linear or nonlinear regression fitting is performed on the collected torque-viscosity data points to obtain the corresponding relationship curve between torque and intrinsic viscosity, which is then stored. For example, the standard threshold for the degree of reaction in the first stage of esterification is an esterification rate ≥ 85%, the standard threshold for the degree of reaction in the second stage of esterification is an esterification rate ≥ 96%, the standard threshold for the degree of reaction in the first stage of pre-polymerization is an intrinsic viscosity ≥ 0.15 dL / g, the standard threshold for the degree of reaction in the second stage of pre-polymerization is an intrinsic viscosity ≥ 0.35 dL / g, and the standard threshold for the degree of reaction in the final stage of polycondensation is an intrinsic viscosity ≥ 0.65 dL / g. A33: If the converted characteristic parameter of a certain detection group reaches the standard threshold of the reaction degree of the corresponding reaction stage and the fluctuation range does not exceed the preset allowable deviation for a time that reaches the preset stability judgment time, then the reaction of this reaction stage of the detection group is determined to be completed, and the steady-state maintenance mode is automatically triggered; the preset allowable deviation is set according to the process control accuracy requirements of industrial polyester production, and it is negatively correlated with the process control accuracy, that is, the higher the process control accuracy, the smaller the value of the preset allowable deviation; the preset stability judgment time is set according to the parameter response time of the reaction system to ensure that the detected parameter stability signal excludes instantaneous fluctuation interference. The parameter response time refers to the time required for the corresponding characteristic process parameter or converted characteristic parameter to stabilize within the target fluctuation range in the polyester reaction system from the change of reaction conditions; for example, the preset allowable deviation is ±0.5%, and the preset stability judgment time is 30s; The steady-state maintenance mode refers to automatically adjusting the reaction conditions of the micro reactor corresponding to the detection group to a low-side-reaction maintenance condition. Specifically, this includes: reducing the reaction temperature by 5–10°C, reducing the stirring speed by 30%, and closing the staged devolatilization pipeline and the reflux pipeline to suppress excessive esterification, thermal degradation, and other side reactions. In the steady-state maintenance mode, the online monitoring unit continues to collect all characteristic process parameters at a preset acquisition frequency.

[0032] A4: When the cumulative reaction time of a certain micro-reactor reaches the preset fixed reaction time, all detection groups simultaneously determine that the reaction stage has ended; synchronously record the characteristic process parameters and conversion characteristic parameters of the steady-state maintenance stage corresponding to the steady-state maintenance mode of each detection group, and automatically and synchronously open the material conveying valves between the current micro-reactor and the next-level micro-reactor of all detection groups, synchronously and quantitatively conveying all materials in each micro-reactor to the next-level micro-reactor, while recording the effective reaction time, characteristic process parameters, and conversion characteristic parameters of the reaction stage; the effective reaction time refers to the time from the start of the reaction stage to the determination of the reaction completion by the detection group; after the conveying is completed, automatically and synchronously close all material conveying valves, and synchronously trigger the start command of the next-level micro-reactor of all detection groups; the start command refers to the control signal used to control the next-level micro-reactor to start the preset steady-state working condition of the corresponding reaction stage, including all process parameters such as the preset temperature, pressure, vacuum degree, and stirring speed of the next-level reaction stage, after triggering, the next-level micro-reactors of all detection groups synchronously start heating, stirring, vacuum adjustment, etc., and enter the corresponding reaction stage; Specifically, the process monitoring module is designed to address the shortcomings of existing polyester catalyst activity testing methods, such as the lack of entry criteria for reaction stages, the chain reaction of non-compliant materials, the inability to automatically terminate invalid experiments, and the lack of traceability of process data. In continuous polyester production, the processes of each reaction stage are interconnected. If the materials in the previous stage fail to meet the standards and proceed to the next stage, it will lead to the accumulation of side reactions, viscosity runaway, and non-compliant endpoint products, thereby causing distortion in catalytic activity testing. Traditional testing methods only focus on the final product indicators, lack the logic for judging the process in different stages, cannot identify stage anomalies, and rely on manual judgment and manual switching, which is prone to human error and timing disorder. At the same time, it cannot terminate samples that fail to meet the standards within the time limit in a timely manner, resulting in energy waste and data interference. This module aims to ensure full process control and prevent error propagation. It establishes quantifiable stage entry standards by pre-setting acceptable thresholds and maximum reaction times for each reaction stage; it dynamically tracks the reaction process by collecting multi-dimensional characteristic parameters in real time through an online monitoring unit; it avoids misjudgments caused by instantaneous fluctuations and ensures reliable stage switching through a parameter stability and compliance determination mechanism; it achieves automated connection between stages by automatically executing material delivery and stage start / stop control; and it directly terminates the reaction and marks abnormal samples that fail to meet the time limit, preventing the propagation of unqualified materials and the continuation of invalid experiments. Simultaneously, it fully records the time consumption and endpoint characteristic parameters of each stage, providing reliable process data support for subsequent precise decoupling and traceability of catalytic performance.

[0033] The data processing module is used to collect product performance data for each reaction stage after each reaction stage is completed. Based on the type of each detection group and the effective reaction time of each reaction stage, it classifies and organizes the characteristic process parameters and converted characteristic parameters of each reaction stage, performs time series standardization and stratified baseline correction, obtains pure catalytic contribution parameters, and generates a standardized performance parameter set. This provides a unified and pure data foundation for the subsequent quantitative detection of the activity, selectivity and comprehensive performance of titanium catalysts.

[0034] Please see Figure 4 Furthermore, the steps for obtaining pure catalytic contribution parameters and generating standardized performance parameters include: B1: Extract the effective reaction time, characteristic process parameters, and converted characteristic parameters for each reaction stage of each detection group, as well as the product performance data after the reaction stage. Construct characteristic process parameter sequences and converted characteristic parameter sequences according to the collection time. The product performance data refers to the physicochemical parameters that can quantitatively characterize the molecular structure, quality, and degree of side reactions of the product obtained by offline standard detection methods after each reaction stage, including the end carboxyl group content in the esterification stage, the intermediate hue index in the pre-condensation stage, the melt intrinsic viscosity, end carboxyl group content, hue L value and b value, and molecular weight distribution index in the final condensation stage.

[0035] B2: Calculate the average and range of the effective reaction time for the same reaction stage in all detection groups, and determine whether the ratio of the range to the average is less than the preset deviation threshold; if so, perform simple time series standardization; otherwise, perform dual-mode time series standardization; the preset deviation threshold is set according to the allowable error of parallel experiments for industrial polyester catalyst detection, for example, the preset deviation threshold is 5%.

[0036] Furthermore, performing simple time series standardization includes: B21.1: Determine a uniform number of sampling points based on the average effective reaction time of all test groups in this reaction phase. B21.2: For the characteristic process parameter sequences and converted characteristic parameter sequences of each detection group at this reaction stage, a linear interpolation method is used to resample, generating a standardized time series of characteristic process parameter sequences and converted characteristic parameter sequences with the same length as the reference time and the same number of sampling points; B21.3: Using the system's unified clock as a reference, align the timestamps of all characteristic process parameter sequences with the converted characteristic parameter sequences to ensure that the data from different detection groups at the same time point are directly comparable.

[0037] Furthermore, performing dual-mode time series standardization includes: B22.1: Retain the original characteristic process parameter sequence and the original converted characteristic parameter sequence of each detection group for this reaction stage, retain its original sampling time axis and complete fixed reaction time length, without performing any interpolation or truncation processing; B22.2: Normalize the time axis of the characteristic process parameter sequence and the converted characteristic parameter sequence of each detection group for this reaction stage to the interval [0,1], where 0 corresponds to the start time of the reaction stage and 1 corresponds to the completion time of this stage of the detection group; select normalized time points at equal intervals within the interval [0,1], and use linear interpolation to calculate the characteristic process parameter value and the converted characteristic parameter value corresponding to each normalized time point, generating a normalized time series of the characteristic process parameter sequence and the converted characteristic parameter sequence, which is used to compare the parameter differences of different detection groups under the same reaction progress.

[0038] B3: If simple time series standardization is performed, then based on the unified absolute time axis of the standardized time series obtained by simple time series standardization, the characteristic process parameters, converted characteristic parameters, and product performance data of the detection group of the titanium catalyst under test and each benchmark detection group at the same absolute time point are stratified and baseline corrected to obtain the pure catalytic contribution parameters. The stratified baseline correction includes: first-level background baseline correction, second-level systematic error correction, and third-level benchmark correction. The pure catalytic contribution parameter refers to the standardized relative performance parameter determined solely by the intrinsic catalytic performance differences of the tested titanium catalyst after systematically eliminating all non-catalytic interferences through the progressive stratified baseline correction process. This includes three categories: the benchmarking factor of the third-level corrected characteristic process parameter, the benchmarking factor of the third-level corrected converted characteristic parameter, and the benchmarking factor of the third-level corrected product performance data. The benchmarking factor of the third-level corrected characteristic process parameter is the relative value of the corresponding parameter of the tested titanium catalyst after three-level correction, reflecting the degree of influence of the catalyst on the physical state of the reaction system. The benchmarking factor of the third-level corrected converted characteristic parameter is the relative value of the corresponding parameter of the tested titanium catalyst after three-level correction, directly quantitatively characterizing the stage-wise catalytic activity of the catalyst. The benchmarking factor of the third-level corrected product performance data is the relative value of the corresponding parameter of the tested titanium catalyst after three-level correction, directly quantitatively characterizing the stage-wise catalytic selectivity of the catalyst.

[0039] Furthermore, stratified baseline correction is performed on the characteristic process parameter sequences, converted characteristic parameter sequences, and product performance data of the detection group containing the titanium-based catalyst under test, including: B31: Perform first-level baseline correction by calculating the difference between the characteristic process parameter values ​​and converted characteristic parameter values ​​of each reaction stage in the detection group of the titanium catalyst under test and the characteristic process parameter values ​​and converted characteristic parameter values ​​of the corresponding reaction stage and the same reference point in the first-level benchmark detection group; calculate the difference between the single-point values ​​of product performance data of each reaction stage in the detection group of the titanium catalyst under test and the single-point values ​​of product performance data of the corresponding reaction stage and the same reference point in the first-level benchmark detection group; obtain the first-level correction parameters; the same reference point refers to the same absolute time point under simple time series standardization and the same relative reaction progress point under dual-mode time series standardization; the first-level correction parameters refer to the pure catalytic contribution basic parameters obtained after the first-level baseline correction, including three categories: first-level corrected characteristic process parameter values, first-level corrected converted characteristic parameter values, and first-level corrected product performance data values.

[0040] B32: Perform second-level systematic error correction by comparing the first-level corrected characteristic process parameter values ​​and first-level corrected converted characteristic parameter values ​​(after first-level background baseline correction) with the first-level corrected characteristic process parameter values ​​and first-level corrected converted characteristic parameter values ​​at the same reference point in the corresponding reaction stage of the second-level benchmark detection group. Also, compare the first-level corrected product performance data values ​​(after first-level background baseline correction) with the first-level corrected product performance data values ​​at the same reference point in the corresponding reaction stage of the second-level benchmark detection group. This yields the second-level correction parameters. These second-level correction parameters are standardized catalytic contribution parameters obtained after second-level systematic error correction, including three categories: relative coefficients of second-level corrected characteristic process parameters, relative coefficients of second-level corrected converted characteristic parameters, and relative coefficients of second-level corrected product performance data. These parameters completely eliminate the dual interference of the reaction system background and experimental systematic errors, retaining only the relative performance contribution of the catalytically active components, eliminating systematic differences between different experimental batches, and serving as standardized data for subsequent third-level benchmark correction.

[0041] B33: Perform third-level benchmark correction. Ratio the relative coefficients of the second-level corrected characteristic process parameters and the relative coefficients of the second-level corrected converted characteristic parameters (after second-level system error correction) with the relative coefficients of the second-level corrected characteristic process parameters and the relative coefficients of the second-level corrected converted characteristic parameters at the corresponding reaction stage and the same benchmark point in the third-level benchmark detection group. Ratio the relative coefficients of the second-level corrected product performance data (after second-level system error correction) with the relative coefficients of the second-level corrected product performance data at the corresponding reaction stage and the same benchmark point in the third-level benchmark detection group. This yields the third-level correction parameters. The third-level correction parameters refer to the parameters obtained after third-level benchmarking. The relative performance parameters obtained after benchmark correction include three categories: the benchmarking ratio of the third-level correction characteristic process parameters, the benchmarking ratio of the third-level correction converted characteristic parameters, and the benchmarking ratio of the third-level correction product performance data. This parameter has completely eliminated the interference of all non-catalytic factors and only reflects the intrinsic performance difference of the tested titanium-based catalyst relative to the industry benchmark product. Among them, the benchmarking ratio of the third-level correction converted characteristic parameters is greater than 1, indicating that the activity of the tested catalyst is better than that of the benchmark product, and the larger the value, the higher the activity. The benchmarking ratio of the third-level correction product performance data is less than 1, indicating that the selectivity of the tested catalyst is better than that of the benchmark product, and the smaller the value, the stronger the side reaction control ability. It can be directly used for horizontal comparison and ranking of catalyst performance.

[0042] B34: While performing baseline correction at each level, simultaneously record the average value of characteristic process parameters, the average value of converted characteristic parameters, the average value of product performance data, and the correction coefficient for each level of the baseline detection group at each reference point under the corresponding reference axis. The correction coefficient for the first level is the parameter value of the corresponding reference point in the first level baseline detection group; the correction coefficient for the second level is the reciprocal of the first level correction parameter value for the corresponding reference point in the second level baseline detection group; and the correction coefficient for the third level is the reciprocal of the second level correction parameter value for the corresponding reference point in the third level baseline detection group. All correction coefficients are bound to the corrected parameters and stored one-to-one to ensure that all correction processes are traceable and reproducible, facilitating subsequent data backtracking and error analysis.

[0043] For example, taking the esterification rate parameter of the first esterification stage, the melt intrinsic viscosity parameter of the final polycondensation stage, and the terminal carboxyl group content parameter as examples, the complete layered baseline correction process is as follows: First-level baseline correction: If the esterification rate of the experimental group of titanium catalyst under test is 75% at the 30th minute of the first stage of esterification, and the esterification rate of the blank control group (first-level benchmark detection group) is 12% at the same time point, then the first-level corrected esterification rate is 75%-12%=63%; If the end carboxyl group content of the experimental group under test is 22mol / t in the final polycondensation stage, and the end carboxyl group content of the blank control group is 15mol / t in the final polycondensation stage, then the first-level corrected end carboxyl group content is 22-15=7mol / t.

[0044] Second-level systematic error correction: If the first-level corrected esterification rate of the antimony glycol reference group (second-level reference detection group) at the 30th minute of the first stage of esterification is 58%, then the relative coefficient of the second-level corrected esterification rate is 63% / 58%=1.086; if the first-level corrected melt intrinsic viscosity of the antimony glycol reference group in the final polycondensation stage is 0.62 dL / g, and the corresponding first-level correction value of the test group is 0.68 dL / g, then the relative coefficient of the second-level corrected intrinsic viscosity is 0.68 / 0.62=1.097.

[0045] Third-level benchmark correction: If the relative coefficient of the second-level corrected esterification rate of the benchmark titanium catalyst group (third-level benchmark detection group) at 30 minutes of the first stage of esterification is 1.05, then the benchmark ratio of the third-level corrected esterification rate is 1.086 / 1.05=1.034, indicating that the activity of the tested catalyst in the first stage of esterification is 1.034 times that of the benchmark titanium catalyst; if the relative coefficient of the second-level corrected end carboxyl content in the final polycondensation stage of the benchmark titanium catalyst group is 1.2, then the benchmark ratio of the third-level corrected end carboxyl content is 7mol / t / 1.2=5.83, indicating that the side reaction control ability of the tested catalyst is better than that of the benchmark titanium catalyst.

[0046] B4: Based on the pure catalytic contribution parameters after hierarchical baseline correction, the characteristic process parameter sequence after time series standardization, the converted characteristic parameter sequence, the original characteristic process parameter sequence, and the converted characteristic parameter sequence, an independent phased structured parameter unit is constructed for each detection group to form a standardized performance parameter set, realizing phased decoupling and standardized storage of catalytic performance; the structure of all phased structured parameter units is completely unified, the parameter names and data formats are fixed, and it supports direct extraction and batch calculation by the decoupled quantization module.

[0047] Furthermore, the phased construction of structured parametric units includes: B41: Each detection group corresponds to an independent staged structured parameter unit. The staged structured parameter unit takes the reaction stage as the first level and constructs sub-units for each reaction stage. Each reaction stage sub-unit takes the parameter category as the second level and includes effective reaction time, characteristic process parameter sequence, converted characteristic parameter sequence, standardized time series, normalized time series, pure catalytic contribution parameter, and correction coefficient. B42: Fill the effective reaction time of each reaction stage in each detection group into the effective reaction time parameter position of the corresponding reaction stage subunit; fill the characteristic process parameter sequence constructed by the acquisition of each reaction stage in each detection group into the characteristic process parameter sequence position of the corresponding reaction stage subunit; fill the converted characteristic parameter sequence constructed by the acquisition of each reaction stage in each detection group into the converted characteristic parameter sequence position of the corresponding reaction stage subunit; if the reaction stage performs simple time series standardization, fill the corresponding generated standardized time series into the standardized time series position of the corresponding reaction stage subunit; if the reaction stage performs dual-mode time series standardization, fill the corresponding generated normalized time series into the normalized time series position of the corresponding reaction stage subunit; fill the pure catalytic contribution parameter obtained by stratified baseline correction into the pure catalytic contribution parameter position of the corresponding reaction stage subunit; fill the correction coefficients of the first level, the second level, and the third level recorded in B34 into the correction coefficient position of the corresponding reaction stage subunit.

[0048] Specifically, the data processing module is designed to address the shortcomings of existing polyester titanium catalyst activity testing methods, such as inconsistent data formats, mismatched time lengths, failure to systematically eliminate interference from non-catalytic factors, and inability to achieve staged performance decoupling. Traditional testing methods often directly compare raw data without considering the time incomparability caused by differences in reaction times between different test groups, and without systematically eliminating interference from spontaneous reactions of raw materials and systematic errors, resulting in large deviations and poor repeatability of test results. This module aims to build a unified, clean, and decoupled foundation for detection data. It achieves standardized data classification through raw data categorization; employs a differentiated time-series standardization strategy to balance data processing efficiency and detection accuracy, resolving the challenge of cross-sectional comparisons due to significant differences in reaction time while preserving the original information of reaction kinetics; utilizes a three-layer baseline correction system to completely eliminate interference from non-catalytic factors, obtaining pure contribution parameters that reflect only the intrinsic performance of the catalyst; and achieves seamless integration of data with subsequent detection algorithms through the construction of structured, staged parameter units and the output of standardized datasets. This provides solid data support for the precise quantitative detection, staged performance decoupling, and industrial adaptability screening of titanium-based catalysts.

[0049] The decoupled quantification module performs multidimensional and multi-stage decoupled calculations on the pure catalytic contribution parameters, quantifying the catalytic activity, catalytic selectivity, and overall catalytic performance of the titanium catalyst under test, and outputting quantitative detection results that can be directly used for industrial screening.

[0050] Furthermore, the pure catalytic contribution parameters were decoupled and calculated in a multi-dimensional and multi-stage manner to quantify the catalytic activity, catalytic selectivity, and overall catalytic performance of the tested titanium-based catalysts, including: C1: The benchmark ratio of the third-level corrected conversion characteristic parameter in the pure catalytic contribution parameters of each reaction stage is extracted as the core quantitative basis for catalytic activity. Specifically, the benchmark ratio of the third-level corrected conversion characteristic parameter corresponding to the esterification rate is used for the esterification stage, and the benchmark ratio of the third-level corrected conversion characteristic parameter corresponding to the melt intrinsic viscosity is used for the pre-condensation and final condensation stages. Combined with the effective reaction time of each reaction stage, a kinetic weighted calculation is performed to obtain the independent catalytic activity index of each reaction stage. Then, the independent catalytic activity indices of all reaction stages are weighted and summed according to the process weight of each reaction stage in industrial polyester production to obtain the total catalytic activity index of the titanium catalyst under test. Both the independent catalytic activity index and the total catalytic activity index being greater than 1 indicate that the catalytic activity in the corresponding dimension is superior to the benchmark titanium catalyst; the larger the value, the higher the catalytic activity. Kinetic weighted calculation refers to the calculation method of multiplying the benchmark ratio of the third-level corrected conversion characteristic parameter with the relative value of the effective reaction time of the reaction stage. This method is used to simultaneously quantify the catalyst's ability to improve both the degree and rate of reaction. Specifically: Independent catalytic activity index = third-level corrected conversion characteristic parameter benchmarking ratio × (effective reaction time of the corresponding reaction stage of the benchmark titanium catalyst / effective reaction time of the corresponding reaction stage of the titanium catalyst under test); Process weight refers to the pre-set percentage coefficient of each reaction stage's contribution to the overall catalytic activity. It is set based on the process importance of each reaction stage in the continuous production of industrial polyester and its impact on the overall production efficiency. For example, the process weight of the first esterification stage is 0.15, the process weight of the second esterification stage is 0.15, the process weight of the first pre-polymerization stage is 0.15, the process weight of the second pre-polymerization stage is 0.2, and the process weight of the final polycondensation stage is 0.35.

[0051] C2: The benchmark ratio of the third-level modified product performance data in the pure catalytic contribution parameters of each reaction stage is extracted as a quantitative basis for the degree of side reaction. Specifically, the benchmark ratio of the third-level modified product performance data corresponding to the end carboxyl group content is used in the esterification stage; the benchmark ratio of the third-level modified product performance data corresponding to the intermediate hue b value is used in the pre-condensation stage; and the benchmark ratio of the third-level modified product performance data corresponding to the end carboxyl group content, hue b value, and molecular weight distribution index is used in the final condensation stage. The side reaction inhibition index of each reaction stage is obtained by reciprocal conversion of the above benchmark ratios. Then, the side reaction inhibition index of all reaction stages is weighted and summed according to the quality control weight of industrial polyester products to obtain the total catalytic selectivity index of the titanium catalyst to be tested. The side reaction inhibition index and the total catalytic selectivity index are quantitative indicators that characterize the ability of the catalyst to inhibit side reactions from two dimensions: single stage and whole process. A value greater than 1 indicates that the catalytic selectivity of the corresponding dimension is better than that of the benchmark titanium catalyst. The larger the value, the stronger the side reaction control ability. Quality control weights refer to the pre-set percentage coefficients of the performance indicators of each product at each reaction stage on the quality of the final product. They are set based on the national standard requirements for industrial polyester products and the quality control priorities of downstream applications such as spinning and bottle chips. For example, the quality control weight of the end carboxyl content in the esterification stage is 0.2, the quality control weight of the intermediate hue b value in the pre-condensation stage is 0.2, and the quality control weight of the end carboxyl content, hue b value, and molecular weight distribution index in the final condensation stage is 0.25.

[0052] C3: Based on the calculated total catalytic activity index and total catalytic selectivity index, the two are weighted according to preset application requirement weights. Then, using the comprehensive catalytic performance score of the benchmark titanium catalyst as the baseline value of 100, the weighted calculation result is normalized to obtain the comprehensive catalytic performance score of the titanium catalyst under test, achieving a unified horizontal comparison between different test samples. The application requirement weight consists of an activity weight and a selectivity weight, the sum of which is always 1. The weight is set based on the contribution ratio of the total catalytic activity index and the total catalytic selectivity index to the comprehensive score. It is directly determined according to the quantitative proportion of the two types of pure catalytic contribution parameters in the staged decoupling calculation. A higher activity contribution ratio results in a larger activity weight, and a higher selectivity contribution ratio results in a larger selectivity weight. When the two contribution ratios are similar, equal weights are used. For example, when the reaction rate and conversion efficiency are the main detection targets, the activity weight is set to 0.7 and the selectivity weight is set to 0.3.

[0053] C4: The performance grade of the titanium catalyst under test is determined according to the preset performance grade classification threshold. The performance grade classification threshold refers to the pre-set comprehensive catalytic performance score range used to distinguish the industrial application value of the catalyst. It is set based on the actual needs of industrial polyester production for catalyst performance and combined with the industry's common catalyst screening standards. The excellent grade corresponds to performance that is significantly better than the benchmark product and can be directly replaced in industrial production. The good grade corresponds to performance that is comparable to the benchmark product and can be used in industrial trials. The medium grade corresponds to performance that is slightly lower than the benchmark product and requires further optimization of the formula. The poor grade corresponds to performance that does not meet the requirements of industrial production and has no application value. For example, a comprehensive catalytic performance score ≥110 is judged as excellent, 100≤comprehensive catalytic performance score<110 is judged as good, 90≤comprehensive catalytic performance score<100 is judged as medium, and comprehensive catalytic performance score<90 is judged as poor. At the same time, all the titanium catalysts under test in the same batch are sorted from high to low according to their comprehensive catalytic performance scores to generate a performance ranking list containing all the titanium catalysts under test.

[0054] Specifically, the decoupling and quantification module is designed to address the shortcomings of existing detection methods for polyester titanium catalysts, such as the inability to separate the coupling between activity and selectivity, the difficulty in quantifying contributions at different stages, and the strong subjectivity of the detection results. Traditional detection methods rely solely on the final product state for qualitative judgment, failing to distinguish the true contribution of the catalyst in each stage of esterification, pre-condensation, and final condensation, and also struggling to balance the relationship between activity enhancement and side reaction control. This module uses pure catalytic contribution parameters as the sole calculation basis, achieving complete decoupling of activity and selectivity and independent quantification of performance at each reaction stage. Through a unified weighting and standardized scoring system, it eliminates human judgment errors, making the detection results objective, repeatable, and comparable across different reactions. By directly outputting performance levels and industrial suitability conclusions, it provides accurate and reliable data support for the rapid screening, formulation optimization, and industrial substitution applications of titanium catalysts.

[0055] Example 2 This embodiment describes a method for detecting the catalytic activity of a polyester titanium-based catalyst, including: The effective titanium mass fraction of the titanium-based catalyst to be tested after homogenization pretreatment was determined, and then the composition ratio of the basic common components and the differentiated catalyst components of each test group was configured. Based on the component ratio of the detection group, the homogenized materials prepared by each detection group are configured and put into the corresponding multi-stage series micro reactor group, and the reaction is started synchronously under the same control conditions. Collect characteristic process parameters of each reaction stage of the multi-stage series micro reactor group corresponding to each detection group, execute access control of each micro reactor group reaction stage, and obtain the effective reaction time and conversion characteristic parameters of each reaction stage. After each reaction stage, product performance data for each detection group corresponding to the reaction stage are collected. Based on each detection group type and the effective reaction time of each reaction stage, the characteristic process parameters and converted characteristic parameters of each reaction stage are classified, time series standardized and stratified baseline corrected to obtain pure catalytic contribution parameters. The pure catalytic contribution parameters were decoupled and calculated in a multidimensional and staged manner to quantify the catalytic activity, catalytic selectivity and comprehensive catalytic performance of the titanium-based catalyst under test.

[0056] Working principle and its effects: The core working principle of this invention is to systematically eliminate various interfering factors in the detection process of polyester titanium catalysts through a closed-loop system of full-process variable control, precise simulation of industrial conditions and decoupling and quantification of pure catalytic performance. This achieves objective and accurate characterization of catalytic performance and fundamentally solves the industry pain points of low condition matching, distorted results and inability to decouple traditional detection methods.

[0057] First, the effective titanium mass fraction of the titanium-based catalysts under test was determined, and the effective titanium concentration of all titanium-containing catalyst test groups was standardized. Simultaneously, a three-tiered progressive benchmark test group system was constructed to fix all non-catalytic variables from the experimental design stage, establishing a unified test benchmark and ensuring direct comparability between different catalyst samples. A multi-stage series micro-reactor group with parallel arrangement and independent control conditions at each stage was employed to synchronously start the entire continuous reaction simulation under identical control conditions. This highly replicates the steady-state operating conditions of industrial polyester production and enables parallel synchronous testing of multiple sample groups, significantly improving detection efficiency and the parallelism of results. Through a phased process monitoring and access control mechanism, characteristic parameters of each reaction stage were collected in real time, and the reaction progress and abnormal conditions were automatically determined. The system synchronously completes material delivery and reaction stage switching for all detection groups at fixed reaction time nodes, accurately records the effective reaction time and key parameters at each stage, and intercepts unqualified materials to prevent errors from propagating downwards. The collected time-series data is processed using differentiated time series standardization to solve the problem of horizontal comparison caused by the difference in reaction time of different catalysts. Then, a three-layer progressive baseline correction is used to successively eliminate background interference, systematic errors, and cross-system differences, extracting pure catalytic contribution parameters that only reflect the intrinsic performance of the catalyst. Finally, based on the pure catalytic contribution parameters, multi-dimensional and multi-stage decoupled calculations are performed to quantify the catalytic activity, side reaction inhibition ability, and overall performance of the catalyst at each reaction stage, achieving complete separation of activity and selectivity and independent characterization of the performance contribution of each reaction stage.

[0058] In summary, this invention, through standardized, automated, and precise design of the entire process, enables rapid and repeatable testing of the catalytic performance of polyester titanium catalysts. The test results are highly consistent with the actual performance in industrial applications, providing accurate and reliable decision-making basis for the rapid screening, formulation optimization, and industrial substitution of titanium catalysts, effectively shortening the R&D cycle and reducing the risks of industrial application.

[0059] The above description is merely a preferred embodiment of the present invention. The scope of protection of the present invention is not limited to the above embodiments. All technical solutions falling within the scope of the present invention's concept are within the scope of protection of the present invention. It should be noted that for those skilled in the art, any improvements and modifications made without departing from the principle of the present invention should also be considered within the scope of protection of the present invention.

Claims

1. A system for detecting the catalytic activity of a polyester titanium catalyst, characterized by comprising: a polyester titanium catalyst; a reaction vessel; a temperature controller; a pressure controller; a gas chromatograph; and a computer. include: The detection group construction module is used to determine the effective titanium mass fraction of the titanium-based catalyst to be tested after homogenization pretreatment, and then configure the composition ratio of the basic common components and differentiated catalyst components of each detection group; the effective titanium mass fraction refers to the proportion of catalytically active chelated titanium in the titanium-based catalyst to the total mass of the catalyst. The reaction simulation module, based on the component ratio of the detection group, configures the homogenized materials prepared by each detection group and puts them into the corresponding multi-stage series micro reactor group to start the reaction synchronously under the same control conditions. The process monitoring module collects the characteristic process parameters of each reaction stage of the multi-stage series micro reactor group corresponding to each detection group, executes the access control of each micro reactor group reaction stage, and obtains the effective reaction time and conversion characteristic parameters of each reaction stage. The conversion characteristic parameters refer to the derived parameters that characterize the degree of reaction completion and product quality, including the esterification rate in the esterification stage and the intrinsic viscosity of the melt in the pre-condensation and final condensation stages. They are quantified by real-time collected characteristic process parameters based on the parameter conversion relationship that has been calibrated and solidified in advance through offline standard detection methods. The data processing module collects product performance data for each reaction stage after each reaction stage is completed. Based on the type of each detection group and the effective reaction time of each reaction stage, it classifies and organizes the characteristic process parameters and converted characteristic parameters of each reaction stage, performs time series standardization and stratified baseline correction, and obtains pure catalytic contribution parameters. The detection group refers to a set of standardized reaction systems used to compare and detect the catalytic activity of titanium-based catalysts, including an experimental group and a control group. The experimental group is a reaction system with the titanium-based catalyst to be tested added, and the control group is a pre-set multi-level benchmark detection group system, which consists of multiple benchmark detection groups with the same group composition ratio as the experimental group but with differences only in the catalyst components. The multi-level benchmark detection group system contains at least three levels: the first level benchmark detection group is a benchmark system without the addition of catalytically active components, the second level benchmark detection group is a benchmark system with the addition of a known universal benchmark catalyst, and the third level benchmark detection group is a benchmark system with the addition of a target type benchmark catalyst. The decoupled quantification module performs multidimensional and multi-stage decoupled calculations on the pure catalytic contribution parameters, and quantifies the catalytic activity, catalytic selectivity and comprehensive catalytic performance of the titanium catalyst under test.

2. The system for detecting the catalytic activity of a polyester titanium catalyst according to claim 1, wherein The steps for implementing access control for each microreactor group's reaction stage include: For each stage of the micro reactor, a reasonable fluctuation range of characteristic process parameters and a fixed reaction time are pre-set for all detection groups to be consistent; After the testing team starts the multi-stage series micro reactor group, the online monitoring unit in each stage of the micro reactor collects the characteristic process parameters of the reaction stage in real time at a preset acquisition frequency. Based on the quantification of characteristic process parameters, the corresponding reaction process conversion characteristic parameters are obtained to determine whether the corresponding reaction process has been completed, and combined with a reasonable fluctuation range, it is determined whether the corresponding reaction process has abnormal operating conditions. When the cumulative reaction time of a certain micro-reactor reaches the preset fixed reaction time, all detection groups simultaneously determine that the reaction stage has ended, open the material conveying valve between the current micro-reactor and the next level micro-reactor in all detection groups, and convey all the material in the current micro-reactor to the next level micro-reactor. After the conveying is completed, the material conveying valve is automatically closed and the start command of the next level micro-reactor is triggered. The effective reaction time, characteristic process parameters and converted characteristic parameters of the reaction stage are recorded.

3. The catalytic activity detection system for a polyester titanium-based catalyst as described in claim 2, characterized in that, The steps of obtaining the converted characteristic parameters of the corresponding reaction process based on the quantization of characteristic process parameters, determining whether the corresponding reaction process has completed, and determining whether there are abnormal operating conditions in the corresponding reaction process in combination with a reasonable fluctuation range include: The system continuously compares the real-time collected characteristic process parameters with the preset reasonable fluctuation range of the corresponding reaction stage. If any characteristic process parameter exceeds the reasonable fluctuation range and the duration reaches the preset abnormal judgment time, it is determined that there is an abnormal working condition in the detection group, and the reaction process corresponding to the detection group is automatically terminated. If all characteristic process parameters are within a reasonable range of fluctuation, then the current reaction stage should be maintained and the reaction should continue. Based on the real-time acquired characteristic process parameters, the corresponding conversion characteristic parameters of the reaction process are extracted; If the converted characteristic parameters of a certain detection group reach the standard threshold of the reaction degree of the corresponding reaction stage and the fluctuation range does not exceed the preset allowable deviation for a preset stable judgment time, then the reaction of this reaction stage of the detection group is determined to be completed, and the steady state maintenance mode is automatically triggered.

4. The catalytic activity detection system for a polyester titanium-based catalyst as described in claim 1, characterized in that, The steps for classifying, organizing, time-series standardizing, and stratified baseline correction of the characteristic process parameters and converted characteristic parameters of each reaction stage based on each detection group type and the effective reaction time of each reaction stage to obtain the pure catalytic contribution parameters include: The effective reaction time, characteristic process parameters and converted characteristic parameters of each reaction stage of each detection group were extracted, as well as the product performance data after the reaction stage. According to the collection time, the characteristic process parameter sequence and the converted characteristic parameter sequence were constructed respectively. Calculate the average and range of the effective reaction time for the same reaction stage for all detection groups, and determine whether the ratio of the range to the average is less than a preset deviation threshold; if so, perform simple time series standardization; otherwise, perform dual-mode time series standardization. Based on the time-series standardized characteristic process parameter sequences and converted characteristic parameter sequences of each reaction stage in each detection group, the characteristic process parameter sequences, converted characteristic parameter sequences, and product performance data of the detection group to which the titanium catalyst under test belongs are subjected to stratified baseline correction to obtain pure catalytic contribution parameters.

5. The catalytic activity detection system for a polyester titanium catalyst as described in claim 4, characterized in that, The simple time series standardization process includes: Using the average effective reaction time of all test groups in this reaction stage as the baseline time, the characteristic process parameter sequence and the converted characteristic parameter sequence of each test group in this reaction stage are resampled using a linear interpolation method to generate a standardized time series of characteristic process parameter sequence and converted characteristic parameter sequence with the same length as the baseline time and the same number of sampling points, and then the timestamps are aligned.

6. The catalytic activity detection system for a polyester titanium catalyst as described in claim 5, characterized in that, The dual-mode time series standardization process includes: The characteristic process parameter sequence and the converted characteristic parameter sequence of each detection group for this reaction stage are retained. At the same time, the time axis of the characteristic process parameter sequence and the converted characteristic parameter sequence of each detection group for this reaction stage are normalized to the interval [0,1], where 0 corresponds to the start time of the reaction stage and 1 corresponds to the completion time of the reaction stage of this detection group. Normalized time points are selected at equal intervals within the interval [0,1], and the characteristic process parameter value and the converted characteristic parameter value corresponding to each normalized time point are calculated using a linear interpolation method to generate the normalized time series of the characteristic process parameter sequence and the converted characteristic parameter sequence.

7. The catalytic activity detection system for a polyester titanium-based catalyst as described in claim 5, characterized in that, The characteristic process parameter sequence, converted characteristic parameter sequence, and product performance data of the detection group to which the titanium catalyst under test belong are subjected to stratified baseline correction to obtain pure catalytic contribution parameters, including: The first-level baseline correction is performed by comparing the characteristic process parameter values, converted characteristic parameter values, and single-point values ​​of product performance data of each reaction stage in the detection group of the titanium catalyst to be tested with the corresponding data of the corresponding reaction stage and the same time point in the first-level benchmark detection group to obtain the first-level correction parameters. To perform the second-level system error correction, the first-level correction characteristic process parameter value, the first-level correction converted characteristic parameter value, and the first-level correction product performance data value after the first-level background baseline correction are compared with the corresponding data of the second-level benchmark detection group at the same time point in the corresponding reaction stage to obtain the second-level correction parameters. The third-level benchmark correction is performed by comparing the relative coefficients of the second-level corrected characteristic process parameters, the relative coefficients of the second-level corrected converted characteristic parameters, and the relative coefficients of the second-level corrected product performance data with the corresponding data at the same time point in the corresponding reaction stage of the third-level benchmark detection group. The resulting third-level correction parameters are used as pure catalytic contribution parameters.

8. The catalytic activity detection system for a polyester titanium catalyst as described in claim 7, characterized in that, The stratified baseline correction of the characteristic process parameter sequence, converted characteristic parameter sequence, and product performance data of the detection group to which the titanium catalyst under test belongs also includes: While performing baseline correction at each level, the average value of characteristic process parameters, the average value of converted characteristic parameters, the average value of product performance data, and the correction coefficient of the corresponding level are recorded simultaneously at each time point of the corresponding level benchmark detection group. The correction coefficient of the first level is the parameter value corresponding to the first level benchmark detection group, the correction coefficient of the second level is the reciprocal of the correction parameter value of the second level benchmark detection group corresponding to the first level, and the correction coefficient of the third level is the reciprocal of the correction parameter value of the third level benchmark detection group corresponding to the second level.

9. The catalytic activity detection system for a polyester titanium catalyst as described in claim 7, characterized in that, The pure catalytic contribution parameters include the benchmarking factor of the third-level corrected characteristic process parameters, the benchmarking factor of the third-level corrected converted characteristic parameters, and the benchmarking factor of the third-level corrected product performance data. The decoupled calculation of the pure catalytic contribution parameters in a multidimensional and staged manner, quantifying the catalytic activity, catalytic selectivity, and overall catalytic performance of the titanium-based catalyst under test, includes: The third-level correction conversion characteristic parameter benchmarking factor was extracted from the pure catalytic contribution parameters of each reaction stage. The independent catalytic activity index of each reaction stage was obtained by kinetic weighting calculation in combination with the effective reaction time of each reaction stage. The independent catalytic activity index of all reaction stages was weighted and summed according to the process weight of each reaction stage to obtain the total catalytic activity index of the titanium catalyst to be tested. The performance data of the third-level modified product in the pure catalytic contribution parameters of each reaction stage were extracted and compared with the benchmark ratio. The side reaction inhibition index of each reaction stage was obtained by reciprocal conversion. The side reaction inhibition index of all reaction stages was weighted and summed according to the quality control weight to obtain the total catalytic selectivity index of the titanium catalyst to be tested. Based on the calculated total catalytic activity index and total catalytic selectivity index, weighted calculations and normalization conversions are performed according to preset application requirement weights to obtain the comprehensive catalytic performance score of the titanium catalyst under test.

10. The catalytic activity detection system for a polyester titanium-based catalyst as described in claim 1, characterized in that, The multi-stage series-connected micro reactor groups are arranged in parallel. Each multi-stage series-connected micro reactor group contains a number of micro reactors connected in series, corresponding to the number of reaction stages. Each micro reactor is used to correspond to a reaction stage in the simulated industrial polyester production process.

11. A method for detecting the catalytic activity of a polyester titanium catalyst, implemented based on the catalytic activity detection system for a polyester titanium catalyst according to any one of claims 1-10, characterized in that, include: The effective titanium mass fraction of the titanium-based catalyst to be tested after homogenization pretreatment was determined, and then the composition ratio of the basic common components and the differentiated catalyst components of each test group was configured. Based on the component ratio of the detection group, the homogenized materials prepared by each detection group are configured and put into the corresponding multi-stage series micro reactor group, and the reaction is started synchronously under the same control conditions. Collect characteristic process parameters of each reaction stage of the multi-stage series micro reactor group corresponding to each detection group, execute access control of each micro reactor group reaction stage, and obtain the effective reaction time and conversion characteristic parameters of each reaction stage. After each reaction stage, product performance data for each detection group corresponding to the reaction stage are collected. Based on each detection group type and the effective reaction time of each reaction stage, the characteristic process parameters and converted characteristic parameters of each reaction stage are classified, time series standardized and stratified baseline corrected to obtain pure catalytic contribution parameters. The pure catalytic contribution parameters were decoupled and calculated in a multidimensional and staged manner to quantify the catalytic activity, catalytic selectivity and comprehensive catalytic performance of the titanium-based catalyst under test.

Images