An analysis method for detecting oxidation of an intermediate synthesis

Abstract

The application belongs to the technical field of intermediate process detection and analysis methods, and provides an oxidation detection and analysis method for intermediate synthesis, which comprises the following steps: in the oxidation reaction treatment process, multiple oxidation monitoring periods are set, the gas oxidant concentration in different oxidation monitoring subdomains divided in the reaction kettle is analyzed in each oxidation monitoring period, the reaction oxygen-rich region and the reaction oxygen-deficient region are identified, the reaction rate difference analysis of the reaction oxygen-rich region and the reaction oxygen-deficient region in the reaction kettle is performed, the local reaction imbalance degree value is obtained, the local reaction imbalance degree is evaluated according to the local reaction imbalance degree value, the reaction conditions of different regions in the reaction kettle can be adjusted in a targeted manner, and in the oxidation reaction process, the stability and consistency of the reaction progress can be understood in real time by continuously monitoring the local reaction imbalance degree value at different oxidation monitoring points, thereby providing data support for subsequent control and adjustment of reaction parameters.

Description

Technical Field

[0001] This invention belongs to the field of intermediate process detection and analysis technology, specifically a method for detecting and analyzing the oxidation of intermediates during synthesis. Background Technology

[0002] In many industrial sectors, such as fine chemicals and pharmaceuticals, the synthesis of intermediates is a crucial step in the production of final products. Oxidation reactions, as a common and important type of reaction in intermediate synthesis, directly determine the quality, yield, and production efficiency of the intermediates through their process control. Currently, the oxidation process for intermediate synthesis faces a series of pressing technical challenges in practical applications.

[0003] During oxidation reactions, reaction conditions often differ in different areas of the reactor, making it difficult to ensure reaction uniformity. Traditional processes lack effective monitoring and analysis methods for the concentration of gaseous oxidant in different areas of the reactor, making it difficult to accurately identify oxygen-rich and oxygen-deficient zones. Even if these zones can be identified, traditional processes lack effective methods to accurately analyze the difference in reaction rates between them, thus failing to effectively assess the degree of local reaction imbalance. Furthermore, traditional processes do not coordinate and compare the aeration and stirring rates within the reactor, leading operators to often adjust these rates based on experience in actual production, lacking scientific basis.

[0004] Therefore, the present invention provides an oxidation detection and analysis method for intermediate synthesis. Summary of the Invention

[0005] In order to overcome the shortcomings of the prior art, at least one technical problem raised in the background art is solved.

[0006] The technical solution adopted by this invention to solve its technical problem is: an oxidation detection and analysis method for intermediate synthesis, comprising the following steps: During the oxidation reaction process, multiple oxidation monitoring cycles are set. In each oxidation monitoring cycle, the concentration of gaseous oxidant in different oxidation monitoring sub-domains of the reactor is analyzed to identify the oxygen-rich zone and the oxygen-deficient zone of the reaction. The reaction rate difference between the oxygen-rich zone and the oxygen-deficient zone in the reactor was analyzed to obtain the local reaction imbalance value. Based on the local reaction imbalance value, the degree of local reaction imbalance was assessed. Among them, the degree of local response imbalance includes a large signal of local response imbalance or a small signal of local response imbalance. If the local reaction imbalance is large, the aeration rate and stirring rate in the reactor are compared and coordinated to obtain the rate coordination matching value. The trend and amplitude of the rate coordination matching value are compared with the local reaction imbalance value to evaluate the correlation between the rate coordination matching and the oxidation reaction imbalance. If the correlation is close, the coordination and matching type of the aeration rate and stirring rate in the reactor are identified, and the rate adjustment coefficient is obtained based on the identified coordination and matching type to perform rate adjustment operation.

[0007] As a further aspect of the present invention, the process for identifying the oxygen-rich reaction zone and the oxygen-deficient reaction zone is as follows: The oxidation reaction region inside the reactor is divided into multiple oxidation monitoring subdomains by a grid-like equal division. The oxidation monitoring cycle is divided into several oxidation monitoring points. The gaseous oxidant concentration of each oxidation monitoring subdomain at each oxidation monitoring point is obtained, and the average value is calculated to output the average oxidation concentration of the subdomain. If the average oxidation concentration of a subdomain is less than the minimum value within the normal concentration range of the subdomain, then it is a reaction hypoxia zone. If the average oxidation concentration of a subdomain is greater than the maximum value within the normal concentration range of the subdomain, then it is considered an oxygen-rich reaction zone.

[0008] As a further aspect of the present invention, the process for obtaining the unit oxygen enrichment rate in the oxygen-enriched reaction zone and the unit anoxic rate in the anoxic reaction zone is as follows: The concentrations of gaseous oxidant in the oxygen-enriched reaction zone at adjacent oxidation monitoring points are obtained respectively. The difference is calculated and then the ratio is calculated with the duration between adjacent oxidation monitoring points to obtain the unit oxygen enrichment rate. The concentration of gaseous oxidant in the reaction anoxic zone at adjacent oxidation monitoring points is obtained, the difference is calculated, and the ratio is calculated with the duration between adjacent oxidation monitoring points to obtain the unit anoxic rate.

[0009] As a further aspect of the present invention, the process of analyzing the difference in reaction rates between the oxygen-rich zone and the oxygen-deficient zone within the reactor to obtain the degree of local reaction imbalance is as follows: The oxygen-rich reaction zone is combined with each oxygen-deficient reaction zone to obtain multiple combinations of rich and deficient reaction rates. The reaction rate difference value is obtained by inputting the oxygen-enriched rate and the oxygen-deficient rate of the same unit in the time dimension into the Euclidean distance formula, and then summing and averaging the values. The average oxygen enrichment rate of each unit in the oxygen-enriched zone of the reaction is calculated by summing the average oxygen enrichment rate. The average hypoxia rate of each unit corresponding to the hypoxia zone in each reaction is calculated by summing the values, and the average hypoxia rate is output. The standard deviation of the oxygen enrichment rate of each unit corresponding to the oxygen enrichment zone of each reaction is calculated and the standard deviation of the oxygen enrichment rate is output. The standard deviation of the unit hypoxia rate corresponding to each reaction hypoxia zone is calculated and the standard deviation of the hypoxia rate is output. Input the mean oxygen-enriched rate, mean hypoxia rate, standard deviation of oxygen-enriched rate, and standard deviation of hypoxia rate into the coefficient of variation formula to output the uniform value of rate distribution. The sum of the reaction rate difference value and the rate distribution uniformity value is used to output the local reaction imbalance value. If the local imbalance value is greater than the local imbalance threshold, it indicates a large signal of local imbalance.

[0010] As a further aspect of the present invention, the method for obtaining the rate coordination matching value is as follows: The oxidation monitoring cycle is divided into several equal oxidation monitoring periods, each of which has an equal duration. The aeration rate and stirring rate for each oxidation monitoring period are obtained. After inputting the aeration rate and stirring rate for each oxidation monitoring period within the oxidation monitoring cycle into the Euclidean distance formula, the rate coordination matching value is output.

[0011] As a further aspect of the present invention, a trend comparison analysis is performed between the rate coordination matching value and the local imbalance degree value, the process of which is as follows: Substitute the rate coordination matching values ​​and the local imbalance degree values ​​corresponding to multiple oxidation monitoring cycles into the two-dimensional coordinate system to construct the rate coordination matching change curve and the local imbalance change curve, respectively. The sub-curves corresponding to adjacent oxidation monitoring cycles on the rate coordination matching change curve are used as rate coordination matching sub-curves to obtain multiple rate coordination matching sub-curves. The slope calculation formula is used to calculate the slope of each rate coordination matching sub-curve and output the rate coordination matching sub-slope. The sub-curves corresponding to adjacent oxidation monitoring cycles on the local imbalance change curve are taken as local imbalance sub-curves, resulting in multiple local imbalance sub-curves. The slope calculation formula is used to calculate the slope of each local imbalance sub-curve, and the local imbalance sub-slope is output. The difference between the slope of the fast-matching sub-slope and the slope of the local anti-imbalance sub-slope corresponding to the same adjacent oxidation monitoring cycle is taken as the absolute value to obtain the slope difference of the same neighboring sub-slope. The summation and mean are then calculated to output the coupling trend comparison value.

[0012] As a further aspect of the present invention, the rate coordination matching value and the local imbalance degree value are compared and analyzed by amplitude, as follows: Extract the coordinates of adjacent peaks and troughs on the rate coordination and matching curve, and subtract them to obtain the unit rate amplitude value. Extract the coordinates of adjacent peaks and troughs on the local imbalance change curve, and subtract them to obtain the unit imbalance amplitude value; The absolute value of the difference between the unit rate amplitude value and the unit imbalance amplitude value in the same time dimension is used to obtain the unit amplitude coupling value. The average of the amplitude coupling values ​​of multiple units is summed to output the coupling amplitude comparison value.

[0013] A further aspect of this invention is: evaluating the correlation between rate coordination and the degree of imbalance in the oxidation reaction, the process of which is as follows: The coupling trend comparison value and the coupling amplitude comparison value are summed to obtain the coupling correlation analysis value. If the coupling correlation analysis value is less than or equal to the coupling correlation analysis threshold, it is displayed as a closely correlated signal.

[0014] A further aspect of the present invention is as follows: identifying the coordination and matching type of the aeration rate and stirring rate inside the reactor, the process of which is as follows: The average ventilation rate during each oxidation monitoring period within the oxidation monitoring cycle is calculated to obtain the average periodic ventilation rate. The average stirring rate during each oxidation monitoring period within the oxidation monitoring cycle is calculated to obtain the average stirring rate for the cycle. If the average periodic ventilation rate is greater than the average periodic stirring rate, it will be displayed as a stirring rate lag signal; if the average periodic ventilation rate is less than the average periodic stirring rate, it will be displayed as a ventilation rate lag signal.

[0015] A further aspect of the present invention is as follows: based on the identified coordination matching type, a rate adjustment coefficient is obtained, and a rate adjustment operation is performed, as follows: If the signal is displayed as a lag signal in stirring rate, the difference between the aeration rate and the stirring rate is calculated, and the ratio of the difference to the aeration rate is calculated to obtain the rate adjustment coefficient. Multiply the stirring rate by the rate adjustment coefficient, and then sum the product with the stirring rate to obtain the adjusted stirring rate, thus completing the stirring rate adjustment operation. If the signal is displayed as a lag signal in the ventilation rate, the difference between the stirring rate and the ventilation rate is calculated, and the ratio of the difference to the stirring rate is calculated to obtain the rate adjustment coefficient. The ventilation rate is multiplied by the rate adjustment factor and then summed with the ventilation rate to obtain the adjusted ventilation rate, thus completing the ventilation rate adjustment operation.

[0016] The beneficial effects of this invention are as follows: In the oxidation reaction process, this invention sets multiple oxidation monitoring cycles. Within each cycle, the concentration of gaseous oxidant in different oxidation monitoring sub-domains of the reactor is analyzed to identify oxygen-rich and oxygen-deficient reaction zones. The reaction rate difference between the oxygen-rich and oxygen-deficient reaction zones in the reactor is analyzed to obtain the local reaction imbalance value. Based on the local reaction imbalance value, the degree of local reaction imbalance is assessed, allowing for targeted adjustment of reaction conditions in different areas of the reactor. Furthermore, by continuously monitoring the local reaction imbalance value at different oxidation monitoring points during the oxidation reaction, the stability and consistency of the reaction process can be understood in real time, providing data support for subsequent control and adjustment of reaction parameters. This invention compares and coordinates the aeration rate and stirring rate within the reactor to obtain a rate coordination matching value. This value is then coupled with the local reaction imbalance value to perform correlation analysis, assessing the degree of correlation between rate coordination matching and the degree of oxidation reaction imbalance. If the correlation is strong, the coordination matching type of the aeration rate and stirring rate within the reactor is identified. Based on the identified coordination matching type, a rate adjustment coefficient is obtained, and rate adjustment operations are performed. This avoids excessive energy consumption caused by excessively high aeration rates or excessively fast stirring rates, while ensuring the smooth progress of the reaction, achieving efficient resource utilization, reducing the occurrence of side reactions, thereby reducing the amount of impurities generated and improving the purity of intermediates. Attached Figure Description

[0017] The invention will now be further described with reference to the accompanying drawings.

[0018] Figure 1 This is a flowchart of the steps of an oxidation detection and analysis method for intermediate synthesis according to the present invention; Figure 2 This is a flowchart of the determination process in the oxidation detection and analysis method for intermediate synthesis according to the present invention. Detailed Implementation

[0019] To make the technical means, creative features, objectives and effects of this invention easier to understand, the invention will be further described below in conjunction with specific embodiments.

[0020] Example 1

[0021] An oxidation detection and analysis method for intermediate synthesis according to an embodiment of the present invention includes: S1. Processing raw materials to remove impurities, including: water washing or alkaline washing for desalination, distillation purification, and drying dehydration; S2, Oxidation reaction treatment, which includes: adding oxidant and catalyst, controlling temperature and pressure parameters, and performing stirring operation; S3. After the oxidation reaction reaches the target conversion rate, the reaction is terminated, solid-liquid separation, liquid-liquid separation / extraction and solvent recovery are carried out respectively. S4. Product purification: Improve product purity by performing vacuum distillation, crystallization purification (for solid products), and chromatographic purification (for small-scale laboratory needs). S5. Product purity and quality testing.

[0022] Example 2

[0023] Please see Figure 1 - Figure 2 As shown in the embodiment of the present invention, an oxidation detection and analysis method for intermediate synthesis includes the following steps: Step 1: During the oxidation reaction process, multiple oxidation monitoring cycles are set. In each oxidation monitoring cycle, the concentration of gaseous oxidant in different oxidation monitoring sub-domains of the reactor is analyzed to identify the oxygen-rich zone and the oxygen-deficient zone of the reaction. It should be noted that the oxidation monitoring cycle refers to the cycle of monitoring the oxidation reaction process during the synthesis of intermediates. It is mainly used to monitor the concentration of gaseous oxidant, the gas flow rate, and the stirring rate during the oxidation reaction process. The oxidation monitoring cycle only monitors the oxidation reaction process during one intermediate synthesis, and the oxidation reaction process during the synthesis of intermediates in multiple oxidation monitoring cycles is monitored synchronously. In some embodiments, the oxidation monitoring area is obtained as follows: The oxidation reaction region inside the reactor is divided into multiple oxidation monitoring subdomains by a grid-like equal division. The oxidation monitoring cycle is divided into several oxidation monitoring points, with the duration between adjacent oxidation monitoring points being equal. At each oxidation monitoring point, the concentration of gaseous oxidant in the divided multiple oxidation monitoring subdomains is monitored simultaneously. Obtain the gaseous oxidant concentration at each oxidation monitoring point in the oxidation monitoring subdomain, sum and calculate the average value, and output the average oxidation concentration of the subdomain. If the average oxidation concentration of the subdomain is within the normal range of the subdomain concentration, it indicates that the concentration of gaseous oxidant in the analyzed oxidation monitoring subdomain is normal throughout the entire oxidation monitoring cycle, which is the normal reaction zone. If the average oxidation concentration of the subdomain is less than the minimum value within the normal range of the subdomain concentration, it indicates that the concentration of gaseous oxidant in the analyzed oxidation monitoring subdomain is low throughout the entire oxidation monitoring period, which is a reaction-deficient region. If the average oxidation concentration of the subdomain is greater than the maximum value within the normal range of the subdomain concentration, it indicates that the concentration of gaseous oxidant in the analyzed oxidation monitoring subdomain is high throughout the entire oxidation monitoring cycle, which is the oxygen-rich reaction zone. It should be noted that the purpose of identifying the oxygen-rich and oxygen-deficient reaction zones is as follows: Spatially, for the oxygen-deficient reaction zone, the aeration rate can be appropriately increased to enhance the concentration of the gaseous oxidant; for the oxygen-rich reaction zone, the aeration rate can be reduced to avoid excessive oxidant. By adjusting parameters such as the stirring rate, the mixing and mass transfer of substances within the reactor can be promoted, allowing the gaseous oxidant to be distributed more evenly across all zones, reducing the differences in oxidation levels between different zones, thereby improving the quality and consistency of intermediate synthesis. From a temporal perspective, within each oxidation monitoring cycle, based on the average oxidation concentration of subdomains obtained from different oxidation monitoring points, the changes in the oxidation state of each region during the reaction process can be understood in real time. Moreover, through data analysis of different oxidation monitoring points, it is possible to predict potential problems and trends during the reaction process. From a quality perspective, accurately identifying the oxygen-deficient and oxygen-rich reaction zones and taking corresponding measures can reduce the occurrence of side reactions caused by uneven oxidation. Moreover, the reduction of side reactions also helps to improve the purity of intermediates and avoid waste of raw materials and loss of products due to incomplete reaction or excessive oxidation. Step 2: Analyze the difference in reaction rates between the oxygen-rich zone and the oxygen-deficient zone in the reactor to obtain the local reaction imbalance value. Based on the local reaction imbalance value, assess the degree of local reaction imbalance. In some embodiments, the process for obtaining the unit enrichment rate of the oxygen-enriched reaction zone is as follows: The concentrations of gaseous oxidant in the oxygen-enriched reaction zone at adjacent oxidation monitoring points are obtained respectively. The difference is calculated and then the ratio is calculated with the duration between adjacent oxidation monitoring points to obtain the unit oxygen enrichment rate. The process for obtaining the unit hypoxia rate in the hypoxic reaction zone is as follows: The concentrations of gaseous oxidant in the reaction hypoxia zone at adjacent oxidation monitoring points are obtained respectively. The difference is calculated and then the ratio is calculated with the duration between adjacent oxidation monitoring points to obtain the unit hypoxia rate. The process of analyzing the difference in reaction rates between the oxygen-rich and oxygen-deficient zones within the reactor to obtain the degree of local reaction imbalance is as follows: The oxygen-rich reaction zone is combined with each oxygen-deficient reaction zone to obtain multiple combinations of rich and deficient reaction rates. The reaction rate difference value is obtained by inputting the oxygen-enriched rate and the oxygen-deficient rate of the same unit in the time dimension into the Euclidean distance formula, and then summing and averaging the values. The average oxygen enrichment rate of each unit in the oxygen-enriched zone of the reaction is calculated by summing the average oxygen enrichment rate. The average hypoxia rate of each unit corresponding to the hypoxia zone in each reaction is calculated by summing the values, and the average hypoxia rate is output. The standard deviation of the oxygen enrichment rate of each unit corresponding to the oxygen enrichment zone of each reaction is calculated and the standard deviation of the oxygen enrichment rate is output. The standard deviation of the unit hypoxia rate corresponding to each reaction hypoxia zone is calculated and the standard deviation of the hypoxia rate is output. Input the mean oxygen-enriched rate, mean hypoxia rate, standard deviation of oxygen-enriched rate, and standard deviation of hypoxia rate into the coefficient of variation formula to output the uniform value of rate distribution. The sum of the reaction rate difference value and the rate distribution uniformity value is used to output the local reaction imbalance value. It is understandable that the local reaction imbalance value represents an index used to quantify the degree of local reaction imbalance between the oxygen-rich zone and the oxygen-deficient zone within the reactor. On the one hand, the reaction rate difference value reflects the direct difference in reaction rates between the oxygen-rich zone and the oxygen-deficient zone within a specific time interval. On the other hand, the rate distribution uniformity value reflects the uniformity of the reaction rate distribution within the oxygen-rich zone and the oxygen-deficient zone, that is, the stability and consistency of the reaction rate in different regions and at different time points. If the local reaction imbalance value is greater than the local reaction imbalance threshold, it indicates that the reaction rate difference between the oxygen-rich area and the hypoxic area is large within a specific time interval, which shows a large signal of local reaction imbalance. If the local reaction imbalance value is less than or equal to the local reaction imbalance threshold, it indicates that the difference in reaction rate between the oxygen-rich area and the hypoxic area is small within a specific time interval, which is displayed as a small signal of local reaction imbalance. The specific scheme of this embodiment is as follows: During the oxidation reaction process, multiple oxidation monitoring cycles are set. In each oxidation monitoring cycle, the concentration of gaseous oxidant in different oxidation monitoring sub-domains of the reactor is analyzed to identify the oxygen-rich reaction zone and the oxygen-deficient reaction zone. The reaction rate difference between the oxygen-rich reaction zone and the oxygen-deficient reaction zone in the reactor is analyzed to obtain the local reaction imbalance value. Based on the local reaction imbalance value, the degree of local reaction imbalance is evaluated, and the reaction conditions in different areas of the reactor can be adjusted in a targeted manner. Moreover, during the oxidation reaction, by continuously monitoring the local reaction imbalance value at different oxidation monitoring points, the stability and consistency of the reaction process can be understood in real time, providing data support for subsequent control and adjustment of reaction parameters.

[0024] Example 3

[0025] Please see Figure 1 - Figure 2 As shown in the embodiment of the present invention, the oxidation detection and analysis method for intermediate synthesis further includes the following steps: Step 3: If the local reaction imbalance is large, the aeration rate and stirring rate in the reactor are compared and coordinated to obtain the rate coordination matching value. The trend and amplitude of the rate coordination matching value are compared and analyzed with the local reaction imbalance value to evaluate the correlation between the rate coordination matching and the degree of oxidation reaction imbalance. In some embodiments, the rate coordination matching value is obtained as follows: The oxidation monitoring cycle is divided into several equal oxidation monitoring periods, each of which has an equal duration. The aeration rate and stirring rate for each oxidation monitoring period are obtained. After inputting the aeration rate and stirring rate for each oxidation monitoring period within the oxidation monitoring cycle into the Euclidean distance formula, the rate coordination matching value is output. The rate coordination matching value and the local imbalance degree value are coupled and correlated, and the process is as follows: Substitute the rate coordination matching values ​​corresponding to multiple oxidation monitoring cycles into a two-dimensional coordinate system, with the X-axis representing time and the Y-axis representing the rate coordination matching value, to construct a rate coordination matching change curve. Substitute the local imbalance degree values ​​corresponding to multiple oxidation monitoring cycles into a two-dimensional coordinate system, with the X-axis representing time and the Y-axis representing the local imbalance degree value, to construct a local imbalance change curve; The sub-curves corresponding to adjacent oxidation monitoring cycles on the rate coordination and matching change curve are used as rate coordination and matching sub-curves to obtain multiple rate coordination and matching sub-curves. Extract the start and end coordinates of each rate coordination matching sub-curve and input them into the slope calculation formula to output the rate coordination matching sub-slope. Similarly, the sub-curves corresponding to adjacent oxidation monitoring cycles on the local imbalance change curve are taken as local imbalance sub-curves, resulting in multiple local imbalance sub-curves. Extract the starting and ending coordinates of each local anti-imbalance sub-curve, input them into the slope calculation formula, and output the local anti-imbalance sub-slope. The difference between the slope of the fast matching sub-slope and the slope of the local anti-imbalance sub-slope corresponding to the same adjacent oxidation monitoring cycle is obtained by taking the absolute value of the difference between the slopes of the same adjacent sub-slopes. The average of the slope differences of all neighboring sub-sub ... Extract the coordinates of adjacent peaks and troughs on the rate coordination and matching curve, and subtract them to obtain the unit rate amplitude value. Extract the coordinates of adjacent peaks and troughs on the local imbalance change curve, and subtract them to obtain the unit imbalance amplitude value; The absolute value of the difference between the unit rate amplitude value and the unit imbalance amplitude value in the same time dimension is used to obtain the unit amplitude coupling value. The average value of the amplitude coupling values ​​of multiple units is summed, and the coupling amplitude comparison value is output. The coupling trend comparison value and the coupling amplitude comparison value are summed to obtain the coupling correlation analysis value; It is understandable that the meaning represented by the coupling correlation analysis value is: to comprehensively consider the degree of correlation between rate coordination and local imbalance of oxidation reaction in two dimensions, namely trend and magnitude. On the one hand, the coupling trend comparison value reflects the similarity or difference between the change trend of rate coordination and the change trend of local imbalance in each oxidation monitoring period. On the other hand, the coupling magnitude comparison value reflects the difference between the change magnitude of rate coordination and the change magnitude of local imbalance in the same time dimension. The purpose of assessing the correlation between rate coordination and the degree of imbalance in oxidation reactions is to: Objective 1: From the perspective of trend correlation, by comparing the coupling trend values, we can clearly understand the relationship between the coordinated matching trend of aeration rate and stirring rate and the local imbalance trend of oxidation reaction, and adjust the aeration and stirring parameters in a timely manner to make their trends more coordinated, thereby stabilizing the oxidation reaction. Furthermore, we can optimize the oxidation process control strategy for intermediate synthesis. By studying the coupling trend comparison values ​​under different process conditions, we can determine the optimal coordination method of aeration rate and stirring rate, as well as the corresponding control time points. Objective 2: From the perspective of the magnitude of change correlation, the coupling magnitude comparison value reflects the difference between the magnitude of rate coordination matching and the magnitude of local imbalance in the oxidation reaction. In the oxidation process control of intermediate synthesis, by controlling the coupling magnitude comparison value, the range of oxidation reaction imbalance can be limited. Moreover, reducing the unit magnitude coupling value, that is, reducing the difference in the magnitude of rate coordination matching and local imbalance in the oxidation reaction on the same time dimension, can improve the stability of the intermediate synthesis oxidation process. In actual production, stable process conditions help to ensure the consistency of intermediate product quality. If the coupling correlation analysis value is greater than the coupling correlation analysis threshold, it indicates that the correlation between rate coordination matching and local imbalance of oxidation reaction is not strong in both the trend and magnitude dimensions, showing a weak correlation signal. If the coupling correlation analysis value is less than or equal to the coupling correlation analysis threshold, it indicates that the correlation between rate coordination matching and local imbalance of oxidation reaction is relatively strong in both trend and magnitude dimensions, showing a strong correlation signal. Step 4: If the correlation is close, identify the coordination and matching type of the aeration rate and stirring rate in the reactor, and obtain the rate adjustment coefficient based on the identified coordination and matching type, and perform rate adjustment operation. In some embodiments, the coordination matching type of the aeration rate and stirring rate in the reactor is identified as follows: The average ventilation rate during each oxidation monitoring period within the oxidation monitoring cycle is calculated to obtain the average periodic ventilation rate. The average stirring rate during each oxidation monitoring period within the oxidation monitoring cycle is calculated to obtain the average stirring rate for the cycle. If the average periodic ventilation rate is greater than the average periodic stirring rate, it indicates that the ventilation rate is faster than the stirring rate during the oxidation monitoring period, which is displayed as a stirring rate lag signal. The difference between the ventilation rate and the stirring rate is then calculated and the ratio is calculated with the ventilation rate to obtain the rate adjustment coefficient. Multiply the stirring rate by the rate adjustment coefficient, and then sum the product with the stirring rate to obtain the adjusted stirring rate, thus completing the stirring rate adjustment operation. If the average periodic ventilation rate is less than the average periodic stirring rate, it indicates that the ventilation rate is slower than the stirring rate during the oxidation monitoring period, which is displayed as a ventilation rate lag signal. The difference between the stirring rate and the ventilation rate is then calculated and the ratio is calculated with the stirring rate to obtain the rate adjustment coefficient. The ventilation rate is multiplied by the rate adjustment factor and then summed with the ventilation rate to obtain the adjusted ventilation rate, thus completing the ventilation rate adjustment operation. The specific scheme of this embodiment is as follows: the aeration rate and stirring rate in the reactor are compared and coordinated to obtain the rate coordination matching value. This value is then coupled and correlated with the local reaction imbalance value to evaluate the correlation between the rate coordination matching and the degree of oxidation reaction imbalance. If the correlation is strong, the coordination matching type of the aeration rate and stirring rate in the reactor is identified. Based on the identified coordination matching type, the rate adjustment coefficient is obtained, and the rate adjustment operation is performed to avoid excessive energy consumption caused by excessively high aeration rate or excessively fast stirring rate. At the same time, the smooth progress of the reaction is ensured, achieving efficient resource utilization. Furthermore, the occurrence of side reactions can be reduced, thereby reducing the amount of impurities generated and improving the purity of intermediates.

[0026] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely illustrative of the principles of the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the present invention as claimed. The scope of protection of the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for detecting and analyzing the oxidation of intermediates during synthesis, characterized in that: include: During the oxidation reaction process, multiple oxidation monitoring cycles are set. In each oxidation monitoring cycle, the concentration of gaseous oxidant in different oxidation monitoring sub-domains of the reactor is analyzed to identify the oxygen-rich zone and the oxygen-deficient zone of the reaction. The reaction rate difference between the oxygen-rich zone and the oxygen-deficient zone in the reactor was analyzed to obtain the local reaction imbalance value. Based on the local reaction imbalance value, the degree of local reaction imbalance was assessed. Among them, the degree of local response imbalance includes a large signal of local response imbalance or a small signal of local response imbalance. If the local reaction imbalance is large, the aeration rate and stirring rate in the reactor are compared and coordinated to obtain the rate coordination matching value. The trend comparison analysis and amplitude comparison analysis are then performed with the local reaction imbalance value to evaluate the correlation between the rate coordination matching and the degree of oxidation reaction imbalance. If the correlation is close, the coordination and matching type of the aeration rate and stirring rate in the reactor are identified, and the rate adjustment coefficient is obtained based on the identified coordination and matching type to perform rate adjustment operation.

2. The oxidation detection and analysis method for intermediate synthesis according to claim 1, characterized in that: The process for identifying the oxygen-rich and oxygen-deficient reaction zones is as follows: The oxidation reaction region inside the reactor is divided into multiple oxidation monitoring subdomains by a grid-like equal division. The oxidation monitoring cycle is divided into several oxidation monitoring points. The gaseous oxidant concentration of each oxidation monitoring subdomain at each oxidation monitoring point is obtained, and the average value is calculated to output the average oxidation concentration of the subdomain. If the average oxidation concentration of a subdomain is less than the minimum value within the normal concentration range of the subdomain, then it is a reaction hypoxia zone. If the average oxidation concentration of a subdomain is greater than the maximum value within the normal concentration range of the subdomain, then it is considered an oxygen-rich reaction zone.

3. The oxidation detection and analysis method for intermediate synthesis according to claim 1, characterized in that: The process for obtaining the unit oxygen enrichment rate in the oxygen-enriched reaction zone and the unit anoxic reaction rate in the anoxic reaction zone is as follows: The concentrations of gaseous oxidant in the oxygen-enriched reaction zone at adjacent oxidation monitoring points are obtained respectively. The difference is calculated and then the ratio is calculated with the duration between adjacent oxidation monitoring points to obtain the unit oxygen enrichment rate. The concentration of gaseous oxidant in the reaction anoxic zone at adjacent oxidation monitoring points is obtained, the difference is calculated, and the ratio is calculated with the duration between adjacent oxidation monitoring points to obtain the unit anoxic rate.

4. The oxidation detection and analysis method for intermediate synthesis according to claim 3, characterized in that: The process of analyzing the difference in reaction rates between the oxygen-rich and oxygen-deficient zones within the reactor to obtain the degree of local reaction imbalance is as follows: The oxygen-rich reaction zone is combined with each oxygen-deficient reaction zone to obtain multiple combinations of rich and deficient reaction rates. The reaction rate difference is obtained by inputting the oxygen-enriched rate and the oxygen-deficient rate of the same unit in the time dimension into the Euclidean distance formula, and then summing and averaging the results. The average oxygen enrichment rate of each unit in the oxygen-enriched zone of the reaction is calculated by summing the average oxygen enrichment rate. The average hypoxia rate of each unit corresponding to the hypoxia zone in each reaction is calculated by summing the values, and the average hypoxia rate is output. The standard deviation of the oxygen enrichment rate of each unit corresponding to the oxygen enrichment zone of each reaction is calculated and the standard deviation of the oxygen enrichment rate is output. The standard deviation of the unit hypoxia rate corresponding to each reaction hypoxia zone is calculated and the standard deviation of the hypoxia rate is output. Input the mean oxygen-enriched rate, mean hypoxia rate, standard deviation of oxygen-enriched rate, and standard deviation of hypoxia rate into the coefficient of variation formula to output the uniform value of rate distribution. The sum of the reaction rate difference value and the rate distribution uniformity value is used to output the local reaction imbalance value. If the local imbalance value is greater than the local imbalance threshold, it indicates a large signal of local imbalance.

5. The oxidation detection and analysis method for intermediate synthesis according to claim 1, characterized in that: The method for obtaining the rate coordination matching value is as follows: The oxidation monitoring cycle is divided into several equal oxidation monitoring periods, each of which has an equal duration. The aeration rate and stirring rate for each oxidation monitoring period are obtained. After inputting the aeration rate and stirring rate for each oxidation monitoring period within the oxidation monitoring cycle into the Euclidean distance formula, the rate coordination matching value is output.

6. The oxidation detection and analysis method for intermediate synthesis according to claim 1, characterized in that: The trend comparison analysis of the rate coordination matching value and the local imbalance degree value is performed as follows: Substitute the rate coordination matching values ​​and the local imbalance degree values ​​corresponding to multiple oxidation monitoring cycles into the two-dimensional coordinate system to construct the rate coordination matching change curve and the local imbalance change curve, respectively. The sub-curves corresponding to adjacent oxidation monitoring cycles on the rate coordination matching change curve are used as rate coordination matching sub-curves to obtain multiple rate coordination matching sub-curves. The slope calculation formula is used to calculate the slope of each rate coordination matching sub-curve and output the rate coordination matching sub-slope. The sub-curves corresponding to adjacent oxidation monitoring cycles on the local imbalance change curve are taken as local imbalance sub-curves, resulting in multiple local imbalance sub-curves. The slope calculation formula is used to calculate the slope of each local imbalance sub-curve, and the local imbalance sub-slope is output. The difference between the slope of the fast-matching sub-slope and the slope of the local anti-imbalance sub-slope corresponding to the same adjacent oxidation monitoring cycle is taken as the absolute value to obtain the slope difference of the same neighboring sub-slope. The summation and mean are then calculated to output the coupling trend comparison value.

7. The oxidation detection and analysis method for intermediate synthesis according to claim 6, characterized in that: The amplitude comparison analysis of the rate coordination matching value and the local imbalance degree value is performed as follows: Extract the coordinates of adjacent peaks and troughs on the rate coordination and matching curve, and subtract them to obtain the unit rate amplitude value. Extract the coordinates of adjacent peaks and troughs on the local imbalance change curve, and subtract them to obtain the unit imbalance amplitude value; The absolute value of the difference between the unit rate amplitude value and the unit imbalance amplitude value in the same time dimension is used to obtain the unit amplitude coupling value. The average of the amplitude coupling values ​​of multiple units is summed to output the coupling amplitude comparison value.

8. The oxidation detection and analysis method for intermediate synthesis according to claim 7, characterized in that: The process for assessing the correlation between rate coordination and the degree of oxidation reaction imbalance is as follows: The coupling trend comparison value and the coupling amplitude comparison value are summed to obtain the coupling correlation analysis value. If the coupling correlation analysis value is less than or equal to the coupling correlation analysis threshold, it is displayed as a closely correlated signal.

9. The oxidation detection and analysis method for intermediate synthesis according to claim 1, characterized in that: The process for identifying the coordination and matching type of aeration rate and stirring rate within the reactor is as follows: The average ventilation rate during each oxidation monitoring period within the oxidation monitoring cycle is calculated to obtain the average periodic ventilation rate. The average stirring rate during each oxidation monitoring period within the oxidation monitoring cycle is calculated to obtain the average stirring rate for the cycle. If the average periodic ventilation rate is greater than the average periodic stirring rate, it will be displayed as a stirring rate lag signal; if the average periodic ventilation rate is less than the average periodic stirring rate, it will be displayed as a ventilation rate lag signal.

10. The oxidation detection and analysis method for intermediate synthesis according to claim 9, characterized in that: Based on the identified coordination matching type, the rate adjustment coefficient is obtained, and the rate adjustment operation is performed as follows: If the signal is a lag in stirring rate, the difference between the aeration rate and the stirring rate is calculated, and the ratio of the difference to the aeration rate is calculated to obtain the rate adjustment coefficient. The stirring rate is then multiplied by the rate adjustment coefficient and summed with the stirring rate to obtain the adjusted stirring rate, thus completing the stirring rate adjustment operation. If the displayed ventilation rate lag signal is obtained, the difference between the stirring rate and the ventilation rate is calculated, and the ratio with the stirring rate is calculated to obtain the rate adjustment coefficient. The ventilation rate is then multiplied by the rate adjustment coefficient and summed with the ventilation rate to obtain the adjusted ventilation rate, thus completing the ventilation rate adjustment operation.

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