High-uniformity temperature control method based on multi-stage heat flow compensation of reaction kettle

Abstract

The invention discloses a high-uniformity temperature control method based on multi-stage heat flow compensation of a reaction kettle, relates to the technical field of reaction kettle control, and solves the technical problem that in the prior art, operation evaluation of the reaction kettle cannot be carried out according to multi-dimensional data acquisition, so that the specific position, needing heat flow compensation, in the reaction kettle cannot be deduced. The method specifically comprises the following steps: multi-dimensional data acquisition: carrying out multi-dimensional data acquisition on a reaction kettle; data analysis and processing: carrying out analysis and processing according to the collected multi-dimensional data; after multi-dimensional data acquisition is completed, data analysis is performed according to the acquired data, the real-time operation state of the reaction kettle is deduced through data analysis, and whether heat flow compensation needs to be executed in the current operation process of the reaction kettle is deduced according to operation state analysis, so that the operation control efficiency of the reaction kettle is improved, and the processing efficiency of the reaction kettle is ensured; and performing mechanism cooperative constraint control, performing analysis according to the operation of the internal mechanism of the reaction kettle, and performing reaction kettle operation decision.

Description

TECHNICAL FIELD

[0001] The application relates to the technical field of reaction kettle control, in particular to a high-uniformity temperature control method based on multi-stage heat flow compensation of a reaction kettle. BACKGROUND

[0002] The reaction kettle is a comprehensive reaction container with physical or chemical reactions. The kettle body is the main part of the reaction kettle and is used for loading reaction materials. The stirring device is used for mixing the reaction materials, improving the reaction rate and reaction uniformity. The heat transfer device, including a jacket, a coil pipe and a tube bank, is used for heating or cooling the reaction materials and maintaining the temperature conditions required for the reaction. The sealing device ensures the high pressure or vacuum state in the kettle and prevents material leakage and the entry of external impurities.

[0003] The patent with the publication number CN114594687A provides a reaction kettle multi-point temperature compensation measurement and control method. The method adopts multi-point temperature measurement, avoids the limitations of single-point temperature measurement, improves the accuracy of compensation, combines feedforward control and fuzzy control, compensates the temperature in the reaction kettle in time, keeps the temperature in the reaction kettle stable, and avoids the unstable temperature in the reaction kettle.

[0004] However, in the prior art, the reaction kettle operation cannot be evaluated according to multi-dimensional data acquisition, so that the specific position of the reaction kettle that needs heat flow compensation cannot be inferred, and the compensation amount cannot be calculated according to the position. In addition, the current reaction kettle execution cannot be inferred according to the internal mechanism operation analysis of the reaction kettle, so as to avoid the phenomenon of heat flow compensation execution decline.

[0005] In view of the above technical defects, a solution is proposed. SUMMARY

[0006] The purpose of the present application is to solve the above-mentioned problems, and a high-uniformity temperature control method based on multi-stage heat flow compensation of a reaction kettle is proposed.

[0007] The purpose of the present application can be achieved by the following technical solutions:

[0008] The high-uniformity temperature control method based on multi-stage heat flow compensation of a reaction kettle is as follows:

[0009] Step one, multi-dimensional data acquisition, multi-dimensional data acquisition of the reaction kettle is performed;

[0010] Step two, data analysis and processing, the collected multi-dimensional data is analyzed and processed;

[0011] Step three, mechanism coordination and constraint control, the reaction kettle operation decision is made according to the internal mechanism operation analysis of the reaction kettle.

[0012] As a preferred embodiment of the present application, the step one multi-dimensional data acquisition process is as follows:

[0013] According to the structure of the reaction kettle, different orientation analysis is carried out, the reaction kettle is divided into three sections in the axial direction, and the collected temperatures are marked as T1, T2 and T3 respectively; and the reaction kettle is divided into two layers in the radial direction, and the collected temperatures are marked as T4 and T5; at the same time, the inlet temperature, outlet temperature and heat flow of the jacket heat medium in the reaction kettle are collected, and are marked as T in , T out and Q respectively; according to the reaction system of the reaction kettle, the real-time heat release rate q and the viscosity μ of the reaction system are collected.

[0014] As a preferred embodiment of the present application, the step two data analysis process is as follows:

[0015] According to the temperature values at each position in the reaction kettle, the mean value is calculated, and the temperature mean value is marked as T 均 ; and according to the temperature values at each position and the temperature mean value, the temperature deviation at each position is obtained, and is marked as T pi ; i takes the value of 1-5, indicating the five positions divided by the reaction kettle;

[0016] The actual heat flow density of the jacket is collected by the formula: ; wherein c is the specific heat capacity of the heat medium, ρ is the density of the heat medium, and S is the heat exchange area of the jacket.

[0017] As a preferred embodiment of the present application, according to the real-time temperature deviation of each position corresponding to the running process of the reaction kettle, if each real-time temperature deviation in the reaction kettle is lower than the set temperature deviation threshold, it is inferred that the temperature uniformity inside the reaction kettle meets the standard, and no multi-stage compensation is needed; if each real-time temperature deviation in the reaction kettle is not lower than the set temperature deviation threshold, it is inferred that the temperature uniformity inside the reaction kettle does not meet the standard, and multi-stage compensation is needed.

[0018] As a preferred embodiment of the present application, according to the comparison between the temperature deviation and the temperature deviation threshold, the position of the reaction kettle that needs to be adjusted for uniformity is determined, and is marked as the position to be compensated;

[0019] The dynamic compensation coefficient is calculated by the formula: K i = K0×(1+k μ ×μ); K0 is the basic compensation coefficient, k μ is the viscosity correction coefficient, and μ is the real-time reaction viscosity.

[0020] According to the temperature deviation T pi of the position to be compensated and the dynamic compensation coefficient K i , the heat flow compensation amount q bi; formula is: q bi = K i * T pi * S i ; S i It is the heat exchange area corresponding to the position to be compensated.

[0021] According to the heat flow compensation amount corresponding to the position to be compensated, the compensation is carried out, and the heat flow compensation amount is sent to the administrator terminal in real time.

[0022] As a preferred embodiment of the present application, the mechanism coordination constraint control process is as follows:

[0023] After the position to be compensated is compensated according to the heat flow compensation amount, the mechanism coordination constraint control is carried out.

[0024] The temperature change rate and the crystallinity change rate in the reaction kettle are collected; the change rate ratio is calculated through the ratio of the temperature change rate and the crystallinity change rate; during the operation stage of the reaction kettle, the valve opening degree of the heat conducting oil and the valve opening degree of the cold water are collected synchronously, and the opening deviation is calculated according to the difference value of the opening degree.

[0025] As a preferred embodiment of the present application, if the change rate ratio of the reaction kettle exceeds the set change rate ratio threshold, or the opening deviation of the reaction kettle exceeds the opening deviation threshold, an execution mechanism operation control signal is generated and sent to the administrator terminal; if the change rate ratio of the reaction kettle does not exceed the set change rate ratio threshold, and the opening deviation of the reaction kettle does not exceed the opening deviation threshold, an execution mechanism operation signal is generated and sent to the administrator terminal.

[0026] Compared with the prior art, the present application has the following advantages:

[0027] 1、In the present application, data analysis is carried out according to the collected data, the real-time running state of the reaction kettle is inferred through data analysis, and whether the current reaction kettle running process needs to execute heat flow compensation is inferred according to the running state analysis, so as to improve the running control efficiency of the reaction kettle and ensure the processing efficiency of the reaction kettle.

[0028] 2、In the present application, the reaction kettle internal mechanism operation is analyzed, the reaction kettle running decision is made, the phase change latent heat amplification execution mechanism response difference is prevented, the fixed constraint threshold cannot inhibit the temperature oscillation under dynamic working condition, which leads to uneven product crystal size distribution; the working efficiency of the reaction kettle is improved. BRIEF DESCRIPTION OF DRAWINGS

[0029] In order to facilitate the understanding of those skilled in the art, the present application will be further described below with reference to the accompanying drawings.

[0030] Fig. 1 The method principle block diagram of the present application;

[0031] Fig. 2 Method flowchart of the present application. DETAILED DESCRIPTION

[0032] In order to make the personnel in the technical field better understand the present application, the technical solutions in the embodiments of the present application will be described clearly and completely in combination with the drawings in the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor are within the protection scope of the present application.

[0033] Reference to "an embodiment" in this document means that a particular feature, structure, or characteristic described in connection with the embodiment can be included in at least one embodiment of the application. The appearances of the phrase in various places in the specification are not necessarily all referring to the same embodiment, nor are they necessarily mutually exclusive of one another. It is expressly understood that the embodiments described herein are merely examples from a multitude of possible embodiments, which can be literally combined or otherwise combined with other embodiments to produce additional embodiments including development sets of patents or publications that may not be explicitly stated as embodiments.

[0034] Please refer to Figs. 1-2 As shown in the figure, the specific temperature control method based on the multi-stage heat flow compensation of the reaction kettle is as follows:

[0035] Step one, multi-dimensional data acquisition, multi-dimensional data acquisition is performed on the reaction kettle;

[0036] Step two, data analysis and processing, the collected multi-dimensional data are analyzed and processed;

[0037] After the multi-dimensional data acquisition is completed, the data analysis is performed according to the collected data, the real-time running state of the reaction kettle is inferred through the data analysis, and whether the heat flow compensation needs to be performed in the current reaction kettle running process is inferred according to the running state analysis, so as to improve the running control efficiency of the reaction kettle and ensure the processing efficiency of the reaction kettle;

[0038] Step three, mechanism coordination constraint control, the reaction kettle running decision is made according to the analysis of the internal mechanism of the reaction kettle, the response difference of the phase change latent heat amplification executing mechanism is prevented, the fixed constraint threshold cannot inhibit the temperature oscillation under the dynamic working condition, and the product crystal size distribution is uneven; it is beneficial to improve the working efficiency of the reaction kettle;

[0039] The multi-dimensional data acquisition process is as follows:

[0040] According to the structure of the reaction kettle, different direction analysis is performed, the reaction kettle is divided into three sections in the axial direction, and the collected temperatures are marked as T1, T2 and T3; and the reaction kettle is divided into two layers in the radial direction, and the collected temperatures are marked as T4 and T5;

[0041] At the same time, the inlet temperature, outlet temperature and heat flow of the jacket heat medium in the reactor are collected, and are marked as T in , T out and Q respectively; mainly used for calculating the actual heat flow density;

[0042] According to the reaction system of the reactor, the real-time heat release rate q (unit: W) and the viscosity μ (unit: Pa·s) of the reaction system are collected, the former is used to predict the heat flow demand, and the latter is used to correct the heat transfer efficiency coefficient;

[0043] After completing the data collection, step two is entered;

[0044] The process of data analysis and processing in step two is as follows:

[0045] The mean value of the temperature values at each position inside the reactor is calculated, and the temperature mean value is marked as T 均 ; and the deviation of each position is obtained by comparing the temperature values at each position with the temperature mean value, and the temperature deviation of each position is set as T pi ; i takes the value of 1-5, indicating the five positions divided by the reactor;

[0046] According to the heat medium parameters, the actual heat flow density of the jacket is calculated according to the formula "heat flow density = specific heat capacity of medium x flow rate x temperature difference" (unit: W / m 2 ), the formula logic is "the actual heat flow into / out of the reactor is deduced by the heat change of the medium", and the specific formula is: q is the actual heat flow density of the jacket, unit W / m 2 ;

[0047] Wherein, c is the specific heat capacity of the heat medium (unit: J / (kg·K), preset constant), ρ is the density of the heat medium (unit: kg / m 3 , preset constant), S is the heat exchange area of the jacket (unit: m 2 , equipment inherent parameter);

[0048] According to the running process of the reactor, the real-time temperature deviation of each position at each running time is obtained, if each real-time temperature deviation in the reactor is lower than the set temperature deviation threshold, it is concluded that the temperature uniformity inside the reactor meets the standard, and no multi-stage compensation is needed; if each real-time temperature deviation in the reactor is not lower than the set temperature deviation threshold, it is concluded that the temperature uniformity inside the reactor does not meet the standard, and multi-stage compensation is needed;

[0049] It needs to be explained that the set temperature deviation threshold is set artificially according to the high uniformity requirement;

[0050] According to the comparison of the temperature deviation and the temperature deviation threshold, the position of the reactor that needs to be adjusted for uniformity is determined, and is marked as the position to be compensated;

[0051] The dynamic compensation coefficient is calculated, the influence of reaction viscosity μ on heat transfer is considered (the higher the viscosity, the lower the heat transfer efficiency, and a higher compensation coefficient is required), and the dynamic compensation coefficient K is defined i (unitless), and the calculation logic is "base coefficient + viscosity correction term": the formula is: K i = K0×(1+k μ × μ);

[0052] K0 is the base compensation coefficient (a preset constant, set according to the characteristics of the device), k μ is the viscosity correction coefficient (a preset constant), and μ is the real-time reaction viscosity;

[0053] According to the temperature deviation T pi of the position to be compensated and the dynamic compensation coefficient K i , the heat flow compensation amount q bi (unit: W) that needs to be additionally inputted / removed in the region is calculated, and the formula logic is "the larger the deviation, the higher the viscosity, and the larger the compensation amount": q bi = K i × T pi × S i ;

[0054] S i is the heat exchange area corresponding to the position to be compensated;

[0055] According to the heat flow compensation amount corresponding to the position to be compensated, targeted compensation is performed, and the heat flow compensation amount is sent to the administrator terminal in real time;

[0056] The mechanism coordination constraint control process is as follows:

[0057] After the position to be compensated is compensated according to the heat flow compensation amount, mechanism coordination constraint control is performed;

[0058] The temperature change rate and the crystallinity change rate in the reaction kettle are collected;

[0059] It needs to be explained that the temperature change amount can be collected by a high-precision thermocouple, and the crystallinity change rate can be collected by an online Raman spectrometer;

[0060] The change rate ratio is calculated by the ratio of the temperature change rate and the crystallinity change rate;

[0061] During the operation stage of the reaction kettle, the valve opening degree of the heat conducting oil and the valve opening degree of the cold water are collected synchronously, and the opening degree deviation is calculated according to the difference value of the opening degree, and the opening degree deviation is ensured to be positive by the absolute value symbol;

[0062] The opening degree deviation and the change rate ratio are respectively the parameters for judging the conflict degree of the reaction kettle mechanism, and thus the analysis is performed:

[0063] If the change rate ratio of the reactor exceeds the set change rate ratio threshold, or the opening deviation of the reactor exceeds the opening deviation threshold, it is inferred that the temperature changes fast and the actuator action difference is large in the reactor running stage, the oscillation risk is high, the actuator running control signal is generated and sent to the administrator terminal, the administrator terminal controls the actuator running in the reactor in the current stage, and the actuator action difference is reduced, such as control sensitivity;

[0064] If the change rate ratio of the reactor does not exceed the set change rate ratio threshold, and the opening deviation of the reactor does not exceed the opening deviation threshold, it is inferred that the actuator action difference is small in the reactor running stage, the oscillation risk is low, the actuator running signal is generated and sent to the administrator terminal;

[0065] In use, the application collects multi-dimensional data, collects multi-dimensional data of the reactor, analyzes and processes the collected multi-dimensional data, analyzes the internal mechanism of the reactor, and makes a decision on the operation of the reactor.

[0066] The threshold or preset value, preset range and the like are set for result comparison and analysis, so as to determine whether it is good or bad, and the size of the value is set according to the large model analysis of sample data and artificial experience, and is recorded and stored, and can be adjusted according to seasonal or rational influence conditions.

[0067] The weight proportion coefficient and influence factor are set according to the influence of each parameter on the result, and the specific value is finally reflected on the influence of the result, and is recorded and stored by combining the large model analysis of sample data and artificial experience, and can be adjusted according to seasonal or rational influence conditions.

[0068] The preferred embodiments of the application disclosed above are only used to help explain the application. The preferred embodiments do not describe all the details, nor limit the application to the specific embodiments. Obviously, many modifications and changes can be made according to the content of the specification. The specification selects and describes these embodiments in order to better explain the principles and practical applications of the application, so that those skilled in the art can well understand and utilize the application. The application is limited by the claims and their entire scope and equivalents.

Claims

1. A high-uniformity temperature control method based on multi-stage heat flow compensation of a reaction kettle, characterized in that, The temperature control method is as follows: Step one, multi-dimensional data acquisition, multi-dimensional data acquisition is performed on the reaction kettle; Step two, data analysis and processing, according to the collected multi-dimensional data for analysis and processing; Step three, mechanism collaborative constraint control, according to the analysis of the internal mechanism operation of the reaction kettle, the operation decision of the reaction kettle is made.

2. The high-uniformity temperature control method based on multi-stage heat flow compensation of a reaction kettle according to claim 1, characterized in that, The process of step one multi-dimensional data acquisition is as follows: According to the structure of the reaction kettle, different orientation analysis is carried out, the reaction kettle is divided into three sections in the axial direction, and the collected temperatures are marked as T1, T2 and T3 respectively; and the reaction kettle is divided into two layers in the radial direction, and the collected temperatures are marked as T4 and T5; at the same time, the inlet temperature, outlet temperature and heat flow of the jacket heat medium in the reaction kettle are collected, and are marked as T in , T out and Q respectively; according to the reaction system of the reaction kettle, the real-time heat release rate q and the viscosity μ of the reaction system are collected.

3. The high-uniformity temperature control method based on multi-stage heat flow compensation of a reaction kettle according to claim 2, characterized in that, The process of step two data analysis and processing is as follows: According to the temperature values of each position inside the reaction kettle, the mean value is calculated, and the temperature mean value is marked as T 均 ; and according to the temperature values of each position and the temperature mean value, the temperature deviation of each position is obtained, and the label T pi is set; i takes the value of 1-5, which represents five positions divided by the reaction kettle; The actual heat flow density of the jacket is collected through the formula.

4. The high-uniformity temperature control method based on multi-stage heat flow compensation of a reaction kettle according to claim 3, characterized in that, According to the running process of the reaction kettle, the real-time temperature deviation of each position corresponding to each running time is obtained, if each real-time temperature deviation in the reaction kettle is lower than the set temperature deviation threshold, it is inferred that the temperature uniformity in the reaction kettle meets the standard, and multi-stage compensation is not needed; If each real-time temperature deviation in the reaction kettle is not lower than the set temperature deviation threshold, it is inferred that the temperature uniformity in the reaction kettle does not meet the standard, and multi-stage compensation is needed.

5. The high-uniformity temperature control method based on multi-stage heat flow compensation of a reaction kettle according to claim 4, characterized in that, According to the comparison of temperature deviation and temperature deviation threshold, the position of the reaction kettle that needs to be adjusted for uniformity is determined, and is marked as a position to be compensated; The dynamic compensation coefficient is calculated; According to the temperature deviation of the position to be compensated and the dynamic compensation coefficient, the heat flow compensation amount is calculated; According to the heat flow compensation amount corresponding to the position to be compensated, targeted compensation is carried out, and the heat flow compensation amount is sent to the administrator terminal in real time.

6. The high-uniformity temperature control method based on multi-stage heat flow compensation of a reaction kettle according to claim 5, characterized in that, The process of step three mechanism collaborative constraint control is as follows: After the targeted compensation according to the heat flow compensation amount at the position to be compensated, mechanism collaborative constraint control is carried out; The temperature change rate and the crystallinity change rate in the reaction kettle are collected; The change rate ratio is calculated through the ratio of the temperature change rate and the crystallinity change rate; During the operation stage of the reaction kettle, the valve opening degree of the heat conducting oil and the valve opening degree of the cold water are collected synchronously, and the opening degree deviation is calculated according to the difference value of the opening degree.

7. The high-uniformity temperature control method based on multi-stage heat flow compensation of a reaction kettle according to claim 6, characterized in that, If the change rate ratio of the reaction kettle exceeds the set change rate ratio threshold, or the opening degree deviation of the reaction kettle exceeds the opening degree deviation threshold, an execution mechanism operation control signal is generated and sent to the administrator terminal; If the change rate ratio of the reaction kettle does not exceed the set change rate ratio threshold, and the opening degree deviation of the reaction kettle does not exceed the opening degree deviation threshold, an execution mechanism operation signal is generated and sent to the administrator terminal.

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