An adipic acid production storage device

By monitoring and optimizing the operating speed of the stirring and cooling structures in real time within the adipic acid production equipment, the problem of unstable reaction conditions under a fixed speed was solved, thereby improving production quality and efficiency.

CN119680475BActive Publication Date: 2025-11-11ZHENGZHOU UNIV
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Patent Information

Application Number
CN202411841192.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-12-13
Publication Date
2025-11-11
Estimated Expiration
2044-12-13

AI Technical Summary

Technical Problem

The fixed operating speed in existing adipic acid production equipment cannot maintain stable reaction conditions, resulting in reduced production quality and efficiency.

Method used

A reaction monitoring module is used to collect temperature, pressure and concentration data in real time. Data analysis and control chips are used to optimize the operating speed of the stirring and cooling structures and adjust the reaction conditions to maintain stability.

Benefits of technology

This improved the quality and efficiency of adipic acid production, ensuring the stability of reaction conditions and product quality.

✦ Generated by Eureka AI based on patent content.

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Abstract

This invention relates to the field of mixing equipment technology, specifically to an adipic acid production and storage device. The device includes a reaction monitoring module, a reaction regulation module, and a substance extraction module. The reaction monitoring module includes a data acquisition module and a data analysis and control chip. The reaction regulation module includes a stirring structure and a cooling structure. The data analysis and control chip analyzes and processes the data acquired in real time by the data acquisition module to obtain the required temperature regulation value, and combines this with the changing trends of reactant and product concentrations over the monitoring period to obtain the reaction condition optimization coefficient. The chip adjusts the operating speed of the stirring and cooling structures in real time until the reactant concentration at the current moment meets the stopping condition, at which point the stirring and cooling structures are stopped, and the substance extraction module extracts adipic acid. This invention provides higher efficiency in the production of adipic acid.
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Description

Technical Field

[0001] This invention relates to the field of mixing equipment technology, and more specifically to an adipic acid production and storage device. Background Technology

[0002] Adipic acid is an important chemical raw material widely used in nylon, plastics, coatings, and synthetic fibers. With increasing market demand for high-performance materials, the technical requirements for adipic acid production and storage equipment are becoming increasingly stringent to ensure production efficiency, product quality, and environmental safety. Therefore, the efficiency and stability of adipic acid production equipment directly affect production costs and product quality, making the development of efficient and safe adipic acid production and storage equipment particularly important.

[0003] In existing adipic acid production equipment, the stirring and cooling structures are adjusted at a fixed operating speed to avoid side reactions during the reaction process and improve product quality. Different reaction conditions occur at different stages of the reaction, but a fixed operating speed cannot maintain stable reaction conditions, thus reducing the production quality and efficiency of adipic acid. Summary of the Invention

[0004] To address the technical problem that a fixed operating speed cannot maintain stable reaction conditions during adipic acid production, thus reducing the quality and efficiency of adipic acid production, the present invention aims to provide an adipic acid production and storage device. The specific technical solution adopted is as follows:

[0005] An adipic acid production and storage device, the adipic acid production and storage device includes a reaction monitoring module, a reaction regulation module, a substance extraction module and a reaction vessel, the reaction monitoring module includes a data acquisition module and a data analysis and control chip, and the reaction regulation module includes a stirring structure and a cooling structure;

[0006] The data acquisition module is connected to the signal input terminal of the data analysis and control chip, and the signal output terminal of the data analysis and control chip is connected to the reaction regulation module. The data acquisition module is used to collect the temperature, pressure, reactant concentration, and product concentration of the reaction vessel at each moment during the monitoring period in real time, and transmit them to the data analysis and control chip. The end time of the monitoring period is the current time.

[0007] The data analysis and control chip is used to obtain the temperature regulation requirement value based on the fluctuation of temperature values ​​and the abrupt change of pressure values ​​in the set of temperature values ​​at all times within the monitoring period.

[0008] Based on the changing trends of reactant and product concentrations during the monitoring period, and the temperature regulation requirement, an optimization coefficient for reaction conditions is obtained. The operating speed of the stirring and cooling structures is adjusted in real time using the optimization coefficient. When the reactant concentration at the current moment meets the stopping condition, the stirring module and cooling structure are stopped, and adipic acid is extracted using the substance extraction module.

[0009] Furthermore, obtaining the temperature regulation requirement value includes:

[0010] The set of temperature values ​​includes a first temperature value and a second temperature value. One of the temperature values ​​is selected from the first temperature value and the second temperature value and recorded as the analysis temperature value. The temperature promotion effect value is obtained based on the fluctuation of the analysis temperature value at all times during the monitoring period and the difference between the first temperature value and the second temperature value.

[0011] The overall mutation value is obtained by comparing the pressure value at each moment within the monitoring period with the pressure value at a time within a preset adjacent window.

[0012] Based on the temperature-promoting effect value and the overall mutation value, the temperature regulation requirement value is obtained.

[0013] Furthermore, obtaining the temperature-promoting effect value includes:

[0014] The variance of the analyzed temperature values ​​at all times within the monitoring period is recorded as the temperature fluctuation index; the mean of the absolute values ​​of the differences between the analyzed temperature values ​​at all times within the monitoring period and the expected constant temperature value is calculated as the constant temperature difference index.

[0015] Based on the temperature fluctuation index and the isothermal difference index, a positive temperature promotion value is obtained; both the temperature fluctuation index and the isothermal difference index are negatively correlated with the positive temperature promotion value.

[0016] The concentrated value of the analyzed temperature values ​​at all times within the monitoring period is obtained and recorded as the temperature concentration index; the absolute value of the difference between the temperature concentration index of the first temperature value and the temperature concentration index of the second temperature value is taken as the temperature difference value.

[0017] The temperature-promoting effect value is obtained based on the temperature difference value and the temperature-positive promoting value; the temperature-positive promoting value and the temperature-promoting effect value are positively correlated, and the temperature difference value and the temperature-promoting effect value are negatively correlated.

[0018] Further, the acquisition of the positive temperature-enhancing value includes:

[0019] Calculate the sum of the differences between the pressure values ​​at each time point and the pressure values ​​at other times within a preset neighboring window, and record the absolute value of the sum as the local abrupt change value at each time point;

[0020] The average of the local mutation values ​​at all times within the monitoring period is taken as the overall mutation value.

[0021] Further, obtaining the reaction condition optimization coefficients includes:

[0022] The concentrations of reactants and products are denoted as analytical concentrations; the correlation coefficients between the analytical concentrations at all times within the monitoring period are obtained and denoted as analytical trend indicators; the difference between the analytical trend indicators of product concentration and reactant concentration is denoted as trend difference indicators.

[0023] The product of the analytical trend index of the product concentration and the trend difference index is used as the reaction efficiency index.

[0024] Based on the temperature regulation requirement and the reaction efficiency index, the reaction condition optimization coefficient is obtained.

[0025] Furthermore, the real-time adjustment of the operating speed of the stirring structure and the cooling structure using the reaction condition optimization coefficient includes:

[0026] The cooling structure achieves cooling through a cooling medium flowing inside it.

[0027] The sum of constant 1 and the reaction condition optimization coefficient is used as the adjustment coefficient at the current moment;

[0028] If the analytical trend index of the product concentration is greater than a preset trend threshold, the preset standard flow rate is weighted using the adjustment coefficient to obtain the optimized flow rate of the cooling medium in the cooling structure at the current moment; otherwise, the preset standard rotation speed is weighted using the adjustment coefficient to obtain the optimized rotation speed of the stirring structure at the current moment.

[0029] The optimized flow rate corresponding to the cooling structure is the operating speed of the cooling structure, and the optimized rotation speed of the stirring structure is the operating speed of the stirring structure.

[0030] Furthermore, the reactant concentration at the current moment satisfies the stopping condition when the reactant concentration at the current moment is less than a preset concentration limit value.

[0031] Furthermore, the setpoint is the mean.

[0032] Furthermore, the correlation coefficient is the Pearson correlation coefficient.

[0033] Furthermore, the length of the preset adjacent window is 3.

[0034] The present invention has the following beneficial effects:

[0035] This invention deploys a reaction monitoring module on adipic acid production and storage equipment. The data acquisition module within this module collects data from the reaction vessel over a specific time period, providing a data foundation for subsequent adjustments to the operating speeds of the stirring and cooling structures in the reaction regulation module. The degree of temperature fluctuation within the monitoring period reflects the temperature's promoting effect on the reaction. Since pressure changes within the reaction vessel cause temperature fluctuations during the isothermal phase, the degree of pressure abrupt changes within the monitoring period reflects the reliability of the temperature values ​​within the reaction vessel. Combining these two factors improves the accuracy of the temperature's promoting effect on the reaction. The temperature-related promoting effect represents the required temperature control intensity within the reaction vessel, thus yielding the temperature regulation demand value. In the actual production of adipic acid, the concentration trends of reactants and products directly represent the reaction efficiency. Analyzing this, combined with the temperature regulation demand value reflecting the required adjustment intensity within the reaction vessel, improves the accuracy of the temperature regulation demand, yielding a reaction condition optimization coefficient. Using this reaction condition optimization coefficient to adjust the operating speeds of the stirring and cooling structures in real time effectively maintains stable reaction conditions within the reaction vessel, thereby improving the production quality and efficiency of adipic acid. Attached Figure Description

[0036] To more clearly illustrate the technical solutions and advantages in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0037] Figure 1 This is an external structural diagram of an adipic acid production and storage device provided in one embodiment of the present invention;

[0038] Figure 2 This is an overall structural diagram of an adipic acid production and storage device provided in one embodiment of the present invention;

[0039] Figure 3 This is an internal structural diagram of an adipic acid production and storage device provided in one embodiment of the present invention;

[0040] Figure 4 This is a flowchart illustrating a method performed by an adipic acid production and storage apparatus according to an embodiment of the present invention.

[0041] The labels in the attached diagram are as follows: 1. Reaction vessel; 2. Drive motor with controller; 3. Bolt; 4. Vessel support; 5. Outlet; 6. Pressure sensor; 7. Online monitoring center; 8. Valve; 9. Filter box; 10. Drying oven; 11. Product outlet; 12. Circulation pipe inlet; 13. Circulation pipe; 14. Temperature sensor; 15. Solid pipe; 16. Agitator; 17. Circulation pipe outlet; 18. Slip ring. Detailed Implementation

[0042] To further illustrate the technical means and effects adopted by the present invention to achieve its intended purpose, the following detailed description, in conjunction with the accompanying drawings and preferred embodiments, details the specific implementation, structure, features, and effects of an adipic acid production and storage device proposed according to the present invention. In the following description, different "one embodiment" or "another embodiment" do not necessarily refer to the same embodiment. Furthermore, specific features, structures, or characteristics in one or more embodiments can be combined in any suitable form.

[0043] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains.

[0044] The adipic acid production and storage device provided in this embodiment of the invention includes a reaction monitoring module, a reaction regulation module, a substance extraction module, and a reaction vessel. The reaction vessel is where the reactants react. The reaction monitoring module is used to detect and analyze the reaction status in the reaction vessel. Therefore, the reaction monitoring module includes a data acquisition module and a data analysis and control chip. The data acquisition module is connected to the data analysis and control chip, which is used for data processing and machine control. The chip type is FPGA, which receives information from the data acquisition module and sends control commands to the reaction regulation module.

[0045] The following description, in conjunction with the accompanying drawings, details a specific scheme for an adipic acid production and storage device provided by the present invention.

[0046] Please see Figure 1 , Figure 2 and Figure 3 These accompanying drawings illustrate a structural diagram of an adipic acid production and storage device according to an embodiment of the present invention. The adipic acid production and storage device includes: a reaction vessel 1; a drive motor 2 with a controller; bolts 3; a container support 4; a water outlet 5; a pressure sensor 6; an online monitoring center 7; a valve 8; a filter box 9; a drying oven 10; a product outlet 11; a circulation pipe inlet 12; a circulation pipe 13; a temperature sensor 14; a solid pipe 15; a water-repellent plate 16; a circulation pipe outlet 17; and a slip ring 18.

[0047] The data acquisition module is connected to the signal input terminal of the data analysis and control chip, and the signal output terminal of the data analysis and control chip is connected to the reaction regulation module. The data acquisition module is used to collect the temperature value, pressure value, reactant concentration and product concentration of the reaction vessel 1 at each moment during the monitoring period in real time, and transmit them to the data analysis and control chip. The end time of the monitoring period is the current time.

[0048] In this embodiment of the invention, a data acquisition module is composed of a pressure sensor 6, a temperature sensor 14, and an online monitoring center 7. The stirring structure consists of a circulation pipe 13, a solid pipe 15, and a water-splashing plate 16; the cooling structure consists of a circulation pipe inlet 12, a circulation pipe 13, and a circulation pipe outlet 17; the stirring structure and the cooling structure together constitute a reaction regulation module. The substance extraction module consists of a filter box 9, a drying box 10, and a product outlet. The online monitoring center 7 is used to collect the concentrations of reactants and products within the reaction vessel.

[0049] In the initial stage of the reaction between reactants and catalyst, the oxidation reaction proceeds from outside the solution to inside the solution. To ensure thorough mixing between reactants and catalyst and to guarantee synchronous reaction, in this embodiment of the invention, the traditional vertical stirring shaft of the adipic acid production and storage equipment is replaced with a crank stirring shaft. The solid pipe 15 of the stirring structure is to avoid the problem of large liquid resistance that hollow pipes are prone to during stirring. The three agitators 16 can also stir the solution during rotation, providing a certain stirring effect.

[0050] The cooling medium enters the cooling structure from the inlet 12 of the circulation pipe, flows through the circulation pipe 13, and then exits from the outlet 17 of the circulation pipe. The circulation pipe 13 is hollow; this hollow structure is used to regulate the temperature during the reaction process and eliminate excess heat generated during the reaction. A slip ring 18, also known as a rotary joint, is located near the inlet 12 of the circulation pipe. It is a device that allows fluid to pass through a rotating component, maintaining a relative stationary position between the inlet 12 of the circulation pipe and the rotating shaft while allowing the cooling medium to flow during rotation.

[0051] It should be noted that in this embodiment of the invention, the pressure sensor 6, temperature sensor 14, and online monitoring center all acquire data once every 3 seconds, and the data acquisition times for all three are the same. Implementers can set this according to their specific circumstances. Figure 3As shown, the device in this embodiment has two temperature sensors. One is located on the left side of the solid pipe 15, and the temperature value collected by this sensor is recorded as the first temperature value. The other is located on the right side of the solid pipe 15, and the temperature value collected by this sensor is recorded as the second temperature value. These sensors are used to collect the temperature at different locations in the solution. The monitoring time period is the time between the moment the reactant and catalyst are added to the reaction vessel and the moment the vessel lid is closed, and the current moment. In this embodiment, the reactant is benzene, but it can also be hexene or cycloethylene; the catalyst is a ruthenium-based catalyst or a nickel catalyst, etc.

[0052] The steps for operating adipic acid production and storage equipment are as follows:

[0053] (1) Add the reactants and catalyst to the reaction vessel 1 and fix the container lid with the bolts 3 on the container lid.

[0054] (2) The drive motor 2 with a controller is connected to the stirring structure. After the reaction vessel is sealed, the drive motor is started by the controller to drive the stirring structure to rotate, thereby stirring the solution.

[0055] (3) When the temperature inside the reaction vessel reaches a certain value, the temperature inside the reaction vessel is adjusted by injecting cooling medium into the cooling structure.

[0056] (4) After the reaction is complete, open valve 8, and the container after the reaction is complete will flow out through outlet 5. Adipic acid will be extracted using the substance extraction module. The specific extraction method is as follows: after the reaction is complete, the container will flow through outlet 5 to filter box 9 of the substance extraction module. Filter box 9 will filter out solid particles in the solution after the reaction. Then, the filtered solution will be distilled and crystallized through drying box 10. After that, the solute in the solution will be further dried through product outlet 11. Finally, the processed adipic acid will be stored.

[0057] Please see Figure 4 The diagram illustrates a method flow chart of an adipic acid production and storage device according to an embodiment of the present invention, the method comprising the following steps:

[0058] Step S100: Based on the degree of temperature fluctuation and the degree of pressure change in the set of temperature values ​​at all times within the monitoring period, obtain the temperature regulation requirement value.

[0059] Since the reactants in the reaction vessel produce products through oxidation, and oxidation is an exothermic process, and the actual reaction process may require heating of the reaction vessel, the temperature change of the reaction vessel during the entire reaction process generally goes through three stages: the heating stage, the isothermal stage, and the cooling stage. The temperature gradually increases in the early stage of the reaction, remains stable after reaching a certain temperature, and gradually decreases after the reaction is completed.

[0060] The degree of temperature fluctuation within the monitoring period reflects the promoting effect of temperature on the reaction. Since pressure changes within the reaction vessel cause temperature fluctuations during the isothermal phase, the degree of pressure abrupt change within the monitoring period reflects the reliability of the temperature values ​​within the reaction vessel. Combining these two factors improves the accuracy of the promoting effect of temperature on the reaction. The promoting effect corresponding to temperature can represent the required level of temperature control within the reaction vessel, thus yielding the temperature regulation demand value.

[0061] Step S110: The temperature value set includes a first temperature value and a second temperature value. Select one temperature value from the first temperature value and the second temperature value and record it as the analysis temperature value. Based on the fluctuation of the analysis temperature value at all times during the monitoring period and the difference between the first temperature value and the second temperature value, obtain the temperature promotion effect value.

[0062] Preferably, in some possible implementations of this embodiment, the method for obtaining the temperature-promoting effect value includes: obtaining the variance of the analyzed temperature values ​​at all times within the monitoring period and recording it as a temperature fluctuation index; calculating the mean of the absolute values ​​of the differences between the analyzed temperature values ​​at all times within the monitoring period and the expected constant temperature value, as a constant temperature difference index; obtaining a positive temperature-promoting value based on the temperature fluctuation index and the constant temperature difference index; both the temperature fluctuation index and the constant temperature difference index are negatively correlated with the positive temperature-promoting value; obtaining the setpoint of the analyzed temperature values ​​at all times within the monitoring period and recording it as a temperature setpoint index; taking the absolute value of the difference between the temperature setpoint index of the first temperature value and the temperature setpoint index of the second temperature value as a temperature difference value; obtaining a temperature-promoting effect value based on the temperature difference value and the positive temperature-promoting value; the positive temperature-promoting value and the temperature-promoting effect value are positively correlated, and the temperature difference value and the temperature-promoting effect value are negatively correlated.

[0063] The expected isothermal value is the temperature that favors product formation. During the reaction, the closer the temperature is to the expected isothermal value and the more stable it remains, the better it is for product formation, thus positively promoting the reaction. The temperature fluctuation index reflects the temperature fluctuations within the monitoring period. The smaller the temperature fluctuation index and the isothermal difference index, the closer the temperature is to the expected isothermal value and the more stable it is during the reaction, which is more conducive to product formation. The greater the degree to which temperature promotes the reaction during the monitoring period, the greater the positive temperature promotion value. Therefore, both the temperature fluctuation index and the isothermal difference index are negatively correlated with the positive temperature promotion value. In this embodiment, the product of the temperature fluctuation index and the isothermal difference index is negatively correlated and normalized to obtain the positive temperature promotion value.

[0064] It should be noted that this embodiment uses an exponential function with the natural constant as the base for negative correlation and normalization. Specifically, the opposite of the product of the temperature fluctuation index and the isothermal difference index is taken, and this opposite is used as the exponent of the exponential function with the natural constant as the base, thus achieving negative correlation and normalization. Variance, standard deviation, and range can all reflect the degree of fluctuation of a set of data. In this embodiment, the variance in the calculation of the temperature fluctuation index can also be replaced with standard deviation or range, etc., which is not limited here. Since the isothermal stage is the longest among the three stages of the solution reaction process, this embodiment uses the mode of the first or second temperature value in the other adipic acid formation process as the preset isothermal value; it can also be set according to the actual situation.

[0065] During a solution reaction, inconsistent reaction conditions at different locations within the solution, i.e., significant temperature differences, can slow down the reaction rate. The first and second temperature values ​​at the same moment represent the temperatures at different locations within the solution; the temperature concentration index reflects the overall level of the analyzed temperature values ​​over the monitoring period. The smaller the difference between the first and second temperature values ​​within the monitoring period—that is, the smaller the absolute value of the difference between the temperature concentration indices of the first and second temperatures—it indicates that the reaction conditions at different locations within the solution are more consistent, and the better the temperature-promoting effect on the reaction during the monitoring period. In summary, a larger positive temperature-promoting value and a smaller temperature difference value indicate a better temperature-promoting effect on the reaction during the monitoring period, and a larger temperature-promoting effect value. Therefore, the temperature difference value and the temperature-promoting effect value are negatively correlated, while the positive temperature-promoting value and the temperature-promoting effect value are positively correlated.

[0066] In this embodiment, the ratio of the positive temperature-promoting value (numerator) to the sum of the temperature difference value and a preset positive number (denominator) is used as the temperature-promoting effect value. It should be noted that the preset positive number is an empirical value of 0.1, used to prevent the fraction from being meaningless due to a denominator of 0. In other embodiments, the correlation between the positive temperature-promoting value, the temperature difference value, and the temperature-promoting effect value can also be constructed through other basic mathematical operations; these are not limited or elaborated upon here.

[0067] Step S120: Obtain the overall mutation value based on the difference between the pressure value of each moment within the monitoring period and the time within the preset neighboring window.

[0068] In actual production, there are many factors that make it difficult to keep the temperature completely constant during the isothermal stage. Specifically, pressure changes in the reaction vessel can affect the boiling point of the liquid. Increased pressure can raise the boiling point of the reactants and solvents. The equipment may require more energy to maintain a constant temperature, which can lead to temperature fluctuations in the reaction vessel.

[0069] Preferably, in some possible implementations of this embodiment, the method for obtaining the overall mutation value includes: calculating the sum of the differences between the pressure values ​​at each time point and the pressure values ​​at other times within a preset neighboring window, and recording the absolute value of the sum as the local mutation value at each time point; and taking the average of the local mutation values ​​at all times within the monitoring period as the overall mutation value.

[0070] Local mutation values ​​represent the degree of change in pressure values ​​at each time point compared to those at neighboring times. A larger local mutation value indicates a greater difference between the pressure value at each time point and its neighboring times, thus indicating a greater degree of mutation at that time. The overall mutation value represents the overall level of mutation across all times within the monitoring period. The average of the local mutation values ​​across all times within the monitoring period can be used as the overall mutation value.

[0071] It should be noted that in this embodiment, the length L of the preset neighboring window is taken as an empirical value of 3, and the width is 1. The position at each moment and the center position of its preset neighboring window can be set by the implementer according to the specific situation. The monitoring period begins... The moment and the end If the preset neighbor window at a given time step is incomplete and local mutation values ​​cannot be obtained, then the local mutation values ​​at the aforementioned time steps need not be considered during the process of obtaining the overall mutation values. Wherein, This is the floor symbol.

[0072] Step S130: Obtain the temperature regulation requirement value based on the temperature promotion effect value and the overall mutation value.

[0073] The smaller the temperature-promoting effect value, the worse the temperature-promoting effect on the reaction during the monitoring period. To accelerate the reaction efficiency, a greater degree of temperature control is needed within the reaction vessel. Conversely, the larger the overall abrupt change value, the stronger the abrupt change in pressure value during the monitoring period. This indicates a greater likelihood that the promoting effect on the reaction solution within the reaction vessel originates from pressure changes within the vessel, thus reducing the reliability of temperature changes. To maintain the accuracy of the control analysis, a smaller degree of temperature control should be applied to the reaction vessel. In this embodiment, the larger the temperature regulation requirement value, the greater the adjustment required to the temperature within the reaction vessel. Therefore, both the temperature-promoting effect value and the overall abrupt change value are negatively correlated with the temperature regulation requirement value.

[0074] In one specific implementation of this embodiment, the temperature regulation requirement is expressed by the formula:

[0075]

[0076] In the formula, w is the temperature regulation requirement; D is the positive temperature promotion value; and H is the temperature difference value. ε is the temperature-enhancing effect value; ST is the overall mutation value; ε is a preset positive number; exp is an exponential function with the natural constant e as the base.

[0077] Step S200: Based on the difference in the changing trends of reactant and product concentrations during the monitoring period, and the temperature adjustment requirements, obtain the reaction condition optimization coefficient; use the reaction condition optimization coefficient to adjust the operating speed of the stirring and cooling structures in real time; until the reactant concentration at the current moment meets the stopping conditions, stop the stirring module and the cooling structure, and use the substance extraction module to extract adipic acid.

[0078] In the actual production process of adipic acid, the concentration trends of reactants and products directly represent the reaction efficiency. This is combined with analysis of the temperature regulation requirements within the reaction vessel to improve the accuracy of temperature control and obtain the reaction condition optimization coefficient. In this example, the reactant is hexene, and the product is adipic acid.

[0079] Preferably, in some possible implementations of this embodiment, the method for obtaining the reaction condition optimization coefficient includes: recording the reactant concentration and product concentration as the analytical concentration; obtaining the correlation coefficient between the analytical concentrations corresponding to all times within the monitoring period, and recording it as the analytical trend index; recording the difference between the analytical trend index of the product concentration and the analytical trend index of the reactant concentration as the trend difference index; using the product of the analytical trend index of the product concentration and the trend difference index as the reaction efficiency index; and obtaining the reaction condition optimization coefficient based on the temperature regulation requirement and the reaction efficiency index.

[0080] The analytical trend index represents the trend of changes in analytical concentrations. Reaction efficiency is usually determined by both the reaction rate and the conversion rate. A larger trend in product concentration indicates a faster reaction rate; a smaller trend in reactant concentration indicates a higher conversion rate. A larger difference between the trends in product and reactant concentrations (i.e., the trend difference index), meaning a larger trend in product concentration and a smaller trend in reactant concentration, indicates a faster reaction and that most reactants are converted into products, thus resulting in higher reaction efficiency. The trend in product concentration directly reflects reaction efficiency; a larger analytical trend index for reactant concentration indicates higher reaction efficiency. Therefore, both the analytical trend index and the trend difference index for product concentration are positively correlated with reaction efficiency. In this embodiment, the product of the analytical trend index and the trend difference index for product concentration is used as the reaction efficiency index.

[0081] A higher reaction efficiency index indicates a faster oxidation rate during the reaction process, potentially releasing more heat. However, excessively high temperatures can easily lead to side reactions. To avoid these side reactions, a greater degree of temperature reduction is required within the reaction vessel. Conversely, a higher temperature regulation requirement necessitates a more drastic adjustment to the temperature within the reaction vessel. Therefore, both the temperature regulation requirement and the reaction efficiency index are positively correlated with the reaction condition optimization coefficient.

[0082] It should be noted that the specific steps for obtaining the correlation coefficient between all times and the corresponding analytical concentrations within the monitoring period are as follows: The times within the monitoring period are constructed into a time sequence, with elements numbered 1, 2, 3, 4, ... from beginning to end, and the last element equals the total number of times within the monitoring period; the analytical concentrations within the monitoring period are arranged chronologically to obtain a concentration sequence; and the correlation coefficient between the time sequence and the concentration sequence is obtained. In this embodiment, the correlation coefficient is the Pearson correlation coefficient; in other embodiments, the correlation coefficient can also be the Spearman correlation coefficient, Kendall rank correlation coefficient, or canonical correlation coefficient, etc.

[0083] In the actual production process of adipic acid, temperature fluctuations in the reaction vessel may be caused by the exothermic oxidation reaction or by various factors during the actual operation of the equipment. The optimization methods for reaction conditions differ depending on the influencing factors.

[0084] During the production and storage of adipic acid, when the analytical trend index of the product concentration exceeds the preset trend threshold, it indicates that the product concentration in the reaction vessel increases over time, the oxidation rate during the reaction is high, and the temperature fluctuations in the reaction vessel are caused by the exothermic behavior of the oxidation reaction, releasing more heat. The temperature of the reaction vessel can be lowered to a stable state by increasing the flow rate of the cooling medium, thereby eliminating the heat generated by the oxidation reaction and ensuring stable reaction conditions and reliable product quality. It should be noted that the cooling structure in the adipic acid production and storage equipment achieves cooling through the cooling medium flowing inside it. Increasing the flow rate of the cooling medium can improve the heat transfer coefficient, thus improving the cooling effect to a certain extent.

[0085] When the analytical trend index of the product concentration is less than or equal to the preset trend threshold, it indicates that there are unexpected temperature fluctuations in the reaction process. The temperature fluctuations in the reaction vessel can be reduced by increasing the stirring speed of the stirring equipment to ensure thorough mixing of the reactants.

[0086] Preferably, in some possible implementations of this embodiment, the method for adjusting the operating speed of the stirring structure and the cooling structure includes: using the sum of the constant 1 and the reaction condition optimization coefficient as the adjustment coefficient at the current moment; determining whether the analytical trend index of the product concentration is greater than a preset trend threshold; if so, using the adjustment coefficient to weight the preset standard flow rate to obtain the optimized flow rate of the cooling medium in the cooling structure at the current moment; if not, using the adjustment coefficient to weight the preset standard rotation speed to obtain the optimized rotation speed of the stirring structure at the current moment; the optimized flow rate corresponding to the cooling structure is the operating speed of the cooling structure, and the optimized rotation speed of the stirring structure is the operating speed of the stirring structure.

[0087] If the structure being adjusted at the current moment is a stirring structure, then the optimal rotational speed of the stirring structure within the time interval between the current moment and the next moment when the structure is adjusted to be a stirring structure is set as the optimal flow rate at the current moment. The adjustment method for the cooling structure is similar and will not be described here. As an example, assume that the structure being adjusted at time t is a stirring structure and the optimal rotational speed is v_b. t At time t+1, the adjusted structure is a cooling structure and the optimized flow rate is v_w. t+1 At time t+2, the adjusted structure is a cooling structure and the optimized flow rate is v_w. t+2 At time t+3, the adjusted structure is a stirring structure and the optimized rotation speed is v_b. t+3 Then, the optimal rotational speed of the stirring structure during the time interval from time t to time t+3 is v_b. t The optimal flow rate of the cooling structure during the time interval between time t+1 and time t+2 is v_w. t+1 .

[0088] It should be noted that the preset trend threshold in this embodiment is an empirical value of 0.6, which implementers can set according to specific circumstances. The stirring equipment in the adipic acid production and storage equipment starts stirring as soon as the reactants begin to react; the cooling structure only starts operating when the temperature inside the reaction vessel exceeds a certain value, which in this embodiment is 157 degrees Celsius, and implementers can set it according to specific circumstances. The optimized rotation speed of the stirring structure and the optimized flow rate of the cooling structure are the operating speeds.

[0089] If the reactant concentration at the current moment is less than the preset concentration limit, it is considered that the reactants in the reaction vessel have reacted sufficiently, the reaction is terminated, the stirring and cooling structures stop operating, and adipic acid is extracted using the substance extraction module. If the reactant concentration at the current moment is greater than or equal to the preset concentration limit, it is considered that the reactants in the reaction vessel have not reacted sufficiently, and the reaction conditions in the production process of the adipic acid production and storage equipment need to be adjusted in real time according to the above method to maintain the stability of the reaction and ensure the quality of the product.

[0090] It should be noted that in this embodiment, the preset concentration limit is set to half of the reactant concentration at the start of the reaction. The implementer can set it according to the specific situation. In other embodiments, the conversion rate of adipic acid production process can be greater than 80% as the stopping condition of the reaction process. The conversion rate of adipic acid at the current moment is the ratio of the amount of product at the current moment to the amount of reactant at the beginning, multiplied by 100%. Other stopping conditions can also be set, which are not limited here.

[0091] The above-described embodiments are only used to illustrate the technical solutions of this application, and are not intended to limit them. Although this application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of this application, and should all be included within the protection scope of this application.

Claims

1. An adipic acid production and storage device, characterized in that, The adipic acid production and storage equipment includes a reaction monitoring module, a reaction regulation module, a substance extraction module, and a reaction vessel. The reaction monitoring module includes a data acquisition module and a data analysis and control chip. The reaction regulation module includes a stirring structure and a cooling structure. The data acquisition module is connected to the signal input terminal of the data analysis and control chip, and the signal output terminal of the data analysis and control chip is connected to the reaction regulation module. The data acquisition module is used to collect the temperature, pressure, reactant concentration, and product concentration of the reaction vessel at each moment during the monitoring period in real time, and transmit them to the data analysis and control chip; the end time of the monitoring period is the current time. The data analysis and control chip is used to obtain the temperature regulation requirement value based on the fluctuation of temperature values ​​and the abrupt change of pressure values ​​in the set of temperature values ​​at all times within the monitoring period. Based on the changing trends of reactant and product concentrations during the monitoring period, and the temperature regulation requirement, an optimization coefficient for reaction conditions is obtained. The operating speed of the stirring and cooling structures is adjusted in real time using the optimization coefficient. When the reactant concentration at the current moment meets the stopping condition, the stirring module and cooling structure are stopped, and adipic acid is extracted using the substance extraction module.

2. The adipic acid production and storage equipment according to claim 1, characterized in that, The acquisition of the temperature regulation requirement value includes: The set of temperature values ​​includes a first temperature value and a second temperature value. One of the temperature values ​​is selected from the first temperature value and the second temperature value and recorded as the analysis temperature value. The temperature promotion effect value is obtained based on the fluctuation of the analysis temperature value at all times during the monitoring period and the difference between the first temperature value and the second temperature value. The overall mutation value is obtained by comparing the pressure value at each moment within the monitoring period with the pressure value at a time within a preset adjacent window. Based on the temperature-promoting effect value and the overall mutation value, the temperature regulation requirement value is obtained.

3. The adipic acid production and storage equipment according to claim 2, characterized in that, The acquisition of the temperature-promoting effect value includes: The variance of the analyzed temperature values ​​at all times within the monitoring period is recorded as the temperature fluctuation index; the mean of the absolute values ​​of the differences between the analyzed temperature values ​​at all times within the monitoring period and the expected constant temperature value is calculated as the constant temperature difference index. Based on the temperature fluctuation index and the isothermal difference index, a positive temperature promotion value is obtained; both the temperature fluctuation index and the isothermal difference index are negatively correlated with the positive temperature promotion value. The concentrated value of the analyzed temperature values ​​at all times within the monitoring period is obtained and recorded as the temperature concentration index; the absolute value of the difference between the temperature concentration index of the first temperature value and the temperature concentration index of the second temperature value is taken as the temperature difference value. The temperature-promoting effect value is obtained based on the temperature difference value and the temperature-positive promoting value; the temperature-positive promoting value and the temperature-promoting effect value are positively correlated, and the temperature difference value and the temperature-promoting effect value are negatively correlated.

4. The adipic acid production and storage equipment according to claim 2, characterized in that, The acquisition of the positive temperature boosting value includes: Calculate the sum of the differences between the pressure values ​​at each time point and the pressure values ​​at other times within a preset neighboring window, and record the absolute value of the sum as the local abrupt change value at each time point; The average of the local mutation values ​​at all times within the monitoring period is taken as the overall mutation value.

5. An adipic acid production and storage device according to claim 1, characterized in that, The process of obtaining the reaction condition optimization coefficients includes: The concentrations of reactants and products are denoted as analytical concentrations; the correlation coefficients between the analytical concentrations at all times within the monitoring period are obtained and denoted as analytical trend indicators; the difference between the analytical trend indicators of product concentration and reactant concentration is denoted as trend difference indicators. The product of the analytical trend index of the product concentration and the trend difference index is used as the reaction efficiency index. Based on the temperature regulation requirement and the reaction efficiency index, the reaction condition optimization coefficient is obtained.

6. The adipic acid production and storage equipment according to claim 5, characterized in that, The method of adjusting the operating speed of the stirring structure and the cooling structure in real time using the reaction condition optimization coefficient includes: The cooling structure achieves cooling through a cooling medium flowing inside it. The sum of constant 1 and the reaction condition optimization coefficient is used as the adjustment coefficient at the current moment; If the analytical trend index of the product concentration is greater than a preset trend threshold, the preset standard flow rate is weighted using the adjustment coefficient to obtain the optimized flow rate of the cooling medium in the cooling structure at the current moment; otherwise, the preset standard rotation speed is weighted using the adjustment coefficient to obtain the optimized rotation speed of the stirring structure at the current moment. The optimized flow rate corresponding to the cooling structure is the operating speed of the cooling structure, and the optimized rotation speed of the stirring structure is the operating speed of the stirring structure.

7. The adipic acid production and storage equipment according to claim 1, characterized in that, The reactant concentration at the current moment meets the stopping condition when the reactant concentration at the current moment is less than a preset concentration limit value.

8. An adipic acid production and storage device according to claim 3, characterized in that, The set value is the mean.

9. An adipic acid production and storage device according to claim 5, characterized in that, The correlation coefficient mentioned is the Pearson correlation coefficient.

10. An adipic acid production and storage device according to claim 2, characterized in that, The length of the preset adjacent window is 3.

Citation Information

Patent Citations

  • Multi-point temperature sensation high-temperature reactor

    CN204485845U

  • Method and apparatus for continuously producing porous materials and metal oxide mixture by using continuous stirring reactor

    KR100627634B1