Safety control method and system for potassium tert-butoxide production based on dynamic parameter feedback

Abstract

The present application provides a safety regulation method and system for the production of potassium tert-butoxide based on dynamic parameter feedback, which relates to the technical field of potassium tert-butoxide production. The method includes the following steps: continuously monitoring the axial temperature field distribution in the evaporation and concentration section and the first concentration gradient of the decomposition products, and obtaining the temperature distribution variation coefficient according to the axial temperature field distribution; if the temperature distribution variation coefficient is greater than the first preset threshold or the first concentration gradient is greater than the second preset threshold, compensating inert gas to the evaporation and concentration section and / or reducing the final evaporation temperature in the evaporation and concentration section; obtaining the target concentration duration, and after the target concentration duration of compensating inert gas and / or reducing the final evaporation temperature is executed, determining whether the actual intermediate product concentration reaches the target product concentration; if so, keeping the preset drying parameters in the vacuum drying section unchanged and performing vacuum drying on the intermediate product to obtain potassium tert-butoxide. This solution can achieve continuous safe production and has high product consistency.

Description

Technical Field

[0001] This application relates to the technical field of potassium tert-butoxide production, and specifically relates to a safety regulation method and system for potassium tert-butoxide production based on dynamic parameter feedback. Background Art

[0002] Potassium tert-butoxide, as an important organic base, is usually industrially produced by reacting metallic potassium with tert-butanol and then through processes such as evaporation and concentration, vacuum drying, etc. The key in the evaporation and concentration section lies in controlling the reaction temperature and the accumulation of by-products. Traditional processes mostly use cyclohexane as a water-carrying agent to continuously remove water through reactive distillation, but this process has extremely high requirements for the uniformity of the temperature field. Since the axial temperature distribution during the evaporation and concentration process is easily affected by local overheating, it may cause the decomposition of potassium tert-butoxide to produce decomposition by-products such as potassium hydroxide or tert-butanol, thereby reducing the product purity. In addition, the accumulation of decomposition products will further exacerbate the stability problems of the reaction system, forming a vicious cycle.

[0003] In the prior art, temperature regulation mostly relies on empirically setting fixed parameters and lacks a real-time response mechanism to the dynamic changes of the axial temperature field. For example, the invention patent with the patent number CN118084615A mentions removing water through reactive distillation technology, but the real-time monitoring of the temperature distribution is insufficient, which may lead to too high an end evaporation temperature, causing local supersaturated crystallization or decomposition reactions. At the same time, fixed parameters are usually adopted in the vacuum drying stage. If the concentration of the intermediate product does not meet the standard and enters the drying link, it may affect the quality of the final product due to residual solvents or decomposition products. These problems lead to limitations such as poor batch stability of the existing process and relatively high safety risks. Summary of the Invention

[0004] In view of the above-mentioned defects or deficiencies in the prior art, this application aims to provide a safety regulation method and system for potassium tert-butoxide production based on dynamic parameter feedback to improve the stability and product consistency of potassium tert-butoxide production.

[0005] In the first aspect, this application proposes a safety regulation method for potassium tert-butoxide production based on dynamic parameter feedback, including the following steps:

[0006] Real-time monitor the axial temperature field distribution and the first concentration gradient of decomposition products in the evaporation and concentration section, and obtain the temperature distribution variation coefficient according to the axial temperature field distribution;

[0007] If the temperature distribution variation coefficient is greater than the first preset threshold or the first concentration gradient is greater than the second preset threshold, then compensate inert gas to the evaporation and concentration section and / or reduce the end evaporation temperature of the evaporation and concentration section;

[0008] Obtain the target concentration duration, and after performing the target concentration duration of compensating for inert gas and / or reducing the terminal evaporation temperature, determine whether the actual intermediate product concentration reaches the target product concentration;

[0009] If so, keep the preset drying parameters in the vacuum drying section unchanged, and perform vacuum drying on the intermediate product to obtain potassium tert-butoxide.

[0010] According to the technical solution provided by the present application, compensating for inert gas to the evaporation concentration section includes the following steps:

[0011] Compensate for the inert gas with the first compensation amount at multiple points to the evaporation concentration section, and monitor the distribution uniformity of the inert gas in real time;

[0012] If the distribution uniformity is less than the third preset threshold, determine the non-uniform distribution area, and then obtain the target points corresponding to the non-uniform distribution area;

[0013] Based on the distribution uniformity, correct the first compensation amount to obtain the second compensation amount;

[0014] Adjust the compensation amount of the inert gas compensated to the evaporation concentration section at the target points to the second compensation amount.

[0015] According to the technical solution provided by the present application, reducing the terminal evaporation temperature of the evaporation concentration section includes the following steps:

[0016] Reduce the terminal evaporation temperature of the evaporation concentration section in a linear temperature reduction mode, and compare the real-time terminal temperature with the dynamic lower limit value in real time; the dynamic lower limit value is dynamically calculated from the supersaturation curve of the current concentrated solution;

[0017] If the absolute value of the difference between the real-time terminal temperature and the dynamic lower limit value is less than the fourth preset threshold, switch the linear temperature reduction mode to a stepped temperature reduction mode.

[0018] According to the technical solution provided by the present application, the stepped temperature reduction mode is a temperature reduction mode in which the temperature drop amplitude between every two adjacent temperature reduction steps is lower than the fifth preset threshold and a constant temperature holding period of the first preset duration is set between adjacent temperature reduction steps.

[0019] According to the technical solution provided by the present application, when performing the stepped temperature reduction mode, it includes the following steps:

[0020] During the constant temperature holding period, the crystallization phase transition characteristic peak intensity of the concentrated solution is detected in real time;

[0021] If the crystallization phase transition characteristic peak intensity exceeds the first safety threshold, terminate the temperature reduction process.

[0022] After terminating the cooling process according to the technical solution provided by the present application, the following steps are further included:

[0023] Start ultrasonic stirring and raise the terminal evaporation temperature at the first temperature recovery rate until the intensity of the crystallization characteristic peak drops below the first safety threshold.

[0024] Before reducing the terminal evaporation temperature of the evaporation concentration section after compensating the evaporation concentration section with inert gas according to the technical solution provided by the present application, the following steps are included:

[0025] Real-time monitor the axial pressure difference of each pipe section. If there is a pipe section with the axial pressure difference greater than the sixth preset threshold, determine this pipe section as the target pipe section;

[0026] Obtain the circumferential multi-point ultrasonic signal data of the target pipe section, and judge whether there is deposition of microcrystalline potassium tert-butoxide in the target pipe section according to the multi-point ultrasonic signal data;

[0027] Reducing the terminal evaporation temperature of the evaporation concentration section includes the following steps:

[0028] If not, reduce the terminal evaporation temperature of the evaporation concentration section.

[0029] Reducing the terminal evaporation temperature of the evaporation concentration section according to the technical solution provided by the present application includes the following steps and further includes the following steps:

[0030] If so, reduce the current flow rate of the concentrated solution to the first flow rate, and the first flow rate is less than half of the current flow rate;

[0031] Gradually increase the flow rate of the concentrated solution in multiple steps. The increase amplitude of the flow rate between every two adjacent steps does not exceed 25%, and control the temperature of the outer wall of the target pipe section during the stage when the flow rate remains unchanged;

[0032] If the deposition amount of microcrystalline potassium tert-butoxide in the target pipe section is less than the second safety threshold within the second preset time period, then reduce the terminal evaporation temperature of the evaporation concentration section.

[0033] Controlling the temperature of the outer wall of the target pipe section according to the technical solution provided by the present application includes the following steps:

[0034] Adjust the thermal radiation power distribution of the outer wall of the target pipe section to form alternating supercooled zones and dissolution zones axially in the target pipe section to eliminate the deposited microcrystalline potassium tert-butoxide in the target pipe section; the supercooled zone is the area where the temperature is lower than the dynamic lower limit value, and the dissolution zone is the area where the temperature is higher than the dynamic lower limit value.

[0035] Second aspect, the present application proposes a potassium tert-butoxide production safety regulation system based on dynamic parameter feedback, which is used to implement the potassium tert-butoxide production safety regulation method based on dynamic parameter feedback as described above; it includes:

[0036] A monitoring module, which is configured to monitor the axial temperature field distribution in the evaporation and concentration section and the first concentration gradient of the decomposition products in real time, and obtain the temperature distribution variation coefficient according to the axial temperature field distribution;

[0037] A control module, which is configured to, if the temperature distribution variation coefficient is greater than the first preset threshold or the first concentration gradient is greater than the second preset threshold, compensate the evaporation and concentration section with inert gas and / or reduce the terminal evaporation temperature of the evaporation and concentration section;

[0038] A judgment module, which is configured to obtain the target concentration duration, and judge whether the actual intermediate product concentration reaches the target product concentration after the target concentration duration of compensating inert gas and / or reducing the terminal evaporation temperature;

[0039] The judgment module is also configured to, when the actual intermediate product concentration reaches the target product concentration, keep the preset drying parameters in the vacuum drying section unchanged and perform vacuum drying on the intermediate product to obtain potassium tert-butoxide.

[0040] Compared with the prior art, the beneficial effects of the present application are as follows: By monitoring the axial temperature field distribution and the decomposition product concentration gradient in the evaporation and concentration section in real time, calculating the temperature distribution variation coefficient, and dynamically judging the local overheating risk, when the variation coefficient or the concentration gradient exceeds the standard, compensating inert gas can inhibit the chain propagation of the decomposition reaction (and also reduce the explosion risk by reducing the oxygen content and improve safety), and at the same time reduce the terminal evaporation temperature to avoid supersaturated crystallization, so as to control the by-product concentration within the safety threshold. Compared with the traditional fixed parameter regulation, this technology uses the temperature field variation coefficient as a quantitative index, significantly improving the regulation accuracy. In addition, verifying the intermediate product concentration after inert gas compensation and temperature reduction regulation ensures that the materials entering the vacuum drying stage meet the purity requirements. This mechanism avoids the problems of premature or late drying in the traditional process. Combined with the maintenance of the vacuum drying section parameters, it can further improve the product consistency. Description of the Drawings

[0041] Figure 1 It is a step flow chart of the potassium tert-butoxide production safety regulation system based on dynamic parameter feedback provided by the present application. Detailed Embodiments

[0042] The present application will be further described in detail below with reference to the accompanying drawings and embodiments. It can be understood that the specific embodiments described herein are only used to explain the related invention, rather than limiting the invention. Additionally, it should be noted that for the convenience of description, only the parts related to the invention are shown in the drawings.

[0043] It should be noted that, without conflict, the embodiments in the present application and the features in the embodiments can be combined with each other. The present application will be described in detail below with reference to the drawings and embodiments.

[0044] Example 1

[0045] The production process of potassium tert - butoxide is as follows: First, a chemical reaction between metallic potassium and tert - butanol occurs in a reaction kettle to generate a reaction solution. The reaction solution is transported to the evaporation and concentration section, where the reaction solution is heated by a heating device to gradually evaporate low - boiling - point substances such as tert - butanol, thereby increasing the concentration of potassium tert - butoxide to form a concentrated solution. After evaporation and concentration, the concentrated solution enters subsequent separation, purification, and other process steps to further remove impurities and improve the purity of potassium tert - butoxide. Finally, through the drying treatment in the vacuum drying section, a high - purity potassium tert - butoxide product is obtained, which can be used in downstream industries such as organic synthesis and drug preparation. As mentioned in the background technology, in response to the problems in the prior art, the present application proposes a safety control method for potassium tert - butoxide production based on dynamic parameter feedback, as Figure 1 shown, including the following steps:

[0046] S1. Real - time monitor the axial temperature field distribution in the evaporation and concentration section and the first concentration gradient of the decomposition products, and obtain the temperature distribution variation coefficient according to the axial temperature field distribution;

[0047] Specifically, the axial temperature field distribution in this step is the temperature distribution along the axial direction of the equipment (such as pipelines, etc.) in the evaporation and concentration section; the first concentration gradient refers to the concentration change rate of the decomposition products in the space of the evaporation and concentration section. The temperature distribution variation coefficient is a statistic that measures the dispersion degree of the axial temperature field distribution. It is obtained by calculating the ratio of the standard deviation to the average value of the temperature data and is used to quantify the non - uniformity of the temperature distribution.

[0048] Specifically, organize and statistically analyze the axial temperature data collected by temperature sensors, calculate the average value and standard deviation of the temperature data, and then take the quotient of the standard deviation and the average value as the temperature distribution variation coefficient. For example, the axial temperature data collected at a certain moment is [50, 52, 48, 55, 49]. By calculation, the average value is 50.8 and the standard deviation is 2.77, so the temperature distribution variation coefficient is approximately 0.055.

[0049] S2. If the coefficient of variation of the temperature distribution is greater than the first preset threshold or the first concentration gradient is greater than the second preset threshold, inert gas is compensated to the evaporation concentration section, and / or the terminal evaporation temperature of the evaporation concentration section is reduced;

[0050] Exemplarily, the first preset threshold is 0.15, and the second preset threshold is 1.2 times the hourly change rate of the decomposition product concentration during normal production.

[0051] Specifically, the coefficient of variation of the temperature distribution reflects the degree of dispersion of the axial temperature field distribution in the evaporation concentration section. If it is greater than the first preset threshold, it means that the axial temperature field distribution is uneven, and there may be local overheating or overcooling areas. Local overheating may lead to an intensified decomposition reaction, increasing the decomposition products, and may also trigger side reactions, affecting the purity and quality of potassium tert-butoxide; local overcooling may cause inconsistent reaction rates, reducing production efficiency, and may even lead to abnormal crystallization of the concentrated solution, clogging the pipeline. When the first concentration gradient is greater than the second preset threshold, it indicates that the concentration change of the decomposition product is too drastic. This implies that the decomposition reaction proceeds rapidly in a short time, which may be due to out-of-control reaction conditions, such as abnormal temperature and pressure, or there are some unstable factors in the reaction system. This will not only increase the content of the decomposition product, but may also cause corrosion or damage to the production equipment, seriously threatening production safety. Therefore, once the above situation occurs, it is necessary to promptly take measures to compensate inert gas to the evaporation concentration section and / or reduce the terminal evaporation temperature to stabilize the production process and ensure product quality and production safety.

[0052] Further, the compensation of inert gas to the evaporation concentration section includes the following steps:

[0053] Compensate the evaporation concentration section with a first compensation amount of inert gas at multiple points, and monitor the distribution uniformity of the inert gas in real time;

[0054] If the distribution uniformity is less than the third preset threshold, determine the non-uniform distribution area, and then obtain the target points corresponding to the non-uniform distribution area;

[0055] Based on the distribution uniformity, correct the first compensation amount to obtain a second compensation amount;

[0056] Adjust the compensation amount of the inert gas compensated to the evaporation concentration section at the target points to the second compensation amount.

[0057] Specifically, gas injection ports are provided at multiple positions such as the top, middle, and bottom of the evaporation and concentration section, and an inert gas (such as nitrogen) with a first compensation amount (such as set at 5 liters per cubic meter according to the equipment volume and safety requirements, for example) is compensated therein. By arranging multiple gas concentration sensors in the section, the distribution uniformity of the inert gas is monitored in real time. If the distribution uniformity is less than the third preset threshold (such as 0.8), the non-uniform distribution area is determined by analyzing the data of each sensor, and then the corresponding target points are located. Based on the distribution uniformity, the first compensation amount is corrected by the proportional correction method. For example, when the distribution uniformity is 0.6, the second compensation amount is adjusted to 1.5 times the first compensation amount (for example), and the compensation amount at the target points is adjusted to the second compensation amount.

[0058] This embodiment gives an optimized method for compensating inert gas during anomalies. Compensating inert gas at multiple points can quickly dilute the decomposition products, reduce their concentration, and reduce the possibility of danger caused by excessive decomposition product concentration. At the same time, monitoring the distribution uniformity and correcting the compensation amount ensure that the inert gas is evenly distributed in the evaporation and concentration section, avoiding potential safety hazards in local areas due to lack of inert gas protection, and comprehensively ensuring production safety. At the same time, a stable reaction environment is the key to ensuring product quality. When there are anomalies in temperature distribution or concentration, compensating inert gas in a timely manner and optimizing its distribution can stabilize the reaction conditions, prevent side reactions caused by local overheating, overcooling, or excessive decomposition product concentration, and then avoid an increase in impurities in the product, ensuring the purity and quality stability of potassium tert-butoxide, and improving the consistency between product batches. Therefore, this inert gas compensation strategy can quickly return the reaction to the normal state, reduce the production interruption or adjustment time caused by anomalies. It avoids repeatedly adjusting process parameters due to production anomalies, enables the evaporation and concentration section to operate more efficiently, shortens the production cycle, and improves the production efficiency of potassium tert-butoxide.

[0059] Further, reducing the terminal evaporation temperature of the evaporation and concentration section includes the following steps:

[0060] Reduce the terminal evaporation temperature of the evaporation and concentration section in a linear cooling mode, and compare the real-time terminal temperature with the dynamic lower limit value in real time; the dynamic lower limit value is dynamically calculated from the supersaturation curve of the current concentrated solution;

[0061] Specifically, the terminal evaporation temperature refers to the temperature at the position where the evaporation and concentration section is about to end. The temperature here directly determines the state of the final concentrated liquid. Reducing the temperature at this position can directly affect the evaporation degree of the concentrated liquid and the final concentration of the product, effectively control the concentration process, avoid excessive evaporation or insufficient concentration, ensure that the product quality meets the requirements, and also conforms to the continuity of the production process. First, it is necessary to experimentally determine the supersaturation data of the concentrated liquid at different temperatures and concentrations. During the experiment, the temperature is precisely controlled, the concentration of the concentrated liquid is gradually changed, and the temperature-concentration correspondence relationship when the concentrated liquid begins to show supersaturation is recorded. Based on these experimental data, a mathematical model of the supersaturation curve of the current concentrated liquid is constructed using a mathematical fitting method such as the least squares method. In actual production, the current concentration of the concentrated liquid is obtained in real time and substituted into the supersaturation curve mathematical model to calculate the corresponding dynamic lower limit value. A temperature controller is used to set a linear cooling mode, such as a 1°C reduction per minute.

[0062] If the absolute value of the difference between the real-time terminal temperature and the dynamic lower limit value is less than the fourth preset threshold, the linear cooling mode is switched to a stepped cooling mode.

[0063] Specifically, if the absolute value of the difference between the real-time terminal temperature and the dynamic lower limit value is less than the fourth preset threshold (such as 0.5°C), it is switched to the stepped cooling mode through the controller.

[0064] Furthermore, the stepped cooling mode is a cooling mode in which the temperature drop amplitude between every two adjacent cooling steps is lower than the fifth preset threshold and a first preset time period of constant temperature holding is set between adjacent cooling steps.

[0065] Specifically, it is set that the temperature drop amplitude between every two adjacent cooling steps is lower than the fifth preset threshold (such as 0.3°C), and a first preset time period (such as 10 minutes) of constant temperature holding is set between adjacent cooling steps. The temperature controller performs stepped cooling according to the set program.

[0066] The cooling mode proposed in this embodiment can improve production safety. By comparing the real-time terminal temperature with the dynamic lower limit value dynamically calculated from the supersaturation curve of the concentrated solution in real time, it can effectively avoid too low temperature. When the temperature is lower than the dynamic lower limit value, the concentrated solution may crystallize excessively, resulting in pipeline blockage, affecting the continuity of production and even causing safety accidents. Through this precise temperature control, the cooling strategy can be adjusted in time to prevent such dangerous situations. The stepwise cooling mode avoids sharp temperature changes and prevents violent boiling or decomposition reaction intensification of the concentrated solution caused by sudden temperature changes, thus ensuring the safety and stability of the production process. The combination of linear cooling and stepwise cooling enables the concentrated solution to crystallize slowly under suitable temperature conditions. During the constant temperature holding period of stepwise cooling, the concentrated solution has enough time to crystallize orderly, avoiding insufficient crystallization or irregular crystal morphology caused by too fast temperature change, thereby improving the crystal quality of potassium tert-butoxide and ensuring the purity and consistency of the product. A reasonable cooling strategy helps to maintain a stable reaction environment and reduce side reactions caused by abnormal temperature. During the evaporation and concentration process, too high or fluctuating temperature may cause the decomposition of potassium tert-butoxide or side reactions with other impurities, affecting the product quality. By strictly controlling the cooling process, the probability of side reactions can be effectively reduced, and the quality and yield of the product can be improved. Through precise temperature control and reasonable switching of the cooling mode, the evaporation and concentration section can reach the target concentration state in the shortest time. Avoiding the extension of the production cycle caused by improper temperature control improves the utilization rate of equipment and thus enhances the overall production efficiency.

[0067] S3. Obtain the target concentration duration, and after executing the target concentration duration of compensating for inert gas and / or reducing the terminal evaporation temperature, determine whether the actual intermediate product concentration reaches the target product concentration;

[0068] Specifically, the target concentration duration refers to the difference between the preset concentration duration and the historical concentration period before starting to execute compensating for inert gas and / or reducing the terminal evaporation temperature, that is, the normal remaining concentration duration. The preset concentration duration is determined before production according to product requirements. For the continuity of production, how long to react, evaporate, dry, etc. are determined in advance. The preset concentration duration can be calculated based on past experience, production process standards or theoretical models, and is an estimated duration from the input of raw materials to the intermediate product reaching the target concentration.

[0069] S4. If so, keep the preset drying parameters of the vacuum drying section unchanged and perform vacuum drying on the intermediate product to obtain potassium tert-butoxide.

[0070] Specifically, the operator can clearly grasp the production progress. By clarifying the remaining normal concentration time, production can be carried out in an orderly manner according to the established plan, avoiding blind waiting or over-concentration. For example, after detecting that the parameter to be regulated is abnormal, the operation can be quickly adjusted according to the target concentration time, and the subsequent process can be reasonably arranged, greatly improving the controllability and planning of the production process. Judging whether the actual intermediate product concentration meets the standard after the target concentration time ensures the stable quality of the intermediate product entering the vacuum drying stage. Only when the intermediate product reaches the appropriate concentration, the subsequent drying process is carried out, avoiding product quality fluctuations caused by concentration deviations. If the concentration is too high or too low, it may affect the purity and crystal form of the final potassium tert-butoxide, and the judgment link in S3 effectively avoids such problems. Then, the concentration of the intermediate product before entering the vacuum drying section meets the standard, and the preset drying parameters in S4 are kept unchanged, ensuring that the conditions for each batch of potassium tert-butoxide are the same during the drying process, jointly achieving the effect of improving the product quality consistency and avoiding differences in indicators such as product water content and crystallinity caused by fluctuations in drying parameters.

[0071] In a preferred embodiment, when implementing the stepwise cooling mode, the following steps are included:

[0072] During the constant temperature holding period, the intensity of the crystallization phase transition characteristic peak of the concentrated solution is detected in real time;

[0073] If the intensity of the crystallization phase transition characteristic peak exceeds the first safety threshold, the cooling process is terminated.

[0074] Further, after the cooling process is terminated, the following steps are also included:

[0075] Start ultrasonic stirring and raise the terminal evaporation temperature at the first temperature rise rate until the intensity of the crystallization characteristic peak drops below the first safety threshold.

[0076] Specifically, during the crystallization process of the concentrated solution, the crystal structure of the substance changes. Different crystal structures will produce characteristic diffraction peaks under specific detection means (such as X-ray diffraction analysis), and the intensity of these diffraction peaks is the intensity of the crystallization phase change characteristic peak. It reflects the crystal growth situation and crystallization degree in the concentrated solution. The acquisition method is as follows: during the constant temperature holding period, align the probe of the X-ray diffractometer with the concentrated solution sample, set an appropriate scanning range and time, and the corresponding characteristic peak intensity value can be obtained. The first safety threshold is a preset critical value used to judge whether the intensity of the crystallization phase change characteristic peak is within the safe range. It is determined based on a large amount of experimental data and production experience. When the intensity of the crystallization phase change characteristic peak exceeds this threshold, it may have an adverse impact on product quality or the production process. The acquisition method is as follows: through a large number of previous experiments, record the product quality and production situation under different intensities of the crystallization phase change characteristic peak, and comprehensively analyze to determine an appropriate value as the first safety threshold. For example, through multiple experiments, it is found that when the intensity of the crystallization phase change characteristic peak exceeds 80 (the unit is determined according to the actual detection means), the purity and crystal form of the product show obvious abnormalities, then 80 can be used as the first safety threshold. The first temperature rise rate refers to the speed at which the terminal evaporation temperature rises after the cooling process is terminated. It determines the speed of temperature rise and has an important impact on adjusting the crystallization state of the concentrated solution. The acquisition method is as follows: it is determined according to the characteristics of the concentrated solution, the heating capacity of the equipment, and the requirements of the production process. For example, for a specific concentrated solution, after experiments and process evaluations, it is determined that when the product quality can be guaranteed and the crystallization state can be adjusted efficiently, the terminal evaporation temperature rises by 0.2 °C per minute, then 0.2 °C / minute is the first temperature rise rate.

[0077] The stepwise cooling mode proposed in this embodiment avoids crystal structure defects and impurity mixing caused by excessive crystallization, ensuring the quality and purity of potassium tert-butoxide crystals. After the cooling is terminated, the crystal structure is further optimized to improve the stability and consistency of product quality, solving the problem of product quality fluctuations caused by improper temperature control in the prior art. During the crystallization process, excessive crystallization may lead to safety hazards such as changes in internal pressure of the equipment and pipeline blockage. By monitoring the intensity of the crystallization phase change characteristic peak, the cooling is terminated in a timely manner and a temperature rise measure is taken, effectively avoiding these potential safety problems, enhancing the safety of the production process, and making up for the deficiency of the prior art in the lack of regulation means in the face of abnormal crystallization. Timely termination of cooling, ultrasonic stirring, and temperature rise operations enable the crystallization process to proceed in the best state, reducing the situation of production interruption and product unqualifiedness caused by crystallization problems and the need for reprocessing, improving production efficiency, increasing product yield, and realizing the efficient operation of the production process.

[0078] In a preferred embodiment, after compensating the evaporation concentration section with inert gas and before reducing the terminal evaporation temperature of the evaporation concentration section, the following steps are included:

[0079] Monitor the axial pressure difference of each pipe section in real time. If there is a pipe section with the axial pressure difference greater than the sixth preset threshold, determine this pipe section as the target pipe section;

[0080] Specifically, in the evaporation concentration section of potassium tert-butoxide production, there are various pipes for transporting fluids such as concentrated liquid and steam. These pipes are divided into different parts according to functions, positions or process requirements, and each part is a pipe section. For example, the feed pipe connecting the reaction kettle to the evaporator can be regarded as a pipe section, the pipes at different levels or in different directions inside the evaporator also form independent pipe sections respectively, and the discharge pipe from the evaporator to the subsequent separation equipment is also one of the pipe sections. The axial pressure difference refers to the pressure difference between two different positions on the axis of the same pipe section. The sixth preset threshold is obtained by collecting the axial pressure difference data of each pipe section in past production, calculating its average value and standard deviation, and adding a certain multiple (such as 2 times the standard deviation) of the standard deviation to the average value, such as 0.05 MPa. If the axial pressure difference of a certain pipe section is greater than the sixth preset threshold, it is the target pipe section that may have a deposition problem, and it is necessary to further judge whether there is a deposition situation.

[0081] Obtain the circumferential multi-point ultrasonic signal data of the target pipe section, and judge whether there is deposition of microcrystalline potassium tert-butoxide in the target pipe section according to the multi-point ultrasonic signal data;

[0082] Optionally, an ultrasonic signal method is selected to further judge whether there is a deposition situation. Specifically, by analyzing parameters such as the intensity, phase and propagation time of the reflected ultrasonic signal, it is possible to judge whether there is a deposition, the position of the deposition and the approximate thickness. Therefore, this step also includes obtaining the position and thickness of the deposition according to the multi-point ultrasonic signal data;

[0083] The reduction of the terminal evaporation temperature of the evaporation concentration section includes the following steps:

[0084] If not, reduce the terminal evaporation temperature of the evaporation concentration section.

[0085] Specifically, if there is deposition of microcrystalline potassium tert-butoxide, as the temperature decreases, the deposition may intensify, leading to pipeline blockage, abnormal local pressure, increasing the risk of equipment damage, and shortening the service life of the equipment. Judging no deposition first and then reducing the temperature can avoid equipment problems caused by deposition, ensure stable operation of the equipment, reduce maintenance costs and downtime, and guarantee production continuity. When there is deposition and the temperature is reduced, the deposition will interfere with the flow and heat transfer uniformity of the concentrated solution, causing abnormal local concentration and temperature, affecting the crystallization process of potassium tert-butoxide, and resulting in a decrease in product purity and irregular crystal morphology. Judging no deposition first and then reducing the temperature can provide a stable environment for crystallization, ensuring stable product quality, high purity, and good crystal morphology. For example, when producing high-purity potassium tert-butoxide for pharmaceutical synthesis, a stable crystallization environment is crucial.

[0086] Further, reducing the terminal evaporation temperature of the evaporation and concentration section includes the following steps:

[0087] If so, reduce the current flow rate of the concentrated solution to a first flow rate, and the first flow rate is less than half of the current flow rate;

[0088] Specifically, the first flow rate refers to a specific flow rate to which the current flow rate of the concentrated solution needs to be reduced when microcrystalline potassium tert-butoxide deposition is detected in the target pipe section. It is to change the flow state of the concentrated solution in the pipe section to reduce further deposition of microcrystalline potassium tert-butoxide and create conditions for subsequent treatment of deposition problems. The acquisition method is: according to the pipe diameter, internal structure of the target pipe section, and the properties of the concentrated solution, it is determined through fluid mechanics calculation or experimental testing. For example, for a target pipe section with a pipe diameter of 50 mm and a current flow rate of 10 L / min, it is determined through calculation or experiment that reducing the flow rate to 4 L / min (less than 5 L / min, that is, half of the current flow rate) is more appropriate, then 4 L / min is the first flow rate. Generally, 30%-40% of the current flow rate is used as the first flow rate.

[0089] Gradually increase the flow rate of the concentrated solution in multiple steps, and the increase amplitude of the flow rate between every two adjacent steps does not exceed 25%, and control the temperature of the outer wall of the target pipe section during the stage when the flow rate remains unchanged;

[0090] If the deposition amount of microcrystalline potassium tert-butoxide in the target pipe section is less than the second safety threshold within the second preset time period, then reduce the terminal evaporation temperature of the evaporation and concentration section.

[0091] Specifically, the second preset duration is a time limit set when dealing with the deposition problem of microcrystalline potassium tert-butoxide in the target pipe section. During this time, by adjusting measures such as flow rate and the temperature of the outer wall of the pipe section, the change in the deposition amount of microcrystalline potassium tert-butoxide is observed. The acquisition method is determined based on production experience and research on the dissolution or removal rate of the deposited substances in the pipe section. For example, after multiple experiments and actual production verification, it is found that it usually takes about 30 minutes to observe obvious effects when dealing with the deposition problem of microcrystalline potassium tert-butoxide, so the second preset duration is set to 30 minutes. The second safety threshold is a critical value used to determine whether the deposition amount of microcrystalline potassium tert-butoxide in the target pipe section is within the safe range. When the deposition amount is less than this threshold, it is considered that the deposition situation in the pipe section will not cause serious impacts on subsequent production, and the operation of reducing the end evaporation temperature can continue. The acquisition method is determined by simulating the operation conditions of the pipe section under different deposition amounts and the impact on product quality, combined with production safety standards. For example, through simulation and experiments, it is found that when the deposition amount of microcrystalline potassium tert-butoxide in the target pipe section is less than 0.5 kg per cubic meter, it will not affect the normal flow of the fluid in the pipe section and product quality, so 0.5 kg / m³ is the second safety threshold.

[0092] Based on the original implementation manner, this implementation manner takes into account the common deposition problem of microcrystalline potassium tert-butoxide in the production scenario. By real-time monitoring of the axial pressure difference of each pipe section, potential pipeline blockages or abnormal conditions can be detected in a timely manner, avoiding production interruptions or even safety accidents caused by pipe section problems. When microcrystalline potassium tert-butoxide deposition is detected, measures such as reducing the flow rate, stepwise increasing the flow rate, and regulating the temperature of the outer wall of the pipe section are taken, effectively reducing the impact of deposition on production, ensuring the safe and stable operation of the production process, and further solving the safety hazards caused by pipeline problems in the prior art. Through the monitoring and treatment of the deposition situation of microcrystalline potassium tert-butoxide in the target pipe section, the normal flow and uniform distribution of the concentrated solution in the pipe section are ensured, avoiding uneven concentration of the concentrated solution caused by deposition, thus ensuring the quality stability of potassium tert-butoxide products, improving product consistency, and making up for the deficiencies in product quality control in the prior art.

[0093] Furthermore, regulating the temperature of the outer wall of the target pipe section includes the following steps:

[0094] Adjust the heat radiation power distribution of the outer wall of the target pipe section to form alternating supercooled zones and dissolution zones axially in the target pipe section, so as to eliminate the deposited microcrystalline potassium tert-butoxide in the target pipe section; the supercooled zone is the area where the temperature is lower than the dynamic lower limit value, and the dissolution zone is the area where the temperature is higher than the dynamic lower limit value.

[0095] Specifically, the thermal radiation power distribution refers to the distribution of the power of heat radiated outward per unit area on the outer wall of the target pipe section in the axial direction. For the target pipe section, by adjusting the power of the outer wall heating element (such as an electric heating wire), its thermal radiation power distribution can be changed. Multiple heat flux sensors are installed on the outer wall of the pipe section. These sensors can measure the heat passing through per unit area per unit time, thereby obtaining the thermal radiation power data at different positions, and further determining the thermal radiation power distribution. For example, a heat flux sensor is installed every certain distance (such as 0.5 meters), data is collected in real time, and a distribution curve of the thermal radiation power along the axial direction of the pipe section is plotted. The outer wall of the target pipe section is axially divided into multiple regions, and each region corresponds to an independent heating element, such as an electric heating wire or a heating sheet. By adjusting the power supply of the heating elements in different regions, differential control of the thermal radiation power is achieved. For example, for the region where a supercooled zone needs to be formed, the power of the heating element is reduced or even turned off; for the dissolution zone, the power of the heating element is increased to form alternating temperature zones.

[0096] Before adjusting the thermal radiation power distribution of the outer wall of the target pipe section to form alternating supercooled zones and dissolution zones axially in the target pipe section, it also includes determining a parameter set, where the parameter set is the setting rules for the supercooled zone and the dissolution zone; determining the parameter set includes the following steps:

[0097] According to the deposition position and thickness obtained from the above ultrasonic signal data, the corresponding setting position and the size of the setting area are obtained;

[0098] According to the size of the setting area, the setting ratio and the number of alternations of the supercooled zone and the dissolution zone are obtained;

[0099] Adjust the thermal radiation power distribution of the outer wall of the target pipe section so as to form a supercooled zone and a dissolution zone with a setting ratio and a number of alternations at the corresponding setting position of the target pipe section.

[0100] Specifically, the number of alternations and the area size are adjusted according to the severity of deposition. For example, in the case of severe deposition, the number of alternations is shortened, so that the supercooled zone and the dissolution zone alternate closely, enhancing the effect of removing deposition; in the case of light deposition, the number of alternations and the area size are appropriately increased; referring to past production experience in dealing with similar deposition problems and experimental data for this concentrate and pipe section conditions. Through multiple experiments, record the deposition removal effects under different arrangements of the supercooled zone and the dissolution zone, establish a database, and provide a reference for actual production. For example, it is found through experiments that under certain concentrate and pipe section conditions, when the length ratio of the supercooled zone to the dissolution zone is 1:2 and the number of alternations is 3, the deposition removal effect is the best, and this parameter setting can be preferentially referred to in actual production.

[0101] The deposition elimination method of alternately forming a supercooled zone and a dissolution zone proposed in this embodiment continuously changes the dissolution and crystallization states of microcrystalline potassium tert-butoxide. The change in the crystal structure in the supercooled zone makes it easier to dissolve when entering the dissolution zone. Repeating this alternation strengthens the deposition elimination effect. Compared with the single temperature zone setting, the alternating zones can process deposits at different positions and degrees in the pipe section more comprehensively and efficiently, improving the efficiency and thoroughness of deposition elimination, thus timely solving the deposition problem and effectively ensuring production continuity and safety.

[0102] Example 2

[0103] Based on Example 1, this example proposes a safety regulation system for the production of potassium tert-butoxide based on dynamic parameter feedback, which is used to implement the safety regulation method for the production of potassium tert-butoxide based on dynamic parameter feedback as described in Example 1; it includes:

[0104] A monitoring module configured to monitor the axial temperature field distribution in the evaporation and concentration section and the first concentration gradient of decomposition products in real time, and obtain the temperature distribution variation coefficient according to the axial temperature field distribution;

[0105] A control module configured to, if the temperature distribution variation coefficient is greater than a first preset threshold or the first concentration gradient is greater than a second preset threshold, compensate inert gas to the evaporation and concentration section and / or reduce the terminal evaporation temperature of the evaporation and concentration section;

[0106] A judgment module configured to obtain the target concentration duration, and after the target concentration duration of compensating inert gas and / or reducing the terminal evaporation temperature is executed, judge whether the actual intermediate product concentration reaches the target product concentration;

[0107] The judgment module is further configured to, when the actual intermediate product concentration reaches the target product concentration, keep the preset drying parameters of the vacuum drying section unchanged and perform vacuum drying on the intermediate product to obtain potassium tert-butoxide.

[0108] Specific examples are used in this article to elaborate on the principles and implementation methods of this application. The descriptions of the above examples are only used to help understand the method and its core idea of this application. The above are only the preferred implementation methods of this application. It should be noted that due to the limited nature of language expression and objectively infinite specific structures, for those of ordinary skill in the art in this technical field, without departing from the principles of the present invention, several improvements, refinements or changes can be made, or the above technical features can be combined in an appropriate manner; these improvements, refinements, changes or combinations, or directly applying the concept and technical solution of the invention to other occasions without improvement, should all be regarded as the protection scope of this application.

Claims

1. A safety control method for the production of potassium tert-butoxide based on dynamic parameter feedback, characterized in that, It includes the following steps: Real-time monitor the axial temperature field distribution in the evaporation and concentration section and the first concentration gradient of the decomposition products, and obtain the temperature distribution coefficient of variation according to the axial temperature field distribution; If the temperature distribution coefficient of variation is greater than the first preset threshold or the first concentration gradient is greater than the second preset threshold, compensate inert gas to the evaporation and concentration section, and / or reduce the terminal evaporation temperature of the evaporation and concentration section; Obtain the target concentration duration, and after the target concentration duration of compensating inert gas and / or reducing the terminal evaporation temperature is executed, judge whether the actual intermediate product concentration reaches the target product concentration; If so, keep the preset drying parameters of the vacuum drying section unchanged, and perform vacuum drying on the intermediate product to obtain potassium tert-butoxide.

2. The safety control method for potassium tert-butoxide production based on dynamic parameter feedback according to claim 1, wherein The compensating inert gas to the evaporation and concentration section includes the following steps: Compensate the inert gas with the first compensation amount to the evaporation and concentration section at multiple positions, and real-time monitor the distribution uniformity of the inert gas; If the distribution uniformity is less than the third preset threshold, determine the non-uniform distribution area, and then obtain the target positions corresponding to the non-uniform distribution area; Based on the distribution uniformity, correct the first compensation amount to obtain the second compensation amount; Adjust the compensation amount of the inert gas compensated to the evaporation and concentration section at the target positions to the second compensation amount.

3. The method for safety regulation and control of potassium tert-butoxide production based on dynamic parameter feedback according to claim 1, characterized in that, The reducing the terminal evaporation temperature of the evaporation and concentration section includes the following steps: Reduce the terminal evaporation temperature of the evaporation and concentration section in a linear cooling mode, and compare the real-time terminal temperature with the dynamic lower limit value in real time; the dynamic lower limit value is dynamically calculated from the supersaturation curve of the current concentrated solution; If the absolute value of the difference between the real-time terminal temperature and the dynamic lower limit value is less than the fourth preset threshold, switch the linear cooling mode to a stepped cooling mode.

4. The method for safety regulation and control of potassium tert-butoxide production based on dynamic parameter feedback according to claim 3, wherein, The stepped cooling mode is a cooling mode in which the temperature drop amplitude between every two adjacent cooling steps is lower than the fifth preset threshold and a first preset duration of constant temperature holding period is set between adjacent cooling steps.

5. The method for safely regulating the production of potassium tert-butoxide based on dynamic parameter feedback according to claim 4, characterized in that, When executing the stepped cooling mode, it includes the following steps: During the constant temperature holding period, the crystallization phase change characteristic peak intensity of the concentrated solution is detected in real time; If the crystallization phase change characteristic peak intensity exceeds the first safety threshold, terminate the cooling process.

6. The safety control method for the production of potassium tert-butoxide based on dynamic parameter feedback according to claim 5, wherein After the termination of the cooling process, it further includes the following steps: Start ultrasonic stirring and raise the terminal evaporation temperature at the first temperature rise rate until the crystallization characteristic peak intensity drops below the first safety threshold.

7. The method for safety control of potassium tert-butoxide production based on dynamic parameter feedback according to claim 1, wherein Before compensating inert gas to the evaporation and concentration section and before reducing the terminal evaporation temperature of the evaporation and concentration section, it includes the following steps: Real-time monitor the axial pressure difference of each pipe section. If there is a pipe section with the axial pressure difference greater than the sixth preset threshold, determine the pipe section as the target pipe section; Obtain the circumferential multi-point ultrasonic signal data of the target pipe section, and judge whether there is deposition of microcrystalline potassium tert-butoxide in the target pipe section according to the multi-point ultrasonic signal data; The reducing the terminal evaporation temperature of the evaporation and concentration section includes the following steps: If not, reduce the terminal evaporation temperature of the evaporation and concentration section.

8. The safety control method for potassium tert-butoxide production based on dynamic parameter feedback according to claim 7, characterized in that, Lowering the terminal evaporation temperature of the evaporation concentration section includes the following steps: If so, reduce the current flow rate of the concentrated liquid to a first flow rate, where the first flow rate is less than half of the current flow rate; Gradually increase the flow rate of the concentrated liquid in multiple steps, with the increase amplitude of the flow rate between every two adjacent steps not exceeding 25%, and regulate the temperature of the outer wall of the target pipe section during the stage when the flow rate remains unchanged; If within a second preset time period, the deposition amount of microcrystalline potassium tert-butoxide in the target pipe section is less than a second safety threshold, then lower the terminal evaporation temperature of the evaporation concentration section.

9. The method for safely regulating the production of potassium tert-butoxide based on dynamic parameter feedback according to claim 8, wherein Regulating the temperature of the outer wall of the target pipe section includes the following steps: Adjust the thermal radiation power distribution of the outer wall of the target pipe section to form alternating supercooled zones and dissolution zones axially in the target pipe section to eliminate the deposited microcrystalline potassium tert-butoxide in the target pipe section; the supercooled zone is the area where the temperature is lower than the dynamic lower limit value, and the dissolution zone is the area where the temperature is higher than the dynamic lower limit value.

10. A production safety control system for potassium tert-butoxide based on dynamic parameter feedback is used to implement the production safety control method for potassium tert-butoxide based on dynamic parameter feedback as described in any one of claims 1-9; characterized in that, Including: A monitoring module configured to monitor the axial temperature field distribution of the evaporation concentration section and the first concentration gradient of the decomposition product in real time, and obtain the temperature distribution variation coefficient according to the axial temperature field distribution; A control module configured to, if the temperature distribution variation coefficient is greater than a first preset threshold or the first concentration gradient is greater than a second preset threshold, compensate inert gas to the evaporation concentration section and / or lower the terminal evaporation temperature of the evaporation concentration section; A judgment module configured to obtain the target concentration duration, and judge whether the actual intermediate product concentration reaches the target product concentration after the target concentration duration of compensating inert gas and / or lowering the terminal evaporation temperature is executed; The judgment module is further configured to, when the actual intermediate product concentration reaches the target product concentration, keep the preset drying parameters of the vacuum drying section unchanged and perform vacuum drying on the intermediate product to obtain potassium tert-butoxide.

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