A pharmaceutical intermediate reaction device with a high-efficiency heat exchange jacket and its reaction control method.

Abstract

This invention relates to the field of automated control in the pharmaceutical and chemical industry, specifically to a pharmaceutical intermediate reaction device and method with a high-efficiency heat exchange jacket; it includes a reaction vessel body, a spiral flow guide jacket, a sensing circulation component, and a controller; the system uses servo motor torque to invert the real-time viscosity of the material and dynamically correct the total heat transfer coefficient, uses flow integral to lock the medium transit time, and aligns the inlet and outlet temperatures in time and space to calculate the instantaneous heat release rate; its core is to generate balanced removed heat power based on the heat release rate, and adopts a graded control strategy that prioritizes adjusting the speed of the circulating pump and the opening of the limit regulating valve; this invention obtains the net stirring torque through friction compensation, accurately reflects the change in boundary layer thermal resistance, and effectively eliminates model parameter deviations.

Description

Technical Field

[0001] This invention relates to the field of pharmaceutical and chemical automation control, specifically to a pharmaceutical intermediate reaction device with a high-efficiency heat exchange jacket and its reaction control method. Background Technology

[0002] In the production of pharmaceutical intermediates, chemical reactions are often accompanied by intense energy exchanges, and the physical properties of materials change significantly as the reaction progresses. Existing reactor temperature control technologies mainly rely on pre-set static thermodynamic models, but in actual production, these technologies have obvious limitations when dealing with complex operating conditions. Existing technologies suffer from severe lag when monitoring reaction heat. Since pharmaceutical intermediate reactions are often accompanied by polymerization or crystallization processes, the viscosity of the material fluctuates dynamically, which directly changes the heat transfer resistance of the inner wall of the reactor. Traditional methods usually assume the heat transfer coefficient to be constant, which cannot capture the fluctuations in heat exchange efficiency caused by changes in the rheological properties of the material in real time, resulting in a deviation between the calculated reaction heat release rate and the actual physical process. Under variable flow conditions, the accuracy of heat conversion is difficult to guarantee; existing control logic often ignores the time difference of the heat exchange medium flowing through the jacket and fails to establish the spatial and temporal correspondence between the medium inlet and outlet temperatures; when the circulating pump adjusts the flow rate, the calculation of the inlet and outlet temperature difference is often a simple subtraction of the fluid energy state at different times and locations. The calculation noise introduced by this measurement time delay makes it difficult for the system to accurately extract the instantaneous heat release rate of the chemical reaction. In addition, the existing equipment's pipeline connection methods and weighing and metering methods are easily interfered with in complex industrial sites; the additional stress generated by rigid pipelines and the lack of real-time monitoring capabilities for the quality of reactants make it impossible for the system to obtain high-confidence real-time heat capacity data, which further limits the accurate determination of the reaction progress and can easily lead to inconsistent reaction levels between batches or misleading phenomena of false isothermal conditions. The information disclosed in the background section is only intended to enhance the understanding of the background of this disclosure, and therefore may include information that does not constitute prior art known to those skilled in the art. Summary of the Invention

[0003] The purpose of this invention is to provide a pharmaceutical intermediate reaction device and method with a high-efficiency heat exchange jacket, so as to solve the problems mentioned in the background art. Specifically, the technical solution of this invention is as follows: A method for controlling the reaction of pharmaceutical intermediates with a high-efficiency heat exchange jacket, comprising: S1. A reactor main body assembly, a high-efficiency heat exchange jacket, a sensing and circulation assembly, and a controller are provided. The reactor main body assembly includes a servo motor, the sensing and circulation assembly includes a circulation pump, and a strain gauge weighing module is provided at the bottom of the inner liner of the reactor main body assembly. The servo motor drives the stirring shaft. The spiral guide plate in the high-efficiency heat exchange jacket divides the cavity between the inner liner and the outer shell into a single spiral flow channel connected end to end. S2. Control the servo motor to stir the material. The controller collects the instantaneous torque value, combines the real-time rotation speed to invert the real-time viscosity of the material, and dynamically corrects the total heat transfer coefficient according to the real-time viscosity and the flow rate of the heat exchange medium. S3. The controller integrates the mass flow data of the sensing and circulation components, locks the transit time of the heat exchange medium through the spiral channel, aligns the medium outlet temperature with the historical inlet temperature in time and space to calculate the change in fluid micro-element enthalpy, and combines the material mass measured by the strain gauge weighing module to calculate the instantaneous heat release rate of the chemical reaction. S4. The controller generates balanced heat removal power based on the instantaneous heat release rate, prioritizes adjusting the speed of the circulating pump, and adjusts the opening of the cold and heat source distribution valve when the limit is reached.

[0004] Preferably, step S2 includes the following prior to: S2.1 Perform no-load friction torque self-learning calibration. When the inner liner is unloaded, control the servo motor to run in the full speed range, record the steady-state torque required to maintain operation at different speeds, and construct and store the correspondence curve between speed and no-load friction torque. In step S2, the controller consults the corresponding relationship curve based on the current real-time rotation speed to obtain the no-load friction torque, and subtracts the no-load friction torque from the instantaneous torque value to obtain the net stirring torque caused by the material viscous resistance, which is used to invert the real-time viscosity.

[0005] Preferably, in step S2, the dynamic correction of the overall heat transfer coefficient specifically includes: The controller calculates the viscosity change of the reactants based on the trend of the net stirring torque. The total heat transfer coefficient used for heat calculation is updated in real time by utilizing the nonlinear negative correlation between the convective heat transfer coefficient on the inner liner side and the material viscosity, as well as the Reynolds number determined by the medium flow velocity on the spiral flow channel side.

[0006] Preferably, in step S3, the spatiotemporal alignment specifically includes: The controller reads the instantaneous flow data measured by the mass flow meter in real time and performs cumulative integration over time. When the cumulative integral value reaches the geometric volume value of the spiral flow channel, the entry time corresponding to the fluid micro-element that flows out of the medium outlet at the current moment is locked. The outlet temperature data at the current moment is selected and paired with the inlet temperature data recorded at the entry moment to calculate the enthalpy change of the fluid element during the transit process.

[0007] Preferably, in step S3, calculating the instantaneous exothermic rate of the chemical reaction specifically includes: The total energy change rate of the control body is calculated as the product of the temperature change slope measured by the temperature probe inside the vessel and the total heat capacity of the material, wherein the total heat capacity of the material is obtained by multiplying the real-time total mass measured by the strain gauge weighing module and the real-time specific heat capacity obtained by looking up a table. Subtract the heat dissipation power from the stirring, which is converted from the servo motor torque data, from the total energy change rate; Furthermore, the physical heat transfer power calculated based on the aforementioned spatiotemporal alignment is added; The remaining residual is determined as the instantaneous exothermic rate of the chemical reaction.

[0008] Preferably, in step S1, the bottom starting end of the spiral flow channel is provided with a medium inlet, and the top end is provided with a medium outlet. Both the medium inlet and the medium outlet are connected to external pipelines through metal corrugated hoses to isolate the interference of pipeline stress on the strain weighing module.

[0009] Preferably, in step S4, the priority adjustment specifically adopts a segmented priority control strategy: The controller prioritizes adjusting the rotational speed of the circulating pump to change the medium flow rate and heat transfer coefficient. During the adjustment process, when the speed of the circulating pump reaches the preset upper limit threshold or the flow channel pressure limit threshold and still cannot meet the cooling requirements, the controller locks the current speed and instead adjusts the opening of the electric three-way proportional regulating valve, which serves as the cold and heat source distribution valve, to change the mixing ratio of the cold and hot media entering the spiral flow channel.

[0010] Preferably, step S4 is followed by: S5. Execution trajectory tracking and endpoint determination: The controller continuously records the change curve of the instantaneous heat release rate over time. When the instantaneous heat release rate returns to the baseline and remains stable, the reaction is determined to have reached the endpoint.

[0011] A pharmaceutical intermediate reaction device with a high-efficiency heat exchange jacket, comprising: The main components of the reactor include an inner liner, a stirring shaft, and a servo motor. The bottom of the inner liner is supported on a strain gauge weighing module. A high-efficiency heat exchange jacket includes an outer shell covering the outside of the inner liner and a spiral guide plate, the spiral guide plate defining a spiral flow channel with a fixed physical path length; Sensing and circulation components, including inlet temperature transmitter, outlet temperature transmitter, mass flow meter, circulating pump, medium pressure transmitter and hot / cold source distribution valve; And the controller; The controller is electrically connected to the main reactor assembly and the sensing and circulation assembly, respectively.

[0012] Preferably, the inner edge of the spiral guide plate is fully welded to the outer wall of the inner liner, and the outer shell is tightly wrapped around the outer edge of the spiral guide plate using a segmented splicing process or a heat-shrinking process.

[0013] Compared with the prior art, the present invention has the following improvements and advantages: 1. This solution obtains a pure net stirring torque by compensating for the no-load friction torque of the servo motor, thereby accurately calculating the material viscosity. Combined with the nonlinear negative correlation between the convective heat transfer coefficient and viscosity on the inner side of the liner, the dynamic correction of the total heat transfer coefficient can truly reflect the change in boundary layer thermal resistance, eliminating the control deviation caused by inaccurate model parameters. 2. This scheme utilizes the characteristic that the volume of the spiral flow channel is a geometric constant, and accurately locates the pairing moment of the medium inlet and outlet temperatures through flow integral, ensuring the physical authenticity of the enthalpy change calculation and providing high-precision input data for the calculation of instantaneous heat release rate; 3. This scheme adopts a split-range priority control strategy, which prioritizes adjusting the heat exchange efficiency by changing the degree of turbulence by adjusting the speed of the circulating pump. This method uses fluid dynamics to balance the heat power, reduces the frequent opening and closing of the cold and heat source distribution valve, effectively reduces energy consumption and avoids severe system oscillation. 4. This solution determines the endpoint based on the logic of the instantaneous heat release rate returning to the baseline, which essentially reflects the reaction process from the energy dimension. It effectively avoids misjudgment caused by heat transfer lag or environmental interference in traditional methods, and ensures a high degree of consistency in product batch quality. 5. This solution achieves mechanical decoupling by installing corrugated metal hoses at the medium inlet and outlet, thus blocking the interference of external pipeline stress on the strain gauge weighing module, ensuring the accuracy of real-time total mass data, and laying a solid physical foundation for heat capacity calculation and heat release rate calculation. Attached Figure Description

[0014] The present invention will be further explained below with reference to the accompanying drawings and embodiments: Figure 1 This is a schematic diagram of the overall connection structure of the device; Figure 2 This is a structural schematic diagram of the main components of the reactor and the stirring shaft; Figure 3 This is a schematic diagram of the spiral flow channel; Figure 4 This is a flowchart of the method of the present invention.

[0015] In the diagram: 100, main reactor assembly; 110, inner liner; 120, stirring shaft; 130, servo motor; 140, internal temperature probe; 200, high-efficiency heat exchange jacket; 210, outer shell; 220, spiral guide plate; 230, spiral flow channel; 240, medium inlet; 250, medium outlet; 300, sensing and circulation assembly; 310, inlet temperature transmitter; 320, outlet temperature transmitter; 330, mass flow meter; 340, circulating pump; 350, medium pressure transmitter; 400, controller. Detailed Implementation

[0016] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to specific embodiments. Example 1:

[0017] Please see Figures 1-4 This invention provides a method for controlling the reaction of pharmaceutical intermediates with a high-efficiency heat exchange jacket 200, comprising: S1. A reactor main assembly 100, a high-efficiency heat exchange jacket 200, a sensing and circulation assembly 300, and a controller 400 are provided. The reactor main assembly 100 includes a servo motor 130, and the sensing and circulation assembly 300 includes a circulation pump 340. A strain gauge weighing module is provided at the bottom of the inner liner 110 of the reactor main assembly 100. The servo motor 130 drives the stirring shaft 120. The spiral guide plate 220 in the high-efficiency heat exchange jacket 200 divides the cavity between the inner liner 110 and the outer shell 210 into a single spiral flow channel 230 connected end to end. S2. Control the servo motor 130 to stir the material, and the controller 400 collects the instantaneous torque value, combines the real-time speed to invert the real-time viscosity of the material, and dynamically corrects the total heat transfer coefficient according to the real-time viscosity and the flow rate of the heat exchange medium. S3, the controller 400 integrates the mass flow data of the sensing and circulation components 300, locks the transit time of the heat exchange medium through the spiral channel 230, aligns the temperature of the medium outlet 250 with the historical inlet temperature in time and space to calculate the change of fluid micro-element enthalpy, and combines the material mass measured by the strain gauge weighing module to calculate the instantaneous heat release rate of the chemical reaction. S4, Controller 400 generates balanced heat removal power based on the instantaneous heat release rate, prioritizes adjusting the speed of the circulating pump 340, and adjusts the opening of the cold and heat source distribution valve when the limit is reached.

[0018] In this embodiment, a pharmaceutical intermediate reaction control method with a high-efficiency heat exchange jacket 200 addresses the problems of lag in reaction heat calculation and inaccurate model parameters in existing technologies. Existing technologies typically assume a constant heat transfer coefficient and ignore the time difference in medium flow through the jacket under varying flow conditions, leading to errors in the calculation of the reaction heat release rate. This control method constructs a physical foundation including a reaction vessel main assembly 100, a high-efficiency heat exchange jacket 200, a sensing and circulation assembly 300, and a controller 400. The controller 400 can be a Siemens S7-1500 series PLC or an industrial controller with equivalent processing capabilities. The controller 400 is used to execute the core algorithm. The strain gauge weighing module is arranged at the bottom of the inner tank 110. At the same time, the inner tank 110 extends into the inner tank temperature probe 140 to obtain the deep temperature data of the reactants in real time. It monitors the gravity change of the materials in the tank in real time, providing an accurate mass data basis for subsequent heat capacity calculation. The high-efficiency heat exchange jacket 200 uses the spiral guide plate 220 to construct a forced spiral flow channel 230. This flow channel forces the fluid to flow in an orderly manner, eliminating short circuits and dead zones, so that the physical path length of the fluid flowing through the jacket is uniquely determined, providing a physical premise for subsequent fluid micro-element tracking. During the reaction process, a pharmaceutical intermediate reaction control method with a high-efficiency heat exchange jacket 200 analyzes the load of the servo motor 130 in real time through the controller 400. Since pharmaceutical intermediate reactions are often accompanied by polymerization or crystallization, which leads to changes in material viscosity and thus affects the inner wall thermal resistance, this method uses torque data to back-calculate the viscosity and combines the medium flow rate to dynamically correct the total heat transfer coefficient, ensuring that the real-time parameters of the thermodynamic model are consistent with the physical reality. To eliminate calculation errors caused by measurement time delay, a pharmaceutical intermediate reaction control method with a high-efficiency heat exchange jacket 200 implements a spatiotemporal alignment strategy. The controller 400 does not rely solely on time delay, but instead performs integral calculations on the mass flow rate data. Since the volume of the spiral channel 230 is a fixed physical constant, when the integral flow rate equals this volume, it can accurately pinpoint the inlet temperature at which historical moment the current medium outlet 250 temperature corresponds. Through this fluid micro-element tracking based on flow integral, the calculated enthalpy change truly reflects the energy exchange of a single fluid micro-element during the transit process. Combined with the real-time mass data provided by the strain gauge weighing module, the system extracts the instantaneous exothermic rate of the chemical reaction through the principle of energy conservation. Based on the accurately calculated heat release rate, a pharmaceutical intermediate reaction control method with a high-efficiency heat exchange jacket 200 performs feedforward control. The controller 400 calculates the balance heat power required to maintain the temperature and converts it into execution instructions. In order to save energy and improve the response speed, the system prioritizes adjusting the speed of the circulating pump 340 and uses the change in turbulence caused by the change in flow rate to adjust the heat exchange efficiency. Only when the flow rate adjustment cannot meet the demand will the opening of the cold or heat source distribution valve be adjusted to introduce more cold or heat sources. The steps preceding S2 include: S2.1 Perform no-load friction torque self-learning calibration. When the inner liner 110 is in no-load state, control the servo motor 130 to run in the full speed range, record the steady-state torque required to maintain operation at different speeds, and construct and store the corresponding curve of speed and no-load friction torque. In step S2, the controller 400 obtains the no-load friction torque by consulting the corresponding relationship curve based on the current real-time rotation speed, and subtracts the no-load friction torque from the instantaneous torque value to obtain the net stirring torque caused by the material viscosity resistance, which is used to invert the real-time viscosity. In this embodiment, a pharmaceutical intermediate reaction control method with a high-efficiency heat exchange jacket 200 must eliminate the resistance interference of the mechanical system itself in order to obtain the true material rheological characteristics. The total torque output by the servo motor 130 includes the no-load torque to overcome non-material factors such as bearing friction and sealing resistance. Therefore, in the preparation stage before feeding, the system performs no-load friction torque self-learning calibration. The controller 400 drives the servo motor 130 to run in a stepped manner within a preset working speed range. For example, it records data every certain speed from low speed to high speed, or performs continuous frequency sweep operation. During this process, the controller 400 records the steady-state torque corresponding to each speed point, thereby generating a curve table of the correspondence between speed and no-load friction torque and storing it in the internal memory. The specific steps of the process are as follows: the controller 400 controls the stirring shaft 120 to increase its speed in a stepwise manner when there is no material, so as to eliminate the influence of starting inertia; within each stable speed range, the mean value of the current and torque feedback from the motor is extracted using the mean value filtering algorithm, which is used as the friction component at that speed; the discrete speed and torque points are connected into a continuous compensation curve using the spline interpolation method. In the subsequent actual reaction stage, when the controller 400 needs to calculate the material viscosity, it will index the curve table based on the current real-time rotation speed, extract the corresponding no-load friction torque, and subtract the no-load component from the instantaneous torque value fed back by the servo motor 130. The system separates the net stirring torque generated only by the material shear resistance. This processing step ensures the purity of the input variables of the subsequent viscosity inversion algorithm and avoids the interference of mechanical friction fluctuations on the judgment of the chemical reaction state. In step S2, the dynamic correction of the overall heat transfer coefficient specifically includes: The controller 400 calculates the viscosity change of the reactants based on the trend of the change in net stirring torque; The total heat transfer coefficient used for heat calculation is updated in real time by utilizing the nonlinear negative correlation between the convective heat transfer coefficient on the inner liner 110 side and the material viscosity, as well as the Reynolds number on the spiral flow channel 230 side determined by the medium flow rate. In this embodiment, the process of dynamically correcting the total heat transfer coefficient establishes a mapping between rheological parameters and thermodynamic parameters. Since the physical properties of materials in the pharmaceutical intermediate reaction will change significantly with the progress of the reaction, a constant heat transfer coefficient K value will lead to serious deviations in heat calculation. The controller 400 analyzes the time series data of the net stirring torque and calculates the viscosity change of the reactants based on the stirring power criterion equation in fluid mechanics. This calculation process is based on a pre-constructed three-dimensional mapping model of speed-torque-viscosity. During the equipment commissioning phase, at least three standard Newtonian fluids with known viscosities, such as silicone oils of different grades, were used to conduct stirring tests within the reactor at a full speed range, and the different viscosities were recorded. and different speeds The corresponding net stirring torque The controller 400 uses the least squares method to fit these discrete data into a polynomial function. And store; considering the temperature sensitivity of non-Newtonian fluid viscosity, the polynomial function further incorporates real-time temperature. As a correction variable, a mapping model of the following form is constructed: ; in, The number of terms in the fitting polynomial is preset based on the accuracy of the experimental data, and the value range is usually from 2 to 5. These are the fitting coefficients. The activation energy for fluid flow. The gas constant is This is the reference temperature used during calibration. The controller 400 uses this model, combined with real-time temperature data, as a reference. Rotation speed and net stirring torque Accurately output dynamic viscosity; In actual production, the controller 400 only needs to input the real-time collected rotation speed and the calculated net stirring torque to directly calculate the current material viscosity value through this function, without relying on complex fluid mechanics theory formulas. This model essentially characterizes the rheological dynamics of non-Newtonian fluids in a stirred field. The model eliminates mechanical heat loss by inputting net stirring torque and maps the shear resistance of the fluid to the stirring blades into dynamic viscosity, thereby sensing the physical process of the reactant changing from a liquid state to a highly viscous state in real time. The controller 400 updates parameters using a built-in heat transfer correlation. On the inner liner 110 side, increased material viscosity thickens the boundary layer, leading to a decrease in the convective heat transfer coefficient. These two factors exhibit a non-linear negative correlation. On the spiral flow channel 230 side, the controller 400 reads data from the mass flow meter 330, calculates the flow velocity of the heat transfer medium, and calculates the Reynolds number based on the flow channel geometry. Specifically, the convective heat transfer coefficient on the spiral flow channel 230 side... Real-time calculations are performed using the following correlation: ; in, The equivalent diameter of the spiral flow channel is denoted as . The thermal conductivity of the medium, For Prandtl numbers, The bulk fluid viscosity, The fluid viscosity at the wall; Reynolds number. Determined by the following formula: ; in, The density of the heat exchange medium, The average flow velocity of the heat exchange medium within the spiral flow channel; the controller 400 will calculate the... With the heat transfer coefficient of the inner liner Calculate the overall heat transfer coefficient in series. : ; in, The heat transfer coefficient of the inner liner side is convective heat transfer coefficient. The thickness of the inner liner wall. The thermal conductivity of the inner liner material. The fouling thermal resistance is used to determine the convective heat transfer coefficient on the medium side. The controller 400 combines the convective heat transfer coefficients on the inner and outer sides and the thermal resistance of the vessel wall to synthesize the real-time total heat transfer coefficient. This mechanism ensures that even when the material changes from a thin liquid to a thick slurry, the control system can still accurately assess the heat exchange capacity and provide mathematical model support for precise temperature control. In the S3 steps, spatiotemporal alignment specifically includes: The controller 400 reads the instantaneous flow data measured by the mass flow meter 330 in real time and performs cumulative integration over time. When the cumulative integral value reaches the geometric volume value of the spiral channel 230, the entry time corresponding to the fluid micro-element at the outlet 250 of the outflow medium at the current moment is locked. The outlet temperature data at the current moment is selected and paired with the inlet temperature data recorded at the entry moment to calculate the enthalpy change of the fluid micro-element during the transit process. In this embodiment, the spatiotemporal alignment step solves the temperature matching problem under variable flow rate conditions. The traditional fixed time delay method cannot adapt to the flow rate changes caused by the variable frequency pump, resulting in incorrect calculation of the inlet and outlet temperature difference. The controller 400 adopts the fluid micro-element tracking method, the core of which is that the spiral flow channel 230 is a rigid entity, and the fluid volume contained inside it is a constant geometric constant. The controller 400 reads the instantaneous flow data output by the mass flow meter 330, such as the Coriolis mass flow meter 330, at an extremely high sampling frequency and performs cumulative integration on the time axis; this integral value represents the total amount of medium flowing into the jacket from a certain moment. When the cumulative integral value increases to equal the control volume... At that time, the control volume is defined by the following formula: ; in, The geometric volume of the spiral flow channel 230 is... The internal dead volume of the pipeline and corrugated metal hose from the mass flow meter installation point 330 to the medium inlet 240; the entry time is locked when the following integration condition is met. : ; In the formula, For the current moment, The time represented by the integral variable, for The instantaneous mass flow rate passing through the mass flow meter at any given moment. for The real-time density of the heat exchange medium; physically, this means that the fluid element that entered the inlet at the start of integration has just reached the outlet at the current moment; at this time, the controller 400 immediately locks this historical moment as the entry moment; The system then retrieves the inlet temperature data stored at the entry time and forms a pair with the outlet temperature data collected at the current time. This pairing method ensures that the temperature difference calculation is applied to the same physical fluid micro-element, eliminating the heat calculation noise caused by the mixing of different fluid micro-elements, thereby calculating the accurate enthalpy change. In step S3, calculating the instantaneous exothermic rate of the chemical reaction specifically includes: The total energy change rate of the control volume is calculated as the product of the temperature change slope measured by the temperature probe 140 inside the vessel and the total heat capacity of the material. The total heat capacity of the material is obtained by multiplying the real-time total mass measured by the strain gauge weighing module and the real-time specific heat capacity obtained by looking up the table. The specific heat capacity table is a database of thermophysical parameters of a specific pharmaceutical intermediate stored in the controller 400 at different temperature ranges and different reaction conversion rates. The controller 400 retrieves values ​​using a two-dimensional index based on the real-time temperature and the integral heat release of the previous cycle. Subtract the heat dissipation power from the stirring, which is converted from the torque data of the servo motor 130, from the total energy change rate; Furthermore, the physical heat transfer power calculated based on spatiotemporal alignment is added; The remaining residual is determined as the instantaneous exothermic rate of the chemical reaction; In this embodiment, the instantaneous exothermic rate of the chemical reaction is calculated by treating the reaction vessel as an energy-conserving system and performing differential calculations. The controller 400 evaluates the sensible heat change of the system, i.e., the rate of change of total energy. This value is obtained by multiplying the rate of change of temperature over time, the differential slope, measured by the temperature probe 140 inside the vessel (e.g., a high-precision PT100 platinum resistance thermometer), by the current total heat capacity of the material. To ensure the accuracy of the heat capacity data, the total heat capacity of the material is not a preset constant, but is obtained by dynamically multiplying the real-time total mass measured by the strain gauge weighing module with the real-time specific heat capacity obtained by looking up a table based on the current temperature and material characteristics. Before this calculation, the controller 400 analyzes the raw mass signal collected by the strain gauge weighing module. Perform a moving average filter to eliminate periodic disturbances caused by stirring vibrations: ; in, This represents the number of sampling points in the moving average filter. The time interval for sampling; simultaneously, the rate of temperature change. A five-point quadratic smoothing algorithm is used for calculation to avoid amplifying measurement noise during differential operations; this takes into account the changes in mass during the feeding process and the effect of temperature on the specific heat capacity of the material. According to the law of conservation of energy, the energy change of the system originates from the heat of chemical reaction, the heat of mechanical stirring, and the heat exchange of the jacket. Therefore, the controller 400 subtracts the heat dissipation power of stirring input by the servo motor 130 from the calculated total energy change rate. This power value is directly converted from the motor speed and torque. The system further subtracts the physical heat transfer power accurately calculated by the aforementioned fluid micro-element tracking algorithm, that is, the heat carried away or brought in by the jacket. After deducting the heat input by stirring and compensating for the heat removed from the jacket, the remaining energy residual is logically attributed to the energy generated inside the system, and is thus determined as the instantaneous exothermic rate of the chemical reaction. Specifically, the reaction progress is not directly measured, but obtained through iterative calculation; in each calculation cycle, the controller 400 integrates the calculated instantaneous heat release rate over time to obtain the current cumulative heat release. The controller 400 has the theoretical total heat release of the chemical reaction pre-stored. ,Should The specific heat value is pre-determined in the laboratory stage using differential scanning calorimetry or reaction calorimetry; if the reaction is unknown, the controller 400 sets the initial default specific heat capacity. The first batch of trial calculations was performed, and the results were corrected by the actual cumulative total heat release after the reaction was completed. For precise control of subsequent batches; real-time reaction conversion rate. The calculation formula is: ; In the formula, for The instantaneous exothermic rate of the chemical reaction calculated at any given time; through calculation and The ratio is used to estimate the current reaction conversion rate, i.e., the reaction progress. When calculating the total heat capacity of the material at the current moment, the controller 400 uses the reaction progress estimated at the end of the previous calculation cycle, combined with the real-time temperature at the current moment, to look up the corresponding specific heat capacity value in the characteristic curve. Since the sampling frequency of the controller 400 is extremely high, such as 100ms, the change in reaction progress between two adjacent cycles is extremely small. Therefore, using the reaction progress of the previous cycle to look up the table will not introduce significant errors, thus solving the calculation deadlock problem where parameters are mutually causal. This data provides a direct thermodynamic basis for subsequent precise temperature control; In step S1, the bottom starting end of the spiral flow channel 230 is provided with a medium inlet 240 and the top end is provided with a medium outlet 250. Both the medium inlet 240 and the medium outlet 250 are connected to the external pipeline through a metal corrugated hose to isolate the interference of pipeline stress on the strain weighing module. In this embodiment, a pharmaceutical intermediate reaction control method with a high-efficiency heat exchange jacket 200 employs a specific mechanical decoupling design for the hardware connection method. To support the reliance on strain gauge weighing module data in the aforementioned steps, the purity of the weighing data must be ensured. Rigid pipelines in industrial settings can generate significant additional stress due to thermal expansion and contraction or installation errors, which, when applied directly to the reactor body, can severely interfere with weighing accuracy. Therefore, the medium inlet 240 and medium outlet 250 of the spiral flow channel 230 are not directly rigidly connected to the rigid pipe, but are instead connected to the external pipeline through corrugated metal hoses. The corrugated metal hoses possess excellent flexibility and multi-directional displacement compensation capabilities, effectively blocking the transmission of mechanical and thermal stress from the external pipelines to the reactor body, thus achieving the purpose of isolating pipeline stress. This improvement in physical connection method ensures that the strain gauge weighing module only senses the gravity changes of the reactor and materials, providing high-confidence mass parameters for heat capacity calculation. In step S4, the priority adjustment specifically adopts a split-range priority control strategy: The controller 400 prioritizes adjusting the speed of the circulating pump 340 to change the medium flow rate and heat transfer coefficient; During the adjustment process, when the speed of the circulating pump 340 reaches the preset upper limit threshold or the flow channel pressure limit threshold and still cannot meet the cooling requirements, the controller 400 locks the current speed and instead adjusts the opening of the electric three-way proportional regulating valve, which serves as a cold and heat source distribution valve, to change the mixing ratio of the cold and hot media entering the spiral flow channel 230. In this embodiment, the priority adjustment strategy aims to optimize energy consumption and improve control stability. Traditional temperature control often involves frequent adjustments to the hot and cold source distribution valves, resulting in high energy consumption and system oscillation. This method adopts a split-range priority control strategy. The medium pressure transmitter 350 is installed on the pipeline between the outlet of the circulating pump 340 and the medium inlet 240 to monitor the pumping pressure in real time. The controller 400 has a flow channel pressure limit threshold set, which is less than the rated pressure resistance of the metal corrugated hose. When the controller 400 receives a cooling or heating command, it prioritizes adjusting the speed of the circulating pump 340. Changing the pump speed directly changes the flow velocity of the medium in the spiral flow channel 230, thereby changing the Reynolds number and convective heat transfer coefficient of the fluid. Within a certain range, the heat exchange requirements can be met simply by increasing the flow velocity to enhance the turbulence, without consuming additional cold or hot source energy, such as chilled water or steam. Only when the speed of the circulating pump 340 increases to a preset upper limit threshold, such as the pump's rated speed or the flow channel pressure limit threshold, to prevent damage to the equipment due to excessive pressure. The upper limit threshold is a logical upper limit set based on the rated safe frequency of the circulating pump 340 motor, while the flow channel pressure limit threshold is a physical safety threshold preset based on the fatigue limit of the metal corrugated hose and jacket welding strength. This triggers the step-by-step switching of the split-range priority control strategy. When the calculated removed heat power is still less than the reaction exothermic rate, the system determines that relying solely on fluid dynamics has reached its limit. At this time, the controller 400 keeps the pump running at the maximum safe speed, locks the current speed, and enters the second segment, starting to adjust the opening of the electric three-way proportional regulating valve. By physically changing the mixing ratio of the cold medium and the return medium, the temperature of the medium entering the jacket is reduced, thereby increasing the heat transfer temperature difference and providing stronger heat exchange capacity. Step S4 is followed by: S5. Execution trajectory tracking and endpoint determination: The controller 400 continuously records the change curve of the instantaneous heat release rate over time. When the instantaneous heat release rate returns to the baseline and remains stable, the reaction is determined to have reached the endpoint. In this embodiment, trajectory tracking and endpoint determination utilize thermodynamic data as a fingerprint of the reaction process. Conventional control often uses reaction time or temperature as the basis for endpoint determination, but this is easily affected by environmental interference. In this method, the controller 400 constructs and continuously records the curve of the instantaneous heat release rate changing over time in memory. As reactants are consumed, the reaction rate of a chemical reaction gradually decreases, and the corresponding exothermic rate also decreases. When the curve shows that the instantaneous exothermic rate returns to the baseline, that is, close to zero or only the stirring heat baseline remains and remains stable in this state for a period of time, the system confirms from an energy perspective that the chemical reaction has stopped. Based on this, the controller 400 automatically determines that the reaction has reached its endpoint and can trigger subsequent cooling or discharge processes. This method avoids the misleading phenomenon of false isothermal effect caused by heat transfer lag and ensures the consistency of reaction degree between batches.

[0019] Example 2: Please see Figures 1-3 A pharmaceutical intermediate reaction device with a high-efficiency heat exchange jacket 200, comprising: The main component 100 of the reactor includes an inner liner 110, a stirring shaft 120 and a servo motor 130. The bottom of the inner liner 110 is supported on a strain gauge weighing module. The high-efficiency heat exchange jacket 200 includes an outer shell 210 covering the outside of the inner liner 110 and a spiral guide plate 220, the spiral guide plate 220 defining a spiral flow channel 230 with a fixed physical path length. The sensing and circulation assembly 300 includes an inlet temperature transmitter 310, an outlet temperature transmitter 320, a mass flow meter 330, a circulation pump 340, a medium pressure transmitter 350, and a cold and heat source distribution valve. And controller 400; The controller 400 is electrically connected to the main reactor assembly 100 and the sensing and circulation assembly 300, respectively.

[0020] In this embodiment, a pharmaceutical intermediate reaction device with a high-efficiency heat exchange jacket 200 realizes the hardware implementation of the above-mentioned control method. The main body component 100 of the reactor serves as the reaction site, and its inner liner 110 is connected to the foundation through a strain gauge weighing module at the bottom, realizing full-range quality monitoring during the reaction process. The stirring shaft 120, in conjunction with the servo motor 130, not only provides stirring power but also functions as a viscometer. The high-efficiency heat exchange jacket 200, through the cooperation of the outer shell 210 and the spiral guide plate 220, constructs a forced turbulent environment. The fixed physical path length of the spiral flow channel 230... It is the physical foundation of the fluid micro-element tracking algorithm. The inlet temperature transmitter 310 and outlet temperature transmitter 320 in the sensing and circulation component 300 capture the incoming and outgoing heat status respectively. The mass flow meter 330 provides high-precision flow velocity integral data. The circulation pump 340, medium pressure transmitter 350 and cold and heat source distribution valve act as actuators to respond to control commands. The controller 400 acts as the computing core and is electrically connected to the above components through an industrial fieldbus or analog interface. It collects data in real time and solves the heat balance equation, and finally outputs control signals to complete the automation process from sensing to execution. The inner edge of the spiral guide plate 220 is fully welded to the outer wall of the inner liner 110, and the outer shell 210 is tightly wrapped around the outer edge of the spiral guide plate 220 using a segmented splicing process or a heat-shrinking process. In this embodiment, the manufacturing process of the spiral guide plate 220 is directly related to the accuracy of the control model. To ensure that the medium flows strictly along the spiral path without any internal short circuits, the inner edge of the spiral guide plate 220 is fully welded to the outer wall of the inner liner 110. The continuity of the weld eliminates the possibility of the medium flowing along the inner wall, ensuring the effective utilization of the heat exchange area. At the same time, in order to solve the problem of external sealing and assembly, the outer shell 210 does not use a common sleeve, but adopts a segmented splicing process. The shell is divided into multiple segments and then welded or heat-fitted, using the principle of thermal expansion and contraction to fasten it. This process ensures that the outer shell 210 can tightly cover the outer edge of the spiral guide plate 220, forming a reliable line seal or surface seal between the two. As a preferred embodiment, the segmented splicing process is as follows: the outer shell 210 is prefabricated into two semi-cylindrical tile-shaped structures, i.e., a split structure; during assembly, the two semi-cylindrical outer shells 210 are fastened to the outside of the inner liner 110 of the already welded spiral guide plate 220; at this time, a radial clamping force is applied to the two outer shells 210 using hydraulic tooling, so that their inner walls make pre-tight contact with the outer edge of the spiral guide plate 220, ensuring that there is no gap between the sheath and the guide plate, and welding is performed along the longitudinal seam of the outer shell 210 for sealing; this process effectively overcomes the assembly difficulties caused by the outer diameter tolerance of the spiral guide plate 220, and at the same time, the stress of welding cooling contraction is used to further lock the mating surfaces, ensuring the sealing between the layers of the spiral flow channel 230 and preventing interlayer short circuits of the heat exchange medium; This structural tightness forces all fluids to flow along the long path of the spiral channel 230, making the residence time and path length of the fluid highly predictable, thus supporting the assumption in the aforementioned fluid element tracking algorithm that the channel volume is constant.

[0021] It should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit it. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims

1. A method for controlling the reaction of pharmaceutical intermediates with a high-efficiency heat exchange jacket, characterized in that, include: S1. A reactor main body assembly (100), a high-efficiency heat exchange jacket (200), a sensing and circulation assembly (300), and a controller (400) are set up. The reactor main body assembly (100) has a strain gauge weighing module at the bottom of the inner liner (110). The servo motor (130) drives the stirring shaft (120). The spiral guide plate (220) in the high-efficiency heat exchange jacket (200) divides the cavity between the inner liner (110) and the outer shell (210) into a single spiral flow channel (230) connected end to end. S2. Control the servo motor (130) to stir the material. The controller (400) collects the instantaneous torque value, combines the real-time rotation speed to invert the real-time viscosity of the material, and dynamically corrects the total heat transfer coefficient according to the real-time viscosity and the flow rate of the heat exchange medium. S3. The controller (400) integrates the mass flow data of the sensing and circulation component (300), locks the transit time of the heat exchange medium through the spiral channel (230), aligns the temperature of the medium outlet (250) with the historical inlet temperature in time and space to calculate the change of fluid micro-element enthalpy, and calculates the instantaneous heat release rate of the chemical reaction by combining the material mass measured by the strain gauge weighing module. S4. The controller (400) generates balanced heat removal power according to the instantaneous heat release rate, prioritizes adjusting the speed of the circulating pump (340), and adjusts the opening of the cold and heat source distribution valve when the limit is reached. The steps preceding S2 include: S2.1 Perform no-load friction torque self-learning calibration. When the inner liner (110) is in a no-load state, control the servo motor (130) to run in the full speed range, record the steady-state torque required to maintain operation at different speeds, and construct and store the corresponding curve of speed and no-load friction torque. In step S2, the controller (400) obtains the no-load friction torque by consulting the corresponding relationship curve based on the current real-time rotation speed, and subtracts the no-load friction torque from the instantaneous torque value to obtain the net stirring torque caused by the material viscosity resistance, which is used to invert the real-time viscosity. In step S2, the dynamic correction of the overall heat transfer coefficient specifically includes: The controller (400) calculates the viscosity change of the reactants based on the trend of the change in the net stirring torque; The total heat transfer coefficient used for heat calculation is updated in real time by utilizing the nonlinear negative correlation between the convective heat transfer coefficient on the inner liner (110) side and the material viscosity, as well as the Reynolds number on the spiral flow channel (230) side determined by the medium flow rate.

2. The method for controlling the reaction of pharmaceutical intermediates with a high-efficiency heat exchange jacket according to claim 1, characterized in that, In step S3, the spatiotemporal alignment specifically includes: The controller (400) reads the instantaneous flow data measured by the mass flow meter (330) in real time and performs cumulative integration over time. When the cumulative integral value reaches the geometric volume value of the spiral channel (230), the entry time corresponding to the fluid micro-element of the current outflow medium outlet (250) is locked. The outlet temperature data at the current moment is selected and paired with the inlet temperature data recorded at the entry moment to calculate the enthalpy change of the fluid element during the transit process.

3. The method for controlling the reaction of pharmaceutical intermediates with a high-efficiency heat exchange jacket according to claim 2, characterized in that, In step S3, calculating the instantaneous exothermic rate of the chemical reaction specifically includes: The total energy change rate of the control body is calculated as the product of the temperature change slope measured by the temperature probe (140) inside the vessel and the total heat capacity of the material, wherein the total heat capacity of the material is obtained by multiplying the real-time total mass measured by the strain gauge weighing module and the real-time specific heat capacity obtained by looking up the table. Subtract the heat dissipation power of stirring, which is converted from the torque data of the servo motor (130), from the total energy change rate; Furthermore, the physical heat transfer power calculated based on the aforementioned spatiotemporal alignment is added; The remaining residual is determined as the instantaneous exothermic rate of the chemical reaction.

4. The method for controlling the reaction of pharmaceutical intermediates with a high-efficiency heat exchange jacket according to claim 1, characterized in that, In step S1, the bottom starting end of the spiral flow channel (230) is provided with a medium inlet (240) and the top end is provided with a medium outlet (250). Both the medium inlet (240) and the medium outlet (250) are connected to the external pipeline through a metal corrugated hose to isolate the pipeline stress from interfering with the strain weighing module.

5. The method for controlling the reaction of pharmaceutical intermediates with a high-efficiency heat exchange jacket according to claim 1, characterized in that, In step S4, the priority adjustment specifically adopts a segmented priority control strategy: The controller (400) preferentially adjusts the rotational speed of the circulating pump (340) to change the medium flow rate and heat transfer coefficient; During the adjustment process, when the speed of the circulating pump (340) reaches the preset upper limit threshold or the flow channel pressure limit threshold and still cannot meet the cooling requirements, the controller (400) locks the current speed and instead adjusts the opening of the electric three-way proportional regulating valve, which serves as the cold and heat source distribution valve, to change the mixing ratio of the cold and hot media entering the spiral flow channel (230).

6. The method for controlling the reaction of pharmaceutical intermediates with a high-efficiency heat exchange jacket according to claim 1, characterized in that, Step S4 is followed by: S5. Execution trajectory tracking and endpoint determination: The controller (400) continuously records the change curve of the instantaneous heat release rate over time. When the instantaneous heat release rate returns to the baseline and remains stable, the reaction is determined to have reached the endpoint.

7. The method for controlling the reaction of pharmaceutical intermediates with a high-efficiency heat exchange jacket according to claim 1, characterized in that, The inner edge of the spiral guide plate (220) is fully welded to the outer wall of the inner liner (110), and the outer shell (210) is tightly wrapped around the outer edge of the spiral guide plate (220) using a segmented splicing process or a heat-shrinking process.

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