Equipment experiment parameter control method, device and parameter control equipment
The parameter control device and method automate the adjustment of multiple device parameters to maintain target reaction system values, addressing manual intervention challenges and ensuring precise control in chemical reaction synthesis experiments.
Patent Information
- Application Number
- CN202411179300.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-08-27
- Publication Date
- 2024-12-20
- Estimated Expiration
- 2044-08-27
AI Technical Summary
In chemical reaction synthesis experiments, technicians spend significant time manually adjusting parameters in response to experimental phenomena, lacking an effective method for automated control of experimental parameters.
A parameter control device and method that continuously calculates and adjusts multiple device parameters to maintain a target reaction system parameter value, using a processor and communication module to connect with various controlled devices, including sensors and actuators, to automate parameter adjustments.
Automated parameter control maintains reaction system parameters near target values, reducing manual intervention and avoiding adverse consequences, while being cost-effective and compatible with existing laboratory setups.
Smart Images

Figure CN118698463B_ABST
Abstract
Description
Technical Field
[0001] The present application relates to the technical field of chemical reaction control, and in particular to a method and device for controlling equipment experimental parameters, and a parameter control device. Background Art
[0002] In actual synthesis experiments in process development laboratories, in addition to a small amount of repeated experimental operations, experimenters need to spend a lot of time observing experimental phenomena, recording data, and manually adjusting experimental parameters according to experimental phenomena. Therefore, how to automatically control experimental parameters has become a technical problem that technicians in this field need to solve urgently. Summary of the invention
[0003] The embodiments of the present application provide a method, apparatus, electronic device and readable storage medium for controlling equipment experimental parameters, which can control equipment experimental parameters of multiple equipment that have an impact on the target parameter of the reaction system when adjusting a single equipment experimental parameter causes a change in the value of the target parameter of the reaction system, thereby maintaining the value of the target parameter of the reaction system near the target value.
[0004] The embodiments of the present application can be implemented as follows:
[0005] In a first aspect, an embodiment of the present application provides a device experiment parameter control method, which is applied to a parameter control device, wherein the parameter control device is communicatively connected with a plurality of controlled devices, and the method includes:
[0006] determining a target value of a reaction system target parameter that the reaction system needs to maintain when adjusting a first device experimental parameter of the first device;
[0007] With the goal of maintaining the target parameter of the reaction system at the target value, a first control value of a first device experimental parameter of the first device and a second control value of a second device experimental parameter of at least one second device are continuously calculated based on the current value of the target parameter of the reaction system and the target value, and corresponding devices are controlled according to the calculated control values, wherein the working states of the first device and at least one second device among the multiple controlled devices both affect the target parameter of the reaction system.
[0008] In a second aspect, an embodiment of the present application provides a device experiment parameter control device, which is applied to a parameter control device, wherein the parameter control device is communicatively connected with a plurality of controlled devices, and the device comprises:
[0009] An information acquisition module, used to determine a target value of a reaction system target parameter that the reaction system needs to maintain when adjusting a first device experimental parameter of the first device;
[0010] A control module is used to maintain the target parameter of the reaction system at the target value, continuously calculate a first control value of a first device experimental parameter of the first device and a second control value of a second device experimental parameter of at least one second device according to a current value of the target parameter of the reaction system and the target value, and control the corresponding device according to the calculated control values, wherein the working states of the first device and at least one second device among the multiple controlled devices both affect the target parameter of the reaction system.
[0011] In a third aspect, an embodiment of the present application provides a parameter control device, including a processor and a memory, wherein the memory stores machine executable instructions that can be executed by the processor, and the processor can execute the machine executable instructions to implement the device experimental parameter control method described in the aforementioned embodiment.
[0012] In a fourth aspect, an embodiment of the present application provides a readable storage medium having a computer program stored thereon, and when the computer program is executed by a processor, the device experimental parameter control method as described in the aforementioned embodiment is implemented.
[0013] The device experimental parameter control method, device, electronic device and readable storage medium provided in the embodiment of the present application, the parameter control device is connected to multiple controlled devices in communication, the parameter control device determines the target value of the reaction system target parameter that the reaction system needs to maintain when adjusting the first device experimental parameter of the first device, and then takes the reaction system target parameter as the target value, and continuously calculates the first control value of the first device experimental parameter of the first device and the second control value of the second device experimental parameter of at least one second device according to the current value and the target value of the reaction system target parameter, and controls the corresponding device according to the calculated control value. Among them, the working states of the first device and at least one second device in the multiple controlled devices all affect the reaction system target parameter. In this way, in the case where the value of the reaction system target parameter changes due to the adjustment of a single device experimental parameter, the value of the reaction system target parameter can be maintained near the target value by controlling the device experimental parameters of multiple devices that have an impact on the reaction system target parameter. BRIEF DESCRIPTION OF THE DRAWINGS
[0014] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for use in the embodiments are briefly introduced below. It should be understood that the following drawings only show certain embodiments of the present invention and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other related drawings can be obtained based on these drawings without creative work.
[0015] Figure 1A block diagram of a parameter control device provided in an embodiment of the present application;
[0016] Figure 2 One of the flow charts of the device experimental parameter control method provided in the embodiment of the present application;
[0017] Figure 3 One of the schematic diagrams of the chemical reaction system provided in the embodiment of the present application;
[0018] Figure 4 2 is a flow chart of the sub-steps included in step S200;
[0019] Figure 5 for Figure 4 A schematic flow chart of the sub-steps included in sub-step S210;
[0020] Figure 6 for Figure 5 A schematic flow chart of the sub-steps included in sub-step S211;
[0021] Figure 7 for Figure 5 A schematic flow chart of the sub-steps included in sub-step S212;
[0022] Figure 8 The second flow chart of the device experimental parameter control method provided in the embodiment of the present application;
[0023] Fig. 9 The second schematic diagram of the chemical reaction system provided in the embodiment of the present application;
[0024] Fig.10 A block diagram of an equipment experimental parameter control device provided in an embodiment of the present application.
[0025] Icons: 100- parameter control device; 110- memory; 120- processor; 130- communication unit; 201- reactor; 210- high and low temperature all-in-one machine; 220- liquid drop acceleration control device; 230- agitator; 240- liquid container; 250- liquid pipeline; 260- reaction container; 270- thermometer; 280- camera; 300- equipment experimental parameter control device; 310- information acquisition module; 320- control module. DETAILED DESCRIPTION
[0026] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Generally, the components of the embodiments of the present invention described and shown in the drawings here can be arranged and designed in various different configurations.
[0027] Therefore, the following detailed description of the embodiments of the present application provided in the accompanying drawings is not intended to limit the scope of the present application for which protection is sought, but merely represents selected embodiments of the present application. Based on the embodiments of the present application, all other embodiments obtained by those skilled in the art without creative work are within the scope of protection of the present application.
[0028] It should be noted that relational terms such as "first" and "second" are used only to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions, the elements defined by the sentence "comprise a ..." do not exclude the existence of other identical elements in the process, method, article or device including the elements.
[0029] In conjunction with the accompanying drawings, some embodiments of the present application are described in detail below. In the absence of conflict, the following embodiments and features in the embodiments can be combined with each other.
[0030] Please refer to Figure 1 , please refer to Figure 1 , Figure 1 The block diagram of the parameter control device 100 provided in the embodiment of the present application. The parameter control device 100 may include a memory 110, a processor 120 and a communication unit 130. The memory 110, the processor 120 and the communication unit 130 are electrically connected to each other directly or indirectly to realize data transmission or interaction. For example, these components can be electrically connected to each other through one or more communication buses or signal lines.
[0031] The memory 110 is used to store programs or data. The memory 110 may be, but is not limited to, a random access memory (RAM), a read only memory (ROM), a programmable read-only memory (PROM), an erasable programmable read-only memory (EPROM), an electrically erasable programmable read-only memory (EEPROM), etc.
[0032] The processor 120 is used to read / write data or programs stored in the memory 110 and execute corresponding functions. For example, the memory 110 stores a device experiment parameter control device 300, and the device experiment parameter control device 300 includes at least one software function module that can be stored in the memory 110 in the form of software or firmware. The processor 120 executes various functional applications and data processing by running software programs and modules stored in the memory 110, such as the device experiment parameter control device 300 in the embodiment of the present application, that is, realizing the device experiment parameter control method in the embodiment of the present application.
[0033] The communication unit 130 is used to establish a communication connection between the parameter control device 100 and other communication terminals through a network, and to send and receive data through the network.
[0034] It should be understood that Figure 1 The structure shown is only a schematic diagram of the structure of the parameter control device 100. The parameter control device 100 may also include Figure 1 More or fewer components as shown, or with Figure 1 Different configurations are shown. Figure 1 Each component shown in the figure can be implemented by hardware, software or a combination thereof.
[0035] Please refer to Figure 2 , Figure 2 One of the flow diagrams of the device experiment parameter control method provided in the embodiment of the present application. The method is applied to a parameter control device in a chemical reaction system, and the parameter control device is connected to a plurality of controlled devices in communication. The specific process of the device experiment parameter control method is described in detail below. In this embodiment, the method may include steps S100 to S200.
[0036] Step S100, determining a target value of a reaction system target parameter that the reaction system needs to maintain when adjusting a first device experimental parameter of the first device.
[0037] Step S200, with the target parameter of the reaction system maintained at the target value, continuously calculate the first control value of the first device experimental parameter of the first device and the second control value of the second device experimental parameter of at least one second device based on the current value of the target parameter of the reaction system and the target value, and control the corresponding device according to the calculated control value.
[0038] In this embodiment, the multiple controlled devices are chemical reaction execution devices, which can be determined in combination with actual needs. The multiple controlled devices include the above-mentioned first device and at least one second device. The working state of each device in the first device and at least one second device affects the target parameter of the reaction system, that is, it will cause the value of the target parameter of the reaction system to change. In the case of adjusting only the first device experimental parameter of the first device, the value of the target parameter of the reaction system of the reaction system will change; in order to avoid the value of the target parameter of the reaction system far deviating from the required value when only controlling the first device, the target value of the target parameter of the reaction system that the reaction system needs to maintain can be determined first, and then the target value of the target parameter of the reaction system is maintained as the target value. In the formal experiment stage, the current value and the target value of the target parameter of the reaction system are continuously calculated to obtain the control value of the device experimental parameter of the first device and at least one second device whose working state has an impact on the value of the target parameter of the reaction system, and the corresponding device is controlled according to the control value, so that the target parameter of the target reaction system is maintained near the target value in the formal experiment stage.
[0039] In the actual synthesis experiment of the process development laboratory. Adjusting a single experimental parameter (i.e., an experimental parameter of a certain device of a device) is likely to cause changes in other parameters. If this is not controlled, it may lead to adverse consequences, such as causing temperature changes and then leading to safety accidents. In view of the above situation, in this embodiment, by controlling the device experimental parameters of multiple controlled devices that have an impact on the value of the target parameter of the reaction system in the chemical reaction, the target parameter of the target reaction system can be maintained near the target value. In this way, the target parameter of the target reaction system can be maintained near the target value through quick multi-parameter control, and no manual adjustment is required.
[0040] Currently, integrated automation equipment and systems are also used to simulate human actions and record processes, so as to replace simple repetitive operations in experimental operations with machines. However, integrated automation equipment is expensive, has a long customization cycle, high use costs, and fixed and inflexible operation processes, requiring major modifications to existing synthesis laboratories. For early drug synthesis laboratories that do not consider costs, it can reduce the number of synthesis engineers, but it is completely inapplicable to flexible and changeable process research and development laboratories. In order to alleviate the above situation, as a possible implementation method, the equipment in the chemical reaction system is the existing equipment in the laboratory and some newly added small equipment. In this way, since no large mechanical devices are involved, the parameter control equipment is small in size, the use process is robust, and it is compatible with the current synthesis laboratory, and no major modification of the laboratory is required.
[0041] Among them, in the above-mentioned equipment experimental parameter control method, it is necessary to collect parameters and control the controlled equipment, and the specific parameters collected and the specific controlled equipment are determined by the actual situation. Optionally, when the equipment in the chemical reaction system is an existing laboratory equipment and some newly added small equipment, various parameters in the reaction process can be collected through the built-in sensors of the existing laboratory equipment and other sensors connected to the multi-parameter control equipment. The collectable parameters include, but are not limited to, temperature (for example, the temperature is collected by the built-in temperature sensor of the high and low temperature integrated machine, and the temperature is collected by the external temperature sensor), liquid addition amount / liquid addition speed (provided by the liquid addition pump), pH (provided by the pH meter), turbidity (provided by the turbidity meter), conductivity (conductivity), spectral signal (near infrared spectrum, mid-infrared spectrum, Raman spectrum, etc.), pressure (pressure gauge), mass (scale), speed (stirrer), etc. The controlled device is a chemical reaction execution device connected to the parameter control device, which can accept the instructions issued by the parameter control device and perform corresponding operations; for example: adjusting the speed of the stirrer, the temperature of the high and low temperature integrated machine, the speed of liquid addition, etc.
[0042] In this embodiment, the parameter A to be controlled (i.e., the target parameter of the reaction system) can be manually selected, and the devices B1, B2, ... (the number of devices is greater than or equal to 1) that affect the parameter A can be determined, and then the control value of each device can be determined and controlled. The process can be shown in the following formula:
[0043]
[0044] in, It represents the total control output of the chemical reaction system, corresponding to the change of the parameter A to be controlled; represents the weight of the output of the i-th device; represents the theoretical control value of the i-th device obtained when only the i-th device is controlled so that the target parameter of the reaction system is the target value; represents the output of the ith device (i.e., the control value of the device experimental parameter of the ith device), and n represents the number of controlled devices to be controlled for parameter A.
[0045] The output of each controlled device can be calculated by the following formula:
[0046]
[0047] in, represents the preset scaling factor of the i-th device, represents the preset integral coefficient of the ith device, represents the preset differential coefficient of the ith device, It represents the difference between the actual value of the target parameter of the reaction system in the reaction system and the target value. It is understood that It can represent the theoretical control value of the i-th device generated by the corresponding PID control module when only the i-th device is controlled so that the target parameter of the reaction system is the target value.
[0048] The collected data can be used to calculate the The value of the controlled device is obtained to obtain the control value corresponding to each controlled device, and the corresponding device is controlled so that the value of the target parameter of the reaction system is maintained near the target value.
[0049] As a possible implementation, Figure 3 As shown, the chemical reaction system includes a parameter control device 100, a reactor 201, a high and low temperature integrated machine 210, a liquid drop acceleration control device 220 and an agitator 230. The reactor 201 may be a jacketed reactor, and the liquid drop acceleration control device 220 may be a liquid adding pump.
[0050] In this embodiment, Figure 3 In the chemical reaction system shown, the target parameter of the reaction system is the temperature of the reaction system in the reactor, that is, the temperature of the reaction solution in the reactor; the first device is a high and low temperature integrated liquid droplet acceleration control device, and the at least one second device includes a liquid droplet acceleration control device, which can take the value of the reaction solution temperature in the reactor as the target value. As a possible implementation method, Figure 4 The corresponding control value is calculated in the manner shown and then the corresponding control is performed. Figure 4 , Figure 4 FIG. 2 is a flow chart of sub-steps included in step S200. In this embodiment, step S200 may include sub-steps S210 to S220.
[0051] Sub-step S210, calculating and obtaining the first weight of the current high and low temperature integrated machine and the second weight of the liquid dripping acceleration control device.
[0052] Sub-step S220, calculating the first control value according to the current value, the target value and the first weight, and calculating the second control value according to the current value, the target value and the second weight.
[0053] In this embodiment, during the formal experiment, the weight of the current high and low temperature integrated machine can be calculated as the first weight, and the weight of the current liquid dripping acceleration control device can be calculated as the second weight. The specific calculation method can be determined according to actual needs. It is worth noting that during the formal experiment, the current first weight and second weight must be determined each time the control is performed. The first weight and second weight at different times may be different, which is specifically determined by the actual situation.
[0054] In one control, when the first weight of the current high and low temperature integrated machine is determined, the first control value can be calculated based on the current value of the temperature of the reaction system, the target value and the first weight. Wherein, the first control value is used to indicate the power adjustment amount of the high and low temperature integrated machine, that is, to indicate how much the heating power increases or decreases. And, when the second weight of the current liquid droplet acceleration control device is determined, the second control value can be calculated based on the current value of the temperature of the reaction system, the target value and the second weight. Wherein, the second control value is used to indicate the speed adjustment amount of the liquid droplet acceleration control device, that is, to indicate how much the liquid droplet acceleration increases or decreases. The above-mentioned first control value for controlling the power of the high and low temperature integrated machine and the second control value for controlling the speed of the liquid droplet acceleration control device are used to maintain the temperature of the reaction system near the target value.
[0055] As a possible implementation, this can be achieved by Figure 5 The current first weight and second weight are obtained as shown. Please refer to Figure 5 , Figure 5 for Figure 4 Schematic diagram of the flow of sub-steps included in sub-step S210. In this embodiment, sub-step S210 may include sub-steps S211 and S212.
[0056] Sub-step S211, in the pre-processing stage, controls the high and low temperature integrated machine to control the temperature of the reaction system according to the target value, records and maintains the current first heating power of the high and low temperature integrated machine until the temperature of the reaction system reaches the target value, and while maintaining the first heating power, controls the liquid dripping acceleration control device to drip liquid into the reaction system for a second preset time, and obtains the reaction heat released by the dripping liquid, and calculates the first reaction system temperature change value corresponding to the reaction system based on the reaction heat released.
[0057] In this embodiment, the target value T of the temperature of the reaction system, as well as the dropping speed L and the stirring speed R can be set in advance.
[0058] In the pre-treatment stage, the high and low temperature all-in-one machine and the stirrer can be turned on first, and then the high and low temperature all-in-one machine works according to the target value T of the temperature of the reaction system, so that the temperature of the reaction system is the target value T; and the stirrer stirs the reaction system according to the stirring speed R. In this process, the actual temperature of the reaction system is collected, and it is judged whether the temperature reaches the target value based on the actual temperature. If it is reached, the reaction system is considered to be stable, and the heating power of the high and low all-in-one machine when determining that the temperature of the reaction system reaches the target value is recorded as the first heating power P0, and the high and low temperature all-in-one machine is controlled to keep the first heating power P0 working, and then liquid can be added to the reaction system. If it is not reached, the actual temperature of the reaction system continues to be collected and judged until it is determined that the temperature of the reaction system reaches the target value.
[0059] Alternatively, if Figure 3 As shown, a thermometer is provided for measuring the temperature T2 of the reaction system. The temperature T2 of the reaction system can be obtained by the thermometer, and it can be determined whether the difference between the temperature T2 and the target value T is less than a first preset value. , the first preset value Can be set smaller; if smaller, , it is determined that the temperature of the reaction system has reached the target value; if it is not less than , it is determined that the temperature of the reaction system has not reached the target value.
[0060] In this embodiment, after determining that the temperature of the reaction system reaches the target value, the high and low integrated machine keeps working at the first heating power P0 and the agitator works at the stirring speed R, and the liquid dripping speed control device is controlled to drip liquid into the reaction system at a dripping speed L, and continues for a second preset time to perform an exothermic test. The exothermic test is to drip liquid into the reaction system at a dripping speed L for a second preset time. Among them, the second preset time can be X1s, which can be set in combination with actual needs. After the liquid is added dropwise, the reaction heat caused by the entire liquid addition process can be analyzed, that is, after the exothermic test is completed, the reaction heat caused by the exothermic test is analyzed.
[0061] Optionally, you can Figure 6 The heat release of the reaction is calculated in the manner shown. Figure 6 , Figure 6 for Figure 5 Schematic diagram of the flow of sub-steps included in sub-step S211. In this embodiment, sub-step S211 may include sub-steps S2111 to S2114.
[0062] Sub-step S2121, when it is determined that the temperature of the reaction system reaches the target value, obtaining a first outlet temperature, a first inlet temperature of the reactor and a first reaction system temperature of the reaction system.
[0063] Sub-step S2122, controlling the liquid dripping speed control device to drip liquid into the reaction system for the second preset time period according to the preset dripping speed, so as to perform an exothermic test.
[0064] Sub-step S2123, judging whether the temperature has recovered to the temperature before the liquid was added based on the first outlet temperature, the first inlet temperature, the first reaction system temperature, the second reaction system temperature of the reaction system after the exothermic test, the second outlet temperature and the second inlet temperature of the reactor.
[0065] In sub-step S2124, when it is determined that the temperature is restored to the temperature before liquid is added, the heat released by the reaction is calculated based on the heat added to the reaction system during the process from adding liquid to determining that the temperature is restored to the temperature before liquid is added, the heat taken away by the flowing medium of the reactor, and the heat exchange amount between the reactor and the air.
[0066] In this embodiment, if Figure 3As shown, in the pre-treatment stage, the inlet temperature T1 of the reactor, the outlet temperature T3 of the reactor, and the temperature T2 of the reaction system in the reactor can also be collected. The first outlet temperature can be obtained according to the outlet temperature T3 obtained when the temperature of the reaction system reaches the target value, and the first inlet temperature can be obtained according to the inlet temperature T1 obtained when the temperature of the reaction system reaches the target value, and the first reaction system temperature can be obtained according to the reaction system temperature T2 obtained when the temperature of the reaction system reaches the target value. Wherein, when the reactor is a jacketed reactor, the above outlet temperature T3 represents the outlet temperature of the jacketed reactor, and the above inlet temperature represents the inlet temperature of the jacketed reactor.
[0067] Optionally, when it is determined that the temperature of the reaction system has reached the target value, data collection can be performed on the outlet temperature T3, the inlet temperature T1, and the reaction system temperature T2, and the outlet temperature T3 collected this time can be used as the first outlet temperature T31, the inlet temperature T1 collected this time can be used as the first inlet temperature T11, and the reaction system temperature T2 collected this time can be used as the first reaction system temperature T21.
[0068] Alternatively, when it is determined that the temperature of the reaction system reaches the target value, multiple data collections can be performed on the outlet temperature T3, the inlet temperature T1, and the reaction system temperature T2 within a first preset time, and the average value of the multiple outlet temperatures T3 collected is used as the first outlet temperature T31, the average value of the multiple inlet temperatures T1 collected is used as the first inlet temperature T11, and the average value of the multiple reaction system temperatures T2 collected is used as the first reaction system temperature T21. The first preset time can be X0s, which can be determined in combination with actual needs.
[0069] When the first outlet temperature T31, the first inlet temperature T11 and the first reaction system temperature T21 are obtained, other parameters can be maintained unchanged, that is, the heating power of the high and low temperature integrated machine is maintained at the first heating power P0, the stirring speed of the agitator is maintained at R, and the liquid droplet speed control device is controlled to drop liquid into the reaction system according to the preset droplet speed L for the second preset time to perform an exothermic test. When the liquid droplet is started (that is, when the exothermic test starts), the real-time values of the outlet temperature T3, the inlet temperature T1 and the reaction system temperature T2 can be recorded.
[0070] Optionally, after the dropwise addition for the second preset time period is completed (i.e., after the exothermic test is completed), the real-time values of the outlet temperature T3, the inlet temperature T1 and the reaction system temperature T2 can continue to be obtained and recorded, and the second outlet temperature, the second inlet temperature of the reactor and the second reaction system temperature of the reaction system can be determined based on the outlet temperature T3, the inlet temperature T1 and the reaction system temperature T2 obtained after the exothermic test.
[0071] Optionally, after determining that the dropwise addition is completed (i.e., after the dropwise addition for the second preset time period is completed in the pre-treatment stage), data collection may be performed on the outlet temperature T3, the inlet temperature T1, and the reaction system temperature T2, and the outlet temperature T3 collected this time may be used as the second outlet temperature T32, the inlet temperature T1 collected this time may be used as the second inlet temperature T12, and the reaction system temperature T2 collected this time may be used as the second reaction system temperature T22.
[0072] Alternatively, after the dropwise addition for the second preset duration is completed, the third preset duration may be waited for, and the real-time values of the outlet temperature T3, the inlet temperature T1, and the reaction system temperature T2 may be continuously recorded during the waiting process; after waiting for the third preset duration, a historical time period may be determined with the current moment as the starting point and the fourth preset duration as the duration, and the average value of the multiple outlet temperatures T3 recorded in the historical time period may be used as the second outlet temperature T32, the average value of the multiple inlet temperatures T1 recorded in the historical time period may be used as the second outlet temperature T12, and the average value of the multiple reaction system temperatures T2 recorded in the historical time period may be used as the second outlet temperature T22. Wherein, the fourth preset duration may be less than or equal to the third preset duration. As a possible implementation, the third preset duration and the fourth preset duration may both be equal to the first preset duration, both being X0s.
[0073] When the second outlet temperature T32, the second inlet temperature T12, and the second reaction system temperature T22 are determined, it can be determined whether the temperature of the reaction system is restored to the temperature before the liquid is added dropwise according to the first outlet temperature T31, the first inlet temperature T11, the first reaction system temperature T21, the second outlet temperature T32, the second inlet temperature T12, and the second reaction system temperature T22. If not, continue to record and judge the temperature until it is determined that the temperature of the reaction system is restored to the temperature before the liquid is added dropwise. When it is determined that the temperature of the reaction system is restored to the temperature before the liquid is added dropwise, the reaction heat can be calculated based on the recorded temperature data.
[0074] Wherein, whether the temperature of the reaction system is restored to the temperature before the liquid is added can be judged in the following manner: Judge whether the first outlet temperature T31, the first inlet temperature T11, the first reaction system temperature T21, the second outlet temperature T32, the second inlet temperature T12, and the second reaction system temperature T22 meet the following conditions: , , If the condition is satisfied, it is determined that the temperature of the reaction system has recovered to the temperature before the liquid was added dropwise. If the condition is not satisfied, it is determined that the temperature of the reaction system has not recovered to the temperature before the liquid was added dropwise. represents the second preset value, represents the third preset value, represents the fourth preset value, , , It can be set smaller, and the specific size can be set according to the actual experimental situation.
[0075] When it is determined that the temperature of the reaction system has returned to the temperature before the liquid is added, the temperature data can be stopped from being recorded, and the heat released by the reaction can be calculated based on the heat added to the reaction system during the process from the addition of liquid to the determination that the temperature has returned to the temperature before the liquid is added, the heat taken away by the flowing medium of the reactor, and the heat exchange amount between the reactor and the air. Among them, the heat added to the reaction system during the process can be calculated based on the temperature T2 of the reaction system recorded during the process from the addition of liquid to the determination that the temperature has returned to the temperature before the liquid is added, and the heat taken away by the flowing medium of the reactor can be calculated based on the outlet temperature T3 and the inlet temperature T1 recorded during the process; the room temperature T4 can also be recorded during the above process, and the heat exchange amount between the reactor and the air can be calculated based on the outlet temperature T3, the inlet temperature T1 and the room temperature T4 recorded during the process.
[0076] Optionally, the reaction exotherm can be calculated by the following formula:
[0077] Among them, Q1 represents the heat released by the reaction, represents the specific heat capacity of the reaction solution (i.e., the specific heat capacity of the reaction system in the reaction axe); m represents the mass of the reaction solution, which can be the mass of the reaction solution before the liquid is added dropwise, the mass of the reaction solution after the addition is completed, or the average mass of the reaction solution before and after the addition of the liquid is completed; Indicates the temperature change of the reaction solution, which is the value of the reaction system temperature T2 at the end of recording minus the reaction system temperature T2 at the start of dropwise addition; Indicates the specific heat capacity of the heat transfer medium in the high and low temperature all-in-one machine; Indicates the outlet mass flow rate of the reactor; It indicates the inlet temperature data of the reactor during the process from the start of dropwise addition to the end of temperature data recording; It indicates the outlet temperature data of the reactor from the beginning of the dropwise addition to the end of the temperature data recording process; represents the convection heat transfer coefficient (W / m²·K); represents the room temperature data from the start of the dripping to the end of the temperature data recording process. That is, , , , represents the inlet temperature and outlet temperature of the reactor, as well as the room temperature, from the start of liquid dropwise addition to the determination of the temperature returning to the temperature before liquid dropwise addition.
[0078] When the reaction exotherm is obtained, the temperature change value of the first reaction system can be calculated based on the reaction exotherm, the heat taken away by the flowing medium of the reactor during the process of dripping the liquid for the second preset time, and the heat exchange amount between the reactor and the air without considering the reaction exotherm delay. The process can be expressed by the following formula: , , in the above formula , represents the temperature data from the start of liquid dripping to the completion of liquid dripping, that is, the temperature data from the start of dripping to the second preset time period, and X0~X0+X1 represents the time period from the start of dripping to the second preset time period; Represents the temperature change value of the first reaction system.
[0079] Sub-step S212, in the formal experimental stage, continuously judges whether the temperature control capability corresponding to the temperature change situation represented by the current high and low temperature integrated machine and the first reaction system temperature change value is greater than or equal to the absolute value of the first reaction system temperature change value, and determines the first weight and the second weight based on the judgment result.
[0080] In this embodiment, it can be determined whether the temperature change corresponding to the temperature change value of the first reaction system is heating up or cooling down, that is, whether the reaction after the liquid is added is exothermic. Then, the temperature control capability of the current high and low temperature integrated machine corresponding to the temperature change is obtained, and it is determined whether the temperature control capability is greater than or equal to the absolute value of the temperature change value of the first reaction system, and then the specific values of the first weight and the second weight are determined according to the obtained judgment result. Among them, the temperature control capability is expressed in temperature.
[0081] In this embodiment, if the high and low temperature integrated machine is heating, the heating power of the high and low temperature integrated machine at this time is greater than 0; if the high and low temperature integrated machine is cooling, the heating power of the high and low temperature integrated machine at this time is less than 0. The temperature control capacity of the high and low temperature integrated machine includes the cooling capacity and heating capacity obtained based on the first heating power P0, and the cooling capacity and heating capacity are both represented by numbers greater than or equal to 0, which can be expressed by Figure 7 The current first weight and second weight are obtained in the manner shown. Figure 7 , Figure 7 for Figure 5 Schematic diagram of the flow of sub-steps included in sub-step S212. In this embodiment, sub-step S212 may include sub-steps S2121 to S2126.
[0082] Sub-step S2121, determining whether the reaction occurring after the liquid is added is exothermic based on the exothermic amount of the reaction.
[0083] If heat release is determined, sub-step S2122 is executed.
[0084] Sub-step S2122, obtaining the current refrigeration capacity of the high and low temperature integrated machine as the corresponding temperature control capacity.
[0085] If it is determined that no heat is released, sub-step S2123 is executed.
[0086] Sub-step S2123, obtaining the current heating capacity of the high and low temperature integrated machine as the corresponding temperature control capacity.
[0087] Sub-step S2124, determining whether the corresponding temperature control capability is greater than or equal to the absolute value of the temperature change value of the first reaction system.
[0088] If the corresponding temperature control capability is greater than or equal to the temperature change value of the first reaction system , execute sub-step S2125.
[0089] Sub-step S2125, determining that the first weight is 1 and the second weight is 0.
[0090] If the corresponding temperature control capability is smaller than the absolute value of the temperature change of the first reaction system, sub-step S2126 is executed.
[0091] Sub-step S2126, determining that the first weight is 1, and calculating the second weight according to the first weight, the absolute value of the temperature change value of the first reaction system and the corresponding temperature control capability.
[0092] The second weight is a value obtained by subtracting a quotient from 1, and the quotient is a result obtained by dividing the temperature control capability by an absolute value of the temperature change of the first reaction system.
[0093] In this embodiment, it can be determined whether the reaction heat release is greater than 0. If the reaction heat release is greater than 0, the reaction is determined to be an exothermic reaction; if the reaction heat release is less than 0, the reaction is determined to be an endothermic reaction.
[0094] When the reaction is determined to be an exothermic reaction, the current refrigeration capacity of the high and low temperature integrated machine can be obtained in the following manner. In the pre-processing stage, after obtaining the exothermic amount of the reaction, the high and low temperature integrated machine can be controlled to reduce and maintain the heating power from the first heating power P0, wherein the reduced power amount is the first adjustment amount , the first adjustment amount Greater than 0. Maintain the second heating power in the high and low temperature integrated machine After working for a second preset time, obtaining a second reaction system temperature change value of the reaction system after the second preset time , the temperature change value of the second reaction system Maintain the heating power for the high and low temperature all-in-one machine The result of subtracting the temperature of the reaction system before the second preset time from the temperature of the reaction system after the second preset time. And the maximum cooling power P2 of the high and low temperature integrated machine can be obtained, wherein the maximum cooling power P2 may be 0 or a value greater than 0, which is determined by the actual situation.
[0095] Finally, the third outlet temperature, the third inlet temperature and the third reaction system temperature of the reaction kettle before the heating power is reduced in the pre-treatment stage, the fourth outlet temperature and the fourth inlet temperature of the current reaction kettle, the fourth reaction system temperature of the current reaction system, the first heating power P0, and the second reaction system temperature change value can be used to control the temperature of the reaction kettle to reduce the heating power. , the first adjustment amount and the maximum cooling power P2, calculate the current cooling capacity. The process can be expressed by the following formula: ,in, T represents the inlet temperature of the reactor when the heating power is the first heating power P0, T3 represents the outlet temperature of the reactor when the heating power is the first heating power P0, Indicates the inlet temperature of the current reactor during the formal experiment. Indicates the outlet temperature of the current reactor during the formal experiment. Indicates the current room temperature during the formal experiment.
[0096] When the current refrigeration capacity is obtained, it is determined whether the current refrigeration capacity is greater than the absolute value of the temperature change value of the first reaction system, that is, it is determined Is it established? If the refrigeration capacity is greater than or equal to the absolute value of the temperature change of the first reaction system, the first weight is determined to be 1 and the second weight is determined to be 0. At this time, the first control value and the second control value can be calculated according to the following formula:
[0097]
[0098]
[0099] in, represents the first control value, that is, the control output of the high and low temperature integrated machine; represents the first weight; Indicates the proportional coefficient corresponding to the high and low temperature integrated machine, Indicates the integral coefficient corresponding to the high and low temperature integrated machine, Indicates the differential coefficient corresponding to the high and low temperature integrated machine, It represents the result of subtracting the target value from the actual value of the reaction system temperature; represents the second control value, i.e., the control output of the liquid drop acceleration control device; represents the second weight; Indicates the proportional coefficient corresponding to the liquid drop acceleration control device, Indicates the integral coefficient corresponding to the liquid drop acceleration control device, Indicates the differential coefficient corresponding to the liquid drop acceleration control device.
[0100] like If it is not true, then the first weight is determined to be 1, the second weight is determined to be 1 minus a quotient value, and the quotient value is the result of dividing the temperature control capability by the absolute value of the temperature change value of the first reaction system. That is, at this time: , .
[0101] It is worth noting that the first control value may be a value that can be achieved by the high and low temperature integrated machine, or it may be a value that cannot be achieved by the high and low temperature integrated machine. When the first control value is a value that cannot be achieved by the high and low temperature integrated machine, the control value actually executed by the high and low temperature integrated machine is the value closest to the first control value within the capacity of the high and low temperature equipment. For example, assuming that the value calculated for the high and low temperature integrated machine is It means reducing the power by 500W, while the high and low temperature integrated machine can only reduce 300W at most. Due to the insufficient capacity of the high and low temperature integrated machine, after controlling the high and low temperature integrated machine based on the first control value 1*500, the actual high and low temperature integrated machine is only reduced by 300W; the rest is achieved by adjusting the dripping speed.
[0102] Similarly, when the reaction is determined to be an exothermic reaction, the current heating capacity of the high and low temperature integrated machine can be measured in the following manner. In the pre-processing stage, after obtaining the exothermic amount of the reaction, the high and low temperature integrated machine can be controlled to increase and maintain the heating power from the first heating power P0, wherein the increased power amount is the second adjustment amount , the second adjustment amount Greater than 0. Maintain the third heating power in the high and low temperature integrated machine After working for a second preset time, obtaining a third reaction system temperature change value of the reaction system after the second preset time , the temperature change value of the third reaction system Maintain the heating power for the high and low temperature all-in-one machine The result of subtracting the temperature of the reaction system before the second preset time from the temperature of the reaction system after the second preset time. And the maximum heating power P3 of the high and low temperature integrated machine can be obtained, wherein the maximum heating power P3 may be 0 or a value greater than 0, which is determined by the actual situation.
[0103] Finally, the third outlet temperature, the third inlet temperature and the third reaction system temperature of the reaction kettle before the heating power is increased in the pre-treatment stage, the fourth outlet temperature and the fourth inlet temperature of the current reaction kettle, the fourth reaction system temperature of the current reaction system, the first heating power P0, the third reaction system temperature change value, and the third reaction system temperature of the reaction kettle can be controlled to increase the heating power in the pre-treatment stage. , the second adjustment amount and the maximum heating power P3, calculate the current heating capacity, and the process can be expressed by the following formula: ,in, T represents the inlet temperature of the reactor when the heating power is the first heating power P0, T3 represents the outlet temperature of the reactor when the heating power is the first heating power P0, Indicates the inlet temperature of the current reactor during the formal experiment. Indicates the outlet temperature of the current reactor during the formal experiment. Indicates the current room temperature during the formal experiment.
[0104] When the current heating capacity is obtained, it is determined whether the current heating capacity is greater than or equal to the absolute value of the temperature change value of the first reaction system, that is, it is determined Is it established? If the heating capacity is greater than or equal to the absolute value of the temperature change value of the first reaction system, the first weight is determined to be 1 and the second weight is determined to be 0. At this time, the first control value and the second control value can be calculated according to the following formula:
[0105] , .
[0106] like If it is not true, then the first weight is determined to be 1, the second weight is determined to be 1 minus a quotient value, and the quotient value is the result of dividing the temperature control capability by the absolute value of the temperature change value of the first reaction system. That is, at this time: , .
[0107] It is worth noting that in the above process, the pre-processing stage is located before the formal experimental stage, and the steps in the pre-processing stage only need to be performed once before the formal experimental stage, that is, the following processing is only performed once before the formal experimental stage: an exothermic test is performed to obtain the heat release of the reaction, and the temperature change value of the first reaction system is calculated based on the heat release of the reaction, and whether the reaction occurring after the liquid is added is determined based on the heat release of the reaction. If it is exothermic, the corresponding second reaction system temperature change value and maximum cooling power are obtained, and if it is endothermic, the corresponding third reaction system temperature change value and maximum heating power are obtained. In the formal experimental stage, multiple controls need to be performed, and each control needs to calculate the current weight of the controlled device to be controlled by combining the second reaction system temperature change value and maximum cooling power obtained in the pre-processing stage, or the third reaction system temperature change value and maximum heating power, and then calculate the control value corresponding to the controlled device based on the calculated weight, and finally control based on the calculated control value. That is, in the formal experimental stage, it is necessary to repeatedly calculate the weight and control value, and control based on the control value.
[0108] Please refer to Figure 8 , Figure 8 The second flow chart of the device experiment parameter control method provided in the embodiment of the present application. In this embodiment, the method may further include step S300.
[0109] Step S300, judging whether the preset conditions are met according to the currently detected data, if so, controlling the corresponding controlled device according to the preset device experimental parameters corresponding to the preset conditions, and recording to obtain the whole process experimental data.
[0110] In this embodiment, the parameters to be controlled can be input, that is, the preset equipment experimental parameters are set, and the trigger conditions (i.e., preset conditions) are set. When the trigger conditions are met, the control of the parameters can be triggered. For example, when the solution changes from colorless to yellow, the high and low temperature integrated machine is turned off; when the time reaches a certain value, stirring is turned on, etc. Data is recorded at the same time. In this way, the control can be completed through the above-mentioned single parameter control method, and the whole process experimental data can be obtained.
[0111] The R&D personnel can add the experimental materials to the reaction container and add the liquid to be added to the drop container. The R&D personnel can also enter the experimental instructions, which include the above-mentioned preset conditions and the corresponding preset equipment experimental parameters, and the experimental instructions indicate the control logic. For example, the R&D personnel entered the temperature control logic of the high and low temperature integrated machine, in which the temperature, time or other conditions that can trigger the temperature change (such as solution discoloration, etc.) can be set. If the conditions are met, the working temperature of the high and low temperature integrated machine will change. For example, after the temperature stabilizes at 25°C for 5 minutes, the temperature is raised to 35°C. For another example, the R&D personnel entered the speed control logic of the stirrer, in which the speed, time or other conditions that can trigger the speed change (such as solution discoloration, high and low temperature start and stop, delay, etc.) can be set. If the conditions are met, the speed of the stirrer will change. For another example, the R&D personnel entered the adjustment logic of the liquid drop speed control device, in which the drop speed, time, drop temperature, pH range and other conditions can be set. If the conditions are met, the liquid drop speed of the liquid drop speed control device will be changed.
[0112] As a possible implementation, Fig. 9 As shown, the chemical reaction system may include a parameter control device 100, a high and low temperature integrated machine 210, a liquid drop acceleration control device 220, an agitator 230, a liquid container 240, a liquid pipeline 250, a reaction container 260, a thermometer 270, and a camera 280. The parameter control device 100 is in communication connection with the high and low temperature integrated machine 210, the liquid drop acceleration control device 220, the agitator 230, the thermometer 270, and the camera 280 for collecting data and performing control.
[0113] The high and low temperature integrated machine 210 is used to control the temperature of the reaction. The liquid droplet acceleration control device 220 may include a pump and / or a valve to control the speed of liquid droplet addition. The liquid container 240 is used to contain the liquid required for the liquid, and the material used for the liquid container 240 includes, but is not limited to, glass / polytetrafluoroethylene. The reaction container 260 is used to contain the reaction solution. The liquid pipeline 250 is used to connect the liquid container 240 with the liquid droplet acceleration control device 220 and the reaction container 260, so that the liquid in the liquid container 240 can be dripped into the reaction container 260 through the liquid droplet acceleration control device 220. The thermometer 270 is used to measure the temperature of the reaction solution in the reaction container 260. The camera 280 is used to collect video to monitor the reaction changes through video.
[0114] Combine the following Fig. 9 , the above single parameter control method is illustrated by examples.
[0115] S1. The parameter control device automatically turns on the high and low temperature integrated machine and automatically sets it to -10°C. The high and low temperature integrated machine controls the temperature of the reaction solution according to -10°C; the stirrer is automatically turned on and automatically set to 300rpm.
[0116] S2. After the parameter control device determines that the temperature of the reaction system has reached the set temperature, the rotation speed is adjusted to 500 rpm and the dropwise addition of the liquid material is started.
[0117] S3. The parameter control device controls the liquid dripping speed control device to automatically start dripping the liquid material, and automatically adjusts the dripping rate according to the detected pH (pH of the reaction solution) to ensure the pH range. The parameter control device determines whether the dripping is completed. If it is determined to be completed, the liquid dripping speed control device is controlled to stop dripping liquid. Optionally, the parameter control device can determine whether the dripping is completed based on whether the total dripping amount reaches a preset total amount, or whether the dripping time reaches a preset time.
[0118] S4. After the dripping is completed, the parameter control device automatically raises the temperature of the high and low temperature integrated machine to 40°C.
[0119] S5. After the reaction continues for 6 hours, solid precipitates. If the parameter control device determines through the video collected by the camera that the reaction liquid changes from red to yellow, and the color change is consistent with the setting, the high and low temperature integrated machine is turned off, and the agitator is turned off when the temperature drops to 30°C.
[0120] S6. Export the automatically stored experimental data of the whole process, including the temperature of the high and low temperature integrated machine (the temperature of the outlet thermometer), the temperature inside the system, the pH value, the stirring speed, the color change, etc.
[0121] The entire experimental process described in steps S1-S6 takes 10 to 12 hours. The experimenter needs to set the parameters and remotely confirm the execution results after get off work.
[0122] In this embodiment, intelligent control is used for parameter regulation in the experiment, various parameters in the chemical reaction process are collected, and the control parameters are automatically calculated. Compared with the manual logic judgment control by R&D personnel or the existing single parameter control equipment (such as potentiometric titrator, etc.), it greatly reduces the large amount of time occupied by R&D personnel, greatly reduces the difficulty of multi-parameter adjustment, and improves the reaction success rate.
[0123] In order to execute the corresponding steps in the above embodiments and various possible methods, a method for implementing the device experiment parameter control device 300 is given below. Optionally, the device experiment parameter control device 300 can adopt the above Figure 1 The device structure of the parameter control device 100 is shown. Fig.10 , Fig.10The block diagram of the device experiment parameter control device 300 provided in the embodiment of the present application. It should be noted that the basic principle and technical effect of the device experiment parameter control device 300 provided in this embodiment are the same as those of the above embodiment. For the sake of brief description, for the parts not mentioned in this embodiment, reference can be made to the corresponding contents in the above embodiment. In this embodiment, the device experiment parameter control device 300 may include: an information acquisition module 310 and a control module 320.
[0124] The information obtaining module 310 is used to determine a target value of a reaction system target parameter that the reaction system needs to maintain when adjusting a first device experimental parameter of the first device.
[0125] The control module 320 is used to maintain the target parameter of the reaction system at the target value, continuously calculate the first control value of the first device experimental parameter of the first device and the second control value of the second device experimental parameter of at least one second device according to the current value of the target parameter of the reaction system and the target value, and control the corresponding device according to the calculated control value. The working states of the first device and at least one second device among the multiple controlled devices both affect the target parameter of the reaction system.
[0126] Optionally, the above modules can be stored in the form of software or firmware. Figure 1 The memory 110 shown in FIG. 100 may be fixed in the operating system (OS) of the parameter control device 100 and may be used by Figure 1 Meanwhile, the data and program codes required for executing the above modules may be stored in the memory 110.
[0127] An embodiment of the present application also provides a readable storage medium on which a computer program is stored. When the computer program is executed by a processor, the device experimental parameter control method is implemented.
[0128] In summary, the embodiment of the present application provides a method, device, electronic device and readable storage medium for controlling equipment experiment parameters, wherein the parameter control device is connected to multiple controlled equipment for communication, and the parameter control device determines the target value of the reaction system target parameter that the reaction system needs to maintain when adjusting the first equipment experiment parameter of the first equipment, and then takes the reaction system target parameter as the target value, and continuously calculates the first control value of the first equipment experiment parameter of the first equipment and the second control value of the second equipment experiment parameter of at least one second equipment according to the current value and the target value of the reaction system target parameter, and controls the corresponding equipment according to the calculated control value. Among them, the working states of the first equipment and at least one second equipment in the multiple controlled equipment all affect the reaction system target parameter. In this way, when adjusting a single equipment experiment parameter causes the value of the reaction system target parameter to change, but it is not desired that the value of the reaction system target parameter deviates from the target value by a large amount, the value of the reaction system target parameter can be maintained near the target value by controlling the equipment experiment parameters of multiple equipment that have an impact on the reaction system target parameter.
[0129] In several embodiments provided in the present application, it should be understood that the disclosed devices and methods can also be implemented in other ways. The device embodiments described above are merely schematic. For example, the flowcharts and block diagrams in the accompanying drawings show the possible architecture, functions and operations of the devices, methods and computer program products according to multiple embodiments of the present application. In this regard, each box in the flowchart or block diagram can represent a module, a program segment or a part of a code, and the module, a program segment or a part of a code contains one or more executable instructions for implementing the specified logical function. It should also be noted that in some alternative implementations, the functions marked in the box can also occur in a different order from the order marked in the accompanying drawings. For example, two consecutive boxes can actually be executed substantially in parallel, and they can sometimes be executed in the opposite order, depending on the functions involved. It should also be noted that each box in the block diagram and / or flowchart, and the combination of boxes in the block diagram and / or flowchart can be implemented with a dedicated hardware-based system that performs a specified function or action, or can be implemented with a combination of dedicated hardware and computer instructions.
[0130] In addition, the functional modules in the various embodiments of the present application may be integrated together to form an independent part, or each module may exist separately, or two or more modules may be integrated to form an independent part.
[0131] If the function is implemented in the form of a software function module and sold or used as an independent product, it can be stored in a computer-readable storage medium. Based on this understanding, the technical solution of the present application can be essentially or partly embodied in the form of a software product that contributes to the prior art. The computer software product is stored in a storage medium and includes several instructions for a computer device (which can be a personal computer, server, or network device, etc.) to perform all or part of the steps of the method described in each embodiment of the present application. The aforementioned storage medium includes: U disk, mobile hard disk, read-only memory (ROM, Read-Only Memory), random access memory (RAM, Random Access Memory), disk or optical disk, and other media that can store program codes.
[0132] The above description is only an optional embodiment of the present application and is not intended to limit the present application. For those skilled in the art, the present application may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims
1. A method for controlling equipment experimental parameters, characterized in that: Applied to a parameter control device, the parameter control device is communicatively connected with a plurality of controlled devices, the method comprising: Determining a target value of a reaction system target parameter that the reaction system needs to maintain when adjusting a first device experimental parameter of the first device, wherein the reaction system target parameter is a reaction system temperature in a reactor, and the reaction system temperature represents a temperature of the reaction system in the reactor; With the goal of maintaining the target parameter of the reaction system at the target value, a first control value of a first device experimental parameter of the first device and a second control value of a second device experimental parameter of at least one second device are continuously calculated based on the current value of the target parameter of the reaction system and the target value, and the corresponding devices are controlled according to the calculated control values, wherein the working states of the first device and at least one second device among the multiple controlled devices both affect the target parameter of the reaction system, the first device is a high and low temperature integrated machine, and the at least one second device includes a liquid dripping acceleration control device.
2. The method according to claim 1, characterized in that The step of continuously calculating a first control value of a first device experimental parameter of the first device and a second control value of a second device experimental parameter of at least one second device according to a current value and the target value of the target parameter of the reaction system comprises: Calculate and obtain the first weight of the current high and low temperature integrated machine and the second weight of the liquid drip acceleration control device; The first control value is calculated based on the current value, the target value and the first weight, and the second control value is calculated based on the current value, the target value and the second weight, wherein the first control value is used to indicate the power adjustment amount of the high and low temperature integrated machine, and the second control value is used to indicate the speed adjustment amount of the liquid drip acceleration control device.
3. The method according to claim 2, characterized in that The calculation to obtain the first weight of the current high and low temperature integrated machine and the second weight of the liquid drop acceleration control device includes: In the pre-processing stage, the high and low temperature integrated machine is controlled to control the temperature of the reaction system according to the target value, and the current first heating power of the high and low temperature integrated machine is recorded and maintained until the temperature of the reaction system reaches the target value, and while maintaining the first heating power, the liquid dripping speed control device is controlled to drip liquid into the reaction system for a second preset time, and the reaction heat caused by the dripping of the liquid is obtained, and the first reaction system temperature change value corresponding to the reaction system is calculated according to the reaction heat; In the formal experimental stage, it is continuously judged whether the temperature control capability corresponding to the temperature change represented by the current high and low temperature integrated machine and the temperature change value of the first reaction system is greater than or equal to the absolute value of the temperature change value of the first reaction system, and the first weight and the second weight are determined according to the judgment result, wherein the temperature control capability is expressed in temperature.
4. The method according to claim 3, characterized in that The step of controlling the liquid droplet speed control device to drop liquid into the reaction system for a second preset time period and obtaining the reaction heat released by the droplet addition includes: When it is determined that the temperature of the reaction system reaches the target value, obtaining a first outlet temperature, a first inlet temperature of the reactor and a first reaction system temperature of the reaction system; Controlling the liquid dropping speed control device to drop liquid into the reaction system for the second preset time period according to a preset dropping speed to perform an exothermic test; According to the first outlet temperature, the first inlet temperature, the first reaction system temperature, the second outlet temperature of the reactor after the exothermic test, the second inlet temperature, and the second reaction system temperature of the reaction system, judging whether the temperature has returned to the temperature before the liquid was added dropwise; When it is determined that the temperature is restored to the temperature before liquid is added dropwise, the heat released by the reaction is calculated based on the heat added to the reaction system during the process from adding liquid to determining that the temperature is restored to the temperature before liquid is added dropwise, the heat taken away by the flowing medium of the reactor, and the heat exchange amount between the reactor and the air.
5. The method according to claim 4, characterized in that The step of calculating a first reaction system temperature change value corresponding to the reaction system according to the reaction heat release comprises: The temperature change value of the first reaction system is calculated based on the heat released by the reaction, the heat taken away by the flowing medium of the reactor during the process of dripping liquid for the second preset time, and the heat exchange amount between the reactor and the air.
6. The method according to claim 3, characterized in that: The temperature control capability of the high and low temperature integrated machine includes the cooling capability and the heating capability obtained based on the first heating power, and the continuously judging whether the temperature control capability corresponding to the temperature change situation represented by the current high and low temperature integrated machine and the first reaction system temperature change value is greater than or equal to the absolute value of the first reaction system temperature change value, and determining the first weight and the second weight according to the obtained judgment result, comprises: Determining whether the reaction occurring after the liquid is added is exothermic based on the exothermic heat of the reaction; If heat release is determined, the current refrigeration capacity of the high and low temperature integrated machine is obtained as the corresponding temperature control capacity; If it is determined that no heat is released, the current heating capacity of the high and low temperature integrated machine is obtained as the corresponding temperature control capacity; Determining whether the corresponding temperature control capability is greater than or equal to the absolute value of the temperature change value of the first reaction system; If it is greater than or equal to, determining that the first weight is 1 and the second weight is 0; If it is less than, the first weight is determined to be 1, and the second weight is calculated based on the first weight, the absolute value of the first reaction temperature change value and the corresponding temperature control capability, wherein the second weight is 1 minus the quotient, and the quotient is the temperature control capability divided by the absolute value of the first reaction system temperature change value.
7. The method according to claim 6, characterized in that The current cooling capacity is obtained as follows: In the pre-treatment stage, after obtaining the reaction heat release, controlling the high and low temperature integrated machine to reduce and maintain the heating power by the first heating power, and after waiting for the second preset time, obtaining the second reaction system temperature change value of the reaction system before and after the second preset time, wherein the reduced power amount is the first adjustment amount; The current refrigeration capacity is calculated according to the third outlet temperature and the third inlet temperature of the reactor and the third reaction system temperature of the reaction system before the heating power is controlled to be reduced in the pre-treatment stage, the fourth outlet temperature and the fourth inlet temperature of the reactor at present, the fourth reaction system temperature of the current reaction system, the first heating power, the second reaction system temperature change value, the first adjustment amount and the maximum refrigeration power of the high and low temperature integrated machine; The current heating capacity is obtained by: In the pre-treatment stage, after obtaining the reaction heat release, controlling the high and low temperature integrated machine to increase and maintain the heating power by the first heating power, and after waiting for the second preset time, obtaining a third reaction system temperature change value of the reaction system before and after the second preset time, wherein the increased power amount is the second adjustment amount; The current heating capacity is calculated based on the third outlet temperature, the third inlet temperature and the third reaction system temperature of the reactor before controlling to increase the heating power in the pre-treatment stage, the current fourth outlet temperature and the fourth inlet temperature of the reactor, the fourth reaction system temperature of the current reaction system, the first heating power, the third reaction system temperature change value, the second adjustment amount and the maximum heating power of the high and low temperature integrated machine.
8. The method according to any one of claims 1 to 7, characterized in that: The method further comprises: According to the currently detected data, it is determined whether the preset conditions are met. If so, the corresponding controlled device is controlled according to the preset device experimental parameters corresponding to the preset conditions, and the data is recorded to obtain the whole process experimental data.
9. A device for controlling equipment experimental parameters, characterized in that: Applied to a parameter control device, the parameter control device is communicatively connected with a plurality of controlled devices, the device comprises: an information acquisition module, used to determine a target value of a reaction system target parameter that the reaction system needs to maintain when adjusting a first device experimental parameter of the first device, wherein the reaction system target parameter is a reaction system temperature in a reactor, and the reaction system temperature represents a temperature of the reaction system in the reactor; A control module is used to maintain the target parameter of the reaction system at the target value, continuously calculate the first control value of the first device experimental parameter of the first device and the second control value of the second device experimental parameter of at least one second device according to the current value of the target parameter of the reaction system and the target value, and control the corresponding devices according to the calculated control values, wherein the working states of the first device and at least one second device among the multiple controlled devices both affect the target parameter of the reaction system, the first device is a high and low temperature integrated machine, and the at least one second device includes a liquid drip acceleration control device.
10. A parameter control device, characterized in that: It includes a processor and a memory, wherein the memory stores machine executable instructions that can be executed by the processor, and the processor can execute the machine executable instructions to implement the device experimental parameter control method described in any one of claims 1-8.
