Crystal solvent removal control method, system, low-solvent residual crystal, and electronic device

Abstract

The present application relates to the technical field of industrial control, and provides a crystal solvent removal control method, system, low-solvent-residual crystal and electronic equipment, wherein the method comprises the following steps: controlling temperature and / or pressure in a drying machine to fluctuate within a preset range; constructing a temperature interference model and / or a pressure interference model based on changes in solvent concentration caused by the fluctuation; and dynamically regulating the temperature and / or pressure in the drying machine based on the temperature interference model and / or the pressure interference model until the solvent removal process is completed. The present application is used to solve the defects in the prior art, such as waste of manpower, time and energy, and inability to ensure the stability of the crystal solvent removal process, caused by controlling parameters according to process index requirements, experience and actual exploration during the drying and desolventizing process.

Description

Technical Field

[0001] This invention relates to the field of low-solution-residue industrial control technology, and in particular to a crystal solvent removal control method, system, low-solution-residue crystal, and electronic equipment. Background Technology

[0002] Currently, solvent removal from crystals is generally achieved through vacuum drying, which involves drying and desolventizing a certain amount of crystals within a specific temperature and pressure range using a vacuum dryer for a certain period of time.

[0003] However, current control of parameters such as temperature, pressure, and drying time during the drying and solvent removal process of low-solvent-residue crystals mainly relies on the process requirements of low-solvent-residue crystals, experience, and practical exploration. Therefore, after the drying time is reached, offline sampling and testing are still needed to determine whether the solvent residue meets the process control standards. However, the actual crystal material entering the dryer, the heating temperature, and the pressure control are subject to fluctuations. Using the above parameter control methods cannot achieve real-time tracking and adjustment of parameters, which not only easily leads to waste of labor, time, and energy, but also results in poor stability of the crystal solvent removal process. Summary of the Invention

[0004] This invention provides a method, system, low-solvent-residue crystal, and electronic equipment for controlling the removal of crystal solvents, in order to solve the defects in the prior art, which is caused by wasting manpower, time, and energy by controlling parameters based on process indicators, experience, and practical exploration during the drying and solvent removal process, and which cannot guarantee the stability of the crystal solvent removal process.

[0005] This invention provides a method for controlling the removal of solvent from crystals, comprising:

[0006] Control the temperature and / or pressure inside the dryer to fluctuate within a preset range;

[0007] Based on the changes in solvent concentration caused by the fluctuations, a temperature disturbance model and / or a pressure disturbance model are constructed.

[0008] Based on the temperature disturbance model and / or the pressure disturbance model, the temperature and / or pressure inside the dryer are dynamically controlled until the solvent removal process is completed.

[0009] According to the crystal solvent removal control method of the present invention, before controlling the temperature and / or pressure fluctuation within the dryer to remain within a preset range, the method further includes:

[0010] The temperature and pressure inside the dryer are controlled to reach preset temperature and preset pressure, respectively, and the preset temperature and preset pressure meet the process parameter control temperature requirements and process parameter control pressure requirements of the crystal to be processed.

[0011] The control of temperature and / or pressure fluctuations within the dryer within a preset range includes:

[0012] The temperature inside the dryer is controlled to fluctuate within the temperature range corresponding to the process control temperature requirement, and / or the pressure inside the dryer is controlled to fluctuate within the pressure range corresponding to the process control pressure requirement.

[0013] According to the crystal solvent removal control method of the present invention, the step of constructing a temperature disturbance model and / or a pressure disturbance model based on the change in solvent concentration caused by the fluctuation includes:

[0014] Obtain the change in solvent concentration corresponding to each fluctuation and the temperature and / or pressure corresponding to the fluctuation;

[0015] Construct the temperature disturbance model and / or the pressure disturbance model.

[0016] According to the crystal solvent removal control method of the present invention, the step of dynamically regulating the temperature and / or pressure within the dryer based on the temperature disturbance model and / or the pressure disturbance model until the solvent removal process is completed includes:

[0017] Based on the temperature disturbance model and / or the pressure disturbance model, the temperature and / or pressure inside the dryer are adjusted to match the temperature and / or pressure in real time with the maximum value of the change in solvent concentration.

[0018] Determine the difference between the concentration change trends corresponding to two adjacent fluctuations;

[0019] When a predetermined number of consecutive differences are all less than or equal to a predetermined difference, the solvent removal process is determined to be over.

[0020] The present invention also provides a crystal solvent removal control system, comprising:

[0021] The temperature control module is used to adjust the temperature inside the dryer;

[0022] A pressure control module is used to adjust the pressure inside the dryer;

[0023] The control module is used to control the temperature and / or pressure inside the dryer to fluctuate within a preset range based on the temperature control module and / or the pressure control module; to construct a temperature disturbance model and / or a pressure disturbance model based on the change in solvent concentration caused by the fluctuation; and to dynamically regulate the temperature and / or pressure inside the dryer based on the temperature disturbance model and / or the pressure disturbance model until the solvent removal process ends.

[0024] According to the crystal solvent removal control system of the present invention, the temperature control module includes: a heating unit, a cooling unit, and a temperature detection unit;

[0025] The control module is also used to control the heating unit and the cooling unit to adjust the temperature inside the dryer based on the temperature detected by the temperature detection unit.

[0026] The crystal solvent removal control system according to the present invention further includes:

[0027] A solvent concentration change detection module is used to determine the concentration change trend of the gaseous solvent residue in the dryer corresponding to each fluctuation, and the concentration change trend is used to determine the amount of change in solvent concentration.

[0028] According to the crystal solvent removal control system of the present invention, the solvent concentration change detection module includes: a laser generating unit, a laser receiving unit, and a control unit;

[0029] The control module is also used to control the laser generating unit to emit a laser signal of a preset wavelength to the laser receiving unit before and after each fluctuation; to obtain the concentration change trend corresponding to each fluctuation as determined by the control unit based on the laser signal received by the laser receiving unit, and to determine the solvent concentration change trend corresponding to each fluctuation based on the concentration change trend and the temperature and / or pressure change trend corresponding to the fluctuation.

[0030] The present invention also provides a low-solution crystal obtained after solvent removal by the crystal solvent removal control method or the crystal solvent removal control system described above.

[0031] The present invention also provides an electronic device, including a memory, a processor, and a computer program stored in the memory and executable on the processor, wherein the processor executes the program to implement the steps of any of the crystal solvent removal control methods described above.

[0032] The present invention provides a method, system, low-solvent-residue crystal, and electronic equipment for controlling solvent removal from crystals. This method controls the temperature and / or pressure within a dryer to fluctuate within a preset range. Based on the changes in solvent concentration caused by these fluctuations, a temperature disturbance model and / or a pressure disturbance model are constructed. Based on these models, the temperature and / or pressure within the dryer are dynamically adjusted until the solvent removal process is complete. This achieves dynamic tracking and adjustment of temperature and / or pressure during the solvent removal process based on changes in solvent concentration, ensuring the dryer operates at its optimal state throughout the drying process. This not only achieves intelligent control of the crystal solvent removal process but also avoids waste of labor, time, and energy during solvent removal and effectively improves the stability of the solvent removal process for crystal products. Attached Figure Description

[0033] To more clearly illustrate the technical solutions in this invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this invention. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0034] Figure 1 This is a schematic flowchart of a crystal solvent removal control method provided in an embodiment of the present invention;

[0035] Figure 2 This is a schematic diagram of the rate of change of tomato red crystal perturbation response as temperature is finely adjusted according to an embodiment of the present invention;

[0036] Figure 3 This is a schematic diagram of a crystal solvent removal control system provided in an embodiment of the present invention;

[0037] Figure 4 This is a schematic diagram of an example of a crystal solvent removal control system provided by the present invention;

[0038] Figure 5 The present invention provides a basis for such Figure 4 The diagram shows the process of constructing a temperature disturbance model for the crystal solvent removal control system.

[0039] Figure 6 The present invention provides a basis for such Figure 4 The diagram shows a process flow chart for removing low-residual crystal solvents using a crystal solvent removal control system.

[0040] Figure 7 This is a schematic diagram of the structure of the electronic device provided by the present invention. Detailed Implementation

[0041] To make the objectives, technical solutions, and advantages of this invention clearer, the technical solutions of this invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of this invention. All other embodiments obtained by those skilled in the art based on the embodiments of this invention without creative effort are within the scope of protection of this invention.

[0042] The following is combined with Figures 1 to 7 The present invention describes a crystal solvent removal control method, system, low-solution-residue crystal, and electronic device.

[0043] This embodiment provides a method for controlling the removal of crystal solvents, which can be executed by software and / or hardware in electronic devices such as computers, tablets, and mobile phones. Figure 1 As shown, the crystal solvent removal control method provided in this embodiment includes at least the following steps:

[0044] 101. Control the temperature and / or pressure inside the dryer to fluctuate within a preset range.

[0045] It is understandable that changes in temperature or pressure inside the dryer will affect the solvent concentration.

[0046] In this embodiment, by controlling the temperature and / or pressure fluctuations within the dryer within a preset range, it is possible to achieve changes in solvent concentration based on temperature perturbation technology and / or pressure perturbation technology, thereby obtaining changes in solvent removal rate under different temperature or pressure fluctuations.

[0047] It should be noted that the preset temperature and pressure ranges are both less than or equal to the temperature and pressure ranges required by the process parameters for low-solution-residue crystals in the current dryer, in order to ensure the quality of low-solution-residue crystals during the solvent removal process.

[0048] Furthermore, the range of single fluctuations in temperature and / or pressure can be controlled by preset ranges, for example, setting the temperature fluctuation range to between 2℃ and 5℃, and the pressure fluctuation range to between 0.005MPa and 0.050MPa.

[0049] 102. Based on the changes in solvent concentration caused by fluctuations, construct temperature disturbance models and / or pressure disturbance models.

[0050] Figure 2 The rate of change in the tomato red crystal perturbation response is obtained by fine-tuning the temperature inside the dryer and determining the change in solvent concentration. Figure 2It is evident that when the temperature inside the dryer is fine-tuned, the solvent removal rate of the crystals to be treated also fluctuates, and the fluctuation gradually slows down and tends to remain constant as the solvent content decreases. Similarly, the same phenomenon occurs when the pressure inside the dryer is fine-tuned. Therefore, not only can the effect of temperature and / or pressure changes on solvent concentration changes be determined by controlling the fluctuation of temperature and / or pressure inside the dryer within a preset range, but it is also possible to determine whether the solvent removal process has ended.

[0051] In this embodiment, the amount of change in solvent concentration caused by each fluctuation will be different. By collecting data on the change in solvent concentration caused by each fluctuation and the corresponding temperature or pressure of the specific fluctuation, the influence of temperature and pressure changes on the amount of change in solvent concentration can be determined, that is, temperature disturbance model and pressure disturbance model can be constructed.

[0052] In one specific embodiment, the pressure value inside the dryer is fine-tuned, and then the trend of the concentration of gaseous residual solvent inside the dryer before and after the pressure change is detected. Then, based on the trend of the concentration of gaseous residual solvent and the trend of the pressure value of this fine-tuning, the solvent concentration 1 in the negative pressure environment is calculated.

[0053] Similarly, by fine-tuning the temperature inside the dryer and then detecting the trend of the concentration of gaseous solvent residue inside the dryer before and after the temperature change, the solvent concentration 2 in the negative pressure environment can be calculated based on the trend of the concentration of gaseous solvent residue and the trend of the temperature value during the fine-tuning.

[0054] In one specific embodiment, based on solvent concentration 1 and solvent concentration 2 in a negative pressure environment, a pressure disturbance model and a temperature disturbance model are modeled respectively using Ansys software through a neural network learning algorithm.

[0055] 103. Based on the temperature disturbance model and / or pressure disturbance model, dynamically regulate the temperature and / or pressure inside the dryer until the solvent removal process is completed.

[0056] In this embodiment, after obtaining the temperature disturbance model and / or pressure disturbance model, the temperature and / or pressure that make the dryer work in the optimal state can be determined in real time based on the temperature disturbance model and / or pressure disturbance model, thereby improving the stability of the solvent removal process of low residual crystals and reducing drying time and energy consumption.

[0057] The crystal solvent removal control method provided in the above embodiments of the present invention utilizes perturbation technology to detect changes in solvent concentration in real time during the drying process, establishing temperature disturbance models and / or pressure disturbance models to dynamically adjust the heating temperature and vacuum pressure within the dryer. This ensures that the dryer remains in optimal condition throughout the entire solvent removal process. Furthermore, it features rapid, efficient, and environmentally friendly operation, and can be applied to various types of low-solution-residue crystals, further improving the stability of the low-solution-residue crystal removal process.

[0058] Based on the above embodiments, before controlling the temperature and / or pressure inside the dryer to fluctuate within a preset range, the method further includes:

[0059] The temperature and pressure inside the dryer are controlled to reach the preset temperature and preset pressure, respectively, and the preset temperature and preset pressure meet the process parameter control temperature requirements and process parameter control pressure requirements of the crystal to be processed.

[0060] Controlling the temperature and / or pressure within the dryer to fluctuate within a preset range includes:

[0061] The temperature inside the dryer is controlled to fluctuate within the temperature range corresponding to the process control temperature requirements, and / or the pressure inside the dryer is controlled to fluctuate within the pressure range corresponding to the process control pressure requirements.

[0062] It is understandable that crystals themselves have boiling points, and organic reagents used to remove solvent residues also have boiling points. Therefore, in order to ensure the stability of the solvent removal process, temperature control requirements and pressure control requirements should be set in the process parameters for each type of crystal.

[0063] Based on this, in this embodiment, the temperature and / or pressure inside the dryer are controlled to fluctuate within the range corresponding to the process parameter control temperature requirements and / or pressure requirements of the crystal to be processed, that is, the preset range is the temperature range corresponding to the process parameter control temperature requirements and the pressure range corresponding to the process parameter control pressure requirements of the crystal to be processed.

[0064] Furthermore, in order to remove solvent residue, the temperature and pressure inside the dryer should at least meet the temperature control requirements and pressure control requirements of the crystals to be treated.

[0065] In this embodiment, before the temperature and / or pressure within the dryer fluctuate within a preset range, the temperature and pressure within the dryer are controlled to meet the preset temperature and pressure requirements of the process parameters for the crystal to be treated. For example, if the process parameter control temperature and pressure requirements for the crystal to be treated are 60℃-65℃ and -0.085MPa--0.075MPa respectively, the preset temperature and pressure can be 62℃ and -0.070MPa respectively. This ensures that the crystal to be treated is first placed in an environment suitable for solvent removal, and then the temperature and / or pressure of this environment are fine-tuned. Based on the different changes in solvent concentration under different temperature and / or pressure variations, the most suitable temperature and pressure for solvent removal of the crystal to be treated are determined in real time. This ensures the stability of the solvent removal process, improves solvent removal efficiency, and reduces energy consumption.

[0066] Based on the above embodiments, and based on the changes in solvent concentration caused by fluctuations, a temperature disturbance model and / or a pressure disturbance model are constructed, including:

[0067] Obtain the change in solvent concentration corresponding to each fluctuation and the temperature and / or pressure corresponding to the fluctuation;

[0068] Construct temperature disturbance models and / or pressure disturbance models.

[0069] In this embodiment, during the solvent removal process, each fluctuation in temperature and / or pressure within the dryer exhibits a trend. For example, when the temperature is adjusted from 62°C to 64°C, the temperature rise and rate of change can be determined, thus obtaining the trend of temperature fluctuation. After the temperature changes from 62°C to 64°C, the residual solvent concentration within the dryer also changes due to the temperature change. Therefore, the trend of residual solvent concentration change corresponding to the temperature fluctuation can be determined. By analyzing the trend of temperature fluctuation and the corresponding trend of residual solvent concentration change, the amount of change in solvent concentration corresponding to that temperature fluctuation can be determined.

[0070] In one specific embodiment, by acquiring the output signals corresponding to the tunable diode laser generator before and after the temperature and / or pressure fluctuations, the trend of the residual solvent concentration change corresponding to the current fluctuation is calculated. From a mathematical point of view, this means determining the slope of the residual solvent concentration change. Therefore, by combining the slope of the fluctuation change, the change in solvent concentration corresponding to the current fluctuation can be calculated.

[0071] Based on the above embodiments, and based on temperature disturbance models and / or pressure disturbance models, the temperature and / or pressure within the dryer are dynamically controlled until the solvent removal process is completed, including:

[0072] Based on temperature disturbance models and / or pressure disturbance models, adjust the temperature and / or pressure inside the dryer to match the temperature and / or pressure in real time with the maximum value of the change in solvent concentration.

[0073] Determine the difference in concentration change trends between two adjacent fluctuations;

[0074] The solvent removal process is considered complete when a preset number of consecutive differences are all less than or equal to a preset difference.

[0075] In this embodiment, the temperature disturbance model and the pressure disturbance model can characterize the impact of dynamic control of temperature and pressure inside the dryer on the change in solvent concentration. Therefore, the temperature and pressure most favorable for improving solvent removal efficiency can be obtained through the temperature disturbance model and the pressure disturbance model, respectively. That is, based on the temperature disturbance model and / or the pressure disturbance model, the temperature and / or pressure inside the dryer can be adjusted to match the temperature and / or pressure corresponding to the maximum value of the change in solvent concentration, thereby improving solvent removal efficiency and avoiding energy waste.

[0076] In this embodiment, as Figure 2 As shown, with the continuous progress of the solvent removal process, the concentration of residual solvent in the dryer gradually decreases. Therefore, the change in residual solvent concentration caused by fluctuations will tend to slow down and gradually reach a stable level. Based on this, by setting a preset difference amount, the difference between the concentration change trends corresponding to two adjacent fluctuations is determined, that is, the difference between the slopes of the two concentration change trends. Whether this difference is less than or equal to the preset difference amount is checked. When a preset number of differences less than or equal to the preset difference amount occur, it can be indicated that the change in residual solvent concentration has tended to or has reached a stable level, thus confirming the end of the solvent removal process. This achieves automatic judgment of whether the solvent removal process has ended, and stops temperature and / or pressure disturbances after determining that the solvent removal process has ended, thereby further improving the intelligence level of the solvent removal process control.

[0077] The practicality and technical effectiveness of the crystal solvent removal control method provided in the above embodiments of the present invention will be verified by applying it to the actual crystal solvent removal process.

[0078] Example 1: Solvent removal from tomato red crystals.

[0079] The main component of the tomato red crystal residue is ethanol. The process requires temperature control at 60℃-65℃ and pressure control at -0.085MPa--0.075MPa, with product residue <50ppm.

[0080] 1. The solvent removal process for tomato red crystals requires temperature control at 60℃-65℃, and the temperature inside the dryer should be controlled at 61℃.

[0081] 2. Add 20 kg of low-solubility residual crystals to the feed port of the dryer, open the feed valve, and feed the crystals. Purge with nitrogen and check that the oxygen content is within acceptable limits (e.g., oxygen content < 3%). Then, open the filter heating valve to preheat the filter for the required preheating time (e.g., 30 minutes). Next, start the vacuum pump to create a vacuum in the dryer. Wait until the vacuum level inside the dryer reaches the pressure required for processing tomato red crystals (e.g., -0.080 MPa).

[0082] 3. Start the dryer and begin the solvent removal process.

[0083] 4. Adjust the temperature to fluctuate between 60℃ and 65℃, record the changes in ethanol concentration with vacuum fluctuations, and establish a temperature interference model. Control the temperature during solvent removal based on the established temperature interference model. After the solvent removal process is complete, cool the dryer. When the material inside the dryer cools to the preset temperature (e.g., 40℃), close the vacuum valve and open the nitrogen valve to continue filling with nitrogen until the internal pressure is zero.

[0084] 5. Open the sampling port to take a sample and test the product. The test result showed a residual solvent concentration of 43 ppm, which is less than the requirement of <50 ppm for the tomato red crystal process. The product is qualified.

[0085] 6. Open the unloading port, take samples for testing, turn on the vacuum feeder, and pneumatically convey the material to the hopper. Then, package the material in the clean room discharge room.

[0086] Example 2: Solvent removal of lutein crystals

[0087] The main component of lutein crystals is n-hexane. The process requires temperature control at 62℃-70℃ and pressure control at -0.090MPa--0.082MPa, with product residue <50ppm.

[0088] 1. According to the solvent removal process requirements of lutein crystals, the temperature is controlled at 62℃-70℃, and the temperature inside the dryer is controlled at 67℃.

[0089] 2. Lift 20kg of low-solubility residual crystals to the feed port of the dryer, open the feed valve of the dryer, and feed the crystals. Purge with nitrogen, and after confirming the oxygen content is within acceptable limits (e.g., oxygen content < 3%), open the heating valve of the dryer filter to preheat the filter. After the preheating time is reached (e.g., 30 minutes), start the vacuum pump to begin creating a vacuum in the dryer. Wait until the vacuum level inside the dryer reaches the pressure required for the lutein crystal process (e.g., -0.085 MPa).

[0090] 3. Start the dryer and begin the solvent removal process.

[0091] 4. Adjust the temperature to fluctuate between 63.5℃ and 66.5℃, record the changes in the detected n-hexane concentration with vacuum fluctuations, and establish a temperature interference model.

[0092] 5. Adjust the vacuum level to fluctuate between -0.088MPa and 0.082MPa, record the changes in the detected n-hexane concentration with vacuum fluctuations, and establish a pressure disturbance model.

[0093] 6. Control the temperature and pressure during the solvent removal process based on the established temperature and pressure disturbance models. After the solvent removal process is completed, cool down the inside of the dryer. When the material inside the dryer cools down to the preset temperature (e.g., 40°C), close the vacuum valve and open the nitrogen valve to continue filling with nitrogen until the internal pressure is zero.

[0094] 7. Open the sampling port to take a sample and test the product. The test result showed a residual solvent concentration of 38 ppm, which is less than the requirement of <50 ppm for the residual solvent concentration in the lutein crystal process. The product is qualified.

[0095] 8. Open the unloading port, take samples for testing, turn on the vacuum feeder, and pneumatically convey the material to the hopper. Then, package the material in the clean room unloading room.

[0096] As can be seen from Examples 1 and 2 above, the crystal solvent removal control method provided by the embodiments of the present invention can accurately control and adjust the solvent removal process of different low-solution crystals, ensuring the stability of the solvent removal process, and is intelligent and environmentally friendly.

[0097] Based on the same general inventive concept, the present invention also provides a crystal solvent removal control system. The crystal solvent removal control system provided by the present invention will be described below, and the crystal solvent removal control system described below can be referred to in correspondence with the crystal solvent removal control method described above.

[0098] Figure 3 This is a schematic diagram of the crystal solvent removal control system provided by the present invention, as shown below. Figure 3 As shown, the system includes: a temperature control module 310, a pressure control module 320, and a control module 330; wherein,

[0099] Temperature control module 310 is used to adjust the temperature inside the dryer;

[0100] Pressure control module 320 is used to adjust the pressure inside the dryer;

[0101] The control module 330 is used to control the temperature and / or pressure inside the dryer to fluctuate within a preset range based on the temperature control module and / or pressure control module; to construct a temperature disturbance model and / or pressure disturbance model based on the change in solvent concentration caused by the fluctuation; and to dynamically regulate the temperature and / or pressure inside the dryer based on the temperature disturbance model and / or pressure disturbance model until the solvent removal process ends.

[0102] The crystal solvent removal control system provided in this invention controls the temperature and / or pressure within the dryer to fluctuate within a preset range. Based on the changes in solvent concentration caused by these fluctuations, a temperature disturbance model and / or pressure disturbance model are constructed. Based on these models, the temperature and / or pressure within the dryer are dynamically adjusted until the solvent removal process is complete. This achieves dynamic tracking and adjustment of temperature and / or pressure during the solvent removal process based on changes in solvent concentration, ensuring the dryer operates at its optimal state throughout the drying process. This not only achieves intelligent control of the crystal solvent removal process but also avoids waste of labor, time, and energy during solvent removal, effectively improving the stability of the solvent removal process for crystal products.

[0103] Based on the above embodiments, the temperature control module 310 includes: a heating unit, a cooling unit, and a temperature detection unit;

[0104] The control module 330 is also used to control the heating unit and cooling unit to adjust the temperature inside the dryer based on the temperature detected by the temperature detection unit.

[0105] In one specific embodiment, the heating unit can be a hot water tank for temperature regulation; the cooling unit can be a cold water tank for temperature regulation; and the temperature detection unit is a temperature sensor for real-time monitoring of the water temperature in both the hot and cold water tanks. Further, the water temperature in the hot water tank is controlled by steam via a regulating valve, and the target temperature of the hot water tank is 1-2°C higher than the preset drying temperature to ensure that the temperature inside the dryer reaches the preset temperature. The temperature of the cold water tank is regulated by controlling the switching valve and the frequency of the circulating water pump, thereby achieving precise temperature regulation according to process requirements.

[0106] Optionally, the pressure control module may include a vacuum pump for adjusting the pressure value within the dryer, a pressure detection unit for detecting the pressure value, and a control system that interacts with the control module. In one specific embodiment, the vacuum pump is a Roots vacuum pump, and the pressure detection unit is a pressure transmitter.

[0107] Optionally, the control module may include a signal acquisition unit, a signal control output unit, and a controller. In one specific embodiment, the signal acquisition unit is a signal acquisition circuit, the signal control output unit is a signal control output circuit, and the controller is an embedded MPU controller.

[0108] Based on the above embodiments, the crystal solvent removal control system further includes: a solvent concentration change detection module, used to determine the concentration change trend of the gas phase solvent residue in the dryer corresponding to each fluctuation, and the concentration change trend is used to determine the amount of change in solvent concentration.

[0109] In this embodiment, the solvent concentration change detection module can be any module that can determine the concentration change trend of gas phase residual solvent, such as an oscillation detection system including a resonant cavity, or a spectral detection system including a laser generator.

[0110] Based on the above embodiments, the solvent concentration change detection module includes: a laser generating unit, a laser receiving unit, and a control unit;

[0111] The control module is also used to control the laser generating unit to emit a laser signal of a preset wavelength to the laser receiving unit before and after each fluctuation; to obtain the concentration change trend corresponding to each fluctuation as determined by the control unit based on the laser signal received by the laser receiving unit, and to determine the solvent concentration change trend corresponding to each fluctuation based on the concentration change trend and the temperature and / or pressure change trend corresponding to the fluctuation.

[0112] In one specific embodiment, the laser-generating unit is a tunable diode laser generator, the laser-receiving unit is a laser receiver, and the control unit is a control system that interacts with the control module. Before and after each fluctuation, the control module controls the tunable diode laser generator to send a laser signal with a wavelength matching the maximum value of the solvent residue absorption peak to the infrared receiver. The control system uses an integral method instead of a resonant cavity to process and sample the output signal of the laser receiver, then calculates the concentration change trend corresponding to each fluctuation. Finally, based on the concentration change trend and the corresponding temperature and / or pressure change trends, the control module determines the solvent concentration change trend corresponding to each fluctuation.

[0113] In one specific embodiment Figure 4 A schematic diagram illustrating an example of a crystal solvent removal control system provided in an embodiment of the present invention is shown. Figure 5 Examples based on, such as Figure 4 The crystal solvent removal control system shown illustrates the specific process of constructing a temperature disturbance model. Figure 6 Examples based on, such as Figure 4 The crystal solvent removal control system shown herein performs a specific process for removing low-residue crystal solvents, which includes the following steps:

[0114] 601. Control the temperature according to the process parameters of the crystal to be processed, and adjust the temperature of the hot water in the hot water tank to a constant temperature (1-2℃ higher than the preset temperature);

[0115] 602. Control the pressure requirements according to the process parameters of the crystal to be processed, and adjust the pressure value inside the dryer to the preset pressure through the pressure control module;

[0116] 603. Fine-tune the pressure value inside the dryer and measure the output value of the laser receiver before and after fine-tuning to calculate the solvent concentration 1;

[0117] 604. Fine-tune the temperature inside the dryer and measure the output value of the laser receiver before and after fine-tuning to calculate the solvent concentration 2;

[0118] 605. Based on solvent concentration 1 and solvent concentration 2, a temperature disturbance model and a pressure disturbance model are modeled using Ansys software through a neural network learning algorithm.

[0119] 606. Based on temperature disturbance model and pressure disturbance model, the temperature and pressure inside the dryer are dynamically controlled.

[0120] As can be seen, the crystal solvent removal control system provided in this embodiment of the invention can accurately control and adjust the solvent removal process of different low-residue crystals, ensuring the stability of the solvent removal process and ensuring that the solvent removal process is intelligent and environmentally friendly.

[0121] Based on the same general inventive concept, the present invention also provides a low-solution-residue crystal, which is obtained by solvent removal through a crystal solvent removal control method or crystal solvent removal control system as provided in any of the above embodiments.

[0122] Figure 7 An example is a schematic diagram of the physical structure of an electronic device, such as... Figure 7 As shown, the electronic device may include a processor 710, a communication interface 720, a memory 730, and a communication bus 740. The processor 710, communication interface 720, and memory 730 communicate with each other via the communication bus 740. The processor 710 can call logic instructions in the memory 730 to execute a crystal solvent removal control method. This method includes: controlling the temperature and / or pressure within the dryer to fluctuate within a preset range; constructing a temperature disturbance model and / or a pressure disturbance model based on the changes in solvent concentration caused by the fluctuations; and dynamically regulating the temperature and / or pressure within the dryer based on the temperature disturbance model and / or pressure disturbance model until the solvent removal process is completed.

[0123] Furthermore, the logical instructions in the aforementioned memory 730 can be implemented as software functional units and, when sold or used as independent products, can be stored in a computer-readable storage medium. Based on this understanding, the technical solution of the present invention, essentially, or the part that contributes to the prior art, or a part of the technical solution, can be embodied in the form of a software product. This computer software product is stored in a storage medium and includes several instructions to cause a computer device (which may be a personal computer, server, or network device, etc.) to execute all or part of the steps of the methods described in the various embodiments of the present invention. The aforementioned storage medium includes various media capable of storing program code, such as USB flash drives, portable hard drives, read-only memory (ROM), random access memory (RAM), magnetic disks, or optical disks.

[0124] On the other hand, the present invention also provides a computer program product, the computer program product comprising a computer program stored on a non-transitory computer-readable storage medium, the computer program comprising program instructions, wherein when the program instructions are executed by a computer, the computer is able to execute the crystal solvent removal control method provided by the above methods, the method comprising: controlling the temperature and / or pressure inside the dryer to fluctuate within a preset range; constructing a temperature disturbance model and / or a pressure disturbance model based on the change in solvent concentration caused by the fluctuation; and dynamically regulating the temperature and / or pressure inside the dryer based on the temperature disturbance model and / or the pressure disturbance model until the solvent removal process is completed.

[0125] In another aspect, the present invention also provides a non-transitory computer-readable storage medium storing a computer program thereon. When executed by a processor, the computer program implements the crystal solvent removal control method provided by the above methods. The method includes: controlling the temperature and / or pressure inside the dryer to fluctuate within a preset range; constructing a temperature disturbance model and / or a pressure disturbance model based on the change in solvent concentration caused by the fluctuation; and dynamically regulating the temperature and / or pressure inside the dryer based on the temperature disturbance model and / or the pressure disturbance model until the solvent removal process ends.

[0126] The device embodiments described above are merely illustrative. The units described as separate components may or may not be physically separate. The components shown as units may or may not be physical units; that is, they may be located in one place or distributed across multiple network units. Some or all of the modules can be selected to achieve the purpose of this embodiment according to actual needs. Those skilled in the art can understand and implement this without any creative effort.

[0127] Through the above description of the embodiments, those skilled in the art can clearly understand that each embodiment can be implemented by means of software plus necessary general-purpose hardware platforms, and of course, it can also be implemented by hardware. Based on this understanding, the above technical solutions, in essence or the part that contributes to the prior art, can be embodied in the form of a software product. This computer software product can be stored in a computer-readable storage medium, such as ROM / RAM, magnetic disk, optical disk, etc., and includes several instructions to cause a computer device (which may be a personal computer, server, or network device, etc.) to execute the methods described in the various embodiments or some parts of the embodiments.

[0128] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for controlling the removal of crystal solvents, characterized in that, include: Control the temperature and / or pressure inside the dryer to fluctuate within a preset range; Determine the concentration change trend of the gaseous solvent residue in the dryer corresponding to each fluctuation, and the concentration change trend is used to determine the amount of change in solvent concentration; Based on the change in solvent concentration caused by the fluctuation, a temperature disturbance model and / or a pressure disturbance model are constructed, specifically including: obtaining the change in solvent concentration caused by each fluctuation and the temperature and / or pressure corresponding to the fluctuation; and constructing the temperature disturbance model and / or the pressure disturbance model. Based on the temperature disturbance model and / or the pressure disturbance model, the temperature and / or pressure inside the dryer are dynamically controlled until the solvent removal process ends. Specifically, this includes: adjusting the temperature and / or pressure inside the dryer to match in real time the temperature and / or pressure corresponding to the maximum value of the change in solvent concentration based on the temperature disturbance model and / or the pressure disturbance model; determining the difference between the concentration change trends corresponding to two adjacent fluctuations; and determining the end of the solvent removal process when a preset number of consecutive differences are all less than or equal to a preset difference.

2. The crystal solvent removal control method according to claim 1, characterized in that, Before controlling the temperature and / or pressure within the dryer to fluctuate within a preset range, the method further includes: The temperature and pressure inside the dryer are controlled to reach preset temperature and preset pressure, respectively, and the preset temperature and preset pressure meet the process parameter control temperature requirements and process parameter control pressure requirements of the crystal to be processed, respectively. The control of temperature and / or pressure fluctuations within the dryer within a preset range includes: The temperature inside the dryer is controlled to fluctuate within the temperature range corresponding to the process control temperature requirement, and / or the pressure inside the dryer is controlled to fluctuate within the pressure range corresponding to the process control pressure requirement.

3. A crystal solvent removal control system, characterized in that, include: The temperature control module is used to adjust the temperature inside the dryer; A pressure control module is used to adjust the pressure inside the dryer; The control module is used to control the temperature and / or pressure inside the dryer to fluctuate within a preset range based on the temperature control module and / or the pressure control module; and to determine the concentration change trend of the gas phase solvent residue inside the dryer corresponding to each fluctuation, wherein the concentration change trend is used to determine the amount of change in solvent concentration. Based on the change in solvent concentration caused by the fluctuation, a temperature disturbance model and / or a pressure disturbance model are constructed; and based on the temperature disturbance model and / or the pressure disturbance model, the temperature and / or pressure inside the dryer are dynamically controlled until the solvent removal process ends. Based on the change in solvent concentration caused by the fluctuation, a temperature disturbance model and / or a pressure disturbance model are constructed, specifically including: obtaining the change in solvent concentration caused by each fluctuation and the temperature and / or pressure corresponding to the fluctuation; and constructing the temperature disturbance model and / or the pressure disturbance model. Based on the temperature disturbance model and / or the pressure disturbance model, the temperature and / or pressure inside the dryer are dynamically controlled until the solvent removal process ends. Specifically, this includes: adjusting the temperature and / or pressure inside the dryer to match in real time the temperature and / or pressure corresponding to the maximum value of the change in solvent concentration based on the temperature disturbance model and / or the pressure disturbance model; determining the difference between the concentration change trends corresponding to two adjacent fluctuations; and determining the end of the solvent removal process when a preset number of consecutive differences are all less than or equal to a preset difference.

4. The crystal solvent removal control system according to claim 3, characterized in that, The temperature control module includes: a heating unit, a cooling unit, and a temperature detection unit; The control module is also used to control the heating unit and the cooling unit to adjust the temperature inside the dryer based on the temperature detected by the temperature detection unit.

5. The crystal solvent removal control system according to claim 3, characterized in that, Also includes: A solvent concentration change detection module is used to determine the concentration change trend of the gaseous solvent residue in the dryer corresponding to each fluctuation, and the concentration change trend is used to determine the amount of change in solvent concentration.

6. The crystal solvent removal control system according to claim 5, characterized in that, The solvent concentration change detection module includes: a laser generating unit, a laser receiving unit, and a control unit; The control module is also used to control the laser generating unit to emit a laser signal of a preset wavelength to the laser receiving unit before and after each fluctuation; to obtain the concentration change trend corresponding to each fluctuation as determined by the control unit based on the laser signal received by the laser receiving unit, and to determine the concentration change trend corresponding to each fluctuation based on the concentration change trend and the temperature and / or pressure change trend corresponding to the fluctuation.

7. A low-solubility residual crystal, characterized in that, The solvent is removed by the crystal solvent removal control method as described in claim 1 or 2, or the crystal solvent removal control system as described in any one of claims 3 to 6.

8. An electronic device comprising a memory, a processor, and a computer program stored in the memory and executable on the processor, characterized in that, When the processor executes the program, it implements the steps of the crystal solvent removal control method as described in claim 1 or 2.

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