CN115138307B - Reaction kettle system, temperature control method thereof, electronic equipment and storage medium - Google Patents

Reaction kettle system, temperature control method thereof, electronic equipment and storage medium Download PDF

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Publication number
CN115138307B
CN115138307B CN202210865533.0A CN202210865533A CN115138307B CN 115138307 B CN115138307 B CN 115138307B CN 202210865533 A CN202210865533 A CN 202210865533A CN 115138307 B CN115138307 B CN 115138307B
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temperature
heating medium
reaction kettle
time
reaction
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CN115138307A (en
Inventor
石晓召
赵振忠
周冬丽
宋伟光
袁志建
李明明
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Chenguang Biotech Group Co Ltd
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Chenguang Biotech Group Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006Controlling or regulating processes
    • B01J19/0013Controlling the temperature of the process
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/02Cleaning by the force of jets or sprays
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01KMEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
    • G01K1/00Details of thermometers not specially adapted for particular types of thermometer
    • GPHYSICS
    • G05CONTROLLING; REGULATING
    • G05DSYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
    • G05D23/00Control of temperature
    • G05D23/19Control of temperature characterised by the use of electric means
    • G05D23/20Control of temperature characterised by the use of electric means with sensing elements having variation of electric or magnetic properties with change of temperature
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00054Controlling or regulating the heat exchange system
    • B01J2219/00056Controlling or regulating the heat exchange system involving measured parameters
    • B01J2219/00058Temperature measurement
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00074Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00094Jackets

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Automation & Control Theory (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

A reaction kettle system, a temperature control method thereof, electronic equipment and a storage medium, wherein the system comprises: the reaction kettle is internally provided with a first temperature sensor for measuring the temperature of the reaction kettle; the jacket is arranged to cover the reaction kettle; the heating medium circulation module and the jacket form a heating medium loop for adjusting the temperature of the reaction kettle, and the heating medium circulation module comprises a heating medium tank for adjusting the temperature of heating medium, a second temperature sensor for measuring the temperature of the heating medium in the heating medium tank, a first valve group for controlling the on-off of the heating medium loop and a heating medium circulation pump for providing heating medium conveying power; the refrigerant circulation module and the jacket form a refrigerant loop for reducing the temperature of the reaction kettle; and a controller. The application utilizes the multistage mixing of the refrigerant and the heating medium to adjust the temperature of the reaction kettle, and the temperature reduction is mild, so that the reaction solution is easier to fall back in the process temperature requirement range.

Description

Reaction kettle system, temperature control method thereof, electronic equipment and storage medium
Technical Field
The application relates to the technical field of reaction kettles, in particular to a reaction kettle system, a temperature control method thereof, electronic equipment and a storage medium.
Background
Crystallization is one of the important methods for refining solid compounds, and when the temperature is lowered for crystallization, solutes are mutually dissolved in a solvent, and the solubility is changed along with the change of the temperature. When the temperature of the saturated solution with high solubility changes and the saturated solution with low solubility is converted into the saturated solution with low solubility, solute in the solution can be separated out in a crystal form in the solvent, and with the further change of the temperature, the crystal can be gradually grown and increased until a crystal structure with stable relative grain size is formed.
However, when liquid is fed, the temperature difference between the material temperature and the temperature of the reaction kettle is too large, and the crystallization liquid can be rapidly cooled to exceed the process temperature or directly skip a certain stage of crystallization; directly introducing steam or chilled water can cause overlarge change rate of crystallization liquid, uneven crystallization of the crystallization liquid, unstable product quality, agglomeration of precipitated crystals on the wall of the reaction kettle, and poor heat exchange capability with the outside caused by adhesion of the agglomerated crystals on the reaction kettle; the caking on the temperature probe causes inaccurate temperature measurement, and affects crystallization effect and product quality; multi-stage crystallization, too many artificial factors, low crystallization rate and more pseudomorphic crystals; the caking is difficult to clean on the temperature probe, and the cleaning efficiency is affected.
Disclosure of Invention
Aiming at the problems existing in the prior art, the application provides a reaction kettle system, a temperature control method thereof, electronic equipment and a storage medium.
The application provides a reaction kettle system, which comprises:
the reaction kettle is internally provided with a first temperature sensor for measuring the temperature of the reaction kettle;
the jacket is arranged to cover the reaction kettle;
the heating medium circulation module and the jacket form a heating medium loop for adjusting the temperature of the reaction kettle, and the heating medium circulation module comprises a heating medium tank for adjusting the temperature of heating medium, a second temperature sensor for measuring the temperature of the heating medium in the heating medium tank, a first valve group for controlling the on-off of the heating medium loop and a heating medium circulation pump for providing heating medium conveying power;
the cooling medium circulation module and the jacket form a cooling medium loop for reducing the temperature of the reaction kettle, and the cooling medium circulation module comprises a cooling medium tank for adjusting the temperature of cooling medium, a third temperature sensor for measuring the cooling temperature in the cooling medium tank, a second valve group for controlling the on-off of the cooling medium loop and a cooling medium circulation pump for providing cooling medium conveying power; and
the control machine is electrically connected with the first temperature sensor, the second temperature sensor, the third temperature sensor, the first valve group, the second valve group, the heating medium circulating pump and the cooling medium circulating pump.
According to the application, a reaction kettle system is provided, and the system further comprises:
and the fourth temperature sensor is used for measuring the ambient temperature of the system and is in signal connection with the controller.
According to the reaction kettle system provided by the application, the stirring device is arranged in the reaction kettle, the crystal scraping plate is arranged on the stirring device, the crystal scraping plate rotates along with the stirring device to form a circular track space, and the outer diameter of the track space is slightly smaller than the inner diameter of the reaction kettle.
According to the reaction kettle system provided by the application, the first temperature sensor is coated with Teflon.
According to the application, a reaction kettle system is provided, and the system further comprises:
the cleaning device comprises a cleaning device body, wherein the cleaning device body is tubular, one end of the cleaning device penetrates out of the reaction kettle and can be connected with an external high-pressure water pipe, the other end of the cleaning device extends into the reaction kettle and is provided with a nozzle facing the first temperature sensor, the nozzle is provided with a sealing ball, and the sealing ball is connected to the nozzle through a spring;
when the cleaning device is connected with the high-pressure water pipe, the sealing ball is separated from the nozzle under the water pressure, and when the cleaning device is removed from being connected with the high-pressure water pipe, the sealing ball seals the nozzle under the action of the spring.
According to the reaction kettle system provided by the application, the heating medium circulation module and/or the cooling medium circulation module is/are provided with the unpowered fan blade device at the connecting pipe for conveying the heating medium or cooling medium to the jacket, and the fan blade device can rotate under the flowing action of the heating medium or cooling medium, so that vortex is formed in the heating medium or cooling medium when the heating medium or cooling medium enters the jacket.
The application also provides a temperature control method of the reaction kettle system, the method divides the reaction process into a plurality of equal temperature regulating periods according to time, and the method comprises the following steps of:
acquiring the real-time temperature of a heating medium in a heating medium tank in the current temperature regulation period;
based on the real-time temperature of the heating medium, comprehensive environmental temperature compensation and periodic prediction cooling compensation are carried out, and the set temperature of the heating medium tank in the current temperature regulation period is obtained;
and operating the heating medium circulating device and the cooling medium circulating device in the temperature regulating period, and ensuring that the operation time of the cooling medium circulating device is kept continuous in the temperature regulating period.
According to the temperature control method of the reaction kettle system provided by the application, the acquisition method of the ambient temperature compensation comprises the following steps:
acquiring a process control temperature required by the reaction process in a current temperature regulation period and an environmental temperature of a reaction kettle system;
and calculating the ambient temperature compensation based on a binary linear function of the process control temperature and the ambient temperature.
According to the temperature control method of the reaction kettle system provided by the application, the periodic prediction cooling compensation acquisition method comprises the following steps:
acquiring a first slope of a tangent line of the time-temperature curve at a current moment point based on a time-temperature curve actually measured by a reaction kettle;
obtaining a second slope of a reaction process standard curve in the current temperature regulation period;
if the quotient of the first slope divided by the second slope is greater than 1, the periodic predictive cooling compensation is set to be a positive number compensation value, and if the quotient of the first slope divided by the second slope is less than or equal to 1, the periodic predictive cooling compensation is set to be a negative number compensation value;
wherein the positive number compensation value is equal to the absolute value of the negative number compensation value.
According to the temperature control method of the reaction kettle system provided by the application, the operation time of the refrigerant circulation device is acquired by the method comprising the following steps:
acquiring the temperature difference between the real-time temperature and the ambient temperature of the heating medium;
and acquiring the operation time of the refrigerant circulation device based on the unitary quadratic function of the temperature difference.
According to the temperature control method of the reaction kettle system provided by the application, the method further comprises the following steps:
based on the set temperature return difference, taking the process control temperature required by the reaction process in the current temperature regulation period as a temperature lower limit, and taking the sum of the process control temperature and the temperature return difference as a temperature upper limit to establish a temperature interval;
dividing a plurality of temperature sections based on the temperature interval, wherein each temperature section corresponds to a preset time weighting coefficient, and the time weighting coefficient corresponding to the temperature section which is closer to the lower temperature limit is smaller;
acquiring the real-time reaction temperature of the reaction kettle in the current temperature regulation period;
judging a temperature section in which the real-time reaction temperature falls, and acquiring a corresponding time weighting coefficient;
and updating the operation time of the refrigerant circulation device to be weighted time based on the corresponding time weighting coefficient.
The application also provides electronic equipment, which comprises a memory, a processor and a computer program stored in the memory and capable of running on the processor, wherein the processor realizes the steps of the temperature control method of the reaction kettle system according to any one of the above steps when executing the program.
The present application also provides a non-transitory computer readable storage medium having stored thereon a computer program which, when executed by a processor, implements the steps of the temperature control method of the reactor system as described in any one of the above.
The application also provides a computer program product comprising a computer program which, when executed by a processor, implements the steps of the method for controlling the temperature of a reactor system as described in any one of the above.
According to the reaction kettle system, the temperature control method thereof, the electronic equipment and the storage medium, provided by the application, the temperature of the reaction kettle is regulated by utilizing multistage mixing of the refrigerant and the heating medium, and the temperature is reduced mildly, so that the reaction solution is easier to fall back in the process temperature requirement range.
Drawings
In order to more clearly illustrate the application or the technical solutions of the prior art, the following brief description will be given of the drawings used in the embodiments or the description of the prior art, it being obvious that the drawings in the following description are some embodiments of the application and that other drawings can be obtained from them without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a reaction kettle system according to the present application;
FIG. 2 is a schematic flow chart of a temperature control method of a reaction kettle system provided by the application;
fig. 3 is a schematic diagram of an entity structure of an electronic device according to the present application.
Reference numerals: 1-a stirring motor; 2-a reaction kettle; 3-stirring device; 4-a crystal scraping plate; 5-a first temperature sensor; 6-a heating medium tank; 7-heating coils; 8-a second temperature sensor; 9-a steam regulating valve; 10-a heating medium circulating pump; 11-a refrigerant circulating pump; 12-a refrigerant tank; 13-a refrigerant liquid inlet valve; 14-a heating medium liquid inlet valve; 15-a refrigerant liquid outlet valve; 16-a heating medium liquid outlet valve; 17-a third temperature sensor; 18-a fan blade arrangement; 19-a liquid inlet valve of the reaction kettle; 20-high-pressure water inlet; 21-a cleaning device; 22-sealing ball.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present application more apparent, the technical solutions of the present application will be clearly and completely described below with reference to the accompanying drawings, and it is apparent that the described embodiments are some embodiments of the present application, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
The reaction kettle system provided by the embodiment of the application is described in detail through specific embodiments and application scenes thereof by combining the accompanying drawings.
Example 1
FIG. 1A schematic structural diagram of a reaction kettle system provided by the application, as shown in FIG. 1, the reaction kettle system provided by the application comprises:
the reaction kettle 2, a first temperature sensor 5 for measuring the temperature of the reaction kettle 2 is arranged in the reaction kettle 2;
a jacket is arranged to cover the reaction kettle 2;
the heating medium circulation module and the jacket form a heating medium loop for adjusting the temperature of the reaction kettle 2, and the heating medium circulation module comprises a heating medium tank 6 for adjusting the temperature of heating medium, a second temperature sensor 8 for measuring the temperature of the heating medium in the heating medium tank 6, a first valve group for controlling the on-off of the heating medium loop and a heating medium circulation pump 10 for providing heating medium conveying power;
the refrigerant circulation module and the jacket form a refrigerant loop for reducing the temperature of the reaction kettle 2, and the refrigerant circulation module comprises a refrigerant tank 12 for adjusting the temperature of the refrigerant, a third temperature sensor 17 for measuring the temperature of the refrigerant in the refrigerant tank 12, a second valve group for controlling the on-off of the refrigerant loop and a refrigerant circulation pump 11 for providing refrigerant conveying power; and
the control machine is electrically connected with the first temperature sensor 5, the second temperature sensor 8, the third temperature sensor 17, the first valve group, the second valve group, the heating medium circulating pump 10 and the cooling medium circulating pump 11.
Preferably, the reactor 2 is used for crystallization or evaporation.
Preferably, the outside of the reaction kettle 2 is provided with an insulating layer.
Preferably, the heating medium circulation module and the cooling medium circulation module share the same jacket inlet and outlet, and all adopted media are ethylene glycol.
Preferably, the jacket inlet is at the bottom and the outlet is at the top.
Preferably, the heating coil 7 is installed outside the heating medium tank 6, steam is introduced into the coil to heat the heating medium, and the heating medium tank 6 is cooled by natural cooling and reflow (the heating medium after temperature reduction).
Preferably, a manual circulation valve is arranged on the heating medium tank 6/cooling medium tank 12 to ensure that the pressure of the heating medium/cooling medium pump outlet is in a normal range.
Preferably, the control machine is a programmable logic controller (Programmable Logic Controller, PLC) which is connected with a computer to realize display and operation. The control machine is used for controlling the reaction kettle system to execute specific operation actions, and the computer is used for displaying the current operation state and inputting operation instructions.
Preferably, the heat medium circulation pump 10 is used for circulating the heat medium into the jacket, and the liquid inlet amount is controlled through the first valve group; the refrigerant circulating pump 11 is used for circulating the refrigerant into the jacket, and the liquid inlet amount is controlled through the second valve group.
Optionally, the system further comprises:
and the fourth temperature sensor is used for measuring the ambient temperature of the system and is in signal connection with the controller.
Optionally, a stirring device 3 is arranged in the reaction kettle, a crystal scraping plate 4 is arranged on the stirring device 3, the crystal scraping plate 4 forms a circular track space after rotating along with the stirring device 3, and the outer diameter of the track space is slightly smaller than the inner diameter of the reaction kettle.
Preferably, the stirring device 3 drives the stirring blade to rotate, and a crystal scraping plate 4 is arranged on the outer side of the stirring blade and used for cleaning precipitated crystals on the inner wall of the reaction kettle.
Optionally, teflon is coated on the first temperature sensor 5.
Preferably, the armoured part of the first temperature sensor 5 is coated with teflon, so that friction between crystals and the first temperature sensor 5 is reduced, and the problem of inaccurate temperature caused by adhesion of crystals and condensation blocks to a temperature probe is reduced.
Optionally, the system further comprises:
the cleaning device 21, the main body of the cleaning device 21 is tubular, one end of the cleaning device 21 is penetrated out of the reaction kettle and can be connected with an external high-pressure water pipe, the other end of the cleaning device 21 extends into the reaction kettle and is provided with a nozzle facing the first temperature sensor 5, the nozzle is provided with a sealing ball 22, and the sealing ball 22 is connected with the nozzle through a spring;
wherein, when the cleaning device 21 is connected with the high-pressure water pipe, the sealing ball 22 leaves the nozzle under the water pressure, and when the cleaning device 21 removes the connection with the high-pressure water pipe, the sealing ball 22 seals the nozzle under the action of the spring. The cleaning device 21 can achieve the purpose of cleaning the first temperature sensor 5 without disassembling an instrument or opening the reaction kettle.
Optionally, the connection pipe of the heat medium circulation module and/or the cooling medium circulation module for conveying the heat medium or cooling medium to the jacket is provided with an unpowered fan blade device 18, and the fan blade device 18 can rotate under the flowing action of the heat medium or cooling medium, so that vortex is formed in the heat medium or cooling medium when entering the jacket.
In the embodiment, the temperature of the reaction kettle is regulated by multistage mixing of the refrigerant and the heating medium, and the temperature is reduced mildly, so that the reaction solution is easier to fall back in the process temperature requirement range; before and after liquid feeding in the jacket, the temperature of the heating medium is adjusted to the temperature range required by the process, so that the liquid feeding temperature of the reaction kettle is ensured to be unchanged to the maximum extent, the jacket is not heated by directly using steam, and the expansion of the difference between the crystallization liquid and the process temperature is avoided; the device is used for crystallization, the crystallization is more stable, the phenomenon of crystallization agglomeration is reduced, the problem that the crystallization is adhered to a temperature probe is reduced, and meanwhile, the device can be used as a simple evaporation container for evaporation and concentration.
Example 2
Fig. 2 is a schematic flow chart of a temperature control method of a reaction kettle system provided by the application, as shown in fig. 2, and the method of the temperature control method of the reaction kettle system provided by the application divides a reaction process into a plurality of equal temperature adjustment periods according to time, and comprises the following steps of:
s100, acquiring the real-time temperature of the heating medium in the heating medium tank 6 in the current temperature regulation period;
s200, based on the real-time temperature of the heating medium, comprehensively compensating the ambient temperature, and periodically predicting and cooling the temperature to obtain the set temperature of the heating medium tank 6 in the current temperature regulation period;
s300, operating the heating medium circulation device and the cooling medium circulation device in a temperature regulation period, and ensuring that the operation time of the cooling medium circulation device is kept continuous in the temperature regulation period.
It should be noted that, at the beginning of the reaction, the controller needs to adjust the temperature in the heat medium tank 6 to be slightly higher than the initial standard temperature of the reaction process. If the reaction solution is initially at a low temperature, it is necessary to raise the temperature first.
Preferably, the temperature adjustment period is 30s, and the total operation time of the heating medium circulation device and the cooling medium circulation device in each temperature adjustment period is 30s.
Preferably, the set temperature of the heating medium tank 6 is the sum of the real-time temperature of the heating medium, the comprehensive environmental temperature compensation and the periodic predictive cooling compensation.
Preferably, the control machine controls the feeding of the refrigerant and the heating medium, the feeding of the refrigerant and the heating medium is different, and the second valve group (the refrigerant feeding valve 13 and the refrigerant discharging valve 15) is interlocked with the first valve group (the heating medium feeding valve 14 and the heating medium discharging valve 16) in a program. When the refrigerant is fed, the refrigerant feed valve 13 and the refrigerant discharge valve 15 output simultaneously, the heating medium is not output, and the refrigerant with the same volume is guaranteed to flow back to the refrigerant tank 12; when the heating medium is fed, the heating medium feed valve 14 and the heating medium discharge valve 16 are simultaneously output, the cooling medium is not output, and the heating medium with the same volume is guaranteed to flow back to the heating medium tank 6.
Preferably, before the reaction starts, the control machine compares the standard temperature of the reaction process with the actual measured temperature in the reaction kettle, and when the measured temperature is lower than the standard temperature of the reaction process, the temperature is preheated to the standard temperature of the reaction process and then reduced; when the measured temperature is higher than the standard temperature of the reaction process, the temperature is pre-reduced to the standard temperature of the reaction process.
Optionally, the method for acquiring the ambient temperature compensation includes:
acquiring a process control temperature required by a reaction process in a current temperature regulation period and an environment temperature of a reaction kettle system;
the ambient temperature compensation is calculated based on a binary linear function of the process control temperature and the ambient temperature.
Preferably, the calculation formula of the ambient temperature compensation is as follows:
ambient temperature compensation = 0.1 (process control temperature-ambient temperature) -1
Optionally, the method for obtaining the periodic prediction cooling compensation includes:
acquiring a first slope of a tangent line of the time-temperature curve at the current moment point based on a time-temperature curve actually measured by the reaction kettle;
obtaining a second slope of a reaction process standard curve in the current temperature regulation period;
if the quotient of the first slope divided by the second slope is greater than 1, the periodic predictive cooling compensation is set to be a positive number compensation value, and if the quotient of the first slope divided by the second slope is less than or equal to 1, the periodic predictive cooling compensation is set to be a negative number compensation value;
wherein the positive number compensation value is equal to the absolute value of the negative number compensation value.
Preferably, the absolute value of the compensation value is 1 °.
The temperature of the heating medium tank 6 is increased when the predicted temperature reduction speed of the reaction kettle exceeds the reaction process standard reduction speed by setting the periodical prediction cooling compensation, so that the temperature of the reaction kettle is increased; conversely, when the predicted temperature decrease rate of the reaction kettle is smaller than the reaction process standard decrease rate, the temperature of the heating medium tank 6 is decreased, so that the temperature of the reaction kettle is decreased.
Optionally, the method for acquiring the operation time of the refrigerant circulation device comprises the following steps:
acquiring the temperature difference between the real-time temperature and the ambient temperature of the heating medium;
and acquiring the operation time of the refrigerant circulation device based on the unitary quadratic function of the temperature difference.
Preferably, the operation time of the refrigerant circulation device is calculated as follows:
operation time of refrigerant cycle device=0.0054 (temperature difference) 2 0.6279 (temperature difference) +18.678
Optionally, the method further comprises:
based on the set temperature return difference, taking the process control temperature required by the reaction process in the current temperature regulation period as a temperature lower limit, and taking the sum of the process control temperature and the temperature return difference as a temperature upper limit to establish a temperature interval;
dividing a plurality of temperature sections based on a temperature interval, wherein each temperature section corresponds to a preset time weighting coefficient, and the time weighting coefficient corresponding to the temperature section which is closer to the lower limit of the temperature is smaller;
acquiring the real-time reaction temperature of the reaction kettle in the current temperature regulation period;
judging a temperature section in which the real-time reaction temperature falls, and acquiring a corresponding time weighting coefficient;
and updating the operation time of the refrigerant circulation device to the weighted time based on the corresponding time weighting coefficient.
Preferably, the number of temperature segments is 3. Preferably, the time weighting coefficient of the temperature section including the temperature lower limit is 1, the time weighting coefficient of the temperature section including the temperature upper limit is 1.5, and the time weighting coefficient of the temperature section located in the middle of the two temperature sections is 1.2.
Preferably, if the weighted operation time of the refrigerant circulation device exceeds the temperature adjustment period, the operation time of the refrigerant circulation device is set as the temperature adjustment period.
It should be noted that, the operation time of the refrigerant circulation device is weighted by the segmentation of the temperature return difference, so that the compensation control of the temperature is finer and more sufficient, and the temperature adjustment of the reaction kettle is smoother.
According to the embodiment, the real-time temperature of the heating medium is controlled to be reduced along with the standard temperature of the reaction process so as to ensure that the temperature of the reaction kettle is not greatly changed, and the continuous refrigerant execution time in the temperature adjustment period is used, so that the alternation of the refrigerant heating medium is not too frequent to damage equipment, most parameters are directly controlled by variable quantities, other factors are not needed to be considered manually, and the frequency of manually inputting parameters for adjustment is greatly reduced.
Example 3
By using the reaction kettle system and the control method thereof, stevioside crystallization cooling control is performed, stevioside pseudomorphic generation is reduced, the crystallization temperature is reduced to +/-0.2 ℃ from the deviation process temperature of +/-1 ℃, the crystallization yield is improved to 97.7% from 94.5%, and the crystallization time is reduced to 8.5 hours from 11 hours.
By using the reaction kettle system and the control method thereof, the piperine crystallization temperature is controlled to be reduced to +/-0.23 ℃ from the deviation process temperature of +/-1.11 ℃, the crystallization yield is improved to 97.1% from 94.8%, and the crystallization time is reduced to 14.5 hours from 18 hours.
Fig. 3 is a schematic physical structure of an electronic device according to the present application, where, as shown in fig. 3, the electronic device may include: processor 810, communication interface (Communications Interface) 820, memory 830, and communication bus 840, wherein processor 810, communication interface 820, memory 830 accomplish communication with each other through communication bus 840. The processor 810 may invoke logic instructions in the memory 830 to perform a method of controlling the temperature of a reactor system that divides a reaction process into a plurality of equal attemperation cycles by time, for each of which the method comprises:
acquiring the real-time temperature of a heating medium in a heating medium tank in the current temperature regulation period;
based on the real-time temperature of the heating medium, comprehensive environmental temperature compensation and periodic prediction cooling compensation are carried out, and the set temperature of the heating medium tank in the current temperature regulation period is obtained;
and operating the heating medium circulating device and the cooling medium circulating device in the temperature regulating period, and ensuring that the operation time of the cooling medium circulating device is kept continuous in the temperature regulating period.
Further, the logic instructions in the memory 830 described above may be implemented in the form of software functional units and may be stored in a computer-readable storage medium when sold or used as a stand-alone product. Based on this understanding, the technical solution of the present application may be embodied essentially or in a part contributing to the prior art or in a part of the technical solution, in the form of a software product stored in a storage medium, comprising several instructions for causing a computer device (which may be a personal computer, a server, a network device, etc.) to perform all or part of the steps of the method according to the embodiments of the present application. And the aforementioned storage medium includes: a U-disk, a removable hard disk, a Read-Only Memory (ROM), a random access Memory (RAM, random Access Memory), a magnetic disk, or an optical disk, or other various media capable of storing program codes.
In another aspect, the present application also provides a computer program product comprising a computer program stored on a non-transitory computer readable storage medium, the computer program comprising program instructions which, when executed by a computer, enable the computer to perform a method of controlling the temperature of a reactor system provided by the above methods, the method dividing a reaction process into a plurality of equal tempering periods in terms of time, the method comprising, for each tempering period:
acquiring the real-time temperature of a heating medium in a heating medium tank in the current temperature regulation period;
based on the real-time temperature of the heating medium, comprehensive environmental temperature compensation and periodic prediction cooling compensation are carried out, and the set temperature of the heating medium tank in the current temperature regulation period is obtained;
and operating the heating medium circulating device and the cooling medium circulating device in the temperature regulating period, and ensuring that the operation time of the cooling medium circulating device is kept continuous in the temperature regulating period.
In yet another aspect, the present application further provides a non-transitory computer readable storage medium having stored thereon a computer program which, when executed by a processor, is implemented to perform the above-provided method of controlling the temperature of a reaction kettle system, the method dividing a reaction process into a plurality of equal tempering periods according to time, the method comprising, for each of the tempering periods:
acquiring the real-time temperature of a heating medium in a heating medium tank in the current temperature regulation period;
based on the real-time temperature of the heating medium, comprehensive environmental temperature compensation and periodic prediction cooling compensation are carried out, and the set temperature of the heating medium tank in the current temperature regulation period is obtained;
and operating the heating medium circulating device and the cooling medium circulating device in the temperature regulating period, and ensuring that the operation time of the cooling medium circulating device is kept continuous in the temperature regulating period.
The apparatus embodiments described above are merely illustrative, wherein the elements illustrated as separate elements may or may not be physically separate, and the elements shown as elements may or may not be physical elements, may be located in one place, or may be distributed over a plurality of network elements. Some or all of the modules may be selected according to actual needs to achieve the purpose of the solution of this embodiment. Those of ordinary skill in the art will understand and implement the present application without undue burden.
From the above description of the embodiments, it will be apparent to those skilled in the art that the embodiments may be implemented by means of software plus necessary general hardware platforms, or of course may be implemented by means of hardware. Based on this understanding, the foregoing technical solution may be embodied essentially or in a part contributing to the prior art in the form of a software product, which may be stored in a computer readable storage medium, such as ROM/RAM, a magnetic disk, an optical disk, etc., including several instructions for causing a computer device (which may be a personal computer, a server, or a network device, etc.) to execute the method described in the respective embodiments or some parts of the embodiments.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present application, and are not limiting; although the application has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present application.

Claims (7)

1. A method of controlling the temperature of a reaction kettle system, said method dividing a reaction process into a plurality of equal tempering periods according to time, said method comprising, for each of said tempering periods:
acquiring the real-time temperature of a heating medium in a heating medium tank in the current temperature regulation period;
based on the real-time temperature of the heating medium, comprehensive environmental temperature compensation and periodic prediction cooling compensation are carried out, and the set temperature of the heating medium tank in the current temperature regulation period is obtained;
operating the heating medium circulation device and the cooling medium circulation device in the temperature regulation period, and ensuring that the operation time of the cooling medium circulation device is kept continuous in the temperature regulation period;
before the reaction starts, comparing the standard temperature of the reaction process with the actual measured temperature in the reaction kettle, and when the actual measured temperature in the reaction kettle is lower than the standard temperature of the reaction process, preheating to the standard temperature of the reaction process and then cooling; when the actual measured temperature in the reaction kettle is higher than the standard temperature of the reaction process, pre-cooling to the standard temperature of the reaction process;
based on the set temperature return difference, taking the process control temperature required by the reaction process in the current temperature regulation period as a temperature lower limit, and taking the sum of the process control temperature and the temperature return difference as a temperature upper limit to establish a temperature interval;
dividing a plurality of temperature sections based on the temperature interval, wherein each temperature section corresponds to a preset time weighting coefficient, and the time weighting coefficient corresponding to the temperature section which is closer to the lower temperature limit is smaller;
acquiring the real-time reaction temperature of the reaction kettle in the current temperature regulation period;
judging a temperature section in which the real-time reaction temperature falls, and acquiring a corresponding time weighting coefficient;
and updating the operation time of the refrigerant circulation device to be weighted time based on the corresponding time weighting coefficient.
2. The method for controlling the temperature of a reactor system according to claim 1, wherein the method for obtaining the ambient temperature compensation comprises:
acquiring a process control temperature required by the reaction process in a current temperature regulation period and an environmental temperature of a reaction kettle system;
and calculating the ambient temperature compensation based on a binary linear function of the process control temperature and the ambient temperature.
3. The method for controlling the temperature of a reactor system according to claim 1, wherein the method for obtaining the periodic predictive cooling compensation comprises:
acquiring a first slope of a tangent line of the time-temperature curve at a current moment point based on a time-temperature curve actually measured by a reaction kettle;
obtaining a second slope of a reaction process standard curve in the current temperature regulation period;
if the quotient of the first slope divided by the second slope is greater than 1, the periodic predictive cooling compensation is set to be a positive number compensation value, and if the quotient of the first slope divided by the second slope is less than or equal to 1, the periodic predictive cooling compensation is set to be a negative number compensation value;
wherein the positive number compensation value is equal to the absolute value of the negative number compensation value.
4. The method for controlling the temperature of a reaction kettle system according to claim 1, wherein the method for obtaining the operation time of the refrigerant circulation device comprises the following steps:
acquiring the temperature difference between the real-time temperature and the ambient temperature of the heating medium;
and acquiring the operation time of the refrigerant circulation device based on the unitary quadratic function of the temperature difference.
5. An electronic device comprising a memory, a processor and a computer program stored on the memory and executable on the processor, wherein the processor, when executing the program, performs the steps of the method for controlling the temperature of the reactor system of any one of claims 1-4.
6. A non-transitory computer readable storage medium having stored thereon a computer program, wherein the computer program when executed by a processor implements the steps of the temperature control method of the reactor system of any of claims 1-4.
7. A computer program product comprising a computer program which, when executed by a processor, implements the steps of the temperature control method of the reactor system of any one of claims 1-4.
CN202210865533.0A 2022-07-21 2022-07-21 Reaction kettle system, temperature control method thereof, electronic equipment and storage medium Active CN115138307B (en)

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