CN114452913A - Flow chemical reaction module and automatic experimental device thereof - Google Patents
Flow chemical reaction module and automatic experimental device thereof Download PDFInfo
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- CN114452913A CN114452913A CN202210165116.5A CN202210165116A CN114452913A CN 114452913 A CN114452913 A CN 114452913A CN 202210165116 A CN202210165116 A CN 202210165116A CN 114452913 A CN114452913 A CN 114452913A
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
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Abstract
The invention discloses a flow chemical reaction module and an automatic experimental device thereof, wherein the reaction module comprises a substrate, a reaction channel, a temperature control plate and a temperature sensor, the temperature sensor comprises an upper temperature sensor and a lower temperature sensor, the upper temperature sensor is arranged at the edge of the reaction channel, and the lower temperature sensor is positioned between the substrate and the temperature control plate; the control terminal is provided with software for controlling the operation of a system, the control terminal exchanges data with the main control module, and the processing and calculation of the data of the control terminal comprise heating/cooling time calculation and temperature compensation calculation; the control terminal also includes a software module capable of performing temperature compensation calculations. According to the invention, the upper temperature sensor and the lower temperature sensor are distributed on the opposite surfaces of the substrate, and the temperature compensation calculation is executed on the substrate through the software module of the control terminal, so that the yield of the product is improved, the quality of the product is ensured, and the controllability and reliability of the reaction are ensured, thereby realizing the accurate control of the device.
Description
Technical Field
The invention relates to a flow chemical reaction module and an automatic experimental device thereof.
Background
Nowadays, the safety problem of the laboratory is concerned more and more, the operation is mainly carried out by personnel when the synthesis reaction is carried out in the laboratory, but when flammable, explosive or toxic and harmful substances are involved in the operation process, the personnel safety of the personnel is caused with great danger hidden trouble; moreover, because the experiment operation is mainly performed by experimenters, the labor cost is high, the efficiency is low, and the experiment operation is more dependent on the experience or proficiency of the experimenters, the yield of the experiment result is easy to be unstable, and even the experiment failure is caused. In such a background, flow synthesis techniques have been developed. Flow synthesis, also known as continuous flow chemistry, has excellent control over reaction conditions such as time, temperature, reagents, etc., and innovatively integrates the conventional independent and separate synthesis operation processes, thereby accelerating the synthesis speed, having strong repeatability, and particularly being capable of carrying out dangerous and difficult-to-implement reactions.
Chinese patent CN201580008455 discloses a scheme of directly heating chemical mixtures inside a flow chemical reactor by using electric heating, which does not need a heating element generating extra resistance, but directly heats the chemical reactor, which is made of metal, so that the application range is narrow, the manufacturing process is complex, and the requirements on the metal material are strict and the cost is high; the above-described embodiments of the present invention are different from the reaction environment of the reaction channel of the reactor of the present invention, and the present invention is applicable to a reaction performed in a microchannel and a fluid reaction in a wider range. In the prior art, the temperature of the flow synthesis reaction microchannel is generally measured by using a temperature sensor, and the temperature sensor is generally not directly attached to a front pipeline of a polymer or silicon dioxide in the flow synthesis reaction, so that on one hand, the sight condition of a reaction pipeline is easily shielded by the mode, a user cannot accurately observe the reaction condition, and on the other hand, the damage failure of the temperature sensor is easily caused in the subsequent panel installation process; furthermore, in the flow synthesis reaction, when the temperature measured by the temperature sensor reaches the set temperature, the reaction module stops heating, however, because of heat transfer loss, the temperature in the reaction microchannel cannot reach the set temperature at this time, and there is a certain influence on the yield of the product of the chemical reaction, and therefore, how to optimize the automation device, so as to finely control the flow chemistry to further improve the yield or quality of the product is an urgent problem to be solved.
Disclosure of Invention
In order to solve the above technical problems, an object of the present invention is to provide a flow chemical reaction module and an automated experimental apparatus thereof.
The invention is realized by the following technical scheme: a flow chemical reaction module comprises a substrate, a reaction channel, a temperature control plate and a temperature sensor, wherein the reaction channel and the temperature control plate are respectively arranged on the upper surface and the lower surface of the substrate; the control terminal is provided with software for controlling the operation of the system, exchanges data with the main control module and processes and calculates the data, the processing and calculation of the data of the control terminal comprises temperature compensation calculation and transmits a temperature compensation value to the main control module.
In a preferred embodiment, the processing and calculation of the data of the control terminal comprises heating/cooling time calculations and temperature compensation calculations at different operating phases.
In a preferred embodiment, the temperature compensation is performed as follows:
step 101: obtaining a target reaction temperature parameter;
step 102: calculating heating/cooling time according to the difference between the target reaction temperature and the temperature measured by the temperature sensor in a fitting manner, and transmitting an instruction to the main control module;
step 103: starting the temperature control board to continuously heat/cool within the heating/cooling time, and transmitting the temperature value measured by the temperature sensor to the control terminal in real time through the main control module;
step 104: after the heating/cooling is finished, the software module executes temperature compensation calculation according to the temperature difference measured by the upper temperature sensor and the lower temperature sensor, and transmits the calculated temperature compensation value to the main control module.
In a preferred embodiment, in step 103, if the measured temperature value meets the target requirement, step 104 is entered for further execution; and if the target requirement is not met, automatically sending alarm information to the control terminal.
In a preferred embodiment, the control terminal may further include an alarm for outputting an alarm signal when receiving alarm information of abnormal temperature conditions sent by the temperature sensor.
In a preferred embodiment, the temperature compensation is performed as follows:
step 201: acquiring target reaction temperature parameters, multi-section heating temperatures and corresponding heat preservation time lengths;
step 202: calculating heating/cooling time according to the difference fit between the reaction temperature of the first gradient and the temperature measured by the temperature sensor, and transmitting an instruction to the main control module;
step 203: starting the temperature control board to continuously heat/cool within the heating/cooling time, and transmitting the temperature value measured by the temperature sensor to the control terminal in real time through the main control module;
step 204: after the heating/cooling is finished, the software module executes temperature compensation calculation according to the temperature difference measured by the upper temperature sensor and the lower temperature sensor and transmits the calculated temperature compensation value to the main control module;
step 205: and (3) repeatedly executing the step 202 to the step 204 until the temperature is increased/decreased to the target reaction temperature and then maintaining the heat preservation state according to the set time length.
In a preferred embodiment, the multiple heating temperatures and the corresponding heat preservation time periods are preset in software of the control terminal or are input and set by a user in a customized manner.
In a preferred embodiment, the multiple heating temperatures and the corresponding holding time periods are set equally or randomly.
In a preferred embodiment, the substrate is provided with a groove, and the reaction channel is embedded in the groove; the reaction channel comprises a reactant inlet, a reaction channel main body and a product outlet, and the upper temperature sensor is clamped between the reactant inlet and the product outlet and is close to the reaction channel main body.
The invention also discloses an automatic experimental device, which comprises a liquid inlet module and the flowing chemical reaction module, wherein the control terminal sends an instruction to the main control module, and the main control module sends the instruction to the liquid inlet module and the flowing chemical reaction module through serial ports; the flow chemical reaction module heats/cools the reaction channel to a target reaction temperature in advance, and then the liquid inlet module starts to feed liquid or synchronously feed liquid.
In a preferred embodiment, a liquid injection device and an electromagnetic valve are respectively arranged on the first liquid inlet path and the second liquid inlet path of the liquid inlet module, and the liquid injection device is used for feeding a reactant or extruding the reactant into the flowing chemical reaction module; and the liquid injection device and the electromagnetic valve are connected to the main control module.
According to the flow chemical reaction module and the automatic experimental device thereof, the upper temperature sensor and the lower temperature sensor are arranged on the opposite surfaces of the substrate, and the temperature compensation calculation is executed through the software module of the control terminal, so that the positive temperature is corrected in the automatic control process, the temperature in the reaction channel can be infinitely close to the target reaction temperature, the yield of a product is improved, the quality of the product is ensured, the controllability and the reliability of the reaction are ensured, and the device is accurately controlled.
Drawings
In order to more clearly illustrate the technical solution of the present invention, the drawings needed for the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
Fig. 1 and 2 are schematic top views of one embodiment of a flow chemical reaction module according to the present invention.
Fig. 3 is a cross-sectional view at a-a in fig. 2.
FIG. 4 is a schematic top view of another embodiment of a flow chemical reaction module of the present invention.
FIG. 5 is a schematic diagram of the automated laboratory apparatus according to the present invention.
FIG. 6 is a flowchart illustrating a temperature compensation execution procedure according to a first embodiment of the present invention.
FIG. 7 is a flowchart illustrating a temperature compensation execution procedure according to a second embodiment of the present invention.
FIG. 8 is a schematic structural diagram of an automated experimental apparatus according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without any inventive step, are within the scope of the present invention.
Referring to the attached drawings 1-3 of the specification, a flow chemical reaction module S comprises a base plate S1, a reaction channel S2, a temperature control plate S3 and a temperature sensor, wherein the temperature control plate S3 and the temperature sensor are connected to a main control module; the substrate S1 includes an upper surface S11 and a lower surface S12, the reaction channel S2 is disposed on the upper surface S11 of the substrate, a groove is disposed on the upper surface S11 of the substrate, the contour of the groove matches with the reaction channel S2, the reaction channel S2 is disposed in the groove, and then a transparent panel is covered on the reaction channel, the substrate is, for example, a metal plate, which has good thermal conductivity and can rapidly transfer heat into the reaction channel S2; in addition, the periphery of the base plate S1 is further opened with a mounting hole S13, which is matched with a screw for stably mounting the flow chemical reaction module into the apparatus. The reaction channel S2 comprises a reactant inlet S21 and a product outlet S22, the reaction channel S2 is designed in a bending mode, and the reaction path can be effectively prolonged through the bending shape design, so that the reaction time is prolonged, and the reaction efficiency is further improved; the diameter of the reaction channel is 100-1000um, and the reaction channel can be made of chemical corrosion resistant high molecular materials or silicon dioxide, and the reaction channel of the invention adopts ETFE polymer (ethylene-tetrafluoroethylene copolymer), polyether ether ketone (PEEK), Polytetrafluoroethylene (PTFE), tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer (PFA) and the like, and has good corrosion resistance; of course, in another embodiment, the reaction channel of the present invention can also use etching to form micro-channels on the substrate.
The temperature control plate S3 may be a heating plate, which can perform a heating operation to make the reaction temperature of the reaction channel S2 reach a target reaction temperature set by itself, such as an electric heating film, a resistance heating wire, a ceramic heating sheet, a carbon fiber heating sheet, a silica gel heating sheet, or other heating sheets; of course, the temperature control plate S3 may be a low-temperature cooling device such as a semiconductor cooling fin or a water-cooled heat sink.
The temperature sensor comprises an upper temperature sensor S41 and a lower temperature sensor S42, the lower temperature sensor S42 is arranged on the lower surface S12 of the substrate and is positioned between the substrate S1 and the temperature control plate S3, the lower temperature sensor S42 can be an integral temperature sensor which is directly attached to the lower surface of the substrate, and certainly in other embodiments, the lower temperature sensor S42 can also be distributed on the lower surface S12 of the substrate in an array arrangement mode by a plurality of sensors; the upper temperature sensors S41 are distributed on the upper surface S11 of the substrate and are disposed near the edge of the reaction channel.
In an embodiment, referring to fig. 1, a reaction channel S2 of a flow chemical reaction module is in a serpentine shape, the reaction channel S2 is embedded in a groove S10 on an upper surface of a substrate, an upper temperature sensor S41 is interposed between a reactant inlet S21 and a product outlet S22 of the reaction channel, the upper temperature sensor S41 is disposed near a main body of the reaction channel, the upper temperature sensor can transmit a sensed value to a control terminal through a main control module in real time, a temperature compensation calculation is performed by using the control terminal, and then the compensation value is transmitted to the main control module, so as to adjust power of the temperature control board.
Optionally, referring to fig. 1, a plurality of upper temperature sensors S41 are disposed around the upper surface S11 of the substrate, the upper temperature sensors S41 are disposed near the reaction channel S2, and the upper temperature sensors S41 are disposed at two sides of the reactant inlet S21 or the product outlet S22 of the reaction channel, the upper temperature sensors S41 are discretely disposed around the reaction channel S2, and are capable of performing multi-point measurement on the temperature near the reaction channel on the upper surface of the substrate, and sending the temperature values measured by the upper temperature sensors and the lower temperature sensors to the control terminal, the control terminal utilizes the average temperature value of the upper temperature sensors and the temperature value of the lower temperature sensors to determine the calculated difference of the temperatures in an operation period, and then performs temperature compensation calculation, so that the temperature in the reaction channel can approach the actually set temperature value infinitely, thereby ensuring that the reaction environment of the reaction channel reaches the set requirement, the product yield is improved; preferably, the upper temperature sensors S41 can be arranged on two sides of the reactant inlet S21 or the product outlet S22 in a multi-row array manner, and the temperature measurement points are increased to calculate the average value of the upper surface temperature, so that the temperature compensation adjustment is more accurate, and the reaction temperature in the reaction channel reaches the target set temperature.
Optionally, in another embodiment, referring to fig. 4, the reaction channel S2 is in a winding and bending shape, the reaction channel S2 is embedded in the groove S10 on the upper surface of the substrate, and the arrangement of other temperature sensors is similar to that of the above embodiment, and will not be repeated herein.
In an alternative embodiment, the panel matched with the substrate S1 is provided with shielding ink in the area corresponding to the arrangement position of the upper temperature sensor, and the shielding ink can hide the upper temperature sensor without affecting the observation of the reaction channel, so that the accuracy of equipment control can be improved while the appearance is ensured, and the yield is improved.
In another alternative embodiment, the substrate S1 is further provided with through holes (not shown) that can accommodate the wires of the upper temperature sensor to pass through, so as to lead the wires of the sensor to the lower surface of the substrate, and lead the wires from the same surface to the main control module.
Fig. 5 is a schematic diagram of the apparatus 100 in a flow chemical reaction module. The apparatus 100 is applied to synthesis of a continuous flow chemical reaction, which can precisely perform a continuous flow chemical reaction of various fluids in hardware, software and a combination thereof, with high safety, and can precisely control a reaction environment, thereby improving a product yield. The device 100 comprises the reaction module, a main control module 50 and a control terminal 51, wherein the reaction module can be in serial communication connection with a communication device by using RS485 or RS232, the reaction module is formed by arranging one or more temperature sensors on the upper surface and the lower surface of a substrate, the temperature sensors are connected into the main control module 50 by using wires, so that the temperature sensors can transmit temperature signals to the main control module 50, the main control module 50 processes the temperature signals received by the temperature sensors and outputs the signals to the control terminal 51 through the communication device (such as Bluetooth wireless communication, WiFi wireless communication, USB and the like); the control terminal 51 receives the input from the temperature sensors through the main control module 50, and responds to the input to execute the temperature compensation calculation action, the control terminal 51 may be a mobile phone, a tablet computer, and the like, the control terminal 51 may issue a command to the communication device through application software installed in a memory thereof, a display interface in the application software may include temperature parameters required for setting a mobile chemical reaction, so that each module can automatically control the reaction conditions according to the customized parameters, and meanwhile, the communication device can also transmit information in the device operation process to the control terminal in real time, thereby implementing human-computer interaction.
In addition to the basic software required for controlling the reaction environment of the reaction module, the memory of the control terminal further includes a software module capable of performing temperature difference compensation processing on the measured temperature difference received from the temperature sensor, the software module includes a temperature compensation calculation, and the control terminal is capable of performing the temperature compensation calculation by receiving the temperature values transmitted by the upper and lower temperature sensors and calculating the temperature difference therebetween, thereby deriving a temperature compensation value using the temperature difference therebetween. The temperature compensation calculation can be carried out, a temperature compensation value can be obtained by fitting or referring to a temperature compensation curve or a temperature compensation table preset by the software module based on the calculated temperature difference, and the temperature compensation value is sent to the main control module, so that the main control module can regulate and control the temperature adjusting plate according to the temperature compensation value; in another embodiment, the temperature compensation calculation can also be formulated to derive a temperature compensation value, and the algorithm can be adapted to derive from historical empirical data, for example.
Example one
Referring to fig. 6, the system having the above-described flow chemical reaction module performs the following steps:
step 101: obtaining a target reaction temperature parameter;
in this step, the user can set the required reaction temperature parameters in a self-defined manner at the control terminal, for example, the temperature T1 higher or lower than the ambient temperature is set in a self-defined manner, and the reaction temperature in the reaction channel is controlled by using an instruction control manner.
Step 102: the temperature sensor transmits the measured temperature information to the control terminal for many times to calculate the average temperature, and calculates the heating/cooling time t1 according to the difference between the target reaction temperature and the average temperature, and transmits the instruction to the main control module 50;
step 103: the main control module 50 starts the temperature control board S3 to continuously heat/cool within the heating/cooling time t1 according to the instruction content, and sends the temperature value measured by the temperature sensor to the control terminal 51 in real time through the main control module;
if the measured temperature value meets the target requirement, for example, the value of the lower temperature sensor has reached the target reaction temperature, step 104 is executed continuously; if the target requirement is not met, automatically sending alarm information to the control terminal 51, specifically, the control terminal 51 may further include an alarm for outputting an alarm signal when receiving alarm information that the temperature condition is abnormal, which is sent by the temperature sensor, where the alarm is, for example, a sound alarm, a light source alarm, or the like; if the reaction module does not reach the target reaction temperature condition within the heating/cooling time t1 or the information fed back by the sensor is not within the preset target control condition range, the main control module sends alarm information to the control terminal through the communication device, so that the user is prompted to check in time, the smooth proceeding of the reaction is ensured, and meanwhile, the service life of the equipment can be prolonged.
Step 104: after the heating/cooling is completed, the software module on the memory of the control terminal 51 performs temperature compensation calculation according to the temperature difference obtained by the calculation and measurement of the upper and lower temperature sensors, and transmits the calculated temperature compensation value to the main control module.
In this step, the substrate transmits the temperature values of the upper temperature sensor S41 (if the temperature sensors are a plurality of upper temperature sensors distributed discretely, the temperature values are transmitted to the control terminal for average calculation) and the lower temperature sensor S42 to the control terminal 51 to calculate the temperature difference therebetween, the software module on the memory of the control terminal 51 performs the temperature compensation calculation according to the temperature difference and transmits the temperature compensation value calculated by the control terminal to the main control module, the temperature control board S3 is automatically adjusted, for example, based on the calculated temperature compensation value, the main control module appropriately increases the power of the temperature control board, the temperature values measured by the upper and lower temperature sensors can be infinitely close to each other, the flow chemical reaction conditions are finely controlled, thereby ensuring that the target reaction temperature condition can be reached in the reaction channel, and the yield and the product quality of the final product can be well ensured.
Example two
Referring to fig. 7, the system having the above-described flow chemical reaction module performs the following steps:
step 201: acquiring a target reaction temperature parameter, a plurality of sectional heating temperatures and corresponding heat preservation time lengths;
in this step, the user can set the required reaction temperature parameters in a self-defined manner at the control terminal, for example, the target reaction temperature T1 higher or lower than the environmental temperature is set in a self-defined manner, and the reaction temperature in the reaction channel is controlled by using an instruction control manner. Meanwhile, the target reaction temperature is decomposed into a plurality of sectional heating temperatures and corresponding heat preservation time lengths, and stepped heating/cooling is realized to reach the target reaction temperature; for example, the target reaction temperature T1 is decomposed into multiple heating/cooling temperature steps, such as T01, T02, and T1, the multiple heating/cooling temperatures are sequentially and gradually heated/cooled until the target reaction temperature T1, the heat preservation time periods corresponding to the first two heating/cooling temperatures are T01 and T02, and when the target reaction temperature T1 is reached, the target reaction temperature is continuously maintained until the reaction is completed or new instruction content is obtained.
During the heating and holding phase of the first gradient (i.e. during the heating temperature gradient T01 and the holding time period T01), the following steps are performed:
step 202: the temperature sensor transmits the measured temperature information to the control terminal for multiple times to calculate the average temperature, and calculates the heating/cooling time of the stage according to the difference between the target reaction temperature and the average temperature, and transmits the instruction to the main control module 50;
step 203: the main control module 50 starts the temperature control board S3 to continuously heat/cool within the heating/cooling time according to the instruction content, and sends the temperature value measured by the temperature sensor to the control terminal 51 in real time through the main control module;
step 204: after the heating/cooling is completed, the software module on the memory of the control terminal 51 executes the temperature compensation calculation of the stage according to the temperature difference calculated after the measurement of the upper and lower temperature sensors, and transmits the calculated temperature compensation value to the main control module to control the reaction module to perform automatic adjustment.
Step 205: repeating the steps 202-204 until the temperature is increased/decreased to the target reaction temperature, and continuously maintaining the reaction environment of the target reaction temperature.
When the heating and heat preservation stages of the second gradient are repeatedly executed, the control terminal can directly calculate the heating/cooling time according to the temperature difference fitting between the temperature of the first gradient and the temperature of the second gradient, the target reaction temperature is reached in the multi-stage temperature correction, and the accuracy is high. In this embodiment, after the system is started, the system is sequentially heated/cooled according to the set multiple temperatures (e.g., T01, T02, and T1), and is kept at a preset temperature for a preset time period, and the temperature values are continuously corrected during the execution of the multiple temperatures until the target reaction temperature T1 is reached, so that the target reaction temperature T1 is decomposed into multiple temperatures and the instruction content is repeatedly executed, so that the temperature values measured by the upper and lower temperature sensors can be infinitely close to each other, thereby ensuring that the target reaction temperature condition can be reached in the reaction channel, finely controlling the flow chemical reaction conditions, being particularly suitable for the fluid reaction sensitive to the temperature conditions, and well ensuring the yield and the product quality of the final product. The multi-section temperature and the respective heat preservation time length thereof can be preset in the control terminal, can also be input and set by a user in a self-defined way, can be equally divided and set according to a certain rule, and can also be randomly set, and the software in the control terminal can realize the functions.
In a specific application device, referring to fig. 8, the device includes a liquid inlet module 1, a premixing connection member 2, a reaction module S and a main control module 50, the liquid inlet module 1 is sequentially communicated with liquid paths of the premixing connection member 2 and the reaction module S, and the liquid inlet module 1 and the reaction module 3 are connected to the main control module 50, the main control module 50 is, for example, an integrated circuit chip such as a microcontroller, a general processor or a digital signal processor, and the main control module is used for converting instruction content of a control terminal into automatic operation of a flow chemical module, so that the whole system can operate automatically.
The liquid inlet module 1 at least comprises a reactant container 11, a liquid injection device 12, an electromagnetic valve 13 and a liquid path channel 14, wherein the liquid path channel 14 comprises a first liquid inlet path 141, a second liquid inlet path 142 and an intermediate liquid path 143 after the two liquid inlet paths are converged, the first liquid inlet path 141 and the second liquid inlet path 142 are respectively and correspondingly connected to a first liquid injection device 121 and a second liquid injection device 122, the intermediate liquid path 143 flows mixed fluid into the reaction module S, and the intermediate liquid path 143 is connected with the first liquid inlet path and the second liquid inlet path through a premixing connecting piece 2; the first liquid inlet path 141 and the second liquid inlet path 142 are uniformly provided with electromagnetic valves 13, the electromagnetic valves 13 are three-way valves, and each path of the three-way valves is respectively communicated with the reactant container 11, the liquid injection device 12 and the premixing connecting piece 2. The liquid injection device 12, the electromagnetic valve 13 and the reaction module S are all connected to the main control module 50, and the liquid injection device 12, the electromagnetic valve 13 and the reaction module S are in communication connection with the communication device through serial ports, for example, the liquid injection device 12 and the reaction module S can be in serial communication connection with the communication device through RS485 or RS232, and the electromagnetic valve 13 is connected with the main control module through an I/O port; the injection device 12 is, for example, a syringe pump, which is used for pumping a medicine from a reactant container or extruding the medicine into a reaction module, and the syringe pump is composed of a driving mechanism (e.g., a motor), a screw rod, a slider and a syringe, wherein the slider is connected with the syringe, the driving mechanism drives the screw rod to rotate, and the slider on the screw rod moves, so that a piston of the syringe can be pulled to slide, and the medicine in the syringe can be pumped or extruded; of course, the liquid injection device can also be a peristaltic pump or a liquid chromatography pump.
Further, the premix connecting piece 2 at least includes a branch path one 21, a branch path two 22 and a main mixing path 23, the fluids of the branch path one 21 and the branch path two 22 are mixed in the main mixing path 23, one end of the main mixing path 23 is communicated with the fluids of the two branch paths, and the other end is communicated to the intermediate fluid path 143, in this embodiment, the premix connecting piece 2 is a Y-shaped valve body.
Referring to fig. 8, the reaction module S of the present invention is a flow chemistry pipeline module, the outlet of the intermediate liquid path 143 is connected to the reaction channel S2 of the flow chemistry for sufficient reaction, and the reacted substance flows into the collection container for collection; in this kind of application apparatus, this temperature control board S3 is connected to main control module and can carry out interactive communication with control terminal 51, the user accessible sets up temperature parameter information on control terminal 51, after system start-up operation, control terminal 51 can be with the information transport of temperature to main control module 50 on, main control module 50 starts temperature control board S3 and carries out the operation with the feed liquor module in proper order, namely after the system starts up, temperature control board S3 heats the reaction channel to target reaction temperature in advance, later, feed liquor module 1 starts the action of carrying out the feed liquor or synchronous feed liquor, after medicine in the feed liquor module 1 has got into the liquid or the synchronous feed liquor is premixed finishes, it directly gets into the reaction channel that has heated to appointed temperature, can begin to react, thereby can make various reactants fully react, effectively improve the productivity of product.
Optionally, a detection device (e.g., a spectrum detection device) may be further disposed at a product outlet of the reaction module S, the detection device is in communication connection with the control terminal through the main control module, the detection device can detect and analyze product information in real time, send the product detection information to the control terminal for display, and if the flowing substance does not meet the characteristic requirement of the target product, the flowing substance is directly discharged from a waste liquid channel of the liquid outlet solenoid valve; if the characteristic requirements of the target product are met, the product channel is switched to flow out of the product channel to the receiving bottle, and therefore the purity of the product is improved.
While the foregoing description shows and describes the preferred embodiments of the present invention, it is to be understood that the invention is not limited to the forms disclosed herein, but is not to be construed as excluding other embodiments and is capable of use in various other combinations, modifications, and environments and is capable of changes within the scope of the inventive concept as described herein, commensurate with the above teachings, or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A flow chemical reaction module is characterized by comprising a substrate, a reaction channel, a temperature control plate and a temperature sensor, wherein the reaction channel and the temperature control plate are respectively arranged on the upper surface and the lower surface of the substrate; the control terminal is provided with software for controlling the operation of the system, exchanges data with the main control module and processes and calculates the data, the processing and calculation of the data of the control terminal comprises temperature compensation calculation and transmits a temperature compensation value to the main control module.
2. A flow chemical reaction module as claimed in claim 1, wherein the temperature compensation is performed by the steps of:
step 101: obtaining a target reaction temperature parameter;
step 102: calculating heating/cooling time according to the difference between the target reaction temperature and the temperature measured by the temperature sensor in a fitting manner, and transmitting an instruction to the main control module;
step 103: starting the temperature control board to continuously heat/cool within the heating/cooling time, and transmitting the temperature value measured by the temperature sensor to the control terminal in real time through the main control module;
step 104: after the heating/cooling is finished, the software module executes temperature compensation calculation according to the temperature difference measured by the upper temperature sensor and the lower temperature sensor, and transmits the calculated temperature compensation value to the main control module.
3. The flow chemical reaction module as claimed in claim 2, wherein in step 103, if the measured temperature value meets the target requirement, the flow chemical reaction module proceeds to step 104; and if the target requirement is not met, automatically sending alarm information to the control terminal.
4. A flow chemical reaction module as claimed in claim 3, wherein the control terminal further comprises an alarm for outputting an alarm signal when receiving the alarm information of abnormal temperature condition sent by the temperature sensor.
5. A flow chemical reaction module as claimed in claim 1, wherein the temperature compensation is performed by the steps of:
step 201: acquiring target reaction temperature parameters, multi-section heating temperatures and corresponding heat preservation time lengths;
step 202: calculating heating/cooling time according to the difference fit between the reaction temperature of the first gradient and the temperature measured by the temperature sensor, and transmitting an instruction to the main control module;
step 203: starting the temperature control board to continuously heat/cool within the heating/cooling time, and transmitting the temperature value measured by the temperature sensor to the control terminal in real time through the main control module;
step 204: after the heating/cooling is finished, the software module executes temperature compensation calculation according to the temperature difference measured by the upper temperature sensor and the lower temperature sensor and transmits the calculated temperature compensation value to the main control module;
step 205: and (5) repeating the step 202 to the step 204 until the temperature is increased/decreased to the target reaction temperature and then maintaining the heat preservation state according to the set time length.
6. The flow chemical reaction module according to claim 5, wherein the plurality of heating temperatures and the corresponding holding time periods are preset in the software of the control terminal or are input by a user.
7. A flow chemical reaction module as claimed in claim 5, wherein the plurality of heating temperatures and the corresponding holding periods are equally spaced or randomly spaced.
8. The flow chemical reaction module of claim 1, wherein the substrate is formed with a groove, and the reaction channel is embedded in the groove; the reaction channel comprises a reactant inlet, a reaction channel main body and a product outlet, and the upper temperature sensor is clamped between the reactant inlet and the product outlet and is close to the reaction channel main body.
9. An automatic experimental device is characterized by comprising a liquid inlet module and the flowing chemical reaction module according to any one of claims 1 to 8, wherein a control terminal sends an instruction to a main control module, and the main control module sends the instruction to the liquid inlet module and the flowing chemical reaction module through serial ports; the flow chemical reaction module heats/cools the reaction channel to a target reaction temperature in advance, and then the liquid inlet module starts to feed liquid or synchronously feed liquid.
10. An automated experimental device according to claim 9, wherein a liquid injection device and an electromagnetic valve are respectively disposed on the first liquid inlet path and the second liquid inlet path of the liquid inlet module, and the liquid injection device is used for feeding a reactant or pressing the reactant into the flowing chemical reaction module; and the liquid injection device and the electromagnetic valve are connected to the main control module.
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| CN202210165116.5A CN114452913A (en) | 2022-02-23 | 2022-02-23 | Flow chemical reaction module and automatic experimental device thereof |
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| CN202210165116.5A CN114452913A (en) | 2022-02-23 | 2022-02-23 | Flow chemical reaction module and automatic experimental device thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN119336091A (en) * | 2024-10-17 | 2025-01-21 | 深圳市艾克斯电子仪器设备有限公司 | Temperature control method, system, equipment and medium for high-low temperature and low-pressure test chamber |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2609476A1 (en) * | 2010-08-23 | 2013-07-03 | Life Technologies Corporation | Temperature control of chemical detection system |
| CN107894720A (en) * | 2017-11-23 | 2018-04-10 | 厦门芯曙光科技有限公司 | A kind of multifactor integrated control system of more pumps of syringe pump |
| CN109634321A (en) * | 2018-12-31 | 2019-04-16 | 西安优耐特容器制造有限公司 | Precise temperature control system and method suitable for micro- reaction experiment |
-
2022
- 2022-02-23 CN CN202210165116.5A patent/CN114452913A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2609476A1 (en) * | 2010-08-23 | 2013-07-03 | Life Technologies Corporation | Temperature control of chemical detection system |
| CN107894720A (en) * | 2017-11-23 | 2018-04-10 | 厦门芯曙光科技有限公司 | A kind of multifactor integrated control system of more pumps of syringe pump |
| CN109634321A (en) * | 2018-12-31 | 2019-04-16 | 西安优耐特容器制造有限公司 | Precise temperature control system and method suitable for micro- reaction experiment |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN119336091A (en) * | 2024-10-17 | 2025-01-21 | 深圳市艾克斯电子仪器设备有限公司 | Temperature control method, system, equipment and medium for high-low temperature and low-pressure test chamber |
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Application publication date: 20220510 |