Intelligent organic synthesis device and implementation method
The intelligent organic synthesis device realizes full-process automation, which solves the problems of cumbersome operation, time-consuming and instability of traditional organic synthesis experiments, improves synthesis efficiency and product quality, and is suitable for university teaching and industrial production.
Patent Information
- Application Number
- CN202510941442.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-09
- Publication Date
- 2025-10-10
AI Technical Summary
Traditional organic synthesis experiments are cumbersome, time-consuming, and require a lot of manual labor, resulting in unstable synthesis results and making it difficult to achieve standardization and large-scale production.
An intelligent organic synthesis device is designed, including a core control module, a solid-liquid separation module, and a chemical synthesis module. A single-chip microcomputer controls fluid delivery and reaction conditions to achieve fully automated operation. Servo motors and stepper motors are used to precisely add reactants, and a heated magnetic stirrer and vacuum pump are used to control reactions and separate products.
It realizes the automation and precision of the organic synthesis process, improves the synthesis efficiency and product quality, reduces manual operation errors, and is suitable for university teaching, scientific research and industrial production.
Smart Images

Figure CN120754800A_ABST
Abstract
Description
Technical Field
[0001] The present invention belongs to the field of chemical organic synthesis and relates to an intelligent synthesizer based on automated control and an implementation method thereof, aiming to realize automation, precision and efficiency of the chemical organic synthesis process through integrated hardware equipment and intelligent software programs. Background Art
[0002] Organic synthesis refers to the process of preparing complex target molecules from relatively simple molecules through the rational design of a series of organic chemical reaction routes. Its primary purpose is to synthesize various new intermediates, pharmaceuticals, new materials, new catalysts, specialty solvents, polymer monomers, high-energy fuels, and more. Organic synthesis can be divided into basic organic synthesis and fine organic synthesis. Fine organic synthesis involves the synthesis of complex molecules from simpler reactants, such as chemical reagents, pharmaceuticals, pesticides, dyes, fragrances, and detergents.
[0003] Organic synthesis experiments are a crucial component of university chemistry teaching, fostering students' practical skills and innovative thinking. However, traditional experimental teaching methods still suffer from numerous issues, such as cumbersome procedures, time-consuming procedures, and unstable student operation. These issues limit students' understanding and mastery of organic synthesis experiments, hindering the effectiveness of experimental teaching.
[0004] However, the existing chemical organic synthesis technology solutions have many shortcomings and deficiencies, as follows:
[0005] Complicated operations: Traditional organic synthesis processes require precise manual manipulation of multiple steps, including the precise measurement and transfer of liquids, the accurate addition of solid reagents, and strict control of reaction conditions. For example, in a multi-step reaction, each step requires manual manipulation, and each step must strictly follow the experimental procedures, otherwise the experiment may fail.
[0006] Time-consuming: Organic synthesis processes typically involve multiple reaction steps, each of which requires a certain amount of time to complete. For example, the entire process, from reagent preparation to isolation and purification of the final product, can take hours or even days. In university laboratory teaching, students often cannot complete complex synthesis experiments due to limited experimental time.
[0007] High manual involvement: Traditional synthesis processes require manual intervention at every step, which not only increases labor intensity but can also lead to poor experimental reproducibility and unstable results. The experience and operating habits of different operators can affect experimental results, making standardization and large-scale production difficult.
[0008] Unstable synthesis results: Due to the limitations of manual operation, it is difficult to accurately control the reaction conditions (such as temperature, stirring speed, reaction time, etc.), resulting in unstable purity and yield of the synthetic products.
[0009] In summary, existing chemical organic synthesis technology solutions have obvious deficiencies in terms of operational convenience, synthesis efficiency, stability, and manual participation. The present invention provides a more efficient, precise, and stable automated organic synthesis device and method. Summary of the Invention
[0010] To overcome the shortcomings of the aforementioned technologies, the present invention provides an intelligent organic synthesis device and method, offering significant advantages such as high automation, precise control, high efficiency, rapidity, strong scalability, intelligent operation, and data recording and analysis. This device automates the entire process of chemical organic synthesis, improves the stability of synthetic results, shortens experimental cycles, and lowers the experimental threshold. It is widely applicable to university teaching, scientific research, and industrial production.
[0011] In order to achieve the above object, the technical solution adopted by the present invention is:
[0012] An intelligent organic synthesis device comprises three parts: a core control module, a solid-liquid separation module, and a chemical synthesis module. The core control module serves as the control center of the entire device, enabling precise fluid delivery and reaction control during chemical organic synthesis. The solid-liquid separation module is where the reaction products are refined and separated. A vacuum pump 21 creates an air pressure differential within a sand core funnel 22, allowing the liquid to flow through the sand core into a collection bottle 24, while the solid remains within the sand core funnel 22, achieving solid-liquid separation. The chemical synthesis module is the core module for chemical synthesis, utilizing a heated magnetic stirrer 25 to provide heating and stirring reaction conditions for chemical synthesis.
[0013] The core control module includes: an organic synthesis device housing 1, a single-chip microcomputer 2, a servo motor controller 3, an analog-to-digital conversion device 4, an electromagnetic relay 5, a DC motor controller 6, a servo motor 11, a stepper motor slide 16, a stepper motor closed-loop controller 17, a power connector and switch 7, a BNC connector 8, an IEC C14 interface 9, an aviation interface 10, a servo motor valve coupling 12, a syringe 13, a multi-valve 14, a double-threaded Luer connector 15, a syringe push rod clamp 18, and multiple reagent bottles 28 located outside the organic synthesis device housing 1. Specifically:
[0014] The organic synthesis device shell 1 is made of PLA material, and is a whole inverted T-shaped, consisting of a horizontal part and a vertical part. The vertical part of the T-shaped is provided with a square hole for passing through the syringe push rod clamp 18 and a crescent syringe shell clamp for fixing the syringe 13, the curvature of the syringe shell clamp closely fits the curvature of the syringe 13 shell, and the shell of the syringe 13 can be fixed relative to the organic synthesis device shell 1 to be stationary. The horizontal part of the T-shaped has N square holes in front, for fixing N servo motors 11.
[0015] The stepping motor sliding table 16 is composed of a stepping motor, a lead screw, a sliding table, an I-shaped steel and a frame. The frame of the stepping motor sliding table 16 is vertically fixed in the vertical part of the organic synthesis device shell 1 by screws, and the stepping motor of the stepping motor sliding table 16 needs to be kept downward. The sliding table of the stepping motor sliding table 16 has a moving range corresponding to the position of the square hole of the vertical part of the organic synthesis device shell 1. The lead screw is installed in the stepping motor as a rotating shaft of the stepping motor, and rotates when the stepping motor receives a control signal. The sliding table moves up and down when the lead screw rotates. The sliding table of the stepping motor sliding table 16 has a side opposite to the position of the square hole of the vertical part of the organic synthesis device shell 1, and the syringe push rod clamp 18 is fixed on the side by screws, so that the syringe push rod clamp 18 can move synchronously with the stepping motor sliding table 16. The syringe push rod clamp 18 passes through the larger square hole of the organic synthesis device shell 1 to the outside of the instrument.
[0016] The stepping motor closed-loop controller 17 is fixed on the stepping motor of the stepping motor sliding table 16 by screws, connected with the stepping motor through a 4P communication line, and connected with the single-chip microcomputer 2 through an 8pXh2.54 line to receive. The stepping motor closed-loop controller 17 has a magnet adhered to the end of the lead screw, and can judge the actual rotating angle of the lead screw by measuring the magnetic force direction of the magnet when the lead screw rotates, so as to perform real-time monitoring and compensation.
[0017] The syringe 13 is a plastic syringe with a luer female thread port at the outlet. The shell of the syringe 13 is fixed on the syringe shell clamp of the organic synthesis device shell 1, the push rod of the syringe 13 is fixed on the syringe push rod clamp 18, and can move synchronously with the syringe push rod clamp 18. The luer female thread port of the syringe 13 is installed on one of the luer male thread ports of the 14 ten-way valve. When the push rod of the syringe 13 moves upward under the driving of the stepping motor sliding table 16, the fluid is drawn into the syringe 13 from the outlet; when the push rod of the syringe 13 moves downward under the driving of the stepping motor sliding table 16, the fluid is pushed out of the syringe 13 from the outlet; and the pulling and pushing action of the syringe 13 can realize the movement of the fluid.
[0018] The servo motors 11 are MG996R-180-degree servo motors, and there are N of them. Each servo motor 11 has four screw holes on the top and bottom, and is fixed from the inside with screws into a square hole on the front of the horizontal portion of the organic synthesis device housing 1. The N servo motors correspond one-to-one with the N smaller square holes on the front of the horizontal portion of the organic synthesis device housing 1.
[0019] The servo motor valve couplings 12 are made of plastic, and there are N of them. Each servo motor valve coupling 12 has a T-shaped groove on one side that nests with a T-shaped handle on the piston of the multi-valve 14. The other side has a groove with a gear pattern that nests on the rotating shaft of the servo motor 11 and is secured with screws. When the servo motor 11 receives a signal to rotate its shaft, the servo motor valve coupling 12 drives the cylindrical piston of the multi-valve 14 to rotate, thereby changing the connection state of the corresponding piston and controlling the connection between the plastic syringe 13 and a specific port of the multi-valve 14.
[0020] The multi-valve 14 consists of N three-way valves connected horizontally via double-threaded Luer connectors 15. Each of the N three-way valves corresponds to N servo motors 11 and N servo motor valve couplings 12. Each three-way valve consists of an inverted T-shaped plastic pipe. Each of the three pipes has a Luer connector at the outlet. The upper pipe of each three-way valve is used to connect to other equipment, while the left and right pipes are used to connect to other three-way valves. The left and right channels of the leftmost and rightmost three-way valves can also be connected to other equipment. Each three-way valve has a cylindrical plastic piston in the middle. The piston has a T-shaped handle that extends out of the valve and fits into the T-shaped groove of the servo motor valve coupling 12. When the piston of each three-way valve is rotated to a specific angle, two or three of the three pipes in the three-way valve can be connected to each other. Each servo motor 11 controls the connection between the three pipes within the three-way valve by rotating its corresponding servo motor valve coupling 12. In order to allow liquid to be transferred between the two channels, any two channels of the multi-valve 14 can be connected. To achieve this purpose, the three-way valve piston where the left channel to be connected is located needs to be turned to a state where the upper channel and the right channel of the three-way valve are connected, and the three-way valve piston where the right channel to be connected is located needs to be turned to a state where the upper channel and the left channel of the three-way valve are connected, and the three-way valve between the two channels to be connected is turned to a state where the left and right are connected. The entire multivalve 14 has a total of N+2 channels, which are divided into the following categories according to the different containers connected: 1 syringe channel, directly connected to the syringe pump, used to control the flow of liquid into and out of syringe 13; 1 sand core funnel channel, which enters sand core funnel 22 through the small hole in sand core funnel cover 23 and is used to input liquid into sand core funnel 22; 1 collection bottle channel, connected to the branch at the bottom of the collection bottle, used to extract filtrate from collection bottle 24; 1 reaction bottle channel, connected to the side branch of reaction bottle 27, used to provide a channel for liquid to enter and exit reaction bottle 27; multiple reagent bottle channels, which enter reagent bottle 28 through the small hole on the reagent bottle 28 and are used to extract reagents from reagent bottle 28. When the channel connected to syringe 13 is connected to any channel, the syringe 13 is drawn in or out of the channel.
[0021] The servo motor controller 3 is installed on the leftmost side of the horizontal interior of the organic synthesis device housing 1 (as viewed from the front), behind the N servo motors 11. The positive power supply of the servo motor controller 3 is connected to the positive terminal of the power connector and switch 7, and the negative power supply is connected to the negative terminal of the power connector and switch 7. The servo motor controller 3 has 16 servo motor interfaces that can be connected to the N servo motors 11 and control the rotation angle of the servo motors 11 via electrical signals. The 40 pins on the servo motor controller 3 are used to install the single-chip microcomputer 2. The servo motor controller 3 also has multiple sets of 5V power supply interfaces to power other electronic devices.
[0022] The single-chip microcomputer 2 is installed on the servo motor controller 3 through 40 pins on the servo motor controller 3; the single-chip microcomputer 2 is connected to the stepper motor closed-loop controller 17 using an 8pXH2.54 connecting line, and controls the movement of the stepper motor slide 16 through electrical signals; the single-chip microcomputer 2 is connected to the analog-to-digital conversion device 4 through a DuPont line to read the potential signal measured by the potential measuring probe 20; the single-chip microcomputer 2 is connected to the electromagnetic relay 5 through a DuPont line to control the power switch of the vacuum pump 21; the single-chip microcomputer 2 is connected to the DC motor controller 6 through the DuPont line to send an electrical signal to the DC motor controller 6 to control the operation of the top stirring 19.
[0023] The analog-to-digital converter 4 is mounted within the horizontal interior of the organic synthesis apparatus housing 1, to the right of the servo motor controller 3. Its communication interface is connected to the microcontroller 2 via a DuPont cable, and its signal interface is connected to the positive and negative terminals of a BNC connector 8. The analog-to-digital converter 4 receives the potential signal transmitted from the BNC connector 8 and converts it into a digital signal, which is then transmitted to the microcontroller 2.
[0024] The electromagnetic relay 5 is an electronic component that combines the functions of a photocoupler and a relay, primarily used to achieve electrical isolation and signal transmission between the input and output circuits. The electromagnetic relay 5 is installed inside the horizontal interior of the organic synthesis device housing 1, to the right of the analog-to-digital converter 4. The positive and negative power terminals of the electromagnetic relay 5 are connected to a set of 5V power interfaces on the servo motor controller 3. The signal terminal of the electromagnetic relay 5 is connected to the microcontroller 2 via a DuPont cable. The control terminal of the electromagnetic relay 5 is connected to two terminals of the IEC C14 interface 9. When GPIO pin 12 of the microcontroller 2 outputs a high level, the NO / CO terminals of the electromagnetic relay 5 are closed, connecting the circuit of the IEC C14 interface 9.
[0025] The DC motor controller 6 is a MOSFET-based dual H-bridge DC motor drive module capable of bidirectional control. It is installed to the right of the electromagnetic relay 5 within the organic synthesis apparatus housing 1. The positive and negative power terminals of the DC motor controller 6 are connected to a set of 5V power interfaces on the servo motor controller 3. The signal terminals of the DC motor controller 6 are connected to the microcontroller 2 via DuPont cables. The control terminals of the DC motor controller 6 are connected to the overhead stirrer 19 via an aviation interface 10. The duty cycle of the output electrical signal from the microcontroller 2 adjusts the magnitude and direction of the current supplied by the DC motor controller 6 to the overhead stirrer 19, thereby adjusting the rotational direction and speed of the DC motor in the overhead stirrer 19.
[0026] The power connector and switch 7, BNC connector 8, IEC C14 port 9, and aviation port 10 are installed on the back panel of the organic synthesis device housing 1, in order from right to left. The power connector and switch 7 includes a 2.5x5.5 DC power connector and a power switch. An external 12V power supply powers the entire device through the power connector and switch 7. The BNC connector 8 has a standard BNC connector and is connected to the potential measurement probe 20. The IEC C14 port 9 is connected to the vacuum pump 21 and controls the vacuum pump's on / off state by switching the circuit on and off. The aviation port 10 is connected to the overhead stirrer 19 of the solid-liquid separation module.
[0027] Reagent bottles 28 are standard glass reagent bottles filled with liquid reagents and equipped with liquid piping. Multiple reagent bottles are placed outside the organic synthesis apparatus housing 1. Each reagent bottle 28 has a small hole in its lid, through which a liquid piping passes. One end of the piping extends into the reagent inside the bottle 28, and the other end connects to one of the reagent bottle channels of the multi-valve 14 via a Luer connector. The number, volume, and connection locations of these bottles should be determined based on the specific experimental requirements.
[0028] The solid-liquid separation module includes: an overhead stirrer 19, a potential measurement probe 20, a vacuum pump 21, a sand core funnel 22, a sand core funnel cover 23, and a collection bottle 24. Specifically:
[0029] The top stirring device 19 includes a micro DC motor and a polytetrafluoroethylene stirring rod. The power cord of the micro DC motor is connected to the aviation interface 10 of the aforementioned core control module, and then connected to the control terminal of the DC motor controller 6. The rotating shaft of the micro DC motor is connected to the polytetrafluoroethylene stirring rod, and the blades of the polytetrafluoroethylene stirring rod pass through the sand core funnel cover 23 and extend into the sand core funnel 22. The top stirring device 19 is installed at the top of the entire solid-liquid separation module through a clamp. After the top stirring device 19 receives the electrical signal from the DC motor controller 6 through the aviation interface 10, the DC motor starts to rotate and drives the polytetrafluoroethylene stirring rod to rotate, and the blades can stir the liquid in the sand core funnel 22.
[0030] The sand core funnel 22 is a glass sand core filtration funnel. The size and sand core specifications can be adjusted according to the volume and characteristics of the solution required for the experiment. The sand core funnel 22 is installed below the overhead stirring device 19. The sand core funnel 22 has a sleeve at the bottom. The inner side of the sleeve is a liquid passage. The upper end is connected to the sand core of the sand core funnel 22, and the lower end extends into the collection bottle 24. The liquid filtered from the sand core funnel 22 flows into the collection bottle through the liquid passage. The outer side of the sleeve is a gas passage. The gas passage is generally in a horizontal T-shape. The upper end of the gas passage is sealed, and the lower end is connected to the upper ground joint of the collection bottle 24 through a ground joint. The horizontal branch serves as the filtration branch and is connected to the air inlet of the vacuum pump 21 through a hose. When the power of the vacuum pump 21 is turned on, the vacuum pump 21 will draw air from the gas passage of the sand core funnel 22, and a pressure difference will be formed above and below the sand core of the sand core funnel 22. Under the action of the pressure difference, the liquid in the sand core funnel 22 will pass through the sand core and flow into the collection bottle 24 through the liquid passage. The solid in the sand core funnel 22 will remain in the sand core funnel because it cannot pass through the sand core, thereby achieving the purpose of solid-liquid separation.
[0031] The sand core funnel cover 23 has three holes and a bracket, and covers the sand core funnel 22. The smallest hole in the sand core funnel cover 23 allows for a liquid pipeline to pass through. The other end of this pipeline is connected to the sand core funnel channel of the multi-valve 14 via a Luer connector, providing a conduit for liquid to enter the sand core funnel 22. The middle hole in the sand core funnel cover 23 allows for the insertion of a polytetrafluoroethylene stirring rod used for the top stirrer 19. The hole in the sand core funnel cover 23 with the bracket allows for the insertion of a potential measuring probe 20, allowing the measuring end of the potential measuring probe 20 to extend into the liquid in the sand core funnel 22.
[0032] The potential measuring probe 20 can be replaced with different probes according to different experiments. The potential measuring probe 20 transmits the potential signal to the single chip microcomputer 2 through the BNC connector 8, thereby determining whether the reaction conditions are met.
[0033] The collection flask 24 is a glass round-bottom flask with an additional branch at the bottom. It is installed below the sand core funnel 22 and tightly connected to the clamping tube of the sand core funnel 22 via a standard ground joint. The additional connection at the bottom of the collection flask 24 is a hollow glass tube, which is connected to the liquid pipeline. The other end of this pipeline is connected to the collection flask channel of the multi-valve 14, providing a channel for liquid to flow out of the collection flask 24. The main function of the collection flask 24 is to collect the liquid separated from the sand core funnel 22.
[0034] The chemical synthesis module includes: a heating magnetic stirrer 25, a metal bath module 26, and a reaction bottle 27. Specifically:
[0035] The heating magnetic stirrer 25 is a heated disk magnetic stirrer located at the bottom of the chemical synthesis module and placed on the table. The heating magnetic stirrer 25 is connected to the computer via an RS232 serial port. The computer controls the heating magnetic stirrer 25 through communication commands to perform heating or stirring operations, providing reaction conditions for chemical synthesis.
[0036] The metal bath module 26 is made of aluminum alloy, with one flat surface and a semicircular groove on the other. The flat surface is placed on the heating plate of the heating magnetic stirrer 25. The metal bath module 26 has excellent thermal conductivity, enabling rapid heat transfer to the reaction flask 27. Its light weight makes it easy to operate and replace.
[0037] The reaction flask 27 is a glass round-bottom flask with a side branch, which is placed in the semicircular groove of the metal bath module 26. There is a larger flask mouth on the top of the reaction flask 27 for manually adding reagents. The side branch of the reaction flask 27 is connected to a liquid pipeline, and the other end of this pipeline is connected to the reaction flask channel of the multi-valve 14 to provide a pipeline for liquid to enter and exit the reaction flask 27. The reaction flask 27 is the place where the organic synthesis reaction mainly occurs. Each reactant enters the reaction flask 27 through the side branch or the top circular hole, and a chemical reaction occurs under the action of the heating type magnetic stirrer 25. The reaction product then leaves the reaction flask through the side branch.
[0038] An intelligent organic synthesis method is implemented based on the above-mentioned intelligent organic synthesis device. This method controls the servo motor 11 and the stepper motor slide 16 through computer instructions, and accurately adds the reactants to the reaction bottle 27 in proportion. Subsequently, the heating magnetic stirrer 25 is started to provide suitable temperature and stirring conditions for the reaction according to preset parameters. The single-chip microcomputer 2 automatically adjusts the parameters according to the potential signal collected by the potential measurement probe 20 to ensure that the reaction proceeds smoothly. After the reaction is completed, the reaction product is transferred to the sand core funnel 22, and the product is separated and collected by the vacuum pump 21 and the sand core funnel 22. The entire process is precisely controlled by the computer and the single-chip microcomputer 2 to achieve automation and precision of organic synthesis, improve synthesis efficiency and product quality, reduce manual operation errors, and is suitable for a variety of organic synthesis experimental scenarios. The specific number of X in this method needs to be determined according to the specific reaction process. The specific method includes the following steps:
[0039] Step 1: Experimental preparation. Design a detailed experimental process and clearly define the reagent bottles or equipment connected to each channel of the multi-valve 14. Prepare high-purity, appropriate amounts of various reagents and place them in the corresponding reagent bottles 28. According to the experimental plan, use liquid pipelines to connect multiple reagent bottles to the reagent bottle channels of the multi-valve 14, with each reagent bottle corresponding to a reagent bottle channel, ensuring that the connections are secure and leak-free. At the same time, connect the side branch of the reaction bottle 27 to the reaction bottle channel of the multi-valve 14 through a liquid pipeline to facilitate the flow of liquid. Use a liquid pipeline to connect the small hole on the sand core funnel cover 23 to the sand core funnel passage of the multi-valve. Connect the branch of the sleeve of the sand core funnel 22 to the air inlet of the vacuum pump 21. Connect the additional interface of the collection bottle 24 to a channel of the multi-valve 14 through a liquid pipeline for liquid outflow. Connect the potential measurement probe 20 to the BNC connector 8, the power cord of the vacuum pump 21 to the IEC C14 interface 9, the overhead stirrer 19 to the aviation interface 10, and the 12V power supply to the power connector and switch 7. Connect the heated magnetic stirrer 25 to the computer using an RS232 serial cable. Turn on the power switch of the intelligent organic synthesis device and allow the device to preheat for 5 minutes. Finally, connect the microcontroller 2 to the computer using a MicroUSB data cable to prepare for subsequent automated control.
[0040] The second step is to add the reactants. The computer sends instructions to the single-chip microcomputer 2, precisely driving the servo motor 11, causing the piston of the multi-valve 14 to rotate until the desired reagent bottle channel containing the raw materials is connected to the syringe 13. Simultaneously, the stepper motor slide 16 is controlled to drive the syringe push rod upward, accurately extracting X milliliters of raw materials from the reagent bottle 28. Then, the servo motor 11 is controlled again to rotate the piston of the multi-valve 14 until the reaction bottle 27 is connected to the syringe 13. The stepper motor slide 16 is controlled to drive the syringe push rod downward, injecting the extracted raw materials into the reaction bottle 27. This process is repeated until all the raw materials have been added to the reaction bottle 27. The remaining raw materials are then manually added to the reaction bottle 27 through the flask opening at the top of the reaction bottle 27.
[0041] The third step is to start the reaction. After confirming that all reactants have been accurately added to the reaction bottle 27, send an instruction to start the heating magnetic stirrer 25. According to the pre-set parameters, the heating magnetic stirrer 25 starts to heat the reaction bottle 27 and stirs it at a set speed to provide a suitable temperature and sufficient mixing conditions for the organic synthesis reaction. At the same time, the single-chip microcomputer 2 monitors the working status of the heating magnetic stirrer in real time to ensure that it operates stably according to the preset parameters. Throughout the reaction process, the set heating and stirring conditions are continuously maintained to ensure that the reaction can proceed smoothly and efficiently until the reaction reaches the predetermined time or conditions.
[0042] The fourth step is to separate and collect the products. After the reaction is completed, the computer sends an instruction to the single-chip microcomputer 2, causing the servo motor 11 to drive the piston of the multi-valve 14 to rotate, connecting the reagent bottle channel connected to the precipitate with the channel where the syringe 13 is located, controlling the stepper motor slide 16 to drive the syringe 13 push rod to move upward, and extracting X milliliters of precipitate. Then, the servo motor 11 drives the piston of the multi-valve 14 to rotate, connecting the syringe 13 with the sand core funnel 22, controlling the stepper motor slide 16 to drive the syringe 13 push rod to move downward, and adding X milliliters of precipitate to the sand core funnel 22. Next, using the same method, all the reaction products are extracted from the reaction bottle 27 and added to the sand core funnel 22. Turn on the overhead stirring 19 and stir for 100 seconds to fully mix the liquid in the sand core funnel 22, cool it, and precipitate the crude product. The vacuum pump 21 is then started, and the pressure difference generated by the filtration branch of the sand core funnel 22 causes the liquid in the sand core funnel 22 to pass through the sand core of the sand core funnel 22 and enter the collection bottle 24, while the solid crude product remains in the sand core funnel 22, achieving solid-liquid separation. At this point, the separation and collection of the crude product are completed.
[0043] The 5th step is to purify the product. After completing solid-liquid separation and collecting the crude product, if the purity of the product is further improved, purification methods such as recrystallization can be adopted. The specific operation is as follows: first, the servo motor 11 drives the piston of the multi-valve 14 to rotate, and the collection bottle 24 is connected to the channel where the syringe 13 is located, and the stepper motor slide 16 is controlled to drive the syringe 13 push rods to move upward, and the filtrate is all extracted. Then, the filtrate is discharged into the waste liquid bottle in the same way. Subsequently, the reagent bottle channel connected with the alkaline reagent extracts X milliliters of alkaline reagent, adds it to the sand core funnel 22, opens and tops up and stirs, and the solid product is fully dissolved, and then starts the vacuum pump 21, and the solution containing the product is allowed to enter the collection bottle 24, and the solid impurities are left in the sand core funnel 22.
[0044] The product-containing solution is withdrawn from the collection flask 24 using the same method and temporarily added to the reaction flask 27. X ml of cleaning solution is then withdrawn from the cleaning fluid channel using the same method and added to the sand core funnel 22. Overhead stirring 19 is activated to redissolve the solid impurities remaining in the sand core funnel 22. The vacuum pump 21 is then activated to allow the liquid in the sand core funnel 22 to enter the collection flask 24. The impurity-containing solution is then withdrawn from the collection flask 24 using the same method and then discharged into a waste liquid bottle.
[0045] Subsequently, the reaction product is extracted from the reaction bottle 27 and added to the sand core funnel 22. The reagent bottle channel connected to the pH adjusting reagent extracts X milliliters of pH adjusting solution and gradually adds it to the sand core funnel 22. During this process, the top stirrer 19 starts stirring, and the potential measuring probe 20 continuously monitors the potential change of the solution. The single chip computer 2 determines the pH value of the solution in the sand core funnel 22 based on the potential change. When the pH value of the solution in the sand core funnel 22 meets the set conditions, the addition of the pH adjusting reagent is stopped, and the remaining pH adjusting reagent in the syringe 13 is discharged into the waste liquid bottle of channel 10.
[0046] Wait 100 seconds to allow the refined product in sand core funnel 22 to reprecipitate. Then start vacuum pump 21 and utilize the suction filtration branch of sand core funnel 22 to generate an air pressure differential, allowing the liquid in sand core funnel 22 to pass through the sand core of sand core funnel 22 and enter collection bottle 24, while the refined aspirin solid product remains in sand core funnel 22, achieving solid-liquid separation. The filtrate is completely withdrawn from collection bottle 24. Then, using the same method, the filtrate is discharged into a waste liquid bottle. After waiting for the refined product in sand core funnel 22 to dry naturally, an intelligent organic synthesis method is completed.
[0047] The beneficial effects of the present invention are:
[0048] The present invention can realize the full process automation operation of chemical organic synthesis process, greatly improving synthesis efficiency and product quality. The present invention can accurately control the addition of reactants, the maintenance of reaction conditions and the separation and purification of products, effectively avoiding the errors and instability caused by human factors in traditional manual operations, and significantly improving the repeatability and reliability of the experiment. At the same time, its modular design makes the device have strong scalability and can be flexibly configured and upgraded according to different experimental requirements. The present invention provides great convenience for experimenters, lowers the experimental threshold, is particularly suitable for fields such as university teaching, scientific research and industrial production, and helps to promote the further development and application of organic synthesis technology. BRIEF DESCRIPTION OF THE DRAWINGS
[0049] Figure 1 This is the internal assembly diagram of the core control module of the device of the present invention (rear side).
[0050] Figure 2 This is the external assembly diagram (rear side) of the core control module of the device of the present invention.
[0051] Figure 3 This is the internal assembly diagram of the core control module of the device of the present invention (front side).
[0052] Figure 4 This is the external assembly diagram (front side) of the core control module of the device of the present invention.
[0053] Figure 5It is a partial enlarged view of the multi-valve device of the present invention.
[0054] Figure 6 This is an assembly diagram of the solid-liquid separation module of the device of the present invention.
[0055] Figure 7 This is an assembly diagram of the chemical synthesis module of the device of the present invention.
[0056] Figure 8 Schematic diagram of the intelligent organic synthesis method of the present invention.
[0057] In the figure: 1. Organic synthesis device housing; 2. Single-chip microcomputer; 3. Servo motor controller; 4. Analog-to-digital converter; 5. Electromagnetic relay; 6. DC motor controller; 7. Power connector and switch; 8. BNC connector; 9. IEC C14 interface; 10. Aviation interface; 11. Servo motor; 12. Servo motor valve coupling; 13. Syringe; 14. Multi-valve; 15. Double-threaded Luer connector; 16. Stepper motor slide; 17. Stepper motor closed-loop controller; 18. Syringe plunger fixture; 19. Overhead stirring; 20. Potentiometer probe; 21. Vacuum pump; 22. Sand core funnel; 23. Sand core funnel cover; 24. Collection bottle; 25. Heating magnetic stirrer; 26. Metal bath module; 27. Reaction bottle; 28. Reagent bottles (multiple). DETAILED DESCRIPTION
[0058] To make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described aspirin intelligent organic synthesis embodiment is a part of the embodiment of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.
[0059] This embodiment is a specific implementation method of synthesizing aspirin using an intelligent organic synthesis device.
[0060] Figure 1 、 Figure 2 、 Figure 3 、 Figure 4This is an assembly diagram of the core control module of the device of the present invention. As shown, the core control module of this embodiment includes: organic synthesis device housing 1, single-chip microcomputer 2, servo motor controller 3, analog-to-digital converter 4, electromagnetic relay 5, DC motor controller 6, power connector and switch 7, BNC connector 8, IEC C14 interface 9, aviation interface 10, servo motor 11, servo motor three-way valve connector 12, syringe 13, multi-valve 14, double-threaded Luer connector 15, stepper motor slide 16, stepper motor closed-loop controller 17, and syringe plunger fixture 18. The core control module of this embodiment is the central nervous system of the entire intelligent organic synthesis device, responsible for precisely controlling and coordinating the operation of various components. The organic synthesis device housing 1 provides physical support and protection for the module. The integrated single-chip microcomputer 2 serves as the core controller, receiving computer commands and connecting and controlling other devices through its pins. The servo motor controller 3 drives the servo motor 11, which precisely controls the piston rotation of the multi-valve 14 through the servo motor three-way valve connector 12, achieving fluid transfer between different channels. In this embodiment, the multi-valve 14 is composed of 10 three-way valves, with a total of 12 channels, which are connected and controlled by 10 servo motors 11 through 10 servo motor three-way valve connectors 12. The 12 channels of the multi-valve 14 are based on the syringe channel directly connected to the syringe 13. There are 6 channels on the right side, which are marked as channels 0 to 5 from near to far according to the distance from the syringe; there are 5 channels on the left side, which are marked as channels 6 to 10 from near to far according to the distance from the syringe.
[0061] The microcontroller 2 is connected to an analog-to-digital converter 4, an electromagnetic relay 5, and a DC motor controller 6 via DuPont cables. The analog-to-digital converter 4 converts the potential signal transmitted from the BNC connector 8 into a digital signal and transmits it to the microcontroller 2 for real-time monitoring of reaction conditions. The electromagnetic relay 5 provides electrical isolation and signal transmission between the input and output circuits, and controls the on / off of the vacuum pump 21 connected to the IEC C14 interface 9. The DC motor controller 6 controls the forward and reverse rotation and speed of the DC motor in the overhead stirrer 19 to meet the reaction stirring requirements. The power connector and switch 7 provide a stable power supply for the entire device, while the BNC connector 8, IEC C14 interface 9, and aviation interface 10 are used to connect the potential measurement probe 20 of the solid-liquid separation module, the vacuum pump 21, and the overhead stirrer 19, respectively, ensuring smooth signal and power transmission between these components. The stepper motor slide 16, under the precise monitoring and calibration of the stepper motor closed-loop controller 17, drives the syringe plunger fixture 18 to achieve precise aspiration and injection of the syringe 13, ensuring accurate addition of reactants. Syringe 13 connects to the syringe channel of multivalve 14, enabling precise fluid transfer. Through the collaborative operation of these components, the entire core control module automates and precisely controls key aspects of the organic synthesis process, including fluid transfer, reaction condition control, and stirring, providing a solid foundation for efficient and stable organic synthesis.
[0062] Figure 5 This is a partial enlarged view of the multi-valve assembly of the present invention. The multi-valve assembly 14 consists of N three-way valves connected horizontally via double-threaded Luer connectors 15. Each of the N three-way valves corresponds to N servo motors 11 and N servo motor valve couplings 12. Each three-way valve consists of an inverted T-shaped plastic pipe. Each of the three pipes in each valve has a Luer connector at its outlet. The upper pipe of each valve is used to connect to other equipment, while the left and right pipes are used to connect to other three-way valves. The left and right channels of the leftmost and rightmost three-way valves can also be connected to other equipment. Each three-way valve has a cylindrical plastic piston in the middle. The piston has a T-shaped handle that extends outward and fits into the T-shaped groove of the servo motor valve coupling 12. When the piston of each three-way valve is rotated to a specific angle, two or three of the three pipes in the valve can be connected to each other. Each servo motor 11 controls the connection between the three pipes in the valve by rotating its corresponding servo motor valve coupling 12. In order to allow liquid to be transferred between the two channels, any two channels of the multi-valve 14 can be connected. To achieve this purpose, the three-way valve piston where the left channel to be connected is located needs to be turned to a state where the upper channel and the right channel of the three-way valve are connected, and the three-way valve piston where the right channel to be connected is located needs to be turned to a state where the upper channel and the left channel of the three-way valve are connected, and the three-way valve between the two channels to be connected is turned to a state where the left and right are connected.
[0063] Figure 6 This is an assembly diagram of the solid-liquid separation module of the device of the present invention, such as Figure 5 As shown, the solid-liquid separation module of this embodiment includes: an overhead stirrer 19, a potential measurement probe 20, a vacuum pump 21, a sand core funnel 22, a sand core funnel cover 23, and a collection flask 24. The solid-liquid separation module of this embodiment is primarily responsible for achieving solid-liquid separation and collection of reaction products during the organic synthesis process. The overhead stirrer 19, driven by a micro-DC motor, rotates a polytetrafluoroethylene stirring rod, stirring the liquid in the sand core funnel 22 to ensure uniform mixing of the reactants. The potential measurement probe 20 utilizes a composite pH probe with a glass electrode as the measuring electrode and a silver / silver chloride electrode as the reference electrode. It monitors the potential changes of the liquid in the sand core funnel 22 in real time and transmits the signal to the microcontroller for precise control of the separation process. The vacuum pump 21 generates an air pressure differential through the filtration branch, forcing the liquid in the sand core funnel 22 to pass through the sand core under pressure, achieving solid-liquid separation. The solid remains in the funnel, while the liquid flows into the collection flask 24. The sand funnel 22 is a 100ml G4 glass sand funnel. It and its cover 23 provide the necessary physical structure for the separation process, ensuring smooth operation. Controlled by the core control module's single-chip microcomputer 2, the entire solid-liquid separation module achieves automated and efficient solid-liquid separation and product collection, improving experimental efficiency and product purity.
[0064] Figure 7 The assembly diagram of the chemical synthesis module of the device of the present invention is as follows: Figure 6 As shown, the chemical synthesis module of the present embodiment includes: a heating type magnetic stirrer 25, a metal bath module 26, and a reaction flask 27. The chemical synthesis module of the present embodiment is mainly responsible for providing accurate reaction conditions and place for organic synthesis reaction. The heating type magnetic stirrer 25 provides suitable temperature and sufficient mixing conditions for the chemical reaction in the reaction flask 27 by heating and stirring functions, and its heating and stirring parameters can be accurately controlled and adjusted by a computer to meet the needs of different reactions. The metal bath module 26 is made of an aluminum alloy with good thermal conductivity, and its semicircular groove fits the reaction flask 27 tightly, and heat can be quickly transferred to the reaction flask, ensuring that the reactants in the reaction flask react in a uniform temperature field, while the portability of the metal bath module is also easy to operate and replace. The reaction flask 27 is a 50ml branch pipe round bottom glass flask, as the main occurrence place of organic synthesis reaction, and its side branch connects the liquid pipeline, which facilitates the addition of reactants and the removal of products, and provides key physical environment and condition support for the smooth progress of the whole organic synthesis reaction.
[0065] Figure 8 The figure is a schematic flow chart of the intelligent organic synthesis method of the present invention. Combined with the process of aspirin synthesis, the specific method steps are as follows:
[0066] First step, experimental preparation. Design a detailed experimental procedure and specify the reagent bottles or equipment connected to each channel of the multi-way valve 14. In this embodiment, the 12 channels of the multi-way valve 14 are connected according to the following rules: channels 0 to 5 are reagent bottle channels, used to connect the multi-way valve 14 and the reagent bottles containing the corresponding reagents; among them, channel 0 is connected to a saturated sodium bicarbonate reagent bottle, channel 1 is connected to an acetic anhydride reagent bottle, channel 2 is connected to a hydrochloric acid reagent bottle, channel 3 is connected to an ethanol reagent bottle, and channel 4 is connected to a cold water reagent bottle. Channels 6 to 8 are reaction vessel channels, used to connect the multi-way valve 14 and each reaction vessel; among them, channel 6 is connected to a sand core funnel 22, channel 7 is connected to a collection bottle 24, and channel 8 is connected to a reaction bottle 27. Channels 5 and 10 are waste liquid channels, connected to a waste liquid bottle. Channel 9 is empty. Prepare high-purity, appropriate amounts of each type of reagent and fill them into the corresponding reagent bottles.
[0067] Connect the connecting line of the potential measurement probe 20 to the BNC connector 8, connect the power line of the vacuum pump 21 to the IECC 14 interface 9, connect the overhead stirrer 19 to the aviation interface 10, and connect the 12V power supply to the power connector and switch 7. Connect the heating type magnetic stirrer 25 to the computer with RS232 serial port line, turn on the power switch of the intelligent organic synthesis device, and let the equipment preheat for 5 minutes. Finally, connect the single-chip microcomputer 2 to the computer using a MicroUSB data line, and prepare for subsequent automated control.
[0068] Second step, add reactants. Send instructions to the single-chip microcomputer 2 through the computer, precisely drive the servo motor 11 to rotate the piston of the multi-way valve 14 to the state where channel 1 (acetic anhydride reagent bottle) is connected to the syringe 13, at the same time, control the stepper motor sliding table 16 to drive the syringe push rod to move upwards, accurately drawing 4 milliliters of acetic anhydride from the reagent bottle; then, control the drive servo motor 11 again to rotate the piston of the multi-way valve 14 to the state where channel 8 (reaction bottle 27) is connected to the syringe 13, control the stepper motor sliding table 16 to drive the syringe 13 push rod to move downwards, and inject acetic anhydride into the reaction bottle 27. Then manually add 1.38 grams of salicylic acid and 4 drops of concentrated sulfuric acid, which have been weighed by hand, into the reaction bottle 27 from the top of the flask.
[0069] The third step is to start the reaction. After confirming that all reactants have been accurately added to the reaction bottle 27, a command is sent to the heating magnetic stirrer 25 through the computer. The heating magnetic stirrer 25 starts to heat the reaction bottle 27 to 85 degrees Celsius and stirs it at a speed of 200 revolutions per minute. At the same time, the single-chip microcomputer 2 monitors the working status of the heating magnetic stirrer in real time to ensure that it operates stably according to the preset parameters. Throughout the reaction process, the set heating and stirring conditions are maintained to ensure that the reaction can proceed smoothly and efficiently. When the feedback temperature of the heating magnetic stirrer 25 reaches above 80 degrees Celsius, the timing starts until the reaction reaches the predetermined reaction time of 10 minutes, and then the heating and stirring are stopped.
[0070] The fourth step is product separation and collection. After the reaction is complete, a computer sends instructions to microcontroller 2, causing servo motor 11 to rotate the piston of multi-valve 14, connecting channel 4 (ice water) with the channel containing syringe 13. This controls stepper motor slide 16 to move the push rod of syringe 13 upward, withdrawing 20 ml of ice water. Next, servo motor 11 rotates the piston of multi-valve 14, connecting syringe 13 with channel 6 (sand core funnel 22). This controls stepper motor slide 16 to move the push rod of syringe 13 downward, adding 20 ml of ice water to sand core funnel 22. Next, using the same method, withdraw all reaction products from channel 8 (reaction flask 27) and add them to sand core funnel 22. Overhead stirring 19 is activated and stirred for 100 seconds to thoroughly mix the liquid in sand core funnel 22, allowing it to cool and precipitate the crude aspirin product. The vacuum pump 21 is then started, and the pressure difference generated by the filtration branch of the sand core funnel 22 causes the liquid in the sand core funnel 22 to pass through the sand core of the sand core funnel 22 and enter the collection bottle 24, while the solid crude product remains in the sand core funnel 22, achieving solid-liquid separation. At this point, the separation and collection of the crude product are completed.
[0071] The fifth step is product purification. After solid-liquid separation is completed and the crude aspirin product is collected, purification methods such as recrystallization can be used to further improve the product's purity. The specific operation is as follows: First, servo motor 11 drives the piston of multi-valve 14 to rotate, connecting channel 7 (collection bottle 24) with the channel containing syringe 13. Stepper motor slide 16 is controlled to move the push rod of syringe 13 upward, completely withdrawing the filtrate. Then, using the same method, the filtrate is discharged into channel 10 (waste bottle). Subsequently, 10 ml of saturated sodium bicarbonate solution is drawn from channel 0 and added to channel 6 (sand core funnel 22). Overhead stirring is activated to fully dissolve the solid product. The vacuum pump 21 is then activated to allow the product-containing solution to enter the collection bottle 24, while the solid impurities remain in the sand core funnel 22.
[0072] Using the same method, the product-containing solution was withdrawn from channel 7 (collection flask 24) and added to reaction flask 27 through channel 8 for temporary storage. Then, using the same method, 20 ml of ethanol was withdrawn from channel 3 and added to channel 6 (sand-core funnel 22). Overhead stirring 19 was activated to redissolve the solid impurities remaining in sand-core funnel 22. Vacuum pump 21 was then activated to allow the liquid in sand-core funnel 22 to enter collection flask 24. The impurity-containing solution was then withdrawn from channel 7 (collection flask 24) using the same method and then discharged into channel 10 (waste bottle).
[0073] Subsequently, the reaction product is extracted from channel 8 (reaction bottle 27) and added to the sand core funnel 22. 10 ml of hydrochloric acid is extracted from channel 2 and gradually added to the sand core funnel 22. During this process, the top stirrer 19 begins stirring, and the potential measuring probe 20 continuously monitors the potential change of the solution. The single chip computer 2 determines the pH value of the solution in the sand core funnel 22 based on the potential change. When the pH value of the solution in the sand core funnel 22 is 7 or slightly lower than 7, the addition of hydrochloric acid is stopped, and the remaining hydrochloric acid in the syringe 13 is discharged into the waste liquid bottle of channel 10.
[0074] Wait 100 seconds to allow the purified aspirin in sand core funnel 22 to reprecipitate. Then start vacuum pump 21 and utilize the suction filtration branch of sand core funnel 22 to generate a pressure differential. This allows the liquid in sand core funnel 22 to pass through the sand core of sand core funnel 22 and enter collection bottle 24, while the purified aspirin solid product remains in sand core funnel 22, achieving solid-liquid separation. The filtrate is completely withdrawn from collection bottle 24. Then, using the same method, the filtrate is discharged into channel 10 (waste bottle). After the purified aspirin solid product in sand core funnel 22 has naturally dried, the intelligent organic synthesis example of aspirin is completed.
[0075] The foregoing description is merely a preferred embodiment of the present invention and is not intended to limit the present invention. Those skilled in the art will readily appreciate that various modifications and variations of the present invention are possible. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of the present invention shall be included within the scope of protection of the present invention.
Claims
1. An intelligent organic synthesis device, characterized in that: The intelligent organic synthesis device includes three parts: a core control module, a solid-liquid separation module, and a chemical synthesis module. The core control module serves as the control center of the entire device, realizing precise fluid delivery and reaction control during the chemical organic synthesis process. The solid-liquid separation module is the place for refining and separating the reaction products. A vacuum pump 21 is used to form an air pressure difference in the sand core funnel 22, so that the liquid passes through the sand core and flows into the collection bottle 24, and the solid remains in the sand core funnel 22, realizing solid-liquid separation. The chemical synthesis module is the core module for chemical synthesis, and uses a heating magnetic stirrer 25 to provide heating and stirring reaction conditions for chemical synthesis.
2. The intelligent organic synthesis device according to claim 1, characterized in that: The core control module includes: an organic synthesis device housing 1, a single-chip microcomputer 2, a servo motor controller 3, an analog-to-digital conversion device 4, an electromagnetic relay 5, a DC motor controller 6, a servo motor 11, a stepper motor slide 16, a stepper motor closed-loop controller 17, a servo motor valve coupling 12, a syringe 13, a multi-valve 14, a syringe push rod fixture 18, and multiple reagent bottles 28 outside the organic synthesis device housing 1. Specifically: The housing 1 of the organic synthesis device is an inverted T-shaped structure, consisting of a horizontal portion and a vertical portion. The vertical portion of the T-shape is provided with a square hole for passing a syringe push rod fixture 18 and a fixture for fixing the syringe 13. The horizontal portion is provided with N square holes for fixing N servo motors 11. The N servo motors 11 are connected to the multi-valve 14 through N servo motor valve couplings 12. When the servo motors 11 rotate, the pistons of the multi-valve 14 are driven to rotate through the servo motor valve couplings 12, changing the connection state of the corresponding pistons and controlling the connection between the plastic syringe 13 and a certain interface of the multi-valve 14. The syringe push rod fixture 18 moves synchronously with the stepper motor slide 16. The stepper motor closed-loop controller 17 is fixed to the stepper motor of the stepper motor slide 16 and is connected to the stepper motor and the single-chip microcomputer 2. The push rod of the syringe 13 is fixed to the syringe push rod fixture 18 and moves synchronously with it. The syringe 13 is installed on an external threaded port of the multi-valve 14. The movement of the fluid is achieved by the pumping action of the syringe 13; The servo motor controller 3 is connected to the power supply and controls the rotation angle of the servo motor 11 through an electrical signal; The single-chip microcomputer 2 is mounted on a servo motor controller 3; the single-chip microcomputer 2 controls the movement of the stepper motor slide 16 through electrical signals; the single-chip microcomputer 2 is connected to an analog-to-digital conversion device 4 to read the potential signal measured by a potential measuring probe 20; the single-chip microcomputer 2 is connected to an electromagnetic relay 5 to control the power switch of a vacuum pump 21; the single-chip microcomputer 2 is connected to a DC motor controller 6 to control the operation of the top stirring 19 of the solid-liquid separation module; the electromagnetic relay 5 is also connected to the servo motor controller 3; The reagent bottles 28 are glass reagent bottles filled with liquid reagents and equipped with liquid pipelines. There are multiple reagent bottles 28 placed outside the organic synthesis device housing 1; a liquid pipeline is installed on the lid of each reagent bottle 28, connecting the liquid reagent with a reagent bottle channel of the multi-valve 14.
3. The intelligent organic synthesis device according to claim 2, characterized in that: In the core control module: The stepper motor closed-loop controller 17 has a magnet attached to the end of the screw of the stepper motor slide 16. When the screw rotates, the stepper motor closed-loop controller 17 determines the actual rotation angle of the screw by measuring the magnetic direction of the magnet, and performs real-time monitoring and calibration compensation. The syringe 13 is a plastic syringe with a Luer internal thread at the outlet. The servo motor controller 3 also has multiple sets of 5V power supply interfaces to supply power to other electronic devices; The DC motor controller 6 is a DC motor drive module based on a dual-path H-bridge of MOSFET, which can realize bidirectional control; the control terminal of the DC motor controller 6 is connected to the top stirring 19 through the aviation interface 10; The multi-valve 14 is composed of N three-way valves connected together horizontally through a double-threaded Luer connector 15, and the N three-way valves correspond one to one with the N servo motors 11 and the N servo motor valve couplings 12.
4. The intelligent organic synthesis device according to claim 3, characterized in that: The solid-liquid separation module includes: an overhead stirrer 19, a potential measurement probe 20, a vacuum pump 21, a sand core funnel 22, a sand core funnel cover 23, and a collection bottle 24; specifically: The top stirring device 19 comprises a micro DC motor and a polytetrafluoroethylene stirring rod; the micro DC motor is connected to the DC motor controller 6, and the blade of the polytetrafluoroethylene stirring rod passes through the sand core funnel cover 23 and extends into the sand core funnel 22; the top stirring device 19 is installed at the top of the entire solid-liquid separation module by a clamp; The sand core funnel 22 is installed under the top stirring 19; the lower part of the sand core funnel 22 has a sleeve, the inner side of the sleeve is a liquid passage, and the outer side of the sleeve is a gas passage to achieve solid-liquid separation; The sand core funnel cover 23 has three holes and a bracket, and covers the sand core funnel 22; The measuring end of the potential measuring probe 20 extends into the liquid in the sand core funnel 22 and transmits the potential signal to the single chip microcomputer 2 to determine whether the reaction conditions are met.
5. The intelligent organic synthesis device according to claim 4, characterized in that: In the solid-liquid separation module: The sand core funnel 22 is a glass sand core filtration funnel; The upper end of the liquid passage inside the casing is connected to the bottom of the sand core of the sand core funnel 22, and the lower end extends into the collection bottle 24. The liquid extracted from the sand core funnel 22 flows into the collection bottle 24 through the liquid passage. The gas passage outside the casing is a horizontal T-shaped structure as a whole. The upper end of the gas passage is sealed, and the lower end is connected to the collection bottle 24. The horizontal branch is connected to the vacuum pump 21 as a filtration branch. The vacuum pump 21 is started to extract air from the gas passage of the sand core funnel 22. A pressure difference is formed above and below the sand core of the sand core funnel 22. The liquid in the sand core funnel 22 passes through the sand core and flows into the collection bottle 24 through the liquid passage. The solid in the sand core funnel 22 remains in the sand core funnel, thereby achieving solid-liquid separation. One of the holes on the sand core funnel cover 23 allows the liquid pipeline to pass through, and the other end of the liquid pipeline is connected to the sand core funnel channel of the multi-valve 14 to provide a pipeline for the liquid to enter the sand core funnel 22; the other two holes are used to pass through the polytetrafluoroethylene stirring rod of the top stirring 19 and the potential measuring probe 20 respectively.
6. The intelligent organic synthesis device according to claim 5, characterized in that: The chemical synthesis module includes: a heating magnetic stirrer 25, a metal bath module 26, and a reaction bottle 27; specifically: The heating magnetic stirrer 25 is located at the bottom of the entire chemical synthesis module and performs heating or stirring operations to provide reaction conditions for chemical synthesis; The metal bath module 26 is made of aluminum alloy and is placed on the heating plate of the heating magnetic stirrer 25 to transfer heat to the reaction bottle 27; The reaction bottle 27 is a glass round-bottom flask with a branch on the side, which is placed on the metal bath module 26; the top of the reaction bottle 27 is open for adding reagents; the branch on the side of the reaction bottle 27 is connected to the liquid pipeline, and the other end of this pipeline is connected to the reaction bottle channel of the multi-valve 14, providing a pipeline for liquid to enter and exit the reaction bottle 27.
7. An intelligent organic synthesis method, characterized in that: The intelligent organic synthesis device according to any one of claims 1 to 6 is implemented. The synthesis method first controls the servo motor 11 and the stepper motor slide 16 to add the reactants into the reaction bottle 27 in sequence; then, the heating magnetic stirrer 25 is started to provide temperature and stirring conditions for the reaction according to preset parameters, and the single-chip microcomputer 2 automatically adjusts the parameters according to the potential signal collected by the potential measurement probe 20 to ensure the smooth progress of the reaction; after the reaction is completed, the reaction product is transferred to the sand core funnel 22, and the product is separated and collected by the vacuum pump 21 and the sand core funnel 22.
8. The intelligent organic synthesis method according to claim 1, characterized in that: The intelligent organic synthesis method comprises the following steps: The first step is experimental preparation; The second step is to add reactants; The servo motor 11 is driven to rotate the piston of the multi-valve 14 until the desired reagent bottle channel containing the raw materials is connected to the syringe 13. At the same time, the stepper motor slide 16 is controlled to drive the syringe push rod upward to accurately extract the raw materials from the reagent bottle 28. Then, the servo motor 11 is controlled again to rotate the piston of the multi-valve 14 until the reaction bottle 27 is connected to the syringe 13. The stepper motor slide 16 is controlled to drive the syringe 13 push rod downward to inject the extracted raw materials into the reaction bottle 27. This process is repeated until all the raw materials have been added to the reaction bottle 27. Then, the remaining raw materials are added to the reaction bottle 27. The third step is to start the reaction; After all reactants have been accurately added to the reaction bottle 27, the heating magnetic stirrer 25 is started to provide a suitable temperature and sufficient mixing conditions for the organic synthesis reaction; at the same time, the single-chip microcomputer 2 monitors the working status of the heating magnetic stirrer 25 in real time to ensure that it operates stably according to the preset parameters; The fourth step is to separate and collect the products; After the reaction is completed, the servo motor 11 drives the piston of the multi-valve 14 to rotate, connecting the reagent bottle channel connected to the precipitate with the channel where the syringe 13 is located, and controls the stepper motor slide 16 to drive the push rod of the syringe 13 to move upward to extract the precipitate; then, the servo motor 11 drives the piston of the multi-valve 14 to rotate, connecting the syringe 13 with the sand core funnel 22, and controls the stepper motor slide 16 to drive the push rod of the syringe 13 to move downward to add the precipitate into the sand core funnel 22; Extract all the reaction products from the reaction bottle 27 and add them to the sand core funnel 22; start the overhead stirring 19 to stir the liquid in the sand core funnel 22 to fully mix, cool and precipitate the crude product; start the vacuum pump 21 to achieve solid-liquid separation, and complete the separation and collection of the crude product; The fifth step is to purify the product.
9. An intelligent organic synthesis method according to claim 8, characterized in that: The fifth step is specifically as follows: First, the servo motor 11 drives the piston of the multi-valve 14 to rotate, connecting the collection bottle 24 with the channel where the syringe 13 is located, and controls the stepper motor slide 16 to drive the push rod of the syringe 13 to move upward to extract all the filtrate; then, the filtrate is discharged into the waste liquid bottle; then, the alkaline reagent is extracted from the reagent bottle channel connected to the alkaline reagent and added to the sand core funnel 22. The top stirring is turned on to fully dissolve the solid product, and then the vacuum pump 21 is started to allow the solution containing the product to enter the collection bottle 24, and the solid impurities remain in the sand core funnel 22; The solution containing the product is drawn from the collection bottle 24 and temporarily stored in the reaction bottle 27. Then, the cleaning liquid is drawn from the channel connected to the cleaning liquid and added to the sand core funnel 22. The overhead stirring 19 is turned on to redissolve the solid impurities remaining in the sand core funnel 22. The vacuum pump 21 is then started to allow the liquid in the sand core funnel 22 to enter the collection bottle 24. The solution containing impurities is then drawn out from the collection bottle 24 and discharged into a waste liquid bottle; Subsequently, the reaction product is extracted from the reaction bottle 27 and added to the sand core funnel 22; the pH adjusting reagent is extracted and added to the sand core funnel 22, the stirring device 19 is placed on top to start stirring, and the potential measuring probe 20 continuously monitors the potential change of the solution. The single chip microcomputer 2 determines the pH value of the solution in the sand core funnel 22 based on the potential change. When the pH value of the solution in the sand core funnel 22 meets the set conditions, the addition of the pH adjusting reagent is stopped, and the remaining pH adjusting reagent in the syringe 13 is discharged into the waste liquid bottle of channel 10; Wait for the refined product in the sand core funnel 22 to re-precipitate, start the vacuum pump 21, and allow the liquid in the sand core funnel 22 to pass through the sand core of the sand core funnel 22 into the collecting bottle 24, while the refined product remains in the sand core funnel 22 to achieve solid-liquid separation; completely extract the filtrate from the collecting bottle 24 and discharge it into the waste liquid bottle.