Reaction device

Abstract

The utility model discloses a reaction device and relates to the field of material preparation. The reaction device comprises a sample introduction system, a reaction system, a discharge system and a controller, the solid metering and transferring assembly is used for metering and transferring solid materials and introducing samples into the reactor, and the fluid sample introduction assembly is used for adding solvents and reaction liquid samples into the reactor through a liquid inlet; each reactor executes four steps of filler sample introduction, air extraction, reaction and liquid extraction, one group of two or more reactors sequentially and alternately execute the steps, reaction products are sequentially extracted, the reaction products are continuously generated, and the requirement of continuous flow preparation of the reaction products is met. According to the utility model, on the basis of effectively considering the consistency of the reaction products, the path for producing the reaction products can be reasonably planned and set, the reaction products can be continuously produced, the automation degree is high, and the mode can liberate manpower and improve the production efficiency.

Description

Technical Field

[0001] This utility model relates to the field of materials preparation, specifically to a reaction apparatus. Background Technology

[0002] In chemical material preparation processes, the preparation of production solutions typically involves using solids and liquids as raw materials. For example, in the synthesis stage of nanocrystalline precursors, such as octadecene solutions of cadmium oleate and octadecene solutions of selenium powder, solids generally participate in the chemical reaction during the preparation process. The quantitative addition of solids is the biggest bottleneck in precursor preparation. This process requires operators to be patient, such as accurately weighing solid materials. The actual work process is repetitive and tedious, resulting in high labor costs. In the actual precursor preparation reaction stage, unreasonable precursor path planning makes continuous production difficult, limiting the production efficiency and batch consistency of precursors. Utility Model Content

[0003] To address the technical problems raised in the background section, this utility model provides a reaction apparatus, comprising:

[0004] The sample introduction system includes a solid metering and transfer component and a fluid sample introduction component, wherein the solid metering and transfer component is used for picking up, placing, and metering solid materials;

[0005] The reaction system includes at least one set of reactors, and the set of reactors includes at least two reactors; each reactor is provided with a solid feed inlet, a liquid inlet, an exhaust outlet, and a liquid outlet; the solid feed inlet is used to receive solid material transferred by the solid metering and transfer component, and the liquid inlet is connected to the liquid inlet path of the fluid injection component.

[0006] The discharge system includes an exhaust component and a discharge component, wherein the input end of the exhaust component is connected to the exhaust port, and the input end of the discharge component is connected to the liquid discharge port.

[0007] A controller is connected to the injection system, reaction system, and discharge system. The controller is used to control at least the fluid injection volume and fluid injection rate of the injection system, the opening and closing status of the inlet and outlet of the reactor, and the discharge volume and discharge rate of the discharge system.

[0008] As a preferred technical solution, the solid metering and transfer assembly includes a pickup component, a weighing component, and a transfer mechanism. The pickup component is fixedly connected to the transfer end of the transfer mechanism. The weighing component is used to carry the container holding the solid material. The transfer mechanism is adapted to drive the pickup component to transfer the solid material to the solid feed inlet. The pickup component is connected to the controller, and the weighing component is connected to the controller.

[0009] As a preferred technical solution, the pickup component includes a first pickup part, a second pickup part, and a moving drive component. Either pickup part is hollowed out internally, and the first pickup part or the second pickup part is drive-connected to the drive end of the moving drive component; and / or

[0010] The transfer mechanism is configured as a two-axis linear displacement module or a three-axis linear displacement module.

[0011] As a preferred technical solution, the fluid injection assembly includes a first liquid injection assembly and a second liquid injection assembly. The reactor is provided with a first liquid inlet and a second liquid inlet at intervals. The output end of the first liquid injection assembly is connected to the first liquid inlet, and the output end of the second liquid injection assembly is connected to the second liquid inlet.

[0012] As a preferred technical solution, the first liquid inlet assembly includes a first liquid storage tank, a first liquid inlet pump, and a first valve connected in sequence. The first valve is configured with a one-inlet, multiple-outlet structure. The inlet end of the first valve is connected to the output end of the first liquid inlet pump, and each outlet end of the first valve is connected to a corresponding first liquid inlet of a group of reactors. The first liquid inlet pump and the first valve are respectively connected to the controller; and / or

[0013] The second liquid inlet assembly includes a second liquid storage tank, a second liquid inlet pump, and a second valve connected in sequence. The second valve is configured as a one-inlet-multiple-outlet structure. The inlet end of the second valve is connected to the output end of the second liquid inlet pump, and each outlet end of the second valve is connected to each of the second liquid inlets of a set of reactors. The second liquid inlet pump and the second valve are respectively connected to the controller.

[0014] As a preferred technical solution, the reaction device further includes a protective gas inlet assembly, the reactor is provided with an inlet, and the output end of the protective gas inlet assembly is connected to the inlet.

[0015] The protective gas inlet assembly includes a protective gas source, a flow controller, and a third valve connected in sequence. The third valve is configured as a one-inlet, multiple-outlet structure. The inlet end of the third valve is connected to the output end of the flow controller, and each outlet end of the third valve is connected to a corresponding air inlet of a group of reactors. The flow controller and the third valve are respectively connected to the controller.

[0016] As a preferred technical solution, the exhaust assembly includes a vacuum pump and a fourth valve. The fourth valve is configured with a multi-inlet and one-outlet structure. Each inlet end of the fourth valve is respectively connected to each exhaust port of a group of reactors. The outlet end of the fourth valve is connected to the input end of the vacuum pump. The vacuum pump and the fourth valve are respectively connected to the controller.

[0017] As a preferred technical solution, the discharge assembly includes a No. 5 valve, a discharge pump, and a collection and storage device connected in sequence. The No. 5 valve is configured with a multi-inlet and one-outlet structure. Each inlet end of the No. 5 valve is respectively connected to each drain port of a group of reactors. The outlet end of the No. 5 valve is connected to the input end of the discharge pump. The No. 5 valve and the discharge pump are respectively connected to the controller.

[0018] As a preferred technical solution, the reaction system further includes a stirring assembly, which is configured correspondingly to the reactor. The stirring assembly includes a stirring motor and a stirrer. The stirring motor is installed outside the reactor, and the stirrer is driven by the driving side of the stirring motor and extends into the reactor. Alternatively, the reactor may also include a cover opening and closing assembly, with one cover opening and closing assembly configured for each reactor.

[0019] As a preferred technical solution, the reaction system further includes a cover opening and closing assembly. Each reactor is equipped with one cover opening and closing assembly. The cover opening and closing assembly includes a sealing cover, a sliding actuator, and a rotating actuator. The mounting end of the sliding actuator is fixedly connected to the reactor. The mounting end of the rotating actuator is fixedly connected to the driving end of the sliding actuator. The sealing cover is connected to the driving end of the rotating actuator. The sliding actuator and the rotating actuator are adapted to drive the sealing cover to move closer to close the solid feed inlet or move away from open the solid feed inlet.

[0020] The technical solution provided by this utility model has the following advantages:

[0021] 1. The reaction apparatus provided by this utility model includes a sample injection system, a reaction system, a discharge system, and a controller; the sample injection system includes a solid metering and transfer component and a fluid injection component; the reaction system includes at least one set of reactors, and each set of reactors includes at least two reactors; each reactor is provided with a solid feed inlet, a liquid inlet, an exhaust outlet, and a liquid outlet; the solid feed inlet is used to receive solid material transferred by the solid metering and transfer component, and the liquid inlet is connected to the liquid inlet path of the fluid injection component; the discharge system includes an exhaust component and a discharge component, the input end of the exhaust component is connected to the exhaust outlet, and the input end of the discharge component is connected to the liquid outlet; the controller is connected to the sample injection system, the reaction system, and the discharge system, and the controller is used to control at least the fluid injection volume and fluid injection flow rate of the sample injection system, the opening and closing state of the inlet and outlet of the reactor, and the discharge volume and discharge flow rate of the discharge system.

[0022] This reaction apparatus utilizes a solid metering and transfer component to meter and transfer solid materials, which are then introduced into the reactor through a solid feed inlet. A fluid injection component introduces solvents and reaction solutions into the reactor through a liquid inlet. An exhaust component in the exhaust system removes gases that interfere with the reaction from the reactor through an exhaust port. In operation, after the solid and liquid materials are introduced, the following steps are performed sequentially in each reactor: gas extraction (exhaust component), reaction, and liquid extraction (discharge component). After the reaction product is prepared, the discharge component discharges the prepared reaction product solution from the reactor through a discharge port. Two or more reactors in a group alternately execute the above steps, sequentially extracting reaction products, continuously generating them to meet the requirements of continuous flow reaction product preparation. For example, in the preparation of quantum dots, it can meet the requirement of continuous preparation of quantum dot precursors. This invention effectively considers the consistency of reaction products and rationally plans and sets the production path of reaction products, enabling continuous production of reaction products with a high degree of automation. This method can free up manpower and improve production efficiency.

[0023] 2. The reaction apparatus provided by this utility model includes a solid metering and transfer component comprising a pickup, a weighing component, and a transfer mechanism. The pickup is fixedly connected to the transfer end of the transfer mechanism. The weighing component is used to support the container holding the solid material. The transfer mechanism is adapted to drive the pickup to transfer the solid material to the solid feed inlet. The pickup is connected to a controller, and the weighing component is connected to the controller.

[0024] This reaction device uses a transfer mechanism to drive a pickup element into a container and grab solid material. The transferred solid material is then transferred to a single reactor. The difference in readings from the weighing device before and after grabbing is used to calculate the single solid sample injection volume. Based on this solid sample injection volume, the controller calculates the required injection volumes of other liquid reactants and solvents. This invention automatically samples and measures solid material, automatically transferring it to the reactor for injection. The automatic operation is convenient. The transfer mechanism is adapted to drive the pickup element to transfer solid material to the solid feed inlet, achieving solid material sampling and injection.

[0025] 3. The reaction apparatus provided by this utility model further includes a protective gas inlet assembly. The reactor is provided with an inlet, and the output end of the protective gas inlet assembly is connected to the inlet. The protective gas inlet assembly includes a protective gas source, a flow controller, and a third valve connected in sequence. The third valve is configured as a one-inlet-multiple-outlet structure. The inlet end of the third valve is connected to the output end of the flow controller, and each outlet end of the third valve is connected to each inlet of a set of reactors. The flow controller and the third valve are respectively connected to the controller.

[0026] This reaction apparatus features a protective gas inlet assembly that introduces high-purity protective gas into each reactor, preventing oxidation of the reactants and ensuring the reaction products are isolated from water vapor and oxygen throughout the process. Specifically, a compressed protective gas source provides the gas, a flow controller regulates the flow rate, and a third valve controls the connection between the flow controller and each reactor. This method allows for rapid liquid medium injection and utilizes the protective gas to provide a protective reaction environment, thereby improving the production efficiency and quality of the reaction product preparation.

[0027] 4. The reaction apparatus provided by this utility model includes an exhaust assembly comprising a vacuum pump and a fourth valve. The fourth valve is configured as a multi-inlet, one-outlet structure. Each inlet end of the fourth valve is respectively connected to each exhaust port of a set of reactors. The outlet end of the fourth valve is connected to the input end of the vacuum pump. The vacuum pump and the fourth valve are respectively connected to a controller.

[0028] This reaction device uses a vacuum pump to remove interfering sources such as oxygen and water vapor from the reactor cavity, allowing protective gas to flow smoothly into the reactor, creating a protective environment for the reaction medium and accelerating work efficiency. Each inlet end of valve number four is connected to the exhaust port of a group of multiple reactors, and one outlet end is connected to the vacuum pump. This setup helps to optimize the structural configuration, centralize the exhaust process, and reduce production costs.

[0029] 5. The reaction device provided by this utility model includes a discharge component comprising a No. 5 valve, a discharge pump, and a collection and storage device connected in sequence. The No. 5 valve is configured as a multi-inlet and one-outlet structure. Each inlet end of the No. 5 valve is respectively connected to each discharge port of a set of reactors. The outlet end of the No. 5 valve is connected to the input end of the discharge pump. The No. 5 valve and the discharge pump are respectively connected to a controller.

[0030] This reaction device uses a discharge pump to provide the driving force for extraction. The reaction product solution of a group of reactors is extracted through the inlet ends of the No. 5 valve. The discharge pump extracts the reaction product solution prepared in the reactor in the liquid extraction stage. As time progresses, another reactor is in the liquid extraction stage, thereby achieving continuous collection and discharge, and enabling the collection and storage device to continuously collect the reaction product solution. Attached Figure Description

[0031] To more clearly illustrate the specific embodiments of this utility model or the technical solutions in the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this utility model. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0032] Figure 1 A schematic diagram of the reaction apparatus provided by this utility model;

[0033] Figure 2 This is a schematic diagram of the reactor structure in the reaction apparatus provided by this utility model;

[0034] Figure 3 This is a top view of the reactor in the reaction apparatus provided by this utility model;

[0035] Explanation of reference numerals in the attached figures:

[0036] 1-Sample introduction system; 11-Pick-up component; 12-Container; 13-Weighing component; 14-Transfer mechanism; 15-First liquid storage tank; 16-First liquid inlet pump; 17-Valve No. 1; 18-Second liquid storage tank; 19-Second liquid inlet pump; 20-Valve No. 2; 21-Protective gas source; 22-Flow controller; 23-Valve No. 3; 3-Discharge system; 31-Vacuum pump; 32-Valve No. 4; 33-Discharge pump; 34-Valve No. 5; 4-Reaction system; 41-Solid feed inlet; 42-First liquid inlet; 43-Second liquid inlet; 44-Air inlet; 45-Exhaust outlet; 46-Liquid outlet; 47-Stirring motor; 48-Stirrer; 49-Sealing cap; 410-Sliding actuator; 411-Rotary actuator; 5-Controller. Detailed Implementation

[0037] The technical solution of this utility model will now be clearly and completely described with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of this utility model. Based on the embodiments of this utility model, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this utility model.

[0038] In the description of this utility model, it should be noted that the terms "center," "upper," "lower," "left," "right," "vertical," "horizontal," "inner," and "outer," etc., indicating the orientation or positional relationship, are based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this utility model. Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Thus, a feature defined with "first" or "second" may explicitly or implicitly include at least one of that feature. Additionally, the meaning of "and / or" throughout the text includes three parallel solutions. Taking "A and / or B" as an example, it includes solution A, or solution B, or a solution that simultaneously satisfies A and B. Furthermore, the technical solutions of the various embodiments can be combined with each other, but this must be based on the ability of those skilled in the art to implement them. When the combination of technical solutions is contradictory or cannot be implemented, it should be considered that such combination of technical solutions does not exist and is not within the scope of protection claimed by this utility model.

[0039] In the description of this utility model, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "joining" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this utility model based on the specific circumstances.

[0040] Example

[0041] The technical solution of this embodiment will be described in detail below with reference to the accompanying drawings. The thickness of the lines in the drawings is only for easy distinction and does not represent the thickness of pipes or other structures.

[0042] This embodiment provides a reaction apparatus, see [link / reference] Figures 1 to 3It includes a sample injection system 1, a reaction system 4, a discharge system 3, and a controller 5. The controller 5 is connected to the sample injection system 1, the reaction system 4, and the discharge system 3. The controller 5 is used to control the fluid injection volume and fluid injection flow rate of the sample injection system 1, the opening and closing status of the inlet and outlet of the reactor, and the discharge volume and discharge flow rate of the discharge system 3.

[0043] In this embodiment, the reaction system 4 includes at least one set of reactors, with two or more reactors in each set. Each reactor is provided with a solid feed inlet 41, a liquid inlet, an exhaust outlet 45, and a liquid outlet 46. The solid feed inlet 41 is used to receive solid materials transferred by the solid metering and transfer component, and the liquid inlet is connected to the liquid inlet path of the fluid injection component. The reactor's inlet and outlet are the solid feed inlet 41, liquid inlet, air inlet 44, exhaust outlet 45, and liquid outlet 46. The solid feed inlet 41 is located at the top of the reactor, while the liquid inlet, air inlet 44, exhaust outlet 45, and liquid outlet 46 are located on the side walls of the reactor.

[0044] The reaction apparatus provided in this embodiment, for a set of two reactors, can be divided into four stages of operation: packing material injection, gas extraction, reaction, and liquid extraction. One reactor performs the first three steps (packing material injection, gas extraction, and reaction), while the other reactor performs the liquid extraction step. The two reactors operate alternately, enabling the reaction apparatus to continuously produce the reaction product solution. This reaction product can be any product, such as a precursor in the quantum dot preparation process.

[0045] The reaction apparatus provided in this embodiment, for a group of three reactors, if the operation of the reactor is divided into four stages, namely packing sample injection, gas extraction, reaction, and liquid extraction, for two of the reactors, the packing sample injection, gas extraction, and reaction are carried out for half the time, while the other reactor carries out the liquid extraction step. The three are operated alternately so that the reaction apparatus can continuously produce the reaction product solution.

[0046] The reaction apparatus provided in this embodiment, in specific operation, preferably consists of four reactors in one group. Each reactor operates in four stages: packing material injection, gas extraction, reaction, and liquid extraction. The duration of each stage can be configured to be the same. The four reactors operate simultaneously, performing one of the four stages respectively, in a cyclical manner. Ideally, the reaction apparatus can continuously produce the reaction product solution. In other embodiments, the reactors are arranged in two groups of eight, three groups of twelve, four groups of sixteen, etc.

[0047] Of course, the reaction apparatus is equipped with a group of five or more reactors, which are set according to the actual steps, rationally planned and allocated, and ensured that at any given time point, at least one reactor is in the last step, so as to achieve the purpose of continuous production of reaction product solution.

[0048] In some embodiments, the reactor further includes a cover opening and closing assembly, with one cover opening and closing assembly corresponding to each reactor. For example, the cover opening and closing assembly includes a sealing cover 49, a sliding actuator 410, and a rotary actuator 411. The mounting end of the sliding actuator 410 is fixedly connected to the reactor, and the mounting end of the rotary actuator 411 is fixedly connected to the driving end of the sliding actuator 410. The sealing cover 49 is connected to the driving end of the rotary actuator 411. The sliding actuator 410 and the rotary actuator 411 are adapted to drive the sealing cover 49 to approach or move away from the solid feed inlet 41. When solid sample injection is required, the sliding actuator 410 and the rotary actuator 411 jointly drive the sealing cover 49 to open and avoid the solid feed inlet 41. When solid sample injection is completed, the sliding actuator 410 and the rotary actuator 411 jointly drive the sealing cover 49 to close the solid feed inlet 41.

[0049] In some implementations, such as Figure 2 As shown, the reaction system 4 also includes a stirring assembly, which is configured correspondingly to the reactor. The stirring assembly includes a stirring motor 47 and a stirrer 48. The stirring motor 47 is installed outside the reactor, and the stirrer 48 is driven by the driving side of the stirring motor 47 and extends into the reactor. The stirrer 48 mechanically stirs the fluid medium inside the reactor, thereby accelerating the mixing reaction rate.

[0050] In some embodiments, the stirrer 48 may be a magnetic stirrer.

[0051] In a specific implementation, the reactor is configured as a reaction vessel, which is heated by a heating device to increase the reaction temperature.

[0052] In this embodiment, the sample introduction system 1 includes a solid metering and transfer component and a fluid sample introduction component. The solid metering and transfer component is used to pick up, place and meter solid materials, and the fluid sample introduction component is used for the sample introduction of reaction liquids, solvents, etc.

[0053] For example, in some implementations of the solid metering and transfer assembly, the solid metering and transfer assembly includes a pickup 11, a weighing component 13, and a transfer mechanism 14. The pickup 11 is fixedly connected to the transfer end of the transfer mechanism 14. The weighing component 13 is used to carry the container 12 containing solid materials. The transfer mechanism 14 is adapted to drive the pickup 11 to transfer solid materials to the solid feed inlet 41. The pickup 11 can be switched between the container 12 and the solid feed inlet 41. The pickup 11 is connected to the controller 5, and the weighing component 13 is connected to the controller 5.

[0054] The transfer mechanism 14 drives the pickup 11 into the container 12 to grab solid material, and then the transfer mechanism 14 transfers the grabbed solid material to a single reactor. The single solid sample injection volume is calculated based on the difference in the readings monitored by the weighing device 13 before and after grabbing. The controller 5 controls the injection volume of other liquid reaction raw materials and liquid solvents that need to be added based on the solid sample injection volume. This utility model can automatically sample and measure solid materials. The transfer mechanism 14 automatically transfers the solid material to the reactor for injection, and the automatic operation is convenient. The transfer mechanism 14 is adapted to drive the pickup 11 to transfer solid material to the solid feed inlet to realize the sampling and injection of solid materials.

[0055] In some embodiments, the pickup element 11 includes a first pickup section, a second pickup section, and a moving drive (not shown in the figure). Each pickup section has a hollowed-out interior. The first or second pickup section is connected to the drive end of the moving drive, which is adapted to drive the first and second pickup sections to move closer together to clamp solid material or to move away to release solid material. During operation, the opening and closing of the pickup element 11 is controlled by the relatively fixed first pickup section and the sliding of the second pickup section. Preferably, the pickup element 11 is submerged in the solid material to maximize the capacity of the solid sample, thereby improving production efficiency. The moving drive can be configured as a moving cylinder or an electric cylinder.

[0056] During metering operations, the mass of the remaining solid material is accurately weighed using the weighing device 13 and compared with the mass before it was picked up by the picking device 11, thereby precisely calculating the amount of solid material to be added to the reactor in a single sampling. This allows for the precise calculation of the injection volume of other substances that need to be added, such as liquid reactants and solvent media.

[0057] In the above description, solid materials include powder materials, granular materials, etc.

[0058] In some embodiments, the transfer mechanism 14 is configured as a two-axis linear displacement module or a three-axis linear displacement module. For example, horizontal and vertical slide rails can be provided to control the pickup 11 to move up and down, left and right, and forward and backward.

[0059] In some embodiments, the fluid injection assembly includes a first liquid injection assembly and a second liquid injection assembly. A first liquid inlet 42 and a second liquid inlet 43 are spaced apart on the reactor. The output end of the first liquid injection assembly is connected to the first liquid inlet 42, and the output end of the second liquid injection assembly is connected to the second liquid inlet 43. Liquid reactants are introduced into the reactor through the first liquid injection assembly, and reaction solvents are introduced into the reactor through the second liquid injection assembly.

[0060] In a specific implementation, both the first inlet pump 16 and the second inlet pump 19 can be HPLC pumps, which provide precise liquid inlet and help ensure the proper ratio of reactants.

[0061] In some embodiments, the first liquid inlet assembly includes a first liquid reservoir 15, a first liquid inlet pump 16, and a first valve 17 connected in sequence. The first valve 17 is configured with a one-inlet, multiple-outlet structure. The inlet end of the first valve 17 is connected to the output end of the first liquid inlet pump 16, and each outlet end of the first valve 17 is connected to a corresponding first liquid inlet 42 of a group of reactors. The first liquid inlet pump 16 and the first valve 17 are respectively connected to a controller 5. Each outlet end of the first valve 17 can be connected to the first liquid inlet 42 of each reactor through an inlet pipe. The first liquid inlet pump 16 provides the liquid inlet driving force to inject the reaction liquid in the first liquid reservoir 15 into the reactor.

[0062] Taking a group of two reactors as an example, valve 17 is configured with a one-inlet, two-outlet structure. For example, valve 17 can be configured as a three-way valve, or it can be configured as three single valves. For a group of N reactors, valve 17 can be configured with a one-inlet, N-outlet structure, or it can be configured as a combined valve structure. When a group consists of four reactors, preferably, valve 17 is configured with a one-inlet, four-outlet structure; for example, it can be configured as a five-way valve.

[0063] In some embodiments, the second liquid inlet assembly includes a second liquid reservoir 18, a second liquid inlet pump 19, and a second valve 20 connected in sequence. The second valve 20 is configured with a one-inlet, multiple-outlet structure. The inlet end of the second valve 20 is connected to the output end of the second liquid inlet pump 19, and each outlet end of the second valve 20 is connected to a corresponding second liquid inlet 43 of a set of reactors. The second liquid inlet pump 19 and the second valve 20 are respectively connected to the controller 5. Each outlet end of the second valve 20 can be connected to the second liquid inlet 43 of each reactor through an inlet pipe. The second liquid inlet pump 19 provides the liquid inlet driving force to inject the solvent in the second liquid reservoir 18 into the reactor.

[0064] Taking a group of two reactors as an example, valve component 20 is configured with a one-inlet, two-outlet structure. For example, valve component 20 can be configured as a three-way valve, or it can be configured as three single valves. For a group of N reactors, valve component 20 can be configured with a one-inlet, N-outlet structure, or it can be configured as a combined valve structure. When a group consists of four reactors, preferably, valve component 20 is configured with a one-inlet, four-outlet structure; for example, it can be configured as a five-way valve.

[0065] In some embodiments, the distance between the first liquid inlet 42 and the second liquid inlet 43 and the solid feed inlet 41 is set to be in the range of one-tenth to one-fifth of the height of the reactor cavity.

[0066] In some embodiments, the reaction apparatus further includes a protective gas inlet assembly. The reactor is provided with an inlet 44, and the output end of the protective gas inlet assembly is connected to the inlet 44. The protective gas inlet assembly includes a protective gas source 21, a flow controller 22, and a third valve 23 connected in sequence. The third valve 23 is configured with a one-inlet, multiple-outlet structure. The inlet end of the third valve 23 is connected to the output end of the flow controller 22, and each outlet end of the third valve 23 is connected to a corresponding inlet 44 of a group of reactors. The flow controller 22 and the third valve 23 are respectively connected to a controller 5. Each outlet end of the third valve 23 can be connected to the inlet 44 of each reactor via an inlet pipe. The protective gas source 21 can be configured as a compressed gas source, automatically filling the reactor when the inlet 44 is open, thereby improving the protective environment for the reaction.

[0067] The reaction apparatus introduces high-purity protective gas into each reactor through a protective gas inlet assembly, which plays a protective role and prevents the reactants from being oxidized. This ensures that the quantum dot reaction products are isolated from water vapor and oxygen throughout the process. Specifically, compressed protective gas is provided by protective gas source 21, flow controller 22 regulates the flow rate of the protective gas, and valve 23 controls the connection between flow controller 22 and each reactor. In this way, liquid medium can be introduced quickly, and the protective gas provides a protective environment for the reaction, which is beneficial to improving the production efficiency and quality of the reaction product preparation.

[0068] In this embodiment, the discharge system 3 includes an exhaust component and a discharge component. The input end of the exhaust component is connected to the exhaust port 45, and the input end of the discharge component is connected to the liquid discharge port 46.

[0069] In some embodiments, the exhaust assembly includes a vacuum pump 31 and a fourth valve 32. The fourth valve 32 is configured with a multi-inlet, one-outlet structure. Each inlet end of the fourth valve 32 is connected to a corresponding exhaust port 45 of a group of reactors, and the outlet end of the fourth valve 32 is connected to the input end of the vacuum pump 31. The vacuum pump 31 and the fourth valve 32 are both connected to the controller 5. The vacuum pump 31 removes oxygen, water vapor, and other interfering sources from the reactor cavity, allowing the protective gas to flow smoothly into the reactor, creating a protective environment for the reaction medium and accelerating the working efficiency. Each inlet end of the fourth valve 32 is connected to a group of multiple reactors, and one outlet end is connected to the vacuum pump 31. This configuration optimizes the structural configuration, centralizes the exhaust process, and reduces manufacturing costs.

[0070] Taking a group of two reactors as an example, valve component 32 is configured with a multi-inlet, one-outlet structure. For instance, valve component 32 can be configured as a three-way valve, or it can be configured as three single valves. For a group of N reactors, valve component 32 is configured with an N-inlet, one-outlet structure, or it can be configured as a combined valve structure. When a group consists of four reactors, preferably, valve component 32 is configured with a four-inlet, one-outlet structure; for example, it can be configured as a five-way valve.

[0071] In some embodiments, the discharge assembly includes a fifth valve 34, a discharge pump 33, and a collection and storage device (not shown) connected in sequence. The fifth valve 34 is configured with a multi-inlet, one-outlet structure. Each inlet end of the fifth valve 34 is connected to a corresponding outlet 46 of a group of reactors, and the outlet end of the fifth valve 34 is connected to the input end of the discharge pump 33. The fifth valve 34 and the discharge pump 33 are connected to the controller 5. The discharge pump 33 provides the extraction driving force, and the reaction product solutions of a group of multiple reactors are extracted through the inlet ends of the fifth valve 34. The discharge pump 33 extracts the reaction product solutions prepared in the reactors in the extraction stage. As time progresses, another reactor enters the extraction stage, thereby achieving continuous collection and discharge, and enabling the collection and storage device to continuously collect the reaction product solutions.

[0072] In a specific implementation, the discharge pump 33 can be an HPLC pump, which has precise liquid discharge and is beneficial for calculating and statistically analyzing the flow rate and total flow of the reaction product solution.

[0073] Taking a group of two reactors as an example, valve component 34 is configured with a multi-inlet, one-outlet structure. For instance, valve component 34 can be configured as a three-way valve, or it can be configured as three single valves. For a group of N reactors, valve component 34 is configured with an N-inlet, one-outlet structure, or it can be configured as a combined valve structure. When a group consists of four reactors, preferably, valve component 34 is configured with a four-inlet, one-outlet structure; for example, it can be configured as a five-way valve.

[0074] The reaction apparatus provided by this invention uses a solid metering and transfer component to meter and transfer solid materials, which are then fed into the reactor through a solid feed inlet 41. A fluid sampler component introduces solvent and reaction liquid into the reactor through a liquid inlet. Protective gas is introduced into the reactor through an air inlet 44, and gases interfering with the reaction are discharged from the reactor through an exhaust port 45 of the exhaust component in the exhaust system 3. In specific operation, after the solid and liquid materials are fed, the following operations are performed sequentially in each reactor: gas extraction, reaction, and liquid extraction. After the reaction product preparation is completed, the discharge component discharges the prepared reaction product solution from the reactor through a liquid outlet 46. Ideally, multiple reactors alternately perform the above steps, sequentially extracting reaction products, resulting in a continuous flow of reaction products and meeting the requirements for continuous production. This invention effectively considers the consistency of reaction products and rationally plans and sets the production path for reaction products, enabling continuous production of reaction products with a high degree of automation. This method can free up manpower and improve production efficiency.

[0075] The reaction apparatus provided in this embodiment is preferably configured as a four-cylinder four-pass continuous flow reaction system 4, which includes four identical reactors. Each reactor has a solid feed inlet 41 for solid sample introduction, two liquid inlets, a gas inlet 44, a vent 45, and a liquid outlet 46. A stirring assembly is also provided on the top of the reactor. The reaction apparatus is provided with a total of 5 valves, of which 3 are used for one inlet and multiple outlets, and the other 2 are used for multiple inlets and one outlet. The inlets of the first 3 valves are respectively introduced into reactants, solvents, and high-purity protective gas, and the latter 2 are respectively connected to a vacuum pump 31 and a discharge pump 33 for extracting reaction products. The four ports of the 5 valves are all connected to four independently configured reactors.

[0076] The reaction apparatus provided in this embodiment performs the following operations sequentially in a single reactor after the packing material (solid material and liquid material) is completed: gas extraction (room temperature extraction and high temperature extraction), reaction (including pre-weighted protective gas), and liquid extraction (including pre-cooling). The reaction apparatus can automatically inject solid samples, automatically calculate the required liquid volume, automatically inject liquid, automatically extract gas, automatically fill gas, and automatically drain liquid according to a preset program, and work in a cycle. There is no need to manually weigh the solid sample volume, and the injection and discharge operations are automatically executed, making the operation simple and fast.

[0077] In the above description, the reaction apparatus is not limited to the solid material prepared from the precursor in the quantum dot synthesis stage, but can also be used to meter solid materials in other reaction stages.

[0078] For a set of four reactors, named reactor A, reactor B, reactor C, and reactor D respectively; the reaction apparatus provided by this utility model, taking the preparation of cadmium oleate precursor as an example, is used as follows:

[0079] 1. The sealing cover of reactor A is opened via the cover opening and closing assembly and rotated to the side to ensure no obstruction above the opening. The weighing device reads the total weight W0 of the container and solid material (cadmium oxide). The two pickup parts of the pickup open and are inserted into the solid material (cadmium oxide) powder, completely submerging the pickup. The two pickup parts close, and the pickup is filled with cadmium oxide solid powder. Slight up-and-down shaking can be used to shake off the solid on the outside of the pickup to avoid spillage and reduce measurement errors. The shaking can be achieved by the transfer mechanism sliding up, down, left, and right. After the transfer mechanism drives the pickup to move above reactor A, it extends into reactor A, and the two pickup parts open again, allowing all the solid material to enter the reactor. After the pickup withdraws, the sealing cover resets to close reactor A. At this time, the weighing device reads the total weight W1 of the container and solid material (cadmium oxide), and the amount of cadmium oxide in the reactor is W. 甲1 (W 甲1 =W0-W1), to ensure batch consistency of the precursor, the ratio of cadmium oxide, oleic acid, and octadecene in each injection must be exactly the same. The controller is based on W 甲1 Calculate the volume V-OA of oleic acid. 甲1 The volume V-ODE of octadecene 甲1 Octadene was injected into V-ODE by the first inlet pump at a flow rate of A mL / min. 甲1 / A minutes, thereafter, oleic acid is injected into V-OA by a second inlet pump at a flow rate of B ml / min. 甲1 / B minutes. After injection, wait; the total duration, including the waiting time, is T.

[0080] At this time, the outlet of valve number one controls the flow into reactor A (input octadecene), the outlet of valve number two controls the flow into reactor A (input oleic acid), and the other valves are closed.

[0081] 2. After a total of T minutes, similarly, the sealing cover of reactor B is opened via the cover opening and closing assembly and rotated to the side to ensure that there is no obstruction above the opening. The weighing device reads the total weight W1 of the container and solid material (cadmium oxide). The two pickup parts of the pickup device open and are inserted into the solid material (cadmium oxide) powder. After sampling, the pickup device extends into reactor B, and the two pickup parts open again, allowing all the solid material to enter the interior of reactor B. After the pickup device withdraws, the sealing cover resets to close reactor B. The weighing device reads the total weight W2 of the container and solid material (cadmium oxide). At this time, the amount of cadmium oxide in the reactor is WB1 (WB1 = W1 - W2). To ensure batch consistency of the precursor, the ratio of cadmium oxide, oleic acid, and octadecene in each injection must be completely consistent. The controller calculates the volume of oleic acid V-OAB1 and the volume of octadecene V-ODEB1 based on WB1. Octadene is injected into V-ODE ethyl 1 / A minute by the first inlet pump at a flow rate of A mL / min. Then, oleic acid is injected into V-OA ethyl 1 / B minute by the second inlet pump at a flow rate of B mL / min. After injection, a waiting period is added, for a total duration of T minutes.

[0082] During this period, the second stage of operation takes place in reactor A. The stirrer is turned on for stirring, and a vacuum pump is used for C minutes (room temperature vacuum) to remove air and water vapor. Afterward, the heating and temperature control devices are turned on, and a vacuum is applied at 150 degrees Celsius for D minutes. Then, a waiting period is taken, totaling T minutes.

[0083] At this point, valve number one controls the flow into reactor B (input octadecene), valve number two controls the flow into reactor B (input oleic acid), valve number three controls the connection to reactor A (vacuuming), and the other two valves are closed.

[0084] After a total of 2 minutes, the sealing cover of reactor C is opened via the cover opening and closing assembly and rotated to the side to ensure that there is no obstruction above the opening. The weighing device reads the total weight W2 of the container and the solid material (cadmium oxide) stored inside. The two pickup parts of the pickup device open and are inserted into the solid material (cadmium oxide) powder under the control of a stepper motor. After sampling, the pickup device extends into reactor C, and the two pickup parts open again, allowing all the solid material to enter the interior of reactor C. After the pickup device withdraws, the sealing cover resets to close reactor C. The weighing device reads the total weight W3 of the container and the solid material (cadmium oxide). At this time, the amount of cadmium oxide in the reactor is W1 (W1 = W2 - W3). To ensure batch consistency of the precursor, the ratio of cadmium oxide, oleic acid, and octadecene in each injection must be exactly the same. The controller calculates the volume of oleic acid V-OA1 and the volume of octadecene V-ODE1 based on W1. Octadene is injected into V-ODE propane 1 / A min via the first inlet pump at a flow rate of A mL / min. Then, oleic acid is injected into V-OA propane 1 / B min via the second inlet pump at a flow rate of B mL / min. After injection, a waiting period is added, for a total duration of T min.

[0085] During this period, the second stage of operation takes place in reactor B. The stirrer is turned on for stirring, and a vacuum pump is used for C minutes (room temperature vacuum) to remove air and water vapor. Afterward, the heating and temperature control devices are turned on, and a vacuum is applied at 150 degrees Celsius for D minutes. Then, a waiting period is taken, totaling T minutes.

[0086] During this period, the third stage of operation takes place in reactor A. The stirrer continues stirring, and protective gas is introduced for E minutes, i.e., protective gas protection is implemented. Afterward, the temperature is raised to 150 degrees Celsius and held at this temperature for F minutes. Then, the temperature is lowered to 50 degrees Celsius, and after reaching 50 degrees Celsius, the process is paused. Including the waiting time, the total duration is T minutes, at which point the precursor has been generated.

[0087] At this point, valve 1 controls the flow into reactor C (input octadecene), valve 2 controls the flow into reactor C (input oleic acid), valve 3 controls the connection to reactor B (vacuuming), valve 4 controls the flow into reactor A (input protective gas), and the last valve is closed.

[0088] 3. After a total of 3 minutes, the sealing cover of reactor D is opened via the cover opening and closing assembly and rotated to the side to ensure that there is no obstruction above the opening. The weighing device reads the total weight W3 of the container and the container (cadmium oxide). The two pickup parts of the pickup device open and are inserted into the solid material (cadmium oxide) powder under the control of a stepper motor. After sampling, the pickup device extends into reactor D, and the two pickup parts open again, allowing all the solid material to enter the interior of reactor D. After the pickup device withdraws, the sealing cover resets to close reactor D. The weighing device reads the total weight W4 of the container and the solid material (cadmium oxide). At this time, the amount of cadmium oxide in the reactor is WD1 (WD1 = W3 - W4). To ensure batch consistency of the precursor, the ratio of cadmium oxide, oleic acid, and octadecene in each injection must be exactly the same. The controller calculates the volume of oleic acid V-OAD1 and the volume of octadecene V-ODED1 based on WD1. Octadene is injected into V-ODE butyl at a flow rate of A mL / min using the first inlet pump for 1 / A min. Then, oleic acid is injected into V-OA butyl at a flow rate of B mL / min using the second inlet pump for 1 / B min. After injection, a waiting period is added, for a total duration of T minutes.

[0089] During this period, the second stage of operation takes place in reactor C. The stirrer is turned on for stirring, and a vacuum pump is used to evacuate for C minutes (room temperature vacuum) to remove air and water vapor. Afterward, the heating and temperature control devices are turned on, and a vacuum is evacuated at 150 degrees Celsius for D minutes. Then, a waiting period is taken, totaling T minutes.

[0090] During this period, the third stage of operation takes place in reactor B. The stirrer continues stirring, and protective gas is introduced for E minutes, i.e., protective gas protection is implemented. Afterward, the temperature is raised to 150 degrees Celsius and held at that temperature for F minutes. Then, the temperature is lowered to 50 degrees Celsius, and after reaching 50 degrees Celsius, the process is paused. Including the waiting time, the total duration is T minutes, at which point the precursor has been generated.

[0091] During this period, reactor A undergoes its fourth stage of operation. The agitator is shut off, and the precursor is pumped out by the discharge pump at a flow rate of G ml / min for H minutes, during which all the precursor is extracted into the collection bottle.

[0092] At this point, the outlet of valve 1 controls the flow into reactor butylene (input octadecene), the outlet of valve 2 controls the flow into reactor butylene (input oleic acid), the inlet of valve 3 controls the connection to reactor propylene (vacuuming), the outlet of valve 4 controls the flow into reactor propylene (input protective gas), and the inlet of valve 5 controls the connection to reactor propylene (precursor extraction).

[0093] 4. After a total of 4 minutes, the sealing cover of reactor A is opened again via the cover opening and closing assembly and rotated to the side to ensure that there is no obstruction above the opening. The weighing device reads the total weight W4 of the container and solid material (cadmium oxide). The two pickup parts of the pickup device open and are inserted into the solid material (cadmium oxide) powder under the control of a stepper motor. After sampling, the pickup device extends into reactor A, and the two pickup parts open again, allowing all the solid material to enter the interior of reactor A. After the pickup device withdraws, the sealing cover resets to close reactor A. The weighing device reads the total weight W5 of the container and solid material (cadmium oxide). At this time, the amount of cadmium oxide in the reactor is W2 (W2 = W4 - W5). To ensure batch consistency of the precursor, the ratio of cadmium oxide, oleic acid, and octadecene in each injection must be exactly the same. The controller calculates the volume of oleic acid V-OA2 and the volume of octadecene V-ODE2 based on W2. Octadene is injected into V-ODE methyl 2 / A minutes via a first inlet pump at a flow rate of A mL / min. Then, oleic acid is injected into V-OA methyl 2 / B minutes via a second inlet pump at a flow rate of B mL / min. After injection, a waiting period is added, for a total duration of T minutes.

[0094] During this period, the second stage of operation takes place in reactor D. The stirrer is turned on for stirring, and a vacuum pump is used for C minutes (room temperature vacuuming) to remove air and water vapor. Afterwards, the heating and temperature control devices are turned on, and a vacuum is applied at 150 degrees Celsius for D minutes. Then, a waiting period is added, totaling T minutes. During this period, the third stage of operation takes place in reactor C. The stirrer continues stirring, and a protective gas is introduced for E minutes (protective gas protection). Then, the temperature is raised to 150 degrees Celsius and held at this temperature for F minutes. Afterwards, the temperature is lowered to 50 degrees Celsius, and a waiting period is added, totaling T minutes. At this point, the precursor has been generated.

[0095] During this period, reactor B undergoes its fourth stage of operation. The agitator is shut off, and the precursor is pumped out by the discharge pump at a flow rate of G ml / min for H minutes, during which all the precursor is extracted into the collection bottle.

[0096] At this point, the outlet of valve 1 controls the flow into reactor A (input octadecene), the outlet of valve 2 controls the flow into reactor A (input oleic acid), the inlet of valve 3 controls the connection to reactor D (vacuuming), the outlet of valve 4 controls the flow into reactor C (input protective gas), and the inlet of valve 5 controls the connection to reactor B (precursor extraction).

[0097] The process repeats continuously, consisting of solid cadmium oxide particles, liquid oleic acid, and liquid octadecene, and collecting the precursor (an octadecene solution of cadmium oleate).

[0098] The reaction apparatus provided by this invention, taking the preparation of selenium precursor as another example, is used as follows:

[0099] 1. The sealing cover of reactor A is opened via the cover opening and closing assembly and rotated to the side to ensure no obstruction above the opening. The weighing device reads the total weight w0 of the container and solid material (selenium powder). The two pickup parts of the pickup device open and are inserted into the solid material (selenium powder) powder. After sampling, the pickup device extends into reactor A, and the two pickup parts open again, allowing all the solid material to enter the interior of reactor A. After the pickup device withdraws, the sealing cover resets to close reactor A. The weighing device reads the total weight w1 of the container and solid material (selenium powder). At this time, the amount of selenium powder in the reactor is wA1 (wA1 = w0 - w1). To ensure batch consistency of the precursor, the ratio of selenium powder, trioctylphosphine, and octadecene in each sample must be exactly the same. The controller calculates the volume of trioctylphosphine V-TPA1 and the volume of octadecene V-ODEA1 based on wA1. Octadene is injected into V-ODE methyl 1 / a min by a first inlet pump at a flow rate of a mL / min. Subsequently, trioctylphosphine is injected into V-TP methyl 1 / b min by a second inlet pump at a flow rate of b mL / min. After injection, a waiting period is added, and the total waiting time is t.

[0100] At this point, the outlet of valve number one controls the flow into reactor A (input octadecene), the outlet of valve number two controls the flow into reactor A (input trioctylphosphine), and the other three valves are closed.

[0101] 2. After a total of T minutes, the sealing cover of reactor B is opened via the cover opening and closing assembly and rotated to the side to ensure that there is no obstruction above the opening. The weighing device reads the total weight w1 of the container and solid material (selenium powder). The two pickup parts of the pickup device open and are inserted into the solid material (selenium powder) powder under the control of a stepper motor. After sampling, the pickup device extends into reactor B, and the two pickup parts open again, allowing all the solid material to enter the interior of reactor B. After the pickup device withdraws, the sealing cover resets to close reactor B. The weighing device reads the total weight w2 of the container and solid material (selenium powder). At this time, the amount of selenium powder in the reactor is wB1 (wB1 = w1 - w2). To ensure batch consistency of the precursor, the ratio of selenium powder, trioctylphosphine, and octadecene in each sample must be exactly the same. The controller calculates the volume of trioctylphosphine V-TPB1 and the volume of octadecene V-ODEB1 based on wB1. Octadene is injected into V-ODE ethyl at a flow rate of a mL / min using a first inlet pump for 1 / a min. Subsequently, trioctylphosphine is injected into V-OA ethyl at a flow rate of b mL / min using a second inlet pump for 1 / b min. After injection, a waiting period is added, for a total duration of t minutes.

[0102] During this period, the second stage of operation takes place in reactor A. The stirrer is turned on for stirring, and a vacuum pump is used for c minutes (i.e., vacuuming at room temperature) to remove air and water vapor. Afterward, the heating and temperature control devices are turned on, and a vacuum is evacuated at 150 degrees Celsius for d minutes. Then, a waiting period is taken, totaling t minutes.

[0103] At this time, the outlet control of valve No. 1 controls the flow into reactor B (input octadecene), the outlet control of valve No. 2 controls the flow into reactor B (input trioctylphosphine), the inlet control of valve No. 3 (five-way outlet valve) controls the connection to reactor A (vacuuming), and the other two valves are closed.

[0104] 3. After a total of 2 minutes, the sealing cover of reactor C is opened via the cover opening and closing assembly and rotated to the side to ensure that there is no obstruction above the opening. The weighing device reads the total weight w2 of the container and solid material (selenium powder). The two pickup parts of the pickup device open and are inserted into the solid material (selenium powder) powder under the control of a stepper motor. After sampling, the pickup device extends into reactor C, and the two pickup parts open again, allowing all the solid material to enter the interior of reactor C. After the pickup device withdraws, the sealing cover resets to close reactor C. The weighing device reads the total weight w3 of the container and solid material (selenium powder). At this time, the amount of selenium powder in the reactor is wC1 (wC1 = w2 - w3). To ensure batch consistency of the precursor, the ratio of selenium powder, trioctylphosphine, and octadecene in each sample must be exactly the same. The controller calculates the volume of trioctylphosphine V-OAC1 and the volume of octadecene V-ODEC1 based on wC1. Octadene is injected into V-ODE propionate at a flow rate of a mL / min using a first inlet pump for 1 / a min. Subsequently, trioctylphosphine is injected into V-TP propionate at a flow rate of b mL / min using a second inlet pump for 1 / b min. After injection, a waiting period is added, for a total duration of t minutes.

[0105] During this period, the second stage of operation takes place in reactor B. The stirrer is turned on for stirring, and a vacuum pump is used for c minutes (room temperature vacuum) to remove air and water vapor. Afterward, the heating and temperature control devices are turned on, and a vacuum is applied at 150 degrees Celsius for d minutes. Then, a waiting period is taken, totaling t minutes.

[0106] During this period, the third stage of operation takes place in reactor A. The stirrer continues stirring, and protective gas is introduced for e minutes, i.e., protective gas protection is implemented. Afterward, the temperature is raised to 150 degrees Celsius and held at that temperature for f minutes. Then, the temperature is lowered to 50 degrees Celsius, and after reaching 50 degrees Celsius, the process is paused. Including the waiting time, the total duration is t minutes, at which point the precursor has been generated.

[0107] At this point, the outlet of valve number one controls the flow into reactor C (input octadecene), the outlet of valve number two controls the flow into reactor C (input trioctylphosphine), the inlet of valve number three (five-way outlet) controls the connection to reactor B (vacuuming), the outlet of valve number four controls the flow into reactor A (input protective gas), and the last valve is closed.

[0108] 4. After a total of 3 minutes, the sealing cover of reactor D is opened via the cover opening and closing assembly and rotated to the side to ensure that there is no obstruction above the opening. The weighing device reads the total weight W3 of the container and solid material (selenium powder). The two pickup parts of the pickup device open and are inserted into the solid material (selenium powder) powder under the control of a stepper motor. After sampling, the pickup device extends into reactor D, and the two pickup parts open again, allowing all the solid material to enter the interior of reactor D. After the pickup device withdraws, the sealing cover resets to close reactor D. The weighing device reads the total weight w4 of the container and solid material (selenium powder). At this time, the amount of selenium powder in the reactor is wD1 (wD1 = w3 - w4). To ensure batch consistency of the precursor, the ratio of selenium powder, trioctylphosphine, and octadecene in each sample must be exactly the same. The controller calculates the volume of trioctylphosphine V-TPD1 and the volume of octadecene V-ODED1 based on WD1. Octadene is injected into V-ODE butyl at a flow rate of a mL / min for 1 / A min by the first inlet pump. Then, oleic acid is injected into V-TP butyl at a flow rate of b mL / min for 1 / b min by the second inlet pump. After injection, a waiting period is added, for a total duration of t minutes.

[0109] During this period, the second stage of operation takes place in reactor C. The stirrer is turned on for stirring, and a vacuum pump is used to evacuate the reactor for c minutes (room temperature vacuum) to remove air and water vapor. Afterward, the heating and temperature control devices are turned on, and a vacuum is evacuated at 150 degrees Celsius for d minutes. Then, a waiting period is taken, totaling t minutes.

[0110] During this period, the third stage of operation takes place in reactor B. The stirrer continues stirring, and protective gas is introduced for e minutes, i.e., protective gas protection is implemented. Afterward, the temperature is raised to 150 degrees Celsius and held at that temperature for f minutes. Then, the temperature is lowered to 50 degrees Celsius, and after reaching 50 degrees Celsius, the process is paused. Including the waiting time, the total duration is t minutes, at which point the precursor has been generated.

[0111] During this period, reactor A undergoes its fourth stage of operation. The agitator is shut off, and the precursor is pumped out by the discharge pump at a flow rate of g mL / min for h minutes, during which all the precursor is extracted into the collection bottle.

[0112] At this point, the outlet control of valve No. 1 controls the flow into reactor No. 1 (inputting octadecene), the outlet control of valve No. 2 controls the flow into reactor No. 1 (inputting trioctylphosphine), the inlet control of valve No. 3 (five-way outlet valve) controls the connection to reactor No. 1 (vacuuming), the outlet control of valve No. 4 controls the flow into reactor No. 2 (inputting protective gas), and the inlet control of valve No. 5 (five-way sample outlet valve) controls the connection to reactor No. 1 (extracting precursors).

[0113] 5. After a total of 4 minutes, the sealing cover of reactor A is opened via the cover opening and closing assembly and rotated to the side to ensure that there is no obstruction above the opening. The weighing device reads the total weight w4 of the container and solid material (selenium powder). The two pickup parts of the pickup device open and are inserted into the solid material (selenium powder) powder under the control of a stepper motor. After sampling, the pickup device extends into reactor A, and the two pickup parts open again, allowing all the solid material to enter the interior of reactor A. After the pickup device withdraws, the sealing cover resets to close reactor A. The weighing device reads the total weight w5 of the container and solid material (selenium powder). At this time, the amount of cadmium oxide in the reactor is w2 (w2 = w4 - w5). To ensure batch consistency of the precursor, the ratio of selenium powder, trioctylphosphine, and octadecene must be exactly the same for each sample. The controller calculates the volume of trioctylphosphine V-TP2 and the volume of octadecene V-ODE2 based on w2. Octadene is injected into V-ODE methyl 2 / A minutes by a first inlet pump at a flow rate of a mL / min. Subsequently, trioctylphosphine is injected into V-TP methyl 2 / b minutes by a second inlet pump at a flow rate of b mL / min. After injection, a waiting period is added, for a total duration of t minutes.

[0114] During this period, the second stage of operation takes place inside reactor D. The stirrer is turned on for stirring, and a vacuum pump is used to evacuate the reactor for c minutes (room temperature vacuum) to remove air and water vapor. Afterward, the heating and temperature control devices are turned on, and a vacuum is evacuated at 150 degrees Celsius for d minutes. Then, a waiting period is added, for a total duration of t minutes.

[0115] During this period, the third stage of operation takes place in reactor C. The stirrer continues stirring, and protective gas is introduced for e minutes, i.e., protective gas protection is implemented. Afterward, the temperature is raised to 150 degrees Celsius and held at this temperature for f minutes. Then, the temperature is lowered to 50 degrees Celsius, and after reaching 50 degrees Celsius, the process is paused. Including the waiting time, the total duration is t minutes, at which point the precursor has been generated.

[0116] During this period, reactor B undergoes its fourth stage of operation. The agitator is shut off, and the precursor is pumped out by the discharge pump at a flow rate of G ml / min for h minutes, during which all the precursor is extracted into the collection bottle.

[0117] At this point, the outlet of valve 1 controls the flow into reactor A (input octadecene), the outlet of valve 2 controls the flow into reactor A (input trioctylphosphine), the inlet of valve 3 (five-way outlet valve) controls the connection to reactor D (vacuuming), the outlet of valve 4 controls the flow into reactor C (input protective gas), and the inlet of valve 5 (five-way sample outlet valve) controls the connection to reactor B (precursor extraction).

[0118] 6. The process repeats continuously, consisting of solid selenium powder particles, liquid trioctylphosphine, and liquid octadecene, and collecting the precursor (a solution of selenium powder and trioctylphosphine in octadecene).

[0119] Of course, the reaction apparatus provided in this embodiment is not limited to the preparation of precursor solutions for quantum dot synthesis, but can also be applied to the preparation of other chemical solutions using solids and liquids as raw materials.

[0120] Obviously, the above embodiments are merely illustrative examples for clear explanation and are not intended to limit the implementation. Those skilled in the art will recognize that other variations or modifications can be made based on the above description. It is neither necessary nor possible to exhaustively list all possible implementations here. However, obvious variations or modifications derived therefrom are still within the protection scope of this invention.

Claims

1. A reaction apparatus, characterized in that, include: The sample introduction system (1) includes a solid metering and transfer component and a fluid sample introduction component, wherein the solid metering and transfer component is used for picking up and metering solid materials; The reaction system (4) includes at least one set of reactors, and each set of reactors is provided with at least two reactors; each reactor is provided with a solid feed inlet (41), a liquid inlet, an exhaust outlet (45) and a liquid outlet (46); the solid feed inlet (41) is used to receive solid materials transferred by the solid metering and transfer component, and the liquid inlet is connected to the liquid inlet path of the fluid injection component; The discharge system (3) includes an exhaust component and a discharge component. The input end of the exhaust component is connected to the exhaust port (45), and the input end of the discharge component is connected to the liquid discharge port (46). The controller (5) is connected to the injection system (1), the reaction system (4), and the discharge system (3). The controller (5) is used to control at least the fluid injection volume and fluid injection flow rate of the injection system (1), the opening and closing status of the inlet and outlet of the reactor, and the discharge volume and discharge flow rate of the discharge system (3).

2. The reaction apparatus according to claim 1, characterized in that, The solid metering and transfer assembly includes a pickup (11), a weighing component (13), and a transfer mechanism (14). The pickup (11) is fixedly connected to the transfer end of the transfer mechanism (14). The weighing component (13) is used to carry the container (12) containing solid materials. The transfer mechanism (14) is adapted to drive the pickup (11) to transfer solid materials to the solid feed inlet (41). The pickup (11) is connected to the controller (5), and the weighing component (13) is connected to the controller (5).

3. The reaction apparatus according to claim 2, characterized in that, The pickup component (11) includes a first pickup part, a second pickup part, and a moving drive component. Each pickup part is hollow inside. The first pickup part or the second pickup part is connected to the drive end of the moving drive component. The transfer mechanism (14) is configured as a two-axis linear displacement module or a three-axis linear displacement module.

4. The reaction apparatus according to claim 1, characterized in that, The fluid injection assembly includes a first liquid injection assembly and a second liquid injection assembly. The reactor is provided with a first liquid inlet (42) and a second liquid inlet (43) spaced apart. The output end of the first liquid injection assembly is connected to the first liquid inlet (42), and the output end of the second liquid injection assembly is connected to the second liquid inlet (43).

5. The reaction apparatus according to claim 4, characterized in that, The first liquid inlet assembly includes a first liquid reservoir (15), a first liquid inlet pump (16), and a first valve (17) connected in sequence. The first valve (17) is configured as a one-inlet, multiple-outlet structure. The inlet end of the first valve (17) is connected to the output end of the first liquid inlet pump (16), and each outlet end of the first valve (17) is connected to each of the first liquid inlets (42) of a set of reactors. The first liquid inlet pump (16) and the first valve (17) are respectively connected to the controller (5); and / or The second liquid inlet assembly includes a second liquid storage tank (18), a second liquid inlet pump (19), and a second valve (20) connected in sequence. The second valve (20) is configured as a one-inlet-multiple-outlet structure. The inlet end of the second valve (20) is connected to the output end of the second liquid inlet pump (19). Each outlet end of the second valve (20) is connected to each of the second liquid inlets (43) of a set of reactors. The second liquid inlet pump (19) and the second valve (20) are respectively connected to the controller (5).

6. The reaction apparatus according to any one of claims 1-5, characterized in that, The reaction device also includes a protective gas inlet assembly. The reactor is provided with an inlet (44), and the output end of the protective gas inlet assembly is connected to the inlet (44). The protective gas inlet assembly includes a protective gas source (21), a flow controller (22), and a third valve (23) connected in sequence. The third valve (23) is configured as a one-inlet-multiple-outlet structure. The inlet end of the third valve (23) is connected to the output end of the flow controller (22). Each outlet end of the third valve (23) is connected to each inlet (44) of a set of reactors. The flow controller (22) and the third valve (23) are respectively connected to the controller (5).

7. The reaction apparatus according to any one of claims 1-5, characterized in that, The exhaust assembly includes a vacuum pump (31) and a fourth valve (32). The fourth valve (32) is configured with a multi-inlet and one-outlet structure. Each inlet end of the fourth valve (32) is respectively connected to each exhaust port (45) of a set of reactors. The outlet end of the fourth valve (32) is connected to the input end of the vacuum pump (31). The vacuum pump (31) and the fourth valve (32) are respectively connected to the controller (5).

8. The reaction apparatus according to any one of claims 1-5, characterized in that, The discharge assembly includes a fifth valve (34), a discharge pump (33), and a collection and storage device connected in sequence. The fifth valve (34) is configured as a multi-inlet and one-outlet structure. Each inlet end of the fifth valve (34) is respectively connected to each drain port (46) of a set of reactors. The outlet end of the fifth valve (34) is connected to the input end of the discharge pump (33). The fifth valve (34) and the discharge pump (33) are respectively connected to the controller (5).

9. The reaction apparatus according to any one of claims 1-5, characterized in that, The reaction system (4) further includes a stirring assembly, which is configured corresponding to the reactor. The stirring assembly includes a stirring motor (47) and a stirrer (48). The stirring motor (47) is installed outside the reactor, and the stirrer (48) is driven by the driving side of the stirring motor (47) and extends into the reactor. Alternatively, the reactor further includes a cover opening and closing assembly, with one cover opening and closing assembly configured for each reactor.

10. The reaction apparatus according to claim 9, characterized in that, The cover opening and closing assembly includes a sealing cover (49), a sliding actuator (410), and a rotary actuator (411). The mounting end of the sliding actuator (410) is fixedly connected to the reactor, and the mounting end of the rotary actuator (411) is fixedly connected to the driving end of the sliding actuator (410). The sealing cover (49) is connected to the driving end of the rotary actuator (411). The sliding actuator (410) and the rotary actuator (411) are adapted to drive the sealing cover (49) to move closer to close the solid feed inlet (41) or away from open the solid feed inlet (41).

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