Reaction kettle for catalytic synthesis reaction and use method thereof
By employing an intervening pressure-bearing gas-conducting structure and an isolated drug chamber mechanism, the problems of high interfacial resistance and catalyst deactivation in traditional three-phase reactions are solved, enabling efficient and stable catalytic synthesis reactions suitable for addition and polymerization reactions of short-chain fluorinated organic compounds.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-26
- Publication Date
- 2026-04-10
AI Technical Summary
In traditional addition and polymerization reactions of short-chain fluorinated organic compounds, the high resistance at the gas-liquid-solid three-phase interface and the tendency for catalysts to aggregate and deactivate during single-stage addition lead to low catalytic efficiency and incomplete reactions.
The system employs an intervening pressure-bearing gas-conducting structure and an isolation drug chamber mechanism. The intervening pressure-bearing gas-conducting structure directly introduces gaseous raw materials into the liquid reaction system, forming a three-dimensional dispersion that breaks the traditional two-dimensional interface. The isolation drug chamber mechanism adds catalysts in batches and in a distributed manner, avoiding catalyst aggregation and deactivation.
It significantly improves the mass transfer efficiency and catalyst utilization of the gas-liquid-solid three-phase reaction system, prolongs the catalytic activity retention time, increases the reaction rate and product yield, reduces equipment burden and safety risks, and is suitable for large-scale continuous production.
Smart Images
Figure CN121819677A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application belongs to the field of organic chemical industry, and particularly relates to a reaction kettle for catalytic synthesis reaction and a use method thereof. BACKGROUND
[0002] Short-chain fluorine-containing organic compounds, such as fluoroether, fluoroalkene, etc., are widely used in high-end materials, medicine, electronics, etc. due to their excellent chemical stability, insulation and biocompatibility. The addition reaction or polymerization reaction of such compounds as monomers is considered as an efficient industrial production method due to its direct synthesis path and high selectivity. In the traditional process of such reactions, gas-phase raw materials (such as short-chain fluoroalkene), liquid organic solvents and slightly soluble solid or liquid-solid mixed catalysts (or initiators, aids) are usually involved, thereby forming a typical gas-liquid-solid three-phase reaction system in the reaction kettle.
[0003] In the above-mentioned three-phase reaction system, due to the difference in density and form of each phase material, a natural stratification state is often presented in the conventional stirred reaction kettle: the gas-phase raw material is concentrated in the upper part of the kettle, the liquid solvent is located in the middle part, and the solid or mixed-state catalyst / aids are deposited at the bottom of the kettle. This state leads to a serious "reaction interface passivation" problem.
[0004] Specifically, this problem mainly manifests in two aspects: Firstly, after the one-time input of the slightly soluble catalyst / aids, the solid particles are prone to aggregate and settle, greatly reducing the effective contact specific surface area of the catalyst with the solvent. This not only prolongs the activation time of the catalyst system, but also in the slow activation process, the outer layer of the catalyst is easily combined with impurities or by-products in the system to be "poisoned" and deactivated, and the active components wrapped inside cannot continue to dissolve and release, ultimately leading to a significant decrease in the efficiency of the entire catalytic system or even complete failure.
[0005] Secondly, the gas-phase raw material mainly contacts with the liquid-solid catalyst system below in a two-dimensional planar interface, the mass transfer resistance is large, and the raw material gas is difficult to quickly and fully dissolve and diffuse to the liquid-phase reaction zone and contact with the catalyst active sites, causing a series of problems such as low reaction rate, incomplete conversion, and unsatisfactory product yield.
[0006] To alleviate the above-mentioned interface mass transfer resistance, the traditional process usually takes measures such as strengthening stirring, increasing reaction temperature or reaction pressure, etc. to improve the interphase mixing. However, these schemes have obvious limitations: for the slightly soluble catalytic system, simply increasing the mechanical stirring intensity has limited effect on improving the solid catalyst aggregation and dissolution efficiency, and easily leads to violent fluctuation of liquid level, increasing material loss; while increasing temperature and pressure can promote mass transfer to a certain extent, but not only can aggravate the side reaction, affect the product selectivity, but also put higher requirements on the pressure-bearing and temperature control capacity of the equipment, introduce potential equipment failure and safety production risk, while the energy consumption and cost also increase accordingly.
[0007] Therefore, the prior art lacks a method and device that can effectively solve the gas-liquid-solid three-phase interface mass transfer resistance and maintain the sustained high activity of the catalyst without significantly increasing the harshness of the reaction conditions and without destroying the stability of the system. SUMMARY
[0008] The purpose of the present application is to provide a reaction kettle for catalytic synthesis reaction and a method for using the same, to solve the problems of low catalytic efficiency and insufficient reaction caused by large gas-liquid-solid three-phase interface resistance and easy aggregation and deactivation of one-time addition of catalyst in traditional short-chain fluorine-containing organic compound addition and polymerization reaction. The present application breaks the gas-liquid two-dimensional contact interface by using an intervening pressure-bearing gas guiding structure, and uses an isolation drug cabin mechanism to distribute the catalyst without interrupting the reaction and destroying the anaerobic environment, forming a stepwise feeding activity maintenance process. Thus, the catalyst utilization efficiency and system activity are significantly improved, and the reaction rate, product yield and batch stability are improved.
[0009] To solve the above-mentioned problems, the first aspect of the present application provides a reaction kettle for catalytic synthesis reaction, comprising: a kettle body (4); a stirring mechanism comprising a driving device (2) and a stirring paddle (5) arranged in the kettle body (4), the driving device (2) being used to drive the stirring paddle (5); an intervening pressure-bearing gas guiding structure comprising a gas guiding pipe section (3), the gas guiding pipe section (3) extending into the kettle body (4), and the end thereof being located in the mixing area acted on by the paddle of the stirring paddle (5), a plurality of gas guiding holes (9) being formed on the pipe wall of the gas guiding pipe section for directly guiding the pressurized gas phase raw material into the liquid reaction system.
[0010] The core of the reactor provided by the present invention lies in the installation of an intervening pressure-bearing gas-guiding structure. This structure directly introduces pressurized gaseous raw materials into the liquid reaction system through a gas-guiding pipe section extending below the liquid surface and gas-guiding holes (9) on its pipe wall, thereby breaking the traditional two-dimensional gas-liquid interface and forming a three-dimensional dispersed bubble group. With the synergistic effect of the stirring paddle (5), this greatly increases the gas-liquid contact area, fundamentally solving the problem of high mass transfer resistance at the gas-liquid interface, and realizing the rapid and uniform dispersion and dissolution of gaseous raw materials in the liquid phase, laying the foundation for efficient catalytic reactions.
[0011] Furthermore, the end of the air guide pipe section (3) is a spiral coil (8), which is coaxially sleeved on the rotating shaft of the stirring paddle (5) and does not rotate with it.
[0012] Furthermore, a valve (1) is provided at the upper end of the air duct section (3).
[0013] Furthermore, the spiral coil (8) extends below the liquid surface to a depth of not less than two-thirds of the liquid level height.
[0014] Furthermore, the reactor also includes a dispersion head (10), which is disposed adjacent to or coaxially connected to the blades of the stirring paddle (5) for shearing and dispersing the bubbles discharged from the air guide hole (9).
[0015] Another aspect of the present invention provides a reaction vessel for a distributed catalytic synthesis reaction, the reaction vessel comprising: a vessel body (4); a stirring mechanism including a driving device (2) and a stirring paddle (5) disposed within the vessel body (4), the driving device (2) being used to drive the stirring paddle (5); and an isolation tank mechanism disposed within the vessel body (4) for dynamically and isolatedly adding pre-stored solid or liquid catalysts and / or additives to the reaction system in batches during the reaction process.
[0016] Further, the isolation drug chamber mechanism includes: a drug chamber mounting frame (30), rotatably disposed within the vessel body (4); at least one isolation drug chamber (21), fixed on the drug chamber mounting frame (30), for pre-storing solid or liquid catalysts and / or additives, the isolation drug chamber (21) having an openable and closable discharge port; a drive assembly for driving the drug chamber mounting frame (30) to rotate; and a feeding execution device, fixedly disposed within the vessel body (4) and opposite to the drug chamber mounting frame (30), for opening the discharge port to feed the solid or liquid catalysts and / or additives into the vessel body (4) when the isolation drug chamber (21) rotates to the feeding position aligned with the feeding execution device.
[0017] The reactor provided by the present invention further incorporates an isolation tank mechanism, which includes a rotatable tank mounting frame (30), at least one isolation tank (21) fixed thereon, a drive assembly, and a fixed feeding execution device. The core working mechanism of this mechanism is as follows: during the reaction, the isolation tank (21) pre-loaded with solid or liquid catalysts and / or additives is rotated to a fixed feeding position by the drive assembly, and its discharge port is opened by the feeding execution device, thereby achieving batch and distributed precise addition of solid or liquid catalysts and / or additives without interrupting the reaction or damaging the oxygen-free sealed environment inside the reactor. This technical solution fundamentally overcomes the defects of solid catalyst aggregation, insufficient dissolution, and easy encapsulation and deactivation caused by one-time feeding in traditional processes, and can dynamically maintain the high activity of the catalytic system, thereby significantly extending the effective reaction time and greatly improving the utilization efficiency of the catalyst and the overall yield of a single reaction.
[0018] Furthermore, the isolation medicine chamber mechanism includes multiple independent isolation medicine chambers (21) arranged circumferentially along the medicine chamber mounting frame (30).
[0019] Furthermore, the feeding execution device is an electromagnetic push rod (24), and the tail of the isolation drug chamber (21) is provided with an execution push rod (22), and the execution push rod (22) is provided with a conductive magnetic contact (23); when the isolation drug chamber (21) rotates to the feeding station, the electromagnetic push rod head contact (12) interacts with the conductive magnetic contact (23) to trigger the execution push rod (22).
[0020] Furthermore, the reactor also includes a controller (14), which is communicatively connected to the drive assembly and the electromagnetic push rod (24); the electromagnetic push rod head contact (12) and the conductive magnetic contact (23) generate a trigger signal based on the action, and the controller (14) is used to control the drive assembly to pause and trigger the push rod (22) to perform the feeding action when the trigger signal is received.
[0021] Furthermore, the structure of the isolation chamber mechanism can withstand a temperature of not less than 100°C and a pressure of not less than 5MPa, and is isolated from the liquid reaction system inside the vessel (4).
[0022] Another aspect of the present invention provides a method for operating a reactor for a distributed catalytic synthesis reaction. The reactor for the distributed catalytic synthesis reaction described above includes the following steps: before the start of the catalytic synthesis reaction, a solid or liquid catalyst and / or auxiliaries are pre-stored in one or more isolation tanks (21); during the catalytic synthesis reaction, when it is necessary to add a solid or liquid catalyst and / or auxiliaries, one of the isolation tanks (21) pre-stored with materials is rotated to a fixed feeding station; at the feeding station, the front door (20) of the isolation tank is opened to add the pre-stored solid or liquid catalyst and / or auxiliaries into the liquid reaction system of the reactor body (4).
[0023] Furthermore, the process of rotating one of the pre-stored material isolation chambers (21) to a fixed feeding station is specifically carried out by manual or automatic control based on a preset reaction sequence, thereby feeding the solid or liquid catalyst and / or additives in batches.
[0024] According to another aspect of the present invention, the present invention also provides a method for a distributed catalytic synthesis reaction using the reaction vessel described above, and comprising the following steps: adding a solvent, an initial solid or liquid catalyst and / or auxiliaries for initiating the reaction to the vessel body (4), and establishing an oxygen-free reaction environment; activating a stirring mechanism and continuously introducing gaseous raw materials through the intervening pressure-bearing gas guiding structure to initiate the reaction; during the reaction, by controlling the isolation tank mechanism, adding supplementary solid or liquid catalysts and / or auxiliaries pre-stored in different isolation tanks (21) to the liquid reaction system in batches.
[0025] The key to the distributed catalytic synthesis reaction method provided by the present invention lies in the use of the aforementioned dedicated reactor and the sequential execution of three core steps: first, establishing an oxygen-free liquid reaction environment in the reactor body (4); then, starting stirring and continuously introducing gaseous raw materials into the liquid through an interventional pressure-bearing gas-conducting structure to initiate the reaction; finally, during the continuous reaction, by controlling the isolation tank mechanism, solid or liquid catalysts and / or additives pre-placed in different isolation tanks (21) are added to the system in batches. The mechanism of this method is to organically combine the two key processes of "deep dispersion of gaseous raw materials" and "dynamic replenishment of catalysts" in time and space: continuous pressurized gas supply ensures a stable supply of reactant concentration and efficient mass transfer, while the distributed addition of catalysts avoids the deactivation and decay of active components caused by one-time addition, thereby dynamically maintaining the high activity of the catalytic system. Its technical effect is to completely solve the problems of large interfacial resistance and low catalyst utilization in traditional three-phase reactions, realize the high efficiency, stability and continuity of the reaction process, and significantly improve the product yield, purity and economic efficiency of the process.
[0026] Furthermore, the solid or liquid catalyst and / or additives are added in batches 4 to 6 times, and the mass of each batch is the proportion of the total mass of the batches added to the total mass of the batches, which meets the following conditions: the proportion of the first batch is 20% to 50%; the proportion of each batch in the second to penultimate batches is 10% to 20%; and the proportion of the last batch is 0% to 10%.
[0027] Furthermore, the distributed catalytic synthesis reaction is a synthesis reaction of short-chain fluorinated organic compounds.
[0028] Furthermore, the synthesis reaction of the short-chain fluorinated organic compound includes the addition reaction of hexafluoropropylene with ethanol or trifluoroethanol, the polymerization reaction of hexafluoropropylene, and the polymerization reaction of trifluoromethyl trifluorovinyl ether.
[0029] Further, the gaseous feedstock includes one or more of trifluoroethylene, trifluoromethyltrifluorovinyl ether, and hexafluoropropylene; the solvent includes one or more of acetonitrile, dimethyl sulfoxide, dimethylformamide, dimethylacetamide, ethylene glycol dimethyl ether, and tetrahydrofuran; the solid or liquid catalyst includes one or more of tetramethylammonium fluoride, tetraethylammonium fluoride, tetrabutylammonium fluoride, potassium cyanate, potassium thiocyanate, potassium fluoride, potassium hydrofluoride, cesium hydrofluoride, cesium fluoride, and potassium hydroxide; and the solid additive includes one or more of crown ether, tetramethylethylenediamine, and polyethylene glycol.
[0030] Furthermore, the total concentration of the solid or liquid catalyst and / or auxiliaries in the liquid reaction system is 0.1-2 mol / L.
[0031] Furthermore, during the distributed catalytic synthesis reaction, the reaction temperature is 30-100℃, and the reaction pressure inside the vessel (4) is 0.1-5MPa.
[0032] The above-described technical solution of the present invention has the following beneficial technical effects: 1. Significantly improves the mass transfer efficiency and reaction interface activity of the gas-liquid-solid three-phase reaction system. Through an intervening pressurized gas-conducting structure, gaseous raw materials are directly pressurized and introduced into the liquid reaction system (preferably through a spiral coil and gas guide holes). Under the synergistic action of the stirring paddle and dispersing head, a three-dimensional dispersion is formed, completely breaking the traditional two-dimensional interface contact mode. This greatly increases the gas-liquid contact area, fundamentally solving the problem of "reaction interface passivation," allowing the raw material gas to dissolve and diffuse rapidly, thereby significantly improving the reaction rate and raw material conversion rate.
[0033] 2. It achieves efficient and dynamic utilization of the catalyst, significantly extending the activity retention time of the catalytic system. Utilizing the isolated catalyst chamber mechanism and its intelligent control system, catalysts and / or additives can be precisely added in batches and in a distributed manner according to a preset program without interrupting the reaction or disrupting the oxygen-free sealed environment. This effectively avoids problems such as solid or liquid catalyst aggregation, encapsulation, incomplete dissolution, and easy "poisoning" deactivation caused by traditional one-time feeding, allowing catalytic activity to be dynamically maintained and significantly improving the total utilization rate and effective action time of the catalyst in a single reaction.
[0034] 3. Improved process continuity, stability, and single-reaction yield efficiency. Combining efficient deep-dispersion gas supply with dynamic catalyst replenishment allows reactant concentration and catalytic activity to be maintained at optimal levels over a longer period. This not only reduces batch interruptions, contamination risks, and energy consumption caused by mid-process reactor refueling, but also extends the run time of a single reaction, thus significantly improving unit-time capacity and product yield, making it particularly suitable for large-scale continuous production.
[0035] 4. Enhanced process safety and controllability, and reduced overall operating costs. This invention optimizes mass transfer and feeding methods, enabling efficient reactions under relatively mild temperature (30-100℃) and pressure (0.1-5MPa) conditions. This reduces dependence on extreme equipment conditions and minimizes equipment wear, safety hazards, and increased side reactions caused by intensified stirring and increased temperature and pressure. Simultaneously, improved catalyst utilization efficiency directly reduces the consumption of expensive catalysts, and distributed feeding facilitates finer process control and more stable product quality.
[0036] 5. This invention provides a highly versatile catalytic synthesis reaction platform. The reaction vessel and method described in this invention are not only clearly applicable to the addition and polymerization reactions of various short-chain fluorinated organic compounds (such as the addition of hexafluoropropylene to alcohols, the polymerization of hexafluoropropylene or trifluoromethyl trifluorovinyl ether, etc.), but also, its core approach to solving the three-phase interface mass transfer and catalyst dynamics maintenance has important reference value and potential for widespread application in other similar heterogeneous catalytic synthesis systems involving gaseous feedstocks and slightly soluble catalysts. Attached Figure Description
[0037] Figure 1 This is a schematic diagram of the internal structure of a reaction vessel used for distributed catalytic synthesis in an embodiment of the present invention; Figure 2 This is a schematic diagram of the structure of an isolation medicine chamber mechanism in an embodiment of the present invention; Figure 3 This is an exploded view of the structure of an isolation medicine compartment in an embodiment of the present invention.
[0038] Figure label: 1: Valve; 2: Drive unit; 3: Gas guide pipe section; 4: Reactor body; 5: Stirring paddle; 6: Liquid solvent; 7: Solid catalyst and / or auxiliaries; 8: Spiral coil; 9: Gas guide hole; 10: Dispersing head; 11: Electromagnetic push rod is in the connected state with the isolation chamber; 12: Electromagnetic push rod head contact; 13: The induction signal control line of the front door of the isolation chamber is in the conductive state; 14: Controller; 15: Relay; 16: Alignment signal detection point; 17: Electromagnetic push rod 18: Power supply line for the pole; 19: Control line for the induction signal of the front door of the isolation medicine compartment is disconnected; 20: Control line for the isolation medicine compartment; 21: Isolation medicine compartment; 22: Actuating push rod; 23: Conductive magnetic contact; 24: Electromagnetic push rod; 25: Drive motor; 26: Drive wheel; 27: Driven wheel; 28: Driven wheel rotation direction; 29: Drive wheel rotation direction; 30: Medicine compartment mounting bracket; 31: Fixing hole between the isolation medicine compartment and the medicine compartment mounting bracket. Detailed Implementation
[0039] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to specific embodiments and the accompanying drawings. It should be understood that these descriptions are merely exemplary and not intended to limit the scope of the invention. Furthermore, descriptions of well-known structures and techniques are omitted in the following description to avoid unnecessarily obscuring the concept of the invention.
[0040] The following is combined Figures 1 to 3 The reaction vessel for distributed catalytic synthesis provided by the present invention will be described.
[0041] Figure 1 This is a schematic diagram of the internal structure of a reaction vessel used for distributed catalytic synthesis in an embodiment of the present invention.
[0042] See Figure 1In some embodiments, the reactor for distributed catalytic synthesis provided by the present invention mainly includes: a reactor body 4, a stirring mechanism, an intervening pressure-bearing gas guiding structure, and a dispersion head 10; wherein, the stirring mechanism includes a driving device 2 and a stirring paddle 5 disposed in the reactor body 4, the driving device 2 being a stirring motor for driving the stirring paddle 5 to rotate, and the stirring paddle 5 preferably having a rudder-type structure; the intervening pressure-bearing gas guiding structure includes a gas guiding pipe section 3, the upper end of which is provided with a valve 1 for controlling the gas flow and pressure; the gas guiding pipe section 3 extends into the reactor, and its end is constructed as a spiral coil 8, which is coaxially sleeved on the rotating shaft of the stirring paddle 5 and does not rotate with it, its The depth of the submerged part is no less than two-thirds of the liquid level and is located within the mixing zone acted upon by the impeller blades of the agitator 5. Multiple gas guide holes 9 are uniformly distributed on the wall of the spiral coil 8 immersed in the liquid. This structural design allows the raw material gas, maintaining a positive pressure above 0.2 MPa, to be directly introduced into the liquid reaction system. Working in conjunction with the dispersing head 10 that rotates with the agitator 5, it shears, breaks, and disperses the escaping bubbles into the liquid phase, thus completely breaking the traditional two-dimensional gas-liquid interface and forming a three-dimensional mixing system. This fundamentally solves the problem of "reaction interface passivation" and greatly improves gas-liquid mass transfer efficiency and reaction rate. Furthermore, the optimized deep gas-liquid mixing mode ensures that the gaseous raw material can be rapidly and uniformly delivered to the catalytic active sites. This creates an ideal reaction environment for the distributed, on-demand, precise addition and dynamic maintenance of catalyst activity through the isolated reagent chamber mechanism. The combination of these two aspects achieves efficient and long-term utilization of the catalyst. Meanwhile, this efficient mass transfer method allows reactions to be carried out under mild conditions (such as 30-100℃, 0.1-5MPa), which significantly reduces the dependence on extreme equipment performance and the safety risks and energy consumption caused by intensified operation, providing reliable support for continuous, stable, and low-cost large-scale production.
[0043] Figure 2 This is a schematic diagram of the structure of an isolation medicine chamber mechanism in an embodiment of the present invention.
[0044] In some embodiments, the reaction vessel provided by the present invention further includes an isolation chemical chamber mechanism disposed inside the vessel body 4. The isolation chemical chamber mechanism mainly includes: a chemical chamber mounting frame 30, multiple isolation chemical chambers 21, a drive assembly, a feeding execution device, and a controller 14; wherein, the chemical chamber mounting frame 30 is rotatably mounted on the upper part of the inner cavity of the vessel body 4; multiple isolation chemical chambers 21 are independently fixed on the chemical chamber mounting frame 30 along the circumference of the mounting frame, each isolation chemical chamber 21 pre-stores a portion of solid catalyst and / or additive 7, and has an openable and closable discharge port at its front end and a tail end with... An actuator 22 with a conductive magnetic contact 23 is included; a drive assembly is connected to the medicine chamber mounting frame 30 to drive its overall rotation; the feeding actuator is specifically an electromagnetic actuator 24, which is fixedly installed on the inner wall of the vessel body 4, and its installation position is relative to the rotating medicine chamber mounting frame 30, so that the electromagnetic actuator head contact 12 can be aligned with the conductive magnetic contact 23 at the tail of the isolated medicine chamber that has rotated to a specific feeding position; the controller 14 is connected to the drive assembly and the electromagnetic actuator 24 respectively through a communication line to receive signals and coordinate the timing of their actions.
[0045] The reactor operation process provided by this invention is as follows: After the reaction begins, the controller 14 instructs the drive assembly to operate, driving the drug chamber mounting frame 30 and the isolation drug chamber 21 on it to rotate. When one of the isolation drug chambers 21 rotates to the feeding position aligned with the fixed electromagnetic push rod 24, the controller 14 detects whether the alignment signal is normal to determine whether the isolation drug chamber 21 and the electromagnetic push rod 24 are aligned. When the isolation drug chamber 21 and the electromagnetic push rod 24 are properly aligned, the head contact 12 of the electromagnetic push rod 24 attracts the conductive magnetic contact 23 at the tail of the isolation drug chamber 21 and generates a trigger signal. After receiving the signal, the controller 14 immediately controls the drive assembly to pause and simultaneously triggers the movement of the electromagnetic push rod 24. Specifically, the push rod of the electromagnetic push rod 24 extends linearly, pushing the execution push rod 22 of the isolation drug chamber 21, thereby opening the discharge port of the isolation drug chamber 21 and adding the pre-stored solid catalyst and / or auxiliary agent 7 into the reaction system. After a single feeding is completed, the electromagnetic push rod 24 resets, and the controller 14 restarts the drive assembly, causing the reagent chamber mounting frame 30 to continue rotating until the next isolation reagent chamber 21 reaches the feeding station, repeating the above process. The isolation reagent chamber mechanism is constructed to withstand temperatures of no less than 100°C and pressures of no less than 5 MPa, and is isolated from the liquid reaction system inside the reactor body 4. This isolation reagent chamber mechanism makes it possible to precisely add catalysts and / or additives 7 on demand and in batches without interrupting the reaction process or disrupting the oxygen-free sealed environment inside the reactor. This fundamentally solves the problems of solid catalysts easily agglomerating, insufficiently dissolving, encapsulating active sites, and easily "poisoned" and deactivated in traditional one-time feeding methods. By dynamically replenishing to maintain the high activity of the catalytic system, the effective reaction time is significantly extended, and the total utilization rate of the catalyst and the yield efficiency of a single reaction are improved. At the same time, fully automatic intelligent control improves the accuracy of the process and operational safety, providing key equipment guarantees for achieving stable and continuous large-scale production.
[0046] See Figure 2In one specific embodiment, the isolation drug chamber mechanism is integrally installed on the top of the reactor. The driving assembly includes a drive motor 25, a drive wheel 26, and a driven wheel 27. The drive motor 25 is fixedly installed, and the central axis of the driven wheel 27 is integrally fixed to the drug chamber mounting frame 30. When the drive motor 25 is turned on, it drives the drive wheel 26 to rotate clockwise. The drive wheel 26 and the driven wheel 27 transmit power through gear engagement, and the driven wheel 27 moves counterclockwise under the drive of the drive wheel 26. When the driven wheel 27 moves counterclockwise, the drug chamber mounting frame 30 moves counterclockwise synchronously, causing the isolation drug chambers 21 to rotate counterclockwise. In this specific embodiment, the reactor is provided with six isolation drug chambers 21, each of which is independent and does not interfere with each other. When the medicine chamber mounting bracket 30 moves counterclockwise with the isolation medicine chamber 21, the medicine dispensing port at the front end of the isolation medicine chamber 21 is closed (the induction signal control line of the front door of the isolation medicine chamber is in the conductive state 13). When the isolation medicine chamber 21 rotates to a position opposite to the electromagnetic push rod 24 (a specific work position), the actuating push rod 22 at the rear of the isolation medicine chamber 21 aligns with the front end of the electromagnetic push rod 24. The controller 14 detects the alignment signal detection point 16 to determine whether the conductive magnetic contact 23 on the actuating push rod 22 is aligned with the metal head contact 12 of the electromagnetic push rod. Specifically, as shown... Figure 2As shown, the alignment signal detection point 16 includes points A and B, which are detection points for the signal status of the isolation drug chamber located inside the controller 14. Point B continuously emits a high-level signal. When the controller 14 detects the high-level signal emitted by point B from point A, it identifies the alignment state. At this time, the drug-throwing port at the front end of the isolation drug chamber 21 is still in the closed state, and the metal head contact 12 of the electromagnetic push rod is attracted to the conductive magnetic contact 23. The high-level signal emitted by point B is connected through the isolation drug chamber control line 19, and the high-level signal will return to point A and be detected by the controller 14, indicating that the isolation drug chamber 21 and the feeding execution device (electromagnetic push rod 24) are in place and the drug-throwing action can be performed. At this time, the electromagnetic push rod and the isolation drug chamber are in the connected state 11, and points A and B in the controller 14 are connected. After detecting a normal alignment signal, the controller 14 immediately stops the drive motor 25 and closes the control relay 15 that supplies power to the electromagnetic push rod 24 (the electromagnetic push rod power supply line 17 is energized). After the electromagnetic push rod 24 is energized, it moves forward in a straight line, pushing the actuator push rod 22 at the rear of the isolation chamber to push the pre-stored catalyst (and / or auxiliary agent) inside the isolation chamber 21 into the reactor to complete the catalytic discharge. At this time, the catalytic discharge port at the front of the isolation chamber is opened by the actuator push rod 22 (the control line of the isolation chamber front door sensor signal is in the disconnected state 18). Points A and B in the controller 14 are disconnected. The controller 14 does not detect the high-level signal emitted by point B, and then disconnects the control relay 15 that supplies power to the electromagnetic push rod (the electromagnetic push rod power supply line 17 is de-energized). The electromagnetic push rod 22 is de-energized and returns to its original position. After the electromagnetic push rod 22 returns to its original position, the controller 14 restarts the drive motor 25, and the driven wheel 27 drives the medicine chamber mounting frame 30 to rotate counterclockwise until the next isolation medicine chamber 21 reaches the metal head contact 12 of the electromagnetic push rod and is attracted to the conductive magnetic contact 23. The controller 14 receives the conduction signal and repeats the medicine throwing action.
[0047] Figure 3 This is an exploded view of the structure of an isolation medicine compartment in an embodiment of the present invention.
[0048] See Figure 3 In some embodiments, the isolation drug chamber 21 mainly includes a chamber body, a drug-dispensing actuator 22 located at the rear of the chamber, a conductive magnetic contact 23 disposed at the rear of the actuator, an openable and closable front door 20 located at the front of the chamber, a status sensor for sensing the status of the door, an isolation drug chamber control line 19 connected to external control logic, and a fixing hole 31 connected to the drug chamber mounting bracket 30. Multiple identical isolation drug chambers 21 can be independently mounted on the drug chamber mounting bracket 30 through the fixing hole so that they can be pre-positioned on top of the reactor together with the drug chamber mounting bracket 30.
[0049] The operating logic of the isolation chamber 21 is as follows: After pre-loading with solid or liquid catalysts and / or additives, the front door 20 of the isolation chamber is closed. When the reaction progresses to the point where solid or liquid catalysts and / or additives need to be replenished, the controller 14 is activated, and the chamber mounting frame 30 rotates under the drive assembly, causing one isolation chamber 21 to move to the feeding station. At this time, the head contact 12 of the fixed electromagnetic push rod 24 aligns, attracts, and contacts the conductive magnetic contact 23 at the tail of the isolation chamber 21, generating a trigger signal. The controller 14 then pauses the drive assembly and triggers the movement of the electromagnetic push rod 24. The push rod of the electromagnetic push rod 24 extends, pushing the discharge actuator push rod 22 of the isolation chamber 21 forward in a straight line, thereby pushing the material inside the chamber into the reaction system and simultaneously opening the front door. The change in the state of the chamber door is detected by the state sensor and fed back to the controller 14. The controller 14 disconnects the control relay 15 that supplies power to the electromagnetic push rod, and the electromagnetic push rod 24 is de-energized and reset. At this time, the drive assembly resumes operation and drives the drug chamber mounting frame 30 to rotate until the next isolation drug chamber 21 to be added arrives at the feeding station. The feeding mechanism composed of isolation drug chambers 21 supports automatic feeding at preset time intervals by the controller 14, and can also receive manual commands to trigger single feeding. As an independent, pressure-resistant sealed unit, the isolation drug chamber 21 is pre-installed in isolation from the reaction system. Combined with its trigger-type mechanical opening design, it ensures that solid or liquid catalysts and / or additives can be added in stages, at fixed points, and in fixed quantities without interrupting the reaction or disrupting the oxygen-free and high-pressure environment inside the reactor. Through the physical mechanism of "pre-stored isolation - on-demand opening and closing", the problems of particle agglomeration, uneven dissolution, encapsulation deactivation, and easy poisoning during activation caused by the one-time addition of solid or liquid catalysts to the reactor are completely avoided, providing a material basis for maintaining the high activity of the catalytic system. The entire feeding process is automatically managed by controller 14 based on signals, ensuring precision and reliability. The status sensor provides closed-loop feedback, guaranteeing the determinism of action execution. This significantly reduces the uncertainty, safety risks, and potential pollution associated with manual operation, making it a key component in achieving continuous, stable, and intelligent production.
[0050] This invention also provides a method for operating a reactor for a distributed catalytic synthesis reaction, for use in the reactor described above for a distributed catalytic synthesis reaction. The method includes the following steps: before the start of the catalytic synthesis reaction, a solid or liquid catalyst and / or auxiliaries are pre-stored in one or more isolation tanks 21; during the catalytic synthesis reaction, when it is necessary to add solid or liquid catalysts and / or auxiliaries, based on a preset reaction sequence (reaction time), the process is carried out by manual or automatic control, sequentially rotating one of the isolation tanks 21 containing materials to a fixed feeding station; at the feeding station, the front door 20 of the isolation tank is opened to add the pre-stored solid or liquid catalysts and / or auxiliaries into the liquid reaction system of the reactor body 4, thereby achieving batch-wise addition of solid or liquid catalysts and / or auxiliaries.
[0051] This invention also provides a method for a distributed catalytic synthesis reaction, which is carried out using the aforementioned reaction vessel. First, a selected solvent, an initial solid or liquid catalyst, and / or auxiliaries for initiating the reaction are added to the vessel body 4, and an oxygen-free reaction environment is established after nitrogen purging and other operations. Subsequently, the stirring mechanism is activated, and gaseous raw materials (such as trifluoroethylene, hexafluoropropylene, trifluoromethyl trifluorovinyl ether, etc.) are continuously introduced through an intervening pressure-bearing gas-conducting structure to initiate the reaction. During the continuous reaction, the controller 14 controls the isolation chamber mechanism according to a preset program, precisely adding supplementary solid or liquid catalysts and / or auxiliaries pre-stored in different isolation chambers 21 to the liquid reaction system in batches. In this embodiment, the number of batches can be 4 to 6, with each batch accounting for 20%-50% of the total batch mass, the second to penultimate batches each accounting for 10%-20%, and the final batch accounting for 0%-10%.
[0052] In some embodiments, the specific material system involved in the distributed catalytic synthesis reaction method may include: a solvent being one or more of the following solvents: acetonitrile, dimethyl sulfoxide, dimethylformamide, dimethylacetamide, ethylene glycol dimethyl ether, and tetrahydrofuran; a solid or liquid catalyst being one or more of the following catalysts: tetramethylammonium fluoride, tetraethylammonium fluoride, tetrabutylammonium fluoride, potassium cyanate, potassium thiocyanate, potassium fluoride, potassium hydrofluoride, cesium hydrofluoride, cesium fluoride, and potassium hydroxide; and a solid additive being one or more of the following solid additives: crown ether, tetramethylethylenediamine, and polyethylene glycol, wherein the total concentration of the solid catalyst and / or additive 7 in the reaction system is controlled at 0.1-2 mol / L, and the reaction is carried out at a temperature of 30-100°C and an internal pressure of 0.1-5 MPa. By employing a strategy of "initial feed to establish activity - distributed dynamic replenishment," the reaction system is ensured to start up rapidly. Simultaneously, the isolated reagent chamber mechanism enables continuous and precise replenishment of the catalytic active centers without interrupting the reaction or disrupting the oxygen-free, high-pressure sealed environment. This effectively overcomes the problems of catalyst aggregation, encapsulation deactivation, and rapid activity decay caused by traditional one-time feed. A clearly defined material system (such as specific short-chain fluorinated monomers and the catalytic system), stepwise addition ratios, and a mild yet effective temperature and pressure window collectively ensure high conversion rates, high selectivity, and high operational stability. The distributed feed mode improves the utilization efficiency of valuable catalysts and reduces unit consumption. Simultaneously, under mild conditions, efficient interventional gas-conducting structures achieve sufficient mass transfer, reducing reliance on extreme stirring, high temperatures, and high pressures. This reduces equipment burden, energy consumption, and safety risks, providing a complete process solution for continuous, stable, and low-cost large-scale production.
[0053] In one specific embodiment, a reactor equipped with five intelligently controlled isolation chambers 21 was used for the synthesis of hydrofluoroether. First, 50 mL of a 0.05 mol / L potassium hydroxide dimethylformamide solution was added to the reactor body 4 of the high-pressure reactor, along with an equal volume of trifluoroethanol liquid. The stirring mechanism was activated, and stirring was performed at 500 rpm. Simultaneously, the reactor body 4 was pressurized to 0.5 MPa with nitrogen gas and purged three times to establish an oxygen-free nitrogen atmosphere. Subsequently, the system was heated to 75°C under continuous stirring. The reactant gas trifluoroethylene was continuously introduced through an intervening pressure-bearing gas-conducting structure (the gas-conducting pipe section 3 has a spiral coil 8 and a gas-conducting hole 9 at its end) for 5 hours, during which the temperature fluctuation was controlled to not exceed ±10°C, and the system pressure was adjusted to 0.3 MPa. After the reaction is complete, without pausing or cooling, the unreacted trifluoroethylene gas is directly recovered, then discharged and distilled to obtain a mixture of the target hydrofluoroethers CF3CH2OCF2CH2F and CF3CH2OCHFCHF2. Subsequently, without opening the reactor body 4, without disrupting the internal oxygen-free environment, and without requiring complete cessation of the reaction, the isolation chamber mechanism is triggered by the pre-programmed controller 14. This isolation chamber mechanism operates automatically at fixed intervals (e.g., 24 hours): the chamber mounting frame 30 rotates under the drive assembly, causing one isolation chamber 21 to move to the feeding position. The electromagnetic push rod 24 then actuates, pushing the isolation chamber's execution push rod 22 to add pre-stored 0.01 mol / L potassium hydroxide dimethylformamide solution and an equal amount of trifluoroethanol as supplementary materials to the reaction system. The system immediately continues to react after addition, and this "replenishment-reaction" cycle is repeated 5 times, ultimately achieving a cumulative yield of 80% for the final product. By using an isolated reaction chamber mechanism, precise and automated replenishment of catalyst and reactants in multiple batches was achieved without interrupting the reaction process or disrupting the sealed, oxygen-free environment. This demonstrates the system's ability to maintain and refresh catalytic activity within a single operating cycle, thereby significantly extending the effective reaction time. Under mild conditions (75°C, 0.3 MPa), efficient mass transfer of gas-phase feedstock was ensured through an intervening gas-conducting structure, and combined with a distributed catalyst replenishment strategy, a product yield of up to 80% was ultimately achieved. This verifies the significant advantages of the implementation method of this invention in solving key problems such as catalyst deactivation and interfacial mass transfer limitations. The entire process, from the initial reaction to multiple distributed feeds, was automatically controlled, and the operation was stable and reliable. This provides strong experimental evidence for achieving high-efficiency, low-cost continuous large-scale synthesis without the need for traditional batch-to-batch reactor opening, cleaning, and refeeding.
[0054] In one specific embodiment, a reactor equipped with three intelligently controlled isolation chambers 21 is used for the synthesis of fluoroolefins. First, 50 mL of a 0.02 mol / L tetrabutylammonium difluoride hydrofluoric acid acetonitrile solution is added to the reactor body 4 of the high-pressure reactor. The stirring mechanism is started and stirred at 500 rpm, while the reactor body 4 is pressurized to 0.5 MPa and purged three times with nitrogen to establish an oxygen-free nitrogen atmosphere. Subsequently, under continuous stirring, the system is heated to 50°C and the reaction gas trifluoromethyl trifluorovinyl ether is continuously introduced through an intervening pressure-bearing gas-conducting structure (the gas-conducting pipe section 3 has a spiral coil 8 and a gas-conducting hole 9 at its end) for 2 hours, during which the temperature fluctuation is controlled to not exceed ±10°C, and the system pressure is adjusted to 0.3 MPa. After the reaction is completed, there is no need to cool the system to room temperature or pause the process; the unreacted gas is directly recovered, then discharged and distilled to obtain the target fluoroolefin CF3OCF=CFCF(OCF3)CF3. Subsequently, without opening the reactor body 4, disrupting the internal oxygen-free environment, and without interrupting the reaction, the isolation catalyst chamber mechanism is triggered by the pre-programmed controller 14. This mechanism operates automatically at fixed intervals (e.g., 24 hours): the catalyst chamber mounting bracket 30 rotates under the drive assembly, moving one isolation catalyst chamber 21 to the feeding position. The electromagnetic push rod 24 then actuates, pushing the actuator push rod 22 of the chamber to add a pre-stored 0.01 mol / L tetra-n-butyldifluoride hydrofluoric acid acetonitrile solution as a supplementary catalyst to the reaction system. The system immediately resumes the reaction after addition, and this "replenishment-reaction" cycle is repeated three times, ultimately achieving a cumulative yield of 89%. Through the isolation catalyst chamber mechanism, multiple precise and automatic replenishments of the homogeneous catalyst are successfully achieved without interrupting the reaction or disrupting the oxygen-free environment. This demonstrates that this strategy is applicable not only to solid catalysts but also to liquid or dissolved catalytic systems requiring replenishment, showcasing the method's versatility. Under mild conditions of 50℃ and 0.3MPa, the efficient dissolution and mixing of gaseous monomers were ensured through an intervening gas-conducting structure. Combined with distributed catalyst replenishment, a final yield of up to 89% was achieved in just 2 hours of main reaction and several additions. This highlights the significant advantages of this invention in improving reaction efficiency, feed conversion rate, and product yield. The entire process achieves a fully automated "reaction-feeding" cycle, with stable operation and good repeatability. While achieving high yield, the precise distributed feeding reduces the total amount of catalyst added and waste, verifying the comprehensive value of this integrated system in improving the economy, safety, and scalability of the synthesis process.
[0055] In one specific embodiment, a reactor equipped with five intelligently controlled isolation chambers 21 was used for the oligomerization reaction of hexafluoropropylene. First, 50 ml of a 0.5 mol / L saturated potassium cyanide acetonitrile solution was added to the reactor body 4 of the high-pressure reactor. The stirring mechanism was started and stirred at 500 rpm, while the reactor body 4 was pressurized to 0.5 MPa and purged three times with nitrogen to establish an oxygen-free nitrogen atmosphere. Subsequently, the system was heated to 50°C under continuous stirring, and the reaction gas hexafluoropropylene was continuously introduced through an intervening pressure-bearing gas-conducting structure (the gas-conducting pipe section 3 has a spiral coil 8 and a gas-conducting hole 9 at its end) for 6 hours, during which the temperature fluctuation was controlled to not exceed ±10°C, and the system pressure was adjusted to 0.1 MPa. After the reaction was completed, there was no need to cool the system to room temperature; the unreacted hexafluoropropylene gas was directly recovered, then discharged and distilled to obtain the target product, hexafluoropropylene oligomer. Subsequently, without opening the reactor body 4 or interrupting the reaction process, the isolation chamber mechanism is triggered by the pre-programmed controller 14. This mechanism operates automatically at fixed intervals (e.g., 24 hours): the chamber mounting frame 30 rotates under the drive assembly, causing an isolation chamber 21 to move to the feeding position. The electromagnetic push rod 24 then actuates, pushing the execution push rod 22 of the chamber to add the pre-stored 0.1 mol / L potassium cyanide solution as a supplementary catalyst into the reaction system. After addition, the system continues to react. This "supplementation-reaction" cycle is repeated 5 times, ultimately achieving a cumulative yield of 92%. This embodiment demonstrates that the "initial activation + dynamic feeding" mechanism provided by this invention is not only applicable to addition reactions but also efficiently controls the polymerization process. During the monomer introduction over a period of up to 6 hours and subsequent multiple feedings, the system activity was maintained continuously, ultimately achieving a yield as high as 92%, verifying the powerful ability of this method to achieve deep conversion and high output. Even at a relatively low pressure of 0.1 MPa, the hexafluoropropylene monomer is directly dispersed in the liquid phase through an intervening pressure-bearing gas-conducting structure. Combined with continuous stirring, this ensures a sufficient supply and uniform reaction of the monomer around the active centers of the growing chains. This is crucial for obtaining oligomers with controllable molecular weight distribution and high yield. This embodiment further verifies the reliability of the fully automated distributed feeding process. Maintaining high activity over a long period by precisely adding small amounts of catalyst several times significantly reduces catalyst consumption per unit product. It also avoids the problems of difficult molecular weight control and short reaction cycles caused by one-time catalyst deactivation in traditional polymerization processes, providing an innovative process model for efficient and controllable continuous polymerization production.
[0056] It should be understood that the term "and / or" in this article is merely a description of the relationship between related objects. For example, A and / or B indicates that there can be three relationships: A alone, A and B simultaneously, and B alone. Another example is A and / or B and / or C, which indicates that there can be eight relationships: A alone, B alone, C alone, A and B simultaneously, A and C simultaneously, B and C simultaneously, A, B, and C simultaneously, and A, B, and C simultaneously not existing. Furthermore, the character " / " in this article indicates that the preceding and following related objects have an "or" relationship.
[0057] In the embodiments of this application, "multiple" refers to two or more items, "multiple" refers to two or more items, and "multiple types" refers to two or more items.
[0058] It should be understood that the specific embodiments described above are merely illustrative or explanatory of the principles of the invention and do not constitute a limitation thereof. Therefore, any modifications, equivalent substitutions, improvements, etc., made without departing from the spirit and scope of the invention should be included within the protection scope of the invention. Furthermore, the appended claims are intended to cover all variations and modifications falling within the scope and boundaries of the appended claims, or equivalent forms of such scope and boundaries.
Claims
1. A reaction vessel for catalytic synthesis reactions, characterized in that, include: The vessel body (4); The stirring mechanism includes a driving device (2) and a stirring paddle (5) disposed in the vessel body (4), wherein the driving device (2) is used to drive the stirring paddle (5). The intervening pressure-bearing gas-conducting structure includes a gas-conducting pipe section (3), which extends into the vessel body (4) and its end is located in the mixing area acted by the blade of the stirring paddle (5). Multiple gas-conducting holes (9) are provided on the pipe wall of the gas-conducting pipe section for directly introducing the pressurized gaseous raw materials into the liquid reaction system.
2. The reaction vessel according to claim 1, wherein, The end of the air guide pipe section (3) is a spiral coil (8), which is coaxially sleeved on the rotating shaft of the stirring paddle (5) and does not rotate with it.
3. The reaction vessel according to claim 1 or 2, wherein, A valve (1) is provided at the upper end of the air duct section (3).
4. The reaction vessel according to claim 2 or 3, wherein, The spiral coil (8) extends below the liquid surface to a depth of not less than two-thirds of the liquid level.
5. The reaction vessel according to any one of claims 1 to 4, wherein, It also includes a dispersing head (10), which is disposed adjacent to or coaxially connected to the blades of the stirring paddle (5) for shearing and dispersing the bubbles discharged from the air guide hole (9).
6. A reaction vessel for distributed catalytic synthesis, characterized in that, include: The vessel body (4); The stirring mechanism includes a driving device (2) and a stirring paddle (5) disposed in the vessel body (4), wherein the driving device (2) is used to drive the stirring paddle (5). An isolation chamber mechanism is installed inside the vessel body (4) for dynamically and isolatedly adding pre-stored solid or liquid catalysts and / or additives to the reaction system in batches during the reaction process.
7. The reaction vessel according to claim 6, wherein, The isolation medicine chamber mechanism includes: The medicine compartment mounting bracket (30) is rotatably mounted inside the vessel body (4); At least one isolation chamber (21) is fixed on the chamber mounting frame (30) for pre-storing solid or liquid catalysts and / or auxiliaries, and the isolation chamber (21) has an openable and closable dispensing port; A drive assembly for driving the rotation of the medicine compartment mounting bracket (30); The feeding execution device is fixedly installed inside the vessel body (4) and opposite to the drug chamber mounting frame (30). It is used to open the drug discharge port to feed the solid or liquid catalyst and / or additive into the vessel body (4) when the isolation drug chamber (21) is rotated to the feeding position aligned with the feeding execution device.
8. The reaction vessel according to claim 7, wherein, The isolation medicine chamber mechanism includes multiple independent isolation medicine chambers (21) arranged circumferentially along the medicine chamber mounting frame (30).
9. The reaction vessel according to claim 7 or 8, wherein, The feeding device is an electromagnetic push rod (24), and the tail of the isolation drug chamber (21) is provided with an execution push rod (22). The execution push rod (22) is provided with a conductive magnetic contact (23). When the isolation drug chamber (21) rotates to the feeding station, the electromagnetic push rod head contact (12) interacts with the conductive magnetic contact (23) to trigger the execution push rod (22).
10. The reaction vessel according to claim 9, wherein, It also includes a controller (14), which is communicatively connected to the drive assembly and the electromagnetic push rod (24); The electromagnetic push rod head contact (12) and the conductive magnetic contact (23) generate a trigger signal based on the aforementioned action. The controller (14) is used to control the drive assembly to pause and trigger the actuator push rod (22) to perform the feeding action when the trigger signal is received.
11. The reaction vessel according to any one of claims 6 to 10, wherein, The isolation chamber mechanism is designed to withstand a temperature of not less than 100°C and a pressure of not less than 5 MPa, and is isolated from the liquid reaction system inside the vessel (4).
12. A method for operating a reactor for a distributed catalytic synthesis reaction, characterized in that, The reactor used in any one of claims 6 to 11 comprises the following steps: Before the catalytic synthesis reaction begins, solid or liquid catalysts and / or auxiliaries are pre-stored in one or more isolated drug chambers (21); During the catalytic synthesis reaction, when it is necessary to add solid or liquid catalysts and / or additives, one of the pre-stored isolation tanks (21) is rotated to the fixed feeding station in sequence; At the feeding station, the front door (20) of the isolation drug chamber is opened to add the pre-stored solid or liquid catalyst and / or additives into the liquid reaction system of the reactor body (4).
13. The method according to claim 12, wherein, The process of rotating one of the pre-stored material isolation chambers (21) to a fixed feeding station is specifically based on a preset reaction sequence and is carried out through manual or automatic control, thereby feeding the solid or liquid catalyst and / or additives in batches.
14. A method for a distributed catalytic synthesis reaction, characterized in that, Using the reactor as described in any one of claims 6-11, and comprising the following steps: Solvent, initial solid or liquid catalyst and / or auxiliaries for starting the reaction are added into the vessel (4) to establish an oxygen-free reaction environment; Start the stirring mechanism and continuously introduce gaseous raw materials to initiate the reaction; During the reaction, supplementary solid or liquid catalysts and / or auxiliaries pre-stored in different isolation drug chambers (21) are added to the liquid reaction system in batches.
15. The method according to claim 14, wherein, The solid or liquid catalyst and / or additives are added in batches 4 to 6 times, and the mass of each batch relative to the total mass of the batches meets the following conditions: The initial investment ratio is 20% to 50%; In the second to penultimate rounds of investment, the investment ratio for each round ranged from 10% to 20%. The final investment percentage is between 0% and 10%.
16. The method according to claim 11, wherein, The distributed catalytic synthesis reaction is a synthesis reaction of short-chain fluorinated organic compounds.
17. The method according to claim 16, wherein, The synthesis reactions of the short-chain fluorinated organic compounds include the addition reaction of hexafluoropropylene with ethanol or trifluoroethanol, the polymerization reaction of hexafluoropropylene, and the polymerization reaction of trifluoromethyl trifluorovinyl ether.
18. The method according to claim 14, wherein, The gaseous feedstock includes one or more of trifluoroethylene, trifluoromethyltrifluorovinyl ether, and hexafluoropropylene; the solvent includes one or more of acetonitrile, dimethyl sulfoxide, dimethylformamide, dimethylacetamide, ethylene glycol dimethyl ether, and tetrahydrofuran; the solid or liquid catalyst includes one or more of tetramethylammonium fluoride, tetraethylammonium fluoride, tetrabutylammonium fluoride, potassium cyanate, potassium thiocyanate, potassium fluoride, potassium hydrofluoride, cesium hydrofluoride, cesium fluoride, and potassium hydroxide; and the solid additive includes one or more of crown ether, tetramethylethylenediamine, and polyethylene glycol.
19. The method according to claim 18, wherein, The total concentration of the solid or liquid catalyst and / or auxiliaries in the liquid reaction system is 0.1-2 mol / L.
20. The method of claim 14, wherein, During the distributed catalytic synthesis reaction, the reaction temperature is 30-100℃ and the reaction pressure inside the vessel (4) is 0.1-5MPa.