Grignard reagent continuous synthesis device and system
By combining a tubular reactor with a propeller-type stirring rod, the problems of insufficient heat transfer and severe backmixing in the synthesis of Grignard reagents were solved, achieving efficient and safe production of Grignard reagents and improving product quality and safety.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-28
- Publication Date
- 2026-03-31
AI Technical Summary
Existing Grignard reagent synthesis equipment suffers from problems such as insufficient heat transfer capacity, slow reaction rate, severe material backmixing, numerous side reactions, and unstable product quality, making it difficult to achieve low-cost, high-safety, and high-purity industrial production.
The design employs a tubular reactor combined with a propeller-type stirring rod and a segmented temperature control jacket to achieve continuous and efficient mixing of raw materials and metallic magnesium, reduce backmixing, increase radial mixing, improve heat transfer efficiency, and ensure safety through an emergency vent.
Shorten reaction time, improve the quality of Grignard reagent products, reduce energy consumption, enhance safety, avoid equipment damage, and achieve efficient and safe production of Grignard reagents.
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Figure CN224057360U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the field of chemical equipment technology, and in particular to a continuous synthesis apparatus and system for Grignard reagents. Background Technology
[0002] Grignard reagents serve as a crucial bridge in organic synthesis, enabling carbon chain elongation through Grignard reactions. They have wide applications in pharmaceuticals, fine chemicals, and materials science. They can be prepared by reacting inexpensive halogens with magnesium scrap or granules, thus finding extensive use in chemical research and development as well as industrial production. During Grignard reagent reactions, the initial reaction is highly exothermic, necessitating careful control of the feeding rate and reaction temperature.
[0003] Traditional Grignard reagent synthesis typically employs a batch reactor, which is a continuously stirred-tank reactor. This reactor presents several problems: different halogenated hydrocarbon feedstocks have varying initiation rates. Some halogenated hydrocarbon feedstocks have slow initiation rates, making it easy to add excessive amounts of material in the early stages. Once the reaction begins, the exothermic reaction is intense, leading to feed surge. To maintain a constant reaction temperature, the material is added slowly dropwise, resulting in a long overall reaction time. Under the conditions of continuous stirring and prolonged operation, Wood's coupling side reactions are highly likely to occur, generating excessive impurities. Furthermore, batch-to-batch product quality varies significantly.
[0004] To address the problems of batch reactors, several improvements are needed: 1. Enhance the heat transfer capacity of the equipment to precisely control the material temperature; 2. Accelerate the reaction rate, making the equipment closer to a plug flow reactor to minimize backmixing and reduce the generation of byproducts; 3. Strengthen radial mixing of materials.
[0005] Fixed-bed continuous processes are one effective solution. A fixed bed is formed by filling a tubular reactor with magnesium shavings or granules. A halogenated reagent is continuously introduced into the reactor, and the reaction between the halogenated reagent and the magnesium shavings or granules continuously synthesizes Grignard reagents. Existing technology, such as patent CN202020547061.0, discloses a design for an oscillating fixed-bed reactor. The oscillation source is fixed at the bottom of the reactor, and intermittent oscillation promotes axial and longitudinal mixing of materials, enhancing mass transfer. However, longitudinal backmixing may lead to the generated halogenated Grignard reagent mixing with the raw materials, producing relatively more impurities; and continuous or intermittent oscillation may cause pipe connections to loosen, resulting in leaks and safety issues; furthermore, continuous oscillation may lead to solid buildup and bridging blockages, affecting reactor efficiency and continuous operation. The German company IMM has also developed a fixed-bed reactor for this reaction (Organic Process Research & Development, 2020, 2, 315-321). The difference lies in the fact that, in addition to the electric motor compacting the added magnesium shavings at the bottom of the reaction equipment, a pulse pump is also used for feeding, providing continuous pulses to the material. The combination of these two methods can reduce backmixing of the material and lower the probability of side reactions. However, as the diameter of this type of reactor increases, the radial mixing of the material deteriorates, and the radial residence time distribution becomes more pronounced.
[0006] Therefore, the equipment for industrial preparation of Grignard reagents still needs further improvement to address issues such as increasing heat exchange efficiency, reducing radial backmixing, and increasing radial mixing, in order to meet the requirements of low-cost, high-safety, and high-purity Grignard reagent preparation for industrial production. Utility Model Content
[0007] The purpose of this invention is to overcome the defects of the prior art by providing a continuous synthesis device and system for Grignard reagents, which reduces backmixing of materials, increases radial mixing between materials, and improves the quality of Grignard reagent products.
[0008] The objective of this utility model can be achieved through the following technical solutions:
[0009] A continuous synthesis apparatus for Grignard reagents includes a tubular reactor body and a stirrer. The reactor body has a liquid inlet and an outlet at its lower and upper ends, respectively. The top of the reactor body is connected to a magnesium powder feeding unit via a magnesium powder inlet. The reactor body is equipped with a jacket for heating and cooling the reactants. The stirrer includes a motor and a support rod connected to the motor output. The motor is located at the top of the reactor body. The support rod extends downward from the top inside the reactor body. A mixing component is provided on the support rod. The mixing component includes a propeller-type stirring rod with holes distributed on it.
[0010] Furthermore, the jacket is provided with multiple longitudinally arranged components, each individually receiving a temperature-controlled medium.
[0011] Furthermore, the reactor body includes a first reaction section, a second reaction section, and a discharge section connected sequentially from bottom to top, and the temperature of the outer jacket of the second reaction section is higher than the temperature of the outer jacket of the second reaction section.
[0012] Furthermore, the reactor body includes multiple reaction sections and a discharge section connected sequentially from bottom to top, and thermometers are installed at the beginning of the first reaction section, between each reaction section, and at the outlet of the discharge section.
[0013] Furthermore, the magnesium powder feeding unit includes a magnesium powder silo, a magnesium powder conveying device, and a feeding funnel connected in sequence. The magnesium powder silo is equipped with an inert gas purging pipeline, and the feeding funnel is connected to the magnesium powder inlet through a valve.
[0014] Furthermore, a viewing window is provided on the upper part of the reactor body.
[0015] Furthermore, an emergency vent is provided at the top of the reactor body.
[0016] Furthermore, the magnesium powder inlet and outlet of the reactor body are each equipped with a filter screen.
[0017] A Grignard reagent continuous synthesis system includes a feed solution supply subsystem, a feed solution receiving subsystem, and a temperature control subsystem, and also includes the Grignard reagent continuous synthesis apparatus as described above. The feed solution supply subsystem is connected to the liquid inlet of the Grignard reagent continuous synthesis apparatus, the feed solution receiving subsystem is connected to the outlet of the Grignard reagent continuous synthesis apparatus, and the temperature control subsystem is connected to the jacket of the Grignard reagent continuous synthesis apparatus.
[0018] Furthermore, the liquid supply subsystem includes a raw material conveying unit, a solvent cleaning unit, and a raw material initiation unit.
[0019] Furthermore, the liquid receiving subsystem includes a Grignard reagent receiving tank and a waste liquid tank, both of which are connected to the discharge port. Both the Grignard reagent receiving tank and the waste liquid tank are provided with a gas outlet connected to the tail gas absorption unit.
[0020] Furthermore, the temperature control subsystem is equipped with temperature measuring points on both the inlet and outlet pipes connected to the jacket.
[0021] Compared with the prior art, the present invention has the following beneficial effects:
[0022] 1. This device can achieve continuous and efficient mixing of raw materials and metallic magnesium, and rapid heat transfer and temperature control, avoiding the problem of unstable pressure caused by cavitation during the use of magnesium powder, greatly shortening the reaction time and obtaining high-purity Grignard reagent; the flow process of materials in the reaction body is close to the plug flow process, reducing backmixing of materials, increasing radial mixing between materials, and improving the quality of Grignard reagent products.
[0023] 2. The mixing component structure of this device promotes the mixing of liquid and solid phases and improves the heat transfer effect with the tube wall. Its design and operation mode avoid the risks of high energy consumption and motor burnout caused by magnesium powder compaction and agitator compaction, greatly improving the safety of operation. On the other hand, the magnesium powder falls through the holes on the stirring rod, avoiding the risk of magnesium powder at the bottom being pushed to the top.
[0024] 3. By using a jacket to ensure that the temperature of the second reaction section is higher than that of the first reaction section, the raw materials can be reacted quickly, reducing the residence time.
[0025] 4. An emergency vent is provided at the top of the tubular reactor body, which can be connected to a safety valve or rupture disc to prevent excessive pressure in the system from causing equipment damage or safety problems. Attached Figure Description
[0026] Figure 1 This is a schematic diagram of the continuous synthesis apparatus for Grignard reagents in the embodiments;
[0027] Figure 2 This is a schematic diagram of the Grignard reagent continuous synthesis system in the example.
[0028] Figure label:
[0029] 1-Upper head; 2-Reactor body; 3-Motor; 4-Magnesium powder inlet; 5-Support rod; 6-Mixing assembly; 7-Liquid inlet; 8-Outlet; 9-First temperature-controlled medium inlet; 10-First temperature-controlled medium outlet; 11-Second temperature-controlled medium inlet; 12-Second temperature-controlled medium outlet; 13-Lower head; 14-Flange; 15-Viewing window; 16-Magnesium powder silo; 17-Magnesium powder conveying device; 18-Feeding funnel; 19-Butterfly valve; 20-First thermometer; 21-Second thermometer; 22-Third thermometer; 23-Emergency relief port; 24-Jacket;
[0030] 100-Continuous synthesis apparatus for Grignard reagents; 200-Feed supply subsystem; 201-Solvent storage tank; 202-First switching valve; 203-First metering pump; 204-Initiator liquid storage tank; 205-Second switching valve; 206-Raw material storage tank; 207-Third switching valve; 208-Second metering pump; 209-Mass flow meter; 300-Feed receiving subsystem; 301-Fourth switching valve; 302-Fifth switching valve; 303-Waste liquid tank; 304-Grignard reagent receiving tank; 400-Temperature control subsystem; 401-First temperature control unit; 402-Second temperature control unit. Detailed Implementation
[0031] The present invention will now be described in detail with reference to the accompanying drawings and specific embodiments. This embodiment is based on the technical solution of the present invention and provides detailed implementation methods and specific operating procedures; however, the scope of protection of the present invention is not limited to the following embodiments.
[0032] like Figure 1 As shown, this application proposes a continuous synthesis apparatus for Grignard reagents, comprising a tubular reactor body 2 and a stirrer. The reactor body 2 has an upper end cap 1 and a lower end cap 13 at its top and bottom, respectively. The reactor body 2 has a liquid inlet 7 and a discharge outlet 8 at its lower and upper ends, respectively. The top of the reactor body 2, specifically the side of the upper end cap 1, is connected to a magnesium powder feeding unit via a magnesium powder inlet 4. The reactor body 2 is externally equipped with a jacket 24 for heating and cooling the reactants.
[0033] The stirrer includes a motor 3 and a support rod 5, with the support rod 5 connected to the output end of the motor 3 via a shaft seal. The motor 3 is mounted on a motor mount at the top of the reactor body 2, and the support rod 5 extends downwards from the top within the reactor body 2. A mixing component 6 is mounted on the support rod 5, comprising an upwardly spiral-shaped propeller-type stirring rod. This propeller-type stirring rod can be a spiral blade or similar structure; in this embodiment, a spiral blade is used. This design promotes the mixing of the liquid and solid phases and prevents magnesium powder compaction. The stirrer makes the flow of materials in the reaction pipe resemble a plug flow process, reducing backmixing, increasing radial mixing between materials, and improving the quality of the Grignard reagent product. During operation, the rotating spiral blades drive the magnesium powder upwards slowly, preventing it from compacting downwards and damaging the motor 3. The spiral blades have holes through which the magnesium powder falls, ensuring that it does not compact downwards or remain continuously at the top, avoiding the risk of lower magnesium powder being pushed upwards and ensuring efficient reaction between the magnesium powder and the raw materials. The aperture size of the holes is maintained between 0.5 mm and 20 mm, preferably between 1 mm and 10 mm, and more preferably between 2 mm and 5 mm. The direction of the support rod 5 is either horizontal to the radial direction or obliquely upward with respect to the reactor body 2, and when obliquely upward, the angle between the support rod and the radial direction is between 0° and 45°. The distance between the mixing component 6 and the inner wall of the tubular reactor body 2 is maintained between 0.1 cm and 1 cm.
[0034] The jacket 24 can be provided in multiple longitudinally arranged, and the temperature control medium can be input in series or individually to achieve series or segmented temperature control.
[0035] In this embodiment, the reactor body 2 includes a first reaction section, a second reaction section, and a discharge section connected sequentially from bottom to top. The two reaction sections are temperature-controlled in separate sections. The corresponding jackets 24 include: a first jacket, located outside the first reaction section, with inlet and outlet for the temperature-controlled medium; and a second jacket, located outside the second reaction section, also with inlet and outlet for the temperature-controlled medium. The outlet 8 for the Grignard reagent product is located in the discharge section. In this embodiment, the temperature of the outer jacket 24 of the second reaction section is set higher than that of the outer jacket 24 of the second reaction section because the initial stage of the material reaction is a stage with a very fast reaction rate and a large amount of heat release. A relatively lower temperature can better control the reaction temperature and reduce side reactions. The slightly higher temperature of the second reaction section compared to the first reaction section ensures rapid reaction of the raw materials and reduces residence time.
[0036] In actual implementation, the reactor body 2 is not limited to two reaction sections; additional reaction sections can be added according to actual conditions. That is, the reactor body 2 includes multiple reaction sections and a discharge section connected sequentially from bottom to top. Thermometers are installed at the beginning of the first reaction section, between each reaction section, and at the outlet of the discharge section. In this embodiment, a first thermometer 20 is installed at the lower part of the first reaction section; a second thermometer 21 is installed between the first and second reaction sections; and a third thermometer 22 is installed at the outlet of the discharge section.
[0037] The magnesium powder feeding unit includes a magnesium powder silo 16, a magnesium powder conveying device 17, and a feeding funnel 18 connected in sequence. The feeding funnel 18 is connected to the magnesium powder inlet 4 via a valve. By opening and closing the valve, magnesium powder can be continuously or intermittently replenished, and the reactor liquid can be prevented from overflowing into the feeding funnel 18. In this embodiment, the valve of the magnesium powder inlet 4 is a butterfly valve 19, but in actual implementation, other valves such as shut-off valves can be used. The magnesium powder silo 16 is equipped with an inert gas purging pipeline. Before the entire system is used, it is purged with inert gas. Magnesium powder is then added to the magnesium powder silo 16 and protected with inert gas. The magnesium powder in the magnesium powder silo 16 is intermittently or continuously fed into the feeding funnel 18 through the magnesium powder conveying device 17. The magnesium powder conveying device 17 can be a star feeder or a solid conveying screw, etc.
[0038] The upper part of the reactor body 2 is provided with a viewing window 15, which is located between the second reaction section and the discharge section. It is used to observe and control the position of magnesium powder and to perform magnesium powder feeding or stopping feeding operations.
[0039] The upper part of the reactor body 2 is provided with an emergency relief port 23, which can be connected to a safety valve or a rupture disc to prevent excessive pressure in the system from causing equipment damage or safety problems.
[0040] The magnesium powder inlet 4 and outlet 8 of the reactor body 2 are each equipped with a filter screen to prevent magnesium powder from clogging the pipe openings.
[0041] The upper end cap 1 is connected to the tubular reactor body 2 by flange connection, welding, or other equivalent methods. In this embodiment, flange 14 is used. The lower end cap 13 is connected to the lower end of the tubular reactor body 2 and sealed by flange or welding. The inner diameter of the reactor body 2 is between 2cm and 50cm, preferably between 4cm and 20cm, and more preferably between 4cm and 10cm.
[0042] like Figure 2 As shown, this application proposes a continuous synthesis system for Grignard reagents, including a feed solution supply subsystem 200, a feed solution receiving subsystem 300, and a temperature control subsystem 400, as well as the continuous synthesis apparatus 100 for Grignard reagents as described above. The feed solution supply subsystem 200 is connected to the liquid inlet 7 of the continuous synthesis apparatus 100 for Grignard reagents, the feed solution receiving subsystem 300 is connected to the outlet 8 of the continuous synthesis apparatus 100 for Grignard reagents, and the temperature control subsystem 400 is connected to the jacket 24 of the continuous synthesis apparatus for Grignard reagents.
[0043] The feed liquid supply subsystem 200 includes a raw material conveying unit, which comprises a raw material liquid storage tank 206, a third switching valve 207, and a second metering pump 208 connected in sequence. The second metering pump 208 is connected to the liquid inlet 7. In this embodiment, the feed liquid supply subsystem 200 also includes a solvent cleaning unit and a raw material initiation unit. The solvent cleaning unit is used to clean the equipment or to fill the system with liquid during equipment operation. For Grignard reactions that are not thermally initiated, a small amount of initiating liquid can be prepared and introduced into the system to initiate the reaction at the start of operation. The solvent cleaning unit comprises a solvent storage tank 201, a first switching valve 202, and a first metering pump 203 connected in sequence. The first metering pump 203 is connected to the liquid inlet 7. The raw material initiation unit includes an initiator liquid storage tank 204, which is connected to the second metering pump 208 via a second switching valve 205. The solvent cleaning unit and the raw material initiation unit can be designed into the entire synthesis system or can be flexibly connected to the system and removed when not in use. A mass flow meter 209 is installed between the metering pump and the liquid inlet 7.
[0044] The liquid receiving subsystem 300 includes a Grignard reagent receiving tank 304 and a waste liquid tank 303, both of which are connected to the discharge port 8. A fourth switching valve 301 and a fifth switching valve 302 are respectively installed at the inlet of the waste liquid tank 303 and the Grignard reagent receiving tank 304. Both the Grignard reagent receiving tank 304 and the waste liquid tank 303 are equipped with gas outlets, which lead to the exhaust gas absorption unit via pipelines.
[0045] The temperature control subsystem 400 can be a combined cooling and heating unit or connected to a factory's common temperature control system. In this embodiment, the temperature control subsystem 400 includes a first temperature control unit 401 and a second temperature control unit 402. The first temperature control unit 401 is connected via pipelines to the first temperature control medium inlet 9 and the first temperature control medium outlet 10 of the corresponding jacket 24 of the first reaction section. The second temperature control unit 402 is connected via pipelines to the second temperature control medium inlet 11 and the second temperature control medium outlet 12 of the corresponding jacket 24 of the second reaction section. Figure 2 The arrow at the jacket 24 indicates the flow direction of the temperature-controlled medium in this embodiment. The temperature control subsystem 400 has temperature measuring points on both the inlet and outlet pipes connected to the jacket 24.
[0046] The workflow of this system is as follows:
[0047] 1. Purge the synthesis system with nitrogen through the liquid inlet 7 until the system is emptied of air and becomes an inert system; then, under nitrogen purging, add magnesium powder to the magnesium powder silo 16; open the butterfly valve 19 to inject magnesium powder into the reactor body 2; when the position of magnesium powder reaches above the viewing window 15, close the butterfly valve 19 to complete the magnesium powder feeding.
[0048] 2. Prepare the bromobenzene feedstock solution and place it in the feedstock solution storage tank 206 for later use. The bromobenzene feedstock solution uses tetrahydrofuran as the solvent and the molar concentration of bromobenzene is 1M.
[0049] 3. Preparation of bromobenzene initiating solution: Place the mixture of bromobenzene, tetrahydrofuran and diisobutylaluminum hydride in the initiator liquid storage tank 204 for later use; the molar concentration of bromobenzene is 1M and the molar concentration of diisobutylaluminum hydride is 0.05M; turn on the first temperature control unit 401 and the second temperature control unit 402, and set the temperature of the temperature control medium entering the jacket 24 of the first reaction section to 20℃ and the temperature of the temperature control medium entering the jacket 24 of the second reaction section to 30℃ respectively.
[0050] 4. Open the first switch valve 202 and start the first metering pump 203 to inject tetrahydrofuran solution to fill the reactor body 2; turn on the motor 3 and open the fourth switch valve 301. The material at the discharge port 8 is collected into the waste liquid tank 303. After running for 10 minutes, turn off the first metering pump 203 and the first switch valve 202.
[0051] 5. Open the second switch valve 205. The bromobenzene initiating solution is injected into the reactor body 2 through the second metering pump 208 and mass flow meter 209. Observe the temperature of the first thermometer 20 at the bottom of the reactor body 2 and the second thermometer 21 in the middle. When the temperature starts to rise, it indicates that the reaction has been initiated.
[0052] 6. Close the second switch valve 205 and open the third switch valve 207 to pump the bromobenzene raw material in the raw material storage tank 206 into the reactor body 2. Set the reaction residence time to 8 min. After the pump runs for 16 min, close the fourth switch valve 301 and open the fifth switch valve 302 to switch the outlet 8 from the waste liquid tank 303 to the Grignard reagent receiving tank 304.
[0053] 7. When the magnesium powder level drops to the lower limit of window 15, open butterfly valve 19 to add magnesium powder; analyze the collected Grignard reagent, the raw materials are completely converted, and the purity of Grignard reagent is 85%.
[0054] In the description of this utility model, it should be understood that the terms "center", "longitudinal", "transverse", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc., indicating the orientation or positional relationship are based on the orientation or positional relationship shown in the accompanying drawings, and are only for the convenience of describing this utility model and simplifying the description, and are not intended to indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this utility model.
[0055] 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 as "first" or "second" may explicitly or implicitly include at least one of that feature. In the description of this utility model, "a plurality of" means at least two, such as two, three, etc., unless otherwise explicitly specified.
[0056] In this utility model, unless otherwise explicitly specified and limited, the terms "installation," "connection," "joining," and "fixing," etc., should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; 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; they can refer to the internal communication of two components or the interaction between two components, unless otherwise explicitly limited. Those skilled in the art can understand the specific meaning of the above terms in this utility model according to the specific circumstances.
[0057] In this utility model, unless otherwise explicitly specified and limited, "above" or "below" the second feature can mean that the first feature is in direct contact with the second feature, or that the first feature is in indirect contact with the second feature through an intermediate medium. Furthermore, "above," "on top of," and "over" the second feature can mean that the first feature is directly above or diagonally above the second feature, or simply that the first feature is at a higher horizontal level than the second feature. "Below," "below," and "under" the second feature can mean that the first feature is directly below or diagonally below the second feature, or simply that the first feature is at a lower horizontal level than the second feature.
[0058] It should be noted that when an element is referred to as being "fixed to" or "set on" another element, it can be directly on the other element or there may be an intervening element. When an element is considered to be "connected to" another element, it can be directly connected to the other element or there may be an intervening element. The terms "vertical," "horizontal," "upper," "lower," "left," "right," and similar expressions used herein are for illustrative purposes only and do not represent the only possible implementation.
[0059] The preferred embodiments of this utility model have been described in detail above. It should be understood that those skilled in the art can make numerous modifications and variations based on the concept of this utility model without creative effort. Therefore, all technical solutions that can be obtained by those skilled in the art based on the concept of this utility model through logical analysis, reasoning, or limited experimentation on the basis of existing technology should be within the scope of protection defined by the claims.
Claims
1. A continuous Grignard reagent synthesis apparatus, characterized by, The device comprises a tubular reactor body (2) and a stirrer, the lower end and the upper end of the reactor body (2) are respectively provided with a liquid inlet (7) and a discharge port (8), the top of the reactor body (2) is connected with a magnesium powder feeding unit through a magnesium powder inlet (4), and the reactor body (2) is externally provided with a jacket (24) for heating and cooling the reaction material; the stirrer comprises a motor (3) and a support rod (5) connected with the output end of the motor (3), the motor (3) is arranged at the top of the reactor body (2), the support rod (5) extends downward from the top in the reactor body (2), and a mixing assembly (6) is arranged on the support rod (5), the mixing assembly (6) comprises a propelling stirring rod, and holes are distributed on the propelling stirring rod.
2. A continuous Grignard reagent synthesis apparatus according to claim 1, wherein, The jacket (24) is provided with a plurality of longitudinally arranged temperature control medium inputting units.
3. A continuous Grignard reagent synthesis apparatus according to claim 2, wherein, The reactor body (2) comprises a first reaction section, a second reaction section and a discharge section which are sequentially communicated from bottom to top, and the temperature of the outer jacket (24) of the second reaction section is higher than that of the outer jacket (24) of the first reaction section.
4. The apparatus for continuous synthesis of Grignard reagent according to claim 1, wherein, The reactor body (2) comprises a plurality of reaction sections and a discharge section which are sequentially communicated from bottom to top, and a temperature detector is arranged at the beginning of the first reaction section, between each reaction section and the outlet of the discharge section.
5. The apparatus for continuous synthesis of Grignard reagent according to claim 1, wherein, The magnesium powder feeding unit comprises a magnesium powder bin (16), a magnesium powder conveying device (17) and a feeding funnel (18) which are sequentially connected, the magnesium powder bin (16) is provided with an inert gas purging pipeline, and the feeding funnel (18) is connected with the magnesium powder inlet (4) through a valve.
6. The apparatus for continuous synthesis of Grignard reagent according to claim 1, wherein, A window (15) is arranged on the upper part of the reactor body (2).
7. The apparatus for continuous synthesis of Grignard reagent according to claim 1, wherein, An emergency discharge port (23) is arranged on the upper part of the reactor body (2).
8. The apparatus for continuous synthesis of Grignard reagent according to claim 1, wherein, The magnesium powder inlet (4) and the discharge port (8) of the reactor body (2) are respectively provided with a filter screen.
9. A Grignard reagent continuous synthesis system comprising a feed solution supply subsystem (200), a feed solution receiving subsystem (300), and a temperature control subsystem (400), characterized in that, The device further comprises the Grignard reagent continuous synthesis device (100) according to any one of claims 1-8, a liquid supply subsystem (200) is connected with the liquid inlet (7) of the Grignard reagent continuous synthesis device (100), a liquid receiving subsystem (300) is connected with the discharge port (8) of the Grignard reagent continuous synthesis device (100), and a temperature control subsystem (400) is connected with the jacket (24) of the Grignard reagent continuous synthesis device (100).
10. The Grignard reagent continuous synthesis system of claim 9, wherein, The liquid supply subsystem (200) comprises a raw material conveying unit, a solvent cleaning unit and a raw material initiating unit.
11. The Grignard reagent continuous synthesis system of claim 9, wherein, The liquid receiving subsystem (300) comprises a Grignard reagent receiving tank (304) and a waste liquid tank (303), the Grignard reagent receiving tank (304) and the waste liquid tank (303) are respectively connected with the discharge port (8), and the Grignard reagent receiving tank (304) and the waste liquid tank (303) are respectively provided with a gas outlet connected with a tail gas absorption unit.
12. The Grignard reagent continuous synthesis system of claim 9, wherein, The temperature control subsystem (400) is provided with a temperature measuring point on the inlet and outlet pipelines connected with the jacket (24).
Citation Information
Patent Citations
Grignard reagent continuous preparation device and system
CN212068771U