Grignard reagent preparation fixed bed reactor device

Abstract

The invention provides a fixed bed reactor device for Grignard reagent preparation, and belongs to the technical field of Grignard reagent preparation. In the Grignard reagent preparation fixed bed reactor device, a first reactor is provided with a first reaction cavity, and a first feed port and a first discharge port which are both communicated with the first reaction cavity, a second reactor is provided with a second reaction cavity, and a second feed port and a second discharge port which are both communicated with the second reaction cavity, and the output end of a feed pump is communicated with the first feed port; the first discharging opening is communicated with the second feeding opening, and the second discharging opening is communicated with the collecting device; the output end of the vacuum conveyor is communicated with the two fixed feeders, and the two solid feeders are respectively communicated with the first reaction cavity and the second reaction cavity; the first reactor and the second reactor are both communicated with a post-treatment device, and the post-treatment device is used for treating gasified tetrahydrofuran. The reaction efficiency can be improved, continuous reaction is realized, the reaction is more thorough, and the product purity is improved.

Description

Technical Field

[0001] The invention belongs to the technical field of Grignard reagent preparation, and in particular relates to a fixed bed reactor device for preparing Grignard reagent. Background Art

[0002] Grignard reagent was created by French chemist Grignard in 1901. Organomagnesium reagent is formed by the reaction of organic halogen compounds (alkyl halides, active aryl halides) and metallic magnesium in absolutely anhydrous ether. Grignard reagent has a wide range of applications in pharmaceutical chemicals and even the entire field of chemical organic synthesis, and plays an important role. Grignard reagent can not only prepare various types of chemical syntheses, but also plays a vital role in real life. The research of relevant technicians on the special properties of Grignard reagent is also becoming more and more in-depth, and in the research of Grignard reagent reaction technology, the research on the preparation of Grignard reagent is also the top priority in the research of this technology. In the preparation process of Grignard reagent, how to successfully prepare Grignard reagent and realize the safe, efficient and continuous production of Grignard reagent is an important research direction for technicians.

[0003] The existing preparation of Grignard reagents is completed in an intermittent manner. In a reaction bottle or a reactor, first place magnesium metal, an initiator and a small amount of solvent at the bottom of the reaction bottle or the reactor, then drop some halides from the top of the reactor or the reactor, and continue to drop the remaining halides after initiation to form. During the reaction, magnesium metal dissolves and turns into Grignard reagents. The reaction is an exothermic reaction and needs to release heat through condensation and reflux. After the reaction is completed, the excess magnesium metal is removed by filtration. It is necessary to add all the halides to form the Grignard reagent before it can be released from the reactor to continue the next batch of reactions. The relative work efficiency is low, and the reaction is an exothermic reaction, which has a great risk of material impact and explosion. Summary of the invention

[0004] In view of this, in order to solve the problem that the existing Grignard reagent preparation is completed in an intermittent manner, all the halides need to be added to form the Grignard reagent before they can be released from the reactor to continue the next batch of reaction, the relatively low working efficiency, and the reaction is an exothermic reaction, and there is a great risk of material impact and explosion, the present invention proposes a fixed bed reactor device for preparing Grignard reagent.

[0005] To achieve the above object, the present invention adopts the following technical solutions:

[0006] A fixed bed reactor device for preparing a Grignard reagent, comprising:

[0007] Feed pump;

[0008] A first reactor, a second reactor and a collecting device, wherein the first reactor is provided with a first reaction chamber and a first feed port and a first discharge port both connected to the first reaction chamber, the second reactor is provided with a second reaction chamber and a second feed port and a second discharge port both connected to the second reaction chamber, the output end of the feed pump is connected to the first feed port, the first discharge port is connected to the second feed port, and the second discharge port is connected to the collecting device;

[0009] A vacuum conveyor and two solid feeders, wherein the output end of the vacuum conveyor is connected to both of the two solid feeders, and the two solid feeders are connected to the first reaction chamber and the second reaction chamber respectively;

[0010] A post-processing device, wherein the first reactor and the second reactor are both connected to the post-processing device, and the post-processing device is used to process the gasified tetrahydrofuran.

[0011] As a preferred embodiment of the above-mentioned fixed bed reactor device for preparing Grignard reagent, the first reactor is also provided with a sieve plate and a containing chamber, the sieve plate is arranged between the containing chamber and the first reaction chamber, the containing chamber is located below the first reaction chamber, the sieve plate is provided with a plurality of through holes, the through holes connect the containing chamber and the first reaction chamber, the first feed port is connected with the containing chamber, the first feed port is arranged below the first reactor, and the first discharge port is arranged above the first reactor.

[0012] As a preferred solution of the above-mentioned fixed bed reactor device for preparing Grignard reagent, the first reactor is also fixedly provided with an ultrasonic vibrator, and the ultrasonic vibrator is located in the first reaction chamber.

[0013] As a preferred solution of the above-mentioned fixed bed reactor device for preparing Grignard reagent, the outer side of the ultrasonic vibrator is coated with a filter screen.

[0014] As a preferred solution of the above-mentioned fixed bed reactor device for preparing Grignard reagent, there are multiple filter screens, and the multiple filter screens are sequentially coated on the outside of the ultrasonic vibrator.

[0015] As a preferred solution of the above-mentioned fixed bed reactor device for preparing Grignard reagent, the post-treatment device includes a condenser and a storage tank, the first reactor is connected to the condenser, and the condenser is connected to the storage tank.

[0016] As a preferred solution of the above-mentioned fixed bed reactor device for preparing Grignard reagent, the first reactor is further provided with a jacket, and the jacket is used to cool the first reaction chamber.

[0017] As a preferred solution of the above-mentioned fixed bed reactor device for preparing Grignard reagent, the inner plate of the jacket is provided with a liquid nitrogen coil.

[0018] As a preferred solution of the above-mentioned fixed bed reactor device for preparing Grignard reagent, the first reactor is also provided with a plurality of temperature-sensitive sensors, and the plurality of temperature-sensitive sensors are arranged at intervals.

[0019] As a preferred solution of the above-mentioned fixed bed reactor device for preparing Grignard reagent, the first reactor is provided with a sight glass, through which the first reaction chamber can be seen.

[0020] Compared with the prior art, the invention provides a Grignard reagent preparation fixed bed reactor device with the following beneficial effects:

[0021] 1. The present invention provides a fixed bed reactor device for preparing Grignard reagents, in which tetrahydrofuran is used as a solvent, and an organic halogen compound is used as a solute, which is transported into a first reactor by a feed pump, and magnesium particles are also involved in the reaction as a catalyst. The magnesium particles are first fed into two solid feeders through a vacuum feeder, and then enter the first reactor through one of the solid feeders, and enter the second reactor through the other solid feeder, so that the magnesium particles can be put into the first reactor without contact, and the timing and automatic feeding can also be set. The material reacts in the first reaction chamber, and then enters the second reaction chamber after passing through the first reaction chamber, and continues to react in the second reaction chamber. After the reaction in the second reaction chamber is completed, the finished product is collected into a collection device. The fixed bed reactor device for preparing Grignard reagents is provided with a first reactor and a second reactor connected in series, and the material after the reaction in the first reactor enters the second reactor, and the part that has not reacted completely in the first reactor reacts again in the second reactor, which can greatly improve the reaction efficiency, realize continuous reaction, and make the reaction more thorough, improve the purity of the product, and avoid the cumbersome steps of reprocessing the impure reactants.

[0022] 2. The present invention provides a fixed-bed reactor device for preparing a Grignard reagent. In the fixed-bed reactor device for preparing a Grignard reagent, a feed pump and a solid feeder are used to add materials into a first reactor and a second reaction chamber, thereby realizing a continuous reaction. This effectively avoids the tedious operation of the experimenter manually dripping initiators to initiate the reaction and adding catalysts and materials during the experiment, thereby greatly improving the experimental efficiency.

[0023] 3. The present invention provides a fixed-bed reactor device for preparing a Grignard reagent. In the fixed-bed reactor device for preparing a Grignard reagent, since the reaction of the Grignard reagent is very intense, the reaction temperature rises sharply, which will cause a large amount of tetrahydrofuran to be vaporized. The vaporized tetrahydrofuran will enter a post-processing device. The post-processing device effectively prevents the leakage of tetrahydrofuran gas and recycles it, thereby saving costs and greatly ensuring the safety of experimenters.

[0024] 4. The present invention provides a fixed bed reactor device for preparing Grignard reagents. In the fixed bed reactor device for preparing Grignard reagents, the first reactor is also provided with a sieve plate and a containing chamber. The sieve plate is arranged between the containing chamber and the first reaction chamber. The containing chamber is located below the first reaction chamber. The sieve plate is provided with a plurality of through holes. The through holes connect the containing chamber and the first reaction chamber. The first feed port is connected with the containing chamber. The first feed port is arranged below the first reactor. The first discharge port is arranged above the first reactor. The material first enters the containing chamber. Since the volume of the containing chamber is very small, the material entering the containing chamber will enter the reaction chamber through the sieve plate. The material passing through the sieve plate can not only achieve the purpose of remixing the material, but also disperse the liquid, increase the contact area between the raw material and the catalyst, that is, increase the reaction phase interface between the material and the magnesium particles, thereby improving the reaction efficiency. In addition, the magnesium particles gradually become smaller during the reaction process. The too small magnesium particles can enter the containing chamber through the sieve plate, thereby preventing the too small magnesium particles from contacting the ultrasonic vibrator through the filter screen. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] The accompanying drawings constituting a part of the present invention are used to provide a further understanding of the present invention. The exemplary embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation of the present invention. In the accompanying drawings:

[0026] Figure 1 is a structural schematic diagram of a fixed-bed reactor device for preparing a Grignard reagent provided by a specific embodiment of the present invention along a first viewing angle;

[0027] Figure 2 is a cross-sectional view of a first reactor of a fixed-bed reactor device for preparing a Grignard reagent provided by a specific embodiment of the present invention;

[0028] Figure 3 2 is a schematic structural diagram of a first reactor of a fixed-bed reactor device for preparing a Grignard reagent provided in a specific embodiment of the present invention;

[0029] Figure 4 It is a structural schematic diagram of a post-processing device of a fixed-bed reactor device for preparing a Grignard reagent provided by a specific embodiment of the present invention;

[0030] Figure 5 It is a structural schematic diagram of a fixed bed reactor device for preparing Grignard reagent provided by a specific embodiment of the present invention along a second viewing angle.

[0031] In the figure:

[0032] 1. Feed pump;

[0033] 2. First reactor; 21. First reaction chamber; 22. First feed port; 23. First discharge port; 24. Accommodation chamber; 25. Discharge port; 26. Sight glass;

[0034] 3. The second reactor;

[0035] 4. Vacuum feeder;

[0036] 5. Solid feeder;

[0037] 6. Post-processing device; 61. Condenser; 62. Storage tank;

[0038] 7. Ultrasonic vibrator;

[0039] 8. Sieve plate;

[0040] 9. Temperature sensor;

[0041] 10. Jacket;

[0042] 11. Liquid nitrogen coil;

[0043] 12. Low temperature circulation pump;

[0044] 13. Control cabinet. DETAILED DESCRIPTION

[0045] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely explain the technical solutions in the embodiments of the present invention. It should be noted that the embodiments of the present invention and the features in the embodiments can be combined with each other without conflict, and the described embodiments are only part of the embodiments of the present invention, not all of the embodiments.

[0046] In the description of the present invention, unless otherwise clearly specified and limited, the terms "connected", "connected", and "fixed" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0047] In the present invention, unless otherwise clearly specified and limited, a first feature being "above" or "below" a second feature may include that the first and second features are in direct contact, or may include that the first and second features are not in direct contact but are in contact through another feature between them. Moreover, a first feature being "above", "above" and "above" a second feature includes that the first feature is directly above and obliquely above the second feature, or simply indicates that the first feature is higher in level than the second feature. A first feature being "below", "below" and "below" a second feature includes that the first feature is directly below and obliquely below the second feature, or simply indicates that the first feature is lower in level than the second feature.

[0048] In the description of this embodiment, the terms "upper", "lower", "right" and other directions or positional relationships are based on the directions or positional relationships shown in the drawings, and are only for the convenience of description and simplified operation, rather than indicating or implying that the device or element referred to must have a specific direction, be constructed and operated in a specific direction, and therefore cannot be understood as limiting the present invention. In addition, the terms "first" and "second" are only used to distinguish in the description and have no special meaning.

[0049] See also Figure 1-5 Description of this embodiment. The present invention provides a fixed-bed reactor device for preparing a Grignard reagent, which includes a feed pump 1, a first reactor 2, a second reactor 3, a collecting device, a vacuum conveyor 4, two solid feeders 5 and a post-processing device 6. The first reactor 2 is provided with a first reaction chamber 21 and a first feed port 22 and a first discharge port 23 both connected to the first reaction chamber 21, the second reactor 3 is provided with a second reaction chamber and a second feed port and a second discharge port both connected to the second reaction chamber, the output end of the feed pump 1 is connected to the first feed port 22, the first discharge port 23 is connected to the second feed port, and the second discharge port is connected to the collecting device; the output end of the vacuum conveyor 4 is connected to the two solid feeders 5, and the two solid feeders 5 are respectively connected to the first reaction chamber 21 and the second reaction chamber; the first reactor 2 and the second reactor 3 are both connected to the post-processing device 6, and the post-processing device 6 is used to process gasified tetrahydrofuran.

[0050] like Figure 1 and Figure 2As shown, in the fixed-bed reactor device for preparing Grignard reagent, tetrahydrofuran is used as a solvent, and an organic halogen compound is used as a solute, which is transported into the first reactor 2 by a feed pump 1. Magnesium particles also participate in the reaction as a catalyst. The magnesium particles are first fed into two solid feeders 5 through a vacuum feeder 4, and then enter the first reactor 2 through one of the solid feeders 5, and enter the second reactor 3 through the other solid feeder 5. It can realize contactless delivery of magnesium particles, and can also be set to automatically deliver them at a fixed time. The material reacts in the first reaction chamber 21, and then enters the second reaction chamber after passing through the first reaction chamber 21, and continues to react in the second reaction chamber. After the reaction in the second reaction chamber is completed, the finished product is collected into a collection device. The fixed-bed reactor device for preparing Grignard reagent is provided with a first reactor 2 and a second reactor 3 connected in series. The material after the reaction in the first reactor 2 enters the second reactor 3, and the part that has not reacted completely in the first reactor 2 reacts again in the second reactor 3, which can greatly improve the reaction efficiency, realize continuous reaction, and make the reaction more thorough, improve the purity of the product, and avoid the cumbersome steps of reprocessing the impure reactants. And by feeding the first reactor 2 and the second reaction chamber with the feed pump 1 and the solid feeder 5, a continuous reaction is realized, which effectively avoids the tedious operation of the experimenter manually dropping the initiator to initiate the reaction and adding the catalyst and materials during the experiment, and greatly improves the experimental efficiency. Since the reaction of the Grignard reagent preparation is very intense, the rapid increase in the reaction temperature will cause a large amount of tetrahydrofuran to be vaporized, and the vaporized tetrahydrofuran will enter the post-processing device 6. The post-processing device 6 effectively prevents the leakage of tetrahydrofuran gas and recycles it, saving costs and greatly ensuring the safety of the experimenters.

[0051] In this embodiment, exhaust holes are also provided on the tops of the first reactor 2 and the second reactor 3, and exhaust holes can be used to exhaust air at regular intervals.

[0052] like Figure 2 As shown, optionally, the first reactor 2 is also fixedly provided with an ultrasonic vibrator 7, which is located in the first reaction chamber 21. It is helpful for material mixing and reaction with magnesium particles.

[0053] Optionally, the outer side of the ultrasonic vibrator 7 is coated with a filter screen, which is used to block the magnesium particles and prevent the magnesium particles from contacting the ultrasonic vibrator 7 and damaging the ultrasonic vibrator 7 .

[0054] Optionally, there are multiple filters, which are sequentially coated on the outside of the ultrasonic vibrator 7. When one layer of filter is damaged, the other filters can block the magnesium particles to ensure that the ultrasonic vibrator 7 is not damaged.

[0055] It can be understood that the structures of the first reactor 2 and the second reactor 3 are basically the same. Optionally, the first reactor 2 is further provided with a sieve plate 8 and a receiving chamber 24, the sieve plate 8 is arranged between the receiving chamber 24 and the first reaction chamber 21, the receiving chamber 24 is located below the first reaction chamber 21, the sieve plate 8 is provided with a plurality of through holes, the through holes connect the receiving chamber 24 and the first reaction chamber 21, the first feed port 22 is connected with the receiving chamber 24, the first feed port 22 is arranged below the first reactor 2, and the first discharge port 23 is arranged above the first reactor 2. The material first enters the receiving chamber 24, and since the volume of the receiving chamber 24 is very small, the material entering the receiving chamber 24 will enter the reaction chamber through the sieve plate 8, and the material passing through the sieve plate 8 can not only achieve the purpose of remixing the material, but also disperse the liquid, increase the contact area between the raw material and the catalyst, that is, increase the reaction phase interface between the material and the magnesium particles, thereby improving the reaction efficiency. Furthermore, the magnesium particles gradually become smaller during the reaction process, and the magnesium particles that are too small can pass through the sieve plate 8 and enter the accommodating chamber 24, thereby preventing the magnesium particles that are too small from passing through the filter screen and contacting the ultrasonic vibrator 7.

[0056] It can be understood that the first feed port 22 is disposed below the first reactor 2, and the first discharge port 23 is disposed above the first reactor 2, so that the first reaction chamber 21 can be filled with materials.

[0057] In this embodiment, a feed pipe is connected to the first feed port 22, the feed pipe is located in the first reaction chamber 21, and the outlet of the feed pipe is connected to the through hole of the sieve plate 8. The material enters the accommodating chamber 24 from the first feed port 22 through the feed pipe and the through hole. Since the volume of the accommodating chamber 24 is very small, the material will enter the first reaction chamber 21 through the sieve plate 8.

[0058] like Figure 1 and Figure 4 As shown, optionally, the post-processing device 6 includes a condenser 61 and a storage tank 62, the first reactor 2 is connected to the condenser 61, and the condenser 61 is connected to the storage tank 62. The vaporized tetrahydrofuran is condensed into liquid in the condenser 61 and stored in the storage tank 62 to be discharged. Since the vaporized tetrahydrofuran is recycled into the post-processing device 6, impurities can be discharged and the purity of the product can be improved.

[0059] In this embodiment, there are two post-processing devices 6, both of which can recover gasified tetrahydrofuran, thereby improving the recovery efficiency and recovery amount.

[0060] like Figure 2 As shown, optionally, the first reactor 2 is further provided with a jacket 10, and the jacket 10 is used to cool the first reaction chamber 21. The jacket 10 is mainly used to maintain the temperature of the first reactor 2 to ensure its reaction conditions. The Grignard reaction is an exothermic reaction, and heat needs to be released by condensation reflux to ensure the reaction conditions of the first reactor 2 to prevent the temperature from being too high so that part of the reactant components are vaporized.

[0061] like Figure 2 As shown, optionally, a liquid nitrogen coil 11 is provided in the inner disk of the jacket 10. The device is provided with a liquid nitrogen quenching structure to prevent the risk of explosion caused by uncontrollable temperature. Liquid nitrogen is introduced into the liquid nitrogen coil 11, which can achieve the effect of quenching the first reactor 2 to ensure the safety of the experiment. The Grignard reaction is very violent and will release a lot of heat. Once the temperature is uncontrollable, the material will be vaporized in large quantities, and the pressure will rise sharply with the risk of explosion. The liquid nitrogen coil 11 can achieve the purpose of rapid cooling to ensure the safety of the experimenters.

[0062] Optionally, the fixed-bed reactor device for preparing Grignard reagent further comprises a low-temperature circulation pump 12 , and the low-temperature circulation pump 12 is used to transport a cooling medium into the jacket 10 and the liquid nitrogen coil 11 .

[0063] like Figure 2 and Figure 3 As shown, optionally, the first reactor 2 is further provided with a plurality of temperature-sensitive sensors 9, and the plurality of temperature-sensitive sensors 9 are arranged at intervals. The temperature-sensitive sensors 9 are used to monitor and chain-control the reaction temperature. Arranging a plurality of groups of temperature-sensitive sensors 9 can comprehensively detect the temperature in the first reactor 2.

[0064] Optionally, the fixed-bed reactor device for preparing Grignard reagent further includes a control cabinet 13 , and the feed pump 1 , the vacuum feeder 4 , the low-temperature circulation pump 12 and the temperature-sensitive sensor 9 are all connected to the control cabinet 13 .

[0065] like Figure 1 and Figure 3 As shown, optionally, the first reactor 2 is provided with a sight glass 26, through which the first reaction chamber 21 can be seen. The experimenter can observe the consumption of magnesium particles through the sight glass 26.

[0066] like Figure 2 As shown, optionally, a discharge port 25 is further provided at the lowermost end of the first reactor 2. The discharge port 25 is used for unloading after the reaction is completed, and can also be used for discharging waste water during cleaning.

[0067] Obviously, the embodiments of the present invention disclosed above are only used to help illustrate the present invention. The embodiments do not describe all the details in detail, nor do they limit the invention to specific implementation methods. According to the content of this specification, many modifications and changes can be made. This specification selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can understand and use the present invention well. It is not necessary and impossible to list all the implementation methods here. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the scope of protection of the claims of the present invention.

Claims

1. A fixed bed reactor device for preparing Grignard reagent, characterized in that: include: Feed pump (1); A first reactor (2), a second reactor (3) and a collecting device, wherein the first reactor (2) is provided with a first reaction chamber (21) and a first feed port (22) and a first discharge port (23) both of which are in communication with the first reaction chamber (21), the second reactor (3) is provided with a second reaction chamber and a second feed port and a second discharge port both of which are in communication with the second reaction chamber, the output end of the feed pump (1) is in communication with the first feed port (22), the first discharge port (23) is in communication with the second feed port, and the second discharge port is in communication with the collecting device; A vacuum conveyor (4) and two solid feeders (5), wherein the output end of the vacuum conveyor (4) is in communication with both of the two solid feeders (5), and the two solid feeders (5) are in communication with the first reaction chamber (21) and the second reaction chamber, respectively; A post-processing device (6), wherein the first reactor (2) and the second reactor (3) are both connected to the post-processing device (6), and the post-processing device (6) is used to process the gasified tetrahydrofuran.

2. The fixed bed reactor device for preparing Grignard reagent according to claim 1, characterized in that: The first reactor (2) is further provided with a sieve plate (8) and a containing chamber (24); the sieve plate (8) is arranged between the containing chamber (24) and the first reaction chamber (21); the containing chamber (24) is located below the first reaction chamber (21); the sieve plate (8) is provided with a plurality of through holes, the through holes connecting the containing chamber (24) and the first reaction chamber (21); the first feed port (22) is connected with the containing chamber (24); the first feed port (22) is arranged below the first reactor (2); and the first discharge port (23) is arranged above the first reactor (2).

3. The fixed bed reactor device for preparing Grignard reagent according to claim 1, characterized in that: The first reactor (2) is also fixedly provided with an ultrasonic vibrator (7), and the ultrasonic vibrator (7) is located in the first reaction chamber (21).

4. The fixed bed reactor device for preparing Grignard reagent according to claim 3, characterized in that: The outer side of the ultrasonic vibrating rod (7) is coated with a filter screen.

5. The fixed bed reactor device for preparing Grignard reagent according to claim 4, characterized in that: There are multiple filter screens, and the multiple filter screens are sequentially wrapped around the outer side of the ultrasonic vibrating rod (7).

6. The fixed bed reactor device for preparing Grignard reagent according to claim 1, characterized in that: The post-processing device (6) comprises a condenser (61) and a storage tank (62), the first reactor (2) is connected to the condenser (61), and the condenser (61) is connected to the storage tank (62).

7. The fixed bed reactor device for preparing Grignard reagent according to claim 1, characterized in that: The first reactor (2) is further provided with a jacket (10), and the jacket (10) is used to cool the first reaction chamber (21).

8. The fixed bed reactor device for preparing Grignard reagent according to claim 7, characterized in that: The inner plate of the jacket (10) is provided with a liquid nitrogen coil (11).

9. The fixed bed reactor device for preparing Grignard reagent according to claim 1, characterized in that: The first reactor (2) is also provided with a plurality of temperature-sensitive sensors (9), and the plurality of temperature-sensitive sensors (9) are arranged at intervals.

10. The fixed bed reactor device for preparing Grignard reagent according to claim 1, characterized in that: The first reactor (2) is provided with a sight glass (26), through which the first reaction chamber (21) can be seen.

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