A continuous flow reactor for grignard reagents

Abstract

The utility model relates to reactor technical field, concretely is a kind of grignard reagent continuous flow reactor, including fixing frame, the upper surface of fixing frame is fixedly connected with bearing frame, the inner wall of bearing frame is fixedly installed with funnel bottle, the top of funnel bottle is fixedly installed with nitrogen balance mouth, the bottom of funnel bottle is fixedly communicated with double-jacket pipe through communicating pipe, the bottom of double-jacket pipe is fixedly communicated with liquid inlet, the surface of double-jacket pipe is fixedly communicated with heat exchange inlet, heat exchange outlet and liquid outlet respectively, the inner wall of fixing frame is fixedly installed with temperature display screen;The utility model is set up novel continuous flow reaction, can improve the security of whole reaction process, control the descending speed of magnesium grain simultaneously, further improve the efficiency of reaction, solve the problem that reaction process is very dangerous and reaction end control is more complex in traditional kettle type reaction synthesis due to the above characteristics of grignard reagent preparation.

Description

Technical Field

[0001] This utility model relates to the field of reactor technology, and in particular to a Grignard reagent continuous flow reactor. Background Technology

[0002] Grignard reagents are a class of organometallic compounds containing magnesium halides. They contain carbanions and are strong nucleophiles, capable of reacting with carbonyl, carboxyl, double bond, and halogenated groups. Therefore, they have a wide range of applications in biology, medicine, and chemical engineering.

[0003] In existing technologies, the preparation of Grignard reagents in chemical synthesis is a violent and difficult-to-control process. The reactants are flammable, explosive, and toxic, and the reaction requires anhydrous and oxygen-free conditions. Traditional batch reactor synthesis is extremely dangerous due to these characteristics, and controlling the reaction termination is complex. Furthermore, traditional batch reactor synthesis often cannot control the descent rate of the reactants. If the magnesium particles enter too slowly, it may prolong the reaction time; if it is too fast, it may lead to incomplete reaction or the formation of byproducts, affecting the reaction outcome. Therefore, a continuous flow reactor for Grignard reagents is proposed to solve these problems. Utility Model Content

[0004] To address the aforementioned technical problems, this invention proposes a Grignard reagent continuous flow reactor. By employing this novel continuous flow reactor design, the safety of the entire reaction process can be improved, while simultaneously controlling the descent rate of magnesium particles to further enhance reaction efficiency.

[0005] The technical solution to achieve the purpose of this utility model is as follows: a Grignard reagent continuous flow reactor, including a fixed frame, a support frame fixedly connected to the upper surface of the fixed frame, a funnel bottle fixedly installed on the inner wall of the support frame, a nitrogen balance port fixedly installed at the top of the funnel bottle, a double-layer jacketed tube fixedly connected to the bottom of the funnel bottle through a connecting pipe, a liquid inlet fixedly connected to the bottom of the double-layer jacketed tube, a heat exchange inlet, a heat exchange outlet and a liquid outlet fixedly connected to the surface of the double-layer jacketed tube respectively, and a temperature display screen fixedly installed on the inner wall of the fixed frame.

[0006] In some embodiments, a rotating rod is rotatably connected to the inner wall of the connecting pipe, a motor is fixedly mounted on one side of the support frame via a mounting bracket, an intermittent gear is rotatably mounted on one side of the support frame, and the output end of the motor is fixedly connected to the intermittent gear.

[0007] In some embodiments, a drive gear is fixedly connected to one end of the rotating rod, the intermittent gear meshes with the drive gear, and a bevel gear is fixedly installed at the end of the rotating rod away from the drive gear.

[0008] In some embodiments, a fixed inclined plate is fixedly connected to the inner wall of the connecting pipe, and an mounting plate is fixedly connected to the upper surface of the fixed inclined plate. A sliding hole is opened on the upper surface of the mounting plate, and a right-angle rod is slidably connected to the inner wall of the sliding hole. A ball is fixedly connected to both ends of the right-angle rod, and a spring is sleeved on the surface of the right-angle rod.

[0009] In some embodiments, the lower surface of the fixed inclined plate is provided with a T-shaped circular groove, and a plurality of T-shaped sliders are slidably connected to the inner wall of the T-shaped circular groove. The lower surfaces of the plurality of T-shaped sliders are fixedly connected to the same rotating plate.

[0010] In some embodiments, the upper surfaces of the fixed inclined plate and the rotating plate are respectively provided with a rotating hole and a through hole. A rotating shaft is fixedly connected to the inner wall of the through hole. The surface of the rotating shaft is rotatably connected to the inner wall of the rotating hole. A spherical rod is fixedly connected to the surface of the rotating shaft. A bevel gear is fixedly connected to the bottom end of the rotating rod. The two bevel gears mesh with each other.

[0011] In some embodiments, the upper surface of the fixed inclined plate is provided with a second discharge hole, and the upper surface of the rotating plate is provided with a plurality of first discharge holes.

[0012] Compared with existing technologies, the significant advantages of this invention are:

[0013] Firstly, this invention fills a funnel-shaped flask with 3mm dry magnesium granules. The magnesium granules fall into the middle tube of a double-jacketed tube, which is connected to external heat exchange oil via the outer jacket. The temperature of the double-jacketed tube is adjusted to the optimal reaction temperature. Nitrogen gas is introduced through the lower inlet for 10 minutes, and then discharged from the nitrogen balance port and outlet to displace the air in the reactor. After this process, a constant flow of 0.1 MPa nitrogen gas is connected to the nitrogen balance port. At the start of the reaction, the reaction solution containing the initiator is pumped into the inlet using a constant flow pump. After the reaction is initiated, the reaction solution without the initiator is continuously pumped into the inlet in a constant flow mode. The reaction solution continues to flow through the gaps between the magnesium granules. The reaction outlet is connected to a multi-necked bottle filled with nitrogen, thus continuously obtaining Grignard reagent. Over time, the magnesium granules in the reaction tube are gradually consumed, and the magnesium granules in the funnel-shaped flask automatically slide back into the reaction tube to fill the air gaps, achieving a continuous Grignard reaction.

[0014] Secondly, this utility model uses a motor to drive an intermittent gear, which in turn drives a rotating rod to rotate. Two bevel gears drive a rotating shaft to rotate, which in turn enables the rotating plate and the spherical rod to rotate synchronously. This causes the first discharge hole on the rotating plate to coincide with the second discharge hole on the fixed inclined plate, allowing the magnesium particles to fall intermittently. This controls the falling speed of the magnesium particles and improves the reaction efficiency. When the spherical rod rotates, it can reciprocate to squeeze one of the spheres on the right-angle rod, enabling the right-angle rod to rise and fall back and forth, thus clearing the second discharge hole.

[0015] This invention solves the problems in traditional batch reactor synthesis, where the preparation of Grignard reagents is inherently dangerous, the reaction process is complex to control, and the rate at which the reaction ends is difficult to control. Furthermore, traditional batch reactor synthesis often cannot control the rate at which the reactants descend. If the rate at which magnesium particles enter is too slow, it may prolong the reaction time; if it is too fast, it may lead to incomplete reaction or the formation of byproducts, thus affecting the reaction efficiency. Attached Figure Description

[0016] The present invention will be further explained below with reference to the accompanying drawings and embodiments:

[0017] Figure 1 This is a three-dimensional structural schematic diagram provided in one embodiment of the present invention;

[0018] Figure 2 This is a cross-sectional structural diagram of the control device provided in one embodiment of the present invention;

[0019] Figure 3 This utility model provides in one embodiment Figure 2 Enlarged structural diagram at point A in the middle;

[0020] Figure 4 This is an exploded structural diagram of the control device provided in one embodiment of the present invention.

[0021] Explanation of reference numerals in the attached figures:

[0022] 1. Fixed frame; 2. Support frame; 3. Funnel bottle; 4. Nitrogen balance port; 5. Connecting pipe; 6. Double-layer jacketed pipe; 7. Liquid inlet; 8. Heat exchange inlet; 9. Heat exchange outlet; 10. Temperature display screen; 11. Liquid outlet; 12. Intermittent gear; 13. Motor; 14. Rotating rod; 15. Drive gear; 16. Fixed inclined plate; 17. Rotating shaft; 18. Rotating plate; 19. Mounting plate; 20. Right angle rod; 21. Spring; 22. Sphere; 23. Spherical rod; 24. T-shaped groove; 25. T-shaped slider; 26. Bevel gear; 27. Discharge hole one; 28. Discharge hole two. Detailed Implementation

[0023] The present invention will now be described in detail, and the technical solutions in the embodiments of the present invention will be clearly and completely described. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the protection scope of the present invention.

[0024] This invention provides an improved Grignard reagent continuous flow reactor. The technical solution of this invention is as follows:

[0025] Example 1

[0026] like Figures 1-4 As shown, a Grignard reagent continuous flow reactor includes a fixed frame 1, a support frame 2 fixedly connected to the upper surface of the fixed frame 1, the support frame 2 can fix the funnel bottle 3, the funnel bottle 3 is fixedly installed on the inner wall of the support frame 2, a nitrogen balance port 4 is fixedly installed at the top of the funnel bottle 3, a double-layer jacketed tube 6 is fixedly connected to the bottom of the funnel bottle 3 through a connecting pipe 5, a liquid inlet 7 is fixedly connected to the bottom of the double-layer jacketed tube 6, and a heat exchange inlet 8, a heat exchange outlet 9 and a liquid outlet 11 are fixedly connected to the surface of the double-layer jacketed tube 6 respectively, and a temperature display screen 10 is fixedly installed on the inner wall of the fixed frame 1.

[0027] Example 2

[0028] like Figure 2 and Figure 3 As shown, in one embodiment, a rotating rod 14 is rotatably connected to the inner wall of the connecting pipe 5, a motor 13 is fixedly installed on one side of the support frame 2 by a mounting bracket, an intermittent gear 12 is rotatably installed on one side of the support frame 2, and the output end of the motor 13 is fixedly connected to the intermittent gear 12.

[0029] One end of the rotating rod 14 is fixedly connected to a drive gear 15. The intermittent gear 12 meshes with the drive gear 15. A bevel gear 26 is fixedly installed at the end of the rotating rod 14 away from the drive gear 15. By setting the drive gear 15 to mesh with the intermittent gear 12, the drive gear 15 can be driven to rotate intermittently when the intermittent gear 12 rotates, thereby realizing the intermittent falling of magnesium particles inside the connecting pipe 5 and controlling the reaction speed.

[0030] A fixed inclined plate 16 is fixedly connected to the inner wall of the connecting pipe 5. The fixed inclined plate 16 is designed so that when the magnesium particles reach the inside of the connecting pipe 5, the magnesium particles gather above the discharge hole 28 opened on the fixed inclined plate 16, which facilitates discharge. A mounting plate 19 is fixedly connected to the upper surface of the fixed inclined plate 16. A sliding hole is opened on the upper surface of the mounting plate 19. A right-angle rod 20 is slidably connected to the inner wall of the sliding hole. A ball 22 is fixedly connected to both ends of the right-angle rod 20. A spring 21 is sleeved on the surface of the right-angle rod 20. The reciprocating motion of the right-angle rod 20 can be realized by the spring 21.

[0031] like Figure 4 As shown, in one embodiment, a T-shaped groove 24 is provided on the lower surface of the fixed inclined plate 16. A plurality of T-shaped sliders 25 are slidably connected to the inner wall of the T-shaped groove 24. The lower surface of the plurality of T-shaped sliders 25 is fixedly connected to the same rotating plate 18. The rotation limit of the rotating plate 18 can be achieved by the T-shaped groove 24 and the T-shaped sliders 25.

[0032] The upper surfaces of the fixed inclined plate 16 and the rotating plate 18 are respectively provided with a rotating hole and a through hole. The inner wall of the through hole is fixedly connected to a rotating shaft 17. The surface of the rotating shaft 17 is rotatably connected to the inner wall of the rotating hole. A ball rod 23 is fixedly connected to the surface of the rotating shaft 17. A bevel gear 26 is fixedly connected to the bottom end of the rotating rod 14. The two bevel gears 26 mesh with each other and are of the same specification.

[0033] The upper surface of the fixed inclined plate 16 is provided with a discharge hole 28, and the upper surface of the rotating plate 18 is provided with multiple discharge holes 27.

[0034] The specific working method is as follows: Before the reaction begins, the funnel flask 3 is filled with 3mm dry magnesium granules. The magnesium granules slide into the connecting tube 5 under gravity. The motor 13 operates, and the intermittent gear 12 drives the drive gear 15 to rotate, which in turn drives the rotating rod 14 to rotate. The two bevel gears 26 drive the rotating shaft 17 to rotate. The rotation of the rotating shaft 17 enables the rotating plate 18 and the ball rod 23 to rotate synchronously, thereby causing the discharge hole 27 on the rotating plate 18 and the fixed inclined plate 16 to rotate synchronously. The two feed holes 28 overlap, allowing for intermittent falling of magnesium particles. This controls the falling speed and improves reaction efficiency. When the spherical rod 23 rotates, it reciprocates by squeezing one of the spheres 22 on the right-angle rod 20, causing the rod to rise and fall. This clears the feed hole 28, allowing the magnesium particles falling through the feed hole 27 to enter the intermediate tube of the double-jacketed tube 6. The outer jacket of the double-jacketed tube 6 is connected to external heat exchange oil, adjusting the temperature of the double-jacketed tube 6 to the optimal reaction temperature. Nitrogen gas is introduced through the lower inlet 7 for 10 minutes, and then discharged from the nitrogen balance port 4 and the outlet 11, replacing the air in the reactor. After this process, the nitrogen balance port 4 is connected to a constant flow of 0.1 MPa nitrogen.

[0035] To initiate the reaction, the reaction solution containing the initiator is pumped into inlet 7 using a constant flow pump. After the reaction is initiated, the solution is replaced with a reaction solution without the initiator, which is then continuously pumped into inlet 7 in a constant flow mode. The reaction solution continues to flow through the gaps between the magnesium particles, and the reaction outlet 11 is connected to a multi-necked flask filled with nitrogen, thus continuously obtaining Grignard reagent. As time progresses, the magnesium particles in the reaction tube are gradually consumed, and the magnesium particles in the funnel flask 3 are intermittently added to the reaction tube inside the double-jacketed tube 6 to fill the voids, achieving a continuous Grignard reaction.

[0036] The technical means disclosed in this utility model are not limited to those described above, but also include technical solutions composed of equivalent substitutions of the above technical features. Matters not covered in this utility model are common knowledge to those skilled in the art.

Claims

1. A Grignard reagent continuous flow reactor, comprising a fixed frame (1), characterized in that: A support frame (2) is fixedly connected to the upper surface of the fixed frame (1). A funnel bottle (3) is fixedly installed on the inner wall of the support frame (2). A nitrogen balance port (4) is fixedly installed at the top of the funnel bottle (3). A double-layer jacketed pipe (6) is fixedly connected to the bottom of the funnel bottle (3) through a connecting pipe (5). A liquid inlet (7) is fixedly connected to the bottom of the double-layer jacketed pipe (6). A heat exchange inlet (8), a heat exchange outlet (9), and a liquid outlet (11) are fixedly connected to the surface of the double-layer jacketed pipe (6). A temperature display screen (10) is fixedly installed on the inner wall of the fixed frame (1).

2. A continuous flow Grignard reagent reactor according to claim 1, wherein: The inner wall of the connecting pipe (5) is rotatably connected to a rotating rod (14). A motor (13) is fixedly installed on one side of the support frame (2) through a mounting bracket. An intermittent gear (12) is rotatably installed on one side of the support frame (2). The output end of the motor (13) is fixedly connected to the intermittent gear (12).

3. A Grignard reagent continuous flow reactor according to claim 2, characterized in that: One end of the rotating rod (14) is fixedly connected to a drive gear (15), the intermittent gear (12) meshes with the drive gear (15), and a bevel gear (26) is fixedly installed at the end of the rotating rod (14) away from the drive gear (15).

4. A continuous flow Grignard reagent reactor according to claim 2, wherein: The inner wall of the connecting pipe (5) is fixedly connected to a fixed inclined plate (16), and the upper surface of the fixed inclined plate (16) is fixedly connected to an mounting plate (19). The upper surface of the mounting plate (19) is provided with a sliding hole, and the inner wall of the sliding hole is slidably connected to a right-angle rod (20). Both ends of the right-angle rod (20) are fixedly connected to a ball (22), and a spring (21) is sleeved on the surface of the right-angle rod (20).

5. A continuous flow Grignard reagent reactor according to claim 4, wherein: The lower surface of the fixed inclined plate (16) is provided with a T-shaped circular groove (24), and a plurality of T-shaped sliders (25) are slidably connected to the inner wall of the T-shaped circular groove (24). The lower surfaces of the plurality of T-shaped sliders (25) are fixedly connected to the same rotating plate (18).

6. A continuous flow Grignard reagent reactor according to claim 5, wherein: The upper surfaces of the fixed inclined plate (16) and the rotating plate (18) are respectively provided with a rotating hole and a through hole. The inner wall of the through hole is fixedly connected to a rotating shaft (17). The surface of the rotating shaft (17) is rotatably connected to the inner wall of the rotating hole. The surface of the rotating shaft (17) is fixedly connected to a spherical rod (23). The bottom end of the rotating rod (14) is fixedly connected to a bevel gear (26). The two bevel gears (26) mesh with each other.

7. A Grignard reagent continuous flow reactor according to claim 6, characterized in that: The upper surface of the fixed inclined plate (16) is provided with a second feeding hole (28), and the upper surface of the rotating plate (18) is provided with a plurality of first feeding holes (27).

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