A reactor for the synthesis of deuterated benzoic acid

Abstract

This utility model discloses a reactor for the synthesis of deuterated benzoic acid, including an insulated box, a reactor body, a coil, a stirring mechanism, and a feed hopper. The reactor body is fixedly connected to the upper end of the insulated box. The coil is installed inside the reactor body. An ultra-low temperature medium inlet and an ultra-low temperature medium outlet are fixedly connected to one side wall of the insulated box, respectively. The ends of the ultra-low temperature medium inlet and outlet inside the insulated box are connected to the two ends of the coil. A low temperature medium inlet is provided on the side wall of the insulated box, and a low temperature medium outlet is provided on the other side wall. A stirring mechanism for stirring the materials is installed inside the reactor body, and a feed hopper is provided at the upper end of the reactor body. This utility model can quickly complete cooling and heating after the reaction, greatly improving the reaction rate, efficiency, and yield.

Description

Technical Field

[0001] This utility model relates to the field of chemical equipment technology, specifically to a deuterated benzoic acid synthesis reactor. Background Technology

[0002] The synthesis of deuterated benzoic acid typically employs two mechanisms: synthesis and exchange. However, both methods have significant drawbacks:

[0003] Synthesis method: Most synthesis methods require long-term heating, but long-term heating may lead to hydrogen-deuterium exchange, reducing the deuteration rate of deuterated benzoic acid.

[0004] Exchange method: This method relies on a precious metal catalyst to exchange benzoic acid with heavy water under high temperature and pressure. However, benzoic acid is prone to decarboxylation under high temperature conditions, and the equipment requirements are high, which is not conducive to large-scale production.

[0005] Therefore, existing methods still face challenges in improving deuteration rate and large-scale production, while low-temperature synthesis is a more ideal approach to prepare benzoic acid with high deuteration rate. Utility Model Content

[0006] In view of this, the present invention provides a deuterated benzoic acid synthesis reactor that can quickly complete the cooling and heating after the reaction is completed, which greatly improves the reaction rate, efficiency and yield.

[0007] The technical solution adopted in this utility model is as follows:

[0008] A deuterated benzoic acid synthesis reactor includes an insulation box, a reactor body, a coil, a stirring mechanism, and a feed hopper;

[0009] The upper end of the insulated box is fixedly connected to the reactor body. The reactor body is equipped with a coil. A cryogenic medium inlet and a cryogenic medium outlet are fixedly connected to one side wall of the insulated box. The ends of the cryogenic medium inlet and the cryogenic medium outlet located inside the insulated box are respectively connected to the two ends of the coil. A cryogenic medium inlet is provided on the side wall of the insulated box, and a cryogenic medium outlet is provided on the other side wall of the insulated box. A stirring mechanism for stirring materials is provided inside the reactor body, and a feed hopper is provided at the upper end of the reactor body.

[0010] Furthermore, the stirring mechanism includes a rotating rod rotatably connected to the top of the reactor body, and a stirring blade is fixedly sleeved on the rotating rod. The stirring blade and the rotating rod are located on the central axis of the space enclosed by the coil.

[0011] Furthermore, a motor is fixedly connected to the upper end of the main body of the reactor, and the output shaft of the motor is fixedly connected to the upper end of the rotating rod.

[0012] Furthermore, the upper end of the feed hopper is provided with a cover plate, and the upper end of the cover plate is provided with a first nitrogen inlet, a first nitrogen outlet and a material inlet.

[0013] Furthermore, the upper end of the reactor body is provided with a liquid inlet and a second nitrogen inlet.

[0014] Furthermore, the feed hopper is connected to the reactor body via a butterfly valve, and a discharge valve is provided at the lower end of the reactor body. The lower end of the discharge valve passes through the lower end of the insulation box and extends to its exterior.

[0015] Beneficial effects:

[0016] 1. This utility model, by setting up an insulated box and coils, allows for rapid cooling. When rapid cooling is required, the cryogenic medium is introduced into the coil through the cryogenic medium inlet and then discharged through the cryogenic medium outlet, enabling the cryogenic medium to circulate within the coil. This achieves rapid cooling of the materials inside the reactor body, greatly improving reaction rate, efficiency, and yield, while avoiding side reactions caused by high temperatures (such as decarboxylation and hydrogen-deuterium exchange). After the reaction, the cryogenic medium is introduced into the insulated box through the cryogenic medium inlet, achieving temperature control of the materials from both inside and outside the reactor body. This dual-layer temperature regulation function allows for rapid cooling followed by reheating after the reaction, further improving efficiency.

[0017] 2. This utility model is equipped with a stirring mechanism. During the reaction process, the output shaft of the drive motor rotates, which drives the rotating rod and stirring blades to rotate, stirring the material in the main body of the reactor so that it is in uniform contact with the coil, thereby achieving a better temperature transfer effect.

[0018] 3. This utility model is equipped with a first nitrogen inlet, a first nitrogen outlet and a second nitrogen inlet. Under nitrogen protection, it is more conducive to obtaining a higher yield of deuterated benzoic acid. Attached Figure Description

[0019] Figure 1 This is a three-dimensional view of the overall structure of this utility model.

[0020] Figure 2 This is a bottom-view perspective view of the overall structure of this utility model.

[0021] Figure 3 This is a sectional perspective view of the overall structure of this utility model.

[0022] Figure 4 This is a perspective view of the overall structure of this utility model from another angle.

[0023] Figure 5 for Figure 3 Enlarged view of the structure at point A in the image.

[0024] Among them, 1-insulation box, 2-cryogenic medium outlet, 3-cryogenic medium inlet, 4-reactor body, 5-feed hopper, 6-cryogenic medium inlet, 7-cryogenic medium outlet, 8-first nitrogen outlet, 9-coil, 10-discharge valve, 11-butterfly valve, 12-liquid inlet, 13-second nitrogen inlet, 14-rotating rod, 15-stirring blade, 16-cover plate, 17-motor, 18-first nitrogen inlet. Detailed Implementation

[0025] The present invention will now be described in detail with reference to the accompanying drawings and embodiments.

[0026] This invention provides a reactor for the synthesis of deuterated benzoic acid, such as... Figure 1-4 As shown, it includes an insulation box 1, a reaction vessel body 4, a coil 9, a stirring mechanism, and a feed hopper 5.

[0027] The upper end of the insulated box 1 is fixedly connected to the reactor body 4. A coil 9 is installed inside the reactor body 4. A cryogenic medium inlet 6 and a cryogenic medium outlet 2 are fixedly connected to one side wall of the insulated box 1. The ends of the cryogenic medium inlet 6 and outlet 2 inside the insulated box 1 are respectively connected to the two ends of the coil 9. Specifically, the end of the cryogenic medium inlet 6 inside the insulated box 1 is connected to the upper end of the coil 9, and the end of the cryogenic medium outlet 2 inside the insulated box 1 is connected to the lower end of the coil 9. Alternatively, the end of the cryogenic medium inlet 6 inside the insulated box 1 can also be connected to the lower end of the coil 9, and the end of the cryogenic medium outlet 2 inside the insulated box 1 can be connected to the upper end of the coil 9. A cryogenic medium inlet 3 is provided on the side wall of the insulated box 1, and a cryogenic medium outlet 7 is provided on the other side wall of the insulated box 1.

[0028] The reactor body 4 is equipped with a stirring mechanism for stirring materials. In this embodiment, the stirring mechanism includes a rotating rod 14 rotatably connected to the top of the reactor body 4. A stirring blade 15 is fixedly sleeved on the rotating rod 14. The stirring blade 15 and the rotating rod 14 are located on the central axis of the space enclosed by the coil 9. A motor 17 is fixedly connected to the upper end of the reactor body 4. The output shaft end of the motor 17 is fixedly connected to the upper end of the rotating rod 14.

[0029] A feed hopper 5 is provided at the upper end of the reactor body 4. A liquid inlet 12 and a second nitrogen inlet 13 are also provided at the upper end of the reactor body 4. A cover plate 16 is provided at the upper end of the feed hopper 5. A first nitrogen inlet 18 and a first nitrogen outlet 8 are provided at the upper end of the cover plate 16. Figure 5As shown, the feed hopper 5 is connected to the reactor body 4 via a butterfly valve 11, and a discharge valve 10 is provided at the lower end of the reactor body 4. The lower end of the discharge valve 10 passes through the lower end of the insulation box 1 and extends to its exterior. Nitrogen gas is continuously introduced into the second nitrogen inlet 13 throughout the reaction process, and nitrogen gas is introduced into the first nitrogen inlet 18 when material is added from the feed hopper 5. After nitrogen gas is introduced, the material is rinsed with the solvent 2-methyltetrahydrofuran under nitrogen protection before being added back into the reactor body 4. This facilitates obtaining a higher yield of deuterated benzoic acid.

[0030] In this embodiment, a material inlet is also provided on the cover plate 16 at the upper end of the feed hopper 5. In other embodiments, if a separate material inlet is not provided, the first nitrogen outlet 8 can also be used as a material inlet.

[0031] In use, this invention employs a peristaltic pump to sequentially inject deuterated bromobenzene and 2-methyltetrahydrofuran into the reactor body 4 through the liquid inlet 12. Then, n-butyllithium is introduced through the liquid inlet 12 to form deuterated phenyllithium. Deuterated phenyllithium is chemically reactive and can react with water and carbon dioxide in the air; therefore, nitrogen is introduced through the first nitrogen inlet 18 and the second nitrogen inlet 13 to protect the deuterated phenyllithium. During the synthesis process, nitrogen also effectively prevents the material from rapidly heating up and deteriorating. When rapid cooling is required, a cryogenic medium (temperature range -60 to -80°C) is introduced into the coil 9 through the cryogenic medium inlet 6 and then discharged through the cryogenic medium outlet 2, allowing the cryogenic medium to circulate within the coil 9. This achieves rapid cooling of the material within the reactor body 4, significantly improving reaction rate, efficiency, and yield. Simultaneously, during the reaction, the output shaft of the drive motor 17 rotates, driving the rotating rod 14 and the stirring blades 15 to rotate, stirring the material inside the reactor body 4, ensuring uniform contact with the coil 9, thereby achieving better temperature transfer. When the temperature reaches the required temperature (below -60℃), the cover plate 16 of the feed hopper 5 is opened to add solid dry ice. After closing the cover plate 16, 2-methyltetrahydrofuran is added to the feed hopper 5 through the material inlet on the cover plate 16 for rinsing. After rinsing, the butterfly valve 11 is opened, and solid dry ice enters the reactor body 4. After the reaction is completed, a low-temperature medium (temperature range of 0 to -40℃) is introduced into the insulation box 1 through the low-temperature medium inlet 3, entering the interlayer between the insulation box 1 and the reactor body 4, thereby raising the temperature inside the reactor body 4. This allows for temperature control of the material from both inside and outside the reactor body 4, providing a dual-layer temperature regulation function and enabling rapid heating and cooling.

[0032] In summary, the above are merely preferred embodiments of this utility model and are not intended to limit the scope of protection of this utility model. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this utility model should be included within the scope of protection of this utility model.

Claims

1. A deuterated benzoic acid synthesis reactor, characterized in that, Includes an insulated box, reactor body, coils, stirring mechanism, and feed hopper; The upper end of the insulated box is fixedly connected to the reactor body. The reactor body is equipped with a coil. A cryogenic medium inlet and a cryogenic medium outlet are fixedly connected to one side wall of the insulated box. The ends of the cryogenic medium inlet and the cryogenic medium outlet located inside the insulated box are respectively connected to the two ends of the coil. A cryogenic medium inlet is provided on the side wall of the insulated box, and a cryogenic medium outlet is provided on the other side wall of the insulated box. A stirring mechanism for stirring materials is provided inside the reactor body, and a feed hopper is provided at the upper end of the reactor body.

2. The deuterated benzoic acid synthesis reactor of claim 1, wherein, The stirring mechanism includes a rotating rod rotatably connected to the top of the reactor body, and stirring blades are fixedly sleeved on the rotating rod. The stirring blades and the rotating rod are located on the central axis of the space enclosed by the coil.

3. The deuterated benzoic acid synthesis reactor of claim 2, wherein, A motor is fixedly connected to the upper end of the main body of the reactor, and the output shaft of the motor is fixedly connected to the upper end of the rotating rod.

4. The deuterated benzoic acid synthesis reactor of claim 1, wherein, The upper end of the feed hopper is provided with a cover plate, and the upper end of the cover plate is provided with a first nitrogen inlet, a first nitrogen outlet and a material inlet.

5. The deuterated benzoic acid synthesis reactor of claim 4, wherein, The upper end of the reactor body is provided with a liquid inlet and a second nitrogen inlet.

6. The deuterated benzoic acid synthesis reactor according to any one of claims 1-5, wherein, The feed hopper is connected to the reactor body via a butterfly valve, and a discharge valve is provided at the lower end of the reactor body. The lower end of the discharge valve passes through the lower end of the insulation box and extends to its exterior.

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