Extraction device for preparing 4-iodine-3-methoxypyridine

Abstract

According to the extraction device for preparing the 4-iodine-3-methoxypyridine, mixing and liquid separation are integrated, and meanwhile, centrifugal ultrasound is arranged, so that layering is accelerated; a first stirring unit and a second stirring unit which rotate oppositely are arranged in the mixing unit, the mixing speed is increased, a first conical discharging opening is formed, mixed liquid is automatically discharged into a centrifugal unit, after centrifugation, the mixed liquid is discharged into a standing pipe through a second conical discharging opening, and by detecting the conductivity and combining electromagnetic valves arranged at outlets in a Y-shaped pipe, the mixing speed is increased. And full-automatic liquid separation is realized.

Description

Technical Field

[0001] The utility model belongs to the technical field of 4-iodine-3-methoxypyridine production devices, and specifically relates to an extraction device for preparing 4-iodine-3-methoxypyridine. Background Art

[0002] 4-iodo-3-methoxypyridine is an important intermediate. The iodine at the 4-position can be used for Suzuki coupling with boron reagents, Stille coupling with tin reagents, Sonogashira coupling with alkynes, Heck coupling with olefins, and Ullmann coupling with amines. It is an important raw material for the synthesis of 4-substituted-3-methoxypyridines.

[0003] (3-methoxypyridin-4-yl)boric acid is dissolved in a solvent, and an iodination reagent is added in the presence of a catalyst to react to obtain 4-iodo-3-methoxypyridine. After the reaction is completed, multiple extractions are required, the organic phases are combined, and then further post-processed. Most existing extraction equipment cannot perform batch automatic extraction operations, and a long period of standing is required during liquid separation, which seriously affects production efficiency. Summary of the invention

[0004] In order to solve the above problems, the utility model discloses an extraction device for preparing 4-iodo-3-methoxypyridine.

[0005] In order to achieve the above object, the technical solution of the utility model is as follows:

[0006] An extraction device for preparing 4-iodo-3-methoxypyridine comprises a mixing unit, a centrifugal unit and a static unit which are arranged in sequence from top to bottom, a sealing cover is arranged on the top of the mixing unit, the sealing cover is a hollow structure, a driving gear is arranged at the center of the hollow cavity of the sealing cover, the driving gear is connected to the motor through a rotating shaft, the driving gear meshes with a driven gear, the driven gear meshes with a ring gear inside, avoiding the gear position, the sealing cover is provided with a plurality of feed ports, the feed ports penetrate the sealing cover and are connected to the mixing unit, a plurality of support rods are vertically arranged on the bottom end surface of the ring gear, a plurality of groups of first stirring units are arranged on the support rods along the radial direction of the ring gear, a second stirring unit is arranged between the first stirring units, the second stirring unit is fixedly arranged on the rotating shaft, and the first stirring unit is connected to the second stirring unit. The two stirring units move toward each other, the rotating shaft passes through the sealing cover, the mixing unit and the centrifugal unit, the bottom end of the rotating shaft is arranged at the bottom of the centrifugal unit through a limit block, a plurality of first conical discharge ports are arranged at the bottom of the mixing unit, the first conical discharge ports are connected with the mixing unit and the centrifugal unit, a centrifugal mechanism is arranged in the centrifugal unit, the centrifugal mechanism is fixedly arranged on the rotating shaft, a plurality of centrifugal grooves are evenly arranged on the centrifugal mechanism in an annular direction, a second conical discharge port is arranged at the bottom of the centrifugal groove, a third conical discharge port corresponding to the second conical discharge port is arranged at the bottom of the centrifugal unit, the third conical discharge port is connected with the centrifugal unit and the static unit, a static tube is arranged in the static unit, a liquid dispensing tube is arranged at the bottom of the static tube, the liquid dispensing tube is connected with the Y-type tube, and each outlet in the Y-type tube is provided with a solenoid valve.

[0007] Furthermore, the first conical discharge port and the second conical discharge port are both provided with solenoid valves to realize the automated operation of discharging and feeding, thereby improving efficiency.

[0008] Furthermore, the upper port of the centrifugal trough is of a flared type, and the first conical discharge port is arranged corresponding to the upper port of the centrifugal trough to ensure that the material coming out of the first conical discharge port enters the centrifugal trough after buffering. The centrifugal trough is inclined toward the rotating shaft to facilitate centrifugal stratification.

[0009] Furthermore, the static unit is provided with an ultrasonic device, and an ultrasonic medium is provided around the static tube to accelerate stratification and avoid / break emulsification.

[0010] Furthermore, the upper port of the still tube is of a flared type, and the upper port of the still tube is arranged corresponding to the third conical discharge port, ensuring that the material coming out of the third conical discharge port enters the still tube after buffering. The diameter of the still tube decreases step by step, and support plates are arranged at the locations where the diameter of the still tube changes, so as to increase the stability of the still tube, improve the accuracy of liquid separation, and reduce errors.

[0011] Furthermore, a solenoid valve and a conductivity detection mechanism are provided in the liquid separation tube, and rapid and accurate liquid separation is achieved through conductivity detection in combination with the solenoid valve.

[0012] Furthermore, the sealing cover, the mixing unit, the centrifugal unit and the static unit are connected by bolts, so that the units are sealed and connected, and are detachable, so the practicability is good.

[0013] All the above solenoid valves, conductivity detection mechanisms, motors, and ultrasonic devices are connected by communication and regulated through the control panel, thus realizing automated operation and improving efficiency.

[0014] The beneficial effects of the utility model are:

[0015] The utility model discloses an extraction device for preparing 4-iodo-3-methoxypyridine, which integrates mixing and liquid separation, and is provided with centrifugal ultrasound to accelerate stratification; a first stirring unit and a second stirring unit which rotate in opposite directions are arranged in a mixing unit to accelerate the mixing speed; a first conical discharge port is arranged to automatically discharge the mixed liquid into the centrifugal unit, and after centrifugation, the mixed liquid is discharged into a static tube through a second conical discharge port; and fully automatic liquid separation is realized by detecting conductivity in combination with electromagnetic valves arranged at each outlet in a Y-shaped tube. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 This is a schematic diagram of the three-dimensional structure of the extraction device for preparing 4-iodo-3-methoxypyridine in the utility model;

[0017] Figure 2 This is a schematic diagram of the internal structure of the extraction device for preparing 4-iodo-3-methoxypyridine in the utility model;

[0018] List of Figure Symbols:

[0019] 1. Mixing unit; 2. Centrifugal unit; 3. Standing unit; 4. Sealing cover; 5. Motor; 6. Feed inlet; 7. Rotating shaft; 8. Second stirring unit; 9. First stirring unit; 10. Support rod; 11. Driving gear; 12. Driven gear; 13. Ring gear; 14. First conical discharge port; 15. Centrifugal tank; 16. Second conical discharge port; 17. Third conical discharge port; 18. Standing tube; 19. Support plate; 20. Dispensing tube; 21. Y-type tube; 22. Ultrasonic device. DETAILED DESCRIPTION

[0020] The present invention will be further described below in conjunction with the accompanying drawings and specific implementations. It should be understood that the following specific implementations are only used to illustrate the present invention and are not used to limit the scope of the present invention. Example 1

[0021] An extraction device for preparing 4-iodo-3-methoxypyridine comprises a mixing unit 1, a centrifugal unit 2 and a static unit 3 arranged in sequence from top to bottom, a sealing cover 4 is arranged on the top of the mixing unit 1, the sealing cover 4 is a hollow structure, a driving gear 11 is arranged at the center of the hollow cavity of the sealing cover 4, the driving gear 11 is connected to the motor 5 through a rotating shaft 7, the driving gear 11 meshes with a driven gear 12, the driven gear 12 is internally meshed with a ring gear 13, avoiding the gear position, and the sealing cover 4 is provided with a plurality of feed ports 6, the feed ports 6 penetrate the sealing cover 4 and are connected to the mixing unit 1. Element 1, a plurality of support rods 10 are vertically arranged on the bottom end surface of the ring gear 13, a plurality of first stirring units 9 are arranged on the support rods 10 along the radial direction of the ring gear 13, a second stirring unit 8 is arranged between the first stirring units 9, the second stirring unit 8 is fixedly arranged on the rotating shaft 7, the first stirring unit and the second stirring unit 8 move towards each other, the rotating shaft 7 passes through the sealing cover 4, the mixing unit 1, and the centrifugal unit 2, the bottom end of the rotating shaft 7 is arranged at the bottom of the centrifugal unit 2 through a limit block, a plurality of first conical discharge ports 14 are arranged at the bottom of the mixing unit 1, and the first conical discharge ports 14 are connected to the first conical discharge ports 14. The mixing unit 1 and the centrifugal unit 2 are provided with a centrifugal mechanism in the centrifugal unit 2, the centrifugal mechanism is fixedly arranged on the rotating shaft 7, a plurality of centrifugal grooves 15 are evenly arranged in the annular direction on the centrifugal mechanism, the upper end of the centrifugal groove 15 is a flared type, the first conical discharge port 14 is arranged corresponding to the upper end of the centrifugal groove 15, the centrifugal groove 15 is inclined to the rotating shaft 7, the second conical discharge port 16 is arranged at the bottom of the centrifugal groove 15, the third conical discharge port 17 corresponding to the second conical discharge port 16 is arranged at the bottom of the centrifugal unit 2, and the third conical discharge port 17 connects the centrifugal unit 2 and the stationary unit Element 3, a stationary tube 18 is arranged in the stationary unit 3, an ultrasonic device 22 is arranged in the stationary unit 3, an ultrasonic medium is arranged around the stationary tube 18, a liquid separator 20 is arranged at the bottom of the stationary tube 18, the upper end of the stationary tube 18 is a flared type, the upper end of the stationary tube 18 is arranged corresponding to the third conical discharge port 17, the diameter of the stationary tube 18 decreases step by step, a support plate 19 is arranged at each place where the diameter of the stationary tube 18 changes, the liquid separator 20 is connected to the Y-type tube 21, each outlet in the Y-type tube 21 is provided with a solenoid valve, and a solenoid valve and a conductivity detection mechanism are arranged in the liquid separator 20. The first conical discharge port 14 and the second conical discharge port 16 are both provided with a solenoid valve; the connection between the sealing cover 4, the mixing unit 1, the centrifugal unit 2 and the stationary unit 3 is connected by bolts, and each unit is sealed; all solenoid valves, conductivity detection mechanisms, motors 5, and ultrasonic devices 22 are connected in communication and regulated through the control panel.

[0022] Working principle: the reaction liquid and extraction solvent for preparing 4-iodo-3-methoxypyridine are added to the mixing unit 1 through the feed port 6, the motor 5 is started, and after uniform stirring, the electromagnetic valve of the first conical discharge port 14 is opened and enters the centrifugal unit 2, and the next batch of reaction liquid and extraction solvent are added to the mixing unit 1. After centrifugation, the liquid enters the static tube 18 through the second conical discharge port 16 and the third conical discharge port 17 for static stratification, and then is separated by the conductivity detection mechanism.

[0023] As a more preferred embodiment of the present invention, two or more still pipes 18 are provided in the still unit 3, and the third conical discharge port 17 and the still pipes 18 are connected via a multi-way valve to allow the liquid to be stilled in turn.

[0024] It should be noted that the above content only illustrates the technical idea of ​​the utility model and cannot be used to limit the protection scope of the utility model. For ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the utility model. These improvements and modifications all fall within the protection scope of the claims of the utility model.

Claims

1. An extraction device for preparing 4-iodo-3-methoxypyridine, characterized in that: The invention comprises a mixing unit, a centrifugal unit and a static unit which are arranged in sequence from top to bottom, a sealing cover is arranged on the top of the mixing unit, the sealing cover is a hollow structure, a driving gear is arranged at the center of the hollow cavity of the sealing cover, the driving gear is connected to the motor through a rotating shaft, the driving gear meshes with a driven gear, the driven gear meshes with a ring gear inside, avoiding the gear position, a plurality of feed ports are arranged on the sealing cover, the feed ports penetrate the sealing cover and connect to the mixing unit, a plurality of support rods are vertically arranged on the bottom end surface of the ring gear, a plurality of groups of first stirring units are arranged on the support rods along the radial direction of the ring gear, a second stirring unit is arranged between the first stirring units, the second stirring unit is fixedly arranged on the rotating shaft, and the first stirring unit and the second stirring unit are connected The units move toward each other, the rotating shaft passes through the sealing cover, the mixing unit and the centrifugal unit, the bottom end of the rotating shaft is arranged at the bottom of the centrifugal unit through a limit block, a plurality of first conical discharge ports are arranged at the bottom of the mixing unit, the first conical discharge ports are connected with the mixing unit and the centrifugal unit, a centrifugal mechanism is arranged in the centrifugal unit, the centrifugal mechanism is fixedly arranged on the rotating shaft, a plurality of centrifugal grooves are evenly arranged in an annular direction on the centrifugal mechanism, a second conical discharge port is arranged at the bottom of the centrifugal groove, a third conical discharge port corresponding to the second conical discharge port is arranged at the bottom of the centrifugal unit, the third conical discharge port is connected with the centrifugal unit and the static unit, a static tube is arranged in the static unit, a liquid dispensing tube is arranged at the bottom of the static tube, and the liquid dispensing tube is connected with the Y-shaped tube.

2. An extraction device for preparing 4-iodo-3-methoxypyridine according to claim 1, characterized in that: The first conical discharge port and the second conical discharge port are both provided with solenoid valves.

3. An extraction device for preparing 4-iodo-3-methoxypyridine according to claim 1, characterized in that: The upper port of the centrifugal trough is of a flared type, the first conical discharge port is arranged corresponding to the upper port of the centrifugal trough, and the centrifugal trough is arranged inclined toward the rotating shaft.

4. An extraction device for preparing 4-iodo-3-methoxypyridine according to claim 1, characterized in that: The stationary unit is provided with an ultrasonic device, and an ultrasonic medium is provided around the stationary tube.

5. An extraction device for preparing 4-iodo-3-methoxypyridine according to claim 1, characterized in that: The upper port of the stationary pipe is of a flared type, and the upper port of the stationary pipe is arranged corresponding to the third conical discharge port. The diameter of the stationary pipe decreases step by step, and support plates are arranged at the locations where the diameter of the stationary pipe changes.

6. An extraction device for preparing 4-iodo-3-methoxypyridine according to claim 1, characterized in that: A solenoid valve and a conductivity detection mechanism are arranged in the liquid dispensing tube.

7. An extraction device for preparing 4-iodo-3-methoxypyridine according to claim 1, characterized in that: The sealing cover, the mixing unit, the centrifugal unit and the static unit are connected by bolts.

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