CN216063207U

CN216063207U - Cyclization reaction kettle for synthesizing 1, 2-cyclopentanedicarboximide

Info

Publication number: CN216063207U
Application number: CN202120319111.4U
Authority: CN
Inventors: 蒋爱萍; 张义文
Original assignee: Anhui Jinding Pharmaceutical Co ltd
Current assignee: Anhui Jinding Pharmaceutical Co ltd
Priority date: 2021-02-04
Filing date: 2021-02-04
Publication date: 2022-03-18
Anticipated expiration: 2031-02-04

Abstract

The utility model provides a cyclization reaction kettle for synthesizing 1, 2-cyclopentanedicarboximide, and relates to the technical field of synthesis reaction equipment. This ring closure reation kettle includes the cauldron body, and the inner chamber top of the cauldron body is equipped with reaction chamber, and the inner chamber below is equipped with the layering and filters the cavity, and reaction chamber and layering filter and separate through the division board between the cavity, are equipped with in the reaction chamber and stir the first rabbling mechanism of reaction to reaction liquid, and the layering filters the intracavity and is equipped with the second rabbling mechanism that stirs the layering to reaction liquid, and the top of the cauldron body is equipped with the feed inlet, and the bottom of the cauldron body is equipped with the bin outlet. According to the utility model, the first stirring mechanism is used for realizing the full dispersion and contact of the raw materials and the solvent, the reaction rate is improved, the second stirring mechanism is used for realizing the rapid separation and layering of oil and water, the layered filtering chamber is used for filtering, deodorizing and removing impurities from the reaction liquid, the content of the 1, 2-cyclopentanedicarboximide in the oil phase is increased, and the yield of the post-treated pure product is improved.

Description

Cyclization reaction kettle for synthesizing 1, 2-cyclopentanedicarboximide

Technical Field

The utility model relates to the technical field of synthesis reaction equipment, in particular to a cyclization reaction kettle for synthesizing 1, 2-cyclopentanedicarboximide.

Background

1, 2-cyclopentanedicarboximide is an important intermediate for preparing gliclazide, and a synthesis process reported at present uses 1, 2-cyclopentanedicarboxamide as a raw material, and is characterized by directly heating and cyclizing in a solvent, layering while hot, decoloring the upper layer in water, crystallizing to obtain a crude product, and recrystallizing in a crystallization solvent to obtain high-purity 1, 2-cyclopentanedicarboximide. The process has mild reaction conditions, high-temperature carbonization prevention, no distillation, good product quality and high yield. The existing cyclization reaction kettle for synthesizing 1, 2-cyclopentanedicarboximide cannot promote the full contact of raw materials and a solvent, and is filtered to remove impurities so as to further improve the yield of a pure product.

SUMMERY OF THE UTILITY MODEL

Aiming at the defects of the prior art, the utility model provides a cyclization reaction kettle for synthesizing 1, 2-cyclopentanedicarboximide.

The utility model solves the technical problems through the following technical means:

1, 2-cyclopentanedioic imide is synthetic with cyclization reation kettle, including the cauldron body, the inner chamber top of the cauldron body is equipped with reaction chamber, and the inner chamber below is equipped with the layering and filters the cavity, and reaction chamber and layering filter to separate through the division board between the cavity, are equipped with the first rabbling mechanism that stirs the reaction to the reaction liquid in the reaction chamber, and the layering filters the intracavity and is equipped with the second rabbling mechanism that stirs the layering to the reaction liquid, and the top of the cauldron body is equipped with the feed inlet, and the bottom of the cauldron body is equipped with the bin outlet.

As a further scheme of the utility model, the first stirring mechanism comprises a first brushless motor and a first stirring shaft, the first brushless motor is arranged at the top of the kettle body, the first stirring shaft vertically extends downwards into the reaction chamber through a first coupler connected with the first brushless motor, and a stirring frame is arranged on the periphery of the bottom of the first stirring shaft.

As a further scheme of the utility model, the second stirring mechanism comprises a second brushless motor and a second stirring shaft, the second brushless motor is arranged at the bottom of the kettle body, the second stirring shaft vertically extends upwards into the layered filtering chamber through a second coupler connected with the second brushless motor, and a plurality of stirring blades are arranged on the periphery of the second stirring shaft.

As a further scheme of the utility model, the side wall of the top of the reaction chamber is provided with an air inlet and an air outlet, and the air outlet is connected with a water tank through an exhaust pipe.

As a further scheme of the utility model, the periphery of the reaction chamber is wrapped by a jacket, and a circulating pipe for introducing heat-conducting oil is wound in the jacket.

As a further scheme of the utility model, the bottom of the partition plate is provided with a discharge valve.

As a further scheme of the utility model, a filter plate is arranged below the layered filtering chamber, a through hole for the second stirring shaft to pass through is arranged in the center of the filter plate, a plurality of sieve pores are arranged in the filter plate in a vertically penetrating manner, and activated carbon is filled in the sieve pores.

The utility model has the beneficial effects that:

according to the cyclization reaction kettle for synthesis, the first stirring mechanism is used for realizing full dispersion and contact of raw materials and a solvent, the reaction speed is improved, the second stirring mechanism is used for realizing rapid oil-water separation and layering, the layered filtering chamber is used for filtering, deodorizing and removing impurities from a reaction liquid, the content of the product 1, 2-cyclopentanedioic imide in an oil phase is increased, and the yield of a pure product after post-treatment is improved.

Drawings

FIG. 1 is a schematic structural diagram of a cyclization reaction kettle for synthesizing 1, 2-cyclopentanedicarboximide according to the utility model;

FIG. 2 is a schematic view of the filter plate of the present invention.

In the figure: 1. a kettle body; 2. a first stirring mechanism; 3. a second stirring mechanism; 4. a water tank; 5. a filter plate; 11. a reaction chamber; 12. a layered filtration chamber; 13. a partition plate; 14. a feed inlet; 15. a discharge outlet; 16. an air inlet; 17. an exhaust port; 18. an exhaust pipe; 19. a jacket; 20. a circulation pipe; 21. a first brushless motor; 22. a first stirring shaft; 23. a first coupling; 24. a stirring frame; 25. a discharge valve; 31. a second brushless motor; 32. a second stirring shaft; 33. a second coupling; 34. a stirring blade; 51. a through hole; 52. and (4) screening holes.

Detailed Description

In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present.

Examples

As shown in fig. 1, the cyclization reaction kettle for synthesizing 1, 2-cyclopentanedicarboximide of the present embodiment includes a kettle body 1, a reaction chamber 11 is disposed above an inner cavity of the kettle body 1, a layered filtering chamber 12 is disposed below the inner cavity, the reaction chamber 11 and the layered filtering chamber 12 are separated by a partition plate 13, a first stirring mechanism 2 for stirring and reacting a reaction liquid is disposed in the reaction chamber 11, a second stirring mechanism 3 for stirring and layering the reaction liquid is disposed in the layered filtering chamber 12, a feed inlet 14 is disposed at the top of the kettle body 1, and a discharge outlet 15 is disposed at the bottom of the kettle body 1.

In the cyclization reaction kettle for synthesizing 1, 2-cyclopentanedicarboximide in the embodiment, a reaction chamber 11 is arranged above an inner cavity of a kettle body 1, a layered filtering chamber 12 is arranged below the inner cavity, a reaction liquid composed of raw materials 1, 2-cyclopentanedicarboxamide and solvent dimethylsilicone oil is stirred and reacted through a first stirring mechanism 2, a second stirring mechanism 3 is used for stirring the completely reacted reaction liquid and standing for layering, a lower oil layer and an upper water layer are formed after water is added, the oil layer is discharged from a discharge port 15 after being filtered to obtain a crude product solution of 1, 2-cyclopentanedicarboximide, the cyclization reaction kettle realizes full dispersion and contact of the raw materials and the solvent through the first stirring mechanism 2, the reaction rate is improved, oil-water quick separation and layering are realized through the second stirring mechanism 3, the layered filtering chamber 12 is used for filtering, deodorizing and removing impurities from the reaction liquid, the content of the product 1, 2-cyclopentanedicarboximide in the oil phase is increased, and the yield of the pure product after the post-treatment is improved.

First rabbling mechanism 2 includes first brushless motor 21, first (mixing) shaft 22, and first brushless motor 21 locates the top of the cauldron body 1, and in first (mixing) shaft 22 stretched into reaction chamber 11 through the vertical downward of first shaft coupling 23 of being connected with first brushless motor 21, the bottom periphery of first (mixing) shaft 22 was equipped with stirring frame 24. The first brushless motor 21 drives the first stirring shaft 22 and the stirring frame 24 to rotate through the first coupler 23, and stirs the reaction solution, so that the raw material and the solvent are fully mixed.

The second stirring mechanism 3 comprises a second brushless motor 31 and a second stirring shaft 32, the second brushless motor 31 is arranged at the bottom of the kettle body 1, the second stirring shaft 32 vertically extends upwards into the layered filtering chamber 12 through a second coupler 33 connected with the second brushless motor 31, and a plurality of stirring blades 34 are arranged on the periphery of the second stirring shaft 32. The second brushless motor 31 drives the second stirring shaft 32 and the stirring blade 34 to rotate through the second coupler 33, and the reaction solution after the water is added is stirred, so that the product fully enters the oil phase.

The side wall of the top of the reaction chamber 11 is provided with an air inlet 16 and an air outlet 17, the air outlet 17 is connected with the water tank 4 through an exhaust pipe 18, and water or alkali liquor is contained in the water tank 4. The air inlet 16 is used for introducing nitrogen to replace air in the reaction chamber 11 before reaction and discharging the nitrogen from the air outlet 17, and ammonia gas generated in the reaction process enters the water tank 4 through the exhaust pipe 18 to be absorbed so as to promote the forward progress of the reaction.

The periphery of the reaction chamber 11 is wrapped with a jacket 19, and a circulation pipe 20 for introducing heat-conducting oil is wound in the jacket 19. After the heat conducting oil is introduced into the circulating pipe 20, the jacket 19 plays a good role in heat preservation, and promotes the temperature rise and heat preservation of the reaction liquid in the reaction chamber 11.

The bottom of the partition plate 13 is provided with a discharge valve 25.

A filter plate 5 is arranged below the layered filtering chamber 12, as shown in fig. 2, a through hole 51 for the second stirring shaft 32 to pass through is arranged in the center of the filter plate 5, a plurality of sieve holes 52 are arranged in the filter plate 5 in an up-and-down penetrating manner, and activated carbon is filled in the sieve holes 52. The activated carbon in the sieve pores 52 adsorbs impurities in the reaction solution, and the extraction efficiency of the post-treatment is improved.

The cyclization reaction kettle for synthesizing 1, 2-cyclopentanedicarboximide in the embodiment has the following working method:

a) introducing nitrogen from an air inlet 16, replacing air in the reaction chamber 11, then discharging the air from an air outlet 17, adding 1, 2-cyclopentadipamide and a solvent simethicone from a feed inlet 14, introducing heat conduction oil at 240-260 ℃ into a circulating pipe 20, heating and heating reaction liquid, driving a first stirring shaft 22 and a stirring frame 24 to rotate by a first brushless motor 21 through a first coupler 23, stirring the reaction liquid, fully mixing the raw materials and the solvent, and allowing ammonia gas generated in the reaction process to enter a water tank 4 from an exhaust pipe 18 to be absorbed;

b) and (3) opening the discharge valve 25, allowing the reaction liquid to enter the layered filtering chamber 12, adding a proper amount of water, driving the second stirring shaft 32 and the stirring blade 34 to rotate by the second brushless motor 31 through the second coupler 33, stirring the reaction liquid after adding the water, standing for layering, filtering the lower oil layer by activated carbon in the sieve pores 52, and discharging the filtered lower oil layer from the discharge port 15 to obtain a crude 1, 2-cyclopentadienimide solution.

It is noted that, in this document, relational terms such as first and second, and the like, if any, are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.

The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims

1.1, 2-synthetic cyclization reation kettle that uses of cyclopentanedicarbonyl imine, including the cauldron body (1), its characterized in that, the inner chamber top of the cauldron body (1) is equipped with reaction chamber (11), the inner chamber below is equipped with layering filter chamber (12), separate through division board (13) between reaction chamber (11) and the layering filter chamber (12), be equipped with in reaction chamber (11) and stir first rabbling mechanism (2) of reaction to the reaction liquid, be equipped with in layering filter chamber (12) and stir second rabbling mechanism (3) of layering to the reaction liquid, the top of the cauldron body (1) is equipped with feed inlet (14), the bottom of the cauldron body (1) is equipped with bin outlet (15).

2. The cyclization reaction kettle for synthesizing 1, 2-cyclopentanedicarboximide according to claim 1, wherein the first stirring mechanism (2) comprises a first brushless motor (21) and a first stirring shaft (22), the first brushless motor (21) is arranged at the top of the kettle body (1), the first stirring shaft (22) vertically extends downwards into the reaction chamber (11) through a first coupling (23) connected with the first brushless motor (21), and a stirring frame (24) is arranged on the periphery of the bottom of the first stirring shaft (22).

3. The cyclization reaction kettle for synthesizing 1, 2-cyclopentanedicarboximide according to claim 1, characterized in that the second stirring mechanism (3) comprises a second brushless motor (31) and a second stirring shaft (32), the second brushless motor (31) is arranged at the bottom of the kettle body (1), the second stirring shaft (32) vertically extends upwards into the layered filtering chamber (12) through a second coupling (33) connected with the second brushless motor (31), and the periphery of the second stirring shaft (32) is provided with a plurality of stirring blades (34).

4. The cyclization reaction kettle for synthesizing 1, 2-cyclopentanedicarboximide according to claim 1, characterized in that the side wall of the top of the reaction chamber (11) is provided with an air inlet (16) and an air outlet (17), and the air outlet (17) is connected with the water tank (4) through an air outlet pipe (18).

5. The cyclization reaction kettle for synthesizing 1, 2-cyclopentanedicarboximide according to claim 4, wherein the periphery of the reaction chamber (11) is wrapped by a jacket (19), and a circulating pipe (20) for introducing heat-conducting oil is wound in the jacket (19).

6. The cyclization reaction kettle for synthesizing 1, 2-cyclopentanedicarboximide according to claim 1, wherein a discharge valve (25) is provided at the bottom of the partition plate (13).

7. The cyclization reaction kettle for synthesizing 1, 2-cyclopentanedicarboximide according to claim 1, wherein a filter plate (5) is arranged below the layered filtering chamber (12), a through hole (51) for passing the second stirring shaft (32) is arranged in the center of the filter plate (5), a plurality of sieve holes (52) are arranged in the upper and lower parts of the filter plate (5), and activated carbon is filled in the sieve holes (52).