A crystallization system for amide acetal preparation

Abstract

The utility model relates to a kind of crystallization systems for amide acetal preparation, comprising: reaction tank, including reaction tank body, the reaction tank body has first internal chamber;Filtering tank, including filtering tank body, the filtering tank body has second internal chamber, the first internal chamber of reaction tank body and the second internal chamber of filtering tank body are communicated by first communication pipeline;Crystallization tank, including crystallization tank body, crystallization tank body has third internal chamber, the second internal chamber of filtering tank body and the third internal chamber of crystallization tank body are communicated by second communication pipeline;The second internal chamber of the filtering tank is provided with the first filter tube of preset quantity, the second filter tube of preset quantity, the first filter tube is communicated with the second filter tube, preset quantity is provided on the first filter tube first liquid hole, preset quantity is provided on the second filter tube second liquid hole;The first filter tube and the second filter tube are filled with activated carbon.

Description

Technical Field

[0001] This utility model relates to the field of chemical reaction machinery and equipment, specifically to a crystallization system for the preparation of amide acetal. Background Technology

[0002] The amide acetal reaction is a type of organic transformation reaction in which aldehydes react with amides (usually formamide or dimethylformamide) under acidic conditions to produce acetals or imine salt intermediates. This reaction has important applications in drug synthesis, natural product protecting strategies, and heterocycle construction. In the preparation of amide acetals, a catalyst is added to difluorobenzoic acid and dichloroacetaldehyde acetal condensate to carry out a condensation reaction. In one existing technology, the reaction vessel is directly connected to a crystallization vessel; after the catalyst is added to difluorobenzoic acid and dichloroacetaldehyde acetal condensate, the condensation reaction occurs in the reaction vessel, and the resulting product flows directly into the crystallization vessel for crystallization. This preparation method and system have low overall yield, low content of effective components, and the crystallized product contains a large amount of impurities and colored substances.

[0003] Therefore, there is a need for a crystallization system for the preparation of amide acetals that can effectively remove impurities, has a high total yield, and a high content of active ingredients. Summary of the Invention

[0004] The purpose of this invention is to address the shortcomings of existing technologies by proposing a crystallization system for the preparation of amide acetals.

[0005] To achieve the above objectives, the present invention adopts the following technical solution: a crystallization system for preparing amide acetals, comprising: A reaction vessel, the reaction vessel including a reaction vessel body having a first internal chamber; A filter tank, the filter tank including a filter tank body, the filter tank body having a second internal chamber, and the first internal chamber of the reaction tank body and the second internal chamber of the filter tank body being connected through a first connecting pipe; A crystallization tank includes a crystallization tank body having a third internal chamber. A second internal chamber of a filtration tank body is connected to the third internal chamber of the crystallization tank body via a second connecting pipe. The second internal chamber of the filtration tank body contains a predetermined number of first filter tubes and a predetermined number of second filter tubes. The first filter tubes are connected to the second filter tubes. The first filter tubes have a predetermined number of first liquid holes, and the second filter tubes have a predetermined number of second liquid holes. Both the first and second filter tubes are filled with activated carbon.

[0006] Preferably, the reaction vessel further includes a first feeding channel, a second feeding channel, and a catalyst channel. The first feeding channel, the second feeding channel, and the catalyst channel are all disposed on the reaction vessel body, and the first feeding channel, the second feeding channel, and the catalyst channel are all connected to the first internal chamber of the reaction vessel body.

[0007] Preferably, the reaction vessel further includes a first drive motor and a first rotating rod, the first rotating rod being connected to the first drive motor so that the first drive motor drives the first rotating rod to rotate; a first stirring rod is also installed on the first rotating rod, the first stirring rod being disposed in the first internal chamber of the reaction vessel body.

[0008] Preferably, a first outflow pipe is provided on the bottom region of the reaction vessel body, and the first outflow pipe is connected to the first internal chamber of the reaction vessel body; the first connecting pipe is connected to and communicates with the first outflow pipe.

[0009] Preferably, the filter canister further includes a second drive motor, a reducer, and a second rotating rod. The second drive motor is connected to the reducer, and the reducer is connected to the second rotating rod, so that the second drive motor drives the second rotating rod to rotate. A second stirring rod and a third stirring rod are mounted on the second rotating rod, with the second stirring rod located above the third stirring rod, so that when the second rotating rod rotates, it drives the second stirring rod and the third stirring rod to rotate. Both the second stirring rod and the third stirring rod are disposed in the second internal cavity of the filter canister body.

[0010] Preferably, the filter tank further includes a first inflow pipe, a transfer cylinder, and a predetermined number of outflow capillary tubes. The first inflow pipe is connected to the transfer cylinder, and the outflow capillary tubes are connected to the transfer cylinder. The first inflow pipe is connected to the first internal chamber of the reaction tank body. The transfer cylinder and the outflow capillary tubes are both located in the second internal chamber of the filter tank body.

[0011] Preferably, the transfer cylinder is provided with a rotating through hole, the rotating through hole is through the transfer cylinder, and the diameter of the rotating through hole is larger than the diameter of the second rotating rod. The second rotating rod passes through the rotating through hole, so that the second rotating rod can rotate in the rotating through hole of the transfer cylinder.

[0012] Preferably, the filter tank further includes a second outflow pipe, which is connected to the second filter tube; the crystallization tank further includes a second inflow pipe and a third outflow pipe, the second inflow pipe being disposed at the top of the crystallization tank body and connected to the third internal chamber of the crystallization tank body; the third outflow pipe being disposed at the bottom of the crystallization tank body and connected to the third internal chamber of the crystallization tank body; the second outflow pipe and the second inflow pipe are connected through a second connecting pipe.

[0013] The working principle of this application is as follows: The substances participating in the amide acetal reaction enter the first internal chamber of the reaction vessel through the first feeding channel, the second feeding channel, and the catalyst channel. After being stirred by the first stirring rod in the reaction vessel, the generated substances flow into the second internal chamber of the filter vessel. The bottom of the second internal chamber is equipped with a first filter tube and a second filter tube, both filled with activated carbon. The generated substances flow into the first and second filter tubes, and after being filtered by the activated carbon, they flow into the crystallization tank for crystallization. A second stirring rod and a third stirring rod are installed in the second internal chamber of the filter vessel. The stirring by the second and third stirring rods makes the generated substances more uniformly mixed, which is beneficial for activated carbon filtration.

[0014] The beneficial effects of this application are: the crystallization system for the preparation of amide acetal provided by this application has the advantages of simple structure and easy assembly. Since a filter tank is set between the reaction tank and the crystallization tank, the substance generated in the reaction tank flows into the filter tank. After being filtered by activated carbon in the first filter tube and the second filter tube, the impurities and color of the generated substance are effectively removed. The substance with removed impurities and color flows into the crystallization tank for crystallization, thereby greatly improving the overall efficiency and the purity of the crystallized substance. Attached Figure Description

[0015] Figure 1 This is a schematic diagram of the structure of a crystallization system for preparing amide acetal provided by this utility model.

[0016] Figure 2 A schematic diagram of the reaction vessel of a crystallization system for the preparation of amide acetal provided by this utility model.

[0017] Figure 3 Another schematic diagram of the reaction vessel for a crystallization system for preparing amide acetal provided by this utility model.

[0018] Figure 4 A schematic diagram of the structure of a filter tank for a crystallization system for preparing amide acetal provided by this utility model.

[0019] Figure 5Another schematic diagram of the filter tank of a crystallization system for preparing amide acetal provided by this utility model. Detailed Implementation

[0020] The present application will now be described in further detail with reference to the accompanying drawings and specific embodiments. Similar elements in different embodiments are referred to by related similar element reference numerals. In the following embodiments, many details are described to facilitate a better understanding of the present application. However, those skilled in the art will readily recognize that some features may be omitted in different situations, or may be replaced by other elements, materials, or methods. In some cases, certain operations related to the present application are not shown or described in the specification. This is to avoid obscuring the core parts of the present application with excessive description. For those skilled in the art, detailed description of these related operations is not necessary; they can fully understand the related operations based on the description in the specification and general technical knowledge in the art.

[0021] Furthermore, the features, operations, or characteristics described in the specification can be combined in any suitable manner to form various embodiments, and the operational steps involved in each embodiment can also be rearranged or adjusted in a manner that is obvious to those skilled in the art. Therefore, the specification and drawings are only for clearly describing a particular embodiment and do not imply that they represent the necessary components and / or order.

[0022] The serial numbers assigned to components in this document, such as "first" and "second," are used only to distinguish the objects being described and have no sequential or technical meaning. Unless otherwise specified, the terms "connection" and "linkage" used in this application include both direct and indirect connections (linkages).

[0023] Please refer to Figure 1-5 This application provides a crystallization system for the preparation of amide acetals (hereinafter referred to as "the crystallization system"), the crystallization system comprising: The reaction vessel 1 includes a reaction vessel body 11, which has a first internal chamber 110. The filter tank 2, the filter tank 1 includes a filter tank body 21, the filter tank body 21 has a second internal chamber 210, the first internal chamber 110 of the reaction tank body 11 and the second internal chamber 210 of the filter tank body 21 are connected by a first connecting pipe 4. The crystallization tank 3 includes a crystallization tank body 32, which has a third internal chamber 320. The second internal chamber 210 of the filter tank body 21 is connected to the third internal chamber 320 of the crystallization tank body 32 via a second connecting pipe 5. The second internal chamber 210 of the filter tank 2 is provided with a predetermined number of first filter tubes 211 and a predetermined number of second filter tubes 212. The first filter tubes 211 and the second filter tubes 212 are connected. The first filter tubes 211 are provided with a predetermined number of first liquid holes 2110, and the second filter tubes 212 are provided with a predetermined number of second liquid holes 2120. Both the first filter tubes 211 and the second filter tubes 212 are filled with activated carbon. Thus, the substance after the amide acetal reaction in reaction tank 1 flows into filter tank 2 through the first connecting pipe 4, and then enters the first filter tube 211 and the second filter tube 212. After being adsorbed by the activated carbon in the first filter tube 211 and the second filter tube 212, the substance is removed of impurities and color, and then flows into the crystallization tank for crystallization.

[0024] In some embodiments of this application, please refer to Figure 1-5 The reaction vessel 1 further includes a first feeding channel 13, a second feeding channel 14, and a catalyst channel 15. The first feeding channel 13, the second feeding channel 14, and the catalyst channel 15 are all disposed on the reaction vessel body 11, and all three are in communication with the first internal chamber 110 of the reaction vessel body 11. In this application, the first feeding channel 13, the second feeding channel 14, and the catalyst channel 15 are all sealed when not in use and can be opened when in use. The first feeding channel 13 is used to add difluorobenzoic acid, the second feeding channel 14 is used to add chloroacetaldehyde dimethyl acetal, and the catalyst channel 15 is used to add a catalyst.

[0025] In some embodiments of this application, please refer to Figure 1-5 The reaction vessel 1 further includes a first drive motor 12 and a first rotating rod 16. The first rotating rod 16 is connected to the first drive motor 12, thereby causing the first drive motor 12 to drive the first rotating rod 16 to rotate. A first stirring rod 17 is also installed on the first rotating rod 16, and the first stirring rod 17 is disposed in the first internal chamber 110 of the reaction vessel body 11. In this way, the substances required for the amide acetal reaction are added to the first internal chamber 110 of the reaction vessel body 11 through the first feeding channel 13 and the second feeding channel 14. The first drive motor 12 starts working, driving the first stirring rod 17 to rotate, thereby mixing the substances and accelerating the amide acetal reaction.

[0026] In some embodiments of this application, please refer to Figure 1-5 A first outflow pipe 18 is provided on the bottom region of the reaction vessel body 11, and the first outflow pipe 18 is connected to the first internal chamber 110 of the reaction vessel body 11; the first connecting pipe 4 is connected to and communicates with the first outflow pipe 18. In this way, the substance after the amide acetal reaction in the first internal chamber 110 of the reaction vessel body 11 first flows into the first outflow pipe 18, then flows out from the first outflow pipe 18 and flows into the first connecting pipe 4, and then flows into the filter tank 2.

[0027] In some embodiments of this application, please refer to Figure 1-5 The filter tank 2 further includes a second drive motor 22, a reducer 23, and a second rotating rod 24. The second drive motor 22 is connected to the reducer 23, and the reducer 23 is connected to the second rotating rod 24, thereby causing the second drive motor 22 to drive the second rotating rod 24 to rotate. A second stirring rod 29 and a third stirring rod 213 are mounted on the second rotating rod 24. The second stirring rod 29 is located above the third stirring rod 213, so that when the second rotating rod 24 rotates, it drives the second stirring rod 29 and the third stirring rod 213 to rotate. The second stirring rod 29 and the third stirring rod 213 are both disposed in the second internal chamber 210 of the filter tank body 21. First, those skilled in the art should understand that the main purpose of the reducer 23 in this application is to convert the high speed of the second drive motor 22 into a low speed. Therefore, the reducer 23 in this application is a known technology, and any reducer that can convert high speed into low speed is part of the solution of this application. Secondly, the arrangement of the second stirring rod 29 and the third stirring rod 213 allows the substances from the amide acetal reaction to be stirred after flowing into the second internal chamber 210 of the filter tank body 21, which makes the subsequent filtration more thorough and efficient.

[0028] In some embodiments of this application, please refer to Figure 1-5The filter tank 2 further includes a first inflow pipe 27, a transfer cylinder 26, and a predetermined number of outflow capillary tubes 28. The first inflow pipe 27 is connected to the transfer cylinder 26, and the outflow capillary tubes 28 are connected to the transfer cylinder 26. The first inflow pipe 27 is connected to the first internal chamber 110 of the reaction tank body 11. The transfer cylinder 26 and the outflow capillary tubes 28 are both located in the second internal chamber 210 of the filter tank body 21. In this way, the substance flowing out from the first outflow pipe 18 on the reaction tank body 1 enters the first connecting pipe 4, which is connected to the first inflow pipe 27. This allows the substance after the amide acetal reaction to flow into the first inflow pipe 27, then into the transfer cylinder 26, and then outflow from the outflow capillary tubes 28 into the second internal chamber 210 of the filter tank body 21.

[0029] In some embodiments of this application, please refer to Figure 1-5 The transfer cylinder 26 is provided with a rotating through hole 260, which extends through the transfer cylinder 26 and has a diameter larger than that of the second rotating rod 24. The second rotating rod 24 passes through the rotating through hole 260, thereby enabling the second rotating rod 24 to rotate within the rotating through hole 260 of the transfer cylinder 26.

[0030] In some embodiments of this application, please refer to Figure 1-5 The filter tank 2 further includes a second outflow pipe 25, which is connected to the second filter tube 212. The crystallization tank 3 further includes a second inflow pipe 31 and a third outflow pipe 33. The second inflow pipe 31 is located at the top of the crystallization tank body 32 and is connected to the third internal chamber 320 of the crystallization tank body 32. The third outflow pipe 33 is located at the bottom of the crystallization tank body 32 and is connected to the third internal chamber 320 of the crystallization tank body 32. The second outflow pipe 25 and the second inflow pipe 31 are connected by the second connecting pipe 5. In this way, the substance filtered by the filter tank 2 flows out from the second outflow pipe 25 of the filter tank 2 and flows into the second inflow pipe 31, and then flows into the third internal chamber 320 of the crystallization tank body 32. After being processed by the crystallization tank 2, crystals are formed, and the crystals flow out from the third outflow pipe 33.

[0031] The working principle of this application is as follows: The substances participating in the amide acetal reaction enter the first internal chamber of the reaction vessel through the first feeding channel, the second feeding channel, and the catalyst channel. After being stirred by the first stirring rod in the reaction vessel, the generated substances flow into the second internal chamber of the filter vessel. The bottom of the second internal chamber is equipped with a first filter tube and a second filter tube, both filled with activated carbon. The generated substances flow into the first and second filter tubes, and after being filtered by the activated carbon, they flow into the crystallization tank for crystallization. A second stirring rod and a third stirring rod are installed in the second internal chamber of the filter vessel. The stirring by the second and third stirring rods makes the generated substances more uniformly mixed, which is beneficial for activated carbon filtration.

[0032] The crystallization system for preparing amide acetal provided in this application has the advantages of simple structure and easy assembly. Since a filter tank is set between the reaction tank and the crystallization tank, the substance generated in the reaction tank flows into the filter tank and is filtered by activated carbon in the first filter tube and the second filter tube, which effectively removes impurities and decolorizes the substance generated. The substance with removed impurities and decolorizes flows into the crystallization tank for crystallization, thereby greatly improving the overall efficiency and the purity of the crystallized substance.

[0033] The above embodiments are only for illustrating the technical concept and features of this utility model, and are intended to enable those skilled in the art to understand the content of this utility model and implement it accordingly. They should not be construed as limiting the scope of protection of this utility model. All equivalent changes or modifications made in accordance with the spirit and essence of this utility model should be included within the scope of protection of this utility model.

Claims

1. A crystallization system for preparing an amide acetal, characterized in that, include: A reaction vessel, the reaction vessel including a reaction vessel body having a first internal chamber; A filter tank, the filter tank including a filter tank body, the filter tank body having a second internal chamber, and the first internal chamber of the reaction tank body and the second internal chamber of the filter tank body being connected through a first connecting pipe; A crystallization tank includes a crystallization tank body having a third internal chamber. A second internal chamber of a filtration tank body is connected to the third internal chamber of the crystallization tank body via a second connecting pipe. The second internal chamber of the filtration tank body contains a predetermined number of first filter tubes and a predetermined number of second filter tubes. The first filter tubes are connected to the second filter tubes. The first filter tubes have a predetermined number of first liquid holes, and the second filter tubes have a predetermined number of second liquid holes. Both the first and second filter tubes are filled with activated carbon.

2. The crystallization system for preparing amide acetal according to claim 1, characterized in that, The reaction vessel further includes a first feeding channel, a second feeding channel, and a catalyst channel. The first feeding channel, the second feeding channel, and the catalyst channel are all disposed on the reaction vessel body, and the first feeding channel, the second feeding channel, and the catalyst channel are all connected to the first internal chamber of the reaction vessel body.

3. The crystallization system for preparing amide acetal according to claim 1, characterized in that, The reaction vessel also includes a first drive motor and a first rotating rod. The first rotating rod is connected to the first drive motor so that the first drive motor drives the first rotating rod to rotate. A first stirring rod is also installed on the first rotating rod, and the first stirring rod is disposed in the first internal chamber of the reaction vessel body.

4. The crystallization system for preparing amide acetal according to claim 1, characterized in that, A first outflow pipe is provided on the bottom region of the reaction vessel body, and the first outflow pipe is connected to the first internal chamber of the reaction vessel body; the first connecting pipe is connected to and communicates with the first outflow pipe.

5. The crystallization system for preparing amide acetal according to claim 1, characterized in that, The filter tank further includes a second drive motor, a reducer, and a second rotating rod. The second drive motor is connected to the reducer, and the reducer is connected to the second rotating rod, so that the second drive motor drives the second rotating rod to rotate. A second stirring rod and a third stirring rod are installed on the second rotating rod, with the second stirring rod located above the third stirring rod, so that when the second rotating rod rotates, it drives the second stirring rod and the third stirring rod to rotate. The second stirring rod and the third stirring rod are both disposed in the second internal cavity of the filter tank body.

6. The crystallization system for preparing amide acetal according to claim 5, characterized in that, The filter tank further includes a first inflow pipe, a transfer cylinder, and a predetermined number of outflow capillary tubes. The first inflow pipe is connected to the transfer cylinder, and the outflow capillary tubes are connected to the transfer cylinder. The first inflow pipe is connected to the first internal chamber of the reaction tank body. The transfer cylinder and the outflow capillary tubes are both located in the second internal chamber of the filter tank body.

7. The crystallization system for preparing amide acetal according to claim 6, characterized in that, The transfer cylinder is provided with a rotating through hole, which extends through the transfer cylinder and has a diameter larger than that of the second rotating rod. The second rotating rod passes through the rotating through hole, thereby enabling the second rotating rod to rotate within the rotating through hole of the transfer cylinder.

8. The crystallization system for preparing amide acetal according to claim 1, characterized in that, The filter tank further includes a second outflow pipe, which is connected to the second filter tube; the crystallization tank further includes a second inflow pipe and a third outflow pipe, the second inflow pipe is disposed at the top of the crystallization tank body and is connected to the third internal chamber of the crystallization tank body; the third outflow pipe is disposed at the bottom of the crystallization tank body and is connected to the third internal chamber of the crystallization tank body; the second outflow pipe and the second inflow pipe are connected through the second connecting pipe.

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