CN219003037U - Continuous synthesis device for cefixime side chain acid active ester - Google Patents
Continuous synthesis device for cefixime side chain acid active ester Download PDFInfo
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- CN219003037U CN219003037U CN202223569929.5U CN202223569929U CN219003037U CN 219003037 U CN219003037 U CN 219003037U CN 202223569929 U CN202223569929 U CN 202223569929U CN 219003037 U CN219003037 U CN 219003037U
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Abstract
The utility model relates to the technical field of synthesis of cefixime side chain acid active ester, in particular to a continuous synthesis device of cefixime side chain acid active ester. The device comprises a reaction kettle, wherein the reaction kettle is sequentially connected with a first full-automatic discharging centrifuge, a refining dissolution kettle, a refining cooling kettle, a second full-automatic discharging centrifuge, a dryer, an airflow mixer and an automatic packaging machine; the top of the reaction kettle is respectively connected with a cefixime side chain acid raw material tank, a dibenzothiazyl disulfide raw material tank, a triethyl phosphite raw material tank, a catalyst triethylamine tank and a dichloroethane solvent tank. The utility model greatly improves the yield of the product, has short reaction time, low energy consumption and small solvent consumption, and is beneficial to industrial production.
Description
Technical Field
The utility model relates to the technical field of synthesis of cefixime side chain acid active ester, in particular to a continuous synthesis device of cefixime side chain acid active ester.
Background
The cefixime side chain acid active ester is fully called (Z) -2- (2-aminothiazole-4-yl) -2-methoxycarbonyl methoxyimino-mercapto benzothiazole ester, and is a main raw material of cefixime. At present, the preparation method of the cefixime side chain acid active ester mainly takes cefixime side chain acid and dibenzothiazyl disulfide as raw materials, dichloroethane is taken as a solvent, triethyl phosphite is dripped for reaction under the catalysis of a catalyst, and the cefixime side chain acid active ester is obtained after post-treatment.
Chinese patent CN113956214a discloses a method for continuously synthesizing cefixime side chain acid active ester, the reaction device disclosed in the patent also comprises a slurry preparation kettle, a reaction kettle, a cooling kettle, a turnover kettle and 7 metering pumps which are connected in series; wherein, the export of thick liquid configuration cauldron is connected with the import of measuring pump, establishes ties a reation kettle between measuring pump and the cooling cauldron, links to each other through the measuring pump between last stage reation kettle and the cooling cauldron, links to each other through the measuring pump between cooling cauldron and the turnover cauldron. And filtering the materials in the turnover kettle to obtain a crude product, and performing post-treatment on the crude product to obtain the cefixime side chain acid active ester product. The patent needs a multistage reaction kettle for reaction, needs a slurry preparation kettle and a turnover kettle, and then needs a post-treatment device for treatment, the whole device is relatively complex, the yield of products is greatly reduced, the reaction time is long, the productivity is low, the energy consumption is high, the solvent consumption is large, and the industrial production is not facilitated.
Disclosure of Invention
The utility model aims to provide a continuous synthesis device of cefixime side chain acid active ester, which greatly improves the yield of products, has short reaction time, low energy consumption and less solvent consumption, and is beneficial to industrial production.
The utility model relates to a continuous synthesis device of cefixime side chain acid active ester, which comprises a reaction kettle, wherein the reaction kettle is sequentially connected with a first full-automatic discharging centrifuge, a refined dissolution kettle, a refined cooling kettle, a second full-automatic discharging centrifuge, a dryer, an airflow mixer and an automatic packaging machine; the top of the reaction kettle is respectively connected with a cefixime side chain acid raw material tank, a dibenzothiazyl disulfide raw material tank, a triethyl phosphite raw material tank, a catalyst triethylamine tank and a dichloroethane solvent tank.
Wherein:
a first screw conveyer is arranged between the first full-automatic discharging centrifugal machine and the refining dissolution kettle, and a second screw conveyer is arranged between the second full-automatic discharging centrifugal machine and the dryer.
The triethyl phosphite raw material tank is connected with the reaction kettle through a first meter, and the catalyst triethylamine tank is connected with the reaction kettle through a second meter.
The reaction kettle top is also connected with a first nitrogen tank, the first full-automatic discharging centrifugal machine is also connected with a second nitrogen tank, and the second full-automatic discharging centrifugal machine is also connected with a third nitrogen tank.
The first full-automatic discharging centrifugal machine and the second full-automatic discharging centrifugal machine are both provided with two.
The top of the refining dissolution kettle is connected with a first methanol tank, and the top of the refining cooling kettle is connected with a second methanol tank.
The air flow mixer is also connected with a voltage stabilizer, and the voltage stabilizer is used for controlling the pressure stabilization in the air flow mixer.
The bottom of the first full-automatic discharging centrifugal machine is provided with a first centrifugate outlet which is connected with the dichloroethane solvent tank.
The bottom of the second full-automatic discharging centrifugal machine is provided with a second centrifugate outlet which is connected with a second methanol tank.
Stirring devices are arranged in the reaction kettle, the refining dissolution kettle and the refining cooling kettle.
The working process of the utility model is as follows:
at normal temperature, nitrogen in a first nitrogen tank and dichloroethane in a dichloroethane solvent tank are put into a reaction kettle, triethyl phosphite from a triethyl phosphite raw material tank is metered by a first meter and is converged with catalyst triethylamine from a catalyst triethylamine tank by a second meter, dibenzothiazyl disulfide in a dibenzothiazyl disulfide raw material tank is put into the reaction kettle, and finally cefixime side chain acid in a cefixime side chain acid raw material tank is dripped into the reaction kettle for reaction under the action of nitrogen, so that crude reaction liquid is obtained.
The crude reaction liquid is conveyed to a first full-automatic discharging centrifugal machine, nitrogen in a second nitrogen tank is injected into the first full-automatic discharging centrifugal machine, the crude reaction liquid in the first full-automatic discharging centrifugal machine is subjected to solid-liquid separation under the action of the nitrogen, and the separated liquid is discharged from a first centrifugal liquid outlet and enters a dichloroethane solvent tank for recycling; the separated solid crude product is sent to a refining dissolution kettle through a first screw conveyer, meanwhile, methanol in a first methanol tank enters the refining dissolution kettle from the top of the refining dissolution kettle to dissolve the crude product, the dissolved material enters a refining cooling kettle to be cooled and crystallized, then the material enters a second full-automatic discharging centrifugal machine, after the material in the refining dissolution kettle flows out, the methanol in the second methanol tank is injected into the refining dissolution kettle to wash the refining dissolution kettle, and the material completely flows into the second full-automatic discharging centrifugal machine.
Injecting nitrogen in the third nitrogen tank into a second full-automatic discharging centrifugal machine, and under the action of the nitrogen, carrying out solid-liquid separation on materials by the second full-automatic discharging centrifugal machine, discharging separated liquid from a second centrifugate outlet, and recycling the separated liquid in a second methanol tank; the separated solid phase is conveyed to a dryer through a second screw conveyor to be dried into powder, and the powder enters an airflow mixer to be stirred and mixed uniformly, and finally enters an automatic packaging machine to be packaged.
Compared with the prior art, the utility model has the following beneficial effects:
the reaction kettle is sequentially connected with a first full-automatic discharging centrifugal machine, a refining dissolution kettle, a refining cooling kettle, a second full-automatic discharging centrifugal machine, a dryer, an airflow mixer and an automatic packaging machine; a first screw conveyer is arranged between the first full-automatic discharging centrifugal machine and the refining dissolution kettle, and a second screw conveyer is arranged between the second full-automatic discharging centrifugal machine and the dryer. The utility model can orderly connect the reaction stage and the post-treatment stage through the arrangement of the first full-automatic discharging centrifugal machine, the first spiral conveyor, the second full-automatic discharging centrifugal machine and the second spiral conveyor, realizes the continuity of the whole reaction, greatly improves the yield of products, has short reaction time and low energy consumption, and is beneficial to industrial production.
In the utility model, a first centrifugate outlet is arranged at the bottom of a first full-automatic discharging centrifugal machine, and the first centrifugate outlet is connected with a dichloroethane solvent tank; the bottom of the second full-automatic discharging centrifugal machine is provided with a second centrifugate outlet which is connected with a second methanol tank. According to the utility model, the first centrifugate outlet is connected with the dichloroethane solvent tank, and the second centrifugate outlet is connected with the second methanol tank, so that the solution separated in the whole preparation process can be recycled, and the use amount of the solvent is greatly reduced.
Drawings
FIG. 1 is a schematic diagram of the structure of the present utility model;
in the figure: 1. triethyl phosphite material tank; 2. a first meter; 3. a dibenzothiazyl disulfide feedstock tank; 4. a first nitrogen tank; 5. cefixime side chain acid raw material tank; 6. a second methanol tank; 7. refining and cooling the kettle; 8. a third nitrogen tank; 9. a second fully automatic discharge centrifuge; 10. a second centrate outlet port; 11. a second screw conveyor; 12. an air flow mixer; 13. an automatic packaging machine; 14. a pressure stabilizing machine; 15. a dryer; 16. a first methanol tank; 17. refining and dissolving the kettle; 18. a first screw conveyor; 19. a first centrate outlet port; 20. a first fully automatic discharge centrifuge; 21. a second nitrogen tank; 22. a reaction kettle; 23. a dichloroethane solvent tank; 24. a second meter; 25. and a catalyst triethylamine tank.
Detailed Description
The utility model is further illustrated by the following examples.
Example 1
As shown in figure 1, the continuous synthesis device of cefixime side chain acid active ester comprises a reaction kettle 22, wherein the reaction kettle 22 is sequentially connected with a first full-automatic discharging centrifuge 20, a refining dissolution kettle 17, a refining cooling kettle 7, a second full-automatic discharging centrifuge 9, a dryer 15, an air flow mixer 12 and an automatic packaging machine 13; the top of the reaction kettle 22 is respectively connected with a cefixime side chain acid raw material tank 5, a dibenzothiazyl disulfide raw material tank 3, a triethyl phosphite raw material tank 1, a catalyst triethylamine tank 25 and a dichloroethane solvent tank 23.
Wherein:
a first screw conveyer 18 is arranged between the first full-automatic discharging centrifugal machine 20 and the refining dissolution kettle 17, and a second screw conveyer 11 is arranged between the second full-automatic discharging centrifugal machine 9 and the dryer 15.
The triethyl phosphite raw material tank 1 is connected with the reaction kettle 22 through a first meter 2, and the catalyst triethylamine tank 25 is connected with the reaction kettle 22 through a second meter 24.
The top of the reaction kettle 22 is also connected with a first nitrogen tank 4, the first full-automatic discharging centrifugal machine 20 is also connected with a second nitrogen tank 21, and the second full-automatic discharging centrifugal machine 9 is also connected with a third nitrogen tank 8.
The first full-automatic discharging centrifugal machine 20 and the second full-automatic discharging centrifugal machine 9 are respectively provided with two.
The top of the refining dissolution kettle 17 is connected with a first methanol tank 16, and the top of the refining cooling kettle 7 is connected with a second methanol tank 6.
The air flow mixer 12 is also connected to a pressure regulator 14, the pressure regulator 14 being used to control the pressure stabilization in the air flow mixer 12.
The bottom of the first full-automatic discharging centrifugal machine 20 is provided with a first centrifugate outlet 19, and the first centrifugate outlet 19 is connected with a dichloroethane solvent tank 23.
The bottom of the second full-automatic discharging centrifugal machine 9 is provided with a second centrifugate outlet 10, and the second centrifugate outlet 10 is connected with the second methanol tank 6.
Stirring devices are arranged in the reaction kettle 22, the refining dissolution kettle 17 and the refining cooling kettle 7.
The continuous synthesis process of cefixime side chain acid active ester is as follows:
at normal temperature, nitrogen in a first nitrogen tank 4 and dichloroethane in a dichloroethane solvent tank 23 are put into a reaction kettle 22, triethyl phosphite from a triethyl phosphite raw material tank 1 is mixed with triethylamine from a catalyst triethylamine tank 25 by a first metering device 2 by a second metering device 24, the mixed solution is put into the reaction kettle 22, dibenzothiazyl disulfide in a dibenzothiazyl disulfide raw material tank 3 is put into the reaction kettle 22, and finally cefixime side chain acid in a cefixime side chain acid raw material tank 5 is dripped into the reaction kettle 22 for reaction under the action of nitrogen, so that crude reaction liquid is obtained.
The crude reaction liquid is conveyed to a first full-automatic discharging centrifugal machine 20, nitrogen in a second nitrogen tank 21 is injected into the first full-automatic discharging centrifugal machine 20, the crude reaction liquid in the first full-automatic discharging centrifugal machine 20 is subjected to solid-liquid separation under the action of the nitrogen, and the separated liquid is discharged from a first centrifugate outlet 19 and enters a dichloroethane solvent tank 23 for recycling; the separated solid crude product is sent to a refining dissolution kettle 17 through a first screw conveyer 18, meanwhile, methanol in a first methanol tank 16 enters the refining dissolution kettle 17 from the top of the refining dissolution kettle 17 to dissolve the crude product, the dissolved material enters a refining cooling kettle 7 to be cooled and crystallized, then the material enters a second full-automatic discharging centrifugal machine 9, after the material in the refining dissolution kettle 17 flows out, the methanol in a second methanol tank 6 is injected into the refining dissolution kettle 17 to wash the refining dissolution kettle 17, and the material totally flows into the second full-automatic discharging centrifugal machine 9.
Nitrogen in a third nitrogen tank 8 is injected into a second full-automatic discharging centrifugal machine 9, under the action of the nitrogen, materials are subjected to solid-liquid separation through the second full-automatic discharging centrifugal machine 9, and separated liquid is discharged from a second centrifugate outlet 10 and enters a second methanol tank 6 for recycling; the separated solid phase is conveyed to a dryer 15 through a second screw conveyor 11 to be dried into powder, and the powder enters an airflow mixer 12 to be stirred and mixed uniformly, and finally enters an automatic packaging machine 13 to be packaged. The yield of cefixime side chain acid active ester is more than 99.5%.
Claims (10)
1. The utility model provides a continuous synthesis device of cefixime side chain acid active ester, includes reation kettle (22), its characterized in that: the reaction kettle (22) is sequentially connected with a first full-automatic discharging centrifugal machine (20), a refining dissolution kettle (17), a refining cooling kettle (7), a second full-automatic discharging centrifugal machine (9), a dryer (15), an air flow mixer (12) and an automatic packaging machine (13); the top of the reaction kettle (22) is respectively connected with a cefixime side chain acid raw material tank (5), a dibenzothiazyl disulfide raw material tank (3), a triethyl phosphite raw material tank (1), a catalyst triethylamine tank (25) and a dichloroethane solvent tank (23).
2. The continuous synthesis device of cefixime side chain acid active ester according to claim 1, characterized in that: a first screw conveyer (18) is arranged between the first full-automatic discharging centrifugal machine (20) and the refining dissolution kettle (17), and a second screw conveyer (11) is arranged between the second full-automatic discharging centrifugal machine (9) and the dryer (15).
3. The continuous synthesis device of cefixime side chain acid active ester according to claim 1, characterized in that: the triethyl phosphite raw material tank (1) is connected with the reaction kettle (22) through a first meter (2), and the catalyst triethylamine tank (25) is connected with the reaction kettle (22) through a second meter (24).
4. The continuous synthesis device of cefixime side chain acid active ester according to claim 1, characterized in that: the top of the reaction kettle (22) is also connected with a first nitrogen tank (4), the first full-automatic discharging centrifugal machine (20) is also connected with a second nitrogen tank (21), and the second full-automatic discharging centrifugal machine (9) is also connected with a third nitrogen tank (8).
5. The continuous synthesis device of cefixime side chain acid active ester according to claim 4, wherein: the first full-automatic discharging centrifugal machine (20) and the second full-automatic discharging centrifugal machine (9) are respectively provided with two.
6. The continuous synthesis device of cefixime side chain acid active ester according to claim 1, characterized in that: the top of the refining dissolution kettle (17) is connected with a first methanol tank (16), and the top of the refining cooling kettle (7) is connected with a second methanol tank (6).
7. The continuous synthesis device of cefixime side chain acid active ester according to claim 1, characterized in that: the air flow mixer (12) is also connected with a pressure stabilizer (14).
8. The continuous synthesis device of cefixime side chain acid active ester according to claim 1, characterized in that: the bottom of the first full-automatic discharging centrifugal machine (20) is provided with a first centrifugate outlet (19), and the first centrifugate outlet (19) is connected with a dichloroethane solvent tank (23).
9. The continuous synthesis device of cefixime side chain acid active ester according to claim 6, wherein: the bottom of the second full-automatic discharging centrifugal machine (9) is provided with a second centrifugate outlet (10), and the second centrifugate outlet (10) is connected with the second methanol tank (6).
10. The continuous synthesis device of cefixime side chain acid active ester according to claim 1, characterized in that: stirring devices are arranged in the reaction kettle (22), the refining dissolution kettle (17) and the refining cooling kettle (7).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202223569929.5U CN219003037U (en) | 2022-12-27 | 2022-12-27 | Continuous synthesis device for cefixime side chain acid active ester |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202223569929.5U CN219003037U (en) | 2022-12-27 | 2022-12-27 | Continuous synthesis device for cefixime side chain acid active ester |
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| CN219003037U true CN219003037U (en) | 2023-05-12 |
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| CN202223569929.5U Active CN219003037U (en) | 2022-12-27 | 2022-12-27 | Continuous synthesis device for cefixime side chain acid active ester |
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