CN211497433U - Production device of 4-bromopyrazole - Google Patents
Production device of 4-bromopyrazole Download PDFInfo
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- CN211497433U CN211497433U CN202020142574.3U CN202020142574U CN211497433U CN 211497433 U CN211497433 U CN 211497433U CN 202020142574 U CN202020142574 U CN 202020142574U CN 211497433 U CN211497433 U CN 211497433U
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Abstract
The utility model relates to the technical field of 4-bromopyrazole production equipment, in particular to a production device of 4-bromopyrazole. The production device of the 4-bromopyrazole comprises a bromination kettle, a neutralization kettle, a refining kettle, a crystallization kettle, a suction filter tank, a centrifugal machine and a double-cone dryer which are connected in sequence; the bromination kettle is circularly connected with the condenser through a gas phase discharge pipeline and a condensate reflux pipeline; the upper end of the bromination cauldron is connected with raw materials feed line, and the upper end of the neutralization cauldron is connected with alkali lye feed line, and the upper end of the refined cauldron is connected with methyl alcohol feed line, and the suction filtration groove links to each other with the methyl alcohol storage tank. The utility model discloses a production device of 4-bromopyrazole, simple structure, equipment input cost is low, accomplishes from throwing the material to packing finished product one line, and production efficiency is high.
Description
Technical Field
The utility model relates to the technical field of 4-bromopyrazole production equipment, in particular to a production device of 4-bromopyrazole.
Background
4-bromopyrazole, having the formula:
the 4-bromopyrazole is light yellow crystal powder, is an important intermediate for organic synthesis, and can be used for synthesizing organic matters such as 4-bromo-1- (tetrahydro-2H-pyran-4-yl) -1H-pyrazole, 4-bromo-1- (tetrahydrofuran-3-yl) -1H-pyrazole, 1-benzyl-4-bromopyrazole, 4-bromo-1-isopropyl-1H-pyrazole, 1H-pyrazole-4-formic acid and the like. The compound is mainly used as an intermediate of certain medicines and pesticides, and plays an important role in research and development of medicines and pesticides. The synthesis route of 4-bromopyrazole mainly comprises the following three routes: firstly, synthesizing 4-bromopyrazole by pyrazole; secondly, synthesizing 4-bromopyrazole by 3, 5-pyrazoledicarboxylic acid; thirdly, synthesizing 4-bromopyrazole by 1- (pyrazine-4-group) ethanone.
In the three synthesis methods, the first method has simple raw materials, and can prepare the 4-bromopyrazole by adopting the reaction of pyrazole and bromine, but aiming at the synthesis method, no complete industrial production device exists in China at present.
SUMMERY OF THE UTILITY MODEL
The utility model provides a technical problem be: the production device of the 4-bromopyrazole is simple in structure, low in equipment investment cost, capable of completing the process from feeding to packaging of finished products in one line and high in production efficiency.
The production device of 4-bromopyrazole comprises a bromination kettle, a neutralization kettle, a refining kettle, a crystallization kettle, a suction filter tank, a centrifugal machine and a double-cone dryer which are connected in sequence; the bromination kettle is circularly connected with the condenser through a gas phase discharge pipeline and a condensate reflux pipeline.
The bromination kettle, the refining kettle and the crystallization kettle are all provided with jackets. And introducing steam or heat conducting oil into the jacket to heat and preserve heat of the materials in each kettle.
The upper end of the bromination kettle is connected with a raw material feeding pipeline. Pyrazole, bromine and hydrogen peroxide are added into a bromination kettle through a feeding pipeline for bromination reaction.
The upper end of the neutralization kettle is connected with an alkali liquor feeding pipeline. And after the bromination reaction is finished, introducing the reacted mixture into a neutralization kettle, adding alkali liquor into the neutralization kettle through an alkali liquor feeding pipe, neutralizing until the pH value is 7-8, standing for layering, and introducing an organic phase into a refining kettle.
The upper end of the refining kettle is connected with a methanol feeding pipeline. Methanol is added into the refining kettle through a methanol feeding pipeline, and then the mixed solution is introduced into a suction filter tank.
The suction filter tank is connected with a methanol storage tank. And introducing the liquid obtained by suction filtration of the suction filtration tank into a methanol storage tank, and introducing the obtained wet product into a centrifugal machine.
The lower end of the centrifuge is connected with a waste liquid discharge pipeline. And centrifuging the wet product after suction filtration by using a centrifugal machine, collecting a liquid phase through a waste liquid discharge pipeline, and adding a solid phase into a double-cone dryer.
The double-cone dryer is provided with a product discharge port. Drying by a double-cone dryer to obtain a finished product of 4-bromopyrazole, discharging from a product discharge port, and packaging.
The condenser is also connected with a cold medium inlet pipe, a cold medium outlet pipe and a noncondensable gas discharge pipeline.
The working process of the production device of the 4-bromopyrazole is as follows:
pyrazole, bromine and hydrogen peroxide are added into a bromination kettle through a feeding pipeline for bromination reaction, gas phase generated in the bromination reaction enters a condenser through a gas phase discharge pipeline for condensation, condensate containing hydrogen bromide enters the bromination kettle through a condensate reflux pipeline for continuous reaction, and non-condensable gas is collected and treated through a non-condensable gas discharge pipeline; after the bromination reaction is finished, introducing the reacted mixture into a neutralization kettle, adding alkali liquor into the neutralization kettle through an alkali liquor feeding pipe, neutralizing until the pH value is 7-8, standing for layering, and introducing an organic phase into a refining kettle; adding methanol into the refining kettle through a methanol feeding pipeline, and then introducing the mixed solution into a suction filter tank; introducing liquid obtained by suction filtration of the suction filtration tank into a methanol storage tank, and introducing the obtained wet product into a centrifugal machine; and centrifuging the filtered wet product by using a centrifugal machine, collecting a liquid phase through a waste liquid discharge pipeline, putting a solid phase into a double-cone dryer, drying to obtain a finished product of the 4-bromopyrazole, and packaging.
Compared with the prior art, the utility model discloses there is following beneficial effect:
the utility model discloses a production device of 4-bromine pyrazole simple structure, equipment input cost is low, carries out the condensation reflux through the hydrogen bromide that the condenser produced in to the bromination reaction process and utilizes, has improved utilization ratio of raw materials, and ensures that production is accomplished from throwing material to packing finished product line, and production efficiency is high.
Drawings
FIG. 1 is a schematic flow diagram of a 4-bromopyrazole production apparatus of the present invention;
in the figure: 1. a bromination kettle; 2. a raw material feed line; 3. a condensate return line; 4. introducing a cold medium into the pipe; 5. a noncondensable gas discharge pipeline; 6. a condenser; 7. a gas phase discharge line; 8. a cold medium outlet pipe; 9. a neutralization kettle; 10. an alkali liquor feeding pipeline; 11. a refining kettle; 12. a methanol feed line; 13. a crystallization kettle; 14. a methanol storage tank; 15. a suction filtration tank; 16. a waste liquid discharge pipeline; 17. a centrifuge; 18. a double cone dryer; 19. and a product discharge port.
Detailed Description
The present invention will be further described with reference to the following examples, but the scope of the present invention is not limited thereto.
Example 1
As shown in figure 1, the production device of 4-bromopyrazole comprises a bromination kettle 1, a neutralization kettle 9, a refining kettle 11, a crystallization kettle 13, a suction filtration tank 15, a centrifuge 17 and a double-cone dryer 18 which are connected in sequence;
the bromination kettle 1 is circularly connected with a condenser 6 through a gas phase discharge pipeline 7 and a condensate return pipeline 3.
The bromination kettle 1, the refining kettle 11 and the crystallization kettle 13 are all provided with jackets. And introducing steam or heat conducting oil into the jacket to heat and preserve heat of the materials in each kettle.
The upper end of the bromination kettle 1 is connected with a raw material feeding pipeline 2.
The upper end of the neutralization kettle 9 is connected with an alkali liquor feeding pipeline 10.
The upper end of the refining kettle 11 is connected with a methanol feeding pipeline 12.
The suction filter 15 is connected to the methanol storage tank 14.
The lower end of the centrifuge 17 is connected to a waste liquid discharge line 16.
The double cone dryer 18 is provided with a product discharge opening 19.
The condenser 6 is also connected with a cold medium inlet pipe 4, a cold medium outlet pipe 8 and a non-condensable gas discharge pipeline 5.
The working process of the production device of the 4-bromopyrazole is as follows:
pyrazole, bromine and hydrogen peroxide are added into a bromination kettle 1 through a feeding pipeline 2 for bromination reaction, gas phase generated in the bromination reaction enters a condenser 6 through a gas phase discharge pipeline 7 for condensation, condensate containing hydrogen bromide enters the bromination kettle 1 through a condensate return pipeline 3 for continuous reaction, and non-condensable gas is collected and treated through a non-condensable gas discharge pipeline 5; after the bromination reaction is finished, introducing the reacted mixture into a neutralization kettle 9, adding alkali liquor into the neutralization kettle 9 through an alkali liquor feeding pipeline 10, neutralizing until the pH value is 7-8, standing for layering, and introducing an organic phase into a refining kettle 11; adding methanol into a refining kettle 11 through a methanol feeding pipeline 12, and then introducing the mixed solution into a suction filter tank 15; introducing liquid obtained by suction filtration of the suction filtration tank 15 into a methanol storage tank 14, and introducing the obtained wet product into a centrifugal machine 17; and centrifuging the filtered wet product by a centrifugal machine 17, collecting a liquid phase through a waste liquid discharge pipeline 16, putting a solid phase into a double-cone dryer 18, drying to obtain a finished product of the 4-bromopyrazole, and packaging.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described in the foregoing embodiments, or equivalents may be substituted for elements thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A production device of 4-bromopyrazole is characterized in that: comprises a bromination kettle (1), a neutralization kettle (9), a refining kettle (11), a crystallization kettle (13), a suction filtration groove (15), a centrifuge (17) and a double-cone dryer (18) which are connected in sequence;
the bromination kettle (1) is circularly connected with the condenser (6) through a gas phase discharge pipeline (7) and a condensate reflux pipeline (3).
2. The apparatus for producing 4-bromopyrazole as claimed in claim 1, wherein: the bromination kettle (1), the refining kettle (11) and the crystallization kettle (13) are all provided with jackets.
3. The apparatus for producing 4-bromopyrazole as claimed in claim 1, wherein: the upper end of the bromination kettle (1) is connected with a raw material feeding pipeline (2).
4. The apparatus for producing 4-bromopyrazole as claimed in claim 1, wherein: the upper end of the neutralization kettle (9) is connected with an alkali liquor feeding pipeline (10).
5. The apparatus for producing 4-bromopyrazole as claimed in claim 1, wherein: the upper end of the refining kettle (11) is connected with a methanol feeding pipeline (12).
6. The apparatus for producing 4-bromopyrazole as claimed in claim 1, wherein: the suction filter tank (15) is connected with a methanol storage tank (14).
7. The apparatus for producing 4-bromopyrazole as claimed in claim 1, wherein: the lower end of the centrifuge (17) is connected with a waste liquid discharge pipeline (16).
8. The apparatus for producing 4-bromopyrazole as claimed in claim 1, wherein: the double cone dryer (18) is provided with a product discharge outlet (19).
9. The apparatus for producing 4-bromopyrazole as claimed in claim 1, wherein: the condenser (6) is also connected with a cold medium inlet pipe (4), a cold medium outlet pipe (8) and a noncondensable gas discharge pipeline (5).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020142574.3U CN211497433U (en) | 2020-01-21 | 2020-01-21 | Production device of 4-bromopyrazole |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020142574.3U CN211497433U (en) | 2020-01-21 | 2020-01-21 | Production device of 4-bromopyrazole |
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| Publication Number | Publication Date |
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| CN211497433U true CN211497433U (en) | 2020-09-15 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202020142574.3U Active CN211497433U (en) | 2020-01-21 | 2020-01-21 | Production device of 4-bromopyrazole |
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| CN (1) | CN211497433U (en) |
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2020
- 2020-01-21 CN CN202020142574.3U patent/CN211497433U/en active Active
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