CN214182994U - Ammoniation reaction device - Google Patents
Ammoniation reaction device Download PDFInfo
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- CN214182994U CN214182994U CN202022912621.0U CN202022912621U CN214182994U CN 214182994 U CN214182994 U CN 214182994U CN 202022912621 U CN202022912621 U CN 202022912621U CN 214182994 U CN214182994 U CN 214182994U
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- ammoniation reaction
- reaction kettle
- ammoniation
- dropwise add
- add jar
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Abstract
The utility model relates to an ammoniation reaction device, including ammoniation reaction kettle, ammoniation reaction kettle's export is through blowing pipeline connection centrifuge, ammoniation reaction kettle's import is located through the flowmeter connection the high-order dropwise add jar of ammoniation reaction kettle top, high-order dropwise add jar is through nitrogen gas union coupling nitrogen gas storage tank, high-order dropwise add jar still connects the ammonia solution jar through the diaphragm pump, high-order dropwise add jar is provided with freezing the clamp cover. The utility model discloses an ammoniation reaction device effectively solves prior art ammoniation reaction and releases heat acutely, and speed is uncontrollable, and the ammonia spills over more among the reaction process, and then causes the drawback that product purity is poor, the yield is low, and its yield is high, with low costs, and product quality is excellent, and has reduced the risk of the environmental protection incident that the ammonia leakage causes.
Description
Technical Field
The utility model belongs to the technical field of the meticulous chemical industry of medicine, concretely relates to ammoniation reaction unit.
Background
The 2, 3-dihydro-1, 4-dioxa [2,3-b ] pyridine-7-sulfonamide is an important medical intermediate in chemical industry, and the current process for producing the 2, 3-dihydro-1, 4-dioxa [2,3-b ] pyridine-7-sulfonamide generally comprises the following steps: 2, 3-dihydro-1, 4-dioxa [2,3-b ] pyridine-7-sulfonyl chloride is taken as an intermediate, through direct ammonia gas in a dichloromethane solvent, the ammoniation reaction is carried out to generate the intermediate, and the intermediate is concentrated, crystallized at low temperature and finally centrifuged and dried to obtain a finished product, but the production process has the following defects:
(1) the reaction process is violent in heat release, the gas flow is difficult to effectively control due to the fact that ammonia is directly introduced, the ammonia concentration of the whole reaction system is completely in a supersaturated state, a large amount of ammonia does not completely participate in the reaction in time, the ammonia overflows more, the tail gas absorption load is increased, and even partial leaked smell is heavier and is not beneficial to environmental protection.
(2) The high ammonia concentration has violent reaction, and impurities are easy to generate, so that the product purity is poor, and qualified products can be obtained only by refining and pulping for many times, so that the yield is low, the production period is prolonged, the waste liquid amount is increased, and the cost is increased.
(3) Ammonia gas is connected with a pressure reducing valve through an ammonia tank and is directly communicated into the reaction kettle through a buffer tank, the leakage risk still exists, and serious safety and environmental protection accidents can be caused once the ammonia gas is leaked.
Disclosure of Invention
The utility model aims at providing an ammoniation reaction device effectively solves prior art ammoniation reaction and releases heat acutely, and speed is difficult to control, and the ammonia spills over more in the reaction process, and then causes the drawback that product purity is poor, the yield is low, and its yield is high, with low costs, and product quality is excellent, and has reduced the risk of the environmental protection incident that the ammonia leaked and causes.
The utility model provides a technical scheme that above-mentioned problem adopted does: the utility model provides an ammoniation reaction device, includes ammoniation reaction kettle, ammoniation reaction kettle's export is through blowing pipeline connection centrifuge, ammoniation reaction kettle's import is connected through the flowmeter and is located the high-order dropwise add jar of ammoniation reaction kettle top, high-order dropwise add jar is through nitrogen gas union coupling nitrogen gas storage tank, high-order dropwise add jar still connects the ammonia solution jar through the diaphragm pump, high-order dropwise add jar is provided with freezing jacket.
Preferably, the ammoniation reaction kettle is also connected with a tail gas treatment unit through a tail gas pipe.
Preferably, a stirring mechanism is arranged in the ammoniation reaction kettle, and the stirring mechanism comprises a stirring shaft and an airfoil-shaped axial-flow type stirring paddle.
Preferably, the inlet pipeline and the outlet pipeline of the ammonification reaction kettle are both provided with regulating valves.
Preferably, the high-level dropwise adding tank and the diaphragm pump communicating pipeline are provided with regulating valves, and the nitrogen pipe is provided with a regulating valve.
Preferably, the high-level dripping tank is also provided with a liquid level meter.
Compared with the prior art, the utility model has the advantages of:
(1) the utility model discloses ammoniation reaction unit adopts the diaphragm pump to go into high-order dropwise add jar with the ammonia solution pump, through the governing valve in high-order dropwise add jar, flowmeter and the ammoniation reaction cauldron feed line, the ammonia solution volume that control got into ammoniation reaction cauldron, it is violent to effectively solve the prior art ammoniation reaction and release heat, speed is uncontrollable, the ammonia spills over more in the reaction process, and then causes the product purity difference, the drawback that the yield is low, its yield is high, and is with low costs, product quality is excellent, and the risk of the environmental protection incident that the ammonia leakage causes has been reduced.
(2) The utility model discloses high-order dropwise add jar is connected with the nitrogen gas storage tank through nitrogen gas pipe, and is provided with freezing clamp cover, effectively prevents the ammonia and spills over through pressurization, low temperature dropwise add.
Drawings
Fig. 1 is a schematic structural diagram of an ammonification reaction device in an embodiment of the present invention.
Wherein: 1 is an ammoniation reaction kettle, 1-1 is a stirring mechanism, 2 is a discharge pipeline, 3 is a centrifugal machine, 4 is a flow meter, 5 is a high-level dropping tank, 5-1 is a liquid level meter, 6 is a nitrogen pipe, 7 is a nitrogen storage tank, 8 is a diaphragm pump, and 9 is an ammonia solution tank.
Detailed Description
The present invention will be described in further detail with reference to the following embodiments.
As shown in fig. 1, the ammonification reaction apparatus in this embodiment has a schematic structural view.
The utility model provides an ammoniation reaction device, includes ammoniation reation kettle 1, 1 export of ammoniation reation kettle connects centrifuge 3 through blow off pipe 2, 1 import of ammoniation reation kettle is connected through flow meter 4 and is located the high-order dropwise add jar 5 of 1 top of ammoniation reation kettle, high-order dropwise add jar 5 is through nitrogen gas pipe 6 connection nitrogen gas storage tank 7, high-order dropwise add jar 5 is through the ammonia solution jar 9 of 8 connections of diaphragm pump, high-order dropwise add jar 5 with the pipeline of 8 intercommunications of diaphragm pump is provided with the governing valve.
The inlet pipeline and the outlet pipeline of the ammoniation reaction kettle 1 are both provided with regulating valves, a stirring mechanism 1-1 is arranged in the ammoniation reaction kettle 1, and the stirring mechanism 1-1 comprises a stirring shaft and an airfoil axial flow type stirring paddle; the ammoniation reaction kettle 1 is also connected with a tail gas treatment unit through a tail gas pipe.
The high-level dripping tank 5 is provided with a liquid level meter 5-1 and a freezing jacket, and the liquid level meter 5-1 is used for observing the liquid level height in the high-level dripping tank 5.
The operation of this embodiment is described in detail below with reference to the accompanying drawings:
2, 3-dihydro-1, 4-dioxa [2,3-b ] pyridine-7-sulfonyl chloride is arranged in an ammoniation reaction kettle 1, ammonia solution (methanol solution of ammonia or ethanol solution of ammonia) in an ammonia solution tank 9 is pumped into a high-level dropping tank 5 through a diaphragm pump 8, then nitrogen in a nitrogen storage tank 7 enters the high-level dropping tank 5 through a nitrogen pipe 6, the pressure in the high-level dropping tank 5 is controlled to be less than or equal to 40kpa, a refrigeration jacket of the high-level dropping tank 5 is opened to cool feed liquid to be less than or equal to-15 ℃, then an adjusting valve between the high-level dropping tank 5 and the ammoniation reaction kettle 1 is opened, the ammonia solution entering the ammoniation reaction kettle 1 is controlled through a flow meter 4, the ammonia solution reacts with the 2, 3-dihydro-1, 4-dioxa [2,3-b ] pyridine-7-sulfonyl chloride, tail gas in the reaction process enters a tail gas treatment unit through a tail gas pipeline, after the dropwise addition is finished, the regulating valve between the high-level dropwise addition tank 5 and the ammonification reaction kettle 1 is closed, the reaction is carried out for a period of time, after the reaction is finished, the regulating valve between the ammonification reaction kettle 1 and the centrifuge 3 is opened, and feed liquid in the ammonification reaction kettle 1 enters the centrifuge 3 through the discharging pipeline 2.
In addition to the above embodiments, the present invention also includes other embodiments, and all technical solutions formed by equivalent transformation or equivalent replacement should fall within the protection scope of the claims of the present invention.
Claims (6)
1. An ammoniation reaction device which is characterized in that: including ammoniation reaction kettle (1), centrifuge (3) is connected through blow off pipe way (2) in the export of ammoniation reaction kettle (1), the import of ammoniation reaction kettle (1) is connected through flow meter (4) and is located high-order dropwise add jar (5) of ammoniation reaction kettle (1) top, nitrogen gas storage tank (7) are connected through nitrogen gas pipe (6) to high-order dropwise add jar (5), high-order dropwise add jar (5) still connect ammonia solution tank (9) through diaphragm pump (8), high-order dropwise add jar (5) are provided with freezing jacket.
2. The ammoniation reaction device as claimed in claim 1, wherein: the ammoniation reaction kettle (1) is also connected with a tail gas treatment unit through a tail gas pipe.
3. The ammoniation reaction device as claimed in claim 1, wherein: a stirring mechanism (1-1) is arranged in the ammoniation reaction kettle (1), and the stirring mechanism (1-1) comprises a stirring shaft and an airfoil-shaped axial-flow type stirring paddle.
4. The ammoniation reaction device as claimed in claim 1, wherein: and the inlet pipeline and the outlet pipeline of the ammonification reaction kettle (1) are both provided with regulating valves.
5. The ammoniation reaction device as claimed in claim 1, wherein: high-order dropwise add jar (5) and diaphragm pump (8) intercommunication pipeline are provided with the governing valve, nitrogen gas pipe (6) are provided with the governing valve.
6. The ammoniation reaction device as claimed in claim 1, wherein: the high-level dripping tank (5) is also provided with a liquid level meter (5-1).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202022912621.0U CN214182994U (en) | 2020-12-08 | 2020-12-08 | Ammoniation reaction device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202022912621.0U CN214182994U (en) | 2020-12-08 | 2020-12-08 | Ammoniation reaction device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN214182994U true CN214182994U (en) | 2021-09-14 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202022912621.0U Active CN214182994U (en) | 2020-12-08 | 2020-12-08 | Ammoniation reaction device |
Country Status (1)
| Country | Link |
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| CN (1) | CN214182994U (en) |
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2020
- 2020-12-08 CN CN202022912621.0U patent/CN214182994U/en active Active
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