CN203625269U - 4-amino-antipyrine production device - Google Patents
4-amino-antipyrine production device Download PDFInfo
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- CN203625269U CN203625269U CN201320803195.4U CN201320803195U CN203625269U CN 203625269 U CN203625269 U CN 203625269U CN 201320803195 U CN201320803195 U CN 201320803195U CN 203625269 U CN203625269 U CN 203625269U
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- quinizine
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- pyrazolone
- hydrolytic decomposition
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Abstract
The utility model relates to a 4-amino-antipyrine production device. The 4-amino-antipyrine production device comprises a first pyrazolone storage bin and is characterized in that the first pyrazolone storage bin and a first dimethyl sulfate measuring tank are respectively connected to a first methylation tank which is connected to a first hydrolysis tank, and the first hydrolysis tank is connected to an alkali treatment tank which is connected to an antipyrine oil storage tank; a second pyrazolone storage bin and a second dimethyl sulfate measuring tank are respectively connected to a second methylation tank which is connected to a second hydrolysis tank, the second hydrolysis tank, the antipyrine oil storage tank and a third water measuring tank are respectively connected to an antipyrine sulfuric acid quaternary ammonium salt allocation tank, the antipyrine sulfuric acid quaternary ammonium salt allocation tank and a sodium nitrite measuring tank are respectively connected to a nitrosation reaction tank which is connected to a reduction reaction tank, and the reduction reaction tank is connected to a hydrolysis neutralization tank; and the first hydrolysis tank is connected to a liquid caustic soda measuring tank. The 4-amino-antipyrine production device is environment-friendly, simple in process, convenient to operate and high in product yield.
Description
Technical field
The utility model belongs to field of medicine and chemical technology, particularly a kind of 4-AA production equipment.
Background technology
Sulpyrine, pyramidon are important ntipyretic analgesic medicine, only the market scale of Sulpyrine is 20,000 tons of left and right, China is main in the world producing country and export State, in addition pyramidon market capacity is also 2500 tons of left and right, therefore the usage quantity of 4-AA is huge, and therefore simple, the environmental friendliness of development and operation, technique that atom utilization is high are extremely urgent.
Traditional technique is take 1-phenyl-3-methyl-5-pyrazolone as starting material and methyl-sulfate high temperature methylates, quinizine oil is produced in hydrolysis, alkaline purification; Quinizine oil is made into quinizine quaternary ammonium sulfate in the proper ratio with the vitriol oil, water, and quinizine quaternary ammonium sulfate generates 4-AA through nitrosification, reduction, hydrolysis and neutralization; During by this explained hereafter, often produce 1 kilogram of 4-AA and need consume 0.5800 kilogram of liquid caustic soda, preparation quinizine quaternary ammonium sulfate consumes 0.2900 kilogram, sulfuric acid, generate 1.2672 kilograms, sodium sulfate, because of Sulpyrine, pyramidon series ntipyretic analgesic medicine market scale huge, huge to sodium sulfate, the high-COD waste water amount of the Nature discharge every year.
Utility model content
The purpose of this utility model is to provide a kind of 4-AA production equipment, is antipyretic and analgesic Sulpyrine, the extremely important intermediate of pyramidon, and the usage quantity of liquid caustic soda, sulfuric acid greatly reduces; Sodium sulfate, hc effluent quantity discharged reduce obviously, environmental friendliness, and technique is simple, easy to operate, and product yield is high.
The utility model 4-AA production equipment, step is as follows:
A kind of 4-AA production equipment described in the utility model, comprise the first pyrazolone feed bin, the first pyrazolone feed bin and the first methyl-sulfate test tank are connected by pipeline and first tank that methylates respectively, first tank that methylates is connected with the first hydrolytic decomposition pot, the first hydrolytic decomposition pot is connected with alkaline purification tank, and alkaline purification tank is connected with quinizine oil tank; The second pyrazolone feed bin and the second methyl-sulfate test tank are connected by pipeline and second tank that methylates respectively, second tank that methylates is connected with the second hydrolytic decomposition pot, the second hydrolytic decomposition pot, quinizine oil tank, the 3rd water metering are filled with and are connected with quinizine quaternary ammonium sulfate batch tank by pipeline respectively, quinizine quaternary ammonium sulfate batch tank is connected with nitrosation reaction tank by pipeline respectively with Sodium Nitrite metering filling, nitrosation reaction tank is connected with reduction reaction can, and reduction reaction can is connected with hydrolysis neutralization tank; The first hydrolytic decomposition pot is filled with and is connected with liquid caustic soda metering by pipeline.
Hydrolysis neutralization tank is connected with ammonium sulfate liquor tank and 4-quinizine oil tank by pipeline respectively.
The first water metering is filled with and is connected with the first hydrolytic decomposition pot by pipeline.
The second water metering is filled with and is connected with the second hydrolytic decomposition pot by pipeline.
Alkaline purification tank is connected with sodium sulfate mother liquor tank by pipeline.
Valve is all set on each pipeline.
Every pipeline has twice valve, is respectively bottom valve and material feeding valve.
Because the half lot number that has suitable traditional technology does not need alkaline purification, alkaline purification equipment, quinizine oil tank can reduce by half.
Using method:
Pyrazolone is put into the first pyrazolone feed bin; Methyl-sulfate is squeezed into the first methyl-sulfate test tank, and the pyrazolone of the first pyrazolone feed bin enters first tank that methylates, and closes the first tank pyrazolone charging opening that methylates; Open the first methyl-sulfate test tank bottom valve, the first tank feed valve that methylates, adds first tank that methylates by methyl-sulfate, finishes, close the first methyl-sulfate bottom valve, first tank feed valve that methylates, temperature reaction, reacts complete, opens the first tank bottom valve that methylates, the first hydrolytic decomposition pot feed valve, first liquid that methylates is put into the first hydrolytic decomposition pot, put completely, close the first tank bottom valve that methylates; Open the first water measuring tank bottom valve, the water of dosage is joined to the first hydrolytic decomposition pot, finish, close the first water measuring tank bottom valve and the first hydrolytic decomposition pot charging valve, reaction is hydrolyzed, hydrolysis is finished, and opens the first hydrolytic decomposition pot bottom valve, alkaline purification tank feed valve, hydrolysis material is put into alkaline purification tank, open alkali lye metering and fill with valve, put into the reaction of alkaline purification tank, reaction is finished, open quinizine oil tank feed valve, lower floor's solution is put into sodium sulfate mother liquor tank and collect, the upper strata quinizine oil of alkaline purification tank is put into quinizine oil tank, for subsequent use;
Pyrazolone is put into the second pyrazolone feed bin; Methyl-sulfate is squeezed into the second methyl-sulfate test tank, and the pyrazolone of the second pyrazolone feed bin enters second tank that methylates, and closes the second tank pyrazolone charging opening that methylates; Open the second methyl-sulfate test tank bottom valve, the second tank feed valve that methylates, adds second tank that methylates by methyl-sulfate, finishes, close the second methyl-sulfate bottom valve, second tank feed valve that methylates, temperature reaction, reacts complete, opens the second tank bottom valve that methylates, the second hydrolytic decomposition pot feed valve, second liquid that methylates is put into the second hydrolytic decomposition pot, put completely, close the second tank bottom valve that methylates; Open the second water measuring tank bottom valve, the water of dosage is joined to the second hydrolytic decomposition pot, finish, close the second water measuring tank bottom valve and the second hydrolytic decomposition pot charging valve, the reaction that is hydrolyzed, hydrolysis is finished, for subsequent use;
Open the second hydrolytic decomposition pot bottom valve, hydrolyzed solution is pressed into quinizine quaternary ammonium sulfate preparing tank, open quinizine oil tank bottom valve quinizine oil is put into quinizine quaternary ammonium sulfate preparing tank, finish, close quinizine oil tank bottom valve, open the 3rd water measuring tank bottom valve, water is added to quinizine quaternary ammonium sulfate preparing tank, regulate quinizine content and sulfuric acid content in quinizine quaternary ammonium sulfate, quinizine quaternary ammonium sulfate is put into reduction reaction can with Sodium Nitrite and is reacted, and reaction is finished; Open reduction tank bottom valve, be transferred to hydrolysis, neutralization tank by pipeline, be hydrolyzed, neutralization reaction.Leave standstill, 4-AA oil is sucked to 4-AA oil tank by stainless-steel vacuum pipe.Mother liquor proceeds to ammonium sulfate liquor tank.
The beneficial effects of the utility model are as follows:
The utility model technique is simple, consumes liquid caustic soda few, and when preparation quinizine quaternary ammonium sulfate, without sulfuric acid, sodium sulfate generation reduces, and discharges high COD sodium sulfate wastewater few, and the usage quantity of liquid caustic soda, sulfuric acid greatly reduces; Sodium sulfate, hc effluent quantity discharged reduce obviously, meet environmental friendliness, Green Chemistry characteristic attribute, and product yield is high.Atom utilization greatly improves; Avoid hydrolyzed solution under strong alkaline condition, to decompose destruction simultaneously, yield is increased than traditional technology; Because Sulpyrine, pyramidon belong to large tonnage product in China, use after this utility model technique economic benefit and social benefit obvious.
Accompanying drawing explanation
Fig. 1 the utility model production equipment figure.
In figure, 1, the first methyl-sulfate test tank, 2, the first pyrazolone feed bin, 3, first tank that methylates, 4, liquid caustic soda metering is filled with, 5, the first hydrolytic decomposition pot, 6, alkaline purification tank, 7, sodium sulfate mother liquor tank, 8, quinizine oil tank, 9, Sodium Nitrite metering is filled with, 10, nitrosation reaction tank, 11, ammonium sulfate liquor tank, 12, hydrolysis, neutralization tank, 13, 4-quinizine oil tank, 14, reduction reaction can, 15, quinizine quaternary ammonium sulfate batch tank, 16, water metering is filled with, 17, the second hydrolytic decomposition pot, 18, second tank that methylates, 19, the second water metering is filled with, 20, the second methyl-sulfate test tank, 21, the second pyrazolone feed bin, 22, the first water metering is filled with.
Embodiment
Below in conjunction with embodiment, the utility model is described in further detail.
Embodiment 1
As Fig. 1, the present embodiment 4-AA production equipment, comprise the first pyrazolone feed bin 2, the first pyrazolone feed bin 2 and the first methyl-sulfate test tank 1 are connected by pipeline and first tank 3 that methylates respectively, first tank 3 that methylates is connected with the first hydrolytic decomposition pot 5, the first hydrolytic decomposition pot 5 is connected with alkaline purification tank 6, and alkaline purification tank 6 is connected with quinizine oil tank 8; The second pyrazolone feed bin 21 and the second methyl-sulfate test tank 20 are connected by pipeline and second tank 18 that methylates respectively, second tank 18 that methylates is connected with the second hydrolytic decomposition pot 17, the second hydrolytic decomposition pot 17, quinizine oil tank 8, water metering are filled with 16 and are connected with quinizine quaternary ammonium sulfate batch tank 15 by pipeline respectively, quinizine quaternary ammonium sulfate batch tank 15 is connected with nitrosation reaction tank 10 by pipeline respectively with Sodium Nitrite metering filling 9, nitrosation reaction tank 10 is connected with reduction reaction can 14, and reduction reaction can 14 is connected with hydrolysis neutralization tank 12; The first hydrolytic decomposition pot 5 is filled with 4 by pipeline with liquid caustic soda metering and is connected.
The first water metering is filled with 22 and is connected with the first hydrolytic decomposition pot 5 by pipeline.
The second water metering is filled with 19 and is connected with the second hydrolytic decomposition pot 17 by pipeline.
Using method:
Pyrazolone is put into the first pyrazolone feed bin 2; Methyl-sulfate drops into the first methyl-sulfate test tank 1, opens the first tank 3 pyrazolone charging openings that methylate, and pyrazolone is entered to first tank 3 that methylates, and closes the first tank 3 pyrazolone charging openings that methylate; Open the first methyl-sulfate test tank 1 bottom valve, the first tank 3 methyl-sulfate feed valves that methylate, methyl-sulfate is added to first tank 3 that methylates, finish, close the first methyl-sulfate tank 1 bottom valve, first tank 3 feed valves that methylate, temperature reaction is complete, open first tank 3 bottom valves that methylate, the first hydrolytic decomposition pot 5 feed valves, the liquid that will methylate is put into the first hydrolytic decomposition pot 5, put completely, close first tank 3 bottom valves that methylate; Open the first water measuring tank 22 bottom valves, water is joined to the first hydrolytic decomposition pot 5, finish, close the first water measuring tank 5 bottom valves and the first hydrolytic decomposition pot 5 charging valves, the reaction that is hydrolyzed, hydrolysis is finished, open the first hydrolytic decomposition pot 5 bottom valves, alkaline purification tank 6 bottom valves, put into alkaline purification tank 6 by hydrolysis material and liquid caustic soda, and reaction is finished, lower floor's solution is put into sodium sulfate mother liquor tank 7 to be collected, open quinizine oil tank 8 feed valves, the upper strata quinizine oil of alkaline purification tank 6 is put into quinizine oil tank 8, for subsequent use;
Pyrazolone is put into the second pyrazolone feed bin 21; The pyrazolone that methyl-sulfate is squeezed into the second methyl-sulfate test tank 20, the second pyrazolone feed bins 21 enters second tank 18 that methylates, and closes the second tank 18 pyrazolone charging openings that methylate; Open the second methyl-sulfate test tank 20 bottom valves, second tank 18 feed valves that methylate, add second tank 18 that methylates by methyl-sulfate, finish, close the second methyl-sulfate tank 20 bottom valves, second tank 18 feed valves that methylate, temperature reaction, reacts complete, opens second tank 18 bottom valves that methylate, the second hydrolytic decomposition pot 17 feed valves, second liquid that methylates is put into the second hydrolytic decomposition pot 17, put completely, close second tank 18 bottom valves that methylate; Open the second water measuring tank 19 bottom valves, water is joined to the second hydrolytic decomposition pot 17, finish, close the second water measuring tank 19 bottom valves and the second hydrolytic decomposition pot 17 charging valves, the reaction that is hydrolyzed, hydrolysis is finished, for subsequent use;
Open the second hydrolytic decomposition pot 17 bottom valves, hydrolyzed solution is pressed into quinizine quaternary ammonium sulfate preparing tank 15, open quinizine oil tank 8 bottom valves quinizine oil is put into quinizine quaternary ammonium sulfate preparing tank 15, finish, close quinizine oil tank 8 bottom valves, open the 3rd water measuring tank 16 bottom valves, water is added to quinizine quaternary ammonium sulfate preparing tank 15, regulate quinizine content and sulfuric acid content in quinizine quaternary ammonium sulfate, quinizine quaternary ammonium sulfate is put into reduction reaction can 14 with Sodium Nitrite and is reacted, and reaction is finished; Open reduction reaction can 14 bottom valves, be transferred to hydrolysis, neutralization tank 12 by pipeline, be hydrolyzed, neutralization reaction, leave standstill, 4-AA oil is sucked to 4-AA oil tank 13 by valve tube, mother liquor proceeds to ammonium sulfate liquor tank 11.
Claims (6)
1. a 4-AA production equipment, comprise the first pyrazolone feed bin (2), it is characterized in that, the first pyrazolone feed bin (2) and the first methyl-sulfate test tank (1) are connected by pipeline and first tank (3) that methylates respectively, first tank (3) that methylates is connected with the first hydrolytic decomposition pot (5), the first hydrolytic decomposition pot (5) is connected with alkaline purification tank (6), and alkaline purification tank (6) is connected with quinizine oil tank (8), the second pyrazolone feed bin (21) and the second methyl-sulfate test tank (20) are connected by pipeline and second tank (18) that methylates respectively, second tank (18) that methylates is connected with the second hydrolytic decomposition pot (17), the second hydrolytic decomposition pot (17), quinizine oil tank (8), the 3rd water metering is filled with (16) and is connected with quinizine quaternary ammonium sulfate batch tank (15) by pipeline respectively, quinizine quaternary ammonium sulfate batch tank (15) is connected with nitrosation reaction tank (10) by pipeline respectively with Sodium Nitrite metering filling (9), nitrosation reaction tank (10) is connected with reduction reaction can (14), reduction reaction can (14) and hydrolysis, neutralization tank (12) connects, the first hydrolytic decomposition pot (5) is filled with (4) by pipeline with liquid caustic soda metering and is connected.
2. 4-AA production equipment according to claim 1, is characterized in that, hydrolysis, neutralization tank (12) are connected with ammonium sulfate liquor tank (11) and 4-quinizine oil tank (13) by pipeline respectively.
3. 4-AA production equipment according to claim 1, is characterized in that, the first water metering is filled with (22) and is connected with the first hydrolytic decomposition pot (5) by pipeline.
4. 4-AA production equipment according to claim 1, is characterized in that, the second water metering is filled with (19) and is connected with the second hydrolytic decomposition pot (17) by pipeline.
5. 4-AA production equipment according to claim 1, is characterized in that, alkaline purification tank (6) is connected with sodium sulfate mother liquor tank (7) by pipeline.
6. 4-AA production equipment according to claim 1, is characterized in that, valve is all set on each pipeline.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320803195.4U CN203625269U (en) | 2013-12-09 | 2013-12-09 | 4-amino-antipyrine production device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320803195.4U CN203625269U (en) | 2013-12-09 | 2013-12-09 | 4-amino-antipyrine production device |
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| Publication Number | Publication Date |
|---|---|
| CN203625269U true CN203625269U (en) | 2014-06-04 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201320803195.4U Withdrawn - After Issue CN203625269U (en) | 2013-12-09 | 2013-12-09 | 4-amino-antipyrine production device |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103613544A (en) * | 2013-12-09 | 2014-03-05 | 山东新华制药股份有限公司 | 4-aminoantipyrene production technology and device thereof |
| CN108958190A (en) * | 2018-07-10 | 2018-12-07 | 山东新华制药股份有限公司 | A kind of analgin controlling of production process system based on computer control |
| CN110526869A (en) * | 2019-08-29 | 2019-12-03 | 青岛科技大学 | A kind of continuous production system of 4-AA |
-
2013
- 2013-12-09 CN CN201320803195.4U patent/CN203625269U/en not_active Withdrawn - After Issue
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103613544A (en) * | 2013-12-09 | 2014-03-05 | 山东新华制药股份有限公司 | 4-aminoantipyrene production technology and device thereof |
| CN103613544B (en) * | 2013-12-09 | 2015-12-02 | 山东新华制药股份有限公司 | 4-AA production technique and device thereof |
| CN108958190A (en) * | 2018-07-10 | 2018-12-07 | 山东新华制药股份有限公司 | A kind of analgin controlling of production process system based on computer control |
| CN110526869A (en) * | 2019-08-29 | 2019-12-03 | 青岛科技大学 | A kind of continuous production system of 4-AA |
| CN110526869B (en) * | 2019-08-29 | 2022-06-28 | 青岛科技大学 | Continuous production system of 4-aminoantipyrine |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20140604 Effective date of abandoning: 20151202 |
|
| C25 | Abandonment of patent right or utility model to avoid double patenting |