CN108117500A - It is a kind of to reduce the method that aminating reaction technique generates waste water abraum salt in ammonia sulphur methyl esters production process - Google Patents
It is a kind of to reduce the method that aminating reaction technique generates waste water abraum salt in ammonia sulphur methyl esters production process Download PDFInfo
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- CN108117500A CN108117500A CN201711193677.1A CN201711193677A CN108117500A CN 108117500 A CN108117500 A CN 108117500A CN 201711193677 A CN201711193677 A CN 201711193677A CN 108117500 A CN108117500 A CN 108117500A
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- ammonia
- waste water
- aminating reaction
- abraum salt
- methyl esters
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/36—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of amides of sulfonic acids
- C07C303/38—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of amides of sulfonic acids by reaction of ammonia or amines with sulfonic acids, or with esters, anhydrides, or halides thereof
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/42—Separation; Purification; Stabilisation; Use of additives
- C07C303/44—Separation; Purification
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention discloses a kind of method for reducing aminating reaction technique generation waste water abraum salt in ammonia sulphur methyl esters production process, after aminating reaction, most of ammonia is blown out by reaction kettle using the method for brushing, recycling is reused, residue is used in a small amount of hydrochloric acid and is acidified, and is realized and is reduced generation waste water abraum salt.The present invention's reduces the method that aminating reaction technique generates waste water abraum salt in ammonia sulphur methyl esters production process, it is simple for process, step is few, easy to operate and control is driven out of most of ammonia using brushing method after aminating reaction, and residue is in a small amount of hydrochloric acid is used and is acidified, the ammonium hydroxide driven out of absorbs rear enclosure through spray column and is used for subsequent batches aminating reaction, it effectively reduces and generates waste water abraum salt, energy conservation and environmental protection has good economic benefit.
Description
Technical field
The invention belongs to medicine synthesising process technical fields, and in particular to ammonification in a kind of reduction ammonia sulphur methyl esters production process
The method that reaction process generates waste water abraum salt.
Background technology
In Sulpiride intermediate ammonia sulphur methyl esters production process, aminating reaction technical process, reaction uses substantial amounts of ammonium hydroxide,
Original post processing can generate substantial amounts of waste water abraum salt, very big trouble is brought to post processing, not only cause resource unrestrained to adjust acid out brilliant
Take, also result in that increased production cost and generate substantial amounts of environmental pollution, it is impossible to meet use demand.
The content of the invention
Goal of the invention：In view of the deficienciess of the prior art, the object of the present invention is to provide a kind of reduction ammonia sulphur methyl esters lifes
The method that aminating reaction technique generates waste water abraum salt during production, simple with method, step is few, effectively reduces generation waste water and gives up
The advantages that salt.
Technical solution：In order to realize foregoing invention purpose, the technical solution adopted by the present invention is as follows：
It is a kind of to reduce the method that aminating reaction technique generates waste water abraum salt in ammonia sulphur methyl esters production process：In aminating reaction knot
Most of ammonia is blown out reaction kettle by Shu Hou using the method for brushing, and recycling is reused, and residue uses in a small amount of hydrochloric acid and acid
Change, realize and reduce generation waste water abraum salt.
Described reduces the method that aminating reaction technique generates waste water abraum salt in ammonia sulphur methyl esters production process, using the method for brushing
70% ammonia is at least blown out into reaction kettle.
Described reduces the method that aminating reaction technique generates waste water abraum salt in ammonia sulphur methyl esters production process, the ammonia of blowout
The aminating reaction of subsequent batches is back to after spray column absorbs.
The aminating reaction, process are as follows：
I 25% ammonium hydroxide for) inhaling proportional quantity is put into ammoniation kettle；
II) open cooling water into, return valve, be slowly added into benzoyl under stirring, control temperature is less than 20 DEG C, after adding, covers
Good feeding port overflows to prevent ammonia；
III) close into, return cooling water valve, slowly open into, return steam valve, temperature in the kettle is allowed to be maintained at 70-75 DEG C about
1.5 it is small when, reaction terminates, and the method for brushing catches up with ammonia, and ammonia is through spray column recovery；Ammonia is caught up with to terminate, close steam into, return valve, open
Cooling water into, return valve, reaction temperature is made to be down to 30 ± 2 DEG C；
IV vacuum pump) is opened, then inhalation of hydrochloric acid adds salt acid for adjusting pH value to control and add to 1.0-1.5 into reaction solution
Sour speed, temperature are no more than 50 DEG C；Acid out terminates, and temperature is risen to 98 ± 2 DEG C, and keeps the temperature 15 minutes, and continuing stirring makes reaction
Liquid temperature degree is down to room temperature, then stops to stir, and puts into, returns cooling water valve, when standing 2 is small；
V) stand and terminate to start to centrifuge, filter cake is rinsed with drinking water to pH 3-4, and filter cake is smashed and puts baking oven, in 83-87
It is DEG C dry 22 it is small when obtain amide.
The mass ratio of the aminating reaction, benzoyl and 25% ammonium hydroxide is 1：1.7.
Advantageous effect：Compared with prior art, aminating reaction technique is produced in reduction ammonia sulphur methyl esters production process of the invention
The method of raw waste water abraum salt, simple for process, step is few, easy to operate and control, will be most of using method of brushing after aminating reaction
Ammonia is driven out of, and residue is in a small amount of hydrochloric acid is used and is acidified, and the ammonium hydroxide driven out of absorbs rear enclosure through spray column and is used for subsequent batches
Aminating reaction, effectively reduces and generates waste water abraum salt, and energy conservation and environmental protection has good economic benefit.
Specific embodiment
With reference to specific embodiment, the present invention is furture elucidated, and embodiment is under based on the technical solution of the present invention
Implemented, it should be understood that these embodiments are only illustrative of the invention and is not intended to limit the scope of the invention.
Embodiment 1
A kind of to reduce the method that aminating reaction technique generates waste water abraum salt in ammonia sulphur methyl esters production process, step is as follows：
1st, the preparation (abbreviation amide) of 2- methoxyl groups -5- sulfamoylbenzoic acids
Raw material proportioning：Benzoyl 1Kg, 25% ammonium hydroxide 1.7Kg.
Aminating reaction, process are as follows：
I 25% ammonium hydroxide for) inhaling proportional quantity is put into ammoniation kettle.
II) open cooling water into, return valve, be slowly added into benzoyl under stirring, control temperature is less than 20 DEG C, after adding, covers
Good feeding port overflows to prevent ammonia.
III) close into, return cooling water valve, slowly open into, return steam valve, temperature in the kettle is allowed to be maintained at 70-75 DEG C about
1.5 it is small when, reaction terminates, and the method for brushing catches up with ammonia, and ammonia is through spray column recovery.Ammonia is caught up with to terminate, close steam into, return valve, open
Cooling water into, return valve, reaction temperature is made to be down to 30 ± 2 DEG C.
IV vacuum pump) is opened, then inhalation of hydrochloric acid adds salt acid for adjusting pH value to control and add to 1.0-1.5 into reaction solution
Sour speed, being no more than 50 DEG C with temperature is advisable.Acid out terminates, and temperature is risen to 98 ± 2 DEG C, and keeps the temperature 15 minutes, continues to stir
Reacting liquid temperature is made to be down to room temperature, then stops to stir, put into, return cooling water valve, stand 2 it is small when (can it is crack into, return cooling water
Valve keeps dwell temperature at 25~35 DEG C).
V) stand and terminate to start to centrifuge, filter cake is rinsed with drinking water to pH 3-4, and filter cake is smashed and puts baking oven, in 83-87
It is DEG C dry 22 it is small when obtain amide.Yield is 65-75%.
The analysis of decrement：Aminating reaction 1mol benzoyls need to consume 2mol ammonia, and the amount that 1kg benzoyls need to consume ammonia is
0.136kg is actually added into the amount of ammonia as 0.425kg, and ammonia is significantly excessive.Abraum salt caused by acid treatment is directly adjusted according to post processing
The amount of ammonium chloride is 0.91kg, and the amount for actually brushing rear generated abraum salt ammonium chloride is 0.273kg, and 1t benzoyls carry out ammonification and are
637kg abraum salts can be reduced.
Ammonia sulphur methyl esters year factory's amount >=100t of the applicant, this process can reduce abraum salt 55t every year, reduce abraum salt landfill warp
Take 14.3 ten thousand yuan, while reduce the dosage of hydrochloric acid, this brushes technique all has very big benefit for environmental protection or cost reduction
Place.
Claims (5)
1. a kind of reduce the method that aminating reaction technique generates waste water abraum salt in ammonia sulphur methyl esters production process, it is characterised in that：
After aminating reaction, most of ammonia is blown out by reaction kettle using the method for brushing, recycling is reused, and residue uses a small amount of salt
Acid neutralizes acidifying, realizes that reduction generates waste water abraum salt.
2. the side according to claim 1 for reducing aminating reaction technique in ammonia sulphur methyl esters production process and generating waste water abraum salt
Method, which is characterized in that 70% ammonia is at least blown out by reaction kettle using method of brushing.
3. the side according to claim 1 for reducing aminating reaction technique in ammonia sulphur methyl esters production process and generating waste water abraum salt
Method, which is characterized in that the ammonia of blowout is back to the aminating reaction of subsequent batches after spray column absorbs.
4. the side according to claim 1 for reducing aminating reaction technique in ammonia sulphur methyl esters production process and generating waste water abraum salt
Method, which is characterized in that the aminating reaction, process are as follows：
I 25% ammonium hydroxide for) inhaling proportional quantity is put into ammoniation kettle；
II) open cooling water into, return valve, be slowly added into benzoyl under stirring, control temperature after adding, covers throwing below 20 DEG C
Material mouth is overflowed to prevent ammonia；
III) close into, return cooling water valve, slowly open into, return steam valve, temperature in the kettle is allowed to be maintained at 70-75 DEG C about 1.5 small
When, reaction terminates, and the method for brushing catches up with ammonia, and ammonia is through spray column recovery；Ammonia is caught up with to terminate, close steam into, return valve, open cooling water
Into, return valve, reaction temperature is made to be down to 30 ± 2 DEG C；
IV vacuum pump) is opened, then inhalation of hydrochloric acid adds salt acid for adjusting pH value to control acid adding speed to 1.0-1.5 into reaction solution
Degree, temperature are no more than 50 DEG C；Acid out terminates, and temperature is risen to 98 ± 2 DEG C, and keeps the temperature 15 minutes, and continuing stirring makes reaction liquid temperature
Degree is down to room temperature, then stops to stir, and puts into, returns cooling water valve, when standing 2 is small；
V) stand and terminate to start to centrifuge, filter cake is rinsed with drinking water to pH 3-4, and filter cake is smashed and puts baking oven, dry in 83-87 DEG C
It is dry 22 it is small when obtain amide.
5. the side according to claim 4 for reducing aminating reaction technique in ammonia sulphur methyl esters production process and generating waste water abraum salt
Method, which is characterized in that the mass ratio of benzoyl and 25% ammonium hydroxide is 1：1.7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711193677.1A CN108117500B (en) | 2017-11-24 | 2017-11-24 | Method for reducing waste water and waste salt generated in amination process in production process of methyl sulfamate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711193677.1A CN108117500B (en) | 2017-11-24 | 2017-11-24 | Method for reducing waste water and waste salt generated in amination process in production process of methyl sulfamate |
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| CN108117500A true CN108117500A (en) | 2018-06-05 |
| CN108117500B CN108117500B (en) | 2020-08-18 |
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Citations (7)
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| CN102320997A (en) * | 2011-08-05 | 2012-01-18 | 丁同富 | Para-acetylsulfanilamide synthesis method combined with waste water treatment |
| CN102659277A (en) * | 2012-05-10 | 2012-09-12 | 杭州蓝然环境技术有限公司 | Ammonium fluoride wastewater treatment technique |
| CN103318918A (en) * | 2013-05-14 | 2013-09-25 | 武汉百富环保工程有限公司 | Method for purification and recovery of ammonia gas |
| CN203469550U (en) * | 2013-08-20 | 2014-03-12 | 中芯国际集成电路制造(北京)有限公司 | Liquid waste disposal device |
| CN104672114A (en) * | 2013-11-26 | 2015-06-03 | 门修信 | A preparing method of 2,4-dichloro-5-sulfamoylbenzoic acid |
| CN104725282A (en) * | 2014-07-17 | 2015-06-24 | 叶良梅 | Novel environment-friendly production process of 1-naphthol-4-sulfonic acid |
| CN105017098A (en) * | 2015-07-17 | 2015-11-04 | 大连奇凯医药科技有限公司 | Preparation technology of alkyloxybenzsulfamide and its derivatives |
-
2017
- 2017-11-24 CN CN201711193677.1A patent/CN108117500B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320997A (en) * | 2011-08-05 | 2012-01-18 | 丁同富 | Para-acetylsulfanilamide synthesis method combined with waste water treatment |
| CN102659277A (en) * | 2012-05-10 | 2012-09-12 | 杭州蓝然环境技术有限公司 | Ammonium fluoride wastewater treatment technique |
| CN103318918A (en) * | 2013-05-14 | 2013-09-25 | 武汉百富环保工程有限公司 | Method for purification and recovery of ammonia gas |
| CN203469550U (en) * | 2013-08-20 | 2014-03-12 | 中芯国际集成电路制造(北京)有限公司 | Liquid waste disposal device |
| CN104672114A (en) * | 2013-11-26 | 2015-06-03 | 门修信 | A preparing method of 2,4-dichloro-5-sulfamoylbenzoic acid |
| CN104725282A (en) * | 2014-07-17 | 2015-06-24 | 叶良梅 | Novel environment-friendly production process of 1-naphthol-4-sulfonic acid |
| CN105017098A (en) * | 2015-07-17 | 2015-11-04 | 大连奇凯医药科技有限公司 | Preparation technology of alkyloxybenzsulfamide and its derivatives |
Non-Patent Citations (1)
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| MARC W. HARROLD等: "Synthesis and D2 Dopaminergic Activity of Pyrrolidinium,Tetrahydrothiophenium, and Tetrahydrothiophene Analogues of Sulpiride", 《J.MED.CHEM.》 * |
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