CN106397284A - Purification process flow of 2-nitro-4-methylsulfonylbenzoic acid - Google Patents
Purification process flow of 2-nitro-4-methylsulfonylbenzoic acid Download PDFInfo
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- CN106397284A CN106397284A CN201610777012.4A CN201610777012A CN106397284A CN 106397284 A CN106397284 A CN 106397284A CN 201610777012 A CN201610777012 A CN 201610777012A CN 106397284 A CN106397284 A CN 106397284A
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- nitro
- benzoic acid
- flow process
- thiamphenicol benzoic
- filtrate
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C315/00—Preparation of sulfones; Preparation of sulfoxides
- C07C315/06—Separation; Purification; Stabilisation; Use of additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention discloses a purification process flow of 2-nitro-4-methylsulfonylbenzoic acid. In an alkalization kettle, the purification process flow of 2-nitro-4-methylsulfonylbenzoic acid comprises the steps of (1) sequentially adding a crude product, the common water and a liquid alkali into the alkalization kettle, stirring and subjecting the above materials to reaction so as to obtain a reaction product; (2) adding the reaction product in a filtration device for filtering the reaction product so as to obtain a filter cake and a filtrate; (3) adding hot hydrochloric acid into the filtrate, and putting the filtrate into a centrifuge device to obtain a finished product and a water solution; (4) drying the finished product in a drying chamber, then packaging and putting the finished product in storage; (5) adding the water solution in a sewage treatment device. According to the technical scheme of the invention, by means of the sewage treatment device, the sewage generated during the purification process can be processed. Therefore, the pollution is reduced and the environment is protected. Meanwhile, water is adopted to replace fatty acid, methanol and other solvents, so that the production cost is lowered. The corrosion to equipment is relieved. Moreover, the discharge of waste acid is reduced, and the clean production is realized. At the same time, the safety of the production process is improved.
Description
Technical field
The present invention relates to chemical products manufacture field, specially a kind of 2- nitro-to thiamphenicol benzoic acid purifying technique stream
Journey.
Background technology
2- nitryl-4-thiamphenicol benzoic acid, also known as adjacent nitro is to thiamphenicol benzoic acid, CAS No. is 110964-79-9；
English name is 2-Nitro-4-methylsulfonylbenzoic acid or O-Nitro-P-Methylsulfonyl
Benzoic Acid (referred to as NMSBA)；Molecular formula is C8H7NO6S, and molecular weight is 245.21, is white or yellowish under normal temperature
Color crystalline powder.2- nitryl-4-thiamphenicol benzoic acid is important organic synthesis intermediate, be widely used in dyestuff, medicine and
The production of agricultural chemicals.2- nitro is a kind of important medicinal intermediate to thiamphenicol benzoic acid.The benzene of 2- nitro -4- methylsulfonyltoluene
Two strong electron-withdrawing groups group is had on ring so that methyl oxidation is relatively difficult for carboxyl, and to the control of degree of oxidation also very
Difficult.At present, existing report is mainly divided by the method that 2- nitro -4- methylsulfonyltoluene prepares 2- nitryl-4-thiamphenicol benzoic acid
For chemical oxidization method and liquid phase oxygen (air) oxidizing process.Prepare this kind of benzoic acid containing multiple electron-withdrawing groups, generally will use
The toluene of the corresponding substituent of strong oxidizer nitric acid oxidation and obtain, because the difficult oxidation of the toluene containing electron-withdrawing group is still needed in five oxidations
Just can carry out under two vanadium catalysis.
But existing 2- nitro-and in thiamphenicol benzoic acid purifying technique, quality cannot be protected with efficiency, and adopts
With fat acid and methyl alcohol equal solvent, improve production cost, the corrosion to equipment is big, and in purification process, can produce a large amount of
Sewage, pollute environment, be unfavorable for our popularization and use.
Content of the invention
It is an object of the invention to provide a kind of 2- nitro-to thiamphenicol benzoic acid purifying technique flow process, above-mentioned to solve
The problem proposing in background technology.
For achieving the above object, the present invention provides following technical scheme：A kind of 2- nitro-work is purified to thiamphenicol benzoic acid
Skill flow process, described alkalization kettle, described 2- nitro-be to thiamphenicol benzoic acid purifying technique flow process：
(1) first crude product, ordinary water, liquid caustic soda are sequentially placed in alkalization kettle and are stirred reacting, obtain reactant；
(2) reactant is put in filter and filtered, obtain filter cake and filtrate；
(3) heat hydrochloric acid in filtrate, be then placed in centrifugal device, obtain finished product and solution water；
(4) place products into drying chamber, then carry out packing into storehouse；
(5) solution water is put in sewage-treatment plant.
Further, the capacity of described alkalization kettle is 2000L.
Further, described crude product be 2- nitro-to after thiamphenicol benzoic acid oxidation technology produce raw material.
Further, described 2- nitro-in thiamphenicol benzoic acid purifying technique flow process (2), will be anti-using vacuum mode
Thing is answered to carry out putting in filter.
Compared with prior art, the invention has the beneficial effects as follows：
A kind of 2- nitro of the present invention-and to thiamphenicol benzoic acid purifying technique flow process, it is provided by sewage-treatment plant,
The sewage producing in purification process can be processed, reduce pollution, protect environment, aliphatic acid and methyl alcohol be replaced with water simultaneously
Equal solvent, not only greatly reduces production cost, reduces the corrosion to equipment, and also reduces the discharge of spent acid, meets clear
Clean produces, and also improves the security in production process simultaneously.
Brief description
Fig. 1 is present invention process schematic flow sheet,
Specific embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation description is it is clear that described embodiment is only a part of embodiment of the present invention, rather than whole embodiments.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of not making creative work
Embodiment, broadly falls into the scope of protection of the invention.
Refer to Fig. 1, the present invention provides a kind of technical scheme：A kind of 2- nitro-to thiamphenicol benzoic acid purifying technique stream
Journey, described alkalization kettle, described 2- nitro-be to thiamphenicol benzoic acid purifying technique flow process：
(1) first crude product, ordinary water, liquid caustic soda are sequentially placed in alkalization kettle and are stirred reacting, obtain reactant；
(2) reactant is put in filter and filtered, obtain filter cake and filtrate；
(3) heat hydrochloric acid in filtrate, be then placed in centrifugal device, obtain finished product and solution water；
(4) place products into drying chamber, then carry out packing into storehouse；
(5) solution water is put in sewage-treatment plant.
The capacity of described alkalization kettle is 2000L.
Described crude product be 2- nitro-to after thiamphenicol benzoic acid oxidation technology produce raw material.
Described 2- nitro-and in thiamphenicol benzoic acid purifying technique flow process (2), using vacuum mode, reactant is put
Enter in filter.
In sum, the present invention is provided by sewage-treatment plant, can process the sewage producing in purification process,
Reduce pollution, protect environment, aliphatic acid and methyl alcohol equal solvent are replaced with water simultaneously, not only greatly reduce production cost,
Reduce the corrosion to equipment, and also reduce the discharge of spent acid, meet cleanly production, also improve in production process simultaneously
Security.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, permissible
Understand and can carry out multiple changes, modification, replacement to these embodiments without departing from the principles and spirit of the present invention
And modification, the scope of the present invention be defined by the appended.
Claims (4)
1. a kind of 2- nitro-to thiamphenicol benzoic acid purifying technique flow process it is characterised in that：Described alkalization kettle, described 2- nitro-
To thiamphenicol benzoic acid purifying technique flow process it is：
(1) first crude product, ordinary water, liquid caustic soda are sequentially placed in alkalization kettle and are stirred reacting, obtain reactant；
(2) reactant is put in filter and filtered, obtain filter cake and filtrate；
(3) heat hydrochloric acid in filtrate, be then placed in centrifugal device, obtain finished product and solution water；
(4) place products into drying chamber, then carry out packing into storehouse；
(5) solution water is put in sewage-treatment plant.
2. a kind of 2- nitro according to claim 1-to thiamphenicol benzoic acid purifying technique flow process it is characterised in that：Institute
The capacity stating alkalization kettle is 2000L.
3. a kind of 2- nitro according to claim 1-to thiamphenicol benzoic acid purifying technique flow process it is characterised in that：Institute
State crude product be 2- nitro-to after thiamphenicol benzoic acid oxidation technology produce raw material.
4. a kind of 2- nitro according to claim 1-to thiamphenicol benzoic acid purifying technique flow process it is characterised in that：Institute
State 2- nitro-in thiamphenicol benzoic acid purifying technique flow process (2), carry out putting into filter by reactant using vacuum mode
In.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610777012.4A CN106397284A (en) | 2016-08-30 | 2016-08-30 | Purification process flow of 2-nitro-4-methylsulfonylbenzoic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610777012.4A CN106397284A (en) | 2016-08-30 | 2016-08-30 | Purification process flow of 2-nitro-4-methylsulfonylbenzoic acid |
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| CN106397284A true CN106397284A (en) | 2017-02-15 |
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|---|---|---|---|
| CN201610777012.4A Pending CN106397284A (en) | 2016-08-30 | 2016-08-30 | Purification process flow of 2-nitro-4-methylsulfonylbenzoic acid |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4781750A (en) * | 1985-08-27 | 1988-11-01 | Rohm And Haas Company | Herbicidally active enols |
| CN1038584C (en) * | 1992-10-19 | 1998-06-03 | Basf公司 | Preparation of methylsulfonylbenzoic acids |
| CN101921215A (en) * | 2010-08-20 | 2010-12-22 | 安吉豪森药业有限公司 | Method for producing 2-nitro-p-methylsullfonyl benzoic acid |
-
2016
- 2016-08-30 CN CN201610777012.4A patent/CN106397284A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4781750A (en) * | 1985-08-27 | 1988-11-01 | Rohm And Haas Company | Herbicidally active enols |
| CN1038584C (en) * | 1992-10-19 | 1998-06-03 | Basf公司 | Preparation of methylsulfonylbenzoic acids |
| CN101921215A (en) * | 2010-08-20 | 2010-12-22 | 安吉豪森药业有限公司 | Method for producing 2-nitro-p-methylsullfonyl benzoic acid |
Non-Patent Citations (3)
| Title |
|---|
| 来虎钦 等: "2-硝基-4-甲磺酰基苯甲酸的绿色合成研究", 《浙江工业大学学报》 * |
| 杨剑波 等: "硝磺酮的合成与除草效果", 《农药》 * |
| 高学彦 等: "2-硝基-4-甲磺酰基苯甲酸的合成研究", 《化学试剂》 * |
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| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170215 |
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| RJ01 | Rejection of invention patent application after publication |