CN104058953A - Production technique for synthesizing 2-bromopropionyl chloride - Google Patents
Production technique for synthesizing 2-bromopropionyl chloride Download PDFInfo
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- CN104058953A CN104058953A CN201410245112.3A CN201410245112A CN104058953A CN 104058953 A CN104058953 A CN 104058953A CN 201410245112 A CN201410245112 A CN 201410245112A CN 104058953 A CN104058953 A CN 104058953A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/58—Preparation of carboxylic acid halides
- C07C51/62—Preparation of carboxylic acid halides by reactions not involving the carboxylic acid halide group
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/58—Preparation of carboxylic acid halides
- C07C51/60—Preparation of carboxylic acid halides by conversion of carboxylic acids or their anhydrides or esters, lactones, salts into halides with the same carboxylic acid part
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a production technique for synthesizing 2-bromopropionyl chloride, relating to the technical field of chemical engineering. The production technique comprises the following steps: reacting thionyl chloride and propionic acid, cooling, adding red phosphorus and dry bromine, reacting, and finally, rectifying in a rectification tower. The production technique has the advantages of convenient and simple preparation process, environmental protection, no pollution, accessible raw materials and low equipment investment, and is convenient for operation; and the prepared 2-bromopropionyl chloride has the advantages of high purity, favorable use effect and high safety and reliability.
Description
Technical field
The present invention relates to chemical technology field, be specifically related to the synthetic production technique of a kind of 2-bromo propionyl chloro.
Background technology
2-bromo propionyl chloro is that outward appearance is micro-yellow, fusing point: 86-90 DEG C, boiling point: 131-133 DEG C, flash-point: 125 ℉, density: 1.7g/ml, 2-bromo propionyl chloro is a kind of very important intermediate, it is applied in and in agricultural chemicals, is mainly used to synthetic oxazole alkanes agricultural chemicals and dithiocarbamate herbicide intermediate, in fuel, be mainly used to the synthetic chromotrichial reactive dyestuffs of sheep that are applied to, be used for producing pyrrolidines medicine at field of medicaments, but at present still more traditional mode of the method for industrial production 2-bromo propionyl chloro, in this traditional production method, exist yield low, the problems such as not high pollution of purity is serious, and production technique is comparatively complicated, be difficult to meet human wants.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of purity high, the synthetic production technique of the simple 2-bromo propionyl chloro of preparation technology.
Technical problem to be solved by this invention realizes by the following technical solutions:
The production technique that 2-bromo propionyl chloro is synthetic, is characterized in that: comprise following processing step,
A. choose the reactor of a 1000L and add the new sulfur oxychloride 350-450kg steaming in reactor, then pass into steam heating heating direct to the post-heating that seethes with excitement by chuck and stop.
B. carry out back flow reaction to the propionic acid that drips 200-300kg in the reaction feed liquid in step a, discharge the sulfurous gas and the hydrogen chloride gas that in back flow reaction, generate.
C. when passing into cold water by chuck after the reaction feed liquid back flow reaction 1.0h in step b, until feed liquid is cooled to 35-45 DEG C.
D. will in cooled feed liquid in above-mentioned steps c, add 20-30kg red phosphorus, be again heated to after 85-95 DEG C and drip dry bromine 450-550kg again, controlling time for adding is that 5.0h continues to reflux.
E. undertaken after back flow reaction 6.5-7.5h reacting feed liquid in above-mentioned steps d, feed liquid is all thrown in to rectifying tower and carried out rectifying.
F. the cut of collecting 130-133 DEG C after the product after above-mentioned rectifying being dried is 2-bromo propionyl chloro finished product packing warehouse-in.
Described reactor all adopts bromination enamel reaction still, and on reactor, is furnished with agitator and chuck.
The sulfurous gas of discharging in described step b and hydrogen chloride gas adopt tail gas to force to absorb and process.
The invention has the beneficial effects as follows: the present invention is easy to prepare simple, and environment friendly and pollution-free, raw material is easy to get, and facility investment is few, and purity is high, convenient operation, the 2-bromo propionyl chloro result of use of preparation is good, safe and reliable.
Embodiment
For technique means, creation characteristic that the present invention is realized, reach object and effect is easy to understand, below in conjunction with specific embodiment, further set forth the present invention.
Embodiment 1
The production technique that 2-bromo propionyl chloro is synthetic, comprises following processing step,
A. choose the bromination enamel reaction still of a 1000L and add the new sulfur oxychloride 350kg steaming in reactor, then pass into steam heating heating direct to the post-heating that seethes with excitement by chuck and stop.
B. carry out back flow reaction to the propionic acid that drips 200kg in the reaction feed liquid in step a, discharge the sulfurous gas and the hydrogen chloride gas that in back flow reaction, generate, the sulfurous gas of discharge and hydrogen chloride gas adopt tail gas to force to absorb and process.
C. when passing into cold water by chuck after the reaction feed liquid back flow reaction 1.0h in step b, until feed liquid is cooled to 35 DEG C.
D. will in cooled feed liquid in above-mentioned steps c, add 20kg red phosphorus, be again heated to after 85 DEG C and drip dry bromine 450kg again, controlling time for adding is that 5.0h continues to reflux.
E. undertaken after back flow reaction 6.5h reacting feed liquid in above-mentioned steps d, feed liquid is all thrown in to rectifying tower and carried out rectifying.
F. the cut of collecting 130 DEG C after the product after above-mentioned rectifying being dried is 2-bromo propionyl chloro finished product packing warehouse-in.
Embodiment 2
The production technique that 2-bromo propionyl chloro is synthetic, comprises following processing step,
A. choose the bromination enamel reaction still of a 1000L and add the new sulfur oxychloride 400kg steaming in reactor, then pass into steam heating heating direct to the post-heating that seethes with excitement by chuck and stop.
B. carry out back flow reaction to the propionic acid that drips 250kg in the reaction feed liquid in step a, discharge the sulfurous gas and the hydrogen chloride gas that in back flow reaction, generate, the sulfurous gas of discharge and hydrogen chloride gas adopt tail gas to force to absorb and process.
C. when passing into cold water by chuck after the reaction feed liquid back flow reaction 1.0h in step b, until feed liquid is cooled to 40 DEG C.
D. will in cooled feed liquid in above-mentioned steps c, add 25kg red phosphorus, be again heated to after 90 DEG C and drip dry bromine 500kg again, controlling time for adding is that 5.0h continues to reflux.
E. undertaken after back flow reaction 7.0h reacting feed liquid in above-mentioned steps d, feed liquid is all thrown in to rectifying tower and carried out rectifying.
F. the cut of collecting 133 DEG C after the product after above-mentioned rectifying being dried is 2-bromo propionyl chloro finished product packing warehouse-in.
More than show and described ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (3)
1. the synthetic production technique of 2-bromo propionyl chloro, is characterized in that: comprise following processing step,
A. choose the reactor of a 1000L and add the new sulfur oxychloride 350-450kg steaming in reactor, then pass into steam heating heating direct to the post-heating that seethes with excitement by chuck and stop.
B. carry out back flow reaction to the propionic acid that drips 200-300kg in the reaction feed liquid in step a, discharge the sulfurous gas and the hydrogen chloride gas that in back flow reaction, generate.
C. when passing into cold water by chuck after the reaction feed liquid back flow reaction 1.0h in step b, until feed liquid is cooled to 35-45 DEG C.
D. will in cooled feed liquid in above-mentioned steps c, add 20-30kg red phosphorus, be again heated to after 85-95 DEG C and drip dry bromine 450-550kg again, controlling time for adding is that 5.0h continues to reflux.
E. undertaken after back flow reaction 6.5-7.5h reacting feed liquid in above-mentioned steps d, feed liquid is all thrown in to rectifying tower and carried out rectifying.
F. the cut of collecting 130-133 DEG C after the product after above-mentioned rectifying being dried is 2-bromo propionyl chloro finished product packing warehouse-in.
2. the synthetic production technique of a kind of 2-bromo propionyl chloro according to claim 1: it is characterized in that: described reactor all adopts bromination enamel reaction still, and be furnished with agitator and chuck on reactor.
3. the synthetic production technique of a kind of 2-bromo propionyl chloro according to claim 1: it is characterized in that: the sulfurous gas of discharging in described step b and hydrogen chloride gas adopt tail gas to force to absorb and process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410245112.3A CN104058953A (en) | 2014-06-04 | 2014-06-04 | Production technique for synthesizing 2-bromopropionyl chloride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410245112.3A CN104058953A (en) | 2014-06-04 | 2014-06-04 | Production technique for synthesizing 2-bromopropionyl chloride |
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| CN104058953A true CN104058953A (en) | 2014-09-24 |
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| CN201410245112.3A Pending CN104058953A (en) | 2014-06-04 | 2014-06-04 | Production technique for synthesizing 2-bromopropionyl chloride |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108997110A (en) * | 2018-07-10 | 2018-12-14 | 盐城市胜达化工有限公司 | A kind of method of silver bicarbonate activation 2- bromo propionyl chloro |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5612336A (en) * | 1979-07-10 | 1981-02-06 | Seitetsu Kagaku Co Ltd | Preparation of alpha-bromocarboxylic acid halide |
| CN103804191A (en) * | 2014-01-23 | 2014-05-21 | 安徽华润涂料有限公司 | Production technology for synthesis of ethyl 2-bromopropionate |
-
2014
- 2014-06-04 CN CN201410245112.3A patent/CN104058953A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5612336A (en) * | 1979-07-10 | 1981-02-06 | Seitetsu Kagaku Co Ltd | Preparation of alpha-bromocarboxylic acid halide |
| CN103804191A (en) * | 2014-01-23 | 2014-05-21 | 安徽华润涂料有限公司 | Production technology for synthesis of ethyl 2-bromopropionate |
Non-Patent Citations (1)
| Title |
|---|
| 王东阳等: ""硫普罗宁的合成工艺改进"", 《中国药物化学杂志》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108997110A (en) * | 2018-07-10 | 2018-12-14 | 盐城市胜达化工有限公司 | A kind of method of silver bicarbonate activation 2- bromo propionyl chloro |
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Application publication date: 20140924 |