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Method of activating 2-bromopropionyl chloride by silver bicarbonate

A technology of silver bicarbonate and bromopropionyl chloride, which is applied in the chemical field, can solve problems affecting the use effect, complex production process, and large-scale production constraints, and achieve good use effect, high purity, and less by-products

Inactive Publication Date: 2018-12-14
盐城市胜达化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] 2-bromopropionyl chloride is slightly yellow in appearance, melting point: 86-90°C, boiling point: 131-133°C, flash point: 125°F, density: 1.7g / ml, 2-bromopropionyl chloride is a very important intermediate It is used in pesticides to synthesize intermediates of oxazolidine pesticides and thiocarbamate herbicides, in fuels to synthesize reactive dyes used in wool coloring, and in the pharmaceutical field to produce pyrrole Alkanes drugs, but the current industrial production method of 2-bromopropionyl chloride is still a relatively traditional way, there are problems such as low yield, low purity and serious pollution in this traditional production method, and the production process is relatively complicated, it is difficult to comply with human needs
[0003] In addition, bromine-containing chemical intermediates or medical intermediates will decompose in a small amount. After decomposition, their activity will decrease, which will affect the use effect. From the perspective of industrial scale, the characteristics of the above methods will restrict large-scale production to a certain extent, which is not conducive to industrialization.

Method used

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  • Method of activating 2-bromopropionyl chloride by silver bicarbonate

Examples

Experimental program
Comparison scheme
Effect test

specific Embodiment 1

[0039] a. Select a 1000L reactor in actual use and add 350kg of freshly steamed thionyl chloride into the reactor, then heat up by steam heating until boiling and stop heating;

[0040] B. in the reaction feed liquid in the step a, drip the propionic acid of 200kg and carry out reflux reaction, discharge the sulfur dioxide and hydrogen chloride gas that generate in the back flow reaction, the sulfur dioxide and hydrogen chloride gas that discharge adopt tail gas forced absorption process.

[0041] c. After the reaction feed liquid in step b was refluxed for 1 hour, cold water was introduced until the feed liquid was cooled to 35°C.

[0042] d. Add 20kg of red phosphorus to the cooled feed liquid in the above step c, heat up to 85°C again, then add 450kg of dry bromine dropwise, and control the dropping time to 5h to continue reflux.

[0043] e. Simultaneously add silver bicarbonate powder to react.

[0044] f. After carrying out the reflux reaction of the reaction feed liquid...

specific Embodiment 2

[0047] a. In actual use, select a 1000L reactor and add 400kg of freshly steamed thionyl chloride to the reactor, then heat it up with steam until it boils and stop heating;

[0048] b. Add 250kg of propionic acid to the reaction feed liquid in step a to carry out reflux reaction, discharge the sulfur dioxide and hydrogen chloride gas generated in the reflux reaction, and the discharged sulfur dioxide and hydrogen chloride gas are treated by forced absorption of tail gas.

[0049] c. The reaction feed liquid in step b was refluxed for 1 hour and then passed into cold water until the feed liquid was cooled to 45°C.

[0050] d. Add 25kg of red phosphorus to the cooled feed liquid in the above step c, heat up to 90°C again, then add 550kg of dry bromine dropwise, and control the dropping time to 5h to continue reflux.

[0051] e. Simultaneously add silver bicarbonate powder to react.

[0052] f. After carrying out the reflux reaction of the reaction feed liquid in the above step...

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Abstract

The invention discloses a method of activating 2-bromopropionyl chloride by silver bicarbonate. The method comprises the following steps: adding thionyl chloride into a reaction kettle; heating the reaction kettle to react; adding propionic acid for a reflux reaction; adding red phosphorus and dried bromine after cooling to react again; adding silver bicarbonate powder; finally, inputting the mixture into a rectifying tower to be rectified and dried to obtain a product 2-bromopropionyl chloride; and then adding silver bicarbonate powder to obtain the product 2-bromopropionyl chloride which ishigh in activity and is unlikely to decompose. By adding the silver bicarbonate powder to remove residual bromine ions, the product is active, unlikely to decompose, environmentally friendly and pollution-free, small in equipment investment, high in purity and easy to operate, raw materials are easily available, and the prepared 2-bromopropionyl chloride is good in using effect and safe and reliable.

Description

technical field [0001] The invention relates to the chemical field, in particular to a method for activating 2-bromopropionyl chloride with silver bicarbonate. Background technique [0002] 2-bromopropionyl chloride is slightly yellow in appearance, melting point: 86-90°C, boiling point: 131-133°C, flash point: 125°F, density: 1.7g / ml, 2-bromopropionyl chloride is a very important intermediate It is used in pesticides to synthesize intermediates of oxazolidine pesticides and thiocarbamate herbicides, in fuels to synthesize reactive dyes used in wool coloring, and in the pharmaceutical field to produce pyrrole Alkanes drugs, but the current industrial production method of 2-bromopropionyl chloride is still a relatively traditional way, there are problems such as low yield, low purity and serious pollution in this traditional production method, and the production process is relatively complicated, it is difficult to comply with human demand. [0003] In addition, bromine-con...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/60C07C51/62C07C53/50
CPCC07C51/60C07C51/62C07C53/50
Inventor 陈士怀周荣军李标刘红霞
Owner 盐城市胜达化工有限公司