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Novel process for preparing chloropropionyl chloride

A chloropropionyl chloride, a new technology, applied in the preparation of carboxylate, the preparation of organic compounds, organic chemistry, etc., can solve the problems of high cost, non-reusable, non-conforming phosphorous acid, etc., and achieve quantity and quality improvement , ideal catalytic effect, high temperature is not easy to carbonize the effect of less residue

Inactive Publication Date: 2020-04-03
XINHUA PHARM (SHOUGUANG) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the acylation process of the traditional production process of chloropropionyl chloride, the separation of phosphorous acid is not complete, the by-product phosphorous acid does not meet the industrial standards, and the phosphorous acid solution is not easy to handle and store; the liquid catalyst used in the chlorination process is easy to carbonize at high temperature and produces side effects. Reaction, the follow-up residue is more difficult to handle and cannot be reused, and the cost is higher

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1: a kind of new process of preparing chloropropionyl chloride, its specific operation steps are as follows:

[0020] 1: Acylation process

[0021] 1.1: Put the quantitative propionic acid in the acylation tank, add phosphorus trichloride dropwise, raise the temperature after the dropwise addition, control the temperature in the acylation tank to 50°C, react for 4 hours, let stand, cool down for 1 hour, and then separate the phosphorous acid in the lower layer;

[0022] 1.2: Place the phosphorous acid obtained in step 1.1 in a barrel, and transfer the crude propionyl chloride in the upper layer to an acylation distillation tank;

[0023] 1.3: Transfer the phosphorous acid in step 1.2 to the hydrolysis tank, add an appropriate amount of activated carbon according to the color of the phosphorous acid to ensure that the phosphorous acid is colorless, and transfer the phosphorous acid in the hydrolysis tank to the storage tank before distillation through the soli...

Embodiment 2

[0033] Embodiment 2: a kind of new process of preparing chloropropionyl chloride, its specific operation steps are as follows:

[0034] 1: Acylation process

[0035] 1.1: Put the quantitative propionic acid in the acylation tank, add phosphorus trichloride dropwise, raise the temperature after the dropwise addition, control the temperature in the acylation tank to 60°C, react for 4 hours, let stand, cool down for 1.5 hours, and then separate the phosphorous acid in the lower layer ;

[0036] 1.2: Place the phosphorous acid obtained in step 1.1 in a barrel, and transfer the crude propionyl chloride in the upper layer to an acylation distillation tank;

[0037] 1.3: Transfer the phosphorous acid in step 1.2 to the hydrolysis tank, add an appropriate amount of activated carbon according to the color of the phosphorous acid to ensure that the phosphorous acid is colorless, and transfer the phosphorous acid in the hydrolysis tank to the storage tank before distillation through the...

Embodiment 3

[0047] Embodiment 3: a kind of new process of preparing chloropropionyl chloride, its specific operation steps are as follows:

[0048] 1: Acylation process

[0049] 1.1: Put quantitative propionic acid in the acylation tank, add phosphorus trichloride dropwise, raise the temperature after the dropwise addition, control the temperature in the acylation tank to 65°C, react for 4 hours, let stand, cool down for 2 hours, and then separate the phosphorous acid in the lower layer;

[0050] 1.2: Place the phosphorous acid obtained in step 1.1 in a barrel, and transfer the crude propionyl chloride in the upper layer to an acylation distillation tank;

[0051] 1.3: Transfer the phosphorous acid in step 1.2 to the hydrolysis tank, add an appropriate amount of activated carbon according to the color of the phosphorous acid to ensure that the phosphorous acid is colorless, and transfer the phosphorous acid in the hydrolysis tank to the storage tank before distillation through the solid-l...

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PUM

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Abstract

The invention discloses a novel process for preparing chloropropionyl chloride, which can overcome the defects that the byproduct phosphorous acid in the existing chloropropionyl chloride production process is not thoroughly separated and is not easy to treat and store; catalyst recycling is impossible to realize; the yield is low; the cost is high, and the like. According to the novel process, inthe acylation process, the product of the reaction of propionic acid and phosphorus trichloride is subjected to standing separation, the lower phosphorous acid is subjected to hydrolysis, decoloration, negative pressure distillation and slicing deep processing to reach the industrial standard of industrial phosphorous acid, the product at solid state is easy to store, byproducts are easy to sell,and extra economic benefits are brought to companies. A novel catalyst is used in the chlorination process of crude propionyl chloride at the upper layer, the catalyst is ideal in catalytic effect, can be repeatedly used, is not easy to carbonize at high temperature and has few residues, so that the quantity and the quality of products are improved.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a new process for preparing chloropropionyl chloride. Background technique [0002] Chloropropionyl chloride is an important raw material for organic synthesis. It is used in medicine to synthesize ibuprofen, and in pesticides to synthesize herbicides. Two reactions are mainly used in the process of preparing chloropropionyl chloride: acylation reaction and chlorination reaction. In the acylation process of the traditional production process of chloropropionyl chloride, the separation of phosphorous acid is not complete, the by-product phosphorous acid does not meet the industrial standards, and the phosphorous acid solution is not easy to handle and store; the liquid catalyst used in the chlorination process is easy to carbonize at high temperature and produces side effects. Reaction, subsequent residues are more difficult to handle and cannot be reused, a...

Claims

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Application Information

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IPC IPC(8): C07C51/60C07C53/42C07C51/64C07C51/62C07C53/50B01J35/02
CPCC07C51/60C07C51/64C07C51/62B01J35/00B01J35/30C07C53/42C07C53/50Y02P20/584
Inventor 曹长峰陆鹏靳延辉周金东毕海涛
Owner XINHUA PHARM (SHOUGUANG) CO LTD
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