Preparation method of 2-chloro-4-bromophonel with high purity

A bromophenol, high-purity technology, applied in the field of preparation of high-purity 2-chloro-4-bromophenol, can solve the problems of reduced purity and yield impact

Active Publication Date: 2013-11-13
山东科源化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, the existing 2-chloro-4-bromophenol production technology can only produce products with a purity of about 94%. The reason is that the production of 2

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) Mix and stir 1750kg of o-chlorophenol and 25kg of nano-positioning catalyst. The nano-positioning catalyst is a mixture of copper chloride, zinc chloride and silver chloride, and the mass ratio is copper chloride: zinc chloride: Silver chloride=1:8:1;

[0018] (2) Cool down to 12℃, add Br 2 , React for 22 hours at a temperature of 12-50°C;

[0019] (3) Raise the temperature to 58°C for 1.5 hours;

[0020] (4) The product is obtained after cooling down, and the product is measured, packaged and stored.

[0021] The method also includes the preparation of hydrobromic acid: while performing the reaction in step (2), water is used to absorb the by-reaction product hydrogen bromide to prepare hydrobromic acid.

[0022] The purity of the brominated product obtained was 97.6%, and the yield was 97.2%.

Embodiment 2

[0024] (1) Mix and stir 1500kg of o-chlorophenol and 15kg of nano-positioning catalyst evenly, the addition amount of the nano-catalyst is 1% of the mass of o-chlorophenol, and the nano-positioning catalyst is copper chloride, zinc chloride, chlorinated For a mixture of silver, the mass ratio is copper chloride: zinc chloride: silver chloride=3:1:2;

[0025] (2) Cool down to 10℃, add Br 2 , Reacting for 20 hours at a temperature of 10-55°C, the o-chlorophenol and Br 2 The molar ratio of is 1:1;

[0026] (3) Raise the temperature to 55°C for 1 hour;

[0027] (4) The product is obtained after cooling down, and the product is measured, packaged and stored.

[0028] The method also includes the preparation of hydrobromic acid: while performing the reaction in step (2), water is used to absorb the by-reaction product hydrogen bromide to prepare hydrobromic acid.

[0029] The obtained brominated product has a purity of over 97.7%, and the product yield is 97.3%.

Embodiment 3

[0031] (1) Mix 1750kg of o-chlorophenol and 30kg of nano-positioning catalyst and stir uniformly, the addition amount of the nano-catalyst is 2% of the mass of o-chlorophenol, and the nano-positioning catalyst is copper chloride, zinc chloride, and chlorinated For a mixture of silver, the mass ratio is copper chloride: zinc chloride: silver chloride = 2:4:1.5;

[0032] (2) Cool down to 15℃, add Br 2 , Reacted for 25 hours at a temperature of 15-60 ℃, the o-chlorophenol and Br 2 The molar ratio of is 1:1.2;

[0033] (3) Raise the temperature to 60°C for 2 hours;

[0034] (4) The product is obtained after cooling down, and the product is measured, packaged and stored.

[0035] The method also includes the preparation of hydrobromic acid: while performing the reaction in step (2), water is used to absorb the by-reaction product hydrogen bromide to prepare hydrobromic acid.

[0036] The purity of the brominated product obtained is over 97.6%, and the product yield is 97.3%.

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PUM

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Abstract

The invention discloses a preparation method of 2-chloro-4-bromophonel with high purity. The preparation method comprises the following steps of mixing and uniformly stirring o-chlorophenol and a locating nanocatalyst, meanwhile, cooling, and adding Br2 to carry out bromination reaction to obtain a product, wherein the locating nanocatalyst is hydrochloride of a transition element. The locating nanocatalyst is a mixture of copper chloride, zinc chloride and silver chloride with the mass ratio of (1-3): (1-8): (1-2). The locating nanocatalyst is used in the preparation method of the 2-chloro-4-bromophonel, so that the purity of the obtained 2-chloro-4-bromophonel is increased from 94% to 97.5%, fewer byproducts are generated, and the yield is very high and can be up to over 97%.

Description

Technical field [0001] The invention relates to a method for preparing high-purity 2-chloro-4-bromophenol. Background technique [0002] 2-Chloro-4-bromophenol, an intermediate for the pesticide profenofos, can also be used in other organic synthesis. 2-Chloro-4-bromophenol is an intermediate of the ternary asymmetric organophosphorus insecticide profenofos. High-purity 2-chloro-4-bromophenol is used to synthesize high-quality profenofos technical. [0003] However, the existing 2-chloro-4-bromophenol production technology can only produce products with a purity of about 94%. The reason is that the production of 2-chloro-4-bromophenol contains 2-chloro-6-bromophenol and more Brominated by-products, the by-products in these raw materials will reduce the purity and at the same time the yield will be affected. Summary of the invention [0004] The technical problem to be solved by the present invention is to provide a method for preparing high-purity 2-chloro-4-bromophenol, which ha...

Claims

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Application Information

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IPC IPC(8): C07C39/27C07C37/62B01J35/02B01J27/138
Inventor 曲江升张云霄邱瑞栋
Owner 山东科源化工有限公司
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