Preparation method of phenylacetic acid

A technology of phenylacetic acid and phenylacetonitrile, which is applied in the field of phenylacetic acid prepared by hydrolysis of phenylacetonitrile, can solve problems such as poor operating environment, difficult recovery, cumbersome operation process, etc., achieve product appearance and quality satisfaction, avoid difficult processing, and atom economy Good results

Inactive Publication Date: 2013-08-07
CHONGQING UNISPLENDOUR CHEM
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Problems solved by technology

[0013] 1) Alkaline hydrolysis consumes both alkali and acid, poor atom economy, and by-product ammonia and salt;
[0014] 2) Alkaline hydrolysis produces ammonia gas, which will bring out organic matter when the ammonia gas escapes, polluting the environment, no matter whether it is absorbed by water or acid, it cannot be used directly because the organic matter exceeds the standard;
[0015] 3) Sodium phenylacetate solution needs to be decolorized, resulting in solid waste, and the decolorization process releases odor, and the operating environment is poor;
[0016] 4) Using sulfuric acid hydrolysis, high temperature reaction will cause carbonization and coki...

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  • Preparation method of phenylacetic acid
  • Preparation method of phenylacetic acid
  • Preparation method of phenylacetic acid

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preparation example Construction

[0033] The preparation method of phenylacetic acid of the present invention comprises the following steps:

[0034] 1) Heat benzyl nitrile to 50~100°C, then add hydrochloric acid dropwise to benzyl nitrile or drop molten benzyl nitrile into hydrochloric acid, the molar ratio of hydrochloric acid to benzyl nitrile is 1.2~5:1, the dropwise addition is completed Post-insulation reaction 1~5 hour, the mass content of phenylacetonitrile in the reaction system terminates reaction when being less than 5%; The massfraction of described hydrochloric acid is preferably 15%~37%;

[0035] 2) Recover the unreacted phenylacetonitrile in the reaction system of step 1) by distillation under reduced pressure until the mass content of phenylacetonitrile in the reaction system is less than 0.2%, then add water to the reaction system, stir and miscible, then cool and crystallize, and suction filter, The obtained crystals are washed with water and dried to obtain the phenylacetic acid product; amm...

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Abstract

The invention discloses a preparation method of phenylacetic acid, which comprises the following steps of: 1) heating benzyl cyanide to 50-100 DEG C, dropwise adding hydrochloric acid to the benzyl cyanide or dropwise adding the molten benzyl cyanide to hydrochloric acid, wherein the molar ratio of the hydrochloric acid to the benzyl cyanide is (1.2-5):1; after dropwise adding, performing a heat preservation reaction for 1-5 hours; and ending the reaction when the mass content of the benzyl cyanide in the reaction system is less than 5%; and 2) performing reduced-pressure distillation for recovering the unreacted benzyl cyanide in the reaction system of the step 1) until the mass content of the benzyl cyanide in the reaction system is less than 0.2%; adding water to the reaction system, and stirring and mixing; cooling for crystallization and performing suction filtration; and washing the obtained crystal with water, and drying to obtain a phenylacetic acid product. According to the preparation method disclosed by the invention, a technology of directly hydrolyzing benzyl cyanide with hydrochloric acid to prepare phenylacetic acid is adopted, few kinds of reactants are used, other organic matters except the raw material benzyl cyanide are not required, the consumption is low, the after-treatment is simple, and both the appearance and quality of the product meet requirements.

Description

technical field [0001] The invention relates to the technical field of synthesis of phenylacetic acid, in particular to a method for preparing phenylacetic acid by hydrolysis of phenylacetonitrile. Background technique [0002] The hydrolysis of phenylacetonitrile is a commonly used method for preparing phenylacetic acid. Its process conditions are relatively simple, and the reaction operation is simple and easy to control. It is the most researched and most mature industrial production method in China. The hydrolysis process is divided into two types: the first one uses strong alkali Such as sodium hydroxide or potassium hydroxide to make phenylacetonitrile into sodium phenylacetate, acidify and crystallize to obtain the product after decolorization; the second is directly hydrolyzed with acid and crystallized to obtain phenylacetic acid. The reaction equation is as follows: [0003] 1. Alkaline hydrolysis [0004] [0005] 2. Acid hydrolysis [0006] 1) Sulfuric ac...

Claims

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Application Information

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IPC IPC(8): C07C57/32C07C51/08
Inventor 丁永良张飞屈洋李静朱丽利
Owner CHONGQING UNISPLENDOUR CHEM
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