Method for simultaneously preparing phenylacetamide and phenylacetic acid by benzyl cyanide hydrolysis in ammonia-containing high temperature aqueous water medium

A high-temperature liquid water and phenylacetamide technology, which is applied in the direction of nitrile preparation, chemical instruments and methods, and carboxylic acid amide preparation, can solve the problems of high reaction temperature, weak catalytic ability, and low yield of phenylacetamide, and achieve a reduction Effects of reaction temperature, increased reaction speed, and shortened reaction time

Inactive Publication Date: 2009-03-11
ZHEJIANG UNIV
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Problems solved by technology

The method for preparing phenylacetic acid by non-catalytic hydrolysis of phenylacetonitrile in near-critical water medium, application number: 200710156869.5, application date: November 15th, 2007), but due to the weak self-catalysis ability of near-critical water, there is no phenylaceton

Method used

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  • Method for simultaneously preparing phenylacetamide and phenylacetic acid by benzyl cyanide hydrolysis in ammonia-containing high temperature aqueous water medium
  • Method for simultaneously preparing phenylacetamide and phenylacetic acid by benzyl cyanide hydrolysis in ammonia-containing high temperature aqueous water medium
  • Method for simultaneously preparing phenylacetamide and phenylacetic acid by benzyl cyanide hydrolysis in ammonia-containing high temperature aqueous water medium

Examples

Experimental program
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Effect test

Embodiment 1

[0041] Add 360g of deionized water and 45g of phenylacetonitrile (mass ratio of deionized water to phenylacetonitrile is 8) into a 500mL intermittent autoclave, start stirring, heat up to boiling under normal pressure, open the exhaust valve for 2 minutes, and use water vapor Take away the oxygen in the kettle; inject ammonia water with a concentration of 25% by weight through a metering pump, so that the ammonia concentration in the reactant in the kettle is 4g / L, continue to heat up to 180°C for 120min; after the hydrolysis, cool down to 100°C, open The exhaust valve recovers the ammonia gas in the kettle, and the ammonia gas is absorbed by water to make ammonia water and reused in step 2; the hydrolyzate is cooled, added with NaOH solution to adjust the pH value to 8-9, crystallized, and filtered to obtain crude phenylacetamide; Phenylacetamide obtains 25.0g phenylacetamide product after activated carbon decolorization, secondary crystallization, vacuum drying, and product i...

Embodiment 2

[0043] Add 350g of deionized water and 50g of phenylacetonitrile (mass ratio of deionized water to phenylacetonitrile is 7) into a 500mL intermittent autoclave, start stirring, heat up to boiling under normal pressure, open the exhaust valve for 3 minutes, and use water vapor Take away the oxygen in the kettle; inject ammonia water with a concentration of 25% by weight through a metering pump, so that the ammonia concentration in the reactant in the kettle is 3g / L, continue to heat up to 190°C for 90 minutes; after the hydrolysis is completed, cool down to 100°C, open The exhaust valve reclaims the ammonia in the kettle, and the ammonia is absorbed by water to make ammonia water and reused in step 2; the hydrolyzate is cooled and added with Na 2 CO 3 Adjust the pH value of the solution to 8-9, crystallize, and filter to obtain crude phenylacetamide; the crude phenylacetamide is decolorized by activated carbon, recrystallized, and vacuum-dried to obtain 27.0g of phenylacetamide...

Embodiment 3

[0045] Add 360g of deionized water and 60g of phenylacetonitrile (the mass ratio of deionized water to phenylacetonitrile is 6) into a 500mL intermittent autoclave, start stirring, heat up to boiling under normal pressure, open the exhaust valve for 4 minutes, and use water vapor Take away the oxygen in the kettle; inject ammonia water with a concentration of 25% by weight through a metering pump, so that the ammonia concentration in the reactant in the kettle is 2g / L, continue to heat up to 200°C for 40min; after the hydrolysis, cool down to 100°C, open The exhaust valve recovers the ammonia gas in the kettle, and the ammonia gas is absorbed by water to make ammonia water and reused in step 2; the hydrolyzate is cooled and added with NaHCO 3 Adjust the pH value of the solution to 8-9, crystallize, and filter to obtain crude phenylacetamide; the crude phenylacetamide is decolorized by activated carbon, recrystallized, and vacuum-dried to obtain 37.9g ​​of phenylacetamide produc...

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Abstract

The invention discloses a method for hydrolyzing phenylacetonitrile in an ammonia-containing high-temperature liquid water medium and preparing phenyl acetamide and phenylacetic acid simultaneously. The method comprises the following steps: 1) deionized water and the phenylacetonitrile with the mass ratio of between 2 to 1 and 8 to 1 are added into a high-pressure reaction kettle, are stirred, and are heated to boil, and an exhaust valve is opened for 2 to 5 minutes; 2) 25 percent ammonia water is pumped through a metering pump to ensure that the ammonia concentration in reactants in the kettle is between 0.05 and 4g/L, and the temperature is increased to be between 180 and 250 DEG C to hydrolyze for 5 to 120 minutes; 3) the temperature is reduced to recover ammonia gas in the kettle; 4) a hydrolysate is cooled, the pH value of the hydrolysate is adjusted to between 8 and 9 , and the hydrolysate is crystallized, and filtered to obtain crude phenyl acetamide; 5) the crude phenyl acetamide is subjected to decolorization by activated carbon, secondary crystallization and vacuum drying to obtain a phenyl acetamide product; and 6) the pH value of filtrate in step 4) is adjusted to between 3 and 4, and the filtrate is crystallized to obtain crude phenylacetic acid, and then the crude phenylacetic acid is subjected to decolorization by the activated carbon, secondary crystallization and vacuum drying to obtain a phenylacetic acid product. The method has a simple and environment-friendly technical process.

Description

technical field [0001] The invention relates to amides and carboxylic acids, in particular to a method for simultaneously preparing phenylacetamide and phenylacetic acid by hydrolyzing phenylacetonitrile in ammonia-containing high-temperature liquid water medium. Background technique [0002] Phenylacetamide (Phenylacetamide, Benzeneacetamide, α-Toluamide, CAS No: 103-81-1), molecular formula C 6 h 5 CH 2 CONH 2 , the structural formula is as follows, white flake or leaf crystal, the solubility is about 10g / L (1<pH<10), the product is used as an intermediate of medicine, pesticide and spice. In the pharmaceutical industry, it is the medium of penicillin G and the raw material of the sedative drug phenobarbital, as well as the raw material of the pesticide Daofengsan and rodenticide. [0003] [0004] At present, the main methods of industrialization of phenylacetamide can be divided into phenylacetonitrile hydrolysis method and styrene method according to the re...

Claims

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Application Information

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IPC IPC(8): C07C233/11C07C231/06C07C63/04C07C51/08
Inventor 吕秀阳任浩明
Owner ZHEJIANG UNIV
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