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Preparation method for phenylacetic acid

A technology of phenylacetic acid and sodium phenylacetate, applied in the directions of carboxylate preparation, carboxylate preparation, nitrile preparation, etc., can solve the problems of harsh operation process, high cost, and high requirements for personnel training, and achieves high efficiency and low cost. Effect

Inactive Publication Date: 2018-02-16
潍坊滨海石油化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation process requires the use of bioengineering bacteria, resulting in relatively high costs, harsh operating procedures, and high requirements for personnel training

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A preparation method for phenylacetic acid, comprising the following steps:

[0020] 1) Add benzyl chloride and sodium cyanide (the molar ratio of benzyl chloride to sodium cyanide is 1.1:1) into the reaction kettle, heat up to 100°C for cyanation reaction, and the reaction time is 8 hours to obtain oil-water two-phase , wherein the upper layer is the crude product of phenylacetonitrile, and the lower layer is the waste water layer;

[0021] 2) Add 32wt% sodium hydroxide solution (the molar ratio of phenylacetonitrile to sodium hydroxide is 0.9:1) to the crude product of phenylacetonitrile for hydrolysis, the hydrolysis temperature is 90°C, and the reaction endpoint PH=10 is controlled to obtain sodium phenylacetate with ammonia, where ammonia enters the absorption system;

[0022] 3) Adding hydrochloric acid with a mass concentration of 30% to the sodium phenylacetate obtained in step 2) for acidification, the reaction temperature is 60° C., subject to the reaction en...

Embodiment 2

[0024] A preparation method for phenylacetic acid, comprising the following steps:

[0025] 1) Add benzyl chloride and sodium cyanide (the molar ratio of benzyl chloride to sodium cyanide is 1.2:1) into the reaction kettle, heat up to 120°C for cyanation reaction, and the reaction time is 2 hours to obtain oil-water two-phase , wherein the upper layer is the crude product of phenylacetonitrile, and the lower layer is the waste water layer;

[0026] 2) Add 32wt% potassium hydroxide solution (the molar ratio of phenylacetonitrile to potassium hydroxide is 1.1:1) to the crude product of phenylacetonitrile for hydrolysis, the hydrolysis temperature is 100°C, and the reaction end point PH=8 is controlled to obtain sodium phenylacetate with ammonia, where ammonia enters the absorption system;

[0027] 3) Adding sulfuric acid with a mass concentration of 30% to the sodium phenylacetate obtained in step 2) for acidification, the reaction temperature is 50° C., subject to the reaction...

Embodiment 3

[0029] A preparation method for phenylacetic acid, comprising the following steps:

[0030] 1) Add benzyl chloride and sodium cyanide (the molar ratio of benzyl chloride to sodium cyanide is 0.9:1) into the reaction kettle, heat up to 60°C for cyanation reaction, and the reaction time is 12 hours to obtain oil-water two-phase , wherein the upper layer is the crude product of phenylacetonitrile, and the lower layer is the waste water layer;

[0031] 2) Add 32wt% potassium hydroxide solution (the molar ratio of phenylacetonitrile to potassium hydroxide is 0.8:1) to the crude product of phenylacetonitrile for hydrolysis, the hydrolysis temperature is 40°C, and the reaction endpoint PH=13 is controlled to obtain sodium phenylacetate with ammonia, where ammonia enters the absorption system;

[0032] 3) Adding sulfuric acid with a mass concentration of 60% to the sodium phenylacetate obtained in step 2) for acidification, the reaction temperature is 80 ° C, and the reaction end poi...

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PUM

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Abstract

The invention provides a preparation method for phenylacetic acid. The method comprises the following steps: 1) adding benzyl chloride and sodium cyanide into a reaction kettle, raising the temperature to 60-120 DEG C, and performing a cyanation reaction for 2-12h to obtain an oil phase and a water phase, wherein the upper layer is a crude product of phenylacetonitrile, and the lower layer is a waste-water layer; 2) adding a strong alkali or a strongly-alkaline solution into the crude product of the phenylacetonitrile, performing hydrolysis, wherein the hydrolysis temperature is 40-120 DEG C,and controlling the pH at a reaction endpoint to be 8-13 to obtain sodium phenylacetate and an ammonia gas, wherein the ammonia gas enters an absorption system; and 3) adding sulfuric acid or hydrochloric acid into the sodium phenylacetate obtained by the step 2) for acidification, wherein the reaction temperature is 20-80 DEG C, enabling the pH at a reaction endpoint to be 1-2, after a reaction is finished, precipitating a product by crystallization, and performing solid-liquid separation to obtain the phenylacetic acid. The preparation method provided by the invention can quickly and effectively prepare the phenylacetic acid, and has low costs and good benefits.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method of phenylacetic acid. Background technique [0002] Phenylacetic acid is an important organic compound. Due to its typical reaction of carboxyl, methylene hydrogen and benzene ring, it can generate a variety of intermediates, so it is widely used in medicine, spices, pesticides and other industries, especially in the penicillin industry There is a huge demand for salt production. [0003] At present, there are dozens of synthesis routes of phenylacetic acid, among which the common ones are: sodium cyanide method, styrene method, acetophenone method and benzyl halide carbonylation method. Chinese patent application 201611110169.8 provides a method for preparing phenylacetic acid by a biological method, which includes the following steps: divide phenylacetonitrile into several batches, each batch has the same volume, and add a batch of ph...

Claims

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Application Information

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IPC IPC(8): C07C51/02C07C57/32
CPCC07C51/02C07C51/08C07C51/41C07C253/14C07C255/33C07C57/32
Inventor 王廷伟孙振民李建明宋帅陈之军陈苏昌
Owner 潍坊滨海石油化工有限公司
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