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Preparation method of phenoxyacetic acid

A technology of phenoxyacetic acid and chloroacetic acid, which is applied in the preparation of carboxylate, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of high production cost and low overall yield, so as to solve the problem of processing and improve the yield. rate effect

Pending Publication Date: 2020-07-24
姜林
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  • Claims
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Problems solved by technology

[0004] Aiming at the problems of low overall yield and high production cost in the existing phenoxyacetic acid preparation methods, the invention provides a preparation method of phenoxyacetic acid

Method used

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  • Preparation method of phenoxyacetic acid

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preparation example Construction

[0024] see figure 1 As shown, the embodiment of the present invention provides a kind of preparation method of phenoxyacetic acid, comprises the following operation steps:

[0025] Condensation reaction: mixing reaction raw materials including chloroacetic acid, phenol and alkali for condensation reaction to obtain reaction mother liquor;

[0026] Acidification and crystallization: Acidification and crystallization of the reaction mother liquor, separation of phenoxyacetic acid crystals and crystallization mother liquor;

[0027] Resin adsorption treatment: Adsorption resin is used to absorb the organic matter in the crystallization mother liquor, and the permeate contains inorganic salts;

[0028] Analyzing the dope: use lye to analyze the adsorption resin, and the obtained analytic dope is used as the reaction raw material for the condensation reaction.

[0029] According to the preparation method of phenoxyacetic acid provided by the present invention, the crystallization...

Embodiment 1

[0051] This embodiment is used to illustrate the preparation method of the phenoxyacetic acid disclosed in the present invention, comprising the following steps:

[0052] a. Material preparation: Add solid chloroacetic acid with a content of not less than 96% in the material preparation tank A, dissolve it in hot water at 50-60°C to a concentration of 50%, add solid alkali according to the molar ratio of chloroacetic acid:NaOH 1:1, and stir After 15 minutes, vinyl chloride material was obtained, which was kept warm for subsequent use. Add phenol with a content of not less than 98% in the material preparation tank B, replace the air with nitrogen, preheat the phenol to 70°C, add 30% (mass content) sodium hydroxide lye and analytical concentrated solution preheated to 75°C After stirring for 15 minutes, the phenol material was obtained, and the preparation was completed and kept warm. The molar ratio of phenol to sodium hydroxide was 1:1.05.

[0053] b. Condensation reaction: ...

Embodiment 2

[0058] This embodiment is used to illustrate the preparation method of the phenoxyacetic acid disclosed in the present invention, comprising the following steps:

[0059] a. Material preparation: Add solid chloroacetic acid with a content of not less than 96% in the material preparation tank A, and dissolve it with 50-60°C hot water (or material) to a concentration of 50%, according to the molar ratio of chloroacetic acid: liquid ammonia 1 : 1 was added, and after the addition was completed, the vinyl chloride material was obtained after stirring for 30 minutes, which was kept warm for subsequent use. Add phenol with a content of not less than 98% in the material preparation tank B, replace the air with nitrogen, preheat the phenol to 70°C, add potassium hydroxide lye preheated to 75°C and mix to achieve the content of phenol in the concentrated solution Equivalent, add pre-heated to 75 ℃ analytical concentrate. After stirring for 15 minutes, the phenol material was obtained,...

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Abstract

In order to solve the problems of low total yield and high production cost in the existing phenoxyacetic acid preparation method, the invention provides a preparation method of phenoxyacetic acid, which comprises the following operation steps: carrying out condensation reaction, namely, mixing reaction raw materials comprising chloroacetic acid, phenol and alkali, and carrying out condensation reaction to obtain a reaction mother liquor; acidifying and crystallizing, namely, acidifying and crystallizing the reaction mother liquor, and separating to obtain phenoxyacetic acid crystals and a crystallization mother liquor; carrying out resin adsorption treatment, namely, adsorbing organic matters in the crystallization mother liquor by adopting adsorption resin, wherein permeate liquid contains inorganic salt; and desorbing the concentrated solution, namely desorbing the adsorption resin by adopting alkali liquor, wherein the obtained desorbed concentrated solution is used as a reaction raw material for condensation reaction. The preparation method of phenoxyacetic acid provided by the invention can effectively improve the yield of phenoxyacetic acid and reduce the wastewater treatmentcost.

Description

technical field [0001] The invention belongs to the technical field of chemical product preparation, and in particular relates to a preparation method of phenoxyacetic acid. Background technique [0002] Phenoxyacetic acid, white needle-like crystals, melting point 98-99 ° C, boiling point 285 ° C, slightly soluble in water, widely used in the production of plant growth hormone and 2.4-dichlorophenoxyacetic acid herbicide (also known as 2.4-D acid ), and phenoxyacetic acid series products are widely used in the pharmaceutical and dye industries. In the synthetic pharmaceutical industry, there are only a dozen kinds of lipid-lowering drugs in the phenoxyacetic acid series. The raw materials of phenoxyacetic acid used in the pesticide and pharmaceutical industries require high quality, especially the free phenol content is required to be below 5mg / kg, and the main content must reach more than 99%. The domestic demand is tens of thousands of tons per year. Production by tradit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/367C07C51/42C07C59/60
CPCC07C51/367C07C51/42C07C59/60
Inventor 姜林刘长飞
Owner 姜林
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