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Method for preparing 2, 4-D acid by using micro-reaction device

A micro-reaction device and micro-reactor technology, applied in the chemical industry, can solve the problems of many by-products, expensive solvents, etc., and achieve the effects of stable product quality, high safety, and reducing the content of by-products and production costs.

Active Publication Date: 2021-03-19
ZAOZHUANG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In view of the problems existing in the prior art, 2,4-D acid post-chlorination technology needs to use expensive solvents, complex catalysts, and many by-products, etc.

Method used

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  • Method for preparing 2, 4-D acid by using micro-reaction device

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Experimental program
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Effect test

Embodiment 1

[0022]The phenoxyacetic acid is mixed with acetic acid to obtain a acetic acid solution of phenoxyacetic acid. The mass fraction of phenoxyacetic acid in the mixture of phenoxy acetic acid is 13%, and the pre-cooling tube 1 pumped at 20 ° C is pre-cooled; 5% sodium sodium sodium sodium sodium sodium sodium Pre-cooling tube 2 in the temperature of temperature 5 ° C, the molar ratio of sodium hypochlorite and phenoxyacetic acid is 2: 1; then the above two solutions are pumped into the microfiter, and the temperature in the microconition is controlled to 5 ° C. The mixture was transferred into the microreactor and continued to react, and the reaction temperature in the microreactor was 30 ° C, and the reaction residence time was 8 min. After the reaction was completed, the reaction solution was cooled to pH = 1, then extracted with diethyl ether, then extracted with diethyl ether, then extracted with diethyl ether phase, and the resulting water phase was acidified to pH = 1. Then, then...

Embodiment 2

[0024]Phenoxyacetic acid is mixed with acetic acid to give a acetic acid solution of phenoxyacetic acid, and the mass fraction of phenoxyacetic acid in the mixture of acetic acid is 15%, and the pre-cooling tube 1 pumped at 20 ° C is pre-cooled; 5% sodium sodium sodium sodium sodium sodium The molar ratio of pre-cooling tube 2 in the temperature of 5 ° C, sodium hypochlorite and phenoxyacetic acid is 2.1: 1; then the above two solutions are pumped into the microfitizer, and the temperature in the microconlease is controlled to 5 ° C. The mixture was transferred into the microreactor and continued to react, and the reaction temperature in the microreactor was 30 ° C, and the reaction residence time was 8 min. After the reaction was completed, the reaction solution was cooled to pH = 1, then extracted with diethyl ether, then extracted with diethyl ether, then extracted with diethyl ether phase, and the resulting water phase was acidified to pH = 1. Then, then filtered, washed, dried,...

Embodiment 3

[0026]The phenoxyacetic acid is mixed with acetic acid to obtain a acetic acid solution of phenoxyacetic acid, and the mass fraction of phenoxyacetic acid in the mixture of acetic acid is 16%, and the pre-cooling tube 1 of the pumped temperature of 18 ° C is pre-cooled; 5% sodium sodium sodium sodium sodium sodium The molar ratio of pre-cooling tube 2 incorporating the temperature 3 ° C, the molar ratio of sodium hypochlorite and phenoxyacetic acid is 2.2: 1; then the above two solutions are pumped into the micro-mixer, and the temperature in the micro-mixer is controlled to 5 ° C. The mixture was transferred into the microreactor and continued to react, and the reaction temperature in the microreactor was 30 ° C, and the reaction residence time was 8 min. After the reaction was completed, the reaction solution was cooled to pH = 1, then extracted with diethyl ether, then extracted with diethyl ether, then extracted with diethyl ether phase, and the resulting water phase was acidifi...

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Abstract

The invention discloses a method for preparing 2, 4-D acid by chlorinating phenoxyacetic acid by using a micro-reaction device. The method comprises the steps: dissolving phenoxyacetic acid in glacialacetic acid to obtain a glacial acetic acid solution of phenoxyacetic acid, and pumping the glacial acetic acid solution of phenoxyacetic acid into a pre-cooling pipe 1 of the micro-reaction device for pre-cooling; pumping a sodium hypochlorite solution into a pre-cooling pipe 2 of the micro-reaction device for pre-cooling; then pumping the two solutions into a micro-mixer in the micro-reaction device to be fully mixed; introducing the mixed solution into a micro-reactor of the micro-reaction device for reaction; after the reaction is finished, carrying out post-treatment on the reaction solution to obtain the 2, 4-D acid. The preparation method of the 2, 4-D acid can overcome the problems that an expensive solvent and a complex catalyst need to be used, many byproducts are produced and the like in the existing 2, 4-D acid post-chlorination technology, the continuous degree of the production process is high, the safety of the production process can be greatly improved, and the yield of the product is increased.

Description

Technical field[0001]The present invention belongs to the chemical technology, and more particularly to a method of preparing 2,4-dichlorobenzoxyacetic acid using a microreactive device.Background technique[0002]2,4-dichlorophenoxic acid referred to as 2,4-D acid, is a representative synthetic plant growth hormone. Due to less dosage, low cost, 2,4-D acid becomes the longest history of history, the most widely used herbicide. At the same time, 2, 4-D acids below 30 ppm can also be used as plant growth regulators to prevent falling fruits such as tomatoes, cotton, pineapple and other falling fruits and form no children.[0003]There are two methods for the preparation of 2,4-dichlorobenzoxic acid: one is chlorinated in a molten state, and then condensate obtained by condensation of the obtained dichlorophenol and chlorination; second, phenol and chlorine The acetic acid is condensed to form phenoxyacetic acid under alkaline conditions, and then the chlorination process is obtained by c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/363C07C59/70
CPCC07C51/363C07C59/70
Inventor 周峰岩马杰张文志程终发王燕平李鹏飞
Owner ZAOZHUANG UNIV
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