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Method for synthesizing phenoxyacetic acid derivative

A technology of phenoxyacetic acid derivatives and phenoxyacetic acid, applied in the field of synthesizing phenoxyacetic acid derivatives, can solve problems such as product decomposition and uneconomical efficiency, and achieve the effects of increasing reaction production capacity, improving production efficiency and reducing manual labor.

Active Publication Date: 2015-07-01
JIANGXI TIANYU CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is also a method of vacuum distillation for purification, but this method is uneconomical, and the product may decompose at high temperature

Method used

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  • Method for synthesizing phenoxyacetic acid derivative
  • Method for synthesizing phenoxyacetic acid derivative
  • Method for synthesizing phenoxyacetic acid derivative

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Synthesis of Phenoxyacetic Acid

[0038]In a 1000 milliliter four-neck flask equipped with stirring, thermometer, reflux condenser and dropping funnel, add 400 grams of phenol sodium brine solution (containing 95 grams of phenol, 1 mole, 40 grams of sodium hydroxide, 1 mole), stir Heat to 90°C, start dropwise adding 460 grams of sodium chloroacetate aqueous solution (containing 125 grams of chloroacetic acid, 1.32 moles, 53 grams of sodium hydroxide, 1.33 moles), heat to reflux, react for 2 hours, cool down to 30°C, start to drop hydrochloric acid , adjust the pH value to 0, stir and cool down to 10°C, suction filter, wash, and dry to obtain 147 grams of the product, the content is greater than 98%, and the yield is 95%.

Embodiment 2

[0040] Synthesis of 2-Methylphenoxyacetic Acid

[0041] Add 450 grams of 2-methylphenol potassium brine solution (containing 108 grams of methylphenol, 1 mole, 56 grams of potassium hydroxide, 1 mole) was heated to reflux, and 450 grams of potassium chloroacetate solution (containing 115 grams of chloroacetic acid, 1.2 moles, 70 grams of potassium hydroxide, 1.25 moles) was added dropwise, heated to reflux, reacted for 2 hours, cooled to 30 ° C, and added dropwise hydrochloric acid to adjust When the pH value reaches 1, stir and crystallize to 10°C, filter with suction, add 100 grams of water to wash, and dry to obtain 162 grams of the product, with a content of 98% and a yield of 96%.

[0042] The mother liquor and washing water were distilled on a rotary evaporator in a 1000 ml bottle, and 600 grams of 2-methylphenol-containing water (containing 0.3% of methylphenol) were steamed out, and 175 grams of potassium chloride was obtained in the bottle for drying. Add and reclaim...

Embodiment 3

[0044] Synthesis of Phenoxyacetic Acid

[0045] In a 2000 ml reaction bottle, add 800 grams of phenol sodium salt solution (containing 190 grams of phenol, 2 moles, 80 grams of sodium hydroxide, 2 moles), stir and heat to 90 ° C, and start to dropwise add 900 grams of sodium chloroacetate solution (containing 243 grams of chloroacetic acid, 2.43 moles, 100 grams of sodium hydroxide, 2.5 moles), heated to reflux, reacted for 2 hours, cooled to 50 ° C, began to drop hydrochloric acid, adjusted the pH value to 0, stirred, and transferred to a 5000 milliliter separatory funnel 3,000 grams of dichloroethane was added for extraction to obtain a solution of phenoxyacetic acid (293 grams of external standard phenoxyacetic acid in the liquid phase, yield 96%).

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PUM

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Abstract

A phenoxyacetic acid derivatives synthesis method, comprising: after mixing the salt compound of phenol or methyl phenol with the salt compound of chloroacetic acid, adding the mixture to a solvent, and heating for reaction; acidifying with an inorganic acid to obtain phenoxyacetic acid, then dissolving the phenoxyacetic acid in a solvent, and adding a catalyst in the solvent; introducing chlorine to the solvent, heating for chlorination reaction, cooling and crystallizing to obtain the chloro-phenoxyacetic acid (or methyl phenoxyacetic acid) derivatives. Compared with prior art, the present method recycles the solvent and waste water of a reaction system during the reaction, satisfying self production balance, and realizing the recycled use of a closed system, with a yield greater than 95%, a content greater than 98%, a utilization rate of the recycled solvent greater than 95%, and the waste water discharge during the whole production process reduced by 95% or more.

Description

technical field [0001] The invention relates to a method for synthesizing herbicides, in particular to a method for synthesizing phenoxyacetic acid derivatives. Background technique [0002] Phenoxyacetic acid chlorinated derivatives such as 2,4-D acid, 2-methyl-4-chloride and other herbicides have a very broad market demand. It has a history of several decades. The traditional production process is to use phenol after chlorination. It is synthesized with sodium chloroacetate, and chlorophenol-containing wastewater is generated during the production process, which has a serious impact on the production environment and the treatment of three wastes. In the process of synthesizing chlorinated phenoxyacetic acid herbicides by condensation after chlorinating phenols, because the chlorinated phenols produced by the chlorination of phenols are not easy to separate, the chlorinated by-product phenols have a great impact on the quality of the product. In addition, in the reaction o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C59/70C07C51/363
CPCC07C51/363C07C51/367
Inventor 郑留清周庆江朱正江谢思勉田晓宏
Owner JIANGXI TIANYU CHEM CO LTD
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