Method for synthesizing phenoxyacetic acid derivatives

A technology of phenoxyacetic acid derivatives and phenoxyacetic acid, which is applied in the field of synthesizing phenoxyacetic acid derivatives, can solve problems such as the production environment and the impact of three wastes treatment, unfavorable biochemical degradation and emissions, and product quality impacts, so as to reduce artificial labor, Ease of automation and reduced labor intensity

Inactive Publication Date: 2018-04-03
青岛九洲千和机械有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Phenoxyacetic acid chlorinated derivatives such as 2,4-D acid, 2-methyl-4-chlorine 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. Synthesized with sodium chloroacetate, chlorinated phenol-containing wastewater is produced during the production process, which has a serious impact on the production environment and the treatment of three wastes
In the process of synthesizing chlorina

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 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

[0030] 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%.

[0031] 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 280 grams of phenol-containing waste water, 105 g...

Embodiment 3

[0033] 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

The invention relates to a method for synthesizing phenoxyacetic acid derivatives. The salt compound of phenol or methylphenol and the salt compound of chloroacetic acid are mixed and placed in a solvent for heating reaction, and then acidified with an inorganic acid to obtain phenoxyacetic acid. Then dissolve it in a solvent and add a catalyst therein, then pass chlorine gas into it and carry out heating and chlorination reaction, and obtain chlorophenoxyacetic acid (or methylphenoxyacetic acid) derivatives after cooling and crystallization. Compared with the prior art, in the reaction process, the present invention recovers and recycles the solvent and waste water of the reaction system, satisfies its own production balance, and can realize the recycling of the closed system, with a yield greater than 95% and a content greater than 98% , The utilization rate of solvent recycling is greater than 95%, and the waste water discharge in the whole production process is reduced by more than 95%.

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-chlorine 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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IPC IPC(8): C07C51/363C07C59/70
CPCC07C51/363C07C51/367C07C59/70
Inventor 李辉
Owner 青岛九洲千和机械有限公司
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