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Preparation method of phenoxyacetic ester

A technology of phenoxyacetate and acetate, applied in the field of preparation of phenoxyacetate, can solve problems such as affecting product quality and being difficult to separate, and achieves the effects of low production cost, short production cycle and readily available raw materials

Inactive Publication Date: 2018-12-07
SHANDONG RUNBO BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is an impurity methyl dichloroacetate in the raw material selected by this scheme—methyl chloroacetate, which will also react with phenate to produce impurity methyl chlorophenoxyacetate, which is not easy to separate and affects product quality

Method used

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  • Preparation method of phenoxyacetic ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Add acetic acid and methanol into the reactive distillation column to synthesize methyl acetate.

[0054] Add the synthesized methyl acetate into the reaction flask and feed chlorine gas to synthesize methyl chloroacetate.

[0055] 47.6g (0.5mol) of phenol, 120g of xylene, 30g of butanol, and 62.8g (0.5mol) of sodium hydroxide aqueous solution with a mass fraction of 32% were mixed and stirred, heated to about 140°C, and reacted with water for 1 hour. The neutralized solution was slightly cooled to 120°C, 53.8 g (0.495 mol) of methyl chloroacetate was added dropwise, and the addition was completed in 4 hours, then the temperature was raised to 146°C, and the reaction was kept for 2 hours. Cool the reaction solution to 100°C, add 150g of water, adjust the pH to 7, let stand to separate layers, add 20g of xylene to the water layer for extraction, and separate the organic layer by vacuum distillation to obtain 81.75g ​​of the product with a purity of 99.1% and a yield of 97....

Embodiment 2

[0057] Add acetic acid and methanol into the reactive distillation column to synthesize methyl acetate.

[0058] Add the synthesized methyl acetate into the reaction flask and feed chlorine gas to synthesize methyl chloroacetate.

[0059] Mix and stir 109.5 g (1 mol) of o-cresol, 350 g toluene, 100 g butanol, and 125.2 g (1 mol) of sodium hydroxide aqueous solution with a mass fraction of 32%, raise the temperature to about 114°C, and react with water for 1 hour. The neutralized solution was slightly cooled to 120°C, 107.7 g (0.98 mol) of methyl chloroacetate was added dropwise, and the addition was completed in 4 hours, then the temperature was raised to 116°C, and the reaction was kept for 2 hours. Cool the reaction solution to 100°C, add 150g of water, adjust the pH to 7, let stand to separate layers, add 40g of toluene to the water layer for extraction, and separate the organic layer by vacuum distillation to obtain 163.35g of the product with a purity of 99.13% and a yiel...

Embodiment 3

[0061] Add acetic acid and methanol into the reactive distillation column to synthesize methyl acetate.

[0062] Add the synthesized methyl acetate into the reaction flask and feed chlorine gas to synthesize methyl chloroacetate.

[0063] Mix and stir 95.5 g (1 mol) of phenol, 350 g toluene, 100 g butanol, and 125.2 g (1 mol) of sodium hydroxide aqueous solution with a mass fraction of 32%, raise the temperature to about 114°C, and react with water for 1 hour. The neutralized solution was slightly cooled to 120°C, 109.8 g (0.99 mol) of methyl chloroacetate was added dropwise, and the addition was completed in 4 hours, then the temperature was raised to 116°C, and the reaction was kept for 2 hours. Cool the reaction solution to 100°C, add 150g of water, adjust the pH to 7, let stand to separate layers, add 40g of toluene to the water layer for extraction, and separate the organic layer by vacuum distillation to obtain 163.35g of the product with a purity of 99.2% and a yield of...

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Abstract

The invention provides a preparation method of phenoxyacetic ester, wherein the preparation method includes the following steps: A) carrying out esterification reaction of acetic acid and alcohol to obtain acetic ester; B) introducing chlorine gas into acetic ester, and carrying out reaction to obtain chloroacetic ester; C) dehydrating a phenol compound and alkaline hydroxide into a salt in an organic solvent to obtain a salt of the phenol compound; D) after salt formation, mixing with chloracetic ester prepared in the step B), and carrying out condensation reaction to obtain phenoxyacetic ester, wherein the organic solvent is a mixture of any two kinds of toluene, xylene, chlorobenzene, phenol, butanol and isobutanol. The phenol is dehydrated into the salt in the mixed organic solvent, the system still maintains a uniform state in the dehydration process, continuous production is achieved, the dehydration efficiency is high and the efficiency of the whole production process is high. Moreover, the raw materials are easy to obtain, the production period is short, water is not needed in the reaction process, the energy consumption is low, the production cost is low, the yield of acetic acid is 99% or more, and the total yield of phenol can reach 99% or more.

Description

technical field [0001] The invention relates to the technical field of herbicide preparation, in particular to a preparation method of phenoxyacetate. Background technique [0002] Phenoxyacetate herbicides are the first type of hormone-type selective herbicides commercially produced in the world. They are environmentally friendly, have the characteristics of short residual period and low toxicity to humans and other organisms, and rarely produce drug resistance. It is mainly used to control dicotyledonous weeds, sedges and some malignant weeds in grass crops such as corn and wheat. The most widely used phenoxyacetate herbicides are chlorophenoxyacetate series. Among them, 2,4-dichlorophenoxyacetate is the most widely used. [0003] At present, the preparation method of 2,4-dichlorophenoxyacetate mainly comprises the following two steps: [0004] 1) Using phenol as the main raw material, 2,4-dichlorophenol is obtained through chlorination; [0005] 2) 2,4-dichlorophenol ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/708C07C67/31C07C67/08C07C69/14C07C67/307C07C69/63C07C37/66C07C39/235
Inventor 孙国庆侯永生贺恩静迟志龙胡义山
Owner SHANDONG RUNBO BIOTECH CO LTD
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