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Method for synthesizing phenoxy carboxylate herbicide original medicine

A technology for phenoxycarboxylic acids and herbicides, applied in the field of pesticide synthesis, can solve the problems of high consumption of chlorinated carboxylic acids, increased environmental protection pressure, and high production costs, achieve obvious economic benefits and cost advantages, and reduce the production environment. Influence, the effect of improving product yield

Active Publication Date: 2013-06-19
SHANDONG WEIFANG RAINBOW CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process conditions of this method are mature, and it is convenient to realize large-scale production. The content of the obtained phenoxycarboxylic acids is > 96%, and the yield > 95%. However, the above-mentioned synthetic method has the following disadvantages: the above-mentioned synthetic method has the following disadvantages: 1. The synthesis reaction is incomplete, and after-treatment is required, the sodium salt is separated and washed, and then dissolved in salt and acidified to obtain a qualified product, which results in large water consumption, complicated process, large equipment investment, and high production cost.
2. In order to make the conversion of chlorophenol higher, the feeding ratio of chlorocarboxylic acid is higher. Usually, the molar ratio of chlorophenol is more than 1.3 times that of chlorophenol, which causes the consumption of chlorocarboxylic acid to be high
3. The solid-liquid separation process after synthesis has a great impact on the environment, especially the smell, which increases the pressure on environmental protection
This not only makes the process complicated, but also the reaction temperature of this method is high, and the requirements for equipment materials are strict. When the post-processing phenol is steamed, the pH must be strictly controlled, and the operation requirements are relatively high.
[0005] It can be seen from the above description that both the aqueous method and the non-aqueous method have certain shortcomings, so finding a new method to improve the synthetic conversion rate and simple process is the focus of the synthesis of phenoxycarboxylic acid pesticides

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035]Add 800g of 2,4-dichlorophenol with an effective content of 98% to the kneader, slowly add 404g of 50% NaOH solution, and after dissolving into sodium salt, raise the temperature and distill off the water to obtain anhydrous solid sodium chlorophenol salt. Take 487g of 98% chloroacetic acid, add 200g of water, and then dropwise add 613.3g of 32% NaOH solution to obtain sodium chloroacetate solution. Add 200g of sodium carbonate solid to the kneader at a constant speed during the process. Afterwards, sodium chloroacetate solution was added to the previous sodium chlorophenol salt, and the temperature was raised to 120°C to carry out the synthesis reaction. During the reaction, the water vapor generated in the system was discharged. After reacting for 5 hours, add 3000ml of water to the kneader to cool down, and add 716g of 30% hydrochloric acid to acidify when the temperature is lowered to 70°C. Suction filtration and washing with 2500g of water to obtain the wet materia...

Embodiment 2

[0037] Add 800g of 2,4-dichlorophenol with an effective content of 98% to the kneader, slowly add 565.6g of 50% KOH solution, and after dissolving into potassium salt, raise the temperature and distill off the water to obtain anhydrous solid potassium chlorophenate. Take 520.3 g of 98% chloroacetic acid, add 250 g of water, and then dropwise add 944.2 g of 32% KOH solution to obtain a potassium chloroacetic acid solution. Afterwards, the potassium chloroacetate solution was added to the potassium chlorophenate, and the temperature was raised to 100°C to carry out the synthesis reaction, and the water vapor generated in the system was discharged during the reaction. In the process, add 260g of potassium carbonate solid to the kneader at a uniform speed. After reacting for 5 hours, add 3000ml of water to the kneader to cool down, and add 656g of 30% hydrochloric acid to acidify when the temperature is lowered to 70°C. Suction filtration and washing with 2500g of water to obtain...

Embodiment 3

[0039] Add 600g of 2-methyl-4-chlorophenol with an effective content of 98% to the kneader, slowly add 346.6g of 50% NaOH solution, and after dissolving into sodium salt, heat up and distill off the water to obtain anhydrous solid sodium chlorophenol salt. Take 437.7g of 98% chloroacetic acid, add 220g of water, and then dropwise add 567.4g of 32% NaOH solution to obtain sodium chloroacetate solution. Afterwards, sodium chloroacetate solution was added to the previous sodium chlorophenol salt, the temperature was raised to 135°C, and the synthesis reaction was carried out, and the water vapor generated in the system was discharged during the reaction. Add 200g of sodium carbonate solid to the kneader at a constant speed during the process. After reacting for 7 hours, add 3000ml of water to the kneader to cool down, and add 602g of 30% hydrochloric acid to acidify when the temperature is lowered to 80°C. Suction filtration and washing with 2500g of water to obtain 2-methyl-4-c...

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PUM

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Abstract

The invention discloses a method for synthesizing a phenoxy carboxylate herbicide original medicine. The method comprises the following steps of: adding chlorophenol and alkaline liquid to a reactor, reacting to produce soluble chlorophenate, and drying liquid through evaporating, so as to obtain solid soluble chlorophenate; adding chlorinated carboxylate liquid into the reactor, reacting to produce soluble phenoxy carboxylate, and additionally adding an alkaline substance during reaction; and adding water to the reactor to cool, adding acid to acidify, filtering and washing so as to obtain a wet phenoxy carboxylate material, and drying the wet material, thereby obtaining the phenoxy carboxylate herbicide original medicine. According to the method, after the reacting synthesis is completed, qualified products can be obtained through direct acidification; and due to the reduction of processing links, the influence on a producing environment is reduced, the water consumption is reduced, the synthesis is more environment-friendly, the problem of high water consumption in the traditional synthesis is solved, and the requirements on clean production are met, so that the method has an obvious economic benefit and a cost advantage.

Description

technical field [0001] The invention relates to a method for synthesizing the original drug of herbicides, in particular to a method for synthesizing the original drug of phenoxycarboxylic acid herbicides, and belongs to the technical field of pesticide synthesis. Background technique [0002] Phenoxycarboxylic acid herbicides are hormone-type systemic herbicides, which have strong physiological activity on plants, promote plant growth at low concentrations, and inhibit the growth of dicotyledonous plants at high concentrations. Deforms the plant until it dies. Because of its excellent characteristics of high efficiency, low toxicity, low residue, and no pollution to the environment, phenoxycarboxylic acid herbicides are now widely used. [0003] Phenoxycarboxylic acid herbicides include 2,4-D (2,4-dichlorophenoxyacetic acid), 2,4-DP (2-(2,4-dichlorophenoxy)-propionic acid), 2, 4-DB (2,4-dichlorophenoxybutyric acid), MCPA (2-methyl-4-chlorophenoxyacetic acid), MCPB (2-meth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/367C07C59/70C07C59/68
Inventor 孙国庆侯永生刘凯李宗清李志清张文华徐淑强王星博于海涛袁国连朱素娟侯明坤李建成周惠
Owner SHANDONG WEIFANG RAINBOW CHEM
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