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Synthetic method of 2-methyl-4-chlorophenoxyacetic acid

A technology of o-methylphenoxyacetic acid and chlorophenoxyacetic acid, which is applied in chemical instruments and methods, carboxylate preparation, carboxylate preparation, etc., can solve the problem of reducing product content and yield, refractory phenol-containing wastewater, Incomplete neutralization and other problems, to achieve the effect of reducing energy consumption, less three wastes, and less by-products

Inactive Publication Date: 2018-02-16
ANHUI HUAXING CHEM IND CO LTD
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  • Abstract
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  • Claims
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Problems solved by technology

Therefore, the global research on 2-methyl-4-chlorophenoxyacetic acid has not stopped so far.
[0003] The synthetic route of 2-methyl-4-chlorophenoxyacetic acid mainly adopts neutralization-condensation-chlorination, and most manufacturers use sodium hydroxide to neutralize and chlorine to chlorinate, but there is no neutralization in sodium hydroxide. The shortcomings of thoroughness and few by-products reduce the content and yield of the product; and the use of chlorine chlorination will produce a large amount of difficult-to-treat phenol-containing wastewater

Method used

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  • Synthetic method of 2-methyl-4-chlorophenoxyacetic acid

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Embodiment 1

[0019] A synthetic method of 2-methyl-4-chlorophenoxyacetic acid includes the following steps:

[0020] (1) Preparation of sodium chloroacetate solution: Add quantitative amounts of chloroacetic acid and sodium bicarbonate to a special reactor, mix and stir for 2 hours, and use water at 25°C for cyclic heating. After sampling, add water to completely dissolve it as the end of the reaction. ;

[0021] (2) Preparation of o-methylphenoxyacetic acid: add o-methylphenol into a special reactor, put it in the reactor together with sodium chloroacetate under stirring and heat to reflux, add dropwise 32% sodium hydroxide solution, and Make sure the pH value of the solution is 8-9. After the dripping, continue to dephenolize the water until the temperature rises to 120℃, then start to cool down and add water, and then add hydrochloric acid to adjust the pH of the solution. After the acid adjustment is finished, filter with suction and dry the filter cake to get it. O-methylphenoxyacetic aci...

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Abstract

The invention discloses a synthetic method of 2-methyl-4-chlorophenoxyacetic acid, and relates to the technical field of organic synthesis. The target product 2-methyl-4-chlorophenoxyacetic acid is prepared by taking o-methylphenol as a raw material, reacting with sodium chloroacetate udner the effect of sodium bicarbonate; neutralizing by hydrochloric acid to obtain a midbody 2-methyl phenoxyacetic acid; finally, chloridizing the midbody 2-methyl phenoxyacetic acid by chlorine. The method applies sodium bicarbonate to replace sodium hydroxide to carry out neutralization, the neutralization reaction is small in heat release and few in side product; the method is good for improving product content and yield; besides, the chorine is applied to chloridize, and methylbenzene is used as the solvent; the generated acid is used as the neutralizing acid of the next batch, thus the massive phenolic wastewater is reduced, and it can meet the requirement of modern green pesticide; carbon dioxideis discharged from the neutralization reaction, the reaction heat is reduced, and the energy consumption is reduced. Compared with an original technique, the reaction technique has obvious advantagesof high yield, few wastes and low energy consumption.

Description

Technical field: [0001] The invention relates to the technical field of organic synthesis, in particular to a method for synthesizing 2-methyl-4-chlorophenoxyacetic acid. Background technique: [0002] There are many types of herbicides on the market, and phenoxyacetic acid herbicides occupy an important position among them. Due to the different substituents and substitution positions on the benzene ring, and the different number of carbon atoms of the carboxylic acid, different phenoxycarboxylic acid herbicides are formed. 2-Methyl-4-chlorophenoxyacetic acid is a hormone-type systemic phenoxycarboxylic acid herbicide developed and popularized by Imperial Chemical Industrirs in 1945. It has strong physiological activity on plants and is easy to become roots and leaves. Surface absorption and conduction. At low concentrations, it has a growth stimulating effect on crops, which can prevent flower drop, fruit drop, seedless fruit formation, promote fruit maturity and rooting of cu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/367C07C51/41C07C51/347C07C51/363C07C59/70
CPCC07C51/367C07C51/347C07C51/363C07C51/412C07C59/70
Inventor 王玉贵庆光平尹仕兵付昌群吴春喜
Owner ANHUI HUAXING CHEM IND CO LTD
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