Chloration method for phenoxyacetic acid and derivatives thereof

A chlorination agent and compound technology, applied in the field of chlorination of phenoxyacetic acid and its derivatives, can solve the problems of large waste water, difficult control of chlorination depth, unsuitable for industrial production, etc., and achieve the effect of easy industrialization

Inactive Publication Date: 2012-02-01
DALIAN RES & DESIGN INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method produces a large amount of waste water, and the chlorination de

Method used

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  • Chloration method for phenoxyacetic acid and derivatives thereof
  • Chloration method for phenoxyacetic acid and derivatives thereof
  • Chloration method for phenoxyacetic acid and derivatives thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 100 g of dichloroethane, 15.2 g of phenoxyacetic acid, 0.1 g of boron trifluoride, and 0.2 g of sulfurous acid into a 250 ml four-necked bottle equipped with a thermometer, stirring, reflux condenser, and tail gas recovery device, and heat up to 50°C 14.0 g of sulfuryl chloride was slowly and uniformly added, and the addition was completed in 2 hours. After the reaction was completed, the temperature was lowered and filtered to obtain 17.8 g of 4-chlorophenoxyacetic acid with a purity of 99.23% and a yield of 94.9%.

[0028] Adopt the same condition as embodiment 1, just change catalyst, the results are shown in Table 1.

[0029] Chlorination of phenoxyacetic acid under different catalysts in table 1

[0030] experiment number

Embodiment 2

[0032] Add 100g of chloroform, 15.2g of phenoxyacetic acid, 0.1g of boron trifluoride, and 0.2g of sulfurous acid into a 250ml four-necked bottle equipped with a thermometer, stirring, reflux condenser, and tail gas recovery device, heat up to 50°C, and slowly Add 14.0 g of sulfuryl chloride at a uniform speed and complete the addition in 2 hours. After the reaction, cool down and filter to obtain 17.1 g of 4-chlorophenoxyacetic acid with a purity of 99.15% and a yield of 91.2%.

[0033] Using the same conditions as in Example 2, only changing the solvent, the results are shown in Table 2.

[0034] Chlorination of phenoxyacetic acid under different solvents in table 2

[0035] experiment number

Embodiment 3

[0037] Add 100 g of dichloroethane, 15.2 g of phenoxyacetic acid, 0.1 g of boron trifluoride, and 0.2 g of sulfurous acid into a 250 ml four-necked bottle equipped with a thermometer, stirring, reflux condenser, and tail gas recovery device, and heat up to 50°C , slowly and uniformly added 29.0 g of sulfuryl chloride, and the addition was completed in 4 hours. After the reaction was completed, the temperature was lowered and filtered to obtain 19.8 g of 2,4-dichlorophenoxyacetic acid with a purity of 98.05% and a yield of 90.5%.

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Abstract

The invention provides a chloration method for phenoxyacetic acid and derivatives thereof, which comprises the following steps that: raw materials of the phenoxyacetic acid or the derivatives of the phenoxyacetic acid and chlorinating agents take reaction at a certain temperature in organic solvents under the effect of catalysts, wherein the chlorinating agents can be chlorine gas, sodium hypochlorite, calcium hypochlorite and sulfuryl chloride, the catalysts can be lewis acid and sulfurated substances, and solvents can be dichloromethane, dichloroethane, trichloromethane, carbon tetrachloride, formic acid, ethyl acetate, benzene, toluene, dimethylbenzene, chlorobenzene and o-dichlorobenzene. The method has the advantages that the operation can be carried out under the waterless condition, the generation of a large amount of industrial waste water is avoided, the used catalysts are safe and are easy to obtain, the solvents can be cyclically used, and the industrialization is easy.

Description

technical field [0001] The invention relates to a chlorination method of phenoxyacetic acid and its derivatives, in particular to a para-chlorination method of phenoxyacetic acid and its derivatives. Background technique [0002] 2-Methyl-4-chlorophenoxyacetic acid (also known as o-methyl-p-chlorophenoxyacetic acid) is one of the earliest organic herbicide species used, and it is still the basic species of herbicides today. 2-Methyl-4-chlorophenoxyacetic acid is an excellent herbicide with the characteristics of high efficiency, low toxicity, low residue, and little environmental pollution. It is not only a hormone-type herbicide, but also a plant growth regulator. [0003] 2-Methyl-4-chlorophenoxyacetic acid can be prepared by chlorination of 2-methyl-phenoxyacetic acid (also known as o-methylphenoxyacetic acid) or a salt thereof. For example, Polish patent PL115188B3 (Inst Przemyslu Organiczego. Process for manufacturing 2-methyl-4-chlorophenoxyacetic acid. 1981-03-31) di...

Claims

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Application Information

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IPC IPC(8): C07C59/70C07C51/363
Inventor 韩建国邵玉昌左洪亮
Owner DALIAN RES & DESIGN INST OF CHEM IND
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