Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

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
View PDF5 Cites 24 Cited by
  • 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 depth is difficult to control, so it is not suitable for industrial production

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • 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%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07C59/70C07C51/363
Inventor 韩建国邵玉昌左洪亮
Owner DALIAN RES & DESIGN INST OF CHEM IND
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com