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

Method for synthesizing 4-amino-3, 6-dichloropicolinic acid through electrolytic dechlorination, product and application

A technology of clopicolinic acid and triclopyralid, which is applied in the field of electrochemical synthesis, can solve the problems of "unstable electrolysis voltage, large amount of waste salt produced, high tank pressure in the later stage, etc., so as to avoid large alkali consumption, excellent quality, The effect of reducing energy consumption

Active Publication Date: 2022-02-22
YONGNONG BIOSCI +1
View PDF8 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to overcome the above deficiencies, the object of the present invention is to provide a method for electrolytic dechlorination to synthesize 4-amino-3,6-dichloropicolinic acid, and the 4-amino-3,6-dichloro Products and applications of picolinic acid; the invention can not only improve the synthesis yield and quality of 4-amino-3,6-dichloropicolinic acid products, but also avoid "large alkali consumption, large amount of waste salt", "electrolysis voltage Unstable" and "high trough pressure in the later stage"

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
  • Method for synthesizing 4-amino-3, 6-dichloropicolinic acid through electrolytic dechlorination, product and application
  • Method for synthesizing 4-amino-3, 6-dichloropicolinic acid through electrolytic dechlorination, product and application
  • Method for synthesizing 4-amino-3, 6-dichloropicolinic acid through electrolytic dechlorination, product and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] The method for synthesizing 4-amino-3,6-dichloropicolinic acid by electrolytic dechlorination of acidic anolyte:

[0054] The electrolysis conditions are: in an H-type electrolytic cell with Nafion 324 cationic membrane as a diaphragm (such as figure 1 ); the activated silver mesh electrode prepared by the above method is the cathode, and the titanium-based iridium oxide coating sheet (geometric size is 0.5cm × 4.0cm × 6.0cm) of the same area is the anode, and the distance between the anode and cathode is 6cm; 200mL Contains 0.5M H 2 SO 4 The aqueous solution is the anolyte, and the 100mL aqueous solution containing 0.3M 4-amino-3,5,6-trichloropicolinic acid + 0.6M NaOH is the catholyte. Stir catholyte at 30-35°C and feed 2A / dm 2 The electric current, stop electrolysis after reacting for 6 hours.

[0055] During the electrolysis, it was observed that the voltage between the cathode and anode stabilized in the range of 4.4–5.1 V.

[0056] After the electrolysis end...

Embodiment 2

[0059] The method for synthesizing 4-amino-3,6-dichloropicolinic acid by electrolytic dechlorination of acidic anolyte:

[0060] The electrolysis conditions are: in an H-type electrolytic cell with Nafion 324 cationic membrane as a diaphragm (such as figure 1 ); the activated silver mesh electrode prepared by the above method is the cathode, and the titanium-based iridium oxide coating sheet (geometric size is 0.5cm × 4.0cm × 6.0cm) of the same area is the anode, and the distance between the anode and cathode is 6cm; 200mL Contains 2.0M H 2 SO 4 The aqueous solution is the anolyte, and the 100mL aqueous solution containing 0.6M 4-amino-3,5,6-trichloropicolinic acid + 1.2M NaOH is the catholyte. Stir catholyte at 55-60°C and feed 5A / dm 2 After 2 hours of reaction, adjust the current density to 2A / dm 2 Electrolysis was performed for another 5 hours, and the electrolysis was stopped.

[0061] During electrolysis, it was observed that the voltage between the cathode and anod...

Embodiment 3

[0065] The method for synthesizing 4-amino-3,6-dichloropicolinic acid by electrolytic dechlorination of acidic anolyte:

[0066] The electrolysis conditions are: in an H-type electrolytic cell with Nafion 324 cationic membrane as a diaphragm (such as figure 1 ); the activated silver mesh electrode prepared by the above method is the cathode, and the titanium-based iridium oxide coating sheet (geometric size is 0.5cm × 4.0cm × 6.0cm) of the same area is the anode, and the distance between the anode and cathode is 6cm; 200mL Contains 5.0M H 2 SO 4 The aqueous solution is the anolyte, 100mL contains 1.0M 4-amino-3,5,6-trichloropicolinic acid + 1.0M K 2 CO 3 The aqueous solution is catholyte (pH ~ 8). At 85-90°C, stir the catholyte and feed it with 10A / dm 2 The electric current, stop electrolysis after reacting for 5 hours.

[0067] During electrolysis, it was observed that the voltage between the cathode and anode stabilized in the range of 4.5–4.7 V.

[0068] After the e...

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 method for synthesizing 4-amino-3, 6-dichloropicolinic acid (aminopyralid) through electrolytic dechlorination, a product and application. The method comprises the steps of dividing an electrolytic cell into an anode region and a cathode region by adopting a cationic membrane, carrying out an electrolytic reaction by taking an acidic electrolyte as an anolyte and an alkaline electrolyte containing 4-amino-3, 5, 6-trichloropicolinic acid or salt thereof as a catholyte, and separating 4-amino-3, 6-dichloropicolinic acid from the catholyte after electrolysis is finished, wherein the acidic electrolyte is an acidic solution or an acidic solution containing metal salt. The invention also provides white powder containing 4-amino-3, 6-dichloropicolinic acid prepared according to the method and a product application. According to the invention, the specific acidic electrolyte is adopted, the yield and quality of the 4-amino-3, 6-dichloropicolinic acid product can be improved in the electrolysis process, and the problems that the alkali consumption is large, the amount of generated waste salt is large, the electrolysis voltage is not stable, and the later-period cell pressure is high are solved.

Description

technical field [0001] The present invention relates to the field of electrochemical synthesis, in particular to a method for electrolytic dechlorination to synthesize 4-amino-3,6-dichloropyridinecarboxylic acid, and a method containing 4-amino-3,6-dichloropyridine prepared according to the method. Products and applications of formic acid. Background technique [0002] 4-Amino-3,6-dichloropicolinic acid, whose trade names are Amazoram, Aminopyralid, and Dichloroaminopyralid, is a pyridinecarboxylic acid herbicide, which can quickly enter the plant body, causing Plant growth interruption and rapid death are used primarily for weed control in pastures, plantations and non-crop areas. In addition, 4-amino-3,6-dichloropicolinic acid is also a key intermediate in the synthesis of halopyridine and halopyridine. Fluclopyridine and cloflupyridine are new aryl picolinate herbicides developed by Dow AgroSciences. They are new varieties of hormonal herbicides and have the characteris...

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
Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/05C25B3/07C25B3/09C25B3/11C25B3/25A01N43/40A01P13/00
CPCC25B3/09C25B3/11C25B3/07C25B3/05C25B3/25A01N43/40
Inventor 吴承骏肖恒侨黄耀师李方明
Owner YONGNONG BIOSCI
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