Selective electrochemical reduction method of halogenated picolinic acid or salt compounds of halogenated picolinic acid

A technology for halogenated picolinic acid and salt compounds, which is applied in the field of halogen substituents at 6-position, can solve the problem of not proving 3- and 6-halogens, etc., and achieve the effect of reducing and removing

Active Publication Date: 2014-10-08
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, there is no relevant report proving that 3- and 6-halogens are easier to reduce in electrolytic reduction.

Method used

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  • Selective electrochemical reduction method of halogenated picolinic acid or salt compounds of halogenated picolinic acid
  • Selective electrochemical reduction method of halogenated picolinic acid or salt compounds of halogenated picolinic acid
  • Selective electrochemical reduction method of halogenated picolinic acid or salt compounds of halogenated picolinic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Example 1 Preparation of active silver electrode

[0041] In the non-diaphragm electrolyzer, the expanded mesh silver is used as the working electrode, the apparent size is 0.1cm×10cm×10cm, the graphite of the same apparent size is the anode, and the anode and cathode are separated by 2cm. The electrolyte is 1000 mL of an aqueous solution of 2.9 wt% sodium chloride + 2 wt% sodium hydroxide, and the electrolyte remains static. Then apply direct current to oxidize the silver electrode, the current density is 50mA / cm 2 After the electrode potential drops to 0.9 volts, reverse the polarity to restore the silver electrode, and the current density is 100mA / cm 2 After the electrode potential rises to -0.8V, stop energizing, control the reaction temperature at 25°C, and the cell voltage at 2.5~3.5V. Take out the silver electrode and immerse it in deionized water for later use.

Embodiment 2

[0042] Example 2 Electrolytic synthesis of 3,5-dichloropicolinic acid (3,5-D)

[0043] The diaphragm plate and frame tank is an electrolytic reactor, the perfluorosulfonic acid membrane is the diaphragm, the activated expanded screen silver is the cathode, and the mesh 316 stainless steel is the anode. 1000mL pH=4 0.25mol / L phosphate buffer solution is the catholyte, and the mass of 3,5,6-trichloropicolinic acid (3,5,6-T, 98wt%) in the catholyte for the first time is 20 grams; 4wt % Sodium hydroxide aqueous solution is the anolyte. During the electrolysis process, 30wt% sulfuric acid is used to control the pH of the catholyte = 3~5, and 30 grams of 3,5,6-T are added to the catholyte step by step, the temperature is controlled at 30~35℃, and the current density is controlled at 3A / dm 2 . Stop electrolysis after supplying 4F / mol3,5,6-T electricity. After the catholyte was transferred to the beaker, sulfuric acid was added to adjust the pH=1, and then the temperature of the cath...

Embodiment 3～ Embodiment 9

[0045] Examples 3 to 9 were performed according to the experimental parameters in Table 1, and the rest of the operations were the same as in Example 2.

[0046] Table 11000mL scale electrolytic dechlorination to prepare 3,5-D experimental conditions and results a

[0047]

[0048]

[0049] a With the activated expanded mesh silver as the cathode, the electricity of 4F / mol reaction substrate is introduced.

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Abstract

The invention discloses a selective electrochemical reduction method of halogenated picolinic acid or salt compounds of the halogenated picolinic acid, and the method is as follows: using an acidic solution as a reaction medium, adding the halogenated picolinic acid or a salt compound of the halogenated picolinic acid, which is shown as formula (II) into the acidic solution to obtain an electrolytic reaction liquid for electrolytic reaction in an electrolytic tank using a chemistry inert material as a positive pole and a metallic material as a negative pole, and after the electrolytic reaction is completed, acidifying the electrolytic reaction liquid to recover a selective reduction product shown as formula (I); according to the method, high selective reduction removal of 6-halogen of multiple halogenated picolinic acid can be realized by the electrolytic reaction in the presence of a 3-and 5-or 3-halogen substituent group.

Description

(1) Technical field [0001] The present invention relates to a method for electrochemical reduction of halogenated picolinic acid or a salt compound of halogenated picolinic acid, in particular to the selective reduction of halogenated compounds by electrolysis in the presence of 3-position and 5-position or 3-position halogen substituents Method for the halogen substituent at the 6-position of picolinic acid or its salt compounds. (2) Background technology [0002] Recently, it has been discovered that derivatives of certain halogenated picolinic acids containing hydrogen at the 6-position (such as 3,5-dichloropicolinic acid, 3-chloropicolinic acid, etc.) not only have herbicidal activity but also can be used to treat and prevent Alzheimer's disease. And diabetes drugs. Therefore, there is a need to be able to prepare certain halogenated picolinic acids containing hydrogen at the 6-position from the corresponding 6-position halogenated derivatives, many of which are 3,6-dichloro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/04C25B3/25
Inventor 马淳安徐颖华丁旭芬马红星
Owner ZHEJIANG UNIV OF TECH
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