Selective electrolysis hydrogenation and dechlorination method for chlorinated organic matter

A chlorinated organic compound, hydrodechlorination technology, applied in electrolysis process, organic chemistry, electrolysis components, etc., can solve problems such as increased energy consumption, graphite influence, fragmentation, etc., to reduce reaction energy consumption and avoid foaming. Effect

Active Publication Date: 2011-09-14
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, the electrolytic cells of the selective electrolytic hydrodechlorination method can not meet the above basic conditions well, so the method is greatly restricted in industrial application
In terms of anode: the graphite electrode proposed by U.S.Pat.No.4,242,185 has the following problems: (1) The type of graphite significantly affects the yield and purity of 3,6-dichloropicolinic acid, even the ATL type with excellent comprehensive performance Graphite will also have serious fragmentation and aging pheno

Method used

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  • Selective electrolysis hydrogenation and dechlorination method for chlorinated organic matter
  • Selective electrolysis hydrogenation and dechlorination method for chlorinated organic matter

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The preparation of embodiment 1 active silver electrode

[0021] In a 250mL beaker, sieve silver was used as the working electrode, with an apparent size of 0.05 cm × 5 cm × 5 cm, graphite with the same apparent size as the anode, and the cathode and anode were separated by 2 cm. The electrolytic solution is 200mL of 2.9wt% sodium chloride+2wt% sodium hydroxide aqueous solution, and the electrolytic solution remains static. Then the silver electrode is oxidized by direct current, the current density is 50mA / cm 2 , after the electrode potential drops to 0.9 volts, the polarity is reversed to reduce the silver electrode, and the current density is 100mA / cm 2 After the electrode potential rises to -0.8 volts, the power supply is stopped, the reaction temperature is controlled at 25°C, and the cell voltage is 2.5-3.5V. Take out the silver electrode and immerse it in deionized water for later use.

Embodiment 2

[0022] Example 2 Preparation of 3,6-dichloropicolinic acid by electrolysis of 3,4,5,6-tetrachloropicolinic acid

[0023] In a 1000 mL beaker, 78 g of 3,4,5,6-tetrachloropicolinic acid (3,4,5,6-TCP) (98% content) was dissolved in 0.5M Na 2 CO 3 in aqueous solution (1000 mL). The active silver electrode prepared with embodiment 1 is negative electrode, and ruthenium titanium electrode is anode (its surface is made up of ruthenium dioxide and titanium dioxide, wherein the content of ruthenium is 15g / m 2 ;Titanium content is 15g / m 2 ;), electrolysis was carried out at 50°C (the current was 5A), and after 2 hours of electrolysis, the electrolysis was stopped for 15 minutes to restore the electrode activity. After the electrode activity was restored, the electrolysis was continued for 2 hours (the current was 5A), and then the electrolysis was stopped for 15 minutes to restore the electrode activity. After the electrode activity is restored again, add 10 grams of sodium hydroxid...

Embodiment 3～ Embodiment 5

[0025] According to the experimental parameters in Table 1:

[0026] Table 1 1000mL scale electrolytic dechlorination to prepare 3.6-dichloropicolinic acid

[0027]

[0028]

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Abstract

The invention discloses a selective electrolysis hydrogenation and dechlorination method for a chlorinated organic matter. The method comprises the following steps of: dissolving the chlorinated organic matter in alkaline solution serving as a reaction medium, and performing an electrolytic reaction; and acidizing after the electrolytic reaction is finished to obtain a target product, wherein a ruthenium titanium positive electrode is used as the positive electrode of the electrolytic reaction, a silver electrode is used as the negative electrode of the electrolytic reaction, and energizationis stopped for 5 to 60 minutes when electrolysis is performed for 1 to 5 hours every time in the electrolysis reaction process. The method is easy to operate; and by the method, the step of repeatedly performing electrochemical oxidation on the activated silver electrode in the reaction process can be prevented, and the energy consumption of the reaction can be effectively reduced.

Description

(1) Technical field [0001] The invention relates to a selective electrolytic hydrodechlorination method for chlorinated organic matter, in particular to a method for preparing 3,6-dichloropicolinic acid through selective electrolytic hydrodechlorination. (2) Technical background [0002] Selective electrolytic hydrodechlorination can be used to synthesize partially chlorinated organic compounds, and many partially chlorinated organic compounds are very important pharmaceuticals, pesticide intermediates or raw materials. Such as 2,3,5,6-tetrachloropyridine and 2,3,5-trichloropyridine are important intermediates for the synthesis of insecticides and herbicides, which can be prepared by selective electrolytic hydrodechlorination of pentachloropyridine ( U.S. Pat. No. 3,694,332 and U.S. Pat. No. 4,242,183). In a similar manner, 3,4,5,6-tetrachloropicolinic acid or 3,5,6-trichloropicolinic acid can be reacted to 3,6-dichloropicolinic acid (U.S. Pat. No. 4,242,185). [0003] If ...

Claims

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Application Information

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IPC IPC(8): C25B3/04C25B11/08C07D213/79C25B3/25
Inventor 马淳安徐颖华褚有群
Owner ZHEJIANG UNIV OF TECH
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