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A kind of electrolytic synthesis process of 3,6-dichloropicolinic acid

A technology of clopicolinic acid and clopyralid, which is applied in the direction of electrolysis process, electrolysis components, electrolysis organic production, etc., can solve the problems of loss and large salty wastewater, and achieve the effect of reducing material consumption

Inactive Publication Date: 2016-01-20
HANGZHOU SAILONG CHEM IND +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantage of this method is that the 3,6-dichloropicolinic acid in the acid analysis mother liquor will be lost in a large amount during the electrodialysis process, and a large amount of saline wastewater will still be produced

Method used

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  • A kind of electrolytic synthesis process of 3,6-dichloropicolinic acid
  • A kind of electrolytic synthesis process of 3,6-dichloropicolinic acid
  • A kind of electrolytic synthesis process of 3,6-dichloropicolinic acid

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Experimental program
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Effect test

Embodiment 1

[0030] Use a bipolar membrane electrodialyzer to treat the acid analysis mother liquor (3), its composition is 0.02mol / L diclopyralid (DCP)+0.005mol / L clopyralid+1mol / LNaCl+0.1mol / LHCl, bipolar The arrangement of membrane electrodialyzers is shown in figure 2(A). Acidic aqueous solution (4), basic aqueous solution (6) and water (7) are separated. The concentration of NaOH in the separated alkaline aqueous solution (6) is 2.5 mol / L, and the alkaline aqueous solution (6) and water (7) are used as a batching solution before electrolysis and supplementary materials during electrolysis for standby use. The concentration of hydrochloric acid in the separated acidic aqueous solution (4) is 2.0 mol / L. First, the pH of the acidic aqueous solution (4) is adjusted to 0, and the acidic aqueous solution (4) is concentrated by the concentrated electrodialysis method. The arrangement of the concentrated electrodialysis method See image 3 . After the treatment, the concentrated solution ...

Embodiment 2

[0039] Use a bipolar membrane electrodialyzer to treat the acid analysis mother liquor (3), its composition is 0.02mol / L diclopyralid (DCP)+0.005mol / L clopyralid+1mol / LNaCl+0.1mol / LHCl, bipolar The arrangement of membrane electrodialyzers is shown in figure 2 (B), the membrane materials used are all provided by Hangzhou Sailong Chemical Co., Ltd. Acidic aqueous solution (4), basic aqueous solution (6) and water (7) are separated. The NaOH concentration in the separated alkaline aqueous solution (6) is 3 mol / L, and the alkaline aqueous solution (6) and water (7) are used as a batching solution before electrolysis and supplementary materials during electrolysis for standby use. The concentration of hydrochloric acid in the separated acidic aqueous solution (4) is 0.5 mol / L, the pH of the acidic aqueous solution (4) is adjusted to 1.0, and then the acidic aqueous solution (4) is concentrated by the concentrated electrodialysis method, the arrangement of the concentrated electro...

Embodiment 3

[0042] Use a bipolar membrane electrodialyzer to treat the acid analysis mother liquor (3), its composition is 0.02mol / L diclopyralid (DCP)+0.005mol / L clopyralid+1mol / LNaCl+0.1mol / LHCl, bipolar The arrangement of membrane electrodialyzers is shown in figure 2 (A), the membrane materials used are all provided by Hangzhou Sailong Chemical Co., Ltd. Acidic aqueous solution (4), basic aqueous solution (6) and water (7) are separated. The NaOH concentration in the separated alkaline aqueous solution (6) is 3 mol / L, and the alkaline aqueous solution (6) and water (7) are used as a batching solution before electrolysis and supplementary materials during electrolysis for standby use. The concentration of hydrochloric acid in the separated acidic aqueous solution (4) is 1.2 mol / L, adjust the acidic aqueous solution (4) to pH = 0.5, and then concentrate the acidic aqueous solution (4) by concentrated electrodialysis. For the arrangement of the concentrated electrodialysis method, see ...

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Abstract

The invention discloses an electrolytic synthesis technology of 3,6-dichloropicolinic acid. The technology includes performing acid precipitation with hydrochloric acid after electrolysis which adopts an alkaline solution (1) of 3,4,5,6-tetrachloropyridine-2-carboxylic acid and / or 3,5,6-trichloropicolinic acid as an electrolyte is completed, filtering to obtain the 3,6-dichloropicolinic acid, and recovering and reutilizing the acid precipitating mother liquor (3) obtained by filtration. A recovering and reutilizing method of the acid precipitating mother liquor (3) comprises steps of treating the acid precipitating mother liquor (3) by bipolar membrane electroosmosis to obtain an aqueous alkaline solution (6), water (7) and an aqueous acid solution (4) having a hydrochloric acid concentration of 0.5-2.0 mol / L; adjusting the pH of the aqueous acid solution (4) to be 0-1; and concentrating the aqueous acid solution (4) by electrolytic concentration to obtain a desalinate liquid (8) having a pH of 2.0-4.0 and a concentrate (5), wherein the aqueous alkaline solution (6) and the water (7) are used for preparing the alkaline solution (1), the concentrate (5) is used for acid precipitation, and the desalinate liquid (8) is used for adjusting the pH of the aqueous acid solution (4) and / or preparing the alkaline solution (1).

Description

(1) Technical field [0001] The invention relates to an electrolytic synthesis process of 3,6-dichloropicolinic acid. (2) Background technology [0002] 3,6-Dichloropicolinic acid is a pesticide with low toxicity and high activity, which can be used not only as insecticide and herbicide, but also as fungicide and plant growth regulator; Not only is it less toxic to mammals, fish and poultry, but it also has a short lifespan in the soil, so it is a green pesticide with high efficiency and low toxicity. [0003] At present, the main synthesis method is the electrolytic reduction dechlorination method of 3,4,5,6-tetrachloropicolinic acid. The preparation of 3,6-dichloropicolinic acid by electrolytic reduction and dechlorination was first proposed by US patent US4217185, and a series of patents reported later US4460441, EP0254982, US4755266, US4592811, ZL200710050524, ZL200710050524, ZL200810059789, ZL2015110 were respectively in the electrode structure and 5 Improvement method...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B3/00
Inventor 马淳安徐颖华毛信表褚有群赵峰鸣
Owner HANGZHOU SAILONG CHEM IND