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Method and apparatus for electrolytic synthesis of 3,6-dichloropyridine-carboxylic acid

A technology of dichloropicolinic acid and electrolytic synthesis, applied in 3 fields, can solve problems such as endangering the health of operators and residents around the factory, large amount of methylene chloride, loss of methylene chloride, etc., and achieves great practical value, social and economic benefits, Stable operation process and high space-time efficiency

Inactive Publication Date: 2006-07-26
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method has the following disadvantages: (1) the amount of dichloromethane is large, and 90% of the 3 in the filtrate is extracted, and the volume of 6-D needs to use dichloromethane to be about three times of the volume of the filtrate; (2) the energy consumption is high, and two Although the boiling point of methyl chloride is low, a large amount of dichloromethane needs to be heated and volatilized, and the energy consumption cannot be ignored; (3) the loss of dichloromethane is serious, because the boiling point of dichloromethane is low, so dichloromethane is easy to volatilize in use (4) Serious pollution, dichloromethane is a highly toxic solvent, and dichloromethane volatilized into the air seriously endangers the health of operating workers and residents around the factory
This method better solves the problems of high energy consumption and serious loss of dichloromethane in conventional separation methods provided by US4217185, etc., but the increase in operation steps makes the process complicated, and the use of toxic chemical dichloromethane cannot be avoided at the same time

Method used

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  • Method and apparatus for electrolytic synthesis of 3,6-dichloropyridine-carboxylic acid
  • Method and apparatus for electrolytic synthesis of 3,6-dichloropyridine-carboxylic acid
  • Method and apparatus for electrolytic synthesis of 3,6-dichloropyridine-carboxylic acid

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Experimental program
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Effect test

Embodiment 1

[0063] refer to figure 1 , 6 , 7, 8, a kind of 3, the electrolytic synthesis equipment of 6-dichloropicolinic acid, comprise power supply 1, batching tank 12, electrolyzer 5, described power supply 1 is the periodic reversing power supply of voltage-stabilizing silicon controlled rectifier, The power supply 1 is connected to a current commutator 2, and the current commutator 2 is provided with a program control unit; the positive pole of the power supply 1 is connected to the anode of the electrolyzer, and the negative pole of the power supply 1 is connected to the cathode of the electrolyzer.

[0064] The anode is composed of a tab 40 , a rhombus mesh plate 41 and a current collector 42 . The cathode is supported by a polypropylene substrate 54 . The anode plate has a longitudinal diamond-shaped network structure, and the cathode plate has a transverse diamond-shaped network structure. The diamond-shaped network structure is formed by connecting a plurality of identical par...

Embodiment 2

[0068] refer to figure 1 , 6 , 7, 8, the only difference between this embodiment and embodiment 1 is the size of the electrolytic cell. The electrolytic cell of the present embodiment adopts the box-type electrolytic cell with a volume of 1200ML. In the electrolytic cell, a vertical rhombic mesh Hastelloy C-276 nickel alloy anode and a zigzag rhombic silver mesh cathode are placed in parallel. The distance between the electrodes is 2cm. Total working area 100cm 2 , the total area of ​​cathode macro work is 100cm 2 , anode size: macro length, width and thickness are 10.0cm×10.0cm×0.3cm, Ts is 1mm, LWD is 5mm, SWD is 2mm, Ws is 3mm; cathode size: macroscopic length, width and thickness are 10.0cm×10.0 cm×0.2cm, Ts is 0.5mm, LWD is 2mm, SWD is 1mm, Ws is 1.5mm.

[0069]Add 50g of 3,4,5,6-tetrachloropicolinic acid, 50g of sodium hydroxide and 1000ML of deionized water into the electrolytic cell. After dissolving, turn on the magnetic pump (the flow rate is 5.5-6.5L / min) to cir...

Embodiment 3

[0071] refer to figure 1 , 3 , 4, 6, 7, 8, a kind of electrolytic synthesis equipment of 3,6-dichloropicolinic acid, comprising a power supply 1, a batching tank 12, and an electrolytic tank 5, and the power supply is a voltage-stabilizing and current-stabilizing thyristor periodically changing To the power supply, the power supply 1 is connected to the current commutator 2, and the current commutator is provided with a program control unit; the positive pole of the power supply 1 is connected to the anode of the electrolyzer, and the negative pole of the power supply 1 is connected to the cathode of the electrolyzer.

[0072] The electrolyzer of this embodiment adopts image 3 A single-stage electrolyser in a battery of box-type electrolysers without diaphragms shown. The interior of the unipolar electrolytic cell is provided with 2 pieces of longitudinal diamond-shaped mesh Hastelloy C-276 nickel alloy as anodes and 1 piece of horizontal diamond-shaped silver mesh as catho...

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Abstract

The invention discloses a 3, 6- dichloro pyridine methanamine electrolytic synthesis method and device, which comprises the following steps: using 3, 4, 5, 6-tetrachloro pyridine aminic acid for main electrolysis material; placing electrolytic solution in electrolysis bath to electrolyze; getting 3, 6- dichloro pyridine methanamine by neutralizing, cooling, crystallizing, filtering and drying; carrying on toughening treatment for cathode of electrolysis bath by periodic reversible power of thyristors. The device is composed of power, dosage bunker, electrolysis bath, wherein the power is stabilized voltage and permanent flow, which can control the cycle reverse power; the power connects to current commutator; program control unit is installed for current commutator; the anode of power is connected to anode of electrolysis bath; the minus pole of power connects to cathode of electrolysis bath.

Description

(1) Technical field [0001] The invention relates to an electrolytic synthesis method of 3,6-dichloropicolinic acid, and also relates to an electrolytic synthesis equipment of 3,6-dichloropicolinic acid. (2) Background technology [0002] The English name of 3,6-dichloropicolinic acid is 3,6-dichloropicolinic acid, commonly known as Bikecao. 3,6-Dichloropicolinic acid (3,6-D) is a highly active plant growth regulator. Since the publication of US3317549, 3,6-D has attracted more and more attention, especially in the control of 2,4-D (2,4-dichlorophenoxy)acetic acid and MCPA (2-methyl- Herbicide-resistant plants such as 4-chlorophenoxy)acetic acid are very effective, such as Canada thistle, Russian nettle and wild buckwheat are very sensitive to 3,6-D. 3,6-D is also very active on pasture shrubs, such as nettle, cat's claw acacia (a kind of silk tree), mesquite is also very sensitive to 3,6-D. In addition, 3,6-D is not only less toxic to mammals, fish and poultry, but also h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/04C07D213/79C25B3/25
Inventor 马淳安
Owner ZHEJIANG UNIV OF TECH
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