Method for preparing 4-amidogen-3,6-dichloropyridine-2-formic acid by means of catalytic electrolysis

A technology of catalytic electrolysis and dichloropyridine, applied in electrolysis process, electrolysis components, electrolysis organic production and other directions, can solve the problems of inability to meet the sustainable development of chemical industry, serious pollution in separation process, unfriendly environment, etc., and achieve obvious economic advantages and environmental advantages, reduce side reactions, reduce the effect of post-processing difficulty

Active Publication Date: 2016-07-27
ZHEJIANG AVILIVE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

First, the chemical method uses mixed acid for nitration, and the amount of waste acid is large and difficult to handle, which is very unfriendly to the environment
Second, there are defects in the electrolytic cell in the electrolysis method, and the electrode has a short life in application and must be replaced frequently
Third, the separation process is seriously polluted and the operation is cumbersome
Therefore, the existing production process can no longer meet the needs of the sustainable development of the chemical industry, and an advanced clean production process is urgently needed to replace it.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Example 1 A method for preparing 4-amino-3,6-dichloropyridine-2-carboxylic acid by catalytic electrolysis, the specific steps are as follows: in a 130-liter electrolyzer equipped with a circulation device, a heat exchange device, a voltmeter, and a thermometer , add 100kg of 5% sodium hydroxide aqueous solution, start the circulation pump, gradually add 15.1kg of 4-amino-3,5,6-trichloropyridine-2-carboxylic acid, 0.83kg of 5% Ru / C; The liquid temperature rises to 50°C; turn on the constant voltage DC power supply and adjust the cell voltage to 3.2V; take samples to control the content of 4-amino-3,5,6-trichloropyridine-2-carboxylic acid in the electrolyte until 4- Amino-3,5,6-trichloropyridine-2-carboxylic acid ≤ 0.2%, turn off the DC power supply; continuously monitor the pH value of the reaction solution during electrolysis, and it is required to keep ph=13.5. If the pH value drops, it is necessary to add 30% sodium hydroxide; after the electrolysis, filter, the filte...

Embodiment 2

[0024] Example 2 The operation was the same as that of Example 1, keeping ph = 12.5 to obtain 11.99 kg of 4-amino-3,6-dichloropyridine-2-carboxylic acid, with a content of 96.3% and a yield of 89.2%.

Embodiment 3

[0025] Example 3 The operation was the same as that of Example 1, but the catalyst was replaced with 5% Pd / C to obtain 12.13 kg of 4-amino-3,6-dichloropyridine-2-carboxylic acid, with a content of 96.9% and a yield of 90.8%.

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PUM

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Abstract

The invention discloses a method for preparing 4-amidogen-3,6-dichloropyridine-2-formic acid by means of catalytic electrolysis, and belongs to the field of production of chemical products. The technical problems that when 4-amidogen-3,5,6-trichloropyridine-2-formic acid is used for preparing the 4-amidogen-3,6-dichloropyridine-2-formic acid by means of electrolysis, the electrolysis time is long, the energy consumption is high, and selectivity is poor are solved. According to the scheme for solving the above technical problems, during electrolysis of the 4-amidogen-3,5,6-trichloropyridine-2-formic acid, a catalyst is added, the specific temperature, the PH value and other conditions are combined, chlorine on a pyridine ring is desorbed, a final product is the 4-amidogen-3,6-dichloropyridine-2-formic acid, and the catalyst is filtered and washed in the aftertreatment procedure to be recycled and reused. On the basis of electrolysis, low input is increased, the content and yield of the product are increased, and the energy consumption is reduced.

Description

technical field [0001] The invention belongs to the production field of chemical products, and in particular relates to a method for preparing 4-amino-3,6-dichloropyridine-2-carboxylic acid by catalytic electrolysis. Background technique [0002] 4-Amino-3,6-dichloropyridine-2-carboxylic acid, trade name Amazoram, aminopyralid, dichloroaminopyralid, is a pyridine carboxylic acid herbicide, it can quickly enter the plant body , easily absorbed by stems and leaves, resulting in growth interruption and rapid death, mainly used for weed control in pastures, plantations and non-crop areas, and for weeding in sugar beet and buckwheat fields. [0003] The synthesis methods of 4-amino-3,6-dichloropyridine-2-carboxylic acid currently include chemical synthesis and electrolysis. The chemical synthesis of 4-amino-3,6-dichloropyridine-2-carboxylic acid is completed by taking 3,6-dichloropyridine-2-carboxylate as raw material through nitration, reduction, hydrolysis, purification and ot...

Claims

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Application Information

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IPC IPC(8): C25B3/00C07D213/79C07D213/803
CPCC07D213/79C07D213/803C25B3/00
Inventor 厉云阳李惠跃金克强徐巍李国斌
Owner ZHEJIANG AVILIVE CHEM CO LTD
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