Method for separating and purifying high-content picloram from picloram production waste residues

A kind of technology of amiloride and clopyralid, applied in the field of reuse of amiloride production waste residue
CN104628635AActive Publication Date: 2015-05-20HUNAN BIDE BIOTECH
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Patent Information

Authority / Receiving Office
CN · China
Current Assignee / Owner
HUNAN BIDE BIOTECH
Publication Date
2015-05-20

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Abstract

The invention belongs to the technical field of production waste residue recycling and discloses a method for separating and purifying high-content picloram from picloram production waste residues. The method comprises the steps of firstly, adding water to dissolve picloram production waste residues, then, starting to circularly filter when heating to 80-90 DEG C, and stopping filtering when the temperature is lower than 40 DEG C to obtain filtrate I; transferring the filtrate I to an acidification kettle, adding an acid to acidify when heating the material to 60-90 DEG C, controlling the pH value of a feed liquid not to be higher than 2, and then, filtering while heating at the temperature of not lower than 60 DEG C to obtain a filter cake; and rinsing the filter cake with water to obtain higher than 95% of picloram. By using the method, most of picloram in the production waste residues is effectively separated and is up to the standard of a qualified product, meanwhile, all isomerides can be recycled after being primarily separated and subjected to a series of chemical synthesis treatment, and therefore, the aims of clean production and environment friendliness are achieved.
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Description

technical field

[0001] The invention belongs to the technical field of reusing production waste residues, and in particular relates to the reutilization technology of amiloride production waste residues. Background technique

[0002] Amiloride, whose chemical name is 4-amino-3,5,6-trichloropyralic acid, is a systemic pyridine herbicide, because of its wide range of applications, low toxicity, high selectivity, and dosage It has the characteristics of small residue in plants and soil, short residue cycle, etc., and has a very broad market prospect.

[0003] CN1923810A discloses a method for synthesizing amiloride through ammonolysis, using tetraclopyralid or tetraclopyridine as a raw material, with a total yield of 75-91%.

[0004] At present, the industry mainly adopts the production process of amclopyralid (4-amino-3,5,6-trichloropyridine) through ammonolysis of tetraclopyridine carboxylic acid and ammonia water, 4-amino-3,5,6-pyridine The yield of formic acid is about 85...

Claims

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