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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

Active Publication Date: 2015-05-20
HUNAN BIDE BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there are no relevant reports in domestic and foreign literature and patents

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 600kg of tap water into the 1500L reactor, start stirring, then put 400kg of amiloride production waste residue (wet residue, water content is 50-55%), heat up the material to 80-90°C, keep stirring for 30 minutes, Then start the filter device while it is hot, and slowly cool the material while circulating the filter, and stop the filter when the temperature of the clear liquid cools below 30°C; the filter cake is the residue-I.

[0024] The filtered clear liquid is transferred to the acidification kettle, the material is heated to 85°C, and metered hydrochloric acid is added to ensure that the pH of the feed liquid is not higher than 2, and it is filtered while it is hot at 85°C, and the filtrate is cooled, crystallized, and filtered. It is the residue-II, and the filter cake is amiloride after washing with water, the HPLC content is 96.3%, and the weight after drying is 89kg;

Embodiment 2

[0026] Add 700kg of tap water to the 1500L reactor, start stirring, then put 400kg of amiloride production waste residue (wet residue, water content is 50-55%), heat the material to 80-90°C, keep stirring for 30 minutes, Then start the filter device while it is hot, and slowly cool the material while circulating the filter, and stop the filter when the temperature of the clear liquid cools below 30°C; the filter cake is the residue-I.

[0027] The filtered clear liquid is transferred to the acidification tank, the temperature of the material is raised to 85°C, and a metered amount of hydrochloric acid is added to ensure that the pH of the feed liquid is not higher than 2, and the temperature is lowered to 65°C to filter while it is hot, and the filtrate is cooled, crystallized, and filtered. , which is residue-II, the filter cake is amiloride after washing with water, the HPLC content is 92.3%, and the weight after drying is 94kg;

Embodiment 3

[0029] Add 500kg of tap water to the 1500L reactor, start stirring, then put 400kg of amiloride production waste residue (wet residue, water content is 50-55%), heat the material to 80-90°C, keep stirring for 30 minutes, Then start the filter device while it is hot, and slowly cool the material while circulating the filter, and stop the filter when the temperature of the clear liquid cools below 30°C; the filter cake is the residue-I.

[0030] The filtered clear liquid is transferred to the acidification kettle, the material is heated to 85°C, and metered hydrochloric acid is added to ensure that the pH of the feed liquid is not higher than 2, and it is filtered while it is hot at 85°C, and the filtrate is cooled, crystallized, and filtered. It is the residue-II, and the filter cake is amiloride after washing with water, the HPLC content is 98.6%, and the weight after drying is 85kg;

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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.

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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Application Information

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IPC IPC(8): C07D213/803C07D213/79
CPCC07D213/79C07D213/803
Inventor 李华轩王宇吴婳婳
Owner HUNAN BIDE BIOTECH
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