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Selective conversion method of waste residue of picloram production

A kind of amiloride, selective technology, applied in the field of resources and environment, to achieve the effect of simple operation, solve the expansion of material liquid, and realize the effect of multi-effect utilization

Active Publication Date: 2017-12-15
HUNAN BIDE BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] Aminopyralic acid and 6-amino-3,4,5-tetrachloropicolinic acid in the waste residue are isomers with relatively similar structures and properties. Highly selective conversion with high difficulty

Method used

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  • Selective conversion method of waste residue of picloram production

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044]300 g of isoamyl alcohol, 100 g of amiloride production waste residue, 70 g of isoamyl nitrite, and 50 g of sodium chloride were sequentially added to a 1000 mL four-necked flask. At room temperature, 80 g of concentrated hydrochloric acid was added for diazotization reaction. After the reaction was completed, 30 g of CuCl was added, and the flask was moved into a water bath at 45°C.

[0045] After the reaction, the reaction liquid was lowered to room temperature, 600 g of water was added, mixed and stirred, and filtered, and the filtrate was separated to obtain isoamyl alcohol, which could be recycled. Move the filter cake into a flask containing an appropriate amount of water, slowly add a certain amount of NaOH solution, and adjust the pH value to stabilize at 9-10. Filtrate, slowly add a certain amount of hydrochloric acid to the filtrate, stir for 20 minutes and then filter, the filter cake is washed with water and dried to obtain the finished product. The dry wei...

Embodiment 2

[0047] Its step is with embodiment 1, and difference is: used the recovery isoamyl alcohol in embodiment 1 and added 20g fresh isoamyl alcohols and reacted. A dry weight of 67.78g was obtained, wherein the content of amiloride was 75.62%, the content of clopyralid was 22.39%, and the product yield was 67.78%.

Embodiment 3

[0049] The steps are the same as in Example 1, except that ethanol is used to replace isoamyl alcohol as a solvent for the reaction. The dry weight of the obtained product was 69.24g, wherein the content of amiloride was 80.47%, the content of clopyralid was 17.30%, and the product yield was 69.24%.

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Abstract

The invention provides a selective conversion method of waste residue of picloram production. According to the method, waste residue of picloram production or secondary residue generated from purification are taken as a raw material; through selection of special reaction reagents and condition, high-value picloram in waste residue can be furthest reserved; a non-effectively used component in waste residue is completely converted; and finally a mixture of picloram and tetrachloropicolinic acid is obtained. The mixture can be recyclably used to preparation technology of picloram, and an efficient circulation of raw materials, products, waste residue, raw materials, and products is completed. Atom economy of a chemical reaction and resource utilization of substances are achieved, and damage to the environment by the waste residue is prevented. The method has great economic benefit and environmental benefit.

Description

technical field [0001] The invention belongs to the technical field of resources and environment, and mainly relates to a selective conversion method of amiloride production waste residue. Background technique [0002] Amiloride, whose chemical name is 4-amino-3,5,6-triclopyralic acid, is a systemic herbicide with broad market prospects. [0003] Amclopyralid is generally prepared by the ammonolysis reaction of 3,4,5,6-tetraclopyralid and ammonia water. During the reaction process, the amino substitution of the 4-position chlorine group mainly occurs, and the amino substitution of the 3-position, 5-position and 6-position chlorine group also occurs, especially the displacement reaction at the 6-position is more obvious, and ammonia will be generated during the crystallization process. Clopyralid waste residue. [0004] The main components of the dry matrix of the primary production waste residue of amiloride are 4-amino-3,5,6-triclopyridine carboxylate ammonium salt and 6-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/803
CPCC07D213/803
Inventor 付林王宇轩晚霞王争王艳
Owner HUNAN BIDE BIOTECH
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