Method for recovering byproduct (ammonium chloride) in kresoxim-methyl production process

A production process and recovery method technology, applied in the direction of ammonium chloride, ammonium halide, etc., can solve the problems of residual organic impurities, complex recovery operation of by-product ammonium chloride, high cost, etc., achieve short cycle, increase actual industrial production output, low cost effect

Inactive Publication Date: 2020-08-18
JINGBO AGROCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the problems of complex recovery operation, high cost, and residual organic impurities in the by-product ammonium chloride synthesis process of kresoxim-methyl in the prior art, the present invention provides a recovery method for the by-product ammonium chloride in the production process of kresoxim-methyl, the operation Simple, high purity, low cost, clean production, realize the industrial production of kresoxim-methyl without solid waste discharge

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 50g of kresoxim-methyl by-product ammonium chloride crude product (containing 40g of ammonium chloride), 100g of water and 25g of toluene into a 500ml four-necked bottle, stir and heat up to 70°C for 1h, then let stand for 30min, separate layers, and collect organic phase, the organic phase is simply distilled to 95°C, and the solvent is evaporated to recover kresoxim-methyl 0.64g intermediate 2-(2-methylphenoxymethyl)phenyl oxalate methyl ester (content 78%), and the recovered solvent can be Continuously apply mechanically; after the water phase is filtered at 60°C to remove impurities, the filtrate is cooled and crystallized to 2°C, and 16.6g of high-purity ammonium chloride is obtained by centrifugation. The content measured by titration is 99.2%, and the yield is 41.2%. Ammonium chloride mother liquor can be applied continuously.

Embodiment 2

[0026] Add 20g of kresoxim-methyl by-product ammonium chloride crude product (containing 16g of ammonium chloride), 120.3g of ammonium chloride mother liquor obtained in Example 1, and 25g of toluene into a 500ml four-necked bottle, stir and heat up to 70°C for 1.5h of reaction, then statically Set aside for 30 minutes, separate layers, collect the organic phase, and simply distill the organic phase to 95°C, distill off the solvent to recover 0.20 g of kresoxim-methyl intermediate 2-(2-methylphenoxy)-methylenephenylacetaldehyde Acetate methyl ester (content 76.5%), the recovered solvent can be used continuously; after the water phase is filtered at 60°C to remove impurities, the resulting filtrate is cooled and crystallized to 2.5°C, and 15.8g of high-purity ammonium chloride is obtained by centrifugation, with a content of 99.5% %, yield 98.3%, obtains 120g ammonium chloride mother liquor, can carry out continuous mechanical application.

Embodiment 3

[0028] Add 500kg of crude ammonium chloride (containing 400kg of ammonium chloride), 1000kg of water, and 250kg of toluene into the 3000L reactor, stir and heat up to 80°C for 2 hours, let stand for 30min, separate layers, and collect the organic phase , the organic phase is simply distilled to 100°C, and the solvent is evaporated to reclaim 6.7kg of kresoxim-methyl oxalate (content 75.9%) as an intermediate 2-(2-methylphenoxymethyl)phenyl oxalate. The recovered solvent can be continuously Apply mechanically; after the water phase is filtered at 60°C to remove impurities, the filtrate is cooled and crystallized to 3°C, and 159kg of high-purity ammonium chloride is obtained by centrifugation. The titration method records a content of 99.4%, and a yield of 39.5%, to obtain 1265kg of ammonium chloride mother liquor , which can be applied continuously.

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Abstract

The invention relates to the technical fields of pesticide and environmental protection, and relates to a byproduct recycling technology in the preparation process of an agricultural bactericide (kresoxim-methyl), in particular to a method for recovering a byproduct (ammonium chloride) in kresoxim-methyl production process. Toluene or petroleum ether is used as an extraction solvent and is mixed with water, a byproduct (crude ammonium chloride) in the kresoxim-methyl production process is used as a raw material, standing and layering are performed after heating, filtrate, which is obtained after the water phase is filtered and subjected to impurity removal, is subjected to cooling crystallization, and finally high-purity ammonium chloride is obtained through centrifugation. The method hasthe advantages of simple process flow, short period, low cost, high product purity (up to 99.6%) and high yield, no solid waste is discharged in industrial production of kresoxim-methyl, and clean production is realized. Meanwhile, the extraction solvent and the ammonium chloride mother liquor can be recycled, and water is saved.

Description

technical field [0001] The invention relates to the technical field of pesticide environmental protection, and relates to a resource recovery technology of by-products in the production process of the agricultural fungicide kresoxim-methyl, in particular to a recovery method for ammonium chloride, a by-product in the production process of kresoxim-methyl. Background technique [0002] Kresoxim-methyl, also known as (E)-2-methoxyimino-[2-(o-methylphenoxymethyl)phenyl]methyl acetate, is a high-efficiency, broad-spectrum, new type of fungicide. During the synthesis process of kresoxim-methyl, there are many three wastes, among which the by-product ammonium chloride has low purity and can only be used as a solid waste product. The disposal cost is high and there is great difficulty in disposal. With the development of industrialization of kresoxim-methyl products, the solid waste ammonium chloride discharged during the production process is increasing day by day, which brings se...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01C1/16
CPCC01C1/164
Inventor 王光金李冰洁张思思高欢于连友王祥传
Owner JINGBO AGROCHEM TECH CO LTD
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