Refining method of difenoconazole crude product

A technology of difenoconazole and a purification method, applied in directions such as organic chemistry, can solve the problems such as inability to recover and waste difenoconazole, and achieve the effects of shortening the refining cycle, low production cost and easy control

Active Publication Date: 2021-11-19
JIANGSU HEBEN BIOCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the process has been optimized, it is essentially the steps of salt formation, alkali hydrolysis, and crystallization, which will still produce a large amount of waste salt, and difenoconazole contained in alkaline water cannot be recovered, resulting in a certain amount of waste

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Put 100g of difenoconazole crude product with a mass content of 70% and 400g of cyclohexane into the reaction kettle, heat up and reflux for extraction for 0.5-1h, cool down to 70°C for phase separation, and continue to add 400g of cyclohexane for the second Secondary extraction, after the second extraction is completed, continue to add 400g cyclohexane for the third extraction, remove the clean cyclohexane and separate to obtain 44g of difenoconazole with a content of 96% to be crystallized, add 44g of mass concentration to be 85- 90% methanol, heated up to 60-70°C to dissolve, cooled down to -10-0°C to crystallize for 6-8 hours after dissolution was complete, suction filtered, dried to obtain 40g of 97% difenoconazole original drug, and the crystallized mother liquor was removed to obtain 53.8 % difenoconazole 3.9g. 56g of difenoconazole with a low content of 50.4% obtained by extracting the mother liquor and precipitating is combined with 3.9g of difenoconazole obtai...

Embodiment 2

[0023] Put 100g of difenoconazole crude product with a mass content of 80% and 500g of n-heptane into the reaction kettle, heat up and reflux for extraction for 0.5-1h, cool down to 70°C for phase separation, and continue to add 500g of n-heptane after separating n-heptane for the second Secondary extraction, after the second extraction is completed, continue to add 500g n-heptane for the third extraction, remove the net n-heptane and separate to obtain 53.5g of difenoconazole with a content of 97% to be crystallized, add 64.2g and the mass concentration is 95% ethanol, heated up to 60-70°C to dissolve, cooled down to -10-0°C to crystallize for 6-8 hours after the dissolution was complete, suction filtered, dried to obtain 48.7g of 98% difenoconazole original drug, and the crystallization mother liquor was removed from the solvent to obtain 68.1% Difenoconazole 4.7g. The extracted mother liquor was desolvated to obtain 46.5g of difenoconazole with a low content of 60.4%. Add s...

Embodiment 3

[0025] Put 100g of difenoconazole crude product with a mass content of 83% and 600g of methylcyclohexane into the reaction kettle, heat up and reflux for extraction for 0.5-1h, cool down to 70°C for phase separation, and continue to add 600g of methylcyclohexane after separating the methylcyclohexane Methylcyclohexane for the second extraction, after the second extraction is completed, continue to add 600g methylcyclohexane for the third extraction, remove the clean methylcyclohexane to obtain a content of 96% to be crystallized Add 61.6g of isopropanol with a mass concentration of 98-99% to 56.0g of azole, heat up to 60-70°C to dissolve, cool down to -10-0°C to crystallize for 6-8h after the dissolution is complete, filter with suction, and dry to obtain 97.5% phenyl ether Metroconazole technical 51.0g, crystallization mother liquor removes solvent to obtain 63.3% difenoconazole 4.9g. Extract the mother liquor and desolventize to obtain 44g of 66.3% low-content difenoconazole...

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PUM

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Abstract

The invention discloses a refining method of a difenoconazole crude product. Difenoconazole is refined by adopting an extraction and crystallization method, extraction is performed firstly and then crystallization is performed, strong acid and alkali liquor are not introduced in the whole refining process, and no waste salt is generated in the refining process; and rectification is not needed, and rectification residues and high-COD wastewater are not generated. The low-content difenoconazole obtained after the extraction solvent of the extraction mother liquor and the crystallization mother liquor is removed is light in color and can be directly made into a 10% difenoconazole emulsion in water, the emulsion in water is high in quality, waste recycling is achieved, and the utilization rate of the difenoconazole crude product reaches 98% or above.

Description

technical field [0001] The invention relates to a method for refining a difenoconazole crude product, which belongs to the post-treatment technology of organic chemistry. Background technique [0002] At present, the content of crude difenoconazole in industrial production is mostly 70-83%. The common refining method is to use concentrated nitric acid or concentrated hydrochloric acid to form a salt, then extract a higher content of difenoconazole through alkaline hydrolysis, and then recrystallize Obtain the original drug of difenoconazole. This method will produce a large amount of sodium nitrate or sodium chloride waste salt, which greatly increases the cost of environmental protection treatment; and the color of the mother liquor after alkaline hydrolysis extraction is dark, it cannot be formulated into a water emulsion, the mother liquor cannot be used, and can only be entrusted to a third party for incineration and other treatment It is not only a waste of resources, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D405/06
CPCC07D405/06
Inventor 冯魏贾利华陈华陈石秀徐鹏鹏邢燕
Owner JIANGSU HEBEN BIOCHEM
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