Crystallization method of abamectin Bla

A technology of crystallization of abamectin, which is applied in the field of crystallization of abamectin B1a, can solve problems such as inability to take into account the crystallization purity and yield, inability to separate B1a and B1b, and long duration, so as to prevent agglomeration and improve Effects of crystal habit and yield improvement

Inactive Publication Date: 2006-08-30
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to overcome the high cost of product production caused by the high number of ethanol crystallization and crystallization in the prior art, the inability to further separate B1a and B1b by using the precipitation crystallization method for the leachate, and the continuation of crystallization of primary coarse powder by ethanol. The time is long, and can not take into account the defects of crystallization purity and yield, thereby providing a kind of crystallization purity and yield are all higher, stability is better and crystallization time is shorter, crystallization number of times is few, the Abamectin B1a of low production cost crystallization method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In the spherical crystallization tank of 500ml, drop into about 40g industrial primary coarse powder (obtain by concentrating and crystallizing the leach solution that utilizes the organic solvent leaching gained to mycelia, the Abamectin B1a purity wherein is 78.21%), add 265ml normal For butanol, heat up to 80°C with stirring in a water bath, and keep the temperature constant for about 25 minutes. After it is fully dissolved, filter out the insoluble impurities while it is hot. When the clarified hot saturated solution of gained is naturally cooled to 68 ℃ in water bath, its degree of supersaturation is 1.1, adds 0.5g by the crystal seed (this crystal seed is the supersaturated solution of avermectin) by ultrasonic auxiliary preparation (prepared by applying ultrasonic waves for 20 min) stirred the solution at a speed of 100 r / min, and kept at this temperature for 20 min.

[0023] Then adjust the stirring speed to 150r / min, and lower the temperature according to the f...

Embodiment 2

[0025] In the spherical crystallization tank of 1000ml, drop into about 80g industrial primary coarse powder (obtain by concentrating and crystallizing the leach solution that utilizes the organic solvent leaching gained to mycelium, the Abamectin B1a purity wherein is 80.05%), add 600ml normal For butanol, stir in a water bath and raise the temperature to 75°C, keep the temperature for about 30 minutes, and after it is fully dissolved, filter out the insoluble impurities while it is hot. When the clear hot saturated solution of gained is naturally cooled to 65 ℃ in water bath, its degree of supersaturation is 1.3, adds 1g by the crystal seed crystal (this crystal seed is applied to the supersaturated solution of avermectin) by ultrasonic auxiliary preparation. Ultrasonic 15min), the solution was stirred at a speed of 120r / min, and kept at this temperature for 20min.

[0026] Then adjust the stirring speed to 180r / min, and lower the temperature according to the following cooli...

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PUM

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Abstract

The present invention relates to a crystallization method of abamectin B 1a. Said method includes the following steps: using crystallization solvent n-butanol to stir and dissolve primary crude powder of abamectin B 1a at 75-100deg.C to saturation, filtering while the saturated solution is hot to obtain clear hot-saturated solution; slowly cooling said solution to that when the supersaturation degree is 1-3, adding crystal seeds, constant stirring for 20-60min, its stirring speed is 120-300rpm, and cooling to make crystallization, fitering crystal slurry or centrifugally-separating said crystal slurry, washing crystal and drying so as to obtain the invented abamectin B 1a.

Description

technical field [0001] The invention relates to a crystallization method of abamectin B1a. Background technique [0002] Avermectins are a group of 16-membered macrolide antibiotics with similar structures, but they do not have antimicrobial and antifungal activity, but have strong insecticidal activity. As an insecticide, it can drive and kill almost all nematodes, insects and mites, and it can achieve 80-100% repelling rate with one application, and it has high safety for humans and mammals, so it is a good of biopesticides. [0003] Abamectin is a group of macrolides produced by Streptomyces avermitilis, including 8 natural components with similar structures. According to the different substituents on the C-5 position, the difference between the single and double bonds between C-22 and C-23 and the difference of the substituents on the C-25 position, use A, B; 1, 2; a, b combination respectively express. Among them, B1a has the best drug effect. [0004] Abamectin B1...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/08
Inventor 刘吉常志东谢智安振涛申淑锋孙兴华胡欣王明梅刘会洲
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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