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Preparation method of Avermectin B2a fine powder

A technology of abamectin and refined powder, applied in the field of preparation of avermectin B2a refined powder, can solve the problem of low product purity, achieve high purity, reduce the number of recrystallizations, and have good impurity removal effects

Active Publication Date: 2013-10-02
DAQING JEFENE BIO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing method for preparing B2a has the problem that the purity of the product obtained is not high

Method used

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  • Preparation method of Avermectin B2a fine powder

Examples

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Effect test

Embodiment 1

[0029] A preparation method of Abamectin B2a fine powder, comprising the following steps:

[0030] A. Weigh 1000g of abamectin B1a crystallization mother liquor (methanol solution), whose B2a content is 15%, add 300g of water under stirring, heat up to 50°C and stir for 4h, then heat up to 60°C for 3h in vacuum azeotropic distillation, and concentrate the solution into a paste.

[0031] B. Weigh the weight of the paste obtained above as 331g, add 662g of sec-butyl acetate, heat up to 50°C and stir to dissolve for 1h, then add 662g of tetrabutylammonium bromide aqueous solution with a mass fraction of 0.25%, stir at 50°C for 1h, and then the material Slowly cool down to 20°C, let stand for 4h, and separate layers. Repeat the above washing for 2 more times and separate layers.

[0032] C. Warm up the layered sec-butyl acetate solution to 80° C. for 2 hours in vacuum distillation, and concentrate the solution into a paste. Weigh 316g of its paste, then add 950g of crystallizat...

Embodiment 2

[0035] A preparation method of Abamectin B2a fine powder, comprising the following steps:

[0036] A. Weigh 1000g of abamectin B1a crystallization mother liquor (methanol solution), its B2a content is 13.46%, add 700g of water under stirring, heat up to 60°C and stir for 5h, then heat up to 75°C for vacuum azeotropic distillation for 2h, and concentrate the solution into a paste.

[0037] B. The weight of the paste is 309g, add 1200g of sec-butyl acetate, heat up to 60°C and stir to dissolve for 2h, then add 1200g of tetrabutylammonium bromide aqueous solution with a mass fraction of 0.6%, stir at 60°C for 1h, the material Slowly cool down to 15°C, let stand for 5h, and separate layers. Repeat the above washing once more, and separate layers.

[0038] C. Warm up the layered sec-butyl acetate solution to 80°C for vacuum distillation for 2h, concentrate the solution into a paste, weigh 288g of the paste, then add 1400g of crystallization solvent benzene to the obtained paste a...

Embodiment 3

[0041] A preparation method of Abamectin B2a fine powder, comprising the following steps:

[0042] A. Weigh 1000g of abamectin B1a crystallization mother liquor (methanol solution), whose B2a content is 12.88%, add 400g of water under stirring, heat up to 60°C and stir for 3h, then heat up to 80°C for 1.5h in vacuum azeotropic distillation, and distill the solution Concentrate into a paste.

[0043]B. The weight of the paste is 317g, add 950g of sec-butyl acetate, heat up to 55°C and stir to dissolve for 2h, then add 950g of tetrabutylammonium bromide aqueous solution with a mass fraction of 0.5%, stir at 55°C for 2h, the material Slowly cool down to 20°C, let stand for 6h, and separate layers. Repeat the above wash 2 more times.

[0044] C. Heat up the layered sec-butyl acetate solution to 90°C for vacuum distillation for 1h, concentrate the solution into a paste, weigh 297g of the paste, then add 1200g of benzene to the obtained paste and stir at 70°C for 3h, after dissolv...

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Abstract

The invention relates to a preparation method of an Abamectin B2a fine powder. The method comprises the following steps: A, concentrating an Abamectin B1a crystallization mother liquor into a paste state; B, dissolving the obtained paste with sec-butyl acetate, and then adding a tetrabutyl ammonium bromide aqueous solution for washing and layering; C, concentrating the sec-butyl acetate solution subjected to washing and layering, then adding a crystallization solvent for dissolution, naturally cooling to room temperature, crystallizing, and filtering to obtain an Abamectin B2a fine powder crude product; and D, recrystallizing the Abamectin B2a fine powder crude product to obtain the Abamectin B2a fine powder. According to the invention, waste Abamectin crystallization mother liquor is recovered and utilized to extract effective substances; tetrabutyl ammonium bromide aqueous solution is used for washing, which has better impurity removal effect than traditional water washing or saturated brine washing, and makes the solution layer more easily; aromatic hydrocarbon is used as the crystallization solvent; and the content of obtained B2a fine powder is higher than 93%.

Description

technical field [0001] The invention relates to a preparation method of antibiotics, in particular to a preparation method of abamectin B2a fine powder. Background technique [0002] Abamectin is a low-toxicity, high-efficiency, high-selection, green, environmental-friendly and bio-sourced insecticide. It completely solves the problems of high toxicity, resistance and environmental impact of traditional pesticides. The key research projects of the "Seventh Five-Year Plan", "Eighth Five-Year Plan", "Ninth Five-Year Plan", "Tenth Five-Year Plan" and "Eleventh Five-Year Plan". With the popularization and promotion of abamectin and its downstream products in recent years, it has not only driven the vigorous development of my country's agriculture and animal husbandry, but also promoted the transformation of agricultural and animal husbandry production to a green and harmless direction. [0003] Abamectin, one of the most effective insecticides in the world, has an annual consum...

Claims

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Application Information

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IPC IPC(8): C07H17/08C07H1/06
Inventor 徐继民沈学庆徐龙广王东丽
Owner DAQING JEFENE BIO CHEM
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