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Method for extracting residual avermectin B1a from primary crystallization mother liquor of avermectin B1a

A technology of abamectin and crystallization mother liquor, applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve the problem of difficult extraction of B1a active components, and achieve the effect of simple process and low cost

Active Publication Date: 2016-03-23
HEBEI XINGBAI AGRI SCI & TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The purpose of the present invention is to provide a kind of high-efficiency, low-cost method for extracting residual abamectin in the primary crystallization mother liquor of abamectin aiming at the technical problem that the B1a active component remaining in the primary crystallization mother liquor of abamectin is difficult to extract at present B1a component method

Method used

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  • Method for extracting residual avermectin B1a from primary crystallization mother liquor of avermectin B1a

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Take 2000mL (equivalent to 2300g) abamectin B1a primary crystallization mother liquor, precipitate at 80°C for 2h, and obtain 715g of the first ointment (the B1a contained in it is 5.76% as detected by HPLC);

[0034] (2) Add 2145g of methyl isobutyl ketone to the first ointment, stir and dissolve the first ointment at 80°C, then program cooling (10°C per hour) to 0°C, and then filter to remove the precipitate (HPLC detects the precipitate B1a content ≤ 0.5%), reclaim the filtrate;

[0035] (3) Gained filtrate is precipitated and concentrated at 70°C under 0.02Mpa to obtain the second ointment 500g (HPLC detects that B1a=8.03% in the second ointment), and 500g of crystallization solvent propanol is added in the second ointment, at 70 Stir at ℃ to dissolve the second ointment, then program the temperature down to 30°C (drop 10°C per hour), then stir at this temperature (the stirring condition is 30rpm) to grow crystals for 5h; filter the obtained crystal slurry, wash...

Embodiment 2

[0043] (1) Take 2000mL (equivalent to 2300g) abamectin B1a primary crystallization mother liquor, precipitate at 80°C for 2h, and obtain 715g of the first ointment (the B1a contained in it is 5.76% as detected by HPLC);

[0044] (2) Add 2860g of methyl vinyl ketone to the first ointment, stir and dissolve the first ointment at 70°C, then program the temperature down (10°C per hour) to 5°C, and then filter to remove the precipitate (HPLC detects that in the precipitate B1a content≤0.5%), reclaim the filtrate;

[0045] (3) The obtained filtrate is precipitated and concentrated at 50°C under 0.01Mpa to obtain 540g of the second ointment (HPLC detects that B1a=7.56% in the second ointment), and 540g of ethanol, the crystallization solvent, is added to the second ointment. Stir to dissolve the second ointment, then program the temperature down to 20°C (10°C per hour), then stir at this temperature (stirring condition is 30rpm) to grow crystals for 5.5h; filter the obtained crystal ...

Embodiment 3

[0053] (1) Take 2000mL (equivalent to 2300g) abamectin B1a primary crystallization mother liquor, precipitate at 80°C for 2h, and obtain 715g of the first ointment (the B1a contained in it is 5.76% as detected by HPLC);

[0054] (2) Add 2500 g of cyclohexanone to the first ointment, stir and dissolve the first ointment at 75°C, then program cooling (10°C per hour) to 10°C, and then filter to remove the precipitate (HPLC detects B1a in the precipitate content≤0.5%), recover the filtrate;

[0055] (3) Gained filtrate is 80 ℃ precipitation concentration under 0.02Mpa to obtain the second ointment 510g (HPLC detects in the second ointment containing B1a=7.76%), in the second ointment, add crystallization solvent n-butanol 510g, in Stir at 60°C to dissolve the second ointment, then program the temperature down to 25°C (10°C per hour), then stir at this temperature (stirring condition is 30rpm) to grow crystals for 6 hours; filter the obtained crystal slurry, and wash the obtained c...

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Abstract

The invention discloses a method for extracting residual avermectin B1a from primary crystallization mother liquor of avermectin B1a. The method comprises the steps that low-grade ketone is added to avermectin factice, heating and stirring are conducted to make the low-grade ketone dissolved, cooling and centrifugation are conducted, obtained supernatant is recycled and concentrated, and second factice is obtained; crystallization solvent is added to the second factice which is dissolved through heating, cooling is conducted to enable crystals to grow, the crystals are separated, and coarse powder is obtained; methanol is added to the coarse powder, then activated carbon is added for decoloring treatment, filtrate is recrystallized twice, and avermectin B1a fine powder with the content of the avermectin B1a larger than or equal to 95% is obtained. By means of the method for extracting the residual avermectin B1a from the primary crystallization mother liquor of the avermectin B1a, the B1a component in the primary crystallization mother liquor can be effectively recycled, 86% of the B1a component in the mother liquor can be recycled through the primary crystallization, and the content of the B1a component in the obtained coarse powder reaches up to 65%. In addition, the method has the advantages of being simple in process, low in cost and suitable for the needs of industrial production and meets the industrial requirements, and meanwhile the realistic problem that the factice is banned from using nationally is solved.

Description

technical field [0001] The invention relates to a method for extracting residual biologically active antibiotic components from antibiotic waste liquid, in particular to a method for extracting residual abamectin B1a from a primary crystallization mother liquor of abamectin B1a. Background technique [0002] Abamectin, the English name Avermectins, is a natural fermentation component of Streptomyces. It is a class of sixteen-element antibiotics with insecticidal, acaricidal and nematicidal activities first developed by Satoshi Omura of Kitasato University in Japan and Merck Company of the United States. Cyclic lactone compounds, which have 8 different structures, are A1a, A1b, A2a, A2b, B1a, B1b, B2a and B2b, forming 4 pairs of homologues. Among them, A1a, A2a, B1a and B2a have higher activity, and among them, B1a has the strongest biological activity. Abamectin has been widely used in animal parasite control and crop control since it came out in the early 1980s. [0003] ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/08C07H1/08
CPCC07H1/08C07H17/08
Inventor 刘中须王琳慧聂会敏郭军杰鲁森宋立斌
Owner HEBEI XINGBAI AGRI SCI & TECH CO LTD
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