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Method preparing abamectin Bla fine powder by secondary crystallization in abamectin Bla

A technology of abamectin and crystallization mother liquor, which is applied to the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of abamectin B1a product purity and low yield, and reduce production costs Effect

Active Publication Date: 2015-09-02
QILU PHARMA INNER MONGOLIA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Above two kinds of methods all are to carry out crystallization at low temperature, and the Abamectin B1a product purity and the yield that crystallization obtains are all not high

Method used

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  • Method preparing abamectin Bla fine powder by secondary crystallization in abamectin Bla
  • Method preparing abamectin Bla fine powder by secondary crystallization in abamectin Bla

Examples

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Effect test

Embodiment 1

[0040] A method for preparing the fine powder of abamectin B1a by secondary crystallization in an abamectin B1a crystallization mother liquor, comprising the following steps:

[0041] 1. Weigh 1500ml of abamectin B1a crystallization mother liquor, heat up to 70°C for vacuum distillation for 2 hours, and concentrate the solution into a paste to obtain a thick ointment. The vacuum degree during concentration is -0.07MPa.

[0042] 2. Weigh the weight of the paste obtained above as 450g (content: Abamectin B1a5.2%), add 1150ml of sec-butyl acetate, heat up to 60°C and stir to dissolve for 30 minutes until the ointment thick material is completely dissolved, then add 350ml of saturated Saline, stirred at 80°C for 1 hour, then allowed to stand for 30 minutes, then separated the water, repeated the above washing twice, separated the layers, and removed the water phase to obtain a sec-butyl acetate solution.

[0043] 3. The obtained sec-butyl acetate solution was heated to 95° C. with...

Embodiment 2

[0046] A method for preparing the fine powder of abamectin B1a by secondary crystallization in an abamectin B1a crystallization mother liquor, comprising the following steps:

[0047] 1. Weigh 1500ml of abamectin B1a crystallization mother liquor, heat up to 78°C for vacuum distillation for 2 hours, concentrate the solution into a paste to obtain a thick ointment, and the vacuum degree during concentration is -0.06MPa.

[0048] 2. Weigh the weight of the paste obtained above as 460g (content: Abamectin B1a5.1%), add 1100ml of sec-butyl acetate, heat up to 60°C and stir to dissolve for 30 minutes until the ointment thick material is completely dissolved, then add 350ml of saturated Saline, stirred at 80°C for 1 hour, then allowed to stand for 30 minutes, then separated the water, repeated the above washing twice, separated the layers, and removed the water phase to obtain a sec-butyl acetate solution.

[0049] 3. The obtained sec-butyl acetate solution was heated to 94° C. with...

Embodiment 3

[0052] A method for preparing the fine powder of abamectin B1a by secondary crystallization in an abamectin B1a crystallization mother liquor, comprising the following steps:

[0053] 1. Weigh 1500ml of abamectin B1a crystallization mother liquor, heat up to 68° C. for 2 hours and distill in vacuum for 2 hours, and concentrate the solution into a paste to obtain a thick ointment. The vacuum degree during concentration is -0.05MPa.

[0054] 2. Weigh the weight of the paste obtained above as 460g (content: Abamectin B1a5.0%), add 960ml of sec-butyl acetate, heat up to 60°C and stir to dissolve for 30 minutes until the ointment thick material is completely dissolved, then add 350ml of saturated Saline, stirred at 80°C for 1 hour, then allowed to stand for 30 minutes, then separated the water, repeated the above washing twice, separated the layers, and removed the water phase to obtain a sec-butyl acetate solution.

[0055] 3. Use a water bath to raise the temperature of the obtai...

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Abstract

The invention relates to a method preparing abamectin Bla fine powder by secondary crystallization in abamectin Bla. The method comprises the steps of condensing an abamectin Bla crystallization mother liquid until no fraction is generated in a vacuum condition, so as to obtain a thick ointment slurry; adopting sec-Butyl acetate as an extraction agent, growing the grain to obtain a plurality of abamectin Blas when the temperature is risen to 90-95 DEG C and the stirring speed is 10-20 r / min, therefore the yield of the abamectin Bla in the abamectin Bla crystallization mother liquid can be improved.

Description

Technical field: [0001] The invention relates to a preparation method of biological pesticides, in particular to a method for preparing abamectin B1a fine powder by secondary crystallization in abamectin B1a crystallization mother liquor, and belongs to the technical field of pesticide preparation. Background technique: [0002] Abamectin is a group of 16-membered macrolide antibiotics with similar structure isolated and extracted from the fermentation product of Streptomyces. of the two components. Abamectin is a new type of biopesticide with broad-spectrum, high efficiency and low toxicity. It is used to control Brassicaceae diamondback moth, cotton spider mite, citrus leafminer rust tick, cotton bollworm, and two-spotted spider mite. and cabbage caterpillar, etc.; the insecticidal mechanism is unique, it can block the nerve conduction of invertebrates, and lasts for a long time; it is easy to decompose in water and soil, and will not pollute the environment. It is a bio...

Claims

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Application Information

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IPC IPC(8): C07H17/08C07H1/06
CPCC07H1/06C07H17/08
Inventor 单辉刘世宽王志敏
Owner QILU PHARMA INNER MONGOLIA
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