Refining method of methylamino abamectin benzoate

A technology of methylamino abamectin and benzoate, applied in the field of pesticides, can solve the problems of low yield, the purity of methylamino abamectin benzoate is less than 98%, etc., and achieves convenient operation and environmental protection Favorable, stability-enhancing effects are required

Active Publication Date: 2018-06-22
武汉回盛生物科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the preparation and refining of emamectin benzoate both at home and abroad have multiple methods, such as foreign patent WO 95 / 05390 domestic patent CN103012525A, CN103497226A, CN104876990A have all adopted recrystallization to purify emamectin The report of benzoate, but the major problem that exists is, the purity of emamectin benzoate is not more than 98% and the yield is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Because after different solvents are mixed, the volume of the mixed solvent is not the sum of each volume, and the mixing ratio of different solvents will also affect the volume of the mixed solvent, so in the present invention, the mixed solvent of n-heptane, tetrahydrofuran, and dichloromethane is based on the mass ratio of each solvent. Proportioning is carried out, and the mixed solvents mentioned in the following examples are also proportioning according to this idea.

[0028] A method for refining emamectin benzoate, comprising the steps of:

[0029] Step 1: Take 50g of emamectin benzoate and add 200ml of acetone at room temperature at 30°C, stir until dissolved, then add 0.3g of granular activated carbon to it, decolorize for 30min, and filter the decolorized solution with suction deal with;

[0030] The emamectin benzoate crude product used in the first step is prepared by the following method: add 8.0kg of emamectin and 15L ethyl acetate in the reactor of 50L ...

Embodiment 2

[0037] The first step: at room temperature at 35°C, take 50 g of emamectin benzoate (same as in Example 1) and add 260 ml of acetone, stir until dissolved, then add 0.5 g of granular activated carbon to it, decolorize for 30 minutes, and decolorize After the treatment, the solution is subjected to suction filtration;

[0038] The second step: cooling the filtrate obtained in the first step to 0 ° C, and filtering to obtain a solid;

[0039] The third step: at 20°C, dissolve the solid obtained in the second step in a mixed solution of 360g n-heptane, tetrahydrofuran, and dichloromethane, and the masses of n-heptane, tetrahydrofuran, and methylene chloride in the mixed solvent are 144g and 180g respectively , 36g, stir until the solid is completely dissolved;

[0040] The fourth step: cool down the solution obtained in the third step to -5°C, and freeze it. The freezing crystallization time is 8 hours. Put into the vacuum drying oven, make the drying room temperature be 55 ℃, ...

Embodiment 3

[0042] The first step: at room temperature at 32°C, take 100 g of emamectin benzoate (same as Example 1) and add 480 ml of acetone, stir until dissolved, then add 0.5 g of granular activated carbon to it, and decolorize it for 30 minutes. After the treatment, the solution is subjected to suction filtration;

[0043]The second step: cooling the filtrate obtained in the first step to 0 ° C, and filtering to obtain a solid;

[0044] The third step: at 15°C, dissolve the solid obtained in the second step in a mixed solution of 600g n-heptane, tetrahydrofuran, and methylene chloride, and the masses of n-heptane, tetrahydrofuran, and methylene chloride in the mixed solvent are 240g and 300g respectively , 60g, stir until the solid is completely dissolved;

[0045] The fourth step: cool down the solution obtained in the third step to -8°C and freeze it for 10 hours. After filtering, the product is rinsed twice with glacial ethyl acetate at 0°C. Put into the vacuum drying oven, make...

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Abstract

The invention discloses a refining method of methylamino abamectin benzoate, and belongs to the technical field of pesticides. The method comprises the steps that the methylamino abamectin benzoate isdissolved first, then the dissolved methylamino abamectin benzoate is cooled after being decolorized, and a solid is obtained with filtration, and the obtained solid is subjected to freeze crystallization treatment in a mixed solution of n-heptane, tetrahydrofuran and dichloromethane, and an obtained crystal is subjected to filtration, washing and drying to obtain a refined product of the methylamino abamectin benzoate. The method disclosed by the invention can obtain the high-yield and extremely high-purity refined product of the methylamino abamectin benzoate after one-time treatment, the yield can reach 80% to 85%, and the purity is not less than 99.0%.

Description

technical field [0001] The invention belongs to the technical field of pesticides, in particular to a method for refining emamectin benzoate. Background technique [0002] Emamectin benzoate, commonly known as emamectin benzoate, was first successfully developed by Merck in 1984. It is a new generation of green pesticide with high activity, less residue, good safety and advanced dosage forms. With many advantages, it is recognized as the leading product of pesticides in the industry; it is widely used in the control of food, economic crops and vegetable pests. Studies have shown that emamectin benzoate has a good effect at a very low dose. It has extremely high activity against pests such as cotton bollworm and mites, and it is still resistant to pests that have developed resistance to other pesticides. High efficiency, the drug is easy to degrade in the soil, no pollution, no residue, safe for beneficial insects, natural enemies of pests, humans, and animals within the con...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/08C07H1/06
CPCC07H1/06C07H17/08
Inventor 沈国春余建飞邱壮吴雨丁文格赵宇
Owner 武汉回盛生物科技股份有限公司
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