Preparation method of azadirachtin dry powder

A technology of azadirachtin and dry powder, applied in the direction of organic chemistry and the like, can solve the problems of not mentioning the solvent recovery rate, unfavorable to the dry powder of azadirachtin, influence on the stability of azadirachtin, etc. Low cost and high equipment requirements

Inactive Publication Date: 2014-09-10
THE RES INST OF RESOURCES INSECTS RIRI OF THE CHINESE ACADEMY OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, the process of extracting at 60°C for 5 hours and heating the extract in a water bath at 50°C for 10 minutes will partially decompose the thermally unstable azadirachtin, which is not conducive to obtaining high-content dry powder of azadirachtin, and in the method No mention of solvent recovery
Chinese patent application CN1423939A has announced the preparation method of the azadirachtin dry powder not containing aflatoxin, has added alkaline oxidizing agent in its preparation process, because azadirachtin is more stable under the weak acidic condition of pH3~5, and in alkaline Unstable in the environment, the addition of alkaline oxidants will have a certain impact on the stability of azadirachtin

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) After mixing 1 kg of dried neem seeds and 1 kg of petroleum ether, place it in the rapid extractor described in Chinese patent ZL200820080967.5 to extract neem oil with stirring, filter to obtain filtrate and filter residue, and add petroleum ether to the filter residue 1kg continued to extract neem oil, filtered to obtain filtrate and filter residue, combined secondary filtrate, and after the filter residue was air-dried, it was neem cake 700g; after the combined secondary filtrate was recovered petroleum ether under reduced pressure, 300g of neem oil was obtained;

[0026] (2) After mixing 700g of neem cake obtained in step (1) with 700g of methanol, place it in the rapid extractor of step (1) for stirring and extraction for 3 minutes, filter to obtain the filtrate and filter residue, add 700g of methanol to the filter residue and mix , stirred and extracted for 3 minutes, repeated extraction three times like this, collected three times of filtrate 2100mL, and then...

Embodiment 2

[0032] (1) After mixing 100kg of dried neem seeds and 200kg of petroleum ether, place it in the rapid extractor described in Chinese patent ZL200820080967.5 to extract neem oil with stirring, filter to obtain filtrate and filter residue, and add petroleum ether to the filter residue 200kg continue to extract neem oil, filter to get filtrate and filter residue, merge the secondary filtrate, after the filter residue is air-dried, it is neem cake 70kg; the combined secondary filtrate obtains neem oil 30kg after decompression reclaiming sherwood oil;

[0033] (2) After mixing 70kg of neem cake obtained in step (1) with 140kg of methanol, place it in the rapid extractor of step (1) for stirring and extraction for 3 minutes, filter to obtain the filtrate and filter residue, add 140kg of methanol to the filter residue and mix , stirred and extracted for 3 minutes, repeated extraction three times like this, collected 420L of filtrate three times, then concentrated the filtrate to 1 / 3 o...

Embodiment 3

[0039] (1) After mixing 1 kg of dried neem seeds with 3 kg of petroleum ether, place it in the rapid extractor described in Chinese patent ZL200820080967.5 to extract neem oil with stirring, filter to obtain filtrate and filter residue, and add petroleum ether to the filter residue 3kg continued to extract neem oil, filtered to obtain filtrate and filter residue, combined secondary filtrate, and after the filter residue was air-dried, it was neem cake 700g; after the combined secondary filtrate recovered petroleum ether under reduced pressure, 300g of neem oil was obtained;

[0040] (2) After mixing 700g of neem cake obtained in step (1) with 700g of methanol, place it in the rapid extractor of step (1) for stirring and extraction for 3 minutes, filter to obtain the filtrate and filter residue, add 700g of methanol to the filter residue and mix , stirred and extracted for 3 minutes, repeated extraction three times like this, collected three times of filtrate 2100mL, and then co...

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PUM

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Abstract

The invention provides a preparation method of azadirachtin dry powder. The preparation method comprises the following steps of mixing dried azadirachtin seeds with petroleum ether, and then stirring to extract azadirachtin oil; drying extracting residues in air to obtain an azadirachtin cake; then, mixing the azadirachtin cake with methanol and then stirring and extracting, filtering to collect filtrate and concentrating, and then oscillating and mixing concentrate with distilled water; extracting by dichloromethane to obtain azadirachtin extract, adding a polar organic solvent A to dissolve and mix with a solvent B; and then filtering under reduced pressure to obtain solid precipitates, and drying the solid precipitates after eluting by a solvent C to obtain the azadirachtin dry powder. The method provided by the invention is simple in process, high in solvent recovery rate, high in azadirachtin active ingredient content and lower in cost. The preparation method disclosed by the invention avoids cross infection of the organic solvent, is beneficial to recycling the solvent, lowers material cost and reduces environment pollution, and is applicable to large-scale production.

Description

technical field [0001] The invention relates to a preparation method of biological pesticides, in particular to a preparation method of azadirachtin dry powder. Background technique [0002] Neem (Azadirachta indica A.Juss.) is a plant of the family Meliaceae, containing more than 300 active ingredients, of which Azadirachtin has the highest insecticidal activity. Azadirachtin (C 35 h 44 o 16 ) is a class of highly oxidized tetracyclic triterpenoids (limonoids), with seven molecular isomers of Azadirachtin A-G, and Azadirachtin A is the azadirachtin compound with the highest content and activity. The whole plant of the neem tree contains azadirachtin, especially the most abundant content in the seed kernel (0.2% to 0.6%). [0003] Azadirachtin has strong biological activity on more than 200 kinds of insects (including almost all important agricultural, forestry, storage, and sanitary pests), and is harmless to higher animals. It is relatively safe to natural enemies of i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D519/00
CPCC07D519/00
Inventor 段琼芬王有琼马李一张重权
Owner THE RES INST OF RESOURCES INSECTS RIRI OF THE CHINESE ACADEMY OF FORESTRY
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