Extraction process for industrial mass production of spinosad

A technology of spinosyn and extraction method, applied in the direction of sugar derivatives, sugar derivatives, organic chemistry, etc., can solve the problems of poor product quality, large amount of solvent used, long production cycle, etc. High extraction efficiency and low solvent usage

Active Publication Date: 2017-12-15
QILU PHARMA INNER MONGOLIA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Aiming at the technical problems of large amount of solvent used, high energy consumption, long production cycle and poor product intrinsic quality existing in the existing spinosyn industrial production process, the present invention provides a low-solvent, high-yield spinosyn Industrial extraction method

Method used

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  • Extraction process for industrial mass production of spinosad
  • Extraction process for industrial mass production of spinosad
  • Extraction process for industrial mass production of spinosad

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] A low-solvent, high-yield industrial extraction method of spinosad, the specific steps are as follows:

[0039] (1) 10m 3 Pretreatment tank access 4.95m 3 Add 99kg of perlite, 24.75kg of yellow blood salt, and 49.5kg of zinc sulfate into the fermented liquid (1201u / ml), heat up to 90°C with direct steam, and keep stirring for 2 hours.

[0040] (2) Utilize the plate and frame filter press to filter the fermented liquid that has been pretreated, after press filtration, collect filter cake, wet filter cake weight 592kg.

[0041] (3) Use flash drying to dry the wet filter cake. The temperature of the flash inlet air is controlled at 80°C to 100°C. The moisture content of the dried mycelia is controlled at 8.1%. The weight of mycocin dry powder is 305kg and the potency is 19277u / mg, the yield was 98.9%.

[0042] (4) Put 305kg of spinosad mycelia with a potency of 19277u / mg into the extraction column after drying, and use 1.5m 3 Soak in methanol for 1-2 hours, then pass ...

Embodiment 2

[0048] A low-solvent, high-yield industrial extraction method of spinosad, the specific steps are as follows:

[0049] (1) 10m 3 Pretreatment tank access 5.5m 3 Add 110kg of perlite, 27.5kg of yellow blood salt, and 55kg of zinc sulfate into the fermented liquid (1355u / ml), and heat up to 90°C with direct steam, and keep stirring for 2 hours.

[0050] (2) Utilize plate and frame filter press to filter the pretreated fermented liquid, after press filtration, collect filter cake, wet filter cake weight 642kg

[0051] (3) Use flash drying to dry the wet filter cake, the temperature of the flash inlet air is controlled at 80°C to 100°C, the moisture content of the dried mycelia is 8.3%, the weight of mycocin dry powder is 330kg, and the potency is 22245u / mg , the yield was 98.5%.

[0052] (4) 330kg of spinosad mycelia with a potency of 22245u / mg after drying are put into the extraction column, and the 1.65m 3 Soak in methanol for 1-2 hours, then pass nitrogen gas from the top ...

experiment example

[0058] at 10m 3 Fermentation broth as an example

[0059]

[0060]

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Abstract

The invention relates to an extraction process for industrial mass production of spinosad. The process includes the steps of: fermentation broth pretreatment, frame and plate filtration, and flash drying; mycelium soaking in methanol; concentration of extract liquid, phase inversion washing; back extraction with tartaric acid; adjustment of pH and centrifugation to obtain a spinosad crude product; and recrystallization with methanol to obtain a spinosad fine product. The process provided by the invention extracts spinosad by means of mycelium separation, drying and extraction, and has the characteristics of high extraction efficiency, small solvent dosage, which is only half of that of fermentation broth direct solvent extraction, relatively low energy consumption, and shortened production cycle. In addition, the equipment needed by frame and plate filtration, flash drying, extraction, concentration, washing, back extraction and refining is general, therefore industrial production can be realized easily. The obtained product has high yield up to 85%-90%, after purification of spinosad coarse crystals by solvent recrystallization, the quality of spinosad is improved, and the product content reaches 95%-98%.

Description

Technical field: [0001] The invention relates to an extraction process for industrial mass production of spinosyns, and belongs to the technical field of spinosyn preparation. Background technique: [0002] Spinosad is a secondary metabolite produced by the soil actinomycete Polyspora spinosa through aerobic fermentation in culture medium. The excellent characteristics of biodegradability have won the "Presidential Green Chemicals Challenge Award" of the United States. Because spinosad can effectively control a variety of stored grain pests, with very little dosage, safety and high efficiency, and low residue, it is considered to be a very promising "green" protective agent for stored grains. [0003] For the extraction of spinosad, most of the researches on domestic technology focus on solvent extraction method and resin adsorption extraction method. Although the resin adsorption extraction method has a better effect to a certain extent, such as higher purity, but in large...

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 梁振兵安文俊刘世宽居亚东
Owner QILU PHARMA INNER MONGOLIA
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