CN1389465A - Supercritical fluid extraction process of nim to produce mimbin extract - Google Patents
Supercritical fluid extraction process of nim to produce mimbin extract Download PDFInfo
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- CN1389465A CN1389465A CN01108503A CN01108503A CN1389465A CN 1389465 A CN1389465 A CN 1389465A CN 01108503 A CN01108503 A CN 01108503A CN 01108503 A CN01108503 A CN 01108503A CN 1389465 A CN1389465 A CN 1389465A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The method for producing nimbin extract of nim by supercritical fluid extraction relates to a method for extracting insecticide from plant, its task is to provide a method for producing nimbin extract using supercritical CO2 extraction under the conditions of low temperature and pressure. The method is: after nim seeds are husked and squeezed, its slag cakes are smashed and put into a supercritical fluid extracting device, and adding entrainer into two extracting cans according to the technical conditions of predetermined temperature and pressure, and carrying out alternately static or dynamic continuous extraction, after filtering, filter liquor by vacuum is concentrated into nimbin concrete. This method has high extraction efficiency, and can reach industrialized production of nimbin concrete of plant source insecticide.
Description
The present invention relates to from vegetable material, extract the method for sterilant, thereby in particular to the method with supercritical fluid extraction neem seed or kind benevolence extracting effective components.
People know that contained in seal chinaberry (neem) seed is tens kinds of effective constituents of representative with nimbin (Azadirachtin), many crop desinsections, insect protected is had extraordinary effect, and can not cause environmental pollution.Existing seed from the seal chinaberry, plant the technology of extracting nimbin the benevolence, the extracting process that generally adopts is before this to seed or plant benevolence and carried out machinery oil expression at present, then with the conventional organic solvents method to oil removing after a blob of slag carry out the nimbin extraction.This respect domestic and foreign literature, patent are more, as No. 1145397, more representative Chinese patent, adopt organic solvent such as methyl alcohol, sherwood oil, ethyl acetate, chloroform, acetone etc., prepare nimbin through step extractions such as degreasing, extraction distribution, upper prop separate, concentrate, its shortcoming is that consumption of organic solvent is big, kind is many, environment there is considerable influence, and processing step is loaded down with trivial details, particularly since nimbin itself to the photo-thermal instability, repeated multiple times high temperature at organic solvent concentrates in the removal process, and greater loss is arranged.Therefore, people make every effort to seek a kind of more advanced, industrial production is feasible, the new technologies that has fewer environmental impacts, to improve the nimbin extraction efficiency and to reduce environmental pollution.Supercritical fluid extraction is exactly comparatively to be appropriate to the class new technology that nimbin extracts, relevant patent of the domestic nothing of this respect or document by retrieval, external pertinent literature mainly concentrate on tests indoor supercritical extraction and prepares the nimbin sample to carry out assay determination.German patent DE 19601482A1 has related at CO
2Subcritical or supercritical state under, by adding the extraction that the lower alcohols entrainment agent carries out neem seed or plants nimbin in the benevolence, in its key technical index, except 10～70 ℃ of the scopes of extraction temperature, especially between 30 ℃ to 45 ℃, be supercritical CO
2Extraction process custom select and the temperature range used outside, in other index extracting pressure be 25MPa (250bar) to 60MPa (600bar), especially at 30MPa (300bar) to 40MPa (400bar) scope, at supercritical CO
2In the extraction, this pressure range belongs to mesohigh extraction scope, and to the equipment requirements height, large-scale production unit non-stop run pressure is not reach this requirement, is exactly that cost is too high; 3～9 hours whole extraction time, especially after 4～6 hours, finish, consuming time longer, this can influence production efficiency; This method only adopts an extractor simultaneously, continuously alternate operation, realization suitability for industrialized production.
Task of the present invention provide a kind of can lesser temps and in, carry out neem seed under the low pressure condition or plant the extraction of nimbin composition in the benevolence, particularly adopt supercritical CO
2Thereby extract the method for producing mimbin extract, and, can shorten the extraction time again, realize suitability for industrialized production guaranteeing both to have reduced organic solvent use kind and usage quantity under the nimbin extraction efficiency condition.
Thereby contriver's process is to the technical study with supercritical fluid extraction neem seed or kind benevolence extracting effective components, found out the key that will realize suitability for industrialized production and be that extracting pressure, time and entrainment agent use the kind ratio, because the extracting pressure height is not only relevant to selectivity, percentage extraction and rate of extraction that nimbin extracts with method, also relate to equipment manufacturing cost, cost of investment; Extraction time length relates to the benefit of method or technology; The use kind of entrainment agent and amount are not only influential to environment, also directly related with cost.Occupy above-mentioned cognition, method provided by the invention is: neem seed is through peeling off, a blob of slag that obtains after the machinery oil expression drops in the supercritical fluid extraction equipment through pulverizing, by processing condition such as the temperature of setting, pressure and add entrainment agent in two extractors hocket respectively static state, (dynamically) continuous extraction of flowing, the extraction liquid that obtains after the extraction after filtration, filtrate is made mimbin extract through the vacuum concentration of routine again.
The used supercutical fluid of the present invention is the CO that is in supercritical state
2
The used entrainment agent of the present invention can select to use a kind of in methyl alcohol, ethanol, acetone or the ethyl acetate.
The processing condition of extractor are controlled to be pressure (promptly in 20～249bar) scopes, temperature are in 30～60 ℃ of scopes, and the static extracting time is 1/4～1 hour at 2～24.9MPa in static extracting.The consumption of entrainment agent is 1: 0.5～1: 1.5 (volume ratio of raw materials quality and entrainment agent).
The processing condition of extractor are controlled to be pressure at 2～24.9MPa (promptly in 20～249bar) scopes in dynamic extraction, temperature is at 30～60 ℃, the mobile extraction time is 1～2 hour, wherein constantly add entrainment agent, reach 1: 5 up to entrainment agent ratio accumulation and stop to add entrainment agent when (volume ratio of raw materials quality and entrainment agent); (promptly in 20～70bar) scopes, temperature is at 30～50 ℃ at 2～7MPa to be controlled to be pressure with corresponding surge tank of dynamic extraction and separating tank processing condition.
The invention provides a kind of industrial process that is used for neem seed or plants the employing supercritical fluid extraction of benevolence nimbin composition, it is characterized in that static extracting combines with the extraction of flowing, two jars of continuous alternate modes of operation are guaranteeing under the nimbin composition extraction efficiency situation, with supercritical CO
2For extraction agent and recycle, a kind of in methyl alcohol, ethanol, acetone or the ethyl acetate is entrainment agent, compare with existing organic solvent method or supercritical fluid extraction, reached and reduced the purpose that organic solvent uses kind and usage quantity, the low extracting pressure of use, shortens the extraction time, not only reduced influence to environment, reduce the input of processing unit simultaneously, extraction efficiency is improved, can realize suitability for industrialized production plant insecticide mimbin extract.
The accompanying drawing 1 expression schematic diagram of producing mimbin extract with supercritical fluid extraction neem seed or kind benevolence of the present invention, 1 is the liquid carbon dioxide basin among the figure, and 2 is the entrainment agent basin, and 3,4 is high-pressure pump, 5,6 is mixing tank, 7,8,9,10,11,12,15,16,17,18,21,22 be valve, 13,14 are respectively No. 1 extractor and No. 2 extractors, and 19 is surge tank, 20 is separating tank, 23 is under meter, and 24 is adsorber, and 25 is compressor.
Expression mixing tank, extractor, surge tank, separating tank are in heat exchange and the temperature controlling system.
Embodiment: with reference to accompanying drawing 1, each 10kg neem kernel machine is pressed a de-oiling blob of slag pulverized 20 orders (nimbin content is 0.4% after measured), drop into respectively in No. 1 extractor (13) and No. 2 extractors (14), squeeze into 1: 1 (raw materials quality and entrainment agent volume ratio) entrainment agent in extractor (13) by entrainment agent pump (4), entrainment agent methyl alcohol starts CO
2Pump (3) makes No. 1 extractor (13) pressure-controlling at 10MPa, and temperature is controlled at 50 ℃, carries out static extracting after 0.5 hour, starts and adjusting CO
2Pump (3) and entrainment agent pump (4), open and regulated valve (15), (16), (22), keep the pressure of No. 1 extractor and temperature and static extracting pressure and temperature in above-mentioned scope, make buffering (19) and separating tank (20) pressure-controlling at 5MPa, 40 ℃ of temperature, flow and extracted 1.5 hours, when raw material: the accumulation of entrainment agent ratio reaches 1: 5 when (raw materials quality and entrainment agent volume ratio), stopping entrainment agent pump (4) carries the entrainment agent of No. 1 extractor (13), switch valve (7), (8), (9), (10) turn to No. 2 extractors (14), import entrainment agent and No. 2 extractors (14) are reached in the same pressure and temp claimed range of above-mentioned static extracting by above-mentioned same requirement, carry out static extracting; Switch valve (9), (10) turn to No. 1 extractor (13) to continue but only use CO
2No. 1 extractor extracted stop extraction in 45 minutes, behind the switch valve No. 1 extractor is loaded and unloaded material.Undertaken after flow (dynamically) to No. 2 extractors (14) be extracted to extraction and finish by above-mentioned steps, the next round that transfers to No. 1 extractor extracts, and alternately operates continuously again.Regularly emit extract from separating tank (20), filter, vacuum decompression concentrates then.By above technology point, 10kg machine in the single extractor is pressed a de-oiling seal chinaberry blob of slag, whole extraction process can be finished in 3 hours, made solid-state yellow-green colour to blackish green mimbin extract 350g, and nimbin content is greater than 10%.
Claims (4)
1. thereby one kind is adopted the supercritical fluid extraction neem seed or plants the method that benevolence is produced mimbin extract, this method be with neem seed through peeling off, a blob of slag that obtains after the machinery oil expression drops into supercritical fluid extraction equipment through pulverizing, usually with supercritical CO
2Extract, the invention is characterized in that extraction process is by processing condition such as the temperature of setting, pressure and adds entrainment agent in two extractors hocket respectively static state, dynamically continuous extraction, the extraction liquid that obtains after the extraction after filtration, filtrate adopts conventional vacuum concentration to make mimbin extract.
2. the method for claim 1 is characterized in that used entrainment agent can select to use a kind of in methyl alcohol, ethanol, acetone or the ethyl acetate.
3. the method for claim 1, (promptly in 20～249bar) scopes, temperature is in 30～60 ℃ of scopes, and the static extracting time is 1/4～1 hour at 2～24.9MPa to it is characterized in that processing condition in the static extracting being controlled to be pressure.The consumption of entrainment agent is 1: 0.5～1: 1.5 (volume ratio of raw materials quality and entrainment agent).
4. the method for claim 1, it is characterized in that processing condition in the dynamic extraction are controlled to be pressure at 2～24.9MPa (promptly in 20～249bar) scopes, temperature is at 30～60 ℃, the mobile extraction time is 1～2 hour, wherein constantly add entrainment agent, reach 1: 5 up to entrainment agent ratio accumulation and stop to add entrainment agent when (volume ratio of raw materials quality and entrainment agent); (promptly in 20～70bar) scopes, temperature is at 30～50 ℃ at 2～7MPa to be controlled to be pressure with corresponding surge tank of dynamic extraction and separating tank processing condition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011085037A CN1184222C (en) | 2001-06-06 | 2001-06-06 | Supercritical fluid extraction process of nim to produce mimbin extract |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011085037A CN1184222C (en) | 2001-06-06 | 2001-06-06 | Supercritical fluid extraction process of nim to produce mimbin extract |
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| Publication Number | Publication Date |
|---|---|
| CN1389465A true CN1389465A (en) | 2003-01-08 |
| CN1184222C CN1184222C (en) | 2005-01-12 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB011085037A Expired - Fee Related CN1184222C (en) | 2001-06-06 | 2001-06-06 | Supercritical fluid extraction process of nim to produce mimbin extract |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102696696A (en) * | 2012-06-11 | 2012-10-03 | 四川农业大学 | Grass meal granular formulation for controlling rodent pests in grassland and preparation method as well as application thereof |
| CN103483358A (en) * | 2013-10-15 | 2014-01-01 | 成都绿金生物科技有限责任公司 | Method for producing neem crude drug by extracting neem with supercritical CO2 |
| CN114247170A (en) * | 2022-01-11 | 2022-03-29 | 深圳市九然生物科技有限公司 | Continuous SPE-SFF production equipment |
| CN116422007A (en) * | 2023-05-12 | 2023-07-14 | 江苏东宝农化股份有限公司 | Extraction device and application thereof in extraction of azadirachtin |
-
2001
- 2001-06-06 CN CNB011085037A patent/CN1184222C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102696696A (en) * | 2012-06-11 | 2012-10-03 | 四川农业大学 | Grass meal granular formulation for controlling rodent pests in grassland and preparation method as well as application thereof |
| CN103483358A (en) * | 2013-10-15 | 2014-01-01 | 成都绿金生物科技有限责任公司 | Method for producing neem crude drug by extracting neem with supercritical CO2 |
| CN103483358B (en) * | 2013-10-15 | 2015-08-05 | 成都绿金生物科技有限责任公司 | A kind of supercritical CO 2extraction print chinaberry produces the method for the former medicine of print chinaberry |
| CN114247170A (en) * | 2022-01-11 | 2022-03-29 | 深圳市九然生物科技有限公司 | Continuous SPE-SFF production equipment |
| CN116422007A (en) * | 2023-05-12 | 2023-07-14 | 江苏东宝农化股份有限公司 | Extraction device and application thereof in extraction of azadirachtin |
| CN116422007B (en) * | 2023-05-12 | 2023-11-07 | 江苏东宝农化股份有限公司 | Extraction device and application thereof in extraction of azadirachtin |
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| Publication number | Publication date |
|---|---|
| CN1184222C (en) | 2005-01-12 |
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Addressee: Chengdu Lujin Biological Sci-Tech Co., Ltd. Document name: Notice of publication of application for patent for invention |
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Owner name: CHENGDU LVJIN HI-TECH CO.LTD. Free format text: FORMER OWNER: CHENGDU LVJIN BIOTECHNOLOGY CO.,LTD. Effective date: 20070921 |
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Effective date of registration: 20070921 Address after: 5 No. 610041 Sichuan province Chengdu city Chengdu high tech Zone Gaopeng Avenue (Dr. Chengdu Park) Patentee after: Chengdu Green Gold High-tech Co., Ltd. Address before: 5 No. 610041 Sichuan province Chengdu city Chengdu high tech Zone Gaopeng Avenue (Dr. Chengdu Park) Patentee before: Chengdu Lujin Biological Sci-Tech Co., Ltd. |
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