CN101857603B - Multi-stage countercurrent extraction method for azadirachtin - Google Patents
Multi-stage countercurrent extraction method for azadirachtin Download PDFInfo
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- CN101857603B CN101857603B CN 201010164897 CN201010164897A CN101857603B CN 101857603 B CN101857603 B CN 101857603B CN 201010164897 CN201010164897 CN 201010164897 CN 201010164897 A CN201010164897 A CN 201010164897A CN 101857603 B CN101857603 B CN 101857603B
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- nimbin
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- countercurrent extraction
- azadirachtin
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Abstract
The invention provides a multi-stage countercurrent extraction method for azadirachtin, which is characterized in that: coarsely crushed neem seeds are put into a multi-stage countercurrent extraction device, and a solvent is pumped into the multi-stage countercurrent extraction device for dynamic countercurrent extraction at normal temperature or by heating properly; and the extracting solution is concentrated to prepare a solid extract containing 10 to 20 percent of azadirachtin, and the solid extract is used for preparing azadirachtin pesticides. The method has the advantages of short process flow, high extraction speed, high yield of azadirachtin, energy and solvent conservation, low production cost, easy industrial production and the like.
Description
Technical field
The present invention relates to a kind of method of from plant, extracting sterilant, be specifically related to a kind of from neem seed the method for pot group type countercurrent extraction nimbin.
Background technology
The nimbin insecticides have wide spectrum, efficient, low toxicity, noresidue, to people and animals have no side effect, to pest natural enemy safety and characteristics such as be difficult for developing immunity to drugs; Be research both at home and abroad at present and application one of biological pesticide the most widely, classified as the public nuisance-free agricultural chemicals of pollution-free food production emphasis recommendation by green food office of State Council.
From neem seed, extracting nimbin, is primary link and important operation unit that the nimbin insecticides is produced.Nimbin content very low (be generally 0.3%～0.4%, high reaches 0.6%) in the neem seed, nimbin extract comparatively difficulty, and the quality of its extraction process technology directly has influence on economic benefit of enterprises.Contain 20%～30% grease in the neem seed; The direct mechanical pulverizing is difficult in small, broken bits; Influence the leaching of nimbin, its form of feed pretreatment adopts mostly at present and shells, squeezes degreasing (like Chinese patent CN1158928C, CN1184222C, CN1362020A, CN1423938A, CN1423939A, CN1524858A, CN101440099A), but the poor heat stability of nimbin; The degradation rate of nimbin obviously increases during greater than 35 ℃; The degradation rate of nimbin is maximum in the time of 65 ℃, therefore promptly has 40% left and right sides nimbin to be degraded at the squeezing skimming processes owing to high temperature, causes the nimbin productive rate to descend; The solvent of employing or supercritical CO 2 degreasing (like Chinese patent CN1049091C, CN1199980C, CN101029276A, CN1116394C) are also arranged,, increased process period and cost though can reduce the loss of nimbin.Chinese patent CN100448871C neem seed only need shell, and promptly stirs to pulverize with the high speed blade cut without degreasing and extracts, and makes material and solvent have good mobility; The nimbin productive rate is higher, but neem kernel need be used 3～5 times of polar organic solvent preimpregnation 6～12 hours, extraction time be 3～5 hours/inferior; Repeat again 2～5 times, accomplish an extracting cycle and need 15 hours at least, 9 times of solvent extractions of minimum need; And high-speed stirring is pulverized easy overheated; Extract the difficult control of temperature, need to adopt chuck or coil pipe cooling, energy consumption is increased to reduce the nimbin degraded.
Summary of the invention
The objective of the invention is to overcome the shortcoming that exists in the existing nimbin extraction process technology; A kind of pot group type countercurrent extraction method of nimbin is provided, to simplify technical process, shorten extracting cycle, improve the nimbin productive rate, cut down the consumption of energy, save solvent, to be beneficial to suitability for industrialized production.
Technical scheme of the present invention is: the pot group type countercurrent extraction method of nimbin, and its step is following:
A, neem seed is broken into 1～4mm particle;
B, get the neem seed powder and place pot group type countercurrent extraction device, extracting temperature is 10～60 ℃, with several jars be one group, pump into 1: 1～solvent of 5W/V, dynamic countercurrent extracts 20～50min/ jar;
C, collection extracting solution reclaim the solids extraction thing that solvent must contain nimbin in 45 ℃ of concentrating under reduced pressure.
Described jar of group is that every group of 1～9 extractor serial or parallel connection or SP are share.
The said extracted solvent is a kind of in water, alcohol, ketone, ester, replacement hydrocarbon, ether, the nitrile or their mixture; The proportioning of mixture is any proportioning, like water, methyl alcohol, ethanol, Virahol, acetone, butanone, ETHYLE ACETATE, methyl acetate, methylene dichloride, trichloromethane, MTBE, acetonitrile etc. or its mixture.
The present invention and existing Technology relatively have advantage and effect:
1. need not to carry out that seed shells, degreasing, the seed coarse crushing gets final product, and has simplified raw materials pretreatment, saves labor, and has avoided the shell loss of defatting step nimbin of seed;
2. it is multiple extraction to adopt the pot group type dynamic countercurrent to extract alternative single-pot, with a plurality of extraction unit scientific combination, forms concentration gradient between the unit; Increase mass transfer power; Improved the nimbin leaching efficiency, every jar of extraction time has shortened extracting cycle greatly in 50min;
3. but normal temperature or suitably heat (＜35 ℃) extract, and reduce the nimbin degraded, and nimbin is extracted fully, improve nimbin productive rate 8.88%～26.97%;
4. solvent is recycled, solvent load few (1: 2～3.33W/V), follow-up concentrated energy consumption is low;
5. pot group type counterflow extraction apparatus parameter is prone to control, simple operation, safety, and treatment capacity is big, is easy to suitability for industrialized production.
The pot group type countercurrent extraction method of nimbin according to the invention can obviously improve the nimbin productive rate, reduces the input of processing unit, shortens extracting cycle, energy-conservation joint solvent, and production cost is low, is easy to realize suitability for industrialized production, and economic benefit and social benefit are good.
Embodiment
Further set forth the present invention below in conjunction with specific embodiment, but protection scope of the present invention is not limited in this.
Embodiment 1
With single jar is one group; Get neem seed powder 1500g and place extractor, establishing and extracting temperature is 32 ℃, pumps into 5 times of methyl alcohol dynamic countercurrent circulation extraction 49min; Solvent load is 1: 5W/V; Collect extracting solution in 45 ℃ of concentrating under reduced pressure, reclaim the yellow-green colour solids extraction thing (high effective liquid chromatography for measuring) that methyl alcohol must contain 10.89% nimbin, the nimbin productive rate is 0.304%.
Embodiment 2
With 3 jars is one group; Every canned neem seed powder 1500g that goes into, establishing and extracting temperature is 32 ℃, 5 times of methyl alcohol dynamic countercurrents of first jar of usefulness circulation extraction 39min; Second jar with the additional 3 times of methyl alcohol dynamic countercurrent circulation extraction 39min of last unit extracting solution; The 3rd jar is replenished 2 times of methyl alcohol dynamic countercurrent circulation extraction 39min with last unit extracting solution, and solvent load is 1: 3.33W/V, collect extracting solution in 45 ℃ of concentrating under reduced pressure; Reclaim the yellow-green colour solids extraction thing (high effective liquid chromatography for measuring) that methyl alcohol must contain 10.46% nimbin, the nimbin productive rate is 0.331%.
Embodiment 3
With 4 jars be one group, every canned neem seed powder 1500g that goes into, establishing and extracting temperature is 32 ℃; 5 times of methyl alcohol dynamic countercurrents of first jar of usefulness circulation extraction 34min; Second jar is replenished 2.5 times of methyl alcohol dynamic countercurrent circulation extraction 34min with last unit extracting solution, and the 3rd jar is replenished 1.5 times of methyl alcohol dynamic countercurrent circulation extraction 34min with last unit extracting solution, and the 4th jar is replenished 1 times of methyl alcohol dynamic countercurrent circulation extraction 34min with last unit extracting solution; Solvent load is 1: 2.5W/V; Collect extracting solution in 45 ℃ of concentrating under reduced pressure, reclaim the yellow-green colour solids extraction thing (high effective liquid chromatography for measuring) that methyl alcohol must contain 10.62% nimbin, the nimbin productive rate is 0.386%.
Embodiment 4
With 4 jars be one group, every canned neem seed powder 1500g that goes into, establishing and extracting temperature is 32 ℃; 5 times of ethanol dynamic countercurrents of first jar of usefulness circulation extraction 34min; Second jar is replenished 2.5 times of ethanol dynamic countercurrent circulation extraction 34min with last unit extracting solution, and the 3rd jar is replenished 1.5 times of ethanol dynamic countercurrent circulation extraction 34min with last unit extracting solution, and the 4th jar is replenished 1 times of ethanol dynamic countercurrent circulation extraction 34min with last unit extracting solution; Solvent load is 1: 2.5W/V; Collect extracting solution in 45 ℃ of concentrating under reduced pressure, reclaim the green solids extraction thing (high effective liquid chromatography for measuring) that ethanol must contain 13.65% nimbin, the nimbin productive rate is 0.337%.
Embodiment 5
With 4 jars is one group; Every canned neem seed powder 1500g that goes into; If extracting temperature is 32 ℃, 5 times of ETHYLE ACETATE dynamic countercurrents of first jar of usefulness circulation extraction 34min, second jar with the additional 2.5 times of ETHYLE ACETATE dynamic countercurrent circulation extraction 34min of last unit extracting solution; The 3rd jar with the additional 1.5 times of ETHYLE ACETATE dynamic countercurrent circulation extraction 34min of last unit extracting solution; The 4th jar is replenished 1 times of ETHYLE ACETATE dynamic countercurrent circulation extraction 34min with last unit extracting solution, and solvent load is 1: 2.5W/V, collect extracting solution in 45 ℃ of concentrating under reduced pressure; Reclaim the green solids extraction thing (high effective liquid chromatography for measuring) that ETHYLE ACETATE must contain 19.34% nimbin, the nimbin productive rate is 0.228%.
Embodiment 6
With 5 jars is one group; Every canned neem seed powder 1500g that goes into, establishing and extracting temperature is 32 ℃, 5 times of methyl alcohol dynamic countercurrents of first jar of usefulness circulation extraction 29min; Second jar with the additional 2 times of methyl alcohol dynamic countercurrent circulation extraction 29min of last unit extracting solution; The 3rd jar to the 5th jar is all replenished 1 times of methyl alcohol dynamic countercurrent circulation extraction 29min with last unit extracting solution, and solvent load is 1: 2W/V, collect extracting solution in 45 ℃ of concentrating under reduced pressure; Reclaim the yellow-green colour solids extraction thing (high effective liquid chromatography for measuring) that methyl alcohol must contain 10.18% nimbin, the nimbin productive rate is 0.299%.
Claims (1)
1. the pot group type countercurrent extraction method of a nimbin, its step comprises:
A, neem seed is broken into 1～4mm particle;
B, get the neem seed powder and place pot group type countercurrent extraction device; Extract 10～60 ℃ of temperature, with several jars be one group, described jar of group share for every group of 1～9 extractor serial or parallel connection or SP; Pump into 1: 1～solvent of 5W/V, dynamic countercurrent extracts 20～50min/ jar; Said solvent is water, methyl alcohol, ethanol, Virahol, acetone, butanone, ETHYLE ACETATE, ethyl ester methyl esters, methylene dichloride, trichloromethane, MTBE, acetonitrile or its mixture, and mixture ratio is any proportioning; C, collection extracting solution reclaim the solids extraction thing that solvent must contain nimbin in 45 ℃ of concentrating under reduced pressure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010164897 CN101857603B (en) | 2010-05-07 | 2010-05-07 | Multi-stage countercurrent extraction method for azadirachtin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010164897 CN101857603B (en) | 2010-05-07 | 2010-05-07 | Multi-stage countercurrent extraction method for azadirachtin |
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| Publication Number | Publication Date |
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| CN101857603A CN101857603A (en) | 2010-10-13 |
| CN101857603B true CN101857603B (en) | 2012-06-13 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 201010164897 Expired - Fee Related CN101857603B (en) | 2010-05-07 | 2010-05-07 | Multi-stage countercurrent extraction method for azadirachtin |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5397571A (en) * | 1993-03-25 | 1995-03-14 | W. R. Grace & Co.-Conn. | Co-extraction of azadirachtin and neem oil |
| IN181845B (en) * | 1995-11-08 | 1998-10-03 | Parry E I D India Ltd | |
| CN1242734C (en) * | 2003-03-27 | 2006-02-22 | 华东中药工程集团有限公司 | Chinese medicine pot group type dynamic countercurrent extraction method |
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