CN101029276A - Fast method for continuouslly extracting nim oil and nimbin raw medicine from nim seed - Google Patents
Fast method for continuouslly extracting nim oil and nimbin raw medicine from nim seed Download PDFInfo
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- CN101029276A CN101029276A CN 200610010722 CN200610010722A CN101029276A CN 101029276 A CN101029276 A CN 101029276A CN 200610010722 CN200610010722 CN 200610010722 CN 200610010722 A CN200610010722 A CN 200610010722A CN 101029276 A CN101029276 A CN 101029276A
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Abstract
A fast method for extracting nim oil and nimbin from nim seed is carried out by leaching while extracting for solvent and agitating at normal temperature and pressure 10000-12000r/min to obtain the final product. The extractive rate can reach to 3.2-3.4wt% and oil-out rate can reach to 31.6-33.7wt%; It's fast, economic and simple and can be used for industrial production.
Description
Technical field
The present invention relates to a kind of plant extraction process, the quick continuous extraction method of especially a kind of nim oil and nimbin raw medicine.
Background technology
Nimbin is a kind of biological pesticide efficiently, is difficult for making insect to develop immunity to drugs, and does not endanger environment, and application prospect is boundless.The extractive technique of nimbin, be the core and the basic technology of the industry development of seal chinaberry, extract yield has determined economic benefit of enterprises even success or failure, and yield is by two aspect factors decisions: the one, and extract the solvent selected for use and technology and determined nimbin in the seal chinaberry to have how much to be utilized; The 2nd, extraction process and concentrate drying method have determined the rate of loss of nimbin.Nim oil is not studied and is used as major product in seal chinaberry product; just in the process of extracting nimbin; nim oil also is extracted out; it plays preferably protective effect to nimbin; simultaneously nim oil is again the raw material of manufacturing the life such as soap and industrial goods and controlling plant diseases medicine, and its purposes is also in constantly research, exploitation.At present, the extracting method of nim oil has two kinds of milling process and solvent extraction methodes.Milling process extracts nim oil can save organic solvent, but weak point is that the temperature of milling process is higher, generally can reach 80 ℃, and nimbin 2-3h under high temperature more than 65 ℃ will decompose half, and loss is serious, and this method can not adopt in actual production.Solvent method lixiviate nim oil is widely adopted in nimbin raw medicine production, and it is low that this method is extracted temperature, can guarantee that nimbin does not decompose in skimming processes, reduces the loss of nimbin, so degreasing is more satisfactory to neem seed to adopt organic solvent.
The technology of extracting nimbin from neem seed has many reports, mainly concentrates on high purity nimbin aspect but extract purpose.Also not to the utmost desirable to being applied in the low cost in the agricultural production, high efficiency nimbin extracting method.Extracting method with regard to present mainly contains: one, conventional solvent extraction; Two, supercritical fluid extraction; Three, microwave radiation auxiliary extraction; Four, intensified by ultrasonic wave extraction.Present these several extracting process are maximum with conventional solvent extraction research, and also comparatively ripe, rear three kinds of methods are at the early-stage.The process of conventional solvent extraction method is loaded down with trivial details, and the extraction yield is low, and product loss is serious, and causes easily decomposition in adding thermal reflow process, causes the nimbin extraction yield to reduce.US 5391779 reports, 1027kg kind benevolence mechanical crushing, squeezing degreasing, the rear methanol extraction of using, extract concentrate semi-solid products, add salt solution-ethyl acetate extraction, acetic acid ethyl acetate extract is through concentrating to such an extent that contain nimbin A10% semi-solid products, and this product stability is relatively poor.For improving its stability, this patent is handled 3200kg kind benevolence with similar approach again, and with the ethyl acetate enriched material with 30% hydrogen peroxide basic treatment, obtain the pressed powder of 12.8kg nimbin A31%.Process through hydrogen peroxide that rear stability increases and content is higher, but the extraction process complexity, yield only 0.12%.
Larson.R.O (U.S. Pat 4556562) report was diluted to 2000-4000ppm with alcohol extraction with extraction liquid in 1985, and accent PH is 3.6-6, adds stablizer etc., directly obtains pesticide preparation.United States Patent (USP) (US5856526) is reported with methyl alcohol or alcohol extraction, and is obtained the product that nimbin content is 10-19% through repeatedly making with extra care.The difficulty of this class technology is the pulverizing of kind of benevolence, because its fat content is higher, in crushing process, can lump, and extremely difficult pulverizing, and also extraction yield is low.
With varsol and polar solvent synergic solvent extraction nim oil and seal chinaberry active component.The characteristics of such technology are that extraction process is simple, but percentage extraction is not high.Process characteristic with water extraction is: can save a large amount of organic solvents, and the less compound of some polarity is not easy to be extracted, gained nimbin content is higher, shortcoming is because water is less to the solubleness of nimbin, cause the extraction time long, the consumption of water is big, and percentage extraction is not high.Its reason is that the part nimbin is dissolved in the nim oil in the squeezing skimming processes, and nimbin is extremely unstable in water, due to the fast decoupled.
Supercritical liquid extraction technique is the sophisticated technology that the eighties grows up.The solvent C O that supercritical fluid extraction is used
2Be a non-polar solvent, be fit to extracting apolar or the less compound of polarity, to there being certain polar nimbin solvability relatively poor, so percentage extraction is low.And this method is higher to the output investment ratio of equipment, is difficult to realize effectively suitability for industrialized production.
With microwave extracting nimbin compounds, studies show that microwave intensity, radiated time, solvent etc. are all influential to the extraction of nimbin.Nimbin in Chinese patent such as the CN02122306.8 Microwave Extraction neem kernel also is used for the extraction nimbin to microwave and reports.Microwave can strengthen infiltration and the dissolving of solvent to solute on the one hand, shorten extraction time, microwave makes the inner high-energy that produces of solvent on the one hand, causes the unstable group generation chemical reaction in the nimbin and decomposes, cause the loss of nimbin, thereby the yield of nimbin is reduced.
Ultrasonic wave is used to extract the research such as the CN03117359.4 ultrasonic wave lixiviate nimbin of nimbin, and the characteristics of this method are that the extraction time is short, and yield is high relatively.The shortcoming of supersonic method is that hyperacoustic high frequency makes extracting system produce a large amount of heats, cause nimbin to decompose, its 21 cover can be used for industrial ultrasonic extraction equipment needs 100,000 yuans approximately, installation cost is not low, also have ultrasonic wave to human body particularly the damage of hearing can not be ignored, so its application in the industrial production nimbin is still waiting to inquire into.
Summary of the invention
The present invention is directed to the extremely difficult problem of pulverizing of neem kernel, and nimbin extracts long problem consuming time and cost of equipment height, problem that the nimbin percentage extraction is low, proposed the quick continuous extraction method of a kind of nim oil and nimbin raw medicine.
The present invention finishes by following technical proposal: the quick continuous extraction method of a kind of nim oil and nimbin raw medicine is characterized in that through following process steps:
A, press neem seed: the ratio of solvent=1: 1～1.3W/V, directly in neem seed, add sherwood oil, be 10000～12000r/min in speed, under normal temperature, the normal pressure, stir extraction 1～1.5min, 1～1.5min intermittently, restir 1～1.5min, 1～1.5min intermittently, stir extraction 1～1.5min once more, so carry out intermittence and stir extraction, churning time is totally 3～4.5min, intermittent time is totally 2～3min, takes out afterwards and filters;
B, in filter cake by the ratio of 1: 1～1.3W/V, add new petroleum ether solvent, be 10000～12000r/min in speed, under normal temperature, the normal pressure, stir extraction 1～1.5min, intermittently 1～1.5min, restir 1～1.5min, intermittently 1～1.5min stirs extraction 1～1.5min once more, so carries out stirring intermittence extraction, churning time is totally 3～4.5min, intermittent time is totally 2～3min, takes out afterwards and filters, and so re-extract is 3～4 times;
C, merge each time filtrate, 40～50 ℃ of temperature, after concentrating under 150～170hpa vacuum degree condition, get nim oil, reclaim simultaneously the solvent benzinum;
D, above-mentioned filter cake dried up with nitrogen after, press seed: the ratio of solvent=1: 1～1.3W/V adds methyl alcohol wherein, is 10000～12000r/min in speed, stirs extraction 1～1.5min under normal temperature, the normal pressure, 1～1.5min intermittently, stir extraction 1～1.5min, intermittently 1～1.5min stirs extraction 1～1.5min again again, so carry out the intermittent stirring extraction, mixing time is totally 3～4.5min, and the intermittent time is totally 2～3min, takes out afterwards and filters;
E, the ratio by 1: 1～1.3W/V in filter cake add methyl alcohol, are 10000～12000r/min in speed, stir extraction 1～1.5min under normal temperature, the normal pressure, intermittently 1～1.5min stirs extraction 1～1.5min, intermittently 1～1.5min again, again stir extraction 1～1.5min, so carry out the intermittent stirring extraction, mixing time is totally 3～4.5min, and the intermittent time is totally 2～3min, take out afterwards and filter, so reprocessing is 3～4 times, merges each time filtrate, and filter cake is used in addition;
F, with E step filtrate 30～35 ℃ of temperature, under 100～120hpa vacuum tightness, being concentrated into liquid volume is 1/3～1/4 o'clock, take out to add equal-volume distilled water balance, with the long-pending ethyl acetate extraction of diploid, ethyl acetate layer is collected in coextraction 3 times again;
G, combined ethyl acetate liquid are 32～35 ℃ of temperature, under 150～160hpa vacuum, be concentrated into and do rear the taking-up, use petroleum ether degreasing 2～3 times, filter, no yellow nim oil occurs to the benzinum, collect filtrate, 40～50 ℃ of temperature, after concentrating under 150～170hpa vacuum, get nim oil, reclaim simultaneously benzinum, filter residue is yellow nimbin raw medicine after air dry.
Described sherwood oil is 60～90 ℃ of technical grades.
Described methyl alcohol, ethyl acetate are technical grade.
The present invention compared with prior art has following advantages and effect: 1, need not to carry out the seed shelling, pulverize, both solved the seal chinaberry when pulverizing because grease is many, viscosity is big, pulverizer can't be rotated, to ceaselessly clear up continually the problem of pulverizer, reduce again broken process, saved cost, and the loss of also having avoided shelling that nimbin is caused; 2, solved conventional extract by solvents nimbin long problem consuming time, conventional solvent method lixiviate generally needs more than the 24h, and extraction required for the present invention is always consuming time to be 60min, can greatly increase work efficiency; 3, equipment needed thereby is few, and expense is low, can not produce any harm to health, simple to operate, safety, and can greatly reduce production costs; 4, recovery rate is higher, almost can extract the nimbin in the neem seed fully, and take band shell seed nimbin raw medicine yield as 3.2%～3.4%, oil yield is 31.6%～33.7%; The heat that produces when 5, stirring can not produce high temperature with the very fast dispersion of flowing of liquid in the system, can not cause nimbin to decompose.
Description of drawings
Fig. 1 is the present invention's process chart.
Embodiment
Embodiment 1
A, press neem seed: the ratio of solvent=1: 1W/V, directly in neem seed, add 60 ℃ of benzinums of technical grade, be 10000r/min in speed, under normal temperature, the normal pressure, stir extraction 1.5min, intermittently 1.5min stirs 1.5min again, 1.5min intermittently, again stir extraction 1.5min, so carry out the intermittent stirring extraction, mixing time is 4.5min altogether, intermittent time is 3min altogether, takes out afterwards and filters;
B, in filter cake by 1: the ratio of 1W/V, add new petroleum ether solvent, be 12000r/min in speed, under normal temperature, the normal pressure, stir extraction 1.5min, intermittently 1.5min, stir again 1.5min, intermittently 1.5min stirs extraction 1.5min again, so carries out the intermittent stirring extraction, mixing time is 4.5min altogether, intermittent time is 3min altogether, takes out afterwards and filters, and so re-extract is 3 times;
C, merge each time filtrate, 40 ℃ of temperature, after concentrating under the 170hpa vacuum degree condition, get nim oil, reclaim simultaneously the solvent benzinum;
D, above-mentioned filter cake dried up with nitrogen after, press seed: the ratio of solvent=1: 1W/V adds industrial grade benzenemethanol wherein, is 10000r/min in speed, stirs extraction 1.5min under normal temperature, the normal pressure, 1.5min intermittently, stir extraction 1.5min, intermittently 1.5min stirs extraction 1.5min again again, so carry out the intermittent stirring extraction, mixing time is 4.5min altogether, and the intermittent time is 3min altogether, takes out afterwards and filters;
E, in filter cake by 1: the ratio of 1W/V adds industrial grade benzenemethanol, is 10000r/min in speed, and normal temperature, normal pressure stir extraction 1.5min down, 1.5min intermittently, restir extraction 1.5min, intermittently 1.5min, stir extraction 1.5min once more, so carry out stirring extraction intermittence, churning time is 4.5min altogether, and the intermittent time is 3min altogether, take out afterwards and filter, so re-treatment is 3 times, merges each time filtrate, and filter cake is used in addition;
F, with E step filtrate 30 ℃ of temperature, under the 120hpa vacuum tightness, being concentrated into liquid volume is 1/3 o'clock, take out to add equal-volume distilled water balance, with the long-pending ethyl acetate extraction of diploid, ethyl acetate layer is collected in coextraction 3 times again;
G, combined ethyl acetate liquid are 32 ℃ of temperature, under the 160hpa vacuum, be concentrated into and do rear the taking-up, use petroleum ether degreasing 2 times, filter, no yellow nim oil occurs to the benzinum, collect filtrate, 40 ℃ of temperature, after concentrating under the 170hpa vacuum, get nim oil, reclaim simultaneously benzinum, filter residue is yellow nimbin raw medicine after air dry.
Embodiment 2
A, press neem seed: the ratio of solvent=1: 1.3W/V, directly in neem seed, add 90 ℃ of benzinums of technical grade, be 12000r/min in speed, under normal temperature, the normal pressure, stir extraction 1min, intermittently 1min stirs 1min again, 1min intermittently, again stir extraction 1min, so carry out the intermittent stirring extraction, mixing time is 3min altogether, intermittent time is 2min altogether, takes out afterwards and filters;
B, in filter cake by 1: the ratio of 1.3W/V, add new petroleum ether solvent, be 12000r/min in speed, under normal temperature, the normal pressure, stir extraction 1min, intermittently 1min, stir again 1min, intermittently 1min stirs extraction 1min again, so carries out the intermittent stirring extraction, mixing time is 3min altogether, intermittent time is 2min altogether, takes out afterwards and filters, and so re-extract is 4 times;
C, merge each time filtrate, 50 ℃ of temperature, after concentrating under the 150hpa vacuum degree condition, get nim oil, reclaim simultaneously the solvent benzinum;
D, above-mentioned filter cake dried up with nitrogen after, press seed: the ratio of solvent=1: 1.3W/V adds industrial grade benzenemethanol wherein, is 12000r/min in speed, stirs extraction 1min under normal temperature, the normal pressure, 1min intermittently, stir extraction 1min, intermittently 1min stirs extraction 1min again again, so carry out the intermittent stirring extraction, mixing time is 3min altogether, and the intermittent time is 2min altogether, takes out afterwards and filters;
E, in filter cake by 1: the ratio of 1.3W/V adds methyl alcohol, is 12000r/min in speed, and normal temperature, normal pressure stir extraction 1min down, 1min intermittently, restir extraction 1min, intermittently 1min, stir extraction 1min once more, so carry out stirring extraction intermittence, churning time is 3min altogether, and the intermittent time is 2min altogether, take out afterwards and filter, so re-treatment is 4 times, merges each time filtrate, and filter cake is used in addition;
F, with E step filtrate 30 ℃ of temperature, under the 120hpa vacuum tightness, being concentrated into liquid volume is 1/4 o'clock, take out to add equal-volume distilled water balance, with the long-pending technical grade ethyl acetate extraction of diploid, ethyl acetate layer is collected in coextraction 3 times again;
G, combined ethyl acetate liquid are 35 ℃ of temperature, under the 150hpa vacuum, be concentrated into and do rear the taking-up, use petroleum ether degreasing 3 times, filter, no yellow nim oil occurs to the benzinum, collect filtrate, 50 ℃ of temperature, after concentrating under the 150hpa vacuum, get nim oil, reclaim simultaneously benzinum, filter residue is yellow nimbin raw medicine after air dry.
Claims (3)
1, the quick continuous extraction method of nim oil and nimbin raw medicine in a kind of neem seed is characterized in that through following process steps:
A, press neem seed: the ratio of solvent=1: 1～1.3W/V, directly in neem seed, add sherwood oil, be 10000～12000r/min in speed, under normal temperature, the normal pressure, stir extraction 1～1.5min, 1～1.5min intermittently, restir 1～1.5min, 1～1.5min intermittently, stir extraction 1～1.5min once more, so carry out intermittence and stir extraction, churning time is totally 3～4.5min, intermittent time is totally 2～3min, takes out afterwards and filters;
B, in filter cake by the ratio of 1: 1～1.3W/V, add new petroleum ether solvent, be 10000～12000r/min in speed, under normal temperature, the normal pressure, stir extraction 1～1.5min, intermittently 1～1.5min, restir 1～1.5min, intermittently 1～1.5min stirs extraction 1～1.5min once more, so carries out stirring intermittence extraction, churning time is totally 3～4.5min, intermittent time is totally 2～3min, takes out afterwards and filters, and so re-extract is 3～4 times;
C, merge each time filtrate, 40～50 ℃ of temperature, after concentrating under 150～170hpa vacuum degree condition, get nim oil, reclaim simultaneously the solvent benzinum;
D, above-mentioned filter cake dried up with nitrogen after, press seed: the ratio of solvent=1: 1～1.3W/V adds methyl alcohol wherein, is 10000～12000r/min in speed, stirs extraction 1～1.5min under normal temperature, the normal pressure, 1～1.5min intermittently, stir extraction 1～1.5min, intermittently 1～1.5min stirs extraction 1～1.5min again again, so carry out the intermittent stirring extraction, mixing time is totally 3～4.5min, and the intermittent time is totally 2～3min, takes out afterwards and filters;
E, the ratio by 1: 1～1.3W/V in filter cake add methyl alcohol, are 10000～12000r/min in speed, stir extraction 1～1.5min under normal temperature, the normal pressure, intermittently 1～1.5min stirs extraction 1～1.5min, intermittently 1～1.5min again, again stir extraction 1～1.5min, so carry out the intermittent stirring extraction, mixing time is totally 3～4.5min, and the intermittent time is totally 2～3min, take out afterwards and filter, so reprocessing is 3～4 times, merges each time filtrate, and filter cake is used in addition;
F, with E step filtrate 30～35 ℃ of temperature, under 100～120hpa vacuum tightness, being concentrated into liquid volume is 1/3～1/4 o'clock, take out to add equal-volume distilled water balance, with the long-pending ethyl acetate extraction of diploid, ethyl acetate layer is collected in coextraction 3 times again;
G, combined ethyl acetate liquid are 32～35 ℃ of temperature, under 150～160hpa vacuum, be concentrated into and do rear the taking-up, use petroleum ether degreasing 2～3 times, filter, no yellow nim oil occurs to the benzinum, collect filtrate, 40～50 ℃ of temperature, after concentrating under 150～170hpa vacuum, get nim oil, reclaim simultaneously benzinum, filter residue is yellow nimbin raw medicine after air dry.
2, extracting method according to claim 1 is characterized in that described sherwood oil is 60～90 ℃ of technical grades.
3, extracting method according to claim 1 is characterized in that described methyl alcohol, ethyl acetate are technical grade.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101440099B (en) * | 2008-12-31 | 2010-08-18 | 牛赡光 | Industrial large scale extracting method for nimbin dry powder |
| 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 |
| CN107432287A (en) * | 2017-06-26 | 2017-12-05 | 浦江县昂宝生物技术有限公司 | Bajiao banana vegetable insecticide and preparation method thereof |
| CN107522721A (en) * | 2017-08-28 | 2017-12-29 | 云南大学 | A kind of technique of efficiently purification nimbin raw medicine |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4943434A (en) * | 1987-10-06 | 1990-07-24 | Rohm And Haas Company | Insecticidal hydrogenated neem extracts |
| US5397571A (en) * | 1993-03-25 | 1995-03-14 | W. R. Grace & Co.-Conn. | Co-extraction of azadirachtin and neem oil |
| IN179008B (en) * | 1995-07-17 | 1997-08-09 | Dalmia Ct For Biotechnology | |
| CN1049091C (en) * | 1996-09-06 | 2000-02-09 | 中国科学院昆明植物研究所 | Preparation technology for nimbin |
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2006
- 2006-03-03 CN CN2006100107220A patent/CN101029276B/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101440099B (en) * | 2008-12-31 | 2010-08-18 | 牛赡光 | Industrial large scale extracting method for nimbin dry powder |
| 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 |
| CN107432287A (en) * | 2017-06-26 | 2017-12-05 | 浦江县昂宝生物技术有限公司 | Bajiao banana vegetable insecticide and preparation method thereof |
| CN107522721A (en) * | 2017-08-28 | 2017-12-29 | 云南大学 | A kind of technique of efficiently purification nimbin raw medicine |
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