CN101029276B - 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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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 main products in seal chinaberry product; just in the process of extracting nimbin; nim oil also is extracted out; it plays the better protecting effect to nimbin; simultaneously nim oil is again a raw material of manufacturing 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 processes.Milling process extracts nim oil can save organic solvent, but weak point is that the temperature of milling process than higher, generally can reach 80 ℃, and nimbin 2-3h under high temperature more than 65 ℃ will decompose half, 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 desirable not to the utmost to being applied in the low cost in the agriculture 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, back 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 decomposition easily in the reflux process, causes the nimbin percentage extraction to reduce.The US5391779 report, 1027kg kind benevolence mechanical disintegration, squeezing degreasing, methanol extraction use in the back, extraction liquid concentrated semi-solid product, add salt solution-ethyl acetate extraction, acetic acid ethyl acetate extract is through concentrating to such an extent that contain nimbin A10% semi-solid product, 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%.Handle 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 transferring PH is 3.6-6, adds stablizer etc., directly obtains pesticide preparation.United States Patent (USP) (US5856526) report is with methyl alcohol or alcohol extraction, and is 10-19% product through the refining nimbin content that obtains repeatedly.The difficulty of this class technology is the pulverizing of kind of benevolence, and is higher because of its fat content, in crushing process, can lump, and extremely difficult pulverizing, and also percentage extraction is low.
With varsol and polar solvent synergistic extraction nim oil and seal chinaberry activeconstituents.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 decomposing fast.
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 to extract 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, nim oil, reclaim the solvent sherwood oil simultaneously;
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, and normal temperature, normal pressure stir extraction 1～1.5min down, 1～1.5min intermittently, restir extraction 1～1.5min, intermittently 1～1.5min stirs extraction 1～1.5min once more, so carry out stirring intermittence extraction, churning 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, and normal temperature, normal pressure stir extraction 1～1.5min down, 1～1.5min intermittently, restir extraction 1～1.5min, intermittently 1～1.5min, stir extraction 1～1.5min once more, so carry out intermittence and stir extraction, churning time is totally 3～4.5min, and the intermittent time is totally 2～3min, take out afterwards and filter, so re-treatment 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 tightness, be concentrated into and do the back taking-up, use petroleum ether degreasing 2～3 times, filter, no yellow nim oil occurs to the sherwood oil, collect filtrate, 40～50 ℃ of temperature, after concentrating under 150～170hpa vacuum tightness, get nim oil, reclaim sherwood oil simultaneously, filter residue is yellow nimbin raw medicine after seasoning.
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 advantage 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 the problem of pulverizer continually, reduce broken process again, saved cost, and the loss of also having avoided shelling that nimbin is caused; 2, solved conventional solvent method and extracted 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 increase work efficiency greatly; 3, required equipment is few, and expense is low, can not produce any harm to HUMAN HEALTH, simple to operate, safety, and can reduce production costs greatly; 4, extraction yield is higher, almost can extract the nimbin in the neem seed fully, and be 3.2%～3.4% in band shell seed nimbin raw medicine yield, 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 flow sheet.
Embodiment
Embodiment 1
A, press neem seed: the ratio of solvent=1: 1W/V, directly in neem seed, add 60 ℃ of sherwood oils of technical grade, be 10000r/min in speed, under normal temperature, the normal pressure, stir extraction 1.5min, 1.5min intermittently, restir 1.5min, 1.5min intermittently, stir extraction 1.5min once more, so carry out stirring extraction intermittence, churning 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, restir 1.5min, intermittently 1.5min stirs extraction 1.5min once more, so carries out stirring intermittence extraction, churning 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, nim oil, reclaim the solvent sherwood oil simultaneously;
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, and normal temperature, normal pressure stir extraction 1.5min down, 1.5min intermittently, restir extraction 1.5min, intermittently 1.5min stirs extraction 1.5min once more, so carry out stirring intermittence extraction, churning 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 tightness, be concentrated into and do the back taking-up, use petroleum ether degreasing 2 times, filter, no yellow nim oil occurs to the sherwood oil, collect filtrate, 40 ℃ of temperature, after concentrating under the 170hpa vacuum tightness, get nim oil, reclaim sherwood oil simultaneously, filter residue is yellow nimbin raw medicine after seasoning.
Embodiment 2
A, press neem seed: the ratio of solvent=1: 1.3W/V, directly in neem seed, add 90 ℃ of sherwood oils of technical grade, be 12000r/min in speed, under normal temperature, the normal pressure, stir extraction 1min, 1min intermittently, restir 1min, 1min intermittently, stir extraction 1min once more, so carry out stirring extraction intermittence, churning 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, restir 1min, intermittently 1min stirs extraction 1min once more, so carries out stirring intermittence extraction, churning 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, nim oil, reclaim the solvent sherwood oil simultaneously;
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, and normal temperature, normal pressure stir extraction 1min down, 1min intermittently, restir extraction 1min, intermittently 1min stirs extraction 1min once more, so carry out stirring intermittence extraction, churning 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 tightness, be concentrated into and do the back taking-up, use petroleum ether degreasing 3 times, filter, no yellow nim oil occurs to the sherwood oil, collect filtrate, 50 ℃ of temperature, after concentrating under the 150hpa vacuum tightness, get nim oil, reclaim sherwood oil simultaneously, filter residue is yellow nimbin raw medicine after seasoning.
Claims (3)
1. the quick continuous extraction method of nim oil and nimbin raw medicine in the 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, nim oil, reclaim the solvent sherwood oil simultaneously;
D, above-mentioned filter cake dried up with nitrogen after, press neem seed: the ratio of solvent=1: 1～1.3W/V adds methyl alcohol wherein, is 10000～12000r/min in speed, and normal temperature, normal pressure stir extraction 1～1.5min down, 1～1.5min intermittently, restir extraction 1～1.5min, intermittently 1～1.5min stirs extraction 1～1.5min once more, so carry out stirring intermittence extraction, churning 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, and normal temperature, normal pressure stir extraction 1～1.5min down, 1～1.5min intermittently, restir extraction 1～1.5mi n, intermittently 1～1.5min, stir extraction 1～1.5min once more, so carry out intermittence and stir extraction, churning time is totally 3～4.5min, and the intermittent time is totally 2～3min, take out afterwards and filter, so re-treatment 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 tightness, be concentrated into and do the back taking-up, use petroleum ether degreasing 2～3 times, filter, no yellow nim oil occurs to the sherwood oil, collect filtrate, 40～50 ℃ of temperature, after concentrating under 150～170hpa vacuum tightness, get nim oil, reclaim sherwood oil simultaneously, filter residue is yellow nimbin raw medicine after seasoning.
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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| EP4385326A1 (en) * | 2022-12-15 | 2024-06-19 | Kimitec Biogorup | Biopesticide composition and method for controlling and treating broad spectrum of pests and diseases in plants |
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| CN101440099B (en) * | 2008-12-31 | 2010-08-18 | 牛赡光 | Industrial large scale extracting method for nimbin dry powder |
| 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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