CN1246284C - Method for extracting pyrethrin from pyrethrum flower - Google Patents
Method for extracting pyrethrin from pyrethrum flower Download PDFInfo
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- CN1246284C CN1246284C CN 200410011076 CN200410011076A CN1246284C CN 1246284 C CN1246284 C CN 1246284C CN 200410011076 CN200410011076 CN 200410011076 CN 200410011076 A CN200410011076 A CN 200410011076A CN 1246284 C CN1246284 C CN 1246284C
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- pyrethrin
- pressure
- pyrethrum flowers
- lixiviate
- film bag
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Abstract
The present invention relates to a method for extracting bioresmethrin from pyrethrum flowers, which comprises the following technological steps: a. after pyrethrum flowers is pulverized by a sieve with 40 meshes, the pyrethrum flowers are put in a polythene film bag, and sufficient hexane for immersing the materials is added; b. after the polythene film bag is sealed, the polythene film bag is put in a high-pressure container, 50 to 600MPa of pressure is applied at normal temperature for lixiviation, and the pressure maintaining time is from 1 to 30 min; c. after the pressure is relieved, extract liquid is filtered, and filtration residues are removed; d. filter liquid is added to concentration equipment to be concentrated so as to obtain bioresmethrin extract. The method of the present invention has the advantages of high extraction rate, low energy consumption and little equipment investment.
Description
Technical field
The present invention relates to a kind of method of from pyrethrum flowers, extracting pyrethrin.
Background technology
The method of producing natural pyrethrin at home is to adopt supercritical carbon dioxide extraction method and subcritical fluid extraction tentatively to extract, crude extract again separation and purification and product, this has become domestic main flow production method.And external main stream approach is that the industrial normal hexane of employing is that solvent carries out slightly carrying of dried flower, gets product then through separation and purification.Used equipment is specific equipment, and investment is big, its technology leaching process time is long, and energy consumption is higher.There is the shortcoming that investment is big, the technology leaching process time is long, energy consumption is high equally in two kinds of methods of present domestic employing.
Summary of the invention
The objective of the invention is for overcoming the shortcoming that present pyrethrin extracting method exists, proposes a kind ofly to save time, the method for energy-conservation, extraction yield is high from pyrethrum flowers extraction pyrethrin.
The present invention extracts the method for pyrethrin from pyrethrum flowers, processing step is as follows:
A. put into polythene film bag after pyrethrum flowers being pulverized 40 mesh sieves, added the normal hexane of enough this materials of submergence,
B. put into high pressure vessel after polythene film bag being sealed, apply the lixiviate of 50～600MPa pressure at normal temperatures, the dwell time is 1～30min,
C. after the release with extracting liquid filtering, remove filter residue,
D. filtrate is joined in the thickening equipment concentrate after, promptly obtain pyrethrin medicinal extract.
Be further to improve extraction yield, the lixiviate of also can repeatedly exerting pressure repeatedly, the filter residue after the lixiviate of soon last time exerting pressure is with the lixiviate of exerting pressure once more of same process condition.Experimental results show that and when extraction time is 1～3 time, pyrethrin all can be extracted.
Pyrethrum flowers is through after pulverizing, and its surface-area increases, and is big with the contact area of solvent, can accelerate the extraction rate of effective constituent, if can increase the isolating difficulty of extracting liquid filtering but granularity is too little, can cross 40 mesh sieves after general the pulverizing and get final product.
The inventive method is compared with the subcritical fluid extraction method with supercritical carbon dioxide extraction method, has following advantage:
1. facility investment is less, only is equivalent to the former 1/10, the latter's 1/4.
2. the extraction yield of high pressure extract method (yield) height.Be supercritical carbon dioxide extraction and two kinds of extracting method of subcritical fluid extraction 1.8 times approximately.
3. the high pressure extract time is short, productive rate is high, is 1% of supercritical carbon dioxide extraction method.
4. energy-conservation.High pressure extract is consumed energy when rising pressure only, and each pressure rising time less than 1 minute.Supercritical carbon dioxide method for extracting and subcritical fluid extraction method then in whole process of production, consumes energy ceaselessly.
The present invention utilizes the polarity characteristics of pyrethrin compounds, and selecting industrial normal hexane is solvent, utilizes the infiltration of solvent under the high pressure and the dissolution equilibrium of solute to carry out character faster, uses pressure technique to extract pyrethrin from pyrethrum flowers.
Embodiment
Embodiment 1
(1) pyrethrum flowers is pulverized, is crossed 40 mesh sieves,
(2) 3 parts of 10g pyrethrum flowers powder are put into 3 polythene film bags respectively, each adds the industrial normal hexane of 50ml,
(3) polythene film bag is sealed put into high pressure vessel, at normal temperatures, apply 50MPa pressure and carry out lixiviate, the dwell time is respectively 1,5 and 30min,
(4) after extraction is finished,, remove filter residue with extracting liquid filtering,
(5) filtrate is placed in the thickening equipment concentrate after, promptly obtain pyrethrin medicinal extract.With gas chromatographic detection get the pyrethrin extraction yield such as following table listed:
| Sequence number | Extraction time (min) | Extraction yield (%) |
| 1 | 1 | 1.80 |
| 2 | 5 | 1.83 |
| 3 | 30 | 1.82 |
Embodiment 2
(1) pyrethrum flowers is pulverized, is crossed 40 mesh sieves,
(2) 10g pyrethrum flowers powder is put into polythene film bag, adds the industrial normal hexane of 50ml,
(3) polythene film bag is sealed put into high pressure vessel, apply 50MPa pressure at normal temperatures and carry out lixiviate, the dwell time is 5min,
(4) after extraction is finished, with extracting liquid filtering,
(5) filtrate is placed in the thickening equipment concentrate after, promptly obtain pyrethrin medicinal extract.Use gas chromatographic detection, the pyrethrin extraction yield is 1.83%.
Filter residue after said extracted liquid filtered is exerted pressure after the lixiviate 2 times more repeatedly with the same process condition, and the whole extracting solutions that obtained are through gas chromatographic detection, and the pyrethrin extraction yield is 1.84%.
Embodiment 3
(1) pyrethrum flowers is pulverized, is crossed 40 mesh sieves,
(2) 3 parts of 10g pyrethrum flowers powder are put into 3 polythene film bags respectively, each adds the industrial normal hexane of 50ml,
(3) polythene film bag sealed put into high pressure vessel, apply respectively at normal temperatures 50,300 and 600MPa pressure carry out lixiviate, the dwell time is 5min,
(4) after extraction is finished,, remove filter residue with extracting liquid filtering,
(5) 3 parts of filtrates are inserted respectively in the thickening equipment concentrate after, the pyrethrin medicinal extract that promptly obtains.Listed with gas chromatographic detection pyrethrin extraction yield such as following table:
| Sequence number | Extract pressure (MPa) | Extraction yield (%) |
| 1 | 50 | 1.83 |
| 2 | 300 | 1.85 |
| 3 | 600 | 1.88 |
Embodiment 4
(1) pyrethrum flowers is pulverized, is crossed 40 mesh sieves,
(2) 3 parts of 10g pyrethrum flowers powder are put into 3 polythene film bags respectively, add 50,200 respectively, the industrial normal hexane of 500ml,
(3) polythene film bag is sealed put into high pressure vessel, apply 50MPa pressure at normal temperatures and carry out lixiviate, the dwell time is 5min,
(4) after extraction is finished,, remove filter residue with extracting liquid filtering,
(5) 3 parts of filtrates are inserted respectively in the thickening equipment concentrate after, promptly obtain pyrethrin medicinal extract.Listed with gas chromatographic detection pyrethrin extraction yield such as following table:
| Sequence number | Add quantity of solvent (ml) | Extraction yield (%) |
| 1 | 50 | 1.83 |
| 2 | 200 | 1.87 |
| 3 | 500 | 1.89 |
Claims (2)
1. method of extracting pyrethrin from pyrethrum flowers is characterized in that processing step is as follows:
A. put into polythene film bag after pyrethrum flowers being pulverized 40 mesh sieves, added the normal hexane of enough this materials of submergence,
B. put into high pressure vessel after polythene film bag being sealed, apply the lixiviate of 50～600MPa pressure at normal temperatures, the dwell time is 1～30min,
C. after the release with extracting liquid filtering, remove filter residue,
D. filtrate is joined in the thickening equipment concentrate after, promptly obtain pyrethrin medicinal extract.
2. the method for extracting pyrethrin from pyrethrum flowers according to claim 1, the lixiviate that it is characterized in that repeatedly exerting pressure repeatedly to be improving extraction yield, and the filter residue after the lixiviate of soon last time exerting pressure is with the lixiviate of exerting pressure once more of same process condition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410011076 CN1246284C (en) | 2004-09-03 | 2004-09-03 | Method for extracting pyrethrin from pyrethrum flower |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410011076 CN1246284C (en) | 2004-09-03 | 2004-09-03 | Method for extracting pyrethrin from pyrethrum flower |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1616395A CN1616395A (en) | 2005-05-18 |
| CN1246284C true CN1246284C (en) | 2006-03-22 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410011076 Expired - Fee Related CN1246284C (en) | 2004-09-03 | 2004-09-03 | Method for extracting pyrethrin from pyrethrum flower |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1246284C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101907562A (en) * | 2010-06-28 | 2010-12-08 | 华中农业大学 | Quick measuring method of pyrethrin |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100418423C (en) * | 2006-08-11 | 2008-09-17 | 云南大学 | Active compound extracted from pyrethrum and use thereof |
| CN102715195A (en) * | 2012-07-09 | 2012-10-10 | 唐桂华 | Preparation method of pesticide for greening plants in public parks, streets and residential districts |
| CN103651592B (en) * | 2013-12-27 | 2016-02-17 | 成都新朝阳作物科学有限公司 | Containing composition pesticide and the preparation method and application of Dalmatian chrysanthemum and extract from Lantana camara |
| CN106748775B (en) * | 2016-11-29 | 2019-08-06 | 广西大学 | A kind of method of quick production pyrethrins |
-
2004
- 2004-09-03 CN CN 200410011076 patent/CN1246284C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101907562A (en) * | 2010-06-28 | 2010-12-08 | 华中农业大学 | Quick measuring method of pyrethrin |
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| Publication number | Publication date |
|---|---|
| CN1616395A (en) | 2005-05-18 |
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