CN100491328C - Method of supercritical carbon dioxide fluid separation for natural pyrethrin constituents - Google Patents
Method of supercritical carbon dioxide fluid separation for natural pyrethrin constituents Download PDFInfo
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- CN100491328C CN100491328C CNB2005100109645A CN200510010964A CN100491328C CN 100491328 C CN100491328 C CN 100491328C CN B2005100109645 A CNB2005100109645 A CN B2005100109645A CN 200510010964 A CN200510010964 A CN 200510010964A CN 100491328 C CN100491328 C CN 100491328C
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- pyrethrin
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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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- Extraction Or Liquid Replacement (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention provides a method for component 1 and component 2 of natural pyrethrin by means of supercritical CO2, which comprises dissolving the natural pyrethrin into supercritical CO2 fluid under the conditions of temperature: 30-45 deg. C, pressure: 4.5-9MPa, and carrying out four-grade analysis separation.
Description
Technical field
The present invention relates to utilize supercritical co (CO
2) fluid (Supercritical Carbon DioxideFluid) separates two components of the right pyrethrin of standing grain.
Background technology
Pyrethrin contains six effective constituents, and the pyrethrin component of saying 1 is made up of the plain I of jasmine chrysanthemum, cinerin I and pyrethrin I usually, and pyrethrin component 2 is made up of the plain II of jasmine chrysanthemum, cinerin ii and pyrethrin II.The performance effect of 2 pairs of insects of the component 1 of pyrethrin and component is different, and pyrethrin 1 mainly shows as knockdown effect, and pyrethrin 2 mainly shows as lethal effect.According to different needs, the ratio of two components of pyrethrin has very big variation when making product, and the ratio of the pyrethrin 1 in the product that has is big, and the ratio of pyrethrin 2 is big in the product that has.So two components need separating pyrethrin to a certain extent.
The ratio regular meeting of two components of pyrethrin is distinguished to some extent because of the difference of kind in the dry pyrethrum flower, but ratio is between 1:1.5 basically.The physicochemical property of six effective constituents of pyrethrin are very approaching, are difficult to separated portion with conventional separated from solvent.
Summary of the invention
The purpose of this invention is to provide a kind of supercritical CO that utilizes
2Fluid is controlled certain separation temperature and separating pressure gradient, realizes two components of natural pyrethrum isolating method to a certain degree.
The physicochemical property of component 1 and component are closely similar in the pyrethrin, but tangible difference but arranged on insecticidal mechanism, therefore are necessary two components are carried out to a certain degree separation.Supercritical CO
2The technology of fluid extraction natural pyrethrum is fairly perfect, and the yield of pyrethrin extracting can reach more than 95%.The present invention is at supercritical CO
2Study on the basis of fluid extraction natural pyrethrum,, control certain separation temperature and separating pressure gradient, just can realize separating of natural pyrethrum component 1 and component 2 according to the special dissolving power that pyrethrin showed.
Technical scheme of the present invention is: at pressure 12Mpa, under the condition of temperature 32 degree, use supercritical CO
2The fluid extraction natural pyrethrum is used supercritical CO again
2Fluid process stage trapping:
The first step: separation temperature 32～34 degree, separating pressure 9Mpa, the pyrethrin component 1 in the separating obtained medicinal extract and the ratio of pyrethrin component 2 are between 0.5～1.0;
The second stage: separation temperature 36～38 degree, separating pressure 7Mpa, the pyrethrin component 1 in the separating obtained medicinal extract and the ratio of pyrethrin component 2 are between 1.0～1.5;
The third stage: separation temperature 39～41 degree, separating pressure 6Mpa, the pyrethrin component 1 in the separating obtained medicinal extract and the ratio of pyrethrin component 2 are between 2.0～3.0;
The fourth stage: separation temperature 42～44 degree, separating pressure 4.5Mpa, the pyrethrin component 1 in the separating obtained medicinal extract and the ratio of pyrethrin component 2 are more than 3.0;
The present invention compared with prior art has following characteristics:
1, utilizes supercritical CO
2Separate pyrethrin, temperature is controlled at 30～45 degree, can guarantee that the activity of pyrethrin is not suffered a loss;
2, sepn process is fairly simple, as long as the certain temperature and pressure of control;
3, separatory medium CO
2Pyrethrin is not polluted, human body is not poisoned;
4, utilize supercritical CO
2Separate pyrethrin, can effectively solve conventional solvent and separate the problem that cann't be solved.
Embodiment
Embodiment 1
Utilize supercritical CO
2Under 12Mpa, 32 ℃ of conditions, from the pyrethrum dried flower, extract natural pyrethrum, use supercritical CO again
2Fluid separates through level Four: first step separation temperature 32～34 degree, separating pressure 9Mpa; Second stage separation temperature 36～38 degree, separating pressure 7Mpa; Third stage separation temperature 39～41 degree, separating pressure 6Mpa; Fourth stage separation temperature 42～44 degree, separating pressure 4.5Mpa; More than in the pyrethrin medicinal extract of separating at different levels, the ratio of pyrethrin component 1 and pyrethrin component 2 differs bigger, has reached separation to a certain degree.
Embodiment 2
From dry pyrethrum flower, during the refluxing extraction pyrethrin, containing pyrethrin component 1 and pyrethrin component 2 in the medicinal extract of gained with the sherwood oil equal solvent.Use supercritical CO
2Fluid process level Four is separated pyrethrin component 1 and the pyrethrin component 2 in the medicinal extract: first step separation temperature 32～34 degree, separating pressure 9Mpa; Second stage separation temperature 36～38 degree, separating pressure 7Mpa; Third stage separation temperature 39～41 degree, separating pressure 6Mpa; Fourth stage separation temperature 42～44 degree, separating pressure 4.5Mpa.Can realize pyrethrin component 1 in the solvent extraction medicinal extract and pyrethrin component 2 to a certain extent to separate through stage trapping.
Claims (1)
1. the method for a method of supercritical carbon dioxide fluid separation for pyrethrin constituents is characterized in that
Utilize supercritical CO
2The solubility property special that fluid showed to pyrethrin, in temperature is that 30～45 ℃, pressure are under the condition of 4.5～9Mpa, through stage trapping, the pyrethrin component 1 that contains the plain I of jasmine chrysanthemum, cinerin I, pyrethrin I in the pyrethrin medicinal extract is separated with the pyrethrin component 2 that contains the plain II of jasmine chrysanthemum, cinerin ii, pyrethrin II; Stage trapping wherein is: the first step: separation temperature 32～34 degree, and separating pressure 9Mpa, the pyrethrin component 1 in the separating obtained medicinal extract and the ratio of pyrethrin component 2 are between 0.5～1.0; The second stage: separation temperature 36～38 degree, separating pressure 7Mpa, the pyrethrin component 1 in the separating obtained medicinal extract and the ratio of pyrethrin component 2 are between 1.0～1.5; The third stage: separation temperature 39～41 degree, separating pressure 6Mpa, the pyrethrin component 1 in the separating obtained medicinal extract and the ratio of pyrethrin component 2 are between 2.0～3.0; The fourth stage: separation temperature 42～44 degree, separating pressure 4.5Mpa, the pyrethrin component 1 in the separating obtained medicinal extract and the ratio of pyrethrin component 2 are more than 3.0.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100109645A CN100491328C (en) | 2005-08-12 | 2005-08-12 | Method of supercritical carbon dioxide fluid separation for natural pyrethrin constituents |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100109645A CN100491328C (en) | 2005-08-12 | 2005-08-12 | Method of supercritical carbon dioxide fluid separation for natural pyrethrin constituents |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1730462A CN1730462A (en) | 2006-02-08 |
| CN100491328C true CN100491328C (en) | 2009-05-27 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100109645A Expired - Fee Related CN100491328C (en) | 2005-08-12 | 2005-08-12 | Method of supercritical carbon dioxide fluid separation for natural pyrethrin constituents |
Country Status (1)
| Country | Link |
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| CN (1) | CN100491328C (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4281171A (en) * | 1979-07-26 | 1981-07-28 | Marc Sims | Liquid carbon dioxide extraction of pyrethrins |
| CN1165811A (en) * | 1997-05-14 | 1997-11-26 | 中国科学院昆明植物研究所 | Tech. for extracting pyrethrin |
| CN1181989A (en) * | 1997-09-08 | 1998-05-20 | 孙传经 | Supercritical continuous carbon dioxide extraction technology |
| CN1421135A (en) * | 2001-11-27 | 2003-06-04 | 泸西森达生物科技开发中心 | Low temperature CO2 pyrethrin extracting process |
-
2005
- 2005-08-12 CN CNB2005100109645A patent/CN100491328C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4281171A (en) * | 1979-07-26 | 1981-07-28 | Marc Sims | Liquid carbon dioxide extraction of pyrethrins |
| CN1165811A (en) * | 1997-05-14 | 1997-11-26 | 中国科学院昆明植物研究所 | Tech. for extracting pyrethrin |
| CN1181989A (en) * | 1997-09-08 | 1998-05-20 | 孙传经 | Supercritical continuous carbon dioxide extraction technology |
| CN1421135A (en) * | 2001-11-27 | 2003-06-04 | 泸西森达生物科技开发中心 | Low temperature CO2 pyrethrin extracting process |
Non-Patent Citations (2)
| Title |
|---|
| 天然除虫菊素母药中主要成分质谱分析研究. 黄修柱.农药科学与管理，第4卷第25期. 2004 |
| 天然除虫菊素母药中主要成分质谱分析研究. 黄修柱.农药科学与管理，第4卷第25期. 2004 * |
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| Publication number | Publication date |
|---|---|
| CN1730462A (en) | 2006-02-08 |
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