CN1548206A - Method of using entrainer to raise efficiency of supercritical CO2 extraction - Google Patents
Method of using entrainer to raise efficiency of supercritical CO2 extraction Download PDFInfo
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- CN1548206A CN1548206A CNA031179428A CN03117942A CN1548206A CN 1548206 A CN1548206 A CN 1548206A CN A031179428 A CNA031179428 A CN A031179428A CN 03117942 A CN03117942 A CN 03117942A CN 1548206 A CN1548206 A CN 1548206A
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Abstract
The present invention is method of using entrainer to raise efficiency of extracting effective plant components through supercritical CO2 extraction. The technological feature is that crushed plant material is mixed homogeneously with proper amount of entrainer before static soaking inside extracting reactor at certain temperature and pressure and subsequent dynamic extraction alternately in two or multiple reactors. The said method is suitable for extracting weak polarity and medium polarity effective components from plant material, and has the advantages of lower extraction pressure and temperature, small amount of entrainer consumption, no need of entrainer pump and similar equipment, high extraction rate, short time and low cost.
Description
The present invention relates to a kind of method of supercritical carbon dioxide extracting active ingredients of plants, particularly is a kind of method of using entrainer to improve supercritical carbon dioxide extracting active ingredients of plants efficient.
Supercritical carbon dioxide extraction method is a kind of environmental type new technology, and this technology is to utilize carbon dioxide extraction function of similar organic solvent character under supercriticality to carry out material extracts active ingredients and a kind of advanced technology of separating.Supercritical carbon dioxide is meant that pressure and temperature is at critical point (7.38MPa, 31.3 ℃) on a kind of special CO 2 fluid, it has the special nature near gas viscosity (diffusivity is stronger) and fluid density (dissolubility is stronger), nonpolar and low pole composition had dissolubility preferably, therefore and solubility can change with pressure, variation of temperature, can pressure and temperature extract by regulating, the active ingredient in the separating plant.Because extraction temperature is low, and extracts in the carbon dioxide of inertia, has avoided pyrolytic and oxidation, supercritical carbon dioxide extraction method is very suitable for extracting the thermal sensitivity natural products of plant class.
Supercritical CO
2Abstraction technique has following several outstanding advantage:
1. use supercritical CO
2The product that extracts does not have dissolvent residual.
2. because extraction temperature is low, help the bioactive reservation of heat-sensitive substance.
3. supercritical CO
2Extracting power depend on the density of fluid, therefore can be at an easy rate change by extraction conditions (pressure, temperature) realize selective extraction.
4. supercritical CO
2Therefore penetration is strong, than shortening greatly with commonsense method extraction time.
5.CO
2Odorless, stable chemical performance, and CO
2Can recycle, so CO
2Use can not pollute this technology compliance with environmental protection requirements to environment; Because CO
2Be inertia, extraction process has been avoided the oxidation of target product.
6.CO
2Cheap and easy to get, nonflammable explosive, extract safety than organic solvent.
7.CO
2Very easy with separating between the product, save the energy.
Owing to have these outstanding advantages, this technology is being widely used when fields such as food substitutes, health products, medicine, spices, especially has bright prospects especially in The biological resources development and utilization, effective components of Chinese medicinal extraction with aspect making with extra care.
Owing to having the characteristics that are better than traditional extraction and separation technology, supercritical carbon dioxide extraction method is subjected to extensive concern.Extracting from plant, separating effective medicinal ingredient is present supercritical CO
2The field that fluid extraction technology is used morely in pharmaceuticals industry.
Floristics is various, complicated component, the nature difference of various compositions is very big, from extracting and refining angle, by the big I of lipophilicity (polarity) plant component is divided into following a few class: strong lipophilicity (nonpolarity) material, lipophilicity (low pole) material, weak lipophilicity (Semi-polarity) material, hydrophily (strong polarity) material, supercritical CO
2Be suitable for extracting apolar to semipolar effective ingredients in plant.Supercritical CO
2Character be similar to non-polar solven, therefore for the strong lipophilic composition in the plant good effect of extracting is arranged, and the application of succeeding already.Lipophilicity in the plant and weak lipophilic composition have aglycon, alkaloid, resin, aldehyde, ketone, alcohol, quinone, phenol, organic acid and some glycoside, and these compositions are the important component that have the medicinal organism activity in the plant, think supercritical CO in the past
2Be difficult to this constituents of extraction, by increasing substantially extracting pressure or adding the method for entrainer, solved this difficult problem preferably now, concrete way is: 1, extracting pressure is improved, generally reaches more than the 40MPa, make target component at CO
2In solubility improve; 2, pass through entrainer pump and blender at supercritical CO
2The middle solvent (being so-called entrainer) that adds with certain polarity changes CO
2Fluid polarity environment, thus target component improved at CO
2Solubility in the fluid.Improve extracting pressure the cost of investment of equipment and extraction cost will be increased, thereby generally use the method for entrainer need dispose entrainer pump and relevant device increase cost of investment.
At present at supercritical CO
2Adding the method for entrainer in the fluid, is at CO
2Mix by a certain percentage with entrainer before entering extraction kettle, enter again and carry out dynamic extraction in the extraction kettle.This method is because CO
2With entrainer be that dynamic flow is crossed material, fluid can not fully and equably contact with material, reaching capacity far away promptly flows away, so consume to carry dosage secretly more, the extraction time is longer relatively, and the method is prone to channel in extraction process, causes local materials abstraction incomplete.
The present invention proposes a kind of use entrainer and improves supercritical CO
2The method of extraction effective ingredients in plant efficient, this method has following outstanding feature: 1, need not entrainer pump and relevant device, reduced equipment investment.2, entrainer is evenly mixed with material before feeding intake, the entrainer consumption few (with the weight ratio of material only be 0.3～1.5: 1), the recovery rate height.3, employed extracting pressure is lower, generally is not higher than 25MPa, thereby has reduced the requirement to equipment, reduces investment, and employed temperature is lower, generally at 30～60 ℃.4, adopt static immersing and two still or many stills juxtaposition to extract, save time, economize gas (CO
2), reduce labor intensity, enhance productivity.
Figure of description is that the present invention uses entrainer to improve supercritical CO
2The process chart of extraction effective ingredients in plant efficient.
The invention process step is: take ethanol, methyl alcohol, acetone or ethyl acetate etc. with the solvent of certain polarity as Entrainer is pulverized rear and an amount of entrainer with plant material and is mixed, and drops among the extraction kettle I6 dioxy Change carbon and emit from gas cylinder 1, enter storage tank 3 through refrigerator 2, by hot water circulation heated extraction kettle I6, separation Still I8 starts plunger displacement pump 4 carbon dioxide heater via 5 in the storage tank 3 is squeezed into extraction kettle to predetermined temperature Among the I6, to predetermined pressure, termination of pumping, static immersing started after a period of time under predetermined pressure, temperature Plunger displacement pump 4 extracts solution to go out, and separates in separation reactor I 8, and carbon dioxide is through separation reactor I I10, refrigerator 2 To storage tank 3, recycle, solution picks out from separation reactor I 8 bottom valve 9, obtains order through corresponding post processing The mark product, entrainer is recyclable. Before extraction kettle I6 carries out dynamic extraction, with the extraction kettle that has fed intake II7 is raised to and carries out static immersing under predetermined pressure, the temperature, and two stills or many stills juxtaposition extract.
The present invention is applicable to active ingredients such as extracting aglycon, alkaloid, resin, aldehyde, ketone, alcohol, quinone, phenol, organic acid and some glycoside from plant material.Now illustrate as follows
The 10kg moutan bark is pulverized the back mix with 95% edible ethanol, 3～5kg, drop among the extraction kettle I, extraction temperature rises to 35～55 ℃, squeezes into CO
2Extraction kettle pressure is risen to 9～18MPa, termination of pumping, static immersing 20～40 minutes carried out dynamic extraction 20 minutes again, picked out solution from the separation reactor I bottom valve, obtained Paeonol through concentrated, washing, drying, and purity is 80～95%, and recovery rate is greater than 85%; Before extraction kettle I carries out dynamic extraction, the extraction kettle II that has fed intake is raised to carries out static extracting under predetermined pressure, the temperature, two stills hocket.
The neem kernel of 10kg after oil expression pulverized the back mix with 8～10kg95% edible ethanol, drop among the extraction kettle I, extraction temperature rises to 35～55 ℃, squeezes into CO
2Extraction kettle pressure is risen to 9～25MPa, termination of pumping, static immersing 20～50 minutes, carried out dynamic extraction again 20 minutes, and picked out solution, obtain mimbin extract through concentrated, drying from the separation reactor I bottom valve, nimbin content is 10～20%, and recovery rate is greater than 85%; Before extraction kettle I carries out dynamic extraction, the extraction kettle II that has fed intake is raised to carries out static extracting under predetermined pressure, the temperature, two stills hocket.
Claims (3)
1, a kind of method of using entrainer to improve supercritical carbon dioxide extracting effective ingredients in plant efficient, it is characterized in that before the extraction material drops into extraction kettle, the mixing of materials of entrainer and pulverizing is even, entrainer is the solvent with certain polarity, as ethanol, methyl alcohol, acetone, ethyl acetate etc.
2, method according to claim 1, static immersing is carried out with material earlier in the back that it is characterized in that feeding intake under certain pressure, temperature, and then carries out dynamic extraction, and extracting pressure is 8～25MPa, and extraction temperature is 30～60 ℃.
3, according to claim 1 and 2 described methods, it is characterized in that adopting two stills or many stills juxtaposition to extract, promptly before first extraction kettle carries out dynamic extraction, second extraction kettle that has fed intake is raised to carries out static immersing under predetermined pressure, the temperature, two stills or many stills hocket.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA031179428A CN1548206A (en) | 2003-05-23 | 2003-05-23 | Method of using entrainer to raise efficiency of supercritical CO2 extraction |
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|---|---|---|---|
| CNA031179428A CN1548206A (en) | 2003-05-23 | 2003-05-23 | Method of using entrainer to raise efficiency of supercritical CO2 extraction |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101905091A (en) * | 2010-07-12 | 2010-12-08 | 新疆大学 | Equipment and method for extracting biologically active ingredients from subcritical fluid |
| CN101380342B (en) * | 2007-09-06 | 2011-07-06 | 上海医药工业研究院 | Total alkaloide extraction method from mixture of angelica and ligusticum wallichii rhizome by supercritical carbon dioxide |
| CN102210943A (en) * | 2011-06-20 | 2011-10-12 | 东莞广州中医药大学中医药数理工程研究院 | Cell-wall-breaking low-temperature extraction method and device with assistance of CO2 |
| US9132363B2 (en) | 2012-11-20 | 2015-09-15 | Apeks Llc | Extraction system |
| US9908062B2 (en) | 2012-11-20 | 2018-03-06 | Andrew Paul Joseph | Extraction apparatus and method |
| CN107760058A (en) * | 2017-11-30 | 2018-03-06 | 广西南宁栩兮科技有限公司 | The extracting method of haematochrome in a kind of rambutan shell |
| CN108938682A (en) * | 2018-10-09 | 2018-12-07 | 淮安安莱生物科技有限公司 | A method of extracting cypress acid and cedar wood alcohol from high mountain cypress |
| CN109157545A (en) * | 2018-10-09 | 2019-01-08 | 淮安安莱生物科技有限公司 | A method of extracting shellac acid and jalaric acid from shellac |
| CN113000588A (en) * | 2021-03-16 | 2021-06-22 | 中国科学院工程热物理研究所 | Mobile supercritical fluid soil remediation system and remediation device |
-
2003
- 2003-05-23 CN CNA031179428A patent/CN1548206A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101380342B (en) * | 2007-09-06 | 2011-07-06 | 上海医药工业研究院 | Total alkaloide extraction method from mixture of angelica and ligusticum wallichii rhizome by supercritical carbon dioxide |
| CN101905091A (en) * | 2010-07-12 | 2010-12-08 | 新疆大学 | Equipment and method for extracting biologically active ingredients from subcritical fluid |
| CN101905091B (en) * | 2010-07-12 | 2012-05-30 | 新疆大学 | Equipment and method for extracting biologically active ingredients from subcritical fluid |
| CN102210943A (en) * | 2011-06-20 | 2011-10-12 | 东莞广州中医药大学中医药数理工程研究院 | Cell-wall-breaking low-temperature extraction method and device with assistance of CO2 |
| US9908063B2 (en) | 2012-11-20 | 2018-03-06 | Andrew Paul Joseph | Extraction apparatus |
| US9908062B2 (en) | 2012-11-20 | 2018-03-06 | Andrew Paul Joseph | Extraction apparatus and method |
| US9132363B2 (en) | 2012-11-20 | 2015-09-15 | Apeks Llc | Extraction system |
| CN107760058A (en) * | 2017-11-30 | 2018-03-06 | 广西南宁栩兮科技有限公司 | The extracting method of haematochrome in a kind of rambutan shell |
| CN108938682A (en) * | 2018-10-09 | 2018-12-07 | 淮安安莱生物科技有限公司 | A method of extracting cypress acid and cedar wood alcohol from high mountain cypress |
| CN109157545A (en) * | 2018-10-09 | 2019-01-08 | 淮安安莱生物科技有限公司 | A method of extracting shellac acid and jalaric acid from shellac |
| CN109157545B (en) * | 2018-10-09 | 2021-10-01 | 海门茂发美术图案设计有限公司 | Method for extracting Lacca acid and Lacca alcohol acid from Lacca |
| CN108938682B (en) * | 2018-10-09 | 2022-03-11 | 淮安安莱生物科技有限公司 | Method for extracting cedarwood acid and cedrol from sabina vulgaris |
| CN113000588A (en) * | 2021-03-16 | 2021-06-22 | 中国科学院工程热物理研究所 | Mobile supercritical fluid soil remediation system and remediation device |
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