CN1295310C - Process for extracting and refining lavender oil - Google Patents
Process for extracting and refining lavender oil Download PDFInfo
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- CN1295310C CN1295310C CNB200510034539XA CN200510034539A CN1295310C CN 1295310 C CN1295310 C CN 1295310C CN B200510034539X A CNB200510034539X A CN B200510034539XA CN 200510034539 A CN200510034539 A CN 200510034539A CN 1295310 C CN1295310 C CN 1295310C
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Abstract
The present invention relates to a method for preparing lavender oil by removing wax by a supercritical CO2 liquid technology. The wax components in essential oil obtained by a traditional supercritical CO2 liquid technology can not be removed clearly. The present invention provides a method for extracting lavender oil by simultaneously extracting lavender oil and removing wax, which has the steps: extracting lavender oil by supercritical CO2; depressurizing the lavender oil by three sections of temperature controlled rectification columns; further depressurizing the lavender oil in an analysis kettle; regulating the temperature of the CO2 after depressurization to effectively separate wax components from essential oil in the lavender oil. The method of the present invention can effectively remove the wax components contained in the essential oil, and ensure that the essential oil is clear and transparent and has high volatility and pure fragrance. The method is convenient for industrial production.
Description
Technical field
The present invention relates to a kind of with supercritical CO
2Fluid technique prepares the method for paraffin removal Oleum lavandula angustifolia.
Background technology
Lavandula angustifolia is the Labiatae per nnial herb, adopts flower fringe extracting section Oleum lavandula angustifolia, and essential oil has sterilization, the scar of dispelling, effect such as refresh oneself, calm.The method that tradition is extracted Oleum lavandula angustifolia is the method for steam distillation, this method is that Oleum lavandula angustifolia is distilled out with water vapor, pass through condensation then, make essential oil and water sepn by water-and-oil separator, this method service temperature height, not only can lose a fragrant composition of Herba Lysimachiae foenumgraeci quintessence oil and easily make facile hydrolysis in the essential oil, easily oxidation and heat-sensitive substance change and lose its original effect, limited it and extracted the application of goods in industries such as medicine, food.
Supercritical CO
2Abstraction technique is a kind of technology of separating substances efficiently that chemical field researchdevelopment in nearly 20 years is got up, this technology is to utilize carbonic acid gas under different pressure and temps, difference to organism solubleness, realize organic separation, have flower class volatile constituent solubleness big, the rate of mass transfer height, the extracting and separating temperature is low, solvent easily reuses and does not have a solvent residues, the nonpoisonous and tasteless advantage such as harmless of solvent, can effectively prevent easily oxidation in the Herba Lysimachiae foenumgraeci quintessence oil, facile hydrolysis and heat-sensitive substance change, and have kept the natural flavor of natural perfume, are a kind of ideal separation methods.
Supercritical CO
2Fluid is similar to non-polar solvent, when extracting flower class plants essential oil, often contains more wax component.Wax component is some white natural fats and oils, wherein mainly is unsettled natural plant grease, is easy to give off a peculiar smell after the oxidation, can cause neural deflation, dizziness or headache, tongue fiber crops or thirsty reflection.The allotment of the pure essential oil of quality can be merged in base oil the time fully, and both molecules are combination fully also, can not be well and the base oil fusion and contain the essential oil of wax component, limited the application of essential oil.Essential oil with one milliliter of dress calculates, and good volatile oil can ooze about 20, and impure essential oil can only ooze 7～8 or 10, and wax component increases the viscosity of essential oil, thereby has reduced the flowability of essential oil.In general, the proportion of flowers and plants class essential oil is the lightest, splashes in one glass of water and can scatter fast, and the water surface can present the oil slick state; Resene essential oil molecule is the heaviest, splash in one glass of water, but integral drip complete fall into glass at the bottom of, unsuitable water-soluble, the essential oil that contains wax has the wax suspended substance when tending to form one deck oil slick on the water surface under water.The essential oil that quality is pure more, seepage force is strong more, and essential oil is dabbed in the back of the hand or wrist inboard, massages several following more a little with finger tip, the essential oil of quality better can be absorbed in moment, and the essential oil that contains wax component absorbs slow and can stay glistening lubricant component on skin.The essential oil of quality better has a thorough knowledge of transparent, no suspended substance in the essential oil, and the essential oil that contains wax component reduces the essential oil transparency and darkens.The Oleum lavandula angustifolia of domestic present extraction substantially all adopts the method for steam distillation, this method is because the temperature height, thereby the material that easily makes thermo-sensitivity, easy oxidation changes and influences the quality of essential oil, adopts the yield of this method extraction Herba Lysimachiae foenumgraeci quintessence oil lower simultaneously, is difficult for suitability for industrialized production.Nineteen ninety-five, people such as gondola E.Reverchon have delivered the paper with supercritical extraction Herba Lysimachiae foenumgraeci quintessence oil and wax component, this paper has utilized the Different Effects rule of extraction temperature to the solubleness of Herba Lysimachiae foenumgraeci quintessence oil and wax component, resolves in the separation at substep to prepare Herba Lysimachiae foenumgraeci quintessence oil by the method for lowering the temperature.Adopt same procedure to remove the extraction respectively that comprises red pepper pigment and essential oil of wax; The preparation of pyrethrum essential oil; The preparation of rosemary ethereal oil.This method is just simply come paraffin removal by separating pressure and variation of temperature, can reach certain purifying purpose, but the variation of simple dependence pressure and temperature, the wax component in the essential oil often is difficult to remove clean.
Summary of the invention
According to problems of the prior art, the present invention proposes the method for the extraction Oleum lavandula angustifolia of an extraction and paraffin removal one, because wax component is relatively more responsive to temperature in overcritical, combine by the rectifying tower of supercritical extraction technique with three sections temperature controls, by the variation of thermograde, can well solve the problem of essential oil paraffin removal.
The objective of the invention is to adopt the method for the extraction Oleum lavandula angustifolia of a kind of novel supercritical carbon dioxide extraction and paraffin removal one, overcome facile hydrolysis in the loss, Oleum lavandula angustifolia of the fragrant composition of the Herba Lysimachiae foenumgraeci quintessence oil head that exists in the prior art, easily oxidation and heat-sensitive substance changes, and characteristics that wax component is difficult to remove in the essential oil and make Oleum lavandula angustifolia yield height, viscosity is low, volatility is good, it is transparent to have a thorough knowledge of, and smell is pure.Both used supercritical CO
2After extracting Oleum lavandula angustifolia, through the rectifying tower step-down of three sections temperature controls, in extraction-container, further reduce pressure subsequently earlier, and CO after the adjusting step-down
2Temperature, make that wax component can effectively separate with essential oil in the Oleum lavandula angustifolia.
The concrete steps of the inventive method are as follows:
1, screening, drying: the flowers are in blossom gathered the flower fringe at nearly 40% o'clock at the lavandula angustifolia bud, through drying in the shade or cryodrying dewaters.
2, pulverize: will dry in the shade or the lavandula angustifolia of cryodrying is ground into 20～80 purpose small-particles with agricultural mill.
3, extraction and refining Oleum lavandula angustifolia: the lavandula angustifolia fine particle with pulverizing is positioned over supercritical CO
2In the extraction kettle of extraction plant, supercritical CO
2Fluid enters in the extraction kettle, has extracted the CO of Oleum lavandula angustifolia
2Gas enters the rectifying tower of three sections temperature controls, utilize the rule of temperature, adopt different thermogrades, wax component is separated with essential oil and stay in the rectifying tower the different solubility of wax and essential oil, enter the extraction-container step-down then and resolve, the orange-yellow transparent liquid that obtains is required extract.Extracting pressure is that 7MPa～30MPa (is generally 8MPa～20Mpa); Extraction temperature is 30 ℃～60 ℃ (being generally 40 ℃～60 ℃); CO
2Flow is that 5L/h～50L/h (is generally 10L/h～20L/h); The extraction time is that 1h～5h (is generally 1h～3h); The pressure of rectifying tower is that 6MPa～20MPa (is generally 7MPa～10Mpa); The temperature of rectifying tower is 20 ℃～80 ℃ (being generally 40 ℃～80 ℃).
Method of the present invention specifically may further comprise the steps: with CO
2Gas feeds in the extraction kettle continuously; Extracted the CO of Oleum lavandula angustifolia
2Gas sends into rectifying tower and the extraction-container step-down is resolved; From rectifying tower, collect wax component; From extraction-container, collect Oleum lavandula angustifolia, CO
2Recycle after the compressed machine pressurization of gas.
Method of the present invention preferably is controlled at the lavandula angustifolia grinding particle size about the 20-60 order; Extracting pressure is 7MPa～30MPa, and extraction temperature is 30 ℃～60 ℃; Rectifying tower pressure is 6MPa～15MPa, and temperature is that 60 ℃～80 ℃, b section are that 40 ℃～70 ℃, c section are 30 ℃～60 ℃ for a section; Extraction-container pressure is 4MPa～6MPa, and temperature is 30 ℃～50 ℃, CO
2Flow is 10L/h～20L/h, and the extraction time is 1h～3h.
The inventive method has the following advantages as a kind of method of being convenient to preparation of industrialization paraffin removal Oleum lavandula angustifolia:
1. the extracting and separating temperature is low, mild condition.The steam distilled extracting and separating temperature of traditional water is at 100 ℃, and present method extracting and separating temperature is at 40 ℃～60 ℃, well below traditional method.
2. Oleum lavandula angustifolia percentage extraction height.The steam distilled percentage extraction of traditional water is 0.6%～0.8%, and present method percentage extraction is 2.0%～2.5%, has improved nearly 3 times than traditional method.
3. contained active substance in effective retention of oil.The general temperature of traditional method is higher, easily make facile hydrolysis in the essential oil, easily oxidation and heat-sensitive substance changes and the essential oil quality is reduced, yield descends, and present method extracting and separating temperature is low, be close to anhydrous and oxygen-free in the extraction process, effectively the activeconstituents of retention of oil.
4. gained Oleum lavandula angustifolia volatilization back does not have remaining.Often contain more wax component in the simple supercritical extraction Oleum lavandula angustifolia, and the volatility of essential oil is reduced, stay after the volatilization and be difficult to the evaporable wax component, be coated in and easily stop up pore on the skin, easily cause the skin discomfort.
5. gained Oleum lavandula angustifolia is as clear as crystal, is orange-yellow liquid.The color that contains the Oleum lavandula angustifolia poor transparency of wax component and essential oil is darker, and the freezing wax component that has is separated out and is suspended in the essential oil, is used for beauty culture etc. and can reduces the acceptance level in market.
6. gained Oleum lavandula angustifolia viscosity is low, and diffustivity is good.The Oleum lavandula angustifolia viscosity that contains wax component is big, and is mobile poor, thereby diffustivity descends.Splash in the water and to be difficult for scattering fast, and the wax component of the white that in water, suspends.
7. gained Oleum lavandula angustifolia smell is pure, and is not perishable, gives out natural faint scent, (is being kept under the normal temperature state) under the goodish preservation condition, can preserve 4～5 years.The Oleum lavandula angustifolia that contains wax component because wax is unsettled natural plant grease, is easy to give off a peculiar smell after the oxidation, not only unlike the natural fragrance of a flower but also smell this fragrance for a long time and also can cause dizziness or headache.
Embodiment
Example 1
Be crushed to 20 purpose lavandula angustifolias with 1 kilogram and drop into extraction kettle, the control extraction temperature is 40 ℃, and extracting pressure is 10MPa, the pressure of rectifying tower is 7MPa, and a place temperature is 80 ℃, and b place temperature is 50 ℃, c place temperature is 35 ℃, the pressure of extraction-container is 4.5MPa, and temperature is 30 ℃, and the flow of carbonic acid gas is 10L/h, extract after 2 hours, from extraction-container, take out and resolve extract, promptly refining Oleum lavandula angustifolia, yield is 2.18%.From rectifying tower, collect wax component, yield 0.13%.
Example 2
Be crushed to 60 purpose lavandula angustifolias with 1.5 kilograms and drop into extraction kettle, the control extraction temperature is 50 ℃, and extracting pressure is 20MPa, the pressure of rectifying tower is 8MPa, and a place temperature is 75 ℃, and b place temperature is 60 ℃, c place temperature is 45 ℃, the pressure of extraction-container is 4.5MPa, and temperature is 30 ℃, and the flow of carbonic acid gas is 15L/h, extract after 2.5 hours, from extraction-container, take out and resolve extract, promptly refining Oleum lavandula angustifolia, yield is 2.5%.From rectifying tower, collect wax component, yield 0.17%.
Example 3
Be crushed to 40 purpose lavandula angustifolias with 1.2 kilograms and drop into extraction kettle, the control extraction temperature is 60 ℃, and extracting pressure is 15MPa, the pressure of rectifying tower is 8MPa, and a place temperature is 70 ℃, and b place temperature is 60 ℃, c place temperature is 50 ℃, the pressure of extraction-container is 4.5MPa, and temperature is 40 ℃, and the flow of carbonic acid gas is 10L/h, extract after 2 hours, from extraction-container, take out and resolve extract, promptly refining Oleum lavandula angustifolia, yield is 2.33%.From rectifying tower, collect wax component, yield 0.15%.
Claims (5)
1, the novel method of a kind of extraction and refining Oleum lavandula angustifolia, the method for employing extraction and paraffin removal one by the variation of thermograde, reaches the purpose of extraction and refining Oleum lavandula angustifolia, it is characterized in that using supercritical CO
2After extracting Oleum lavandula angustifolia, through the rectifying tower step-down of three sections temperature controls, in extraction-container, further reduce pressure earlier, and reconcile the carbonic acid gas temperature after the step-down, the wax component of lavandula angustifolia can effectively be separated with essential oil, comprise that specifically step is as follows:
Lavandula angustifolia fine particle with pulverizing is positioned over supercritical CO
2In the extraction kettle of extraction plant, supercritical CO
2Fluid enters in the extraction kettle, has extracted the CO of Oleum lavandula angustifolia
2Gas enters the rectifying tower of three sections temperature controls, adopt different thermogrades, wax component is separated with essential oil and stay in the rectifying tower, enter the extraction-container step-down then and resolve, the orange-yellow transparent liquid that obtains is required extract, and extracting pressure is 7MPa～30MPa; Extraction temperature is 30 ℃～60 ℃; CO
2Flow is 5L/h～50L/h; The extraction time is 1h～5h; The pressure of rectifying tower is 6MPa～20MPa; The temperature of rectifying tower is three sections temperature controls: a section is that 70 ℃～80 ℃, b section are that 50 ℃～60 ℃, c section are 35 ℃～50 ℃.
2, according to the novel method of extraction described in the claim 1 and refining Oleum lavandula angustifolia, it is characterized in that described extracting pressure is 8MPa～20Mpa, extraction temperature is 40 ℃～60 ℃.
3,, it is characterized in that described CO according to the novel method of extraction described in the claim 1 and refining Oleum lavandula angustifolia
2Flow is 10L/h～20L/h, and the extraction time is 1h～3h.
4, according to the novel method of extraction described in the claim 1 and refining Oleum lavandula angustifolia, the pressure that it is characterized in that described rectifying tower is 7MPa～10Mpa.
5, according to the novel method of extraction described in the claim 1 and refining Oleum lavandula angustifolia, it is characterized in that described lavandula angustifolia raw material is that the flowers are in blossom gathered the flower fringe at nearly 40% o'clock at the lavandula angustifolia bud, through drying in the shade or cryodrying dewaters, be ground into 20～80 purpose particles and get.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200510034539XA CN1295310C (en) | 2005-05-12 | 2005-05-12 | Process for extracting and refining lavender oil |
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| CNB200510034539XA CN1295310C (en) | 2005-05-12 | 2005-05-12 | Process for extracting and refining lavender oil |
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| CN1295310C true CN1295310C (en) | 2007-01-17 |
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| CNB200510034539XA Expired - Fee Related CN1295310C (en) | 2005-05-12 | 2005-05-12 | Process for extracting and refining lavender oil |
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Families Citing this family (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100415859C (en) * | 2006-07-28 | 2008-09-03 | 上海应用技术学院 | Preparation method of lavender nano-essential oil |
| CN100999696B (en) * | 2006-12-26 | 2010-05-19 | 中国科学院新疆理化技术研究所 | Extracting process of lavender flower |
| CN101824366B (en) * | 2010-05-24 | 2012-04-25 | 新疆雪莲新技术有限公司 | Method for extracting absolute oil of lavender by using fixed bed extraction method |
| CN103666758A (en) * | 2012-09-11 | 2014-03-26 | 天津天士力现代中药资源有限公司 | Refining method of volatile oil |
| CN102965198A (en) * | 2012-11-14 | 2013-03-13 | 陈和平 | Method for extracting and processing lavender essential oil |
| CN103627528A (en) * | 2013-06-30 | 2014-03-12 | 金玛瑙香水（明光）有限公司 | Method for extracting lavender essential oil |
| CN103333744B (en) * | 2013-07-11 | 2015-01-07 | 厦门大学 | Apparatus for separating oxygen-containing compounds in concentrated orange essential oil through supercritical chromatography, and method thereof |
| CN104479881A (en) * | 2014-12-25 | 2015-04-01 | 北京化工大学常州先进材料研究院 | Supercritical CO2 continuous extraction and distillation and low-temperature separation method for rose essential oil |
| CN105213272B (en) * | 2015-11-09 | 2019-02-01 | 北京工商大学 | A kind of fresh and alive water of lavender and the preparation method and application thereof |
| CN105950294A (en) * | 2016-05-28 | 2016-09-21 | 黄宇松 | Lavandula pedunculata flower aromatic material extraction method |
| CN106047500A (en) * | 2016-05-31 | 2016-10-26 | 铜仁职业技术学院 | Method for efficiently extracting lavender and application of extract of lavender |
| CN106085598A (en) * | 2016-07-28 | 2016-11-09 | 南京正宽医药科技有限公司 | The extracting method of a kind of antibacterial care essential oil and essential oil product |
| CN106281712A (en) * | 2016-08-28 | 2017-01-04 | 广西灏源盛世生物科技有限公司 | A kind of extracting method of Herba Lysimachiae foenum-graeci quintessence oil |
| CN107177420A (en) * | 2017-06-23 | 2017-09-19 | 广西万山香料有限责任公司 | A kind of preparation method of Lavender |
| CN113197935B (en) * | 2021-04-13 | 2022-06-24 | 开平健之源保健食品有限公司 | Extraction method of magnolia officinalis extract |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1380380A (en) * | 2002-05-09 | 2002-11-20 | 大连理工大学 | Method for extracting and purifying natural volatile oil from sophora flower by using supercritical CO2 fluid extraction process |
| CN1557521A (en) * | 2004-01-19 | 2004-12-29 | 中 孟 | Extraction method of wild rose under supercritical CO2 condition |
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- 2005-05-12 CN CNB200510034539XA patent/CN1295310C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1380380A (en) * | 2002-05-09 | 2002-11-20 | 大连理工大学 | Method for extracting and purifying natural volatile oil from sophora flower by using supercritical CO2 fluid extraction process |
| CN1557521A (en) * | 2004-01-19 | 2004-12-29 | 中 孟 | Extraction method of wild rose under supercritical CO2 condition |
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