CN1414077A - Extraction method of high quality lingxiang grass purified oil - Google Patents
Extraction method of high quality lingxiang grass purified oil Download PDFInfo
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- CN1414077A CN1414077A CN 02133854 CN02133854A CN1414077A CN 1414077 A CN1414077 A CN 1414077A CN 02133854 CN02133854 CN 02133854 CN 02133854 A CN02133854 A CN 02133854A CN 1414077 A CN1414077 A CN 1414077A
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Abstract
A process for extracting high-quality and high-purity Lingxiang herb oil includes such steps as extracting by supercritical CO2 fluid at 35 deg.C and 12 MPa for 1.5 hr, low-temp freeze dewaxing at -15- -20 deg.C, and high-speed centrifugal separation at 45 deg.C and 5 MPa. Its advantages are high output rate increased by 5 times high quality, no residual solvent, and special fragrance.
Description
(1) technical field:
The present invention relates to the extracting method of a kind of extracting method of natural phant absolute oil, particularly high quality lingxiang grass purified oil.
(2) background technology:
Lysimachia foenum-graecum (Lysimachia foenum-graecum Hance) is a Primulaceae Lysimachia plant, another name Lysimachia sikokiana, Ocimum basilicum L., eupatorium, perfume etc., and main product is in counties such as the gold show in Guangxi, melt waters, and there is cultivation in Guangdong, Yunnan, Sichuan, Guizhou.Lysimachia foenum-graecum has extremely special fragrance breath, the expensive perfume base of generic name.Traditional natural perfume extraction method mainly is solvent method and steam distillation, and solvent method can produce dissolvent residual, and to the extract non-selectivity, the solvent recuperation process temperature is higher, and the destructible aroma component also may have certain pollution to environment, technical process is long, length consuming time.Vapour method temperature height, the destructible aroma component, especially to famous and precious spices, the bottom note material is difficult to propose, and extraction yield is low, and resource is caused waste.
(3) summary of the invention:
The present invention will disclose a kind of no solvent residue, not destroy aroma component, and the extracting method of the high a kind of high quality lingxiang grass purified oil of extraction yield.
A kind of extracting method of high quality lingxiang grass purified oil is characterized in that: adopted supercritical CO
2Fluid is that extraction solvent extracts the Lysimachia foenum-graecum raw material, and extracting solution is again through the cryogenic freezing dewaxing, and the high speed centrifugation separation obtains high quality lingxiang grass purified oil.
Supercritical CO
2The extraction process optimum condition is: extracting pressure is 10～15MPa, and temperature is 25～50 ℃, and the time is 1～3h, and flow is 150～200L/h.
Supercritical CO
2The extraction process top condition is: extracting pressure is 12MPa, and temperature is 35 ℃, and the time is 1.5h, and flow is 180L/h.
Supercritical CO
2The isolating optimum condition of technology is: pressure is 4.5～5.5MPa, and temperature is 40～55 ℃.
Supercritical CO
2Technology is separated top condition: pressure is 5MPa, and temperature is 45 ℃.
The optimum condition of cryogenic freezing centrifugation is: 4000～8000 rev/mins of rotating speeds, temperature are-15～-20 ℃.
Supercritical CO
2Extraction process (SCF-CO
2) be defined as: CO
2Under supercritical state, have the dissolving properties of non-polar liquid Ji agent, and the dissolving power of material is depended on the size of density and the molecular weight and the polarity of solute.And density is the majorant of pressure and temperature, and especially pressure is regulated CO
2Pressure optionally extract or separate some component.Utilize supercritical CO
2These character can extract, desirable component in the separate substance (plant), this lock out operation just meaning be supercritical CO
2Extraction process.Utilize supercritical CO
2Extraction process extracts spices following several respects benefit: the 1. the most approaching nature of fragrance, and aroma substance extracts fully; 2. extract at low temperature does not destroy aroma component; 3. by adjusting pressure and temperature, make SFE-CO
2Extract there is selectivity preferably; 4. CO
2Can be recycled, free from environmental pollution, and reduce cost; 5. technical process is short, consuming time few, need not or seldom use organic solvent.
Advantage of the present invention place:
(1) uses supercritical CO
2Extract the Lysimachia foenum-graecum absolute oil, extract and kept the peculiar fragrance of Lysimachia foenum-graecum preferably, it is low, consuming time few to extract temperature, no solvent residue.
(2) use supercritical CO
2Best extraction process condition is extracted the Lysimachia foenum-graecum absolute oil that obtains, and is yellow oil, and wax is few, and good fluidity is transparent, can be dissolved in dehydrated alcohol fully.
(3) supercritical CO
2Technology is extracted the Lysimachia foenum-graecum absolute oil, and the yield height on average can reach more than 1.1%, and conventional steam distillation yield is high more than 5 times (the steam distillation yield is 0.22～0.25%), CO
2Can be recycled, energy consumption is low, and good industrialized application prospect is arranged.
Hence one can see that adopts the present invention to extract Lysimachia foenum-graecum, and extracting solution is again through freezing dewaxing, and high speed centrifugation separates, and can obtain being close to perfect high quality lingxiang grass purified oil.
It is low, consuming time few that present method is extracted temperature, extracts and kept the peculiar fragrance of Lysimachia foenum-graecum preferably, the yield height, and of light color, wax is few, and good fluidity has good industrialized application prospect.
(4) description of drawings:
Fig. 1 is the concrete process flow sheet of the present invention.
(5) embodiment:
When concrete enforcement was of the present invention, as shown in Figure 1, its technical process was with the Lysimachia foenum-graecum raw material after crushed earlier, uses CO
2Fluid extraction, extraction liquid be again through cryogenic freezing, and the high speed centrifugation dewaxing can obtain absolute oil content and reach Lysimachia foenum-graecum absolute oil more than 90%.
At supercritical CO
2In the fluid extraction processing step, investigated of the influence of each factor such as pressure, temperature, time, flow velocity, granularity, entrainment agent to absolute oil yield and quality, and design L9 (3
4) orthogonal experiment, mainly investigated the influence of extracting pressure, temperature, time and four factors of flow, from experimental result, pressure has the greatest impact to Lysimachia foenum-graecum absolute oil yield and quality, and pressure raises, CO
2Density is also along with rising, and dissolving power strengthens, and cause yield to rise, but the rising of pressure also makes some under low pressure be difficult for dissolved substances simultaneously, comes out as pigment, wax etc. are dissolved, and the absolute oil quality is descended.The supercritical CO that we choose is considered in comprehensive absolute oil yield and quality two aspects
2The extraction process condition is: extracting pressure is 10～15MPa, and temperature is 25～50 ℃, and the time is 1～3h, and flow is 150～200L/h; Best extraction process condition is: extracting pressure 12Mpa, 35 ℃ of temperature, time 1.5h, flow 180L/h, separating pressure 5Mpa, 45 ℃ of temperature.
Adopt this condition that Lysimachia foenum-graecum has been carried out ten batches extraction, the extract yield on average can reach 1.2%.Extract is ℃ freezing in low temperature-15～-20 again, and high speed centrifugation (rotating speed is greater than 4000 rev/mins) separates dewaxing, can obtain high-quality Lysimachia foenum-graecum absolute oil, and absolute oil content can reach more than 90%, and the absolute oil yield is more than 1.1%.
Ten batches are adopted supercritical CO
2The result that extraction process extracts the Lysimachia foenum-graecum absolute oil is as follows:
Embodiment 1: charging capacity 10kg, and extracting pressure 12MPa, temperature is 50 ℃, the time is 1h, CO
2Flow is 150L/h; Separating pressure 5MPa, 40 ℃ of separation temperatures, freezing temp in the frozen centrifugation wax removing process-20 ℃, rotating speed is 4000 rev/mins, Lysimachia foenum-graecum absolute oil 118g, absolute oil yield 1.18%, absolute oil content 93.5%.Lysimachia foenum-graecum absolute oil fragrance is good, good fluidity, yellow transparent.
Embodiment 2: charging capacity 10kg, extracting pressure 14MPa, 35 ℃ of extraction temperature, extraction time 1.5h, flow 180L/h, separating pressure 5.5MPa, 55 ℃ of separation temperatures, freezing temp in the frozen centrifugation wax removing process-18 ℃, rotating speed is 4500 rev/mins, get Lysimachia foenum-graecum absolute oil 121g, absolute oil yield 1.21%, absolute oil content 92.5% at last.Lysimachia foenum-graecum absolute oil color is dark than example 1.
Embodiment 3: charging capacity 10kg, extracting pressure 15MPa, 35 ℃ of extraction temperature, extraction time 1.5h, flow 170L/h, separating pressure 4.5MPa, 45 ℃ of separation temperatures, freezing temp in the frozen centrifugation wax removing process-18 ℃, rotating speed is 4500 rev/mins, get Lysimachia foenum-graecum absolute oil 125g, absolute oil yield 1.25%, absolute oil content 91.5% at last.Lysimachia foenum-graecum absolute oil color is dark than example 1.
Embodiment 4: charging capacity 10kg, extracting pressure 12MPa, 40 ℃ of extraction temperature, extraction time 1.5h, flow 180L/h, separating pressure 5.5MPa, 55 ℃ of separation temperatures, freezing temp in the frozen centrifugation wax removing process-18 ℃, rotating speed is 4500 rev/mins, Lysimachia foenum-graecum absolute oil 119g, absolute oil yield 1.19%, absolute oil content 93.1%.Lysimachia foenum-graecum absolute oil fragrance is good, good fluidity, yellow transparent.
Embodiment 5: charging capacity 10kg, extracting pressure 12MPa, 50 ℃ of extraction temperature, extraction time 2h, flow 180L/h, separating pressure 4.5MPa, 45 ℃ of separation temperatures, freezing temp in the frozen centrifugation wax removing process-18 ℃, rotating speed is 4500 rev/mins, Lysimachia foenum-graecum absolute oil 122g, absolute oil yield 1.22%, absolute oil content 92.8%.Lysimachia foenum-graecum absolute oil fragrance is good, good fluidity, yellow transparent.
Embodiment 6: charging capacity 10kg, extracting pressure 12MPa, 35 ℃ of extraction temperature, extraction time 2h, flow 180L/h, separating pressure 5MPa, 40 ℃ of separation temperatures, freezing temp in the frozen centrifugation wax removing process-18 ℃, rotating speed is 4500 rev/mins, Lysimachia foenum-graecum absolute oil 117g, absolute oil yield 1.17%, absolute oil content 92.5%.Lysimachia foenum-graecum absolute oil fragrance is good, good fluidity, yellow transparent.
Embodiment 7: charging capacity 12kg, extracting pressure 12MPa, 30 ℃ of extraction temperature, extraction time 2.5h, flow 170L/h, separating pressure 5MPa, 40 ℃ of separation temperatures, freezing temp in the frozen centrifugation wax removing process-20 ℃, rotating speed is 5000 rev/mins, absolute oil yield 1.15%, absolute oil content 92.7%.Lysimachia foenum-graecum absolute oil fragrance is good, good fluidity, yellow transparent.
Embodiment 8: charging capacity 12kg, extracting pressure 11MPa, 25 ℃ of extraction temperature, extraction time 2h, flow 160L/h, separating pressure 5MPa, 45 ℃ of separation temperatures, freezing temp in the frozen centrifugation wax removing process-20 ℃, rotating speed is 6000 rev/mins, Lysimachia foenum-graecum absolute oil 132g, absolute oil yield 1.10%, absolute oil content 92.5%.Lysimachia foenum-graecum absolute oil fragrance is good, good fluidity, yellow transparent.
Embodiment 9: charging capacity 12kg, extracting pressure 12MPa, 30 ℃ of extraction temperature, extraction time 3h, flow 180L/h, separating pressure 5MPa, 45 ℃ of separation temperatures, freezing temp in the frozen centrifugation wax removing process-15 ℃, rotating speed is 7000 rev/mins, Lysimachia foenum-graecum absolute oil 134.4g absolute oil yield 1.12%, absolute oil content 92.0%.Lysimachia foenum-graecum absolute oil fragrance is good, good fluidity, yellow transparent.
Embodiment 10: charging capacity 12kg, extracting pressure 12MPa, 25 ℃ of extraction temperature, extraction time 3h, flow 180L/h, separating pressure 5MPa, 55 ℃ of separation temperatures, freezing temp in the frozen centrifugation wax removing process-18 ℃, rotating speed is 8000 rev/mins, Lysimachia foenum-graecum absolute oil 138g, absolute oil yield 1.15%, absolute oil content 92.1%.Lysimachia foenum-graecum absolute oil fragrance is good, good fluidity, yellow transparent.
Above absolute oil content measuring reference standard: GB/T 14458-93.
Claims (8)
1, a kind of extracting method of high quality lingxiang grass purified oil is characterized in that: adopted supercritical CO
2Fluid is that extraction solvent extracts the Lysimachia foenum-graecum raw material, and extracting solution is again through the cryogenic freezing dewaxing, and the high speed centrifugation separation obtains high quality lingxiang grass purified oil.
2, the extracting method of a kind of high quality lingxiang grass purified oil according to claim 1 is characterized in that: described supercritical CO
2The extraction process condition is: extracting pressure is 10～15MPa, and temperature is 25～50 ℃, and the time is 1～3h, and flow is 150～200L/h.
3, the extracting method of a kind of high quality lingxiang grass purified oil according to claim 2 is characterized in that: described supercritical CO
2The extraction process condition is: extracting pressure is 12MPa, and temperature is 35 ℃, and the time is 1.5h, and flow is 180L/h.
4, according to the extracting method of claim 2 or 3 described a kind of high quality lingxiang grass purified oils, it is characterized in that: described supercritical CO
2The technology separation condition is: pressure is 4.5～5.5MPa, and temperature is 40～55 ℃.
5, the extracting method of a kind of high quality lingxiang grass purified oil according to claim 4 is characterized in that: described supercritical CO
2The technology separation condition is: pressure is 5MPa, and temperature is 45 ℃.
6, according to the extracting method of claim 2 or 3 described a kind of high quality lingxiang grass purified oils, it is characterized in that: centrifugal its freezing temp of described cryogenic freezing is-15～-20 ℃, and centrifugal rotational speed is 4000～5000 rev/mins.
7, the extracting method of a kind of high quality lingxiang grass purified oil according to claim 4 is characterized in that: centrifugal its freezing temp of described cryogenic freezing is-15～-20 ℃, and centrifugal rotational speed is 4000～5000 rev/mins.
8, the extracting method of a kind of high quality lingxiang grass purified oil according to claim 5 is characterized in that: centrifugal its freezing temp of described cryogenic freezing is-15～-20 ℃, and centrifugal rotational speed is 4000～5000 rev/mins.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100383228C (en) * | 2005-09-02 | 2008-04-23 | 天津春发食品配料有限公司 | Process and apparatus for extracting edible volatile plant essence oil |
| CN101875685A (en) * | 2010-06-25 | 2010-11-03 | 广西师范大学 | Lysimachia foenum-graecum hance saponin extract having more than or equal to 30 percent of saponin and extraction process thereof |
| CN101928654B (en) * | 2009-06-23 | 2011-11-16 | 湖北中烟工业有限责任公司 | Natural herbal degerming and parasite-expelling toilet soap and preparation method thereof |
| CN101678060B (en) * | 2007-06-08 | 2013-03-27 | 纽吉克斯有限公司 | Medicinal herbal extract having anti-obesity effect |
| CN103421611A (en) * | 2013-09-10 | 2013-12-04 | 文笃祥 | Method for extracting effective constituents from holy basil |
| CN103497834A (en) * | 2013-10-22 | 2014-01-08 | 中国烟草总公司郑州烟草研究院 | Method for preparing dandelion absolute oil and application of dandelion absolute oil in cigarettes |
| CN103710152A (en) * | 2013-10-28 | 2014-04-09 | 黄山神草生物科技有限公司 | Method for using supercritical carbon dioxide for extraction of chrysanthemum essential oil |
| CN104082846A (en) * | 2014-07-24 | 2014-10-08 | 中国烟草总公司郑州烟草研究院 | Application of althaea rosa seed extractive to cigarettes |
| CN107836646A (en) * | 2017-12-12 | 2018-03-27 | 茗（杭州）投资控股有限公司 | Cool skin and preparation method thereof |
| CN108018117A (en) * | 2017-12-25 | 2018-05-11 | 湖南宇山玉月农业科技有限公司 | A kind of extracting method of styrax essential oil |
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2002
- 2002-09-27 CN CN 02133854 patent/CN1414077A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100383228C (en) * | 2005-09-02 | 2008-04-23 | 天津春发食品配料有限公司 | Process and apparatus for extracting edible volatile plant essence oil |
| CN101678060B (en) * | 2007-06-08 | 2013-03-27 | 纽吉克斯有限公司 | Medicinal herbal extract having anti-obesity effect |
| CN101928654B (en) * | 2009-06-23 | 2011-11-16 | 湖北中烟工业有限责任公司 | Natural herbal degerming and parasite-expelling toilet soap and preparation method thereof |
| CN101875685A (en) * | 2010-06-25 | 2010-11-03 | 广西师范大学 | Lysimachia foenum-graecum hance saponin extract having more than or equal to 30 percent of saponin and extraction process thereof |
| CN103421611A (en) * | 2013-09-10 | 2013-12-04 | 文笃祥 | Method for extracting effective constituents from holy basil |
| CN103497834B (en) * | 2013-10-22 | 2015-07-08 | 中国烟草总公司郑州烟草研究院 | Method for preparing dandelion absolute oil and application of dandelion absolute oil in cigarettes |
| CN103497834A (en) * | 2013-10-22 | 2014-01-08 | 中国烟草总公司郑州烟草研究院 | Method for preparing dandelion absolute oil and application of dandelion absolute oil in cigarettes |
| CN103710152A (en) * | 2013-10-28 | 2014-04-09 | 黄山神草生物科技有限公司 | Method for using supercritical carbon dioxide for extraction of chrysanthemum essential oil |
| CN103710152B (en) * | 2013-10-28 | 2016-04-27 | 黄山神草生物科技有限公司 | A kind of method of supercritical carbon dioxide extraction chrysanthemum essential oil |
| CN104082846A (en) * | 2014-07-24 | 2014-10-08 | 中国烟草总公司郑州烟草研究院 | Application of althaea rosa seed extractive to cigarettes |
| CN104082846B (en) * | 2014-07-24 | 2016-02-24 | 中国烟草总公司郑州烟草研究院 | The application of a kind of hollyhock seed extract in cigarette |
| CN107836646A (en) * | 2017-12-12 | 2018-03-27 | 茗（杭州）投资控股有限公司 | Cool skin and preparation method thereof |
| CN108018117A (en) * | 2017-12-25 | 2018-05-11 | 湖南宇山玉月农业科技有限公司 | A kind of extracting method of styrax essential oil |
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