CN105038946A - Peony essential oil supercritical CO2 extraction method - Google Patents
Peony essential oil supercritical CO2 extraction method Download PDFInfo
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- CN105038946A CN105038946A CN201510377536.XA CN201510377536A CN105038946A CN 105038946 A CN105038946 A CN 105038946A CN 201510377536 A CN201510377536 A CN 201510377536A CN 105038946 A CN105038946 A CN 105038946A
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Abstract
The invention discloses a peony essential oil supercritical CO2 extraction method. The method comprises the steps of washing, drying, grinding, supercritical extraction, and molecular distillation, and has the advantages that the operation temperature is low, the heating time is short, the grease oxidation and rancidity caused by high temperature can be avoided, moreover, the separation degree and product yield are high, the acid value of grease is reduced by the molecular distillation; high efficient extraction and separation can be achieved, the essential oil does not contain any impurity, the purity of the extraction product is high, the operation and technology are simple, the extraction time is short, the cost is reduced, and the production efficiency is improved.
Description
Technical field
The present invention relates to the extractive technique field of peony seed oil, especially a kind of supercritical CO of peony essential oil
2extracting process.
Background technology
Luoyang Peony resource is abundant especially, because tree peony originates in China, there is long cultivation history, Luoyang is native place and the place of origin of research of Paeonia suffruticosa, tree peony is the distinctive rare flower of China, its elegant and poised, gorgeous dignity, have the laudatory title of " aromatic ", " king in spending ", since ancient times by as rich and honour lucky, flourishing symbol." vein of the earth flower in Luoyang is the most suitable, and tree peony is strange particularly all over the world ", therefore also known as " Luoyang flower ".Luoyang flower starts from Shanxi, is contained in Tang, unsurpassed Song Yu, so far the history in existing more than 1600 years.Tree peony not only has ornamental value, and also has very high health, beauty treatment, pharmaceutical use.Tree peony is classified as " middle product " by Shennong's Herbal, " except crux extravasated blood, five viscera settling "; In " Huatuo highly skilled doctor's secret recipe ", relevant tree peony prescription just reaches 22 kinds more than; Its beauty and health care is worth and is all documented in Qing Dynasty's " florilegium ", " beauty treatment record "; Record and modern chemical analysis according to another other pharmacopeia: in peony petal, pollen and seed, be rich in 8 seed amino acids of multivitamin, enzyme, carbohydrate and flavones and needed by human, 7 kinds of major elements and 8 kinds of trace elements, and there is the effects such as anti-cancer reducing blood-fat.The peony seeds deep processing product of listing are little, this greatly reduces the economic worth of China's peony seeds.
A kind of kiwifruit nut oil and extracting method thereof disclosed in Chinese patent Authorization Notice No. CN1483795, adopt supercritical CO
2abstraction technique, obtained essential oil of low quality, and complex process, extraction time is long, and production cost is high, and yield is low.
In view of the foregoing, a kind of supercritical CO of peony essential oil is now developed
2extracting process.
Summary of the invention
The object of the invention is, in order to overcome deficiency of the prior art, to provide a kind of supercritical CO of peony essential oil
2extracting process, achieves efficient extraction, separation, inclusion-free, the object that extracted products purity is high, and operating procedure is simple, and extraction time is short, reduces cost, improves production efficiency.
The present invention to achieve these goals, adopts following technical scheme: a kind of supercritical CO of peony essential oil
2extracting process:
Step 1: peony seeds is carried out preferably, wash the removal of impurity and earth with water, pick out coloury peony petal to wash, the ratio of peony seeds and peony petal is 2: 1-10: 1, clean peony seeds and peony petal are drenched solid carbon dioxide to be divided stand-by, the peony seeds divide pouring solid carbon dioxide and peony petal put into solar energy baking equipment dries, wherein be provided with temperature sensor in drying shed, guarantee that bake out temperature in drying shed is between 40-70 DEG C, drying time is at 3-8 hour, water content is less than 7%, peony seeds after oven dry and peony petal are ground into chaff shape by disintegrating apparatus, obtain peony seeds and peony petal particle, for subsequent use,
Be encased in extraction kettle by 250-400kg peony seeds and peony petal particle, start extraction, extraction temperature is 35-55 DEG C, extracting pressure is 25-28Mpa, extraction time 120-150min, closes extractor, inspection guarantees that sealing is tight, uses high-pressure pump by the liquid CO in hold tank
2pump into vaporizer, gasification is input in extractor after critical fluids state, adds peony petal in the supercritical extraction of peony seed oil, peony seeds and peony petal particle are extracted, pressure in setting extractor is 10-32Mpa, and temperature is 32-80 DEG C, the CO after extraction
2input separator with the mixed stream of peony seeds and peony petal essential oil and carry out decompression separation, carbon dioxide flow 25-30kg/h, the pressure in separator is 4-10Mpa, and temperature is 20-80 DEG C, the CO after separation
2through liquefier liquefaction directly the defeated time hold tank of 20-30 DEG C recycle for next round extracting and separating, each takes turns extracting and separating time 2-8 hour, and after being separated, obtained elementary peony seeds and peony petal crude oil, for subsequent use;
Step 2: the elementary peony seeds obtained by step 1 and peony petal crude oil join in molecular still, vacuum tightness in setting molecular still is 1.0-2.0Pa, temperature is 60-80 DEG C, rotating brush film rotating speed in molecular still is 120r/min, until elementary peony seeds and peony petal crude oil are collected by heavy phase holding tank and light phase holding tank completely, collect in heavy phase holding tank and obtain peony seeds and peony petal crude oil, for subsequent use;
Step 3: the peony seeds obtained by step 2 and peony petal crude oil join in molecular still again, the vacuum tightness reset in molecular still is 1.0-2.0Pa, temperature is 60-80 DEG C, rotating brush film rotating speed in molecular still is 120r/min, until peony seeds and peony petal crude oil are collected by heavy phase holding tank and light phase holding tank completely, collect in heavy phase holding tank and obtain peony essential oil.
The invention has the beneficial effects as follows: peony seeds is the elite crystallization of peony plant; pass on outside all characteristics that tree peony itself has; it more has medicine and the nutritive ingredient of oneself uniqueness, and Paeonia suffruticosa seed is by shell and the nut of planting shell double shielding, has natural " longevity " gene.
In order to overcome the deficiency in background technology, the invention discloses a kind of supercritical CO of peony essential oil
2extracting process, the peony seed oil that the present invention obtains completes in course of processing distribution simultaneously, achieves efficient extraction, separation, inclusion-free, the object that extracted products purity is high, supercritical CO
2the peony seed oil stable in properties that extraction obtains, by level higher for peony seeds value promotion, turns waste into wealth.
The aminoacids content that peony petal protein content forms Tree Peony flower protein up to 10.1%. reaches 8.1%, wherein the highest with the content of aspartic acid in 17 seed amino acids measured, and reaches 1.12%.L-glutamic acid takes second place, and content reaches 1.09%, and L-glutamic acid is a kind of amino acid playing maintenance function in cerebral tissue, in carbohydrate metabolism and protein metabolism process, also account for critical role, and L-Ala has the effect promoting alcohol metabolism, can protect liver; Glycine and Serine have reduction cholesterol, prevent and treat the effects such as hypertension, muscle vitality can be improved, prevent hyperchlorhydria and treatment tuberculosis etc., the content of VB1 (VitB1) is higher, reach 141mg/kg, so add peony petal in the supercritical extraction of peony seed oil, the property of medicine of peony seed oil can be made to be worth higher, the fragrance of peony seed oil can be increased simultaneously.Peony seeds particle after extraction is from extractor bottom discharge, and peony seeds particle material slag can be used as farmland fertilizer.
Embodiment
Below in conjunction with embodiment and embodiment, the present invention is described in further detail:
Embodiment 1
Step 1: peony seeds is carried out preferably, wash the removal of impurity and earth with water, pick out coloury peony petal to wash, the ratio of peony seeds and peony petal is 6: 1, clean peony seeds and peony petal are drenched solid carbon dioxide to be divided stand-by, the peony seeds divide pouring solid carbon dioxide and peony petal put into solar energy baking equipment dries, wherein be provided with temperature sensor in drying shed, guarantee that bake out temperature in drying shed is between 65 DEG C, drying time was at 4 hours, water content is less than 7%, peony seeds after oven dry and peony petal are ground into chaff shape by disintegrating apparatus, obtain peony seeds and peony petal particle, for subsequent use,
Be encased in extraction kettle by 380kg peony seeds and peony petal particle, start extraction, extraction temperature is 41 DEG C, and extracting pressure is 27Mpa, extraction time 145min, closes extractor, checks and guarantees that sealing is tight, uses high-pressure pump by the liquid CO in hold tank
2pump into vaporizer, gasification is input in extractor after critical fluids state, adds peony petal, extract peony seeds and peony petal particle in the supercritical extraction of peony seed oil, and the pressure in setting extractor is 30Mpa, and temperature is 70 DEG C, the CO after extraction
2input separator with the mixed stream of peony seeds and peony petal essential oil and carry out decompression separation, carbon dioxide flow 27kg/h, the pressure in separator is 8Mpa, and temperature is 45 DEG C, the CO after separation
2through liquefier liquefaction directly the defeated time hold tank of 28 DEG C recycle for next round extracting and separating, each takes turns 6 hours extracting and separating time, and after being separated, obtained elementary peony seeds and peony petal crude oil, for subsequent use;
Step 2: the elementary peony seeds obtained by step 1 and peony petal crude oil join in molecular still, vacuum tightness in setting molecular still is 1.6Pa, temperature is 73 DEG C, rotating brush film rotating speed in molecular still is 120r/min, until elementary peony seeds and peony petal crude oil are collected by heavy phase holding tank and light phase holding tank completely, collect in heavy phase holding tank and obtain peony seeds and peony petal crude oil, for subsequent use;
Step 3: the peony seeds obtained by step 2 and peony petal crude oil join in molecular still again, the vacuum tightness reset in molecular still is 1.9Pa, temperature is 64 DEG C, rotating brush film rotating speed in molecular still is 120r/min, until peony seeds and peony petal crude oil are collected by heavy phase holding tank and light phase holding tank completely, collect in heavy phase holding tank and obtain peony essential oil.
Embodiment 2
Step 1: peony seeds is carried out preferably, wash the removal of impurity and earth with water, pick out coloury peony petal to wash, the ratio of peony seeds and peony petal is 8: 1, clean peony seeds and peony petal are drenched solid carbon dioxide to be divided stand-by, the peony seeds divide pouring solid carbon dioxide and peony petal put into solar energy baking equipment dries, wherein be provided with temperature sensor in drying shed, guarantee that bake out temperature in drying shed is between 68 DEG C, drying time was at 7 hours, water content is less than 7%, peony seeds after oven dry and peony petal are ground into chaff shape by disintegrating apparatus, obtain peony seeds and peony petal particle, for subsequent use,
Be encased in extraction kettle by 280kg peony seeds and peony petal particle, start extraction, extraction temperature is 45 DEG C, and extracting pressure is 26Mpa, extraction time 135min, closes extractor, checks and guarantees that sealing is tight, uses high-pressure pump by the liquid CO in hold tank
2pump into vaporizer, gasification is input in extractor after critical fluids state, adds peony petal, extract peony seeds and peony petal particle in the supercritical extraction of peony seed oil, and the pressure in setting extractor is 26Mpa, and temperature is 77 DEG C, the CO after extraction
2input separator with the mixed stream of peony seeds and peony petal essential oil and carry out decompression separation, carbon dioxide flow 27kg/h, the pressure in separator is 9Mpa, and temperature is 76 DEG C, the CO after separation
2through liquefier liquefaction directly the defeated time hold tank of 28 DEG C recycle for next round extracting and separating, each takes turns 7 hours extracting and separating time, and after being separated, obtained elementary peony seeds and peony petal crude oil, for subsequent use;
Step 2: the elementary peony seeds obtained by step 1 and peony petal crude oil join in molecular still, vacuum tightness in setting molecular still is 1.7Pa, temperature is 77 DEG C, rotating brush film rotating speed in molecular still is 120r/min, until elementary peony seeds and peony petal crude oil are collected by heavy phase holding tank and light phase holding tank completely, collect in heavy phase holding tank and obtain peony seeds and peony petal crude oil, for subsequent use;
Step 3: the peony seeds obtained by step 2 and peony petal crude oil join in molecular still again, the vacuum tightness reset in molecular still is 1.3Pa, temperature is 68 DEG C, rotating brush film rotating speed in molecular still is 120r/min, until peony seeds and peony petal crude oil are collected by heavy phase holding tank and light phase holding tank completely, collect in heavy phase holding tank and obtain peony essential oil.
Claims (1)
1. the supercritical CO of a peony essential oil
2extracting process, is characterized in that:
Step 1: peony seeds is carried out preferably, wash the removal of impurity and earth with water, pick out coloury peony petal to wash, the ratio of peony seeds and peony petal is 2: 1-10: 1, clean peony seeds and peony petal are drenched solid carbon dioxide to be divided stand-by, the peony seeds divide pouring solid carbon dioxide and peony petal put into solar energy baking equipment dries, wherein be provided with temperature sensor in drying shed, guarantee that bake out temperature in drying shed is between 40-70 DEG C, drying time is at 3-8 hour, water content is less than 7%, peony seeds after oven dry and peony petal are ground into chaff shape by disintegrating apparatus, obtain peony seeds and peony petal particle, for subsequent use,
Be encased in extraction kettle by 250-400kg peony seeds and peony petal particle, start extraction, extraction temperature is 35-55 DEG C, extracting pressure is 25-28Mpa, extraction time 120-150min, closes extractor, inspection guarantees that sealing is tight, uses high-pressure pump by the liquid CO in hold tank
2pump into vaporizer, gasification is input in extractor after critical fluids state, adds peony petal in the supercritical extraction of peony seed oil, peony seeds and peony petal particle are extracted, pressure in setting extractor is 10-32Mpa, and temperature is 32-80 DEG C, the CO after extraction
2input separator with the mixed stream of peony seeds and peony petal essential oil and carry out decompression separation, carbon dioxide flow 25-30kg/h, the pressure in separator is 4-10Mpa, and temperature is 20-80 DEG C, the CO after separation
2through liquefier liquefaction directly the defeated time hold tank of 20-30 DEG C recycle for next round extracting and separating, each takes turns extracting and separating time 2-8 hour, and after being separated, obtained elementary peony seeds and peony petal crude oil, for subsequent use;
Step 2: the elementary peony seeds obtained by step 1 and peony petal crude oil join in molecular still, vacuum tightness in setting molecular still is 1.0-2.0Pa, temperature is 60-80 DEG C, rotating brush film rotating speed in molecular still is 120r/min, until elementary peony seeds and peony petal crude oil are collected by heavy phase holding tank and light phase holding tank completely, collect in heavy phase holding tank and obtain peony seeds and peony petal crude oil, for subsequent use;
Step 3: the peony seeds obtained by step 2 and peony petal crude oil join in molecular still again, the vacuum tightness reset in molecular still is 1.0-2.0Pa, temperature is 60-80 DEG C, rotating brush film rotating speed in molecular still is 120r/min, until peony seeds and peony petal crude oil are collected by heavy phase holding tank and light phase holding tank completely, collect in heavy phase holding tank and obtain peony essential oil.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105273833A (en) * | 2015-11-30 | 2016-01-27 | 中华全国供销合作总社南京野生植物综合利用研究所 | Method for carrying out supercritical CO2 extraction on kosteletzkya virginica L. flower essential oil |
| CN105273846A (en) * | 2015-11-30 | 2016-01-27 | 中华全国供销合作总社南京野生植物综合利用研究所 | Method for carrying out supercritical CO2 extraction on kosteletzkya virginica L. leaf essential oil |
| CN105733812A (en) * | 2016-03-17 | 2016-07-06 | 金沙鑫顺农业发展有限公司 | Supercritical CO2 extraction method of peony essence |
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| CN101647872A (en) * | 2009-09-07 | 2010-02-17 | 兰州牡丹园艺开发公司 | Peony essential oil soft capsule and preparation method thereof |
| CN102391913A (en) * | 2011-10-10 | 2012-03-28 | 杨永庆 | Supercritical extraction method for peony essence and application of method |
| CN103271860A (en) * | 2013-06-18 | 2013-09-04 | 菏泽尧舜牡丹生物科技有限公司 | Skin care oil containing peony oil and preparation method thereof |
| CN103815059A (en) * | 2014-03-06 | 2014-05-28 | 洛阳春魁农业开发有限公司 | Blend oil containing peony seed oil and preparation method thereof |
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2015
- 2015-06-24 CN CN201510377536.XA patent/CN105038946A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101647872A (en) * | 2009-09-07 | 2010-02-17 | 兰州牡丹园艺开发公司 | Peony essential oil soft capsule and preparation method thereof |
| CN102391913A (en) * | 2011-10-10 | 2012-03-28 | 杨永庆 | Supercritical extraction method for peony essence and application of method |
| CN103271860A (en) * | 2013-06-18 | 2013-09-04 | 菏泽尧舜牡丹生物科技有限公司 | Skin care oil containing peony oil and preparation method thereof |
| CN103815059A (en) * | 2014-03-06 | 2014-05-28 | 洛阳春魁农业开发有限公司 | Blend oil containing peony seed oil and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105273833A (en) * | 2015-11-30 | 2016-01-27 | 中华全国供销合作总社南京野生植物综合利用研究所 | Method for carrying out supercritical CO2 extraction on kosteletzkya virginica L. flower essential oil |
| CN105273846A (en) * | 2015-11-30 | 2016-01-27 | 中华全国供销合作总社南京野生植物综合利用研究所 | Method for carrying out supercritical CO2 extraction on kosteletzkya virginica L. leaf essential oil |
| CN105733812A (en) * | 2016-03-17 | 2016-07-06 | 金沙鑫顺农业发展有限公司 | Supercritical CO2 extraction method of peony essence |
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Application publication date: 20151111 |