CN104087424A - Method for one-step extraction and separation of essential oil, water solution and lipid of fresh peony flowers - Google Patents
Method for one-step extraction and separation of essential oil, water solution and lipid of fresh peony flowers Download PDFInfo
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Abstract
The invention relates to a method for one-step extraction and separation of essential oil, water solution and lipid of fresh peony flowers. The method comprises the following steps: on the basis of taking methyl ether or a mixed liquid of methyl ether, butane, propane and ethanol as a solvent, extracting the preprocessed fresh peony flowers in a sealed state at 10-50 DEG C under the pressure of 0.1-0.2MPa for 10-60 minutes; after the extraction is finished, performing solid-liquid separation, collecting an extraction liquid, and statically layering, wherein the peony essential oil is on the upper layer and the peony flower water solution and the peony flower lipid are on the lower layer; performing negative-pressure concentration on the lower-layer solution, and cooling and recovering a condensed liquid to obtain a peony flower water solution extraction liquid, wherein the concentrated liquid is the peony flower lipid. According to the method, the raw material variety is not limited, raw material resources can be fully utilized, the extraction rate is high, the residue content is low, the process is simple, the efficiency is high, the investment is low, and clean dewatered peony petals (filaments), peony flower essential oil, peony flower water solution extraction liquid and peony flower lipid can be obtained at the same time. The method is suitable for not only the fresh peony flowers but also rose flowers, rosa chinensis flowers, jasmine flowers, tea flowers, lavender and the like, the production cost is low, and the competitive advantage in market is remarkable.
Description
Technical field
The present invention relates to an a kind of step abstracting tree peony ethereal oil of flower, the aqueous solution, lipid and separated method thereof.
Background technology
Tree Peony flower is national flower in China, just views and admires in the past, the economic worth of Tree Peony flower is not further developed, and utilizes.Tree Peony flower essential oil, the aqueous solution etc. are mainly used in makeup aspect, and the extraction of fresh peony flower essential oil, the aqueous solution, lipid, separation will have certain pushing effect to tree peony industry development.
CN102080018A discloses the making method of Tree Peony flower essential oil: fresh flower with 10% NaCL pickle, wet distillation, water molecules hold back method removal of impurities, ethyl acetate extraction, reclaim under reduced pressure ethyl acetate, with wet distillation, anhydrous sodium sulfate dehydration, filtration etc., produce Tree Peony flower essential oil method again.This technique is loaded down with trivial details, essential oil yield is low, there is no this product of Tree Peony flower aqueous solution extraction liquid.
CN10239193A discloses the supercritical extraction method of peony essential oil: tree peony root, stem, leaf and Hua Lingan, oven dry moisture, in 7%, are pulverized, by the technique of supercritical carbon dioxide extraction, produced peony essential oil method.Technique shortcoming is: dry cause the loss of tree peony fresh idea perfume (or spice), facility investment large, there is no this product of Tree Peony flower aqueous solution extraction liquid.
CN103305344A disclose a kind of from fresh peony flower the method for abstracting tree peony essential oil: the fresh peony flower of plucking of take is raw material, with supercritical carbon dioxide extraction tree peony medicinal extract, makes the method for peony essential oil with molecular distillation abstracting tree peony medicinal extract.This technique shortcoming is: production cost is high, facility investment is large, there is no this product of Tree Peony flower aqueous solution extraction liquid.
CN100577783C discloses a kind of method of oil and grease extracting: plant seed is pulverized to 10～20 orders, take methyl ether as solvent, according to the molten ratio of material, be 1:2～1:24, extraction time is 30～120 minutes, extraction temperature is under 30～90 ℃ of conditions, in extraction, separating plant seed, the method for grease, does not relate to the extraction of ethereal oil of flower and the fresh flower aqueous solution.
CN101484562B discloses the method with liquid methyl ether extraction highly unsaturated lipids: plant, marine animal, microorganism are dried, moisture be raw material heavy 5～30%, with approaching critical CO
2state under, the method for highly unsaturated lipids of extraction gained, does not relate to the extraction of ethereal oil of flower and the fresh flower aqueous solution.
The large production cost of the loaded down with trivial details essential oil of these processing method techniques loss part fragrance facility investment is high or do not relate to the extraction of fresh flower above, therefore propose a step abstracting tree peony ethereal oil of flower, the aqueous solution, lipid and separated method thereof, can make up the deficiency of above processing method.
Summary of the invention
The object of the present invention is to provide a kind of method of a step abstracting tree peony ethereal oil of flower, the aqueous solution, lipid.
With the mixed solution of methyl ether or methyl ether and butane, propane, ethanol as solvent, under air-tight state, extraction is through the fresh peony flower of pre-treatment, and the weight ratio of material and solvent is 1:0.8～6,10～50 ℃ of temperature, pressure 0.1～1.2MPa, extraction time is 10～60min; After extraction finishes, carry out solid-liquid separation, the solid phase after extraction is degreasing (water) peony petal (silk); Collect extraction liquid, static layering, upper strata is peony essential oil, lower floor is the Tree Peony flower aqueous solution and lipid; Lower floor's solution is carried out to negative pressure and concentrate, cooling recovery phlegma, obtains Tree Peony flower aqueous solution extraction liquid, and concentrated solution is Tree Peony flower lipid.
Adopt the present invention, not limited by raw material variety, can make full use of raw material resources, percentage extraction is high, slag is residual low, and technique is simple, efficiency is high, it is little to invest, and can obtain peony petal (silk), Tree Peony flower essential oil, Tree Peony flower aqueous solution extraction liquid, four kinds of products of Tree Peony flower lipid of clean dehydration simultaneously.The present invention is not only applicable to fresh peony flower, is also applicable to Rose, Flos Rosae Chinensis, Flower of Arabian Jasmine, camellia, lavandula angustifolia etc., and production cost is low, and market competition advantage is obvious.
Embodiment
Illustrate below and realize technical process of the present invention and implementation:
(1), technical process
(1) fresh flower pre-treatment: by the fresh peony flower of harvesting through rubbing, compressing tablet or directly remove Paeonia suffruticosa fresh flower juice through squeezing water;
(2) extraction: using the mixed solution of methyl ether or methyl ether and butane, propane, ethanol as solvent, fresh peony flower through pre-treatment is extracted, and the weight ratio of material and solvent is 1:0.8～6, and extraction temperature is 10～50 ℃, pressure 0.1～1.2MPa, extraction time is 10～60min; After extraction finishes, carry out solid-liquid separation, separated solid phase is pressed to above-mentioned extractant condition re-extract 2～8 times, the solid phase after extraction is degreasing (water) peony petal (silk);
(3) reclaim solvent: the liquid phase that (2) are separated is filtered or sedimentation, remove fine impurities wherein, decompression separation is gas phase and enriched material, and gas phase is compressed and liquefied to recovery solvent;
(4) thick product: will (3) separated enriched material control temperature is at 20～50 ℃, under condition of negative pressure, desolvation, obtains the mixed solution of Tree Peony flower essential oil, Tree Peony flower lipid, Tree Peony flower aqueous solution extraction liquid;
(5) static separation: by (4) gained mixed solution sedimentation, static, separated, obtaining upper strata is peony essential oil, and lower floor is the Tree Peony flower aqueous solution and lipid;
(6) refining Tree Peony flower aqueous solution extraction liquid: (1) gained Tree Peony flower juice is filtered, with (5) gained Tree Peony flower aqueous solution and lipid mixed solution, drop into vacuum concentration equipment, 30～85 ℃ of temperature, in pressure 1～1500Pa, carry out vacuum concentration, the collected phlegma of cooling recovery is Tree Peony flower aqueous solution extraction liquid, and the material after concentrating is Tree Peony flower lipid;
Described operating process all completes under complete totally enclosed processing condition.
(2), implementation
By embodiment, further illustrate method of the present invention below:
Embodiment 1: get according to the fresh peony flower sheet of step 1 preparation in above-mentioned technical process or silk 100 ㎏, be placed in extraction container, add 100 ㎏ methyl ethers, extraction temperature is 45 ℃, and extraction time is 60min; After extraction finishes, carry out solid-liquid separation, separated solid phase is pressed to above-mentioned processing condition re-extract 2～8 times, the solid phase after repeatedly extracting is degreasing (water) peony petal (silk); Liquid phase is filtered or sedimentation, remove fine impurities wherein, decompression separation is gas phase and enriched material, and gas phase is compressed and liquefied to recovery solvent; Enriched material is controlled to temperature at 20～50 ℃, and desolvation under the condition of be less than-0.085Mpa of gauge pressure, has just obtained the mixed solution of Tree Peony flower essential oil, Tree Peony flower lipid, Tree Peony flower aqueous solution extraction liquid; By this mixed solution sedimentation, static, separated, obtaining upper strata is peony essential oil, and lower floor is the Tree Peony flower aqueous solution and lipid; Lower floor's mixed solution is mixed with the Tree Peony flower liquid filtered liquid of pre-treatment gained, drop into vacuum concentration equipment, 30～85 ℃ of temperature, in pressure 1～1500Pa, carry out vacuum concentration, the collected phlegma of cooling recovery is Tree Peony flower aqueous solution extraction liquid, and the material after concentrating is Tree Peony flower lipid.
Embodiment 2: get according to the fresh peony flower sheet of step 1 preparation in above-mentioned technical process or silk 100 ㎏, be placed in extraction container, add 100 ㎏ methyl ethers and butane mixed solution, extraction temperature is 45 ℃, and extraction time is 30min; After extraction finishes, carry out solid-liquid separation, separated solid phase is pressed to above-mentioned processing condition re-extract 2 times, the solid phase after repeatedly extracting is degreasing (water) peony petal (silk); Liquid phase is filtered or sedimentation, remove fine impurities wherein, decompression separation is gas phase and enriched material, and gas phase is compressed and liquefied to recovery solvent; Enriched material is controlled to temperature at 20～50 ℃, and desolvation under the condition of be less than-0.085Mpa of gauge pressure, has just obtained the mixed solution of Tree Peony flower essential oil, Tree Peony flower lipid, Tree Peony flower aqueous solution extraction liquid; By this mixed solution sedimentation, static, separated, obtaining upper strata is peony essential oil, and lower floor is the Tree Peony flower aqueous solution and lipid; Lower floor's mixed solution is mixed with the Tree Peony flower liquid filtered liquid of pre-treatment gained, drop into vacuum concentration equipment, 30～85 ℃ of temperature, in pressure 1～1500Pa, carry out vacuum concentration, the collected phlegma of cooling recovery is Tree Peony flower aqueous solution extraction liquid, and the material after concentrating is Tree Peony flower lipid.
Embodiment 3: get according to the fresh peony flower sheet of step 1 preparation in above-mentioned technical process or silk 100 ㎏, be placed in extraction container, add the mixed solution of 100 ㎏ methyl ethers and ethanol, extraction temperature is 45 ℃, and extraction time is 40min; After extraction finishes, carry out solid-liquid separation, separated solid phase is pressed to above-mentioned processing condition re-extract 5 times, the solid phase after repeatedly extracting is degreasing (water) peony petal (silk); Liquid phase is filtered or sedimentation, remove fine impurities wherein, decompression separation is gas phase and enriched material, and gas phase is compressed and liquefied to recovery solvent; Enriched material is controlled to temperature at 20～50 ℃, and desolvation under the condition of be less than-0.085Mpa of gauge pressure, has just obtained the mixed solution of Tree Peony flower essential oil, Tree Peony flower lipid, Tree Peony flower aqueous solution extraction liquid; By this mixed solution sedimentation, static, separated, obtaining upper strata is peony essential oil, and lower floor is the Tree Peony flower aqueous solution and lipid; Lower floor's mixed solution is mixed with the Tree Peony flower liquid filtered liquid of pre-treatment gained, drop into vacuum concentration equipment, 30～85 ℃ of temperature, in pressure 1～1500Pa, carry out vacuum concentration, the collected phlegma of cooling recovery is Tree Peony flower aqueous solution extraction liquid, and the material after concentrating is Tree Peony flower lipid.
Embodiment 4: get according to the fresh peony flower sheet of step 1 preparation in above-mentioned technical process or silk 100 ㎏, be placed in extraction container, add 600 ㎏ methyl ethers, extraction temperature is 35 ℃, and extraction time is 40min; After extraction finishes, carry out solid-liquid separation, separated solid phase is pressed to above-mentioned processing condition re-extract 5 times, the solid phase after repeatedly extracting is degreasing (water) peony petal (silk); Liquid phase is filtered or sedimentation, remove fine impurities wherein, decompression separation is gas phase and enriched material, and gas phase is compressed and liquefied to recovery solvent; Enriched material is controlled to temperature at 20～50 ℃, and desolvation under the condition of be less than-0.085Mpa of gauge pressure, has just obtained the mixed solution of Tree Peony flower essential oil, Tree Peony flower lipid, Tree Peony flower aqueous solution extraction liquid; By this mixed solution sedimentation, static, separated, obtaining upper strata is peony essential oil, and lower floor is the Tree Peony flower aqueous solution and lipid; Lower floor's mixed solution is mixed with the Tree Peony flower liquid filtered liquid of pre-treatment gained, drop into vacuum concentration equipment, 30～85 ℃ of temperature, in pressure 1～1500Pa, carry out vacuum concentration, the collected phlegma of cooling recovery is Tree Peony flower aqueous solution extraction liquid, and the material after concentrating is Tree Peony flower lipid.
Embodiment 5: get according to the fresh peony flower sheet of step 1 preparation in above-mentioned technical process or silk 100 ㎏, be placed in extraction container, add the mixed solution of 200 ㎏ methyl ethers and butane, extraction temperature is 45 ℃, and extraction time is 40min; After extraction finishes, carry out solid-liquid separation, separated solid phase is pressed to above-mentioned processing condition re-extract 5 times, the solid phase after repeatedly extracting is degreasing (water) peony petal (silk); Liquid phase is filtered or sedimentation, remove fine impurities wherein, decompression separation is gas phase and enriched material, and gas phase is compressed and liquefied to recovery solvent; Enriched material is controlled to temperature at 20～50 ℃, and desolvation under the condition of be less than-0.085Mpa of gauge pressure, has just obtained the mixed solution of Tree Peony flower essential oil, Tree Peony flower lipid, Tree Peony flower aqueous solution extraction liquid; By this mixed solution sedimentation, static, separated, obtaining upper strata is peony essential oil, and lower floor is the Tree Peony flower aqueous solution and lipid; Lower floor's mixed solution is mixed with the Tree Peony flower liquid filtered liquid of pre-treatment gained, drop into vacuum concentration equipment, 30～85 ℃ of temperature, in pressure 1～1500Pa, carry out vacuum concentration, the collected phlegma of cooling recovery is Tree Peony flower aqueous solution extraction liquid, and the material after concentrating is Tree Peony flower lipid.
Claims (5)
1. the method for a step abstracting tree peony ethereal oil of flower, the aqueous solution, lipid, with the mixed solution of methyl ether or methyl ether and butane, propane, ethanol as solvent, under air-tight state, extraction is through the fresh peony flower of pre-treatment, after extraction finishes, carry out solid-liquid separation, the solid phase after extraction is degreasing Tree Peony flower; Collect extraction liquid, static layering, upper strata is peony essential oil, lower floor is the Tree Peony flower aqueous solution and lipid; Lower floor's solution is carried out to negative pressure and concentrate, cooling recovery phlegma, obtains Tree Peony flower aqueous solution extraction liquid, and concentrated solution is Tree Peony flower lipid; It is characterized in that:
(1) fresh flower pre-treatment: by the fresh peony flower of harvesting through rubbing, compressing tablet or directly remove Paeonia suffruticosa fresh flower juice through squeezing water;
(2) extraction: using the mixed solution of methyl ether or methyl ether and butane, propane, ethanol as solvent, fresh peony flower through pre-treatment is extracted, and the weight ratio of material and solvent is 1:0.8～6, and extraction temperature is 10～50 ℃, pressure 0.1～1.2MPa, extraction time is 10～60min; After extraction finishes, carry out solid-liquid separation, separated solid phase is pressed to above-mentioned extractant condition re-extract 2～8 times, the solid phase after extraction is degreasing (water) peony petal (silk);
(3) reclaim solvent: the liquid phase that (2) are separated is filtered or sedimentation, remove fine impurities wherein, decompression separation is gas phase and enriched material, and gas phase is compressed and liquefied to recovery solvent;
(4) thick product: will (3) separated enriched material control temperature is at 20～50 ℃, under condition of negative pressure, desolvation, obtains the mixed solution of Tree Peony flower essential oil, Tree Peony flower lipid, Tree Peony flower aqueous solution extraction liquid;
(5) static separation: by (4) gained mixed solution sedimentation, static, separated, obtaining upper strata is peony essential oil, and lower floor is the Tree Peony flower aqueous solution and lipid;
(6) refining Tree Peony flower aqueous solution extraction liquid: (1) gained Tree Peony flower juice is filtered, with (5) gained Tree Peony flower aqueous solution and lipid mixed solution, drop into vacuum concentration equipment, 30～85 ℃ of temperature, in pressure 1～1500Pa, carry out negative pressure concentrated, the collected phlegma of cooling recovery is Tree Peony flower aqueous solution extraction liquid, and the material after concentrating is Tree Peony flower lipid;
Described operating process all completes under complete totally enclosed processing condition.
2. the method for a step abstracting tree peony ethereal oil of flower according to claim 1, the aqueous solution, lipid, is characterized in that: described solvent is methyl ether single solvent or methyl ether and the mixed solvent of butane, propane, one or more any ratios of ethanol.
3. the method for a step abstracting tree peony ethereal oil of flower according to claim 1, the aqueous solution, lipid, it is characterized in that: the weight ratio of described fresh peony flower and solvent is 1:0.8～3, extraction temperature is 10～50 ℃, and extraction time is 10～60min, and re-extract number of times is 2～8 times.
4. the method for a step abstracting tree peony ethereal oil of flower according to claim 1, the aqueous solution, lipid, it is characterized in that: the temperature that described product separation is controlled enriched material is 20～50 ℃, under the condition of be less than-0.085Mpa of gauge pressure, desolvation, adopts settlement separate method that essential oil and aqueous solution extraction liquid, lipid mixed solution are separated.
5. the method for a step abstracting tree peony ethereal oil of flower according to claim 1, the aqueous solution, lipid, it is characterized in that: the separation method of aqueous solution extraction liquid, lipid adopts vacuum concentration, the liquid water that the method that condensation is reclaimed is collected is aqueous solution extraction liquid, material after concentrated is lipid, 30～85 ℃ of temperature, in pressure 1～1500Pa.
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| CN106552442A (en) * | 2016-11-21 | 2017-04-05 | 菏泽尧舜牡丹生物科技有限公司 | A kind of handling process to peony slag after SCF-CO 2 |
| CN108219945A (en) * | 2018-03-14 | 2018-06-29 | 河南科技大学 | A kind of fresh flower crystal oil and more odor types flower crystal's oil |
| CN108865440A (en) * | 2018-05-23 | 2018-11-23 | 菏泽瑞璞牡丹产业科技发展有限公司 | A kind of method of subcritical abstraction fresh peony flower medicinal extract |
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| CN109370779A (en) * | 2018-11-29 | 2019-02-22 | 重庆唐风绿榄农业科技发展有限公司 | A kind of production method of olive floral type olive oil |
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| CN112961729A (en) * | 2021-03-24 | 2021-06-15 | 西北农林科技大学 | Method for optimizing extraction of peony hydrolat under negative pressure distillation condition |
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| CN106552442B (en) * | 2016-11-21 | 2018-08-31 | 菏泽尧舜牡丹生物科技有限公司 | It is a kind of to supercritical CO2The treatment process of peony slag after extraction |
| CN108219945B (en) * | 2018-03-14 | 2021-07-30 | 河南科技大学 | Flower water essential oil and multi-fragrance flower water essential oil |
| CN108219945A (en) * | 2018-03-14 | 2018-06-29 | 河南科技大学 | A kind of fresh flower crystal oil and more odor types flower crystal's oil |
| CN108865440A (en) * | 2018-05-23 | 2018-11-23 | 菏泽瑞璞牡丹产业科技发展有限公司 | A kind of method of subcritical abstraction fresh peony flower medicinal extract |
| CN109055012A (en) * | 2018-08-08 | 2018-12-21 | 阜阳师范学院 | A kind of extracting method and its application of chinese rose essential oil |
| CN109370779A (en) * | 2018-11-29 | 2019-02-22 | 重庆唐风绿榄农业科技发展有限公司 | A kind of production method of olive floral type olive oil |
| CN111849642A (en) * | 2020-07-16 | 2020-10-30 | 菏泽瑞璞牡丹产业科技发展有限公司 | Peony fresh flower water and preparation method thereof |
| CN112961729A (en) * | 2021-03-24 | 2021-06-15 | 西北农林科技大学 | Method for optimizing extraction of peony hydrolat under negative pressure distillation condition |
| CN112961729B (en) * | 2021-03-24 | 2023-10-13 | 西北农林科技大学 | Method for extracting peony hydrosol under optimized negative pressure distillation condition |
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