CN104087424B - The method that one step extracts, separates fresh peony flower quintessence oil, aqueous solution, lipid - Google Patents
The method that one step extracts, separates fresh peony flower quintessence oil, aqueous solution, lipid Download PDFInfo
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Abstract
A kind of method that the present invention relates to a step abstracting tree peony ethereal oil of flower, aqueous solution, lipid.With methyl ether or methyl ether and butane, propane, ethanol mixed liquor as solvent, under air-tight state, extract the fresh peony flower through pre-treatment, temperature 10～50 DEG C, pressure 0.1～1.2MPa, extraction time is 10～60min；After extraction terminates, carrying out solid-liquid separation, collect extract, static layering, upper strata is peony essential oil, and lower floor is Flos Moutan aqueous solution and lipid；Lower floor's solution carries out negative pressure concentration, and condensed fluid is reclaimed in cooling, obtains Flos Moutan aqueous solution extraction liquid, and concentrated solution is Flos Moutan lipid.Adopt the present invention, do not limited by raw material variety, raw material resources can be made full use of, extraction yield is high, slag is residual low, and technique is simple, efficiency is high, it is little to invest, and can obtain the peony petal (silk) of clean dehydration, peony essential oil, Flos Moutan aqueous solution extraction liquid, four kinds of products of Flos Moutan lipid simultaneously.Being applicable not only to fresh peony flower, apply also for Flos Rosae Rugosae, Flos Rosae Chinensis, Flos Jasmini Sambac, Flos Camelliae Japonicae, lavandula angustifolia etc., production cost is low, and market competition advantage is obvious.
Description
Technical field
A kind of method that the present invention relates to a step abstracting tree peony ethereal oil of flower, aqueous solution, lipid and separation thereof.
Background technology
Flos Moutan is national flower in China, simply views and admires in the past, it does not have the economic worth of Flos Moutan is developed further, utilizes.Peony essential oil, aqueous solution etc. are used primarily in cosmetics aspect, and Paeonia suffruticosa industry development will be had certain impetus by fresh peony flower quintessence oil, aqueous solution, the extraction of lipid, separation.
CN102080018A discloses the manufacture method of peony essential oil: flower with the NaCL of 10% pickle, vapor distillation, hydrone retain method remove impurity, extraction into ethyl acetate, recovered under reduced pressure ethyl acetate, produce peony essential oil method with vapor distillation, anhydrous sodium sulfate dehydration, filtration etc. again.This technique is loaded down with trivial details, quintessence oil yield is low, do not have Flos Moutan this product of aqueous solution extraction liquid.
CN10239193A discloses the supercritical extraction method of peony essential oil: by root of Paeonia suffruticosa Ardr., stem, leaf and Hua Lingan, drying moisture within 7%, pulverizes, produces peony essential oil method by the technique of supercritical carbon dioxide extraction.Processing disadvantages is: drying causes the loss of Paeonia suffruticosa fresh idea perfume, equipment investment is big, do not have Flos Moutan this product of aqueous solution extraction liquid.
CN103305344A discloses a kind of method of abstracting tree peony quintessence oil from fresh peony flower: with the fresh peony flower of harvesting for raw material, by supercritical carbon dioxide extraction Paeonia suffruticosa extractum, the method preparing peony essential oil with molecular distillation abstracting tree peony extractum.This processing disadvantages is: production cost is high, equipment investment is big, do not have Flos Moutan this product of aqueous solution extraction liquid.
CN100577783C discloses a kind of method of oil and grease extracting: plant seed is pulverized 10～20 orders, with methyl ether for solvent, according to expecting that molten ratio is 1:2～1:24, extraction time is 30～120 minutes, extraction temperature is under 30～90 DEG C of conditions, the method of oils and fats in extraction, separating plant seed, it does not have relate to ethereal oil of flower and the extraction of flower aqueous solution.
CN101484562B discloses the method extracting highly unsaturated lipids with liquid methyl ether: plant, marine animal, microorganism being dried, moisture is the 5～30% of raw material weight, uses close to critical CO2State under, extract the method for highly unsaturated lipids of gained, it does not have relate to ethereal oil of flower and the extraction of flower aqueous solution.
The loaded down with trivial details quintessence oil of the above process technique loses the big production cost height of part fragrance equipment investment or is not related to the extraction of flower, therefore the method proposing a step abstracting tree peony ethereal oil of flower, aqueous solution, lipid and separation thereof, can overcome the disadvantages that the deficiency of process above method.
Summary of the invention
A kind of method that it is an object of the invention to provide a step abstracting tree peony ethereal oil of flower, aqueous solution, lipid.
With methyl ether or methyl ether and butane, propane, ethanol mixed liquor as solvent, under air-tight state, the weight ratio extracting the fresh peony flower through pre-treatment, material and solvent is 1:0.8～6, temperature 10～50 DEG C, pressure 0.1～1.2MPa, extraction time is 10～60min；After extraction terminates, carrying out solid-liquid separation, the solid phase after extracting is defat (water) peony petal (silk)；Collecting extract, static layering, upper strata is peony essential oil, and lower floor is Flos Moutan aqueous solution and lipid；Lower floor's solution carries out negative pressure concentration, and condensed fluid is reclaimed in cooling, obtains Flos Moutan aqueous solution extraction liquid, and concentrated solution is Flos Moutan lipid.
Adopt the present invention, do not limited by raw material variety, raw material resources can be made full use of, extraction yield is high, slag is residual low, and technique is simple, efficiency is high, it is little to invest, and can obtain the peony petal (silk) of clean dehydration, peony essential oil, Flos Moutan aqueous solution extraction liquid, four kinds of products of Flos Moutan lipid simultaneously.The present invention is applicable not only to fresh peony flower, applies also for Flos Rosae Rugosae, Flos Rosae Chinensis, Flos Jasmini Sambac, Flos Camelliae Japonicae, lavandula angustifolia etc., and production cost is low, and market competition advantage is obvious.
Detailed description of the invention
The technological process and implementation that realize the present invention are specifically described below:
(1), technological process
(1) flower pre-treatment: by the fresh peony flower of harvesting through rubbing, tabletting or directly through squeezing water elimination Paeonia suffruticosa flower juice；
(2) extract: using methyl ether or methyl ether and butane, propane, ethanol mixed liquor 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 DEG C, pressure 0.1～1.2MPa, extraction time is 10～60min；Extraction carries out solid-liquid separation after terminating, and the solid phase separated is repeated extraction 2～8 times by above-mentioned extractant condition, and the solid phase after extracting is defat (water) peony petal (silk)；
(3) recycling design: the liquid phase that (2) are separated is filtered or settles, and removes fine impurities therein, and decompression separation is gas phase and concentrate, and gas phase is compressed and liquefied recycling design；
(4) thick product: the concentrate (3) separated controls temperature at 20～50 DEG C, under condition of negative pressure, desolvation, obtain the mixed liquor of peony essential oil, Flos Moutan lipid, Flos Moutan aqueous solution extraction liquid；
(5) static separation: by the sedimentation of (4) gained mixed liquor, static, separation, obtaining upper strata is peony essential oil, and lower floor is Flos Moutan aqueous solution and lipid；
(6) refining Flos Moutan aqueous solution extraction liquid: (1) gained Flos Moutan juice is filtered, with (5) gained Flos Moutan aqueous solution and lipid mixed liquor, put into vacuum concentration equipment, temperature 30～85 DEG C, within pressure 1～1500Pa, carrying out vacuum concentration, cooling is reclaimed collected condensed fluid and is Flos Moutan aqueous solution extraction liquid, and the material after concentration is Flos Moutan lipid；
Described operating process is all complete under completely enclosed process conditions.
(2), implementation
The method further illustrating the present invention by detailed description of the invention below:
Embodiment 1: take according in above-mentioned technological process step 1 preparation fresh peony flower sheet or silk 100, be placed in extraction container, add 100 methyl ethers, extraction temperature is 45 DEG C, and extraction time is 60min；Extraction carries out solid-liquid separation after terminating, and the solid phase separated is repeated extraction 2～8 times by above-mentioned process conditions, and the solid phase after repeatedly extracting is defat (water) peony petal (silk)；Liquid phase being filtered or settles, removing fine impurities therein, decompression separation is gas phase and concentrate, and gas phase is compressed and liquefied recycling design；Concentrate is controlled temperature at 20～50 DEG C, desolvation when gauge pressure is less than-0.085Mpa, just obtain the mixed liquor of peony essential oil, Flos Moutan lipid, Flos Moutan aqueous solution extraction liquid；By the sedimentation of this mixed liquor, static, separation, obtaining upper strata is peony essential oil, and lower floor is Flos Moutan aqueous solution and lipid；Lower floor's mixed liquor is mixed with the Flos Moutan liquid filtrate of pre-treatment gained, puts into vacuum concentration equipment, temperature 30～85 DEG C, within pressure 1～1500Pa, carrying out vacuum concentration, cooling is reclaimed collected condensed fluid and is Flos Moutan aqueous solution extraction liquid, and the material after concentration is Flos Moutan lipid.
Embodiment 2: taking according to the fresh peony flower sheet of step 1 preparation in above-mentioned technological process or silk 100, be placed in extraction container, add 100 methyl ethers and butane mixed liquor, extraction temperature is 45 DEG C, and extraction time is 30min；Extraction carries out solid-liquid separation after terminating, and repeats to extract 2 times by above-mentioned process conditions to the solid phase separated, and the solid phase after repeatedly extracting is defat (water) peony petal (silk)；Liquid phase being filtered or settles, removing fine impurities therein, decompression separation is gas phase and concentrate, and gas phase is compressed and liquefied recycling design；Concentrate is controlled temperature at 20～50 DEG C, desolvation when gauge pressure is less than-0.085Mpa, just obtain the mixed liquor of peony essential oil, Flos Moutan lipid, Flos Moutan aqueous solution extraction liquid；By the sedimentation of this mixed liquor, static, separation, obtaining upper strata is peony essential oil, and lower floor is Flos Moutan aqueous solution and lipid；Lower floor's mixed liquor is mixed with the Flos Moutan liquid filtrate of pre-treatment gained, puts into vacuum concentration equipment, temperature 30～85 DEG C, within pressure 1～1500Pa, carrying out vacuum concentration, cooling is reclaimed collected condensed fluid and is Flos Moutan aqueous solution extraction liquid, and the material after concentration is Flos Moutan lipid.
Embodiment 3: take according in above-mentioned technological process step 1 preparation fresh peony flower sheet or silk 100, be placed in extraction container, add the mixed liquor of 100 methyl ethers and ethanol, extraction temperature is 45 DEG C, and extraction time is 40min；Extraction carries out solid-liquid separation after terminating, and repeats to extract 5 times by above-mentioned process conditions to the solid phase separated, and the solid phase after repeatedly extracting is defat (water) peony petal (silk)；Liquid phase being filtered or settles, removing fine impurities therein, decompression separation is gas phase and concentrate, and gas phase is compressed and liquefied recycling design；Concentrate is controlled temperature at 20～50 DEG C, desolvation when gauge pressure is less than-0.085Mpa, just obtain the mixed liquor of peony essential oil, Flos Moutan lipid, Flos Moutan aqueous solution extraction liquid；By the sedimentation of this mixed liquor, static, separation, obtaining upper strata is peony essential oil, and lower floor is Flos Moutan aqueous solution and lipid；Lower floor's mixed liquor is mixed with the Flos Moutan liquid filtrate of pre-treatment gained, puts into vacuum concentration equipment, temperature 30～85 DEG C, within pressure 1～1500Pa, carrying out vacuum concentration, cooling is reclaimed collected condensed fluid and is Flos Moutan aqueous solution extraction liquid, and the material after concentration is Flos Moutan lipid.
Embodiment 4: take according in above-mentioned technological process step 1 preparation fresh peony flower sheet or silk 100, be placed in extraction container, add 600 methyl ethers, extraction temperature is 35 DEG C, and extraction time is 40min；Extraction carries out solid-liquid separation after terminating, and repeats to extract 5 times by above-mentioned process conditions to the solid phase separated, and the solid phase after repeatedly extracting is defat (water) peony petal (silk)；Liquid phase being filtered or settles, removing fine impurities therein, decompression separation is gas phase and concentrate, and gas phase is compressed and liquefied recycling design；Concentrate is controlled temperature at 20～50 DEG C, desolvation when gauge pressure is less than-0.085Mpa, just obtain the mixed liquor of peony essential oil, Flos Moutan lipid, Flos Moutan aqueous solution extraction liquid；By the sedimentation of this mixed liquor, static, separation, obtaining upper strata is peony essential oil, and lower floor is Flos Moutan aqueous solution and lipid；Lower floor's mixed liquor is mixed with the Flos Moutan liquid filtrate of pre-treatment gained, puts into vacuum concentration equipment, temperature 30～85 DEG C, within pressure 1～1500Pa, carrying out vacuum concentration, cooling is reclaimed collected condensed fluid and is Flos Moutan aqueous solution extraction liquid, and the material after concentration is Flos Moutan lipid.
Embodiment 5: take according in above-mentioned technological process step 1 preparation fresh peony flower sheet or silk 100, be placed in extraction container, add the mixed liquor of 200 methyl ethers and butane, extraction temperature is 45 DEG C, and extraction time is 40min；Extraction carries out solid-liquid separation after terminating, and repeats to extract 5 times by above-mentioned process conditions to the solid phase separated, and the solid phase after repeatedly extracting is defat (water) peony petal (silk)；Liquid phase being filtered or settles, removing fine impurities therein, decompression separation is gas phase and concentrate, and gas phase is compressed and liquefied recycling design；Concentrate is controlled temperature at 20～50 DEG C, desolvation when gauge pressure is less than-0.085Mpa, just obtain the mixed liquor of peony essential oil, Flos Moutan lipid, Flos Moutan aqueous solution extraction liquid；By the sedimentation of this mixed liquor, static, separation, obtaining upper strata is peony essential oil, and lower floor is Flos Moutan aqueous solution and lipid；Lower floor's mixed liquor is mixed with the Flos Moutan liquid filtrate of pre-treatment gained, puts into vacuum concentration equipment, temperature 30～85 DEG C, within pressure 1～1500Pa, carrying out vacuum concentration, cooling is reclaimed collected condensed fluid and is Flos Moutan aqueous solution extraction liquid, and the material after concentration is Flos Moutan lipid.
Claims (1)
1. the method for a step abstracting tree peony ethereal oil of flower, aqueous solution, lipid, with mixed liquor in one or more of methyl ether or methyl ether and butane, propane and ethanol as solvent, under air-tight state, extract the fresh peony flower through pre-treatment, after extraction terminates, carrying out solid-liquid separation, the solid phase after extracting is defat Flos Moutan；Collecting extract, static layering, upper strata is peony essential oil, and lower floor is Flos Moutan aqueous solution and lipid；Lower floor's solution carries out negative pressure concentration, and condensed fluid is reclaimed in cooling, obtains Flos Moutan aqueous solution extraction liquid, and concentrated solution is Flos Moutan lipid；It is characterized in that:
(1) flower pre-treatment: by the fresh peony flower of harvesting through rubbing, tabletting or directly through squeezing water elimination Paeonia suffruticosa flower juice；
(2) extract: using mixed liquor in one or more of methyl ether or methyl ether and butane, propane and ethanol as solvent, fresh peony flower through pre-treatment is extracted, the weight ratio of material and solvent is 1:0.8～6, extraction temperature is 10～50 DEG C, pressure 0.1～1.2MPa, extraction time is 10～60min；Extraction carries out solid-liquid separation after terminating, and the solid phase separated is repeated extraction 2～8 times by above-mentioned extractant condition, and the solid phase after extracting is defat peony petal；
(3) recycling design: the liquid phase that (2) are separated is filtered or settles, and removes fine impurities therein, and decompression separation is gas phase and concentrate, and gas phase is compressed and liquefied recycling design；
(4) thick product: the concentrate (3) separated controls temperature at 20～50 DEG C, under condition of negative pressure, desolvation, obtain the mixed liquor of peony essential oil, Flos Moutan lipid, Flos Moutan aqueous solution extraction liquid；
(5) static separation: by the sedimentation of (4) gained mixed liquor, static, separation, obtaining upper strata is peony essential oil, and lower floor is Flos Moutan aqueous solution and lipid；
(6) refining Flos Moutan aqueous solution extraction liquid: (1) gained Flos Moutan juice is filtered, with (5) gained Flos Moutan aqueous solution and lipid mixed liquor, put into vacuum concentration equipment, temperature 30～85 DEG C, within pressure 1～1500Pa, carrying out negative pressure concentration, cooling is reclaimed collected condensed fluid and is Flos Moutan aqueous solution extraction liquid, and the material after concentration is Flos Moutan lipid；
Described operating process is all complete under completely enclosed process conditions.
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