CN108219959A - A kind of method that essential oil is extracted from peony petal - Google Patents
A kind of method that essential oil is extracted from peony petal Download PDFInfo
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- CN108219959A CN108219959A CN201810185707.2A CN201810185707A CN108219959A CN 108219959 A CN108219959 A CN 108219959A CN 201810185707 A CN201810185707 A CN 201810185707A CN 108219959 A CN108219959 A CN 108219959A
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- peony
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F289/00—Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds not provided for in groups C08F251/00 - C08F287/00
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Polymers & Plastics (AREA)
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- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a kind of methods that essential oil is extracted from peony petal, include the following steps：Fresh peony petal and water are mixed, by crushing, after ultrasonication, are centrifugally separating to obtain peong flower juice；Super absorbent resin is added in peong flower juice, stirring 10 after twenty minutes, stands 20 30 minutes, obtains gel peony extract；Supercritical carbon dioxide extracting is carried out to gel peony extract, obtains peony essential oil.The method of the present invention extracts the derived essential oil in peony to greatest extent using fresh peony petal as raw material, is a kind of method that peony essential oil efficiently, is quickly extracted from peony.
Description
Technical field
The present invention relates to peony essential oil preparation field more particularly to a kind of methods that essential oil is extracted from peony petal.
Background technology
Peony essential oil is that isolated volatile oily liquids that has is extracted from peony, therein most of
Volatile ingredient is the substance for having the aromatic odors such as the fragrance of a flower, fruity.In addition, peony essential oil is rich in the ammonia that a variety of human bodies need
Base acid and trace element, have and resist sensitivity, improve blood circulation, and beautifying face and moistering lotion promotes cytothesis, alleviates skin ageing,
The effects that adjusting skin problem, balancing hormone secretion in women body can make the raw material of medicine, food, beverage, cosmetics.
At present, the extraction of plants essential oil and isolation technics mainly have steam distillation, solvent extraction, microwave abstracting
Method, ultrasonic extraction, supercritical fluid extraction etc..Supercritical carbon dioxide extraction method is a kind of emerging extraction of essential oil skill
Art, compared with traditional chemical extraction method, not only extraction efficiency is high for supercritical carbon dioxide extraction method, the essential oil purity extracted
Height, and the active constituent of essential oil is saved to greatest extent.Supercritical carbon dioxide extraction method is chiefly used in using dried flower as raw material
Essential oil is prepared, such as using fresh flower as raw material, then contain moisture in the extract being obtained by extraction, it is also necessary to carry out water-oil separating ability
Obtain pure essential oil.And dried flower is during preparation and preservation, the volatile ingredient in flowers can be largely lost in, prepared by dried flower
The yield of essential oil prepares essential oil less than fresh flower.For this purpose, the present invention has developed a kind of side that essential oil is extracted from fresh peony petal
Method.
Invention content
Technical problems based on background technology, the present invention propose a kind of side that essential oil is extracted from peony petal
Method, the method for the present invention extract the derived essential oil in peony to greatest extent using fresh peony petal as raw material.
The present invention provides a kind of methods that essential oil is extracted from peony petal, include the following steps：
S1, fresh peony petal and water are mixed, by crushing, after ultrasonication, is centrifugally separating to obtain peong flower juice；
Super absorbent resin is added in S2, the peong flower juice obtained in S1, after stirring 10-20 minutes, stands 20-30 minutes,
Obtain gel peony extract；
S3, supercritical carbon dioxide extracting is carried out to obtaining gel peony extract in S2, obtains peony essential oil.
Preferably, the raw material of super absorbent resin includes by weight in S2：12-15 parts of cornstarch, acrylic acid 65-70
Part, 5-8 parts of corn stalk powder, 0.5-0.7 parts of potassium peroxydisulfate, N, N ' -0.06-0.08 parts of methylene-bisacrylamide, quality point
Sodium hydroxide solution 85-95 part, water 15-17 part of the number for 26%-29%.
Preferably, in the raw material of super absorbent resin, the water content of corn stalk powder is 5%-8%, and granularity is 60-80 mesh
Preferably, the preparation method of super absorbent resin includes the following steps in S2：
Step 1: cornstarch is added in 70-80 DEG C of water, constant temperature stirs 40-50 minutes, the starch solution A being gelatinized；
Step 2: acrylic acid is added in sodium hydroxide solution, stirs 20-30 minutes, add corn stalk powder, persulfuric acid
Potassium, N, N '-methylene-bisacrylamide, stir evenly, and obtain mixed solution B；
Step 3: the mixed solution B obtained in the starch solution A and step 2 that are obtained in step 1 is uniformly mixed, it is put into micro-
Microwave treatment 3-5 minutes, microwave power 250-300W in wave reactor, dry, crushing obtains being used to prepare peony essential oil
Super absorbent resin.
Preferably, temperature dry in step 3 is 70-80 DEG C, and the time is 15-20 hours.
Preferably, the super absorbent resin granularity for being used to prepare peony essential oil that step 3 obtains after crushing is 70-80 mesh.
Preferably, the weight ratio of fresh peony petal and water is 1 in S1:1-1.3.
Preferably, the additive amount of super absorbent resin is 0.02-0.04 times of peong flower juice weight in S2.
Preferably, S3, which surpasses, closes in carbon dioxide abstraction, and the pressure of extraction is 23-35Mpa, and extraction temperature is 35-45 DEG C,
Extraction time is 50-90 minutes, carbon dioxide flow 15-18L/h.
Preferably, S3, which surpasses, closes in carbon dioxide abstraction, the supercritical carbon dioxide extracting instrument used there are two separating still,
The pressure of first separating still is 8-10Mpa, and temperature is 40-45 DEG C, and the pressure of the second separating still is 3-5Mpa, temperature 30-35
℃。
Preferably, surpass in S3 and close on carbon dioxide abstraction and use cyclohexane as entrainer.
Preferably, surpass in S3 and close on carbon dioxide abstraction, the flow of entrainer cyclohexane is the 6%- of carbon dioxide flow
8%。
Preferably, the ultrasonic power of ultrasonication is 200-300w, frequency 28-32Hz, ultrasonic time 15- in S1
20min。
The method provided by the invention that essential oil is extracted from peony petal is using fresh peony petal as raw material, to greatest extent
The derived essential oil in peony is extracted, is a kind of method that peony essential oil efficiently, is quickly extracted from peony.
The present invention first crushes fresh peony petal, supersonic wave wall breaking, and the derived essential oil in peony is made to be released from cell
It releases.Supercritical carbon dioxide extracting is carried out after absorbing peong flower juice with super absorbent resin, super absorbent resin has very
Strong absorbability and water-retaining property, is hardly lost moisture by external pressure.Super absorbent resin is to hydrone and derived essential oil
Binding ability it is different, when carbon dioxide is by the super absorbent resin that absorbs peong flower juice, volatilizable oiliness therein
Ingredient is taken away, and moisture is then stayed in super absorbent resin, realizes water-oil separating, can be directly recovered to from separating still pure
Essential oil.Super absorbent resin can absorb water repeatedly, and recycling reduces production cost.In supercritical carbon dioxide extracting with
Cyclohexane is entrainer, can improve the efficiency of extraction.
Specific embodiment
In the following, technical scheme of the present invention is described in detail by specific embodiment.
Embodiment 1
The present invention provides a kind of methods that peony essential oil is extracted from peony petal, include the following steps：
S1,1 part of fresh peony petal and 1.2 parts of water are mixed, crushed 20 mesh, with ultrasonic power be 240w, frequency 30Hz
After ultrasonication 17min, it is centrifugally separating to obtain peong flower juice；
Super absorbent resin is added in S2, the peong flower juice obtained in S1, the additive amount of super absorbent resin is peong flower juice
0.028 times of weight after stirring 13 minutes, stands 26 minutes, obtains gel peony extract；
S3, supercritical carbon dioxide extracting is carried out to obtaining gel peony extract in S2, it is super to close in carbon dioxide abstraction,
The pressure of extraction is 27Mpa, and extraction temperature is 42 DEG C, and extraction time is 71 minutes, carbon dioxide flow 16.8L/h；It uses
Supercritical carbon dioxide extracting instrument there are two separating still, the pressure of the first separating still is 8.9Mpa, and temperature is 42 DEG C, second point
Pressure from kettle is 3.6Mpa, and temperature is 33 DEG C；Surpass in S3 and close on carbon dioxide abstraction and use cyclohexane as entrainer, cyclohexane
Flow for 1.13L/h, the extract of the first separating still and the second separating still is merged, obtains peony essential oil.
Wherein, the raw material of super absorbent resin includes by weight in S2：13 parts of cornstarch, 67 parts of acrylic acid, corn
6.8 parts of straw powder, 0.62 part of potassium peroxydisulfate, N, N ' -0.074 part of methylene-bisacrylamide, the hydroxide that mass fraction is 27%
86 parts of sodium solution, 15.8 parts of water.The water content of corn stalk powder is 5.4%, and granularity is 70 mesh.
The preparation method of super absorbent resin includes the following steps：
Step 1: cornstarch is added in 76 DEG C of water, constant temperature stirs 43 minutes, the starch solution A being gelatinized；
Step 2: acrylic acid is added in sodium hydroxide solution, stirs 27 minutes, add corn stalk powder, potassium sulfate, N,
N '-methylene-bisacrylamide, stirs evenly, and obtains mixed solution B；
Step 3: the mixed solution B obtained in the starch solution A and step 2 that are obtained in step 1 is uniformly mixed, it is put into micro-
Microwave treatment 4.3 minutes in wave reactor, microwave power 280W is 18 hours dry at 76 DEG C, crushed 70 mesh sieve, obtains height
Water-absorbing resins.
Embodiment 2
The present invention provides a kind of methods that peony essential oil is extracted from peony petal, include the following steps：
S1,1 part of fresh peony petal and 1.1 parts of water are mixed, crushed 20 mesh, with ultrasonic power be 280w, frequency 29Hz
After ultrasonication 16min, it is centrifugally separating to obtain peong flower juice；
Super absorbent resin is added in S2, the peong flower juice obtained in S1, the additive amount of super absorbent resin is peong flower juice
0.033 times of weight after stirring 15 minutes, stands 22 minutes, obtains gel peony extract；
S3, supercritical carbon dioxide extracting is carried out to obtaining gel peony extract in S2, it is super to close in carbon dioxide abstraction,
The pressure of extraction is 33Mpa, and extraction temperature is 37 DEG C, and extraction time is 86 minutes, carbon dioxide flow 15.4L/h；It uses
Supercritical carbon dioxide extracting instrument there are two separating still, the pressure of the first separating still is 8.3Mpa, and temperature is 43 DEG C, second point
Pressure from kettle is 4.2Mpa, and temperature is 31 DEG C；Surpass in S3 and close on carbon dioxide abstraction and use cyclohexane as entrainer, cyclohexane
Flow for 1.20 L/h, the extract of the first separating still and the second separating still is merged, obtains peony essential oil.
Wherein, the raw material of super absorbent resin includes by weight in S2：12 parts of cornstarch, 68 parts of acrylic acid, corn
7.7 parts of straw powder, 0.53 part of potassium peroxydisulfate, N, N ' -0.066 part of methylene-bisacrylamide, the hydroxide that mass fraction is 26%
91 parts of sodium solution, 16.2 parts of water.The water content of corn stalk powder is 5.8%, and granularity is 65 mesh.
The preparation method of super absorbent resin includes the following steps：
Step 1: cornstarch is added in 73 DEG C of water, constant temperature stirs 48 minutes, the starch solution A being gelatinized；
Step 2: acrylic acid is added in sodium hydroxide solution, stir 24 minutes, add corn stalk powder, potassium peroxydisulfate,
N, N '-methylene-bisacrylamide, stir evenly, and obtain mixed solution B；
Step 3: the mixed solution B obtained in the starch solution A and step 2 that are obtained in step 1 is uniformly mixed, it is put into micro-
Microwave treatment 3.4 minutes in wave reactor, microwave power 260W is 19.4 hours dry at 73 DEG C, crushed 75 mesh sieve, obtains
Super absorbent resin.
Embodiment 3
The present invention provides a kind of methods that peony essential oil is extracted from peony petal, include the following steps：
S1,1 part of fresh peony petal and 1 part of water are mixed, crushed 20 mesh, with ultrasonic power be 210w, frequency is that 31Hz surpasses
After sonicated 19min, it is centrifugally separating to obtain peong flower juice；
Super absorbent resin is added in S2, the peong flower juice obtained in S1, the additive amount of super absorbent resin is peong flower juice
0.023 times of weight after stirring 19 minutes, stands 29 minutes, obtains gel peony extract；
S3, supercritical carbon dioxide extracting is carried out to obtaining gel peony extract in S2, it is super to close in carbon dioxide abstraction,
The pressure of extraction is 24Mpa, and extraction temperature is 44 DEG C, and extraction time is 54 minutes, carbon dioxide flow 16.1L/h；It uses
Supercritical carbon dioxide extracting instrument there are two separating still, the pressure of the first separating still is 9.7Mpa, and temperature is 41 DEG C, second point
Pressure from kettle is 4.8Mpa, and temperature is 34 DEG C；Surpass in S3 and close on carbon dioxide abstraction and use cyclohexane as entrainer, cyclohexane
Flow for 1.01L/h, the extract of the first separating still and the second separating still is merged, obtains peony essential oil.
Embodiment 4
The present invention provides a kind of methods that peony essential oil is extracted from peony petal, include the following steps：
S1,1 part of fresh peony petal and 1.3 parts of water are mixed, crushed 20 mesh, ultrasonic power 260w, frequency are that 28Hz surpasses
After sonicated 18min, it is centrifugally separating to obtain peong flower juice；
Super absorbent resin is added in S2, the peong flower juice obtained in S1, the additive amount of super absorbent resin is peong flower juice
0.037 times of weight after stirring 17 minutes, stands 24 minutes, obtains gel peony extract；
S3, supercritical carbon dioxide extracting is carried out to obtaining gel peony extract in S2, it is super to close in carbon dioxide abstraction,
The pressure of extraction is 31Mpa, and extraction temperature is 39 DEG C, and extraction time is 62 minutes, carbon dioxide flow 17.7L/h；It uses
Supercritical carbon dioxide extracting instrument there are two separating still, the pressure of the first separating still is 9.4Mpa, and temperature is 44 DEG C, second point
Pressure from kettle is 3.2Mpa, and temperature is 32 DEG C, and the extract of the first separating still and the second separating still is merged, and obtains tree peony essence
Oil.
Embodiment 5
The method that peony essential oil is extracted in slave peony petal in embodiment 1, wherein, surpass in S3 and close on carbon dioxide abstraction entrainment
The flow of agent cyclohexane can also be 1.21L/h.
Embodiment 6
The method that peony essential oil is extracted in slave peony petal in embodiment 1, wherein, the raw material of super absorbent resin is pressed in S2
Parts by weight can also include：14 parts of cornstarch, 66 parts of acrylic acid, 5.2 parts of corn stalk powder, 0.57 part of potassium peroxydisulfate, N, N '-
0.078 part of methylene-bisacrylamide, 88 parts of the sodium hydroxide solution that mass fraction is 29%, 15.3 parts of water.Corn stalk powder
Water content is 6.9%, and granularity is 75 mesh.
Embodiment 7
The method that peony essential oil is extracted in slave peony petal in embodiment 1, wherein, the raw material of super absorbent resin is pressed in S2
Parts by weight can also include：15 parts of cornstarch, 69 parts of acrylic acid, 6.1 parts of corn stalk powder, 0.68 part of potassium peroxydisulfate, N, N '-
0.062 part of methylene-bisacrylamide, 93 parts of the sodium hydroxide solution that mass fraction is 28%, 16.7 parts of water.Corn stalk powder
Water content is 7.8%, and granularity is 80 mesh.
Embodiment 8
The method that peony essential oil is extracted in slave peony petal in embodiment 1, wherein, the preparation method of super absorbent resin may be used also
To include the following steps：
Step 1: cornstarch is added in 78 DEG C of water, constant temperature stirs 46 minutes, the starch solution A being gelatinized；
Step 2: acrylic acid is added in sodium hydroxide solution, stir 22 minutes, add corn stalk powder, potassium peroxydisulfate,
N, N '-methylene-bisacrylamide, stir evenly, and obtain mixed solution B；
Step 3: the mixed solution B obtained in the starch solution A and step 2 that are obtained in step 1 is uniformly mixed, it is put into micro-
Microwave treatment 4.8 minutes in wave reactor, microwave power 270W is 16.4 hours dry at 79 DEG C, crushed 80 mesh sieve, obtains
Super absorbent resin.
Existing device on the market can be selected in microwave reactor involved in the present invention, as long as required function of the present invention can be realized
, preferred Nanjing optically-active Science and Technology Ltd. LWMC-201 type microwave reactors.
Involved in the present invention is the common knowledge of this field the methods of being uniformly mixed, stir evenly, centrifuging,
This is repeated no more.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
- A kind of 1. method that essential oil is extracted from peony petal, which is characterized in that include the following steps：S1, fresh peony petal and water are mixed, by crushing, after ultrasonication, is centrifugally separating to obtain peong flower juice；Super absorbent resin is added in S2, the peong flower juice obtained in S1, after stirring 10-20 minutes, stands 20-30 minutes, Obtain gel peony extract；S3, supercritical carbon dioxide extracting is carried out to obtaining gel peony extract in S2, obtains peony essential oil.
- 2. a kind of method that essential oil is extracted from peony petal according to claim 1, which is characterized in that high in the S2 The raw material of water-absorbing resins includes by weight：12-15 parts of cornstarch, 65-70 parts of acrylic acid, 5-8 parts of corn stalk powder, mistake 0.5-0.7 parts of potassium sulfate, N, N ' -0.06-0.08 parts of methylene-bisacrylamide, the sodium hydroxide that mass fraction is 26%-29% 85-95 parts of solution, 15-17 parts of water.
- 3. a kind of method that essential oil is extracted from peony petal according to claim 2, which is characterized in that high in the S2 The preparation method of water-absorbing resins includes the following steps：Step 1: cornstarch is added in 70-80 DEG C of water, constant temperature stirs 40-50 minutes, the starch solution A being gelatinized；Step 2: acrylic acid is added in sodium hydroxide solution, stirs 20-30 minutes, add corn stalk powder, persulfuric acid Potassium, N, N '-methylene-bisacrylamide, stir evenly, and obtain mixed solution B；Step 3: the mixed solution B obtained in the starch solution A and step 2 that are obtained in step 1 is uniformly mixed, it is put into micro- Microwave treatment 3-5 minutes, microwave power 250-300W in wave reactor, dry, crushing obtains super absorbent resin.
- 4. a kind of method that essential oil is extracted from peony petal according to claim 1, which is characterized in that new in the S1 The weight ratio of fresh peong flower valve and water is 1:1-1.3.
- 5. a kind of method that essential oil is extracted from peony petal according to claim 1, which is characterized in that high in the S2 The additive amount of water-absorbing resins is 0.02-0.04 times of peong flower juice weight.
- 6. a kind of method that essential oil is extracted from peony petal according to claim 1, which is characterized in that the S3, which surpasses, to be faced In nearly carbon dioxide abstraction, the pressure of extraction is 23-35Mpa, and extraction temperature is 35-45 DEG C, and extraction time is 50-90 minutes, Carbon dioxide flow is 15-18L/h.
- 7. a kind of method that essential oil is extracted from peony petal according to claim 1, which is characterized in that the S3, which surpasses, to be faced In nearly carbon dioxide abstraction, there are two separating stills for the supercritical carbon dioxide extracting instrument used, and the pressure of the first separating still is 8- 10Mpa, temperature are 40-45 DEG C, and the pressure of the second separating still is 3-5Mpa, and temperature is 30-35 DEG C.
- 8. a kind of method that essential oil is extracted from peony petal according to claim 1, which is characterized in that surpass in the S3 It closes on carbon dioxide abstraction and uses cyclohexane as entrainer.
- 9. a kind of method that essential oil is extracted from peony petal according to claim 8, which is characterized in that surpass in the S3 Carbon dioxide abstraction is closed on, the flow of entrainer cyclohexane is the 6%-8% of carbon dioxide flow.
- 10. a kind of method that essential oil is extracted from peony petal according to claim 1, which is characterized in that in the S1 The ultrasonic power of ultrasonication is 200-300w, frequency 28-32Hz, ultrasonic time 15-20min.
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| CN111205927A (en) * | 2020-01-16 | 2020-05-29 | 河北瑞龙生物科技有限公司 | Peony essential oil extraction method |
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| CN114437870A (en) * | 2021-12-22 | 2022-05-06 | 广东石丰农业科技有限公司 | Extraction preparation process of essential oil of Abelmoschus manihot |
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Application publication date: 20180629 |