CN109988673A - A method of improving borneol essential oil yield - Google Patents
A method of improving borneol essential oil yield Download PDFInfo
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- CN109988673A CN109988673A CN201910283652.3A CN201910283652A CN109988673A CN 109988673 A CN109988673 A CN 109988673A CN 201910283652 A CN201910283652 A CN 201910283652A CN 109988673 A CN109988673 A CN 109988673A
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- essential oil
- borneol
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- oil yield
- borneol essential
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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
-
- 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
- C11B9/022—Refining
-
- 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
-
- 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
- C11B9/027—Recovery of volatiles by distillation or stripping
Abstract
The application provides a kind of method for improving borneol essential oil yield, belongs to from raw materials recovery or purification essential oil technical field.Borneol camphortree leaf is dried, is first handled through mechanical activation, powder is heated with microwave, is extracted after extracting solution boiling and is obtained mixed vapour, and the oil water mixture that mixed vapour is obtained by condensation is by isolated borneol crude oil；Borneol essential oil can be obtained using extraction and separation in borneol crude oil.The application is applied to extraction of essential oil, has many advantages, such as to have a wide range of application, extraction rate is fast, recovery rate is high, reproducibility is good, saves reagent, shortens extraction time, reducing energy consumption, reducing and pollute, is environmentally friendly.
Description
Technical field
This application involves a kind of method for improving borneol essential oil yield, belong to from raw materials recovery or purification essence oil tech neck
Domain.
Background technique
Natural borneol original name kapur, also known as d-Bomeol are to be permitted as natural rare Chinese medicine medicinal material and food additives
Indispensable good adjuvant in more borneol products.The history that natural borneol is used as drug in China is more than 1500.Study table
Bright, borneol is proven to have anti-inflammatory, antithrombotic and excellent antioxidation.
Borneol essential oil is suitble to prepare flavouring essence for tobacco, medical essence, cosmetics and a variety of drugs, and borneol essential oil value is high, uses
Way is wide, and borneol development prospect is wide.However in recent years, few about the research report for extracting borneol essential oil.Borneol essential oil mentions
Taking most-often used is traditional steam distillation, and traditional steam distillation is that borneol is put into alembic directly to distill, and is steamed
The mixed vapour evaporated obtains oil water mixture by condensation, and borneol essential oil can be obtained in oil water mixture essential oil water-oil separating again.
The problems such as that there are recovery rates is low for this method, time-consuming, energy consumption is high, product purity is low.
Summary of the invention
In view of this, the application provides one kind has a wide range of application, extraction rate is fast, recovery rate is high, reproducibility is good, saves examination
Agent shortens extraction time, reduces energy consumption, reduces pollution, the environment amenable method for improving borneol essential oil yield.
To achieve the above object, the technical solution that the application takes is as follows:
A method of improving borneol essential oil yield, comprising the following steps: (1) take borneol camphortree leaf, dry；(2) it is stirring
It mixes in ball mill, the drying borneol camphortree leaf mechanical activation of step (1) is obtained into powder；(3) add into powder according to liquid-solid ratio
Enter distilled water and heated with microwave, is extracted after extracting solution boiling and obtain mixed vapour；(4) mixed vapour is cold through condenser pipe
It is solidifying, obtain oil water mixture；(5) oil water mixture is subjected to water-oil separating, obtains borneol essential oil crude product and water；(6) by borneol
Essential oil crude product is transferred to extractor and is extracted, and after layering, upper layer is finished product borneol essential oil.
In extraction scheme provided by this programme, in a manner of microwave-assisted distillation, mechanical lapping is carried out to borneol essential oil
After pretreatment, in distillation process, original traditional water distillation heating, moisture in plant cell are substituted using microwave as heating unit
Isopolarity substance can absorb microwave energy, make to generate amount of heat in plant cell, temperature steeply rises, so that cell interior pressure
Power increases, and when cell interior pressure is more than cell wall expansion ability to bear, cell membrane walls rupture is cracked or micropore, carefully
Effective component intracellular quickly flows out, to improve recovery rate, recovery rate can be improved 27% or more.
On the basis of the studies above, we study drying, the results showed that when be dried to moisture content be 8-
When 12%, on the basis of being suitable for drying cost, the water content in raw material not only can be effectively reduced, cooperate with mechanical lapping, have
Effect improves the efficiency pulverized.
On the basis of the studies above, we also study mechanical activation, and more preferred stirring has been determined
Grinder parameter: the revolving speed 90-130r/min of agitating ball mill, the time of mechanical activation are 3-7min.Under the grinding condition,
Before borneol essential oil is extracted in distillation, mechanical activation processing is first passed through after borneol camphortree leaf is dried, mechanical activation is by borneol camphor tree
Leaf destroys the cell wall of plant under the mechanical forces such as friction, collision, impact, shearing, and refines particle, so that imperial
Essential oil in brain camphor tree is more easier to extract, to improve the recovery rate of essential oil.
On the basis of the studies above, we also study the concrete technology of microwave-assisted distillation process: described micro-
Wave power is 425-625W.Research is found: when microwave power is lower than 425W, when the recovery rate of essential oil is distilled with conventional water substantially
Yield maintains an equal level；When microwave power increases, especially when microwave power is more than 475W, microwave to the heating effect of powder gradually
Significantly, the pressure in cell membrane walls is gradually increased, and the rupture of part cell wall, effective component is gradually overflowed, to effectively increase essence
Oily yield；Continue to increase microwave power, when reaching 575W, then the expansion ability to bear that can be born due to cell membrane walls is limited,
Thermal accumlation to a certain extent after, the increase of microwave power no longer contributes to recovery rate, therefore, microwave power be suitable for control
In 425-625W, and preferably 475-575W.This method is simple with device, have a wide range of application, extraction rate is fast, recovery rate
Height, reproducibility are good, save reagent, shorten extraction time, reduce energy consumption, reduce the advantages that polluting, is environmentally friendly.
On the basis of the studies above, we continue to study the handling duration of microwave-assisted distillation, as a result table
It is bright: when the microwave irradiation time is 25-45min, preferable essential oil yield can be obtained.Selecting microwave-assisted distillation
When mode, with the extension of microwave radiation heating time, the heat accumulated in cell membrane walls gradually increases, and corresponding cell wall is broken
It splits or the probability of pore-forming is higher, essential oil yield is gradually promoted, when microwave heating time reaches 30min, especially when radiation adds
When the hot time reaches 30-35min, the increment of essential oil yield is maximum, and when more than 35min, essential oil yield tends towards stability, and continues to extend
The radiant heating time does not have essential oil yield and is obviously improved, and therefore, comprehensive treatment effect is considered with processing cost, is suitable for
It is 25-45min, and preferably 30-40min by microwave irradiation time.
On the basis of the studies above, we also test the liquid-solid ratio of distillation process, the results showed that work as extraction
Liquid-solid ratio (i.e. distilled water volume and raw material powder mass ratio) control of liquid is at (3-7): 1, especially when liquid-solid ratio is (4-6): 1
When (unit: ml/g), heats with microwave radiation and cooperate, good distillation extraction effect can be obtained.Microwave radiation is needle
Entire object to be processed is heated, liquid-solid ratio will affect the being heated evenly property and thermal exposure of specific powder, liquid-solid ratio
It is too low, then since leachable purpose essential oil is limited, under the conditions of this kind, no matter how high microwave radiation is, real work
Efficiency is all limited；Liquid-solid ratio is too high, then since the cell wall that heat is unable to satisfy all tape handling objects ruptures demand, equally
It will affect essential oil yield.
Detailed description of the invention
Fig. 1 is influence of the microwave power to borneol essential oil yield；
Fig. 2 is influence of the microwave irradiation time to borneol essential oil yield；
Fig. 3 is influence of the liquid-solid ratio to borneol essential oil yield；
Fig. 4 is the representative processes flow chart of the application.
Specific embodiment
In the extraction scheme of the essential oil provided by present application, the principal element for influencing essential oil yield is divided into: dry, machine
Tool activation, the microwave-assisted several aspects of distillation:
A. the dry water content being mainly concerned with after drying mode and degree of drying i.e. drying.Borneol essential oil raw material mainly selects
From borneol camphortree leaf, it is contemplated that the characteristic of the characteristics such as a large amount of property of the raw material, disunity and borneol essential oil is suitable for using nature
The mode dried carries out；In terms of degree of drying, moisture content is excessively high, can be unfavorable for mechanical activation, also can band in subsequent distillation
Enter a large amount of moisture, causes essential oil entirety recovery rate relatively low.On the basis of by our lot of experiments, water content is selected
It is set to 8-12%, the water content in raw material not only can be effectively reduced, also effectively improve the efficiency pulverized.
B. mechanical activation is mainly concerned with the grinding mode and revolving speed or specific breakage rate of selection.In grinding mode side
Face, we have selected agitating ball mill, complete grinding while agitating, raw material is enable rapidly and uniformly to grind sufficiently, and
By revolving speed control in 90-130r/min, the time of mechanical activation is 3-7min, can meet grinding and adequately require.
The main influence with regard to microwave-assisted distillation of following case is analyzed.
C. microwave-assisted distillation includes selected microwave power, distillation time and raw material liquid-solid ratio, hereafter mainly
The acquisition that microwave power, distillation time and material liquid compare essential oil admittedly influences to carry out concrete case explanation and analysis, specific to join
See embodiment 1-3.
Embodiment 1: influence of the different microwave to essential oil yield
In early-stage study, it has been found that preferred microwave power is suitable for control within the scope of 425-625W, therefore this
Five nodes of 425W, 475W, 525W, 575W, 625W in the range are chosen in case as representing, and complete microwave power to essence
The experiment that oily yield influences, and with blank assay (drying → mechanical activation → water distillation → condensation → water-oil separating → extraction,
Essential oil yield is about 0.35%) to compare.
The results showed that in conjunction with Fig. 1, when being handled respectively using aforesaid way, under the same terms, in 425W, essential oil
Yield is although low (at this point, essential oil yield is about 0.37%), but still has exceeded conventional water distillation mode；Continue growing microwave function
Rate, then before reaching 475W, essential oil yield amplification is significant；When power is increased to 575W by 475W, essential oil yield is in stabilization
The situation of sustainable growth continues to increase radiant power, does not then contribute more essential oil yield, therefore more suitable microwave spoke
Penetrating power is the 475-575W in the section 425-625W.
Therefore distillation time is studied using the microwave power of 570W as main microwave intensity in following experiment.
Embodiment 2: influence of the different distillation times to essential oil yield
On the basis of embodiment 1, we test distillation time (remaining parameter is referring to embodiment 1), as a result table
Bright: in conjunction with Fig. 2, when distillation time is lower than 25min, the recovery rate of essential oil is about 0.37%, obtaining when being only slightly higher than water distillation
Rate；With the extension of distillation time, especially 30-35min this period, recovery rate increment are significant；When reaching 35min, essence
Oily yield reaches peak value (0.46%) under this condition；Continue to extend distillation time, then may be limited because of spill-out, essential oil mentions
It takes rate not have to rise appreciably, and substantially remains near 0.46-0.47%.Therefore, under comprehensive consideration, distillation time is suitable for control
For system in 25-45min, and when preferably 30-40min, extraction of essential oil effect is preferable.
Embodiment 3: influence of the different material liquid-solid ratio to essential oil yield
On the basis of embodiment 1 and embodiment 2, we constitute (remaining parameter is referring to embodiment 1) to raw material and carry out in fact
It tests, raw material process is mainly the liquid-solid ratio of raw material.The result shows that: in conjunction with Fig. 3, with raw material powder (consolidating ingredient) in extracting solution
Accounting in extracting solution is reduced, i.e., when liquid-solid ratio is less than 3:1, due to being unable to get sufficient heating, the cell wall actually ruptured
Limited, corresponding target extraction of essential oil rate is relatively low (maintaining essentially in 0.336% or less), with the increase of liquid-solid ratio, raw material
Powder gradually spreads out, and obtains the heated face of radiation and increases with it, rupture cell wall is more abundant, and leachable essential oil amount also increases
Greatly, corresponding essential oil yield increases with it, and reaches peak value (0.46%) under this condition when liquid-solid ratio is 5:1, continues to increase
Big liquid-solid ratio, then since the solid powder in extracting solution is limited, the heat of microwave radiation is gone by liquid point, and practical function is in solid
It is limited on powder, therefore sporoderm-broken rate reduces, the dissolution essential oil concentration in extracting solution is lower, and the essential oil yield of extraction drops therewith
It is low.Therefore, comprehensive treatment effect is considered with processing cost, and liquid-solid ratio is selected at (3-7): 1, and preferably (4-6): when 1, essential oil
Extraction effect is preferable.
On the basis of above-mentioned experiment and analysis of cases, we in a manner of microwave-assisted distillation to raw material powder at
Reason, and using following step as representative,
(1) borneol camphortree leaf is taken, is dried；(2) in agitating ball mill, dry borneol camphortree leaf mechanical activation is obtained into powder
End；(3) powder is heated to boiling with microwave radiation, and extraction obtains mixed vapour；(4) mixed vapour condenses to obtain oil mixing with water
Object；(5) oil water mixture is subjected to water-oil separating, obtains borneol essential oil crude product (borneol crude oil i.e. hereafter) and water；It (6) will be imperial
Brain essential oil crude product is transferred to extractor and is extracted, and after layering, upper layer is finished product borneol essential oil,
In conjunction with Fig. 4 and four concrete cases (embodiment 4,5,6,7) selected, whole annotate is done to the extraction scheme of the application
It releases.
Embodiment 4
(1) the borneol camphortree leaf of harvesting is dried, makes its moisture content 10%；
(2) mechanical activation: the borneol camphortree leaf dried is added in agitating ball mill, mechanical in the case where revolving speed is 90r/min
7min is activated, powder is obtained；
(3) microwave-assisted distillation: raw material liquid-solid ratio is 5:1 (mL/g), uses power for the microwave heating of 570W, and auxiliary is steamed
35min is evaporated, mixed vapour is obtained；
(4) condense: mixed vapour obtained above is condensed by condenser, and oil water mixture is obtained after condensation；
(5) water-oil separating: the oil water mixture condensed carries out water-oil separating by oil water separator, and it is thick to obtain borneol
Oil and water；
(6) extract: obtained borneol crude oil is extracted using extractor, and after layering, separating upper layer is borneol essence
Oil, borneol extraction of essential oil rate can be improved 24% or so compared to traditional steam distillation.
Embodiment 5
(1) the borneol camphortree leaf of harvesting is dried, makes its moisture content 10%；
(2) mechanical activation: the borneol camphortree leaf dried is added in agitating ball mill, mechanical in the case where revolving speed is 100r/min
5min is activated, powder is obtained；
(3) microwave-assisted distillation: raw material liquid-solid ratio is 5:1 (mL/g), uses power for the microwave heating of 570W, and auxiliary is steamed
35min is evaporated, mixed vapour is obtained；
(4) condense: mixed vapour obtained above is condensed by condenser, and oil water mixture is obtained after condensation；
(5) water-oil separating: the oil water mixture condensed carries out water-oil separating by oil water separator, and it is thick to obtain borneol
Oil and water；
(6) extract: obtained borneol crude oil is extracted using extractor, and after layering, separating upper layer is borneol essence
Oil, borneol extraction of essential oil rate can be improved 25% or so compared to traditional steam distillation.
Embodiment 6
(1) the borneol camphortree leaf of harvesting is dried, makes its moisture content 10%；
(2) mechanical activation: the borneol camphortree leaf dried is added in agitating ball mill, mechanical in the case where revolving speed is 110r/min
5min is activated, powder is obtained；
(3) microwave-assisted distillation: raw material liquid-solid ratio is 5:1 (mL/g), uses power for the microwave heating of 570W, and auxiliary is steamed
35min is evaporated, mixed vapour is obtained；
(4) condense: mixed vapour obtained above is condensed by condenser, and oil water mixture is obtained after condensation；
(5) water-oil separating: the oil water mixture condensed carries out water-oil separating by oil water separator, and it is thick to obtain borneol
Oil and water；
(6) extract: obtained borneol crude oil is extracted using extractor, and after layering, separating upper layer is borneol essence
Oil, borneol extraction of essential oil rate can be improved 26.5% or so compared to traditional steam distillation.
Embodiment 7
(1) the borneol camphortree leaf of harvesting is dried, makes its moisture content 10%；
(2) mechanical activation: the borneol camphortree leaf dried is added in agitating ball mill, mechanical in the case where revolving speed is 130r/min
3min is activated, powder is obtained；
(3) microwave-assisted distillation: raw material liquid-solid ratio is 5:1 (mL/g), uses power for the microwave heating of 570W, and auxiliary is steamed
35min is evaporated, mixed vapour is obtained；
(4) condense: mixed vapour obtained above is condensed by condenser, and oil water mixture is obtained after condensation；
(5) water-oil separating: the oil water mixture condensed carries out water-oil separating by oil water separator, and it is thick to obtain borneol
Oil and water；
(6) extract: obtained borneol crude oil is extracted using extractor, and after layering, separating upper layer is borneol essence
Oil, borneol extraction of essential oil rate can be improved 27% or so compared to traditional steam distillation.
The above content is the preferred embodiments of combination the invention to further detailed made by provided technical solution
Describe in detail bright, and it cannot be said that the invention specific implementation is confined to these above-mentioned explanations, technology affiliated for the invention
For the those of ordinary skill in field, without departing from the concept of the premise of the invention, several simple deductions can also be made
Or replacement, it all shall be regarded as belonging to the protection scope of the invention.
Claims (10)
1. a kind of method for improving borneol essential oil yield, which comprises the following steps: take borneol camphortree leaf, dry；
(2) in agitating ball mill, the drying borneol camphortree leaf mechanical activation of step (1) is obtained into powder；(3) powder is carried out with microwave
Heating extracts after extracting solution boiling and obtains mixed vapour；(4) mixed vapour is obtained into oil water mixture through condensing tube condensation；
(5) oil water mixture is subjected to water-oil separating, obtains borneol essential oil crude product and water；(6) borneol essential oil crude product is transferred to extractor
It is extracted, after layering, upper layer is finished product borneol essential oil.
2. a kind of method for improving borneol essential oil yield as described in claim 1, it is characterised in that: in step (1), be dried to
Moisture content is 8-12%.
3. a kind of method for improving borneol essential oil yield as described in claim 1, it is characterised in that: in step (2), stir ball
The revolving speed 90-130r/min of grinding machine, the time of mechanical activation are 3-7min.
4. a kind of method for improving borneol essential oil yield as described in any one of claims 1-3, it is characterised in that: step (3)
In, the power of the microwave is 425-625W.
5. a kind of method for improving borneol essential oil yield as claimed in claim 4, it is characterised in that: described micro- in step (3)
The power of wave is 475-575W.
6. a kind of method for improving borneol essential oil yield as described in any one of claims 1-3, it is characterised in that: step (3)
In, distillation time 25-45min.
7. a kind of method for improving borneol essential oil yield as claimed in claim 6, it is characterised in that: in step (3), when distillation
Between be 30-40min.
8. a kind of method for improving borneol essential oil yield as described in any one of claims 1-3, it is characterised in that: step (3)
In, the liquid-solid ratio of extracting solution is (3-7): 1.
9. a kind of method for improving borneol essential oil yield as claimed in claim 8, it is characterised in that: in step (3), extracting solution
Liquid-solid ratio be (4-6): 1.
10. a kind of method for improving borneol essential oil yield as described in any one of claims 1-3, it is characterised in that: step (3)
In, the power of the microwave is 475-575W, and distillation time 30-40min, the liquid-solid ratio of extracting solution is (4-6): 1.
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| CN114133987A (en) * | 2021-12-10 | 2022-03-04 | 江西师范大学 | Method for extracting essential oil from cinnamomum camphora leaves |
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Application publication date: 20190709 |