CN110003985A - A kind of combination sound wave extracting method of borneol essential oil - Google Patents
A kind of combination sound wave extracting method of borneol essential oil Download PDFInfo
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- CN110003985A CN110003985A CN201910283720.6A CN201910283720A CN110003985A CN 110003985 A CN110003985 A CN 110003985A CN 201910283720 A CN201910283720 A CN 201910283720A CN 110003985 A CN110003985 A CN 110003985A
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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
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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
- C11B9/022—Refining
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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
- 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
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Fats And Perfumes (AREA)
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Abstract
The application provides a kind of combination sound wave extracting method of borneol essential oil, belongs to from raw materials recovery or purification essential oil technical field.Borneol camphortree leaf is dried, is first handled through mechanical activation, is then handled with ultrasonic-microwave；The raw material handled distillation is extracted to obtained mixing vapor by condensation, condensed oil water mixture passes through 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 take that speed is fast, low energy consumption, conducive to polarity and unstability constituents extraction.
Description
Technical field
This application involves a kind of combination sound wave extracting method of borneol essential oil, belong to from raw materials recovery or purification essential oil skill
Art field.
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 is easy to operate, extraction rate is fast, low energy consumption, is conducive to polarity and unstability
The combination sound wave extracting method of the borneol essential oil of constituents extraction.
To achieve the above object, the technical solution that the application takes is as follows:
A kind of combination sound wave extracting method of borneol essential oil, comprising the following steps: (1) 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 with ultrasonic-microwave
After processing, it is transferred to alembic, and be passed through vapor from distillation pot bottom and heated, is extracted after boiling, obtain 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 to extract, after layering, upper layer is finished product borneol essential oil.
In extraction scheme provided by this programme, in such a way that ultrasonic-microwave collaboration processing is with distillation cooperation, first to dragon
Brain essential oil carries out mechanical lapping pretreatment, then it is distilled after ultrasonic-microwave is handled, condenses, separate, extracting, this method
In conjunction with the pre-treatment of mechanical activation, plant cell wall is destroyed under mechanical force, and refines particle, and raw material is in ultrasound
Under wave-microwave synergistic effect, realize have complementary advantages, it is more serious to raw cell structural damage, act on it is more abundant, by its with
Distillation cooperation, effectively improves infiltration, emulsification and the solubilization of purpose essential oil in distillation, achievees the purpose that improve extraction efficiency,
Recovery rate can be improved 30% 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 processing method of ultrasonic-microwave, and determined compared with
Power when acting synergistically for preferred ultrasonic-microwave: in the ultrasonic-microwave processing, acoustic power 100-400W.
Research is found: when combining acoustic power lower than 100W, the recovery rate of essential oil is relatively low；With the increase of acoustic power, chorus is organized
Wave enhances raw cell structural damage, and effect is more abundant, and recovery rate is linearly incremented by therewith；When reaching 250W, continue
Increase combination acoustic power, then recovery rate does not increase anti-drop, and therefore, acoustic power is preferably 100-400W, and preferably 200-
300W.This method is easy with operation, extraction rate is fast, energy consumption is small, and it is excellent to be conducive to extraction of polarity and unstability ingredient etc.
Point.On the basis of studying power, we also test the processing time, find: the processing time is suitable for setting
For 2-15min.When selecting the mode of ultrasonic-microwave combination sound wave to be further processed, as raw material powder is combining
Processing time in sound wave extends, and essential oil yield is gradually promoted, when treated between when reaching 5-10min, especially work as processing
Time reaches 7-8min, at this point, essential oil yield reaches peak value, continues to extend the processing time, can't be helpful to essential oil yield,
Therefore, comprehensive treatment effect is considered with processing cost, is suitable for that will handle selection of time in 2-15min, and preferably 5-10min.
On the basis of the studies above, we also study distillation technique, and during the extraction process, distillation is mainly
It is carried out after boiling, therefore temperature parameter can be ignored, it is preferred that emphasis is influence of the time parameter to extraction, the choosing of time parameter
It selects, is not only required to meet the demand sufficiently extracted, also to meet the needs of energy consumption cost and process cycle.The study found that with
Time is incremented by, and extraction of essential oil rate is incremented by any time and improves, and speedup is significant after 1h, but when the time extends to 2.5h
Afterwards, speedup is no longer obvious, therefore distillation time is suitable for being selected in 1-3 hours, and preferably 2-3h.
Detailed description of the invention
Fig. 1 is influence of the application ultrasonic-microwave power to borneol essential oil yield；
Fig. 2 is influence of the handling duration to borneol essential oil yield in the processing of table ultrasonic-microwave；
Fig. 3 is influence of the distillation time 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, ultrasonic-microwave and the 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 influence that following case mainly combines sound wave and distillation with regard to ultrasonic-microwave is analyzed.
C. ultrasonic-microwave includes selected acoustic power, handling duration, hereafter mainly with regard to the sound of ultrasonic-microwave
Wave power, handling duration influence the acquisition of essential oil to carry out concrete case explanation and analysis, referring specifically to embodiment 1-3.
Embodiment 1: influence of the different acoustic powers to essential oil yield
In present case in ultrasonic-microwave processing mode, for acoustic power, below with 100W, 150W, 200W, 250W,
Seven nodes of 300W, 350W, 400W carry out specific experiment, and will use simple steam distillation (process are as follows: borneol essential oil blade
→ drying → mechanical activation → distillation → condensation → water-oil separating → extraction, essential oil yield be mode 0.36%) as a comparison
Group, remaining parameter then use: the water content of raw material drying is under 130r/min after mechanical activation 3min, boiling for 10%, revolving speed
Extract 2.5h；Wherein, the handling duration of seven nodes of 100W, 150W, 200W, 250W, 300W, 350W, 400W is 7.5h.
The present embodiment mainly using seven nodes of 100W, 150W, 200W, 250W, 300W, 350W, 400W as represent and with
Contrast groups are compared, as a result shown in Figure 1.It will be seen from figure 1 that using ultrasonic-microwave combination sonicated when,
Under the same terms, with the raising of acoustic power, essential oil yield is gradually promoted, especially when acoustic power reaches 150W (at this time
Essential oil yield be about 0.462%) after, the raising of acoustic power improves significantly on the increment of essential oil yield, and in 250W
Reaching maximum value, (about 0.495%, the essential oil yield increase rate of relative contrast's group is about 37.5, increase rate=(0.495-
0.36)/0.36, multiplied by 100%, remaining increase rate refers to the calculation)；Continue increase sound wave power, then due to
Concussion is serious, is unfavorable for the dissolution of active chemical instead, therefore, after power is more than 250W, essential oil yield is not risen instead
Drop.
Therefore the processing time is studied using 250W as the major experimental power of combination sound wave in following experiment.
Embodiment 2: influence of the different ultrasonic-microwave processing times to essential oil yield
On the basis of embodiment 1, we to processing time (remaining parameter is referring to embodiment 1) of ultrasonic-microwave into
Row experiment, the results showed that in conjunction with Fig. 2, when treated between be lower than 3min when, the recovery rate of essential oil is near 0.455%；With place
The increase of time is managed, recovery rate is almost linear therewith to be incremented by；When reaching 7-7.5min, essential oil yield reaches under this condition
Peak value (0.488%)；Continue to extend the processing time, then may not increase anti-drop because of the interference of concussion, recovery rate.Therefore, synthesis is examined
Under amount, the processing time is selected as 2-15min, and when preferably 5-10min, extraction of essential oil effect is preferable.
D. distillation mainly includes distillation mode, vapo(u)rizing temperature, the aspect of distillation time three, distillation on the acquisition of essential oil influence into
Row concrete case explanation is with analysis referring to embodiment 3.
Embodiment 3: influence of the different distillation times to essential oil yield
On the basis of embodiment 1, embodiment 2, since distillation mainly carries out after boiling, and distill general in industry
Distilled all over using stream mode, therefore temperature parameter can be ignored, in the present embodiment mainly to distillation time (remaining parameter referring to
Embodiment 1) it is tested, the results showed that in conjunction with Fig. 3, within preceding half an hour, since energy is mainly used for maintaining boiling,
The essential oil yield in the stage not counts；With being incremented by for time, extraction of essential oil rate is incremented by any time and improves, and in 1h (this
When essential oil yield be about that 0.385%) speedup is significant later, and reaches peak (0.449%) under this condition in 2.5h, when
After time extends to 2.5h, speedup is no longer obvious, therefore distillation time is suitable for being selected in 1-3 hours, and when preferably 2-3h, essential oil
Extraction effect is preferable.
On the basis of above-mentioned experiment and analysis of cases, we are in a manner of the combination sound wave of ultrasonic-microwave to raw material powder
It is handled, 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) after powder is handled with ultrasonic-microwave, it is transferred to alembic, and is passed through vapor and is heated, extracts and obtains after boiling
Mixed vapour；(4) mixed vapour condenses to obtain oil water mixture；(5) oil water mixture is subjected to water-oil separating, obtains borneol essence
Oily crude product (borneol crude oil i.e. hereafter) and water；(6) borneol essential oil crude product extractor is transferred to extract, after layering, upper layer
As 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) ultrasonic-microwave combines sonicated: power being used to handle powder 7.5min for the ultrasonic-microwave of 250W；
(4) it distills: being passed through vapor from the bottom of alembic and extracting solution is heated, extracted after extracting solution boiling
2.5h obtains mixed vapour；
(5) condense: mixed vapour obtained above is condensed by condenser, and oil water mixture is obtained after condensation；
(6) 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；
(7) 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 28% 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) ultrasonic-microwave combines sonicated: power being used to handle powder 7.5min for the ultrasonic-microwave of 250W；
(4) it distills: being passed through vapor from the bottom of alembic and extracting solution is heated, extracted after extracting solution boiling
2.5h obtains mixed vapour；
(5) condense: mixed vapour obtained above is condensed by condenser, and oil water mixture is obtained after condensation；
(6) 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；
(7) 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 29% 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) ultrasonic-microwave combines sonicated: power being used to handle powder 7.5min for the ultrasonic-microwave of 250W；
(4) it distills: being passed through vapor from the bottom of alembic and extracting solution is heated, extracted after extracting solution boiling
2.5h obtains mixed vapour；
(5) condense: mixed vapour obtained above is condensed by condenser, and oil water mixture is obtained after condensation；
(6) 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；
(7) 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 29.5% 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) ultrasonic-microwave combines sonicated: power being used to handle powder 7.5min for the ultrasonic-microwave of 250W；
(4) it distills: being passed through vapor from the bottom of alembic and extracting solution is heated, extracted after extracting solution boiling
2.5h obtains mixed vapour；
(5) condense: mixed vapour obtained above is condensed by condenser, and oil water mixture is obtained after condensation；
(6) 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；
(7) 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 30% 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 (9)
1. a kind of combination sound wave extracting method of borneol essential oil, which comprises the following steps: (1) borneol camphortree leaf is taken,
Drying；(2) in agitating ball mill, dry borneol camphortree leaf mechanical activation is obtained into powder；(3) powder is with ultrasonic-microwave
After processing, it is transferred to alembic, and is passed through vapor and is heated, is extracted after boiling and obtains mixed vapour；(4) mixed vapour condenses
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 extracted, and after layering, upper layer is finished product borneol essential oil.
2. a kind of combination sound wave extracting method of borneol essential oil as described in claim 1, it is characterised in that: in step (1), dry
Doing to moisture content is 8-12%.
3. a kind of combination sound wave extracting method of borneol essential oil as described in claim 1, it is characterised in that: in step (2), stir
The revolving speed 90-130r/min of ball mill is mixed, the time of mechanical activation is 3-7min.
4. a kind of combination sound wave extracting method of borneol essential oil as described in claim 1, it is characterised in that: the ultrasonic wave-
In microwave treatment, acoustic power 100-400W.
5. a kind of combination sound wave extracting method of borneol essential oil as claimed in claim 4, it is characterised in that: the ultrasonic wave-
In microwave treatment, acoustic power 200-300W.
6. a kind of combination sound wave extracting method of borneol essential oil as described in claim 1, it is characterised in that: the ultrasonic wave-
In microwave treatment, handling duration 2-15min.
7. a kind of combination sound wave extracting method of borneol essential oil as claimed in claim 6, it is characterised in that: the ultrasonic wave-
In microwave treatment, handling duration 5-10min.
8. such as a kind of described in any item combination sound wave extracting methods of borneol essential oil of claim 1-7, it is characterised in that: described
Distillation time is selected in 1-3h.
9. a kind of combination sound wave extracting method of borneol essential oil as claimed in claim 8, it is characterised in that: the distillation time
For 2-3h.
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| CN111019761A (en) * | 2019-11-08 | 2020-04-17 | 华侨大学 | Method for extracting grapefruit flower essential oil through ultrasonic-microwave synergistic extraction |
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Application publication date: 20190712 |