CN110003982A - A kind of combined type borneol method of extraction of essential oil - Google Patents
A kind of combined type borneol method of extraction of essential oil Download PDFInfo
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- CN110003982A CN110003982A CN201910283647.2A CN201910283647A CN110003982A CN 110003982 A CN110003982 A CN 110003982A CN 201910283647 A CN201910283647 A CN 201910283647A CN 110003982 A CN110003982 A CN 110003982A
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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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Abstract
The application provides a kind of combined type borneol method of extraction of essential oil, belongs to from raw materials recovery or purification essential oil technical field.Borneol camphortree leaf is taken, is dried；In agitating ball mill, dry borneol camphortree leaf mechanical activation is obtained into powder；Powder is added in supercritical device, is pressurized to supercriticality, is dissolved with supercritical medium to raw material powder；After stable operation to be extracted, ultrasonic wave is opened；After reaching extraction time, solute, as finished product borneol essential oil is precipitated dissolved with the supercritical medium decompression separation of solute.The application is applied to extraction of essential oil, has many advantages, such as that extraction efficiency is high, extracting cycle is short, energy conservation.
Description
Technical field
This application involves a kind of combined type borneol method of extraction of essential oil, 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, a kind of extraction efficiency is high, extracting cycle is short, energy conservation combined type borneol essential oil
Extracting method.
To achieve the above object, the technical solution that the application takes is as follows:
A kind of combined type borneol method of extraction of essential oil, 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) powder is added to supercritical device
In, it is pressurized to supercriticality, raw material powder is dissolved with supercritical medium；(4) it after stable operation to be extracted, opens super
Sound wave；(5) after reaching extraction time, solute, as finished product borneol essential oil is precipitated dissolved with the supercritical medium decompression separation of solute.
In extraction scheme provided by this programme, activating pretreatment is first carried out with mechanical lapping, under the action of mechanical force,
It is preliminary to destroy plant cell wall and particle is made to glide, recycle the high-dissolvability of supercritical medium to extract effective in borneol powder
Ingredient, while passing through the extraction process of the assisted and strengthened supercritical fluid of ultrasonic wave, decompression separation obtains finished product later.Ultrasonic wave with
Postcritical cooperation not only realizes the high dissolutionization of effective component, and also further reinforcing destroys cell wall, quickening effectively at
The dissolution divided, therefore entire extraction process has had both extraction and isolated double action, process, technical process are simple without phase-change for material
Single, the residual of organic solvent, does not only improve recovery rate, but also shorten extraction time, achievees the purpose that improve extraction efficiency,
Recovery rate can reach 0.49% or so.
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 first study the powder mesh number in raw material layer, the results showed that ginseng
10 mesh or more should be maintained at by adding the powder size of supercritical extract, and mesh number is too small, then since particle is larger, with supercritical fluid
Effective contact surface is reduced, and the residue that purpose essential oil is precipitated in particle appearance can stop the precipitation of internal layer essential oil；Increase powder mesh number,
Especially after mesh number increases to 20 mesh, the atmosphere of supercritical fluid reaches compatible cooperation with the effective contact area of particle, this
When extraction yield can reach 0.4% or more；Continue to increase mesh number, although extraction yield has a degree of promotion, but meeting in this way
Increase the work of mechanical activation early period, it is between the promotion of extraction yield and early period pretreated cost and incompatible, therefore, raw material grain
Degree is suitable for control between 10-50 mesh, and preferably 20-40 mesh.
On the basis of the studies above, we also study the technique of supercritical extract, and have determined more excellent
The supercritical process of choosing: supercritical extract temperature is 30-70 DEG C.We to extraction temperature carry out research process in, Wo Menfa
It is existing: with CO2CO for spe medium, when extraction temperature is higher than 30 DEG C, in equipment2It is initially located in supercriticality, the atmosphere in equipment
It encloses and is rendered as the critical special state of gas-liquid, in the overcritical atmosphere, the purpose essential oil in raw material powder is gradually separated simultaneously
It is precipitated；Especially when extraction temperature rises to 40 DEG C or more, this overcritical atmosphere is more significant, the purpose being precipitated accordingly
Essential oil increment is significant, continues to increase temperature, then since the device space is limited, open ended spe medium such as CO2Almost all locate
In supercriticality, therefore, when temperature is more than after 60 DEG C, continue heating to extraction yield/recovery rate there is no too many contribution, it should
Trend has similar embodiment under different ultrasonic frequencies, and therefore, supercritical extract temperature is 30-70 DEG C, and preferably
50-60℃.The extraction process will not generate phase transformation, and extraction yield is high, and without using organic solvent, good product quality does not have yet
Environmental pollution.
On the basis of the studies above, we test the extracting pressure under different ultrasonic frequencies respectively, as a result
Show: under different ultrasonic frequencies, extracting pressure is in 10-22MPa range, essential oil yield trend having the same, and essence
Oily yield is generally ideal, and especially when extracting pressure is 16-19MPa, effect of extracting is significant.
On the basis of the studies above, we test the extraction time under different supersonic frequencies, the results showed that
Under different ultrasonic frequencies, extraction time is in 60-100min, essential oil yield trend having the same, and essential oil yield is general
All over ideal, especially when extraction time control is in 80-100min, effect of extracting is significant.
On the basis of the studies above, we test the extraction time under different supersonic frequencies, the results showed that
Under different ultrasonic frequencies, ultrasonic power is in 80-400W, essential oil yield trend having the same, and essential oil yield is general
All over traditional essential oil yield is higher than, especially when ultrasonic power is in 160-320W, effect of extracting is significant.
Detailed description of the invention
Fig. 1 is influence of the extraction temperature to borneol essential oil yield.
Fig. 2 is influence of the extracting pressure to borneol essential oil yield.
Fig. 3 is influence of the extraction time to borneol essential oil yield；
Fig. 4 is influence of the ultrasonic power to borneol essential oil yield；
Fig. 5 is the representative means of supercritical extraction device figure of the application.
Figure label: 1. solvent tanks；2. pressure charging system；3. shut-off valve；4. heat exchanger；5. extractor；6. reset valve；7. point
From device；8. spinner flowmeter；9. wet flow indicator.
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, surfactant 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.
Influence of the following case mainly with regard to surfactant and distillation is analyzed.
C. supercritical CO2Refer to, pressure locating for fluid (P) and temperature (T) are more than critical pressure (Pc) and stagnation temperature
This state when spending (Tc) is referred to as overcritical, hereafter mainly obtains with regard to extraction temperature extraction time and extraction time to essential oil
It influences to carry out concrete case explanation and analysis.
Wherein, supercritical CO is being carried out2Extraction temperature, pressure and three factor of time to essential oil yield influence research
Before, we first test with regard to granularity/mesh number of raw material powder, to determine the state for the treatment of material, referring specifically to embodiment
1。
Embodiment 1: influence of the different material powder size to essential oil yield
Carrying out suitable supercritical CO2When the raw material powder particle size of extraction determines, by the rough experiment of early period, we are first
First it has been determined that minimum purpose is 10 mesh, when (when carrying out mesh number confirmation, we have selected following raw material powder particle size in 10 mesh
Two kinds of extraction conditions, which are used as, to be represented: 1. extraction temperature is 35 DEG C, extracting pressure 20MPa, extraction time 2.5h；2. 45 DEG C, extraction
Pressure 25MPa, extraction time 2.5h), essential oil yield substantially with traditional water distillation (processing route: drying → mechanical activation →
Water distillation extraction → condensation → water-oil separating → water-oil separating, drying therein and mechanical activation are consistent with present case；Essential oil
Yield is about that essential oil yield 0.35%) maintains an equal level；When improving raw material powder mesh number, especially more than 20 mesh of mesh number raising value
When, essential oil yield is promoted to 0.4% or more, and the increase rate of essential oil yield is 14% (increase rate=raising of traditional water distillation
Essential oil yield when the ratio between value and traditional essential oil yield such as mesh number are 20 mesh is 0.40%, increase rate=(0.40-
0.35)/0.35, multiplied by 100%, as 14%；Essential oil yield when mesh number is 30 mesh is 0.42%, increase rate 20%)
More than.Therefore, raw material particle size/mesh number is suitable for control in 10-50 mesh in present case, because of the entire process flow in the application
In, the refinement of raw material mesh number is from the mechanical activation of preceding working procedure, therefore overall cost and treatment effeciency consider, participate in super faces
Raw material mesh number/partial size of boundary's extraction reaction is suitable for control in 20-40 mesh, and preferably 30 mesh.
Therefore in following experiment using 30 mesh as overcritical raw material layer in dominant powder partial size, select CO2It is situated between as extraction
Matter, and to extraction temperature, extracting pressure and extraction time is further is studied, referring to embodiment 2-4.
Embodiment 2: influence of the different extraction temperatures to essential oil yield
On the basis of embodiment 1, we test extraction temperature (remaining parameter is referring to embodiment 1), as a result table
It is bright: in conjunction with Fig. 1, when extraction temperature 30 DEG C nearby when, the recovery rate of essential oil is substantially and traditional water distillation deviation is little, wherein without
Sonication assisted treatment near 0.35%, the more low this deviation of ultrasonic frequency is bigger, when ultrasonic frequency be 20KHz
When, essential oil yield can reach 0.4% at 30 DEG C；Increase extraction temperature, recovery rate is then almost incremented by therewith, in 30-40 DEG C of area
Between in range when, the amplification under different ultrasonic frequencies is almost the same；But when temperature is more than 40 DEG C of (as shown in Figure 1 40-50 DEG C
Section) when, the amplification and 30-40 DEG C of temperature range amplification of no ultrasonic wave auxiliary are almost the same, and the amplification of 20KHz significantly mentions
Height, then without so significant under 25KHz, 30KHz ultrasonic frequency；Continue to heat up, the amplification of 30KHz ultrasonic frequency will continue to
It keeps, since the supercritical temperature of particular medium has a specific supercritical temperature, essential oil yield under other ultrasonic frequencies
Do not increase significantly then；Therefore when extraction temperature is at 50-60 DEG C, the condition can be reached substantially under different ultrasonic frequencies
Under peak value (peak value that the peak value of 20KHz is 0.5%, 30KHz be 0.45%)；Continue to heat up, then since overcritical atmosphere is full
With, heating to essential oil yield there is no notable contribution, recovery rate does not have and rises appreciably.Therefore, under comprehensive consideration, extraction temperature
It is suitable for control at 30-70 DEG C, and at preferably 50-60 DEG C, extraction of essential oil effect is preferable.
Embodiment 3: influence of the different extracting pressures to essential oil yield
On the basis of embodiment 1 and embodiment 2, we carry out extracting pressure (remaining parameter is referring to embodiment 1) real
It tests, the results showed that in conjunction with Fig. 2, under different ultrasonic frequencies, when extracting pressure rises to 13MPA from 10MPa, no ultrasonic treatment
Under essential oil yield it is substantially consistent (near i.e. 0.35%) with the essential oil yield under the distillation of traditional water, and the essence under ultrasonication
Oily yield is generally higher than the essential oil yield of traditional water distillation；Extracting pressure is increased, when extracting pressure is promoted to 13-16MPa, no
Generally reach maximum with the extraction of essential oil rate amplification under ultrasonic frequency, extraction of essential oil rate is 0.4% or more；Continue to improve extraction
Pressure power, the amplification of extraction of essential oil rate slows down (then amplification continues to increase under 30KHz vibration wave frequency rate), but essential oil yield is still mentioning
It rises, and arrives separately in 16-19MPa peak value (essential oil under essential oil yield is about 0.46%, 20KHz under 30KHz under this condition
0.49%) yield is about；Continue to be pressurized, then since the device space is limited, the substantially overcritical saturation of spe medium in the space,
Therefore boosting is no longer significant to the contribution of extraction, and essential oil yield tends towards stability near 0.46%-0.49%；The trend is at other
Also there is consistent embodiment under ultrasonic wave, will not enumerate herein.Therefore, comprehensive treatment effect is considered with processing cost, extraction pressure
Power is selected in 10-22MPa, and when preferably 16-19MPa, extraction of essential oil effect is preferable.
Embodiment 4: influence of the different extraction times to essential oil yield
On the basis of embodiment 1, embodiment 2 and embodiment 3, due to extraction temperature and extraction time determined substantially it is super
Critical state, therefore influence of the extraction time to effect of extracting is relatively weak, with being incremented by for time, essential oil yield is in incremental
Trend in conjunction with Fig. 3, and substantially exceeds traditional essential oil yield in 60min；Essential oil yield when more than the section 60-80min
Amplification is significant；Continue extension extraction time and the peak value of extraction of essential oil is basically reached in 90min due to the saturation of spe medium
(under 30KHz essential oil yield be about under 0.45%, 25KHz essential oil yield be about under 0.46%, 20KHz essential oil yield be about
0.48%)；The trend also has consistent embodiment under other ultrasonic waves, will not enumerate herein.
Embodiment 5: influence of the different ultrasonic power to essential oil yield
Embodiment 2, embodiment 3 and embodiment 4 on the basis of, we determined that the overcritical power in extraction process,
Below based on above-mentioned experimental result, the ultrasonic technique of auxiliary first supercritical processing is tested, due to the frequency of ultrasonic wave
Rate cardinal temperature, therefore test mainly using ultrasonic power as research object.
In conjunction with Fig. 4, under different ultrasonic frequencies, with the raising of ultrasonic power, in low ultrasonic power, essential oil is obtained
Rate shows different trend, and (essential oil yield persistently increases under the conditions of 25KHz, 20KHz, then there is essential oil yield under the conditions of 30KHz
Downward trend), but universal 0.35% for being all higher than traditional water and distilling；When ultrasonic power is more than 160W, essential oil yield is with super
The raising of acoustic power shows raising trend, wherein the essential oil yield amplification under the conditions of 20KHz still maintains, and 25KHz
Under the conditions of essential oil yield amplification significantly improve；Continue to improve ultrasonic power, the essential oil yield under the conditions of 25KHz, 30KHz continues
It improves, but has reached peak value under the conditions of 20KHz；Become under different ultrasonic frequencies as difference is presented in the raising of ultrasonic power
Gesture, main cause may be related with the intensity (i.e. ultrasonic frequency and ultrasonic power is integrated) of ultrasonic wave, therefore synthesis is examined
Be suitable for controlling ultrasonic power in 80-400W under amount, especially when ultrasonic power is in 160-320W, essential oil yield compared with
For ideal.
On the basis of above-mentioned experiment and analysis of cases, we carry out raw material powder in such a way that ultrasonic wave auxiliary is postcritical
Extraction processing, 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 extracts in overcritical atmosphere；(4) after supercritical fluid extraction system stable operation, it is auxiliary to open ultrasonic wave
Help processing；(5) after reaching extraction time, dissolved with the CO of solute2Solute, as finished product borneol essential oil is precipitated by decompression separation.
Wherein, the structure of means of supercritical extraction device can refer to shown in Fig. 5:
First the suitable mesh number raw material powder after mechanical activation is placed on the raw material layer in extractor 5, is former in solvent tank 1
Expect solvent C O2, it is entered into after pressure charging system 2 is pressurized to setting value, opening stop valve 3 is heated to setting value through heat exchanger 4
Afterwards, it is transferred in extractor 5 and carries out supercritical extract, and pass through T1、P1Control the temperature and pressure in extraction process；Wait extract
Take that the time is up to standard, after extraction process, close the shut-off valve 3 and separator rear in front of heater shut-off valve 3 and point
Reset valve 6 from 7 rear of device opens reset valve 6, dissolved with the CO of solute2Enter separator 7 by reset valve 6 (pressure reducing valve), and
Pass through T2、P2The temperature and pressure in extraction process is controlled, after solute is precipitated；Open the reset valve 6 at 7 rear of separator, material warp
Spinner flowmeter 8, wet flow indicator 9 export, as finished product borneol essential oil.
In conjunction with above-mentioned means of supercritical extraction device and four concrete cases (embodiment 6,7,8,9) selected, to the application's
Extraction scheme does whole annotation.
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 90r/min
7min is activated, powder is obtained；
(3) supercritical CO2Extraction and separation: 30 mesh powders are put into raw material layer, regulation system temperature is 50 DEG C, and pressure is
16MPa, extraction time 80min；
(4) ultrasonic wave assists: after supercritical fluid extraction system reaches stable operation, opening ultrasonic wave, ultrasonic wave frequency
Rate is 20KHz, ultrasonic power 240W；
(5) decompression separation: after reaching extraction time, dissolved with the CO of solute2Enter separator by pressure reducing valve and solute be precipitated,
Borneol essential oil is obtained, borneol extraction of essential oil rate is 0.45% or so.
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 100r/min
5min is activated, powder is obtained；
(3) supercritical CO2Extraction and separation: 30 mesh powders are put into raw material layer, regulation system temperature is 50 DEG C, and pressure is
16MPa, extraction time 80min；
(4) ultrasonic wave assists: after supercritical fluid extraction system reaches stable operation, opening ultrasonic wave, ultrasonic wave frequency
Rate is 20KHz, ultrasonic power 240W；
(5) decompression separation: after reaching extraction time, dissolved with the CO of solute2Enter separator by pressure reducing valve and solute be precipitated,
Borneol essential oil is obtained, borneol extraction of essential oil rate is 0.46% or so.
Embodiment 8
(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) supercritical CO2Extraction and separation: 30 mesh powders are put into raw material layer, regulation system temperature is 50 DEG C, and pressure is
16MPa, extraction time 80min；
(4) ultrasonic wave assists: after supercritical fluid extraction system reaches stable operation, opening ultrasonic wave, ultrasonic wave frequency
Rate is 20KHz, ultrasonic power 240W；
(5) decompression separation: after reaching extraction time, dissolved with the CO of solute2Enter separator by pressure reducing valve and solute be precipitated,
Borneol essential oil is obtained, borneol extraction of essential oil rate is 0.48% or so.
Embodiment 9
(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) supercritical CO2Extraction and separation: 30 mesh powders are put into raw material layer, regulation system temperature is 50 DEG C, and pressure is
16MPa, extraction time 80min；
(4) ultrasonic wave assists: after supercritical fluid extraction system reaches stable operation, opening ultrasonic wave, ultrasonic wave frequency
Rate is 20KHz, ultrasonic power 240W；
(5) decompression separation: after reaching extraction time, dissolved with the CO of solute2Enter separator by pressure reducing valve and solute be precipitated,
Borneol essential oil is obtained, borneol extraction of essential oil rate is 0.49% or so.
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 combined type borneol method of extraction of essential oil, which comprises the following steps: (1) take borneol camphortree leaf, dry
It is dry；(2) in agitating ball mill, the drying borneol camphortree leaf mechanical activation of step (1) is obtained into powder；(3) powder is added to
In supercritical device, it is pressurized to supercriticality, raw material powder is dissolved with supercritical medium；(4) stable fortune to be extracted
After row, ultrasonic wave is opened；(5) after reaching extraction time, dissolved with solute supercritical medium decompression separation be precipitated solute, as at
Product borneol essential oil.
2. a kind of combined type borneol method of extraction of essential oil 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 combined type borneol method of extraction of essential oil 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 combined type borneol method of extraction of essential oil as described in claim 1, it is characterised in that: in step (3), powder grain
Diameter is 10-50 mesh.
5. a kind of combined type borneol method of extraction of essential oil as claimed in claim 4, it is characterised in that: in step (3), powder grain
Diameter is 20-40 mesh.
6. a kind of combined type borneol method of extraction of essential oil as described in any one in claim 1-5, it is characterised in that: step (3)
In, supercritical medium CO2。
7. a kind of combined type borneol method of extraction of essential oil as claimed in claim 6, it is characterised in that: the extraction temperature is
30-70 DEG C, extracting pressure 10-22MPa.
8. a kind of combined type borneol method of extraction of essential oil as claimed in claim 7, it is characterised in that: the extraction temperature is
50-60 DEG C, extracting pressure 16-19MPa.
9. a kind of combined type borneol method of extraction of essential oil as described in any one in claim 1-5, it is characterised in that: step (4)
In, ultrasonic frequency 20-30KHz, ultrasonic power 80-400W.
10. a kind of combined type borneol method of extraction of essential oil as claimed in claim 9, it is characterised in that: the ultrasonic power
For 160-320W.
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| CN112322390A (en) * | 2020-10-20 | 2021-02-05 | 安徽省泰林生态农业科技发展有限公司 | Method for extracting essential oil of sequoia zhongshanensis |
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