CN109913318A - A kind of supercritical extraction method of borneol essential oil - Google Patents
A kind of supercritical extraction method of borneol essential oil Download PDFInfo
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Abstract
The application provides a kind of supercritical extraction method of borneol 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 put into raw material layer, and regulation system temperature and pressure to setting value extracts effective component in the atmosphere of supercritical CO 2；After reaching extraction time, simultaneously solute is precipitated in CO2 decompression separation dissolved with solute, obtains finished product borneol essential oil.The application is applied to extraction of essential oil, has many advantages, such as material process, extraction yield height, organic solvent-free residual without phase-change.
Description
Technical field
This application involves a kind of supercritical extraction method of borneol essential oil, belong to from raw materials recovery or purification essence oil tech
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 a kind of material, process, extraction yield be high without phase-change, the remaining borneol essence of organic solvent-free
The supercritical extraction method of oil.
To achieve the above object, the technical solution that the application takes is as follows:
A kind of supercritical extraction method of borneol essential oil, comprising the following steps: (1) take borneol camphortree leaf, dry；(2) exist
In agitating ball mill, the drying borneol camphortree leaf mechanical activation of step (1) is obtained into powder；(3) powder is put into raw material layer, adjusts
System temperature and pressure are to setting value, in supercritical CO2Atmosphere in extract effective component；(4) molten after reaching extraction time
There is the CO of solute2Simultaneously solute is precipitated in decompression separation, obtains finished product borneol essential oil.
In extraction scheme provided by this programme, with supercritical CO2The mode that atmosphere carries out extraction and separation obtains borneol essence
Oil first carries out mechanical lapping pretreatment to borneol essential oil, is allowed to mesh number and is reduced to optimum range before carrying out supercritical extract,
It is placed in overcritical equipment again, the direct extraction of borneol essential oil is completed in control temperature, pressure and practice.The technique is by means of CO2
Strong extractibility the extraction and separation of purpose essential oil can be completed, entire separation process does not have solvent without carrying out phase transition process
Addition, DNA purity is high, and without post-processing, recovery rate is 0.41% 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 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 30-60 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 35 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 CO2Almost it all is at supercritical state
Therefore state when temperature is more than after 50 DEG C, continues heating to extraction yield/recovery rate there is no too many contribution, therefore, overcritical
Extraction temperature is 30-60 DEG C, and preferably 35-50 DEG C.The extraction process will not generate phase transformation, and extraction yield is high, and without using
Organic solvent, good product quality, also without environmental pollution.
On the basis of the studies above, we test the extracting pressure under different temperatures respectively, the results showed that
Under different temperatures, extracting pressure is in 15-30MPa range, essential oil yield trend having the same, and essential oil yield is generally more
Ideal, especially when extracting pressure is 20-25MPa, effect of extracting is significant.
On the basis of the studies above, we test the extraction time under different extraction temperatures, force combination,
The result shows that: under the conditions of different temperatures, force combination, extraction time in 1.5-3.5h, essential oil yield it is having the same become
Gesture, and essential oil yield is generally ideal, especially when extraction time control is in 2-3h, effect of extracting is significant.
In summary the considerations of three aspect of temperature, pressure and time, supercritical CO that we finally obtain2Ideal technology
Condition is 35-45 DEG C of extraction temperature, extracting pressure 20-25MPa, extraction time 2-3h.
Detailed description of the invention
Fig. 1 is influence of the powder size to borneol essential oil yield.
Fig. 2 is influence of the extraction temperature to borneol essential oil yield.
Fig. 3 is influence of the extracting pressure to borneol essential oil yield.
Fig. 4 is influence of the extraction time 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, supercritical CO2The aspect of technique three:
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.
Following case is mainly with regard to supercritical CO2Influence 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, in conjunction with Fig. 1, essential oil yield is promoted to 0.4% or more, and the increase rate of essential oil yield is 14% (raising of traditional water distillation
Essential oil yield when the ratio between rate=raising 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%, and increase rate is
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 processing in the application
In process, 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
Raw material mesh number/partial size of supercritical extract 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
Bright: in conjunction with Fig. 2, when extraction temperature is lower than 30 DEG C, the recovery rate of essential oil is substantially consistent with the distillation of traditional water (i.e. attached 0.35%
Closely)；Increase extraction temperature, recovery rate is then almost linear therewith to be incremented by；Since the supercritical temperature of particular medium has one
Specific supercritical temperature, therefore when extraction temperature is higher than 50 DEG C, reach peak value (0.42%) under this condition；Continue to heat up,
Then since overcritical atmosphere is saturated, to essential oil yield there is no notable contribution, recovery rate does not have and rises appreciably for heating, and basic
It is maintained near 0.41-0.42%.Therefore, under comprehensive consideration, extraction temperature is suitable for control at 30-60 DEG C, and preferably 35-50
DEG C when, 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. 3, when extraction temperature is 25 DEG C, when extracting pressure rises to 15MPA from 10MPa, essential oil yield can
Persistently it is increased to the level of traditional water distillation；Extracting pressure is increased, when extracting pressure is promoted to 20MPa, extraction of essential oil rate increases
Width reaches maximum, and extraction of essential oil rate is 0.4% at this time, continues to improve extracting pressure, the amplification of extraction of essential oil rate slows down, but essential oil
Yield is still being promoted, and peak value (about 0.42%) under this condition is reached in 25MPa；Continue to be pressurized, then due to equipment sky
Between limited, the substantially overcritical saturation of spe medium in the space, therefore boost, essential oil yield no longer significant to the contribution of extraction
It tends towards stability near 0.4%-0.42%；We have carried out same similar experiment to 35 DEG C, 50 DEG C, also obtain similar
Trend, therefore, comprehensive treatment effect are considered with processing cost, and extracting pressure is selected in 15-30MPa, and preferably 20-25MPa
When, 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, and essential oil yield and traditional water distilling effect maintain an equal level in 1.5h, it is significant more than essential oil yield amplification after 1.5h, due to extraction
The saturation for taking medium basically reaches the peak value (about 0.42%) of extraction of essential oil in 2.5h, and the trend is in different temperature, pressure
It is unanimously embodied under power, 20MPa35 DEG C and 25MPa45 DEG C as given by Fig. 3.
On the basis of above-mentioned experiment and analysis of cases, we carry out extraction processing to raw material powder in a manner of overcritical, 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 reaching extraction time, dissolved with the CO of solute2It is analysed by decompression separation
Solute out, as finished product borneol essential oil.
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 5,6,7,8) selected, to the application's
Extraction scheme does whole annotation.
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 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 35 DEG C, and pressure is
20MPa, extraction time 2.5h；
(4) 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 0.37% or so.
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 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 35 DEG C, and pressure is
20MPa, extraction time 2.5h；
(4) 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 0.38% 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 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 45 DEG C, and pressure is
25MPa, extraction time 2.5h；
(4) 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 0.40% 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 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 45 DEG C, and pressure is
25MPa, extraction time 2.5h；
(4) 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 0.41% 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 supercritical extraction method of borneol 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 put into original
The bed of material, regulation system temperature and pressure to setting value extract effective component in the atmosphere of supercritical CO 2；(4) reach extraction
After time, simultaneously solute is precipitated in CO2 decompression separation dissolved with solute, obtains finished product borneol essential oil.
2. a kind of supercritical extraction method of borneol essential oil as described in claim 1, it is characterised in that: in step (1), drying
It is 8-12% to moisture content.
3. a kind of supercritical extraction method of borneol essential oil as described in claim 1, it is characterised in that: in step (2), stirring
The revolving speed 90-130r/min of ball mill, the time of mechanical activation are 3-7min.
4. a kind of supercritical extraction method of borneol essential oil as described in claim 1, it is characterised in that: described in step (3)
Powder mesh number is 10-50 mesh.
5. a kind of supercritical extraction method of borneol essential oil as claimed in claim 4, it is characterised in that: the powder mesh number is
20-40 mesh.
6. a kind of supercritical extraction method of borneol essential oil as described in any one in claim 1-5, it is characterised in that: step
(3) in, the extraction temperature is 30-60 DEG C, extracting pressure 15-30MPa.
7. a kind of supercritical extraction method of borneol essential oil as claimed in claim 6, it is characterised in that: the extraction temperature is
35-50 DEG C, extracting pressure 20-25MPa.
8. a kind of supercritical extraction method of borneol essential oil as described in any one in claim 1-5, it is characterised in that: step
(3) in, the extraction time is 1.5-3.5h.
9. a kind of supercritical extraction method of borneol essential oil as claimed in claim 8, it is characterised in that: the extraction time is
2-3h。
10. a kind of supercritical extraction method of borneol essential oil as described in any one in claim 1-5, it is characterised in that: step
(3) in, extraction temperature is 35-45 DEG C, extracting pressure 20-25MPa, extraction time 2-3h.
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Cited By (1)
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Application publication date: 20190621 |