CN107904017A - A kind of agilawood essential oil preparation process - Google Patents
A kind of agilawood essential oil preparation process Download PDFInfo
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- CN107904017A CN107904017A CN201711157274.1A CN201711157274A CN107904017A CN 107904017 A CN107904017 A CN 107904017A CN 201711157274 A CN201711157274 A CN 201711157274A CN 107904017 A CN107904017 A CN 107904017A
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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
- C11B9/022—Refining
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
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- Medicines Containing Plant Substances (AREA)
- Fats And Perfumes (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of preparation method of agilawood essential oil, the described method comprises the following steps:Step 1 Chinese Eaglewood Wood and solvent mixing, wherein Chinese Eaglewood Wood:Solvent=1:10, heating is until slightly boiling;Be refluxed 1.5 2.5 it is small when;Temperature fall 20 30 minutes, continues to cool to precipitation solid;Filtering, obtains solid powder, recycles filtrate;The solid powder being obtained by filtration is carried out second extraction by step 2 with solvent, and method is the same as step 1;Step 3 is extracted the solid powder being obtained by filtration with solvent three times, and method is the same as step 1;Step 4 merges obtained filtrate after extraction three times, it is closed be stored at room temperature 12 24 it is small when;Filtrate is filtered after step 5 is stood, and filters out solid, collects filtrate;During step 6 heating concentration filtrate to dusting, stop heating, concentrate is obtained by filtration, mix, obtain agilawood essential oil.
Description
Technical field:
The present invention relates to a kind of extraction of spices, a kind of more particularly to a kind of extraction of aromatic oil, and in particular to agalloch eaglewood essence
The preparation method of oil.
Background technology:
Agalloch eaglewood originates in north India, Laos, Cambodia, Malaysia, Indonesia, the Southeast Asia such as Vietnam and China
13 states.These trees can usually be infected by fungi, and slowly form a kind of knot of the resin to give out a sweet perfume and sawdust
Zoarium, this material are commonly referred to as agalloch eaglewood (Aloeswood), agalloch eaglewood (Agarwood) and trichoderma.
Agilawood essential oil be extracted from agalloch eaglewood there is certain fragrance and volatile oily mater, be the virtue that agalloch eaglewood has
Fragrant component concentrates material, the agilawood essential oils such as the oil obtained afterwards, fat, alcohol, wax, terpenes through refinement has human body multiple work(
Effect, such as:Improvement gas field, pressure of releiving, sleeping resist strongly fragrant, conditioning body and mind and promote body metabolism etc..In shower and steep foot
Hot water in instill a few drop agilawood essential oils, can achieve the purpose that invigorate blood circulation channels and collaterals, moreover it is possible to reach remove tinea pedis foot odour effect.By
Linaloe oil after the non-renewable of natural agilawood, refinement just more seems rare and precious.
The preparation of agilawood essential oil.The following three kinds of methods of generally use:
First, steam distillation method.
The component of agilawood essential oil, bubble point have certain volatility under normal pressure usually between 150 to 300 degrees Celsius.
In a heated condition, can be escaped with vapor.Distilled after plant is crushed containing fragrant position, essential oil and water are distilling
Azeotropic occurs in kettle, agglomerates oil droplet after condensing unit, carries out respectively obtaining essential oil and Hua Shui after water-oil separating.Having
On gymnastics is made, and there is air-distillation, distillation under pressure, vacuum distillation, also there is immersion distillation and water proof distillation.From oil water separator point
Separate out the essential oil come and be known as " crude oil ", it is necessary to carry out static, clarification, dehydration, obtain " directly oil ".Direct oil is taken off
Refined essential oil is obtained after water, filtering, purification.The essential oil that steam distillation method obtains is typically only capable to access in plant fragrance component
High volatile ingredient, therefore extraction yield is than relatively low.Agilawood essential oil adopts this method rare in the industry.
2nd, solvent extraction.
This method is also referred to as solvent extraction method, is to utilize volatile organic solvent by some components of the plant containing fragrant position
It is dissolved out, and solvent is removed by the method distilled or evaporated using the features such as organic solvent low boiling point and high volatile,
So as to obtain plants essential oil.Through frequently with organic solvent include ethanol, ether, acetone, petroleum ether, benzene, formaldehyde etc..Simply
Say that can be dissolved in the material of water can largely be dissolved in organic solvent, so the result that solvent extraction obtains includes in ground
Most of material that steam distillation obtains.In addition, the solvability of organic solvent is much stronger than water, therefore some is original
The material that can not be dissolved in water can be dissolved into organic solvent, therefore the result that solvent extraction obtains also includes vapor
The material that the way of distillation cannot access -- these materials are mainly chromone, vegetable wax, resin and pigment.Therefore solvent extraction
The yield for preparing essential oil is usually more much higher than the method for steam distillation.Such a method is used in the industry relatively generally, by molten
Agent extraction prepares refined agilawood essential oil, and the ratio that it is obtained is higher than steam distillation, the agalloch eaglewood volatile constituent of reservation
It is abundant.
3rd, supercritical extraction.
This method can be understood as a kind of special shape of solvent extraction, and what is used is not usual vehicle, but
Liquid carbon dioxide under high pressure conditions.Under elevated pressure conditions, carbon dioxide can be a kind of liquid, have very strong molten
Solution ability, can come out plant containing the terpene compound in fragrant component, chromone, vegetable wax, resin and pigmentolysis.These
Compound and liquid carbon dioxide are depressurized after being transferred to separating still, and carbon dioxide becomes gas effusion under normal pressure, remains
Under be exactly terpene compound, chromone, vegetable wax, resin and pigment mixture (crude oil).Pass through the method for rectification under vacuum
These mixtures are handled, it is possible to obtain refined essential oil.
The prior art also discloses following methods:Microwave assisting method extracts agilawood essential oil,
Method is:Weigh the 25g eaglewood powders for being crushed to 10-20 mesh.Microwave power 300W, 55-50 DEG C of temperature bound,
It is 1 according to total solid-to-liquid ratio respectively using 85%, 93%, 95% ethanol as solvent:14, point 3 progress intermittent type microwave extractions.
Or the agalloch eaglewood powder for taking 3kg to crush and sieving, load extractor, 93% second is added according to certain solid-to-liquid ratio
Alcohol;Adjusting screw rod pump makes material reach certain flow, when circulation is preheated to required temperature, starts microwave, microwave power is arrived in adjusting
2400~3200W, makes material in flow process while receives microwave irradiation, records temperature rise;Centrifuge, filter residue carries repeatedly
Take;After extraction, merge extracting solution, take part solution that solvent is recovered under reduced pressure.
Optimal parameter is:Concentration of alcohol 93%, material size are 40 mesh, solid-to-liquid ratio 1:8.5, mass flow 78L/h, preheating
Temperature is 45 DEG C, and 15 DEG C of temperature rise, is extracted 2 times.The yield 6.9% of crude extract, agilawood essential oil yield 0.68%.
Chinese patent CN201410180768.1 discloses a kind of extracting method of agilawood essential oil.Agalloch eaglewood raw material is crushed simultaneously
Water is added to stir into slurries, slurries cross colloid mill;The slurries after colloid mill are completed through ultrasonication, then with cellulase water
Solution;Enzyme-deactivating after hydrolysis, filters, and the first filtrate of gained is extracted with 95% ethanol, takes organic phase to filter again, the second filtrate of gained
Ethanol is distilled off, obtains agilawood essential oil.
In addition CN201410028499.7 and CN201410266392.6 also discloses that the extracting method of agilawood essential oil
The present inventor has found that there are following defect for the above method by research:
1, for organic reagent based on petroleum ether, n-hexane, chloroform, ether or ethyl acetate, the reagent toxicity is larger;And make
Extracted with ethanol microwave or enzyme, security is relatively low or cost is higher.
2, supercritical carbon dioxide extracting, equipment and pertinent instruments cost are higher, and whether ultralow temperature has this product principal component
Correlative study is not done in influence, though can obtain compared with high yield pulp1, causes the price of product to remain high since cost is higher.
3, agalloch eaglewood crushing mesh number is larger, it is difficult to which main component is effectively extracted, causes the waste of agalloch eaglewood raw material, no
Abundant beneficial to the rare medicinal material uses.
4, extraction temperature is not suitable for, and temperature is excessive, there is degraded risk to main component;Temperature is relatively low, to main component
Extraction yield does not reach preferable state.
To overcome drawbacks described above, the present inventor designs and has tested a kind of extracting method of brand-new agilawood essential oil.
The content of the invention:
The present inventor designs and has tested a kind of extracting method of brand-new agilawood essential oil on the basis of existing technology,
The method technique of the present invention is simple, easy to operate, using common ethanol, propane diols and water, securely and reliably, while not
Introduce other organic reagents.
The present invention is common reagent using ethanol, propane diols and water, while it can be controlled to meet the requirement of IIG, is grasped
Make simple for process, original rare agalloch eaglewood resource can be played to maximum, it is condensed go out essential oil so that more people can
Safe to use, effective agalloch eaglewood product.
Our test of many times, determine preparation process feasibility, and simple easily operated, at the same will finally prepare it is heavy
Essential oil censorship SGS is detected, and indices meet regulation requirement.For this reason, the present invention provides a kind of system of agilawood essential oil
Preparation Method, the described method comprises the following steps:Step 1 Chinese Eaglewood Wood and solvent mixing, wherein Chinese Eaglewood Wood:Solvent=1:10
(weight g:Volume ml), heating is until slightly boiling;Be refluxed 1.5-2.5 it is small when;Temperature fall 20-30 minutes, continues to cool to
Separate out solid;Filtering, obtains solid powder, recycles filtrate;
The solid powder being obtained by filtration is carried out second extraction by step 2 with solvent, and method is the same as step 1;
Step 3 is extracted the solid powder being obtained by filtration with solvent three times, and method is the same as step 1;
Step 4 merges obtained filtrate after extraction three times, it is closed be stored at room temperature 12-24 it is small when;
Filtrate is filtered after step 5 is stood, and filters out solid, collects filtrate;
During step 6 heating concentration filtrate to dusting, stop heating, concentrate is obtained by filtration, agalloch eaglewood powder is added in concentrate
The propane diols of last weight 10-20%, obtains agilawood essential oil.
Wherein, the solvent is selected from:Ethanol, propane diols and water or its mixture.Ethanol is 100% ethanol, second alcohol and water
Mixture be 95% ethanol (v/v), 90% ethanol (v/v), 85% ethanol (v/v), or 80% ethanol (v/v),
And 95% ethanol different volumes and the mixture of 5% propane diols different volumes, wherein it is preferred that 95% ethanol, ethanol,
The mixed solvent of the mixed solvent of propane diols and water, the ethanol, propane diols and water is the alcohol 95 parts by volume of 95% (V/V),
With the mixture of the propane diols of 5 parts by volume.
Preferably, preparation method of the present invention, step are as follows:
Step 1 Chinese Eaglewood Wood:95% ethanol=1:10;Heating is until ethanol slightly boiling;Condensing reflux stirring 1.5-2.5 is small
When;Temperature fall is to room temperature;Filter, recycle filtrate;
Muffin second extraction after step 2 filters, method is the same as step 1;
Muffin extracts three times after step 3 filters, and method is the same as step 1;
Step 4 merges filtrate three times, when standing 24 is small;
Filtrate filters after step 5 is stood, and removes solid, when filtrate decompression is concentrated into dusting, stops concentration, concentrate is taken
Go out, brown insoluble matter is arranged at bottom, is rinsed with 95% ethanol and is totally merged into concentrate, adds the 10- of Chinese Eaglewood Wood weight
20% propane diols (stabilizer) to obtain the final product.Another preferable, preparation method of the present invention, step is as follows:
Step is as follows:
Step 1 Chinese Eaglewood Wood:Water=1:10;Heating is until water slightly boiling;Be refluxed 1.5-2.5 it is small when;Cool to room temperature;
Filter recycling filtrate;
Muffin second extraction after step 2 filters, method is the same as step 1;
Muffin extracts three times after step 3 filters, and method is the same as step 1;
Step 4 merges filtrate three times;Stand overnight;
Step 5 filters after standing, and removes a small amount of solid impurity;60-65 DEG C of filtrate is concentrated under reduced pressure into solution muddiness, stops dense
Contracting, obtains concentrate, after filtering to obtain the final product.
Particularly preferred, preparation method of the present invention, step is as follows:
Step is as follows:
Step 1 Chinese Eaglewood Wood (150-300 mesh):Water=1:10;Heating is until water slightly boiling;Be refluxed 1.5-2.5 it is small when;
Cool to room temperature;Filter recycling filtrate;
Muffin second extraction after step 2 filters, method is the same as step 1;
Muffin carries out third time extraction using 95% ethanol for solvent after step 3 filters, and method obtains second with step 1
Alcohol extract, recycling ethanol obtain alcohol extract;
Step 4 merges water twice and carries filtrate, closed to stand overnight;
Filtrate is filtered after step 5 is stood, and removes a small amount of impurity;Filtrate is concentrated under reduced pressure into solution muddiness at 60-65 DEG C, stops
Concentration, concentrate and the alcohol extract of step 3 is merged, the 23-25% propane diols (stabilizer) of Chinese Eaglewood Wood weight, to obtain the final product.
Most preferably, preparation method of the present invention, step are as follows:
Step is as follows:
Step 1 Chinese Eaglewood Wood (150-300 mesh) adds mixed solvent (the wherein institute of the ethanol of 10 times of amounts, propane diols and water
State 10 times of amounts and add 10ml solvents, the ethanol for 1g Chinese Eaglewood Woods, the mixed solvent of propane diols and water is the second of 95% (V/V)
95 parts by volume of alcohol, and the mixture of the propane diols of 5 parts by volume);Heating is until slightly boiling;Be refluxed 1.5-2.5 it is small when;Cool to
Room temperature;Filter recycling filtrate;
Muffin second extraction after step 2 filters, method is the same as step 1;
Muffin carries out third time extraction using 95% ethanol for solvent after step 3 filters, and method obtains second with step 1
Alcohol extract, recycling ethanol obtain alcohol extract;
Step 4 merge it is all above-mentioned carry filtrate, it is closed to stand overnight;
Filtrate is filtered after step 5 is stood, and filtrate is concentrated under reduced pressure into solution muddiness at 60-65 DEG C, stops concentration, adds agalloch eaglewood
The propane diols (as stabilizer) of the 23-25% of powder weight, to obtain the final product.In the preparation method of the present invention, alcohol extracting can be by agalloch eaglewood
Required constituents extraction is complete in powder, and the alcohol extract of acquisition has alcohol fragrance;Water, which carries, to carry most of component in Chinese Eaglewood Wood
Take, and keep primitive character and state, but extract not exclusively, the Aqueous extracts of acquisition have sweet taste;The present invention, which devises, uses second
The mixed solvent extraction of alcohol, propane diols and water, propane diols had not only been taken into account the primitive component that water is put forward and had been destroyed by minimum, but also will can sink
Face powder end makes full use of, and reduces the wasting of resources.The above method of the present invention is obtained by screening, and screening process is as follows:
Include the screening of the contents such as technological parameter, solvent strength, extraction step, extracting method, method for concentration
1) technological parameter:The temperature consistent with the actual boiling point of reagent is selected to be extracted, such as:75-85 DEG C of (boiling point of ethanol
78 DEG C), 110-120 DEG C of water (100 DEG C of boiling point), fully main component can be extracted, without destroy main component.
2) solvent strength:Striking point judges, simple and practicable, alcohol extracting-striking point observation revolving bottle bottom dusting, explanation
Concentrate and finished;Water carries-and striking point observation revolving bottle solution is muddy, and illustrate to have concentrated and finish.
3) extracting method:It is divided into alcohol extracting and water carries, ethanol, mixed solvent extraction of propane diols and water etc..Through experiment, alcohol extracting
Three times, agalloch eaglewood filter cake is directly abandoned substantially without aromatic odor;And after water carries twice, alcohol extracting can be reused once, and with ethanol,
The mixed solvent of propane diols and water extracts, and propane diols had not only been taken into account the primitive component that water is put forward and destroyed by minimum, but also can be by agalloch eaglewood
Powder makes full use of, and reduces the wasting of resources, and the maximization that agilawood essential oil is obtained with this uses.
4) method for concentration:It is concentrated under reduced pressure.Alcohol extracting -40-50 DEG C of thickening temperature, water carry -60-65 DEG C of thickening temperature.
Compared to the prior art product of the invention has the advantage that as follows:
1) product keeps the main component of its original this product, will not introduce other reagents or make its equivalent risk of degrading, finally
Concentration can remove ethanol or a large amount of water.
2) extraction solvent and temperature are screened meticulously, and extraction solvent is conventional second alcohol and water, and extraction temperature, that is, solvent is in itself
The boiling point of attribute, therefore stable is kept in whole leaching process to principal component and can farthest extract out main component
There is some superiority.
3) mesh number that agalloch eaglewood crushes has fastidious, and it is 150-300 mesh that design, which crushes mesh number, can make raw material and leaching liquor
Come into full contact with, effectively main component in agalloch eaglewood can to greatest extent be extracted, the waste of raw material will not be caused.
4) preparation method is simple and practicable, and endpoint is very clear, and without production equipment costly, so as to be conducive to
The ultimate cost of agalloch eaglewood product is reduced, has certain positive effect to extending to general marketplace.
Finally evaluated by expert, it is believed that the method fragrance of the embodiment of the present invention 4 is optimal, yield highest, is most suitable for industry
Metaplasia is produced.
Optimal for fragrance below, the highest data of yield embody:
Brief description of the drawings:
The alcohol extracting of Fig. 1 first times is contrasted with second of alcohol extracting;
Second of alcohol extracting of Fig. 2 is contrasted with third time alcohol extracting;
Fig. 3 water extracts are static, solution after filtering.
Embodiment:
The present invention is further illustrated by the following examples, but not as limitation of the present invention.
Embodiment 1
Preparation method, step are as follows:
Step 1 Chinese Eaglewood Wood:95% ethanol=1:10;Heating is until ethanol slightly boiling;Condensing reflux stirring 1.5-2.5 is small
When;Temperature fall is to room temperature;Filter, recycle filtrate;
Muffin second extraction after step 2 filters, method is the same as step 1;
Muffin extracts three times after step 3 filters, and method is the same as step 1;
Step 4 merges filtrate three times, when standing 24 is small;
Filtrate filters after step 5 is stood, and removes solid, when filtrate decompression is concentrated into dusting, stops concentration, concentrate is taken
Go out, brown insoluble matter is arranged at bottom, is rinsed with 95% ethanol and is totally merged into concentrate, adds the 10- of Chinese Eaglewood Wood weight
20% propane diols (stabilizer) to obtain the final product.
Embodiment 2
Preparation method, step are as follows:
Step 1 Chinese Eaglewood Wood:Water=1:10;Heating is until water slightly boiling;Be refluxed 1.5-2.5 it is small when;Cool to room temperature;
Filter recycling filtrate;
Muffin second extraction after step 2 filters, method is the same as step 1;
Muffin extracts three times after step 3 filters, and method is the same as step 1;
Step 4 merges filtrate three times;Stand overnight;
Step 5 filters after standing, and removes a small amount of solid impurity;60-65 DEG C of filtrate is concentrated under reduced pressure into solution muddiness, stops dense
Contracting, obtains concentrate, after filtering to obtain the final product.
Embodiment 3
Preparation method, step are as follows:
Step 1 Chinese Eaglewood Wood (150-300 mesh):Water=1:10;Heating is until water slightly boiling;Be refluxed 1.5-2.5 it is small when;
Cool to room temperature;Filter recycling filtrate;
Muffin second extraction after step 2 filters, method is the same as step 1;
Muffin carries out third time extraction using 95% ethanol for solvent after step 3 filters, and method obtains second with step 1
Alcohol extract, recycling ethanol obtain alcohol extract;
Step 4 merges water twice and carries filtrate, closed to stand overnight;
Filtrate is filtered after step 5 is stood, and removes a small amount of impurity;Filtrate is concentrated under reduced pressure into solution muddiness at 60-65 DEG C, stops
Concentration, concentrate and the alcohol extract of step 3 is merged, the 23-25% propane diols (stabilizer) of Chinese Eaglewood Wood weight,.
Embodiment 4
Step is as follows:
Step 1 Chinese Eaglewood Wood (150-300 mesh) adds mixed solvent (the wherein institute of the ethanol of 10 times of amounts, propane diols and water
State 10 times of amounts and add 10ml solvents, the ethanol for 1g Chinese Eaglewood Woods, the mixed solvent of propane diols and water is the second of 95% (V/V)
95 parts by volume of alcohol, and the mixture of the propane diols of 5 parts by volume);Heating is until slightly boiling;Be refluxed 1.5-2.5 it is small when;Cool to
Room temperature;Filter recycling filtrate;
Muffin second extraction after step 2 filters, method is the same as step 1;
Muffin carries out third time extraction using 95% ethanol for solvent after step 3 filters, and method obtains second with step 1
Alcohol extract, recycling ethanol obtain alcohol extract;
Step 4 merge it is all above-mentioned carry filtrate, it is closed to stand overnight;
Filtrate is filtered after step 5 is stood, and filtrate is concentrated under reduced pressure into solution muddiness at 60-65 DEG C, stops concentration, to obtain the final product.
Claims (7)
1. a kind of preparation method of agilawood essential oil, it is characterised in that the described method comprises the following steps:
Step 1 Chinese Eaglewood Wood and solvent mixing, wherein Chinese Eaglewood Wood:Solvent=1:10, heating is until slightly boiling;It is refluxed 1.5-
2.5 it is small when;Temperature fall 20-30 minutes, continues to cool to precipitation solid;Filtering, obtains solid powder, recycles filtrate;
The solid powder being obtained by filtration is carried out second extraction by step 2 with solvent, and method is the same as step 1;
Step 3 is extracted the solid powder being obtained by filtration with solvent three times, and method is the same as step 1;
Step 4 merges obtained filtrate after extraction three times, it is closed be stored at room temperature 12-24 it is small when;
Filtrate is filtered after step 5 is stood, and filters out solid, collects filtrate;
During step 6 heating concentration filtrate to dusting, stop heating, concentrate is obtained by filtration, Chinese Eaglewood Wood weight is added in concentrate
The 10-20% propane diols of amount, obtains agilawood essential oil;
Wherein, the solvent is selected from:Ethanol, propane diols and water or their mixture.
2. preparation method according to claim 1, it is characterised in that wherein, the solvent is selected from:95% ethanol, with
And ethanol, the mixed solvent of propane diols and water.
3. preparation method according to claim 2, it is characterised in that wherein, the ethanol, the mixing of propane diols and water is molten
Agent is 95% alcohol 95 parts by volume, and the mixture of the propane diols of 5 parts by volume.
4. preparation method according to claim 1, it is characterised in that the preparation method, step are as follows:
Step 1 Chinese Eaglewood Wood:95% ethanol=1:10;Heating is until ethanol slightly boiling;When condensing reflux stirring 1.5-2.5 is small;
Temperature fall is to room temperature;Filter, recycle filtrate;
Muffin second extraction after step 2 filters, method is the same as step 1;
Muffin extracts three times after step 3 filters, and method is the same as step 1;
Step 4 merges filtrate three times, when standing 24 is small;
Filtrate filters after step 5 is stood, and removes solid, when filtrate decompression is concentrated into dusting, stops concentration, concentrate is taken out,
Brown insoluble matter is arranged at bottom, is rinsed with 95% ethanol and is totally merged into concentrate, adds the 10-20% of Chinese Eaglewood Wood weight
Propane diols to obtain the final product.
5. preparation method according to claim 1, it is characterised in that the preparation method, step are as follows:
Step 1 Chinese Eaglewood Wood:Water=1:10;Heating is until water slightly boiling;Be refluxed 1.5-2.5 it is small when;Cool to room temperature;Filter
Recycle filtrate;
Muffin second extraction after step 2 filters, method is the same as step 1;
Muffin extracts three times after step 3 filters, and method is the same as step 1;
Step 4 merges filtrate three times;Stand overnight;
Step 5 filters after standing, and removes a small amount of solid impurity;60-65 DEG C of filtrate is concentrated under reduced pressure into solution muddiness, stops concentration,
Concentrate is obtained after filtering, to obtain the final product.
6. preparation method according to claim 1, it is characterised in that the preparation method, step are as follows:
Step 1, the Chinese Eaglewood Wood of 150-300 mesh:Water=1:10;Heating is until water slightly boiling;Be refluxed 1.5-2.5 it is small when;Drop
Temperature arrives room temperature;Filter recycling filtrate;
Step 2, muffin second extraction after suction filtration, method is the same as step 1;
Step 3, muffin carries out third time extraction using 95% ethanol for solvent after suction filtration, and method obtains ethanol and carry with step 1
Liquid is taken, recycling ethanol obtains alcohol extract;
Step 4, merge water twice and carry filtrate, it is closed to stand overnight;
Step 5, filtrate is filtered after standing, removes a small amount of impurity;Filtrate is concentrated under reduced pressure into solution muddiness at 60-65 DEG C, stops dense
Contracting, concentrate and the alcohol extract of step 3 is merged, the 23-25% propane diols of Chinese Eaglewood Wood weight, to obtain the final product.
7. preparation method according to claim 1, it is characterised in that the preparation method, step are as follows:
Step 1 Chinese Eaglewood Wood adds the mixed solvent of the ethanol of 10 times of amounts, propane diols and water, wherein 10 times of amounts are 1g agalloch eaglewood
The alcohol 95 parts by volume that the mixed solvent of powder addition 10ml solvents, the ethanol, propane diols and water is 95%, and 5 parts by volume
Propane diols mixture;Heating is until slightly boiling;Be refluxed 1.5-2.5 it is small when;Cool to room temperature;Filter recycling filtrate;
Muffin second extraction after step 2 filters, method is the same as step 1;
Muffin carries out third time extraction using 95% ethanol for solvent after step 3 filters, and method obtains ethanol and carry with step 1
Liquid is taken, recycling ethanol obtains alcohol extract;
Step 4 merge it is all above-mentioned carry filtrate, it is closed to stand overnight;
Filtrate is filtered after step 5 is stood, and filtrate is concentrated under reduced pressure into solution muddiness at 60-65 DEG C, stops concentration, to obtain the final product.
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CN109055010A (en) * | 2018-08-01 | 2018-12-21 | 太仓市高新区青沐文艺创作工作室 | A kind of extracting method of agilawood essential oil |
CN109504541A (en) * | 2018-12-28 | 2019-03-22 | 佛山科学技术学院 | A kind of agilawood essential oil extracting process |
CN112806605A (en) * | 2020-12-31 | 2021-05-18 | 海南贵本南药科技有限公司 | Kyara fragrance type cigar tobacco leaf and tobacco preparation method |
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CN115305206A (en) * | 2022-06-14 | 2022-11-08 | 杨敦阶 | Endophyte for rapidly producing incense from non-traumatic Michelia gigantea seedlings, preparation method and application thereof |
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