CN108277088A - A kind of preparation method of fir essential oil and products thereof - Google Patents
A kind of preparation method of fir essential oil and products thereof Download PDFInfo
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- CN108277088A CN108277088A CN201810305964.5A CN201810305964A CN108277088A CN 108277088 A CN108277088 A CN 108277088A CN 201810305964 A CN201810305964 A CN 201810305964A CN 108277088 A CN108277088 A CN 108277088A
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- essential oil
- fir
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- fir essential
- surfactant
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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
-
- 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
- C11B9/0003—Compounds of unspecified constitution defined by the chemical reaction for their preparation
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Fats And Perfumes (AREA)
- Cosmetics (AREA)
Abstract
This hair discloses a kind of preparation method of fir essential oil, and this approach includes the following steps:(1) China fir raw material is worn into powder, surfactant is added, is put into destilling tower after stirring, vapor is then passed through into destilling tower carried out distillation and handle to obtain mixed vapour;(2) mixed vapour that step (1) obtains is sent into cooling tower and carries out the oil mixing with water liquid progress rectification process that cooling treatment obtains oil mixing with water liquid (3) by step (2), collect the fir essential oil after rectifying.On the other hand the present invention also provides a kind of fir essential oils prepared by the above method.The present invention is easy to operate, of low cost, and the oil yield of China fir raw material is high, is suitble to large-scale industrial production.
Description
Technical field
The invention belongs to the extractive technique fields of essential oil, and in particular to a kind of preparation method of fir essential oil and products thereof.
Background technology
China fir is the most important reproducting tree species of south China, and more than 9,110,000 hectares, accumulation is more than lanceolata forest area
3.43 hundred million m3.Contain a large amount of fir essential oil in China fir, main component is cedar wood alcohol, eneα-cedar, β-cedrene, Thujopsis dolabrata
Alkene, australene and alpha-terpineol etc., all very close cedar wood oil from the point of view of primary chemical composition and fragrance, so can use completely
To substitute Cypress ethereal oil for perfume industry.Cedar wood oil has strong woody-musky-ambergris fragrance, is mainly used for feeling well
The cosmetics class cosmetics such as body powder, muffin, kermes and soaps could be applicable in supplying illusion type essence.Cedar wood oil is the world ten
One of big essential oil, market is in great demand.Since the growth cycle of cypress is very long, can just become a useful person within about 60 years, so causing
Cypress scarcity of resources, to seriously affect the development of China's cedar wood oil industry.China fir has the characteristics that fast-growth, general 15
~20 years, some places can even become a useful person for 7~8 years, and a large amount of tree root resources left after trees felling can be used for fir essential oil
Production, and substitute cedar wood oil in perfume industry.
The extraction of san-mou oil at present mainly uses steam distillation, solvent extraction and cracking process.It is extracted using steam method
Fir essential oil aroma of pure, substantially conform to blending requirement, but yield is very low;The fir essential oil yield of extract by solvents is steamed compared with water
Gas is high, but needs a large amount of solvent, and subsequent processing is complicated, there are high energy consumption, the problem of dissolvent residual;Cracking process extracts yield
Height, can obtain the products such as wood vinegar, charcoal, wood tar and fuel gas simultaneously, but empyreumatic oil contain a large amount of tar, phenol,
The substances such as aldehyde and ketone, seriously affect the quality of san-mou oil, and thick empyreumatic oil has to pass through burnt deodorization processing of dispelling, can just substantially meet tune
Perfume requires.China fir raw material oil yield can either be made high so being badly in need of research and development one kind, solvent materials are at low cost, and can be environmentally friendly
Fir essential oil preparation method.
Invention content
The purpose of the invention is to overcome the technological deficiency present in the prior art, a kind of preparation of fir essential oil is provided
Method and products thereof.
To achieve the goals above, one aspect of the present invention provides a kind of preparation method of fir essential oil, and this method includes
Following steps:
(1) China fir raw material is worn into powder, surfactant is added, is put into destilling tower after stirring, then to distillation
It it is passed through vapor in tower carries out distillation and handle to obtain mixed vapour;
(2) mixed vapour that step (1) obtains is sent into progress cooling treatment in cooling tower and obtains oil mixing with water liquid;
(3) the oil mixing with water liquid of step (2) is subjected to rectification process, collects the fir essential oil after rectifying.
Preferably, the powder is the particle that granularity is 40-120 mesh, it is highly preferred that it is 60-80 that the powder, which is granularity,
Purpose particle.
Preferably, the weight ratio of both the powder and described surfactant is 1:(0.01-0.04).
Preferably, the surfactant is nonionic surfactant, it is highly preferred that the surfactant is epoxy
At least one of ethane, ethanol amine, butylphenol three, most preferably, the surfactant are ethylene oxide.
Preferably, the distillation, condition include:Vapo(u)rizing temperature is 160-200 DEG C, distillation time 6-8h.
The present invention also provides a kind of fir essential oils being made by the above method.
Through the above technical solutions, the preparation method of fir essential oil provided by the invention has the following advantages:
(1) present invention is easy to operate, of low cost, and the oil yield of China fir raw material is high, is suitble to large-scale industrial production;
(2) by the present invention in that China fir raw material wears into powder, surfactant is then used to destroy the cell of Chinese fir cell
Structure enables fir essential oil adequately to be distilled from China fir raw material.
(3) present invention is simple using raw material, and is all nontoxic environmentally protective raw material, reduces the row of harmful substance
It puts, protects ecological environment.
Specific implementation mode
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
The present invention provides a kind of preparation method of fir essential oil, and this approach includes the following steps:
(1) China fir raw material is worn into powder, surfactant is added, is put into destilling tower after stirring, then to distillation
It it is passed through vapor in tower carries out distillation and handle to obtain mixed vapour;
(2) mixed vapour that step (1) obtains is sent into progress cooling treatment in cooling tower and obtains oil mixing with water liquid;
(3) the oil mixing with water liquid of step (2) is subjected to rectification process, collects the fir essential oil after rectifying.
The present inventor has found in the course of the study, when surfactant solution reaches a certain concentration, in water
In tend to be formed micelle, outwardly, hydrophobic moiety aggregation is at center, when stirring China fir powder and surface-active for hydrophilic part
When agent solution, Chinese fir cell comes into full contact with surfactant, and the lipid on Chinese fir cell wall is wrapped surfactant molecule,
And in micelle, make clasmatosis, to increase the permeability of Chinese fir cell wall.Wherein, in order to preferably make China fir thin
Born of the same parents and surfactant come into full contact with, and need the powdered granule for China fir raw material first being worn into certain particle size, it is preferable that the powder
For the particle that granularity is 40-120 mesh;The more preferably described powder is the particle that granularity is 60-80 mesh.
Processing method according to the present invention, the surfactant are not particularly limited, and can be known in the art
It is various can be used for destroy cell wall surfactants, in order to keep China fir raw material preferably fuel-displaced, obtain it is higher fuel-displaced
Rate, it is preferable that the surfactant is nonionic surfactant, it is further preferred that the surfactant is epoxy
At least one of ethane, ethanol amine, butylphenol three;Most preferably, the surfactant is ethylene oxide.
In accordance with the present invention it is preferred that the weight ratio of both the powder and described surfactant is 1:(0.01-
0.04);It is highly preferred that the weight ratio of both the powder and described surfactant is 1:(0.02-0.03).
In order to preferably distill China fir powder, to reach better effect, in the present invention, and the distillation, condition packet
It includes:Vapo(u)rizing temperature is 160-200 DEG C, distillation time 6-8h.
The present invention also provides a kind of fir essential oils being made by the above method.
Invention is further explained by the following examples, but the present invention is not limited in following embodiments.
Embodiment 1
The present embodiment is used to illustrate the preparation method and products thereof of fir essential oil of the present invention.
The powder that 10kg China firs raw material is worn into 60 mesh with flour mill is added the ethamine alcohol of 200g, is put into after being sufficiently stirred
Into destilling tower, continues 6h into destilling tower and be passed through 160 DEG C of vapor and carry out distillation to handle to obtain mixed vapour, then will mix
It closes steam feeding cooling tower progress cooling treatment and obtains oil mixing with water liquid, oil mixing with water liquid is subjected to rectification process, is collected
Fir essential oil after rectifying.
Embodiment 2
The present embodiment is used to illustrate the preparation method and products thereof of fir essential oil of the present invention.
10kg China firs raw material is worn into purpose powder with flour mill, the ethamine alcohol of 300g is added, is put into after being sufficiently stirred
In destilling tower, continue 8h into destilling tower and be passed through 200 DEG C of vapor and carry out distillation to handle to obtain mixed vapour, it then will mixing
Steam is sent into cooling tower progress cooling treatment and obtains oil mixing with water liquid, and oil mixing with water liquid is carried out rectification process, collects essence
Fir essential oil after evaporating.
Embodiment 3
The present embodiment is used to illustrate the preparation method and products thereof of fir essential oil of the present invention.
The powder that 10kg China firs raw material is worn into 70 mesh with flour mill is added the ethamine alcohol of 300g, is put into after being sufficiently stirred
Into destilling tower, continues 7h into destilling tower and be passed through 180 DEG C of vapor and carry out distillation to handle to obtain mixed vapour, then will mix
It closes steam feeding cooling tower progress cooling treatment and obtains oil mixing with water liquid, oil mixing with water liquid is subjected to rectification process, is collected
Fir essential oil after rectifying.
Embodiment 4
The present embodiment is used to illustrate the preparation method and products thereof of fir essential oil of the present invention.
The powder that 10kg China firs raw material is worn into 40 mesh with flour mill is added the ethamine alcohol of 200g, is put into after being sufficiently stirred
Into destilling tower, continues 8h into destilling tower and be passed through 200 DEG C of vapor and carry out distillation to handle to obtain mixed vapour, then will mix
It closes steam feeding cooling tower progress cooling treatment and obtains oil mixing with water liquid, oil mixing with water liquid is subjected to rectification process, is collected
Fir essential oil after rectifying.
Embodiment 5
The present embodiment is used to illustrate the preparation method and products thereof of fir essential oil of the present invention.
The powder that 10kg China firs raw material is worn into 100 mesh with flour mill is added the ethamine alcohol of 400g, is put into after being sufficiently stirred
Into destilling tower, continues 7h into destilling tower and be passed through 190 DEG C of vapor and carry out distillation to handle to obtain mixed vapour, then will mix
It closes steam feeding cooling tower progress cooling treatment and obtains oil mixing with water liquid, oil mixing with water liquid is subjected to rectification process, is collected
Fir essential oil after rectifying.
Embodiment 6
The present embodiment is used to illustrate the preparation method and products thereof of fir essential oil of the present invention.
The powder that 10kg China firs raw material is worn into 120 mesh with flour mill is added the ethamine alcohol of 100g, is put into after being sufficiently stirred
Into destilling tower, continues 8h into destilling tower and be passed through 190 DEG C of vapor and carry out distillation to handle to obtain mixed vapour, then will mix
It closes steam feeding cooling tower progress cooling treatment and obtains oil mixing with water liquid, oil mixing with water liquid is subjected to rectification process, is collected
Fir essential oil after rectifying.
Comparative example 1
Fir essential oil is prepared according to the method for embodiment 1, the difference is that China fir raw material is prepared into bulk.
Comparative example 2
Fir essential oil is prepared according to the method for embodiment 1, the difference is that not adding surfactant.
Test case
Above example 1-6 and comparative example the 1-2 fir essential oil prepared are collected, while calculating fir essential oil
Oil yield, the results are shown in table below:
Table 1
As shown in Table 1, China fir raw material is first worn into powder by technical method using the present invention, is then lived by adding surface
It is higher than the oil yield of the fir essential oil of the prior art that property agent using distillation, condensation, rectifying obtains fir essential oil.
The preferred embodiment of the present invention has been described above in detail, and still, the present invention is not limited thereto.In the skill of the present invention
In art conception range, technical scheme of the present invention can be carried out a variety of simple variants, including each technical characteristic with it is any its
Its suitable method is combined, and it should also be regarded as the disclosure of the present invention for these simple variants and combination, belongs to
Protection scope of the present invention.
Claims (9)
1. a kind of preparation method of fir essential oil, which is characterized in that this approach includes the following steps:
(1) China fir raw material is worn into powder, surfactant is added, is put into destilling tower after stirring, then into destilling tower
It is passed through vapor and carries out distillation and handle to obtain mixed vapour;
(2) mixed vapour that step (1) obtains is sent into progress cooling treatment in cooling tower and obtains oil mixing with water liquid;
(3) the oil mixing with water liquid of step (2) is subjected to rectification process, collects the fir essential oil after rectifying.
2. the preparation method of fir essential oil according to claim 1, which is characterized in that the powder is that granularity is 40-120
Purpose particle.
3. the preparation method of fir essential oil according to claim 2, which is characterized in that the powder is that granularity is 60-80
Purpose particle.
4. the preparation method of fir essential oil according to claim 1, which is characterized in that the powder and the surface-active
The weight ratio of both agent is 1:(0.01-0.04).
5. the preparation method of fir essential oil according to claim 1, which is characterized in that the surfactant is nonionic
Surfactant.
6. the preparation method of fir essential oil according to claim 5, which is characterized in that the surfactant is epoxy second
At least one of alkane, ethanol amine, butylphenol three.
7. the preparation method of fir essential oil according to claim 6, which is characterized in that the surfactant is epoxy second
Alkane.
8. the preparation method of fir essential oil according to claim 1, which is characterized in that the distillation, condition include:It steams
It is 160-200 DEG C to evaporate temperature, distillation time 6-8h.
9. a kind of fir essential oil, which is characterized in that the fir essential oil is by any one of the claim 1-8 China fir essences
The preparation method of oil is made.
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Cited By (5)
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CN109321363A (en) * | 2018-09-30 | 2019-02-12 | 四川桧元素生物科技有限公司 | A kind of method that low-temperature negative-pressure extracts Chinese juniper another name for oil and polyphenol powde |
CN109943412A (en) * | 2019-04-10 | 2019-06-28 | 范加家 | A kind of borneol method of extraction of essential oil |
CN110776993A (en) * | 2019-10-31 | 2020-02-11 | 江城中澳农业科技发展有限公司 | Preparation method and application of macadamia nut oil |
CN112159726A (en) * | 2020-09-26 | 2021-01-01 | 江西天美生物科技有限公司 | Production method for preparing biological essential oil of Chinese fir by using Chinese fir sawdust |
CN113201405A (en) * | 2021-04-26 | 2021-08-03 | 常州工学院 | Extraction method of lavender essential oil |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109321363A (en) * | 2018-09-30 | 2019-02-12 | 四川桧元素生物科技有限公司 | A kind of method that low-temperature negative-pressure extracts Chinese juniper another name for oil and polyphenol powde |
CN109321363B (en) * | 2018-09-30 | 2022-02-08 | 四川桧元素生物科技有限公司 | Method for extracting juniper essential oil and phytoncide at low temperature under negative pressure |
CN109943412A (en) * | 2019-04-10 | 2019-06-28 | 范加家 | A kind of borneol method of extraction of essential oil |
CN110776993A (en) * | 2019-10-31 | 2020-02-11 | 江城中澳农业科技发展有限公司 | Preparation method and application of macadamia nut oil |
CN112159726A (en) * | 2020-09-26 | 2021-01-01 | 江西天美生物科技有限公司 | Production method for preparing biological essential oil of Chinese fir by using Chinese fir sawdust |
CN113201405A (en) * | 2021-04-26 | 2021-08-03 | 常州工学院 | Extraction method of lavender essential oil |
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Application publication date: 20180713 |