CN108690722A - A kind of synthetic perfume composition and preparation method with root of Aucklandia lappa Decne ambergris fragrance - Google Patents
A kind of synthetic perfume composition and preparation method with root of Aucklandia lappa Decne ambergris fragrance Download PDFInfo
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- CN108690722A CN108690722A CN201810639022.0A CN201810639022A CN108690722A CN 108690722 A CN108690722 A CN 108690722A CN 201810639022 A CN201810639022 A CN 201810639022A CN 108690722 A CN108690722 A CN 108690722A
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- fragrance
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- root
- aucklandia lappa
- lappa decne
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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
- C11B9/0003—Compounds of unspecified constitution defined by the chemical reaction for their preparation
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Cosmetics (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention discloses a kind of synthetic perfume composition and preparation method with root of Aucklandia lappa Decne ambergris fragrance, semisynthetic perfume the composition by weight percentage is made of component below:Ambrox 2%-10%, vertofix coeur, 15%-25%, ambrotone, 5% hereinafter, B position violet ketone, and 3% or less;Dihydromyrcenol, 20%-30%;Jujube extract, 1%-5%, berry extract, 1%-3%;Vanillic aldehyde, 1%-3%, Ethyl vanillin, 0.5%-2%, labdanum concrete, 5%-6%, beta oxidation carypohyllene, 2%-5%;Valerian oil, 0.5%-2%.The present invention is easy to operate, and reaction condition is mild, and yield is high, and fragrance remaining time is all very long, all coordinates very much with the fragrance of the various fragrance of a flower, fruity, root of Aucklandia lappa Decne, cream perfume (or spice) fragrance, and reaction temperature is low, the reaction time is short.Also have many advantages, such as that environmental pollution is small, product cost is low, post-processing is convenient, is more suitable for industrialized production.
Description
Technical field
It is specifically a kind of with root of Aucklandia lappa Decne ambergris fragrance the present invention relates to the synthesis technology field of synthetic perfume
Synthetic perfume composition and preparation method.
Background technology
Ambergris is one of high-grade fragrance of most worthy, the metabolite in sperm whale body.Natural imperial saliva
Perfume has been difficult to obtain, and is mostly substituted with sintetics.The Ambergris perfuming agent of synthesis is generally using forest resourceies as raw material, this kind of production
Product have both the fragrance of root of Aucklandia lappa Decne and ambergris, and lasting is lasting, can be used for preparing the productions such as daily chemical essence, articles for washing and fragrance for detergents
Product.
Chinese patent (CN1730636) discloses a kind of synthetic perfume composition and system with root of Aucklandia lappa Decne ambergris fragrance
Preparation Method, and specifically disclose following technical characteristic:A kind of synthetic perfume composition with root of Aucklandia lappa Decne ambergris fragrance, under
It states made of the raw material of weight proportion:Epoxy himachalane is 1 part, and acetyl cedrene is 1~80 part.Preparation method be with
San-mou oil is raw material, and cedrene is extracted after rectification under vacuum, by weight addition polyphosphoric acids and aceticanhydride, cedrene: polyphosphoric acids
: aceticanhydride 1: 0.15~0.35: 0.5~0.8 carries out acetylization reaction 7 hours at 100 DEG C, obtains acetyl cedrene,
Rectification under vacuum, then sodium carbonate peroxide, aceticanhydride and toluene, wherein acetyl cedrene: mistake is added in rectifying product by weight
Oxygen sodium carbonate: aceticanhydride: toluene 1: 0.10~0.20: 0.05~0.25: 0.2~0.6 carries out epoxidation reaction at 25 DEG C
12 hours, obtain product.It the advantage is that:It prepares while having using san-mou oil resource that is cheap, can largely supplying
The synthetic perfume product of root of Aucklandia lappa Decne, ambergris fragrance can be widely used in the applicable composition of vertofix coeur.
But in fact due to long-term large-scale utilization, the resource of cedar wood oil is fairly limited, and cypress regeneration is also very slow
Slowly;And content of the cedrol in cedar wood oil is very low, and only 3%~14%, refine extraction more difficulty, therefore cedrol
Long run supply is insufficient, and price rising all the way causes the production cost of cedrol methyl ether higher.
Invention content
The purpose of the present invention is to provide a kind of synthetic perfume composition with root of Aucklandia lappa Decne ambergris fragrance and preparation sides
Method, to solve the problems, such as to propose in background technology.
To achieve the above object, the present invention provides the following technical solutions;
A kind of synthetic perfume composition and preparation method with root of Aucklandia lappa Decne ambergris fragrance, the semisynthetic perfume is by weight
Amount percentages the composition is made of component below:
Ambrox 2%-10%, vertofix coeur, 15%-25%, ambrotone, 5% hereinafter, B position violet ketone,
3% or less;Dihydromyrcenol, 20%-30%;Jujube extract, 1%-5%, berry extract, 1%-3%;Vanillic aldehyde, 1%-
3%, Ethyl vanillin, 0.5%-2%, labdanum concrete, 5%-6%, beta oxidation carypohyllene, 2%-5%;Valerian oil,
0.5%-2%.
Preferably, the berry extract is that Fructus Fici extract, Noni extract, black meal berry extract, fruit carry
Take one kind in object, Fructus Monordicae extract, goat milk berry extract.
Preferably, semisynthetic perfume the composition by weight percentage is made of component below:Ambergris drops
Ether 5%, vertofix coeur, 15%, ambrotone, 5%, B position violet ketone, 2%;Dihydromyrcenol, 25%;Jujube extracts
Object, 3%, berry extract, 2%;Vanillic aldehyde, 2%, Ethyl vanillin, 1%, labdanum concrete, 6%, beta oxidation carypohyllene,
3%;Valerian oil, 1%.
It is described the present invention also provides a kind of preparation method of the synthetic perfume composition with root of Aucklandia lappa Decne ambergris fragrance
The preparation method of synthetic perfume composition with root of Aucklandia lappa Decne ambergris fragrance includes:
Sclareol is extracted in plant, using the sclareol as raw material, is made the oxidation scission of its side chain and then is gone back
It obtains dropping imperial saliva glycol after original;
The CBV320 zeolites of NaY types are immersed in 10% ammonium nitrate solution, the temperature of immersion is at 90 DEG C or more, reaction
Time be more than 24 hours, to carry out ion exchange;
Drying is filtered to CBV320 zeolites, drying time be more than it is 12 hours dry, dry temperature 105 DEG C-
Between 120 DEG C;
CBV320 zeolites after filtration drying carry out ion exchange with 10% calcium nitrate and filter;
The CBV320 zeolites handle to obtain the CBV320 zeolites of CaY types by 500 DEG C of vacuum activatings;
The CBV320 zeolites of the CaY types are dehydrated at 110 DEG C to obtain ambrox, dehydration when to be more than 24 small
When;
The ambrox and vertofix coeur, ambrotone, B position violet ketone, dihydromyrcenol, jujube are extracted
Object, berry extract, vanillic aldehyde, Ethyl vanillin, labdanum concrete, beta oxidation carypohyllene, valerian oil are put into organic solvent simultaneously
It is stirred, the reactant after reaction is filtered;
Filtrate is subjected to distillation processing, to be distilled finish obtains crude product fragrance;
The crude product fragrance carries out recrystallization and handles to obtain the fragrance of high-quality.
Preferably, the organic solvent is benzene, acetone, dichloromethane, chloroform, toluene, ethylbenzene, chlorobenzene, diformazan
Benzene, acetonitrile, tetrahydrofuran, dioxane, diglycol, poly- diethylene glycol dimethyl ether, poly- diethylene glycol diethyl ether or N
Or one kind of dinethylformamide.
Preferably, the crude product fragrance is completely dissolved in solvent, then carries out recrystallization again and handles to obtain high-quality
Fragrance, solvent is by n-hexane, petroleum ether, ether, dichloromethane, methyl tertiary butyl ether(MTBE), ethyl acetate, ethyl alcohol or methanol
One or more of constitute.
The beneficial effects of the invention are as follows:The present invention is easy to operate, and reaction condition is mild, and yield is high, and fragrance remaining time is all very
It is long, all coordinate very much with the fragrance of the various fragrance of a flower, fruity, root of Aucklandia lappa Decne, cream perfume (or spice) fragrance, and reaction temperature is low, the reaction time is short.
Also have many advantages, such as that environmental pollution is small, product cost is low, post-processing is convenient, is more suitable for industrialized production.
Compared with prior art, the creativeness in the technology of the present invention is embodied in:1, it is carried out by raw material of the sclareol
The mode of ion exchange prepares the synthetic perfume with root of Aucklandia lappa Decne ambergris fragrance, and the condition and equipment requirement of preparation are relatively low, reaction
Mildly, cost is relatively low;2, so that synthetic perfume is had a variety of smells by adding the materials such as all kinds of extracts, essence, lasting when
Between it is longer.
Specific implementation mode
Below in conjunction in the embodiment of the present invention, the technical aspect in the embodiment of the present invention is clearly and completely retouched
It states, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the present invention
In embodiment, every other implementation obtained by those of ordinary skill in the art without making creative efforts
Example, shall fall within the protection scope of the present invention.
A kind of embodiment provided by the invention:
A kind of synthetic perfume composition and preparation method with root of Aucklandia lappa Decne ambergris fragrance, the semisynthetic perfume is by weight
Amount percentages the composition is made of component below:
Ambrox 2%-10%, vertofix coeur, 15%-25%, ambrotone, 5% hereinafter, B position violet ketone,
3% or less;Dihydromyrcenol, 20%-30%;Jujube extract, 1%-5%, berry extract, 1%-3%;Vanillic aldehyde, 1%-
3%, Ethyl vanillin, 0.5%-2%, labdanum concrete, 5%-6%, beta oxidation carypohyllene, 2%-5%;Valerian oil,
0.5%-2%.Vanillic aldehyde also known as vanillic aldehyde, chemical name are Vanillin.Ethyl vanillin, also known as
Ethyl vanillin, chemical name are vanirom.Labdanum concrete, also known as uncle is relied to work as medicinal extract or cistus creticus
Medicinal extract;The preparation of labdanum concrete:After dry ladanum leaf, branch chopping, labdanum concrete is produced with petroleum ether extraction.β-
Caryophyllene oxide also known as beta epoxide carypohyllene;Valerian oil is life of the selected Guizhou higher than the Valeriana Fauriei Briq of 1000 meters of height above sea level
Root, volatile plant essence oil obtained by being processed by water distillation apparatus.B position violet ketone also known as sweet violet ketone, β-ionone,
β-ring citrylidene acetone;Chemical name is 4- (2,6,6- trimethyl-1- cyclohexenyl groups)-3- butene-2 -one.
In the present embodiment, the berry extract is Fructus Fici extract, Noni extract, black meal berry extract, water
One kind in berry extract, Fructus Monordicae extract, goat milk berry extract.Above-mentioned berry extract may be used commercially available.Root
According to the embodiment of the present invention, the Fructus Monordicae extract is using obtained by following step extraction:Siraitia grosvenorii is taken, is added 5
Extracting solution is stood cooled and filtered by the water of~8 times of weight, 1~3h of refluxing extraction, and it is Fructus Monordicae extract to collect filtrate.
The extract from fruit is extracted using the following method and is obtained:It after fruit smashing, is placed in edible alcoholic solution, returns
Extracting solution is stood cooled and filtered by stream, and it is extract from fruit to collect filtrate.The fruit extract can be single
The extract that fruit or various fruits extract.Above-mentioned Fructus Fici extract, Noni extract, black meal fruit carry
The extracting method that fruit extract may be used in object, goat milk berry extract is taken to extract.
Jujube extract can be used extracting method below and extract:There are the core jujube dry fruit, moisture to be by commercially available
20% ± 2%, mouldy, rotten jujube is rejected, then cleans, drain;Jujube is flattened, it is broken after be put into reaction kettle, press
According to jujube:75% edible alcohol=1:4 ratio mixing, agitating and heating reflux extraction 6 hours at a temperature of 90 ± 5 DEG C, cooling
To room temperature;By the solution left standstill 5h clarifications after cooling, supernatant is extracted;After lower layer's slurry centrifugation, reject dregs merge clear
Liquid;Clear liquid is poured into concentration kettle and is concentrated, is concentrated back under conditions of 80 ± 2 DEG C of temperature, vacuum degree are more than 0.95MPa
Alcohol is received, stops concentration when concentrate Baume degrees is 25 °, gained dark-brown thick liquid is red date extract.According to this
Another embodiment of invention, jujube extract may be commercially available.
In the present embodiment, semisynthetic perfume the composition by weight percentage is made of component below:Drop dragon
Saliva perfume (or spice) ether 5%, vertofix coeur, 15%, ambrotone, 5%, B position violet ketone, 2%;Dihydromyrcenol, 25%;Jujube carries
Take object, 3%, berry extract, 2%;Vanillic aldehyde, 2%, Ethyl vanillin, 1%, labdanum concrete, 6%, beta oxidation carypohyllene,
3%;Valerian oil, 1%.
The present embodiment additionally provides a kind of preparation method of the synthetic perfume composition with root of Aucklandia lappa Decne ambergris fragrance, institute
The preparation method for stating the synthetic perfume composition with root of Aucklandia lappa Decne ambergris fragrance includes:
Sclareol is extracted in plant, using the sclareol as raw material, is made the oxidation scission of its side chain and then is gone back
It obtains dropping imperial saliva glycol after original;
The CBV320 zeolites of NaY types are immersed in 10% ammonium nitrate solution, the temperature of immersion is at 90 DEG C or more, reaction
Time be more than 24 hours, to carry out ion exchange;
Drying is filtered to CBV320 zeolites, drying time be more than it is 12 hours dry, dry temperature 105 DEG C-
Between 120 DEG C;
CBV320 zeolites after filtration drying carry out ion exchange with 10% calcium nitrate and filter;
The CBV320 zeolites handle to obtain the CBV320 zeolites of CaY types by 500 DEG C of vacuum activatings;
The CBV320 zeolites of the CaY types are dehydrated at 110 DEG C to obtain ambrox, dehydration when to be more than 24 small
When;
By the ambrox and vertofix coeur, ambrotone, B position violet ketone, dihydromyrcenol, jujube extraction
Object, berry extract, vanillic aldehyde, Ethyl vanillin, labdanum concrete, beta oxidation carypohyllene, valerian oil are put into organic solvent simultaneously
It is stirred, the reactant after reaction is filtered;
Filtrate is subjected to distillation processing, to be distilled finish obtains crude product fragrance;
The crude product fragrance carries out recrystallization and handles to obtain the fragrance of high-quality.
In the present embodiment, the organic solvent is benzene, acetone, dichloromethane, chloroform, toluene, ethylbenzene, chlorobenzene, two
Toluene, acetonitrile, tetrahydrofuran, dioxane, diglycol, poly- diethylene glycol dimethyl ether, poly- diethylene glycol diethyl ether or
One kind of n,N-Dimethylformamide.
In the present embodiment, the crude product fragrance is completely dissolved in solvent, recrystallization is then carried out again and handles to obtain height
The fragrance of quality, solvent by n-hexane, petroleum ether, ether, dichloromethane, methyl tertiary butyl ether(MTBE), ethyl acetate, ethyl alcohol or
One or more of methanol is constituted.
In order to determine the synthetic perfume in the application lasting time and existing fragrance fragrance remaining time, inventor
By test of many times, result as shown in the table is obtained:
Can be seen that from upper table, the synthetic perfume composition lasting with root of Aucklandia lappa Decne ambergris fragrance in the application when
Between longest.
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art,
It still can be with technical scheme described in the above embodiments is modified, or is carried out to which part technical characteristic
Equivalent replacement, all within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should all include
Within protection scope of the present invention.
Claims (6)
1. a kind of synthetic perfume composition with root of Aucklandia lappa Decne ambergris fragrance, it is characterised in that:The semisynthetic perfume is by weight
Percentages the composition is made of component below:
Ambrox 2%-10%, vertofix coeur, 15%-25%, ambrotone, 5% hereinafter, B position violet ketone, and 3% or less;Two
Hydrogen myrcenol, 20%-30%;Jujube extract, 1%-5%, berry extract, 1%-3%;Vanillic aldehyde, 1%-3%, Ethyl vanillin,
0.5%-2%, labdanum concrete, 5%-6%, beta oxidation carypohyllene, 2%-5%;Valerian oil, 0.5%-2%.
2. a kind of synthetic perfume composition with root of Aucklandia lappa Decne ambergris fragrance according to claim 1, it is characterised in that:Institute
The berry extract stated be Fructus Fici extract, Noni extract, black meal berry extract, fruit extract, Fructus Monordicae extract,
One kind in goat milk berry extract.
3. a kind of synthetic perfume composition with root of Aucklandia lappa Decne ambergris fragrance according to claim 1, it is characterised in that:Institute
Semisynthetic perfume the composition by weight percentage is stated to be made of component below:Ambrox 5%, vertofix coeur,
15%, ambrotone, 5%, B position violet ketone, 2%;Dihydromyrcenol, 25%;Jujube extract, 3%, berry extract, 2%;Chinese cymbidium
Element, 2%, Ethyl vanillin, 1%, labdanum concrete, 6%, beta oxidation carypohyllene, 3%;Valerian oil, 1%.
4. a kind of preparation method of the synthetic perfume composition with root of Aucklandia lappa Decne ambergris fragrance, which is characterized in that described that there is wood
The preparation method of the synthetic perfume composition of fragrant ambergris fragrance includes:
Sclareol is extracted in plant, using the sclareol as raw material, after making the oxidation scission of its side chain and then restoring
To the imperial saliva glycol of drop;
The CBV320 zeolites of NaY types are immersed in 10% ammonium nitrate solution, the temperature of immersion is at 90 DEG C or more, the time of reaction
More than 24 hours, to carry out ion exchange;
Drying is filtered to CBV320 zeolites, drying time be more than it is 12 hours dry, dry temperature 105 DEG C -120 DEG C it
Between;
CBV320 zeolites after filtration drying carry out ion exchange with 10% calcium nitrate and filter;
The CBV320 zeolites handle to obtain the CBV320 zeolites of CaY types by 500 DEG C of vacuum activatings;
The CBV320 zeolites of the CaY types are dehydrated at 110 DEG C to obtain ambrox, dehydration when be more than 24 hours;
The ambrox and vertofix coeur, ambrotone, B position violet ketone, dihydromyrcenol, jujube extract, fruit are carried
Take object, vanillic aldehyde, Ethyl vanillin, labdanum concrete, beta oxidation carypohyllene, valerian oil are put into organic solvent and are stirred
It mixes, the reactant after reaction is filtered;
Filtrate is subjected to distillation processing, to be distilled finish obtains crude product fragrance;
The crude product fragrance carries out recrystallization and handles to obtain the fragrance of high-quality.
5. a kind of preparation method of synthetic perfume composition with root of Aucklandia lappa Decne ambergris fragrance according to claim 4, special
Sign is that the organic solvent is benzene, acetone, dichloromethane, chloroform, toluene, ethylbenzene, chlorobenzene, dimethylbenzene, acetonitrile, four
Hydrogen furans, dioxane, diglycol, poly- diethylene glycol dimethyl ether, poly- diethylene glycol diethyl ether or N or N- dimethyl methyls
Amide it is one or more.
6. a kind of preparation method of synthetic perfume composition with root of Aucklandia lappa Decne ambergris fragrance according to claim 5,
It is characterized in that, the crude product fragrance is completely dissolved in solvent, then carry out recrystallization again and handle to obtain the fragrance of high-quality,
Its solvent is by one kind in n-hexane, petroleum ether, ether, dichloromethane, methyl tertiary butyl ether(MTBE), ethyl acetate, ethyl alcohol or methanol
Or several compositions.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810639022.0A CN108690722A (en) | 2018-06-20 | 2018-06-20 | A kind of synthetic perfume composition and preparation method with root of Aucklandia lappa Decne ambergris fragrance |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810639022.0A CN108690722A (en) | 2018-06-20 | 2018-06-20 | A kind of synthetic perfume composition and preparation method with root of Aucklandia lappa Decne ambergris fragrance |
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| CN108690722A true CN108690722A (en) | 2018-10-23 |
Family
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810639022.0A Pending CN108690722A (en) | 2018-06-20 | 2018-06-20 | A kind of synthetic perfume composition and preparation method with root of Aucklandia lappa Decne ambergris fragrance |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100248316A1 (en) * | 2009-03-25 | 2010-09-30 | Csir | Process for the Production of Ambrafuran |
| CN103584276A (en) * | 2013-11-13 | 2014-02-19 | 川渝中烟工业有限责任公司 | Ambergris cigarette and ambergris spices |
| CN105037308A (en) * | 2015-07-06 | 2015-11-11 | 川渝中烟工业有限责任公司 | Preparation method for ambrox |
-
2018
- 2018-06-20 CN CN201810639022.0A patent/CN108690722A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100248316A1 (en) * | 2009-03-25 | 2010-09-30 | Csir | Process for the Production of Ambrafuran |
| CN103584276A (en) * | 2013-11-13 | 2014-02-19 | 川渝中烟工业有限责任公司 | Ambergris cigarette and ambergris spices |
| CN105037308A (en) * | 2015-07-06 | 2015-11-11 | 川渝中烟工业有限责任公司 | Preparation method for ambrox |
Non-Patent Citations (1)
| Title |
|---|
| 俞根发等: "《日用香精调配技术》", 30 September 2007, 中国轻工业出版社 * |
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