CN106433973A - Preparation method of perfume composition - Google Patents
Preparation method of perfume composition Download PDFInfo
- Publication number
- CN106433973A CN106433973A CN201610936273.6A CN201610936273A CN106433973A CN 106433973 A CN106433973 A CN 106433973A CN 201610936273 A CN201610936273 A CN 201610936273A CN 106433973 A CN106433973 A CN 106433973A
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- CN
- China
- Prior art keywords
- preparation
- flavor compositions
- valerolactone
- gamma
- reaction
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Classifications
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/12—Steaming, curing, or flavouring tobacco
-
- 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
-
- 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
-
- 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
- C11B9/0007—Aliphatic compounds
- C11B9/0015—Aliphatic compounds containing oxygen as the only heteroatom
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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
The invention discloses a preparation method of a perfume composition, which comprises the following steps: taking levulinate as a raw material and taking secondary alcohol as a hydrogen source and a solvent, performing reaction under a catalytic action of aluminium isopropoxide to prepare gamma-valerolactone, and uniformly mixing prepared gamma-valerolactone, dihydroactinidiolide, menthyl acetate, coumarin, a compound for enhancement and a carrier to prepare the perfume composition. The raw material adopted by the preparation method is cheap; the preparation cost of the perfume composition is effectively lowered; and a preparation technology is mild in condition and easy to operate.
Description
Technical field：
The present invention relates to field of perfumery, is specifically related to a kind of preparation method of flavor compositions.
Background technology：
Synthetic perfume as the important component part of fine organic chemical industry, food, cosmetics, weaving, medicine, rubber,
The aspects such as plastics, feedstuff, coating are widely used.The development approach of synthetic perfume has a lot, it is possible to use low price, be easy to get
Natural perfume material or petroleum and intermediate synthesis, natural perfume material of the reconstruction structure complicated difficult to synthesize, using new synthesis
Method, improves traditional handicraft etc..Synthetic perfume has reached kind more than 5000 in the world at present, and conventional product has kind more than 400.
In numerous spice, ester perfume is the very important spice product essence of a class, and ester perfume is that purposes is most wide, uses
The maximum class of amount.Gamma-valerolactone has fresh fruital, medicated incense, fragrant and sweet fragrance, and soft lasting, can be not only used for edible perfume
Essence and flavouring essence for tobacco, while also be used as solvent, organic synthesis intermediate, coating and cleaning agent etc..But which is individually used for volume
When in cigarette, the plumpness of obtained Medicated cigarette cigarette perfume, mellow and full sense, fluency are inadequate, on the other hand due to the synthesis side of gamma-valerolactone
Method condition is more harsh, relatively costly, limits its application.
Content of the invention：
In order to solve above-mentioned technical problem, the invention provides a kind of preparation method of flavor compositions, the preparation method
Raw material is cheap and easy to get, and preparation process condition is gentle, it is easy to operate, and obtained flavor compositions can effectively improve the clear of Medicated cigarette
Sweet rhythm sense, improves the quality of Medicated cigarette.
In order to preferably solve above-mentioned technical problem, the present invention is employed the following technical solutions：
A kind of preparation method of flavor compositions, comprises the following steps：
(1) with levulic acid esters as raw material, with secondary alcohol as hydrogen source and solvent, anti-under the catalytic action of aluminum isopropylate.
Gamma-valerolactone should be obtained；
(2) by gamma-valerolactone, dihydroactinidiolide, menthyl acetate, coumarin, enhancing obtained in step (1)
Compound, carrier mix homogeneously, prepared flavor compositions.
Used as the preferred of technique scheme, the process of step (1) reaction is specially：Add in microwave reactor
Levulic acid esters raw material, secondary alcohol and aluminum isopropylate.；Initial microwave power is set, reaction temperature and response time is set, instead
Lower the temperature through system air blast cooling after should terminating, reactant mixture is taken out, is isolated to gamma-valerolactone.
As the preferred of technique scheme, in step (1), the levulic acid esters are methyl ester levulinate, acetyl
One or more mixing in ethyl propionate, Butyl acetylpropanoate.
As the preferred of technique scheme, in step (1), the secondary alcohol is 2- butanol, the one kind in isopropanol.
As the preferred of technique scheme, in step (1), the secondary alcohol, the mass ratio of levulic acid esters raw material
For (8-25)：1.
Used as the preferred of technique scheme, the aluminum isopropylate. is 1 with the mass ratio of levulic acid esters raw material：(1-
8).
As the preferred of technique scheme, in step (2), the enhancing compound is diacetyl, n-butyric acie, 12
One or more mixing in acid, 4- methyl -5 (beta-hydroxyethyl) thiazole.
As the preferred of technique scheme, in step (2), the carrier is sodium glutamate, maltodextrin, distilled water
Mixture, three's mass ratio is 1：(2-3)：(5-10).
As the preferred of technique scheme, in step (2), in parts by weight, the gamma-valerolactone, dihydro-actinidia
Lactone, menthyl acetate, coumarin, enhancing compound, the consumption of carrier are specially：Gamma-valerolactone 1-2 part, dihydro macaque
Fructus Persicae lactone 0.5-1 part, menthyl acetate 0.5-0.8 part, coumarin 0.03-0.07 part, enhancing compound 0.005-0.015
Part, carrier 0.007-0.1 part.
Used as the preferred of technique scheme, the initial microwave power for setting as 300W, the temperature of the reaction is
130-170 DEG C, the time of the reaction is 10-60min.
Compared with prior art, the present invention has advantages below：
First the present invention with cheap levulic acid esters as raw material, secondary alcohol as hydrogen source and solvent, aluminum isopropylate.
Gamma-valerolactone being obtained for catalyst, high pressure hydrogen is not needed in course of reaction, effectively reduce preparation cost；And reaction condition
Gently, low for equipment requirements, process is simple, easy to operate；
The present invention rationally controls the consumption of each component in flavor compositions so that obtained flavor compositions have fruital,
Medicated incense, fragrant and sweet odor characteristic, can be effectively increased the plumpness of cigarette perfume, mellow and full sense, fluency, improve cigarette quality, and
Can project that sound tobacco Nicotiana tabacum L. sheet is sweet, lift the sweet rhythm of Medicated cigarette.
Specific embodiment：
In order to be better understood from the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solution
The present invention is released, any restriction will not be constituted to the present invention.
Embodiment 1
A kind of preparation method of flavor compositions, comprises the following steps：
(1) methyl ester levulinate, 2- butanol and aluminum isopropylate. are added in microwave reactor；Set initial microwave power as
300W, sets reaction temperature as 130 DEG C and response time 60min, and reaction is lowered the temperature through system air blast cooling after terminating, and takes out anti-
Mixture is answered, gamma-valerolactone is isolated to, wherein, 2- butanol, the mass ratio of methyl ester levulinate are 10：1, aluminum isopropylate.
Mass ratio with methyl ester levulinate is 1：2；
(2) in parts by weight, will be thin to 1 part of gamma-valerolactone, 0.5 part of dihydroactinidiolide, acetic acid obtained in step (1)
0.5 part of lotus ester, 0.03 part of coumarin, 0.005 part of diacetyl, 0.007 part of mix homogeneously of carrier, prepared flavor compositions；Wherein,
The carrier is sodium glutamate, maltodextrin, the mixture of distilled water, and three's mass ratio is 1：2：5.
Embodiment 2
A kind of preparation method of flavor compositions, comprises the following steps：
(1) Butyl acetylpropanoate, isopropanol and aluminum isopropylate. are added in microwave reactor；Set initial microwave power as
300W, sets reaction temperature as 170 DEG C and response time 10min, and reaction is lowered the temperature through system air blast cooling after terminating, and takes out anti-
Mixture is answered, gamma-valerolactone is isolated to, wherein, isopropanol, the mass ratio of Butyl acetylpropanoate are 8：1, aluminum isopropylate. with
The mass ratio of Butyl acetylpropanoate is 1：3；
(2) in parts by weight, by 2 parts of gamma-valerolactone, 1 part of dihydroactinidiolide, acetic acid Herba Menthae obtained in step (1)
0.8 part of ester, 0.07 part of coumarin, 0.015 part of 4- methyl -5 (beta-hydroxyethyl) thiazole, 0.1 part of mix homogeneously of carrier, prepared spice
Compositionss；Wherein, the carrier is sodium glutamate, maltodextrin, the mixture of distilled water, and three's mass ratio is 1：3：10.
Embodiment 3
A kind of preparation method of flavor compositions, comprises the following steps：
(1) ethyl levulinate, 2- butanol and aluminum isopropylate. are added in microwave reactor；Set initial microwave power as
300W, sets reaction temperature as 140 DEG C and response time 50min, and reaction is lowered the temperature through system air blast cooling after terminating, and takes out anti-
Mixture is answered, is isolated to gamma-valerolactone；2- butanol, the mass ratio of ethyl levulinate are 14：1, aluminum isopropylate. and acetyl
The mass ratio of ethyl propionate is 1：4；
(2) in parts by weight, by 1.2 parts of gamma-valerolactone, 0.6 part of dihydroactinidiolide, acetic acid obtained in step (1)
0.6 part of menthyl ester, 0.04 part of coumarin, 0.007 part of n-butyric acie, 0.009 part of mix homogeneously of carrier, prepared flavor compositions；Its
In, it is 1 that the carrier is sodium glutamate, maltodextrin, the mixture of distilled water, three's mass ratio：2：6.
Embodiment 4
A kind of preparation method of flavor compositions, comprises the following steps：
(1) methyl ester levulinate, isopropanol and aluminum isopropylate. are added in microwave reactor；Set initial microwave power as
300W, sets reaction temperature as 150 DEG C and response time 40min, and reaction is lowered the temperature through system air blast cooling after terminating, and takes out anti-
Mixture is answered, is isolated to gamma-valerolactone；2- butanol, the mass ratio of methyl ester levulinate are 18：1, aluminum isopropylate. and acetyl
The mass ratio of methyl propionate is 1：5；
(2) in parts by weight, by 1.4 parts of gamma-valerolactone, 0.7 part of dihydroactinidiolide, acetic acid obtained in step (1)
0.65 part of menthyl ester, 0.05 part of coumarin, 0.009 part of lauric acid/dodecanoic acid, 0.011 part of mix homogeneously of carrier, prepared flavor compositions；Its
In, it is 1 that the carrier is sodium glutamate, maltodextrin, the mixture of distilled water, three's mass ratio：2：7.
Embodiment 5
A kind of preparation method of flavor compositions, comprises the following steps：
(1) ethyl levulinate, 2- butanol and aluminum isopropylate. are added in microwave reactor；Set initial microwave power as
300W, sets reaction temperature as 160 DEG C and response time 30min, and reaction is lowered the temperature through system air blast cooling after terminating, and takes out anti-
Mixture is answered, is isolated to gamma-valerolactone；2- butanol, the mass ratio of ethyl levulinate are 20：1, aluminum isopropylate. and acetyl
The mass ratio of ethyl propionate is 1：6；
(2) in parts by weight, by 1.6 parts of gamma-valerolactone, 0.8 part of dihydroactinidiolide, acetic acid obtained in step (1)
0.7 part of menthyl ester, 0.05 part of coumarin, 0.011 part of 4- methyl -5 (beta-hydroxyethyl) thiazole, 0.013 part of mix homogeneously of carrier, system
Obtain flavor compositions；Wherein, the carrier is sodium glutamate, maltodextrin, the mixture of distilled water, and three's mass ratio is 1：3：
7.
Embodiment 6
A kind of preparation method of flavor compositions, comprises the following steps：
(1) Butyl acetylpropanoate, isopropanol and aluminum isopropylate. are added in microwave reactor；Set initial microwave power as
300W, sets reaction temperature as 160 DEG C and response time 20min, and reaction is lowered the temperature through system air blast cooling after terminating, and takes out anti-
Mixture is answered, is isolated to gamma-valerolactone；Isopropanol, the mass ratio of Butyl acetylpropanoate are 23：1, aluminum isopropylate. and acetyl
The mass ratio of butyl propionate is 1：7；
(2) in parts by weight, by 1.8 parts of gamma-valerolactone, 0.9 part of dihydroactinidiolide, acetic acid obtained in step (1)
0.75 part of menthyl ester, 0.06 part of coumarin, 0.013 part of 4- methyl -5 (beta-hydroxyethyl) thiazole, 0.016 part of mix homogeneously of carrier,
Prepared flavor compositions；Wherein, the carrier is sodium glutamate, maltodextrin, the mixture of distilled water, and three's mass ratio is 1：
3：8.
Claims (10)
1. a kind of preparation method of flavor compositions, it is characterised in that comprise the following steps：
(1) with levulic acid esters as raw material, with secondary alcohol as hydrogen source and solvent, reaction system under the catalytic action of aluminum isopropylate.
Obtain gamma-valerolactone；
(2) by gamma-valerolactone, dihydroactinidiolide, menthyl acetate, coumarin, enhancing chemical combination obtained in step (1)
Thing, carrier mix homogeneously, prepared flavor compositions.
2. a kind of preparation method of flavor compositions as claimed in claim 1, it is characterised in that step (1) reaction
Process is specially：Levulic acid esters raw material, secondary alcohol and aluminum isopropylate. is added in microwave reactor；Set initial microwave work(
Rate, sets reaction temperature and response time, and reaction is lowered the temperature through system air blast cooling after terminating, and takes out reactant mixture, warp point
From obtaining gamma-valerolactone.
3. a kind of preparation method of flavor compositions as claimed in claim 1, it is characterised in that：In step (1), the acetyl
Propionic acid ester is methyl ester levulinate, ethyl levulinate, one or more mixing in Butyl acetylpropanoate.
4. a kind of preparation method of flavor compositions as claimed in claim 1, it is characterised in that：In step (1), described two grades
Alcohol is 2- butanol, the one kind in isopropanol.
5. a kind of preparation method of flavor compositions as claimed in claim 1, it is characterised in that：In step (1), described two grades
Alcohol, the mass ratio of levulic acid esters raw material are (8-25)：1.
6. a kind of preparation method of flavor compositions as claimed in claim 1, it is characterised in that：The aluminum isopropylate. and acetyl
The mass ratio of propionic acid ester raw material is 1：(1-8).
7. a kind of preparation method of flavor compositions as claimed in claim 1, it is characterised in that：In step (2), the enhancing
With compound be diacetyl, one or more mixing in n-butyric acie, lauric acid/dodecanoic acid, 4- methyl -5 (beta-hydroxyethyl) thiazole.
8. a kind of preparation method of flavor compositions as claimed in claim 1, it is characterised in that：In step (2), the carrier
For sodium glutamate, maltodextrin, distilled water mixture, three's mass ratio be 1：(2-3)：(5-10).
9. a kind of preparation method of flavor compositions as claimed in claim 1, it is characterised in that：In step (2), with weight portion
Meter, the gamma-valerolactone, dihydroactinidiolide, menthyl acetate, coumarin, enhancing compound, carrier consumption concrete
For：Gamma-valerolactone 1-2 part, dihydroactinidiolide 0.5-1 part, menthyl acetate 0.5-0.8 part, coumarin 0.03-0.07
Part, enhancing is with compound 0.005-0.015 part, carrier 0.007-0.1 part.
10. a kind of preparation method of flavor compositions as claimed in claim 2, it is characterised in that：The setting initially micro-
Wave power is 300W, and the temperature of the reaction is 130-170 DEG C, and the time of the reaction is 10-60min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610936273.6A CN106433973A (en) | 2016-10-25 | 2016-10-25 | Preparation method of perfume composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610936273.6A CN106433973A (en) | 2016-10-25 | 2016-10-25 | Preparation method of perfume composition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106433973A true CN106433973A (en) | 2017-02-22 |
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ID=58178546
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610936273.6A Withdrawn CN106433973A (en) | 2016-10-25 | 2016-10-25 | Preparation method of perfume composition |
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| Country | Link |
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| CN (1) | CN106433973A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116138430A (en) * | 2023-03-02 | 2023-05-23 | 四川味欣食品科技有限公司 | Method for extracting ester spice from cheese by biological fermentation |
-
2016
- 2016-10-25 CN CN201610936273.6A patent/CN106433973A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116138430A (en) * | 2023-03-02 | 2023-05-23 | 四川味欣食品科技有限公司 | Method for extracting ester spice from cheese by biological fermentation |
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Application publication date: 20170222 |
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