CN85106638A - The extracting method of China oak moss - Google Patents
The extracting method of China oak moss Download PDFInfo
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- CN85106638A CN85106638A CN198585106638A CN85106638A CN85106638A CN 85106638 A CN85106638 A CN 85106638A CN 198585106638 A CN198585106638 A CN 198585106638A CN 85106638 A CN85106638 A CN 85106638A CN 85106638 A CN85106638 A CN 85106638A
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Abstract
The extracting method of China oak moss.The present invention is a kind of extracting method of natural perfume material, and it is that lichen Evernia with Chinese NW YUNNAN is a raw material, with extracting with benzinum after ethanol or the benzene extracted many times again.Mellow and full with the clear taste of Chinese oak moss product that this method extracts, tongue delicate fragrance is stronger, and lighter color, solubility can be used for spices and essence industry well.
Description
The present invention is a kind of extracting method of natural perfume material, more particularly is the method for extracting Chinese oak moss with the lichen Evernia of Chinese NW YUNNAN.
Oak moss is a kind of famous natural perfume material.Oak moss since the fragrance of its uniqueness and it in adding incense products, can give prominence to delicate fragrance and have a good fixation effect, can constitute odor type after the blending with special style, oak moss has become in the spices and essence industry indispensable, is at present a kind of the situation of selling well and high-grade lichens perfume material in the international market.External oak moss product mainly is to be that raw material is obtained through refining and formed by the flat clothes of Usneaceae Evernia oak.On the trunk and branch of this plant because of the sub-Oak Tree that often grows nonparasitically upon another plant (being robur), be celadon, so be commonly referred to oak moss.Oakmoss originates in central Europe and south, wherein especially with the oak moss product fine of states such as France of Mediterranean bank, Italy, Yugoslavia.China does not have the resource of oakmoss, and the past is not produced the oak moss product.
The extracting method that the purpose of this invention is to provide a kind of Chinese oak moss, this method can be that raw material extracts Chinese oak moss with the lichen Evernia of Chinese NW YUNNAN.
This extracting method is a raw material with the lichen Evernia of Chinese NW YUNNAN, the main note composition of products obtained therefrom is the divaricatic acid ethyl ester, this is from the isolated first compound with tongue delicate fragrance and fixation effect of occurring in nature, and its molecular structure is measured to obtain proving conclusively through every spectroscopic data and is:
The crystallization of colourless minute hand shape, fusing point are 42～43 ℃.
The technical process that this method is concrete is that the Evernia raw material is put into the lixiviate jar, add etoh solvent or benzene, the weight ratio of solvent and raw material is 11～12.5: 1, boiling reflux, lixiviate is three times altogether, the time of each lixiviate is respectively: 4～5 hours for the first time, and 1～2 hour for the second time, 1～2 hour for the third time.At normal temperatures with preceding twice leaching liquor heating recovery solvent to pasty state, make solvent with benzinum, extract four times, the each stirring 20～40 minutes, left standstill 20～40 minutes, the each consumption of solvent is respectively: 60～80 kilograms for the first time, and 50～60 kilograms for the second time, 30～45 kilograms for the third time, the 4th time 30～45 kilograms.Merge four times extract, leave standstill 11～14 hours after, reclaim benzinum after filtration to pasty state.With the high purity ethanol heating for dissolving of pastel with free from extraneous odour, up to both miscible (weight ratio of ethanol and pastel is 6: 1), leave standstill and filtered in 11～14 hours again, the heating filtrate recycling ethanol flows out the absolute oil product that obtains until no ethanol and is Chinese oak moss No. 1.Under-5 ℃～0 ℃ condition, make the absolute oil freezing and crystallizing, and with being recrystallized behind the ethanol washing crystal, the divaricatic acid ethyl ester crystallization that makes is Chinese oak moss No. 2.
Chinese oak moss extracting method provided by the invention is that raw material has been produced new lichens spices with the Evernia.The characteristic perfume of China oak moss existing oak moss has own characteristic again, and the blue or green perfume (or spice) of tongue is stronger, and moisten in the taste garden clearly, lighter color, and solubility is good, for Chinese fragrance product has been filled up blank.Production technology that this law provides and product specification are feasible through facts have proved.
Accompanying drawing is the process diagram of Chinese oak moss extracting method.Sketch has illustrated overall process of the Chinese oak moss of extraction from Evernia and the correlation between each procedure.
Working of an invention:
Embodiment 1.
Evernia is dropped into 3 cubic metres of fixing vertical digesters for 150 kilograms, and adding the ethanol raw material Evernia is 1 with the consumption of ethanol ratio: the 12(weight ratio), boiling reflux, lixiviate is three times altogether, and the time of each lixiviate is respectively: 5 hours for the first time; 1 hour for the second time; 1 hour for the third time.
At normal temperatures with preceding twice leaching liquor heating recovery solvent to pasty state, extract again, do the solvent coextraction four times with benzinum, the each consumption of solvent is respectively: 70 kilograms for the first time, 50 kilograms for the second time, 30 kilograms for the third time, the 4th time 30 kilograms.The each stirring half an hour left standstill half an hour.Merge four times extract, left standstill 12 hours after the filtered and recycled benzinum to pasty state.
With pastel with the high purity ethanol heating for dissolving of free from extraneous odour up to both miscible (ratio of ethanol and pastel 6: 1), leave standstill filtration in 12 hours, heat filtrate recycling ethanol and flow out up to no ethanol, the absolute oil product that obtains is Chinese oak moss No. 1.Under-2 ℃ condition, make the absolute oil freezing and crystallizing, and with being recrystallized behind the ethanol washing crystal, the divaricatic acid ethyl ester crystallization that makes is Chinese oak moss No. 2.
Embodiment 2.
Evernia is put into the lixiviate jar for 150 kilograms, add solvent benzol, the weight ratio of solvent and raw material is 1: 11, and lixiviate is three times altogether, and the time of each lixiviate is respectively: 4 hours for the first time, and 1.5 hours for the second time, 1 hour for the third time.At normal temperatures with preceding twice leaching liquor heating recovery benzene to pasty state, make solvent with benzinum, extract four times, the each consumption of solvent is respectively: 60 kilograms for the first time, 55 kilograms for the second time, 35 kilograms for the third time, the 4th time 35 kilograms.The each stirring 35 minutes left standstill 35 minutes.Merge four times extract, leave standstill 13 hours after, reclaim benzinum after filtration to pasty state.With the high purity ethanol heating for dissolving of pastel with free from extraneous odour, up to both miscible (weight ratio of ethanol and pastel is 6: 1), leave standstill and filtered in 11 hours again, the heating filtrate recycling ethanol flows out the absolute oil product that obtains until no ethanol and is Chinese oak moss No. 1.Under-1 ℃ condition, make the absolute oil freezing and crystallizing, and with being recrystallized behind the ethanol washing crystal, the divaricatic acid ethyl ester crystallization that makes is Chinese oak moss No. 2.
Claims (8)
1, the extracting method of Chinese oak moss is characterized in that the raw material that is adopted is the lichen Evernia of Chinese NW YUNNAN, and the main note composition of product is the divaricatic acid ethyl ester, and molecular structure is
2, a kind of extracting method as claimed in claim 1, it is characterized in that the concrete technical process of this method is that the Evernia raw material is put into the lixiviate jar, add etoh solvent or benzene, the weight ratio of solvent and raw material is 11～12.5: 1, boiling reflux, lixiviate is three times altogether, and the time of each lixiviate is respectively: 4～5 hours for the first time, 1～2 hour for the second time, 1～2 hour for the third time.
3, a kind of extracting method as claimed in claim 2 is characterized in that at normal temperatures preceding twice leaching liquor being heated, and reclaims solvent and extracts to pasty state again.
4, a kind of extracting method as claimed in claim 3, it is characterized in that pastel petroleum ether extraction four times, the each consumption of benzinum is respectively: 60～80 kilograms for the first time, 50～60 kilograms for the second time, 30～45 kilograms for the third time, the 4th time 30～45 kilograms, stirred 20～40 minutes at every turn, left standstill 20～40 minutes.
5, a kind of extracting method as claimed in claim 4 is characterized in that merging extract four times, left standstill 11～14 hours after the filtered and recycled benzinum to pasty state.
6, a kind of extracting method as claimed in claim 5 is characterized in that with pastel with the high purity ethanol heating for dissolving of free from extraneous odour, the weight ratio of ethanol and pastel is 6: 1, leaves standstill after pastel and ethanol are miscible and filters in 11～14 hours again.
7, a kind of extracting method as claimed in claim 6 is characterized in that heating filtrate recycling ethanol and flows out until no ethanol and obtain the absolute oil product and be Chinese oak moss No. 1.
8, a kind of extracting method as claimed in claim 7 is characterized in that making absolute oil product freezing and crystallizing under-5 ℃～0 ℃ condition, and with being recrystallized behind the ethanol washing crystal, the divaricatic acid ethyl ester crystallization that makes is Chinese oak moss No. 2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN198585106638A CN85106638A (en) | 1985-08-30 | 1985-08-30 | The extracting method of China oak moss |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN198585106638A CN85106638A (en) | 1985-08-30 | 1985-08-30 | The extracting method of China oak moss |
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| Publication Number | Publication Date |
|---|---|
| CN85106638A true CN85106638A (en) | 1987-04-15 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN198585106638A Pending CN85106638A (en) | 1985-08-30 | 1985-08-30 | The extracting method of China oak moss |
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| CN (1) | CN85106638A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351706A (en) * | 2011-08-04 | 2012-02-15 | 江苏中烟工业有限责任公司 | Method for synthesizing ethyldivaricatinate and application of ethyldivaricatinate |
| CN105765045A (en) * | 2013-11-29 | 2016-07-13 | 花王株式会社 | Perfume composition |
-
1985
- 1985-08-30 CN CN198585106638A patent/CN85106638A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351706A (en) * | 2011-08-04 | 2012-02-15 | 江苏中烟工业有限责任公司 | Method for synthesizing ethyldivaricatinate and application of ethyldivaricatinate |
| CN102351706B (en) * | 2011-08-04 | 2013-08-07 | 江苏中烟工业有限责任公司 | Method for synthesizing ethyldivaricatinate and application of ethyldivaricatinate |
| CN105765045A (en) * | 2013-11-29 | 2016-07-13 | 花王株式会社 | Perfume composition |
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