CN1077217A - The method of purification of trans-anethole - Google Patents
The method of purification of trans-anethole Download PDFInfo
- Publication number
- CN1077217A CN1077217A CN 92110181 CN92110181A CN1077217A CN 1077217 A CN1077217 A CN 1077217A CN 92110181 CN92110181 CN 92110181 CN 92110181 A CN92110181 A CN 92110181A CN 1077217 A CN1077217 A CN 1077217A
- Authority
- CN
- China
- Prior art keywords
- anethole
- trans
- purification
- degree
- oil
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Fats And Perfumes (AREA)
Abstract
The method of purification of trans-anethole, the composition of star aniseed oil mainly contains six kinds, utilizes the difference of their zero pour, with the physical means trans-anethole of purifying.With illicium verum oil under the low temperature of negative 30 degree Celsius～negative 10 degree freezing 16 hours, then Frozen Body is crushed to 20 mesh sieve hole sizes, put into the whizzer separation that per minute 1450 changes again.Respectively Frozen Body and impurity liquid are collected respectively, through repeated multiple times freezing-pulverizing-separation, rectifying in material 1Cr18Ni9Ti distillation tower then, oil bath is heated, oil temperature is at 130～170 degree Celsius.Cost of the present invention is low, and power consumption is few, the purification degree height, and impurity is few, and technology is simple.
Description
The present invention relates to a kind of method of purification of trans-anethole.
Star anise (Illicium Verum Hook.f.) chain timbers the orchid family.Aiphyllium is China's south subtropics special product.From the volatility olium anisi of anistree branches and leaves and fruit distillation extraction, be the monomer perfume that is widely used in daily cosmetics and candy, drinks.700 tons of olium anisis are produced in Guangxi per year.Trans-anethole is the fennel main body of oil.The world market is to the rush of demand of trans-anethole, and the purity that requires trans-anethole is more than 99%.According to Yulin City of Guangxi Zhuang Autonomous perfume oil factory, number of patent application: 90109608.3, be entitled as " processing of anise camphor with high freezing point " disclosed technology, solubilizing agent alcohol or acetone are removed the terpenes mixture in the star aniseed oil during production, and then solubilizing agent carries out recrystallization again, the isoesdragol crystal that still obtains with the solvent wash recrystallization is rectified purified at last then.Whole technology exists not enough: 1. operational path is long; 2. complicated operation; 3. energy consumption is big; The loss of 4. uncontrollable material and solvent; 5. cost height.
The objective of the invention is to provides a kind of material condition unrestricted to the public, does not want plus solvent, with the method for physical means purification trans-anethole.
Principle of the present invention is: the star aniseed oil that distills out contains 55 kinds of compositions, has proved conclusively 39 kinds of compounds and content thereof.Main have six kinds, i.e. trans-anethole, limonene, p-allylphenol methyl ether, caryophyllene, cis isoesdragol, β-bergapten etc.Because their physical properties difference, zero pour is also inequality.The zero pour of trans-anethole is 21～22 degree Celsius, boiling point 239.5C/0.1MPa.Adopt the freezing method that combines with rectifying can reach the purpose of purification trans-anethole.Under the low temperature of negative 10 degree Celsius～negative 30 degree, star aniseed oil is carried out freezing and crystallizing and handle, then Frozen Body is crushed to about 20 purpose screen sizes.Particle is too big, is included in the intravital impurity of crystallization and is difficult to separated; Particle is too thin, and crystal easily melts, and causes the trans-anethole loss to increase.Utilize the difference of zero pour, through repeated multiple times freezing-pulverizing-separation, rectifying then can reach more than 99.575% the purity of trans-anethole.Remaining impurity liquid can collect at every turn, adopts this technology the exhausted major part of trans-anethole can be proposed.
Cost of the present invention is low, and power consumption is few, the purity height, and impurity is few, and technology is simple.
Fig. 1 process flow sheet
Embodiment: get 580 kilograms of content and be 89.125% star aniseed oil, wherein foreign matter content is mainly: 1. the p-allylphenol methyl ether 4.138%; 2. the cis caryophyllene 0.68%; 3. the cis isoesdragol 0.38%; 4. β-bergapten 0.51%; 5. anisyl aldehyde 0.101%.Raw material is placed on freezing treatment was crushed to 20 mesh sieve hole sizes to xln in 16 hours then under-10 ℃～-30 ℃ low temperature, puts into whizzer and carry out liquid-solid separation.1450 rev/mins of centrifuge speeds.Frozen Body and impurity liquid after the separation are collected respectively.The crystal of collecting, impurity liquid are distinguished so again twice repeatedly.The trans-anethole crystal is dropped into distillation tower rectifying.The material of distillation tower is 1Cr18Ni9Ti.Heat with oil bath, the oil temperature is 130 degree～170 degree Celsius, collects the trans-anethole of purifying.Trans-anethole purity after the rectifying is 99.33%, and 397 kilograms of weight, yield are 68.45%, and is still impure in the trans-anethole product, but pettiness very, p-allylphenol methyl ether 0.136%; Cis caryophyllene and β-bergapten sum 0.211%, cis isoesdragol 0.125%, anisyl aldehyde 0.113%, all the other impurity 0.085%.
Claims (1)
1, the method of purification of trans-anethole, the star aniseed oil that distills out contains 55 kinds of compositions, wherein topmost have six kinds, it is trans-anethole, limonene, the p-allylphenol methyl ether, caryophyllene, the cis isoesdragol, β-bergapten, it is characterized in that: utilize the inequality of their zero pour, with the physical means trans-anethole of purifying, with the star anise cerebrol negative 30 degree Celsius to the low temperature of negative 10 degree freezing 16 hours, then Frozen Body is crushed to 20 mesh sieve hole sizes, the whizzer that putting into per minute 1450 again changes separates, respectively Frozen Body and impurity liquid are collected respectively, through repeated multiple times freezing-pulverizing-separation, rectifying then, rectifying tower is: 1Cr18Ni9Ti, oil bath is heated, and oily temperature control is spent to 170 degree Celsius 130.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92110181 CN1077217A (en) | 1992-08-25 | 1992-08-25 | The method of purification of trans-anethole |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92110181 CN1077217A (en) | 1992-08-25 | 1992-08-25 | The method of purification of trans-anethole |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1077217A true CN1077217A (en) | 1993-10-13 |
Family
ID=4944661
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 92110181 Pending CN1077217A (en) | 1992-08-25 | 1992-08-25 | The method of purification of trans-anethole |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1077217A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102070424A (en) * | 2009-11-24 | 2011-05-25 | 浙江医药股份有限公司新昌制药厂 | Method for preparing all-trans pseudo-ionone |
| CN102976905A (en) * | 2012-12-06 | 2013-03-20 | 广西京桂香料有限公司 | Extracting process method for anethole |
| CN105237364A (en) * | 2015-09-08 | 2016-01-13 | 广西中烟工业有限责任公司 | Preparation method and application of trans-anethole |
| CN111534379A (en) * | 2020-04-02 | 2020-08-14 | 涟源康麓生物科技有限公司 | Method and equipment for extracting essential oil from citrus aurantium flowers, leaves and fruits |
| CN114644959A (en) * | 2020-12-21 | 2022-06-21 | 大连理工江苏研究院有限公司 | Purification system and method of trans-anethole |
-
1992
- 1992-08-25 CN CN 92110181 patent/CN1077217A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102070424A (en) * | 2009-11-24 | 2011-05-25 | 浙江医药股份有限公司新昌制药厂 | Method for preparing all-trans pseudo-ionone |
| CN102976905A (en) * | 2012-12-06 | 2013-03-20 | 广西京桂香料有限公司 | Extracting process method for anethole |
| CN102976905B (en) * | 2012-12-06 | 2014-10-01 | 广西京桂香料有限公司 | Extracting process method for anethole |
| CN105237364A (en) * | 2015-09-08 | 2016-01-13 | 广西中烟工业有限责任公司 | Preparation method and application of trans-anethole |
| CN111534379A (en) * | 2020-04-02 | 2020-08-14 | 涟源康麓生物科技有限公司 | Method and equipment for extracting essential oil from citrus aurantium flowers, leaves and fruits |
| CN114644959A (en) * | 2020-12-21 | 2022-06-21 | 大连理工江苏研究院有限公司 | Purification system and method of trans-anethole |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102198937B (en) | Static multistage melting crystallization method for preparing electronic grade phosphoric acid | |
| CN110846513A (en) | Method for filtering and centrifugally separating mixture containing aluminum, silicon, iron and the like, removing impurities and purifying | |
| CN108046993B (en) | Method for preparing peppermint oil and menthol with various specifications by azeotropic and vacuum rectification technology | |
| CN101735018B (en) | Method for extracting natural D-bornel from branches and leaves of camphor trees | |
| CN102001946A (en) | Novel method for simultaneously extracting and separating chlorogenic acid and honeysuckle flower essential oil from honeysuckle flower | |
| CN107304196A (en) | A kind of method of vacuum distillation-refined glycolide of fusion-crystallization coupling | |
| CN101074258B (en) | Method for separating and extracting phytosterin and Vitamin E from soyabean deodorization distillate | |
| US3370082A (en) | Purification of adipodinitrile | |
| CN1077217A (en) | The method of purification of trans-anethole | |
| CN107954845A (en) | Method for purifying 4-hydroxyacetophenone | |
| CN104045519B (en) | High-purity Delta terpilenol separation and purification method | |
| JPH01132558A (en) | Low or high boiling point product of caprolactam distillation or method for obtaining caprolactam therefrom | |
| CN102206241B (en) | Technological process for extracting ergosterol with high purity and feed protein from penicillin waste residue | |
| CN102249865B (en) | Method for purifying high-purity transacomhole | |
| CN104230668B (en) | Cedrene and the method for cedar wood alcohol is extracted from oleum Cunninghamiae lanceolatae | |
| CN102826959A (en) | Method for extracting erythritol from erythritol mother liquor | |
| CN102850370A (en) | Method for recovering 1,8-eucalyptol from eucalyptus oil by product | |
| CN112125794A (en) | Improved preparation method of trifluoro-chloro-chrysanthemic acid | |
| CN111606918B (en) | Method for preparing high-purity 1, 8-cineole from crude cinnamomum camphora oil | |
| CN101417917A (en) | Method for preparing high-purity all-trans lycopene crystal | |
| CN101580494A (en) | Method for extracting phenazine from RT base production waste | |
| CN109574928A (en) | A method of purification cyclohexanone oxime vapour phase rearrangement product | |
| CN102526334A (en) | Industrial method for producing tomato red by using tomato peel residues | |
| CN111647002A (en) | Method for preparing high-purity 1, 8-cineole by using alkane diol mixed green solvent | |
| EP0067224B1 (en) | Process for producing dibenzofuran |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication |