CN108864126A - A kind of method of eucalyptus oil series classification rectifying - Google Patents
A kind of method of eucalyptus oil series classification rectifying Download PDFInfo
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- CN108864126A CN108864126A CN201810566562.0A CN201810566562A CN108864126A CN 108864126 A CN108864126 A CN 108864126A CN 201810566562 A CN201810566562 A CN 201810566562A CN 108864126 A CN108864126 A CN 108864126A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/02—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains two hetero rings
- C07D493/08—Bridged systems
Abstract
The invention discloses a kind of methods of eucalyptus oil series classification rectifying, include the following steps：(1) inorganic agent is added in thick eucalyptus oil, is uniformly mixed, and thick eucalyptus oil is preheated to 100~250 DEG C, kept for 2~3 hours, it is cooling；(2) the thick eucalyptus oil after cooling is filtered, and retains filtered fluid；(3) filtered fluid is passed through rectifying in first rectifying column；(4) after via first rectifying column rectifying, the tower reactor of first rectifying column residual night is passed through rectifying in Second distillation column, obtains the eucalyptus oil.Inorganic agent is added in the present invention in thick eucalyptus oil to pre-process, and carry out the impurity being removed by filtration in thick eucalyptus oil or deposit, then it is passed through progress first time rectifying in first rectifying column again, after first time rectifying, tower reactor residual night in first rectifying column is passed through in Second distillation column and carries out secondary rectifying, finally obtains the eucalyptus oil.The present invention passes through secondary rectifying, improves the purity of eucalyptus oil, and the rate of recovery greatly improves.
Description
Technical field
The invention belongs to essential oil technical fields, and in particular to a kind of method of eucalyptus oil series classification rectifying.
Background technique
Eucalyptus oil extracts essential oil, then essence with steam distillation from the leaf, branch of blue gum, folium eucalypti tree, cinnamomum camphora tree and camphor tree etc.
System processing is made.The ground such as Spain, Portugal, the Congo and South America mainly are originated in, Yunnan Province of China, Guangdong, Guangxi also there are a large amount of lifes
It produces.
Eucalyptus oil is a kind of volatile oil, is the mixture containing a variety of organic principles.Eucalyptus oil is according to main ingredient and purposes
It can be divided into three classes：Medicine, fragrance and iundustrial oil.Most important of which is that pharmaceutical eucalyptus oil, main ingredient 1,8- eucalyptus oil
Element.
The thick eucalyptus oil impurity of natural products is more, wherein there are also a small amount of nopinene, laurene, α-water based on australene
Celery alkene, limonene dissipate florigen, γ-terpinene, linalool etc. to poly-.Plurality of impurities and 1,8- cineole be isomer or
Person's molecular structure and molecular weight are very close, have similar physicochemical properties, for cineole purification bring it is very big
Difficulty.
It is existing separation cineole method there are many kinds of, as supercritical extraction, silica gel column chromatography, chemical reaction method,
Catalytic rectification process, the crystallizing process under low temperature, film-falling crystallization method etc., but the rate of recovery of existing eucalyptus oil need to be improved.
Summary of the invention
To solve the above-mentioned problems, the present invention provides a kind of method of the series classification rectifying of eucalyptus oil, eucalyptus oil is improved
The rate of recovery.
The technical scheme is that：A kind of method of the series classification rectifying of eucalyptus oil, includes the following steps：
(1) inorganic agent is added in thick eucalyptus oil, is uniformly mixed, and thick eucalyptus oil is preheated to 100~250 DEG C, keep 2~3
Hour, it is cooling；
(2) the thick eucalyptus oil after cooling is filtered, and retains filtered fluid；
(3) filtered fluid is passed through rectifying in first rectifying column；
(4) after via first rectifying column rectifying, the tower reactor of first rectifying column residual night is passed through rectifying in Second distillation column,
Obtain the eucalyptus oil.
Preferably, the tower top operation temperature of the first rectifying column be 70~80 DEG C, top vacuum degree be 1.0~
2.0KPa。
Preferably, the tower top operation temperature of the Second distillation column be 100~110 DEG C, top vacuum degree be 1.0~
3.0KPa。
Preferably, the inorganic agent is propyl alcohol.
Preferably, the mass ratio of the inorganic agent and thick eucalyptus oil is 1~5.5:100.
Preferably, the thick eucalyptus oil is preheated to 180 DEG C, kept for 2 hours.
Preferably, the content of 1,8- cineole is 45~50% in the thick eucalyptus oil.
Compared with prior art, the beneficial effects of the present invention are embodied in：
In the present invention in thick eucalyptus oil be added inorganic agent pre-process, and carry out the impurity being removed by filtration in thick eucalyptus oil or
It is deposit, progress first time rectifying in first rectifying column is then passed through again, after first time rectifying, by the first rectifying
Tower reactor residual night in tower, which is passed through in Second distillation column, carries out secondary rectifying, finally obtains the eucalyptus oil.The present invention passes through secondary fine
It evaporates, improves the purity of eucalyptus oil, and the rate of recovery greatly improves.
Specific embodiment
Embodiment 1
A kind of method of the series classification rectifying of eucalyptus oil, includes the following steps：
(1) in thick eucalyptus oil, (propyl alcohol is added to be 45%) middle in the content of 1,8- cineole, is uniformly mixed, and thick eucalyptus oil is preheated
It to 250 DEG C, is kept for 3 hours, cooling, wherein the mass ratio of propyl alcohol and thick eucalyptus oil is 2:100；
(2) the thick eucalyptus oil after cooling is filtered, and retains filtered fluid；
(3) filtered fluid is passed through rectifying in first rectifying column, wherein the tower top operation temperature of first rectifying column is 70~80
DEG C, top vacuum degree is 1.0~2.0KPa；
(4) after via first rectifying column rectifying, the tower reactor of first rectifying column residual night is passed through rectifying in Second distillation column,
Wherein the tower top operation temperature of Second distillation column is 100~110 DEG C, and top vacuum degree is 1.0~3.0KPa, obtains the eucalyptus
Oil.
The product containing 1,8- cineole 94.22%, total recovery 79.15% are obtained via the above method.
Embodiment 2
A kind of method of the series classification rectifying of eucalyptus oil, includes the following steps：
(1) in thick eucalyptus oil, (propyl alcohol is added to be 50%) middle in the content of 1,8- cineole, is uniformly mixed, and thick eucalyptus oil is preheated
It to 120 DEG C, is kept for 2 hours, cooling, wherein the mass ratio of propyl alcohol and thick eucalyptus oil is 1:100；
(2) the thick eucalyptus oil after cooling is filtered, and retains filtered fluid；
(3) filtered fluid is passed through rectifying in first rectifying column, wherein the tower top operation temperature of first rectifying column is 70~80
DEG C, top vacuum degree is 1.0~2.0KPa；
(4) after via first rectifying column rectifying, the tower reactor of first rectifying column residual night is passed through rectifying in Second distillation column,
Wherein the tower top operation temperature of Second distillation column is 100~110 DEG C, and top vacuum degree is 1.0~3.0KPa, obtains the eucalyptus
Oil.
The product containing 1,8- cineole 93.99%, total recovery 80.12% are obtained via the above method.
Embodiment 3
A kind of method of the series classification rectifying of eucalyptus oil, includes the following steps：
(1) in thick eucalyptus oil, (propyl alcohol is added to be 48%) middle in the content of 1,8- cineole, is uniformly mixed, and thick eucalyptus oil is preheated
It to 180 DEG C, is kept for 2.5 hours, cooling, wherein the mass ratio of propyl alcohol and thick eucalyptus oil is 4.5:100；
(2) the thick eucalyptus oil after cooling is filtered, and retains filtered fluid；
(3) filtered fluid is passed through rectifying in first rectifying column, wherein the tower top operation temperature of first rectifying column is 70~80
DEG C, top vacuum degree is 1.0~2.0KPa；
(4) after via first rectifying column rectifying, the tower reactor of first rectifying column residual night is passed through rectifying in Second distillation column,
Wherein the tower top operation temperature of Second distillation column is 100~110 DEG C, and top vacuum degree is 1.0~3.0KPa, obtains the eucalyptus
Oil.
The product containing 1,8- cineole 95.11%, total recovery 80.15% are obtained via the above method.
Embodiment 4
A kind of method of the series classification rectifying of eucalyptus oil, includes the following steps：
(1) in thick eucalyptus oil, (propyl alcohol is added to be 45%) middle in the content of 1,8- cineole, is uniformly mixed, and thick eucalyptus oil is preheated
To 100, kept for 2 hours, cooling, wherein the mass ratio of propyl alcohol and thick eucalyptus oil is 5.5:100；
(2) the thick eucalyptus oil after cooling is filtered, and retains filtered fluid；
(3) filtered fluid is passed through rectifying in first rectifying column, wherein the tower top operation temperature of first rectifying column is 70~80
DEG C, top vacuum degree is 1.0~2.0KPa；
(4) after via first rectifying column rectifying, the tower reactor of first rectifying column residual night is passed through rectifying in Second distillation column,
Wherein the tower top operation temperature of Second distillation column is 100~110 DEG C, and top vacuum degree is 1.0~3.0KPa, obtains the eucalyptus
Oil.
The product containing 1,8- cineole 93.55%, total recovery 79.75% are obtained via the above method.
Claims (7)
1. a kind of method of eucalyptus oil series classification rectifying, which is characterized in that include the following steps：
(1) inorganic agent is added in thick eucalyptus oil, is uniformly mixed, and thick eucalyptus oil is preheated to 100~250 DEG C, kept for 2~3 hours,
It is cooling；
(2) the thick eucalyptus oil after cooling is filtered, and retains filtered fluid；
(3) filtered fluid is passed through rectifying in first rectifying column；
(4) after via first rectifying column rectifying, the tower reactor of first rectifying column residual night is passed through rectifying in Second distillation column, is obtained
The eucalyptus oil.
2. the method for eucalyptus oil series classification rectifying as described in claim 1, which is characterized in that the tower top of the first rectifying column
Operation temperature is 70~80 DEG C, and top vacuum degree is 1.0~2.0KPa.
3. the method for eucalyptus oil series classification rectifying as described in claim 1, which is characterized in that the tower top of the Second distillation column
Operation temperature is 100~110 DEG C, and top vacuum degree is 1.0~3.0KPa.
4. the method for eucalyptus oil series classification rectifying as described in claim 1, which is characterized in that the inorganic agent is propyl alcohol.
5. the method for eucalyptus oil series classification rectifying as described in claim 1, which is characterized in that the inorganic agent and thick eucalyptus oil
Mass ratio is 1~5.5:100.
6. the method for eucalyptus oil series classification rectifying as described in claim 1, which is characterized in that the thick eucalyptus oil is preheated to 180
DEG C, it is kept for 2 hours.
7. the method for eucalyptus oil series classification rectifying as described in claim 1, which is characterized in that 1,8- eucalyptus oil in the thick eucalyptus oil
The content of element is 45~50%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115449434A (en) * | 2022-10-13 | 2022-12-09 | 江西安邦药业有限公司 | Method for continuously and hierarchically rectifying eucalyptus oil |
Citations (5)
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|---|---|---|---|---|
| EP0125539B1 (en) * | 1983-05-12 | 1989-08-23 | Union Camp Corporation | Separation of 1,8-cineole |
| CN1181415A (en) * | 1996-11-04 | 1998-05-13 | 中国林业科学研究院林产化学工业研究所 | Euclyptus oil continuous rectificating technique |
| CN101899361A (en) * | 2010-08-04 | 2010-12-01 | 厦门百度科技开发有限公司 | Single-tower continuous rectification method of eucalyptus oil |
| CN102504955A (en) * | 2011-11-01 | 2012-06-20 | 昆明理工大学 | Processing for extracting and purifying eucalyptus oil |
| CN106674244A (en) * | 2016-12-14 | 2017-05-17 | 盐城市春竹香料有限公司 | Preparation method of cineole |
-
2018
- 2018-06-05 CN CN201810566562.0A patent/CN108864126B/en active Active
Patent Citations (5)
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|---|---|---|---|---|
| EP0125539B1 (en) * | 1983-05-12 | 1989-08-23 | Union Camp Corporation | Separation of 1,8-cineole |
| CN1181415A (en) * | 1996-11-04 | 1998-05-13 | 中国林业科学研究院林产化学工业研究所 | Euclyptus oil continuous rectificating technique |
| CN101899361A (en) * | 2010-08-04 | 2010-12-01 | 厦门百度科技开发有限公司 | Single-tower continuous rectification method of eucalyptus oil |
| CN102504955A (en) * | 2011-11-01 | 2012-06-20 | 昆明理工大学 | Processing for extracting and purifying eucalyptus oil |
| CN106674244A (en) * | 2016-12-14 | 2017-05-17 | 盐城市春竹香料有限公司 | Preparation method of cineole |
Non-Patent Citations (3)
| Title |
|---|
| 刘文婷: "1,8-桉叶油素的结晶及精馏提纯工艺研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
| 张健生，等: "助剂辅助真空间歇精馏分离1，8-桉叶素", 《化工进展》 * |
| 杨素华: "真空精馏法分离樟油主要成分的研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115449434A (en) * | 2022-10-13 | 2022-12-09 | 江西安邦药业有限公司 | Method for continuously and hierarchically rectifying eucalyptus oil |
| CN115449434B (en) * | 2022-10-13 | 2023-11-17 | 江西安邦药业有限公司 | Method for continuous fractional distillation of eucalyptus oil |
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