CN106831335A - A kind of technique of 4 terpinenol isolated from eucalyptus oil - Google Patents
A kind of technique of 4 terpinenol isolated from eucalyptus oil Download PDFInfo
- Publication number
- CN106831335A CN106831335A CN201710049512.0A CN201710049512A CN106831335A CN 106831335 A CN106831335 A CN 106831335A CN 201710049512 A CN201710049512 A CN 201710049512A CN 106831335 A CN106831335 A CN 106831335A
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- CN
- China
- Prior art keywords
- terpinenols
- eucalyptus oil
- isolated
- technique
- accurate
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- 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.)
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/42—Regulation; Control
- B01D3/4205—Reflux ratio control splitter
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
Abstract
It is as follows the invention discloses a kind of technique of 4 terpinenol isolated from eucalyptus oil, including processing step：1）Charging, 2）Fractionation, 3）Precise collection, 4）Accurate multiple steaming.The present invention utilizes accurate tower, increases reflux ratio, and 4 terpinenols of accurate fractionation purification improve the rate of recovery, reduce production cost, increase productivity effect.
Description
Technical field
The present invention relates to a kind of technique of 4- terpinenols isolated from eucalyptus oil.
Background technology
Chinese yunnan reputation is referred to as natural perfume material kingdom, and it is the big fine work oil of the world ten to produce eucalyptus oil, and yield is about 20000
Ton, accounts for the 95% of volume of world trade, is the big characteristic spices kind of China one, and eucalyptus oil is widely used in pharmacy, food additives, day
Change and fragrance industry.
4- terpinenols are the important active component in tea oil, and inner is antibacterial most excellent in plant kingdom, bactericide,
It is important medicine chemical material, can efficiently kills the fungi and bacterium of skin surface, medically using quite extensively, is having
More than 100 kinds of first aid purposes, daily use chemicals, food, spices are also largely used in recent years, as the business that supply falls short of demand on international market
Product.
Byproduct after isolated Cineole is detected using modern analytical technique, it is still special containing about 10% natural tea tree oil
Some 4- terpinenols, if the purity of this 10% 4- terpinenol is brought up into more than 99%, can greatly improve life
Produce income.
The content of the invention
For above-mentioned technical problem, the purpose of the present invention is：Propose the purity of 10% 4- terpinenols
Bring up to more than 98% technique of isolated 4- terpinenols from eucalyptus oil.
What technical solution of the invention was realized in：A kind of technique of 4- terpinenols isolated from eucalyptus oil,
It is as follows including processing step：
1) feed：Eucalyptus oil raw material is loaded into rectifying still；
2) it is fractionated：In vacuum condition control below -0.6Pa, 105-115 DEG C is warming up to, reflux ratio is 19-21:1, return
The stream time is 38-42 minutes, component before collecting；
3) Precise collection：The concentration of on-line checking 4- terpinenols, when 4- terpinenols concentration reaches more than 60%, opens
Beginning Precise collection distillate；
4) accurate multiple steaming：By the distillate of Precise collection in 3) carry out it is accurate it is multiple steam, temperature control is returned at 125-130 DEG C
Stream is than being 24-26:1；Collect object 4- terpinenols.
Preferably, the step 2) fractional distillation process use tower diameter below 500mm accurate tower.
Preferably, the step 1) feeding uses the stainless steel wave net filler of small peak height.
Due to the utilization of above-mentioned technical proposal, the present invention has following advantages compared with prior art：
A kind of technique of 4- terpinenols isolated from eucalyptus oil of the invention, using accurate tower, increases reflux ratio, accurately
Fractionation purification 4- terpinenols, improve the rate of recovery, reduce production cost, increase productivity effect.
Specific embodiment
Specific embodiment 1：
A kind of technique of 4- terpinenols isolated from eucalyptus oil of the present invention, including processing step is as follows：
1) feed：Eucalyptus oil raw material is loaded into rectifying still；
2) it is fractionated：In vacuum condition control below -0.6Pa, 110 DEG C are warming up to, temperature fluctuation control is at 1 DEG C to -1
DEG C, reflux ratio is 20:1, return time is 40 minutes, collects firpene, hesperidene, spends the preceding components such as footpath, r terpinenes to umbrella；
3) Precise collection：The concentration of on-line checking 4- terpinenols, when 4- terpinenols concentration reaches more than 60%, opens
Beginning Precise collection distillate；On-line checking 4- terpinenols concentration stops collecting distillate when reaching less than 40%；
4) accurate multiple steaming：Concentration by Precise collection in 3) be 80% 4- terpinenols distillate carry out it is accurate it is multiple steam,
At 127.5 DEG C, reflux ratio is 25 to temperature control:1；The object 4- terpinenols that concentration is more than 98% can be collected into；System
Yield is 82%.
The step 2) fractional distillation process use tower diameter below 500mm accurate tower；The step 1) feed using small
The stainless steel wave net filler of peak height.
The parameter of specific embodiment 2-5 is as shown in the table：
As can be seen from the above table, by the processing step of above-mentioned record, in high vacuum conditions, use tower diameter for
The accurate tower of below 500mm, while increasing reflux ratio, realizes gas-liquid exchange equilibrium, using the stainless steel wave net filler of small peak height,
Being conducive to the composition complicated to component carries out precision fractionation, can make the 4- terpinenols that concentration in raw material is 10%, and concentration is carried
Height to more than 98%, and obtain up to more than 80% the rate of recovery, substantially increase productivity effect, reduce production cost.
The above embodiments merely illustrate the technical concept and features of the present invention, its object is to allow person skilled in the art
Scholar will appreciate that present disclosure and be carried out that it is not intended to limit the scope of the present invention, all according to the present invention
The equivalent change or modification that Spirit Essence is made, should all cover within the scope of the present invention.
Claims (3)
1. a kind of technique of 4- terpinenols isolated from eucalyptus oil, it is characterised in that：It is as follows including processing step：
1）Charging：Eucalyptus oil raw material is loaded into rectifying still；
2）Fractionation：In vacuum condition control below -0.6Pa, 105-115 DEG C is warming up to, reflux ratio is 19-21:1, during backflow
Between be 38-42 minute, collect preceding component；
3）Precise collection：The concentration of on-line checking 4- terpinenols, when 4- terpinenols concentration reaches more than 60%, starts essence
Acknowledgement collection distillate；
4）Accurate multiple steaming：By 3）The distillate of middle Precise collection carries out accurate multiple steaming, and temperature control is in 125-130 DEG C, reflux ratio
It is 24-26:1；Collect object 4- terpinenols.
2. the technique of a kind of 4- terpinenols isolated from eucalyptus oil according to claim 1, it is characterised in that：The step
Rapid 2）Accurate tower of the tower diameter of the fractionating column that fractional distillation process is used in below 500mm.
3. the technique of a kind of 4- terpinenols isolated from eucalyptus oil according to claim 1, it is characterised in that：The step
Rapid 1）Charging uses the stainless steel wave net filler of small peak height.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710049512.0A CN106831335A (en) | 2017-01-21 | 2017-01-21 | A kind of technique of 4 terpinenol isolated from eucalyptus oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710049512.0A CN106831335A (en) | 2017-01-21 | 2017-01-21 | A kind of technique of 4 terpinenol isolated from eucalyptus oil |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106831335A true CN106831335A (en) | 2017-06-13 |
Family
ID=59120214
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710049512.0A Pending CN106831335A (en) | 2017-01-21 | 2017-01-21 | A kind of technique of 4 terpinenol isolated from eucalyptus oil |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106831335A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108179662A (en) * | 2018-02-27 | 2018-06-19 | 山东仁丰特种材料股份有限公司 | A kind of antibacterial anti-curd food wrapping paper and preparation method thereof |
| CN108902140A (en) * | 2018-06-27 | 2018-11-30 | 魔范（中山）科技有限公司 | A method of mentioning antibacterial liquid from tea tree hydrosol |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101829074A (en) * | 2010-05-18 | 2010-09-15 | 南宁辰康生物科技有限公司 | Standardized recombinant tea tree oil and preparing method thereof |
| CN102850370A (en) * | 2012-07-13 | 2013-01-02 | 北京工商大学 | Method for recovering 1,8-eucalyptol from eucalyptus oil by product |
-
2017
- 2017-01-21 CN CN201710049512.0A patent/CN106831335A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101829074A (en) * | 2010-05-18 | 2010-09-15 | 南宁辰康生物科技有限公司 | Standardized recombinant tea tree oil and preparing method thereof |
| CN102850370A (en) * | 2012-07-13 | 2013-01-02 | 北京工商大学 | Method for recovering 1,8-eucalyptol from eucalyptus oil by product |
Non-Patent Citations (1)
| Title |
|---|
| 田玉红等: "不同蒸馏时段的粗皮桉叶精油的化学成分", 《中国中药杂志》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108179662A (en) * | 2018-02-27 | 2018-06-19 | 山东仁丰特种材料股份有限公司 | A kind of antibacterial anti-curd food wrapping paper and preparation method thereof |
| CN108902140A (en) * | 2018-06-27 | 2018-11-30 | 魔范（中山）科技有限公司 | A method of mentioning antibacterial liquid from tea tree hydrosol |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170613 |
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| RJ01 | Rejection of invention patent application after publication |