CN106854138A - The method that sclareol is separated by sclareol mother liquor - Google Patents
The method that sclareol is separated by sclareol mother liquor Download PDFInfo
- Publication number
- CN106854138A CN106854138A CN201611244742.4A CN201611244742A CN106854138A CN 106854138 A CN106854138 A CN 106854138A CN 201611244742 A CN201611244742 A CN 201611244742A CN 106854138 A CN106854138 A CN 106854138A
- Authority
- CN
- China
- Prior art keywords
- sclareol
- solvent
- mixed solution
- parsing
- mother liquor
- 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.)
- Granted
Links
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
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Fats And Perfumes (AREA)
Abstract
A kind of method that sclareol is separated by sclareol mother liquor, comprises the steps successively：Add parsing solvent, the silicon particle for making parsing solvent flood completely in chromatographic column；Under normal temperature and pressure, the sclareol mother liquor of certain volume is added in chromatographic column；Under normal temperature and pressure, parsing solvent is continuously added in chromatographic column, the sclareol mother liquor in chromatographic column is eluted；Cured and parsing solvent the mixed solution of plant to chromatographing column outlet is collected；The mixed solution of sclareol and parsing solvent to chromatographing column outlet is collected；Mixed solution concentration to sclareol and parsing solvent.Advantage is：Production efficiency is improve, production cost has been saved.
Description
Technical field
The present invention relates to the separation technology field of natural perfume material, one kind is related in particular to by sclareol mother liquor point
From the method for sclareol.
Background technology
Sclareol mother liquor be by 80% sclareol through acetone crystallization, centrifugation, separate after the concentration of remaining mixed solution and
, the sclareol content in this some residual mixed solution is between 20%-30%, it is generally the case that in sclareol mother liquor,
Sclareol and vegetable wax other method are difficult to efficiently separate, and are at present have two for the processing method of this part mixed solution
Kind, it is respectively to extract, recrystallize, but extraction is used, can not efficiently separate, and the quantity of solvent of consumption is larger, what it was obtained
Sclareol purity is relatively low；And the result for recrystallizing is then to regenerate sclareol mother liquor, fragrant purple perilla can not be at all solved
Sclareol is separated with vegetable wax in alcohol mother liquor, and resulting sclareol purity can not reach requirement.In prior art
In, the method taken can not completely be reclaimed to the sclareol in sclareol mother liquor, cause the wave of sclareol
Take, so as to increase processing cost.
The content of the invention
The present invention be directed to above-mentioned deficiency, there is provided a kind of side that sclareol is completely separated by sclareol mother liquor
Method.Its particular content is：
A kind of method that sclareol is separated by sclareol mother liquor, comprises the steps successively：
（1）Parsing solvent is added in chromatographic column, the silicon particle for making parsing solvent flood completely in chromatographic column；
（2）Under normal temperature and pressure, the sclareol mother liquor of certain volume is added in chromatographic column；
（3）Under normal temperature and pressure, parsing solvent is continuously added in chromatographic column, the sclareol mother liquor in chromatographic column is carried out
Wash-out；
（4）The mixed solution of vegetable wax and parsing solvent to chromatographing column outlet is collected into the distillation still of vegetable wax and parsing solvent
It is interior；
（5）The mixed solution of sclareol and parsing solvent to chromatographing column outlet is collected into the steaming of sclareol and parsing solvent
Evaporate in kettle；
（6）Distillation and concentration is carried out to the mixed solution in two kinds of distillation stills respectively；
Described parsing solvent is No. 120 mixed solutions of solvent naphtha, petroleum ether and acetone, and No. 120 solvent naphthas, petroleum ether and
Ratio between acetone is 3:1:1；Step（5）During the mixed solution of middle recovery sclareol and parsing solvent, chromatography need to be detected
Whether contain sclareol in the mixed solution of column outlet, if containing fragrant purple perilla in detecting the mixed solution for chromatographing column outlet
Alcohol, then start to be collected the mixed solution of sclareol and parsing solvent.
Further, the draw ratio of described chromatographic column is 13:1.
Further, step（6）The condensed device of parsing solvent obtained after middle distillation and concentration is reclaimed to be reused, two steamings
Evaporate kettle and obtain vegetable wax raffinate and 90% sclareol respectively.
Compared with prior art, advantages of the present invention is：The sclareol and vegetable wax in sclareol mother liquor can be made
Thoroughly separated, improved the yield of sclareol in clary sage concrete process, and can be to the parsing in separation process
Solvent carries out recovery and uses, and so as to improve production efficiency, has saved production cost.
Brief description of the drawings
Fig. 1 is the sectional view of chromatographic column.
Fig. 2 is the left view of chromatographic column.
Fig. 3 is schematic flow sheet of the invention.
Fig. 4 is process chart of the invention.
Specific embodiment
The present invention is made completely with reference to embodiments of the invention, be explicitly described.
Embodiment 1：
A kind of method that sclareol is separated by sclareol mother liquor as shown in Figure 3 and Figure 4, will parse solvent from containing first
Kettle 9 in parsing solvent be added to through pump in the chromatographic column 5 for being filled with the silicon particle of 800 mesh, until parsing solvent flood layer completely
, then be added to the sclareol mother liquor of 10kg in chromatographic column 5 by the silicon particle in analysis post 5, and then will contain parsing solvent
Kettle 9 in parsing solvent be continuously added in chromatographic column through pump sclareol mother liquor in chromatographic column 5 eluted, due to
Silicon particle is weaker to the adsorptivity of vegetable wax, and the adsorptivity to sclareol is stronger, so vegetable wax is first eluted, this
When, need to detect whether the mixed solution in the exit of chromatographic column 5 contains vegetable wax, if containing vegetable wax, by 10 dozens, the first valve
Open, now the mixed solution of vegetable wax and parsing solvent can then flow into the first of the mixed solution for collecting vegetable wax and parsing solvent
In distillation still 7, finally, rule of thumb, the mixed solution for chromatographing column outlet is detected in real time, if detecting containing fragrant purple
Soviet Union's alcohol, then open the second valve 11, flows into the mixed solution of sclareol and parsing solvent and collects sclareol and parsing
In the after-fractionating kettle 6 of solvent mixed solution, the mixed solution in the first distillation still 7 and after-fractionating kettle 6 is entered respectively then
Row distillation and concentration, the parsing solvent obtained after distillation and concentration reclaimed through the first condenser 8 and the second condenser 12 enter into containing
Parse in the kettle 9 of solvent and reuse, the first distillation still 7 and after-fractionating kettle 6 obtains vegetable wax raffinate respectively and 2kg contains
The product of 90% sclareol.
Embodiment 2：
Chromatographic column as shown in Figure 1 and Figure 2, chromatographic column includes cylinder 1 and silicon particle 2, and silicon particle 2 is filled in inside cylinder 1,
When being eluted to sclareol mother liquor, parsing solvent is set to flood the silicon particle in chromatographic column completely first, then by fragrant purple perilla
Alcohol mother liquor is added by the inlet 4 of chromatographic column, due to silicon particle 2 for the vegetable wax adsorption capacity in sclareol mother liquor compared with
It is weak, when parsing solvent is continuously added chromatographic column, sclareol mother liquor can be eluted, because silicon particle is to vegetable wax
Adsorption capacity is relatively weak, then vegetable wax can first be eluted, because silicon particle is stronger for the adsorption capacity of sclareol,
The time that then sclareol is eluted is more long, according to the sequencing of wash-out, adjusts the flow divider of chromatographic column liquid outlet 3,
The mixed solution of chromatographic column liquid outlet 3 is set to be collected into corresponding container.
Advantages of the present invention is：The sclareol in sclareol mother liquor can be enable thoroughly to be separated with vegetable wax,
Improving the yield of sclareol in clary sage concrete process, and can carry out recovery to the parsing solvent in separation process makes
With so as to improve production efficiency, having saved production cost.
Claims (3)
1. a kind of method that sclareol is separated by sclareol mother liquor, comprises the steps successively：
（1）Parsing solvent is added in chromatographic column, the silicon particle for making parsing solvent flood completely in chromatographic column；
（2）Under normal temperature and pressure, the sclareol mother liquor of certain volume is added in chromatographic column；
（3）Under normal temperature and pressure, will parsing solvent be continuously added in chromatographic column, to chromatographic column in fragrant purple perilla mother liquor wash
It is de-；
（4）The mixed solution of vegetable wax and parsing solvent to chromatographing column outlet is collected into the distillation still of vegetable wax and parsing solvent
It is interior；
（5）The mixed solution of sclareol and parsing solvent to chromatographing column outlet is collected into the steaming of sclareol and parsing solvent
Evaporate in kettle；
（6）Distillation and concentration is carried out to the mixed solution in two kinds of distillation stills respectively；
It is characterized in that：Described parsing solvent is No. 120 mixed solutions of solvent naphtha, petroleum ether and acetone, and No. 120 solvents
Oil, the ratio between petroleum ether and acetone are 3:1:1；Step（5）During the mixed solution of middle recovery sclareol and parsing solvent,
Whether contain sclareol in the mixed solution that chromatography column outlet need to be detected, if containing in detecting the mixed solution for chromatographing column outlet
There is sclareol, then start to be collected the mixed solution of sclareol and parsing solvent.
2. it is according to claim 1 it is a kind of by sclareol mother liquor separate sclareol method, it is characterised in that：It is described
Chromatographic column draw ratio be 13:1.
3. it is according to claim 1 it is a kind of by sclareol mother liquor separate sclareol method, it is characterised in that：Step
（6）The condensed device of the parsing solvent that is obtained after middle distillation and concentration is reclaimed to be reused, and it is residual that two distillation stills obtain vegetable wax respectively
Liquid and 90% sclareol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611244742.4A CN106854138B (en) | 2016-12-29 | 2016-12-29 | Method for separating sclareol from sclareol mother liquor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611244742.4A CN106854138B (en) | 2016-12-29 | 2016-12-29 | Method for separating sclareol from sclareol mother liquor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106854138A true CN106854138A (en) | 2017-06-16 |
| CN106854138B CN106854138B (en) | 2020-04-21 |
Family
ID=59127099
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611244742.4A Active CN106854138B (en) | 2016-12-29 | 2016-12-29 | Method for separating sclareol from sclareol mother liquor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106854138B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114988983A (en) * | 2022-06-09 | 2022-09-02 | 新疆师范大学 | Method for separating sclareol from sclareol extract |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU417408A1 (en) * | 1972-01-07 | 1974-02-28 | Г. В. Лазурьевский, Л. А. Салей , Д. П. Попа Институт химии Молдавской ССР | METHOD OF EXTRACTING SKLAREOLA |
| FR2741065A1 (en) * | 1995-11-15 | 1997-05-16 | Inst Francais Du Petrole | Preparation of sclareol from sage by dissolving in solvent |
| CN101229992A (en) * | 2008-01-10 | 2008-07-30 | 华东理工大学 | Method for preparing sclaveol by sclaveol concrete |
-
2016
- 2016-12-29 CN CN201611244742.4A patent/CN106854138B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU417408A1 (en) * | 1972-01-07 | 1974-02-28 | Г. В. Лазурьевский, Л. А. Салей , Д. П. Попа Институт химии Молдавской ССР | METHOD OF EXTRACTING SKLAREOLA |
| FR2741065A1 (en) * | 1995-11-15 | 1997-05-16 | Inst Francais Du Petrole | Preparation of sclareol from sage by dissolving in solvent |
| CN101229992A (en) * | 2008-01-10 | 2008-07-30 | 华东理工大学 | Method for preparing sclaveol by sclaveol concrete |
Non-Patent Citations (2)
| Title |
|---|
| 周敏: "层析法分离回收香紫苏内酯", 《万方学位论文库硕士学位论文》 * |
| 蒲湘渝: "米团花的化学成分研究", 《云南植物研究》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114988983A (en) * | 2022-06-09 | 2022-09-02 | 新疆师范大学 | Method for separating sclareol from sclareol extract |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106854138B (en) | 2020-04-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| AU2019250112B2 (en) | Cannabinoid extraction and distillation | |
| EP3461546A1 (en) | Cannabinoid extraction process and system | |
| Li et al. | Extraction of Cuminum cyminum essential oil by combination technology of organic solvent with low boiling point and steam distillation | |
| CN104761528B (en) | A method of natural VE is extracted with ion liquid abstraction agent | |
| CN105602719B (en) | A kind of supercritical extraction method of tea oil | |
| CN107473967A (en) | A kind of method that ion liquid abstraction rectifying removes acid and water simultaneously | |
| CN102633597B (en) | Process of recovering ethanol, propyl alcohol and isobutyl alcohol from polyalcohol-water mixture | |
| CN103289717A (en) | Method for solvent extraction-column chromatography separation of coal tar, and apparatus thereof | |
| CN106854138A (en) | The method that sclareol is separated by sclareol mother liquor | |
| CN103215073A (en) | Production method for extracting lignite wax from brown coal | |
| US2847368A (en) | Extraction of hydrocarbons from water | |
| CN108003082A (en) | A kind of solvent recovery process for the production of poly arylidene thio-ester resinoid | |
| CN105385716B (en) | A kind of method that sulfur-containing compound in garlic is separated using countercurrent chromatography | |
| JP7134644B2 (en) | Determination method of dialkyl ketone in fats and oils | |
| CN106433951A (en) | Extraction method of camphorated oil | |
| CN108935868B (en) | Method for extracting aromatic substances from plant products | |
| CN104596834A (en) | Method for enriching aroma components of cherry wine | |
| CN108484603A (en) | The method that tabersonine is extracted from African Voacanga | |
| CN106831336B (en) | Ethyl alcohol and the recycling of hydrazine hydrate mixed liquor and circulation utilization method in a kind of production of pyraclostrobin | |
| CN104130096A (en) | Method for continuously separating high-purity longifolene from heavy turpentine | |
| CN112457917A (en) | Method for recovering flavor components in reconstituted tobacco condensed water, eluent formed by method and application | |
| CN108690658A (en) | A method of aromatic hydrocarbons in recycling low arene content oil | |
| CN107619716A (en) | A kind of method of bitter substance in removal linseed oil | |
| CN105121615B (en) | Method for handling fat and oil | |
| US1870854A (en) | Process for separating mixtures of substances only partially miscible |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |