CN106854138B - Method for separating sclareol from sclareol mother liquor - Google Patents
Method for separating sclareol from sclareol mother liquor Download PDFInfo
- Publication number
- CN106854138B CN106854138B CN201611244742.4A CN201611244742A CN106854138B CN 106854138 B CN106854138 B CN 106854138B CN 201611244742 A CN201611244742 A CN 201611244742A CN 106854138 B CN106854138 B CN 106854138B
- Authority
- CN
- China
- Prior art keywords
- sclareol
- solvent
- chromatographic column
- mixed solution
- 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.)
- Active
Links
Images
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 method for separating sclareol from sclareol mother liquor sequentially comprises the following steps: adding an analytic solvent to ensure that the analytic solvent completely submerges silica gel particles in the chromatographic column; adding a certain volume of sclareol mother liquor into a chromatographic column at normal temperature and normal pressure; continuously adding an analytic solvent into a chromatographic column at normal temperature and normal pressure, and eluting sclareol mother liquor in the chromatographic column; collecting the mixed solution of the plant wax and the analytic solvent at the outlet of the chromatographic column; collecting the mixed solution of sclareol and the analytic solvent at the outlet of the chromatographic column; the mixed solution of sclareol and the resolving solvent was concentrated. Has the advantages that: the production efficiency is improved, and the production cost is saved.
Description
Technical Field
The invention relates to the technical field of separation of natural perfume, in particular to a method for separating sclareol from sclareol mother liquor.
Background
The sclareol mother liquor is obtained by concentrating a residual mixed solution after 80% of sclareol is crystallized, centrifuged and separated by acetone, the content of the sclareol in the residual mixed solution is between 20% and 30%, generally, the sclareol and the vegetable wax in the sclareol mother liquor are difficult to effectively separate by other methods, at present, two treatment methods for the mixed solution are adopted, namely extraction and recrystallization respectively, but the extraction method is adopted, the effective separation cannot be realized, the consumed solvent amount is large, and the obtained sclareol has low purity; the result of recrystallization is that sclareol mother liquor is regenerated, the separation of sclareol and vegetable wax in the sclareol mother liquor cannot be fundamentally solved, and the purity of the obtained sclareol cannot meet the requirement. In the prior art, none of the methods adopted can completely recover the sclareol in the sclareol mother liquor, which causes the waste of the sclareol and further increases the processing and production cost.
Disclosure of Invention
The invention provides a method for thoroughly separating sclareol from sclareol mother liquor, aiming at the defects. The concrete content is as follows:
a method for separating sclareol from sclareol mother liquor sequentially comprises the following steps:
(1) adding an analytic solvent into the chromatographic column to ensure that the analytic solvent completely submerges silica gel particles in the chromatographic column;
(2) adding a certain volume of sclareol mother liquor into a chromatographic column at normal temperature and normal pressure;
(3) continuously adding an analytic solvent into a chromatographic column at normal temperature and normal pressure, and eluting sclareol mother liquor in the chromatographic column;
(4) collecting the mixed solution of the vegetable wax and the resolving solvent at the outlet of the chromatographic column into a distillation still of the vegetable wax and the resolving solvent;
(5) collecting the mixed solution of sclareol and the resolving solvent at the outlet of the chromatographic column into a distillation still of the sclareol and the resolving solvent;
(6) respectively carrying out distillation concentration on the mixed solution in the two distillation kettles;
the resolving solvent is a mixed solution of No. 120 solvent oil, petroleum ether and acetone, and the ratio of the No. 120 solvent oil to the petroleum ether to the acetone is 3:1: 1; when the mixed solution of sclareol and the desolvation solvent is recovered in the step (5), whether the mixed solution at the outlet of the chromatographic column contains sclareol or not is detected, and if the mixed solution at the outlet of the chromatographic column contains sclareol, the mixed solution of sclareol and the desolvation solvent is collected.
Further, the aspect ratio of the chromatographic column is 13: 1.
Further, the resolving solvent obtained after distillation and concentration in the step (6) is recycled and reused by a condenser, and the two distillation kettles respectively obtain vegetable wax raffinate and 90% sclareol.
Compared with the prior art, the invention has the advantages that: the method can thoroughly separate the sclareol and the vegetable wax in the sclareol mother liquor, improve the yield of the sclareol in the processing process of the sclareol extract, and can recycle the resolving solvent in the separation process, thereby improving the production efficiency and saving the production cost.
Drawings
FIG. 1 is a cross-sectional view of a chromatography column.
FIG. 2 is a left side view of the chromatography column.
FIG. 3 is a schematic flow chart of the present invention.
FIG. 4 is a process flow diagram of the present invention.
Detailed Description
The invention will be described more fully and clearly in connection with the following examples of the invention.
Example 1:
as shown in FIGS. 3 and 4, a method for separating sclareol from sclareol mother liquor comprises feeding a resolving solvent from a kettle 9 containing the resolving solvent to a chromatographic column 5 filled with 800 mesh silica gel particles by a pump until the resolving solvent completely submerges the silica gel particles in the chromatographic column 5, feeding 10kg of sclareol mother liquor to the chromatographic column 5, continuously feeding the resolving solvent from the kettle 9 containing the resolving solvent to the chromatographic column by a pump to elute the sclareol mother liquor from the chromatographic column 5, wherein the plant wax is eluted first because the adsorption of the plant wax is weak and the adsorption of the sclareol mother liquor in the chromatographic column 5 is strong, and at this time, it is required to detect whether the mixed solution at the outlet of the chromatographic column 5 contains the plant wax, and if the plant wax is contained, a first valve 10 is opened, and at this time, the mixed solution of the plant wax and the resolving solvent flows into a first distillation kettle 7 for collecting the mixed solution of the plant wax and the resolving solvent, finally, the mixed solution at the outlet of the chromatographic column is detected in real time according to experience, if the mixed solution containing sclareol is detected, the second valve 11 is opened, the mixed solution of sclareol and a desolvation solvent flows into the second distillation kettle 6 for collecting the mixed solution of sclareol and the desolvation solvent, then the mixed solution in the first distillation kettle 7 and the second distillation kettle 6 is distilled and concentrated respectively, the resolution solvent obtained after distillation and concentration is recycled into the kettle 9 containing the resolution solvent through the first condenser 8 and the second condenser 12 for reuse, and the first distillation kettle 7 and the second distillation kettle 6 respectively obtain plant wax residual liquid and 2kg of products containing 90% of sclareol.
Example 2:
as shown in fig. 1 and fig. 2, the chromatographic column comprises a column body 1 and silica gel particles 2, the silica gel particles 2 are filled in the column body 1, when the sclareol mother liquor is eluted, firstly, the analytical solvent completely submerges silica gel particles in the chromatographic column, then the sclareol mother liquor is added from a liquid inlet 4 of the chromatographic column, because the adsorption capacity of the silica gel particles 2 to the plant wax in the sclareol mother liquor is weaker, when the resolving solvent is continuously added into the chromatographic column, sclareol mother liquor is eluted, and the plant wax is eluted firstly because the adsorption capacity of the silica gel particles to the plant wax is relatively weak, because the silica gel particles have stronger adsorption capacity to the sclareol, the time for the sclareol to be eluted is longer, and adjusting the flow divider of the liquid outlet 3 of the chromatographic column according to the elution sequence to collect the mixed solution of the liquid outlet 3 of the chromatographic column into the corresponding container.
The invention has the advantages that: the method can thoroughly separate the sclareol and the vegetable wax in the sclareol mother liquor, improve the yield of the sclareol in the processing process of the sclareol extract, and can recycle the resolving solvent in the separation process, thereby improving the production efficiency and saving the production cost.
Claims (2)
1. A method for separating sclareol from sclareol mother liquor sequentially comprises the following steps:
(1) adding an analytic solvent into the chromatographic column to ensure that the analytic solvent completely submerges silica gel particles in the chromatographic column;
(2) adding a certain volume of sclareol mother liquor into a chromatographic column at normal temperature and normal pressure;
(3) continuously adding an analytic solvent into the chromatographic column at normal temperature and normal pressure, and eluting the sclarema aromatica mother liquor in the chromatographic column;
(4) collecting the mixed solution of the vegetable wax and the resolving solvent at the outlet of the chromatographic column into a distillation still of the vegetable wax and the resolving solvent;
(5) collecting the mixed solution of sclareol and the resolving solvent at the outlet of the chromatographic column into a distillation still of the sclareol and the resolving solvent;
(6) respectively carrying out distillation concentration on the mixed solution in the two distillation kettles;
the method is characterized in that: the resolving solvent is a mixed solution of No. 120 solvent oil, petroleum ether and acetone, and the ratio of the No. 120 solvent oil to the petroleum ether to the acetone is 3:1: 1; when the mixed solution of sclareol and the desolvation solvent is recovered in the step (5), whether the mixed solution at the outlet of the chromatographic column contains sclareol needs to be detected, and if the mixed solution at the outlet of the chromatographic column contains sclareol, the mixed solution of sclareol and the desolvation solvent starts to be collected; the length-diameter ratio of the chromatographic column is 13: 1.
2. The method of claim 1, wherein the sclareol is isolated from a sclareol mother liquor by: and (4) recovering the resolving solvent obtained after distillation and concentration in the step (6) through a condenser for reuse, and respectively obtaining vegetable wax residual liquid and 90% sclareol in two distillation kettles.
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 CN106854138A (en) | 2017-06-16 |
| CN106854138B true 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) |
Families Citing this family (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 |
|---|
| 层析法分离回收香紫苏内酯;周敏;《万方学位论文库硕士学位论文》;20101231;全文 * |
| 米团花的化学成分研究;蒲湘渝;《云南植物研究》;19891231(第3期);263-266 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106854138A (en) | 2017-06-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100384797C (en) | Method for extracting high-purity solanesol | |
| EP0187883A1 (en) | Acidulation and recovery of crude tall oil from tall oil soaps | |
| CN105367370B (en) | A kind of method that squalene is extracted in heel after the natural VE from extraction | |
| CN110041303B (en) | Process for extracting neophytadiene, carotenoid and nicotine from waste tobacco leaf | |
| CN105016956A (en) | Squalene extracting method | |
| CN107778277B (en) | Process for the recovery of squalene, vitamin E and/or sterols | |
| CN107473967A (en) | A kind of method that ion liquid abstraction rectifying removes acid and water simultaneously | |
| WO2008071985A3 (en) | Extraction process and purification process | |
| CN106854138B (en) | Method for separating sclareol from sclareol mother liquor | |
| CN105315704A (en) | Method for recovering organic acid from waste liquid produced after pigment is extracted from roselle | |
| CN106349324A (en) | Method for extracting and separating maslinic acid from olive leaves | |
| CN107089750A (en) | A kind of processing method containing high-concentration phenolic wastewater | |
| CN108047016B (en) | Method for extracting bisdemethoxycurcumin from turmeric | |
| CN105385716B (en) | A kind of method that sulfur-containing compound in garlic is separated using countercurrent chromatography | |
| CN105061250A (en) | Method for extracting oxytetracycline from oxytetracycline mother liquor | |
| CN1712392A (en) | Extraction of solanesol from potato leaves | |
| CN113336755B (en) | Method for separating and purifying trigonelline, chlorogenic acid and caffeine | |
| CN105503981A (en) | Method for extracting and separating anthocyanin from red cabbage | |
| CN108484603A (en) | The method that tabersonine is extracted from African Voacanga | |
| Prapakornwiriya et al. | Recovery of sinapic acid from the waste effluent of mustard protein isolation by ion exchange chromatography | |
| CN110746473B (en) | Purification process for reducing content of lincomycin B component | |
| CN104187536A (en) | Method for extracting and purifying capsaicin compound from chilli extract | |
| CN112939744A (en) | Efficient extraction method of cannabidiol | |
| CN103951560B (en) | A kind of method of preparative chromatography purifying alpha-linolenic acid ethyl ester | |
| CN104528861A (en) | Method for extraction dephenolization of phenol-containing wastewater through mixing settling |
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 |