CN108947773A - A kind of preparation method of linalool - Google Patents
A kind of preparation method of linalool Download PDFInfo
- Publication number
- CN108947773A CN108947773A CN201710384691.3A CN201710384691A CN108947773A CN 108947773 A CN108947773 A CN 108947773A CN 201710384691 A CN201710384691 A CN 201710384691A CN 108947773 A CN108947773 A CN 108947773A
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- China
- Prior art keywords
- linalool
- preparation
- added
- extract
- temperature
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Classifications
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- 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
- C07C29/78—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by condensation or crystallisation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention discloses a kind of preparation methods of linalool.Preparation method is added in supercritical extraction reactor, under conditions of extracting pressure 5-15MPa, 60-80 DEG C of temperature, is passed through liquid CO the following steps are included: (1) takes rhizoma homalonemae pulverizing medicinal materials 40-60 mesh2Supercritical extract 3-5 hours, in pressure 15-20MPa, 60-70 DEG C of temperature parsing obtained extract；(2) above-mentioned extract is added in macroreticular resin and adsorbs, and the elution of 70% ethanol solution collects eluent concentration, obtains sediment；(3) above-mentioned sediment is recrystallized, and is drying to obtain linalool.Using preparation method of the present invention, technological operation is easy, yield is high, pollutes small, the production of suitable high-purity linalool.
Description
Technical field
The invention discloses the preparation method and application of a Plant Extracts, in particular to a kind of preparation side of linalool
Method.
Background technique
Linalool (Linalol), also known as linalool, coriandrol, coriandrol, Linalool, CAS 78-70-6, molecular formula
C10H18O, molecular weight 154.25, structural formula are
Linalool is derived from rhizoma homalonemae medicinal material.Linalool has a general character and feature of pure and mild alkenes compounds, such as can be with
It is esterified, dehydration, is easy to be reduced to corresponding hydrocarbon compound.In the presence of metallic sodium, dihydro laurel is generated
Alkene；When restoring on colloidal platinum or skeleton nickel, then dihydro linalool and tetrahydrolinalool are generated.Due to the active chemistry of linalool
Performance is applied on sweetening treatment, medicine, daily chemical industry extensively so the derivative of a multitude of names can be made.
Summary of the invention
To achieve the goals above, the invention adopts the following technical scheme:
The preparation method of linalool, which comprises the following steps:
(1) rhizoma homalonemae pulverizing medicinal materials 40-60 mesh is taken, is added in supercritical extraction reactor, in extracting pressure 5-15MPa, temperature 60-80
Under conditions of DEG C, it is passed through liquid CO2Supercritical extract 3-5 hours, in pressure 15-20MPa, 60-70 DEG C of temperature parsing must be extracted
Object；
(2) above-mentioned extract is added in macroreticular resin and adsorbs, and the elution of 70% ethanol solution collects eluent concentration, obtains sediment；
(3) above-mentioned sediment is recrystallized, and is drying to obtain linalool.
Macroreticular resin described in step (2) is one of HZ816 and HPD100.
Recrystallization solvent is 70% methanol in step (3).
Linalool is prepared using this law, simple process is easy to operate, and preparation amount is big, and product yield is high, and low pollution.
The present invention is further illustrated below in conjunction with specific embodiment, but the scope of protection of present invention is not limited to
In following embodiments.
Specific embodiment
Embodiment 1:
40 mesh of rhizoma homalonemae pulverizing medicinal materials is taken, is added in supercritical extraction reactor, under conditions of extracting pressure 5MPa, temperature 60 C,
It is passed through liquid CO2Supercritical extract 3 hours, in pressure 15MPa, temperature 60 C parsing obtained extract, and above-mentioned extract is added
It is adsorbed in macroreticular resin HZ816, eluent concentration is collected in the elution of 70% ethanol solution, obtains sediment, and above-mentioned sediment is added 70%
Methanol solution recrystallization, is drying to obtain linalool, and HPLC measures content.
Embodiment 2:
60 mesh of rhizoma homalonemae pulverizing medicinal materials is taken, is added in supercritical extraction reactor, under conditions of extracting pressure 15MPa, 80 DEG C of temperature,
It is passed through liquid CO2Supercritical extract 5 hours, in pressure 20MPa, temperature 70 C parsing obtained extract, and above-mentioned extract is added
It is adsorbed in macroreticular resin HPD100, eluent concentration is collected in the elution of 70% ethanol solution, obtains sediment, and above-mentioned sediment is added
70% methanol solution recrystallization, is drying to obtain linalool, and HPLC measures content.
Embodiment 3:
50 mesh of rhizoma homalonemae pulverizing medicinal materials is taken, is added in supercritical extraction reactor, under conditions of extracting pressure 10MPa, temperature 70 C,
It is passed through liquid CO2Supercritical extract 4 hours, in pressure 20MPa, temperature 60 C parsing obtained extract, and above-mentioned extract is added
It is adsorbed in macroreticular resin HZ816, eluent concentration is collected in the elution of 70% ethanol solution, obtains sediment, and above-mentioned sediment is added 70%
Methanol solution recrystallization, is drying to obtain linalool, and HPLC measures content.
Claims (3)
1. a kind of preparation method of linalool, it is characterised in that the following steps are included:
(1) rhizoma homalonemae pulverizing medicinal materials 40-60 mesh is taken, is added in supercritical extraction reactor, in extracting pressure 5-15MPa, temperature 60-80
Under conditions of DEG C, it is passed through liquid CO2Supercritical extract 3-5 hours, in pressure 15-20MPa, 60-70 DEG C of temperature parsing must be extracted
Object；
(2) above-mentioned extract is added in macroreticular resin and adsorbs, and the elution of 70% ethanol solution collects eluent concentration, obtains sediment；
(3) above-mentioned sediment is recrystallized, and is drying to obtain linalool.
2. the preparation method of linalool according to claim 1, it is characterised in that: macroreticular resin described in step (2)
For one of HZ816 and HPD100.
3. the preparation method of linalool according to claim 1, it is characterised in that: recrystallization solvent is 70% in step (3)
Methanol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710384691.3A CN108947773A (en) | 2017-05-26 | 2017-05-26 | A kind of preparation method of linalool |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710384691.3A CN108947773A (en) | 2017-05-26 | 2017-05-26 | A kind of preparation method of linalool |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108947773A true CN108947773A (en) | 2018-12-07 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710384691.3A Pending CN108947773A (en) | 2017-05-26 | 2017-05-26 | A kind of preparation method of linalool |
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| CN (1) | CN108947773A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111485422A (en) * | 2020-04-17 | 2020-08-04 | 苏州丝之源纺织科技有限公司 | Anti-mite antibacterial finishing agent and finishing method and application thereof |
-
2017
- 2017-05-26 CN CN201710384691.3A patent/CN108947773A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111485422A (en) * | 2020-04-17 | 2020-08-04 | 苏州丝之源纺织科技有限公司 | Anti-mite antibacterial finishing agent and finishing method and application thereof |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20181207 |