CN106554252A - A kind of method that high-purity 2 phenylethyl alcohol is extracted from roseleaf - Google Patents
A kind of method that high-purity 2 phenylethyl alcohol is extracted from roseleaf Download PDFInfo
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- CN106554252A CN106554252A CN201510625623.2A CN201510625623A CN106554252A CN 106554252 A CN106554252 A CN 106554252A CN 201510625623 A CN201510625623 A CN 201510625623A CN 106554252 A CN106554252 A CN 106554252A
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- roseleaf
- phenylethyl alcohol
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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
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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
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
-
- 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
- C07C29/86—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by liquid-liquid treatment
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses the step such as a kind of method that high-purity 2 phenylethyl alcohol is extracted from roseleaf, the cleaning of the method roseleaf, the distillation of 2 phenylethyl alcohol, the extraction of 2 phenylethyl alcohol and rectification of 2 phenylethyl alcohol, obtains 2 phenylethyl alcohol of the purity higher than 99.9.The present invention extracts the 2 phenylethyl alcohol of high-purity and safety from natural material, can apply to cosmetics, medicine and other fields, and market prospect is good, and easy to operate, low manufacturing cost of the invention, is adapted to large-scale production.
Description
Technical field
The invention belongs to technical field of fine, is related to a kind of method that high-purity 2 phenylethyl alcohol is extracted from roseleaf.
Background technology
2 phenylethyl alcohol (
2-phenylethanol) it is a kind of aromatic alcohol with rose local flavor, it is present in the various plants quintessence oil such as Flos Rosae Rugosae, jasmine, and the natural flavor material of various fermented foods such as wine, yellow wine, medicated beer, bread, it is a key factor for determining fermented food quality.The fragrance of 2 phenylethyl alcohol is quite popular to people, is the main flow style of international essence and flavoring agent, is widely used in the field such as food and cosmetics of everyday use, and its usage amount is only second to vanillin, is second largest fragrance component.Additionally, 2 phenylethyl alcohol also has important application in pharmaceuticals industry as antibacterial and angiotensin-convertion enzyme inhibitor., more than 1000 dollars/kilogram, supply falls short of demand for the market price of natural 2-benzyl carbinol.
Industrial production 2 phenylethyl alcohol has chemical method and natural method.Chemical synthesiss are to synthesize 2 phenylethyl alcohol by raw material through chemical reaction of benzene or styrene, and not only raw material has in carcinogenic risk, and product and to be often difficult to the by-product that removes containing some, has had a strong impact on product quality, strongly limit the use range of product.Natural method production 2 phenylethyl alcohol includes using physical method two kinds of approach of extracting directly and Production by Microorganism Fermentation from natural material, and natural prodcuts purity is high, nontoxic, and with good biological safety, therefore market demand is increasing.But traditionally from the natural materials such as Flos Rosae Rugosae, jasmine, extraction 2 phenylethyl alcohol high cost, purity are low, it is difficult to meet the market demand.
The content of the invention
It is an object of the invention to provide a kind of method that high-purity 2 phenylethyl alcohol is extracted from roseleaf.
In order to realize the purpose of the present invention, the present invention is implemented by below scheme:
A kind of method that high-purity 2 phenylethyl alcohol is extracted from roseleaf, comprises the following steps：
（1）Cleaning：Fresh roseleaf is chosen, is cleaned with clean water, is put into after chopping in condensing distillator；
（2）Distillation：The 2-8% sodium salt solutions of 50-100 times of roseleaf weight are added toward condensing distillator, sodium salt solution is heated to and is seethed with excitement and kept for 30-90 minutes, while being passed through condensed water, collect distillate；
（3）Extraction：Distillate is added into separatory funnel, while adding organic extractant, vibration mixes 3-10 minutes, organic faciess is isolated after standing 5-15 minutes；
（4）Rectification：The organic faciess being obtained by extraction are put in precise distillation tower, vacuum precision is distilled off the impurity in organic faciess, purity is obtained higher than 99.9
The 2 phenylethyl alcohol of %.
Preferably, the sodium salt solution be Sodium Chloride, sodium acetate, sodium carbonate, one or more in sodium sulfate.
Preferably, 1-3 times for distillate volume of the volume of the organic extractant.
Preferably, the organic extractant is ethyl acetate, petroleum ether, dichloromethane, normal hexane, any one in normal heptane.
Preferably, the precise distillation tower is filled with high efficiency separation filler.
Preferably, the high efficiency separation filler is metal plate ripple arranged packing, metal gauze structured packing, grid packing, any one in Impulse packing.
Preferably, the vacuum precision distillation is continuous still.
It is an advantage of the invention that：
（1）The purity of the 2 phenylethyl alcohol that the present invention is extracted is higher than 99.9%, best in quality.
（2）It is Nantural non-toxic product that the present invention prepares highly purified 2 phenylethyl alcohol, can apply to cosmetics, medicine and other fields, and market prospect is good.
（3）Solution reagent used by of the invention can reclaim reuse, not produce discarded waste liquid.
（4）Easy to operate, low manufacturing cost of the invention, is adapted to large-scale production.
Specific embodiment
Technical scheme is described in further detail with reference to specific embodiment, but embodiments of the present invention not limited to this.
Embodiment
1
A kind of method that high-purity 2 phenylethyl alcohol is extracted from roseleaf, comprises the following steps：
（1）Cleaning：Fresh roseleaf is chosen, is cleaned with clean water, is put into after chopping in condensing distillator；
（2）Distillation：3% sodium carbonate liquor of 75 times of roseleaf weight is added toward condensing distillator, sodium salt solution is heated to and is seethed with excitement and kept for 45 minutes, while being passed through condensed water, collect distillate；
（3）Extraction：Distillate is added into separatory funnel, while adding the ethyl acetate of 2 times of distillate volumes, vibration is mixed 5 minutes, organic faciess is isolated after standing 10 minutes.
（4）Rectification：The organic faciess being obtained by extraction are put in the precise distillation tower equipped with Impulse packing, continuous vacuum precise distillation removes the impurity in organic faciess, obtain 2 phenylethyl alcohol of the purity higher than 99.90%.
Embodiment
2
（1）Cleaning：Fresh roseleaf is chosen, is cleaned with clean water, is put into after chopping in condensing distillator；
（2）Distillation：8% sodium chloride solution of 50 times of roseleaf weight is added toward condensing distillator, sodium salt solution is heated to and is seethed with excitement and kept for 30 minutes, while being passed through condensed water, collect distillate；
（3）Extraction：Distillate is added into separatory funnel, while adding the dichloromethane of 3 times of distillate volumes, vibration is mixed 3 minutes, organic faciess is isolated after standing 15 minutes.
（4）Rectification：The organic faciess being obtained by extraction are put in the precise distillation tower equipped with metal plate ripple arranged packing, continuous vacuum precise distillation removes the impurity in organic faciess, purity is obtained higher than 99.91
The 2 phenylethyl alcohol of %.
Embodiment
3
（1）Cleaning：Fresh roseleaf is chosen, is cleaned with clean water, is put into after chopping in condensing distillator；
（2）Distillation：2% sodium acetate solution of 100 times of roseleaf weight is added toward condensing distillator, sodium salt solution is heated to and is seethed with excitement and kept for 90 minutes, while being passed through condensed water, collect distillate；
（3）Extraction：Distillate is added into separatory funnel, while adding the petroleum ether of 1 times of distillate volume, vibration is mixed 10 minutes, organic faciess is isolated after standing 5 minutes.
（4）Rectification：The organic faciess being obtained by extraction are put in the precise distillation tower equipped with metal gauze structured packing, continuous vacuum precise distillation removes the impurity in organic faciess, purity is obtained higher than 99.93
The 2 phenylethyl alcohol of %.
Embodiment
4
（1）Cleaning：Fresh roseleaf is chosen, is cleaned with clean water, is put into after chopping in condensing distillator；
（2）Distillation：5% metabisulfite solution of 80 times of roseleaf weight is added toward condensing distillator, sodium salt solution is heated to and is seethed with excitement and kept for 60 minutes, while being passed through condensed water, collect distillate；
（3）Extraction：Distillate is added into separatory funnel, while adding the normal hexane of 2.5 times of distillate volumes, vibration mixes 3-10 minutes, organic faciess is isolated after standing 5-15 minutes.
（4）Rectification：The organic faciess being obtained by extraction are put in the precise distillation tower equipped with grid packing, continuous vacuum precise distillation removes the impurity in organic faciess, purity is obtained higher than 99.92
The 2 phenylethyl alcohol of %.
Embodiment
5
（1）Cleaning：Fresh roseleaf is chosen, is cleaned with clean water, is put into after chopping in condensing distillator；
（2）Distillation：Toward condensing distillator, 4% Sodium Chloride of 60 times of roseleaf weight of addition, sodium carbonate, sodium sulfate mixed solution, are heated to sodium salt solution and seethe with excitement and kept for 75 minutes, while being passed through condensed water, collect distillate；
（3）Extraction：Distillate is added into separatory funnel, while adding the normal heptane of 3 times of distillate volumes, vibration is mixed 8 minutes, organic faciess is isolated after standing 8 minutes.
（4）Rectification：The organic faciess being obtained by extraction are put in the precise distillation tower equipped with Impulse packing, continuous vacuum precise distillation removes the impurity in organic faciess, purity is obtained higher than 99.93
The 2 phenylethyl alcohol of %.
Claims (7)
1. it is a kind of from roseleaf extract high-purity 2 phenylethyl alcohol method, it is characterised in that comprise the following steps：
（1）Cleaning：Fresh roseleaf is chosen, is cleaned with clean water, is put into after chopping in condensing distillator；
（2）Distillation：The 2-8% sodium salt solutions of 50-100 times of roseleaf weight are added toward condensing distillator, sodium salt solution is heated to and is seethed with excitement and kept for 30-90 minutes, while being passed through condensed water, collect distillate；
（3）Extraction：Distillate is added into separatory funnel, while adding organic extractant, vibration mixes 3-10 minutes, organic faciess is isolated after standing 5-15 minutes；
（4）Rectification：The organic faciess being obtained by extraction are put in precise distillation tower, vacuum precision is distilled off the impurity in organic faciess, obtain 2 phenylethyl alcohol of the purity higher than 99.9 %.
2. the method that high-purity 2 phenylethyl alcohol is extracted from roseleaf according to claim 1, it is characterised in that the sodium salt solution be Sodium Chloride, sodium acetate, sodium carbonate, one or more in sodium sulfate.
3. the method that high-purity 2 phenylethyl alcohol is extracted from roseleaf according to claim 1, it is characterised in that the volume of the organic extractant is 1-3 times of distillate volume.
4. the method that high-purity 2 phenylethyl alcohol is extracted from roseleaf according to claim 3, it is characterised in that the organic extractant is ethyl acetate, petroleum ether, dichloromethane, normal hexane, any one in normal heptane.
5. it is according to claim 1 from roseleaf extract high-purity 2 phenylethyl alcohol method, it is characterised in that the precise distillation tower is filled with high efficiency separation filler.
6. the method that high-purity 2 phenylethyl alcohol is extracted from roseleaf according to claim 5, it is characterised in that the high efficiency separation filler is metal plate ripple arranged packing, metal gauze structured packing, grid packing, any one in Impulse packing.
7. the method that high-purity 2 phenylethyl alcohol is extracted from roseleaf according to claim 5, it is characterised in that vacuum precision distillation is continuous still.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510625623.2A CN106554252A (en) | 2015-09-28 | 2015-09-28 | A kind of method that high-purity 2 phenylethyl alcohol is extracted from roseleaf |
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| CN201510625623.2A CN106554252A (en) | 2015-09-28 | 2015-09-28 | A kind of method that high-purity 2 phenylethyl alcohol is extracted from roseleaf |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110028384A (en) * | 2019-03-15 | 2019-07-19 | 江西省科学院微生物研究所 | A method of molecular distillation separation prepares 2 phenylethyl alcohol from bioconversion broth |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101691522A (en) * | 2009-09-30 | 2010-04-07 | 云南省农业科学院药用植物研究所 | Method for extracting rose damascana and rose flower water from roses |
| CN103610192A (en) * | 2013-10-12 | 2014-03-05 | 浙江工商大学 | Rose function beverage and preparation method thereof |
| CN103642592A (en) * | 2013-11-01 | 2014-03-19 | 西安银能科技发展有限责任公司 | Full utilization technology of rose flower |
| CN104498539A (en) * | 2014-11-19 | 2015-04-08 | 上海应用技术学院 | Method for preparing 2-phenylethyl alcohol |
-
2015
- 2015-09-28 CN CN201510625623.2A patent/CN106554252A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101691522A (en) * | 2009-09-30 | 2010-04-07 | 云南省农业科学院药用植物研究所 | Method for extracting rose damascana and rose flower water from roses |
| CN103610192A (en) * | 2013-10-12 | 2014-03-05 | 浙江工商大学 | Rose function beverage and preparation method thereof |
| CN103642592A (en) * | 2013-11-01 | 2014-03-19 | 西安银能科技发展有限责任公司 | Full utilization technology of rose flower |
| CN104498539A (en) * | 2014-11-19 | 2015-04-08 | 上海应用技术学院 | Method for preparing 2-phenylethyl alcohol |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110028384A (en) * | 2019-03-15 | 2019-07-19 | 江西省科学院微生物研究所 | A method of molecular distillation separation prepares 2 phenylethyl alcohol from bioconversion broth |
| CN110028384B (en) * | 2019-03-15 | 2020-06-26 | 江西省科学院微生物研究所 | Method for preparing 2-phenethyl alcohol from biotransformation liquid by molecular distillation and separation |
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Application publication date: 20170405 |