CN101191103A - Method for extracting pine needle essential oil from pine needle - Google Patents
Method for extracting pine needle essential oil from pine needle Download PDFInfo
- Publication number
- CN101191103A CN101191103A CNA2007101686935A CN200710168693A CN101191103A CN 101191103 A CN101191103 A CN 101191103A CN A2007101686935 A CNA2007101686935 A CN A2007101686935A CN 200710168693 A CN200710168693 A CN 200710168693A CN 101191103 A CN101191103 A CN 101191103A
- Authority
- CN
- China
- Prior art keywords
- pine needle
- essential oil
- ionic liquid
- pine
- extracting
- 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
Landscapes
- Cosmetics (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention relates to a method for extracting pine needle essential oil from pine needles. The difference is that: at first, the shade-dried pine needles are crushed and are passed through a 40-mesh sieve, then the hydrophilic ionic liquid is added, the mass-volume ratio of the pine needles and the ionic liquid is 1:2-20 (g: ml), the microwave is adopted to heat the pine needles for complete dissolving, the microwave frequency is 2450MHz, then the conventional steam distillation is adopted to extract the pine needle essential oil, the heating temperature of the microwave is between 80 and 120 DEG C, the hydrophilic ionic liquid is any one of [BMIM]AcO, [BMIM]Cl or[AMIM]Cl. The invention has the advantages that: 1) the preparation method is simple, the obtained pine needle essential oil has good quality and higher yield, the yield is increased by 30 to 49 percent or so compared with that of directly adopting the steam distillation; 2) the hydrophilic ionic liquid can be reclaimed and recycled by adopting the ion exchange method, which can not cause the environmental pollution.
Description
Technical field
The present invention relates to a kind of method of from pine needle, extracting the pine needle essential oil.
Background technology
China is pine tree big country, and pine tree occupies very important position in the forest reserves of China, and for a long time, the pine needle resource fails to obtain good development and utilization, and extracting the pine needle essential oil by pine needle is a kind of effective way of pine needle recycling.The pine needle essential oil is a kind of lurid oily liquids with happy fragrance, its chemical ingredients more complicated, mainly comprise terpene alcohol, terpenes, ether, ketone, phenol, phenol fat etc., be widely used in perfume cosmetic industry, spraying essence, perfumed soap, toothpaste, pharmacy and foodstuffs industry.Extract the pine needle essential oil by pine needle at present and mainly adopt steam distillation, organic solvent extractionprocess and supercritical extraction, wherein steam distillation is most widely used, and it is good to obtain pine needle essential oil quality, but yield is lower.
Hydrophilic ionic liquid is a kind of organic liquid material of at room temperature being made up of ion fully, than organic solvent commonly used, because it is non-volatile, can recycle, and is considered to green solvent.Do not see at present that hydrophilic ionic liquid is used for being extracted by pine needle the report of pine needle essential oil.
Summary of the invention
Problem to be solved by this invention is to propose a kind of method of extracting the pine needle essential oil from pine needle at above-mentioned prior art, and pine needle essential oil quality obtained by this method is good, and the essential oil productive rate is significantly improved.
The present invention for the solution that problem adopts of the above-mentioned proposition of solution is: a kind of method of extracting the pine needle essential oil from pine needle, its difference is that the pine needle that at first will dry in the shade pulverizes, pulverize the back and cross 40 mesh sieves, then to wherein adding hydrophilic ionic liquid, described pine needle and hydrophilic ion liquid mass volume ratio are 1: 2-20 (g: ml), adopt microwave heating to pine needle to dissolve fully again, described microwave frequency 2450MHz adopts conventional steam distillation to extract then and obtains the pine needle essential oil.
Press such scheme, described microwave heating temperature is 80～120 ℃.
Press such scheme, described hydrophilic ionic liquid is [BMIM] AcO, any one among [BMIM] Cl or [AMIM] Cl.
Advantage of the present invention:
1) preparation method is simple, and it is good to obtain pine needle essential oil quality, and yield is higher, and is higher by about 30～49% than the productive rate of direct employing steam distillation;
2) adopt hydrophilic ionic liquid can adopt the ion exchange method recycling use, can not cause environmental pollution substantially.
Embodiment
Embodiment 1:
The pine needle that 20g dries in the shade is pulverized, pulverize the back and cross 40 mesh sieves, then to wherein adding the hydrophilic ionic liquid of 100ml [BMIM] AcO, adopt microwave heating (Heating temperature is 120 ℃) to pine needle to dissolve fully again, described microwave frequency 2450MHz, adopting conventional steam distillation to extract then and obtaining lurid oily liquids is pine needle essential oil 102mg, and adopt conventional steam distillation to get lurid oily liquids 68.5mg, productive rate improves 48.9%, both relative densities, refractive index is consistent with the UV absorption peak.
Embodiment 2:
The pine needle that 20g dries in the shade is pulverized, pulverize the back and cross 40 mesh sieves, then to wherein adding the hydrophilic ionic liquid of 150ml [BMIM] Cl, adopt microwave heating (Heating temperature is 100 ℃) to pine needle to dissolve fully again, described microwave frequency 2450MHz, adopting conventional steam distillation to extract then and obtaining lurid oily liquids is pine needle essential oil 90mg, and adopt conventional steam distillation to get lurid oily liquids 68.5mg, productive rate improves 31.4%, both relative densities, refractive index is consistent with the UV absorption peak.
Embodiment 3:
The pine needle that 20g dries in the shade is pulverized, pulverize the back and cross 40 mesh sieves, then to wherein adding the hydrophilic ionic liquid of 120ml [AMIM] Cl, adopt microwave heating (Heating temperature is 80 ℃) to pine needle to dissolve fully again, described microwave frequency 2450MHz, adopting conventional steam distillation to extract then and obtaining lurid oily liquids is pine needle essential oil 92mg, and adopt conventional steam distillation to get lurid oily liquids 68.5mg, productive rate improves 34.3%, both relative densities, refractive index is consistent with the UV absorption peak.
Embodiment 4:
The pine needle that 20g dries in the shade is pulverized, pulverize the back and cross 40 mesh sieves, then to wherein adding the hydrophilic ionic liquid of 100ml [BMIM] AcO, adopt microwave heating (Heating temperature is 80 ℃) to pine needle to dissolve fully again, described microwave frequency 2450MHz, adopting conventional steam distillation to extract then and obtaining lurid oily liquids is pine needle essential oil 98mg, and adopt conventional steam distillation to get lurid oily liquids 68.5mg, productive rate improves 43.1%, both relative densities, refractive index is consistent with the UV absorption peak.
Embodiment 5:
The pine needle that 20g dries in the shade is pulverized, pulverize the back and cross 40 mesh sieves, then to wherein adding the hydrophilic ionic liquid of 40ml [BMIM] Cl, adopt microwave heating (Heating temperature is 105 ℃) to pine needle to dissolve fully again, described microwave frequency 2450MHz, adopting conventional steam distillation to extract then and obtaining lurid oily liquids is pine needle essential oil 96mg, and adopt conventional steam distillation to get lurid oily liquids 68.5mg, productive rate improves 40.1%, both relative densities, refractive index is consistent with the UV absorption peak.
Embodiment 6:
The pine needle that 20g dries in the shade is pulverized, pulverize the back and cross 40 mesh sieves, then to wherein adding the hydrophilic ionic liquid of 400ml [BMIM] AcO, adopt microwave heating (Heating temperature is 100 ℃) to pine needle to dissolve fully again, described microwave frequency 2450MHz, adopting conventional steam distillation to extract then and obtaining lurid oily liquids is pine needle essential oil 99mg, and adopt conventional steam distillation to get lurid oily liquids 68.5mg, productive rate improves 44.5%, both relative densities, refractive index is consistent with the UV absorption peak.
The hydrophilic ionic liquid that the foregoing description 1-6 is adopted all adopts industry or laboratory chemical reagent, and its weight percent concentration is more than 95%.
Claims (3)
1. method of from pine needle, extracting the pine needle essential oil, it is characterized in that the pine needle that at first will dry in the shade pulverizes, pulverize the back and cross 40 mesh sieves, then to wherein adding hydrophilic ionic liquid, described pine needle and hydrophilic ion liquid mass volume ratio are 1: 2-20 (g: ml), adopt microwave heating to pine needle to dissolve fully again, described microwave frequency 2450MHz adopts conventional steam distillation to extract then and obtains the pine needle essential oil.
2. by the described method of from pine needle, extracting the pine needle essential oil of claim 1, it is characterized in that described microwave heating temperature is 80～120 ℃.
3. by claim 1 or the 2 described methods of from pine needle, extracting the pine needle essential oil, it is characterized in that described hydrophilic ionic liquid is [BMIM] AcO, any one among [BMIM] Cl or [AMIM] Cl.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101686935A CN101191103B (en) | 2007-12-10 | 2007-12-10 | Method for extracting pine needle essential oil from pine needle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101686935A CN101191103B (en) | 2007-12-10 | 2007-12-10 | Method for extracting pine needle essential oil from pine needle |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101191103A true CN101191103A (en) | 2008-06-04 |
| CN101191103B CN101191103B (en) | 2012-01-11 |
Family
ID=39486305
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2007101686935A Expired - Fee Related CN101191103B (en) | 2007-12-10 | 2007-12-10 | Method for extracting pine needle essential oil from pine needle |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101191103B (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880597A (en) * | 2010-07-08 | 2010-11-10 | 河北科技大学 | Method for extracting rice bran oil by using ionic liquid and supercritical carbon dioxide (CO2) |
| CN101411468B (en) * | 2008-12-01 | 2012-07-04 | 浙江师范大学 | Pine needle extract of slash pine and use thereof in food fresh keeping |
| CN103215120A (en) * | 2013-05-09 | 2013-07-24 | 刘映良 | Extracting process of pine needle volatile oil of masson pine by steam distillation method |
| CN103725418A (en) * | 2013-12-20 | 2014-04-16 | 茂名市德威圣科技有限责任公司 | Method for extracting jack fruit aromatherapy oil from ionic liquid |
| US8791282B2 (en) | 2011-06-28 | 2014-07-29 | Givudan S.A. | Ionic liquids for agricultural residue removal |
| CN104232311A (en) * | 2014-09-02 | 2014-12-24 | 华南理工大学 | Extraction method of ginger essential oil |
| CN104490947A (en) * | 2014-12-12 | 2015-04-08 | 广西科技大学 | Application of pinus crassicorticea pine needle essential oil |
| CN108851195A (en) * | 2018-07-26 | 2018-11-23 | 湖北中烟工业有限责任公司 | A kind of preparation method of cigarette alfalfa extract |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1510119A (en) * | 2002-09-14 | 2004-07-07 | 白山市科学技术研究所 | Firconcrete, extrait, essential oil and preparing method thereof |
-
2007
- 2007-12-10 CN CN2007101686935A patent/CN101191103B/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101411468B (en) * | 2008-12-01 | 2012-07-04 | 浙江师范大学 | Pine needle extract of slash pine and use thereof in food fresh keeping |
| CN101880597A (en) * | 2010-07-08 | 2010-11-10 | 河北科技大学 | Method for extracting rice bran oil by using ionic liquid and supercritical carbon dioxide (CO2) |
| US8791282B2 (en) | 2011-06-28 | 2014-07-29 | Givudan S.A. | Ionic liquids for agricultural residue removal |
| CN103215120A (en) * | 2013-05-09 | 2013-07-24 | 刘映良 | Extracting process of pine needle volatile oil of masson pine by steam distillation method |
| CN103725418A (en) * | 2013-12-20 | 2014-04-16 | 茂名市德威圣科技有限责任公司 | Method for extracting jack fruit aromatherapy oil from ionic liquid |
| CN104232311A (en) * | 2014-09-02 | 2014-12-24 | 华南理工大学 | Extraction method of ginger essential oil |
| CN104232311B (en) * | 2014-09-02 | 2016-09-21 | 华南理工大学 | A kind of extracting method of ginger essential oil |
| CN104490947A (en) * | 2014-12-12 | 2015-04-08 | 广西科技大学 | Application of pinus crassicorticea pine needle essential oil |
| CN108851195A (en) * | 2018-07-26 | 2018-11-23 | 湖北中烟工业有限责任公司 | A kind of preparation method of cigarette alfalfa extract |
| CN108851195B (en) * | 2018-07-26 | 2021-05-18 | 湖北中烟工业有限责任公司 | Preparation method of alfalfa refined extract for cigarettes |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101191103B (en) | 2012-01-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101191103B (en) | Method for extracting pine needle essential oil from pine needle | |
| CN101195789B (en) | Method for extracting pomelo ped essential oil from pomelo ped | |
| New et al. | Potential use of pure and diluted choline chloride-based deep eutectic solvent in delignification of oil palm fronds | |
| Brahim et al. | Optimization of polyphenols extraction from grape residues in water medium | |
| CN105754114B (en) | A kind of method of eutectic ionic liquid separation and Extraction straw lignin | |
| Prado et al. | Effect of the photocatalytic activity of TiO2 on lignin depolymerization | |
| CN105802738B (en) | Extraction method of wild chrysanthemum flower volatile oil | |
| CN107602362A (en) | The method that molybdenum oxide catalyst Catalytic lignin prepares single phenols aromatic compound | |
| CN106366134A (en) | Process for separating product of mild acid-catalyzed depolymerization of lignin and extraction products thereof | |
| Mao et al. | Lignin recovery from cocoa bean shell using microwave-assisted extraction and deep eutectic solvents | |
| CN102659898A (en) | Microwave-assisted method for extracting tea saponin | |
| CN102839053B (en) | Method for extracting aurantiamarin from orange peel | |
| Roy et al. | Recent advances in lignin depolymerization techniques: A comparative overview of traditional and greener approaches | |
| CN106854264A (en) | A kind of rice husk sill quality modified phenolic resin adhesive preparation method | |
| CN108034499A (en) | A kind of method of fragrant camphor tree essential oil using ionic liquid as green medium Extraction and enrichment 1,8- Cineoles | |
| CN101177447A (en) | Novel technique for preparing tea saponin by solvent extraction and selectively separating integration | |
| Segneanu et al. | Biomass extraction methods | |
| Subbotina et al. | Pd/C-catalyzed hydrogenolysis of dibenzodioxocin lignin model compounds using silanes and water as hydrogen source | |
| Rishikesh et al. | A comprehensive review on lignin obtained from agro-residues: Potential source of useful chemicals | |
| CN106400564B (en) | A kind of method that lignin prepares high value added product and cellulose in direct oxidation wood powder | |
| Wang et al. | Tuning lignin properties by mild ionic-liquid-mediated selective alcohol incorporation | |
| WO2019120956A1 (en) | Ultra-fast lignin depolymerization process | |
| CN100575325C (en) | Cable type extractor according cycling extraction method is extracted the method for eggplant Buddhist nun alcohol in the biomass | |
| CN101205504B (en) | Method for extracting persimmon leaf essential oil from persimmon leaves | |
| CN106866382A (en) | The extracting method of aldehydes matter in a kind of catalytic lignin depolymerization product liquid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120111 Termination date: 20141210 |
|
| EXPY | Termination of patent right or utility model |