CN106929159A - A kind of extracting method of recovery rate tea tree ethereal oil high - Google Patents
A kind of extracting method of recovery rate tea tree ethereal oil high Download PDFInfo
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- CN106929159A CN106929159A CN201710310526.3A CN201710310526A CN106929159A CN 106929159 A CN106929159 A CN 106929159A CN 201710310526 A CN201710310526 A CN 201710310526A CN 106929159 A CN106929159 A CN 106929159A
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- tea
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- tea tree
- filter residue
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
Abstract
The invention discloses a kind of extracting method of recovery rate tea tree ethereal oil high, step is as follows：After tea free freeze-drying, crush, obtain tea leaf powder；By tea leaf powder heating and refluxing extraction twice, the total liquid of refluxing extraction and the second backflow filter residue are obtained；By tea tree branch seepage pressure effects, percolate is obtained；After by the tea tree branch freeze-drying after seepage pressure effects, crush, obtain tea branch powder；Second backflow filter residue and tea branch powder are merged, ultrasonic wave extraction, filtering obtains ultrasonic extract and ultrasonic wave filter residue；Ultrasonic wave filter residue is put into supercritical extraction reactor, supercritical extract is carried out, supercritical extract liquid is obtained；The total liquid of refluxing extraction, percolate, ultrasonic extract and supercritical extract liquid are merged, is added in alembic, concentration obtains concentrate；Concentrate is carried out into vacuum distillation, you can.The extracting method of the tea tree ethereal oil, recovery rate is high, and raw material effectively can be utilized, and improves productivity effect.
Description
Technical field
The present invention relates to plants essential oil extractive technique field, the extraction side of specifically a kind of recovery rate tea tree ethereal oil high
Method.
Background technology
Tea oil, also known as Australian gold, are famous magical skin treatment articles in the original inhabitants' legend of Australia.Botany
On be defined as titrol, the several plants of Myrtaceae cajeputtree tree are mainly derived from because of it, be to use narrow leaved tea tree
The fresh branches and leaves of tree are through essential oil obtained from steam distillation.Tea oil is a kind of colourless or light yellow liquid, with making us pleased
Fast cardamom smell.Exactly because tea oil complicated, and the influence of the maturity of climate, manufacturing process and raw material,
So the property of tea oil is not determined by certain discrete component, and depend on its uniqueness, exquisite mixing composition.Tea tree
Oil nature is gentle, and percutaneous permeability is good, does not stimulate skin, and toxicity is low.Research has shown that tea oil has disinfecting properties, can be effective
Ground suppresses the malignant bacteria and mould of many generally existings.
2002, Australian tea oil was successfully listed in European Pharmacopoeia.Tea oil is second quilt after eucalyptus oil
List the crude vegetal of European Pharmacopoeia in.In Australia, the tea oil of common retail in pharmacy and supermarket, its concentration is about
Be 15%, used directly as disinfectant for consumer, and most family also standing tea oil as first aid medicine.U.S. FDA is
Approval tea oil can be as the first aid medicine and health products for not needing prescription just to sell.In daily use chemicals industry, because it contains
The sterilization of various active composition and uniqueness, cleaning action, tea oil are widely used in personal care articles, such as cosmetics, toothpaste,
Perfumed soap, mousse, toner, shampoo, ISl are red, skin cream, shower cream etc., can also be applied to air freshener, household cleaning
Agent, bactericide, pet amenities etc..In medical industry, tea oil is important medicine chemical material, can efficiently kill skin
The fungi and bacterium on surface.Medically using quite extensively, having more than 100 kinds of first aid purposes.Tea oil can be used to treat flower
Spot, acne, tinea, refer to bacterium, gynecological infection, oral cavity pain, furuncle, corn, gingivitis, bleb, pernio, have a sore throat, insect bite, lice sting,
Knife wound, burn, scratch and other traumatic wounds etc..In food service industry, tea oil is used as food flavor and obtains the U.S. already
Approval, No. PEMA be 3902.Its bakery product, soft drink, alcoholic beverages, breakfast cereal, cheese, chewing gum, candy,
Egg products, fish product, grease, frozen dairy product, fruit product, instant coffee, tea, meat products, dairy products, nut product and grain
Food product etc..In fragrance industry, tea oil has warm pungent perfume (or spice), the fragrant terpene breath of band.In daily blending industry, it can be used
In men's pungent fragrant cologne, aftershave lotion etc..It is with lavandin oil, lavender oil, compounding acetic isoborneol ester, caryophyllus oil, rosemary
Oil, oak moss product, cananga oil, amyl salicylate, cumarin, geraniol and nerol etc. mix it is good, thus in blending
Using more convenient.
The tea oil of current China's production is mainly used in outlet, although some enterprises of the country also recognize the work of tea oil
With also having certain exploitation on product, but still be only confined to the aspects such as perfumed soap, bath foam, conditioning liquid, toothpaste, mildy wash.
Pharmaceuticals industry, food flavor industry are almost blank.As people are to the continuous of the composition of tea oil, characteristic and application study
Deeply, effect of the tea oil in medicine, daily use chemicals, food, fragrance industry also will increasingly be paid attention to, and novel product will be continuous
Emerge in large numbers, this certainly will promote the progress of tea tree planting and secondary industry.However, the extracting method generally existing of existing tea tree ethereal oil
The defect that recovery rate is low, product purity is low.
The content of the invention
It is an object of the invention to provide a kind of extracting method of recovery rate tea tree ethereal oil high, to solve above-mentioned background skill
The problem proposed in art.
To achieve the above object, the present invention provides following technical scheme：
A kind of extracting method of recovery rate tea tree ethereal oil high, step is as follows：
1) 2 are compared according to weight:1 weighs tea free and tea tree branch respectively, standby；
2) by after tea free freeze-drying, crush, cross 100-120 mesh sieves, obtain tea leaf powder；
3) tea leaf powder is put into container, adds the 12-15 times of ethanol water of weight, heating and refluxing extraction 1-2h, mistake
Filter, obtains the first reflux extracting liquid and the first backflow filter residue, and the first backflow filter residue is added into the 8-10 times of ethanol water of weight again
Solution, heating and refluxing extraction 40-50min, filtering obtains the second reflux extracting liquid and the second backflow filter residue, and the first backflow is carried
Take liquid and the second reflux extracting liquid merges, obtain the total liquid of refluxing extraction；
4) tea tree branch is put into percolator, using ethanol water as solvent, after extraction is finished, filtering obtains diacolation
Extract solution；
5) after by the tea tree branch freeze-drying after seepage pressure effects, crush, cross 50-80 mesh sieves, obtain tea branch powder；
6) the second backflow filter residue and tea branch powder are merged, adds the 10-12 times of ethanol water of weight, ultrasonic wave extraction
50-60min, filtering obtains ultrasonic extract and ultrasonic wave filter residue；
7) ultrasonic wave filter residue is put into supercritical extraction reactor, the carbon dioxide using absolute ethyl alcohol as entrainer is used as extraction
Fluid carries out supercritical extract, and extraction time is 1-2h, obtains supercritical extract liquid；
8) the total liquid of refluxing extraction, percolate, ultrasonic extract and supercritical extract liquid are merged, adds alembic
In, heating recovery solvent is concentrated into when vapor (steam) temperature is 42 DEG C and terminates, and obtains concentrate；
9) concentrate is carried out into vacuum distillation, you can.
As further scheme of the invention：Step 3) in, the ethanol volumetric concentration of ethanol water is 70%.
As further scheme of the invention：Step 4) in, the ethanol volumetric concentration of ethanol water is 85%.
As further scheme of the invention：Step 6) in, the ethanol volumetric concentration of ethanol water is 70%.
As further scheme of the invention：Step 7) in, the flow for extracting fluid is 18-20kg/h.
Compared with prior art, the beneficial effects of the invention are as follows：
The extracting method of tea tree ethereal oil of the present invention, can effectively extract the tea tree ethereal oil in tea free and tea tree branch, extract
Rate is high, and raw material effectively can be utilized, and improves productivity effect；The extracting method of tea tree ethereal oil of the present invention, is obtained
Tea tree ethereal oil purity is high, and moisture content is low, is conducive to preserving, with wide market prospects.
Specific embodiment
Technical scheme is described in more detail with reference to specific embodiment.
Embodiment 1
A kind of extracting method of recovery rate tea tree ethereal oil high, step is as follows：
1) 2 are compared according to weight:1 weighs tea free and tea tree branch respectively, standby；
2) by after tea free freeze-drying, crush, cross 100 mesh sieves, obtain tea leaf powder；
3) tea leaf powder is put into container, adds 12 times of ethanol waters of weight, heating and refluxing extraction 1h, filtering is obtained
The first reflux extracting liquid and the first backflow filter residue are obtained, the first backflow filter residue is added into 8 times of ethanol waters of weight again, heated
Refluxing extraction 40min, filtering obtains the second reflux extracting liquid and the second backflow filter residue, by the first reflux extracting liquid and second time
Stream extract solution merges, and obtains the total liquid of refluxing extraction, wherein, the ethanol volumetric concentration of ethanol water is 70%；
4) tea tree branch is put into percolator, using ethanol water as solvent, after extraction is finished, filtering obtains diacolation
Extract solution, wherein, the ethanol volumetric concentration of ethanol water is 85%；
5) after by the tea tree branch freeze-drying after seepage pressure effects, crush, cross 50 mesh sieves, obtain tea branch powder；
6) the second backflow filter residue and tea branch powder are merged, adds 10 times of ethanol waters of weight, ultrasonic wave extraction
50min, filtering obtains ultrasonic extract and ultrasonic wave filter residue, wherein, the ethanol volumetric concentration of ethanol water is 70%；
7) ultrasonic wave filter residue is put into supercritical extraction reactor, the carbon dioxide using absolute ethyl alcohol as entrainer is used as extraction
Fluid carries out supercritical extract, and extraction time is 1h, obtains supercritical extract liquid, wherein, the flow for extracting fluid is 18kg/h；
8) the total liquid of refluxing extraction, percolate, ultrasonic extract and supercritical extract liquid are merged, adds alembic
In, heating recovery solvent is concentrated into when vapor (steam) temperature is 42 DEG C and terminates, and obtains concentrate；
9) concentrate is carried out into vacuum distillation, you can.
Embodiment 2
A kind of extracting method of recovery rate tea tree ethereal oil high, step is as follows：
1) 2 are compared according to weight:1 weighs tea free and tea tree branch respectively, standby；
2) by after tea free freeze-drying, crush, cross 100 mesh sieves, obtain tea leaf powder；
3) tea leaf powder is put into container, adds 13 times of ethanol waters of weight, heating and refluxing extraction 1.5h to filter,
The first reflux extracting liquid and the first backflow filter residue are obtained, the first backflow filter residue is added into 8 times of ethanol waters of weight again, plus
Circumfluence distillation 43min, filtering obtains the second reflux extracting liquid and the second backflow filter residue, by the first reflux extracting liquid and second
Reflux extracting liquid merges, and obtains the total liquid of refluxing extraction, wherein, the ethanol volumetric concentration of ethanol water is 70%；
4) tea tree branch is put into percolator, using ethanol water as solvent, after extraction is finished, filtering obtains diacolation
Extract solution, wherein, the ethanol volumetric concentration of ethanol water is 85%；
5) after by the tea tree branch freeze-drying after seepage pressure effects, crush, cross 60 mesh sieves, obtain tea branch powder；
6) the second backflow filter residue and tea branch powder are merged, adds 11 times of ethanol waters of weight, ultrasonic wave extraction
55min, filtering obtains ultrasonic extract and ultrasonic wave filter residue, wherein, the ethanol volumetric concentration of ethanol water is 70%；
7) ultrasonic wave filter residue is put into supercritical extraction reactor, the carbon dioxide using absolute ethyl alcohol as entrainer is used as extraction
Fluid carries out supercritical extract, and extraction time is 1.5h, obtains supercritical extract liquid, wherein, the flow for extracting fluid is 18kg/
h；
8) the total liquid of refluxing extraction, percolate, ultrasonic extract and supercritical extract liquid are merged, adds alembic
In, heating recovery solvent is concentrated into when vapor (steam) temperature is 42 DEG C and terminates, and obtains concentrate；
9) concentrate is carried out into vacuum distillation, you can.
Embodiment 3
A kind of extracting method of recovery rate tea tree ethereal oil high, step is as follows：
1) 2 are compared according to weight:1 weighs tea free and tea tree branch respectively, standby；
2) by after tea free freeze-drying, crush, cross 110 mesh sieves, obtain tea leaf powder；
3) tea leaf powder is put into container, adds 14 times of ethanol waters of weight, heating and refluxing extraction 1.5h to filter,
The first reflux extracting liquid and the first backflow filter residue are obtained, the first backflow filter residue is added into 9 times of ethanol waters of weight again, plus
Circumfluence distillation 45min, filtering obtains the second reflux extracting liquid and the second backflow filter residue, by the first reflux extracting liquid and second
Reflux extracting liquid merges, and obtains the total liquid of refluxing extraction, wherein, the ethanol volumetric concentration of ethanol water is 70%；
4) tea tree branch is put into percolator, using ethanol water as solvent, after extraction is finished, filtering obtains diacolation
Extract solution, wherein, the ethanol volumetric concentration of ethanol water is 85%；
5) after by the tea tree branch freeze-drying after seepage pressure effects, crush, cross 70 mesh sieves, obtain tea branch powder；
6) the second backflow filter residue and tea branch powder are merged, adds 11 times of ethanol waters of weight, ultrasonic wave extraction
55min, filtering obtains ultrasonic extract and ultrasonic wave filter residue, wherein, the ethanol volumetric concentration of ethanol water is 70%；
7) ultrasonic wave filter residue is put into supercritical extraction reactor, the carbon dioxide using absolute ethyl alcohol as entrainer is used as extraction
Fluid carries out supercritical extract, and extraction time is 1.5h, obtains supercritical extract liquid, wherein, the flow for extracting fluid is 19kg/
h；
8) the total liquid of refluxing extraction, percolate, ultrasonic extract and supercritical extract liquid are merged, adds alembic
In, heating recovery solvent is concentrated into when vapor (steam) temperature is 42 DEG C and terminates, and obtains concentrate；
9) concentrate is carried out into vacuum distillation, you can.
Embodiment 4
A kind of extracting method of recovery rate tea tree ethereal oil high, step is as follows：
1) 2 are compared according to weight:1 weighs tea free and tea tree branch respectively, standby；
2) by after tea free freeze-drying, crush, cross 120 mesh sieves, obtain tea leaf powder；
3) tea leaf powder is put into container, adds 14 times of ethanol waters of weight, heating and refluxing extraction 1.5h to filter,
The first reflux extracting liquid and the first backflow filter residue are obtained, the first backflow filter residue are added into 10 times of ethanol waters of weight again,
Heating and refluxing extraction 50min, filtering obtains the second reflux extracting liquid and the second backflow filter residue, by the first reflux extracting liquid and the
Two reflux extracting liquids merge, and obtain the total liquid of refluxing extraction, wherein, the ethanol volumetric concentration of ethanol water is 70%；
4) tea tree branch is put into percolator, using ethanol water as solvent, after extraction is finished, filtering obtains diacolation
Extract solution, wherein, the ethanol volumetric concentration of ethanol water is 85%；
5) after by the tea tree branch freeze-drying after seepage pressure effects, crush, cross 70 mesh sieves, obtain tea branch powder；
6) the second backflow filter residue and tea branch powder are merged, adds 12 times of ethanol waters of weight, ultrasonic wave extraction
58min, filtering obtains ultrasonic extract and ultrasonic wave filter residue, wherein, the ethanol volumetric concentration of ethanol water is 70%；
7) ultrasonic wave filter residue is put into supercritical extraction reactor, the carbon dioxide using absolute ethyl alcohol as entrainer is used as extraction
Fluid carries out supercritical extract, and extraction time is 1.5h, obtains supercritical extract liquid, wherein, the flow for extracting fluid is 20kg/
h；
8) the total liquid of refluxing extraction, percolate, ultrasonic extract and supercritical extract liquid are merged, adds alembic
In, heating recovery solvent is concentrated into when vapor (steam) temperature is 42 DEG C and terminates, and obtains concentrate；
9) concentrate is carried out into vacuum distillation, you can.
Embodiment 5
A kind of extracting method of recovery rate tea tree ethereal oil high, step is as follows：
1) 2 are compared according to weight:1 weighs tea free and tea tree branch respectively, standby；
2) by after tea free freeze-drying, crush, cross 120 mesh sieves, obtain tea leaf powder；
3) tea leaf powder is put into container, adds 15 times of ethanol waters of weight, heating and refluxing extraction 2h, filtering is obtained
The first reflux extracting liquid and the first backflow filter residue are obtained, the first backflow filter residue is added into 10 times of ethanol waters of weight again, plus
Circumfluence distillation 50min, filtering obtains the second reflux extracting liquid and the second backflow filter residue, by the first reflux extracting liquid and second
Reflux extracting liquid merges, and obtains the total liquid of refluxing extraction, wherein, the ethanol volumetric concentration of ethanol water is 70%；
4) tea tree branch is put into percolator, using ethanol water as solvent, after extraction is finished, filtering obtains diacolation
Extract solution, wherein, the ethanol volumetric concentration of ethanol water is 85%；
5) after by the tea tree branch freeze-drying after seepage pressure effects, crush, cross 80 mesh sieves, obtain tea branch powder；
6) the second backflow filter residue and tea branch powder are merged, adds 12 times of ethanol waters of weight, ultrasonic wave extraction
60min, filtering obtains ultrasonic extract and ultrasonic wave filter residue, wherein, the ethanol volumetric concentration of ethanol water is 70%；
7) ultrasonic wave filter residue is put into supercritical extraction reactor, the carbon dioxide using absolute ethyl alcohol as entrainer is used as extraction
Fluid carries out supercritical extract, and extraction time is 2h, obtains supercritical extract liquid, wherein, the flow for extracting fluid is 20kg/h；
8) the total liquid of refluxing extraction, percolate, ultrasonic extract and supercritical extract liquid are merged, adds alembic
In, heating recovery solvent is concentrated into when vapor (steam) temperature is 42 DEG C and terminates, and obtains concentrate；
9) concentrate is carried out into vacuum distillation, you can.
The extracting method of tea tree ethereal oil of the present invention, can effectively extract the tea tree ethereal oil in tea free and tea tree branch, extract
Rate is high, and raw material effectively can be utilized, and improves productivity effect；The extracting method of tea tree ethereal oil of the present invention, is obtained
Tea tree ethereal oil purity is high, and moisture content is low, is conducive to preserving, with wide market prospects.
Better embodiment of the invention is explained in detail above, but the present invention is not limited to above-mentioned embodiment party
Formula, in the ken that one skilled in the relevant art possesses, can also be on the premise of present inventive concept not be departed from
Various changes can be made.
Claims (5)
1. the extracting method of a kind of recovery rate tea tree ethereal oil high, it is characterised in that step is as follows：
1) 2 are compared according to weight:1 weighs tea free and tea tree branch respectively, standby；
2) by after tea free freeze-drying, crush, cross 100-120 mesh sieves, obtain tea leaf powder；
3) tea leaf powder is put into container, adds the 12-15 times of ethanol water of weight, heating and refluxing extraction 1-2h, filtering is obtained
The first reflux extracting liquid and the first backflow filter residue are obtained, the first backflow filter residue are added into the 8-10 times of ethanol water of weight again,
Heating and refluxing extraction 40-50min, filtering obtains the second reflux extracting liquid and the second backflow filter residue, by the first reflux extracting liquid and
Second reflux extracting liquid merges, and obtains the total liquid of refluxing extraction；
4) tea tree branch is put into percolator, using ethanol water as solvent, after extraction is finished, filtering obtains seepage pressure effects
Liquid；
5) after by the tea tree branch freeze-drying after seepage pressure effects, crush, cross 50-80 mesh sieves, obtain tea branch powder；
6) the second backflow filter residue and tea branch powder are merged, adds the 10-12 times of ethanol water of weight, ultrasonic wave extraction 50-
60min, filtering obtains ultrasonic extract and ultrasonic wave filter residue；
7) ultrasonic wave filter residue is put into supercritical extraction reactor, the carbon dioxide using absolute ethyl alcohol as entrainer as extraction fluid
Supercritical extract is carried out, extraction time is 1-2h, obtain supercritical extract liquid；
8) the total liquid of refluxing extraction, percolate, ultrasonic extract and supercritical extract liquid are merged, in addition alembic,
Heating recovery solvent, is concentrated into when vapor (steam) temperature is 42 DEG C and terminates, and obtains concentrate；
9) concentrate is carried out into vacuum distillation, you can.
2. the extracting method of recovery rate according to claim 1 tea tree ethereal oil high, it is characterised in that step 3) in, second
The ethanol volumetric concentration of alcohol solution is 70%.
3. the extracting method of recovery rate according to claim 2 tea tree ethereal oil high, it is characterised in that step 4) in, second
The ethanol volumetric concentration of alcohol solution is 85%.
4. the extracting method of recovery rate according to claim 1 or 2 or 3 tea tree ethereal oil high, it is characterised in that step 6)
In, the ethanol volumetric concentration of ethanol water is 70%.
5. the extracting method of recovery rate according to claim 4 tea tree ethereal oil high, it is characterised in that step 7) in, extraction
The flow for taking fluid is 18-20kg/h.
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| CN108272704A (en) * | 2018-04-20 | 2018-07-13 | 江西金思康药业有限公司 | A kind of nursing essential oil and preparation method thereof |
| CN108822963A (en) * | 2018-05-28 | 2018-11-16 | 贵州湄潭兰馨茶业有限公司 | The extracting method of tealeaves essential oil and obtained tealeaves essential oil |
| CN110317678A (en) * | 2019-07-22 | 2019-10-11 | 东源县大地农林发展有限公司 | A kind of tea tree ethereal oil extracting method and the skin care item using tea tree ethereal oil preparation |
| CN114644960A (en) * | 2022-03-23 | 2022-06-21 | 宝爵生物科技(广州)有限公司 | Plant essential oil and preparation method thereof |
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| CN108822963A (en) * | 2018-05-28 | 2018-11-16 | 贵州湄潭兰馨茶业有限公司 | The extracting method of tealeaves essential oil and obtained tealeaves essential oil |
| CN110317678A (en) * | 2019-07-22 | 2019-10-11 | 东源县大地农林发展有限公司 | A kind of tea tree ethereal oil extracting method and the skin care item using tea tree ethereal oil preparation |
| CN114644960A (en) * | 2022-03-23 | 2022-06-21 | 宝爵生物科技(广州)有限公司 | Plant essential oil and preparation method thereof |
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