CN85102396A - Overcritical (or liquid) carbon dioxide draw fragrant volatile of fresh flowers essential oil - Google Patents
Overcritical (or liquid) carbon dioxide draw fragrant volatile of fresh flowers essential oil Download PDFInfo
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- CN85102396A CN85102396A CN198585102396A CN85102396A CN85102396A CN 85102396 A CN85102396 A CN 85102396A CN 198585102396 A CN198585102396 A CN 198585102396A CN 85102396 A CN85102396 A CN 85102396A CN 85102396 A CN85102396 A CN 85102396A
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 239000000341 volatile oil Substances 0.000 title claims abstract description 80
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 48
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 45
- 239000007788 liquid Substances 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 33
- 239000003463 adsorbent Substances 0.000 claims abstract description 24
- 238000000605 extraction Methods 0.000 claims abstract description 10
- 235000013599 spices Nutrition 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims description 28
- 239000012530 fluid Substances 0.000 claims description 22
- 239000000284 extract Substances 0.000 claims description 14
- 241000207840 Jasminum Species 0.000 claims description 12
- 235000010254 Jasminum officinale Nutrition 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 4
- 241000234479 Narcissus Species 0.000 claims description 3
- 241000233855 Orchidaceae Species 0.000 claims description 3
- 244000273928 Zingiber officinale Species 0.000 claims description 2
- 235000006886 Zingiber officinale Nutrition 0.000 claims description 2
- 239000002250 absorbent Substances 0.000 claims description 2
- 230000002745 absorbent Effects 0.000 claims description 2
- 235000008397 ginger Nutrition 0.000 claims description 2
- 238000002386 leaching Methods 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 238000005243 fluidization Methods 0.000 claims 1
- 239000003205 fragrance Substances 0.000 abstract description 7
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 238000000926 separation method Methods 0.000 description 8
- 238000000638 solvent extraction Methods 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 239000006096 absorbing agent Substances 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 241001579180 Matthiola longipetala Species 0.000 description 2
- 239000002156 adsorbate Substances 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 230000008542 thermal sensitivity Effects 0.000 description 2
- 210000004885 white matter Anatomy 0.000 description 2
- 241000628997 Flos Species 0.000 description 1
- 241000218922 Magnoliophyta Species 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- -1 cured matter Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000003306 harvesting Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000010656 jasmine oil Substances 0.000 description 1
- 238000002803 maceration Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
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Abstract
The invention belongs to the application of overcritical (or liquid) carbon dioxide extraction technique on ethereal oil of flower separates.
Feature of the present invention is directly not use supercritical carbon dioxide extracting fresh flower spices, and be to use the adsorbents adsorb fresh flower to open the fragrance that comes out in the process, use the extracting of overcritical (or liquid) carbon dioxide to be adsorbed the two step method of the adsorbed essential oil of agent then, separate ethereal oil of flower.Thereby can reduce running cost, increase ethereal oil of flower output, and produce a essential oil with the peculiar fragrance of fresh flower.
Description
The invention belongs to the application of overcritical (or liquid) carbon dioxide extraction technique on ethereal oil of flower separates.
The essential oil that the present invention distributes fresh flower concentrates by stable absorbing process and collects, use then overcritical (or liquid) carbon dioxide from adsorbent essential oil expeditiously desorption come out, reach the purpose of fragrant volatile of fresh flowers essential oil extraction.Whole separation process is carried out under near the condition of room temperature, is specially adapted to the extraction of thermal sensitivity ethereal oil of flower component.
The method of volatile solvent lixiviate is generally adopted in the extraction of current perfume industry ethereal oil of flower.Use careful refined benzinum dipping fresh flower in concrete technological process, the essential oil in the fresh flower is by petroleum ether dissolution, and maceration extract is through concentrating, and steps such as vacuum distillation are separated the solvent benzinum with extract, thereby obtain fresh flower medicinal extract.Give birth to produce Net oil if desired, need medicinal extract is dissolved with ethanol, take off curedly, steam series of steps such as desolventizing and just can obtain through freezing.
From above-mentioned technological process as can be known, for fresh flower extract and solvent benzinum are separated, need to adopt repeatedly distillation.Therefore the fresh flower extract must stand the heating of long period, and the result might destroy some tender and lovely especially composition in the ethereal oil of flower, causes the difference of medicinal extract fragrance and fresh flower.
The fresh flower solvent extraction method can only be collected on the moment flower that feeds intake and contain essential oil on the other hand.(for example: fresh flowers such as jasmine, white orchid, narcissus, jasmine) solvent extraction method can not be collected fresh flower in open process, the essential oil that flower constantly generates for the fresh flower that can also constantly produce essential oil after plucking.Therefore will influence the ethereal oil of flower yield.The more important thing is that the head of above-mentioned ethereal oil of flower is fragrant and partly will deposit in the process major part and scatter and disappear in atmosphere that scattering and disappearing that head is fragrant will influence the fragrance of medicinal extract at fresh flower.
Produce the part ethereal oil of flower except that France also adopts ancient grease enfleurage method in the world at present, the fragrant volatile of fresh flowers extracts essential oil yet there are no report.Grease enfleurage method takes a lot of work, time-consuming, production scale is less, and product can not obtain the essential oil of Chun Net.
At last, when using solvent extraction method to produce fresh flower medicinal extract, the essential oil of volatile solvent in extracting fresh flower out, also dissolve the other plant composition of a great deal of, as cured matter, dawn white matter, pigment.Thereby product is dark fat shape, even Zhi Cheng Net oil can not remove above-mentioned impurity fully.
The extracting of overcritical (or liquid) carbon dioxide is a development in recent years separating technology faster.Because that supercritical carbon dioxide fluid has is big for difficult volatile materials solubility, mass transfer rate is high, selectivity is easy to regulate, flow process is simple, series of advantages such as solvent recovery is easy, pollution-free problem, is subjected to general attention in chemical separation process.Moderate (the 72.9kg/Cm of carbon dioxide critical pressure in addition
2), critical-temperature makes the supercritical carbon dioxide extractive process to carry out under near the condition of room temperature near room temperature (31 ℃), therefore is particularly suitable for the separation and purification of effective ingredient in the natural products.This technology has obtained some practicality progress in recent years.On fragrance industry, particularly delivered many result of the tests on the separation and purification of natural perfume plant, coverage is very wide, seen the patent (Geyman) 2.709 of the direct extracting Flos Chrysanthemi of supercritical carbon dioxide (or liquid) carbon dioxide, 033, German DE 3,105, and 557).But the extracting of ethereal oil of flower supercritical carbon dioxide yet there are no the industrialization report.
Though we think that the supercritical carbon dioxide extraction technique has many good qualities for the separation and purification of natural perfume plant effective ingredient, but ethereal oil of flower content very low (generally about 0.2%), volume is loose, bulk density is very little, so directly that a large amount of volumes are loose fresh flower is introduced autoclave extracting essential oil, under present condition, to obtain industrial practical application and also have certain Technological Economy difficulty.The economy of the direct supercritical fluid extracting of fresh flower once was some authors' a call for Votes.
The present invention is directed to the defective of present industrial fresh flower extraction and directly fresh flower is introduced the Technological Economy difficulty that high-pressure system is carried out the supercritical fluid extracting, propose a brand-new fragrant volatile of fresh flowers extraction of essential oil new method.
Main purpose of the present invention is to guarantee in the fresh flower that thermal sensitivity essential oil group part can heat damage in leaching process, and produces the essential oil with the peculiar fragrance of fresh flower.
Main purpose of the present invention also is to create one and helps plucking the environment that the back fresh flower continues to form essential oil, so that increase the total output of ethereal oil of flower in the process of collecting the fragrant volatile of fresh flowers essential oil.
Another object of the present invention is to concentrate the essential oil content that is used for supercritical carbon dioxide extracting raw material.Thereby reduce supercritical carbon dioxide extractive process Technological Economy difficulty, reduce running cost.
Purpose of the present invention comprises that also production does not contain other compositions of plant De Chun Net fragrant volatile of fresh flowers essential oils such as cured matter, pigment and dawn white matter by adopting the method for the scentetd adsorbing and trapping of fresh flower.
, produce medicinal extract by traditional petroleum ether solvent extraction after the finished fresh flower of this law can be sent to fresh flower solvent lixiviate workshop section equally.Because this law can make the fresh flower storage environment help the formation of essential oil, so fresh flower medicinal extract yield and the physicochemical property handled through this law can also be near the industrial index of fresh flower solvent extraction method (part index number is improvement to some extent also).
Characteristics of the present invention are whole separation process is divided into two steps.(1) at room temperature, air is flow through the fresh flower layer through suction, take fragrant volatile of fresh flowers out of, the air that contains the essential oil high-efficiency adsorbent bed (fluid bed or fixed bed) of flowing through, essential oil is adsorbed capture.(2) carbon dioxide that is in " solvent state " fully contacts the essential oil that extracting goes out to be adsorbed with the adsorbent that has adsorbed the fragrant volatile of fresh flowers essential oil.Residual flower after said process is handled still can be used as the raw material of lixiviate spices.
Fragrant volatile of fresh flowers is bled absorption partly.The firm fresh flower of plucking (partly the seeds of flowering plants can be the bud that a bud just ready to burst) is on the flower stand that seals around layering is placed on.Bleed from the flower stand upper end with air blast, fresh air is entered by the flower stand lower end.When air passes through the flower layer, take the essential oil that fresh flower comes out out of.Air mass flow 1 liter/kilogram fresh flower minute-50 liters/kilogram fresh flower minute.The air that contains the essential oil absorber of flowing through, essential oil is by high-efficient granule adsorbent adsorbed (porous adsorbent comprises active carbon and macroporous absorbent resin) in the air.Bleed the adsorbing and trapping head essential oil time between 3～48 hours.Be applicable to that this law collects the fresh flower of an essential oil and belong to the fresh flower that can also constantly form essential oil after the harvesting.For example: jasmine, jasmine, white orchid, ginger, narcissus ... Deng.
Be adsorbed an essential oil part in the supercritical fluid extracting, it is extraction solvent that the present invention adopts carbon dioxide.CO 2 fluid depends on its physical state to organic solvability.Under typical temperature and pressure, carbon dioxide is minimum to the solvability of ethereal oil of flower.Along with the increase of pressure, solvability progressively increases, and the growth of a hop is generally arranged under super critical condition.We claim carbon dioxide that the higher state of the solvability of one or more adsorbates is " solvent state " herein, generally are a certain states that is higher than critical pressure.With carbon dioxide to the relatively poor state of the solvability of one or more adsorbates.We are referred to as " non-solvent state ".It generally is a certain state of subcritical pressure.Above-mentioned two kinds of states only represent that solvability has the carbon dioxide of relative difference, does not represent the meaning of absolute solubility property.
Among the present invention, be in the CO 2 fluid or the liquid of " solvent state " and adsorbed the adsorbent of fragrant volatile of fresh flowers essential oil, fully contact in autoclave, the essential oil that extracting goes out to be adsorbed." solvent state " carbon dioxide becomes " non-solvent state " through a special decompressor, and solubility descends, and dissolved fragrant volatile of fresh flowers essential oil is separated out major part and collect.Carbon dioxide will recycle.Whole separation process is carried out (about 30 ℃ of room temperatures) under near the condition of room temperature, prevent that effectively the fragrant volatile of fresh flowers essential oil component is rotten in process.
Indication carbon dioxide of the present invention " solvent state " is meant that temperature is that 10～60 ℃ of pressure are 73～300kg/cm
2CO 2 fluid under the condition, " non-solvent state " are meant that temperature is-76 ℃～35 ℃, and pressure is lower than 73kg/cm
2Carbon dioxide.
Embodiment that is description of drawings.Fresh flower is Jasmine in this example.144 kilograms of jasmonic buds that a bud just ready to burst evenly are sub-packed in 24 flower sieves, and flower screening layer is loaded in the flower stand, sealing around the flower stand.Utilize air blast 9 to bleed from flower stand head tube 2, air enters from the flower stand bottom, evenly by the flower layer, takes the fragrance that comes out in the open process of Jasmine out of.The air that contains an essential oil enters absorber 3, and the adsorbent of loading in the absorber is an active carbon.400 grams.When containing an essential oil air through active carbon layer, most of essential oil is adsorbed by the charcoal layer, and flow through flowmeter 5, valve 8, air blast 9 of air is last by pipe 10 emptying then, and air mass flow is 130 meters/hour.Jasmine bled the said equipment to 0: 30 morning of next day from 19: 30 and captured an essential oil totally 5 hours, drove out then, and Jasmine is sent solvent lixiviate Workshop Production medicinal extract.The active carbon that has adsorbed essential oil draws off from absorber, is stored in the container 6, makes the super carbon dioxide extracting raw material that faces.The carbon dioxide that obtains from steel cylinder is managed 11 valves 12 and is entered clarifier 13, and the carbon dioxide after the purification enters carbon dioxide storage tank 16 through managing 14 valves 15.The active carbon that 80 grams have adsorbed a jasmine essential oil is added to the autoclave 23 through valve 25 pipes 24 from container 6 before each test.It is 10～60 ℃ of temperature that carbon dioxide is adjusted to " solvent state " by pipe 17 compression sets 18 hot converters 20, pressure 73～300kg/cm
2, enter in the autoclave 23 through managing 21, fully contact with the active carbon that is filled in the essential oil of adsorption head wherein before the test.Carbon dioxide is with 50～300 liter atmospheric carbon dioxides/100 gram adsorbents.Hour flow velocity continuously by adsorbent bed, and extracting goes out essential oil in the adsorbent.Leave autoclave through managing 26 then, CO 2 fluid is through decompressor 27 step-downs and adjust to " non-solvent state ", and promptly pressure is lower than 73kg/cm
2Temperature-76～35 ℃.At this moment because carbon dioxide significantly reduces the solvability of refined jasmine oil, and the essential oil that is dissolved in originally wherein will be separated out, be collected in resolver 28, an essential oil is regularly emitted through valve 30 from managing 29.The carbon dioxide of " non-solvent state " is from managing 31 through valve 32,33 with manage 35 times storage tanks 16 and recycle.Through valve 34, spinner flowmeter 36 meterings are after manage 37 emptying in case of necessity.Experiment is carried out continuously, can get an essential oil 8.0 grams.The active carbon adsorbing and trapping that is used for a jasmine essential oil capable of circulation through the extracting of overcritical (or liquid) carbon dioxide.
Reference:
（1）A.B.Caraguy.Perfumer and Flavorst Vol.6.Aug/Sept.43（1981）
（2）L.G.Randall.Separation Science and Technology 17 No.1（1982）
（3）German Offen 2，709，033
（4）German Offen DE 3，105，557
（5）USP 4，124，528
（6）USP 4，400，398
（7）German Offen DE 3，016，917
Claims (16)
- The invention belongs to the super application of fluid extraction technology on fresh flower spices extracts of facing.The invention is characterized in: divided for two steps carried out fragrant volatile of fresh flowers essential oil leaching process.Use earlier adsorbent to capture an essential oil that distributes in the open process of fresh flower, and then an essential oil that is adsorbed with the extracting of overcritical (or liquid) carbon dioxide.1, a kind of super method of facing fluid extracting fragrant volatile of fresh flowers essential oil.Be characterized in that this method comprises two steps 1. at room temperature, in a period of time, make the air Continuous Flow, take the fragrant volatile of fresh flowers essential oil out of, contain an essential oil air and capture a wherein essential oil with high-efficiency adsorbent after the fresh flower layer of just having plucked.2. carbon dioxide becomes the CO 2 fluid of " solvent state " through physical process, this fluid fully contacts with the adsorbent that has adsorbed the fragrant volatile of fresh flowers essential oil in autoclave, the essential oil that extraction is adsorbed, " solvent state " CO 2 fluid that contains the fragrant volatile of fresh flowers essential oil becomes the carbon dioxide of " non-solvent state " by a device.The fragrant volatile of fresh flowers essential oil will be separated out to visit from carbon dioxide and will be collected.Fresh flower after an above-mentioned capture essential oil is handled still can be used as the raw material of solvent lixiviate spices.
- 2, make the air Continuous Flow described in the claim (1) in the fresh flower layer of just having plucked, its flow is 1 liter air/kilogram fresh flower minute to 50 liters air/kilogram fresh flower minute.
- 3, in the claim (1) in a period of time the indication time be 3～48 hours.
- 4, the fresh flower of just having plucked in the claim (1) refers to bud or the just open fresh flower that a bud just ready to burst.
- 5, high-efficiency adsorbent is meant granular porous adsorbent in the claim (1).
- 6, granular porous adsorbent can be active carbon or macroporous absorbent resin described in the claim (5).
- 7, fresh flower also has the fresh flower that forms the essential oil ability for after plucking in the claim (1).
- 8, capturing wherein with high-efficiency adsorbent in the claim (1), an essential oil refers to contain the air of an essential oil continuously by the porous adsorbent layer.(comprising fixed bed and fluidization bed that layering is placed).
- 9, indication " solvent state " CO 2 fluid is meant that temperature is 10～60 ℃, pressure 73～300kg/Cm in the claim (1) 2CO 2 fluid under the condition.
- 10, indication " non-solvent state " carbon dioxide is meant temperature-76～35 ℃ in the claim (1), and pressure is lower than 73kg/Cm 2Carbon dioxide under the state.
- 11, carbon dioxide contracts and regulates temperature through the physical process finger pressure in the claim (1).
- 12, this fluid fully contacts the CO 2 fluid that is meant " solvent state " with the adsorbent that has adsorbed the fragrant volatile of fresh flowers essential oil and flows through the porous adsorbent bed with constant speed in the claim (1).
- 13, " solvent state " CO 2 fluid is meant the pressure loading valve of a particular design in the claim (1) by a device.
- 14, fresh flower can be jasmine, white orchid, jasmine, ginger, narcissus in the claim (7).
- 15, " solvent state " CO 2 fluid can be that supercritical carbon dioxide fluid can be a supercritical carbon dioxide fluid in the claim (9), also can be the flow of liquid carbon dioxide body.
- 16, constant speed flows through that indication speed is 50 liter carbon dioxides/100 gram adsorbents in the porous adsorbent bed in the claim (12).Hour to 300 liter carbon dioxides/100 gram adsorbents hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85102396A CN85102396B (en) | 1985-04-01 | 1985-04-01 | Extraction of essence for hair oil from fresh flowers with supercritical (or liquids) carbon dioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85102396A CN85102396B (en) | 1985-04-01 | 1985-04-01 | Extraction of essence for hair oil from fresh flowers with supercritical (or liquids) carbon dioxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN85102396A true CN85102396A (en) | 1986-10-29 |
| CN85102396B CN85102396B (en) | 1988-04-27 |
Family
ID=4792479
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN85102396A Expired CN85102396B (en) | 1985-04-01 | 1985-04-01 | Extraction of essence for hair oil from fresh flowers with supercritical (or liquids) carbon dioxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN85102396B (en) |
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| CN101230308B (en) * | 2007-11-02 | 2011-04-20 | 景谷傣族彝族自治县邦永生物资源开发有限公司 | Method for absorbing and extracting fragrant volatile of fresh flowers |
| CN101317649B (en) * | 2007-06-05 | 2013-05-08 | 深圳市汇康生物科技有限公司 | Method for preparing glossy ganoderma spore oil |
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- 1985-04-01 CN CN85102396A patent/CN85102396B/en not_active Expired
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| CN105066590A (en) * | 2015-07-22 | 2015-11-18 | 大闽食品（漳州）有限公司 | Methods for adsorbing fragrance volatiles of grapefruit fresh flowers and drying grapefruit fresh flowers at low temperature |
| CN105062691A (en) * | 2015-09-28 | 2015-11-18 | 朱翠帮 | Extraction method of tea tree essential oil |
| CN108034501A (en) * | 2017-12-30 | 2018-05-15 | 刘莹艳 | A kind of essential oil gel and preparation method thereof |
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Also Published As
| Publication number | Publication date |
|---|---|
| CN85102396B (en) | 1988-04-27 |
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