EP0698076A1 - Procede et installation d'extraction sans solvant de produits naturels par micro-ondes - Google Patents
Procede et installation d'extraction sans solvant de produits naturels par micro-ondesInfo
- Publication number
- EP0698076A1 EP0698076A1 EP94915607A EP94915607A EP0698076A1 EP 0698076 A1 EP0698076 A1 EP 0698076A1 EP 94915607 A EP94915607 A EP 94915607A EP 94915607 A EP94915607 A EP 94915607A EP 0698076 A1 EP0698076 A1 EP 0698076A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- enclosure
- biological material
- microwaves
- natural product
- extract
- 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
Classifications
-
- 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
Definitions
- the invention relates to the field of extraction of natural products contained in biological material and in particular, but not exclusively, the extraction of such products from plants.
- the extraction of natural products from biological material can be carried out according to several processes using or not using one or more extraction solvents, depending on the nature of the biological material used and that of the product or products which it is desired to extract. of it. It should be noted in this regard that the name given to an extract is often a function of the technology used to achieve it.
- the concretes, the resinoids, the oleoresins ... which are extracts consisting of volatile compounds or waxy and fatty and non-volatile products, are conventionally obtained in the presence of at least one organic solvent.
- Essential oils mainly consisting of odorous volatile compounds, are generally obtained by distillation with water vapor (hydrodistillation) and / or by mechanical processes.
- oilseeds, essential oils of citrus peel, fish oils ... is conventionally carried out using physical processes such as grinding and / or pressing, by absence of solvent or by hydrodistillation.
- such techniques have the advantage of making it possible to obtain extraction products (and biological material after extraction) free from solvent residues and therefore having no not undergo subsequent treatment for the removal of such residues.
- extraction techniques using organic solvents. Thanks to such techniques the product to be extracted diffuses into the solvent and dissolves there. However, it is then necessary to separate the extracted product from the solvent, in order to allow the concentration of the extract.
- Many parameters are involved in the extraction yields carried out in the presence of solvent, among which may be mentioned: - the solubility of the product extracted in the chosen solvent,
- the diffusion of the extracted product could be greatly improved by subjecting the biological material to a pretreatment which may consist in particular of grinding, enzymatic digestion or even drying.
- a pretreatment which may consist in particular of grinding, enzymatic digestion or even drying.
- sonication methods which consist in applying ultrasound to the mixture constituted by the biological material and the solvent in order to promote the passage of the extract into the solvent.
- the mechanical waves formed by the ultrasounds indeed make it possible to locally generate a cavitation of the biological material and consequently a heating of the latter promoting the release of the extract.
- European patent EP 0398798 discloses a technique for extracting products from biological material assisted by microwaves, comprising the following steps consisting in: subdivide a biological material (peppermint, Scottish lovage, cedar or garlic) having a dispersed component absorbing microwaves (water), put this subdivided material in a transparent or partially transparent solvent in microwaves and absorbing less micro -waves as the dispersed component, such as hexane, ethanol or dichloromethane, exposing the mixture constituted by the subdivided material and the solvent to the microwaves in order to allow the extraction of the soluble products by heating the subdivided material preferentially with solvent, - separate the residual biological material from the solvent and recover the extracted product.
- subdivide a biological material peppermint, Scottish lovage, cedar or garlic
- a dispersed component absorbing microwaves (water)
- a transparent or partially transparent solvent in microwaves and absorbing less micro -waves as the dispersed component, such as hexan
- the objective of the present invention is to provide a process for extracting natural products by microwave, without having the drawbacks of the processes of the prior art.
- one of the objectives of the invention is to provide such a process allowing extraction in the absence of solvent and therefore obtaining an extract free from any solvent residue.
- Another objective of the invention is to propose such a process without requiring an excessive energy supply, for a given quantity of biological material to be treated.
- Another objective of the invention is to propose an installation for the implementation of such a method.
- the invention relates to a process for the microwave extraction of at least one natural product from biological material, said process consisting in: placing said biological material in an enclosure, in the absence of any solvent, - subjecting said biological material present in said enclosure to microwave irradiation, in order to cause the evaporation of at least part of the water contained in said biological material and consequently the bursting of the cellular structures of said biological material.
- said method being characterized in that it comprises the following additional steps consisting in: applying, intermittently, a reduced pressure inside said enclosure during said step of applying microwaves, in order to promote bursting cellular structures of said biological material induced by the application of microwaves, heating, during at least most of said step of applying microwaves, said enclosure, in order to compensate for the drop in temperature resulting from evaporation water from biological material, the combination of said steps of applying microwaves, applying reduced pressure inside the enclosure and heating the enclosure allowing the hydrodistillation of said natural product by entraining it in water vapor from said biological material.
- Such a process can be advantageously implemented on all natural biological materials, whether they are of animal, plant or micro ⁇ biological origin as long as these contain at least about 30% water.
- This process can in particular be used to extract essential oils from plants, tissues of animal origin and especially from fish, but also from algae, micro-algae and even possibly micro-organisms.
- this biological material may, depending on its nature, be subdivided before being introduced into the enclosure in order to increase its factor of exposure to microwaves.
- the process according to the invention makes it possible to carry out the hydrodistillation of the product which it is desired to extract, not thanks to water brought from outside during the process, but thanks to the water contained in the biological material. treaty.
- this water will be called water of constitution, whereas it may have been brought beforehand to the biological material, when the latter will be available in dehydrated form, during a rehumidification stage.
- the method according to the invention therefore consists in subjecting the treated biological material to microwave radiation, in the absence of extracting solvent, allowing the contents of the cells of this material to be ejected outside.
- the pressure of the enclosure is reduced. This reduction in pressure makes it possible, on the one hand, to increase the mechanical stress exerted on the walls of the cells of the biological material and on the other hand to increase the volatility of the azeotropic mixture constituted by the product which it is desired to extract and water vapor.
- the concomitant heating of the enclosure makes it possible to compensate for the very rapid decrease in temperature resulting from the evaporation of the water of constitution under the effect of the lowering of the pressure in the enclosure.
- Such a decrease in temperature is indeed capable of completely masking the action of microwaves.
- the method according to the invention has many advantages. In addition to the fact that it leads to extracts without residual solvent, it also makes it possible, with respect to a conventional hydrodistillation, to obtain an extract of equivalent composition and with an equivalent yield, in a substantially shorter time. While the conventional hydrodistillation times are generally counted in hours, the hydrodistillation times under reduced pressure according to the invention are counted in minutes. For certain products, it is thus possible to obtain a given quantity of extract ten times faster than with a conventional steam distillation.
- the method according to the invention consumes much less energy than the microwave assisted extraction methods of the prior art.
- the energy used in the context of the invention is also less than that necessary for hydrodistillation.
- hydrodistillation it is indeed necessary to heat the biological material and the added water, the mass of which can represent up to 10 times the mass of biological material.
- the residual biological material obtained at the end of the process is in a dry form, since the water of constitution which it contained was used for the entrainment of the extracted product and that the process does not put using external water supply. Consequently, this residual material can easily be degraded thermally and therefore possibly recycled as fuel.
- said step of the method according to the invention consisting of the intermittent application of a reduced pressure, consists in subjecting the interior of said enclosure to vacuum cycles.
- said step of separation of the residual biological material from the extract consists:
- said heating step is preferably carried out at a temperature below 100 ° C.
- the process can be carried out at a temperature advantageously below 75 ° C so as to allow the extraction of products which tend to degrade under the effect of heat.
- the microwaves used during said microwave irradiation step advantageously have a frequency at least equal to 300 MHz. It should be noted, however, that in many countries the use of frequencies is very strictly regulated and that, for example in France, only frequencies of 915 MHz and
- said microwave irradiation step will preferably be carried out so as to apply a power ranging from approximately 100 W to approximately 10,000 W per kilogram of product treated.
- said microwave irradiation step is carried out with mechanical stirring of said biological material. Such agitation will increase the factor of exposure of biological material to microwaves.
- the invention also relates to an installation for implementing such a method, characterized in that it comprises:
- Means for recovering the extract at its exit from said enclosure comprise means for refrigerating the water vapor containing the extract.
- said installation has means for operating said means making it possible to reduce the pressure inside the enclosure cyclically.
- said enclosure is provided with stirring means.
- said installation comprises means making it possible to redirect the waste water obtained at the level of the means for recovering the extract inside said enclosure.
- FIG. 1 shows a schematic view of an installation according to the invention
- FIG. 2 translates the evolution of the pressure of the enclosure and the temperature of the biological material, in the context of a first example of implementation of the method according to the invention with the installation shown schematically in Figure 1 , for the extraction of peppermint essential oil;
- FIG. 4 shows the evolution of the pressure of the enclosure and the temperature of the biological material, in the context of a comparative example of extraction of peppermint essential oil
- FIG. 6 shows the evolution of the pressure of the enclosure and the temperature of the biological material, in the context of a second example of implementation of the method according to the invention for the extraction of essential oil from officinal sage;
- FIG. 7 shows the evolution of the essential oil yield of sage sage obtained during the second example of implementation of the method according to the invention.
- an installation for extracting natural products from biological material is shown schematically.
- Such an installation comprises an enclosure 1 equipped with means 2 making it possible to generate microwaves in the interior volume which it delimits.
- these means 2 allow the emission of microwaves having a frequency equal to 2450 MHz. (Note that it would also have been possible to use a microwave generator with a frequency of 915 MHz, this other frequency being also authorized in France).
- the enclosure 1 is also provided in its lower part with stirring means 9, constituted by a turbine with three blades, making it possible to stir the biological material during its presence inside the enclosure 1, when subjected to the action of microwaves.
- stirring means 9 constituted by a turbine with three blades, making it possible to stir the biological material during its presence inside the enclosure 1, when subjected to the action of microwaves.
- Such stirring makes it possible to increase the exposure of the biological material to microwaves and to prevent certain areas of the latter from being insufficiently irradiated to carry out the extraction operation.
- the enclosure 1 is connected on the one hand with means 5 making it possible to reduce the pressure prevailing therein and, on the other hand, with means 6 for recovering the natural product extracted thanks to the action of microwaves on biological material.
- the means 5 making it possible to reduce the pressure in the enclosure can consist of any means conventionally used for the purpose of creating a partial vacuum inside an enclosure, such as, for example, a pump or a suction tube. water.
- the means 6 for recovering the extracted product comprise a pipe 11 installed in the upper part of the enclosure 1, around which are provided cooling means 7 formed by a coil in which a liquid circulates. cooling.
- Line 11 makes it possible to recover the vapors resulting from the action of microwaves on biological material and in which the essential oil is found. Thanks to the refrigeration means 7 these water vapors are condensed.
- a decanter 12 is provided at the outlet of the pipe 11 to recover these condensed vapors and separate the essential oil. The remaining waste water, after decantation is advantageously re-routed, through a pipe 10 in the enclosure 1 where it is recycled to complete the extraction.
- the enclosure 1 In order to allow heating of the interior of the enclosure 1 to compensate for the decrease in temperature resulting from the lowering of the pressure induced by the vacuum pump 5, the enclosure 1 has a thermostated double wall 3 connected to heating means 4.
- a kilogram of peppermint (Mentha piperita L., Hungarian variety) with 15% dry matter was placed inside the enclosure 1.
- the heating means 4 were adjusted so that the thermostatically controlled wall 3 induce a temperature of about 70 ° C inside the enclosure 1 and the stirring means 9 have been implemented so as to have a speed of 40 revolutions per minute.
- the power emitted by the microwave generation means 2 is 1150 W and the reflected power varies between 170 W and 220 W. During the extraction operation, which lasted 15 min, the power actually absorbed therefore been from 930 to 980 W.
- the pump 5 was implemented so as to lower the pressure to 250 mb. This pressure reduction was carried out after 5 min, 10 min and 13 min.
- the temperature of the refrigeration medium circulating in the coil 7 was fixed at 5 ° C. so as to cause the condensation of the vapors resulting from the action of the microwaves on the peppermint and containing the essential oil.
- the evolution of the temperature of the mint present in the enclosure and of the pressure prevailing inside it is represented in FIG. 2.
- the temperature of the product rapidly changes from room temperature up to about 75 ° C.
- the temperature drops. This drop in temperature is quickly compensated for by heating the enclosure so as not to mask the action of the microwaves.
- Example 1 The same quantity of peppermint as in Example 1 was treated using the same operating conditions as in Example 1 but by continuously operating the pump 5 so that the pressure prevailing inside the enclosure 1 is fixed at 250 mb during the entire extraction operation.
- Example 3 The change in the temperature of the mint and the pressure in the enclosure is given in FIG. 4. With reference to FIG. 5, the yield of essential oil was then only 0.2 ml per 100 g, or 5 times less than in Example 1. 1150 mg of essential oil were recovered from the mint residue after the extraction operation. These results show the importance of the intermittent nature which must be given, according to the invention, to the lowering of the pressure inside the enclosure.
- the heating means 4 have been adjusted so that the thermostatically controlled wall 3 induces a temperature of around 70 ° C. inside the enclosure 1 and the stirring means 9 have been implemented so as to have a speed of 40 revolutions per minute.
- the power emitted by the microwave generation means 2 is 1000 W and the reflected power varies between 150 W and 200 W. During the extraction operation, which lasted 10 min, the power actually absorbed therefore was from 800 to 850 W. During the extraction, the pump 5 was implemented so as to reduce the pressure to 250 mb. This pressure reduction was carried out after 3.5 min and 7 min.
- the temperature of the refrigeration medium circulating in the coil 7 was fixed at 5 ° C. so as to cause the condensation of the vapors resulting from the action of the microwaves on the peppermint and containing the oil. essential.
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
- Fats And Perfumes (AREA)
- Compounds Of Unknown Constitution (AREA)
- Medicines Containing Plant Substances (AREA)
Description
Claims
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR9305810 | 1993-05-11 | ||
FR9305810A FR2705035B1 (fr) | 1993-05-11 | 1993-05-11 | Procédé et installation d'extraction sans solvant de produits naturels par micro-ondes. |
PCT/FR1994/000551 WO1994026853A1 (fr) | 1993-05-11 | 1994-05-10 | Procede et installation d'extraction sans solvant de produits naturels par micro-ondes |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0698076A1 true EP0698076A1 (fr) | 1996-02-28 |
EP0698076B1 EP0698076B1 (fr) | 1998-01-14 |
Family
ID=9447117
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP94915607A Expired - Lifetime EP0698076B1 (fr) | 1993-05-11 | 1994-05-10 | Procede et installation d'extraction sans solvant de produits naturels par micro-ondes |
Country Status (16)
Country | Link |
---|---|
EP (1) | EP0698076B1 (fr) |
JP (1) | JPH08512337A (fr) |
CN (1) | CN1059920C (fr) |
AT (1) | ATE162211T1 (fr) |
AU (1) | AU682035B2 (fr) |
BG (1) | BG62367B1 (fr) |
BR (1) | BR9406717A (fr) |
CA (1) | CA2161127C (fr) |
DE (1) | DE69407965T2 (fr) |
DK (1) | DK0698076T3 (fr) |
ES (1) | ES2114688T3 (fr) |
FR (1) | FR2705035B1 (fr) |
GR (1) | GR3026603T3 (fr) |
HU (1) | HU218708B (fr) |
RU (1) | RU2115700C1 (fr) |
WO (1) | WO1994026853A1 (fr) |
Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1439218A1 (fr) * | 2003-01-21 | 2004-07-21 | Milestone S.r.l. | Extraction par microondes sans utilisation de solvant, de composés naturels volatils |
FR2955331A1 (fr) * | 2010-01-15 | 2011-07-22 | Archimex Pibs | Procede et installation d'extraction de biomasse assistee par micro-onde |
WO2012056141A2 (fr) | 2010-10-29 | 2012-05-03 | Bernard Mompon | Procédé de fabrication d'articles d'origine végétale imprégnés de substance liquide végétale |
WO2012156361A1 (fr) | 2011-05-13 | 2012-11-22 | Universite D'avignon Et Des Pays De Vaucluse | Obtention d'un extrait végétal à l'aide de micro-ondes |
FR3003181A1 (fr) * | 2013-03-18 | 2014-09-19 | Innovation & Dev Company Idco | Procede et installation d'extraction de produits biologiques par micro-ondes. |
FR3017309A1 (fr) | 2014-02-10 | 2015-08-14 | Idco | Procede d'extraction de produits biologiques par recyclage de solvant en couche mince assistee par micro-ondes |
CN106190574A (zh) * | 2016-07-28 | 2016-12-07 | 河南科技学院 | 一种茅苍术挥发油及其制备方法 |
WO2019106313A1 (fr) | 2017-12-01 | 2019-06-06 | Université D'avignon Et Des Pays De Vaucluse | Dispositif d'extraction et de séparation de composés volatils et non-volatils d'une matière biologique et procédé associé |
FR3099991A1 (fr) | 2019-08-22 | 2021-02-26 | Société de Courtage et de Diffusion - CODIF INTERNATIONAL | Ingrédient de composition cosmétique pour cuir chevelu sensible |
FR3113248A1 (fr) | 2020-08-04 | 2022-02-11 | Société de Courtage et de Diffusion - CODIF INTERNATIONAL | Extrait de cellules de Lavandula stoechas, compositions le comprenant, utilisations cosmétiques et procédé de culture des cellules de Lavandula stoechas. |
FR3115695A1 (fr) | 2020-10-30 | 2022-05-06 | Société de Courtage et de Diffusion - CODIF INTERNATIONAL | Principe actif constitué d’un extrait de pomme amère activant des récepteurs à l’amertume Tas2Rs présents sur la peau humaine et utilisations cosmétiques et dermato-cosmétiques correspondantes. |
Families Citing this family (52)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2763795B1 (fr) * | 1997-05-30 | 1999-08-20 | Archimex Pibs | Procede de preparation de vegetaux tels que les epices, les plantes aromatiques et les aromates |
FR2793008B1 (fr) | 1999-04-30 | 2001-07-27 | Valeurs Bois Ind | Procede d'extraction de jus naturel de matieres vegetales ligneuses, dispositif permettant la mise en oeuvre du procede et utilisation du procede pour la production de vegetaux ligneux seches |
FR2787347B1 (fr) * | 1998-12-17 | 2001-01-19 | Gattefosse Ets Sa | Procede de fabrication d'une emulsion a base de materiel vegetal aromatique, emulsion susceptible d'etre obtenue par ledit procede et utilisation de ladite emulsion |
CN1112953C (zh) * | 1999-10-29 | 2003-07-02 | 汤大卫 | 一种液相/固相萃取的方法 |
CN1120736C (zh) * | 2000-09-14 | 2003-09-10 | 中国科学院山西煤炭化学研究所 | 工业用固体物料抽提法 |
DE502004004959D1 (de) * | 2004-07-20 | 2007-10-25 | Milestone Srl | Mikrowellen-unterstützte Extraktion von flüchtigen Naturstoffen |
CN100379754C (zh) * | 2004-11-22 | 2008-04-09 | 王煊 | 一种微波无溶剂加热萃取皂甙的方法 |
CN100421759C (zh) * | 2006-03-10 | 2008-10-01 | 山东轻工业学院 | 一种用于植物有效成分提取的减压微波萃取装置和方法 |
EP2011568B1 (fr) * | 2006-03-16 | 2016-08-24 | Universidad Tecnica Federico Santa Maria (Usm) | Dispositif d'extraction de composés chimiques organiques à propriétés toxiques présents dans des échantillons atmosphériques, au moyen de solvants chauffés par des micro-ondes focalisées dans des systèmes ouverts (n'ayant pas été mis sous pression) |
CN101290277B (zh) * | 2007-04-20 | 2011-05-11 | 财团法人食品工业发展研究所 | 利用微波辐射的快速提取方法 |
TW200842336A (en) * | 2007-04-26 | 2008-11-01 | Food Industry Res & Dev Inst | Microwave accelerating extraction equipment |
FR2925898A1 (fr) * | 2007-12-28 | 2009-07-03 | Jean Pierre Lablanchy | Procede et systeme d'extraction d'huile essentielle a forte teneur en thymoquinone a partir de la plante de nigella sativa |
JP5508388B2 (ja) * | 2009-02-26 | 2014-05-28 | エステー株式会社 | 高モノテルペン成分含有精油、その製造方法および当該精油を用いた環境汚染物質浄化方法 |
RU2395766C1 (ru) * | 2009-05-25 | 2010-07-27 | Закрытое Акционерное Общество "Твин Трейдинг Компани" | Способ сушки материалов растительного, животного происхождения, рыбы и морепродуктов и устройство для его осуществления |
JP2011052086A (ja) * | 2009-08-31 | 2011-03-17 | Actree Corp | 蘚苔類からの油脂類抽出方法 |
JP6087485B2 (ja) * | 2010-02-25 | 2017-03-01 | エステー株式会社 | 芳香組成物およびこれを利用した芳香剤、消臭剤並びに抗菌剤 |
TWI468506B (zh) * | 2011-01-17 | 2015-01-11 | Nat Univ Chung Hsing | 微波輔助萃取微藻油脂方法及其應用 |
CN102252889A (zh) * | 2011-03-15 | 2011-11-23 | 重庆大学 | 微波辅助无溶剂固相顶空提取装置及其提取方法 |
LV14481B (lv) * | 2011-11-21 | 2012-06-20 | Latvijas Valsts Mežzinātnes Institūts 'silava' | Ūdenī nešķīstošu un ūdenī šķīstošu ēterisko eļļu iegūšanas paņēmiens no augu izejvielām |
RU2473356C1 (ru) * | 2011-12-07 | 2013-01-27 | Общество с ограниченной ответственностью "Компания Клевер" | Способ получения водных экстрактов из растительного сырья с повышенным содержанием извлекаемых активных веществ |
US9486716B2 (en) * | 2012-03-14 | 2016-11-08 | State Of Oregon Acting By And Through The State Board Of Higher Education On Behalf Of Oregon State University | Essential oil extraction apparatus |
CN103194312A (zh) * | 2013-03-24 | 2013-07-10 | 西北农林科技大学 | 一种从柏叶中提取挥发油的方法 |
FR3013563B1 (fr) * | 2013-11-28 | 2017-06-30 | Finat Conseil & Distrib | Procede de fabrication de preparations aromatisantes naturelles et stables et preparations aromatisantes obtenues par le dit procede |
CN103725420B (zh) * | 2013-12-20 | 2016-07-13 | 江南大学 | 一种提取黑种草属植物种子挥发油的方法、装置及应用 |
CN103820218A (zh) * | 2014-03-07 | 2014-05-28 | 张家界金绿油脂有限责任公司 | 一种油菜籽微波提取油脂的方法 |
JP5899604B2 (ja) * | 2014-03-24 | 2016-04-06 | 兼松エンジニアリング株式会社 | マイクロ波を利用したバイオマス再資源化装置 |
TWI601565B (zh) * | 2014-06-05 | 2017-10-11 | Timing Pharmaceutical Co Ltd | Essential oil extraction device |
CN104327951A (zh) * | 2014-10-23 | 2015-02-04 | 郑州工业应用技术学院 | 一种热空气精油提取装置 |
CN104872605B (zh) * | 2014-12-08 | 2018-02-06 | 中国热带农业科学院南亚热带作物研究所 | 制备液熏香料的方法和液熏香料 |
RO130896A0 (ro) * | 2015-01-19 | 2016-02-26 | Mariana Pătraşcu | Reactor continuu pentru extracţia asistată de microunde şi ultrasunete a compuşilor biologic activi din plante |
CN104711121A (zh) * | 2015-02-28 | 2015-06-17 | 湖北中烟工业有限责任公司 | 一种超声辅助无溶剂微波萃取野菊花精油的方法 |
CN104784965B (zh) * | 2015-04-20 | 2016-10-05 | 张新泉 | 一种中药微波萃取装置 |
RU2582292C1 (ru) * | 2015-05-07 | 2016-04-20 | федеральное государственное автономное образовательное учреждение высшего образования "Российский университет дружбы народов" (РУДН) | Способ выделения эфирного масла из лекарственного растительного сырья |
CN105219526A (zh) * | 2015-09-25 | 2016-01-06 | 四川省林业科学研究院 | 一种油樟油微波提取装置及方法 |
CN105250180B (zh) * | 2015-11-09 | 2018-11-27 | 北京工商大学 | 一种玫瑰鲜活水及其制备方法与应用 |
CN105213273B (zh) * | 2015-11-09 | 2018-11-13 | 北京工商大学 | 一种柠檬鲜活水及其制备方法与应用 |
CN105232782B (zh) * | 2015-11-09 | 2019-11-22 | 北京工商大学 | 一种鲜茶鲜活水及其制备方法与应用 |
CN105213272B (zh) * | 2015-11-09 | 2019-02-01 | 北京工商大学 | 一种薰衣草鲜活水及其制备方法与应用 |
CN105232400B (zh) * | 2015-11-09 | 2018-11-02 | 北京工商大学 | 一种茉莉鲜活水及其制备方法与应用 |
CN105713726A (zh) * | 2016-03-31 | 2016-06-29 | 李颖 | 一种快速无溶剂萃取天然植物精油和纯露的方法及装置 |
JP2017008111A (ja) * | 2016-10-17 | 2017-01-12 | エステー株式会社 | 芳香組成物およびこれを利用した芳香剤、消臭剤並びに抗菌剤 |
RU2636155C1 (ru) * | 2016-12-20 | 2017-11-21 | Федеральное Государственное Бюджетное Образовательное Учреждение Высшего Образования "Нижегородская Государственная Сельскохозяйственная Академия" (ФГБОУ ВО НГСХА) | Микроволновая технология извлечения жира из жиросодержащего сырья |
RU2649024C1 (ru) * | 2017-01-10 | 2018-03-29 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Кубанский государственный технологический университет" (ФГБОУ ВО "КубГТУ") | Способ получения эфирного масла мяты перечной |
FR3066703B1 (fr) * | 2017-05-24 | 2020-10-16 | Erpim | Procede et dispositif d’extraction solide/liquide a contre-courant comportant une etape de sechage |
CN111051484A (zh) * | 2017-08-31 | 2020-04-21 | 弗门尼舍有限公司 | 从植物生物质中微波辅助提取精油 |
JP6359752B1 (ja) * | 2017-12-22 | 2018-07-18 | 日本フレーバー工業株式会社 | バニラエキストラクトの製造方法及びバニラエキストラクト |
CN110747060A (zh) * | 2019-10-21 | 2020-02-04 | 华侨大学 | 一种超声辅助无溶剂微波萃取互叶白千层精油的方法 |
KR20230116912A (ko) * | 2020-12-08 | 2023-08-04 | 에스테 가부시키가이샤 | 배설물 처리재 및 이것을 이용한 배설물의 소취 방법 |
CN112760166A (zh) * | 2021-01-08 | 2021-05-07 | 四川轻化工大学 | 藤椒油生产设备 |
JPWO2022163063A1 (fr) * | 2021-01-28 | 2022-08-04 | ||
CN113388459B (zh) * | 2021-05-26 | 2022-03-01 | 宁波芮颂生物科技有限公司 | 一种抗猫、狗过敏原整理组合物溶液的制备方法 |
US11702615B1 (en) | 2022-03-09 | 2023-07-18 | Chemtech Services, Inc. | Microwave extraction of essential oils |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CA1336968C (fr) * | 1989-05-16 | 1995-09-12 | J. R. Jocelyn Pare | Methode amelioree d'extraction de produits naturels a l'aide d'energie ondulatoire |
SE9003593D0 (sv) * | 1990-11-12 | 1990-11-12 | T G Owe Berg | Foerfarande foer omvandling av vaerme till arbete |
DE69024961T2 (de) * | 1990-11-16 | 1996-08-14 | United Kingdom Government | Mikrowellenaussonderung von flüchtigen Ölen und Vorrichtung dafür |
-
1993
- 1993-05-11 FR FR9305810A patent/FR2705035B1/fr not_active Expired - Fee Related
-
1994
- 1994-05-10 DE DE69407965T patent/DE69407965T2/de not_active Expired - Lifetime
- 1994-05-10 RU RU95122234A patent/RU2115700C1/ru active
- 1994-05-10 BR BR9406717A patent/BR9406717A/pt not_active IP Right Cessation
- 1994-05-10 CN CN94192507A patent/CN1059920C/zh not_active Expired - Fee Related
- 1994-05-10 JP JP6525060A patent/JPH08512337A/ja not_active Ceased
- 1994-05-10 EP EP94915607A patent/EP0698076B1/fr not_active Expired - Lifetime
- 1994-05-10 HU HU9503230A patent/HU218708B/hu not_active IP Right Cessation
- 1994-05-10 DK DK94915607T patent/DK0698076T3/da active
- 1994-05-10 WO PCT/FR1994/000551 patent/WO1994026853A1/fr active IP Right Grant
- 1994-05-10 CA CA002161127A patent/CA2161127C/fr not_active Expired - Fee Related
- 1994-05-10 AU AU67251/94A patent/AU682035B2/en not_active Ceased
- 1994-05-10 ES ES94915607T patent/ES2114688T3/es not_active Expired - Lifetime
- 1994-05-10 AT AT94915607T patent/ATE162211T1/de not_active IP Right Cessation
-
1995
- 1995-12-04 BG BG100187A patent/BG62367B1/bg unknown
-
1998
- 1998-04-10 GR GR980400799T patent/GR3026603T3/el unknown
Non-Patent Citations (1)
Title |
---|
See references of WO9426853A1 * |
Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1439218A1 (fr) * | 2003-01-21 | 2004-07-21 | Milestone S.r.l. | Extraction par microondes sans utilisation de solvant, de composés naturels volatils |
FR2955331A1 (fr) * | 2010-01-15 | 2011-07-22 | Archimex Pibs | Procede et installation d'extraction de biomasse assistee par micro-onde |
WO2012056141A2 (fr) | 2010-10-29 | 2012-05-03 | Bernard Mompon | Procédé de fabrication d'articles d'origine végétale imprégnés de substance liquide végétale |
WO2012156361A1 (fr) | 2011-05-13 | 2012-11-22 | Universite D'avignon Et Des Pays De Vaucluse | Obtention d'un extrait végétal à l'aide de micro-ondes |
FR3003181A1 (fr) * | 2013-03-18 | 2014-09-19 | Innovation & Dev Company Idco | Procede et installation d'extraction de produits biologiques par micro-ondes. |
FR3017309A1 (fr) | 2014-02-10 | 2015-08-14 | Idco | Procede d'extraction de produits biologiques par recyclage de solvant en couche mince assistee par micro-ondes |
CN106190574A (zh) * | 2016-07-28 | 2016-12-07 | 河南科技学院 | 一种茅苍术挥发油及其制备方法 |
WO2019106313A1 (fr) | 2017-12-01 | 2019-06-06 | Université D'avignon Et Des Pays De Vaucluse | Dispositif d'extraction et de séparation de composés volatils et non-volatils d'une matière biologique et procédé associé |
FR3099991A1 (fr) | 2019-08-22 | 2021-02-26 | Société de Courtage et de Diffusion - CODIF INTERNATIONAL | Ingrédient de composition cosmétique pour cuir chevelu sensible |
FR3113248A1 (fr) | 2020-08-04 | 2022-02-11 | Société de Courtage et de Diffusion - CODIF INTERNATIONAL | Extrait de cellules de Lavandula stoechas, compositions le comprenant, utilisations cosmétiques et procédé de culture des cellules de Lavandula stoechas. |
FR3115695A1 (fr) | 2020-10-30 | 2022-05-06 | Société de Courtage et de Diffusion - CODIF INTERNATIONAL | Principe actif constitué d’un extrait de pomme amère activant des récepteurs à l’amertume Tas2Rs présents sur la peau humaine et utilisations cosmétiques et dermato-cosmétiques correspondantes. |
Also Published As
Publication number | Publication date |
---|---|
DE69407965D1 (de) | 1998-02-19 |
BG100187A (bg) | 1996-05-31 |
FR2705035A1 (fr) | 1994-11-18 |
GR3026603T3 (en) | 1998-07-31 |
AU682035B2 (en) | 1997-09-18 |
HUT75578A (en) | 1997-05-28 |
CN1125461A (zh) | 1996-06-26 |
CA2161127A1 (fr) | 1994-11-24 |
BG62367B1 (bg) | 1999-09-30 |
ATE162211T1 (de) | 1998-01-15 |
AU6725194A (en) | 1994-12-12 |
JPH08512337A (ja) | 1996-12-24 |
HU9503230D0 (en) | 1996-01-29 |
EP0698076B1 (fr) | 1998-01-14 |
HU218708B (hu) | 2000-11-28 |
DK0698076T3 (da) | 1998-09-14 |
ES2114688T3 (es) | 1998-06-01 |
WO1994026853A1 (fr) | 1994-11-24 |
CA2161127C (fr) | 2005-09-27 |
BR9406717A (pt) | 1996-02-06 |
RU2115700C1 (ru) | 1998-07-20 |
CN1059920C (zh) | 2000-12-27 |
FR2705035B1 (fr) | 1995-08-04 |
DE69407965T2 (de) | 1998-09-10 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
EP0698076B1 (fr) | Procede et installation d'extraction sans solvant de produits naturels par micro-ondes | |
US7001629B1 (en) | Method and plant for solvent-free microwave extraction of natural products | |
EP0398798B1 (fr) | Extraction de produits naturels assistée par micro-ondes | |
EP1261684B1 (fr) | Procede de fractionnement d'une huile de cuisson | |
EP0238527B1 (fr) | Procede et dispositif pour l'extraction de constituants par un fluide supercritique ou un liquide sous pression | |
FR2817556A1 (fr) | Procede et appareil de valorisation integrale des drupes oleiferes, en particulier des olives et les produits specifiques obtenus | |
CN1061729A (zh) | 微波辅助的萃取方法及其设备 | |
FR3032892A1 (fr) | Dispositif et procede pour l'extraction assistee de l'actif d'un produit | |
US5338557A (en) | Microwave extraction of volatile oils | |
FR3003181A1 (fr) | Procede et installation d'extraction de produits biologiques par micro-ondes. | |
FR3074425A1 (fr) | Dispositif d’extraction et de separation de composes volatiles et non-volatiles d’une matiere biologique et procede associe | |
EP3362078B1 (fr) | Nouveau solvant d'extraction et/ou de solubilisation organique, procédé d'extraction mettant en oeuvre ledit solvant, et extraits issus dudit procédé | |
FR2955331A1 (fr) | Procede et installation d'extraction de biomasse assistee par micro-onde | |
WO1995003380A1 (fr) | Procede d'extraction des huiles essentielles vegetales par maceration a froid et de deterpenation a froid | |
EP1109464A1 (fr) | Processus de traitement thermo-mecanique par detente instantanee controlee des fruits, jus et peaux d'agrumes | |
FR2763795A1 (fr) | Procede de preparation de vegetaux tels que les epices, les plantes aromatiques et les aromates | |
WO2021219963A1 (fr) | Procede d'extraction d'odeur a partir d'une matiere vegetale, notamment de fleurs muettes, sous forme solide | |
WO1989000187A1 (fr) | Procede d'extraction des huiles essentielles de plantes aromatiques et produits obtenus | |
WO2024002842A1 (fr) | Système et procédé d'extraction de molécules volatiles provenant de matière première végétale | |
FR2960000A1 (fr) | Procede destine a reduire la teneur en furocoumarines lors de la preparation d'une huile essentielle | |
IL111684A (en) | Process and installation for extracting products of biological origin without solvents using microwave heating | |
FR3141353A1 (fr) | Dispositif DIY basé sur la macération par micro-ondes pour l’obtention d’huiles aromatisées | |
CH270047A (fr) | Procédé pour éliminer de l'eau d'un produit, et dispositif pour la mise en oeuvre de ce procédé. | |
BE569278A (fr) | ||
CH269796A (fr) | Procédé et installation pour l'extraction, sous forme d'émulsions et à partir de matières oléagineuses d'origine végétale, de matières grasses destinées à des usages techniques. |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
|
17P | Request for examination filed |
Effective date: 19951113 |
|
AK | Designated contracting states |
Kind code of ref document: A1 Designated state(s): AT BE CH DE DK ES FR GB GR IE IT LI LU MC NL PT SE |
|
17Q | First examination report despatched |
Effective date: 19960607 |
|
GRAG | Despatch of communication of intention to grant |
Free format text: ORIGINAL CODE: EPIDOS AGRA |
|
GRAG | Despatch of communication of intention to grant |
Free format text: ORIGINAL CODE: EPIDOS AGRA |
|
GRAH | Despatch of communication of intention to grant a patent |
Free format text: ORIGINAL CODE: EPIDOS IGRA |
|
GRAH | Despatch of communication of intention to grant a patent |
Free format text: ORIGINAL CODE: EPIDOS IGRA |
|
GRAA | (expected) grant |
Free format text: ORIGINAL CODE: 0009210 |
|
AK | Designated contracting states |
Kind code of ref document: B1 Designated state(s): AT BE CH DE DK ES FR GB GR IE IT LI LU MC NL PT SE |
|
REF | Corresponds to: |
Ref document number: 162211 Country of ref document: AT Date of ref document: 19980115 Kind code of ref document: T |
|
REG | Reference to a national code |
Ref country code: CH Ref legal event code: EP |
|
REF | Corresponds to: |
Ref document number: 69407965 Country of ref document: DE Date of ref document: 19980219 |
|
ITF | It: translation for a ep patent filed |
Owner name: PORTA CHECCACCI E BOTTI S.R.L. |
|
GBT | Gb: translation of ep patent filed (gb section 77(6)(a)/1977) |
Effective date: 19980414 |
|
REG | Reference to a national code |
Ref country code: ES Ref legal event code: FG2A Ref document number: 2114688 Country of ref document: ES Kind code of ref document: T3 |
|
REG | Reference to a national code |
Ref country code: IE Ref legal event code: FG4D Free format text: 78404 |
|
REG | Reference to a national code |
Ref country code: PT Ref legal event code: SC4A Free format text: AVAILABILITY OF NATIONAL TRANSLATION Effective date: 19980407 |
|
REG | Reference to a national code |
Ref country code: DK Ref legal event code: T3 |
|
PLBE | No opposition filed within time limit |
Free format text: ORIGINAL CODE: 0009261 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT |
|
26N | No opposition filed | ||
REG | Reference to a national code |
Ref country code: GB Ref legal event code: IF02 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: CH Payment date: 20020429 Year of fee payment: 9 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: IE Payment date: 20020508 Year of fee payment: 9 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: BE Payment date: 20020517 Year of fee payment: 9 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: PT Payment date: 20020520 Year of fee payment: 9 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: GR Payment date: 20020523 Year of fee payment: 9 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: SE Payment date: 20020524 Year of fee payment: 9 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: LU Payment date: 20020527 Year of fee payment: 9 Ref country code: DK Payment date: 20020527 Year of fee payment: 9 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: NL Payment date: 20020528 Year of fee payment: 9 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: MC Payment date: 20020529 Year of fee payment: 9 Ref country code: AT Payment date: 20020529 Year of fee payment: 9 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: LU Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20030510 Ref country code: AT Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20030510 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: SE Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20030511 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: IE Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20030512 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: LI Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20030531 Ref country code: CH Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20030531 Ref country code: BE Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20030531 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: MC Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20030915 |
|
BERE | Be: lapsed |
Owner name: *ARCHIMEX Effective date: 20030531 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: PT Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20031130 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: NL Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20031201 Ref country code: DK Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20031201 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: GR Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20031203 |
|
REG | Reference to a national code |
Ref country code: DK Ref legal event code: EBP |
|
EUG | Se: european patent has lapsed | ||
REG | Reference to a national code |
Ref country code: CH Ref legal event code: PL |
|
NLV4 | Nl: lapsed or anulled due to non-payment of the annual fee |
Effective date: 20031201 |
|
REG | Reference to a national code |
Ref country code: PT Ref legal event code: MM4A Free format text: LAPSE DUE TO NON-PAYMENT OF FEES Effective date: 20031130 |
|
REG | Reference to a national code |
Ref country code: IE Ref legal event code: MM4A |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: GB Payment date: 20090521 Year of fee payment: 16 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: ES Payment date: 20100520 Year of fee payment: 17 |
|
REG | Reference to a national code |
Ref country code: FR Ref legal event code: TP |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: IT Payment date: 20100519 Year of fee payment: 17 Ref country code: DE Payment date: 20100609 Year of fee payment: 17 |
|
GBPC | Gb: european patent ceased through non-payment of renewal fee |
Effective date: 20100510 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: GB Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20100510 |
|
REG | Reference to a national code |
Ref country code: DE Ref legal event code: R119 Ref document number: 69407965 Country of ref document: DE |
|
REG | Reference to a national code |
Ref country code: DE Ref legal event code: R119 Ref document number: 69407965 Country of ref document: DE |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: IT Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20110510 |
|
REG | Reference to a national code |
Ref country code: ES Ref legal event code: FD2A Effective date: 20120717 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: ES Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20110511 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: DE Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20111130 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: FR Payment date: 20130530 Year of fee payment: 20 |
|
REG | Reference to a national code |
Ref country code: FR Ref legal event code: TP Owner name: SAS AMADEITE, FR Effective date: 20141119 |