EP0698076B1 - Method and plant for solvent-free microwave extraction of natural products - Google Patents
Method and plant for solvent-free microwave extraction of natural products Download PDFInfo
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- EP0698076B1 EP0698076B1 EP94915607A EP94915607A EP0698076B1 EP 0698076 B1 EP0698076 B1 EP 0698076B1 EP 94915607 A EP94915607 A EP 94915607A EP 94915607 A EP94915607 A EP 94915607A EP 0698076 B1 EP0698076 B1 EP 0698076B1
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- biological material
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- natural product
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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
- C11B9/027—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.
- Extraction of natural products from biological material can be carried out according to several methods, whether or not employing one or more extraction solvents, depending on the nature of the biological material used and that of the product or products you want to extract from it. It should be noted on this subject 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 products and non-volatile, are conventionally obtained in the presence of at least one solvent organic.
- Essential oils mainly consisting of volatile compounds odorants are generally obtained by distillation with water vapor (hydrodistillation) and / or by mechanical processes.
- oilseeds, essential oils citrus peel, fish oil ... is conventionally carried out using physical processes such as grinding and / or pressing, in the absence of solvent or by hydrodistillation.
- physical processes such as grinding and / or pressing, in the absence of solvent or by hydrodistillation.
- such techniques have the advantage of making it possible to obtain products of extraction (and biological material after extraction) free of solvents and therefore do not have to undergo a subsequent treatment for the elimination of such residues.
- the diffusion of the extracted product could be greatly improved by subjecting biological material a pretreatment which may consist in particular of a grinding, enzymatic digestion or even drying.
- a pretreatment which may consist in particular of a grinding, enzymatic digestion or even drying.
- sonication processes consisting in applying ultrasound to the mixture formed by the biological material and the solvent in order to favor the passage of the extract in the solvent.
- the mechanical waves formed by the ultrasound indeed allow locally generate a cavitation of the biological material and consequently a heating thereof promoting the release of the extract.
- EP 0 485 668 also describes an extraction process involving an extraction liquid which may be a supercritical liquid.
- the objective of the present invention is to propose an extraction process by microwave of natural products, not having the disadvantages of state of the art processes.
- one of the objectives of the invention is to provide such a method allowing extraction in the absence of solvent and therefore obtaining an extract free of any solvent residue.
- Another object of the invention is to propose such a process without both require excessive energy intake, for a given amount of biological material to be treated.
- Another objective of the invention is to propose an installation for the implementation of such a method.
- Such a method can be advantageously implemented on all natural biological materials, whether of animal, plant or micro-biological origin since 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 fish, but also from algae, microalgae and even possibly microorganisms.
- this biological material may, depending on its nature, be subdivided before being introduced in the enclosure to increase its microwave exposure factor.
- the process according to the invention makes it possible to carry out the hydrodistillation of product that we want to extract, not thanks to water brought from outside to during the process, but thanks to the water contained in the treated biological material.
- this water will be called water of constitution, when it may have been previously brought biological material, when it is available in dehydrated form, when a rehumidification stage.
- the method according to the invention therefore consists in subjecting the material biological treated with 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 decrease in pressure allows, on the one hand, to increase the mechanical stress exerted on the cell walls of biological material and secondly increase volatility of the azeotropic mixture constituted by the product which it is desired to extract and the water vapour.
- the concomitant heating of the enclosure makes it possible to compensate for the very rapid decrease in temperature resulting from evaporation water of constitution under the effect of the lowering of the pressure in the enclosure. Such a decrease in temperature is indeed likely to mask completely the action of microwaves.
- the method according to the invention has many advantages.
- the method according to the invention is much less consuming of energy that microwave assisted extraction processes the state of the technical.
- the energy used work in the context of the invention is also less than that necessary for hydrodistillation.
- 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 training of the extracted product and that the process does not using external water supply. Consequently, this residual material may easily be degraded thermally and therefore possibly recycled as combustible.
- said step of the method according to the invention consisting in the intermittent application of a reduced pressure, consists in subjecting the interior from said enclosure to cycles of depression.
- said heating step is preferably carried out at a temperature below 100 ° C. It should be noted that the process could be carried out at a temperature advantageously below 75 ° C so as to allow 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.
- a frequency at least equal to 300 MHz We will note however, in many countries the use of frequencies is very strictly regulated and that for example in France, only the frequencies of 915 MHz and 2450 MHz is authorized for industrial equipment generating microwaves.
- said microwave irradiation step will preferably be conducted so as to apply a power ranging from approximately 100 W to approximately 10,000 W per kilogram of product treated.
- said irradiation step in the microwave is carried out with mechanical stirring of said biological material. Such agitation will increase the exposure factor of the material organic in the microwave.
- said means for recovering the extract comprise means for refrigerating the water vapor containing the extract.
- said installation has means for operate said means for reducing the pressure inside the enclosure cyclically.
- said enclosure is provided with stirring means.
- said installation comprises means for redirecting the waste water obtained from the means recovery of the extract inside said enclosure.
- an extraction facility for natural products from biological material is shown schematically.
- Such a installation includes an enclosure 1 equipped with means 2 making it possible to generate microwaves in the interior volume it defines.
- 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 having a frequency of 915 MHz, this other frequency is also authorized in France).
- the enclosure 1 is moreover provided in its lower part with means agitation 9, constituted by a turbine with three blades, making it possible to agitate the biological material during its presence inside enclosure 1, when it is subjected to the action of microwaves.
- means agitation 9 constituted by a turbine with three blades, making it possible to agitate the biological material during its presence inside enclosure 1, when it is subjected to the action of microwaves.
- Such agitation increases exposure of biological material to microwaves and avoid certain areas of it are not sufficiently irradiated to carry out the operation extraction.
- the enclosure 1 is connected on the one hand with means 5 making it possible to reduce the pressure inside it 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 decrease 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 water pump.
- the means 6 for recovering the extracted product comprise a pipe 11 installed in the upper part of the enclosure 1, around which cooling means 7 are provided, formed by a coil in which circulates a coolant.
- Line 11 allows vapor recovery from the action of microwaves on biological material and in which the oil is found essential. 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 line 10 in 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 for 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.
- One kilogram of peppermint (Mentha piperita L., Hungarian variety) with 15% dry matter was placed inside the enclosure 1.
- the heating means 4 have been adjusted so that the thermostatically controlled wall 3 induce a temperature of around 70 ° C inside the enclosure 1 and the means agitation 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 minutes, 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 at the end 5 min, 10 min and 13 min.
- the temperature of the refrigeration medium circulating in the coil 7 has been set at 5 ° C so as to cause vapor condensation resulting from the action of microwaves on peppermint and containing oil essential.
- Example 1 The same amount of peppermint as in Example 1 was processed using the same operating conditions as in Example 1 but making operate pump 5 continuously so that the pressure at the interior of enclosure 1 is fixed at 250 mb during the entire extraction operation.
- sage sage (Salvia officinalis L.,) presenting 25% of dry matter has been placed inside enclosure 1.
- the means of heating 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 minutes, the power actually absorbed therefore been from 800 to 850 W.
- the pump 5 was implemented so as to lower the pressure to 250 mb. This pressure reduction was carried out at the end 3.5 min and 7 min.
- the temperature of the refrigeration medium circulating in the coil 7 has been set at 5 ° C so as to cause vapor condensation resulting from the action of microwaves on peppermint and containing oil essential.
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- 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)
Abstract
Description
L'invention concerne le domaine de l'extraction de produits naturels contenus dans un matériel biologique et notamment, mais non exclusivement, l'extraction de tels produits à partir de végétaux.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.
L'extraction des produits naturels à partir de matériel biologique peut être effectuée selon plusieurs procédés mettant ou non en oeuvre un ou plusieurs solvants d'extraction, selon la nature du matériel biologique utilisé et celle du produit ou des produits que l'on veut extraire de celui-ci. On notera à ce sujet que le nom donné à un extrait est souvent fonction de la technologie mise en oeuvre pour parvenir à son obtention. Ainsi, les concrètes, les résinoïdes, les oléorésines... qui sont des extraits constitués de composés volatils ou de produits cireux et gras et non volatils, sont classiquement obtenus en présence d'au moins un solvant organique. Les huiles essentielles, constituées principalement de composés volatils odorants sont, quant à elles, obtenues généralement par distillation avec de la vapeur d'eau (hydrodistillation) et/ou par des procédés mécaniques.Extraction of natural products from biological material can be carried out according to several methods, whether or not employing one or more extraction solvents, depending on the nature of the biological material used and that of the product or products you want to extract from it. It should be noted on this subject that the name given to an extract is often a function of the technology used to achieve it. Thus, the concretes, the resinoids, the oleoresins ... which are extracts consisting of volatile compounds or waxy and fatty products and non-volatile, are conventionally obtained in the presence of at least one solvent organic. Essential oils, mainly consisting of volatile compounds odorants are generally obtained by distillation with water vapor (hydrodistillation) and / or by mechanical processes.
A titre d'exemple, l'extraction des oléagineux, des huiles essentielles d'écorces d'agrumes, des huiles de poisson... est classiquement effectuée grâce à des procédés physiques tels que le broyage et/ou le pressage, en l'absence de solvant ou par hydrodistillation. Outre le fait qu'elles présentent un faible coût de mise en oeuvre, de telles techniques ont l'avantage de permettre l'obtention de produits d'extraction (et un matériel biologique après extraction) exempts de résidus de solvants et n'ayant donc pas à subir de traitement subséquent d'élimination de tels résidus.For example, the extraction of oilseeds, essential oils citrus peel, fish oil ... is conventionally carried out using physical processes such as grinding and / or pressing, in the absence of solvent or by hydrodistillation. Besides the fact that they have a low cost of implementation work, such techniques have the advantage of making it possible to obtain products of extraction (and biological material after extraction) free of solvents and therefore do not have to undergo a subsequent treatment for the elimination of such residues.
Il existe cependant de nombreux produits qui ne peuvent être extraits à partir du matériel naturel qui les contient selon de telles méthodes et pour lesquels il est nécessaire d'employer des techniques d'extraction utilisant des solvants organiques. Grâce à de telles techniques le produit à extraire diffuse dans le solvant et s'y dissout. Cependant, il est ensuite nécessaire de séparer le produit extrait du solvant, dans le but de permettre la concentration de l'extrait. De nombreux paramètres interviennent dans les rendements d'extraction effectuée en présence de solvant, au rang desquels on peut citer :
- la solubilité du produit extrait dans le solvant choisi,
- la diffusion du produit extrait au sein de la matrice solide du matériel biologique utilisé.
- the solubility of the product extracted in the chosen solvent,
- the diffusion of the extracted product within the solid matrix of the biological material used.
Il est possible d'agir sur le premier paramètre notamment en faisant varier la température opératoire ou encore la concentration du solvant employé.It is possible to act on the first parameter in particular by varying the operating temperature or the concentration of the solvent used.
Par ailleurs, il est possible d'agir également sur le second paramètre, soit préalablement à l'étape d'extraction, soit concomitamment à celle-ci. Par exemple, la diffusion du produit extrait pourra être grandement améliorée en faisant subir au matériel biologique un prétraitement pouvant consister notamment en un broyage, une digestion enzymatique ou encore un séchage. On pourra aussi choisir d'agir sur le matériel biologique durant l'opération même d'extraction, par exemple en le chauffant ou en l'agitant. On connaít ainsi dans l'état de la technique, des procédés de sonication consistant à appliquer des ultra-sons au mélange constitué par le matériel biologique et le solvant afin de favoriser le passage de l'extrait dans le solvant. Les ondes mécaniques constituées par les ultra-sons permettent en effet de générer localement une cavitation du matériel biologique et conséquemment un échauffement de celui-ci favorisant la libération de l'extrait.In addition, it is also possible to act on the second parameter, namely prior to the extraction step, or concomitantly with it. For example, the diffusion of the extracted product could be greatly improved by subjecting biological material a pretreatment which may consist in particular of a grinding, enzymatic digestion or even drying. We can also choose act on the biological material during the actual extraction operation, for example by heating or agitating it. We thus know in the prior art, sonication processes consisting in applying ultrasound to the mixture formed by the biological material and the solvent in order to favor the passage of the extract in the solvent. The mechanical waves formed by the ultrasound indeed allow locally generate a cavitation of the biological material and consequently a heating thereof promoting the release of the extract.
Il a également été proposé dans l'art antérieur de favoriser l'extraction d'un produit à partir d'un matériel biologique en soumettant celui-ci à une irradiation par des micro-ondes. L'action des micro-ondes sur les matériels biologiques est aujourd'hui bien connue. De telles ondes électro-magnétiques sont en effet absorbées sélectivement par les milieux possédant une constante diélectrique élevée et donc, dans le cas de matériel biologique, principalement par l'eau c'est-à-dire essentiellement par les tissus vasculaires et glandulaires et plus particulièrement les vacuoles dans le cas de matériel végétal. Lors d'une telle absorption, l'énergie du rayonnement est convertie en énergie calorifique, ce qui permet l'échauffement sélectif des parties du matériel biologique absorbant les micro-ondes.It has also been proposed in the prior art to favor the extraction of a produced from biological material by subjecting it to irradiation by microwaves. The action of microwaves on biological materials is well known today. Such electromagnetic waves are indeed selectively absorbed by media with a high dielectric constant and therefore, in the case of biological material, mainly by water, i.e. essentially by the vascular and glandular tissues and more particularly the vacuoles in the case of plant material. During such absorption, the energy of the radiation is converted into heat energy, which allows heating selective parts of biological material absorbing microwaves.
Le brevet européen EP 0398798 divulgue une technique d'extraction de produits à partir de matériel biologique assistée par micro-ondes, comprenant les étapes suivantes consistant à :
- subdiviser un matériel biologique (menthe poivrée, livèche écossaise, cèdre ou ail) possédant une composante dispersée absorbant les micro-ondes (l'eau),
- mettre ce matériel subdivisé dans un solvant transparent ou partiellement transparent aux micro-ondes et absorbant moins les micro-ondes que la composante dispersée, tel que l'hexane, l'éthanol ou le dichlorométhane,
- exposer le mélange constitué par le matériel subdivisé et le solvant aux micro-ondes afin de permettre l'extraction des produits solubles en chauffant le matériel subdivisé préférentiellement au solvant,
- séparer le matériel biologique résiduel du solvant et,
- récupérer le produit extrait.
- 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 the microwave and absorbing microwaves less than 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 preferably with solvent,
- separate the residual biological material from the solvent and,
- recover the extracted product.
Bien que présentant l'avantage d'améliorer les rendements d'extraction, la technique décrite dans le brevet EP 0398798 ne permet pas de s'affranchir des inconvénients déjà cités liés à la présence de solvant dans l'extrait obtenu.Although having the advantage of improving the extraction yields, the technique described in patent EP 0398798 does not overcome the disadvantages already mentioned linked to the presence of solvent in the extract obtained.
EP 0 485 668 décrit également un procédé d'extraction faisant intervenir un liquide d'extraction pouvant être un liquide supercritique.EP 0 485 668 also describes an extraction process involving an extraction liquid which may be a supercritical liquid.
On notera qu'il a également déjà été proposé dans l'état de la technique de procéder à l'extraction d'huile essentielles à partir d'un matériel biologique par irradiation aux micro-ondes et en l'absence de solvant.Note that it has also already been proposed in the state of the art extract essential oils from biological material by microwave irradiation and in the absence of solvent.
L'article paru dans la revue "Flavour and Fragrance journal", vol.4, pp 43-44
et ayant pour titre "Microwave Oven Extraction of an Essential Oil" décrit en
effet une technique d'extraction de l'huile essentielle de Lippia sidoides par
chauffage aux micro-ondes, selon laquelle des échantillons de plante de 30 à 40
grammes sont placés, en l'absence de tout solvant, dans un flacon à l'intérieur d'un
four micro-ondes et subissent une irradiation aux micro-ondes pendant une durée
de 5 mn. Le flacon utilisé est conçu de façon à permettre un entraínement de
l'huile essentielle par un flux d'air provenant de l'extérieur.The article published in the journal "Flavor and Fragrance journal", vol.4, pp 43-44
and entitled "Microwave Oven Extraction of an Essential Oil" described in
effect a technique of extracting the essential oil of Lippia sidoides by
microwave heating, whereby plant samples from 30 to 40
grams are placed, in the absence of any solvent, in a bottle inside a
microwave oven and undergo microwave irradiation for a period of
Bien qu'autorisant une extraction dans un temps beaucoup plus court que les temps nécessaires pour mener à bien les opérations d'extraction par hydrodistillation, une telle méthode présente l'inconvénient majeur de nécessiter un apport énergétique très important pour permettre l'extraction, ce qui en fait un procédé n'offrant aucun intérêt d'ordre économique. Although allowing extraction in a much shorter time than the time required to carry out the hydrodistillation extraction operations, such a method has the major drawback of requiring an intake very important energy to allow the extraction, which makes it a process offering no economic interest.
Tous les procédés d'extraction de produits naturels par micro-ondes décrits dans la littérature ne peuvent être mis en oeuvre que sur des masses de matériel biologique traité très faibles par rapport à la puissance des micro-ondes appliquées. Généralement cette puissance varie de 10 000 W à 20 000 W par kilogramme de matériel biologique. La puissance maximale des émetteurs de micro-ondes sur le marché, fonctionnant à une fréquence de 2450 MHz, est de 6 KW. En conséquence, ces procédés, pour être mis en oeuvre à l'échelle industrielle, doivent être adaptés à un fonctionnement en continu, afin de présenter ponctuellement une faible masse en face d'une source de micro-ondes de puissance raisonnable.All the processes for extracting natural products by microwave described in the literature can only be used on masses of material biological processed very low compared to the power of the microwaves applied. Generally this power varies from 10,000 W to 20,000 W per kilogram of biological material. The maximum power of microwave transmitters on the market, operating at a frequency of 2450 MHz, is 6 KW. Consequently, to be implemented on an industrial scale, these processes must be adapted to continuous operation, in order to present a small mass on time in front of a microwave source of reasonable power.
L'objectif de la présente invention est de proposer un procédé d'extraction par micro-ondes de produits naturels, ne présentant pas les inconvénients des procédés de l'état de la technique.The objective of the present invention is to propose an extraction process by microwave of natural products, not having the disadvantages of state of the art processes.
En particulier, un des objectifs de l'invention est de fournir un tel procédé permettant une extraction en l'absence de solvant et donc l'obtention d'un extrait exempt de tout résidu de solvant.In particular, one of the objectives of the invention is to provide such a method allowing extraction in the absence of solvent and therefore obtaining an extract free of any solvent residue.
Un autre objectif de l'invention est de proposer un tel procédé sans pour autant nécessiter un apport énergétique excessif, pour une quantité donnée de matériel biologique à traiter.Another object of the invention is to propose such a process without both require excessive energy intake, for a given amount of biological material to be treated.
Un autre objectif de l'invention est de proposer une installation pour la mise en oeuvre d'un tel procédé.Another objective of the invention is to propose an installation for the implementation of such a method.
L'invention concerne un procédé d'extraction par micro-ondes d'au moins un produit naturel à partir d'un matériel biologique, ledit procédé consistant à:
- placer ledit matériel biologique dans une enceinte, en l'absence de tout solvant,
- faire subir une irradiation aux micro-ondes audit matériel biologique présent dans ladite enceinte, afin de provoquer l'évaporation d'au moins une partie de l'eau contenue dans ledit matériel biologique et conséquemment l'éclatement des structures cellulaires dudit matériel biologique, de façon à permettre la libération d'au moins une partie dudit produit naturel,
- séparer le matériel biologique résiduel du produit naturel extrait, ledit procédé étant caractérisé en ce qu'il comprend les étapes complémentaires suivantes consistant à :
- appliquer, de façon intermittente, une pression réduite à l'intérieur de ladite enceinte durant ladite étape d'application des micro-ondes, afin de favoriser l'éclatement des structures cellulaire dudit matériel biologique induit par l'application des micro-ondes,
- chauffer, durant au moins l'essentiel de ladite étape d'application des micro-ondes, ladite enceinte, afin de compenser la chute de température résultant de l'évaporation de l'eau du matériel biologique,
- place 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 breakdown of the cellular structures of said biological material, so as to allow the release of at least part of said natural product,
- separating the residual biological material from the extracted natural product, said process 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 the bursting of the 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 the evaporation of the water from the biological material,
Un tel procédé peut être avantageusement mis en oeuvre sur tous les matériels biologiques naturels, qu'ils soient d'origine animale, végétale ou micro-biologique dès lors que ceux-ci contiennent au moins environ 30 % d'eau. Ce procédé pourra notamment être utilisé pour extraire des huiles essentielles à partir de plantes, de tissus d'origine animale et notamment de poissons, mais aussi à partir d'algues, de micro-algues et même éventuellement de micro-organismes. Bien sûr, ce matériel biologique pourra, selon sa nature, être subdivisé avant d'être introduit dans l'enceinte afin d'augmenter son facteur d'exposition aux micro-ondes.Such a method can be advantageously implemented on all natural biological materials, whether of animal, plant or micro-biological origin since 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 fish, but also from algae, microalgae and even possibly microorganisms. Of course, this biological material may, depending on its nature, be subdivided before being introduced in the enclosure to increase its microwave exposure factor.
Le procédé selon l'invention permet de réaliser l'hydrodistillation du produit que l'on désire extraire, non pas grâce à de l'eau apportée de l'extérieur au cours du procédé, mais grâce à l'eau contenue dans le matériel biologique traité. On notera à ce titre que, dans le cadre de la présente description, cette eau sera appelée eau de constitution, alors qu'elle pourra avoir été apportée préalablement au matériel biologique, lorsque celui-ci sera disponible sous forme déshydratée, lors d'une étape de réhumidification.The process according to the invention makes it possible to carry out the hydrodistillation of product that we want to extract, not thanks to water brought from outside to during the process, but thanks to the water contained in the treated biological material. It will be noted in this respect that, in the context of the present description, this water will be called water of constitution, when it may have been previously brought biological material, when it is available in dehydrated form, when a rehumidification stage.
Le procédé selon l'invention consiste donc à soumettre le matériel biologique traité à un rayonnement micro-ondes, en l'absence de solvant extractant, permettant au contenu des cellules de ce matériel d'être éjecté à l'extérieur. Afin de favoriser ce phénomène et dans le but de réaliser l'entraínement azéotropique du produit extrait, la pression de l'enceinte est réduite. Cette diminution de pression permet, d'une part, d'accroítre la contrainte mécanique exercée sur les parois des cellules du matériel biologique et d'autre part d'augmenter la volatilité du mélange azéotrope constitué par le produit que l'on souhaite extraire et la vapeur d'eau. Selon l'invention, le chauffage concomitant de l'enceinte permet de compenser la diminution très rapide de la température résultant de l'évaporation de l'eau de constitution sous l'effet de l'abaissement de la pression dans l'enceinte. Une telle diminution de température est en effet susceptible de masquer complètement l'action des micro-ondes.The method according to the invention therefore consists in subjecting the material biological treated with microwave radiation, in the absence of extracting solvent, allowing the contents of the cells of this material to be ejected outside. To to promote this phenomenon and in order to achieve azeotropic training of the extracted product, the pressure of the enclosure is reduced. This decrease in pressure allows, on the one hand, to increase the mechanical stress exerted on the cell walls of biological material and secondly increase volatility of the azeotropic mixture constituted by the product which it is desired to extract and the water vapour. According to the invention, the concomitant heating of the enclosure makes it possible to compensate for the very rapid decrease in temperature resulting from evaporation water of constitution under the effect of the lowering of the pressure in the enclosure. Such a decrease in temperature is indeed likely to mask completely the action of microwaves.
Le procédé selon l'invention présente de nombreux avantages.The method according to the invention has many advantages.
Outre le fait qu'il conduit à des extraits sans solvant résiduel, il permet de plus, par rapport à une hydrodistillation classique, d'obtenir un extrait de composition équivalente et avec un rendement équivalent, en un temps substantiellement plus court. Alors que les temps d'hydrodistillation classique se comptent généralement en heures, les temps d'hydrodistillation sous pression réduite selon l'invention se comptent en minutes. Pour certains produits, il est ainsi possible d'obtenir une quantité donnée d'extrait dix fois plus rapidement qu'avec une distillation classique à la vapeur d'eau.Besides the fact that it leads to extracts without residual solvent, it allows more, compared to a conventional hydrodistillation, to obtain an extract of equivalent composition and with equivalent yield, in substantially time shorter. While classic hydrodistillation times are counted generally in hours, the hydrodistillation times under reduced pressure according to the invention can be counted in minutes. For some products, it is thus possible to obtain a given amount of extract ten times faster than with a classic steam distillation.
Par ailleurs, le procédé selon l'invention est beaucoup moins consommateur d'énergie que les procédés d'extraction assistée par micro-ondes de l'état de la technique. Pour une même quantité de matériel biologique traité, l'énergie mise en oeuvre dans le cadre de l'invention est également moindre que celle nécessaire à une hydrodistillation. Dans le cadre d'une hydrodistillation, il est en effet nécessaire de chauffer le matériel biologique et l'eau ajoutée, dont la masse peut représenter jusqu'à 10 fois la masse de matériel biologique.Furthermore, the method according to the invention is much less consuming of energy that microwave assisted extraction processes the state of the technical. For the same quantity of biological material treated, the energy used work in the context of the invention is also less than that necessary for hydrodistillation. In the context of a 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.
Enfin, on notera que le matériel biologique résiduel obtenu à l'issue du procédé se présente sous une forme sèche, puisque l'eau de constitution qu'il contenait a servi à l'entraínement du produit extrait et que le procédé ne met pas en oeuvre d'apport extérieur d'eau. En conséquence, ce matériau résiduel pourra facilement être dégradé par voie thermique et donc éventuellement recyclé comme combustible.Finally, it should be noted that 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 training of the extracted product and that the process does not using external water supply. Consequently, this residual material may easily be degraded thermally and therefore possibly recycled as combustible.
Préférentiellement, ladite étape du procédé selon l'invention, consistant en l'application intermittente d'une pression réduite, consiste à soumettre l'intérieur de ladite enceinte à des cycles de dépression.Preferably, said step of the method according to the invention, consisting in the intermittent application of a reduced pressure, consists in subjecting the interior from said enclosure to cycles of depression.
Selon une variante de l'invention, ladite étape de séparation du matériel biologique résiduel de l'extrait consiste :
- à réfrigérer la vapeur d'eau contenant ledit produit naturel extrait,
- à décanter le mélange liquide résultant d'une telle réfrigération et,
- à séparer ledit produit naturel extrait et l'eau résultant d'une telle décantation.
- refrigerating the water vapor containing said extracted natural product,
- decanting the liquid mixture resulting from such refrigeration and,
- separating said extracted natural product and the water resulting from such decantation.
Bien qu'un autre avantage du procédé soit de conduire à l'obtention de beaucoup moins d'eau résiduaire que les procédés classiques d'hydrodistillation, au moins une partie de ladite eau résultant de ladite étape de décantation est avantageusement injectée dans l'enceinte pour effectuer l'hydrodistillation du produit naturel restant dans ledit résidu de matériel biologique.Although another advantage of the process is to lead to obtaining much less waste water than conventional hydrodistillation processes, at least at least part of said water resulting from said decantation step is advantageously injected into the enclosure to effect the hydrodistillation of the natural product remaining in said residue of biological material.
Par ailleurs, ladite étape de chauffage est préférentiellement menée à une température inférieure à 100°C. On notera que le procédé pourra être mené à une température avantageusement inférieure à 75°C de façon à permettre l'extraction de produits ayant tendance à se dégrader sous l'effet de la chaleur.Furthermore, said heating step is preferably carried out at a temperature below 100 ° C. It should be noted that the process could be carried out at a temperature advantageously below 75 ° C so as to allow extraction of products which tend to degrade under the effect of heat.
Les micro-ondes utilisées lors de ladite étape d'irradiation aux micro-ondes possèdent avantageusement une fréquence au moins égale à 300 MHz. On notera toutefois que dans de nombreux pays l'usage des fréquences est très strictement réglementé et que par exemple en France, seules les fréquences de 915 MHz et 2450 MHz sont autorisées pour les équipements industriels générant des micro-ondes.The microwaves used during said microwave irradiation step advantageously have a frequency at least equal to 300 MHz. We will note however, in many countries the use of frequencies is very strictly regulated and that for example in France, only the frequencies of 915 MHz and 2450 MHz is authorized for industrial equipment generating microwaves.
Par ailleurs, ladite étape d'irradiation aux micro-ondes sera préférentiellement menée de façon à appliquer une puissance allant d'environ 100 W à environ 10 000 W par kilogramme de produit traité. Furthermore, said microwave irradiation step will preferably be conducted so as to apply a power ranging from approximately 100 W to approximately 10,000 W per kilogram of product treated.
Selon une variante de mise en oeuvre du procédé, ladite étape d'irradiation aux micro-ondes est menée sous agitation mécanique dudit matériel biologique. Une telle agitation permettra d'augmenter le facteur d'exposition du matériel biologique aux micro-ondes.According to a variant implementation of the method, said irradiation step in the microwave is carried out with mechanical stirring of said biological material. Such agitation will increase the exposure factor of the material organic in the microwave.
L'invention concerne également une installation pour la mise en oeuvre d'un tel procédé caractérisée en ce qu'elle comprend:
- une enceinte pourvue de moyens de génération de micro-ondes à l'intérieur de ladite enceinte et présentant une double-paroi thermostatée ;
- des moyens de chauffage permettant de réguler la température de ladite double-paroi thermostatée ;
- des moyens permettant de réduire la pression à l'intérieur de ladite enceinte ;
- des moyens de récupération de l'extrait à sa sortie de ladite enceinte.
- an enclosure provided with means for generating microwaves inside said enclosure and having a thermostated double wall;
- heating means making it possible to regulate the temperature of said thermostated double wall;
- means for reducing the pressure inside said enclosure;
- means for recovering the extract on leaving said enclosure.
Préférentiellement, lesdits moyens de récupération de l'extrait comprennent des moyens de réfrigération de la vapeur d'eau contenant l'extrait.Preferably, said means for recovering the extract comprise means for refrigerating the water vapor containing the extract.
Egalement préférentiellement, ladite installation présente des moyens pour faire fonctionner lesdits moyens permettant de réduire la pression à l'intérieur de l'enceinte de façon cyclique.Also preferably, said installation has means for operate said means for reducing the pressure inside the enclosure cyclically.
Avantageusement, ladite enceinte est pourvue de moyens d'agitation.Advantageously, said enclosure is provided with stirring means.
Enfin, également avantageusement, ladite installation comprend des moyens permettant de réacheminer l'eau résiduaire obtenue au niveau des moyens de récupération de l'extrait à l'intérieur de ladite enceinte.Finally, also advantageously, said installation comprises means for redirecting the waste water obtained from the means recovery of the extract inside said enclosure.
L'invention, ainsi que les avantages qu'elle présente, seront plus facilement compris grâce à la description qui va suivre d'exemples de réalisation de celle-ci en référence aux dessins, dans lesquels :
- la figure 1 représente une vue schématique d'une installation selon l'invention ;
- la figure 2 traduit l'évolution de la pression de l'enceinte et de la température du matériel biologique, dans le cadre d'un premier exemple de mise en oeuvre du procédé selon l'invention avec l'installation schématisée à la figure 1, pour l'extraction d'huile essentielle de menthe poivrée ;
- la figure 3 représente l'évolution du rendement d'huile essentielle de menthe poivrée obtenu lors du premier exemple de mise en oeuvre du procédé ;
- la figure 4 traduit l'évolution de la pression de l'enceinte et de la température du matériel biologique, dans le cadre d'un exemple comparatif d'extraction d'huile essentielle de menthe poivrée ;
- la figure 5 représente l'évolution du rendement d'huile essentielle de menthe poivrée obtenu lors de l'exemple comparatif ;
- la figure 6 traduit l'évolution de la pression de l'enceinte et de la température du matériel biologique, dans le cadre d'un deuxième exemple de mise en oeuvre du procédé selon l'invention pour l'extraction d'huile essentielle de sauge officinale ;
- la figure 7 représente l'évolution du rendement d'huile essentielle de sauge officinale obtenu lors du deuxième exemple de mise en oeuvre du procédé selon l'invention.
- FIG. 1 represents 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, within the framework of a first example of implementation of the method according to the invention with the installation shown diagrammatically in FIG. 1, for the extraction of peppermint essential oil;
- FIG. 3 represents the change in the yield of peppermint essential oil obtained during the first example of implementation of the method;
- FIG. 4 translates the evolution of the pressure of the enclosure and the temperature of the biological material, within the framework of a comparative example of extraction of essential oil of peppermint;
- FIG. 5 represents the change in the yield of essential oil of peppermint obtained during the comparative example;
- FIG. 6 translates the evolution of the pressure of the enclosure and of the temperature of the biological material, within the framework of a second example of implementation of the method according to the invention for the extraction of essential oil of sage officinalis;
- FIG. 7 represents the evolution of the yield of essential oil of officinal sage obtained during the second example of implementation of the method according to the invention.
En référence à la figure 1, une installation d'extraction de produits naturels
à partir d'un matériel biologique est représentée schématiquement. Une telle
installation comprend une enceinte 1 équipée de moyens 2 permettant de générer
des micro-ondes dans le volume intérieur qu'elle délimite. Conformément aux
dispositions légales, ces moyens 2 permettent l'émission de micro-ondes présentant
une fréquence égale à 2450 MHz. (On notera qu'il aurait été également possible
d'utiliser un générateur de micro-ondes présentant une fréquence de 915 MHz, cet
autre fréquence étant également autorisée en France).Referring to Figure 1, an extraction facility for natural products
from biological material is shown schematically. Such a
installation includes an
L'enceinte 1, est par ailleurs munie dans sa partie inférieure de moyens
d'agitation 9, constitués par une turbine à trois pâles, permettant d'agiter le
matériel biologique au cours de sa présence à l'intérieur de l'enceinte 1, lorsqu'il
est soumis à l'action des micro-ondes. Une telle agitation permet d'augmenter
l'exposition du matériel biologique aux micro-ondes et d'éviter que certaines zones
de celui-ci ne soient insuffisamment irradiées pour mener à bien l'opération
d'extraction. The
Conformément à la présente invention, l'enceinte 1 est reliée d'une part
avec des moyens 5 permettant de réduire la pression régnant en son intérieur et,
d'autre part, avec des moyens de récupération 6 du produit naturel extrait grâce à
l'action des micro-ondes sur le matériel biologique. Les moyens 5 permettant de
diminuer la pression dans l'enceinte peuvent être constitués de tout moyen
classiquement utilisé à l'effet de créer un vide partiel à l'intérieur d'une enceinte,
tel que, par exemple, une pompe ou une trompe à eau. Dans le cadre du présent
exemple, les moyens 6 de récupération du produit extrait comprennent une
canalisation 11 installée dans la partie supérieure de l'enceinte 1, autour de laquelle
sont prévus des moyens de réfrigération 7 formés par un serpentin dans lequel
circule un liquide de refroidissement.In accordance with the present invention, the
La canalisation 11 permet de récupérer les vapeurs résultant de l'action des
micro-ondes sur le matériel biologique et dans lesquelles se trouve l'huile
essentielle. Grâce aux moyens de réfrigération 7 ces vapeurs d'eau sont condensées.
Un décanteur 12 est prévu à la sortie de la canalisation 11 pour récupérer ces
vapeurs condensées et séparer l'huile essentielle. L'eau résiduaire restante, après
décantation est avantageusement réacheminée, par une canalisation 10 dans
l'enceinte 1 où elle est recyclée pour compléter l'extraction.
Afin de permettre un réchauffement de l'intérieur de l'enceinte 1 pour
compenser la diminution de température résultant de l'abaissement de la pression
induit par la pompe à vide 5, l'enceinte 1 présente une double-paroi 3 thermostatée
reliée à des moyens de chauffage 4.In order to allow heating of the interior of the
L'installation ci-dessus décrite a été utilisée pour mettre en oeuvre le procédé d'extraction par micro-ondes de la présente invention afin d'extraire des huiles essentielles de menthe poivrée (exemples 1) et de sauge officinale (exemple 3).The installation described above was used to implement the microwave extraction method of the present invention for extracting essential oils of peppermint (examples 1) and officinal sage (example 3).
Un kilogramme de menthe poivrée (Mentha piperita L., variété hongroise)
présentant 15 % de matière sèche a été placée à l'intérieur de l'enceinte 1. Les
moyens de chauffage 4 ont été réglés de façon telle que la paroi thermostatée 3
induise une température d'environ 70°C à l'intérieur de l'enceinte 1 et les moyens
d'agitation 9 ont été mis en oeuvre de façon à présenter une vitesse de 40 tours par
minute.One kilogram of peppermint (Mentha piperita L., Hungarian variety)
with 15% dry matter was placed inside the
La puissance émise par les moyens 2 de génération de micro-ondes est de 1150 W et la puissance réfléchie varie entre 170 W et 220 W. Au cours de l'opération d'extraction, qui a duré 15 mn, la puissance effectivement absorbée a donc été de 930 à 980 W.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 minutes, the power actually absorbed therefore been from 930 to 980 W.
Au cours de l'extraction, la pompe 5 a été mise en oeuvre de façon à
abaisser la pression à 250 mb. Cet abaissement de pression a été effectué au bout
de 5 mn, 10 mn et 13 mn.During the extraction, the
Par ailleurs, la température du milieu de réfrigération circulant dans le serpentin 7 a été fixée à 5 °C de façon à provoquer la condensation des vapeurs résultant de l'action des micro-ondes sur la menthe poivrée et contenant l'huile essentielle.Furthermore, the temperature of the refrigeration medium circulating in the coil 7 has been set at 5 ° C so as to cause vapor condensation resulting from the action of microwaves on peppermint and containing oil essential.
L'évolution de la température de la menthe présente dans l'enceinte et de la pression régnant à l'intérieur de celle-ci est représentée à la figure 2. Sous l'action des micro-ondes, la température du produit passe rapidement de la température ambiante jusqu'à environ 75°C. Dès que l'intérieur de l'enceinte est mis sous vide partiel (250 mb) grâce à la pompe 5, la température chute. Cet baisse de température est rapidement compensée grâce au chauffage de l'enceinte de façon à ne pas masquer l'action des micro-ondes.The evolution of the temperature of the mint present in the enclosure and of the pressure inside it is shown in Figure 2. Under the action of microwaves, the temperature of the product rapidly changes from room temperature up to about 75 ° C. As soon as the interior of the enclosure is put under partial vacuum (250 mb) thanks to pump 5, the temperature drops. This drop temperature is quickly compensated by heating the enclosure so as not to mask the action of microwaves.
En référence à la figure 3, après 15 mn d'extraction et 3 cycles de dépression, 1,52 ml d'huile essentielle ont été récupérés (soit un rendement de 1,01 ml pour 100g de matière sèche).Referring to Figure 3, after 15 min of extraction and 3 cycles of depression, 1.52 ml of essential oil were recovered (i.e. a yield of 1.01 ml per 100g of dry matter).
L'hydrodistillation du résidu de menthe poivrée résultant d'une telle opération d'extraction par micro-ondes n'a permis de n'obtenir que moins de 50 mg d'huile essentielle. Le procédé selon l'invention autorise donc l'obtention de rendement en huile essentielle approchant l'épuisement du matériel biologique.Hydrodistillation of the peppermint residue resulting from such microwave extraction only obtained less than 50 mg essential oil. The method according to the invention therefore allows obtaining essential oil yield approaching the exhaustion of biological material.
La comparaison des profils de chromatographie en phase gazeuse deux huiles essentielles obtenues par le procédé d'extraction selon l'invention et par hydrodistillation classique n'a pas fait apparaítre de différence majeure de composition.Comparison of two gas chromatography profiles essential oils obtained by the extraction process according to the invention and by conventional hydrodistillation did not show any major difference from composition.
La même quantité de menthe poivrée que dans l'exemple 1 a été traitée
en utilisant les mêmes conditions opératoires que dans l'exemple 1 mais en faisant
fonctionner continûment la pompe 5 de façon telle que la pression régnant à
l'intérieur de l'enceinte 1 soit fixée à 250 mb durant toute l'opération d'extraction.The same amount of peppermint as in Example 1 was processed
using the same operating conditions as in Example 1 but making
operate
L'évolution de la température de la menthe et de la pression dans l'enceinte est donnée à la figure 4.The evolution of mint temperature and pressure in the enclosure is given in Figure 4.
En référence à la figure 5, le rendement en huile essentielle n'a alors été que de 0,2 ml pour 100g, soit 5 fois moindre que dans l'exemple 1. 1150 mg d'huile essentielle ont été récupérée dans le résidu de menthe après l'opération d'extraction. Ces résultats montrent l'importance du caractère intermittent qui doit être donné, selon l'invention, à l'abaissement de la pression à l'intérieur de l'enceinte.Referring to Figure 5, the essential oil yield was then than 0.2 ml per 100g, which is 5 times less than in Example 1. 1150 mg of oil essential were recovered in 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.
Cinq cents grammes de sauge officinale (Salvia officinalis L.,) présentant
25 % de matière sèche ont été placés à l'intérieur de l'enceinte 1. Les moyens de
chauffage 4 ont été réglés de façon telle que la paroi thermostatée 3 induise une
température d'environ 70°C à l'intérieur de l'enceinte 1 et les moyens d'agitation
9 ont été mis en oeuvre de façon à présenter une vitesse de 40 tours par minute.Five hundred grams of sage sage (Salvia officinalis L.,) presenting
25% of dry matter has been placed inside
La puissance émise par les moyens 2 de génération de micro-ondes est de 1000 W et la puissance réfléchie varie entre 150 W et 200 W. Au cours de l'opération d'extraction, qui a duré 10 mn, la puissance effectivement absorbée a donc été de 800 à 850 W.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 minutes, the power actually absorbed therefore been from 800 to 850 W.
Au cours de l'extraction, la pompe 5 a été mise en oeuvre de façon à
abaisser la pression à 250 mb. Cet abaissement de pression a été effectué au bout
de 3,5 mn et 7 mn.During the extraction, the
Par ailleurs, la température du milieu de réfrigération circulant dans le serpentin 7 a été fixée à 5 °C de façon à provoquer la condensation des vapeurs résultant de l'action des micro-ondes sur la menthe poivrée et contenant l'huile essentielle.Furthermore, the temperature of the refrigeration medium circulating in the coil 7 has been set at 5 ° C so as to cause vapor condensation resulting from the action of microwaves on peppermint and containing oil essential.
L'évolution de la température de la sauge présente dans l'enceinte et de la pression régnant à l'intérieur de celle-ci est représentée à la figure 6.The evolution of the temperature of the sage present in the enclosure and of the pressure inside it is shown in Figure 6.
En référence à la figure 7, après 10 mn d'extraction et 2 cycles de dépression, 3,06 ml d'huile essentielle ont été récupérés (soit un rendement de 2,55 ml pour 100g de matière sèche).Referring to Figure 7, after 10 min extraction and 2 cycles of depression, 3.06 ml of essential oil were recovered (a yield of 2.55 ml per 100g of dry matter).
Le rendement théorique par hydrodistillation classique de la même quantité de sauge est de 2,77 ml pour 100 g ce qui montre que la mise en oeuvre du procédé selon l'invention a permis de récupérer plus de 90 % de l'huile essentielle de la sauge officinale traitée.The theoretical yield by conventional hydrodistillation of the same quantity of sage is 2.77 ml per 100 g which shows that the implementation of the process according to the invention made it possible to recover more than 90% of the oil essential of the officinal sage treated.
Claims (13)
- Process for extracting at least one natural product from a biological material by microwaves, the said process comprising stages consisting of :placing the said biological material in a chamber, in the absence of any solvent,subjecting the said biological material present in the said chamber to irradiation by microwaves, so as to bring about the evaporation of at least part of the water contained in the said biological material and consequently the bursting of the cell structures of the said biological material, so as to enable at least part of the said natural product to be liberated,separating the residual biological material from the extracted natural product,applying a reduced pressure in an intermittent manner inside the said chamber during the said stage in which microwaves are applied, so as to promote the bursting of the cell structures of the said biological material induced by application of microwaves,heating the said chamber during at least a substantial part of the said stage in which microwaves are applied, so as to compensate for the fall in temperature resulting from evaporation of water from the biological material,
- Process according to claim 1, characterized in that the said stage of applying a reduced pressure consists of subjecting the interior of the said chamber to cycles of reduced pressure.
- Process according to either of claims 1 or 2,
characterized in that the said stage of separating the residual biological material from the extract consists of:cooling the water vapour containing the said extracted natural product,decanting the liquid mixture resulting from such cooling and,separating the said extracted natural product and water resulting from such decantation. - Process according to claim 3, characterized in that at least part of the said water resulting from the said decantation stage is injected into the chamber to bring about hydrodistillation of the natural product remaining in the said biological material residue.
- Process according to one of claims 1 to 4,
characterized in that the said heating stage is carried out at a temperature below 100°C. - Process according to one of claims 1 to 5,
characterized in that the microwaves used during the said microwave irradiation stage have a frequency at least equal to 300 MHz. - Process according to one of claims 1 to 6,
characterized in that the said microwave irradiation stage is carried out so as to apply a power ranging from approximately 100 W to approximately 10,000 W per kilogram of product treated. - Process according to one of claims 1 to 7,
characterized in that the said microwave irradiation stage is carried out with mechanical stirring of the said biological material. - Plant for putting the process according to one of claims 1 to 8 into practice, characterized in that it comprises :a chamber (1) provided with means for generating microwaves (2) inside the said chamber (1) and having a thermostatically controlled jacket (3);means of heating (4) enabling the temperature of the said thermostatically controlled jacket (3) to be regulated;means for reducing the pressure (5) inside the said chamber;means for recovering the extract (6) on leaving the said chamber.
- Plant according to claim 9, characterized in that the said means for recovering the extract (6) comprise means for cooling (7).
- Plant according to claim 9 or 10, characterized in that it has means (8) for operating the said means (5) for reducing the pressure inside the chamber in a cyclic manner.
- Plant according to one of claims 9 to 11,
characterized in that the said chamber is provided with means of stirring (9). - Plant according to one of claims 9 to 12,
characterized in that it comprises means (10) enabling the residual water obtained in the means for recovering the extract to be returned to the interior of the said chamber (1).
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR9305810A FR2705035B1 (en) | 1993-05-11 | 1993-05-11 | Process and installation for solvent-free extraction of natural products by microwave. |
FR9305810 | 1993-05-11 | ||
PCT/FR1994/000551 WO1994026853A1 (en) | 1993-05-11 | 1994-05-10 | Method and plant for solvent-free microwave extraction of natural products |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0698076A1 EP0698076A1 (en) | 1996-02-28 |
EP0698076B1 true EP0698076B1 (en) | 1998-01-14 |
Family
ID=9447117
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP94915607A Expired - Lifetime EP0698076B1 (en) | 1993-05-11 | 1994-05-10 | Method and plant for solvent-free microwave extraction of natural products |
Country Status (16)
Country | Link |
---|---|
EP (1) | EP0698076B1 (en) |
JP (1) | JPH08512337A (en) |
CN (1) | CN1059920C (en) |
AT (1) | ATE162211T1 (en) |
AU (1) | AU682035B2 (en) |
BG (1) | BG62367B1 (en) |
BR (1) | BR9406717A (en) |
CA (1) | CA2161127C (en) |
DE (1) | DE69407965T2 (en) |
DK (1) | DK0698076T3 (en) |
ES (1) | ES2114688T3 (en) |
FR (1) | FR2705035B1 (en) |
GR (1) | GR3026603T3 (en) |
HU (1) | HU218708B (en) |
RU (1) | RU2115700C1 (en) |
WO (1) | WO1994026853A1 (en) |
Cited By (2)
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EP1618798A1 (en) | 2004-07-20 | 2006-01-25 | Milestone S.r.l. | Microwave extraction of volatile natural substances |
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Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CA1336968C (en) * | 1989-05-16 | 1995-09-12 | J. R. Jocelyn Pare | Microwave-assisted natural products extraction |
SE9003593D0 (en) * | 1990-11-12 | 1990-11-12 | T G Owe Berg | PROCEDURE FOR CONVERSION OF HEATS TO WORK |
ES2082822T3 (en) * | 1990-11-16 | 1996-04-01 | United Kingdom Government | MICROWAVE EXTRACTION OF VOLATILE OILS AND APPARATUS FOR THE SAME. |
-
1993
- 1993-05-11 FR FR9305810A patent/FR2705035B1/en not_active Expired - Fee Related
-
1994
- 1994-05-10 RU RU95122234A patent/RU2115700C1/en active
- 1994-05-10 AU AU67251/94A patent/AU682035B2/en not_active Ceased
- 1994-05-10 CA CA002161127A patent/CA2161127C/en not_active Expired - Fee Related
- 1994-05-10 HU HU9503230A patent/HU218708B/en not_active IP Right Cessation
- 1994-05-10 BR BR9406717A patent/BR9406717A/en not_active IP Right Cessation
- 1994-05-10 ES ES94915607T patent/ES2114688T3/en not_active Expired - Lifetime
- 1994-05-10 EP EP94915607A patent/EP0698076B1/en not_active Expired - Lifetime
- 1994-05-10 CN CN94192507A patent/CN1059920C/en not_active Expired - Fee Related
- 1994-05-10 DE DE69407965T patent/DE69407965T2/en not_active Expired - Lifetime
- 1994-05-10 WO PCT/FR1994/000551 patent/WO1994026853A1/en active IP Right Grant
- 1994-05-10 JP JP6525060A patent/JPH08512337A/en not_active Ceased
- 1994-05-10 DK DK94915607T patent/DK0698076T3/en active
- 1994-05-10 AT AT94915607T patent/ATE162211T1/en not_active IP Right Cessation
-
1995
- 1995-12-04 BG BG100187A patent/BG62367B1/en unknown
-
1998
- 1998-04-10 GR GR980400799T patent/GR3026603T3/en unknown
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1618798A1 (en) | 2004-07-20 | 2006-01-25 | Milestone S.r.l. | Microwave extraction of volatile natural substances |
EP1629725A1 (en) * | 2004-07-20 | 2006-03-01 | Milestone S.r.l. | Microwave extraction of volatile natural substances |
TWI601565B (en) * | 2014-06-05 | 2017-10-11 | Timing Pharmaceutical Co Ltd | Essential oil extraction device |
Also Published As
Publication number | Publication date |
---|---|
ATE162211T1 (en) | 1998-01-15 |
CN1125461A (en) | 1996-06-26 |
HUT75578A (en) | 1997-05-28 |
FR2705035B1 (en) | 1995-08-04 |
DK0698076T3 (en) | 1998-09-14 |
BG100187A (en) | 1996-05-31 |
BG62367B1 (en) | 1999-09-30 |
ES2114688T3 (en) | 1998-06-01 |
DE69407965T2 (en) | 1998-09-10 |
HU9503230D0 (en) | 1996-01-29 |
BR9406717A (en) | 1996-02-06 |
AU6725194A (en) | 1994-12-12 |
DE69407965D1 (en) | 1998-02-19 |
EP0698076A1 (en) | 1996-02-28 |
FR2705035A1 (en) | 1994-11-18 |
AU682035B2 (en) | 1997-09-18 |
JPH08512337A (en) | 1996-12-24 |
CA2161127A1 (en) | 1994-11-24 |
CN1059920C (en) | 2000-12-27 |
WO1994026853A1 (en) | 1994-11-24 |
RU2115700C1 (en) | 1998-07-20 |
CA2161127C (en) | 2005-09-27 |
HU218708B (en) | 2000-11-28 |
GR3026603T3 (en) | 1998-07-31 |
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