EP0698076A1 - Method and plant for solvent-free microwave extraction of natural products - Google Patents

Method and plant for solvent-free microwave extraction of natural products

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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
Application number
EP94915607A
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German (de)
French (fr)
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EP0698076B1 (en
Inventor
Philippe Mengal
Bernard Mompon
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Archimex
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Archimex
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Publication date
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Publication of EP0698076A1 publication Critical patent/EP0698076A1/en
Application granted granted Critical
Publication of EP0698076B1 publication Critical patent/EP0698076B1/en
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Expired - Lifetime legal-status Critical Current

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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.

Abstract

The microwave extraction method involves the steps of placing the biological material in an enclosure without any solvent whatsoever and exposing it to microwave radiation to free at least some of the natural product, and then separating the residual biological material from the extracted natural product. Additionally, it involves the steps of applying reduced pressure in said enclosure during said microwave radiation stage and heating the enclosure during at least most of the microwave radiation stage to compensate the temperature drop resulting from water evaporation from the biological material.

Description

Procédé et installation d'extraction sans solvant de produits naturels par micro-ondes. Process and installation for solvent-free extraction of natural products by microwave.
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.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. Thus, 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.
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. II 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,For example, the extraction of 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. In addition to the fact that they have a low cost of implementation, 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. There are however many products which cannot be extracted from the natural material which contains them according to such methods and for which it is necessary to use 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,
- la diffusion du produit extrait au sein de la matrice solide du matériel biologique utilisé.- 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 even 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 connaît 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.Furthermore, it is possible to act also on the second parameter, either prior to the extraction step, or concomitantly with the latter. For example, 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. One can also choose to act on the biological material during the actual extraction operation, for example by heating or agitating it. Thus, in the state of the art, sonication methods are known 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.
D 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 réchauffement 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 product from a biological material by subjecting it to irradiation by microwaves. The action of microwaves on biological materials is well known today. Such electromagnetic waves are in fact selectively absorbed by media having a high dielectric constant and therefore, in the case of biological material, mainly by water, that is to say essentially by vascular and glandular tissues and more particularly vacuoles in the case of plant material. During such an absorption, the energy of the radiation is converted into heat energy, which allows selective heating of the parts of the biological material absorbing the 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.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.
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. 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.Although having the advantage of improving the extraction yields, the technique described in patent EP 0398798 does not make it possible to overcome the drawbacks already mentioned linked to the presence of solvent in the extract obtained. It will be noted that it has also already been proposed in the prior art to 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 Essentiel 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 entraînement 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 Essentiel Oil" indeed describes a technique for extracting the essential oil of lippia sidoides by microwave heating, whereby 30 to 40 gram plant samples are placed, in the absence of any solvent, in a vial inside a microwave oven and undergo microwave irradiation -waves for a period of 5 min. The bottle used is designed to allow the essential oil to be entrained by a flow of air from outside.
Bien qu'autorisant une extraction dans un temps beaucoup plus court que les temps nécessaires pour mener à bien les opérations d'extraction par hydrodistil¬ lation, 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. 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. 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.Although allowing an extraction in a much shorter time than the time necessary to carry out the operations of extraction by hydrodistilation, such a method has the major drawback of requiring a very significant energy contribution to allow the extraction , which makes it a process offering no economic interest. All the processes for extracting natural products by microwaves described in the literature can only be implemented on masses of treated biological material that are very small 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, these methods, to be implemented on an industrial scale, must be adapted to continuous operation, in order to present a small mass punctually in front of a microwave source of reasonable power. 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.
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 process allowing extraction in the absence of solvent and therefore obtaining an extract free from 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 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.
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 conséquem- ment 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, la combinaison desdites étapes d'application des micro-ondes, d'application d'une pression réduite à l'intérieur de l'enceinte et de chauffage de l'enceinte autorisant l'hydrodistillation dudit produit naturel par entraînement de celui-ci dans la vapeur d'eau provenant dudit matériel biologique.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. , so as to allow the release of at least part of said natural product, - separate the residual biological material from the extracted natural product, 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.
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 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. Of course, 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.
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 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. It will be noted in this respect that, within the framework of the present description, 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.
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'entraînement azéotropique du produit extrait, la pression de l'enceinte est réduite. Cette diminution de pression permet, d'une part, d'accroître 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 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. In order to promote this phenomenon and in order to carry out the azeotropic entrainment of the extracted product, 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. According to the invention, 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.
Le procédé selon l'invention présente de nombreux avantages. 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 substantiel¬ lement 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.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.
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 consumes much less energy than the microwave assisted extraction methods of the prior art. For the same quantity of biological material treated, the energy used in the context of the invention is also less than that necessary for hydrodistillation. In the context of 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'entraînement 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 will 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 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.
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 of the intermittent application of a reduced pressure, consists in subjecting the interior of said enclosure to vacuum cycles.
Selon une variante de l'invention, ladite étape de séparation du matériel biologique résiduel de l'extrait consiste :According to a variant of the invention, said step of separation of the residual biological material from the extract consists:
- à réfrigérer la vapeur d'eau contenant ledit produit naturel extrait, - à décanter le mélange liquide résultant d'une telle réfrigération et,- refrigerating the water vapor containing said extracted natural product, - decanting the liquid mixture resulting from such refrigeration and,
- à séparer ledit produit naturel extrait et l'eau résultant d'une telle décantation.- 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 that it results in much less waste water being obtained than conventional hydrodistillation processes, at least part of said water resulting from said decantation step is advantageously injected into the enclosure. to carry out 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. Note that 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.
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 etThe 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
2450 MHz sont autorisées pour les équipements industriels générant des micro- ondes.2450 MHz is authorized for industrial equipment generating microwaves.
Par ailleurs, ladite étape d'irradiation aux micro-ondes sera préférentielle¬ ment menée de façon à appliquer une puissance allant d'environ 100 W à environ 10 000 W par kilogramme de produit traité. 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. L'invention concerne également une installation pour la mise en oeuvre d'un tel procédé caractérisée en ce qu'elle comprend :Furthermore, 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. According to a variant implementation of the method, 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:
- une enceinte pourvue de moyens de génération de micro-ondes à l'intérieur de ladite enceinte et présentant une double-paroi thermostatée ;- an enclosure provided with means for generating microwaves inside said enclosure and having a thermostated double wall;
- des moyens de chauffage permettant de réguler la température de ladite double-paroi thermostatée ;- heating means making it possible to regulate the temperature of said thermostated double wall;
- des moyens permettant de réduire la pression à l'intérieur de ladite enceinte ;- means making it possible to reduce the pressure inside said enclosure;
- des moyens de récupération de l'extrait à sa sortie de ladite enceinte. Préférentiellement, lesdits moyens de récupération de l'extrait comprennent des moyens de réfrigération de la vapeur d'eau contenant l'extrait.- Means for recovering the extract at its exit from said enclosure. 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 operating said means making it possible to reduce the pressure inside the enclosure cyclically.
Avantageusement, ladite enceinte est pourvue de moyens d'agitation. 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.Advantageously, said enclosure is provided with stirring means. Finally, also advantageously, 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.
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 :The invention, as well as the advantages which it presents, will be more easily understood thanks to the following description of embodiments thereof with reference to the drawings, in which:
- la figure 1 représente une vue schématique d'une installation selon l'invention ;- Figure 1 shows a schematic view of an installation according to the 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 ;- Figure 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;
- 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 ;- Figure 3 shows the evolution of the yield of peppermint essential oil obtained during the first example of implementation of the method;
- 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 ;- Figure 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;
- la figure 5 représente l'évolution du rendement d'huile essentielle de menthe poivrée obtenu lors de l'exemple comparatif ;- Figure 5 shows the evolution of the yield of peppermint essential oil obtained during the comparative example;
- 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 ;- Figure 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;
- 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.- Figure 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.
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 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. In accordance with legal provisions, 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).
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. 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.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. 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. In accordance with the present invention, 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. In the context of this example, 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.
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 conden- sées. 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.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.
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 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.
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 (exempleThe installation described above was used to implement the microwave extraction process of the present invention in order to extract essential oils of peppermint (examples 1) and officinal sage (example
3)-3) -
Exemple 1Example 1
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.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.
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 min, 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 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.
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. 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.Furthermore, 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. 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 placed under partial vacuum (250 mb) using pump 5, 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.
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). 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.With reference to FIG. 3, after 15 min of extraction and 3 vacuum cycles, 1.52 ml of essential oil were recovered (ie a yield of 1.01 ml per 100 g of dry matter). The hydrodistillation of the peppermint residue resulting from such a microwave extraction operation made it possible to obtain less than 50 mg of essential oil. The method according to the invention therefore allows obtaining an 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 apparaître de différence majeure de composition.The comparison of the gas chromatography profiles of two essential oils obtained by the extraction process according to the invention and by conventional hydrodistillation did not show any major difference in composition.
Exemple 2Example 2
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 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.
L'évolution de la température de la menthe et de la pression dans l'enceinte est donnée à la 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'extrac¬ tion. 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. Exemple 3The 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. Example 3
Cinq cents grammes de sauge officinale (Salvia officinalis L.,) présentantFive hundred grams of sage sage (Salvia officinalis L.,) presenting
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.25% of dry matter has been placed inside the enclosure 1. 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.
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. 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.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.
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 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.
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 prevailing inside it is represented in FIG. 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).With reference to FIG. 7, after 10 min of extraction and 2 vacuum cycles, 3.06 ml of essential oil were recovered (ie a yield of 2.55 ml per 100 g 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 has made it possible to recover more than 90% of the essential oil of the processed sage.
Les exemples de réalisation de l'invention ici décrits n'ont pas pour objet de réduire la portée de celle-ci. En particulier, il pourra être envisager de faire agir les micro-ondes pendant un temps plus long ou plus court, d'utihser des fréquences de micro-ondes différentes ou de séparer l'extrait de la vapeur selon une autre technique que celle décrite sans sortir du cadre de l'invention. The examples of embodiment of the invention described here are not intended to reduce the scope thereof. In particular, it may be envisaged to act on the microwaves for a longer or shorter time, to use different microwave frequencies or to separate the extract from the vapor by another technique than that described without depart from the scope of the invention.

Claims

REVENDICATIONS
1. Procédé d'extraction par micro-ondes d'au moins un produit naturel à partir d'un matériel biologique, ledit procédé comprenant les étapes consistant à: placer ledit matériel biologique dans une enceinte, en l'absence de tout solvant, faire subir une irradiation par micro-ondes audit matériel biologique présent dans ladite enceinte, afin de provoquer l'évaporation d'au moins une partie de l'eau de 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 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 cellulaires 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, la combinaison desdites étapes d'application des micro-ondes, d'application d'une pression réduite à l'intérieur de l'enceinte et de chauffage de l'enceinte autorisant l'hydrodistillation dudit produit naturel par entraînement de celui-ci dans la vapeur d'eau même provenant dudit matériel biologique .1. A method of microwave extraction of at least one natural product from biological material, said method comprising the steps of: placing said biological material in an enclosure, in the absence of any solvent, making undergo microwave irradiation to said biological material present in said enclosure, 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 a portion of said natural product, separate the residual biological material from the extracted natural product, said process being characterized in that it comprises the additional steps consisting in: - applying intermittently, reduced pressure inside said enclosure during said step of applying microwaves, in order to promote the bursting of cell structures ires 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 l of 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 entrainment of it in the same water vapor from said biological material.
2. Procédé selon la revendication 1 caractérisé en ce que ladite étape d'application d'une pression réduite consiste à soumettre l'intérieur de ladite enceinte à des cycles de dépression.2. Method according to claim 1 characterized in that said step of applying a reduced pressure consists in subjecting the interior of said enclosure to vacuum cycles.
3. Procédé selon l'une des revendications 1 ou 2 caractérisé en ce que ladite étape de séparation du matériel biologique résiduel de l'extrait consiste : - à réfrigérer la vapeur d'eau contenant ledit produit naturel extrait,3. Method according to one of claims 1 or 2 characterized in that said step of separation of the residual biological material from the extract consists: - refrigerating the water vapor containing said extracted natural product,
- à décanter le mélange liquide résultant d'une telle réfrigération et,decanting the liquid mixture resulting from such refrigeration and,
- à séparer ledit produit naturel extrait et l'eau résultant d'une telle décantation. - Separating said extracted natural product and the water resulting from such decantation.
4. Procédé selon la revendication 3 caractérisé en ce qu'au moins une partie de ladite eau résultant de ladite étape de décantation est injectée dans l'enceinte pour effectuer l'hydrodistillation du produit naturel restant dans ledit résidu de matériel biologique.4. Method according to claim 3 characterized in that at least part of said water resulting from said decantation step is injected into the enclosure to effect the hydrodistillation of the natural product remaining in said residue of biological material.
5. Procédé selon l'une des revendications 1 à 4 caractérisé en ce que ladite étape de chauffage est menée à une température inférieure à 100°C.5. Method according to one of claims 1 to 4 characterized in that said heating step is carried out at a temperature below 100 ° C.
6. Procédé selon l'une des revendications 1 à 5 caractérisé en ce que les micro-ondes utilisées lors de ladite étape d'irradiation aux micro-ondes possèdent une fréquence au moins égale à 300 MHz.6. Method according to one of claims 1 to 5 characterized in that the microwaves used during said step of irradiation with microwaves have a frequency at least equal to 300 MHz.
7. Procédé selon l'une des revendications 1 à 6 caractérisé en ce que ladite étape d'irradiation aux micro-ondes est menée de façon à appliquer une puissance allant d'environ 100 W à environ 10 000 W par kilogramme de produit traité.7. Method according to one of claims 1 to 6 characterized in that said microwave irradiation step is carried out so as to apply a power ranging from about 100 W to about 10,000 W per kilogram of product treated.
8. Procédé selon l'une des revendications 1 à 7 caractérisé en ce que ladite étape d'irradiation aux micro-ondes est menée sous agitation mécanique dudit matériel biologique. 9. Installation pour la mise en oeuvre du procédé selon l'une des revendications 1 à 8 caractérisée en ce qu'elle comprend :8. Method according to one of claims 1 to 7 characterized in that said microwave irradiation step is carried out with mechanical stirring of said biological material. 9. Installation for implementing the method according to one of claims 1 to 8 characterized in that it comprises:
- une enceinte (1) pourvue de moyens de génération de micro-ondes (2) à l'intérieur de ladite enceinte (1) et présentant une double-paroi thermostatée (3);- an enclosure (1) provided with means for generating microwaves (2) inside said enclosure (1) and having a thermostated double wall (3);
- des moyens de chauffage (4) permettant de réguler la température de ladite double-paroi thermostatée (3) ;- heating means (4) for regulating the temperature of said thermostated double wall (3);
- des moyens permettant de réduire la pression (5) à l'intérieur de ladite enceinte ;- means making it possible to reduce the pressure (5) inside said enclosure;
- des moyens de récupération de l'extrait (6) à sa sortie de ladite enceinte. 10. Installation selon la revendication 9 caractérisée en ce que lesdits moyens de récupération de l'extrait (6) comprennent des moyens de réfrigération 11. Installation selon la revendication 9 ou 10 caractérisée en ce qu'elle présente des moyens (8) pour faire fonctionner lesdits moyens (5) permettant de réduire la pression à l'intérieur de l'enceinte de façon cyclique 12. Installation selon l'une des revendications 9 à 11 caractérisée en ce que ladite enceinte est pourvue de moyens d'agitation (9).- Means for recovering the extract (6) at its exit from said enclosure. 10. Installation according to claim 9 characterized in that said means for recovering the extract (6) comprise refrigeration means 11. Installation according to claim 9 or 10 characterized in that it has means (8) for operating said means (5) making it possible to reduce the pressure inside the enclosure cyclically 12. Installation according to l 'One of claims 9 to 11 characterized in that said enclosure is provided with stirring means (9).
13. Installation selon l'une des revendications 9 à 12 caractérisée en ce qu'elle comprend des moyens (10) permettant de réacheminer l'eau résiduaire obtenue au niveau des moyens de récupération de l'extrait à l'intérieur de ladite enceinte (1). 13. Installation according to one of claims 9 to 12 characterized in that it comprises means (10) making it possible to redirect the residual water obtained at the level of the means for recovering the extract inside said enclosure ( 1).
EP94915607A 1993-05-11 1994-05-10 Method and plant for solvent-free microwave extraction of natural products Expired - Lifetime EP0698076B1 (en)

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FR9305810 1993-05-11
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CN106190574A (en) * 2016-07-28 2016-12-07 河南科技学院 A kind of Atractylodes lancea (Thunb.) DC. volatile oil and preparation method thereof
WO2019106313A1 (en) 2017-12-01 2019-06-06 Université D'avignon Et Des Pays De Vaucluse Device for extracting and separating volatile and non-volatile compounds from a biological material, and associated process
FR3099991A1 (en) 2019-08-22 2021-02-26 Société de Courtage et de Diffusion - CODIF INTERNATIONAL Cosmetic composition ingredient for sensitive scalp
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FR3115695A1 (en) 2020-10-30 2022-05-06 Société de Courtage et de Diffusion - CODIF INTERNATIONAL Active ingredient consisting of a bitter apple extract activating Tas2Rs bitterness receptors present on human skin and corresponding cosmetic and dermato-cosmetic uses.

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AU6725194A (en) 1994-12-12
HUT75578A (en) 1997-05-28
CA2161127A1 (en) 1994-11-24
ES2114688T3 (en) 1998-06-01
FR2705035A1 (en) 1994-11-18
CA2161127C (en) 2005-09-27
FR2705035B1 (en) 1995-08-04
BR9406717A (en) 1996-02-06
EP0698076B1 (en) 1998-01-14
WO1994026853A1 (en) 1994-11-24
CN1125461A (en) 1996-06-26
DK0698076T3 (en) 1998-09-14
CN1059920C (en) 2000-12-27
HU9503230D0 (en) 1996-01-29
HU218708B (en) 2000-11-28
ATE162211T1 (en) 1998-01-15
BG100187A (en) 1996-05-31
BG62367B1 (en) 1999-09-30
AU682035B2 (en) 1997-09-18
GR3026603T3 (en) 1998-07-31
DE69407965D1 (en) 1998-02-19
RU2115700C1 (en) 1998-07-20
JPH08512337A (en) 1996-12-24
DE69407965T2 (en) 1998-09-10

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