EP0698076B1 - Procede et installation d'extraction sans solvant de produits naturels par micro-ondes - Google Patents

Procede et installation d'extraction sans solvant de produits naturels par micro-ondes Download PDF

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Publication number
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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EP
European Patent Office
Prior art keywords
biological material
chamber
microwaves
stage
natural product
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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.)
Expired - Lifetime
Application number
EP94915607A
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German (de)
English (en)
French (fr)
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EP0698076A1 (fr
Inventor
Philippe Mengal
Bernard Mompon
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Archimex
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Archimex
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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.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • Fats And Perfumes (AREA)
  • Compounds Of Unknown Constitution (AREA)
  • Medicines Containing Plant Substances (AREA)
EP94915607A 1993-05-11 1994-05-10 Procede et installation d'extraction sans solvant de produits naturels par micro-ondes Expired - Lifetime EP0698076B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR9305810A FR2705035B1 (fr) 1993-05-11 1993-05-11 Procédé et installation d'extraction sans solvant de produits naturels par micro-ondes.
FR9305810 1993-05-11
PCT/FR1994/000551 WO1994026853A1 (fr) 1993-05-11 1994-05-10 Procede et installation d'extraction sans solvant de produits naturels par micro-ondes

Publications (2)

Publication Number Publication Date
EP0698076A1 EP0698076A1 (fr) 1996-02-28
EP0698076B1 true EP0698076B1 (fr) 1998-01-14

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP94915607A Expired - Lifetime EP0698076B1 (fr) 1993-05-11 1994-05-10 Procede et installation d'extraction sans solvant de produits naturels par micro-ondes

Country Status (16)

Country Link
EP (1) EP0698076B1 (zh)
JP (1) JPH08512337A (zh)
CN (1) CN1059920C (zh)
AT (1) ATE162211T1 (zh)
AU (1) AU682035B2 (zh)
BG (1) BG62367B1 (zh)
BR (1) BR9406717A (zh)
CA (1) CA2161127C (zh)
DE (1) DE69407965T2 (zh)
DK (1) DK0698076T3 (zh)
ES (1) ES2114688T3 (zh)
FR (1) FR2705035B1 (zh)
GR (1) GR3026603T3 (zh)
HU (1) HU218708B (zh)
RU (1) RU2115700C1 (zh)
WO (1) WO1994026853A1 (zh)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1618798A1 (de) 2004-07-20 2006-01-25 Milestone S.r.l. Mikrowellen-unterstützte Extraktion von flüchtigen Naturstoffen
TWI601565B (zh) * 2014-06-05 2017-10-11 Timing Pharmaceutical Co Ltd Essential oil extraction device

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1618798A1 (de) 2004-07-20 2006-01-25 Milestone S.r.l. Mikrowellen-unterstützte Extraktion von flüchtigen Naturstoffen
EP1629725A1 (de) * 2004-07-20 2006-03-01 Milestone S.r.l. Mikrowellen-unterstützte Extraktion von flüchtigen Naturstoffen
TWI601565B (zh) * 2014-06-05 2017-10-11 Timing Pharmaceutical Co Ltd Essential oil extraction device

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EP0698076A1 (fr) 1996-02-28
CN1059920C (zh) 2000-12-27
HUT75578A (en) 1997-05-28
DE69407965T2 (de) 1998-09-10
CN1125461A (zh) 1996-06-26
HU218708B (hu) 2000-11-28
JPH08512337A (ja) 1996-12-24
HU9503230D0 (en) 1996-01-29
WO1994026853A1 (fr) 1994-11-24
FR2705035B1 (fr) 1995-08-04
FR2705035A1 (fr) 1994-11-18
ES2114688T3 (es) 1998-06-01
GR3026603T3 (en) 1998-07-31
BR9406717A (pt) 1996-02-06
BG62367B1 (bg) 1999-09-30
AU682035B2 (en) 1997-09-18
AU6725194A (en) 1994-12-12
CA2161127C (en) 2005-09-27
DK0698076T3 (da) 1998-09-14
ATE162211T1 (de) 1998-01-15
BG100187A (bg) 1996-05-31
DE69407965D1 (de) 1998-02-19
CA2161127A1 (en) 1994-11-24
RU2115700C1 (ru) 1998-07-20

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