Classifications

• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D11/00—Solvent extraction
  • B01D11/02—Solvent extraction of solids
  • B01D11/0211—Solvent extraction of solids in combination with an electric or magnetic field
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D1/00—Evaporating
  • B01D1/0011—Heating features
  • B01D1/0017—Use of electrical or wave energy
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D1/00—Evaporating
  • B01D1/0011—Heating features
  • B01D1/0017—Use of electrical or wave energy
  • B01D1/0023—Induction heating
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D1/00—Evaporating
  • B01D1/0011—Heating features
  • B01D1/0029—Use of radiation
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D19/00—Degasification of liquids
  • B01D19/0073—Degasification of liquids by a method not covered by groups B01D19/0005 - B01D19/0042
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
  • B01D3/02—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in boilers or stills
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
  • B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
  • B01D3/40—Extractive distillation
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
  • B01D5/0033—Other features
  • B01D5/0054—General arrangements, e.g. flow sheets
• • 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
• • 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
  • C11B9/025—Recovery by solvent extraction
• • 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 present invention relates to a device for extracting and separating volatile and non-volatile compounds from a biological material, more particularly a device using microwaves to carry out the extraction of these compounds.
• the invention also relates to a process for extracting and separating these compounds.
• One of the aims of the present invention is therefore to at least partially overcome the disadvantages of the prior art and to provide a microwave assisted extraction device for the extraction and separation of volatile and non-volatile compounds as well as the associated extraction process.
• the present invention relates to a device for extracting and separating volatile and non-volatile compounds from a biological material, said device comprising:
• a microwave oven having a microwave chamber for receiving biological material, said microwave chamber having a first discharge opening at its upper part to allow the evacuation of volatile compounds and a second opening drain located on its lower part to allow the evacuation of non-volatile compounds, and a reservoir for the introduction of the biological material in the microwave chamber,
• the microwave chamber comprises a hermetic sealing device leaving as evacuation only the first and the second discharge opening.
• the microwave chamber comprises a filter container inside which is intended to be disposed the biological material.
• the filtering container comprises a device for mechanical stirring of the biological material.
• the first and second cooling and recovery devices each comprise:
• a circulation channel for recovered compounds comprising an inlet connected to an outlet opening and an outlet opening onto a collection container, and
• a cooling circuit wherein a refrigerant fluid is intended to flow and surrounding the flow channel.
• the inlet of the circulation channel is disposed at a height greater than its outlet so that the recovered compounds flow by gravity into said circulation channel.
• the first cooling and recovery device comprises a vapor evacuation valve disposed at the outlet of the circulation channel.
• the extraction and separation device comprises a return water pipe adapted to allow a return of the lower phase of the liquid contained in the bottom of the collection container of the first cooling device and recovery in the microwave chamber.
• the present invention also relates to a method for extracting and separating natural substances from a biological material, said method comprising the following steps:
• microwave chamber having a first discharge opening located on its upper part and a second discharge opening located on its lower part
• the biological material is introduced into the microwave chamber and said biological material has a humidity of at least 50%.
• the biological material undergoes a preliminary pretreatment step before its introduction into the microwave chamber.
• the frequency of the microwaves of the microwave oven is between 915 MHz and 2450 MHz, preferably 2450 MHz.
• the irradiation power density of the biological material is between 125 and 1750 Watts per kilogram of biological material, preferably between 500 and 1500 Watts.
• the method comprises a decanted water return step from the first cooling and recovery device in the microwave chamber.
• FIG. 1 shows a schematic representation of an extraction and separation device according to the invention
• FIG. 2A shows a schematic representation of a first variant of the extraction and separation device of FIG. 1,
• FIG. 2B shows a schematic representation of a second variant of the extraction and separation device of FIG. 1,
• FIG. 3 shows a flowchart of an extraction and separation process according to the invention •
• Figures 4 to 10 show experimental diagrams of variations of different parameters and their impact on the extraction of compounds.
• first element or second element as well as first parameter and second parameter or else first criterion and second criterion, etc.
• first criterion and second criterion etc.
• it is a simple indexing to differentiate and name elements or parameters or criteria close but not identical.
• This indexing does not imply a priority of one element, parameter or criterion with respect to another, and it is easy to interchange such denominations without departing from the scope of the present description.
• This indexing does not imply either an order in time for example to appreciate such or such criteria.
• FIG. 1 shows a schematic representation of a miro-wave assisted extraction and separation device 1 according to the invention.
• This device comprises a microwave oven 3 inside which is arranged a microwave chamber 4 intended to receive biological material 2.
• the microwave chamber 4 comprises in particular a first discharge opening 44a located on its upper part to allow the evacuation of volatile compounds and a second discharge opening 44b located on its lower part to allow the evacuation of non-volatile compounds.
• the first 44a and second 44b discharge openings allow double extraction during the same heating process using a simple installation, that is to say an extraction of volatile compounds and non-volatile compounds during the heating process. the same heating process.
• the microwave chamber 4 comprises a tank 41, in particular open on the top, in order to allow the introduction of the biological material 2 into the microwave chamber 4.
• the bottom of this tank 41 is inclined so as to redirect the liquids towards the second discharge opening 44b.
• the tank 41 is covered by a cover 42 on which is disposed the first discharge opening 44a.
• the microwave chamber 4 may in particular comprise a hermetic sealing device leaving as evacuation only the first 44a and the second 44b discharge opening.
• the cover 42 is thus hermetically fixed on the reservoir 41, for example by means of flanges (not shown).
• the loading capacity in biological material 2 of the microwave chamber 4 corresponds to the mass of biological material 2 introduced into the microwave chamber 4 divided by the volume of said microwave chamber 4. for example, from 100 to 500 kg of biological material 2 per m 3 of microwave chamber 4, preferably between 125 and 440 kg.
• the biological material 2 is more particularly disposed in a filter container 7.
• This filtering container 7 keeps the biological material 2 in the center of the microwave chamber 4 and in particular in elevation with respect to the bottom and the second discharge opening 44b. This facilitates the flow and diffusion of liquid through the biological material 2 and its recovery in the second discharge opening 44b.
• This filter container 7 makes it possible to maintain the biological material 2 by passing condensates containing the non-volatile compounds.
• a filtering container 7 may, for example, have a filter made, for example, of fine-meshed mesh or in the form of a screen.
• the biological material 2 is intended to be arranged at least partly on this filter to allow the passage of condensates.
• such a filtering container 7 also allows the evacuation of the volatile compounds during the heating of the biological material 2, this evacuation of the volatile compounds being through the openings of the filtering container 7.
• the filtering container 7 may also comprise a mechanical stirring device (not shown) of the biological material 2.
• This mechanical stirring may be carried out in particular by rotating, for example according to a vertical or horizontal axis of the filter container 7. This rotating the filter container 7 may also allow the biological material 2 to be uniformly exposed to microwaves.
• the extraction and separation device 1 also comprises a first device for cooling and recovering the compounds connected to the first discharge opening 44a and a second device for cooling and recovering the compounds connected to the second opening. evacuation 44b.
• the first cooling and recovery device 5 comprises a circulation channel 51 of the recovered compounds, here volatile compounds, having an inlet connected to the first discharge opening 44a and an outlet opening to a collection container 53.
• the first device cooling and recovery device 5 also comprises a cooling circuit 52, in which a coolant is intended to circulate, and surrounding the circulation channel 51.
• the vapors recovered at the first discharge opening 44a thus pass into the circulation channel 51 in which they are cooled and condense due to the cooling circuit 52.
• the liquid A resulting from this condensation also called intrinsic water or in situ water of the biological material, is recovered in the collection container 53.
• the first cooling and recovery device 5 may also comprise a steam evacuation valve 54 disposed at the outlet of the circulation channel 5 in order to regulate the pressure within said first cooling and recovery device 5 but also within the microwave chamber 4.
• the second cooling and recovery device 6 also comprises a circulation channel 61 of the recovered compounds, here non-volatile compounds.
• This circulation channel 61 has an inlet connected to the second discharge opening 44b and an outlet opening to a collection container 63.
• the second cooling device and recovery device 6 also comprises a cooling circuit 62, in which a coolant is intended to circulate, and surrounding the circulation channel 61.
• the liquid recovered at the level of the second discharge opening 44b thus passes into the circulation channel 61 in which it is cooled by the cooling circuit 62.
• the liquid B resulting from this cooling also called the sap of the biological material, is recovered in the collection container 63.
• the inlet of the circulation channel 5, 6 is preferably disposed at a height greater than its outlet so that the recovered compounds flow by gravity in said circulation channel 5, 6.
• the collection container 53 of the intrinsic water A may be a decanter and allow separation into at least two phases of the intrinsic water A.
• the upper phase Al then comprises compounds volatile and aromatic and lower phase A2 mainly water.
• the extraction and separation device 1 may then comprise a water return line 8 adapted to allow a return of the lower phase of the liquid contained in connecting the bottom of the collection container 53 of the first cooling and recovery device 5 in the microwave chamber 4.
• This return water pipe 8 allows a replenishment of the microwave chamber 4 in order to maintain a certain level of humidity and thus assist the process of extraction and separation of the different compounds.
• the water outlet of the water return line 8 in the microwave chamber 4 is disposed at a height greater than its water inlet at the collection vessel 53. collection 53 can not be completely emptied into the microwave chamber 4.
• This return water pipe 8 may in particular comprise a valve 81 for controlling the return of water in the microwave chamber 4.
• the water return line 8 connects the bottom of the collection container 53 directly to the microwave chamber 4.
• the water return line 8 connects the bottom of the collection container 53 with the circulation channel 51 above the first discharge opening 44a. This makes it possible to avoid having an additional opening in the microwave chamber 4 and in particular in the wall of the microwave oven 3 in order to pass the water return pipe 8. According to this second variant, the recovered water trickles into the microwave chamber 4 through the first discharge opening 44a.
• the present invention also relates to a process for extracting and separating natural substances from a biological material 2 by means of an extraction and separation device 1 described above.
• Figure 3 shows a flowchart of the different steps of this extraction and separation process 100.
• biological material 2 is meant natural products of the plant, animal or microbial world.
• the biological material 2 is a plant material, more particularly fruits, vegetables and aromatic plants whose extraction of compounds is valuable.
• Intrinsic water A comprising, in particular, volatile compounds such as aromatic compounds and essential oils,
• Sap B including non-volatile compounds such as antioxidants, and
• the first step 101 is a step of introducing the biological material 2 into the microwave chamber 4.
• the biological material 2 can be introduced into the microwave chamber 4 as long as the biological material 2 has a humidity of at least 50%. This moisture content makes it possible to carry out the extraction and separation process 100 without the additional addition of a solvent such as water in the microwave chamber 4.
• the biological material 2 may undergo a preprocessing step 110.
• This pretreatment may for example be a grinding, an enzymatic treatment or a fermentation.
• a second step 102 is a step of irradiating the biological material 2 with microwaves until at least a portion of the volatile and non-volatile compounds of the biological material 2 are released.
• the frequency of the microwaves of the oven to microwaves 3 may especially be between 915 MHz and 2450 MHz, preferably 2450 MHz.
• the irradiation power density of the biological material 2 can more particularly be between 125 and 1750 Watts per kilogram of biological material 2, preferably between 500 and 1500 Watts.
• This second irradiation step 102 makes it possible to heat the water molecules present in the biological material 2. Part of this water is transformed into vapor and increases the pressure within the microwave chamber 4. Because of the formation of this vapor, the cells of the biological material burst and release volatile and non-volatile compounds.
• a third step 103 is a step in which the volatile compounds released and transported in the vapor are evacuated by convection to the first discharge opening 44a and conveyed to the first cooling and recovery device 5.
• a fourth step 104 is a step of cooling the volatile compounds in the first cooling and recovery device 5 and cooling the non-volatile compounds in the second cooling and recovery device 6.
• the steam flowing in the circulation channel 51 of the first cooling and recovery device 5 cools and condenses thanks to the cooling circuit 52.
• the condensate corresponding to the intrinsic water A is recovered in the collection container 53.
• the extraction and separation process 100 may comprise an additional step 120 of reintroduction of the decanted water coming from the first cooling and recovery device 5, that is to say the lower phase A2 of the intrinsic water A, in the microwave chamber 4 by means of the return water pipe 8.
• This additional step 120 is useful only in the case where the lower phase A2 of the intrinsic water A is not likely to be useful and therefore preserved.
• the liquid water circulating in the circulation channel 61 of the second cooling and recovery device 6 cools down thanks to the cooling circuit 62.
• the liquid corresponding to the sap B is recovered in the second stage. collection container 63.
• the extraction time of intrinsic water A and sap B tends to decrease as the irradiation power density increases.
• the extraction time of the intrinsic water A and the sap B tends to decrease when the capacity of the microwave chamber A increases.
• Figures 4 to 10 show examples of extraction and separation of olive using the device and method described above to illustrate the results obtained with such a device and such a method of extraction and separation.
• Figure 4 shows the effects of the variation of the irradiation power density on the extraction time in order to reach a yield of 30%.
• yield of 30% is meant that the sum of the masses of olive sap and intrinsic olive water extracted is equal to 30% of the fresh olive mass before extraction.
• the capacity of the microwave chamber 4 is 200kg / m 3 .
• FIG. 4 thus shows that the higher the irradiation power density, the lower the extraction time.
• FIG. 5 shows the effects of the variation of the irradiation power density on the extraction yield (expressed in g / gMH, gMH being the mass in gram of fresh olive material before extraction) of the sap of olive (expressed by the curve xB and the rods in black) and the intrinsic olive water (expressed by the curve xA and the rods in gray).
• the capacity of the microwave chamber 4 is 200 kg / m 3 and the total extraction efficiency is 30%.
• FIG. 5 thus shows that for an irradiation power density of less than
• Figure 6 shows the effects of varying the capacity of the microwave chamber 4 on the extraction time to achieve a yield of 30%.
• the irradiation power density is 1000W / kg.
• FIG. 6 thus shows that the higher the capacity of the microwave chamber 4, the lower the extraction time.
• Figure 7 shows the effect of pretreatment milling olives before their introduction into the microwave chamber 4 on the extraction yield of the olive sap, expressed by the rods in black, and the intrinsic water of olive, expressed by the sticks in gray.
• the irradiation power density is 1 000 W / kg
• the Microwave chamber capacity 4 is 200kg / m 3
• the total extraction yield is 30%.
• Figure 7 shows that grinding promotes the extraction of intrinsic olive water to the detriment of olive sap.
• Figure 8 shows the effects of the variation of the irradiation power density on the concentration of polyphenols of interest present in the olive sap.
• Polyphenols are antioxidants and are potentially valuable especially for pharmacological applications.
• After extraction, only the olive sap and the valuable residues of olives include polyphenols of interest such as Oleuropein, Tyrosol or Hydroxytyrosol.
• the capacity of the microwave chamber 4 is 200kg / m 3 and the total extraction efficiency is 30%.
• Figure 8 thus shows that the concentration of polyphenols of interest in olive sap increases the higher the power density of irradiation is high.
• FIG. 9 shows the effects of the variation of the irradiation power density on the free radical scavenging activity by an antioxidant, DPPH (2,2-diphenyl-1-picrylhydrazyl) present in the olive.
• raw symbolized by the hatched stick
• olive sap sap
• valuable residues of olives asymbolized by the gray sticks.
• Free radical scavenging is expressed as a percentage of reduced DPPH for a quantity of extract.
• the capacity of the microwave chamber 4 is 200 kg / m 3 and the total extraction efficiency is 30%.
• FIG. 9 thus shows that the higher the irradiation power density, the greater the percentage inhibition of DPPH in olive sap increases.
• the lower the irradiation power density the lower the percentage inhibition of DPPH in the recoverable residues of olives.
• Figure 10 shows the effects of variation in irradiation power density on olive oil extraction.
• the capacity of the microwave chamber 4 is 200 kg / m 3 and the total extraction efficiency is 30%.
• Figure 10 shows that the olive oil content in the recoverable residues of olives is relatively identical to that in the raw olive (the hatched stick). Olive oil is almost exclusively contained in the valuable residues of olives after microwave treatment. In addition, the olive oil content varies only slightly with variations in microwave power density.
• aromatic compounds extracted from the green olive during the extraction and separation process some are present in the olive sap or the intrinsic olive water. Other extracted aromatic compounds are present in both olive sap and intrinsic water. Other aromatic compounds are not present in olive sap or in the intrinsic olive water.
• Furfural is a molecule resulting from a heating process. This molecule appears after intense heating of sugars.
• the power density of microwave irradiation has an impact on the extraction of aromatic molecules.
• an optimum extraction yield at an irradiation power density of 1 W / g for the family of acids, esters and furanones .
• the optimum extraction yield is at a higher irradiation power density of the order of 1.5 W / g.
• the extraction and separation device 1 and its associated extraction process not only allow a differentiated extraction of different compounds depending on whether they are volatile or not, but also to favor the extraction or not of certain compounds according to settings of various parameters such as in particular the power density of microwave irradiation.

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• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Life Sciences & Earth Sciences (AREA)
• Engineering & Computer Science (AREA)
• Oil, Petroleum & Natural Gas (AREA)
• Wood Science & Technology (AREA)
• Organic Chemistry (AREA)
• Health & Medical Sciences (AREA)
• Toxicology (AREA)
• Extraction Or Liquid Replacement (AREA)
• Constitution Of High-Frequency Heating (AREA)
• Apparatus Associated With Microorganisms And Enzymes (AREA)

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• 2017
  • 2017-12-01 FR FR1761535A patent/FR3074425B1/fr not_active Expired - Fee Related
• 2018
  • 2018-11-29 WO PCT/FR2018/053054 patent/WO2019106313A1/fr not_active Ceased
  • 2018-11-29 EP EP18826427.9A patent/EP3717092A1/de not_active Withdrawn

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