Classifications

• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
  • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
  • B02C23/00—Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
  • B02C23/08—Separating or sorting of material, associated with crushing or disintegrating
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23J—PROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
  • A23J1/00—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites
  • A23J1/14—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites from leguminous or other vegetable seeds; from press-cake or oil-bearing seeds
  • A23J1/146—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites from leguminous or other vegetable seeds; from press-cake or oil-bearing seeds by using wave energy or electric current
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
  • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
  • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
  • A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
  • B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
  • B03C7/00—Separating solids from solids by electrostatic effect
  • B03C7/006—Charging without electricity supply, e.g. by tribo-electricity, pyroelectricity
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
  • C08H8/00—Macromolecular compounds derived from lignocellulosic materials
• • C—CHEMISTRY; METALLURGY
  • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
  • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
  • C10L1/00—Liquid carbonaceous fuels
  • C10L1/02—Liquid carbonaceous fuels essentially based on components consisting of carbon, hydrogen, and oxygen only
• • C—CHEMISTRY; METALLURGY
  • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
  • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
  • C10L2200/00—Components of fuel compositions
  • C10L2200/04—Organic compounds
  • C10L2200/0461—Fractions defined by their origin
  • C10L2200/0469—Renewables or materials of biological origin
  • C10L2200/0484—Vegetable or animal oils
• • C—CHEMISTRY; METALLURGY
  • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
  • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
  • C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
  • C10L2290/28—Cutting, disintegrating, shredding or grinding
• • C—CHEMISTRY; METALLURGY
  • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
  • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
  • C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
  • C10L2290/38—Applying an electric field or inclusion of electrodes in the apparatus
• • C—CHEMISTRY; METALLURGY
  • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
  • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
  • C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
  • C10L2290/54—Specific separation steps for separating fractions, components or impurities during preparation or upgrading of a fuel
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
  • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
  • Y02E50/00—Technologies for the production of fuel of non-fossil origin
  • Y02E50/10—Biofuels, e.g. bio-diesel
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
  • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
  • Y02P30/00—Technologies relating to oil refining and petrochemical industry
  • Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock

Definitions

• the present invention is directed to a process for fractionating an oilseed cake and applications thereof. It is particularly applicable to the extraction of lignocellulose and protein from a meal, the production of biomolecules and biopolymers of interest and the production of biofuel or biogas.
• Oilseed cake is defined as solid residues obtained after extraction of oil from seeds or fruits of oil plants, such as sunflower, rapeseed or soybeans, for example.
• Oilseed cakes are a poorly valued material, usually used for animal feed, once the oil is extracted from the seed or fruit of the oleaginous plant.
• these cakes are rich in constituents of interest for the industry such as proteins and ligno-cellulose (also called “fiber”), whose applications within “biorefineries” lead to the creation of bioenergy, biomolecules and of biomaterials.
• the main difficulty for this type of recovery lies in the separation of the fibers and proteins contained in the cakes without altering their structures and their functional properties.
• the present invention aims to remedy all or part of these disadvantages.
• the present invention is directed to a process for fractionating oilseed cakes by the dry route, which comprises:
• At least one trajectory deflection step in the electric field of the charged particles to sort the particles and to provide at least one fraction enriched in lignocellulose.
• ultrastavian particles is meant a set of particles whose median diameter (d50) is less than 500 ⁇ .
• the homogeneity of the particles resulting from the grinding of oilseed cakes increases when their size decreases. Indeed, some particles are mainly composed of lignin present in the walls of oilseeds and others are mainly composed of proteins of oilseed cells.
• the tribo-electrostatic charging step allows the particles to charge or discharge into electrons based on their main chemical component. The deflection step thus separates the particles whose main components are different. The method which is the subject of the invention thus makes it possible to collect the fractions of cake enriched with lignocellulose.
• the lignocellulose thus obtained is in the native state, that is to say that it is not modified or denatured, unlike the methods of the state of the art such as the Organosolv process ( registered trademark) lignin extraction (see “Quantitative structural characterization and thermal properties of birch lignins after auto-catalyzed organosolv pretreatment and enzymatic hydrolysis” Jia-Long Wen, et al September 2013 in Journal of Chemical Technology and Biotechnology Volume 88, Issue 9, pp. 1,663-1,671), which comprises denaturation by chemical treatment.
• Organosolv process registered trademark
• a device embodying the method that is the subject of the present invention is concentrated in a single device, a grinding means, a receiving means, a load means and each deflection means.
• the device is more compact.
• the powder does not have time to aggregate, load moisture, oxidize or, more generally, to change state, between grinding and deflection.
• the implementation of the method which is the subject of the present invention is improved.
• the grinding step includes a step of configuring the mill to obtain a predetermined fineness. These embodiments allow a user to adjust the fineness of the grinding according to the crushed cake and the quality of the desired sorting.
• the method which is the subject of the present invention further comprises an electrode scraping step of an electrostatic sorting means implemented during the deflection step, in order to collect the particles fixed on an electrode after the particle deflection step.
• the method which is the subject of the present invention further comprises a step of cyclically inverting the polarity of each electrode of an electrostatic sorting means implemented during the deflection step.
• the method which is the subject of the present invention comprises, downstream of the deflection step, at least one secondary deviation step.
• a tribo-electrostatic charge means is fed to particles which, during Deflection steps are alternately deflected to a positive electrode and a negative electrode or vice versa.
• the method that is the subject of the present invention further comprises, downstream of at least one deflection step, a step of enzymatic purification of the sorted particles,
• purification and / or enzymatic extraction are carried out to enrich the fractions in proteins and in polyphenols (lignin and phenolic acids) by degradation or hydrolysis of the polysaccharides into monosaccharides (glucose, xylose, arabinose, etc.). ).
• the method which is the subject of the present invention comprises, downstream from at least one deflection step, a step of comparing the particle dimensions with respect to a predetermined limit value and a feed step of particle grinding means whose dimensions are greater than the predetermined limit.
• a dynamic fluidized air bed is implemented.
• the present invention aims, according to a second aspect, an application of the method that is the subject of the present invention to obtaining fractions enriched in lignocellulose.
• the present invention aims, according to a third aspect, an application of the method object of the present invention to obtain fractions enriched in proteins.
• the present invention aims, according to a fourth aspect, an application of the method that is the subject of the present invention to the generation of biofuel from fractions enriched in ligno-cellulose.
• This biofuel comprises, for example, biohydrogen and / or bioethanol.
• the present invention aims, according to a fifth aspect, an application of the method that is the subject of the present invention to the generation of biogas from fractions enriched in ligno-cellulose.
• the present invention aims, according to a sixth aspect, an application of the method that is the subject of the present invention to obtain fractions enriched in polysaccharides.
• the present invention aims, according to a seventh aspect, an application of the method object of the present invention to the extraction and obtaining fractions enriched in phenolic derivatives.
• Phenolic derivatives include, in particular, tannins and phenolic acids.
• FIG. 1 represents, schematically and in section, a first particular embodiment of the device that is the subject of the present invention
• FIG. 2 represents, schematically and in section, a second particular embodiment of the device that is the subject of the present invention
• FIG. 3 represents, schematically and in section, a part of one of the embodiments illustrated in FIGS. 1 and 2,
• FIG. 4 represents, in the form of a logic diagram, steps of a particular embodiment of the method that is the subject of the present invention
• FIG. 5 represents, in the form of a histogram, the distribution of the phenolic acids obtained by the implementation of the method that is the subject of the present invention with a sunflower cake
• FIG. 6 represents, schematically, a purification and / or enzymatic extraction to enrich further the protein and polyphenol fractions and
• FIG. 7 represents an experimental example of yield of sugars after enzymatic hydrolysis.
• An “ultrafine” is a powder whose particles have a median diameter of less than 500 micrometers, preferably between 10 micrometers and 500 micrometers, more preferably between 30 micrometers and 500 micrometers, and even more preferably between 50 micrometers and 500 micrometers.
• ultrastyrene is a powder whose half (50%) by volume, fibers with a diameter of less than 500 micrometers, preferably less than 200 micrometers, more preferably less than 100 micrometers and even more preferentially less than 50 micrometers.
• FIG. 1 shows a first embodiment of the device 10 which is the subject of the present invention.
• This device 10 comprises:
• a means 120 for the main electrostatic sorting of the particles transmitted is a means 120 for the main electrostatic sorting of the particles transmitted.
• the inlet 105 of ultrafine particles is, for example, a hopper or a funnel configured to allow the pouring of a powder of ultrafine particles from the grinding of oilcakes.
• the particles thus poured into the particle inlet 105 pass through a charging means 1 placed, for example, under the inlet 105 of particles.
• This charging means is configured so that the particles pass through this means. of charge thanks to gravitational force.
• the movement of the particles is ensured by a fluidized air bed system, that is to say ventilated by means of a turbine or a fan.
• the tribo-electrostatic charge is made by collision between the particles and the inner surface of a conduit.
• This surface comprises at least one portion of polyvinyl chloride (abbreviated "PVC").
• this surface comprises at least a Teflon portion.
• this surface comprises at least one glass part.
• this surface comprises at least one steel part.
• PVC, Teflon, glass and steel have optimal properties for the charge of protein-rich particles or lignocellulose.
• the charging means 1 is connected to the input of the sorting means 120.
• the means 120 for main electrostatic sorting of the transmitted particles comprises at least one electrode 125.
• This sorting means 120 is configured to sort the particles transmitted into fractions enriched in lignocellulose. This sorting is performed by using the electrode 125 polarized positively or negatively. Thus, the charged particles are attracted or repelled by the electrode 125.
• two conduits allow the particles to flow into two containers 130 and 135. In a first container 130 are discharged the particles have been attracted or repelled by the electrode 125 according to the polarization of the electrode 125. In the second container 135 are poured the other particles.
• the particles enriched in lignocellulose are charged in the means 1 load of positive charges.
• these ligno-cellulose enriched particles are attracted to a negatively polarized electrode.
• the particles flowing into the conduit and then into the container 130 in the vicinity of the negatively charged electrode comprise fractions enriched in lignocellulose.
• FIG. 2 shows a second particular embodiment of the device 20 of the present invention. This device comprises:
• a means 240 for grinding powder cake with ultrafine particles comprising:
• a means 220 for main electrostatic sorting of the transmitted particles comprising:
• two secondary electrostatic sorting means 250 each comprising two electrodes 255 and
• the means 240 for grinding the powder cake of ultrafine particles is, for example, a centrifugal grinder configured to grind the cake into particles whose diameter is between 50 micrometers and 500 micrometers.
• This milling means 240 comprises means 245 for configuring the grinding fineness achieved by the milling means 240.
• This means 245 for configuring the fineness of the grinding is, for example, a touch screen on which a computer program shows the current grinding fineness, an interactive zone allowing a user to increase the fineness of grinding and an interactive zone allowing the user to reduce the fineness of grinding.
• the milling means 240 is configured to grind the powder cake of particles whose diameter has been defined by the configuration means 245.
• This milling means 240 also comprises a means 275 of setting the temperature of the milling medium 240.
• This means 275 for configuring the temperature is, for example, a touch screen on which a computer program displays the current temperature of the milling means 240, an interactive zone enabling a user to increase said temperature and an interactive zone allowing the user to reduce said temperature.
• the inlet 205 of ultrafine particles resulting from a grinding of oilcake is, for example, a conduit connecting the grinding means 240 and the means 210 for tribo-electrostatic charging of the particles received.
• the means 210 for tribo-electrostatic charging of the particles received is, for example, an inner surface of a duct of which at least a portion is made of glass, Teflon, PVC or steel.
• the particles passing through the conduit are charged in contact with the means 210 charge.
• ligno-cellulose charges positive charges and negative charge proteins.
• the particles move in the charging means 210 through the implementation of a dynamic fluidized air bed set in motion by a turbine, for example.
• the means 220 for main electrostatic sorting of the transmitted particles is, for example, a cylindrical conduit on the inner surface of which two diametrically opposite electrodes 225 are placed. One of these electrodes 225 is positively polarized, and the other electrode 225 is negatively polarized. Near each of these electrodes 225 and downstream of the sorting means 220 are positioned two ducts configured to allow the passage of the particles being attracted by one or the other of the electrodes 225. The negatively charged particles by means 210 of charge are attracted to the positively charged electrode 225. The positively charged particles by the charging means 210 are attracted to the negatively charged electrode 225.
• This main electrostatic sorting means 220 further comprises means 280 for scraping the electrode of the main electrostatic sorting means 220.
• This scraper means 280 is, for example, a flexible plastic shape configured to match the shapes of the electrode 225 on which the shape is placed. This form is set in motion by a mechanical motor when the device is stopped.
• This scraping means 280 is configured to collect the particles thus scraped.
• Scraped particles have the particularity of having a large number of fractions attracted by the electrode 225, to the point that these particles are attached to the electrode 225.
• the particles collected by the scraping means 280 comprise mainly fractions comprising ligno-cellulose.
• This means 220 of main electrostatic sorting further comprises a means
• This polarity inversion means is for example an electronic circuit, implemented a tenth of a second every minute, configured to invert the polarity of the electrode 225.
• the polarity inversion makes it possible to collect the particles fixed on said electrode 225.
• the main electrostatic sorting means 220 comprises a scraper means 280 and a polarity reversal means 285 for each electrode 225 of the sorting means 220.
• a means 250 secondary electrostatic sorting is positioned at the end of each of the conduits of the main electrostatic sorting means 220.
• Each of these secondary electrostatic sorting means 250 comprises a positively or negatively polarized electrode.
• the electrode of the secondary sorting means 250 is similarly polarized to the electrode near the conduit to which said secondary sorting means 250 is attached.
• the electrode of the secondary sorting means 250 is reverse biased to the electrode near the conduit to which said secondary sorting means 250 is attached.
• At least one secondary electrostatic sorting means 250 comprises two oppositely polarized electrodes situated on either side of said secondary sorting means 250. In this manner, the particles having a majority of ligno-cellulose-containing moieties are attracted to one of the electrodes while the particles having a majority of protein-containing moieties are attracted to the other electrode.
• Each secondary electrostatic sorting means 250 thus makes it possible, on the one hand, to sort the particles comprising a majority of lignocellulose and, on the other hand, the particles comprising a majority of proteins.
• each secondary sorting means 250 At the outlet of each secondary sorting means 250 are positioned two ducts.
• a first conduit corresponds to a similar sorting result, referred to as "convergent", by the first sorting means 220 and the secondary sorting means 250 the output of which this conduit is positioned.
• a particle having a large proportion of lignocellulose is positively charged, then attracted by the negatively charged electrode in the sorting means 220, and finally attracted by the negatively charged electrode in the secondary sorting means 250.
• the sorting result In the case where the result of the sorting of a particle by the sorting means 220 and the secondary sorting means 250 is different, it is said that the sorting result "diverges”. In the case where the result of the sorting by the sorting means 220 and the secondary sorting means 250 diverges, the particle enters the second conduit at the output of said secondary sorting means 250.
• At least one secondary sorting means 250 comprises at least one scraping means 280 and / or a reverse polarity reversing means 285 similar to those configured for the main electrostatic sorting means 220.
• Each duct configured to receive the particles whose sorting result by the sorting means 220 and the secondary sorting means 250 diverges comprises a means 270 for comparing the particle dimensions with respect to a predetermined limit value.
• This comparison means 270 is, for example, a cyclone type sorter. In variants, this comparison means 270 is a filter configured to retain particles whose dimensions are greater than the predetermined limit value.
• Particles whose dimensions are greater than the predetermined limit value are transmitted to the grinding means 240 to be crushed again.
• Particles smaller than the predetermined limit value are passed back to the load means 210 for sorting.
• the ultrafine particles resulting from the grinding of oilcakes have the advantage of having a very homogeneous chemical composition.
• the tribo-electrostatic charging means 210 allows the particles to charge or discharge in electrons as a function of their main component.
• the main electrostatic sorting means 220 thus separates the particles whose main components are different.
• the device 20 thus separates the ligno-cellulose enriched cake fractions from the protein enriched fractions, these two components having different industrial properties and applications.
• the separation of the components resulting from the plurality of successive sorts produced by the main sorting means 220 and the two means 250 secondary device sorting 20 is then more accurate than if the device 20 had only one means 220 of main electrostatic sorting, as in the device 10 illustrated in FIG.
• the device 20 concentrates the grinding means 240, the receiving means 205, the charging means 210 and each sorting means 220, 250. Thus, the device 20 is more compact. In addition, the powder does not have time to aggregate, to load in moisture, to oxidize or, more generally, to change state between grinding and sorting. The operation of the device is improved.
• the average diameter of the particles at the outlet of the grinding means 240 of the device 20 makes it possible to obtain particles which:
• the means 270 for comparing the device 20 Thanks to the means 270 for comparing the device 20, the particles too large to be efficiently sorted are ground again so as to optimize the sorting of these particles. On the other hand, particles whose dimensions are nominal can be re-sorted without new grinding.
• the means 275 for configuring the temperature of the milling means 240 configured so that the cake reaches a temperature at which at least one component of oilcake becomes brittle allows the milling means 240 to grind the cake more easily into cake particles. oilseeds. It is noted that cryogenics has the advantage of safeguarding proteins and vitamins.
• the electrode-scavenging means 280 of the main electrostatic sorting means 220 makes it possible to collect the particles fixed on the electrode 225), whose electric charge is high, which means that their constitution is particularly homogeneous.
• the means 285 for cyclically inverting the polarity of each electrode 225 of the main electrostatic sorting means 220 makes it possible to detach the particles attached to the electrodes 225), the constitutions of which are particularly homogeneous and of collect the particles fixed on each electrode without mechanical action such as scraping.
• FIG. 3 shows two cyclonic separation units 305 and 310 connected to the same single suction means 315.
• a cyclonic separation unit is a technological unit requiring rapid rotation with a gas in order to separate it. by centrifugation, the fine solid particles which are mixed therein.
• the entries of the cyclonic separation units 305 and 310 respectively constitute the containers 130 or 230, on the one hand, and 135 or 235, on the other hand.
• FIG. 4 shows a particular step logic of the method 40 of the present invention.
• This method 40 comprises:
• step 425 for electrostatically sorting the charged particles to sort the particles into fractions enriched in ligno-cellulose and
• the step 405 of removing the lipid phase of the cake is preferably carried out by a press configured to receive cake, squeeze and add supercritical carbon dioxide.
• the step 410 of grinding the cake thus treated is done with a mill known per se, for example impact or centrifugal.
• the step 415 of ultrafine particles input from the grinding of oilcakes is carried out, for example, by the implementation of a hopper or a funnel configured to allow the reception of ultrafine particles.
• Step 420 of tribo-electrostatic charging is carried out, for example, by the collision between the particles received in the course of the input step 415 and an inner surface of a conduit comprising a portion of PVC, Teflon and / or glass and steel, for example by the implementation of a ventilated air bed with a turbine or a fan for example.
• This air bed displaces the particles to perform charging step 420 and move these charged particles to an electrostatic sorting means.
• Each electrostatic sorting step 425 is carried out, for example, by an electrostatic sorting means, comprising at least one electrode, configured to sort the particles into fractions enriched in lignocellulose.
• the particles comprising fractions enriched in ligno-cellulose are positively charged during step 420.
• the electrostatic sorting means further comprises a conduit near the electrode and a conduit remote from the electrode so that the particles attracted by the electrode penetrate the conduit near the electrode.
• the enzymatic purification step 430 is, for example, carried out by mixing the powdery fraction either with a solution containing an enzymatic cocktail that hydrolyzes the polysaccharides or with water without the enzymes. After enzymatic hydrolysis and / or extraction with water, the purified solid phase is separated by filtration or by centrifugation of the liquid phase which contains the sugars and molecules of interest resulting from hydrolysis and / or extraction .
• step 430 use is made, for example, of a stirred reactor in which the powdery fraction is mixed either with a solution containing an enzymatic cocktail hydrolyzing the polysaccharides, or with water without the enzymes.
• the purified solid phase is separated by filtration or by centrifugation of the liquid phase which contains the sugars resulting from the hydrolysis of the polysaccharides.
• the cellulose which gives the glucose.
• Hemicelluloses in cakes are xylans and arabinogalactans) give xylose and arabinose and galactose.
• This liquid phase rich in monosaccharides such as glucose and xylose, can be used as a fermentation substrate for the production of biofuels or biomolecules for green chemistry.
• solid fractions are richer in proteins or polyphenols including lignin.
• F0 represents the initial sample
• F1 B + represents the fraction obtained on the positively charged electrode when only one stage is used
• F1 - represents the fraction obtained on the negatively charged electrode when only one stage is used
• F2AA- represents the fraction obtained on the negatively charged electrode when, at the input of a second stage, the sample is the fraction F1 A-.
• Table 1 gives the composition, as a percentage of dry mass, of fractions derived from sunflower cake after grinding with a centrifugal grinder equipped with a 0.25 mm grid and separation according to the method which is the subject of the present invention. a difference of potential of 15 KVolts, are at a distance, between them, of 3 cm and measure 30 cm of height for 10 cm of width):
• Table 2 details the protein, lignin and phenolic acid contents, in the case of an impact mill set at 0.1 mm:
• FA is the acronym for "ferulic acid”, for ferulic acid, which has antioxidant properties (food and non-food use).
• p-CA is the acronym for "p-coumaric acid” for p-coumaric acid, which has antioxidant properties (food and non-food use).
• di-FA is the acronym for "Dimer FA", a chemical intermediate for polymer synthesis.
• Vanillic Ac is the abbreviation for vanillic acid.
• the lignin assay method is, for example, the Klason method discussed in the publication Barakat et al. 2014 Applied Energy, 1 13, 97-105.
• Phenolic acids are small molecules bound to both polysaccharides (xylan) and lignin via ester and ether linkages. These phenolic acids can be indicators of fractionation and separation. Phenolic acids also have interesting functional properties including antioxidants.
• Figure 5 shows the composition of the phenolic acids for sunflower from Table 2.
• the leftmost bar, 505 represents the ferulic acid content, the next one to the right, 510, the acid p - coumaric, then dimer ferulic acid, bar 515 and finally vanillic acid, bar 520.
• the implementation of the present invention makes it possible, in the first separation step, to separate a fraction rich in lignin, p-coumaric acid and FA dimer. and vanillic acid, on the one hand, and a protein-rich fraction, on the other hand.
• the second electrostatic sorting step substantially increases the enrichment, especially for the lignin for which the ratio of contents passes from 28.1 (fraction F1 A-), after the first separation step. at 42.2 (fraction F2AA-) after the second.
• fraction F2BB + is very rich in molecules of interest.
• a simple extraction with water is sufficient to extract molecules of interest and to concentrate more the solid fraction in protein.
• the addition of enzyme has an effect on the extraction yield of the molecule, which is almost doubled (see Barakat et al, Applied Energy 2013, 1 13 (2014) 97-105, which details the methods used here to analyze the sugars, the lignin and the enzymatic degradation part mentioned later).
• fraction F2AA- is very rich in sugars (glucose and xylose) and less rich in molecules of interest compared to fractions F2BB +.
• extraction is useful for extracting sugars and further concentrating the lignin solid fraction (see Figure 6).
• Table 3 shows the enrichment of cellulose and hemicellulose, from which bioethanol (cellulose) or biogas (cellulose and hemicellulose) can be generated after grinding with an impact mill (Alpine Hozokawa, registered trademark). with a 0.1 mm grid.
• the electrodes have a difference of potential of 15 KVolts, are at a distance, between them, of 3 cm and measure 30 cm of height for 10 cm of width.
• Xyl means Xylose
• UA means uronic acid
• the Ara / Xyl and Gal / Xyl ratios and the uronic acid content of UA give an indication of the structure of the polymers or polysaccharides. These ratios as well as AUs can be an indicator of splitting and separation.
• uronic acids are often linked to lignin and polysaccharides. These molecules have many applications in green chemistry. Again, the effectiveness of the implementation of the present invention is noted.
• composition As a percentage of dry mass, fractions of cake after grinding on a centrifugal mill with a 0.25 mm grid. (The electrodes have a potential difference of 15 KVolts, are at a distance, between them of 3 cm and measure 30 cm of height and 10 cm of width):
• fraction F1 B + and even more the fraction F2BB +, are enriched in protein and ash and lignin-depleted, compared to the initial sample.
• simple extraction with water is sufficient to extract proteins and thus further concentrate the solid fraction into protein.
• addition of enzyme has an effect on the extraction yield of the molecule, which is almost doubled.
• fraction F1 A- and even more the fraction F2AA-, are enriched in lignin, and depleted in protein and ash, compared to the initial sample.
• extraction is useful for extracting sugars and thereby further concentrating the solid fraction into lignin.
• the lignocellulose obtained by the implementation of the present invention is in the native state, that is to say that it is not modified or denatured, unlike the processes of state of the art.
• the lignin fractions were characterized in terms of ⁇ - ⁇ -4 ⁇ ⁇ "1 binding and S / G ratio (S: syringyl unit and G: guaiacyl unit, two monomers constituting lignin ) in the initial fraction and the fractions enriched in lignin (F-).
• the ⁇ - ⁇ -4 bonds are lignin interpolymer ether bonds, they are the most abundant bonds of native lignin (see "Dry fractionation process as an important step in the future and future lignocellulose biorefineries: A review" in Barakat, H de Vries, Rouau X. Bioresource technology 134, 362-373, incorporated herein by reference).
• the enrichment process comprising a dry fractionation by electrostatic separation followed by a step of enzymatic treatment of the fractions obtained is described.
• the fraction F1 A-, and even more the fraction F2AA- are enriched in lignin, and depleted in protein and ash, relative to the original sample.
• extraction is useful for extracting sugars and thereby further concentrating the solid fraction into lignin.
• enzymatic purification and / or extraction is described in detail to enrich the protein and polyphenol fractions (lignin and phenolic acids) by degradation or hydrolysis of the polysaccharides to monosaccharides (glucose , xylose, arabinose ).
• Figure 6 shows the mechanical and enzymatic fractionation of the cake.
• the electrostatic separation provides a F2BB + 610 fraction and a F2AA-615 fraction.
• F2BB + 610 fraction fractions are hydrolyzed by a commercial enzyme (cellulase + xylanase) cocktail (Sigma, registered trademark) in a 10% liquid medium.
• w / v mass per volume
• pH 5 pH 5 at 37 ° C for 72 hours.
• the solutions were centrifuged or filtered, two solid and liquid fractions were obtained:
• the solid fraction 620 rich in proteins (72% w / w), comes from the fraction F2BB + 610,
• the liquid fraction 625 rich in sugars and soluble proteins comes from the fraction F2BB + 610
• the solid fraction 630 rich in lignin, comes from the fraction F2AA-615 and
• the liquid fraction 635 rich in soluble sugars, is derived from the fraction F2AA-615.
• Liquid fractions 625 and 635 were characterized in terms of soluble sugars and solid fractions 620 and 630 were characterized in terms of lignins and proteins.
• the white rectangles represent the proportions, by mass, in the liquid fraction 625 resulting from the fraction F2BB + 610,
• the hatched rectangles represent the proportions, by mass, in the liquid fraction 635 resulting from the fraction F2AA-615,
• the fiber-rich fraction F2AA-615 produces more glucose (C6) in a proportion of 0.25 kg. kg -1 , 0.087 kg.kg -1 xylose (C5) and 0.0064 kg. kg- 1 of arabinose (C5) in a proportion of 0.09 kg.kg- 1 .
• the fraction F2BB + 610 produces practically no glucose (approximately 0.002 kg.kg- 1 ), 0.032 kg.kg- 1 xylose (C5) and 0.035 kg.kg- 1 arabinose (C5), this fraction being rich in soluble proteins (and other molecules of interest).
• the fractions (F-) can be valorized, by fermentation, in bioenergy in the form of ethanol 640.
• the sugars resulting from the F2AA- fraction after the enzymatic hydrolysis are fermented by yeasts to produce the ethanol according to the method described by Barakat et al. 2015 ("Innovative Combined Dry Fractionation Technologies for Rice Stripping to Biofuels", Chuetor S, Luque R, Barron C, Solhy A, Rouau X, Barakat A, Green Chemistry, 2015 DOI: 10.1039 / C4GC01718H, incorporated herein by reference).
• the yield of ethanol produced after a fermentation of 72 hours is of the order of 0.1035 kg.kg-1 obtained with the negatively charged fraction (F2A-).
• Solid fractions (scheme 1) were also characterized. The results clearly show that this enzymatic hydrolysis step further enriched the positively charged protein fractions (72% w / w) and negatively charged lignin fractions (65% w / w).

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