• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
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    • 专利摘要:
    The process (40) for fractionating dry oil cake comprises: - a step (410) of grinding oilseed cake into a powder of ultrafine particles, - a step (420) of tribo-electrostatic particle loading ultrafine particles of said powder and at least one trajectory deflection step (425) in the electric field of the charged particles to sort the particles and provide at least one fraction enriched in lignocellulose.
    公开号:FR3015311A1
    申请号:FR1363534
    申请日:2013-12-24
    公开日:2015-06-26
    发明作者:Abdellatif Barakat；Xavier Rouau
    申请人:Institut National de la Recherche Agronomique INRA；
    IPC主号:
    专利说明:

    [0001] TECHNICAL FIELD OF THE INVENTION 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. STATE OF THE ART Oilseed cakes are the solid residues obtained after the extraction of oil from seeds or fruits of oleaginous plants, such as sunflower, rapeseed or soya beans, 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. However, 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. In current systems, as described in European Patent No. 1,908,355 published April 9, 2008, it is first carried out a grinding of oilcakes. These particles rich in proteins or fibers resulting from the grinding are then separated by sorting in a corona electric field. However, the efficiency of this sorting in an electric field is low and therefore the separation of protein rich fractions and fiber rich fractions is unsatisfactory. In addition, the separation rate is very low. On the other hand, these systems operate with particles whose size is between 250 micrometers and 1400 micrometers and therefore do not allow sorting of finer particles. However, the finer the particles, and the more homogeneous their composition, and their content in protein or fiber is likely to be high. On the other hand, the particles resulting from a grinding of oilcakes are not very prone to electric attraction. In another system of the prior art, described in European Patent No. 1,441,858 published on August 4, 2004, the sorting of particles resulting from the grinding of its wheat in an electric field makes it possible to separate particles respectively corresponding to the aleurone and the envelopes of cereal grains. However, these systems do not work in the case of fine particles. On the other hand, these particles, even fine, are after grinding naturally little prone to electrical attraction. OBJECT OF THE INVENTION The present invention aims to remedy all or part of these disadvantages. For this purpose, according to a first aspect, the present invention is directed to a process for fractionating dry oil cake, which comprises: a step of grinding oilseed cake into a powder of ultrafine particles, a step tribo-electrostatically charging ultrafine particles of said powder and - at least one trajectory deflection step in the electric field of the charged particles to sort the particles and provide at least one enriched lignocellulose fraction. By "ultrafine particles" is meant a set of particles whose median diameter (d50) is less than 500 μm. 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 the oleaginous and others are mainly composed of proteins of the oleaginous 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. It is observed that the lignocellulose thus obtained is in the native state, that is to say, it is not modified or denatured, unlike the methods of the state of the art such as the ORGANOSOLV process ( trademark) of lignin extraction (see "Quantitative structural characterization and thermal properties of birch lignins after 30 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, pages 1663-1671), which comprises denaturation by chemical treatment.
    [0002] In advantageous embodiments, 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. Thus, the device is more compact. In addition, 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. In embodiments, 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. In embodiments, the method that 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. These embodiments make it possible to collect the particles fixed on the electrode, whose electric charge is high, which means that their constitution is particularly homogeneous. In embodiments, the method which is the subject of the present invention further comprises a step of cyclically reversing the polarity of each electrode of an electrostatic sorting means implemented during the deflection step. These embodiments make it possible to detach the particles attached to the electrodes, whose constitutions are particularly homogeneous and to collect the particles fixed on each electrode without mechanical action such as scraping.
    [0003] In embodiments, the method which is the subject of the present invention comprises, downstream of the deflection step, at least one secondary deviation step. The separation of the components resulting from the plurality of successive sorts produced by the method is then more precise.
    [0004] In embodiments, during a secondary deflection step, a particulate tribo-electrostatic charging means is supplied which, during the deflection steps, is alternately deflected to a positive electrode and a negative electrode or vice versa.
    [0005] The advantage of these embodiments is that they allow the particles which, during two successive sorts (first and second stages), have been deviated once towards the positive electrode and once towards the negative electrode, to follow a new implementation of the method object of the present invention.
    [0006] In embodiments, the method which 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. Thus purification and / or enzymatic extraction (cellulase and hemicellulases) 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.). ). In embodiments, 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. Thanks to these provisions, the particles that are too large to be sorted efficiently are crushed again so as to optimize their sorting. On the other hand, particles whose dimensions are nominal can be sorted again without further grinding. In embodiments, during the charging step, a dynamic fluidized air bed is used. The implementation of a fluidized air bed allows both the formation of electrostatic charges on moving particles and their separation for sorting. The present invention aims, according to a second aspect, an application of the method that is the subject of the present invention to obtain fractions enriched with lignocellulose. The object of the present invention is, according to a third aspect, an application of the method which is the subject of the present invention to obtain fractions enriched in proteins.
    [0007] 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.
    [0008] 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 object 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 of phenolic derivatives from lignin-enriched fractions. The phenolic derivatives include, in particular, tannins and phenolic acids. The advantages, aims and particular characteristics of the applications object of the present invention being similar to those of the method object of the present invention, they are not recalled here. BRIEF DESCRIPTION OF THE FIGURES Other advantages, aims and particular characteristics of the invention will emerge from the following nonlimiting description of at least one particular embodiment of the device and the fractionation method which are the subject of the present invention, with regard to FIG. FIG. 1 is a diagrammatic sectional representation of a first particular embodiment of the device which is the subject of the present invention, and FIG. 2 is a diagrammatic sectional view of a second particular embodiment. 3 shows 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 which is the subject of the present invention and FIG. 5 represents, in the form of a histogram, the distribution phenolic acids obtained by carrying out the process which is the subject of the present invention with a sunflower cake.
    [0009] DESCRIPTION OF EXAMPLES OF EMBODIMENT OF THE INVENTION The present description is given in a non-limiting manner. As of now, we note that the figures are not to scale. 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. According to another definition, an "ultrafine" is a powder of which half (50%) by volume, fibers have a diameter of less than 500 micrometers, preferably less than 200 micrometers, more preferably less than 100 micrometers and even more preferentially less than 100 micrometers. 50 micrometers. To measure the particles, a laser granulometer can be implemented. FIG. 1 shows a first embodiment of the device 10 which is the subject of the present invention. This device 10 comprises: an inlet 105 of ultrafine particles resulting from a grinding of oilcake, a means 110 for tribo-electrostatic charging of the particles received and a means 120 for the main electrostatic sorting of the particles transmitted. The inlet 105 of ultrafine particles is, for example, a hopper or 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 110 arranged, for example, under the inlet 105 of particles. This charging means 110 is configured so that the particles pass through this charging means 110 by gravitational force. In variants, 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"). In variants, this surface comprises at least a Teflon portion. In other variants, this surface comprises at least one glass part. In other variants, 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 110 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. At the outlet of this main electrostatic sorting means 120, 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. In particular, the particles enriched in ligno-cellulose are charged in the means 110 for charging positive charges. As a result, these ligno-cellulose enriched particles are attracted to a negatively polarized electrode.
    [0010] Thus, 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. The ultrafine particles resulting from the grinding of oilcakes have the advantage of having a very homogeneous chemical composition. The tribo-electrostatic charging means 110 allows the particles to charge or discharge into electrons according to their main chemical component. The main electrostatic sorting means 120 thus separates the particles whose main components are different. The device 10 thus separates the fractions of cake enriched with lignocellulose.
    [0011] FIG. 2 shows a second particular embodiment of the device 20 of the present invention. This device comprises: a means 240 for grinding ultrafine particle powder cake comprising: a means 245 for configuring the grinding fineness achieved by the grinding means 240 and a means 275 for configuring the temperature of the medium 240 grinding; an inlet 205 of ultrafine particles resulting from a grinding of oilseed cake, a means 210 for tribo-electrostatic charging of the particles received, a means 220 for the main electrostatic sorting of the transmitted particles which comprises: two electrodes 225; an electrode-scraping means 280 of the main electrostatic sorting means 220 and a means 285 for inverting the polarity of an electrode 225 of the main electrostatic sorting means 220; two secondary electrostatic sorting means 250 each comprising two electrodes 255 and two means 270 for comparing the particle dimensions with respect to a predetermined limit value. 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. Depending on the fineness of grinding configured, the milling means 240 is configured to grind the powder cake of particles whose diameter has been defined by the configuration means 245. This grinding means 240 also comprises a means 275 for configuring the temperature of the milling means 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. In particular, 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.
    [0012] 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.
    [0013] 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.
    [0014] This scraping means 280 is configured to collect the particles thus scraped. The 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. For example, in the case of a negatively charged electrode 225, the particles collected by the scraping means 280 comprise mainly fractions comprising lignocellulose. This main electrostatic sorting means 220 further comprises a means 285 for inverting the polarity of an electrode 225 of the main electrostatic sorting means 220. 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 In variants, 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. At the end of each of the conduits of the main electrostatic sorting means 220, a means 250 secondary electrostatic sorting is positioned. 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. In variants, the electrode of the secondary sorting means 250 is reverse biased to the electrode in the vicinity of the conduit to which said secondary sorting means z0 250 is attached. In variants, 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, particles having a majority of ligno-cellulose-containing moieties are attracted to one of the electrodes while 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. 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 at the output of which this conduit is positioned. For example, a particle having a large proportion of ligno-cellulose 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. 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. In variants, 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. Ultrafine particles 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, both of which have different industrial properties and applications. In addition, the separation of the components resulting from the plurality of successive sorts made by the main sorting means 220 and the two means 250 secondary sorting device 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 Figure 1. The device 20 concentrates the grinding means 240, the receiving means 205, the means 210 for charging 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 mean diameter of the particles at the outlet of the grinding means 240 of the device 20 makes it possible to obtain particles which: have a homogeneous chemical composition and, once charged, remain mobile as a function of their charge in the presence of the electrodes. Thanks to the means 270 for comparing the device 20, the particles that are 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 grinding means 240 configured so that the cake reaches a temperature at which at least one component of oilcake becomes brittle allows the grinding means 240 to grind the cake more easily. oilseed cakes. It is noted that cryogenics has the advantage of safeguarding proteins and vitamins. The implementation of a fluidized air bed allows both the formation of electrostatic charges on the moving particles and their separation for sorting. The electrode scraper means 225 of the main electrostatic sorting means 220 collects the particles attached to the electrically charged electrode 225, 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) whose constitutions are particularly homogeneous and to collect the fixed particles. on each electrode without mechanical action such as scraping. By scraping or reversing the polarity, the particles attached to each electrode are peeled off and collected. FIG. 3 shows two cyclonic separation units 305 and 310 connected to the same single suction means 315. It is recalled that a cyclonic separation unit is a technological unit requiring a fast rotation to a gas in order to to separate, 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 process 40 comprises: a step 405 for removing the lipid phase from the cakes, a step 410 for grinding the cakes, a step 415 for entering ultrafine particles resulting from the grinding of oilcake, a step 420 tribo-electrostatic charge of the particles received, - at least one step 425 of electrostatic sorting of the charged particles to sort the particles into fractions enriched in lignocellulose and - a step 430 of enzymatic purification. 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. In particular, the particles comprising fractions enriched in ligno-cellulose are positively charged during step 420. Consequently, these fractions enriched in ligno-cellulose are attracted by a negatively polarized electrode during the sorting step 425. . 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 . To carry out 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. 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 resulting from the hydrolysis of the polysaccharides. In the degradation of the polysaccharides of the cakes by the enzymes, it is especially 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. In contrast, solid fractions are richer in protein or polyphenols. EXAMPLE 1 - Fractionation of sunflower cake 301 5 3 1 1 An ultrafine powder was obtained by grinding in an impact mill provided with a 0.1 mm grid and subjected to separation of the fractions as set out with reference to FIGS. 4. In the result tables below: FO represents the initial sample, F1 B + represents the fraction obtained on the positively charged electrode when only one stage is used, F1A- represents the fraction obtained on the When a negatively charged electrode is used when only one stage is used, F2BB + represents the fraction obtained on the positively charged electrode 10 when, at the input of a second stage, the sample is the fraction F1 B + and 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 provided with a 0.25 mm grid and separation according to the process which is the subject of the present invention. have a difference of potential of 15 KVolts, are at a distance, between them, of 3 cm and measure 30 cm of height and 10 cm of width): Substrate Fraction Protein Ash Lignin zo Sunflower FO 30.4 6.2 21.2 F1B + 46.7 7.4 6.7 F1 A - 10.6 5.2 28.1 F2BB + 58.8 8.6 1.1 F2AA-10.2 4.2 42.2 25 Table 2 details the protein, lignin and phenolic acid contents in the case of an impact mill set at 0.1 mm: 30 Fractions Composition (mg / g) Vanillic Ac (4) 0.049 0.011 0.100 0.012 Lignin FO Proteins Phenolic acids 21.2 7.5 39.4 4.2 F1B + F1 A-F2BB + FA (1) p-CA (2) di-FA (3) 30 , 80 0.068 0.028 0.019 57.43 0.044 0.026 0.003 5.10 0.087 0.034 0.040 55.67 0.042 0.025 0.003 F2AA-6.99 0.094 0.034 0 , 039 0.098 40.8 (1) "FA" is the acronym for "ferulic acid", for ferulic acid, which has antioxidant properties (food and non-food use). (2) "p-CA" is the acronym for "p-coumaric acid" for p-coumaric acid, which has antioxidant properties (food and non-food use). (3) "di-FA" is the acronym for "Dimer FA", a chemical intermediate for polymer synthesis. (4) "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, 113, 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 phenolic acids for sunflower from Table 2. For each fraction, the leftmost bar, 505, represents the ferulic acid content, the next one to the right, 510, the coumarinic acid then dimer ferulic acid, bar 515 and, finally, vanillic acid, bar 520. As can be seen from Table 1 and FIG. 5, the use of the present invention makes it possible, as soon as the first separation step, to separate a fraction rich in lignin, p-coumaric acid, FA dimer and vanillic acid, on the one hand, and a protein-rich fraction, on the other hand. It can also be seen in this table 1 that the second electrostatic sorting step substantially increases the enrichment, especially for the lignin for which the ratio of contents passes from 28.1 (fraction F1A-), after the first separation step. at 42.2 (fraction F2AA-) after the second. After analysis, it is found that the F2BB + fraction is very rich in molecules of interest. For this fraction, a simple extraction with water is sufficient to extract molecules of interest and to concentrate more the solid fraction in protein. It is noted, however, that 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, 113 (2014) 97-105, which details the methods used here to analyze the sugars, the lignin and the enzymatic degradation part mentioned later). For its part, the fraction F2AA- is very rich in sugars (glucose and xylose) and less rich in molecules of interest compared to fractions F2BB +. For this fraction, extraction is useful for extracting sugars and further concentrating the solid fraction into lignin. Table 3, below, 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.
    [0015] Fractions Cellulose Hemicelluloses Gal 0.11 0.35 0.02 0.38 0.03 Ac Glc Ac Gal Total FO 17.61 7.79 23.00 7.82 24.02 Xyl Ara 2.23 0.40 13, 60 F1 B + F1 A- F2BB + F2AA- 9.53 1.32 1.93 0.03 7.79 4.42 1.06 3.05 0.46 17.17 12.35 1.29 1.99 0, 04 8.49 4.87 1.21 3.24 0.76 19.37 13.75 1.59 The Ara / Xyl, Gal / Xyl and UA ratios then stand out as given in Table 4, below: Ara / Xyl 0.138 0.239 0.104 0.248 0.116 G al / Xyl 0.012 0.079 0.002 0.078 0.002 AU 2.63 1.96 3.51 2.03 4.00 FO F1 B + F1 A-F2BB + F2AA- "Ara" means Arabinose "Xyl" means Xylose "Gal" means Galactose "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. In addition, uronic acids are often linked to lignin and polysaccharides. These molecules have many applications in green chemistry. Again, the effectiveness of the practice of the present invention is found. To estimate the interest of the enzymatic purification, 2 g of each Fraction were dissolved in 20 ml of water with no commercial enzyme (20 U / g substrate) with stirring for 72 hours at 37 ° C. Both liquid and solid fractions were separated by centrifugation.
    [0016] EXAMPLE 2 - Separation of rapeseed meal With regard to the 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): Substrate Fraction Protein Lignin Coir FO 38.5 5.6 14.6 F1B + 47.6 6.2 9.6 F1 A- 27.6 4.4 24.7 F2BB + 57.9 6.8 7.6 F2AA- 18.4 4.2 35.4 After analysis, it can be seen that the fraction F1 B +, and even more the fraction F2BB +, are enriched in protein and ash and are depleted in lignin, compared to the initial sample. . For these fractions, simple extraction with water is sufficient to extract proteins and thus further concentrate the solid fraction into protein. It is noted, however, that the addition of enzyme has an effect on the extraction yield of the molecule, which is almost doubled. For its part, the fraction F1 A-, and even more the fraction F2AA-, are enriched in lignin, and depleted in protein and ash, compared to the initial sample.
    [0017] For these fractions, extraction is useful for extracting sugars and thereby further concentrating the solid fraction into lignin.
    权利要求:
    Claims (15)
    [0001]
    REVENDICATIONS1. A process (40) for fractionating dry oil cake, characterized in that it comprises: - a step (410) of grinding oilseed cake into a powder of ultrafine particles, - a step (420) of tribo-electrostatic charge of ultrafine particles of said powder and - at least one step (425) of path deflection in the electric field of the charged particles to sort the particles and provide at least one fraction enriched in ligno-cellulose.
    [0002]
    The method (40) of claim 1, wherein the grinding step (410) comprises a step of configuring the mill to obtain a predetermined fineness.
    [0003]
    3. Method (40) according to one of claims 1 or 2, which further comprises an electrode scraping step of an electrostatic sorting means implemented during the step (425) of deflection to collect particles attached to an electrode after the particle deflection step.
    [0004]
    4. Method (40) according to one of claims 1 to 3, which further comprises a cyclic reversal step of the polarity of each electrode of an electrostatic sorting means implemented during the step deviation.
    [0005]
    5. Method (40) according to one of claims 1 to 4, which comprises, downstream of the step (425) deflection, at least one secondary deflection step.
    [0006]
    The method (40) of claim 5, wherein, during a secondary deflection step, a tribo-electrostatic charge means is supplied to particles which, during the deflection steps, are alternately deflected to a positive electrode. and a negative electrode or vice versa.
    [0007]
    7. Process (40) according to one of claims 1 to 6, which further comprises, downstream of at least one deflection step, a step (430) of enzymatic purification of the sorted particles.
    [0008]
    8. Method (40) according to one of claims 1 to 7, which comprises, downstream of at least one deflection step (425), a step of comparing the particle dimensions with respect to a predetermined limit value and a step of feeding a grinding means into particles whose dimensions are greater than the predetermined limit.
    [0009]
    9. Process (40) according to one of claims 1 to 8, wherein, during the charging step (420), is implemented a dynamic fluidized air bed.
    [0010]
    10. Application of the method (40) according to one of claims 1 to 9 for obtaining fractions enriched in ligno-cellulose.
    [0011]
    11. Application of the method (40) according to one of claims 1 to 9 for obtaining enriched fractions protein. zo
    [0012]
    12. Application of the method (40) according to one of claims 1 to 9 for the generation of biofuel from ligno-cellulose enriched fractions.
    [0013]
    13. Application of the process (40) according to one of claims 1 to 9 for the generation of biogas from fractions enriched in lignocellulose. 25
    [0014]
    14. Application of the process (40) according to one of claims 1 to 9 for obtaining fractions enriched polysaccharides.
    [0015]
    15. Application of the process (40) according to one of claims 1 to 9 to the extraction of phenolic derivatives from lignin-enriched fractions.
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    同族专利:
    公开号 | 公开日
    US20160310957A1|2016-10-27|
    FR3015311B1|2016-01-01|
    WO2015097290A1|2015-07-02|
    EP3086880A1|2016-11-02|
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    法律状态:
    2015-12-23| PLFP| Fee payment|Year of fee payment: 3 |
    2016-12-29| PLFP| Fee payment|Year of fee payment: 4 |
    2018-09-28| ST| Notification of lapse|Effective date: 20180831 |
    优先权:
    申请号 | 申请日 | 专利标题
    FR1363534A|FR3015311B1|2013-12-24|2013-12-24|PROCESS FOR FRACTIONING OIL MEALS AND APPLICATIONS THEREOF|FR1363534A| FR3015311B1|2013-12-24|2013-12-24|PROCESS FOR FRACTIONING OIL MEALS AND APPLICATIONS THEREOF|
    EP14824012.0A| EP3086880A1|2013-12-24|2014-12-24|Method for the fractionation of an oilseed cake, and applications of said method|
    US15/103,843| US20160310957A1|2013-12-24|2014-12-24|Method for the fractionation of an oilseed cake, and applications of said method|
    PCT/EP2014/079320| WO2015097290A1|2013-12-24|2014-12-24|Method for the fractionation of an oilseed cake, and applications of said method|
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