EP3156474A1 - Method for recovering lipids using a ball mill - Google Patents
Method for recovering lipids using a ball mill Download PDFInfo
- Publication number
- EP3156474A1 EP3156474A1 EP16193842.8A EP16193842A EP3156474A1 EP 3156474 A1 EP3156474 A1 EP 3156474A1 EP 16193842 A EP16193842 A EP 16193842A EP 3156474 A1 EP3156474 A1 EP 3156474A1
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- EP
- European Patent Office
- Prior art keywords
- biomass
- volume
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- phase
- ball mill
- Prior art date
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- 150000002632 lipids Chemical class 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000002028 Biomass Substances 0.000 claims abstract description 44
- 239000000203 mixture Substances 0.000 claims abstract description 22
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 238000011049 filling Methods 0.000 claims abstract description 8
- 239000011324 bead Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000005119 centrifugation Methods 0.000 claims description 15
- 238000000926 separation method Methods 0.000 claims description 9
- 239000006228 supernatant Substances 0.000 claims description 8
- 239000008188 pellet Substances 0.000 claims description 6
- 238000011084 recovery Methods 0.000 claims description 5
- 240000009108 Chlorella vulgaris Species 0.000 claims description 4
- 235000007089 Chlorella vulgaris Nutrition 0.000 claims description 4
- 241000195646 Parachlorella kessleri Species 0.000 claims description 4
- 241000405713 Tetraselmis suecica Species 0.000 claims description 4
- 230000001133 acceleration Effects 0.000 claims description 3
- 241000195633 Dunaliella salina Species 0.000 claims description 2
- 241000362749 Ettlia oleoabundans Species 0.000 claims description 2
- 241000168517 Haematococcus lacustris Species 0.000 claims description 2
- 241001300629 Nannochloropsis oceanica Species 0.000 claims description 2
- 241000159660 Nannochloropsis oculata Species 0.000 claims description 2
- 241000509521 Nannochloropsis sp. Species 0.000 claims description 2
- 241001494715 Porphyridium purpureum Species 0.000 claims description 2
- 239000012071 phase Substances 0.000 description 28
- 102000004169 proteins and genes Human genes 0.000 description 16
- 108090000623 proteins and genes Proteins 0.000 description 16
- 238000009482 thermal adhesion granulation Methods 0.000 description 9
- 150000001875 compounds Chemical class 0.000 description 7
- 235000020777 polyunsaturated fatty acids Nutrition 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 238000000605 extraction Methods 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 239000011521 glass Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 150000003626 triacylglycerols Chemical class 0.000 description 4
- 229930186217 Glycolipid Natural products 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 210000004027 cell Anatomy 0.000 description 3
- 229940082150 encore Drugs 0.000 description 3
- 238000005194 fractionation Methods 0.000 description 3
- 239000002609 medium Substances 0.000 description 3
- 150000003904 phospholipids Chemical class 0.000 description 3
- 241000195649 Chlorella <Chlorellales> Species 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 150000004676 glycans Chemical class 0.000 description 2
- 239000001963 growth medium Substances 0.000 description 2
- 238000000265 homogenisation Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000002207 metabolite Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 229920001282 polysaccharide Polymers 0.000 description 2
- 239000005017 polysaccharide Substances 0.000 description 2
- 238000011403 purification operation Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 235000000346 sugar Nutrition 0.000 description 2
- 206010001488 Aggression Diseases 0.000 description 1
- 238000000035 BCA protein assay Methods 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- 230000005526 G1 to G0 transition Effects 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 241001639412 Verres Species 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000016571 aggressive behavior Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000010296 bead milling Methods 0.000 description 1
- 239000003225 biodiesel Substances 0.000 description 1
- 239000002551 biofuel Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 210000003850 cellular structure Anatomy 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000009089 cytolysis Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
- 230000036425 denaturation Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 125000003473 lipid group Chemical group 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000002417 nutraceutical Substances 0.000 description 1
- 235000021436 nutraceutical agent Nutrition 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000008194 pharmaceutical composition Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 1
- 238000002525 ultrasonication Methods 0.000 description 1
- 238000010977 unit operation Methods 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
-
- 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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
-
- 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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/06—Production of fats or fatty oils from raw materials by pressing
-
- 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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
Definitions
- the present invention relates to the field of valorization of algal biomass, more precisely the present invention relates to a process for extracting lipids from microalgae.
- Microalgae are eukaryotic organisms, mostly unicellular, delimited by a plasma membrane and a wall.
- the composition and structure of this wall may be variable depending on the microalga considered.
- some green microalgae such as Chlorella, it is made of cellulose and has a high rigidity resulting in a high resistance of the alga vis-à-vis mechanical stresses.
- the wall also called frustule, is made of crystallized silica.
- the latter is more brittle than that of Chlorella.
- microalgae find many applications in particular in food, cosmetics, pharmaceuticals ...
- many research is conducted on algal biomass from the perspective of use as biofuel.
- microalgae The main metabolites of microalgae, namely polysaccharides, proteins and pigments, are generally soluble in the culture medium.
- microalgae can, under certain conditions, accumulate large amounts of lipids in the form of triglyceride globules known as "TAG” (for triglycerides of fatty acids).
- TAG triglyceride globules
- PUFAs polyunsaturated fatty acids
- the object of the present invention is precisely the recovery of lipids from the algal biomass and more precisely triglycerides of fatty acids and polyunsaturated fatty acids.
- This method involves a high energy consumption linked to the drying of the biomass, which also causes a degradation of certain thermosensitive compounds such as vitamins, pigments or certain proteins.
- certain thermosensitive compounds such as vitamins, pigments or certain proteins.
- the series of operations and the large quantities of solvents involved complicate the process and increase production costs.
- One of the main advantages of the process according to the invention is that it can be used on a biomass without it being dried beforehand.
- the method according to the invention thus makes it possible to avoid the implementation of a drying step, which is long and expensive, both in energy and in financial terms.
- US2013 / 0338384 discloses a method of recovering lipids from a microalgal biomass comprising heating said biomass at a temperature of from 80 ° C to 150 ° C at a pressure of from 1 to 5 bar.
- the technical problem at the origin of the present application was to have a lipid fractionation process contained in a micro-algal biomass that does not require drying said biomass, which makes it possible to overcome the use of solvents and which leads to the production of a composition whose different constituents can then be easily separated.
- the conditions for carrying out grinding according to the invention make it possible to ensure the release of almost all the droplets of triglycerides, while ensuring a partial deconstruction of the cellular structures causing the release of some or all of the phospholipids and glycolipids.
- the conditions for carrying out the grinding according to the invention make it possible to avoid excessive homogenization of the medium, and consequently to avoid emulsion formation.
- composition obtained after grinding has the advantage of being then easily recoverable.
- a second object of the invention is the composition that may be by the method according to the invention.
- the centrifugation step is carried out directly on the composition obtained at the end of the step using a ball mill, that is to say that the centrifugation step is carried out after the step using a ball mill without intermediate step (s) except the step of recovering said composition obtained.
- the process according to the invention thus makes it possible to fractionate the lipids and the proteins contained in microalgae without drying the biomass (wet extraction) nor to use solvents, thus avoiding the denaturation of the compounds while limiting the volumes to be treated.
- Another advantage of the process according to the invention is that it can be used directly on the culture medium, in particular on a suspension of micro-algae at the output of production, which contributes to reducing the volumes of water used. to implement said method.
- the process according to the invention makes it possible to work on a concentrated biomass directly harvested after cultivation.
- a grinding step and a phase separation step it is possible to obtain directly three phases selectively enriched in different compounds: a first phase called “superculot” rich in lipids, a second phase called “supernatant” rich in proteins and a third phase called “pellet” rich in insoluble compounds.
- the superculot and the pellet can thus be directly recoverable, the supernatant can be subjected to a membrane filtration operation allowing either the separation of proteins and solubilized sugars from TAGs, ie the concentration of proteins and TAGs to arrive at two purified fractions.
- the process according to the present invention is carried out using a micro-algal biomass sufficiently rich in lipids and sufficiently concentrated, so that the microalgal biomass comprises at least 15%, preferably approximately 17.5% by weight of lipids. relative to the total mass of the biomass, in addition the micro-algal biomass has a dry matter concentration of between 1 g / l and 200 g / l, preferably between 5 g / l and 150 g / l and even more preferably between 35 g / l and 100 g / l, that is to say with respect to the volume of microalgal biomass to be treated.
- the microalgal biomass comprises at least one microalga chosen from Nannochloropsis sp., Nannochloropsis oceanica, Nannochloropsis oculata, Tetraselmis suecica , Porphyridium cruentum, Parachlorella kessleri, Dunaliella salina, Chlorella vulgaris, Neochloris oleoabundans and Haematococcus pluvialis and preferably from the following strains Nannochloropis oceanica, Parachlorella kessleri, Tetraselmis suecica.
- the method according to the invention comprises a step during which a ball mill is used.
- Ball mills are typically used for the homogenization of viscous products such as paints and also for grinding minerals.
- Ball mills comprise an enclosure, for example a bowl closed by a cover, intended to receive the composition to be treated, said enclosure being fed via a pump in composition to be treated.
- the filling rate in balls of the mill corresponding to the percentage of the volume of the bowl occupied by the beads, ranges from 50% to 80%, preferably from 70% to 80% volume / volume and preferably from about 75% volume / volume.
- the content of the enclosure excluding beads, essentially includes microalgal biomass.
- the filling rate may be adapted in particular according to the nature of the balls used. Indeed in some cases, an agglomeration of the balls between the blades of the agitator could be observed.
- the feed rate of the composition in the mill generally ranges from 150 ml / min to 200 ml / min. It is also within the skill of those skilled in the art to select the feed rate adapted to the medium to be treated.
- the treatment in a ball mill is carried out for a duration (residence time) ranging from 1 to 30 minutes, preferably from 2 to 20 minutes, more preferably from 4 to 10 minutes and advantageously from about 6 to 10 minutes. minutes.
- duration time ranging from 1 to 30 minutes, preferably from 2 to 20 minutes, more preferably from 4 to 10 minutes and advantageously from about 6 to 10 minutes. minutes.
- Ball mill treatment is generally carried out at a temperature, generally controlled, ranging from 18 ° C to 40 ° C, preferably from 18 to 25 ° C.
- the composition obtained is advantageously recovered.
- a single ball milling step is performed.
- the treatment in a ball mill is repeated at least twice, preferably between two and ten times and advantageously between three and four times.
- this method is implemented in " batch " in order to be able to treat a biomass volume in a simple manner.
- the first phase, the superculot generally comprises more than 30%, preferably more than 60% of lipids, it also comprises proteins in a limited amount of between 10 and 30% allowing a direct valuation of the superculot.
- the first phase essentially comprises a mixture of triglycerides (TAG) and polyunsaturated fatty acids called "PUFA", in the form of phospholipids and glyco lipids.
- TAG triglycerides
- PUFA polyunsaturated fatty acids
- the second phase generally comprises more than 20%, preferably more than 40% of proteins and also a large amount of lipids.
- the supernatant can be subjected to one or more operation (s) of separation of proteins and lipids including TAG to obtain two purified fractions, advantageously this / these operation (s) separation can be performed (s) by means of a membrane.
- At least one lipid separation step is performed on the second phase.
- the lipids in particular TAGs isolated at the end of the separation operation (s) and the superculot or even the lipids isolated from the superculot are advantageously gathered.
- the third phase, the pellet, is rich in insoluble compounds.
- the base can be directly valorizable.
- the purification operations of the components are facilitated in particular due to the fact that the three phases are selectively enriched in different compounds.
- the method according to the invention should be considered as allowing a targeted and almost total recovery of lipids.
- Lipids are used in chemical, cosmetic or pharmaceutical compositions, in nutraceuticals, especially in animal feed.
- Nannochloropis oceanica a biomass of Nannochloropis oceanica is used. This biomass was grown in tubular photobioreactor of 10 L.
- the biomass was treated using a glass ball mill (DynoMill Mutlilab, WAB, Switzerland) under the conditions specified in each example.
- the lipid assay is performed by Folch's method.
- Proteins are measured by absorbance at 280 nm, possibly supplemented by a BCA protein assay to verify the accuracy of spectrophotometric measurements.
- the superculot and the pellet can thus be directly recoverable, the supernatant can be subjected to an operation of separation of proteins and TAG (membranes) leading to two purified fractions.
Abstract
La présente invention un procédé de traitement d'une biomasse micro-algale caractérisé en ce qu'il comprend les étapes suivantes : - disposer d'une biomasse micro-algale comprenant au moins 15 %, en poids de lipides par rapport à la masse totale de ladite biomasse et présentant une concentration en matière sèche comprise entre 1 g/l et 200 g/l, - broyer ladite biomasse au moyen d'un broyeur à billes mis en oeuvre dans les conditions suivantes : - le diamètre moyen des billes (d GM ) varie de 0,2 à 2,5.10 -3 m, de préférence de 0,4 à 1,0 10 -3 m et de manière préférée est d'environ 0,6 10 -3 m, - la vitesse d'agitation en bout de pale (u) varie de 4 à 50 m.s -1 , de préférence de 5 à 20 m.s -1 et de manière préférée est d'environ 8 m.sec -1 ; - le taux de remplissage en billes du broyeur varie de 50 % à 80 % volume/volume, - récupérer la composition obtenue.The present invention provides a method for treating a microalgal biomass characterized in that it comprises the following steps: - Have a micro-algal biomass comprising at least 15%, by weight of lipids relative to the total mass of said biomass and having a dry matter concentration of between 1 g / l and 200 g / l, - Grinding said biomass by means of a ball mill implemented under the following conditions: the mean diameter of the beads (d GM) varies from 0.2 to 2.5 × 10 -3 m, preferably from 0.4 to 1.0 × 10 -3 m, and is preferably about 0.6 × 10 -3 m, 3 m, the stirring speed at the end of the blade (u) varies from 4 to 50 m.s -1, preferably from 5 to 20 m.s.sup.-1, and is preferably about 8 m.sec -1; - The bead filling rate of the mill varies from 50% to 80% volume / volume, - recover the composition obtained.
Description
La présente invention se rapporte au domaine de la valorisation de la biomasse algale, plus précisément la présente invention concerne un procédé d'extraction de lipides issus de micro-algues.The present invention relates to the field of valorization of algal biomass, more precisely the present invention relates to a process for extracting lipids from microalgae.
Les micro-algues sont des organismes eucaryotes, la plupart du temps unicellulaires, délimitées par une membrane plasmique et une paroi. La composition et la structure de cette paroi peuvent être variables selon la microalgue considérée.Microalgae are eukaryotic organisms, mostly unicellular, delimited by a plasma membrane and a wall. The composition and structure of this wall may be variable depending on the microalga considered.
Ainsi, chez certaines microalgues vertes telles que Chlorella, elle est constituée de cellulose et possède une forte rigidité entraînant une résistance élevée de l'algue vis-à-vis des contraintes mécaniques.Thus, in some green microalgae such as Chlorella, it is made of cellulose and has a high rigidity resulting in a high resistance of the alga vis-à-vis mechanical stresses.
Pour les micro-algues appartenant à la classe des diatomées, la paroi, aussi appelée frustule, est constituée de silice cristallisée. Cette dernière est plus cassante que celle de Chlorella. For micro-algae belonging to the diatom class, the wall, also called frustule, is made of crystallized silica. The latter is more brittle than that of Chlorella.
Enfin, d'autres espèces mettent en place autour de leur cellule, une gangue polysaccharidique pour se protéger des agressions environnementales. L'épaisseur de cette gangue varie au cours du temps, elle est assez fine lors de la croissance exponentielle de la micro-algue puis plus épaisse en phase stationnaire.Finally, other species put up around their cell, a gangue polysaccharide to protect themselves from environmental aggressions. The thickness of this gangue varies over time, it is quite fine during the exponential growth of microalgae and then thicker in stationary phase.
L'intérêt pour la valorisation des microalgues est croissant, ainsi les microalgues trouvent de nombreuses applications en particulier dans les aliments, les produits cosmétiques, les produits pharmaceutiques... en outre de nombreuses recherches sont menées sur la biomasse algale dans la perspective de l'utiliser comme biocarburant.The interest in the development of microalgae is growing, and microalgae find many applications in particular in food, cosmetics, pharmaceuticals ... In addition, many research is conducted on algal biomass from the perspective of use as biofuel.
Dans le but de valoriser la totalité de la biomasse micro-algale, dans un objectif de bioraffinage, il est nécessaire de fractionner, d'isoler les différents métabolites de ladite micro-algue.In order to valorize the totality of the micro-algal biomass, with a view to biorefining, it is necessary to fractionate and isolate the different metabolites of said micro-algae.
Les principaux métabolites des microalgues, à savoir les polysaccharides, les protéines et les pigments, sont généralement solubles dans le milieu de culture. De plus les microalgues peuvent, dans certaines conditions, accumuler d'importantes quantités de lipides sous la forme de globules de triglycérides dits « TAG » (pour triglycérides d'acides gras). En outre elles produisent également des acides gras polyinsaturés dites « AGPI », sous la forme de phospholipides et de glycolipides possédant une forte valeur ajoutée.The main metabolites of microalgae, namely polysaccharides, proteins and pigments, are generally soluble in the culture medium. In addition, microalgae can, under certain conditions, accumulate large amounts of lipids in the form of triglyceride globules known as "TAG" (for triglycerides of fatty acids). In addition, they also produce polyunsaturated fatty acids called "PUFAs", in the form of phospholipids and glycolipids having a high added value.
Le but de la présente invention est précisément la récupération des lipides de la biomasse algale et plus précisément des triglycérides d'acides gras et des acides gras polyinsaturés.The object of the present invention is precisely the recovery of lipids from the algal biomass and more precisely triglycerides of fatty acids and polyunsaturated fatty acids.
La récupération de ces deux fractions se fait classiquement via une extraction par solvant organique sur une biomasse préalablement séchée, puis par un fractionnement des différentes classes de lipides via des opérations unitaires variées (extraction sélective, précipitation sélective, distillation...). Les lipides sont ainsi recueillis dans la phase organique et les protéines dans la fraction qui est insoluble dans ledit solvant organique. Cette technologie est notamment décrite dans : "
Cette méthode implique une forte consommation d'énergie liée au séchage de la biomasse qui entraine également une dégradation de certains composés thermosensibles comme les vitamines, les pigments ou certaines protéines. La série d'opérations ainsi que les importantes quantités de solvants mises en jeu complexifient le procédé et augmentent les coûts de production.This method involves a high energy consumption linked to the drying of the biomass, which also causes a degradation of certain thermosensitive compounds such as vitamins, pigments or certain proteins. The series of operations and the large quantities of solvents involved complicate the process and increase production costs.
Un des principaux avantages du procédé selon l'invention est qu'il peut être mis en oeuvre sur une biomasse sans que celle-ci soit préalablement séchée. Le procédé selon l'invention permet ainsi d'éviter la mise en oeuvre d'une étape de séchage, longue et coûteuse, tant en énergie que financièrement.One of the main advantages of the process according to the invention is that it can be used on a biomass without it being dried beforehand. The method according to the invention thus makes it possible to avoid the implementation of a drying step, which is long and expensive, both in energy and in financial terms.
Des méthodes de désintégration de cellules de Chlorella vulgaris en vue de récupérer les lipides aptes à la production de biodiesel sont également décrites notamment dans la publication
Cette publication ne décrit pas les conditions du procédé selon l'invention qui met en oeuvre un broyeur à billes et qui permet l'obtention d'une composition qui peut être ensuite facilement valorisée par simple centrifugation.This publication does not describe the conditions of the process according to the invention which uses a ball mill and which makes it possible to obtain a composition which can then be easily recovered by simple centrifugation.
Le problème technique posé à l'origine de la présente demande était de disposer d'un procédé de fractionnement des lipides contenus dans une biomasse micro-algale qui ne nécessite pas de sécher ladite biomasse, qui permet de s'affranchir de l'utilisation de solvants et qui conduit à l'obtention d'une composition dont les différents constituants peuvent être ensuite facilement séparés.The technical problem at the origin of the present application was to have a lipid fractionation process contained in a micro-algal biomass that does not require drying said biomass, which makes it possible to overcome the use of solvents and which leads to the production of a composition whose different constituents can then be easily separated.
En effet dans l'optique de bioraffinage de la biomasse, une extraction sélective de chacun des constituants est recherchée.Indeed in the biomass biorefining optics, a selective extraction of each of the constituents is sought.
Le procédé selon l'invention répond à ces exigences.The process according to the invention meets these requirements.
Un premier objet de la présente invention vise un procédé de traitement d'une biomasse micro-algale comprenant les étapes suivantes :
- disposer d'une biomasse micro-algale comprenant au moins 15 % en poids de lipides par rapport à la masse totale de ladite biomasse et présentant une concentration en matière sèche comprise entre 1g/l et 200 g/l,
- broyer ladite biomasse au moyen d'un broyeur à billes mis en oeuvre dans les conditions suivantes :
- le diamètre moyen des billes (dGM) varie de 0,2 à 2,5.10-3m, de préférence de 0,4 à 1,0. 10-3m et de manière préférée est d'environ 0,6 10-3 m,
- la vitesse d'agitation en bout de pale(u) varie de 4 à 50 m.s-1, de préférence de 5 à 20 m.s-1 et de manière préférée est d'environ 8 m.sec-1 ;
- récupérer la composition obtenue.
- having a micro-algal biomass comprising at least 15% by weight of lipids with respect to the total mass of said biomass and having a dry matter concentration of between 1 g / l and 200 g / l,
- grinding said biomass by means of a ball mill operated under the following conditions:
- the mean diameter of the beads (d GM ) varies from 0.2 to 2.5 × 10 -3 m, preferably from 0.4 to 1.0. 10 -3 m and preferably is about 0.6 10 -3 m,
- the end-of-blade stirring speed (u) varies from 4 to 50 ms -1 , preferably from 5 to 20 ms -1 and preferably is about 8 m.sec -1 ;
- recover the composition obtained.
Les conditions de mise en oeuvre du broyage selon l'invention permettent d'assurer le relargage de la quasi totalité des gouttelettes de triglycérides, tout en assurant une déconstruction partielle des structures cellulaires entrainant la libération de certains voire de tous les phospholipides et glycolipides.The conditions for carrying out grinding according to the invention make it possible to ensure the release of almost all the droplets of triglycerides, while ensuring a partial deconstruction of the cellular structures causing the release of some or all of the phospholipids and glycolipids.
En outre les conditions de mise en oeuvre du broyage selon l'invention permettent d'éviter une homogénéisation trop poussée du milieu, et par conséquent d'éviter la formation d'émulsion.In addition, the conditions for carrying out the grinding according to the invention make it possible to avoid excessive homogenization of the medium, and consequently to avoid emulsion formation.
La composition obtenue à l'issue du broyage présente l'avantage d'être ensuite facilement valorisable.The composition obtained after grinding has the advantage of being then easily recoverable.
Un deuxième objet de l'invention vise la composition susceptible d'être par le procédé selon l'invention.A second object of the invention is the composition that may be by the method according to the invention.
L'étape mettant en oeuvre un broyeur à billes selon l'invention est avantageusement suivie des étapes suivantes, dans cet ordre :
- une étape de centrifugation à une accélération centrifuge comprise entre 3500g et 20 000g, pendant une durée comprise entre 2 et 40 minutes, à une température comprise entre 5 et 40 °C de la composition obtenue, ladite étape de centrifugation conduisant à l'obtention d'au moins 3 phases ;
- une étape de récupération des phases permettant d'isoler une première phase dite « superculot », une deuxième phase dite « surnageant » plus dense que la première phase et d'une troisième phase dite « culot » plus dense que la deuxième phase.
- a centrifugation step at a centrifugal acceleration of between 3500 g and 20 000 g, for a duration of between 2 and 40 minutes, at a temperature of between 5 and 40 ° C. of the composition obtained, said centrifugation step leading to the obtaining of at least 3 phases;
- a phase recovery step to isolate a first phase called "superculot", a second phase called "supernatant" denser than the first phase and a third phase called "pellet" denser than the second phase.
Avantageusement, l'étape de centrifugation est effectuée directement sur la composition obtenue à l'issue de l'étape mettant en oeuvre un broyeur à billes, c'est-à-dire que l'étape de centrifugation est mise en oeuvre après l'étape mettant en oeuvre un broyeur à billes sans étape(s) intermédiaire(s) hormis l'étape visant à récupérer ladite composition obtenue.Advantageously, the centrifugation step is carried out directly on the composition obtained at the end of the step using a ball mill, that is to say that the centrifugation step is carried out after the step using a ball mill without intermediate step (s) except the step of recovering said composition obtained.
Le procédé selon l'invention permet donc de fractionner les lipides et les protéines contenus dans des microalgues sans sécher la biomasse (extraction en voie humide) ni utiliser de solvants, évitant ainsi la dénaturation des composés tout en limitant les volumes à traiter.The process according to the invention thus makes it possible to fractionate the lipids and the proteins contained in microalgae without drying the biomass (wet extraction) nor to use solvents, thus avoiding the denaturation of the compounds while limiting the volumes to be treated.
Un autre avantage du procédé selon l'invention est qu'il peut être mis en oeuvre directement sur le milieu de culture, en particulier sur une suspension de micro-algues en sortie de production, ce qui contribue à réduire les volumes d'eau utilisés pour mettre en oeuvre ledit procédé.Another advantage of the process according to the invention is that it can be used directly on the culture medium, in particular on a suspension of micro-algae at the output of production, which contributes to reducing the volumes of water used. to implement said method.
Ainsi le procédé selon l'invention permet de travailler sur une biomasse concentrée directement récoltée après culture.Thus, the process according to the invention makes it possible to work on a concentrated biomass directly harvested after cultivation.
Avantageusement en mettant en oeuvre seulement deux étapes : une étape de broyage et une étape de séparation de phases, il est possible d'obtenir directement trois phases sélectivement enrichies en différents composés : une première phase dite « superculot » riche en lipides, une deuxième phase dite « surnageant » riche en protéines et une troisième phase dite « culot » riche en composés insolubles.Advantageously, by using only two steps: a grinding step and a phase separation step, it is possible to obtain directly three phases selectively enriched in different compounds: a first phase called "superculot" rich in lipids, a second phase called "supernatant" rich in proteins and a third phase called "pellet" rich in insoluble compounds.
Le superculot et le culot peuvent ainsi être directement valorisables, le surnageant peut être soumis à une opération de filtration membranaire permettant soit la séparation des protéines et des sucres solubilisés des TAG soit la concentration des protéines et des TAG pour arriver à deux fractions purifiées.The superculot and the pellet can thus be directly recoverable, the supernatant can be subjected to a membrane filtration operation allowing either the separation of proteins and solubilized sugars from TAGs, ie the concentration of proteins and TAGs to arrive at two purified fractions.
Aucune altération de molécules liée au séchage de la biomasse et à l'utilisation de solvant n'est dans ce cas là observée.No alteration of molecules related to the drying of the biomass and the use of solvent is in this case observed.
Le procédé selon la présente invention est mis en oeuvre à partir d'une biomasse micro-algale suffisamment riche en lipides et suffisamment concentrée, ainsi la biomasse micro-algale comprend au moins 15 %, de préférence environ 17,5 % en poids de lipides par rapport à la masse totale de la biomasse, en outre la biomasse micro-algale présente une concentration en matière sèche comprise entre 1g/l et 200 g/l, de préférence entre 5g/l et 150g/l et de façon encore préférée entre 35g/l et 100g/l, c'est-à-dire par rapport au volume de la biomasse micro-algale à traiter.The process according to the present invention is carried out using a micro-algal biomass sufficiently rich in lipids and sufficiently concentrated, so that the microalgal biomass comprises at least 15%, preferably approximately 17.5% by weight of lipids. relative to the total mass of the biomass, in addition the micro-algal biomass has a dry matter concentration of between 1 g / l and 200 g / l, preferably between 5 g / l and 150 g / l and even more preferably between 35 g / l and 100 g / l, that is to say with respect to the volume of microalgal biomass to be treated.
De préférence la biomasse microalgale comprend au moins une microalgue choisie parmi Nannochloropsis sp., Nannochloropsis oceanica, Nannochloropsis oculata, Tetraselmis suecica, Porphyridium cruentum, Parachlorella kessleri, Dunaliella salina, Chlorella vulgaris, Neochloris oleoabundans, Haematococcus pluvialis et de préférence parmi les souches suivantes Nannochloropis oceanica, Parachlorella kessleri, Tetraselmis suecica. Preferably, the microalgal biomass comprises at least one microalga chosen from Nannochloropsis sp., Nannochloropsis oceanica, Nannochloropsis oculata, Tetraselmis suecica , Porphyridium cruentum, Parachlorella kessleri, Dunaliella salina, Chlorella vulgaris, Neochloris oleoabundans and Haematococcus pluvialis and preferably from the following strains Nannochloropis oceanica, Parachlorella kessleri, Tetraselmis suecica.
Le procédé selon l'invention comprend une étape lors de laquelle est utilisé un broyeur à billes.The method according to the invention comprises a step during which a ball mill is used.
Les broyeurs à billes sont classiquement utilisés pour l'homogénisation des produits visqueux tels que les peintures et aussi pour broyer les minéraux. Les broyeurs à billes comprennent une enceinte, par exemple un bol fermé par un couvercle, destinée à recevoir la composition à traiter, ladite enceinte étant alimentée via une pompe en composition à traiter.Ball mills are typically used for the homogenization of viscous products such as paints and also for grinding minerals. Ball mills comprise an enclosure, for example a bowl closed by a cover, intended to receive the composition to be treated, said enclosure being fed via a pump in composition to be treated.
Classiquement le taux de remplissage en billes du broyeur, correspondant au pourcentage du volume du bol occupé par les billes, va de 50 % à 80 %, de préférence de 70 % à 80 % volume/volume et avantageusement d'environ 75 % volume/volume.Conventionally, the filling rate in balls of the mill, corresponding to the percentage of the volume of the bowl occupied by the beads, ranges from 50% to 80%, preferably from 70% to 80% volume / volume and preferably from about 75% volume / volume.
Le contenu de l'enceinte, hors billes, comprend essentiellement la biomasse micro algale.The content of the enclosure, excluding beads, essentially includes microalgal biomass.
Le taux de remplissage pourra être adapté notamment en fonction de la nature des billes utilisées. En effet dans certains cas, une agglomération des billes entre les pâles de l'agitateur a pu être observée.The filling rate may be adapted in particular according to the nature of the balls used. Indeed in some cases, an agglomeration of the balls between the blades of the agitator could be observed.
Il relève des compétences de l'homme du métier de sélectionner le taux de remplissage adapté au milieu à traiter.It is within the skills of a person skilled in the art to select the filling rate adapted to the medium to be treated.
Le débit d'alimentation de la composition dans le broyeur va généralement de 150 ml/min à 200 ml/min. Il relève également des compétences de l'homme du métier de sélectionner le débit d'alimentation adapté au milieu à traiter.The feed rate of the composition in the mill generally ranges from 150 ml / min to 200 ml / min. It is also within the skill of those skilled in the art to select the feed rate adapted to the medium to be treated.
De préférence, le traitement dans un broyeur à billes est réalisé pendant une durée (temps de séjour) variant de 1 à 30 minutes, de préférence de 2 à 20 minutes, de manière encore préférée de 4 à 10 minutes et avantageusement d'environ 6 minutes.Preferably, the treatment in a ball mill is carried out for a duration (residence time) ranging from 1 to 30 minutes, preferably from 2 to 20 minutes, more preferably from 4 to 10 minutes and advantageously from about 6 to 10 minutes. minutes.
Le traitement au broyeur à billes est généralement effectué à une température, généralement régulée, allant de 18 °C à 40 °C, de préférence allant de 18 à 25 °C.Ball mill treatment is generally carried out at a temperature, generally controlled, ranging from 18 ° C to 40 ° C, preferably from 18 to 25 ° C.
Comme déjà mentionné, le procédé de traitement mécanique selon l'invention met en oeuvre un broyeur à billes, de préférence en verre, dans les conditions suivantes :
- le diamètre moyen des billes (dGM) varie de 0,2 à 2,5.10-3m, de préférence de 0,4 à 1,0. 10-3m et de manière préférée est d'environ 0,6 10-3 m,
- la vitesse d'agitation en bout de pale(u) varie de 4 à 50 m.s-1, de préférence de 5 à 20 m.s-1 et de manière préférée est d'environ 8 m.sec-1 ;
- the mean diameter of the beads (d GM ) varies from 0.2 to 2.5 × 10 -3 m, preferably from 0.4 to 1.0. 10 -3 m and preferably is about 0.6 10 -3 m,
- the end-of-blade stirring speed (u) varies from 4 to 50 ms -1 , preferably from 5 to 20 ms -1 and preferably is about 8 m.sec -1 ;
A l'issue de l'étape de broyage à billes, la composition obtenue est avantageusement récupérée.At the end of the ball milling step, the composition obtained is advantageously recovered.
Selon une mise en oeuvre du procédé, une seule étape de broyage à billes est effectuée.According to one implementation of the method, a single ball milling step is performed.
Selon une mise en oeuvre préférée du procédé, le traitement dans un broyeur à billes est répété au moins deux fois, de préférence entre deux et dix fois et avantageusement entre trois et quatre fois.According to a preferred implementation of the process, the treatment in a ball mill is repeated at least twice, preferably between two and ten times and advantageously between three and four times.
De préférence, ce procédé est mis en oeuvre en « batch » afin de pouvoir traiter un volume de biomasse de manière simple.Preferably, this method is implemented in " batch " in order to be able to treat a biomass volume in a simple manner.
Comme déjà mentionné, les conditions opératoires permettant une centrifugation conduisant aux 3 phases annoncée sont
- une accélération centrifuge comprise entre 3500g et 20 000g, de préférence entre 6000g et 15 000g et de façon encore préférée environ de 12 000g,
- pendant une durée comprise entre 2 et 40 minutes, de préférence entre 5 et 30 minutes et de façon encore préférée entre 10 et 20 minutes,
- à une température comprise entre 5 et 40°C, de préférence entre 10 et 30°C et de façon encore préférée entre 20 et 25°C de la composition obtenue;
- a centrifugal acceleration of between 3500 g and 20 000 g, preferably between 6000 g and 15 000 g and more preferably approximately 12 000 g,
- for a period of between 2 and 40 minutes, preferably between 5 and 30 minutes and even more preferably between 10 and 20 minutes,
- at a temperature between 5 and 40 ° C, preferably between 10 and 30 ° C and more preferably between 20 and 25 ° C of the composition obtained;
Comme déjà mentionné, à l'issue de l'étape de centrifugation trois phases sont essentiellement obtenues, ces trois phases étant sélectivement enrichies en différents composés.As already mentioned, at the end of the centrifugation step, three phases are essentially obtained, these three phases being selectively enriched with different compounds.
La première phase, le superculot, comprend généralement plus de 30 %, de préférence plus de 60 % de lipides, elle comprend également des protéines en une quantité limitée comprise entre 10 et 30 % permettant une valorisation directe du superculot.The first phase, the superculot, generally comprises more than 30%, preferably more than 60% of lipids, it also comprises proteins in a limited amount of between 10 and 30% allowing a direct valuation of the superculot.
Néanmoins, en fonction des utilisations visées, une opération de séparation des protéines présentes dans le superculot peut être effectuée.Nevertheless, depending on the intended uses, a separation operation of the proteins present in the superculot can be performed.
Il relève des compétences de l'homme du métier de choisir la méthode de séparation à mettre en oeuvre.It is within the skills of a person skilled in the art to choose the separation method to be used.
En outre, les opérations de purification du superculot sont facilitées à cause de la proportion réduite des protéines.In addition, the purification operations of the superculot are facilitated because of the reduced proportion of proteins.
La première phase comprend essentiellement un mélange de triglycérides (TAG) et d'acides gras polyinsaturés dites « AGPI », sous la forme de phospholipides et de glyco lipides.The first phase essentially comprises a mixture of triglycerides (TAG) and polyunsaturated fatty acids called "PUFA", in the form of phospholipids and glyco lipids.
La deuxième phase, le surnageant, comprend généralement plus de 20 %, de préférence plus de 40 % de protéines et également une quantité importante de lipides.The second phase, the supernatant, generally comprises more than 20%, preferably more than 40% of proteins and also a large amount of lipids.
Par conséquent le surnageant peut être soumis à une ou plusieurs opération(s) de séparation des protéines et des lipides notamment des TAG pour obtenir deux fractions purifiées, avantageusement cette /ces opération(s) de séparation peuvent être effectuée(s) au moyen d'une membrane.Therefore the supernatant can be subjected to one or more operation (s) of separation of proteins and lipids including TAG to obtain two purified fractions, advantageously this / these operation (s) separation can be performed (s) by means of a membrane.
Avantageusement au moins une étape de séparation des lipides est effectuée sur la deuxième phase.Advantageously, at least one lipid separation step is performed on the second phase.
Les lipides notamment des TAG isolés à l'issue de la ou des opération(s) de séparation et le superculot voire les lipides isolés du superculot sont avantageusement rassemblés.The lipids in particular TAGs isolated at the end of the separation operation (s) and the superculot or even the lipids isolated from the superculot are advantageously gathered.
La troisième phase, le culot, est riche en composés insolubles. Le culot peut être directement valorisable.The third phase, the pellet, is rich in insoluble compounds. The base can be directly valorizable.
Les opérations de purification des composants sont facilitées notamment dû au fait que les trois phases sont sélectivement enrichies en différents composés.The purification operations of the components are facilitated in particular due to the fact that the three phases are selectively enriched in different compounds.
Le procédé selon l'invention doit être considéré comme permettant une récupération ciblée et quasi-totale des lipides.The method according to the invention should be considered as allowing a targeted and almost total recovery of lipids.
Les lipides sont utilisés dans des compositions chimiques, cosmétiques ou pharmaceutiques, en nutraceutique, en alimentation notamment animale.Lipids are used in chemical, cosmetic or pharmaceutical compositions, in nutraceuticals, especially in animal feed.
Les exemples qui suivent illustrent l'invention sans en limiter la portée.The examples which follow illustrate the invention without limiting its scope.
Pour tous ces exemples, on utilise une biomasse de Nannochloropis oceanica. Cette biomasse a été cultivée en photobioréacteur tubulaire de 10 L.For all these examples, a biomass of Nannochloropis oceanica is used. This biomass was grown in tubular photobioreactor of 10 L.
La biomasse a été traitée au moyen d'un broyeur à billes (DynoMill Mutlilab, WAB, Suisse) en verre dans les conditions précisée dans chaque exemple.The biomass was treated using a glass ball mill (DynoMill Mutlilab, WAB, Switzerland) under the conditions specified in each example.
Le dosage des lipides est réalisé par la méthode de Folch.The lipid assay is performed by Folch's method.
Les protéines sont mesurées par absorbance à 280 nm, mesure éventuellement complétée d'un dosage des protéines réalisé selon le protocole BCA afin de vérifier la justesse des mesures spectro-photométriques.Proteins are measured by absorbance at 280 nm, possibly supplemented by a BCA protein assay to verify the accuracy of spectrophotometric measurements.
- Biomasse de Nannochloropis oceanica contenant 17,5 % de lipides,Biomass of Nannochloropis oceanica containing 17.5% lipids,
- Concentration en matière sèche de l'alimentation 75g/L,Dry matter concentration of the feed 75g / L,
- Billes en verre de 0,6 mm de diamètre,Glass balls 0.6 mm in diameter,
- Vitesse d'agitation de 8m.s-1,Stirring speed of 8m.s -1 ,
- cp : Taux de remplissage du broyeur : 75 %,cp: Crusher filling rate: 75%,
- Q : débit d'alimentation en ml/min : 200,Q: feed rate in ml / min: 200,
- Température régulée à 20 °C,Temperature regulated at 20 ° C,
- Temps de séjour moyen de 6 minutes.Average residence time of 6 minutes.
Dans cet exemple on récupère bien les trois fractions précédemment citées.In this example, the three fractions mentioned above are well recovered.
Biomasse de Nannochloropis oceanica contenant 12,5 % de lipides,
- Concentration en matière sèche de l'alimentation 75g/L,
- Billes en verre de 0,6 mm de diamètre,
- Vitesse d'agitation de 8m.s-1,
- ϕ : Taux de remplissage du broyeur : 75 %,
- Q : débit d'alimentation en ml/min 200,
- Température régulée à 20 °C,
- Temps de séjour moyen de 6 minutes.
- Dry matter concentration of the feed 75g / L,
- Glass balls 0.6 mm in diameter,
- Stirring speed of 8m.s -1 ,
- φ: Mill filling rate: 75%,
- Q: feed rate in ml / min 200,
- Temperature regulated at 20 ° C,
- Average residence time of 6 minutes.
Dans cet exemple, avec une biomasse moins riche en lipides, seulement deux phases sont obtenues après la centrifugation.In this example, with a biomass less rich in lipids, only two phases are obtained after centrifugation.
Il est donc possible, via l'invention décrite et en seulement deux opérations, d'aboutir à une extraction de près de 70 % des lipides totaux sans solvant sur une biomasse humide ainsi qu'à un fractionnement des TAG et des lipides polaires riches en AGPI.It is therefore possible, via the described invention and in only two operations, to result in an extraction of nearly 70% of the total lipids without solvent on a wet biomass as well as a fractionation of TAGs and polar lipids rich in PUFA.
Le superculot et le culot peuvent ainsi être directement valorisables, le surnageant peut être soumis à une opération de séparation des protéines et des TAG (membranes) conduisant à deux fractions purifiées.The superculot and the pellet can thus be directly recoverable, the supernatant can be subjected to an operation of separation of proteins and TAG (membranes) leading to two purified fractions.
Claims (7)
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| FR1559840A FR3042505B1 (en) | 2015-10-16 | 2015-10-16 | METHOD FOR RECOVERING LIPIDS BY MEANS OF A BALL GRINDER |
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| US (1) | US20170107445A1 (en) |
| EP (1) | EP3156474A1 (en) |
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| US5330913A (en) * | 1991-09-11 | 1994-07-19 | Hideo Nakayama | Method of disrupting the chlorella cell wall by cell rupture |
| WO2012109642A1 (en) * | 2011-02-12 | 2012-08-16 | Phycal, Inc. | Aqueous extraction methods for high lipid microorganisms |
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| WO2015001261A1 (en) * | 2013-07-04 | 2015-01-08 | Roquette Freres | Optimised method for breaking chlorella walls by mechanical crushing |
| WO2015007997A1 (en) * | 2013-07-19 | 2015-01-22 | Roquette Freres | Optimised method for breaking chlorella cell walls by means of very high pressure homogenisation |
-
2015
- 2015-10-16 FR FR1559840A patent/FR3042505B1/en active Active
-
2016
- 2016-10-14 JP JP2016202343A patent/JP2017074039A/en active Pending
- 2016-10-14 EP EP16193842.8A patent/EP3156474A1/en not_active Withdrawn
- 2016-10-17 US US15/295,651 patent/US20170107445A1/en not_active Abandoned
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| US5330913A (en) * | 1991-09-11 | 1994-07-19 | Hideo Nakayama | Method of disrupting the chlorella cell wall by cell rupture |
| US20130338384A1 (en) | 2010-12-20 | 2013-12-19 | Karin BUS | Process for the release of lipids from microalgae |
| WO2012109642A1 (en) * | 2011-02-12 | 2012-08-16 | Phycal, Inc. | Aqueous extraction methods for high lipid microorganisms |
| WO2015001261A1 (en) * | 2013-07-04 | 2015-01-08 | Roquette Freres | Optimised method for breaking chlorella walls by mechanical crushing |
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| FR3042505B1 (en) | 2019-12-13 |
| FR3042505A1 (en) | 2017-04-21 |
| US20170107445A1 (en) | 2017-04-20 |
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