EP3156474A1 - Verfahren zur aufbereitung von lipiden mittels einer kugelmühle - Google Patents

Verfahren zur aufbereitung von lipiden mittels einer kugelmühle Download PDF

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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
Authority
EP
European Patent Office
Prior art keywords
biomass
volume
minutes
phase
ball mill
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP16193842.8A
Other languages
English (en)
French (fr)
Inventor
Sébastien JUBEAU
Valéria Montalescot
Thomas Rinaldi
Sergio Rios
Luc Marechal
Jérémy PRUVOST
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Universite de Nantes
Algosource SAS
Original Assignee
Universite de Nantes
Algosource SAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Universite de Nantes, Algosource SAS filed Critical Universite de Nantes
Publication of EP3156474A1 publication Critical patent/EP3156474A1/de
Withdrawn legal-status Critical Current

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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.
EP16193842.8A 2015-10-16 2016-10-14 Verfahren zur aufbereitung von lipiden mittels einer kugelmühle Withdrawn EP3156474A1 (de)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR1559840A FR3042505B1 (fr) 2015-10-16 2015-10-16 Procede de recuperation des lipides au moyen d'un broyeur a billes

Publications (1)

Publication Number Publication Date
EP3156474A1 true EP3156474A1 (de) 2017-04-19

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EP16193842.8A Withdrawn EP3156474A1 (de) 2015-10-16 2016-10-14 Verfahren zur aufbereitung von lipiden mittels einer kugelmühle

Country Status (4)

Country Link
US (1) US20170107445A1 (de)
EP (1) EP3156474A1 (de)
JP (1) JP2017074039A (de)
FR (1) FR3042505B1 (de)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
US20130338384A1 (en) 2010-12-20 2013-12-19 Karin BUS Process for the release of lipids from microalgae
WO2015001261A1 (fr) * 2013-07-04 2015-01-08 Roquette Freres Procede optimise de rupture des parois de chlorelles par broyage mecanique
WO2015007997A1 (fr) * 2013-07-19 2015-01-22 Roquette Freres Procédé optimise de rupture des parois de chlorelles par homogénéisation a très haute pression

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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 (fr) * 2013-07-04 2015-01-08 Roquette Freres Procede optimise de rupture des parois de chlorelles par broyage mecanique
WO2015007997A1 (fr) * 2013-07-19 2015-01-22 Roquette Freres Procédé optimise de rupture des parois de chlorelles par homogénéisation a très haute pression

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
ANSARI, F. A.; A. SHRIWASTAV; S. K. GUPTA; I. RAWAT; A. GULDHE; F. BUX: "Lipid extracted algae as a source for protein and reduced sugar: a step closer to the biorefinery", BIORESOUR TECHNOL, vol. 179, 2015, pages 559 - 564, XP029190416, DOI: doi:10.1016/j.biortech.2014.12.047
HONGLI ZHENG ET AL.: "Disruption of Chlorella vulgaris Cells for the Release of Biodiesel-Producing Lipids : A Comparison of Grinding, Ultrasonication, Bead Milling, Enzymatic Lysis, and Microwaves", APPL. BIOCHEM BIOTECHNOL, vol. 164, 2011, pages 1215 - 1224
HONGLI ZHENG ET AL: "Disruption ofCells for the Release of Biodiesel-Producing Lipids: A Comparison of Grinding, Ultrasonication, Bead Milling, Enzymatic Lysis, and Microwaves", APPLIED BIOCHEMISTRY AND BIOTECHNOLOGY ; PART A: ENZYME ENGINEERING AND BIOTECHNOLOGY, HUMANA PRESS INC, NEW YORK, vol. 164, no. 7, 24 February 2011 (2011-02-24), pages 1215 - 1224, XP019918055, ISSN: 1559-0291, DOI: 10.1007/S12010-011-9207-1 *

Also Published As

Publication number Publication date
FR3042505A1 (fr) 2017-04-21
JP2017074039A (ja) 2017-04-20
US20170107445A1 (en) 2017-04-20
FR3042505B1 (fr) 2019-12-13

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