EP4056670A1 - Method for fractionating a shea extract - Google Patents

Method for fractionating a shea extract Download PDF

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Publication number
EP4056670A1
EP4056670A1 EP21162465.5A EP21162465A EP4056670A1 EP 4056670 A1 EP4056670 A1 EP 4056670A1 EP 21162465 A EP21162465 A EP 21162465A EP 4056670 A1 EP4056670 A1 EP 4056670A1
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EP
European Patent Office
Prior art keywords
solvent system
shea
cas
acid
process according
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.)
Pending
Application number
EP21162465.5A
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German (de)
French (fr)
Inventor
Thierry Bernoud
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Biosynthis SARL
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Biosynthis SARL
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 Biosynthis SARL filed Critical Biosynthis SARL
Priority to EP21162465.5A priority Critical patent/EP4056670A1/en
Priority to PCT/EP2022/056583 priority patent/WO2022189678A1/en
Priority to EP22710126.8A priority patent/EP4305134A1/en
Priority to US18/280,705 priority patent/US20240158719A1/en
Publication of EP4056670A1 publication Critical patent/EP4056670A1/en
Pending legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B7/00Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils
    • C11B7/0008Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils by differences of solubilities, e.g. by extraction, by separation from a solution by means of anti-solvents
    • C11B7/0025Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils by differences of solubilities, e.g. by extraction, by separation from a solution by means of anti-solvents in solvents containing oxygen in their molecule

Definitions

  • the invention relates to a process for fractionating a shea extract allowing the fractionation, separation and recovery of the two constituent factions of shea, namely olein and shea stearin.
  • shea extract a material derived from the fruit or seeds of shea.
  • the shea extract can be obtained by traditional method, mechanical pressure, cold extraction and/or solvent extraction. These techniques are detailed in the body fat manual of Alain KARLESKIND (TEC & DOCS, 1993 ).
  • the shea extract is a shea butter.
  • a shea butter is a vegetable fatty substance which is solid at room temperature, extracted from the fruit or the seeds of the shea tree, and which melts at temperatures close to those of the skin.
  • the shea butter used in the present invention can be obtained by traditional method, solvent extraction and/or cold extraction.
  • the shea butter used in the present invention is preferentially refined and comes from organic farming certified CEE/NOP organic by FR-BIO-01 and ECOCERT SA.
  • the shea butter can undergo a degumming step, a bleaching step, a deodorization step and/or a neutralization step.
  • the degumming step also called the degumming step, removes the latex from the vegetable butter.
  • latex is a liquid substance, with a more or less thick consistency, secreted by certain plants or by certain fungi and circulating in the laticiferous ducts.
  • raw vegetable butter is degummed by mixing the oil with water or steam and passing the mixture through centrifuges which separate the gummy residue from the oil.
  • the discoloration step eliminates colored pigments (chlorophylls and carotenoids), residual soaps, traces of mucilage, heavy metals, in particular through the use of activated earths.
  • Bleaching earths are generally plastic clays that are simply dried and finely ground to increase their contact surface. You can also use activated charcoal.
  • the deodorization step is intended to remove odorous substances (essentially sulfur compounds) from the decolorized oil. This operation is commonly carried out under vacuum at high temperature. This involves steam distillation under vacuum of these compounds which result from the degradation of the oil.
  • neutralization eliminates all phospholipids, traces of metals and products degraded by oxidation.
  • the shea butter used in the present invention can be raw shea butter.
  • Raw shea butter means shea butter that has not undergone any refining step.
  • fractionation process is meant a process for separating a mixture into several successive fractions whose physical properties are different.
  • the fractionation consists in separating the shea extract into fractions of different physical characteristics.
  • the shea extract can thus be separated into an oil commonly referred to as the shea olein fraction and a solid fraction, the shea stearin, whose melting point is higher than the starting shea extract.
  • the shea olein fraction is a fraction of fatty acids, liquid at ambient temperature and whose mass percentage of oleic acid is greater than the mass percentage of each fatty acid which composes it. More specifically, the mass percentage of oleic acid is at least 50% relative to the total mass of fatty acid of the shea olein fraction.
  • the shea stearin fraction is a fatty acid fraction, solid at room temperature and whose mass percentage of stearic acid is greater than the mass percentage of each fatty acid which composes it. More specifically, the mass percentage of stearic acid is at least 45% relative to the total mass of fatty acid of the shea stearin fraction
  • a “mass percentage” is the ratio of the mass of a first compound relative to the total mass of a mixture of compounds or composition, reduced to a percentage.
  • Such plant fractions can have various uses in the food and cosmetics industry.
  • JP2011132207A cosmetic compositions comprising a raw material derived from shea butter have been described.
  • compositions of edible creams comprising a raw material derived from shea butter have been described.
  • cocoa butter equivalents comprising shea stearin have been disclosed.
  • the nature or the quantity of the solvents used during the solvent fractionation processes may be unsuitable both from an economic point of view and from a toxicological and environmental point of view.
  • the solvents most commonly used to fractionate the shea extract are aliphatic solvents of the hexane type or preferably acetone.
  • Hexane is an organic solvent considered to be toxic and is classified as CMR category 2. In addition, given its physico-chemical properties, this solvent presents a danger in handling and even more so on an industrial scale (flash point-23, 3°C / auto-ignition temperature 233°C).
  • acetone is a volatile and flammable solvent (flash point at -18°C) widely used in the chemical industry.
  • flash point at -18°C flash point at -18°C
  • its high volatility requires in industrial processes a volume of solvent that may be unsuitable from an economic and environmental point of view.
  • the present invention makes it possible to fractionate directly without subsequent treatment, a shea extract using a solvent system and to simultaneously recover a fraction of shea olein and shea stearin, the two fractions being in accordance with the requirements of the cosmetic and food industry regulations.
  • the solvents in the solvent system are biobased.
  • a biobased compound or an organic composition in which the organic carbon present in the compound or composition is of plant origin is qualified by a radiocarbon analysis according to one of the following standards ASTM D6866, EN 16640 or EN 16785-1.
  • the method according to the invention is characterized in that the shea extract is derived from shea seeds.
  • the method according to the invention is characterized in that the shea extract is a shea butter.
  • the method according to the invention is characterized in that the shea extract is a so-called natural shea butter.
  • the process according to the invention is characterized in that the shea extract is a refined shea butter.
  • the method according to the invention is characterized in that the shea extract is a refined shea butter having undergone a refining comprising a degumming step.
  • the process according to the invention is characterized in that the shea extract is a refined shea butter having undergone a refining comprising a decolorization step.
  • the method according to the invention is characterized in that the shea extract is a refined shea butter having undergone a refining comprising a deodorization step.
  • the method according to the invention is characterized in that the shea extract is a refined shea butter having undergone a refining comprising a neutralization step.
  • the method according to the invention is characterized in that the shea extract is a refined shea butter having undergone the refining steps comprising a degumming step, a bleaching step, a deodorization step and a neutralization step.
  • the method according to the invention is characterized in that the ratio Y is at most 1/2.
  • the method according to the invention is characterized in that the ratio Y is at most 1/3.
  • the method according to the invention is characterized in that the ratio Y is at most 1/5.
  • the method according to the invention is characterized in that the ratio Y is between 1/5 and 1/1.
  • the method according to the invention is characterized in that the ratio Y is 1/1.
  • the method according to the invention is characterized in that the ratio Y is 1/2.
  • the method according to the invention is characterized in that the ratio Y is 1/3.
  • the method according to the invention is characterized in that the ratio Y is 1/4.
  • the method according to the invention is characterized in that the solvent system is free of solvent categorized as CMR.
  • the method according to the invention is characterized in that the solvent system has a flash point of less than or equal to 110° C. measured according to the ATSM D93 standard.
  • the process according to the invention is characterized in that the solvent system has a flash point of less than or equal to 100° C. measured according to the ATSM D93 standard.
  • the method according to the invention is characterized in that the solvent system has a flash point of less than or equal to 95° C. measured according to the ATSM D93 standard.
  • the process according to the invention is characterized in that the solvent system has a flash point of less than or equal to 90° C. measured according to the ATSM D93 standard.
  • the process according to the invention is characterized in that the solvent system has a boiling point of less than or equal to 250°C.
  • the method according to the invention is characterized in that the solvent system has a boiling point of less than or equal to 230°C.
  • the method according to the invention is characterized in that the solvent system has a boiling point of less than or equal to 210°C.
  • the process according to the invention is characterized in that the solvent system consists of an oxo-ester alone or as a mixture.
  • the process according to the invention is characterized in that the oxo-ester alone or as a mixture is chosen from the group comprising: methyl levulinate ( CAS 624-45-3 ), ethyl levulinate ( CAS 539-88-8 ), propyl levulinate (645-67-0), isopropyl levulinate ( CAS 21884-26-4 ), butyl levulinate ( CAS 2052-15-5 ), isobutyl levulinate ( CAS 3757-32-2 ), tert-butyl levulinate ( CAS 2854-10-6 ), s-butyl levulinate ( CAS 85734-01-6 ), penthyl levulinate ( CAS 20279-49-6 ) hexyl levulinate ( CAS 24431-34-3 ), octyl levulinate ( CAS 41780-57-8 ), 2-Methyl-4-oxovaleric acid ethyl ester ( CAS 4749-12-6 ), 2-Methy
  • the process according to the invention is characterized in that the oxo-ester alone or as a mixture is chosen from the group of levulinates comprising: methyl levulinate ( CAS 624-45-3 ), ethyl levulinate ( CAS 539-88-8 ), propyl levulinate (645-67-0), isopropyl levulinate ( CAS 21884-26-4 ), butyl levulinate ( CAS 2052-15-5 ), isobutyl levulinate ( CAS 3757-32-2 ), tert-butyl levulinate ( CAS 2854-10-6 ), s-butyl levulinate ( CAS 85734-01-6 ), penthyl levulinate ( CAS 20279-49-6 ) hexyl levulinate ( CAS 24431-34-3 ), octyl levulinate ( CAS 41780-57-8 ).
  • levulinates comprising: methyl levulinate ( CAS 624-45-3 ), ethy
  • the process according to the invention is characterized in that the oxo-ester alone or as a mixture is chosen from the group comprising: methyl 3-methyl-4-oxopentanoate ( CAS 25234-83-7 ), methyl 2-methyl-4 oxopentanoate ( CAS 32811-25-9 ), pentanoic acid 2,3 dimethyl-4-oxo, methyl ester ( CAS 35140-52-4 ), pentanoic acid 2-ethyl-4-oxo-methyl ester ( CAS 62359-06-2 ), pentanoic acid 3-methyl-4-oxo ethyl ester ( CAS 55424-74-3 ), pentanoic acid-4-oxo-2-propyl-methyl ester ( CAS 244196-06-3 ), methyl 2-(1methylethyl)-4-oxopentaoate ( CAS 99183-33-2 ), Ethyl 2 ethyl-4-oxopentanoate ( CAS 99183
  • the process according to the invention is characterized in that the oxo-ester alone or as a mixture is chosen from the group comprising: methyl 4-oxohexanoate ( CAS 2955-62-6 ), methyl 5-oxohexanoate ( CAS 13984-50-4 ), methyl 3-methyl -5-oxohexanoate ( CAS 14983-18-7 ), 4-Oxo-5-methylhexanoic acid methyl ester ( CAS 34553-37-2 ), hexanoic acid, 4-methyl-5-oxo, methyl ester ( CAS 36045-56-4 ), methyl 3-methyl-4-oxohexanoate ( CAS 69448-35-7 ), hexanoic acid 2-methyl-5-oxo methyl ester ( CAS 38872-30-9 ), hexanoic acid 2-ethyl-4-oxo methyl ester ( CAS 75436-59-8 ), hexanoic acid, 2, 4-oxo
  • the process according to the invention is characterized in that the oxo-ester alone or as a mixture is chosen from the group comprising: 2-Methyl-4-oxovaleric acid ethyl ester ( CAS 4749-12-6 ), methyl-6-oxoheptanoate ( CAS 2046-21-1 ), 5-ketoenanthic acid methyl ester (17745-32-3), octanoic acid 4 oxo-methyl ester ( CAS: 4316-48-7 ), heptanoic acid 2-methyl-6-oxo-methyl ester ( CAS 2570-90-3 ), heptanoic acid 3-methyl 6-oxo methyl ester ( CAS 5128-55-2 ), heptanoic acid 6-methyl-5-oxo methyl ester ( CAS 23575-33-9 ), heptanoic acid 2-methyl-5-oxo methyl ester ( CAS 25912-38-3 ), heptanoic acid 4-methyl-6
  • the process according to the invention is characterized in that the oxo-ester has a molecular mass less than or equal to 200 g/mol.
  • the process according to the invention is characterized in that the oxo-ester has a molecular mass less than or equal to 180 g/mol.
  • the process according to the invention is characterized in that the oxo-ester has a molecular mass less than or equal to 160 g/mol.
  • the process according to the invention is characterized in that the oxo-ester has a molecular mass less than or equal to 150 g/mol.
  • the method according to the invention is characterized in that the oxo-ester is methyl levulinate.
  • the method according to the invention is characterized in that the oxo-ester is butyl levulinate.
  • the method according to the invention is characterized in that the oxo-ester is ethyl levulinate.
  • an “alkane” is a saturated hydrocarbon consisting solely of carbon and hydrogen atoms linked together by single covalent bonds, the general formula of which is C n H 2n+2 , it is called “linear alkane when each carbon atom is bonded to a maximum of two carbon atoms and “branched alkane” when certain carbon atoms are bonded to three or even four carbon atoms.
  • a “bioalkane” is a biobased alkane.
  • biobased compound or an organic composition in which the organic carbon present in the compound or composition is of plant origin is described as biobased by radiocarbon analysis according to one of the following standards ASTM D6866, EN 16640 or EN 16785-1.
  • the method according to the invention is characterized in that the solvent system further comprises at least one alkane
  • the method according to the invention is characterized in that the solvent system further comprises at least one volatile alkane
  • the process according to the invention is characterized in that the volatile alkane is chosen from the group comprising linear and/or branched alkanes comprising from 10 to 12 carbon atoms, alone or in mixtures.
  • the process according to the invention is characterized in that the volatile alkane is chosen from the group comprising linear and/or branched bioalkanes comprising from 10 to 12 carbon atoms, alone or in mixtures.
  • the method according to the invention is characterized in that the solvent system further comprises a decane.
  • the method according to the invention is characterized in that the solvent system further comprises a dodecane.
  • the method according to the invention is characterized in that the solvent system further comprises a decane, a dodecane
  • the process according to the invention is characterized in that the solvent system further comprises a branched alkane of 10 carbon atoms.
  • the process according to the invention is characterized in that the branched alkane of 10 carbon atoms is chosen from the group comprising: 2-methylnonane ( CAS 871-83-0 ), 4-methylnonane ( CAS 17301-94-9 ), 3-methyl nonane ( CAS 5911-04-6 ), 3-ethyl octane ( CAS 5881-17-4 ), 2,2-dimethyloctane ( CAS 15869-87-1 ), 2,3 dimethyl octane ( CAS 7146-60-3 ), 2,5-dimethyl octane ( CAS 15869-89-3 ), 3,5 dimethyl octane ( CAS 15869-93-9 ), 4-propylheptane ( CAS 3178-29-8 ), 3-ethyl-2-methylheptane ( CAS 14676-29-0 ), 2,2,3-trimethylheptane ( CAS 52896-92-1 ), 2,3,5 trimethylheptan
  • the process according to the invention is characterized in that the solvent system further comprises a branched alkane of 12 carbon atoms.
  • the process according to the invention is characterized in that the branched alkane with 12 carbon atoms is chosen from the group comprising: 2-methylundecane ( CAS 7045-71-8 ), 3-methylundecane ( CAS 1002-43-3 ), 4-methylundecane ( CAS 2980-69-0 ), 5-methylundecane ( CAS 1632-70-8 ), 6-methylundecane ( CAS 17302-33-9 ), 2,4-dimethyldecane ( CAS 2801-84-5 ) 4,4-dimethyldecane ( CAS 17312-39-9 ), 3,5-dimethyldecane ( CAS 17312-48-0 ), 2,5-dimethyldecane ( CAS 17312-50-4 ), 2,3-dimethyldecane ( CAS 17312-44-6 ), 3,3-dimethyldecane ( CAS 17302-38-4 ), 3,7-dimethyldecane ( CAS 17312-54-8 ), 3,4,6-trimethylnon
  • the method according to the invention is characterized in that the solvent system comprises at least one volatile alkane and one ethyl levulinate.
  • the process according to the invention is characterized in that the solvent system comprises a decane and an ethyl levulinate.
  • the method according to the invention is characterized in that the solvent system comprises a dodecane and an ethyl levulinate.
  • the process according to the invention is characterized in that the solvent system comprises a decane, a dodecane and an ethyl levulinate.
  • the method according to the invention is characterized in that the solvent system comprises a branched alkane of 10 carbon atoms and an ethyl levulinate.
  • the method according to the invention is characterized in that the solvent system comprises a branched alkane of 12 carbon atoms and an ethyl levulinate.
  • the method according to the invention is characterized in that the solvent system comprises at least one volatile alkane and one butyl levulinate.
  • the method according to the invention is characterized in that the solvent system comprises a decane and a butyl levulinate.
  • the process according to the invention is characterized in that the solvent system comprises a dodecane and a butyl levulinate.
  • the process according to the invention is characterized in that the solvent system comprises a decane, a dodecane and a butyl levulinate.
  • the process according to the invention is characterized in that the solvent system comprises a branched alkane of 10 carbon atoms and a butyl levulinate.
  • the process according to the invention is characterized in that the solvent system comprises a branched alkane of 12 carbon atoms and a butyl levulinate.
  • the method according to the invention is characterized in that the solvent system is a solvent mixture further comprising an ethyl lactate
  • the method according to the invention is characterized in that the solvent system comprises an ethyl lactate and a butyl levulinate.
  • the method according to the invention is characterized in that the solvent system comprises an ethyl lactate and an ethyl levulinate.
  • the method according to the invention is characterized in that the volume ratio X is at least 1/1.
  • the method according to the invention is characterized in that the volume ratio X is at least 2/1.
  • the method according to the invention is characterized in that the volume ratio X is between 2/1 and 100/1.
  • the method according to the invention is characterized in that the volume ratio X is between 2/1 and 50/1.
  • the method according to the invention is characterized in that the volume ratio X is between 2/1 and 20/1.
  • the method according to the invention is characterized in that the volume ratio X is between 2/1 and 10/1.
  • the process according to the invention is characterized in that the volume ratio X is 1/1.
  • the method according to the invention is characterized in that the volume ratio X is 2/1.
  • the method according to the invention is characterized in that the volume ratio X is 3/1.
  • the method according to the invention is characterized in that the volume ratio X is 5/1.
  • the method according to the invention is characterized in that the volume ratio X is 10/1.
  • the method according to the invention is characterized in that the volume ratio X is 25/1.
  • the process according to the invention is characterized in that the volume ratio X is 50/1.
  • solvent content is understood to mean the ratio of the volume of a solvent relative to the total volume of a solvent mixture, reduced to a percentage.
  • the method according to the invention is characterized in that the solvent system comprises an oxo-ester content of at least 25%, relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent system comprises an oxo-ester content of at least 50%, relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent system comprises an oxo-ester content of between 70 and 100% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent system comprises an oxo-ester content of between 80 and 100% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent system comprises a methyl levulinate content of at least 25% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent system comprises a methyl levulinate content of at least 50% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent system comprises a methyl levulinate content of between 70 and 100% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent system comprises a methyl levulinate content of between 80 and 100% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent system comprises an ethyl levulinate content of at least 25% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent system comprises an ethyl levulinate content of at least 50% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent system comprises an ethyl levulinate content of between 70 and 100% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent system comprises an ethyl levulinate content of between 80 and 100% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent system comprises a butyl levulinate content of at least 25% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent system comprises a butyl levulinate content of at least 50% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent system comprises a butyl levulinate content of between 70 and 100% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent system comprises a butyl levulinate content of between 80 and 100% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent mixture comprises a volatile alkane content of at least 1% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent mixture comprises a volatile alkane content of at least 5% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent mixture comprises a volatile alkane content of between 1 and 50% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent mixture comprises a volatile alkane content of between 5 and 30% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent mixture comprises a decane content of at least 1% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent mixture comprises a decane content of at least 5% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent mixture comprises a decane content of between 1 and 50% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent mixture comprises a decane content of between 5 and 30% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent mixture comprises a dodecane content of at least 1% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent mixture comprises a dodecane content of at least 5% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent mixture comprises a dodecane content of between 1 and 50% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent mixture comprises a dodecane content of between 5 and 30% relative to the total volume of the solvent system.
  • the process according to the invention is characterized in that the solvent mixture comprises a content of branched alkanes with 10 carbon atoms, of at least 1% relative to the total volume of the solvent system.
  • the process according to the invention is characterized in that the solvent mixture comprises a content of branched alkanes with 10 carbon atoms, of at least 5% relative to the total volume of the solvent system.
  • the process according to the invention is characterized in that the solvent mixture comprises a content of branched alkanes of 10 carbon atoms, comprised between 1 and 50% relative to the total volume of the solvent system.
  • the process according to the invention is characterized in that the solvent mixture comprises a content of branched alkanes with 10 carbon atoms, of between 5 and 30% relative to the total volume of the solvent system.
  • the process according to the invention is characterized in that the solvent mixture comprises a content of branched alkanes with 12 carbon atoms, of at least 1% relative to the total volume of the solvent system.
  • the process according to the invention is characterized in that the solvent mixture comprises a content of branched alkanes of 12 carbon atoms, of at least 5% relative to the total volume of the solvent system.
  • the process according to the invention is characterized in that the solvent mixture comprises a content of branched alkanes of 12 carbon atoms, comprised between 1 and 50% relative to the total volume of the solvent system.
  • the process according to the invention is characterized in that the solvent mixture comprises a content of branched alkanes with 12 carbon atoms, of between 5 and 30% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent mixture comprises an ethyl lactate content of at least 1% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent mixture comprises an ethyl lactate content of at least 5% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent mixture comprises an ethyl lactate content of between 1 and 50% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the solvent mixture comprises an ethyl lactate content of between 30 and 50% relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the mixing and the homogenization of the shea butter is carried out at a temperature of at least 20°C.
  • the method according to the invention is characterized in that the mixing and homogenization of the shea butter is carried out at a temperature of between 20 and 80°C.
  • the method according to the invention is characterized in that the mixing and homogenization of the shea butter is carried out at a temperature of between 35 and 55°C.
  • the method according to the invention is characterized in that the mixing and homogenization of the shea butter is carried out at a temperature of 40°C
  • the process according to the invention is characterized in that the cooling of the reaction mixture is carried out at a temperature below 20°C.
  • the process according to the invention is characterized in that the cooling of the reaction mixture is carried out at a temperature comprised between -10 and 20°C.
  • the process according to the invention is characterized in that the cooling of the reaction mixture is carried out at a temperature comprised between 5 and 10°C.
  • the process according to the invention is characterized in that the cooling of the reaction mixture is carried out at a temperature equal to 4°C.
  • the method according to the invention is characterized in that the cooling of the reaction mixture is carried out for a period of at least 12 hours.
  • the method according to the invention is characterized in that the cooling of the reaction mixture is carried out for a preferential duration of 24 hours.
  • the method according to the invention is characterized in that the filtration of the reaction mixture is carried out using a filter chosen from the group: a monoplate filter, a filter press, a rotary filter or a candle filter.
  • the method according to the invention is characterized in that the elimination of the solvent system comprises at least one step of concentration by evaporation of the reaction mixture.
  • the method according to the invention is characterized in that the removal of the solvent system further comprises at least one step of washing with water.
  • the process according to the invention is characterized in that the concentration by evaporation of the reaction mixture makes it possible to eliminate at least 98% of the solvent system relative to the total volume of the solvent system.
  • the process according to the invention is characterized in that the concentration by evaporation of the reaction mixture makes it possible to eliminate at least 99.5% of the solvent system relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the at least one step of washing with water is carried out at a temperature of at least 20°C.
  • the method according to the invention is characterized in that the at least one step of washing with water is carried out at a temperature of at least 40°C.
  • the method according to the invention is characterized in that the at least one step of washing with water is carried out at a temperature of between 40 and 80°C.
  • the method according to the invention is characterized in that the at least one step of washing with water is carried out at a temperature of 40°C.
  • the method according to the invention is characterized in that the at least one step of washing with water is carried out at a temperature of 60°C.
  • the method according to the invention is characterized in that the at least one step of washing with water is carried out with a mass percentage of water less than or equal to 10% relative to the total mass of split product.
  • the method according to the invention is characterized in that the at least one step of washing with water is carried out with a mass percentage of water less than or equal to 5% relative to the total mass. of split product.
  • the method according to the invention is characterized in that the at least one step of washing with water is carried out with a mass percentage of water equal to 10% relative to the total mass of product split.
  • the method according to the invention is characterized in that the at least one step of washing with water is carried out with a mass percentage of water equal to 5% relative to the total mass of product split.
  • the method according to the invention is characterized in that the elimination of the solvent system makes it possible to eliminate at least 99.5% of the solvent system relative to the total volume of the solvent system.
  • the method according to the invention is characterized in that the elimination of the solvent system makes it possible to eliminate at least 99.9% of the solvent system relative to the total volume of the solvent system.
  • the process according to the invention is characterized in that the shea olein fraction is a liquid fraction which comprises the following fatty acids: palmitic acid, stearic acid, oleic acid, linoleic acid and arachidic acid.
  • the process according to the invention is characterized in that the shea olein fraction is a clear liquid fraction.
  • turbidity is defined as being the reduction in the transparency of a liquid due to the presence of undissolved matter (NF EN ISO 7027). In other words, it corresponds to the property of the sample to scatter and absorb incident light.
  • the process according to the invention is characterized in that the olein fraction comprises a mass percentage of palmitic acid of at most 10% relative to the total mass of fatty acid of the fraction of shea olein.
  • the process according to the invention is characterized in that the shea olein fraction comprises a mass percentage of palmitic acid of at most 5% relative to the total mass of fatty acid of the fraction of shea olein.
  • the process according to the invention is characterized in that the olein fraction comprises a mass percentage of palmitic acid of at most 4% relative to the total mass of fatty acid of the fraction of shea olein.
  • the method according to the invention is characterized in that the shea olein fraction comprises a mass percentage of oleic acid of at least 45% relative to the total mass of fatty acid of the fraction of shea olein.
  • the process according to the invention is characterized in that the olein fraction comprises a mass percentage of oleic acid of at least 50% relative to the total mass of fatty acid of the fraction of shea olein.
  • the process according to the invention is characterized in that the olein fraction comprises a mass percentage of oleic acid of between 50 and 75% relative to the total mass of fatty acid of the fraction of shea olein.
  • the process according to the invention is characterized in that the olein fraction comprises a mass percentage of stearic acid of at most 35% relative to the total mass of fatty acid of the fraction of shea olein.
  • the process according to the invention is characterized in that the olein fraction comprises a mass percentage of stearic acid of at most 29% relative to the total mass of fatty acid of the fraction of shea olein.
  • the process according to the invention is characterized in that the olein fraction comprises a mass percentage of stearic acid of at most 25% relative to the total mass of fatty acid of the fraction of shea olein.
  • the process according to the invention is characterized in that the olein fraction comprises a mass percentage of linoleic acid of at least 5% relative to the total mass of fatty acid of the fraction of shea olein.
  • the process according to the invention is characterized in that the olein fraction comprises a mass percentage of linoleic acid of between 5 and 20% relative to the total mass of fatty acid of the fraction of shea olein.
  • the process according to the invention is characterized in that the olein fraction comprises a mass percentage of linoleic acid of between 5 and 15% relative to the total mass of fatty acid of the fraction of shea olein.
  • the process according to the invention is characterized in that the olein fraction comprises a mass percentage of arachidic acid of at most 5% relative to the total mass of fatty acid of the fraction of shea olein.
  • the process according to the invention is characterized in that the olein fraction comprises a mass percentage of arachidic acid of at most 3% relative to the total mass of fatty acid of the fraction of shea olein.
  • the process according to the invention is characterized in that the olein fraction comprises a mass percentage of arachidic acid of at most 2% relative to the total mass of fatty acid of the fraction of shea olein.
  • the method according to the invention is characterized in that the shea olein fraction, preferably, comprises a mass percentage of at most 5% of palmitic acid, between 5 and 15% linoleic acid, not more than 3% arachidic acid, not more than 29% stearic acid and not less than 50% oleic acid, relative to the total mass of fatty acid of the fraction d shea olein.
  • the process according to the invention is characterized in that the shea stearin fraction is a solid fraction which comprises the following fatty acids: palmitic acid, stearic acid, oleic acid, linoleic acid and arachidic acid.
  • the process according to the invention is characterized in that the stearin fraction comprises a mass percentage of palmitic acid of at most 10% relative to the total mass of fatty acid of the stearin fraction of shea.
  • the process according to the invention is characterized in that the stearin fraction comprises a mass percentage of palmitic acid of at most 5% relative to the total mass of fatty acid of the stearin fraction of shea.
  • the process according to the invention is characterized in that the stearin fraction comprises a mass percentage of palmitic acid of at most 4% relative to the total mass of fatty acid of the stearin fraction of shea.
  • the process according to the invention is characterized in that the stearin fraction comprises a mass percentage of oleic acid of between 20 and 40% relative to the total mass of fatty acid of the stearin fraction of shea.
  • the process according to the invention is characterized in that the stearin fraction comprises a mass percentage of oleic acid of between 30 and 50% relative to the total mass of fatty acid of the stearin fraction of shea.
  • the process according to the invention is characterized in that the stearin fraction comprises a mass percentage of oleic acid of between 30 and 40% relative to the total mass of fatty acid of the stearin fraction of shea.
  • the method according to the invention is characterized in that the stearin fraction comprises a mass percentage of stearic acid of between 40 and 60% relative to the total mass of fatty acid of the stearin fraction of shea.
  • the process according to the invention is characterized in that the stearin fraction comprises a mass percentage of stearic acid of between 50 and 70% relative to the total mass of fatty acid of the stearin fraction of shea.
  • the method according to the invention is characterized in that the stearin fraction comprises a mass percentage of stearic acid of between 50 and 60% relative to the total mass of fatty acid of the stearin fraction of shea.
  • the process according to the invention is characterized in that the stearin fraction comprises a mass percentage of linoleic acid of at most 10% relative to the total mass of fatty acid of the stearin fraction of shea.
  • the process according to the invention is characterized in that the stearin fraction comprises a mass percentage of linoleic acid between 5 and 10% relative to the total fatty acid mass of the shea stearin fraction.
  • the process according to the invention is characterized in that the stearin fraction comprises a mass percentage of linoleic acid of at most 5% relative to the total mass of fatty acid of the stearin fraction of shea.
  • the method according to the invention is characterized in that the stearin fraction comprises a mass percentage of arachidic acid of at most 5% relative to the total mass of fatty acid of the stearin fraction of shea.
  • the method according to the invention is characterized in that the stearin fraction comprises a mass percentage of arachidic acid of at most 3% relative to the total mass of fatty acid of the stearin fraction of shea.
  • the method according to the invention is characterized in that the stearin fraction comprises a mass percentage of arachidic acid of at most 2% relative to the total mass of fatty acid of the stearin fraction of shea.
  • the process according to the invention is characterized in that the fraction of shea stearin, preferably, comprises a mass percentage of at most 5% palmitic acid, at most 5% palmitic acid linoleic acid, of at most 3% in arachidic acid, comprised between 30 and 40% in oleic acid and comprised between 50 and 60% in stearic acid, relative to the total mass of fatty acid of the shea stearin fraction.
  • the applications of the shea olein and stearin fractions obtained by applying the process according to the invention are applications aimed at incorporating cosmetic and/or food compositions
  • Food applications include, for example, use in the chocolate and confectionery industry, use in pastry
  • the targeted applications are more particularly the commonly used applications in the context of shea oleins and stearins which can be used in the following products or compositions:
  • Facial formulation makeup formulation, facial treatment, moisturizing formulation, UV protection, anti-aging formulation, anti-wrinkle formulation.
  • Body formulation UV protection formulation, anti-aging formulation, anti-wrinkle formulation, moisturizing formulation, depigmenting formulation, pro-pigmenting formulation.
  • compositions care of joint pain, rheumatism.
  • other examples of use in compositions aimed at solving skin problems Dermatitis, bruises, wound care.
  • the refined butter used in the rest of these examples has the fatty acid composition indicated in the table below: Table 1: fatty acid composition of refined shea butter Refined shea butter Mass percentage (in %) palmitic acid 3.5 Stearic acid 44.1 Oleic acid 45.1 Linoleic acid 5.8 arachidic acid 1.5
  • Table 2 Target fatty acid composition of shea olein and stearin fractions Shea olein fraction Shea stearin fraction Palmitic acid (%) [0-5] [0-5] Stearic acid (%) Max 29 [50-60] Oleic acid (%) Min 45 [30-40] Linoleic acid (%) [5-15] [0-5] Arachidic acid (%) [0-3] [0-3]
  • Example 1 Comparative Example, Fractionation of Refined Shea Butter with Biosourced Dodecane:
  • 60g of refined shea butter is mixed with 40g of BIOSYNTHIS dodecane at a temperature of 40°C.
  • the mixture is stirred for 5 minutes so as to obtain a liquid and homogeneous fraction.
  • the reaction mixture is cooled to a temperature of 4° C. for 24 hours.
  • the reaction mixture is filtered through 11um paper.
  • the solvent is evaporated from the shea olein fraction and from the shea stearin fraction.
  • the olein fraction (liquid phase) is concentrated after evaporation under vacuum of 30mbar and a temperature of 150°C.
  • the stearin fraction (solid phase) is concentrated under the same conditions.
  • Table 3 Composition of the products obtained according to a fractionation process carried out with dodecane:
  • Product obtained according to the process of the invention Shea olein fraction Shea stearin fraction Physical state/ Appearance cloudy liquid Solid Fatty acid mass percentage of the fractions obtained according to the process of the invention (%) Shea olein fraction Shea stearin fraction palmitic acid 3.6 3.6 Stearic acid 37.7 48.1 Oleic acid 49.9 42 Linoleic acid 7.4 5.1 arachidic acid 1.4 1.2
  • Example 2 Fractionation of a refined shea butter with ethyl levulinate.
  • the reaction mixture is cooled to a temperature of 4°C overnight.
  • the reaction mixture is filtered through 11um paper.
  • the solvent is evaporated from the shea olein fraction and from the shea stearin fraction.
  • the olein fraction (liquid phase) is concentrated after evaporation under vacuum of 30mbar and a temperature of 150°C.
  • the stearin fraction (solid phase) is concentrated under the same conditions.
  • Table 4 shows the fatty acid compositions of the olein and shea stearin fractions obtained according to the process of the present invention.
  • Table 4 Composition of the products obtained according to the process of the present invention (100% ethyl levulinate)
  • Product obtained according to the process of the invention Shea olein fraction Shea stearin fraction Physical state/ Appearance Clear liquid Solid Fatty acid mass percentage of the fractions obtained according to the process of the invention (%) Shea olein fraction Shea stearin fraction palmitic acid 3.6 3.1 Stearic acid 28.2 47.9 Oleic acid 57.9 42.6 Linoleic acid 9.2 4.8 arachidic acid 1.1 1.6
  • fractionation process carried out with 100% ethyl levulinate makes it possible to obtain a clear olein and a shea stearin with a satisfactory fatty acid composition.
  • Example 3 Fractionation of a refined shea butter by ethyl levulinate: 40 g of refined shea butter are mixed with 60 g of ethyl levulinate) at a temperature of 40°C. The mixture is stirred for 5 minutes so as to obtain a liquid and homogeneous fraction.
  • the reaction mixture is cooled to a temperature of 4°C overnight.
  • the reaction mixture is filtered through 11um paper.
  • the solvent is evaporated from the shea olein fraction and from the shea stearin fraction.
  • the olein fraction (liquid phase) is concentrated after evaporation under vacuum of 30mbar and a temperature of 150°C.
  • the stearin fraction (solid phase) is concentrated under the same conditions.
  • Table 5 shows the fatty acid compositions of the olein and shea stearin fractions obtained according to the process of the present invention.
  • Table 5 Composition of the products obtained according to the process of the present invention (100% ethyl levulinate)
  • Product obtained according to the process of the invention Shea olein fraction Shea stearin fraction Physical state/ Appearance Clear liquid Solid Fatty acid mass percentage of the fractions obtained according to the process of the invention (%) Shea olein fraction Shea stearin fraction palmitic acid 3.7 3.1 Stearic acid 27.9 45.7 Oleic acid 57.5 44.3 Linoleic acid 9.8 5.3 arachidic acid 1.1 1.6
  • the reaction mixture is cooled to a temperature of 4°C overnight.
  • the reaction mixture is filtered through 11um paper.
  • the solvent is evaporated from the shea olein fraction and from the shea stearin fraction.
  • the olein fraction (liquid phase) is concentrated after evaporation under vacuum of 30mbar and a temperature of 150°C.
  • the stearin fraction (solid phase) is concentrated under the same conditions.
  • the table below shows the fatty acid compositions of the olein and shea stearin fractions obtained according to the process of the present invention.
  • Table 6 Composition of the products obtained according to the process of the present invention (70% ethyl levulinate, 30% decane)
  • Product obtained according to the process of the invention Shea olein fraction Shea stearin fraction Physical state/ Appearance Clear liquid Solid Fatty acid mass percentage of the fractions obtained according to the process of the invention (%) Shea olein fraction Shea stearin fraction palmitic acid 3.4 2.6 Stearic acid 39.9 56.9 Oleic acid 48.3 35.8 Linoleic acid 6.5 3.3 arachidic acid 1.9 1.4
  • the reaction mixture is cooled to a temperature of 4°C overnight.
  • the reaction mixture is filtered through 11um paper.
  • the solvent is evaporated from the shea olein fraction and from the shea stearin fraction.
  • the olein fraction (liquid phase) is concentrated after evaporation under vacuum of 30mbar and a temperature of 150°C.
  • the stearin fraction (solid phase) is concentrated under the same conditions.
  • the table below shows the fatty acid compositions of the olein and shea stearin fractions obtained according to the process of the present invention.
  • Table 7 Composition of the products obtained according to the process of the present invention (87.5% ethyl levulinate, 12.5% decane)
  • Product obtained according to the process of the invention Shea olein fraction Shea stearin fraction Physical state/ Appearance Clear liquid Solid Fatty acid mass percentage of the fractions obtained according to the process of the invention (%) Shea olein fraction Shea stearin fraction palmitic acid 3.5 3.1 Stearic acid 29.4 46.1 Oleic acid 56.8 43.8 Linoleic acid 9.1 5.4 arachidic acid 1.2 1.6
  • the reaction mixture is cooled to a temperature of 4°C overnight.
  • the reaction mixture is filtered through 11um paper.
  • the solvent is evaporated from the shea olein fraction and from the shea stearin fraction.
  • the olein fraction (liquid phase) is concentrated after evaporation under vacuum of 30mbar and a temperature of 150°C.
  • the stearin fraction (solid phase) is concentrated under the same conditions.
  • Table 8 shows the fatty acid compositions of the olein and shea stearin fractions obtained according to the process of the present invention.
  • Table 8 Composition of the products obtained according to the process of the present invention (94% ethyl levulinate, 6% decane)
  • Product obtained according to the process of the invention Shea olein fraction Shea stearin fraction Physical state/ Appearance Clear liquid Solid Fatty acid mass percentage of the fractions obtained according to the process of the invention (%) Shea olein fraction Shea stearin fraction palmitic acid 3.5 3.2 Stearic acid 25.4 44.6 Oleic acid 60.1 45.0 Linoleic acid 10.0 5.6 arachidic acid 1.0 1.6
  • Example 7 Fractionation of a refined shea butter with an ethyl levulinate-dodecane mixture:
  • the reaction mixture is cooled to a temperature of 4°C overnight.
  • the reaction mixture is filtered through 11um paper.
  • the solvent is evaporated from the shea olein fraction and from the shea stearin fraction.
  • the olein fraction (liquid phase) is concentrated after evaporation under vacuum of 30mbar and a temperature of 150°C.
  • the stearin fraction (solid phase) is concentrated under the same conditions.
  • the table below shows the fatty acid compositions of the olein and shea stearin fractions obtained according to the process of the present invention.
  • Table 9 Composition of the products obtained according to the process of the present invention (94% ethyl levulinate, 6% dodecane).
  • Product obtained according to the process of the invention Shea olein fraction Shea stearin fraction Physical state/ Appearance Clear liquid Solid Fatty acid mass percentage of the fractions obtained according to the process of the invention (%) Shea olein fraction Shea stearin fraction palmitic acid 4.3 3.4 Stearic acid 22.1 44.1 Oleic acid 61.3 45.4 Linoleic acid 12 5.6 arachidic acid 0.3 1.5
  • Example 8 Fractionation of a refined shea butter with a mixture of ethyl levulinate and ethyl lactate.
  • the reaction mixture is cooled to a temperature of 4°C overnight.
  • the reaction mixture is filtered through 11um paper.
  • the solvent is evaporated from the shea olein fraction and from the shea stearin fraction.
  • the olein fraction (liquid phase) is concentrated after evaporation under vacuum of 30mbar and a temperature of 150°C.
  • the stearin fraction (solid phase) is concentrated under the same conditions.
  • Table 10 shows the fatty acid compositions of the olein and shea stearin fractions obtained according to the process of the present invention.
  • Table 10 Composition of the products obtained according to the process of the present invention (50% ethyl levulinate and 50% ethyl lactate)
  • Product obtained according to the process of the invention Shea olein fraction Shea stearin fraction Physical state/ Appearance cloudy liquid Solid Fatty acid mass percentage of the fractions obtained according to the process of the invention (%) Shea olein fraction* Shea stearin fraction palmitic acid 3.9 3.4 Stearic acid 28 48.8 Oleic acid 57.2 41.2 Linoleic acid 9.9 5.1 arachidic acid 1 1.5

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Abstract

L'invention concerne un procédé de fractionnement d'un extrait de karité qui comprend au moins les étapes suivantes :
a) mélange et homogénéisation du beurre de karité à l'aide d'un système de solvant comprenant au moins un oxo-ester de formule I,

Figure imga0001
dans laquelle,
- R1 est choisi dans le groupe constitué par les alkyles linéaires ou ramifiés comprenant de 1 à 8 atomes de carbone ;
- R2, R3 et R4 identiques ou différents sont choisis dans le groupe constitué par l'atome d'hydrogène ou les alkyles linéaires ou ramifiés comprenant de 1 à 4 atomes de carbone; et
- et n est un entier naturel compris entre 1 et 4.

b) obtention d'un mélange homogène,
c) refroidissement du mélange
d) filtration et élimination du système de solvant afin de récupérer les fractions d'oléine et de stéarine.The invention relates to a process for fractionating a shea extract which comprises at least the following steps:
a) mixing and homogenizing the shea butter using a solvent system comprising at least one oxo-ester of formula I,
Figure imga0001
in which,
- R 1 is chosen from the group consisting of linear or branched alkyls comprising from 1 to 8 carbon atoms;
- R 2 , R 3 and R 4 , which are identical or different, are chosen from the group consisting of the hydrogen atom or linear or branched alkyls comprising from 1 to 4 carbon atoms; and
- and n is a natural number between 1 and 4.

b) obtaining a homogeneous mixture,
c) cooling of the mixture
d) filtration and removal of the solvent system to recover the olein and stearin fractions.

Description

L'invention concerne un procédé de fractionnement d'un extrait de karité permettant le fractionnement, la séparation et la récupération des deux factions constitutives du karité que sont l'oléine et la stéarine de karité.The invention relates to a process for fractionating a shea extract allowing the fractionation, separation and recovery of the two constituent factions of shea, namely olein and shea stearin.

On entend par extrait de karité, une matière issue du fruit ou des graines de karité. L'extrait de karité peut être obtenu par méthode traditionnelle, pression mécanique, extraction à froid et/ou extraction par solvants. Ces techniques sont détaillées dans le manuel des corps gras d' Alain KARLESKIND (TEC & DOCS, 1993 ).By shea extract is meant a material derived from the fruit or seeds of shea. The shea extract can be obtained by traditional method, mechanical pressure, cold extraction and/or solvent extraction. These techniques are detailed in the body fat manual of Alain KARLESKIND (TEC & DOCS, 1993 ).

De manière préférentielle, dans la présente demande, l'extrait de karité est un beurre de karité.Preferably, in the present application, the shea extract is a shea butter.

Au sens de la présente invention, un beurre de karité est un corps gras végétal solide à température ambiante, extrait du fruit ou des graines de karité, et qui fond à des températures voisines de celles de la peau.Within the meaning of the present invention, a shea butter is a vegetable fatty substance which is solid at room temperature, extracted from the fruit or the seeds of the shea tree, and which melts at temperatures close to those of the skin.

Le beurre de karité utilisé dans la présente invention peut être obtenu par méthode traditionnelle, extraction par solvant et/ou extraction à froid.The shea butter used in the present invention can be obtained by traditional method, solvent extraction and/or cold extraction.

Le beurre de karité utilisé dans la présente invention est de manière préférentielle raffiné et est issu de l'agriculture biologique certifié CEE/ NOP organic par FR-BIO-01 et ECOCERT SA.The shea butter used in the present invention is preferentially refined and comes from organic farming certified CEE/NOP organic by FR-BIO-01 and ECOCERT SA.

Pour ce faire, le beurre de karité peut subir une étape de dégommage, une étape de décoloration, une étape de désodorisation et/ou une étape de neutralisation.To do this, the shea butter can undergo a degumming step, a bleaching step, a deodorization step and/or a neutralization step.

L'étape de dégommage, également appelée étape de démucilagination permet d'ôter les latex du beurre végétal. En botanique, on appelle latex une substance liquide, à consistance plus ou moins épaisse, sécrétée par certaines plantes ou par certains champignons et circulant dans les canaux laticifères. Lors du raffinage, le beurre végétal brut est dégommé en mélangeant l'huile avec de l'eau ou de la vapeur et en faisant passer le mélange dans des centrifugeuses qui séparent le résidu gommeux de l'huile.The degumming step, also called the degumming step, removes the latex from the vegetable butter. In botany, latex is a liquid substance, with a more or less thick consistency, secreted by certain plants or by certain fungi and circulating in the laticiferous ducts. During refining, raw vegetable butter is degummed by mixing the oil with water or steam and passing the mixture through centrifuges which separate the gummy residue from the oil.

L'étape de décoloration permet d'éliminer les pigments colorés (chlorophylles et caroténoïdes), les savons résiduels, les traces de mucilage, des métaux lourds notamment par l'utilisation de terres activées. Les terres décolorantes sont généralement des argiles plastiques simplement séchées et finement broyées pour accroître leur surface de contact. On peut également utiliser des charbons activés.The discoloration step eliminates colored pigments (chlorophylls and carotenoids), residual soaps, traces of mucilage, heavy metals, in particular through the use of activated earths. Bleaching earths are generally plastic clays that are simply dried and finely ground to increase their contact surface. You can also use activated charcoal.

L'étape de désodorisation est destinée à éliminer les substances odorantes (essentiellement les composés soufrés) de l'huile décolorée. Cette opération est couramment réalisée sous vide à haute température. Il s'agit, d'un entraînement à la vapeur d'eau sous vide de ces composés qui résultent de la dégradation de l'huile.The deodorization step is intended to remove odorous substances (essentially sulfur compounds) from the decolorized oil. This operation is commonly carried out under vacuum at high temperature. This involves steam distillation under vacuum of these compounds which result from the degradation of the oil.

La neutralisation ou la désacidification consiste à éliminer les acides gras libres de l'huile démucilaginée. Les techniques de neutralisation des huiles végétales les plus utilisées sont :

  • La neutralisation chimique ou alcaline (par la soude ou par la chaux).
  • La neutralisation physique (par distillation).
Neutralization or deacidification consists of removing the free fatty acids from the degummed oil. The most commonly used vegetable oil neutralization techniques are:
  • Chemical or alkaline neutralization (using soda or lime).
  • Physical neutralization (by distillation).

Outre l'élimination des acides gras libres, la neutralisation permet d'éliminer la totalité des phospholipides, les traces de métaux et les produits dégradés par oxydationIn addition to the elimination of free fatty acids, neutralization eliminates all phospholipids, traces of metals and products degraded by oxidation.

Le beurre de karité utilisé dans la présente invention peut être un beurre de karité brut. On entend par beurre de karité brut un beurre de karité n'ayant subi aucune étape de raffinage.The shea butter used in the present invention can be raw shea butter. Raw shea butter means shea butter that has not undergone any refining step.

On entend par procédé de fractionnement un procédé de séparation d'un mélange en plusieurs fractions successives dont les propriétés physiques sont différentes.By fractionation process is meant a process for separating a mixture into several successive fractions whose physical properties are different.

Dans le cas de la présente invention, le fractionnement consiste à séparer l'extrait de karité en fractions de caractéristiques physiques différentes. L'extrait de karité peut ainsi être séparé en une huile communément désignée comme la fraction d'oléine de karité et une fraction solide, la stéarine de karité, dont le point de fusion est plus élevé que l'extrait de karité de départ.In the case of the present invention, the fractionation consists in separating the shea extract into fractions of different physical characteristics. The shea extract can thus be separated into an oil commonly referred to as the shea olein fraction and a solid fraction, the shea stearin, whose melting point is higher than the starting shea extract.

Au sens de la présente invention, la fraction d'oléine de karité est une fraction d'acides gras, liquide à température ambiante et dont le pourcentage massique en acide oléique est supérieur au pourcentage massique de chaque acide gras qui la compose. De manière plus précise, le pourcentage massique en acide oléique est d'au moins 50% par rapport à la masse totale d'acide gras de la fraction d'oléine de karité.Within the meaning of the present invention, the shea olein fraction is a fraction of fatty acids, liquid at ambient temperature and whose mass percentage of oleic acid is greater than the mass percentage of each fatty acid which composes it. More specifically, the mass percentage of oleic acid is at least 50% relative to the total mass of fatty acid of the shea olein fraction.

De manière analogue, la fraction de stéarine de karité est une fraction d'acide gras, solide à température ambiante et dont le pourcentage massique en acide stéarique est supérieur au pourcentage massique de chaque acide gras qui la compose. De manière plus précise, le pourcentage massique en acide stéarique est d'au moins 45% par rapport à la masse totale d'acide gras de la fraction de stéarine de karitéSimilarly, the shea stearin fraction is a fatty acid fraction, solid at room temperature and whose mass percentage of stearic acid is greater than the mass percentage of each fatty acid which composes it. More specifically, the mass percentage of stearic acid is at least 45% relative to the total mass of fatty acid of the shea stearin fraction

Dans la présente demande un « pourcentage massique » est le rapport de la masse d'un premier composé par rapport à la masse totale d'un mélange de composés ou composition, ramené à un pourcentage.In the present application, a “mass percentage” is the ratio of the mass of a first compound relative to the total mass of a mixture of compounds or composition, reduced to a percentage.

De telles fractions végétales peuvent avoir divers usages dans l'industrie alimentaire et cosmétique.Such plant fractions can have various uses in the food and cosmetics industry.

Dans JP2011132207A , des compositions cosmétiques comprenant une matière première issue du beurre de karité ont été décrites.In JP2011132207A , cosmetic compositions comprising a raw material derived from shea butter have been described.

Dans JP2016054675A , des compositions de crèmes comestibles (cafés,etc.) comprenant une matière première issue du beurre de karité ont été décrites.In JP2016054675A , compositions of edible creams (coffees, etc.) comprising a raw material derived from shea butter have been described.

Dans WO2018226149 ou encore EP0460722A1 , des équivalents de beurre de cacao comprenant de la stéarine de karité ont été divulgués.In WO2018226149 or EP0460722A1 , cocoa butter equivalents comprising shea stearin have been disclosed.

Comme illustré dans US2015264956A1 et WO2011122278 , les procédés usuels de fractionnement d'huiles végétales et notamment de beurre de karité peuvent comprendre plusieurs étapes de fractionnement et/ou de traitements supplémentaires.As illustrated in US2015264956A1 and WO2011122278 , the usual processes for fractionating vegetable oils and in particular shea butter can comprise several stages of fractionation and/or additional treatments.

Par ailleurs, la nature ou la quantité des solvants utilisés lors des procédés de fractionnement par solvant peuvent être inadaptées tant du point de vue économique que d'un point de vue toxicologique et environnemental.Moreover, the nature or the quantity of the solvents used during the solvent fractionation processes may be unsuitable both from an economic point of view and from a toxicological and environmental point of view.

Les solvants, les plus communément utilisés pour fractionner l'extrait de karité sont les solvants aliphatiques de type hexane ou de manière préférentielle l'acétone.The solvents most commonly used to fractionate the shea extract are aliphatic solvents of the hexane type or preferably acetone.

La demande EP18757927 divulgue des procédés de fractionnement effectués par ces deux types de solvant.Requirement EP18757927 discloses fractionation processes carried out by these two types of solvent.

L'hexane est un solvant organique considéré comme toxique et est classé CMR de catégorie 2. De plus, au vu de ses propriétés physico-chimiques ce solvant présente un danger en manipulation et encore plus à l'échelle industrielle (point éclair-23,3°C / température d'auto-inflammation 233°C).Hexane is an organic solvent considered to be toxic and is classified as CMR category 2. In addition, given its physico-chemical properties, this solvent presents a danger in handling and even more so on an industrial scale (flash point-23, 3°C / auto-ignition temperature 233°C).

En revanche, l'acétone est un solvant volatil et inflammable (point éclair à - 18°C) très utilisé dans l'industrie chimique. Cependant, sa haute volatilité, nécessite dans les procédés industriels un volume de solvant pouvant être inadapté d'un point de vue économique et environnemental.On the other hand, acetone is a volatile and flammable solvent (flash point at -18°C) widely used in the chemical industry. However, its high volatility requires in industrial processes a volume of solvent that may be unsuitable from an economic and environmental point of view.

La présente invention permet de fractionner directement sans traitement ultérieur, un extrait de karité à l'aide d'un système de solvant et de récupérer simultanément une fraction d'oléine de karité et de stéarine de karité, les deux fractions étant conformes aux exigences des règlementations de l'industrie cosmétique et alimentaire.The present invention makes it possible to fractionate directly without subsequent treatment, a shea extract using a solvent system and to simultaneously recover a fraction of shea olein and shea stearin, the two fractions being in accordance with the requirements of the cosmetic and food industry regulations.

La présente invention est un procédé de fractionnement d'un extrait de karité comprenant au moins les étapes suivantes :

  1. a) mélange et homogénéisation du beurre de karité à l'aide d'un système de solvants comprenant au moins un oxo-ester de formule I,
    Figure imgb0001
    dans laquelle,
    • R1 est choisi dans le groupe constitué par les alkyles linéaires ou ramifiés comprenant de 1 à 8 atomes de carbone ;
    • R2, R3 et R4 identiques ou différents sont choisis dans le groupe constitué par l'atome d'hydrogène ou les alkyles linéaires ou ramifiés comprenant de 1 à 4 atomes de carbone; et
    • n est un entier naturel compris entre 1 et 4.
  2. b) obtention d'un mélange homogène,
  3. c) refroidissement du mélange
  4. d) filtration et élimination du système de solvant afin de récupérer les fractions d'oléine et de stéarine.
The present invention is a process for fractionating a shea extract comprising at least the following steps:
  1. a) mixing and homogenizing the shea butter using a solvent system comprising at least one oxo-ester of formula I,
    Figure imgb0001
    in which,
    • R 1 is chosen from the group consisting of linear or branched alkyls comprising from 1 to 8 carbon atoms;
    • R 2 , R 3 and R 4 which are identical or different are chosen from the group consisting of the hydrogen atom or linear or branched alkyls comprising from 1 to 4 carbon atoms; and
    • n is a natural number between 1 and 4.
  2. b) obtaining a homogeneous mixture,
  3. c) cooling of the mixture
  4. d) filtration and removal of the solvent system to recover the olein and stearin fractions.

Dans un mode de réalisation, les solvants du système de solvants sont biosourcés. Au sens de la présente invention, on qualifie de biosourcé un composé ou une composition organique dont le carbone organique présent dans le composé ou la composition est d'origine végétale par une analyse au radiocarbone selon l'une des normes suivantes ASTM D6866, EN 16640 ou EN 16785-1.In one embodiment, the solvents in the solvent system are biobased. Within the meaning of the present invention, a biobased compound or an organic composition in which the organic carbon present in the compound or composition is of plant origin is qualified by a radiocarbon analysis according to one of the following standards ASTM D6866, EN 16640 or EN 16785-1.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'extrait de karité est issu des graines de karité.In one embodiment, the method according to the invention is characterized in that the shea extract is derived from shea seeds.

Dans un mode de réalisation préféré, le procédé selon l'invention est caractérisé en ce que l'extrait de karité est un beurre de karité.In a preferred embodiment, the method according to the invention is characterized in that the shea extract is a shea butter.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'extrait de karité est un beurre de karité dit naturel.In one embodiment, the method according to the invention is characterized in that the shea extract is a so-called natural shea butter.

Dans un mode de réalisation préféré, le procédé selon l'invention est caractérisé en ce que l'extrait de karité est un beurre de karité raffiné.In a preferred embodiment, the process according to the invention is characterized in that the shea extract is a refined shea butter.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'extrait de karité est un beurre de karité raffiné ayant subi un raffinage comprenant une étape de dégommage.In one embodiment, the method according to the invention is characterized in that the shea extract is a refined shea butter having undergone a refining comprising a degumming step.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'extrait de karité est un beurre de karité raffiné ayant subi un raffinage comprenant une étape de décoloration.In one embodiment, the process according to the invention is characterized in that the shea extract is a refined shea butter having undergone a refining comprising a decolorization step.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'extrait de karité est un beurre de karité raffiné ayant subi un raffinage comprenant une étape de désodorisation.In one embodiment, the method according to the invention is characterized in that the shea extract is a refined shea butter having undergone a refining comprising a deodorization step.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'extrait de karité est un beurre de karité raffiné ayant subi un raffinage comprenant une étape de neutralisation.In one embodiment, the method according to the invention is characterized in that the shea extract is a refined shea butter having undergone a refining comprising a neutralization step.

Dans un mode de réalisation préféré, le procédé selon l'invention est caractérisé en ce que l'extrait de karité est un beurre de karité raffiné ayant subi les étapes de raffinage comprenant une étape de dégommage, une étape de décoloration, une étape de désodorisation et une étape de neutralisation.In a preferred embodiment, the method according to the invention is characterized in that the shea extract is a refined shea butter having undergone the refining steps comprising a degumming step, a bleaching step, a deodorization step and a neutralization step.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que dans le mélange homogène obtenu à l'étape b), défini par le ratio Y, Y = Pourcentage massique d un extrait de karité Pourcentage massique du système de solvant

Figure imgb0002
est d'au plus 1/1.In one embodiment, the method according to the invention is characterized in that in the homogeneous mixture obtained in step b), defined by the ratio Y, Y = Mass percentage d a shea extract Solvent System Mass Percentage
Figure imgb0002
is at most 1/1.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le ratio Y est d'au plus 1/2.In one embodiment, the method according to the invention is characterized in that the ratio Y is at most 1/2.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le ratio Y est d'au plus 1/3.In one embodiment, the method according to the invention is characterized in that the ratio Y is at most 1/3.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le ratio Y est d'au plus 1/5.In one embodiment, the method according to the invention is characterized in that the ratio Y is at most 1/5.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le ratio Y est compris entre 1/5 et 1/1.In one embodiment, the method according to the invention is characterized in that the ratio Y is between 1/5 and 1/1.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le ratio Y est 1/1.In one embodiment, the method according to the invention is characterized in that the ratio Y is 1/1.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le ratio Y est 1/2.In one embodiment, the method according to the invention is characterized in that the ratio Y is 1/2.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le ratio Y est 1/3.In one embodiment, the method according to the invention is characterized in that the ratio Y is 1/3.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le ratio Y est 1/4.In one embodiment, the method according to the invention is characterized in that the ratio Y is 1/4.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant est exempt de solvant catégorisé comme CMR.In one embodiment, the method according to the invention is characterized in that the solvent system is free of solvent categorized as CMR.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant a un point éclair inférieur ou égal à 110°C mesuré selon la norme ATSM D93.In one embodiment, the method according to the invention is characterized in that the solvent system has a flash point of less than or equal to 110° C. measured according to the ATSM D93 standard.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant a un point éclair inférieur ou égal à 100°C mesuré selon la norme ATSM D93.In one embodiment, the process according to the invention is characterized in that the solvent system has a flash point of less than or equal to 100° C. measured according to the ATSM D93 standard.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant a un point éclair inférieur ou égal à 95°C mesuré selon la norme ATSM D93.In one embodiment, the method according to the invention is characterized in that the solvent system has a flash point of less than or equal to 95° C. measured according to the ATSM D93 standard.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant a un point éclair inférieur ou égal à 90°C mesuré selon la norme ATSM D93.In one embodiment, the process according to the invention is characterized in that the solvent system has a flash point of less than or equal to 90° C. measured according to the ATSM D93 standard.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant a une température d'ébullition inférieure ou égale à 250°C.In one embodiment, the process according to the invention is characterized in that the solvent system has a boiling point of less than or equal to 250°C.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant a une température d'ébullition inférieure ou égale à 230°C.In one embodiment, the method according to the invention is characterized in that the solvent system has a boiling point of less than or equal to 230°C.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant a une température d'ébullition inférieure ou égale à 210°C.In one embodiment, the method according to the invention is characterized in that the solvent system has a boiling point of less than or equal to 210°C.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend au moins un oxo-ester de formule II :

Figure imgb0003
dans laquelle,

  • R1 est choisi dans le groupe constitué par les alkyles linéaires ou ramifiés comprenant de 1 à 4 atomes de carbone ;
  • R2, R3 et R4 identiques ou différents sont choisis dans le groupe constitué par l'atome d'hydrogène ou les alkyles linéaires ou ramifiés comprenant de 1 à 4 atomes de carbone; et
  • et n est un entier naturel compris entre 1 et 4.
In one embodiment, the process according to the invention is characterized in that the solvent system comprises at least one oxo-ester of formula II:
Figure imgb0003
in which,
  • R 1 is chosen from the group consisting of linear or branched alkyls comprising from 1 to 4 carbon atoms;
  • R 2 , R 3 and R 4 which are identical or different are chosen from the group consisting of the hydrogen atom or linear or branched alkyls comprising from 1 to 4 carbon atoms; and
  • and n is a natural number between 1 and 4.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend au moins un oxo-ester de formule III :

Figure imgb0004

  • R1 est choisi dans le groupe constitué par les alkyles linéaires ou ramifiés comprenant de 1 à 4 atomes de carbone ;
  • R2 et R3 identiques ou différents sont choisis dans le groupe constitué par l'atome d'hydrogène, le groupement méthyl ou le groupement éthyl
  • R4 est choisi dans le groupe constitué par les alkyls linéaires ou ramifiés comprenant de 1 à 3 atomes de carbone ;
  • et n est un entier naturel compris entre 1 et 3.
In one embodiment, the process according to the invention is characterized in that the solvent system comprises at least one oxo-ester of formula III:
Figure imgb0004
  • R 1 is chosen from the group consisting of linear or branched alkyls comprising from 1 to 4 carbon atoms;
  • R 2 and R 3 , which are identical or different, are chosen from the group consisting of the hydrogen atom, the methyl group or the ethyl group
  • R 4 is chosen from the group consisting of linear or branched alkyls comprising from 1 to 3 carbon atoms;
  • and n is a natural number between 1 and 3.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend au moins un oxo-ester de formule IV :

Figure imgb0005

  • R1 est choisi dans le groupe constitué par les alkyles linéaires ou ramifiés comprenant de 1 à 8 atomes de carbone ;
  • R2 et R3 sont un atome d'hydrogène
  • R4 est un groupement méthyl
  • et n est égal à 1.
In one embodiment, the process according to the invention is characterized in that the solvent system comprises at least one oxo-ester of formula IV:
Figure imgb0005
  • R 1 is chosen from the group consisting of linear or branched alkyls comprising from 1 to 8 carbon atoms;
  • R 2 and R 3 are a hydrogen atom
  • R 4 is a methyl group
  • and n is equal to 1.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend au moins un oxo-ester de formule V :

Figure imgb0006

  • R1 est choisi dans le groupe constitué par les alkyles linéaires ou ramifiés comprenant de 1 à 4 atomes de carbone ;
  • R2 et R3 sont un atome d'hydrogène
  • R4est un groupement méthyl
  • et n est égal à 1.
In one embodiment, the process according to the invention is characterized in that the solvent system comprises at least one oxo-ester of formula V:
Figure imgb0006
  • R 1 is chosen from the group consisting of linear or branched alkyls comprising from 1 to 4 carbon atoms;
  • R 2 and R 3 are a hydrogen atom
  • R4 is a methyl group
  • and n is equal to 1.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant est constitué d'un oxo-ester seul ou en mélange.In one embodiment, the process according to the invention is characterized in that the solvent system consists of an oxo-ester alone or as a mixture.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'oxo-ester seul ou en mélange est choisi dans le groupe comprenant : le lévulinate de méthyle ( CAS 624-45-3 ), le lévulinate d'éthyle ( CAS 539-88-8 ), le lévulinate de propyle (645-67-0), le lévulinate d'isopropyle ( CAS 21884-26-4 ), le lévulinate de butyle ( CAS 2052-15-5 ), le lévulinate d'isobutyle ( CAS 3757-32-2 ), le lévulinate de tert-butyle ( CAS 2854-10-6 ), le lévulinate de s-butyle ( CAS 85734-01-6 ), le lévulinate de penthyl ( CAS 20279-49-6 ) le lévulinate d'hexyle ( CAS 24431-34-3 ), le lévulinate d'octyl ( CAS 41780-57-8 ), 2-Methyl-4-oxovaleric acid ethyl ester ( CAS 4749-12-6 ), methyl-6-oxoheptanoate ( CAS 2046-21-1 ), methyl 4-oxohexanoate ( CAS 2955-62-6 ), methyl 5-oxohexanoate ( CAS 13984-50-4 ), methyl 3-methyl -5-oxohexanoate ( CAS 14983-18-7 ), 5-ketoenanthic acid methyl ester (17745-32-3), methyl 3-methyl-4-oxopentanoate ( CAS 25234-83-7 ), methyl 2-methyl-4 oxopentanoate ( CAS 32811-25-9 ), 4-Oxo-5-methylhexanoic acid methyl ester ( CAS 34553-37-2 ), pentanoic acid 2,3 dimethyl-4-oxo, methyl ester ( CAS 35140-52-4 ), hexanoic acid, 4-methyl-5-oxo, methyl ester ( CAS 36045-56-4 ), pentanoic acid 2-ethyl-4-oxo-methyl ester ( CAS 62359-06-2 ), methyl 3-methyl-4-oxohexanoate ( CAS 69448-35-7 ), hexanoic acid 2-methyl-5-oxo methyl ester ( CAS 38872-30-9 ), pentanoic acid 3-methyl-4-oxo ethyl ester ( CAS 55424-74-3 ), hexanoic acid 2-ethyl-4-oxo methyl ester ( CAS 75436-59-8 ), hexanoic acid, 2, 4-dimethyl-5-oxo methyl ester ( CAS 93176-58-0 ), pentanoic acid-4-oxo-2-propyl-methyl ester ( CAS 244196-06-3 ), hexanoic acid 2,5-dimethyl-4-oxo methyl ester ( CAS 1249353-11-4 ), octanoic acid 4 oxo-methyl ester ( CAS : 4316-48-7 ), heptanoic acid 2-methyl-6-oxo-methyl ester ( CAS 2570-90-3 ), heptanoic acid 3-methyl 6-oxo methyl ester ( CAS 5128-55-2 ), heptanoic acid 6-methyl-5-oxo methyl ester ( CAS 23575-33-9 ), hexanoic acid 3-methyl-5-oxo- ethyl ester ( CAS 38052-21-0 ), heptanoic acid 2-methyl-5-oxo methyl ester ( CAS 25912-38-3 ), heptanoic acid 4 methyl-6-oxo methyl ester ( CAS 41841-53-6 ), heptanoic acid 5 methyl-4-oxo methyl ester ( CAS 42511-74-0 ), heptanoic acid-4-methyl-5-oxo methyl ester ( CAS 54225-40-0 ), hexanoic acid 3,5-dimethyl-4-oxo methyl ester ( CAS 64712-02-3 ), heptanoic acid 6-methyl-4-oxo methyl ester ( CAS 76678-33-6 ), heptanoic acid, 2-methyl-4-oxo- methyl ester ( CAS 90647-21-5 ), hexanoic aicd, 4-ethyl-5-oxo methyl ester ( CAS 90647-24-8 ), heptanoic aid 3-methyl-5-oxo, methyl ester ( CAS 103252-99-9 ), hexanoic acid, 2-ethyl-5-oxo-, methyl ester ( CAS 103260-39-5 ), hexanoic acid 3 acetyl methyl ester ( CAS 1081559-93-4 ), heptanoic acid 5 methyl-6-oxo methyl ester ( CAS 344295-02-9 ), heptanoic acid 3-methyl-4-oxo methyl ester ( CAS 64712-01-2 ), methyl 2-(1methylethyl)-4-oxopentaoate ( CAS 99183-33-2 ), methyl 2,3-dimethyl-4-oxohexanoate ( CAS 86044-19-1 ), Ethyl 2 ethyl-4-oxopentanoate ( CAS 101514-30-1 ), hexanoic acid 5-oxo ethyl ester ( CAS 13984-57-1 ), ethyl 3 methyl-4-oxohexanoate ( CAS 42895-72-7 ), ethyl 2,3-dimethyl-4-oxopentanoate ( CAS 136964-44-8 ), hexanoic acid 4 oxo ethyl ester ( CAS 3249-33-0 ), heptanoic acid 6-oxo-ethyl ester ( CAS 30956-41-3 ), 1-methylethyl-4-oxohexanoate ( CAS 939422-07-8 ), pentanoic 2-ethyl-4-oxo- ethyl ester ( CAS 101514-30-1 ), hexanoic acid-2ethyl-5-methyl-4-oxo- methyl ester ( CAS 1195311-69-3 ).In one embodiment, the process according to the invention is characterized in that the oxo-ester alone or as a mixture is chosen from the group comprising: methyl levulinate ( CAS 624-45-3 ), ethyl levulinate ( CAS 539-88-8 ), propyl levulinate (645-67-0), isopropyl levulinate ( CAS 21884-26-4 ), butyl levulinate ( CAS 2052-15-5 ), isobutyl levulinate ( CAS 3757-32-2 ), tert-butyl levulinate ( CAS 2854-10-6 ), s-butyl levulinate ( CAS 85734-01-6 ), penthyl levulinate ( CAS 20279-49-6 ) hexyl levulinate ( CAS 24431-34-3 ), octyl levulinate ( CAS 41780-57-8 ), 2-Methyl-4-oxovaleric acid ethyl ester ( CAS 4749-12-6 ), methyl-6-oxoheptanoate ( CAS 2046-21-1 ), methyl 4-oxohexanoate ( CAS 2955-62-6 ), methyl 5-oxohexanoate ( CAS 13984-50-4 ), methyl 3-methyl -5-oxohexanoate ( CAS 14983-18-7 ), 5-ketoenanthic acid methyl ester (17745-32-3), methyl 3-methyl-4-oxopentanoate ( CAS 25234-83-7 ), methyl 2-methyl-4 oxopentanoate ( CAS 32811-25-9 ), 4-Oxo-5-methylhexanoic acid methyl ester ( CAS 34553-37-2 ), pentanoic acid 2,3 dimethyl-4-oxo, methyl ester ( CAS 35140-52-4 ), hexanoic acid, 4-methyl-5-oxo, methyl ester ( CAS 36045-56-4 ), pentanoic acid 2-ethyl-4-oxo-methyl ester ( CAS 62359-06-2 ), methyl 3-methyl-4-oxohexanoate ( CAS 69448-35-7 ), hexanoic acid 2-methyl-5-oxo methyl ester ( CAS 38872-30-9 ), pentanoic acid 3-methyl-4-oxo ethyl ester ( CAS 55424-74-3 ), hexanoic acid 2-ethyl-4-oxo methyl ester ( CAS 75436-59-8 ), hexanoic acid, 2, 4-dimethyl-5-oxo methyl ester ( CAS 93176-58-0 ), pentanoic acid-4-oxo-2-propyl-methyl ester ( CAS 244196-06-3 ), hexanoic acid 2,5-dimethyl-4-oxo methyl ester ( CAS 1249353-11-4 ), octanoic acid 4 oxo-methyl ester ( CAS: 4316-48-7 ), heptanoic acid 2-methyl-6-oxo-methyl ester ( CAS 2570-90-3 ), heptanoic acid 3-methyl 6-oxo methyl ester ( CAS 5128-55-2 ), heptanoic acid 6-methyl-5-oxo methyl ester ( CAS 23575-33-9 ), hexanoic acid 3-methyl-5-oxo-ethyl ester ( CAS 38052-21-0 ), heptanoic acid 2-methyl-5-oxo methyl ester ( CAS 25912-38-3 ), heptanoic acid 4-methyl-6-oxo methyl ester ( CAS 41841-53-6 ), heptanoic acid 5-methyl-4-oxo methyl ester ( CAS 42511-74-0 ), heptanoic acid-4-methyl-5-oxo methyl ester ( CAS 54225-40-0 ), hexanoic acid 3,5-dimethyl-4-oxo methyl ester ( CAS 64712-02-3 ), heptanoic acid 6-methyl-4-oxo methyl ester ( CAS 76678-33-6 ), heptanoic acid, 2-methyl-4-oxo-methyl ester ( CAS 90647-21-5 ), hexanoic aicd, 4-ethyl-5-oxo methyl ester ( CAS 90647-24-8 ), heptanoic aid 3-methyl-5-oxo, methyl ester ( CAS 103252-99-9 ), hexanoic acid, 2-ethyl-5-oxo-, methyl ester ( CAS 103260-39-5 ), hexanoic acid 3 acetyl methyl ester ( CAS 1081559-93-4 ), heptanoic acid 5 methyl-6-oxo methyl ester ( CAS 344295-02-9 ), heptanoic acid 3-methyl-4-oxo methyl ester ( CAS 64712-01-2 ), methyl 2-(1methylethyl)-4-oxopentaoate ( CAS 99183-33-2 ), methyl 2,3-dimethyl-4-oxohexanoate ( CAS 86044-19-1 ), Ethyl 2 ethyl-4-oxopentanoate ( CAS 101514-30-1 ), hexanoic acid 5-oxo ethyl ester ( CAS 13984-57-1 ), ethyl 3 methyl-4-oxohexanoate ( CAS 42895-72-7 ), ethyl 2,3-dimethyl-4-oxopentanoate ( CAS 136964-44-8 ), hexanoic acid 4 oxo ethyl ester ( CAS 3249-33-0 ), heptanoic acid 6-oxo-ethyl ester ( CAS 30956-41-3 ), 1-methylethyl-4-oxohexanoate ( CAS 939422-07-8 ), pentanoic 2-ethyl-4-oxo-ethyl ester ( CAS 101514-30-1 ), hexanoic acid-2ethyl-5-methyl-4-oxo-methyl ester ( CAS 1195311-69-3 ).

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'oxo-ester seul ou en mélange est choisi dans le groupe des lévulinates comprenant : le lévulinate de méthyle ( CAS 624-45-3 ), le lévulinate d'éthyle ( CAS 539-88-8 ), le lévulinate de propyle (645-67-0), le lévulinate d'isopropyle ( CAS 21884-26-4 ), le lévulinate de butyle ( CAS 2052-15-5 ), le lévulinate d'isobutyle ( CAS 3757-32-2 ), le lévulinate de tert-butyle ( CAS 2854-10-6 ), le lévulinate de s-butyle ( CAS 85734-01-6 ), le lévulinate de penthyl ( CAS 20279-49-6 ) le lévulinate d'hexyle ( CAS 24431-34-3 ), le lévulinate d'octyl ( CAS 41780-57-8 ).In one embodiment, the process according to the invention is characterized in that the oxo-ester alone or as a mixture is chosen from the group of levulinates comprising: methyl levulinate ( CAS 624-45-3 ), ethyl levulinate ( CAS 539-88-8 ), propyl levulinate (645-67-0), isopropyl levulinate ( CAS 21884-26-4 ), butyl levulinate ( CAS 2052-15-5 ), isobutyl levulinate ( CAS 3757-32-2 ), tert-butyl levulinate ( CAS 2854-10-6 ), s-butyl levulinate ( CAS 85734-01-6 ), penthyl levulinate ( CAS 20279-49-6 ) hexyl levulinate ( CAS 24431-34-3 ), octyl levulinate ( CAS 41780-57-8 ).

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'oxo-ester seul ou en mélange est choisi dans le groupe comprenant : methyl 3-methyl-4-oxopentanoate ( CAS 25234-83-7 ), methyl 2-methyl-4 oxopentanoate ( CAS 32811-25-9 ), pentanoic acid 2,3 dimethyl-4-oxo, methyl ester ( CAS 35140-52-4 ), pentanoic acid 2-ethyl-4-oxo-methyl ester ( CAS 62359-06-2 ), pentanoic acid 3-methyl-4-oxo ethyl ester ( CAS 55424-74-3 ), pentanoic acid-4-oxo-2-propyl-methyl ester ( CAS 244196-06-3 ), methyl 2-(1methylethyl)-4-oxopentaoate ( CAS 99183-33-2 ), Ethyl 2 ethyl-4-oxopentanoate ( CAS 101514-30-1 ), ethyl 2,3-dimethyl-4-oxopentanoate ( CAS 136964-44-8 ), pentanoic 2-ethyl-4-oxo- ethyl ester ( CAS 101514-30-1 ).In one embodiment, the process according to the invention is characterized in that the oxo-ester alone or as a mixture is chosen from the group comprising: methyl 3-methyl-4-oxopentanoate ( CAS 25234-83-7 ), methyl 2-methyl-4 oxopentanoate ( CAS 32811-25-9 ), pentanoic acid 2,3 dimethyl-4-oxo, methyl ester ( CAS 35140-52-4 ), pentanoic acid 2-ethyl-4-oxo-methyl ester ( CAS 62359-06-2 ), pentanoic acid 3-methyl-4-oxo ethyl ester ( CAS 55424-74-3 ), pentanoic acid-4-oxo-2-propyl-methyl ester ( CAS 244196-06-3 ), methyl 2-(1methylethyl)-4-oxopentaoate ( CAS 99183-33-2 ), Ethyl 2 ethyl-4-oxopentanoate ( CAS 101514-30-1 ), ethyl 2,3-dimethyl-4-oxopentanoate ( CAS 136964-44-8 ), pentanoic 2-ethyl-4-oxo-ethyl ester ( CAS 101514-30-1 ).

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'oxo-ester seul ou en mélange est choisi dans le groupe comprenant : methyl 4-oxohexanoate ( CAS 2955-62-6 ), methyl 5-oxohexanoate ( CAS 13984-50-4 ), methyl 3-methyl -5-oxohexanoate ( CAS 14983-18-7 ), 4-Oxo-5-methylhexanoic acid methyl ester ( CAS 34553-37-2 ), hexanoic acid, 4-methyl-5-oxo, methyl ester ( CAS 36045-56-4 ), methyl 3-methyl-4-oxohexanoate ( CAS 69448-35-7 ), hexanoic acid 2-methyl-5-oxo methyl ester ( CAS 38872-30-9 ), hexanoic acid 2-ethyl-4-oxo methyl ester ( CAS 75436-59-8 ), hexanoic acid, 2, 4-dimethyl-5-oxo methyl ester ( CAS 93176-58-0 ), hexanoic acid 2,5-dimethyl-4-oxo methyl ester ( CAS 1249353-11-4 ), octanoic acid 4 oxo-methyl ester ( CAS : 4316-48-7 ), hexanoic acid 3-methyl-5-oxo- ethyl ester ( CAS 38052-21-0 ), hexanoic acid 3,5-dimethyl-4-oxo methyl ester ( CAS 64712-02-3 ), hexanoic aicd, 4-ethyl-5-oxo methyl ester ( CAS 90647-24-8 ), hexanoic acid, 2-ethyl-5-oxo-, methyl ester ( CAS 103260-39-5 ), hexanoic acid 3 acetyl methyl ester ( CAS 1081559-93-4 ), methyl 2,3-dimethyl-4-oxohexanoate ( CAS 86044-19-1 ), hexanoic acid 5-oxo ethyl ester ( CAS 13984-57-1 ), ethyl 3 methyl-4-oxohexanoate ( CAS 42895-72-7 ), hexanoic acid 4 oxo ethyl ester ( CAS 3249-33-0 ), 1-methylethyl-4-oxohexanoate ( CAS 939422-07-8 ), hexanoic acid-2ethyl-5-methyl-4-oxo- methyl ester ( CAS 1195311-69-3 ).In one embodiment, the process according to the invention is characterized in that the oxo-ester alone or as a mixture is chosen from the group comprising: methyl 4-oxohexanoate ( CAS 2955-62-6 ), methyl 5-oxohexanoate ( CAS 13984-50-4 ), methyl 3-methyl -5-oxohexanoate ( CAS 14983-18-7 ), 4-Oxo-5-methylhexanoic acid methyl ester ( CAS 34553-37-2 ), hexanoic acid, 4-methyl-5-oxo, methyl ester ( CAS 36045-56-4 ), methyl 3-methyl-4-oxohexanoate ( CAS 69448-35-7 ), hexanoic acid 2-methyl-5-oxo methyl ester ( CAS 38872-30-9 ), hexanoic acid 2-ethyl-4-oxo methyl ester ( CAS 75436-59-8 ), hexanoic acid, 2, 4-dimethyl-5-oxo methyl ester ( CAS 93176-58-0 ), hexanoic acid 2,5-dimethyl-4-oxo methyl ester ( CAS 1249353-11-4 ), octanoic acid 4 oxo-methyl ester ( CAS: 4316-48-7 ), hexanoic acid 3-methyl-5-oxo-ethyl ester ( CAS 38052-21-0 ), hexanoic acid 3,5-dimethyl-4-oxo methyl ester ( CAS 64712-02-3 ), hexanoic aicd, 4-ethyl-5-oxo methyl ester ( CAS 90647-24-8 ), hexanoic acid, 2-ethyl-5-oxo-, methyl ester ( CAS 103260-39-5 ), hexanoic acid 3 acetyl methyl ester ( CAS 1081559-93-4 ), methyl 2,3-dimethyl-4-oxohexanoate ( CAS 86044-19-1 ), hexanoic acid 5-oxo ethyl ester ( CAS 13984-57-1 ), ethyl 3 methyl-4-oxohexanoate ( CAS 42895-72-7 ), hexanoic acid 4 oxo ethyl ester ( CAS 3249-33-0 ), 1-methylethyl-4-oxohexanoate ( CAS 939422-07-8 ), hexanoic acid-2ethyl-5-methyl-4-oxo-methyl ester ( CAS 1195311-69-3 ).

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'oxo-ester seul ou en mélange est choisi dans le groupe comprenant : 2-Methyl-4-oxovaleric acid ethyl ester ( CAS 4749-12-6 ), methyl-6-oxoheptanoate ( CAS 2046-21-1 ), 5-ketoenanthic acid methyl ester (17745-32-3), octanoic acid 4 oxo-methyl ester ( CAS : 4316-48-7 ), heptanoic acid 2-methyl-6-oxo-methyl ester ( CAS 2570-90-3 ), heptanoic acid 3-methyl 6-oxo methyl ester ( CAS 5128-55-2 ), heptanoic acid 6-methyl-5-oxo methyl ester ( CAS 23575-33-9 ), heptanoic acid 2-methyl-5-oxo methyl ester ( CAS 25912-38-3 ), heptanoic acid 4 methyl-6-oxo methyl ester ( CAS 41841-53-6 ), heptanoic acid 5 methyl-4-oxo methyl ester ( CAS 42511-74-0 ), heptanoic acid-4-methyl-5-oxo methyl ester ( CAS 54225-40-0 ), heptanoic acid 6-methyl-4-oxo methyl ester ( CAS 76678-33-6 ), heptanoic acid, 2-methyl-4-oxo- methyl ester ( CAS 90647-21-5 ), heptanoic aid 3-methyl-5-oxo, methyl ester ( CAS 103252-99-9 ), heptanoic acid 5 methyl-6-oxo methyl ester ( CAS 344295-02-9 ), heptanoic acid 3-methyl-4-oxo methyl ester ( CAS 64712-01-2 ), heptanoic acid 6-oxo-ethyl ester ( CAS 30956-41-3 ).In one embodiment, the process according to the invention is characterized in that the oxo-ester alone or as a mixture is chosen from the group comprising: 2-Methyl-4-oxovaleric acid ethyl ester ( CAS 4749-12-6 ), methyl-6-oxoheptanoate ( CAS 2046-21-1 ), 5-ketoenanthic acid methyl ester (17745-32-3), octanoic acid 4 oxo-methyl ester ( CAS: 4316-48-7 ), heptanoic acid 2-methyl-6-oxo-methyl ester ( CAS 2570-90-3 ), heptanoic acid 3-methyl 6-oxo methyl ester ( CAS 5128-55-2 ), heptanoic acid 6-methyl-5-oxo methyl ester ( CAS 23575-33-9 ), heptanoic acid 2-methyl-5-oxo methyl ester ( CAS 25912-38-3 ), heptanoic acid 4-methyl-6-oxo methyl ester ( CAS 41841-53-6 ), heptanoic acid 5-methyl-4-oxo methyl ester ( CAS 42511-74-0 ), heptanoic acid-4-methyl-5-oxo methyl ester ( CAS 54225-40-0 ), heptanoic acid 6-methyl-4-oxo methyl ester ( CAS 76678-33-6 ), heptanoic acid, 2-methyl-4-oxo-methyl ester ( CAS 90647-21-5 ), heptanoic aid 3-methyl-5-oxo, methyl ester ( CAS 103252-99-9 ), heptanoic acid 5 methyl-6-oxo methyl ester ( CAS 344295-02-9 ), heptanoic acid 3-methyl-4-oxo methyl ester ( CAS 64712-01-2 ), heptanoic acid 6-oxo-ethyl ester ( CAS 30956-41-3 ).

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'oxo-ester a une masse moléculaire inférieure ou égale à 200g/mol.In one embodiment, the process according to the invention is characterized in that the oxo-ester has a molecular mass less than or equal to 200 g/mol.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'oxo-ester a une masse moléculaire inférieure ou égale à 180 g/mol.In one embodiment, the process according to the invention is characterized in that the oxo-ester has a molecular mass less than or equal to 180 g/mol.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'oxo-ester a une masse moléculaire inférieure ou égale à 160 g/mol.In one embodiment, the process according to the invention is characterized in that the oxo-ester has a molecular mass less than or equal to 160 g/mol.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'oxo-ester a une masse moléculaire inférieure ou égale à 150 g/mol.In one embodiment, the process according to the invention is characterized in that the oxo-ester has a molecular mass less than or equal to 150 g/mol.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'oxo-ester est le lévulinate de méthyle.In one embodiment, the method according to the invention is characterized in that the oxo-ester is methyl levulinate.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'oxo-ester est le lévulinate de butyle.In one embodiment, the method according to the invention is characterized in that the oxo-ester is butyl levulinate.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'oxo-ester est le lévulinate d'éthyle.In one embodiment, the method according to the invention is characterized in that the oxo-ester is ethyl levulinate.

Dans la présente demande un « alcane » est un hydrocarbure saturé étant constitué uniquement d'atomes de carbone et d'hydrogènes liés entre eux par des liaisons covalentes simples dont la formule générale est CnH2n+2, il est appelé « alcane linéaire » lorsque chaque atome de carbone est lié au maximum à deux atomes de carbone et « alcane ramifié » lorsque certains atomes de carbone sont liés à trois atomes, voire quatre atomes de carbones.In the present application, an “alkane” is a saturated hydrocarbon consisting solely of carbon and hydrogen atoms linked together by single covalent bonds, the general formula of which is C n H 2n+2 , it is called “linear alkane when each carbon atom is bonded to a maximum of two carbon atoms and “branched alkane” when certain carbon atoms are bonded to three or even four carbon atoms.

Dans la présente demande un « bioalcane » est un alcane biosourcé.In the present application, a “bioalkane” is a biobased alkane.

Dans la présente demande, on qualifie de biosourcé un composé ou une composition organique dont le carbone organique présent dans le composé ou la composition est d'origine végétale par une analyse au radiocarbone selon l'une des normes suivantes ASTM D6866, EN 16640 ou EN 16785-1.In the present application, a biobased compound or an organic composition in which the organic carbon present in the compound or composition is of plant origin is described as biobased by radiocarbon analysis according to one of the following standards ASTM D6866, EN 16640 or EN 16785-1.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend en outre au moins un alcaneIn one embodiment, the method according to the invention is characterized in that the solvent system further comprises at least one alkane

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend en outre au moins un alcane volatilIn one embodiment, the method according to the invention is characterized in that the solvent system further comprises at least one volatile alkane

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'alcane volatil est choisi dans le groupe comprenant les alcanes linéaires et/ou ramifiés comprenant de 10 à 12 atomes de carbones, seuls ou en mélanges.In one embodiment, the process according to the invention is characterized in that the volatile alkane is chosen from the group comprising linear and/or branched alkanes comprising from 10 to 12 carbon atoms, alone or in mixtures.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'alcane volatil est choisi dans le groupe comprenant les bioalcanes linéaires et/ou ramifiés comprenant de 10 à 12 atomes de carbones, seuls ou en mélanges.In one embodiment, the process according to the invention is characterized in that the volatile alkane is chosen from the group comprising linear and/or branched bioalkanes comprising from 10 to 12 carbon atoms, alone or in mixtures.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend en outre un décane.In one embodiment, the method according to the invention is characterized in that the solvent system further comprises a decane.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend en outre un dodécane.In one embodiment, the method according to the invention is characterized in that the solvent system further comprises a dodecane.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend en outre un décane, un dodécaneIn one embodiment, the method according to the invention is characterized in that the solvent system further comprises a decane, a dodecane

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend en outre un alcane ramifié de 10 atomes de carbones.In one embodiment, the process according to the invention is characterized in that the solvent system further comprises a branched alkane of 10 carbon atoms.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'alcane ramifié de 10 atomes de carbone est choisi dans le groupe comprenant :le 2-méthylnonane ( CAS 871-83-0 ), le 4-methylnonane ( CAS 17301-94-9 ), le 3-méthyl nonane ( CAS 5911-04-6 ), le 3-éthyloctane ( CAS 5881-17-4 ), le 2,2-diméthyloctane ( CAS 15869-87-1 ), le 2,3 dimethyl octane ( CAS 7146-60-3 ), le 2,5- diméthyl octane ( CAS 15869-89-3 ), le 3,5 diméthyl octane ( CAS 15869-93-9 ), le 4-propylheptane ( CAS 3178-29-8 ), le 3-éthyl-2-méthylheptane ( CAS 14676-29-0 ), le 2,2,3-triméthylheptane ( CAS 52896-92-1 ), le 2,3,5 trimethylheptane ( CAS 20278-85-7 ), le 2,3,6-trimethylheptane ( CAS 4032-93-3 ), le 3,3,4-triméthylheptane ( CAS 20278-87-9 ), le 2,3,4 triméthylheptane ( CAS 52896-95-4 ), le 2,2,4 triméthylheptane ( CAS : 14720-74-2 ) le 3,3-diéthylhexane ( CAS 17302-02-2 ), le 2,2,3,3-tétraméthylhexane ( CAS 13475-81-5 ), le 3-éthyl-2,2,3-triméthylpentane ( CAS 52897-17-3 ), et leurs mélanges.In one embodiment, the process according to the invention is characterized in that the branched alkane of 10 carbon atoms is chosen from the group comprising: 2-methylnonane ( CAS 871-83-0 ), 4-methylnonane ( CAS 17301-94-9 ), 3-methyl nonane ( CAS 5911-04-6 ), 3-ethyl octane ( CAS 5881-17-4 ), 2,2-dimethyloctane ( CAS 15869-87-1 ), 2,3 dimethyl octane ( CAS 7146-60-3 ), 2,5-dimethyl octane ( CAS 15869-89-3 ), 3,5 dimethyl octane ( CAS 15869-93-9 ), 4-propylheptane ( CAS 3178-29-8 ), 3-ethyl-2-methylheptane ( CAS 14676-29-0 ), 2,2,3-trimethylheptane ( CAS 52896-92-1 ), 2,3,5 trimethylheptane ( CAS 20278-85-7 ), 2,3,6-trimethylheptane ( CAS 4032-93-3 ), 3,3,4-trimethylheptane ( CAS 20278-87-9 ), 2,3,4 trimethylheptane ( CAS 52896-95-4 ), 2,2,4 trimethylheptane ( CAS: 14720-74-2 ) 3,3-diethylhexane ( CAS 17302-02-2 ), 2,2,3,3-tetramethylhexane ( CAS 13475-81-5 ), 3-ethyl-2,2,3-trimethylpentane ( CAS 52897-17-3 ), and mixtures thereof.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend en outre un alcane ramifié de 12 atomes de carbones.In one embodiment, the process according to the invention is characterized in that the solvent system further comprises a branched alkane of 12 carbon atoms.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'alcane ramifié de 12 atomes de carbone est choisi dans le groupe comprenant : 2-méthylundécane ( CAS 7045-71-8 ), 3-méthylundécane ( CAS 1002-43-3 ), 4-méthylundécane ( CAS 2980-69-0 ), 5-méthylundécane ( CAS 1632-70-8 ), 6-méthylundécane ( CAS 17302-33-9 ), 2,4-diméthyldécane ( CAS 2801-84-5 ) 4,4-diméthyldécane ( CAS 17312-39-9 ), 3,5-diméthyldécane ( CAS 17312-48-0 ), 2,5-diméthyldécane ( CAS 17312-50-4 ), 2,3-diméthyldécane ( CAS 17312-44-6 ), 3,3-dimethyldecane ( CAS 17302-38-4 ), 3,7-dimethyldécane ( CAS 17312-54-8 ), 3,4,6-triméthylnonane ( CAS 62184-24-1 ) 3,5,6-triméthylnonane ( CAS 62184-26-3 ), 3,5,7-triméthylnonane ( CAS 62184-27-4 ), 2,5,7-triméthylnonane ( CAS 62184-14-9 ), 2,5,6-triméthylnonane ( CAS 62184-13-8 ), 2,5,7-triméthylnonane ( CAS 62184-14-9 ), 2,5,8-triméthylnonane ( CAS 49557-09-7 ), 3,3,4,5-tétraméthyloctane ( CAS 62185-21-1 ), 2,3,4,5-tétraméthyloctane ( CAS 62199-27-3 ), 2,2,4,5-tétraméthyloctane ( CAS 62183-80-6 ), 2,2,5,7-tétraméthyloctane ( CAS 62199-19-3 ), 2,3,4,7-tétraméthyloctane ( CAS 62199-29-5 ), 2,4,4,7-tétraméthyloctane ( CAS 35866-96-7 ), 3-éthyl-4-méthylnonane ( CAS 62184-45-6 ), 3-éthyl-4,5-diméthyloctane ( CAS 62183-72-6 ), 2,5-diméthyl-6-éthyloctane ( CAS 62183-50-0 ), et leurs mélanges.In one embodiment, the process according to the invention is characterized in that the branched alkane with 12 carbon atoms is chosen from the group comprising: 2-methylundecane ( CAS 7045-71-8 ), 3-methylundecane ( CAS 1002-43-3 ), 4-methylundecane ( CAS 2980-69-0 ), 5-methylundecane ( CAS 1632-70-8 ), 6-methylundecane ( CAS 17302-33-9 ), 2,4-dimethyldecane ( CAS 2801-84-5 ) 4,4-dimethyldecane ( CAS 17312-39-9 ), 3,5-dimethyldecane ( CAS 17312-48-0 ), 2,5-dimethyldecane ( CAS 17312-50-4 ), 2,3-dimethyldecane ( CAS 17312-44-6 ), 3,3-dimethyldecane ( CAS 17302-38-4 ), 3,7-dimethyldecane ( CAS 17312-54-8 ), 3,4,6-trimethylnonane ( CAS 62184-24-1 ) 3,5,6-trimethylnonane ( CAS 62184-26-3 ), 3,5,7-trimethylnonane ( CAS 62184-27-4 ), 2,5,7-trimethylnonane ( CAS 62184-14-9 ), 2,5,6-trimethylnonane ( CAS 62184-13-8 ), 2,5,7-trimethylnonane ( CAS 62184-14-9 ), 2,5,8-trimethylnonane ( CAS 49557-09-7 ), 3,3,4,5-tetramethyloctane ( CAS 62185-21-1 ), 2,3,4,5-tetramethyloctane ( CAS 62199-27-3 ), 2,2,4,5-tetramethyloctane ( CAS 62183-80-6 ), 2,2,5,7-tetramethyloctane ( CAS 62199-19-3 ), 2,3,4,7-tetramethyloctane ( CAS 62199-29-5 ), 2,4,4,7-tetramethyloctane ( CAS 35866-96-7 ), 3-ethyl-4-methylnonane ( CAS 62184-45-6 ), 3-ethyl-4,5-dimethyloctane ( CAS 62183-72-6 ), 2,5-dimethyl-6-ethyloctane ( CAS 62183-50-0 ), and mixtures thereof.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend au moins un alcane volatil et un lévulinate d'éthyle.In one embodiment, the method according to the invention is characterized in that the solvent system comprises at least one volatile alkane and one ethyl levulinate.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend un décane et un lévulinate d'éthyle.In one embodiment, the process according to the invention is characterized in that the solvent system comprises a decane and an ethyl levulinate.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend un dodécane et un lévulinate d'éthyle.In one embodiment, the method according to the invention is characterized in that the solvent system comprises a dodecane and an ethyl levulinate.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend un décane, un dodécane et un lévulinate d'éthyle.In one embodiment, the process according to the invention is characterized in that the solvent system comprises a decane, a dodecane and an ethyl levulinate.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend un alcane ramifié de 10 atomes de carbones et un lévulinate d'éthyle.In one embodiment, the method according to the invention is characterized in that the solvent system comprises a branched alkane of 10 carbon atoms and an ethyl levulinate.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend un alcane ramifié de 12 atomes de carbones et un lévulinate d'éthyle.In one embodiment, the method according to the invention is characterized in that the solvent system comprises a branched alkane of 12 carbon atoms and an ethyl levulinate.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend au moins un alcane volatil et un lévulinate de butyle.In one embodiment, the method according to the invention is characterized in that the solvent system comprises at least one volatile alkane and one butyl levulinate.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend un décane et un lévulinate de butyle.In one embodiment, the method according to the invention is characterized in that the solvent system comprises a decane and a butyl levulinate.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend un dodécane et un lévulinate de butyle.In one embodiment, the process according to the invention is characterized in that the solvent system comprises a dodecane and a butyl levulinate.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend un décane, un dodécane et un lévulinate de butyle.In one embodiment, the process according to the invention is characterized in that the solvent system comprises a decane, a dodecane and a butyl levulinate.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend un alcane ramifié de 10 atomes de carbones et un lévulinate de butyle.In one embodiment, the process according to the invention is characterized in that the solvent system comprises a branched alkane of 10 carbon atoms and a butyl levulinate.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend un alcane ramifié de 12 atomes de carbones et un lévulinate de butyle.In one embodiment, the process according to the invention is characterized in that the solvent system comprises a branched alkane of 12 carbon atoms and a butyl levulinate.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant est un mélange de solvant comprend en outre un lactate d'éthyleIn one embodiment, the method according to the invention is characterized in that the solvent system is a solvent mixture further comprising an ethyl lactate

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend un lactate d'éthyle et un lévulinate de butyle.In one embodiment, the method according to the invention is characterized in that the solvent system comprises an ethyl lactate and a butyl levulinate.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend un lactate d'éthyle et un lévulinate d'éthyle.In one embodiment, the method according to the invention is characterized in that the solvent system comprises an ethyl lactate and an ethyl levulinate.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le ratio volumique X défini par la relation : X = Volume de l oxo ester Volume des autres composés du système de solvant

Figure imgb0007
est d'au moins 1/3.In one embodiment, the method according to the invention is characterized in that the volume ratio X defined by the relationship: X = Volume of the oxo ester Volume of other solvent system compounds
Figure imgb0007
is at least 1/3.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le ratio volumique X est d'au moins 1/1.In one embodiment, the method according to the invention is characterized in that the volume ratio X is at least 1/1.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le ratio volumique X est d'au moins 2/1.In one embodiment, the method according to the invention is characterized in that the volume ratio X is at least 2/1.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le ratio volumique X est compris entre 2/1 et 100/1.In one embodiment, the method according to the invention is characterized in that the volume ratio X is between 2/1 and 100/1.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le ratio volumique X est compris entre 2/1 et 50/1.In one embodiment, the method according to the invention is characterized in that the volume ratio X is between 2/1 and 50/1.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le ratio volumique X est compris entre 2/1 et 20/1.In one embodiment, the method according to the invention is characterized in that the volume ratio X is between 2/1 and 20/1.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le ratio volumique X est compris entre 2/1 et 10/1.In one embodiment, the method according to the invention is characterized in that the volume ratio X is between 2/1 and 10/1.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le ratio volumique X est 1/1.In one embodiment, the process according to the invention is characterized in that the volume ratio X is 1/1.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le ratio volumique X est 2/1.In one embodiment, the method according to the invention is characterized in that the volume ratio X is 2/1.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le ratio volumique X est 3/1.In one embodiment, the method according to the invention is characterized in that the volume ratio X is 3/1.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le ratio volumique X est 5/1.In one embodiment, the method according to the invention is characterized in that the volume ratio X is 5/1.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le ratio volumique X est 10/1.In one embodiment, the method according to the invention is characterized in that the volume ratio X is 10/1.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le ratio volumique X est 25/1.In one embodiment, the method according to the invention is characterized in that the volume ratio X is 25/1.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le ratio volumique X est 50/1.In one embodiment, the process according to the invention is characterized in that the volume ratio X is 50/1.

Dans la présente demande, on entend par teneur en solvant le rapport du volume d'un solvant par rapport au volume total d'un mélange de solvant, ramené à un pourcentage.In the present application, solvent content is understood to mean the ratio of the volume of a solvent relative to the total volume of a solvent mixture, reduced to a percentage.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend une teneur en oxo-ester d'au moins 25%, par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent system comprises an oxo-ester content of at least 25%, relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend une teneur en oxo-ester d'au moins 50%, par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent system comprises an oxo-ester content of at least 50%, relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend une teneur en oxo-ester comprise entre 70 et 100% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent system comprises an oxo-ester content of between 70 and 100% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend une teneur en oxo-ester comprise entre 80 et 100% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent system comprises an oxo-ester content of between 80 and 100% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend une teneur en lévulinate de méthyle d'au moins 25% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent system comprises a methyl levulinate content of at least 25% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend une teneur en lévulinate de méthyle d'au moins 50% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent system comprises a methyl levulinate content of at least 50% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend une teneur en lévulinate de méthyle comprise entre 70 et 100% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent system comprises a methyl levulinate content of between 70 and 100% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend une teneur en lévulinate de méthyle comprise entre 80 et 100% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent system comprises a methyl levulinate content of between 80 and 100% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend une teneur en lévulinate d'éthyle d'au moins 25% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent system comprises an ethyl levulinate content of at least 25% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend une teneur en lévulinate d'éthyle d'au moins 50% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent system comprises an ethyl levulinate content of at least 50% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend une teneur en lévulinate d'éthyle comprise entre 70 et 100% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent system comprises an ethyl levulinate content of between 70 and 100% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend une teneur en lévulinate d'éthyle comprise entre 80 et 100% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent system comprises an ethyl levulinate content of between 80 and 100% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend une teneur en lévulinate de butyle d'au moins 25% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent system comprises a butyl levulinate content of at least 25% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend une teneur en lévulinate de butyle d'au moins 50% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent system comprises a butyl levulinate content of at least 50% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend une teneur en lévulinate de butyle comprise entre 70 et 100% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent system comprises a butyl levulinate content of between 70 and 100% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le système de solvant comprend une teneur en lévulinate de butyle comprise entre 80 et 100% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent system comprises a butyl levulinate content of between 80 and 100% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange de solvant comprend une teneur en alcane volatil, d'au moins 1% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent mixture comprises a volatile alkane content of at least 1% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange de solvant comprend une teneur en alcane volatil, d'au moins 5% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent mixture comprises a volatile alkane content of at least 5% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange de solvant comprend une teneur en alcane volatil, comprise entre 1 et 50% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent mixture comprises a volatile alkane content of between 1 and 50% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange de solvant comprend une teneur en alcane volatil, comprise entre 5 et 30% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent mixture comprises a volatile alkane content of between 5 and 30% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange de solvant comprend une teneur en décane, d'au moins 1% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent mixture comprises a decane content of at least 1% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange de solvant comprend une teneur en décane, d'au moins 5% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent mixture comprises a decane content of at least 5% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange de solvant comprend une teneur en décane, comprise entre 1 et 50% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent mixture comprises a decane content of between 1 and 50% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange de solvant comprend une teneur en décane, comprise entre 5 et 30% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent mixture comprises a decane content of between 5 and 30% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange de solvant comprend une teneur en dodécane, d'au moins 1% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent mixture comprises a dodecane content of at least 1% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange de solvant comprend une teneur en dodécane, d'au moins 5% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent mixture comprises a dodecane content of at least 5% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange de solvant comprend une teneur en dodécane, comprise entre 1 et 50% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent mixture comprises a dodecane content of between 1 and 50% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange de solvant comprend une teneur en dodécane, comprise entre 5 et 30% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent mixture comprises a dodecane content of between 5 and 30% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange de solvant comprend une teneur en alcanes ramifiés de 10 atomes de carbones, d'au moins 1% par rapport au volume total du système de solvant.In one embodiment, the process according to the invention is characterized in that the solvent mixture comprises a content of branched alkanes with 10 carbon atoms, of at least 1% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange de solvant comprend une teneur en alcanes ramifiés de 10 atomes de carbones, d'au moins 5% par rapport au volume total du système de solvant.In one embodiment, the process according to the invention is characterized in that the solvent mixture comprises a content of branched alkanes with 10 carbon atoms, of at least 5% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange de solvant comprend une teneur en alcanes ramifiés de 10 atomes de carbones, comprise entre 1 et 50% par rapport au volume total du système de solvant.In one embodiment, the process according to the invention is characterized in that the solvent mixture comprises a content of branched alkanes of 10 carbon atoms, comprised between 1 and 50% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange de solvant comprend une teneur en en alcanes ramifiés de 10 atomes de carbones, comprise entre 5 et 30% par rapport au volume total du système de solvant.In one embodiment, the process according to the invention is characterized in that the solvent mixture comprises a content of branched alkanes with 10 carbon atoms, of between 5 and 30% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange de solvant comprend une teneur en alcanes ramifiés de 12 atomes de carbones, d'au moins 1% par rapport au volume total du système de solvant.In one embodiment, the process according to the invention is characterized in that the solvent mixture comprises a content of branched alkanes with 12 carbon atoms, of at least 1% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange de solvant comprend une teneur en alcanes ramifiés de 12 atomes de carbones, d'au moins 5% par rapport au volume total du système de solvant.In one embodiment, the process according to the invention is characterized in that the solvent mixture comprises a content of branched alkanes of 12 carbon atoms, of at least 5% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange de solvant comprend une teneur en alcanes ramifiés de 12 atomes de carbones, comprise entre 1 et 50% par rapport au volume total du système de solvant.In one embodiment, the process according to the invention is characterized in that the solvent mixture comprises a content of branched alkanes of 12 carbon atoms, comprised between 1 and 50% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange de solvant comprend une teneur en en alcanes ramifiés de 12 atomes de carbones, comprise entre 5 et 30% par rapport au volume total du système de solvant.In one embodiment, the process according to the invention is characterized in that the solvent mixture comprises a content of branched alkanes with 12 carbon atoms, of between 5 and 30% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange de solvant comprend une teneur en lactate d'éthyle d'au moins 1% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent mixture comprises an ethyl lactate content of at least 1% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange de solvant comprend une teneur en lactate d'éthyle d'au moins 5% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent mixture comprises an ethyl lactate content of at least 5% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange de solvant comprend une teneur en lactate d'éthyle comprise entre 1 et 50% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent mixture comprises an ethyl lactate content of between 1 and 50% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange de solvant comprend une teneur en lactate d'éthyle comprise entre 30 et 50% par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the solvent mixture comprises an ethyl lactate content of between 30 and 50% relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange et l'homogénéisation du beurre de karité est réalisé à une température d'au moins 20°C.In one embodiment, the method according to the invention is characterized in that the mixing and the homogenization of the shea butter is carried out at a temperature of at least 20°C.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange et l'homogénéisation du beurre de karité est réalisé à une température comprise entre 20 et 80°C.In one embodiment, the method according to the invention is characterized in that the mixing and homogenization of the shea butter is carried out at a temperature of between 20 and 80°C.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange et l'homogénéisation du beurre de karité est réalisé à une température comprise entre 35 et 55°C.In one embodiment, the method according to the invention is characterized in that the mixing and homogenization of the shea butter is carried out at a temperature of between 35 and 55°C.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le mélange et l'homogénéisation du beurre de karité est réalisé à une température de 40°CIn one embodiment, the method according to the invention is characterized in that the mixing and homogenization of the shea butter is carried out at a temperature of 40°C

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le refroidissement du mélange réactionnel est réalisé à une température inférieure à 20°C.In one embodiment, the process according to the invention is characterized in that the cooling of the reaction mixture is carried out at a temperature below 20°C.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le refroidissement du mélange réactionnel est réalisé à une température comprise entre -10 et 20°C.In one embodiment, the process according to the invention is characterized in that the cooling of the reaction mixture is carried out at a temperature comprised between -10 and 20°C.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le refroidissement du mélange réactionnel est réalisé à une température comprise entre 5 et 10°C.In one embodiment, the process according to the invention is characterized in that the cooling of the reaction mixture is carried out at a temperature comprised between 5 and 10°C.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le refroidissement du mélange réactionnel est réalisé à une température égale à 4°C.In one embodiment, the process according to the invention is characterized in that the cooling of the reaction mixture is carried out at a temperature equal to 4°C.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le refroidissement du mélange réactionnel est réalisé pendant une durée d'au moins 12h.In one embodiment, the method according to the invention is characterized in that the cooling of the reaction mixture is carried out for a period of at least 12 hours.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que le refroidissement du mélange réactionnel est réalisé pendant une durée préférentielle de 24h.In one embodiment, the method according to the invention is characterized in that the cooling of the reaction mixture is carried out for a preferential duration of 24 hours.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la filtration du mélange réactionnel est réalisé à l'aide d'un filtre choisi parmi le groupe : d'un filtre monoplaque, d'un filtre presse, d'un filtre rotatif ou d'un filtre à bougie.In one embodiment, the method according to the invention is characterized in that the filtration of the reaction mixture is carried out using a filter chosen from the group: a monoplate filter, a filter press, a rotary filter or a candle filter.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'élimination du système de solvant comprend au moins une étape de concentration par évaporation du mélange réactionnel.In one embodiment, the method according to the invention is characterized in that the elimination of the solvent system comprises at least one step of concentration by evaporation of the reaction mixture.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'élimination du système de solvant comprend en outre au moins une étape de lavage à l'eau.In one embodiment, the method according to the invention is characterized in that the removal of the solvent system further comprises at least one step of washing with water.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la concentration par évaporation du mélange réactionnel permet d'éliminer au moins 98% du système de solvant par rapport au volume total du système de solvant.In one embodiment, the process according to the invention is characterized in that the concentration by evaporation of the reaction mixture makes it possible to eliminate at least 98% of the solvent system relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la concentration par évaporation du mélange réactionnel permet d'éliminer au moins 99,5% du système de solvant par rapport au volume total du système de solvant.In one embodiment, the process according to the invention is characterized in that the concentration by evaporation of the reaction mixture makes it possible to eliminate at least 99.5% of the solvent system relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'au moins une étape de lavage à l'eau est réalisée à une température d'au moins 20°C.In one embodiment, the method according to the invention is characterized in that the at least one step of washing with water is carried out at a temperature of at least 20°C.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'au moins une étape de lavage à l'eau est réalisée à une température d'au moins 40°C.In one embodiment, the method according to the invention is characterized in that the at least one step of washing with water is carried out at a temperature of at least 40°C.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'au moins une étape de lavage à l'eau est réalisée à une température comprise entre 40 et 80°C.In one embodiment, the method according to the invention is characterized in that the at least one step of washing with water is carried out at a temperature of between 40 and 80°C.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'au moins une étape de lavage à l'eau est réalisée à une température de 40°C.In one embodiment, the method according to the invention is characterized in that the at least one step of washing with water is carried out at a temperature of 40°C.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'au moins une étape de lavage à l'eau est réalisée à une température de 60°C.In one embodiment, the method according to the invention is characterized in that the at least one step of washing with water is carried out at a temperature of 60°C.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'au moins une étape de lavage à l'eau est réalisée avec un pourcentage massique d'eau inférieur ou égal à 10% par rapport à la masse totale de produit fractionné.In one embodiment, the method according to the invention is characterized in that the at least one step of washing with water is carried out with a mass percentage of water less than or equal to 10% relative to the total mass of split product.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'au moins une étape de lavage à l'eau est réalisée avec un pourcentage massique d'eau inférieur ou égal à 5% par rapport à la masse totale de produit fractionné.In one embodiment, the method according to the invention is characterized in that the at least one step of washing with water is carried out with a mass percentage of water less than or equal to 5% relative to the total mass. of split product.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'au moins une étape de lavage à l'eau est réalisée avec un pourcentage massique d'eau égal à 10% par rapport à la masse totale de produit fractionné.In one embodiment, the method according to the invention is characterized in that the at least one step of washing with water is carried out with a mass percentage of water equal to 10% relative to the total mass of product split.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'au moins une étape de lavage à l'eau est réalisée avec un pourcentage massique d'eau égal à 5% par rapport à la masse totale de produit fractionné.In one embodiment, the method according to the invention is characterized in that the at least one step of washing with water is carried out with a mass percentage of water equal to 5% relative to the total mass of product split.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'élimination du système de solvant permet d'éliminer au moins 99,5% du système de solvant par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the elimination of the solvent system makes it possible to eliminate at least 99.5% of the solvent system relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que l'élimination du système de solvant permet d'éliminer au moins 99,9% du système de solvant par rapport au volume total du système de solvant.In one embodiment, the method according to the invention is characterized in that the elimination of the solvent system makes it possible to eliminate at least 99.9% of the solvent system relative to the total volume of the solvent system.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction d'oléine de karité est une fraction liquide qui comprend les acides gras suivants : l'acide palmitique, l'acide stéarique, l'acide oléique, l'acide linoléique et l'acide arachidique.In one embodiment, the process according to the invention is characterized in that the shea olein fraction is a liquid fraction which comprises the following fatty acids: palmitic acid, stearic acid, oleic acid, linoleic acid and arachidic acid.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction d'oléine de karité est une fraction liquide limpide.In one embodiment, the process according to the invention is characterized in that the shea olein fraction is a clear liquid fraction.

Au sens de la présente invention, la limpidité d'un fluide peut être évaluée par la mesure de sa turbidité. Pour information, la turbidité est définie comme étant la réduction de la transparence d'un liquide due à la présence de matières non dissoutes (NF EN ISO 7027). En d'autres termes, elle correspond à la propriété de l'échantillon de diffuser et d'absorber la lumière incidente.Within the meaning of the present invention, the clarity of a fluid can be evaluated by measuring its turbidity. For information, turbidity is defined as being the reduction in the transparency of a liquid due to the presence of undissolved matter (NF EN ISO 7027). In other words, it corresponds to the property of the sample to scatter and absorb incident light.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction d'oléine comprend un pourcentage massique en acide palmitique d'au plus 10% par rapport à la masse totale d'acide gras de la fraction d'oléine de karité.In one embodiment, the process according to the invention is characterized in that the olein fraction comprises a mass percentage of palmitic acid of at most 10% relative to the total mass of fatty acid of the fraction of shea olein.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction d'oléine de karité comprend un pourcentage massique en acide palmitique d'au plus 5% par rapport à la masse totale d'acide gras de la fraction d'oléine de karité.In one embodiment, the process according to the invention is characterized in that the shea olein fraction comprises a mass percentage of palmitic acid of at most 5% relative to the total mass of fatty acid of the fraction of shea olein.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction d'oléine comprend un pourcentage massique en acide palmitique d'au plus 4% par rapport à la masse totale d'acide gras de la fraction d'oléine de karité.In one embodiment, the process according to the invention is characterized in that the olein fraction comprises a mass percentage of palmitic acid of at most 4% relative to the total mass of fatty acid of the fraction of shea olein.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction d'oléine de karité comprend un pourcentage massique en acide oléique d'au moins 45% par rapport à la masse totale d'acide gras de la fraction d'oléine de karité.In one embodiment, the method according to the invention is characterized in that the shea olein fraction comprises a mass percentage of oleic acid of at least 45% relative to the total mass of fatty acid of the fraction of shea olein.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction d'oléine comprend un pourcentage massique en acide oléique d'au moins 50% par rapport à la masse totale d'acide gras de la fraction d'oléine de karité.In one embodiment, the process according to the invention is characterized in that the olein fraction comprises a mass percentage of oleic acid of at least 50% relative to the total mass of fatty acid of the fraction of shea olein.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction d'oléine comprend un pourcentage massique en acide oléique compris entre 50 et 75% par rapport à la masse totale d'acide gras de la fraction d'oléine de karité.In one embodiment, the process according to the invention is characterized in that the olein fraction comprises a mass percentage of oleic acid of between 50 and 75% relative to the total mass of fatty acid of the fraction of shea olein.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction d'oléine comprend un pourcentage massique en acide stéarique d'au plus 35% par rapport à la masse totale d'acide gras de la fraction d'oléine de karité.In one embodiment, the process according to the invention is characterized in that the olein fraction comprises a mass percentage of stearic acid of at most 35% relative to the total mass of fatty acid of the fraction of shea olein.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction d'oléine comprend un pourcentage massique en acide stéarique d'au plus 29% par rapport à la masse totale d'acide gras de la fraction d'oléine de karité.In one embodiment, the process according to the invention is characterized in that the olein fraction comprises a mass percentage of stearic acid of at most 29% relative to the total mass of fatty acid of the fraction of shea olein.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction d'oléine comprend un pourcentage massique en acide stéarique d'au plus 25% par rapport à la masse totale d'acide gras de la fraction d'oléine de karité.In one embodiment, the process according to the invention is characterized in that the olein fraction comprises a mass percentage of stearic acid of at most 25% relative to the total mass of fatty acid of the fraction of shea olein.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction d'oléine comprend un pourcentage massique en acide linoléique d'au moins 5% par rapport à la masse totale d'acide gras de la fraction d'oléine de karité.In one embodiment, the process according to the invention is characterized in that the olein fraction comprises a mass percentage of linoleic acid of at least 5% relative to the total mass of fatty acid of the fraction of shea olein.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction d'oléine comprend un pourcentage massique en acide linoléique compris entre 5 et 20% par rapport à la masse totale d'acide gras de la fraction d'oléine de karité.In one embodiment, the process according to the invention is characterized in that the olein fraction comprises a mass percentage of linoleic acid of between 5 and 20% relative to the total mass of fatty acid of the fraction of shea olein.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction d'oléine comprend un pourcentage massique en acide linoléique compris entre 5 et 15% par rapport à la masse totale d'acide gras de la fraction d'oléine de karité.In one embodiment, the process according to the invention is characterized in that the olein fraction comprises a mass percentage of linoleic acid of between 5 and 15% relative to the total mass of fatty acid of the fraction of shea olein.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction d'oléine comprend un pourcentage massique en acide arachidique d'au plus 5% par rapport à la masse totale d'acide gras de la fraction d'oléine de karité.In one embodiment, the process according to the invention is characterized in that the olein fraction comprises a mass percentage of arachidic acid of at most 5% relative to the total mass of fatty acid of the fraction of shea olein.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction d'oléine comprend un pourcentage massique en acide arachidique d'au plus 3% par rapport à la masse totale d'acide gras de la fraction d'oléine de karité.In one embodiment, the process according to the invention is characterized in that the olein fraction comprises a mass percentage of arachidic acid of at most 3% relative to the total mass of fatty acid of the fraction of shea olein.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction d'oléine comprend un pourcentage massique en acide arachidique d'au plus 2% par rapport à la masse totale d'acide gras de la fraction d'oléine de karité.In one embodiment, the process according to the invention is characterized in that the olein fraction comprises a mass percentage of arachidic acid of at most 2% relative to the total mass of fatty acid of the fraction of shea olein.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction d'oléine de karité, de manière préférentielle, comprend un pourcentage massique d'au plus 5% d'acide palmitique, compris entre 5 et 15% d'acide linoléique, d'au plus 3% d'acide arachidique, d'au plus 29% en acide stéarique et d'au moins 50% en acide oléique, par rapport à la masse totale d'acide gras de la fraction d'oléine de karité.In one embodiment, the method according to the invention is characterized in that the shea olein fraction, preferably, comprises a mass percentage of at most 5% of palmitic acid, between 5 and 15% linoleic acid, not more than 3% arachidic acid, not more than 29% stearic acid and not less than 50% oleic acid, relative to the total mass of fatty acid of the fraction d shea olein.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction de stéarine de karité est une fraction solide qui comprend les acides gras suivants : l'acide palmitique, l'acide stéarique, l'acide oléique, l'acide linoléique et l'acide arachidique.In one embodiment, the process according to the invention is characterized in that the shea stearin fraction is a solid fraction which comprises the following fatty acids: palmitic acid, stearic acid, oleic acid, linoleic acid and arachidic acid.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction de stéarine comprend un pourcentage massique en acide palmitique d'au plus 10% par rapport à la masse totale d'acide gras de la fraction de stéarine de karité.In one embodiment, the process according to the invention is characterized in that the stearin fraction comprises a mass percentage of palmitic acid of at most 10% relative to the total mass of fatty acid of the stearin fraction of shea.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction de stéarine comprend un pourcentage massique en acide palmitique d'au plus 5% par rapport à la masse totale d'acide gras de la fraction de stéarine de karité.In one embodiment, the process according to the invention is characterized in that the stearin fraction comprises a mass percentage of palmitic acid of at most 5% relative to the total mass of fatty acid of the stearin fraction of shea.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction de stéarine comprend un pourcentage massique en acide palmitique d'au plus 4% par rapport à la masse totale d'acide gras de la fraction de stéarine de karité.In one embodiment, the process according to the invention is characterized in that the stearin fraction comprises a mass percentage of palmitic acid of at most 4% relative to the total mass of fatty acid of the stearin fraction of shea.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction de stéarine comprend un pourcentage massique en acide oléique compris entre 20 et 40% par rapport à la masse totale d'acide gras de la fraction de stéarine de karité.In one embodiment, the process according to the invention is characterized in that the stearin fraction comprises a mass percentage of oleic acid of between 20 and 40% relative to the total mass of fatty acid of the stearin fraction of shea.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction de stéarine comprend un pourcentage massique en acide oléique compris entre 30 et 50% par rapport à la masse totale d'acide gras de la fraction de stéarine de karité.In one embodiment, the process according to the invention is characterized in that the stearin fraction comprises a mass percentage of oleic acid of between 30 and 50% relative to the total mass of fatty acid of the stearin fraction of shea.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction de stéarine comprend un pourcentage massique en acide oléique comprise entre 30 et 40% par rapport à la masse totale d'acide gras de la fraction de stéarine de karité.In one embodiment, the process according to the invention is characterized in that the stearin fraction comprises a mass percentage of oleic acid of between 30 and 40% relative to the total mass of fatty acid of the stearin fraction of shea.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction de stéarine comprend un pourcentage massique en acide stéarique compris entre 40 et 60% par rapport à la masse totale d'acide gras de la fraction de stéarine de karité.In one embodiment, the method according to the invention is characterized in that the stearin fraction comprises a mass percentage of stearic acid of between 40 and 60% relative to the total mass of fatty acid of the stearin fraction of shea.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction de stéarine comprend un pourcentage massique en acide stéarique compris entre 50 et 70% par rapport à la masse totale d'acide gras de la fraction de stéarine de karité.In one embodiment, the process according to the invention is characterized in that the stearin fraction comprises a mass percentage of stearic acid of between 50 and 70% relative to the total mass of fatty acid of the stearin fraction of shea.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction de stéarine comprend un pourcentage massique en acide stéarique comprise entre 50 et 60% par rapport à la masse totale d'acide gras de la fraction de stéarine de karité.In one embodiment, the method according to the invention is characterized in that the stearin fraction comprises a mass percentage of stearic acid of between 50 and 60% relative to the total mass of fatty acid of the stearin fraction of shea.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction de stéarine comprend un pourcentage massique en acide linoléique d'au plus 10% par rapport à la masse totale d'acide gras de la fraction de stéarine de karité.In one embodiment, the process according to the invention is characterized in that the stearin fraction comprises a mass percentage of linoleic acid of at most 10% relative to the total mass of fatty acid of the stearin fraction of shea.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction de stéarine comprend un pourcentage massique en acide linoléique comprise entre 5 et 10% par rapport à la masse totale d'acide gras de la fraction de stéarine de karité.In one embodiment, the process according to the invention is characterized in that the stearin fraction comprises a mass percentage of linoleic acid between 5 and 10% relative to the total fatty acid mass of the shea stearin fraction.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction de stéarine comprend un pourcentage massique en acide linoléique d'au plus 5% par rapport à la masse totale d'acide gras de la fraction de stéarine de karité.In one embodiment, the process according to the invention is characterized in that the stearin fraction comprises a mass percentage of linoleic acid of at most 5% relative to the total mass of fatty acid of the stearin fraction of shea.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction de stéarine comprend un pourcentage massique en acide arachidique d'au plus 5% par rapport à la masse totale d'acide gras de la fraction de stéarine de karité.In one embodiment, the method according to the invention is characterized in that the stearin fraction comprises a mass percentage of arachidic acid of at most 5% relative to the total mass of fatty acid of the stearin fraction of shea.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction de stéarine comprend un pourcentage massique en acide arachidique d'au plus 3% par rapport à la masse totale d'acide gras de la fraction de stéarine de karité.In one embodiment, the method according to the invention is characterized in that the stearin fraction comprises a mass percentage of arachidic acid of at most 3% relative to the total mass of fatty acid of the stearin fraction of shea.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction de stéarine comprend un pourcentage massique en acide arachidique d'au plus 2% par rapport à la masse totale d'acide gras de la fraction de stéarine de karité.In one embodiment, the method according to the invention is characterized in that the stearin fraction comprises a mass percentage of arachidic acid of at most 2% relative to the total mass of fatty acid of the stearin fraction of shea.

Dans un mode de réalisation, le procédé selon l'invention est caractérisé en ce que la fraction de stéarine de karité, de manière préférentielle, comprend un pourcentage massique d'au plus 5% en acide palmitique, d'au plus 5% en acide linoléique, d'au plus 3% en acide arachidique, compris entre 30 et 40% en acide oléique et compris entre 50 et 60% en acide stéarique, par rapport à la masse totale d'acide gras de la fraction de stéarine de karité.In one embodiment, the process according to the invention is characterized in that the fraction of shea stearin, preferably, comprises a mass percentage of at most 5% palmitic acid, at most 5% palmitic acid linoleic acid, of at most 3% in arachidic acid, comprised between 30 and 40% in oleic acid and comprised between 50 and 60% in stearic acid, relative to the total mass of fatty acid of the shea stearin fraction.

Les applications des fractions d'oléine et de stéarine de karité obtenues en appliquant le procédé selon l'invention sont des applications visant à incorporer des compositions cosmétiques et/ou alimentairesThe applications of the shea olein and stearin fractions obtained by applying the process according to the invention are applications aimed at incorporating cosmetic and/or food compositions

Parmi les applications visées on s'intéresse aux applications dans le domaine de la cosmétique, on citera par exemple les applications au visage, corps, cheveux.Among the targeted applications, we are interested in applications in the field of cosmetics, mention will be made, for example, of applications to the face, body, hair.

Parmi les applications alimentaires, on citera par exemple l'utilisation dans l'industrie du chocolat et des confiseries, l'utilisation dans la pâtisserieFood applications include, for example, use in the chocolate and confectionery industry, use in pastry

Les applications visées sont plus particulièrement les applications communément répandues dans le cadre des oléines et stéarines de karité utilisables dans les produits ou compositions suivantes :The targeted applications are more particularly the commonly used applications in the context of shea oleins and stearins which can be used in the following products or compositions:

Formulation pour les cheveux (crèmes, soins, produits de coiffages, produit de défrisage)Hair formulation (creams, treatments, styling products, straightening product)

Formulation pour le visage (formulation maquillante, soin du visage, formulation hydratante, protection contre les UV, formulation anti-âge, formulation anti-ride).Facial formulation (makeup formulation, facial treatment, moisturizing formulation, UV protection, anti-aging formulation, anti-wrinkle formulation).

Formulation pour le corps (formulation protégeant contre les UV, formulation anti-âge, formulation anti-ride, formulation hydratante, formulation dépigmentante, formulation pro-pigmentante).Body formulation (UV protection formulation, anti-aging formulation, anti-wrinkle formulation, moisturizing formulation, depigmenting formulation, pro-pigmenting formulation).

Utilisation en tant que substitut du beurre de cacao.Use as a cocoa butter substitute.

Utilisation dans les pâtes feuilletées pour rendre la pâte malléable.Use in puff pastry to make the dough malleable.

Utilisation dans les pâtes à tartiner ou dans la margarine.Use in spreads or margarine.

Ces exemples d'utilisation ne sont nullement limitatifs car les fractions d'oléines et de stéarine de karité ont de nombreuses applications notamment dans le domaine pharmaceutique.These examples of use are in no way limiting since the olein and shea stearin fractions have numerous applications, in particular in the pharmaceutical field.

Par exemple des compositions anti-inflammatoires (soins des douleurs articulaires, rhumatismes). Par ailleurs, d'autres exemples d'utilisation dans des compositions visant à résoudre des problèmes cutanées (dermatites, contusions, soins des plaies).For example anti-inflammatory compositions (care of joint pain, rheumatism). Furthermore, other examples of use in compositions aimed at solving skin problems (dermatitis, bruises, wound care).

EXEMPLES :EXAMPLES:

Les exemples qui illustrent ci-dessous le procédé de la présente invention ne sont nullement limitatifs.The examples which illustrate the method of the present invention below are in no way limiting.

Le beurre raffiné utilisé dans la suite de ces exemples présente la composition en acide gras indiquée dans le tableau ci-dessous : Tableau 1 : composition en acide gras du beurre de karité raffiné Beurre de karité raffiné Pourcentage massique (en %) Acide palmitique 3,5 Acide stéarique 44,1 Acide oléique 45,1 Acide linoléique 5,8 Acide arachidique 1,5 The refined butter used in the rest of these examples has the fatty acid composition indicated in the table below: Table 1: fatty acid composition of refined shea butter Refined shea butter Mass percentage (in %) palmitic acid 3.5 Stearic acid 44.1 Oleic acid 45.1 Linoleic acid 5.8 arachidic acid 1.5

Le tableau ci-dessous présente une gamme de valeur cible des compositions des fractions d'oléine et de stéarine de karité. Tableau 2 : composition cible en acide gras des fractions d'oléine et de stéarine de karité Fraction d'oléine de karité Fraction de stéarine de karité Acide palmitique (%) [0-5] [0-5] Acide stéarique (%) Max 29 [50-60] Acide oléique (%) Min 45 [30-40] Acide linoléique (%) [5-15] [0-5] Acide arachidique (%) [0-3] [0-3] The table below presents a range of target values of the compositions of the shea olein and stearin fractions. Table 2: Target fatty acid composition of shea olein and stearin fractions Shea olein fraction Shea stearin fraction Palmitic acid (%) [0-5] [0-5] Stearic acid (%) Max 29 [50-60] Oleic acid (%) Min 45 [30-40] Linoleic acid (%) [5-15] [0-5] Arachidic acid (%) [0-3] [0-3]

Exemple 1 : Exemple comparatif, fractionnement d'un beurre de karité raffiné par le dodécane biosourcé :Example 1: Comparative Example, Fractionation of Refined Shea Butter with Biosourced Dodecane:

On mélange 60g de beurre de karité raffiné à 40g de dodécane BIOSYNTHIS à une température de 40°C. On agite 5 minutes de façon à obtenir une fraction liquide et homogène.60g of refined shea butter is mixed with 40g of BIOSYNTHIS dodecane at a temperature of 40°C. The mixture is stirred for 5 minutes so as to obtain a liquid and homogeneous fraction.

On rafraîchit le mélange réactionnel à une température de 4°C pendant 24h.The reaction mixture is cooled to a temperature of 4° C. for 24 hours.

On filtre le mélange réactionnel sur papier 11um. On évapore le solvant de la fraction d'oléine de karité et de la fraction de stéarine de karité.The reaction mixture is filtered through 11um paper. The solvent is evaporated from the shea olein fraction and from the shea stearin fraction.

La fraction d'oléine (phase liquide) est concentrée après évaporation sous vide de 30mbar et une température de 150°C.The olein fraction (liquid phase) is concentrated after evaporation under vacuum of 30mbar and a temperature of 150°C.

La fraction de stéarine (phase solide) est concentrée dans les mêmes conditions.The stearin fraction (solid phase) is concentrated under the same conditions.

Le tableau ci-dessous présente les compositions en acide gras des fractions d'oléine et de stéarine de karité obtenues par un fractionnement au dodécane. Tableau 3 : Composition des produits obtenus selon un procédé de fractionnement réalisé avec du dodécane : Produit obtenu selon le procédé de l'invention : Fraction d'oléine de karité Fraction de stéarine de karité Etat physique/ Aspect Liquide trouble Solide Pourcentage massique en acide gras des fractions obtenues selon le procédé de l'invention (%) Fraction d'oléine de karité Fraction de stéarine de karité Acide palmitique 3,6 3,6 Acide stéarique 37,7 48,1 Acide oléique 49,9 42 Acide linoléique 7,4 5,1 Acide arachidique 1,4 1,2 The table below shows the fatty acid compositions of the shea olein and stearin fractions obtained by dodecane fractionation. Table 3: Composition of the products obtained according to a fractionation process carried out with dodecane: Product obtained according to the process of the invention: Shea olein fraction Shea stearin fraction Physical state/ Appearance cloudy liquid Solid Fatty acid mass percentage of the fractions obtained according to the process of the invention (%) Shea olein fraction Shea stearin fraction palmitic acid 3.6 3.6 Stearic acid 37.7 48.1 Oleic acid 49.9 42 Linoleic acid 7.4 5.1 arachidic acid 1.4 1.2

Le procédé de fractionnement réalisé avec du dodécane BIOSYNTHIS seul ne permet pas d'obtenir la composition cible définie au tableau 2 et l'oléine obtenue n'est pas limpide.The fractionation process carried out with BIOSYNTHIS dodecane alone does not make it possible to obtain the target composition defined in Table 2 and the olein obtained is not clear.

Exemple 2 : Fractionnement d'un beurre de karité raffiné par le lévulinate d'éthyle.Example 2: Fractionation of a refined shea butter with ethyl levulinate.

On mélange 20g de beurre de karité raffiné à 80g de lévulinate d'éthyle à une température de 40°C. On agite 5 minutes de façon à obtenir une fraction liquide et homogène.20g of refined shea butter are mixed with 80g of ethyl levulinate at a temperature of 40°C. The mixture is stirred for 5 minutes so as to obtain a liquid and homogeneous fraction.

On rafraîchit le mélange réactionnel à une température de 4°C pendant une nuit.The reaction mixture is cooled to a temperature of 4°C overnight.

On filtre le mélange réactionnel sur papier 11um. On évapore le solvant de la fraction d'oléine de karité et de la fraction de stéarine de karité.The reaction mixture is filtered through 11um paper. The solvent is evaporated from the shea olein fraction and from the shea stearin fraction.

La fraction d'oléine (phase liquide) est concentrée après évaporation sous vide de 30mbar et une température de 150°C.The olein fraction (liquid phase) is concentrated after evaporation under vacuum of 30mbar and a temperature of 150°C.

La fraction de stéarine (phase solide) est concentrée dans les mêmes conditions.The stearin fraction (solid phase) is concentrated under the same conditions.

Le tableau ci-dessous présente les compositions en acide gras des fractions d'oléine et de stéarine de karité obtenues selon le procédé de la présente invention. Tableau 4 : Composition des produits obtenus selon le procédé de la présente invention (100% lévulinate d'éthyle) Produit obtenu selon le procédé de l'invention : Fraction d'oléine de karité Fraction de stéarine de karité Etat physique/ Aspect Liquide limpide Solide Pourcentage massique en acide gras des fractions obtenues selon le procédé de l'invention (%) Fraction d'oléine de karité Fraction de stéarine de karité Acide palmitique 3,6 3,1 Acide stéarique 28,2 47,9 Acide oléique 57,9 42,6 Acide linoléique 9,2 4,8 Acide arachidique 1,1 1,6 The table below shows the fatty acid compositions of the olein and shea stearin fractions obtained according to the process of the present invention. Table 4: Composition of the products obtained according to the process of the present invention (100% ethyl levulinate) Product obtained according to the process of the invention: Shea olein fraction Shea stearin fraction Physical state/ Appearance Clear liquid Solid Fatty acid mass percentage of the fractions obtained according to the process of the invention (%) Shea olein fraction Shea stearin fraction palmitic acid 3.6 3.1 Stearic acid 28.2 47.9 Oleic acid 57.9 42.6 Linoleic acid 9.2 4.8 arachidic acid 1.1 1.6

Le procédé de fractionnement réalisé avec 100% de lévulinate d'éthyle permet d'obtenir une oléine limpide et une stéarine de karité avec une composition en acides gras satisfaisante.The fractionation process carried out with 100% ethyl levulinate makes it possible to obtain a clear olein and a shea stearin with a satisfactory fatty acid composition.

Exemple 3 : Fractionnement d'un beurre de karité raffiné par le lévulinate d'éthyle : On mélange 40g de beurre de karité raffiné à 60g de lévulinate d'éthyle) à une température de 40°C. On agite 5 minutes de façon à obtenir une fraction liquide et homogène.Example 3: Fractionation of a refined shea butter by ethyl levulinate: 40 g of refined shea butter are mixed with 60 g of ethyl levulinate) at a temperature of 40°C. The mixture is stirred for 5 minutes so as to obtain a liquid and homogeneous fraction.

On rafraîchit le mélange réactionnel à une température de 4°C pendant une nuit.The reaction mixture is cooled to a temperature of 4°C overnight.

On filtre le mélange réactionnel sur papier 11um. On évapore le solvant de la fraction d'oléine de karité et de la fraction de stéarine de karité.The reaction mixture is filtered through 11um paper. The solvent is evaporated from the shea olein fraction and from the shea stearin fraction.

La fraction d'oléine (phase liquide) est concentrée après évaporation sous vide de 30mbar et une température de 150°C.The olein fraction (liquid phase) is concentrated after evaporation under vacuum of 30mbar and a temperature of 150°C.

La fraction de stéarine (phase solide) est concentrée dans les mêmes conditions.The stearin fraction (solid phase) is concentrated under the same conditions.

Le tableau ci-dessous présente les compositions en acide gras des fractions d'oléine et de stéarine de karité obtenues selon le procédé de la présente invention. Tableau 5 : Composition des produits obtenus selon le procédé de la présente invention (100% lévulinate d'éthyle) Produit obtenu selon le procédé de l'invention : Fraction d'oléine de karité Fraction de stéarine de karité Etat physique/ Aspect Liquide limpide Solide Pourcentage massique en acide gras des fractions obtenues selon le procédé de l'invention (%) Fraction d'oléine de karité Fraction de stéarine de karité Acide palmitique 3,7 3,1 Acide stéarique 27,9 45,7 Acide oléique 57,5 44,3 Acide linoléique 9,8 5,3 Acide arachidique 1,1 1,6 The table below shows the fatty acid compositions of the olein and shea stearin fractions obtained according to the process of the present invention. Table 5: Composition of the products obtained according to the process of the present invention (100% ethyl levulinate) Product obtained according to the process of the invention: Shea olein fraction Shea stearin fraction Physical state/ Appearance Clear liquid Solid Fatty acid mass percentage of the fractions obtained according to the process of the invention (%) Shea olein fraction Shea stearin fraction palmitic acid 3.7 3.1 Stearic acid 27.9 45.7 Oleic acid 57.5 44.3 Linoleic acid 9.8 5.3 arachidic acid 1.1 1.6

Le procédé de fractionnement réalisé avec 100% de lévulinate d'éthyle permet d'obtenir une oléine limpide et une stéarine de karité avec des compositions en acides gras satisfaisantes.The fractionation process carried out with 100% ethyl levulinate makes it possible to obtain a clear olein and a shea stearin with satisfactory fatty acid compositions.

Exemple 4 : Fractionnement d'un beurre de karité raffiné par un mélange lévulinate d'éthyle - décane :Example 4: Fractionation of a refined shea butter with an ethyl levulinate-decane mixture:

On mélange 20g de beurre de karité raffiné à 56g de lévulinate d'éthyle et 24g de décane BIOSYNTHIS à une température de 40°C. On agite 5 minutes de façon à obtenir une fraction liquide et homogène.20g of refined shea butter are mixed with 56g of ethyl levulinate and 24g of BIOSYNTHIS decane at a temperature of 40°C. The mixture is stirred for 5 minutes so as to obtain a liquid and homogeneous fraction.

On rafraîchit le mélange réactionnel à une température de 4°C pendant une nuit.The reaction mixture is cooled to a temperature of 4°C overnight.

On filtre le mélange réactionnel sur papier 11um. On évapore le solvant de la fraction d'oléine de karité et de la fraction de stéarine de karité.The reaction mixture is filtered through 11um paper. The solvent is evaporated from the shea olein fraction and from the shea stearin fraction.

La fraction d'oléine (phase liquide) est concentrée après évaporation sous vide de 30mbar et une température de 150°C.The olein fraction (liquid phase) is concentrated after evaporation under vacuum of 30mbar and a temperature of 150°C.

La fraction de stéarine (phase solide) est concentrée dans les mêmes conditions.The stearin fraction (solid phase) is concentrated under the same conditions.

Le tableau ci-dessous présente les compositions en acide gras des fractions d'oléine et de stéarine de karité obtenues selon le procédé de la présente invention. Tableau 6 : Composition des produits obtenus selon le procédé de la présente invention (70% lévulinate d'éthyle, 30% décane) Produit obtenu selon le procédé de l'invention : Fraction d'oléine de karité Fraction de stéarine de karité Etat physique/ Aspect Liquide limpide Solide Pourcentage massique en acide gras des fractions obtenues selon le procédé de l'invention (%) Fraction d'oléine de karité Fraction de stéarine de karité Acide palmitique 3,4 2,6 Acide stéarique 39,9 56,9 Acide oléique 48,3 35,8 Acide linoléique 6,5 3,3 Acide arachidique 1,9 1,4 The table below shows the fatty acid compositions of the olein and shea stearin fractions obtained according to the process of the present invention. Table 6: Composition of the products obtained according to the process of the present invention (70% ethyl levulinate, 30% decane) Product obtained according to the process of the invention: Shea olein fraction Shea stearin fraction Physical state/ Appearance Clear liquid Solid Fatty acid mass percentage of the fractions obtained according to the process of the invention (%) Shea olein fraction Shea stearin fraction palmitic acid 3.4 2.6 Stearic acid 39.9 56.9 Oleic acid 48.3 35.8 Linoleic acid 6.5 3.3 arachidic acid 1.9 1.4

Le procédé de fractionnement réalisé avec 70% de lévulinate d'éthyle et 30% de décane permet d'obtenir une oléine limpide et une stéarine de karité avec des compositions en acides gras satisfaisantes.The fractionation process carried out with 70% ethyl levulinate and 30% decane makes it possible to obtain a clear olein and a shea stearin with satisfactory fatty acid compositions.

Exemple 5 : Fractionnement d'un beurre de karité raffiné par un mélange lévulinate d'éthyle - décane :Example 5: Fractionation of a refined shea butter with an ethyl levulinate - decane mixture:

On mélange 20g de beurre de karité raffiné à 70g de lévulinate d'éthyle et 10g de décane BIOSYNTHIS à une température de 40°C. On agite 5 minutes de façon à obtenir une fraction liquide et homogène.20g of refined shea butter are mixed with 70g of ethyl levulinate and 10g of BIOSYNTHIS decane at a temperature of 40°C. The mixture is stirred for 5 minutes so as to obtain a liquid and homogeneous fraction.

On rafraîchit le mélange réactionnel à une température de 4°C pendant une nuit.The reaction mixture is cooled to a temperature of 4°C overnight.

On filtre le mélange réactionnel sur papier 11um. On évapore le solvant de la fraction d'oléine de karité et de la fraction de stéarine de karité.The reaction mixture is filtered through 11um paper. The solvent is evaporated from the shea olein fraction and from the shea stearin fraction.

La fraction d'oléine (phase liquide) est concentrée après évaporation sous vide de 30mbar et une température de 150°C.The olein fraction (liquid phase) is concentrated after evaporation under vacuum of 30mbar and a temperature of 150°C.

La fraction de stéarine (phase solide) est concentrée dans les mêmes conditions.The stearin fraction (solid phase) is concentrated under the same conditions.

Le tableau ci-dessous présente les compositions en acide gras des fractions d'oléine et de stéarine de karité obtenues selon le procédé de la présente invention. Tableau 7 : Composition des produits obtenus selon le procédé de la présente invention (87,5% lévulinate d'éthyle, 12,5% décane) Produit obtenu selon le procédé de l'invention : Fraction d'oléine de karité Fraction de stéarine de karité Etat physique/ Aspect Liquide limpide Solide Pourcentage massique en acide gras des fractions obtenues selon le procédé de l'invention (%) Fraction d'oléine de karité Fraction de stéarine de karité Acide palmitique 3,5 3,1 Acide stéarique 29,4 46,1 Acide oléique 56,8 43,8 Acide linoléique 9,1 5,4 Acide arachidique 1,2 1,6 The table below shows the fatty acid compositions of the olein and shea stearin fractions obtained according to the process of the present invention. Table 7: Composition of the products obtained according to the process of the present invention (87.5% ethyl levulinate, 12.5% decane) Product obtained according to the process of the invention: Shea olein fraction Shea stearin fraction Physical state/ Appearance Clear liquid Solid Fatty acid mass percentage of the fractions obtained according to the process of the invention (%) Shea olein fraction Shea stearin fraction palmitic acid 3.5 3.1 Stearic acid 29.4 46.1 Oleic acid 56.8 43.8 Linoleic acid 9.1 5.4 arachidic acid 1.2 1.6

Le procédé de fractionnement réalisé avec 87,5% de lévulinate d'éthyle et 12,5% de décane permet d'obtenir une oléine limpide et une stéarine de karité avec des compositions en acides gras satisfaisantes.The fractionation process carried out with 87.5% ethyl levulinate and 12.5% decane makes it possible to obtain a clear olein and a shea stearin with satisfactory fatty acid compositions.

Exemple 6 : Fractionnement d'un beurre de karité raffiné par un mélange lévulinate d'éthyle - décane :Example 6: Fractionation of a refined shea butter with an ethyl levulinate - decane mixture:

On mélange 20g de beurre de karité raffiné à 75g de lévulinate d'éthyle et 5g de décane BIOSYNTHIS à une température de 40°C. On agite 5 minutes de façon à obtenir une fraction liquide et homogène.20g of refined shea butter are mixed with 75g of ethyl levulinate and 5g of BIOSYNTHIS decane at a temperature of 40°C. The mixture is stirred for 5 minutes so as to obtain a liquid and homogeneous fraction.

On rafraîchit le mélange réactionnel à une température de 4°C pendant une nuit.The reaction mixture is cooled to a temperature of 4°C overnight.

On filtre le mélange réactionnel sur papier 11um. On évapore le solvant de la fraction d'oléine de karité et de la fraction de stéarine de karité.The reaction mixture is filtered through 11um paper. The solvent is evaporated from the shea olein fraction and from the shea stearin fraction.

La fraction d'oléine (phase liquide) est concentrée après évaporation sous vide de 30mbar et une température de 150°C.The olein fraction (liquid phase) is concentrated after evaporation under vacuum of 30mbar and a temperature of 150°C.

La fraction de stéarine (phase solide) est concentrée dans les mêmes conditions.The stearin fraction (solid phase) is concentrated under the same conditions.

Le tableau ci-dessous présente les compositions en acide gras des fractions d'oléine et de stéarine de karité obtenues selon le procédé de la présente invention. Tableau 8 : Composition des produits obtenus selon le procédé de la présente invention (94% lévulinate d'éthyle, 6% décane) Produit obtenu selon le procédé de l'invention : Fraction d'oléine de karité Fraction de stéarine de karité Etat physique/ Aspect Liquide limpide Solide Pourcentage massique en acide gras des fractions obtenues selon le procédé de l'invention (%) Fraction d'oléine de karité Fraction de stéarine de karité Acide palmitique 3,5 3,2 Acide stéarique 25,4 44,6 Acide oléique 60,1 45,0 Acide linoléique 10,0 5,6 Acide arachidique 1,0 1,6 The table below shows the fatty acid compositions of the olein and shea stearin fractions obtained according to the process of the present invention. Table 8: Composition of the products obtained according to the process of the present invention (94% ethyl levulinate, 6% decane) Product obtained according to the process of the invention: Shea olein fraction Shea stearin fraction Physical state/ Appearance Clear liquid Solid Fatty acid mass percentage of the fractions obtained according to the process of the invention (%) Shea olein fraction Shea stearin fraction palmitic acid 3.5 3.2 Stearic acid 25.4 44.6 Oleic acid 60.1 45.0 Linoleic acid 10.0 5.6 arachidic acid 1.0 1.6

Le procédé de fractionnement réalisé avec 94% de lévulinate d'éthyle et 6% de décane permet d'obtenir une oléine limpide et une stéarine de karité avec des compositions en acides gras satisfaisantes.The fractionation process carried out with 94% ethyl levulinate and 6% decane makes it possible to obtain a clear olein and a shea stearin with satisfactory fatty acid compositions.

Exemple 7 : Fractionnement d'un beurre de karité raffiné par un mélange lévulinate d'éthyle - dodécane :Example 7: Fractionation of a refined shea butter with an ethyl levulinate-dodecane mixture:

On mélange 20g de beurre de karité raffiné à 75g de lévulinate d'éthyle et 5g de dodécane BIOSYNTHIS à une température de 40°C. On agite 5 minutes de façon à obtenir une fraction liquide et homogène.20g of refined shea butter are mixed with 75g of ethyl levulinate and 5g of BIOSYNTHIS dodecane at a temperature of 40°C. The mixture is stirred for 5 minutes so as to obtain a liquid and homogeneous fraction.

On rafraîchit le mélange réactionnel à une température de 4°C pendant une nuit.The reaction mixture is cooled to a temperature of 4°C overnight.

On filtre le mélange réactionnel sur papier 11um. On évapore le solvant de la fraction d'oléine de karité et de la fraction de stéarine de karité.The reaction mixture is filtered through 11um paper. The solvent is evaporated from the shea olein fraction and from the shea stearin fraction.

La fraction d'oléine (phase liquide) est concentrée après évaporation sous vide de 30mbar et une température de 150°C.The olein fraction (liquid phase) is concentrated after evaporation under vacuum of 30mbar and a temperature of 150°C.

La fraction de stéarine (phase solide) est concentrée dans les mêmes conditions.The stearin fraction (solid phase) is concentrated under the same conditions.

Le tableau ci-dessous présente les compositions en acide gras des fractions d'oléine et de stéarine de karité obtenues selon le procédé de la présente invention. Tableau 9 : Composition des produits obtenus selon le procédé de la présente invention (94% lévulinate d'éthyle, 6% dodécane). Produit obtenu selon le procédé de l'invention : Fraction d'oléine de karité Fraction de stéarine de karité Etat physique/ Aspect Liquide limpide Solide Pourcentage massique en acide gras des fractions obtenues selon le procédé de l'invention (%) Fraction d'oléine de karité Fraction de stéarine de karité Acide palmitique 4,3 3,4 Acide stéarique 22,1 44,1 Acide oléique 61,3 45,4 Acide linoléique 12 5,6 Acide arachidique 0,3 1,5 The table below shows the fatty acid compositions of the olein and shea stearin fractions obtained according to the process of the present invention. Table 9: Composition of the products obtained according to the process of the present invention (94% ethyl levulinate, 6% dodecane). Product obtained according to the process of the invention: Shea olein fraction Shea stearin fraction Physical state/ Appearance Clear liquid Solid Fatty acid mass percentage of the fractions obtained according to the process of the invention (%) Shea olein fraction Shea stearin fraction palmitic acid 4.3 3.4 Stearic acid 22.1 44.1 Oleic acid 61.3 45.4 Linoleic acid 12 5.6 arachidic acid 0.3 1.5

Le procédé de fractionnement réalisé avec 94% de lévulinate d'éthyle et 6% de dodécane permet d'obtenir une oléine limpide et une stéarine de karité avec des compositions en acide gras satisfaisantes.The fractionation process carried out with 94% ethyl levulinate and 6% dodecane makes it possible to obtain a clear olein and a shea stearin with satisfactory fatty acid compositions.

Exemple 8 : Fractionnement d'un beurre de karité raffiné par un mélange de lévulinate d'éthyle et de lactate d'éthyle.Example 8: Fractionation of a refined shea butter with a mixture of ethyl levulinate and ethyl lactate.

On mélange 20g de beurre de karité raffiné à 40g de lévulinate d'éthyle et 40g de lactate d'éthyle à une température de 40°C. On agite 5 minutes de façon à obtenir une fraction liquide et homogène.20g of refined shea butter are mixed with 40g of ethyl levulinate and 40g of ethyl lactate at a temperature of 40°C. The mixture is stirred for 5 minutes so as to obtain a liquid and homogeneous fraction.

On rafraîchit le mélange réactionnel à une température de 4°C pendant une nuit.The reaction mixture is cooled to a temperature of 4°C overnight.

On filtre le mélange réactionnel sur papier 11um. On évapore le solvant de la fraction d'oléine de karité et de la fraction de stéarine de karité.The reaction mixture is filtered through 11um paper. The solvent is evaporated from the shea olein fraction and from the shea stearin fraction.

La fraction d'oléine (phase liquide) est concentrée après évaporation sous vide de 30mbar et une température de 150°C.The olein fraction (liquid phase) is concentrated after evaporation under vacuum of 30mbar and a temperature of 150°C.

La fraction de stéarine (phase solide) est concentrée dans les mêmes conditions.The stearin fraction (solid phase) is concentrated under the same conditions.

Le tableau ci-dessous présente les compositions en acide gras des fractions d'oléine et de stéarine de karité obtenues selon le procédé de la présente invention. Tableau 10 : Composition des produits obtenus selon le procédé de la présente invention (50% lévulinate d'éthyle et 50% lactate d'éthyle) Produit obtenu selon le procédé de l'invention : Fraction d'oléine de karité Fraction de stéarine de karité Etat physique/ Aspect Liquide trouble Solide Pourcentage massique en acide gras des fractions obtenues selon le procédé de l'invention (%) Fraction d'oléine de ka rité* Fraction de stéarine de karité Acide palmitique 3,9 3,4 Acide stéarique 28 48,8 Acide oléique 57,2 41,2 Acide linoléique 9,9 5,1 Acide arachidique 1 1,5 The table below shows the fatty acid compositions of the olein and shea stearin fractions obtained according to the process of the present invention. Table 10: Composition of the products obtained according to the process of the present invention (50% ethyl levulinate and 50% ethyl lactate) Product obtained according to the process of the invention: Shea olein fraction Shea stearin fraction Physical state/ Appearance cloudy liquid Solid Fatty acid mass percentage of the fractions obtained according to the process of the invention (%) Shea olein fraction* Shea stearin fraction palmitic acid 3.9 3.4 Stearic acid 28 48.8 Oleic acid 57.2 41.2 Linoleic acid 9.9 5.1 arachidic acid 1 1.5

Le procédé de fractionnement réalisé avec 50% de lévulinate d'éthyle et 50% de lactate d'éthyle permet d'obtenir une oléine de karité avec une composition d'acide gras satisfaisante mais sous forme de liquide trouble.The fractionation process carried out with 50% ethyl levulinate and 50% ethyl lactate makes it possible to obtain a shea olein with a satisfactory fatty acid composition but in the form of a cloudy liquid.

Claims (11)

Procédé de fractionnement d'un extrait de karité comprenant au moins les étapes suivantes : a) mélange et homogénéisation du beurre de karité à l'aide d'un système de solvant comprenant au moins un oxo-ester de formule I,
Figure imgb0008
dans laquelle, - R1 est choisi dans le groupe constitué par les alkyles linéaires ou ramifiés comprenant de 1 à 8 atomes de carbone ; - R2, R3 et R4 identiques ou différents sont choisis dans le groupe constitué par l'atome d'hydrogène ou les alkyles linéaires ou ramifiés comprenant de 1 à 4 atomes de carbone; et - et n est un entier naturel compris entre 1 et 4.
b) obtention d'un mélange homogène, c) refroidissement du mélange d) filtration et élimination du système de solvant afin de récupérer les fractions d'oléine et de stéarine.
Process for fractionating a shea extract comprising at least the following steps: a) mixing and homogenizing the shea butter using a solvent system comprising at least one oxo-ester of formula I,
Figure imgb0008
in which, - R 1 is chosen from the group consisting of linear or branched alkyls comprising from 1 to 8 carbon atoms; - R 2 , R 3 and R 4 , which are identical or different, are chosen from the group consisting of the hydrogen atom or linear or branched alkyls comprising from 1 to 4 carbon atoms; and - and n is a natural number between 1 and 4.
b) obtaining a homogeneous mixture, c) cooling of the mixture d) filtration and removal of the solvent system to recover the olein and stearin fractions.
Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que dans le mélange homogène obtenu à l'étape b) est défini par le ratio Y tel que : Y = Pourcentage massique d un extrait de karité Pourcentage massique du système de solvant
Figure imgb0009
est d'au plus 1/1.
Process according to any one of the preceding claims, characterized in that in the homogeneous mixture obtained in step b) is defined by the ratio Y such that: Y = Mass percentage d a shea extract Solvent System Mass Percentage
Figure imgb0009
is at most 1/1.
Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que le système de solvant a un point éclair inférieur ou égal à 100°C mesuré selon la norme ATSM D93.Process according to any one of the preceding claims, characterized in that the solvent system has a flash point of less than or equal to 100°C measured according to standard ATSM D93. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que le système de solvant a une température d'ébullition inférieure ou égale à 210°C.Process according to any one of the preceding claims, characterized in that the solvent system has a boiling point of less than or equal to 210°C. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que le système de solvant comprend au moins un oxo-ester de formule II :
Figure imgb0010
dans laquelle, - R1 est choisi dans le groupe constitué par les alkyles linéaires ou ramifiés comprenant de 1 à 4 atomes de carbone ; - R2, R3 et R4 identiques ou différents sont choisis dans le groupe constitué par l'atome d'hydrogène ou les alkyles linéaires ou ramifiés comprenant de 1 à 4 atomes de carbone; et - et n est un entier naturel compris entre 1 et 4.
Process according to any one of the preceding claims, characterized in that the solvent system comprises at least one oxo-ester of formula II:
Figure imgb0010
in which, - R 1 is chosen from the group consisting of linear or branched alkyls comprising from 1 to 4 carbon atoms; - R 2 , R 3 and R 4 , which are identical or different, are chosen from the group consisting of the hydrogen atom or linear or branched alkyls comprising from 1 to 4 carbon atoms; and - and n is a natural number between 1 and 4.
Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que le système de solvant comprend au moins un oxo-ester de formule III :
Figure imgb0011
- R1 est choisi dans le groupe constitué par les alkyles linéaires ou ramifiés comprenant de 1 à 4 atomes de carbone ; - R2 et R3 identiques ou différents sont choisis dans le groupe constitué par l'atome d'hydrogène, le groupement méthyl ou le groupement éthyl - R4 est choisi dans le groupe constitué par les alkyls linéaires ou ramifiés comprenant de 1 à 3 atomes de carbone ; - et n est un entier naturel compris entre 1 et 3.
Process according to any one of the preceding claims, characterized in that the solvent system comprises at least one oxo-ester of formula III:
Figure imgb0011
- R 1 is chosen from the group consisting of linear or branched alkyls comprising from 1 to 4 carbon atoms; - R 2 and R 3 , identical or different, are chosen from the group consisting of the hydrogen atom, the methyl group or the ethyl group - R 4 is chosen from the group consisting of linear or branched alkyls comprising from 1 to 3 carbon atoms; - and n is a natural number between 1 and 3.
Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que le système de solvant comprend au moins un alcane volatil et un lévulinate d'éthyle.Process according to any one of the preceding claims, characterized in that the solvent system comprises at least one volatile alkane and one ethyl levulinate. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que le système de solvant comprend un alcane ramifié de 10 atomes de carbones et un lévulinate d'éthyle.Process according to any one of the preceding claims, characterized in that the solvent system comprises a branched alkane of 10 carbon atoms and an ethyl levulinate. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que le système de solvant est un mélange de solvant comprend en outre un lactate d'éthyleProcess according to any of the preceding claims, characterized in that the solvent system is a solvent mixture further comprising an ethyl lactate Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que le système de solvant comprend une teneur en oxo-ester comprise entre 70 et 100% par rapport au volume total du système de solvant.Process according to any one of the preceding claims, characterized in that the solvent system comprises an oxo-ester content of between 70 and 100% relative to the total volume of the solvent system. Procédé selon l'une quelconques des revendications précédentes, caractérisé en ce que l'élimination du système de solvant permet d'éliminer au moins 99,9% du système de solvant par rapport au volume total du système de solvant.Process according to any one of the preceding claims, characterized in that the elimination of the solvent system makes it possible to eliminate at least 99.9% of the solvent system relative to the total volume of the solvent system.
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