SOLID/LIQUID EXTRACTION

20200069978 ยท 2020-03-05

    Inventors

    Cpc classification

    International classification

    Abstract

    The present application relates to an oil extracted from a solid vegetable matter or a micro-organism comprising a high unsaponifiable content, the solid vegetable from which the oil has been extracted and the micro-organism from which the oil has been extracted.

    Claims

    1-19. (canceled)

    20. An oil extracted from a solid vegetable matter or a micro-organism, comprising at least 1% by mass of unsaponifiable compounds initially present in the solid vegetable matter or micro-organism.

    21. The oil according to claim 20, wherein said oil is devoid of solvents classified in EU1 CMR list, EU2 CMR list and/or the US CMR list.

    22. The oil according to claim 20, wherein the solid vegetable matter is obtained from soybean, rapeseed, corn, sunflower, sesame, lupin, cotton, coconut, olive, avocado, cocoa, illipe, shea, palm kernel, peanut, copra, linseed, castor, grape seeds, gourd seeds, blackcurrant seeds, melon seeds, tomato seeds, pumpkin seeds, almond, hazelnut, walnut, evening primrose, borage, safflower, camelina, or poppy seed, or a mixture thereof.

    23. The oil according to claim 20, wherein the micro-organism is obtained from macroalgae, microalgae, yeasts, moulds, or bacteria, or a mixture thereof.

    24. An oil obtainable according to a method of solid/liquid extraction, comprising the steps of: providing a solid vegetable matter or a micro-organism; extracting said oil from said solid vegetable matter or a micro-organism by solid/liquid extraction using a first solvent system comprising a concentration of a solvent selected from the group consisting of a fluorinated aromatic solvent, a tert-butyl ether, a solvent comprising at least one silicon atom, and methyl-tetrahydrofuran (MeTHF), or a mixture thereof, representing at least 50% by volume in relation to the total volume of the solvent system; and recovering a fraction comprising the oil.

    25. The oil according to claim 24, wherein the solid vegetable matter is obtained from soybean, rapeseed, corn, sunflower, sesame, lupin, cotton, coconut, olive, avocado, cocoa, illipe, shea, palm kernel, peanut, copra, linseed, castor, grape seeds, gourd seeds, blackcurrant seeds, melon seeds, tomato seeds, pumpkin seeds, almond, hazelnut, walnut, evening primrose, borage, safflower, camelina, or poppy seed, or a mixture thereof.

    26. The oil according to claim 24, wherein the micro-organism is obtained from macroalgae, microalgae, yeasts, moulds, or bacteria, or a mixture thereof.

    27. A composition, comprising an oil extracted from a solid vegetable matter or a micro-organism, said oil comprising at least 1% by mass of unsaponifiable compounds initially present in the solid vegetable matter or micro-organism.

    28. A solid vegetable matter from which an oil has been extracted, prepared by a process comprising the steps of: providing a solid vegetable matter comprising said oil; extracting said oil by solid/liquid extraction using a first solvent system comprising a concentration of a solvent selected from the group consisting of a fluorinated aromatic solvent, a tert-butyl ether, a solvent comprising at least one silicon atom, and methyl-tetrahydrofuran (MeTHF), or a mixture thereof, representing at least 50% by volume in relation to the total volume of the solvent system; and recovering said solid vegetable matter from which an oil has been extracted.

    29. A micro-organism from which an oil has been extracted, prepared by a process comprising the steps of: providing a micro-organism comprising said oil; extracting said oil by solid/liquid extraction using a first solvent system comprising a concentration of a solvent selected from the group consisting of a fluorinated aromatic solvent, a tert-butyl ether, a solvent comprising at least one silicon atom, and methyl-tetrahydrofuran (MeTHF), or a mixture thereof, representing at least 50% by volume in relation to the total volume of the solvent system; and recovering said micro-organism from which an oil has been extracted.

    30. The oil according to claim 23, wherein said micro-organism is Haematocococcus, Dunaliella, Spirulina, or Chorella, or a mixture thereof.

    31. The oil according to claim 24, wherein said solvent is trifluorotoluene (BTF), hexafluorobenzene (BHF), 2-ethoxy-2-methylpropane, ethyl-tert-butyl-ether (ETBE), 2-methoxy-2-methylpropane, methyl-tert-butylether (MTBE), hexamethyl disiloxane (HMDS), tetramethylsilane (TMS) or methyl-tetrahydrofuran (MeTHF).

    32. The oil according to claim 26, wherein said micro-organism is Haematocococcus, Dunaliella, Spirulina, or Chorella, or a mixture thereof.

    33. The solid vegetable matter from which an oil has been extracted according to claim 28, wherein said solvent is trifluorotoluene (BTF), hexafluorobenzene (BHF), 2-ethoxy-2-methylpropane, ethyl-tert-butyl-ether (ETBE), 2-methoxy-2-methylpropane, methyl-tert-butylether (MTBE), hexamethyl disiloxane (HMDS), tetramethylsilane (TMS), or methyl-tetrahydrofuran (MeTHF), or a mixture thereof.

    34. The micro-organism from which an oil has been extracted according to claim 29, wherein said solvent is trifluorotoluene (BTF), hexafluorobenzene (BHF), 2-ethoxy-2-methylpropane, ethyl-tert-butyl-ether (ETBE), 2-methoxy-2-methylpropane, methyl-tert-butylether (MTBE), hexamethyl disiloxane (HMDS), tetramethylsilane (TMS), or methyl-tetrahydrofuran (MeTHF), or a mixture thereof.

    Description

    EXAMPLES

    [0073] In all the examples, a reference test using hexane was carried out.

    Example 1: Extraction from Dried Avocados

    [0074] Extraction from dried avocados was carried out with hexane (reference) and with the following solvents: HMDS, MeTHF, BTF, BHF, MTBE, ETBE.

    [0075] Dried avocado is ground and introduced into a cellulose cartridge (30 to 40 g). The extraction is carried out in a Soxhlet type device (BUCHI B-811). Four extractions are then launched in parallel and each consists of 20 extraction/siphoning cycles. Once the extraction has been finalised, the extraction solvent is evaporated and the residue from which solvent has been removed is weighed. The mass yields are then compared. The results are given in table 1.

    TABLE-US-00001 TABLE 1 Unsaponifiable Extraction oil content solvent Oil yield (% m/m) (% m/m) Hexane 61.1 1.88 ETBE 59.7 2.75 MeTHF 61.3 3.05 HFB 59.3 2.32 BTF 64.0 2.41 HMDS 60.5 1.92 MTBE 65.3 1.92

    [0076] This demonstrates that the solvents according to the invention have an equivalent extraction capacity to that of hexane.

    [0077] The unsaponifiable content of the extracted oil is higher for the solvents according to the invention than for hexane; it is increased by 50% in the case of ETBE and MeTHF.

    Example 2: Extraction from Freeze-Dried Avocado Pulp Powder

    [0078] Freeze-dried avocado pulp powder was extracted according to the method described in example 1 with hexane (reference) and with the following solvents: HMDS, MeTHF, BTF, MTBE, ETBE. The results are given in table 2.

    TABLE-US-00002 TABLE 2 Unsaponifiable Extraction oil content solvent Oil yield (% m/m) (% m/m) Hexane 70.1 2.15 ETBE 69.6 2.25 MeTHF 71.7 3.02 BTF 67.3 2.22 HMDS 68.8 2.22 MTBE 70.1 2.35

    [0079] This demonstrates that the solvents according to the invention have an equivalent extraction capacity to that of hexane.

    [0080] The unsaponifiable content of the extracted oil is higher for the solvents according to the invention than for hexane; it is increased by 50% in the case of 50% in the case of MeTHF.

    Example 3: Oil Extraction from Dried Avocados

    [0081] Extraction from dried avocados is carried out with hexane (reference) and the following solvents: BTF and ETBE.

    [0082] Dried avocado is ground and introduced into a cellulose cartridge (30 to 40 g). The extraction is carried out in a Soxhlet type device (BUCHI B-811). Four extractions are then launched in parallel, the first consisting of 5 extraction cycles, the second of 10 cycles, the third of 15 cycles and the fourth of 20 cycles. Once the extraction has been finalised, the extraction solvent is evaporated and the residue from which solvent has been removed is weighed. The mass yields are then compared.

    [0083] The results are given in table 3 below.

    TABLE-US-00003 TABLE 3 Solvent Hexane ETBE BTF Cycles 5 10 15 20 5 10 15 20 5 (% m/m) Oil yield 18.3% 31.3% 33.1% 40.9% 17.6% 26.8% 30.2% 40.3% 39.0%

    [0084] The mass yields obtained with ETBE are similar to those obtained with the hexane reference: ETBE thus offers an alternative to the use of hexane in solid/liquid extraction methods.

    [0085] The extraction power of BTF is suitable for obtaining, in only 5 extraction cycles, the same yield as those obtained in 20 extraction cycles with hexane or ETBE. BTF thus offers a satisfactory alternative to the use of hexane suitable for reducing the quantity of solvent and/or contact time involved significantly.

    Example 4: Extraction from Dried Chorella

    [0086] Extraction from dried Chorella powder was carried out according to the method described in example 1 with hexane (reference) and with the following solvents: BTF and MTBE. The results are given in table 4.

    TABLE-US-00004 TABLE 4 Extraction Oil yield Unsaponifiable oil content solvent (% m/m) (% m/m) Hexane 70 3.0 MTBE 65.4 3.7 BTF 72 3.4

    [0087] This demonstrates that the solvents according to the invention have an equivalent extraction capacity to that of hexane.

    [0088] The unsaponifiable content of the extracted oil is higher for the solvents according to the invention than for hexane.