EP3344379A1 - Procede et dispositif de traitement en continu d'un melange - Google Patents
Procede et dispositif de traitement en continu d'un melangeInfo
- Publication number
- EP3344379A1 EP3344379A1 EP16777711.9A EP16777711A EP3344379A1 EP 3344379 A1 EP3344379 A1 EP 3344379A1 EP 16777711 A EP16777711 A EP 16777711A EP 3344379 A1 EP3344379 A1 EP 3344379A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- transducers
- mixture
- tube
- phase
- wall
- 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.)
- Granted
Links
- 239000000203 mixture Substances 0.000 title claims abstract description 146
- 238000000034 method Methods 0.000 title claims abstract description 65
- 239000012071 phase Substances 0.000 claims description 93
- 239000000839 emulsion Substances 0.000 claims description 90
- 238000011282 treatment Methods 0.000 claims description 54
- 230000008569 process Effects 0.000 claims description 30
- 239000002502 liposome Substances 0.000 claims description 15
- 150000002632 lipids Chemical class 0.000 claims description 14
- 239000008346 aqueous phase Substances 0.000 claims description 10
- 239000003995 emulsifying agent Substances 0.000 claims description 8
- 239000004480 active ingredient Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 33
- 238000003860 storage Methods 0.000 description 26
- 238000010276 construction Methods 0.000 description 25
- 238000005191 phase separation Methods 0.000 description 22
- 239000002245 particle Substances 0.000 description 19
- 238000009826 distribution Methods 0.000 description 18
- 239000003921 oil Substances 0.000 description 15
- 235000019198 oils Nutrition 0.000 description 15
- 239000006185 dispersion Substances 0.000 description 13
- 238000002156 mixing Methods 0.000 description 12
- 229910001220 stainless steel Inorganic materials 0.000 description 11
- 239000010935 stainless steel Substances 0.000 description 11
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 9
- 239000002537 cosmetic Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000004006 olive oil Substances 0.000 description 7
- 235000008390 olive oil Nutrition 0.000 description 7
- 230000015556 catabolic process Effects 0.000 description 6
- 238000006731 degradation reaction Methods 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 239000000341 volatile oil Substances 0.000 description 6
- 235000018936 Vitellaria paradoxa Nutrition 0.000 description 5
- 241001135917 Vitellaria paradoxa Species 0.000 description 5
- 239000000654 additive Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 229940057910 shea butter Drugs 0.000 description 5
- ACTIUHUUMQJHFO-UHFFFAOYSA-N Coenzym Q10 Natural products COC1=C(OC)C(=O)C(CC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)C)=C(C)C1=O ACTIUHUUMQJHFO-UHFFFAOYSA-N 0.000 description 4
- 235000017471 coenzyme Q10 Nutrition 0.000 description 4
- ACTIUHUUMQJHFO-UPTCCGCDSA-N coenzyme Q10 Chemical compound COC1=C(OC)C(=O)C(C\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CCC=C(C)C)=C(C)C1=O ACTIUHUUMQJHFO-UPTCCGCDSA-N 0.000 description 4
- 229940110767 coenzyme Q10 Drugs 0.000 description 4
- 235000013305 food Nutrition 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- 239000013543 active substance Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 230000004075 alteration Effects 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 235000014121 butter Nutrition 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000004945 emulsification Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 230000002572 peristaltic effect Effects 0.000 description 3
- 150000003904 phospholipids Chemical class 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000011144 upstream manufacturing Methods 0.000 description 3
- 235000015112 vegetable and seed oil Nutrition 0.000 description 3
- 239000008158 vegetable oil Substances 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 235000013628 Lantana involucrata Nutrition 0.000 description 2
- 235000006677 Monarda citriodora ssp. austromontana Nutrition 0.000 description 2
- 240000007673 Origanum vulgare Species 0.000 description 2
- 235000019484 Rapeseed oil Nutrition 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- -1 etc.) Substances 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000011328 necessary treatment Methods 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- 235000017060 Arachis glabrata Nutrition 0.000 description 1
- 244000105624 Arachis hypogaea Species 0.000 description 1
- 235000010777 Arachis hypogaea Nutrition 0.000 description 1
- 235000018262 Arachis monticola Nutrition 0.000 description 1
- 240000002791 Brassica napus Species 0.000 description 1
- 235000004977 Brassica sinapistrum Nutrition 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229930186217 Glycolipid Natural products 0.000 description 1
- 244000020551 Helianthus annuus Species 0.000 description 1
- 235000003222 Helianthus annuus Nutrition 0.000 description 1
- 206010020751 Hypersensitivity Diseases 0.000 description 1
- 235000006679 Mentha X verticillata Nutrition 0.000 description 1
- 235000002899 Mentha suaveolens Nutrition 0.000 description 1
- 235000001636 Mentha x rotundifolia Nutrition 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 240000007817 Olea europaea Species 0.000 description 1
- 239000005662 Paraffin oil Substances 0.000 description 1
- 229920005372 Plexiglas® Polymers 0.000 description 1
- 235000019486 Sunflower oil Nutrition 0.000 description 1
- 208000026935 allergic disease Diseases 0.000 description 1
- 230000007815 allergy Effects 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 239000010775 animal oil Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 239000010478 argan oil Substances 0.000 description 1
- 239000008163 avocado oil Substances 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000004581 coalescence Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000013270 controlled release Methods 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000001687 destabilization Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000002296 dynamic light scattering Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000021474 generally recognized As safe (food) Nutrition 0.000 description 1
- 235000021472 generally recognized as safe Nutrition 0.000 description 1
- 235000021473 generally recognized as safe (food ingredients) Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 125000005456 glyceride group Chemical group 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 125000001475 halogen functional group Chemical group 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000008131 herbal destillate Substances 0.000 description 1
- 239000008240 homogeneous mixture Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 229940057995 liquid paraffin Drugs 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000007764 o/w emulsion Substances 0.000 description 1
- 239000004533 oil dispersion Substances 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 235000020232 peanut Nutrition 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 102000004196 processed proteins & peptides Human genes 0.000 description 1
- 108090000765 processed proteins & peptides Proteins 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002600 sunflower oil Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 150000003626 triacylglycerols Chemical class 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 239000013598 vector Substances 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/40—Mixing liquids with liquids; Emulsifying
- B01F23/41—Emulsifying
- B01F23/411—Emulsifying using electrical or magnetic fields, heat or vibrations
- B01F23/4111—Emulsifying using electrical or magnetic fields, heat or vibrations using vibrations
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/40—Mixing liquids with liquids; Emulsifying
- B01F23/41—Emulsifying
- B01F23/414—Emulsifying characterised by the internal structure of the emulsion
- B01F23/4145—Emulsions of oils, e.g. fuel, and water
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F31/00—Mixers with shaking, oscillating, or vibrating mechanisms
- B01F31/80—Mixing by means of high-frequency vibrations above one kHz, e.g. ultrasonic vibrations
- B01F31/84—Mixing by means of high-frequency vibrations above one kHz, e.g. ultrasonic vibrations for material continuously moving through a tube, e.g. by deforming the tube
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/81—Combinations of similar mixers, e.g. with rotary stirring devices in two or more receptacles
- B01F33/811—Combinations of similar mixers, e.g. with rotary stirring devices in two or more receptacles in two or more consecutive, i.e. successive, mixing receptacles or being consecutively arranged
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/82—Combinations of dissimilar mixers
- B01F33/821—Combinations of dissimilar mixers with consecutive receptacles
- B01F33/8212—Combinations of dissimilar mixers with consecutive receptacles with moving and non-moving stirring devices
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F2215/00—Auxiliary or complementary information in relation with mixing
- B01F2215/04—Technical information in relation with mixing
- B01F2215/0413—Numerical information
- B01F2215/0436—Operational information
- B01F2215/0454—Numerical frequency values
Definitions
- the invention relates to a method for continuously treating a mixture and a device for such treatment.
- the invention relates to a method for treating a mixture with high frequency piezoelectric vibration.
- Stable emulsion preparation methods comprising a lipid phase in an aqueous phase are already known using piezoelectric transducers.
- patent FR 2 947 186 describes a process for preparing an oil-in-water emulsion produced in a container in which a piezoelectric transducer operating at high frequencies, in particular greater than 900 kHz, is immersed.
- This method of preparation has many advantages, in particular the absence of use of surfactant or emulsifier, the absence of degradation of the sensitive compounds of the mixture during the process, as well as a low energy consumption of the process to prepare the product. 'emulsion.
- the invention thus aims to solve this drawback.
- the invention relates to a method of treating a mixture comprising at least a first phase and a second phase immiscible with each other, the process comprising the steps of:
- the treatment method according to the invention makes it possible to treat the mixture continuously, while allowing incorporation of a dispersed phase, aqueous or lipidic, important, in a controlled manner and without degradation of materials. In addition, a dispersion is obtained, in particular rapid emulsification of the mixture.
- the dispersion of 20% by mass of oil in water requires sixteen hours to obtain a final volume of 500 ml with an already known emulsion preparation process such as that described in patent FR 2 947 186 With the process according to the invention, a continuous flow rate of treated mixture of 750 ml / min can be obtained as will be described hereinafter in more detail.
- At least one stage is such that it is devoid of two transducers arranged facing each other and parallel to each other; in other words, on one stage or even several stages, the configuration is avoided where two transducers would be arranged vis-à-vis respectively on two parallel walls flanking the product to be treated; thanks to this arrangement, the formation of stationary waves (face-to-face transducers) which would be counter-productive for the desired result is avoided;
- vibratory energy is adapted to form an emulsion and / or liposomes and / or elements of vectorization of active principle
- the mixture does not contain added emulsifier
- the mixture once treated is stable for at least two weeks, or at least two years at room temperature;
- the first phase is an aqueous phase while the second phase is a lipid phase, or conversely;
- the cross section of the wall of the tube is polygonal, the polygonal section comprising an odd number of sides;
- the wall defines an interior space in which the mixture is circulated, the transducers being disposed on the wall outside the interior space;
- the transducers are arranged in a number of discrete positions each corresponding to a cross-sectional plane to the wall of the tube;
- the transducers are adapted to operate at different frequencies, the transducers being arranged in an order of increasing frequency on the tube; and the mixture circulates repeatedly in the tube until the first phase has a micrometric or nanometric, preferably monodisperse, particle size distribution,
- the number of transducers at each stage is greater than or equal to the number of transducers of the preceding stage.
- the invention also relates to a device for treating a mixture comprising at least a first phase and a second immiscible phase with each other, the device comprising a tube comprising a wall and extending between a portion of an input and an output portion, transducers operating at a frequency greater than 900 kHz being disposed on the wall of the tube and being adapted to apply vibratory energy to the mixture.
- the cross section of the wall of the tube is polygonal, the polygonal section comprising an odd number of sides p.
- Figure 1 is a schematic view of the device for implementing the method of treating a mixture according to the invention
- Figure 1A shows a sectional view of the wall of the tube of Figure 1 according to sectional plane IA;
- Figure 2 is a schematic view of another embodiment of the device for implementing the method of treating a mixture according to the invention.
- Figure 3 shows the particle size distribution of the water droplets in a water (5%) emulsion in shea butter (95%) after six hours of treatment by the method according to the invention
- Figure 4 shows the particle size distribution of the water droplets in a water emulsion (5%) in Anhydrous Milk Fatty Material (MGLA; 95%) after six hours of treatment by the method according to the invention
- FIG. 5 represents the particle size distribution of the water droplets in a water (5%) emulsion in oregano essential oil (95%) after four hours of treatment by the process according to the invention
- Figure 6 shows the particle size distribution of the water droplets in a water (5%) emulsion in olive oil (95%) after five hours of treatment by the method according to the invention
- Figure 7 shows the particle size distribution of the water droplets in a water (5%) emulsion in olive oil (95%) after six hours of treatment by the method according to the invention
- FIG. 8 represents the particle size distribution of the water droplets in a water (5%) emulsion in olive oil (95%) after five hours of treatment by the process according to the invention after storage at ambient temperature for a period of two years ;
- FIGS 9A to 9D show different embodiments of the tube of the device according to the invention.
- FIGS. 10A to 10M show different configurations of transducers on the tube of the device according to the invention.
- FIGS. 11A and 11B respectively represent the particle size distribution of a mixture comprising liposomes after four hours of treatment by the process according to the invention and a halos of light view of nanoliposomes obtained by dynamic light scattering with a magnification of 10000.
- FIG. 1 represents an embodiment of a device 1 configured to implement the process for treating a mixture 2 according to the invention.
- the mixture 2 comprises at least a first phase 2a and a second phase 2b.
- the first phase 2a and the second phase 2b are in particular fluid products, in particular liquid or in the form of powder.
- the first phase 2a and the second phase 2b are immiscible with each other. By immiscible, it is therefore understood that the first phase 2a and the second phase 2b can not be mixed, especially at room temperature (about twenty degrees Celsius) to obtain a completely homogeneous mixture.
- the percentages of first phase 2a or second phase 2b in the exemplary embodiments described below are percentages by weight.
- the first phase 2a may be an aqueous phase, while the second phase 2b is a lipid phase, or vice versa.
- lipid phase refers to all oily substances, liquid at the process temperature, natural, plant or animal, or synthetic having or not one or more biological activities proven, and insoluble in the water (less than 2% by weight at room temperature).
- vegetable oils oil (olive, sunflower, rapeseed, peanut, vegetable oil mixtures, etc.), animal oils (fish, etc.).
- butters Mention may also be made, as an example of a lipid phase, especially for dermatology and cosmetics, avocado oils, argan oils and other vegetable oils, essential oils and mineral oils.
- aqueous (or hydrophilic) phase refers to any phase containing water and / or alcohol.
- water softened or not distilled or not, mineral or not, spring water, ultra-pure water, floral waters, fruit water.
- the mixture 2 can comprise one or more additives.
- An additive may be added to one of the first or second phases 2a, 2b, depending on whether it is fat-soluble or water-soluble. If necessary, it may first solubilize such an additive in a solvent.
- a biomolecule of interest can be added in the aqueous phase (peptides, vitamins, flavonoids, etc.) or in the lipid phase (triacylglycerols, fatty acids, flavors, etc.). ).
- the composition of the mixture 2 typically depends on the intended end use of the mixture 2 once treated by the process.
- the mixture 2 does not comprise an emulsifier or a compound adapted to facilitate the dispersion of the first phase 2a in the second phase 2b during the treatment of the mixture 2.
- the mixture 2 does not comprise an emulsifier, surfactant, stabilizer, or any other additive of any kind adapted to prevent or slow the separation of the dispersion of the first phase 2a and the second phase 2b of the mixture 2.
- the mixture 2 may comprise an emulsifier such as phospholipids.
- the device 1 comprises at least one tube 3.
- tube 3 comprises a conduit not necessarily cylindrical, but may have other shapes as will be described below.
- the tube 3 comprises a wall 4 delimiting an interior space 5 in which the mixture 2 is intended to circulate continuously. By continuous, it should be understood that the treatment of the mixture 2 is carried out when the mixture 2 circulates in the tube 3.
- the wall 4 is thin, in practice 1 to 2 mm, for a useful section of the tube of several cm 2 , in practice for example between 2 cm 2 and 30 cm 2 , typically between 5 cm 2 and 15 cm 2 .
- the wall 4 is thin and transmits the ultrasonic vibrations integrally; the wall 4 produces attenuation or amplification because its main eigenfrequencies are much lower than those of the forced excitation.
- the tube 3 extends more particularly between an inlet portion 3a and an outlet portion 3b. This defines a flow direction Se of the mixture 2 in the tube 3 from the inlet portion 3a to the outlet portion 3b.
- the tube 3 is rectilinear between the inlet portion 3a and the outlet portion 3b as shown in FIG. 1. This also defines a flow direction Of the mixture 2 in the tube 3.
- the tube 3 can be placed vertically. Thus, the inlet portion 3a of the tube 3 is located downward while the outlet portion 3b is located upward (the terms “up” and “down” to be understood in their current sense).
- this embodiment is not limiting and the tube 3 can also be arranged horizontally, for example as shown in Figures 1 and 2, or at any other inclination.
- the tube 3 may further comprise at least one or more curved portions.
- the tube 3 can then have the shape of a coil, a spiral or be corrugated, this in order to minimize the space occupied by the device 1.
- the wall 4 of the tube 3 may be made of stainless steel, glass, plexiglass, plastics or other materials.
- the tube 3 is made of stainless steel and / or a plastic material.
- the wall 4 of the tube is thin with respect to the length of each side and / or the useful cross section of the treated product.
- the material of the wall 4 of the tube 3 is neutral, or inert, vis-à-vis the mixture 2.
- the material of the wall 4 of the tube 3 is not degraded in contact with the mixture 2.
- a tube 3 made of polytetrafluoroethylene (PTFE) is not degraded in contact with essential oils.
- the wall 4 of the tube 3 is advantageously of substantially polygonal section.
- the wall 4 of the tube 3 may in particular have slightly rounded corners between its different faces as shown in Figure 1A.
- the wall 4 of the tube 3 is of regular polygonal section (all its faces having the same dimension) over at least one length L.
- the polygonal wall 4 of the tube 3 preferably comprises an odd number of faces.
- FIGS. 9A to 9D show exemplary embodiments in perspective of the tube 3, the sections of the wall 4 of which are triangular, pentagonal, heptagonal and annular, respectively.
- the device 1 also comprises transducer elements 6. These transducers 6 make it possible to apply a vibratory energy to the mixture 2 in a determined frequency range.
- the transducers 6 chosen are more particularly of the piezoelectric type, in particular ceramic. Such transducers are adapted for stable operation in the chosen frequency range and their manufacturing technology is well controlled.
- the transducers 6 may have various shapes, especially in the form of disc or more or less elongated and extended elements.
- the transducers 6 are disposed on the wall 4 of the tube 3.
- the transducers 6 are in particular fixed on the wall 4 of the tube 3, by glue, a seal or any other fastening element.
- the transducers 6 can be placed on the wall 4 inside the tube 3, that is to say in the internal space 5 delimited by the tube 3.
- the transducers 6 can be advantageously placed at the outside the tube 3 on the wall 4, that is to say outside the interior space 5 delimited by the tube 3.
- the vibrations emitted by the transducers 6 then pass through the wall 4 of the tube 3 to reach the mixture 2
- Such an arrangement makes it possible not to put the transducers 6 directly in contact with the mixture 2 and to keep the inner space 5 of the tube for example sterile, which may be necessary for cosmetic and pharmaceutical applications of the mixture 2. This also makes it easier to the cleaning of the tube 3 and limits the possible contaminations of the mixture 2 by a degradation of the elements fixing the transducers 6 to the wall 4.
- each of the transducers 6 can be disposed in a cavity through 4. A seal then sealingly seals the cavity once the transducer disposed therein.
- the transducers 6 are arranged against the wall 4 of the tube 3, the transducers 6 being for example in the form of discs, one of the faces of which is applied to the wall 4 of the tube 3.
- the energy vibratory emitted by the transducers 6 has a component perpendicular to the wall 4 of the tube 3, and in particular perpendicular to the flow direction De of the mixture 2.
- some or all of the transducers 6 may also be inclined relative to the wall 4 of the tube 3, so that the vibratory energy emitted has, in addition to its component perpendicular to the flow direction mixture 2, a component parallel to the flow direction De and oriented for example in the opposite direction to the flow direction Se.
- This positioning of the transducers 6 can indeed make it possible to increase the efficiency of the process.
- the transducers 6, in particular all the transducers 6, are adapted to operate in a frequency range, called high frequency, that is to say greater than or equal to 900 kHz, or even greater than 1000 kHz.
- the transducers 6, in particular all the transducers 6, are adapted to operate in a frequency range between 900 kHz and 3 MHz, more preferably between 900 kHz and 2000 kHz, even more preferably between 1400 and 1800 kHz.
- the application of a high-frequency vibratory energy by means of transducers 6 has the advantage of eliminating the cavitation phenomenon generally used for its shear intensity.
- the conventionally used frequency ranges of between 20 and 200 kHz, and generally less than 80 kHz lead to the formation of cavitation bubbles in the mixture 2, in which the local temperature increases to several hundred hours. degrees Celsius and where the pressure increases sharply.
- This cavitation shears the mixture 2 which allows rapid emulsification but causes the physicochemical and biochemical alteration of the mixture 2.
- the use of high frequencies in accordance with the present invention does not cause such alterations and preserves the mixture 2, by making it possible to obtain stable dispersions.
- the transducers 6 do not all operate at the same frequency.
- the use of several different frequencies, while remaining in the high frequency range (this term should be understood as above), may allow more stable emulsions to be obtained whose quantity of dispersed phase is greater while reducing the necessary treatment time.
- the transducers 6 may for example operate at three different frequencies F1, F2, F3, the transducers 6 being arranged in an increasing frequency order. In other words, the transducers 6 having the lowest frequency F1 are located near the input portion 3a of the tube 3.
- the transducers 6, in particular the active transducers are arranged advantageously in a discrete manner on the preferably polygonal wall 4 of the tube 3 by "stage".
- a stage is defined by a cross-sectional plane to the wall 4 of the tube 3.
- a cross-sectional plane to the wall 4 of the tube 3 defining a stage passes in particular through the center of the transducers 6 of this stage. It can also be said that a stage is provided with transducers located in the plane transverse to the local circulation direction of the product to be treated.
- nine stages of transducers 6 may be arranged on the tube 3.
- all the transducers 6 shown in FIGS. 9A to 9D are not necessarily active, and some may be inactive as will be explained below.
- two consecutive stages of transducers 6 are spaced apart by a distance of less than 30 centimeters, in particular of the order of 10 centimeters.
- the stages of transducers 6, however, are not necessarily necessarily spaced by the same distance d.
- the distance d is more particularly measured between the centers of two transducers 6 disposed on the same face of the tube 3 and respectively belonging to two consecutive stages.
- the transducers 6 are arranged on the faces of the polygonal wall 4 of the tube 3. As will be described hereinafter, the arrangement of the transducers in different stages form a "pattern" or a succession of patterns capable of responding to construction rules determined to optimize the treatment of the mixture 2.
- two transducers 6 of a stage are not arranged opposite each other.
- two transducers 6 are not arranged facing each other directly parallel to each other. Indeed the interaction of the vibratory waves emitted by two transducers face to face is likely to cause the appearance of a stationary wave of the mixture 2 creating areas without treatment in the tube 3 during the process.
- the device 1 also comprises a container 7 in fluid communication with the inlet portion 3a of the tube 3.
- the container 7 is intended to contain the mixture 2 before its circulation in the tube 3.
- the first phase 2a and the second phase 2b can initially be simply combined without prior mixing in the container 7.
- the first phase 2a and the second phase 2b can also be premixed.
- a mechanical or membrane mixing device 8 can be used in the container 7.
- the premix can be produced by applying a vibratory energy to the mixture 2 using transducers, in particular low frequencies. .
- This mixing device 8 allows rapid shearing of the first phase 2a in the second phase 2b, which makes it possible to shorten the treatment step of the subsequent mixture 2 without, for all that, alone making it possible to obtain a stable mixture 2.
- a pump may also be used to introduce one of the phases gradually into the container 7 during this pre-mixing.
- several pumps can also be used to introduce each phase 2a, 2b and optionally other additives, of the mixture 2 into the container 7.
- a heating system 9 makes it possible to heat the mixture 2 (or one of the phases 2a, 2b) beforehand or during its treatment according to the method.
- the mixture 2 can thus be heated, insofar as this does not cause degradation of the materials of the wall 4 of the tube 3 or the other elements of the device 1.
- a cooling system 10 allows the mixture 2 to be cooled beforehand or during the treatment according to the method. This allows in particular to treat the mixture 2 cold, to easily limit the losses and / or degradation of the mixture 2 related to a too high temperature.
- the heating systems 9 and / or cooling 10 allow in particular, for specific needs of implementation or fragility, to maintain the temperature of the phases 2a, 2b treated constant throughout the process.
- a pH control system 1 or possibly several systems 1 1 distributed on the tube 3, to regulate the pH of the mixture 2 during its treatment.
- treatment of the mixture is liable to result in acidification of the mixture Treaty 2, due to the specific organization of HO ions "induced by the method in the mixture 2.
- a pH-stat coupled to a pump mounted soda on the tube 3 allow for example to regulate the pH of the mixture 2 to a determined value during the treatment.
- the device may also comprise a pump 12, in particular peristaltic, adapted to allow the circulation of the mixture 2 in the tube 3.
- the control of the flow rate of the pump 12 makes it possible to control the speed of the mixture 2 during the process and the necessary treatment time.
- the circulation of the mixture is carried out by the effect of gravity, especially when the tube 3 is vertical or inclined in the device 1.
- the treatment of the mixture 2 is carried out continuous manner by circulation of the mixture 2 in the tube 3 on the wall 4 of which are disposed the transducers 6.
- the flow rate of the mixture 2 in the tube 3 is for example between 10 g / min and 2 kg / min, or even between 50 g / min and 900 g / min, in some particular cases of the order of 60 g / min.
- a vibratory energy is then applied to the mixture 2 during its circulation in the tube 3.
- the entire interior space 5 of the tube 3 is preferably occupied by the mixture 2.
- the tube 3 does not include a free interior space, this in order to limit the exchanges between the mixture 2 and the air that would be contained in this free space and which could cause the dissolution of gas in the mixture 2 or losses of volatile compounds.
- the mixture 2 can circulate continuously in a tube 3 which can comprise several wall portions 4 of polygonal section as shown in FIG. 2.
- the tube 3 can thus have different configurations, and can in particular have a length adapted to the mixture 2 to treat.
- the mixture 2 can also circulate several times in a tube 3 recurrently by a closed loop system, until the treatment of the desired mixture 2 is obtained.
- the treatment times given in the exemplary embodiments described below relate to the duration during which the mixture 2 circulates in closed loop in the device 1.
- the dimensions and shape of the tube may vary depending on the type of mixture 2 and the volume to be treated.
- the tube 3 may have an equilateral triangular section over a length L equal to one hundred and twenty centimeters. Each side p of the section of the tube 3 is then equal to five centimeters and the transducers 6 have a disc shape of the order of about two centimeters in diameter.
- the method thus makes it possible to treat the mixture 2 in order to obtain a dispersion of the first phase 2a in the second phase 2b.
- a dispersion can be obtained by mixing 2 at the micrometer, submicron or nanometric scale of the first phase 2a in the second phase 2b in the form of droplets or particles.
- the first phase 2a then constitutes the dispersed phase while the second phase 2b constitutes the continuous phase.
- the treatment of the mixture 2 does not entail alteration or chemical modification of the first and second phases 2a, 2b.
- the generic terms "direct dispersion” or “oil-in-water dispersion” denote a dispersed mixture in which a lipid phase is dispersed in an aqueous phase (also denoted as H / E).
- the generic terms “reverse dispersion” or “water-in-oil dispersion” denote a dispersed mixture in which an aqueous phase is dispersed in a lipid phase (also denoted W / H).
- Multiple or multiphase mixtures can also be obtained by several successive applications of the process according to the invention (also denoted H / E / H or E / H / E for example).
- the mixture is recovered after obtaining the desired final particle size of the first phase 2a, or more simply when the maximum dispersion of the first phase 2a is reached.
- the average particle size of the first phase 2a in the second phase 2b after treatment is less than 50 microns, more preferably less than 20 microns. Shorter processing times produce larger first phase particles 2a with a wide size distribution while longer processing times produce smaller first phase particles 2a with very narrow size distributions; thus the stability of the treated mixture 2 is greater.
- the process is all the faster because it comprises a large number of transducer stages 6.
- the process duration of the method also depends on the mass percentage of the first phase 2a with respect to the second phase 2b.
- the method makes it possible to obtain an emulsion. It is thus possible to obtain a simple emulsion, direct or inverse, or a multiple emulsion.
- the method can also provide a structured blend.
- the method makes it possible to obtain monolayer structured mixtures, such as micelles or colloidosomes, in bilayer such as vesicles, single liposomes, membranes, or in multilayer, such as multilamellar liposomes.
- Liposomes are in the form of lamellar capsules, the layers consist alternately of lipid phase and aqueous phase.
- a lipid phase allowing such structuring can be chosen from glycerides, phospholipids, glycolipids, terpenoids, essential oils and / or polar lipids.
- the structuring of the mixture 2 may also make it possible to obtain a vectorization of active principles or of molecules of interest, cosmetic and pharmaceutical, such as coenzyme Q10.
- Liposomes allow, for example, nano-encapsulation of active agents in the dispersed phase in order to protect these active agents from any degradation during storage of the mixture. The principles thus vectorized are more effective and more bioavailable when released into living organisms. Liposomes are particularly suitable for use in the food industry as a controlled release system of active agents because they are easily achievable, adaptable, biocompatible and are generally considered safe (Generally Recognized As Safe - GRAS). United States Food and Drug Administration (FDA). Liposomes are also widely used in the cosmetics and health sectors for the stabilization and vectorization of active ingredients.
- the method according to the invention also makes it possible to obtain a maximum electrostatic charge on the surface of the liposome in order to obtain a satisfactory stability of the mixture 2 over time.
- the treated mixture 2 obtained is stable.
- the stability of the mixture 2 that is to say the non-macroscopic separation of the first phase 2a and the second phase 2b between them, can last two weeks, several months, two years or more and is therefore suitable for a industrial use.
- the mixture 2 once treated can be used as it is or be incorporated in other lipidic or aqueous phases.
- Construction rules have been established on the basis of analyzes and measurements to determine the configuration of the transducers emitting vibratory energy, or the pattern formed by the transducers and the number of stages on the wall 4 of the tube 3 during the implementation of the method. These rules have been established in particular for a tube 3 of triangular section, although these apply or can be transposed to walls of tubes having other polygonal shapes.
- the construction rules can be combined with each other, selectively selecting some of them or taking them into account in their entirety, in order to form an optimal configuration of transducers 6 arranged on the tube 3.
- i index of the transducer stage on the tube in which the mixture circulates.
- the stages are defined starting from the input portion 3a and then going to the output portion 3b of the tube 3, the first stage being the one that is located closest to the input portion;
- n k number of successive stages comprising the same number k of transducers.
- n ci k for n k successive stages.
- the configuration of the transducers 6 in a pattern is noted as follows: (nc- ⁇ , nc 2 , nc 3 , nc 4 , etc.).
- the configuration noted (2, 3, 2, 2) thus comprises two transducers at the first stage, three transducers at the second stage, and two transducers at the third and fourth stages.
- each stage comprises at most one transducer 6 on each side of the polygon constituting the section of the tube in which the mixture circulates.
- the maximum number of transducers at a given stage is therefore equal to the number of sides p of the polygon. In other words, ne, ⁇ p.
- At least one stage comprises transducers 6 not regularly distributed around the periphery of the tube 3
- stage there are several successive stages of treatment along the tube and on at least one particular stage, there is an arrangement of active transducers not regularly distributed around the perimeter of the tube 3 (ie the stage is devoid of active transducers regularly distributed / spaced around its periphery).
- a first face comprises an active transducer, and the other two faces do not contain an active transducer; in a second configuration, a first face comprises an active transducer and a second face comprises an active transducer, but the third face does not contain an active transducer (it is in fact absent or passive / non-active).
- n- ⁇ 0.
- nc- ⁇ 2.
- the number of transducers at each stage is at least equal to the number of transducers of the preceding stage.
- nc i + 1 > ne the number of transducers at each stage.
- the number of successive stages comprising the same number k of transducers is decreasing.
- n k + 1 ⁇ n k is decreasing.
- This fifth construction rule also differs from known transducer configurations that require the stages to have more transducers and apply more vibratory energy to the mixture to speed up the mixing process.
- a sixth rule of construction there must be at least four stages on the tube 3.
- a seventh rule of construction for two successive stages having the same number of transducers, these are placed on the same faces of the polygon constituting the section of the tube in which circulates the mixture to be treated.
- some stages comprise two transducers and some stages comprise three transducers.
- more than 50% of the stages comprise 2 transducers.
- Even more preferably, between 50% and 75% of the stages comprise 2 transducers.
- the distance d between the consecutive stages can be variable.
- the distance d is in particular less than thirty centimeters, preferably between ten and twenty centimeters.
- a stage without transducer can be considered as a spacing between two adjacent stages.
- Figures 10A to 10M show possible configurations established from the construction rules described above. In these figures, the transducers shown in white are active while the transducers shown in dark and dotted are then inactive, that is to say that they do not emit vibratory energy during the treatment of the mixture 2 (which corresponds de facto to an absence of transducer).
- the emulsion produced shows no phase separation after 30 days. storage at room temperature.
- transducer configuration comprising stages of two and three five-stage transducers but of which the first stages comprise 3 transducers (3, 3, 2, 2, 2), about 25% of the emulsified oil separates from the emulsion after 30 days of storage at room temperature, which therefore has a phase separation.
- a 30% continuous phase emulsion is produced with 2000 g of demineralized water at twenty degrees Celsius to which 860 g of sunflower oil are added gradually at twenty degrees Celsius.
- a membrane emulsification system allows the addition of the oil during the treatment.
- the emulsion is treated for four hours by piezoelectric transducers arranged on the faces of a triangular section stainless steel tube. The stages of transducers are 10 centimeters apart.
- a pH-stat and a soda pump (0.1% by mass) make it possible to maintain the pH of the emulsion at 7.
- a cryostat set at ten degrees Celsius makes it possible to keep the temperature of the emulsion constant during the treatment.
- the oil is added at a rate of 10 g / min.
- the emulsion circulates in the pilot at a speed of 900 g / min.
- the emulsion produced shows no phase separation after 30 days of storage at room temperature.
- a configuration comprising at least four stages of transducers makes it possible to obtain a better stability of the treated mixture according to the sixth construction rule specified above.
- An emulsion is made with 1500 g of demineralised water at seventy degrees Celsius, and 1500 g of shea butter at 70 degrees Celsius are gradually added. It is treated for four hours by piezoelectric transducers arranged on three sides of a triangular section stainless steel tube. The stages of transducers are 8 centimeters apart.
- a pH-stat as well as a soda pump (0.1% by weight) make it possible to maintain the pH of the emulsion at 8.
- a cryostat set at 70 degrees Celsius makes it possible to keep the temperature of the emulsion constant during the treatment.
- a mechanical premix system is used upstream of the tube. The butter is added gradually to the premix at a rate of 10 g / min.
- the mixture circulates in the device at a speed of 900 g / min.
- a transducer configuration comprising stages of two and three five-stage transducers (2, 2, 2, 3, 3)
- the emulsion produced shows no phase separation after 30 days of storage at room temperature, which being stable.
- the emulsion produced has a significant phase separation after 30 days of storage at room temperature.
- about 45% of the emulsified shea butter separates from the emulsion.
- the emulsion produced has a significant phase separation after 30 days of storage at room temperature.
- about 72% of the emulsified shea butter separates from the emulsion.
- a 30% emulsion is produced with 2000 g of demineralized water at twenty degrees Celsius and 860 g of rapeseed oil at twenty degrees Celsius.
- the premix of the emulsion is made via a high pressure homogenizer. It is then treated for four hours by piezoelectric transducers arranged on three sides of a triangular section stainless steel tube. The stages of transducers are 6 centimeters apart.
- a pH-stat and a soda pump (0.1% by weight) make it possible to maintain the pH of the emulsion at 8.
- a cryostat set at ten degrees Celsius makes it possible to keep the temperature of the emulsion constant during the treatment.
- the emulsion circulates in the pilot at a speed of 60 g / min.
- the emulsion produced shows no phase separation after 30 days of storage at room temperature, the latter being stable.
- the emulsion produced shows no phase separation after 30 days of storage at room temperature, the latter being stable.
- a 30% continuous phase emulsion is produced with 2000 g of demineralized water at twenty degrees Celsius to which 860 g of liquid paraffin oil, very apolar, is added gradually at twenty degrees Celsius. It is treated for four hours by piezoelectric transducers arranged on three sides of a triangular section stainless steel tube. The stages of transducers are 20 centimeters apart.
- a pH-stat and a soda pump (0.1% by weight) make it possible to maintain the pH of the emulsion at 8.
- a cryostat set at ten degrees Celsius makes it possible to keep the temperature of the emulsion constant during the treatment.
- a mechanical pre-mixing system and a peristaltic pump allowing the addition of oil during the treatment are used upstream of the transducers. The oil is added at a rate of 10 g / min.
- the emulsion circulates in the pilot at a speed of 60 g / min.
- the emulsion produced shows no phase separation after 30 days of storage at room temperature.
- the emulsion produced shows no phase separation after 30 days storage at room temperature.
- two consecutive stages comprising transducers are 18 centimeters apart.
- the emulsion produced has a significant phase separation after 30 days of storage at room temperature.
- about 75% of the emulsified oil separates from the emulsion.
- two consecutive stages comprising transducers are separated by 28 centimeters.
- a 30% continuous phase emulsion is produced with 2000 g of demineralized water at twenty degrees Celsius to which 860 g of olive oil are added gradually at twenty degrees Celsius. It is treated for four hours by piezoelectric transducers arranged on three sides of a triangular section stainless steel tube. The transducer stages are 1.5 centimeters apart.
- a pH-stat and a soda pump (0.1% by weight) make it possible to maintain the pH of the emulsion at 8.
- a cryostat set at ten degrees Celsius makes it possible to keep the temperature of the emulsion constant during the treatment.
- a mechanical pre-mixing system and a peristaltic pump allowing the addition of oil during the treatment are used upstream of the transducers. The oil is added at a rate of 10 g / min.
- the emulsion circulates in the pilot at a speed of 60 g / min.
- the emulsion produced shows no phase separation after 30 days of storage at room temperature .
- the emulsion produced has no phase separation. after 30 days of storage at room temperature.
- the emulsion produced has no phase separation. after 30 days of storage at room temperature.
- the emulsion produced has no phase separation. after 30 days of storage at room temperature.
- the emulsion produced has no phase separation. after 30 days of storage at room temperature.
- the emulsion produced has no phase separation. after 30 days of storage at room temperature.
- the emulsified oil separates from the emulsion after 30 days of storage at room temperature.
- the treatment time as well as the number of stages of transducers affect the stability of the treated mixture according to the tenth rule of construction specified above.
- a continuous phase 90% emulsion is carried out with 900 g of demineralized water at twenty degrees Celsius to which is added 100 g of phospholipids at twenty degrees Celsius. It is treated for two hours by piezoelectric transducers arranged on three sides of a triangular section stainless steel tube.
- the configuration implemented includes stages to two transducers and stages with three transducers on four stages (2, 2, 3, 3). Each of the transducer stages are 6 centimeters apart.
- the pH of the mixture is maintained at 6.5 during the treatment.
- a cryostat set at ten degrees Celsius keeps the temperature of the mixture constant during treatment. Mechanical pre-mixing is performed prior to the circulation of the phases in the tube 3. The dispersion circulates in the tube at a speed of 60 g / min.
- FIG. 11B a microscopic observation as shown in FIG. 11B reveals the presence of liposomes in the mixture 2 having a diameter of the order of 200 nanometers.
- FIG. 11A represents in particular the particle size distribution of these liposomes in the mixture 2. After 30 days of storage at ambient temperature, the mixture 2 produced shows no phase separation.
- a continuous phase 15% emulsion is carried out with 1800 g of demineralized water at twenty degrees Celsius and a mixture of 167 g of rapeseed oil of 33 g of coenzyme Q10 at twenty degrees Celsius.
- the premix of the emulsion is made via a high pressure homogenizer. It is then treated for four hours by piezoelectric transducers arranged on three sides of a triangular section stainless steel tube.
- the implemented configuration comprises stages of two transducers and three four-stage transducers (2, 2, 3, 3). Each of the transducer stages are 6 centimeters apart.
- a pH-stat and a soda pump (0.1% by weight) make it possible to maintain the pH of the emulsion at 8.
- a cryostat set at ten degrees Celsius makes it possible to keep the temperature of the emulsion constant during the treatment.
- the emulsion circulates in the pilot at a speed of 60 g / min.
- Such an emulsion thus makes it possible to obtain a vectorization of coenzyme Q10, which has all the properties, in particular the antioxidant, of the molecule of interest. After 30 days of storage at ambient temperature, the emulsion produced shows no phase separation. . Production of a powder suspension
- a continuous phase suspension of 5% is carried out with 1425 g of demineralized water at twenty degrees Celsius and a mixture of 75 g of an iron oxide powder at twenty degrees Celsius.
- the premix of the emulsion is made via a mechanical stirring system. It is then treated for four hours by piezoelectric transducers arranged on three sides of a triangular section stainless steel tube.
- the implemented configuration comprises stages of two transducers and three four-stage transducers (2, 2, 3, 3). Each of the floors of transducers are 8 centimeters apart.
- a pH-stat and a soda pump (0.1% by weight) make it possible to maintain the pH of the emulsion at 8.
- a cryostat set at ten degrees Celsius makes it possible to keep the temperature of the emulsion constant during the treatment.
- the emulsion circulates in the pilot at a speed of 600 g / min.
- Blends 2 were made as follows:
- Figures 3 to 6 illustrate the particle size dispersion of the water droplets which remain in suspension in the lipid phase thus forming an inverse emulsion.
- the inverse emulsions can be characterized by dynamic diffraction of light.
- Figure 7 shows the particle size distribution of water droplets (5%) in inverse emulsion (W / O) in olive oil (95%) after six hours of treatment according to the method.
- the droplets have a diameter of less than 500 nanometers and 90% of the population has a diameter of less than 314 nanometers.
- the average diameter of the droplets of this emulsion is 175 nanometers.
- FIG. 8 thus shows the particle size distribution of the emulsion particles measured just after its treatment (solid line curve) as well as measured following its two-year storage (in dashed line). Measuring the particle size distribution of the emulsion two years after its treatment shows that the water droplets have slightly increased in size, which reflects a very slight phenomenon of coalescence after the long storage time of the emulsion. However, this emulsion does not show a phase separation phenomenon and the average size of the droplets remains of the order of 100 nm to 200 nanometers.
- the emulsion stored for a period of two years shows no apparent phenomenon of destabilization, phase separation or settling of the water.
- the process is of general application in all sectors of industry, and finds a particularly interesting application when the use of emulsifiers in a mixture can cause comfort problems, irritation, allergy or intolerance for example in the agri-food, dermatology, cosmetics, relaxation products and pharmacy sectors. Other interesting sectors are, for example, paint or polymers.
- the suppression of emulsifiers can reduce costs, and is therefore attractive in all emulsion preparations on an industrial scale.
- the mixtures treated by the process according to the invention may be creams, lotions, sprays and any other form of pharmaceutical and / or cosmetic product distribution.
- the mixture 2 can be treated firstly in a first container in which the transducer or transducers operate at a frequency F1 and then be transferred to a second container in which the transducer or transducers operate at a frequency F2 different from the frequency F1, and so continued if necessary until the complete treatment of the mixture.
- F1 the frequency of the mixture
- F2 the frequency of the mixture
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Mixers With Rotating Receptacles And Mixers With Vibration Mechanisms (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR1558061A FR3040312B1 (fr) | 2015-08-31 | 2015-08-31 | Procede de traitement en continu d'un melange |
PCT/FR2016/052135 WO2017037372A1 (fr) | 2015-08-31 | 2016-08-29 | Procede et dispositif de traitement en continu d'un melange |
Publications (2)
Publication Number | Publication Date |
---|---|
EP3344379A1 true EP3344379A1 (fr) | 2018-07-11 |
EP3344379B1 EP3344379B1 (fr) | 2022-02-09 |
Family
ID=54291523
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP16777711.9A Active EP3344379B1 (fr) | 2015-08-31 | 2016-08-29 | Procede et dispositif de traitement en continu d'un melange |
Country Status (6)
Country | Link |
---|---|
EP (1) | EP3344379B1 (fr) |
DK (1) | DK3344379T3 (fr) |
ES (1) | ES2913242T3 (fr) |
FR (1) | FR3040312B1 (fr) |
PT (1) | PT3344379T (fr) |
WO (1) | WO2017037372A1 (fr) |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR3098732B1 (fr) | 2019-07-15 | 2022-08-12 | Genialis | Procede d’amelioration de la biodisponibilite de composes hydrophiles dans une solution aqueuse |
FR3118869A1 (fr) | 2021-01-20 | 2022-07-22 | Genialis | Procede d’amelioration de l’activite antioxydante de la vitamine c en solution aqueuse |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4071225A (en) * | 1976-03-04 | 1978-01-31 | Holl Research Corporation | Apparatus and processes for the treatment of materials by ultrasonic longitudinal pressure oscillations |
US6465015B1 (en) * | 1998-02-24 | 2002-10-15 | Arch Chemicals, Inc. | Sonic method of enhancing chemical reactions to provide uniform, non-agglomerated particles |
US6506584B1 (en) * | 2000-04-28 | 2003-01-14 | Battelle Memorial Institute | Apparatus and method for ultrasonic treatment of a liquid |
WO2005051511A1 (fr) * | 2003-11-28 | 2005-06-09 | Mitsubishi Chemical Corporation | Methode de production de particules fines d'un compose organique |
FI123956B (fi) * | 2011-03-11 | 2014-01-15 | Dewaco Ltd | Menetelmä ja järjestely jätevesilietteen käsittelemiseksi jätevesilietteen käsittelyprosessissa |
-
2015
- 2015-08-31 FR FR1558061A patent/FR3040312B1/fr active Active
-
2016
- 2016-08-29 ES ES16777711T patent/ES2913242T3/es active Active
- 2016-08-29 PT PT167777119T patent/PT3344379T/pt unknown
- 2016-08-29 EP EP16777711.9A patent/EP3344379B1/fr active Active
- 2016-08-29 WO PCT/FR2016/052135 patent/WO2017037372A1/fr unknown
- 2016-08-29 DK DK16777711.9T patent/DK3344379T3/da active
Also Published As
Publication number | Publication date |
---|---|
ES2913242T3 (es) | 2022-06-01 |
PT3344379T (pt) | 2022-05-11 |
FR3040312B1 (fr) | 2019-06-07 |
WO2017037372A1 (fr) | 2017-03-09 |
DK3344379T3 (da) | 2022-05-09 |
EP3344379B1 (fr) | 2022-02-09 |
FR3040312A1 (fr) | 2017-03-03 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
EP2445619B1 (fr) | Procédé de préparation d'une émulsion huile-dans-eau stable | |
Santana et al. | High-and low-energy emulsifications for food applications: A focus on process parameters | |
EP0843589B1 (fr) | Procede de preparation d'une emulsion | |
Charcosset | Preparation of emulsions and particles by membrane emulsification for the food processing industry | |
Pathak | Nanoemulsions and their stability for enhancing functional properties of food ingredients | |
McClements et al. | Food-grade nanoemulsions: formulation, fabrication, properties, performance, biological fate, and potential toxicity | |
Komaiko et al. | Formation of oil-in-water emulsions from natural emulsifiers using spontaneous emulsification: sunflower phospholipids | |
Zahi et al. | Formation and stability of d-limonene organogel-based nanoemulsion prepared by a high-pressure homogenizer | |
EP3344379B1 (fr) | Procede et dispositif de traitement en continu d'un melange | |
Wang et al. | Preparation and characterization of micro/nano-emulsions containing functional food components | |
Khalid et al. | Formulation characteristics of triacylglycerol oil-in-water emulsions loaded with ergocalciferol using microchannel emulsification | |
Sundar et al. | Advances and trends in encapsulation of essential oils | |
FR2964017A1 (fr) | Procede de fabrication d'une serie de capsules de taille submillimetrique | |
Malode et al. | A critical review on nanoemulsion: Advantages, techniques and characterization | |
Bhushani et al. | Food-grade nanoemulsions for protection and delivery of nutrients | |
Neves et al. | Formulation of controlled size PUFA-loaded oil-in-water emulsions by microchannel emulsification using β-carotene-rich palm oil | |
Shen et al. | Use of Adaptive Focused Acoustics™ ultrasound in controlling liposome formation | |
FR2976824A1 (fr) | Dispositif de formation de gouttes d'une phase interne dispersees dans une phase externe, ensemble et procede associes | |
Charcosset | Preparation of nanomaterials for food applications using membrane emulsification and membrane mixing | |
Iglesias et al. | Lipid transfer in oil-in-water isasome emulsions: influence of arrested dynamics of the emulsion droplets entrapped in a hydrogel | |
EP3708143A1 (fr) | Procédé de fabrication d'une émulsion aqueuse d'une substance active huileuse pour application cosmétique, alimentaire ou pharmaceutique | |
JP7067786B2 (ja) | 連続乳化装置 | |
Je Lee et al. | Nanoemulsions | |
Ocampo-Salinas et al. | Application of high pressure homogenization to improve stability and decrease droplet size in emulsion-flavor systems | |
EP3902625A1 (fr) | Dispositif et procede pour creer une emulsion |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: UNKNOWN |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: THE INTERNATIONAL PUBLICATION HAS BEEN MADE |
|
PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: REQUEST FOR EXAMINATION WAS MADE |
|
17P | Request for examination filed |
Effective date: 20180228 |
|
AK | Designated contracting states |
Kind code of ref document: A1 Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR |
|
AX | Request for extension of the european patent |
Extension state: BA ME |
|
DAV | Request for validation of the european patent (deleted) | ||
DAX | Request for extension of the european patent (deleted) | ||
GRAP | Despatch of communication of intention to grant a patent |
Free format text: ORIGINAL CODE: EPIDOSNIGR1 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: GRANT OF PATENT IS INTENDED |
|
INTG | Intention to grant announced |
Effective date: 20210610 |
|
GRAJ | Information related to disapproval of communication of intention to grant by the applicant or resumption of examination proceedings by the epo deleted |
Free format text: ORIGINAL CODE: EPIDOSDIGR1 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: REQUEST FOR EXAMINATION WAS MADE |
|
GRAP | Despatch of communication of intention to grant a patent |
Free format text: ORIGINAL CODE: EPIDOSNIGR1 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: GRANT OF PATENT IS INTENDED |
|
INTC | Intention to grant announced (deleted) | ||
INTG | Intention to grant announced |
Effective date: 20211028 |
|
GRAS | Grant fee paid |
Free format text: ORIGINAL CODE: EPIDOSNIGR3 |
|
GRAA | (expected) grant |
Free format text: ORIGINAL CODE: 0009210 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: THE PATENT HAS BEEN GRANTED |
|
AK | Designated contracting states |
Kind code of ref document: B1 Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR |
|
REG | Reference to a national code |
Ref country code: GB Ref legal event code: FG4D Free format text: NOT ENGLISH |
|
REG | Reference to a national code |
Ref country code: CH Ref legal event code: EP Ref country code: AT Ref legal event code: REF Ref document number: 1467160 Country of ref document: AT Kind code of ref document: T Effective date: 20220215 |
|
REG | Reference to a national code |
Ref country code: DE Ref legal event code: R096 Ref document number: 602016068980 Country of ref document: DE |
|
REG | Reference to a national code |
Ref country code: IE Ref legal event code: FG4D Free format text: LANGUAGE OF EP DOCUMENT: FRENCH |
|
REG | Reference to a national code |
Ref country code: DK Ref legal event code: T3 Effective date: 20220506 |
|
REG | Reference to a national code |
Ref country code: PT Ref legal event code: SC4A Ref document number: 3344379 Country of ref document: PT Date of ref document: 20220511 Kind code of ref document: T Free format text: AVAILABILITY OF NATIONAL TRANSLATION Effective date: 20220505 |
|
REG | Reference to a national code |
Ref country code: NO Ref legal event code: T2 Effective date: 20220209 |
|
REG | Reference to a national code |
Ref country code: NL Ref legal event code: FP |
|
REG | Reference to a national code |
Ref country code: SE Ref legal event code: TRGR |
|
REG | Reference to a national code |
Ref country code: ES Ref legal event code: FG2A Ref document number: 2913242 Country of ref document: ES Kind code of ref document: T3 Effective date: 20220601 |
|
REG | Reference to a national code |
Ref country code: LT Ref legal event code: MG9D |
|
REG | Reference to a national code |
Ref country code: AT Ref legal event code: MK05 Ref document number: 1467160 Country of ref document: AT Kind code of ref document: T Effective date: 20220209 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: RS Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20220209 Ref country code: LT Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20220209 Ref country code: HR Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20220209 Ref country code: BG Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20220509 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: PL Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20220209 Ref country code: LV Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20220209 Ref country code: GR Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20220510 Ref country code: FI Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20220209 Ref country code: AT Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20220209 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: IS Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20220609 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: SM Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20220209 Ref country code: SK Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20220209 Ref country code: RO Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20220209 Ref country code: EE Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20220209 Ref country code: CZ Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20220209 |
|
REG | Reference to a national code |
Ref country code: DE Ref legal event code: R097 Ref document number: 602016068980 Country of ref document: DE |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: AL Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20220209 |
|
PLBE | No opposition filed within time limit |
Free format text: ORIGINAL CODE: 0009261 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT |
|
26N | No opposition filed |
Effective date: 20221110 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: SI Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20220209 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: MC Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20220209 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: NO Payment date: 20230814 Year of fee payment: 8 Ref country code: IT Payment date: 20230725 Year of fee payment: 8 Ref country code: ES Payment date: 20230901 Year of fee payment: 8 Ref country code: CH Payment date: 20230901 Year of fee payment: 8 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: SE Payment date: 20230804 Year of fee payment: 8 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: HU Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT; INVALID AB INITIO Effective date: 20160829 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: CY Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20220209 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: MK Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20220209 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: LU Payment date: 20240715 Year of fee payment: 9 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: NL Payment date: 20240723 Year of fee payment: 9 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: MT Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20220209 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: DE Payment date: 20240716 Year of fee payment: 9 Ref country code: IE Payment date: 20240828 Year of fee payment: 9 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: DK Payment date: 20240812 Year of fee payment: 9 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: GB Payment date: 20240830 Year of fee payment: 9 Ref country code: PT Payment date: 20240716 Year of fee payment: 9 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: BE Payment date: 20240821 Year of fee payment: 9 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: FR Payment date: 20240722 Year of fee payment: 9 |