EP3344379B1 - Method and device for continuously treating a mixture - Google Patents

Description

The invention relates to a method for continuously treating a mixture and a device for such treatment.

More particularly, the invention relates to a method for treating a mixture by high-frequency piezoelectric vibration.

Methods for preparing a stable emulsion comprising a lipid phase in an aqueous phase using piezoelectric transducers are already known. In particular, the patent FR 2 947 186 describes a method for preparing an oil-in-water emulsion produced in a container in which is immersed a piezoelectric transducer operating at high frequencies, in particular greater than 900 kHz. This preparation process 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 low energy consumption of the process to prepare the 'emulsion.

However, although such a process is satisfactory, it requires a preparation time which is generally long, in particular for the preparation of a large volume of emulsion or emulsion containing a high proportion of dispersed phase, in particular greater than at 30%.

US 4,071,225 discloses a method according to the preamble of claim 1 and a device according to the preamble of claim 11.

The invention thus aims to solve this drawback.

Thus, the invention relates to a process for treating a mixture according to claim 1.

The treatment method according to the invention makes it possible to treat the mixture continuously, while allowing incorporation of a large dispersed, aqueous or lipid phase, in a controlled manner and without degradation of materials.

In addition, a dispersion is obtained, in particular a rapid emulsification of the mixture. For example, the dispersion of 20% by weight 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 the patent FR 2 947 186 . With the method according to the invention, it is possible to obtain a continuous flow rate of treated mixture of 750 mL/min as will be described below in more detail.

• au moins un étage est tel qu'il est dépourvu de deux transducteurs disposés face à face et parallèles l'un de l'autre ; autrement dit, sur un étage ou même plusieurs étages, on évite la configuration où deux transducteurs seraient disposés en vis-à-vis respectivement sur deux parois parallèles encadrant du produit à traiter; grâce à cette disposition, on évite la formation d'ondes stationnaires (transducteurs face-à-face) qui seraient contre-productives pour le résultat recherché ;
• l'application de l'énergie vibratoire est adaptée pour former une émulsion et/ou des liposomes et/ou des éléments de vectorisation de principe actif ;
• le mélange ne contient pas d'émulsifiant ajouté ;
• le mélange une fois traité est stable pendant au moins deux semaines, voire au moins deux ans à température ambiante ;
• la première phase est une phase aqueuse tandis que la seconde phase est une phase lipidique, ou inversement ;
• la section transversale de la paroi du tube est polygonale, la section polygonale comprenant un nombre impair de côtés ;
• la paroi délimite un espace intérieur dans lequel on fait circuler le mélange, les transducteurs étant disposés sur la paroi en dehors de l'espace intérieur ;
• les transducteurs sont disposés selon plusieurs positions discrètes correspondant chacune à un plan de section transversal à la paroi du tube ;
• les transducteurs sont adaptés pour opérer à des fréquences différentes, les transducteurs étant disposés dans un ordre de fréquence croissant sur le tube ; et
• le mélange circule de façon répétée dans le tube jusqu'à ce que la première phase présente une granulométrie micrométrique ou nanométrique, de préférence monodisperse,
• le nombre de transducteurs à chaque étage est supérieur ou égal au nombre de transducteurs de l'étage précédent.

In various embodiments according to the present invention, one and/or the other of the following arrangements, taken separately or in combination, according to which:

• at least one stage is such that it does not have two transducers arranged face to face and parallel to each other; in other words, on one floor or even several floors, the configuration is avoided where two transducers would be arranged facing each other respectively on two parallel walls framing the product to be treated; thanks to this arrangement, the formation of standing waves (face-to-face transducers) which would be counter-productive for the desired result is avoided;
• the application of vibrational energy is suitable for forming an emulsion and/or liposomes and/or active principle vectorization elements;
• the mixture contains no added emulsifier;
• the mixture, once treated, is stable for at least two weeks, or even at least two years at ambient temperature;
• the first phase is an aqueous phase while the second phase is a lipid phase, or vice versa;
• the cross section of the tube wall is polygonal, the polygonal section comprising an odd number of sides;
• the wall delimits an interior space in which the mixture is circulated, the transducers being arranged on the wall outside the interior space;
• the transducers are arranged in several discrete positions, each corresponding to a section plane transverse 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 particle size, preferably monodisperse,
• the number of transducers in each stage is greater than or equal to the number of transducers in the previous stage.

The invention also relates to a device for treating a mixture according to claim 11.

The cross section of the tube wall is polygonal. According to one embodiment, the polygonal section comprising an odd number of sides p.

Of course, the different characteristics, variants and/or embodiments of the present invention can be associated with each other in various combinations insofar as they are not incompatible or exclusive of each other.

• la figure 1 est une vue schématique du dispositif pour mettre en œuvre le procédé de traitement d'un mélange selon l'invention ;
• la figure 1A représente une vue en coupe de la paroi du tube de la figure 1 selon le plan de section IA ;
• la figure 2 est une vue schématique d'une autre réalisation du dispositif pour mettre en œuvre le procédé de traitement d'un mélange selon l'invention ;
• la figure 3 représente la répartition granulométrique des gouttelettes d'eau dans une émulsion eau (5%) dans beurre de karité (95%) après six heures de traitement par le procédé selon l'invention ;
• la figure 4 représente la répartition granulométrique des gouttelettes d'eau dans une émulsion eau (5%) dans Matière Grasse Laitière Anhydre (MGLA ; 95%) après six heures de traitement par le procédé selon l'invention ;
• la figure 5 représente la répartition granulométrique des gouttelettes d'eau dans une émulsion eau (5%) dans huile essentielle d'origan (95%) après quatre heures de traitement par le procédé selon l'invention ;
• la figure 6 représente la répartition granulométrique des gouttelettes d'eau dans une émulsion eau (5%) dans huile d'olive (95%) après cinq heures de traitement par le procédé selon l'invention ;
• la figure 7 représente la répartition granulométrique des gouttelettes d'eau dans une émulsion eau (5%) dans huile d'olive (95%) après six heures de traitement par le procédé selon l'invention ;
• la figure 8 représente la répartition granulométrique des gouttelettes d'eau dans une émulsion eau (5%) dans huile d'olive (95%) après cinq heures de traitement par le procédé selon l'invention après stockage à température ambiante pendant une durée de deux ans ;
• les figures 9A à 9D représentent différentes réalisation du tube du dispositif selon l'invention ; et
• les figures 10A à 10M représentent différentes configurations de transducteurs sur le tube du dispositif selon l'invention ; et
• les figures 11A et 11B représentent respectivement la répartition granulométrique d'un mélange comprenant des liposomes après quatre heures de traitement par le procédé selon l'invention et une vue d'halos de lumière de nanoliposomes obtenues par diffusion dynamique de lumière avec un grossissement de 10000.

The present invention will be better understood and other characteristics and advantages will become apparent on reading the following detailed description comprising embodiments given by way of illustration with reference to the appended figures, presented by way of non-limiting examples, which may be used to complete the understanding of the present invention and the presentation of its realization and, if necessary, contribute to its definition, on which:

• the figure 1 is a schematic view of the device for implementing the process for treating a mixture according to the invention;
• the Figure 1A shows a sectional view of the tube wall of the figure 1 according to section plan IA;
• the figure 2 is a schematic view of another embodiment of the device for implementing the process for treating a mixture according to the invention;
• the picture 3 represents the particle size distribution of the water droplets in a water (5%) in shea butter (95%) emulsion after six hours of treatment by the method according to the invention;
• the figure 4 represents the particle size distribution of the water droplets in a water emulsion (5%) in Anhydrous Dairy Fat (MGLA; 95%) after six hours of treatment by the process according to the invention;
• the figure 5 represents the particle size distribution of the water droplets in an emulsion of water (5%) in essential oil of oregano (95%) after four hours of treatment by the process according to the invention;
• the figure 6 represents the particle size distribution of the water droplets in a water (5%) in olive oil (95%) emulsion after five hours of treatment by the process according to the invention;
• the figure 7 represents the particle size distribution of the water droplets in a water (5%) in olive oil (95%) emulsion after six hours of treatment by the process according to the invention;
• the figure 8 represents the particle size distribution of the water droplets in a water (5%) in olive oil (95%) emulsion after five hours of treatment by the method according to the invention after storage at room temperature for a period of two years;
• the figures 9A to 9D represent different embodiments of the tube of the device according to the invention; and
• the figures 10A to 10M represent different configurations of transducers on the tube of the device according to the invention; and
• the figures 11A and 11B respectively represent the particle size distribution of a mixture comprising liposomes after four hours of treatment by the method according to the invention and a view of halos of light of nanoliposomes obtained by dynamic light scattering with a magnification of 10000.

Below is a detailed description of several embodiments of the invention accompanied by examples and reference to the drawings.

The figure 1 represents an embodiment of a device 1 configured to implement the method for processing a mixture 2 according to the invention.

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 powder form. The first phase 2a and the second phase 2b are not mutually miscible. By immiscible, it is therefore understood that the first phase 2a and the second phase 2b cannot be mixed, in particular at ambient temperature (ie approximately twenty degrees Celsius), to obtain a completely homogeneous mixture. Unless specified On the contrary, the percentages of first phase 2a or of second phase 2b in the embodiments described below are mass percentages.

The first phase 2a can be an aqueous phase, while the second phase 2b is a lipid phase, or vice versa.

The term lipid phase (or lipophilic or hydrophobic) designates all oily substances, liquid at the temperature of implementation of the process, natural, vegetable or animal, or synthetic having or not having one or more proven biological activities, and insoluble in the water (less than 2% by weight at room temperature). By way of non-limiting illustration of these lipid phases, mention may in particular be made, for the food industry, of vegetable oils (olive, sunflower, rapeseed, peanut, mixtures of vegetable oils, etc.), animal oils (fish, etc.) , butters. Mention may also be made, as an example of a lipid phase, in particular for dermatology and cosmetics, of avocado, argan and other vegetable oils, essential oils, mineral oils.

The term aqueous (or hydrophilic) phase denotes any phase containing water and/or alcohol. Mention may be made of water that is softened or not, distilled or not, mineral or not, spring water, ultra-pure water, floral waters, fruit waters.

Furthermore, mixture 2 may comprise one or more additives. An additive can be added to one of the first or second phases 2a, 2b, depending on whether it is fat-soluble or water-soluble. If necessary, such an additive can be solubilized beforehand in a solvent. By way of non-exhaustive example, in the food sector, a biomolecule of interest can be added in the aqueous phase (peptides, vitamins, flavonoids, etc.) or in the lipid phase (triacylglycerols, fatty acids, aromas, etc. ). In general, the composition of mixture 2 typically depends on the intended end use of mixture 2 once treated by the process.

Preferably, mixture 2 does not include an emulsifier or compound suitable for facilitating the dispersion of the first phase 2a in the second phase 2b during the treatment of mixture 2. In particular, mixture 2 does not include an emulsifier, surfactant, stabilizer, or any other additive of any kind suitable for preventing or slowing down the separation of the dispersion of the first phase 2a and of the second phase 2b of the mixture 2. However, in certain specific embodiments of the method, in particular to form liposomes as will be described later, mixture 2 may comprise an emulsifier such as phospholipids.

As shown on the figure 1 , the device 1 comprises at least one tube 3. By tube 3, there is understood a conduit which is not necessarily cylindrical, but which 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 mixture 2 is carried out when mixture 2 circulates in 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 fully transmits the ultrasonic vibrations; the wall 4 produces no attenuation or amplification because its main natural frequencies 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 direction of circulation Sc of the mixture 2 in the tube 3 going from the inlet portion 3a to the outlet portion 3b.

According to one embodiment, the tube 3 is straight between the inlet portion 3a and the outlet portion 3b as shown in the figure 1 . This also defines a circulation direction Dc 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 downwards while the outlet portion 3b is located upwards (the terms “top” and “bottom” to be understood according to their current meanings). However, this embodiment is not limiting and the tube 3 can also be arranged horizontally, for example as shown in the figures 1 and 2 , or according to any other inclination.

According to another embodiment not shown, the tube 3 may further comprise at least one or more curved portions. The tube 3 can then have the shape of a serpentine, a spiral or be corrugated, in order to minimize the space occupied by the device 1.

The wall 4 of the tube 3 can be made of stainless steel, glass, Plexiglas, plastic or other materials. Preferably, the tube 3 is made of stainless steel and/or a plastic material. The wall 4 of the tube is thin with regard to the length of each side and/or the useful passage section of the treated product.

Preferably, the material of the wall 4 of the tube 3 is neutral, or inert, with respect to the mixture 2. In particular, the material of the wall 4 of the tube 3 is not degraded in contact with the mixture 2. By way of example, a tube 3 made of polytetrafluoroethylene (PTFE) is not degraded on contact with essential oils.

The wall 4 of the tube 3 is advantageously of substantially polygonal section. Thus, the wall 4 of the tube 3 may in particular comprise slightly rounded corners between its different faces as shown in the Figure 1A . In particular, 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. In other words, the polygonal section includes an odd number of sides p. The figures 9A to 9D show examples of realization in perspective of the tube 3 whose sections of the wall 4 are respectively triangular, pentagonal, heptagonal and enneagonal.

The device 1 also comprises transducer elements 6. These transducers 6 make it possible to apply 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 suitable for stable operation in the chosen frequency range and their manufacturing technology is well mastered. The transducers 6 can have various shapes, in particular in the form of a disc or more or less elongated and extended elements.

The transducers 6 are arranged on the wall 4 of the tube 3. The transducers 6 are in particular fixed to the wall 4 of the tube 3, by glue, a joint or any other fixing element.

The transducers 6 can be placed on the wall 4 inside the tube 3, that is to say in the interior space 5 delimited by the tube 3. Alternatively, the transducers 6 can be advantageously placed outside 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 cross 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 interior space 5 of the tube, for example sterile, which may be necessary for cosmetic and pharmaceutical applications of the mixture 2. This also facilitates the cleaning of the tube 3 and limits the possible contamination of the mixture 2 by a degradation of the elements fixing the transducers 6 to the wall 4. According to yet another variant, each of the transducers 6 can be arranged in a cavity passing through the wall 4. A seal lets nsuite sealing the cavity once the transducer disposed inside thereof.

According to one embodiment, 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. Thus, the energy vibration emitted by the transducers 6 has a component perpendicular to the wall 4 of the tube 3, and in particular perpendicular to the direction of circulation Dc of the mixture 2.

According to another embodiment, part or all of the transducers 6 can also be inclined with respect to the wall 4 of the tube 3, so that the vibratory energy emitted presents, in addition to its component perpendicular to the direction of circulation Dc of the mixture 2, a component parallel to the direction of circulation Dc and oriented for example in the opposite direction to the direction of circulation Sc. This positioning of the transducers 6 can indeed make it possible to increase the efficiency of the method.

The transducers 6, in particular all the transducers 6, are suitable for operating in a so-called high-frequency frequency range, that is to say greater than 900 kHz, or even greater than 1000 kHz. In particular, the transducers 6, in particular all the transducers 6, are adapted to operate in a range of frequencies comprised between 900 kHz and 3 MHz, more preferably between 900 kHz and 2000 kHz, even more preferably between 1400 and 1800kHz. The application of high frequency vibratory energy by means of transducers 6 has the advantage of eliminating the phenomenon of cavitation generally used for its shear intensity. Indeed, the frequency ranges conventionally used 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 up to several hundreds of degrees Celsius and where the pressure rises sharply. This cavitation shears the mixture 2 which allows rapid emulsification but causes the physico-chemical 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.

According to one embodiment, 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 to be understood as previously), can make it possible to obtain more stable emulsions and in which the quantity of dispersed phase is greater while reducing the required treatment time. For this purpose, the transducers 6 can for example operate according to three different frequencies F1, F2, F3, the transducers 6 being arranged in an order of increasing frequency. In other words, the transducers 6 having the lowest frequency F1 are located close to the inlet portion 3a of the tube 3.

The transducers 6, in particular the active transducers (that is to say which emit vibrational energy during the treatment of the mixture 2), are arranged discretely on the polygonal wall 4 of the tube 3 by "floor". A stage is defined by a plane of section transverse to the wall 4 of the tube 3. A plane of section transverse 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 situated in the plane transverse to the direction of local circulation of the product to be treated.

As shown on the figures 9A to 9D and 10A to 10M , nine stages of transducers 6 can be arranged on the tube 3. In particular, all the transducers 6 represented on the figures 9A to 9D are not necessarily active, and some may be inactive as will be explained below.

According to one embodiment, two consecutive stages of transducers 6 are spaced apart by a distance d of less than 30 centimeters, in particular of the order of 10 centimeters. However, the stages of transducers 6 are not all necessarily spaced apart by the same distance d. The distance d is more particularly measured between the centers of two transducers 6 arranged on the same face of the tube 3 and belonging respectively to two consecutive stages. In one stage, the transducers 6 are arranged on the faces of the polygonal wall 4 of the tube 3. As will be described below, the arrangement of the transducers in different stages forms a "pattern" or a succession of patterns capable of responding to determined construction rules in order to optimize the treatment of the mixture 2.

Preferably, due to the odd polygonal shape of the wall 4 of the tube 3, two transducers 6 of a stage are not arranged facing each other. In other words, two transducers 6 are not arranged facing directly parallel to each other. In fact, the interaction of the vibratory waves emitted by two face-to-face transducers is capable of causing the appearance of a stationary wave of the mixture 2 creating zones 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. Thus, the first phase 2a and the second phase 2b can initially be simply combined without prior mixing in container 7.

As a variant, the first phase 2a and the second phase 2b can also be the subject of a premix. For this purpose, a mechanical or membrane mixing device 8 can be used in the container 7. As a variant, the pre-mixing can be carried out by applying vibrational 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 subsequent stage of treatment of the mixture 2 without, however, allowing a stable mixture 2 to be obtained alone. A pump can also be used to introduce one of the phases gradually into the container 7 during this pre-mixing. Furthermore, several pumps can also be used to introduce each phase 2a, 2b and possibly other additives, of the mixture 2 into the container 7.

According to one embodiment, 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 lead to a degradation of the materials of the wall 4 of the tube 3 or of the other elements of the device 1.

According to another embodiment, a cooling system 10 makes it possible to cool the mixture 2 beforehand or during the treatment according to the method. This makes it possible in particular to treat the mixture 2 cold, to easily limit the losses and/or degradations of the mixture 2 linked to an excessively high temperature.

The heating 9 and/or cooling 10 systems make it possible in particular, for specific implementation or fragility needs, to keep the temperature of the treated phases 2a, 2b constant throughout the process.

According to another embodiment, a pH control system 11, or possibly several systems 11 distributed over the tube 3, make it possible to regulate the pH of the mixture 2 during its treatment. Indeed, the treatment of the mixture is likely to lead to an acidification of the treated mixture 2, due to the specific organization of the HO ^- ions induced by the process in the mixture 2. A pH-stat coupled to a soda pump mounted on the tube 3 make it possible, for example, to regulate the pH of the mixture 2 to a determined value during the treatment.

Once the mixture 2 comprising the first phase 2a and the second phase 2b contained in the container 7, optionally pre-mixed, the mixture is then circulated in the tube 3 between the inlet portion 3a and the outlet portion 3b. For this purpose, the device can also comprise a pump 12, in particular peristaltic, adapted to allow the circulation of the mixture 2 in the tube 3. Depending on the configuration of the device 1, in particular the length of the tube 3 and the number of transducers 6, adjusting 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. As a variant, the circulation of the mixture is carried out by the effect of gravity, in particular 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 the transducers 6 are arranged. 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 special 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.

When the method is implemented, all of the interior space 5 of the tube 3 is preferably occupied by the mixture 2. Thus, the tube 3 does not include any free interior space, in order to limit the exchanges between the mixture 2 and the air which would be contained in this free space and which would be liable to lead to the dissolution of gas in 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 the figure 2 . The tube 3 can thus have different configurations, and can in particular have a length adapted to the mixture 2 to be treated. For this purpose, mixture 2 outlets or diversion passages may be provided located at different places on the tube 3 of the device 1 in order to adapt the duration of the treatment of the mixture 2.

As a variant, as for the examples which are described below, the mixture 2 can also circulate several times in a tube 3 in a recurring manner by a closed-loop system, until the desired treatment of the mixture 2 is obtained. Thus, the processing times given in the embodiments described below relate to the time during which the mixture 2 circulates in a closed loop in the device 1.

In general, the dimensions and the shape of the tube can vary according to the type of mixture 2 as well as the volume to be treated. By way of non-limiting example, 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 the shape of a disc of the order of approximately 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. Such a dispersion can be obtained by mixing 2 at the micrometric, 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. Of Preferably, the treatment of the mixture 2 does not lead to any alteration or chemical modification of the first and second phases 2a, 2b.

In the following, the generic terms “direct dispersion” or “oil-in-water dispersion” designate a dispersed mixture in which a lipid phase is dispersed in an aqueous phase (also denoted O/W). Conversely, the generic terms “inverse dispersion” or “water-in-oil dispersion” denote a dispersed mixture in which an aqueous phase is dispersed in a lipid phase (also denoted W/O).

Multiple or multiphase mixtures can also be obtained by several successive applications of the process according to the invention (also denoted O/W/O or W/O/W 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. In particular, the average particle size of the first phase 2a in the second phase 2b after treatment is less than 50 micrometers, more preferably less than 20 micrometers.

Shorter treatment times produce larger first phase 2a particles with a broad size distribution while longer treatment times produce smaller first phase 2a particles with very narrow size distributions; thus the stability of the treated mixture 2 is greater. The method is all the more rapid when it comprises a large number of stages of transducers 6. The processing time of the method also depends on the percentage by mass of the first phase 2a with respect to the second phase 2b.

According to one embodiment, the method makes it possible to obtain an emulsion. It is thus possible to obtain a simple, direct or inverse emulsion, or a multiple emulsion.

The method can also make it possible to obtain a structured mixture. In particular, the process makes it possible to obtain mixtures structured in monolayer, such as micelles or colloidosomes, in bilayer such as vesicles, simple liposome, membranes, or else in multilayer such as multilamellar liposomes.

The process according to the invention makes it possible in particular to obtain structured mixtures in the form of liposomes. Liposomes are in the form of lamellar capsules, whose 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 mixture 2 can also make it possible to obtain a vectorization of active principles or of molecules of interest, cosmetics and pharmaceuticals, such as coenzyme Q10. Liposomes allow for example the nano-encapsulation of active agents in the dispersed phase in order to protect these active agents from possible degradation during the storage of the mixture. The principles thus vectorized are more effective and more bioavailable when they are released into living organisms. Liposomes are particularly suitable for use in the food industry as a controlled release system for active agents because they are easily made, adaptable, they are biocompatible and are generally considered safe ( Generally Recognized As Safe - GRAS - by the 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 process 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.

At the end of the process, the treated mixture 2 obtained is stable. The stability of mixture 2, that is to say the macroscopic non-separation of the first phase 2a and the second phase 2b from each other, can last two weeks, several months, two years, or more and is therefore suitable for a industrial use. Mixture 2, once treated, can be used as it is or can be incorporated into other lipid or aqueous phases.

Construction rules have been established on the basis of analyzes and measurements in order 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 process. These rules have been established in particular for a tube 3 of triangular section, although these apply or can be transposed to the walls of tubes having other polygonal shapes. The construction rules can be combined with each other, by selectively choosing some of them or taking them into account in total, in order to form an optimal configuration of transducers 6 arranged on the tube 3.

• p : nombre de côtés de la section polygonale du tube dans lequel circule le mélange à traiter ;
• e : nombre d'étages de transducteurs sur le tube dans lequel circule le mélange ;
• i : indice de l'étage de transducteur sur le tube dans lequel circule le mélange. Par convention, on définit les étages en partant depuis la portion d'entrée 3a puis en allant vers la portion de sortie 3b du tube 3, le premier étage étant donc celui qui est situé le plus proche de la portion d'entrée ;
• nc_i : nombre de transducteurs placés sur les parois du tube dans lequel circule le mélange au ième étage ; et
• n_k : nombre d'étages successifs comportant un même nombre k de transducteurs. Ainsi, n_ci = k pour n_k étages successifs.

For this purpose, we first define the following elements:

• p: number of sides of the polygonal section of the tube in which the mixture to be treated circulates;
• e: number of transducer stages on the tube in which the mixture circulates;
• i: index of the transducer stage on the tube in which the mixture circulates. By convention, the stages are defined starting from the inlet portion 3a then going towards the outlet portion 3b of the tube 3, the first stage therefore being the one which is located closest to the inlet portion;
• nc _i : number of transducers placed on the walls of the tube in which the mixture circulates at the ith stage; and
• n _k : number of successive stages comprising the same number k of transducers. Thus, n _ci =k for n _k successive stages.

The configuration of the transducers 6 in stages of a pattern is noted as follows: (nc ₁ , nc ₂ , nc ₃ , nc ₄ , etc.). By way of example, the configuration noted (2, 3, 2, 2) thus comprises two transducers on the first stage, three transducers on the second stage, and two transducers on the third and fourth stages.

According to a first construction rule, and according to the invention, each stage comprises at most one transducer 6 on each face 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, nc _i ≤ p.

At least one stage comprises transducers 6 not regularly distributed around the periphery of the tube 3 More precisely, according to the invention, there are several successive processing stages along the tube and on at least one particular stage, there is an arrangement of active transducers not regularly distributed around the periphery of the tube 3 (in other words the stage has no active transducers regularly distributed/spaced around its periphery).

For example, on a triangular section, according to a first configuration, a first face comprises an active transducer, and the other two faces do not contain an active transducer; according to 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).

Even if on the stage in question there is the presence of as many transducers as there are faces, at least one of the transducers is not activated which makes it possible to obtain the particular characteristic of absence of regular distribution on the periphery.

This particular characteristic of the absence of regular distribution on the periphery unexpectedly gives better results than those obtained with a regular distribution.

According to a second construction rule, and according to the invention, there is no stage comprising a single transducer.

In other words, n ₁ = 0.

According to a third construction rule, at least the first stage comprises two transducers. In other words, nc ₁ =2. This third construction rule differs in particular from known transducer configurations which generally seek to maximize the number of transducers for each of the stages in order to allow a greater vibratory shear applied to the mixture.

According to a fourth construction rule, the number of transducers on each stage is at least equal to the number of transducers on the previous stage. In other words, nc _i+1 ≥ nc _i . Increasing the number of transducers on the last stages of a pattern makes it possible to accelerate the process and to process large volumes of mixture.

According to a fifth construction rule, the number of successive stages comprising the same number k of transducers is decreasing. In other words, n _k+1 ≤ n _k . This fifth rule of construction also differs from known transducer configurations which seek to have stages have more transducers and apply more vibrational energy to the mix to speed up mixing processing.

According to a sixth construction rule, there must be at least four floors on tube 3.

In other words, $\mathrm{and}={\displaystyle {\sum }_{{\mathrm{not}}_k=1}^p{\mathrm{not}}_k\ge 4}$

According to a seventh construction rule, 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 the mixture to be treated circulates.

According to an eighth rule of construction, and according to the invention, certain stages comprise two transducers and certain stages comprise three transducers. Between 50% and 75% of the stages include 2 transducers.

According to a ninth construction rule, the distance d between consecutive floors can be variable. The distance d is in particular less than thirty centimeters, preferably between ten and twenty centimeters.

According to a tenth construction rule, it is possible to multiply the number of transducers 6 of a pattern to reduce the processing time of the mixture 2. In the following, a stage without a transducer can be considered as a spacing between two adjacent stages.

The figure 10A to 10M represent possible configurations established from the construction rules described above. In these figures, the transducers represented in white are active while the transducers represented in dark and in dotted lines are then inactive, that is to say that they do not emit vibrational energy during the treatment of the mixture 2 ( which corresponds de facto to an absence of transducer).

Examples of transducer configuration rules Comparative example concerning the third construction rule

A 30% emulsion in continuous phase is produced with 2000 g of demineralized water at twenty degrees Celsius and 860 g of mint essential oil at twenty degrees Celsius. The pre-mixing of the emulsion is done by sonication. It is then processed for four hours by piezoelectric transducers arranged on the three sides of a stainless steel tube with a triangular section. The transducer stages are 10 centimeters apart. A pH-stat and a caustic pump (0.1% by mass) 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.

With a configuration of transducers comprising stages of two and three transducers over five stages but whose first stages comprise 2 transducers, (2, 2, 2, 3, 3), the emulsion produced shows no phase separation after 30 days. storage at room temperature.

With a transducer configuration comprising stages of two and three transducers in alternating five stages (2, 3, 2, 3, 2), approximately 6% of the emulsified oil separated from the emulsion after 30 days of storage at room temperature, which therefore exhibits phase separation.

With a transducer configuration comprising stages of two and three transducers out of five stages but with the first stages comprising 3 transducers, (3, 3, 2, 2, 2), approximately 25% of the emulsified oil separates from the emulsion after 30 days of storage at room temperature, which therefore exhibits phase separation.

Thus, a configuration starting with stages comprising two transducers makes it possible to obtain better stability of the mixture treated in accordance with the third construction rule specified above.

Comparative example concerning the sixth construction rule

A 30% emulsion in continuous phase is produced with 2000 g of demineralized water at twenty degrees Celsius to which is gradually added 860 g of sunflower oil at twenty degrees Celsius. A membrane emulsification system allows the addition of oil during processing. The emulsion is processed for four hours by piezoelectric transducers placed on the faces of a stainless steel tube with a triangular section. The transducer stages are 10 centimeters apart. A pH-stat and a caustic 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.

With a configuration of transducers comprising stages of two and three transducers on four stages (2, 2, 3, 3), the emulsion produced shows no phase separation after 30 days of storage at ambient temperature.

With a transducer configuration comprising stages of two and three transducers on three stages (2, 2, 3), approximately 22% of the emulsified oil separates from the emulsion after 30 days of storage at room temperature, and therefore presents a phase separation.

With a transducer configuration comprising two-stage and three-stage two-stage transducers (2, 3), approximately 61% of the emulsified oil separates from the emulsion after 30 days of storage at room temperature, and therefore exhibits separation phase.

Thus, a configuration comprising at least four stages of transducers makes it possible to obtain better stability of the mixture treated in accordance with the sixth construction rule specified above.

Comparative example concerning the eighth construction rule

An emulsion is made with 1500 g of demineralized water at seventy degrees Celsius to which is gradually added 1500 g of shea butter at 70 degrees Celsius. It is processed for four hours by piezoelectric transducers arranged on the three sides of a stainless steel tube with a triangular section. The transducer stages are 8 centimeters apart. A pH-stat and a caustic pump (0.1% by mass) 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 pre-mixing system is used upstream of the tube. The butter is gradually added to the level of the premix at a rate of 10 g/min. The mixture circulates in the device at a speed of 900 g/min.

With a configuration of transducers comprising stages of two and three transducers on five stages (2, 2, 2, 3, 3), the emulsion produced shows no phase separation after 30 days of storage at room temperature, this being stable.

With a configuration implemented comprising only stages of two transducers out of five stages (2, 2, 2, 2, 2), the emulsion produced shows a significant phase separation after 30 days of storage at room temperature. In particular, approximately 45% of the emulsified shea butter separates from the emulsion.

With a configuration implemented comprising only stages of three transducers out of five stages (3, 3, 3, 3, 3), the emulsion produced shows a significant phase separation after 30 days of storage at room temperature. In particular, approximately 72% of the emulsified shea butter separates from the emulsion.

Thus, a configuration comprising both stages of two transducers and stages of three transducers makes it possible to obtain better stability of the mixture treated in accordance with the eighth construction rule specified above.

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 pre-mixing of the emulsion is done via a high pressure homogenizer. It is then processed for four hours by piezoelectric transducers arranged on the three sides of a stainless steel tube with a triangular section. The transducer stages are 6 centimeters apart. A pH-stat and a caustic pump (0.1% by mass) 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.

With a configuration of transducers comprising 50% of stages of two transducers and 50% of stages of three transducers on four stages (2, 2, 3, 3), the emulsion produced shows no phase separation after 30 days of storage at room temperature, which is stable.

With a configuration of transducers comprising 75% of stages of two transducers and 25% of stages of three transducers on four stages (2, 2, 2, 3), the emulsion produced shows no phase separation after 30 days of storage at room temperature, which is stable.

With a configuration of transducers comprising 25% of stages of two transducers and 75% of stages of three transducers on four stages (2, 3, 3, 3), the emulsion produced shows a significant phase separation after 30 days of storage at room temperature. In particular, about 7% of the emulsified oil separates from the emulsion.

Thus, a configuration comprising at least 50% of stages of two transducers makes it possible to obtain better stability of the mixture treated in accordance with the eighth construction rule specified above.

Comparative example concerning the ninth construction rule

A 30% emulsion in continuous phase is produced with 2000 g of demineralised water at twenty degrees Celsius to which is gradually added 860 g of liquid paraffin oil, very apolar, at twenty degrees Celsius. It is processed for four hours by piezoelectric transducers arranged on the three sides of a stainless steel tube with a triangular section. The transducer stages are 20 centimeters apart. A pH-stat and a caustic pump (0.1% by mass) 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.

With a configuration of transducers comprising stages of two and three transducers over five stages (2, 2, 2, 3, 3), the emulsion produced shows no phase separation after 30 days of storage at ambient temperature.

With a configuration of transducers comprising stages of two and three transducers over five stages alternating with stages comprising no transducers (2, 0, 2, 0, 2, 0, 3, 0, 3), the emulsion produced does not shows no phase separation after 30 days storage at room temperature. According to this configuration, two consecutive stages comprising transducers are 18 centimeters apart.

With a transducer configuration comprising stages of two and three transducers over five stages alternating with stages comprising no transducers (2, 0, 0, 2, 0, 0, 2, 0, 0, 3, 0, 0, 3), the emulsion produced exhibits significant phase separation after 30 days of storage at room temperature. In particular, about 75% of the emulsified oil separates from the emulsion. According to this configuration, two consecutive stages comprising transducers are 28 centimeters apart.

Thus, a variation of the distance d between the stages of transducers does not influence the stability of the mixture treated in accordance with the ninth rule of construction specified above. It is however necessary that the stages of transducers 6 remain sufficiently close together and in particular separated by a distance d of less than twenty-eight centimeters.

Comparative example concerning the tenth construction rule

A 30% emulsion in continuous phase is produced with 2000 g of demineralized water at twenty degrees Celsius to which is gradually added 860 g of olive oil at twenty degrees Celsius. It is processed for four hours by piezoelectric transducers arranged on the three sides of a stainless steel tube with a triangular section. The transducer stages are 1.5 centimeters apart. A pH-stat and a caustic pump (0.1% by mass) 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.

With a configuration comprising stages of two and three transducers on four stages (2, 2, 3, 3) and a processing time of four hours, the emulsion produced shows no phase separation after 30 days of storage at room temperature. .

With a configuration comprising stages of two and three transducers on eight stages (2, 2, 3, 3, 2, 2, 3, 3) and a treatment time of two hours, the emulsion produced shows no phase separation. after 30 days of storage at room temperature. With a configuration comprising stages of two and three transducers on eight stages (2, 2, 2, 2, 3, 3, 3, 3) and a treatment time of two hours, the emulsion produced shows no phase separation. after 30 days of storage at room temperature. With a configuration comprising two and three transducer stages on four stages (2, 2, 3, 3) and a treatment time of two hours, approximately 43% of the emulsified oil separates from the emulsion after 30 days of storage at room temperature.

Thus, the duration of treatment as well as the number of stages of transducers influence the stability of the mixture treated in accordance with the tenth rule of construction specified above.

Example of mixture

Examples of mixture treated according to the process of the invention are described below.

Realization of liposomes in an aqueous phase

A 90% emulsion in continuous phase is produced with 900 g of demineralized water at twenty degrees Celsius to which is added 100 g of phospholipids at twenty degrees Celsius. It is processed for two hours by piezoelectric transducers arranged on the three sides of a stainless steel tube with a triangular section. The configuration implemented includes stages with two transducers and three transducer stages 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 the treatment. A mechanical premix is carried out prior to the circulation of the phases in the tube 3. The dispersion circulates in the tube at a speed of 60 g/min.

At the end of the treatment, a microscopic observation as represented on the figure 11B reveals the presence of liposomes in the mixture 2 having a diameter of the order of 200 nanometers. The figure 11A represents in particular the particle size distribution of these liposomes in the mixture 2. After 30 days of storage at room temperature, the mixture 2 produced shows no phase separation.

Production of coenzyme Q10 vectors

A 15% continuous phase emulsion is produced with 1800g of demineralised water at twenty degrees Celsius and a mixture of 167g of rapeseed oil and 33g of coenzyme Q10 at twenty degrees Celsius. The pre-mixing of the emulsion is done via a high pressure homogenizer. It is then processed for four hours by piezoelectric transducers arranged on the three sides of a stainless steel tube with a triangular section. The implemented configuration includes stages of two transducers and three transducers on four stages (2, 2, 3, 3). Each of the transducer stages are 6 centimeters apart. A pH-stat and a caustic pump (0.1% by mass) 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, having all the properties, in particular antioxidant, of the molecule of interest. After 30 days of storage at room temperature, the emulsion produced shows no phase separation. .

Production of a powder suspension

A 5% suspension in continuous phase is produced with 1425 g of demineralised water at twenty degrees Celsius and a mixture of 75 g of an iron oxide powder at twenty degrees Celsius. The pre-mixing of the emulsion is done via a mechanical agitation system. It is then processed for four hours by piezoelectric transducers arranged on the three sides of a stainless steel tube with a triangular section. The implemented configuration includes stages of two transducers and three transducers on four stages (2, 2, 3, 3). Each of the floors of transducers are 8 centimeters apart. A pH-stat and a caustic pump (0.1% by mass) 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.

After 30 days of storage at room temperature, the suspension produced shows no phase separation.

Realization of inverse emulsions

Several tests have been carried out with different oils: anhydrous butter and olive oil for the food sector, shea butter and essential oil of oregano for cosmetics.

Mixes 2 were made as follows: Reference Mixed (%) Emulsification time (hour) Fig. 1 95% shea butter + 5% distilled water 6am 3 2 95% MGLA+ 5% distilled water 6am 4 3 95% oregano essential oil + 5% distilled water 4h 5 4 95% olive oil + 5% distilled water 5am 6

The figures 3 to 6 illustrate the particle size dispersion of the water droplets which remain suspended in the lipid phase thus forming an inverse emulsion.

Furthermore, inverse emulsions can be characterized by dynamic light diffraction. In particular, the figure 7 represents 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 process. As can be seen in this figure 7 , 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 droplet diameter of this emulsion is 175 nanometers.

Stability study

An emulsion of water in olive oil as produced referenced 4 above was stored at room temperature for a period of two years. The figure 8 thus shows the particle size distribution of the particles of the emulsion measured just after its treatment (curve in solid line) as well as measured after its storage for two years (in dotted line). The measurement of 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 period of the emulsion. However, this emulsion does not show any phase separation phenomenon and the average size of the droplets remains of the order of 100 nm to 200 nanometers. In addition, the emulsion stored for a period of two years does not show any apparent phenomenon of destabilization, phase separation, or decantation of 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 pose problems of comfort, irritation, allergy or intolerance. such as in the agri-food, dermatology, cosmetics, relaxation products and pharmacy sectors. Other interesting sectors are, for example, paint or polymers. Of course, the elimination of emulsifiers makes it possible to reduce costs, and therefore has an appeal in all the preparations of emulsions on an industrial scale. The mixtures treated by the process according to the invention can be creams, lotions, sprays and any other form of distribution of pharmaceutical and/or cosmetic product.

Obviously, the invention is not limited to the embodiments described above and provided solely by way of example. It encompasses various modifications, alternative forms and other variants that a person skilled in the art may consider in the context of the present invention and in particular all combinations of the various modes of operation described previously, which may be taken separately or in combination.

Thus, it is also possible to envisage treating the mixture, not by continuous treatment in a tube, but by successive treatment steps in several containers each comprising one or more transducers operating at high frequencies. In particular, the mixture 2 can be treated first of all in a first container in which the transducer(s) operate at a frequency F1 and then be transferred into a second container in which the transducer(s) operate at a frequency F2 different from the frequency F1, and so on continue if necessary until the complete treatment of the mixture. This thus makes it possible to obtain a stable mixture by the successive application of vibratory energy according to different frequencies F1, F2.

Claims (12)

1. Method for treating a mixture (2) comprising at least a first phase (2a) and a second phase (2b) which cannot be mixed with one another, the method comprising the steps of:

   - circulating the mixture (2) in a tube (3) comprising a wall (4) and extending between an inlet portion (3a) and an outlet portion (3b), the tube having a polygonal section, and

   - applying vibratory energy to the mixture (2) by means of a plurality of transducers (6) arranged on the wall (4) of the tube (3) and operating at a frequency greater than 900 kHz, the vibratory energy making it possible to disperse the first phase (2a) in the second phase (2b), the transducers (6) being arranged in a plurality of positions forming a plurality of successive treatment stages along the tube (3),

   characterized in that each stage comprises at most one transducer on each surface of the polygonal section;

   in that, at least in one stage, the active transducers are not evenly distributed over the circumference of the tube (3);

   in that there are at least two transducers per stage;

   in that there are stages having two transducers and stages having three transducers; and

   in that the number of transducers in 50% to 75% of stages is two.
2. Method according to claim 1, wherein the first phase (2a) is an aqueous phase while the second phase (2b) is a lipid phase, or vice versa.
3. Method according to claim 1, wherein at least one stage is such that it is devoid of two transducers (6) arranged opposite and in parallel with one another.
4. Method according to any of the preceding claims, wherein the polygonal section comprises an odd number of sides (p).
5. Method according to any of the preceding claims, wherein the application of vibratory energy is suitable for forming an emulsion and/or liposomes and/or elements for vectorization of the active principle.
6. Method according to any of the preceding claims, wherein the mixture (2) does not include an added emulsifier.
7. Method according to any of the preceding claims, wherein the mixture (2), once treated, is stable for at least two weeks, or even at least two years at room temperature.
8. Method according to any of the preceding claims, wherein the number of transducers in each stage is greater than or equal to the number of transducers in the previous stage.
9. Method according to any of the preceding claims, wherein the wall (4) delimits an internal space (5) in which the mixture (2) is circulated, the transducers (6) being arranged on the wall (4) outside the interior space (5).
10. Method according to any of the preceding claims, wherein the transducers (6) are suitable for operating at different frequencies (F1, F2, F3), the transducers (6) being arranged in order of increasing frequency on the tube (3).
11. Device (1) for treating a mixture (2) comprising at least a first phase (2a) and a second phase (2b) which cannot be mixed with one another, the device (1) comprising a tube (3) having a wall (4) and extending between an inlet portion (3a) and an outlet portion (3b), the tube having a polygonal section, and transducers (6) operating at a frequency greater than 900 kHz being arranged on the wall (4) of the tube (3) in a plurality of positions forming a plurality of successive treatment stages along the tube (3) so as to apply vibratory energy to the mixture (2),

    characterized in that each stage comprises at most one transducer on each surface of the polygonal section;

    the transducers are configured so that, at least in one stage, the active transducers are not evenly distributed around the circumference of the tube (3), in that there are at least two transducers per stage, in that there are stages having two transducers and stages having three transducers and in that the number of transducers in 50% to 75% of stages is two.
12. Device (1) according to claim 11, wherein the cross section of the wall (4) of the tube (3) is polygonal, the polygonal section comprising an odd number of sides (p).

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