EP1202795B1 - Method for making emulsions and implementing devices - Google Patents
Method for making emulsions and implementing devices Download PDFInfo
- Publication number
- EP1202795B1 EP1202795B1 EP00958582A EP00958582A EP1202795B1 EP 1202795 B1 EP1202795 B1 EP 1202795B1 EP 00958582 A EP00958582 A EP 00958582A EP 00958582 A EP00958582 A EP 00958582A EP 1202795 B1 EP1202795 B1 EP 1202795B1
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- Prior art keywords
- coherent jet
- phase
- dispersed phase
- emulsion
- jet
- Prior art date
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- 239000000839 emulsion Substances 0.000 title claims abstract description 77
- 238000000034 method Methods 0.000 title claims abstract description 21
- 230000001427 coherent effect Effects 0.000 claims abstract description 65
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 60
- 239000012530 fluid Substances 0.000 claims abstract description 38
- 239000000203 mixture Substances 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 230000000694 effects Effects 0.000 claims description 10
- 238000007654 immersion Methods 0.000 claims description 7
- 239000012263 liquid product Substances 0.000 claims description 3
- 230000003068 static effect Effects 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims 3
- 230000001804 emulsifying effect Effects 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- 239000003921 oil Substances 0.000 description 26
- 235000019198 oils Nutrition 0.000 description 26
- 229920001213 Polysorbate 20 Polymers 0.000 description 19
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 description 19
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 description 19
- 239000012141 concentrate Substances 0.000 description 12
- 239000006260 foam Substances 0.000 description 12
- KEUKAQNPUBYCIC-UHFFFAOYSA-N ethaneperoxoic acid;hydrogen peroxide Chemical compound OO.CC(=O)OO KEUKAQNPUBYCIC-UHFFFAOYSA-N 0.000 description 10
- 235000019486 Sunflower oil Nutrition 0.000 description 7
- 239000002600 sunflower oil Substances 0.000 description 7
- 230000033228 biological regulation Effects 0.000 description 4
- 239000002270 dispersing agent Substances 0.000 description 4
- 238000000265 homogenisation Methods 0.000 description 4
- 230000036961 partial effect Effects 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- 241000208838 Asteraceae Species 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000004581 coalescence Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 230000006641 stabilisation Effects 0.000 description 3
- 238000011105 stabilization Methods 0.000 description 3
- 238000010923 batch production Methods 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 230000001687 destabilization Effects 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000011144 upstream manufacturing Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 239000007764 o/w emulsion Substances 0.000 description 1
- 239000003348 petrochemical agent Substances 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 235000014438 salad dressings Nutrition 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
Images
Classifications
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- 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
- B01F23/4105—Methods of emulsifying
-
- 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
- B01F23/45—Mixing liquids with liquids; Emulsifying using flow mixing
- B01F23/451—Mixing liquids with liquids; Emulsifying using flow mixing by injecting one liquid into another
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/20—Jet mixers, i.e. mixers using high-speed fluid streams
- B01F25/23—Mixing by intersecting jets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/30—Injector mixers
- B01F25/31—Injector mixers in conduits or tubes through which the main component flows
- B01F25/313—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced in the centre of the conduit
-
- 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
- B01F33/834—Mixing in several steps, e.g. successive steps
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/71—Feed mechanisms
- B01F35/715—Feeding the components in several steps, e.g. successive steps
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F2101/00—Mixing characterised by the nature of the mixed materials or by the application field
- B01F2101/06—Mixing of food ingredients
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F2101/00—Mixing characterised by the nature of the mixed materials or by the application field
- B01F2101/22—Mixing of ingredients for pharmaceutical or medical compositions
Definitions
- the present invention relates to a method of manufacture of emulsions as well as an emulsifier this process.
- Such a process will find many applications, particularly in the fields of cosmetology, food industry for the making salad dressings for example, pharmacy, petrochemicals, etc.
- the manufacture of an emulsion consists of the mixture of two fluids, i.e. two liquids, determining two phases, by hypotheses not miscible, one being called dispersed phase and the other dispersing phase, one of which forms droplets microscopic in the other.
- This mixture or emulsion, and more particularly the size of the droplets of the dispersed phase in the dispersing phase depends in particular of energy supplied in the form of agitation to the medium which shears the fluid and thus allows the reduction in the size of the emulsion droplets.
- foam concentrates such as high pressure homogenizers or even "microfluidizers" producing emulsions comprising a emulsifier, for example an oil type emulsion in water.
- Homogenizers are conventionally made up a homogenization head and a high pressure pump to pressurize a fluid contained in a tank.
- the pressurized fluid is usually a pre-emulsion, i.e. it is a mixture partial of the dispersed phase, the dispersing phase and emulsifier; this fluid is then sent through the homogenization head mainly consisting of a base, valve and impact plates.
- the fluid is brutally relaxed through an appropriate opening, to reach a speed of the order of several hundreds of meters per second and then comes into contact with the valve which splits the fluid and projects it on the impact plates thus providing the necessary energy, in the form of agitation in the middle, for the manufacture of the emulsion.
- These homogenizers benefiting from current technologies operate at pressures up to 200 MPa.
- This module is mainly consisting of a cylindrical body each having its ends respectively a direct input block and an output block.
- the cylindrical body contains a succession of hollow and open cylindrical cartridges on one of their transverse faces and they are connected between them by springs.
- These cartridges contain a plurality of vibrating discs which can slide the along the central hollow axis of the cylindrical body of the module.
- microfluidizers conventionally made up of an interaction chamber and a high pressure pump to pressurize a fluid contained in a suitable reservoir.
- the fluid under pressure is usually a pre emulsion which is sent to the interaction room in which this last one is bombarded by itself with energy important brought by the pressurization of the fluid, this which allows the manufacture of the emulsion.
- a disadvantage of these devices is the important amount of emulsifier required to stabilize such emulsion. This high supply of emulsifier is then reflected by an excess of said emulsifier in the dispersing phase of the emulsion after its manufacture, which affects in particular the organoleptic qualities of the emulsion and increases the production costs.
- Document DE-A-2549026 describes, moreover, a emulsification process comprising the introduction of the dispersed phase in a jet of the dispersing phase and the mixing in a chamber of this jet with a part additional of the dispersing phase.
- Another disadvantage of all these devices is that provide an emulsion whose droplets have a average diameter of the order of a micrometer, which is not fully satisfactory for applications in food and cosmetology, by example.
- One of the aims of the invention is therefore to overcome these disadvantages by proposing a method of manufacturing a mixture or emulsion, for example of the oil type in water, to obtain greater fineness of the droplets using a minimum amount of emulsifier for stabilize said emulsion over time.
- the process for the continuous or batch production of a mixture or an emulsion from at least one emulsifier and at least two fluids known to be immiscible, for example a body fatty liquid mixed with water and an appropriate emulsifier, said fluids defining a dispersed phase and a dispersing phase is remarkable in that, the dispersed phase being either contained in a suitable tank, or delivered continuously, it comprises a first step of pressurizing the dispersed phase by conventional high-pressure pumping means, then a sudden depressurization of said dispersed phase is carried out using means making it possible to create a needle jet, that is to say a jet of narrow section, or coherent jet in which the dispersed phase can reach a speed of about 900 ms -1 . It is then conceivable to introduce the coherent jet of the dispersed phase into a dispersing phase in which an appropriate emulsifier has been dissolved to obtain the emulsion.
- the dispersed phase being either contained in a suitable tank,
- Such a method does not make it possible to obtain a size average droplet size small enough why, we prefer to introduce the appropriate emulsifier in said coherent jet by means ensuring the mixing the dispersed phase with said emulsifier.
- This resulting coherent jet is finally brought into contact with the dispersing phase to obtain the mixture or the emulsion.
- bringing the coherent jet into contact resulting with the dispersing phase is obtained by positioning said jet coherent resulting in immersion in the dispersing phase in a static or quasi-static position in means of racking.
- the implementation contact of the resulting coherent jet with the dispersing phase is obtained by means ensuring the introduction of the dispersing phase in said resulting coherent jet and simultaneously their emulsion which then constitutes a jet consistent final.
- the phase dispersed under pressure is regulated according to a range of temperature between -20 ° C and + 80 ° C so that the the emulsion is more homogeneous over time.
- the dispersed phase is pressurized to a pressure greater than or equal to 200 MPa.
- Another object of the invention relates to a device foam concentrate for continuous or batch production a mixture or an emulsion from at least one emulsifier and at least two fluids known to be immiscible, for example a fatty liquid product mixed with water and an emulsifier, said fluids defining a phase dispersed and a dispersing phase, and said device comprising a high pressure pump the inlet of which is connected to a fluid source such as a reservoir containing a dispersed phase;
- this device is remarkable in that the high pump output pressure is connected, by connection means, to means for projecting the dispersed phase in the form of a coherent jet cooperating with means of introduction, connected to an open tank and using the Venturi effect, of an emulsifier in said jet coherent emerging, in immersion, in the phase dispersant contained in means of continuous or discontinuous withdrawal of the emulsion.
- the pump outlet at high pressure is connected, by connection means, to means for projecting the phase dispersed under the form of a coherent jet, provided at their outlet with at least two introduction means which are mounted in series connected to an open tank respectively and using the Venturi effect, respectively at least the emulsifier in said coherent jet and phase dispersant in the resulting coherent jet, to provide the emulsion which is advantageously continuously recovered at the output of said introduction means or discontinuously.
- connection means between the high pressure pump and the projection means, are provided with temperature regulation means on all or part of their length.
- emulsion all mixtures and emulsions obtained according to the invention and by emulsifier all the mixing devices, homogenizer, "microfluidizer”, foam concentrate and homogenizer-emulsifier.
- the device for continuous or discontinuous emulsion which is represented on the Figures 1 to 4, includes a tank 1 containing a phase dispersed and the output of which is connected to a pump high pressure 2.
- a booster pump not shown on the figures, will advantageously be positioned between the tank 1 and the high pressure pump 2 to prime the latter in a conventional manner.
- connection means 3 to means of projection 4 of the dispersing phase in the form of a jet needle or coherent jet 5.
- the means of connection 3, between the high pressure pump 2 and the projection means 4 are provided with means for regulation 6 of the temperature of the dispersed phase, under pressure in said connection means 3, on all or part of their length.
- the output of the means of projection 4 is provided with introduction means 7 into the coherent jet 5 of an emulsifier contained in a second tank 8 connected to said means of introduction 7 of such so that when they come out a coherent jet resulting 9 consisting of the dispersed phase and the emulsifier.
- the resulting coherent jet 9 is then set contact with the dispersing phase contained in means withdrawal 10 continuously or discontinuously as is will see further.
- the resulting coherent throw 9 is preferably positioned in immersion in said phase dispersant to benefit from optimal energy, said resulting coherent jet, necessary to obtain a fine emulsion.
- the output of the introduction means 7 is provided with second introduction means 11, shown in dotted lines in FIG. 1, in the coherent jet resulting from a dispersing phase contained in a third tank 12, also shown in lines dashed in Figure 1, connected to said means introduction 11 so that when they come out a final coherent jet 13 consisting of the emulsion.
- the jet coherent final 13, i.e. the emulsion, is then collected continuously or discontinuously in the means of racking 10.
- the reservoir 1, containing the dispersed phase is connected to the high pump pressure 2 by a pipe 14.
- the high pressure pump 2 is advantageously a return pump which has a very short time constant which therefore does not present time out. It provides a pressure of 400 MPa while ensuring high flow and pressure constant.
- the connection means 3 between the pump high pressure 2 and the projection means 4, not shown in Figure 2 are constituted by a pipe armored 15 capable of carrying the dispersed pressurized phase and they have a branch circuit 16 provided with control valves 17 such as solenoid valves.
- the branch circuit 16 includes means for regulation 6 of the temperature of the dispersed phase pressurized, shown in dotted lines on the Figure 2.
- the regulating means 6 are, moreover, consisting of a coil of coils 18 surrounding the pipe shielded 15 on part of the branch circuit 16 and connected to a heat exchanger 19.
- the length of the coil 18 depends, in particular, on the heat coefficients of the fluid calorific circulating in said coil with turns 18 and of the dispersed phase used.
- the means of connection 3 may not include a circuit bypass 16 and the coil 18 will then be positioned directly around the armored pipe 15.
- the regulating means 6 comprise also a probe 20, preferably mounted upstream of the coil with turns 18 on the branch circuit 16, allowing to control the phase temperature dispersed in the armored pipe 15.
- the means projection 4 are conventionally mounted at the end of the armored pipe 15, facing the ground and they are made up a nozzle 21 supported by a nozzle holder 22 comprising a calibrated hole 23.
- the nozzle 21 is conventionally constituted a body 24 comprising at its lower end a second calibrated hole 25 and a needle 26 having a third hole calibrated 27 coaxial with first 23 and at second 25.
- the diameter of the calibrated hole 26 is advantageously between 0.08 and 0.15 mm for a pressure delivered by the high pressure pump 2 of 200 MPa in order to prevent said calibrated hole 26 from clogs.
- the projection means 4 can be directed upward to provide a straight stream.
- the nozzle 21 provides a needle jet, that is to say a jet of narrow section, or coherent jet 5 of the phase dispersed which is brutally depressurized and which gushes out in the introduction means 7.
- Said means introduction 7 are positioned at the lower end of the nozzle holder 22 and are constituted by a Venturi tube 28, with a length of about 15 mm for a pressure included between 200 MPa and 300 MPa, forming in its central part a mixing chamber 29 and at its lower end a focusing tube 30.
- the coherent jet 5 thus springs in the mixing chamber 29 where the emulsifier, initially contained in the reservoir 8 and which is brought, by a flexible conduit 31 provided with a control valve 17 and a flow control system 32, in the room 29 by Venturi effect, mix to provide in the focusing tube 30 a coherent jet resulting 9.
- the reservoir 8 is a reservoir open so that the emulsifier is under pressure atmospheric and can benefit from the Venturi effect for be brought into the mixing chamber 29. Furthermore, there it would be possible to introduce the emulsifier into the jet coherent dispersed phase by means of an incident jet making a very small angle with said coherent jet 5.
- the focusing tube 30 is positioned in immersion in a static or quasi-static dispersing phase contained in the withdrawal means 10 which are consisting of a main cylindrical container 33, a median cylindrical container 34 and a central cylinder 35 coaxial.
- the main cylindrical container 33 has the larger section and includes two openings 36.37 in its upper part for the introduction of a fluid calorific and two other openings 38.39 in its part lower for the output of said heat fluid, as we will see it later.
- the openings 36, 37, 38 and 39 of the main cylindrical container 33 are advantageously connected to the heat exchanger 19 by means of conventional connections not shown in the figures.
- the median cylindrical container 34 positioned inside of the main cylindrical container 33, includes a bottom reinforced 40 to avoid its deformation due to the pressure of the coherent jet resulting 9.
- the central cylinder 35 open to its two ends is positioned in the container cylindrical median 34 so that its end lower 41 is not in contact with the bottom reinforced 40. Furthermore, the cylindrical container median 34 and central cylinder 35 include respectively an opening 42 in its central part for drawing off the emulsion and an opening 43 in its upper part for the introduction of the phase dispersing as we will see later.
- the withdrawal means 10 can consist of a single cylindrical container comprising the dispersed phase and whether or not provided with a opening in its upper part for the introduction of the dispersing phase and another opening in its lower part for drawing off the emulsion either continuous, or discontinuous.
- the projection means 4 provide a coherent jet 5 which springs in a first Venturi tube 28 as described above allowing the mixture of the emulsifier, previously contained in the tank 8, with the phase dispersed and providing a jet coherent resulting 9 as already seen. Said jet resulting coherent 9 then springs into a second tube Venturi 44 mounted in series with the first 28 and forming a second mixing chamber 45 in its central part and a second focusing tube 46 in its lower part.
- the resulting coherent jet 9 thus flows in the second mixing chamber 45 where the dispersing phase, initially contained in the reservoir 12 then brought, by a conduit flexible 31 provided with a control valve 17 and a system flow control 32, in the second chamber mix 45 by Venturi effect, mix with said jet coherent resulting 9 to provide the flowing emulsion in the second focusing tube 46 in the form of a final coherent stream 13.
- the device can include several Venturi tubes mounted in series allowing to successively introduce into the coherent jet 5 several emulsifiers and several dispersing phases to manufacture so-called ternary emulsions such as water / oil / water type emulsions.
- the final coherent jet 13, that is to say the emulsion, is collected in the withdrawal means 10 placed at the vertical under the second focusing tube 46.
- the withdrawal means 10 then consist of a simple cylindrical container 47 provided with an opening 48 in its lower part to continuously draw the emulsion as indicated by arrow 49.
- the emulsion could be drawn off in discontinuous using a simple cylindrical container.
- FIGS. 2, 3, 5 and 6 The operation of the foam concentrate device according to the invention will now be explained with reference to FIGS. 2, 3, 5 and 6.
- the high-pressure pump 2 is primed which then pressurizes the oil in the armored pipe 15. Then actuates, if necessary, the various valves of control 17 so that the oil circulates in the bypass circuit 16 in order to regulate it in temperature.
- the pressurized oil spurts from the nozzle 21 (FIG. 3) to form a coherent jet 5 through the venturi tube 28.
- the oil is pressurized, preferably, at a pressure greater than or equal to 200 MPa so that the coherent jet 5 has sufficient energy to form the emulsion without the nozzle 21 becoming blocked.
- the oil speed can then reach 900 ms -1 for a pressure of 200 MPa and a diameter of the nozzle 21 of between 0.08 and 0.15 mm.
- Tween 20 the emulsifier used, Tween 20 being a registered trademark for an emulsifier. which we will call later "Tween 20".
- the "Tween 20" does not dissolve in the dispersed phase, that is to say the oil.
- the emulsifier dissolves only in the dispersing phase; thus, the "Tween 20" mixes with a homogeneously in coherent jet 5 without being there dissolves.
- the resulting coherent jet 9 is then introduced in immersion in water, corresponding to the dispersing phase, which is continuously injected into the central cylinder 35 through opening 43 as indicated by arrow 50 of the figure 3.
- the size of the emulsion droplets depends in particular on the energy brought in the form of agitation in the middle as we have already seen but also fluids used.
- the size of the droplets will depend in particular on the type of oil used.
- Figure 5 shows the percentage of droplets according to their diameter, expressed in nanometer (nm) for an oil-in-water type emulsion, including 10% sunflower oil, 89% water and 1% of emulsifier "Tween 20", and obtained by projecting a jet sunflower oil, pressurized to 200 MPa, in water in which the "Tween 20" was previously dissolved.
- the general shape of the curve and the peak around 500 nm indicate that the average droplet diameter of the emulsion is between 500 and 600 nm.
- the graph in Figure 7 represents the destabilization expressed as a percentage, on the ordinate, which corresponds to the percentage of the quantity of the phase destabilized compared to its initial quantity, in function of the emulsifier / dispersed phase ratio, abscissa, i.e. the ratio of percentages emulsifier and dispersed phase of the emulsion.
- the curve in dotted lines corresponds to an emulsion obtained by introducing a jet of water, pressurized to 200 MPa, in oil in which been previously mixed the "Tween 20" and the curve in solid line corresponds to an emulsion obtained according to the invention.
- the stabilization i.e.
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Abstract
Description
La présente invention concerne un procédé de fabrication d'émulsions ainsi qu'un émulseur mettant en oeuvre ce procédé. Un tel procédé trouvera de nombreuses applications, notamment dans les domaines de la cosmétologie, de l'industrie alimentaire pour la fabrication de vinaigrette par exemple, de la pharmacie, de la pétrochimie, etc...The present invention relates to a method of manufacture of emulsions as well as an emulsifier this process. Such a process will find many applications, particularly in the fields of cosmetology, food industry for the making salad dressings for example, pharmacy, petrochemicals, etc.
D'une manière générale, la fabrication d'une émulsion consiste dans le mélange de deux fluides, c'est-à-dire de deux liquides, déterminant deux phases, par hypothèses non miscibles, l'une étant appelée phase dispersée et l'autre phase dispersante, et dont l'une forme des gouttelettes microscopiques dans l'autre. Ce mélange ou émulsion, et plus particulièrement la taille des gouttelettes de la phase dispersée dans la phase dispersante, dépend notamment de l'énergie fournie sous forme d'agitation au milieu qui provoque un cisaillement du fluide et permet ainsi la réduction de la taille des gouttelettes de l'émulsion.In general, the manufacture of an emulsion consists of the mixture of two fluids, i.e. two liquids, determining two phases, by hypotheses not miscible, one being called dispersed phase and the other dispersing phase, one of which forms droplets microscopic in the other. This mixture or emulsion, and more particularly the size of the droplets of the dispersed phase in the dispersing phase, depends in particular of energy supplied in the form of agitation to the medium which shears the fluid and thus allows the reduction in the size of the emulsion droplets.
Par ailleurs, il est souvent nécessaire d'ajouter un émulsifiant pour stabiliser l'émulsion dans le temps en évitant la coalescence de la phase dispersée et permettre ainsi le stockage de l'émulsion. En effet, dans une émulsion du type huile dans eau où l'eau correspond à la phase dispersante et l'huile à la phase dispersée, l'huile et l'eau n'étant pas miscibles, les gouttelettes d'huile auront tendance à se regrouper entre elles pour former des gouttelettes plus grosses créant ainsi un phénomène de coalescence.In addition, it is often necessary to add a emulsifier to stabilize the emulsion over time while avoiding the coalescence of the dispersed phase and allowing thus storing the emulsion. Indeed, in a oil in water type emulsion where the water corresponds to the dispersing phase and the dispersed phase oil, the oil and water is immiscible, the oil droplets will tend to group together to form larger droplets creating a phenomenon of coalescence.
On connaít bien, notamment dans le domaine de l'industrie alimentaire, des émulseurs tels que des homogénéisateurs haute pression ou bien encore des "microfluidizers" produisant des émulsions comprenant un émulsifiant, par exemple une émulsion du type huile dans eau.We know well, especially in the area of the food industry, foam concentrates such as high pressure homogenizers or even "microfluidizers" producing emulsions comprising a emulsifier, for example an oil type emulsion in water.
Les homogénéisateurs sont classiquement constitués d'une tête d'homogénéisation et d'une pompe haute pression pour mettre sous pression un fluide contenu dans un réservoir. Le fluide sous pression est habituellement une pré émulsion, c'est-à-dire qu'il s'agit d'un mélange partiel de la phase dispersée, de la phase dispersante et de l'émulsifiant ; ce fluide est ensuite envoyé à travers la tête d'homogénéisation principalement constituée d'une base, d'un clapet et de plaques d'impact. Le fluide est brutalement détendu à travers une ouverture appropriée, pour atteindre une vitesse de l'ordre de plusieurs centaines de mètres par seconde, puis entre en contact avec le clapet qui scinde le fluide et le projette sur les plaques d'impact fournissant ainsi l'énergie nécessaire, sous forme d'agitation au milieu, pour la fabrication de l'émulsion. Ces homogénéisateurs, bénéficiant des technologies actuelles, fonctionnent à des pressions pouvant atteindre 200 MPa.Homogenizers are conventionally made up a homogenization head and a high pressure pump to pressurize a fluid contained in a tank. The pressurized fluid is usually a pre-emulsion, i.e. it is a mixture partial of the dispersed phase, the dispersing phase and emulsifier; this fluid is then sent through the homogenization head mainly consisting of a base, valve and impact plates. The fluid is brutally relaxed through an appropriate opening, to reach a speed of the order of several hundreds of meters per second and then comes into contact with the valve which splits the fluid and projects it on the impact plates thus providing the necessary energy, in the form of agitation in the middle, for the manufacture of the emulsion. These homogenizers, benefiting from current technologies operate at pressures up to 200 MPa.
Ces homogénéisateurs présentent comme principaux inconvénients une usure de la tête d'homogénéisation due aux frottements importants du fluide sur le clapet et les plaques d'impact ainsi qu'un échauffement de l'émulsion. Par ailleurs, pour ces dispositifs fonctionnant à partir d'une préémulsion, un procédé de préémulsion est nécessaire en amont des homogénéisateurs, augmentant ainsi les coûts de production.These homogenizers have as main disadvantages due to wear of the homogenization head high friction of the fluid on the valve and the impact plates and heating of the emulsion. Furthermore, for these devices operating from of a pre-emulsion, a pre-emulsion process is necessary upstream of homogenizers, thereby increasing costs of production.
A cet égard, on a conçu des têtes d'homogénéisation réduisant significativement leur usure ; c'est par exemple le cas du brevet français FR 2748954 concernant un module homogénéisateur-émulsionneur. Ce module est principalement constitué d'un corps cylindrique présentant à chacune de ses extrémités respectivement un bloc d'entrée directe et un bloc de sortie. Le corps cylindrique renferme une succession de cartouches cylindriques creuses et ouvertes sur une de leur face transversale et elles sont reliées entre elles par des ressorts. Ces cartouches contiennent une pluralité de disques vibrants qui peuvent coulisser le long de l'axe creux central du corps cylindrique du module. Lorsqu'un fluide sous pression est introduit par le bloc d'entrée directe dans le corps cylindrique, l'ensemble des disques vibrants se mettent en mouvement créant ainsi un effet de cisaillement du fluide qui permet la réduction de la taille des gouttes de l'émulsion.In this regard, we have designed homogenization heads significantly reducing their wear; it's for example the case of French patent FR 2748954 concerning a module homogenizer-emulsifier. This module is mainly consisting of a cylindrical body each having its ends respectively a direct input block and an output block. The cylindrical body contains a succession of hollow and open cylindrical cartridges on one of their transverse faces and they are connected between them by springs. These cartridges contain a plurality of vibrating discs which can slide the along the central hollow axis of the cylindrical body of the module. When a pressurized fluid is introduced through the block direct entry into the cylindrical body, all of the vibrating discs set in motion thus creating a fluid shear effect which allows reduction of the size of the emulsion drops.
Il existe également des "'microfluidizers" classiquement constitués d'une chambre d'interactions et d'une pompe haute pression pour mettre sous pression un fluide contenu dans un réservoir approprié. Le fluide sous pression est habituellement une pré émulsion qui est envoyée dans la chambre d'interaction dans laquelle cette dernière est bombardée par elle-même avec une énergie importante apportée par la mise sous pression du fluide, ce qui permet la fabrication de l'émulsion.There are also "microfluidizers" conventionally made up of an interaction chamber and a high pressure pump to pressurize a fluid contained in a suitable reservoir. The fluid under pressure is usually a pre emulsion which is sent to the interaction room in which this last one is bombarded by itself with energy important brought by the pressurization of the fluid, this which allows the manufacture of the emulsion.
Un inconvénient de ces dispositifs est l'importante quantité d'émulsifiant nécessaire pour stabiliser une telle émulsion. Cet apport élevé d'émulsifiant se traduit alors par un excès dudit émulsifiant dans la phase dispersante de l'émulsion après sa fabrication, ce qui affecte notamment les qualités organoleptiques de l'émulsion et augmente les coûts de production.A disadvantage of these devices is the important amount of emulsifier required to stabilize such emulsion. This high supply of emulsifier is then reflected by an excess of said emulsifier in the dispersing phase of the emulsion after its manufacture, which affects in particular the organoleptic qualities of the emulsion and increases the production costs.
Le document DE-A-2549026 décrit, par ailleurs, un procédé d'émulsification comprenant l'introduction de la phase dispersée dans un jet de la phase dispersante et le mélange dans une chambre de ce jet avec une partie additionnelle de la phase dispersante.Document DE-A-2549026 describes, moreover, a emulsification process comprising the introduction of the dispersed phase in a jet of the dispersing phase and the mixing in a chamber of this jet with a part additional of the dispersing phase.
Un autre inconvénient de tous ces dispositifs est de procurer une émulsion dont les gouttelettes présentent un diamètre moyen de l'ordre du micromètre, ce qui n'est pas pleinement satisfaisant pour des applications dans les domaines de l'alimentaire et de la cosmétologie, par exemple.Another disadvantage of all these devices is that provide an emulsion whose droplets have a average diameter of the order of a micrometer, which is not fully satisfactory for applications in food and cosmetology, by example.
L'un des buts de l'invention est donc de palier ces inconvénients en proposant un procédé de fabrication d'un mélange ou d'une émulsion, par exemple du type huile dans eau, pour obtenir une plus grande finesse des gouttelettes en utilisant une quantité minimale d'émulsifiant pour stabiliser ladite émulsion dans le temps.One of the aims of the invention is therefore to overcome these disadvantages by proposing a method of manufacturing a mixture or emulsion, for example of the oil type in water, to obtain greater fineness of the droplets using a minimum amount of emulsifier for stabilize said emulsion over time.
A cet égard et conformément à l'invention, le procédé pour la fabrication en continu ou en discontinu d'un mélange ou d'une émulsion à partir d'au moins un émulsifiant et au moins deux fluides réputés non miscibles, par exemple un corps liquide gras mélangé à de l'eau et à un émulsifiant approprié, lesdits fluides définissant une phase dispersée et une phase dispersante, est remarquable en ce que, la phase dispersée étant soit contenue dans un réservoir adapté, soit délivrée en continu, il comporte une première étape de mise sous pression de la phase dispersée par de classiques moyens de pompage haute pression puis, on effectue une dépressurisation brutale de ladite phase dispersée grâce à des moyens permettant de créer un jet aiguille, c'est-à-dire un jet de section étroite, ou jet cohérent dans lequel la phase dispersée peut atteindre une vitesse d'environ 900 m.s-1. Il est alors envisageable d'introduire le jet cohérent de la phase dispersée dans une phase dispersante dans laquelle a été dissout un émulsifiant approprié pour obtenir l'émulsion.In this regard and in accordance with the invention, the process for the continuous or batch production of a mixture or an emulsion from at least one emulsifier and at least two fluids known to be immiscible, for example a body fatty liquid mixed with water and an appropriate emulsifier, said fluids defining a dispersed phase and a dispersing phase, is remarkable in that, the dispersed phase being either contained in a suitable tank, or delivered continuously, it comprises a first step of pressurizing the dispersed phase by conventional high-pressure pumping means, then a sudden depressurization of said dispersed phase is carried out using means making it possible to create a needle jet, that is to say a jet of narrow section, or coherent jet in which the dispersed phase can reach a speed of about 900 ms -1 . It is then conceivable to introduce the coherent jet of the dispersed phase into a dispersing phase in which an appropriate emulsifier has been dissolved to obtain the emulsion.
Un tel procédé ne permet pas d'obtenir une taille moyenne des gouttelettes suffisamment petite, c'est pourquoi, on préfère introduire l'émulsifiant approprié dans ledit jet cohérent grâce à des moyens assurant le mélange de la phase dispersée avec ledit émulsifiant. On obtient alors un jet cohérent résultant qui comprend la phase dispersée et l'émulsifiant. Ce jet cohérent résultant est finalement mis en contact avec la phase dispersante pour obtenir le mélange ou l'émulsion.Such a method does not make it possible to obtain a size average droplet size small enough why, we prefer to introduce the appropriate emulsifier in said coherent jet by means ensuring the mixing the dispersed phase with said emulsifier. We then gets a resulting coherent throw which includes the dispersed phase and emulsifier. This resulting coherent jet is finally brought into contact with the dispersing phase to obtain the mixture or the emulsion.
On obtient ainsi une émulsion dont les gouttelettes présentent un diamètre moyen compris entre quelques dizaines et quelques centaines de nanomètres, suivant les fluides utilisés, tout en nécessitant un apport réduit d'émulsifiant contrairement à l'art antérieur où le diamètre des gouttelettes diminuant, c'est-à-dire leur surface totale augmentant, une plus grande quantité d'additif aurait été nécessaire.An emulsion is thus obtained, the droplets of which have an average diameter of between a few tens and a few hundred nanometers, depending on the fluids used, while requiring a reduced intake emulsifier unlike the prior art where the decreasing droplet diameter, i.e. their increasing total surface, a greater quantity additive would have been necessary.
Par ailleurs, la mise en contact du jet cohérent résultant avec la phase dispersante, selon une première variante du procédé, est obtenue en positionnant ledit jet cohérent résultant en immersion dans la phase dispersante en position statique ou quasi statique dans des moyens de soutirage.Furthermore, bringing the coherent jet into contact resulting with the dispersing phase, according to a first variant of the process, is obtained by positioning said jet coherent resulting in immersion in the dispersing phase in a static or quasi-static position in means of racking.
Selon une seconde variante du procédé, la mise en contact du jet cohérent résultant avec la phase dispersante est obtenue grâce à des moyens assurant l'introduction de la phase dispersante dans ledit jet cohérent résultant et simultanément leur émulsion qui constitue alors un jet cohérent final.According to a second variant of the method, the implementation contact of the resulting coherent jet with the dispersing phase is obtained by means ensuring the introduction of the dispersing phase in said resulting coherent jet and simultaneously their emulsion which then constitutes a jet consistent final.
Lors de la dépressurisation brutale de la phase dispersée, cette dernière subit un échauffement pouvant notamment modifier ses caractéristiques hydrodynamiques et organoleptiques, c'est pourquoi la température de la phase dispersée sous pression est régulée selon une gamme de température comprise entre -20°C et +80°C pour que la fabrication de l'émulsion soit plus homogène dans le temps.During the abrupt depressurization of the phase dispersed, the latter undergoes heating which can notably modify its hydrodynamic characteristics and organoleptics, that's why the temperature of the phase dispersed under pressure is regulated according to a range of temperature between -20 ° C and + 80 ° C so that the the emulsion is more homogeneous over time.
De plus, la phase dispersée est pressurisée à une pression supérieure ou égale à 200 MPa.In addition, the dispersed phase is pressurized to a pressure greater than or equal to 200 MPa.
Un autre but de l'invention concerne un dispositif émulseur pour la fabrication en continu ou en discontinu d'un mélange ou d'une émulsion à partir d'au moins un émulsifiant et au moins deux fluides réputés non miscibles, par exemple un produit liquide gras mélangé à de l'eau et un émulsifiant, lesdits fluides définissant une phase dispersée et une phase dispersante, et ledit dispositif comportant une pompe à haute pression dont l'entrée est connectée à une source de fluide telle qu'un réservoir contenant une phase dispersée ; ce dispositif est remarquable en ce que la sortie de la pompe à haute pression est reliée, par des moyens de raccordement, à des moyens de projection de la phase dispersée sous la forme d'un jet cohérent coopérant avec des moyens d'introduction, connectés à un réservoir ouvert et utilisant l'effet Venturi, d'un émulsifiant dans ledit jet cohérent débouchant, en immersion, dans la phase dispersante contenue dans des moyens de soutirage, en continu ou en discontinu, de l'émulsion.Another object of the invention relates to a device foam concentrate for continuous or batch production a mixture or an emulsion from at least one emulsifier and at least two fluids known to be immiscible, for example a fatty liquid product mixed with water and an emulsifier, said fluids defining a phase dispersed and a dispersing phase, and said device comprising a high pressure pump the inlet of which is connected to a fluid source such as a reservoir containing a dispersed phase; this device is remarkable in that the high pump output pressure is connected, by connection means, to means for projecting the dispersed phase in the form of a coherent jet cooperating with means of introduction, connected to an open tank and using the Venturi effect, of an emulsifier in said jet coherent emerging, in immersion, in the phase dispersant contained in means of continuous or discontinuous withdrawal of the emulsion.
Selon une variante d'exécution du dispositif comportant une pompe à haute pression dont l'entrée est connectée à une source de fluide telle qu'un réservoir contenant une phase dispersée, la sortie de la pompe à haute pression est reliée, par des moyens de raccordement, à des moyens de projection de la phase dispersée sous la forme d'un jet cohérent, munis à leur sortie d'au moins deux moyens d'introduction qui sont montés en série reliés à un réservoir ouvert respectivement et utilisant l'effet Venturi, respectivement au moins de l'émulsifiant dans ledit jet cohérent et de la phase dispersante dans le jet cohérent résultant, pour procurer l'émulsion qui est avantageusement récupérée en continu à la sortie desdits moyens d'introduction ou en discontinu.According to an alternative embodiment of the device comprising a high pressure pump the inlet of which is connected to a fluid source such as a reservoir containing a dispersed phase, the pump outlet at high pressure is connected, by connection means, to means for projecting the phase dispersed under the form of a coherent jet, provided at their outlet with at least two introduction means which are mounted in series connected to an open tank respectively and using the Venturi effect, respectively at least the emulsifier in said coherent jet and phase dispersant in the resulting coherent jet, to provide the emulsion which is advantageously continuously recovered at the output of said introduction means or discontinuously.
Selon une caractéristique secondaire des dispositifs selon l'invention, les moyens de raccordement, entre la pompe à haute pression et les moyens de projection, sont munis de moyens de régulation de la température sur tout ou partie de leur longueur.According to a secondary characteristic of the devices according to the invention, the connection means, between the high pressure pump and the projection means, are provided with temperature regulation means on all or part of their length.
D'autres avantages et caractéristiques ressortiront mieux de la description qui va suivre de plusieurs variantes d'exécution, données à titre d'exemples non limitatifs, du procédé et du dispositif émulseur le mettant en oeuvre conformément à l'invention en référence aux dessins annexés sur lesquels :
- la figure 1 est une représentation schématique du dispositif émulseur selon l'invention,
- la figure 2 est un schéma partiel en légère perspective du dispositif émulseur selon l'invention comportant le réservoir de phase dispersée, la pompe à haute pression, les moyens de raccordement et les moyens de régulation de la température,
- la figure 3 est un schéma partiel de la première variante d'exécution du dispositif émulseur selon l'invention comportant les moyens de projection de la phase dispersée, les moyens d'introduction de l'émulsifiant dans le jet et les moyens de soutirage,
- la figure 4 est un schéma partiel de la seconde variante d'exécution du dispositif émulseur selon l'invention comportant les moyens de projection de la phase dispersée, deux moyens d'introduction respectivement de l'émulsifiant et de la phase dispersante montés en série et les moyens de soutirage,
- la figure 5 est un graphique représentant le pourcentage (%) des gouttelettes en fonction de leur diamètre exprimé en nanomètre (nm) pour un exemple d'émulsion du type huile dans eau, comprenant 10% d'huile de tournesol, 89% d'eau et 1% d'émulsifiant Tween 20 (marque déposée), et obtenue en projetant un jet d'huile de tournesol, pressurisée à 200 MPa, dans de l'eau dans laquelle a été préalablement dissout le Tween 20 (marque déposée),
- la figure 6 est un graphique représentant le pourcentage (%) des gouttelettes en fonction de leur diamètre exprimé en nanomètre (nm) pour une émulsion du type huile dans eau, comprenant 10% d'huile de tournesol, 89.5% d'eau et 0.5% d'émulsifiant Tween 20 (marque déposée) et obtenue selon le procédé.
- la figure 7 est un graphique représentant l'influence du rapport émulsifiant/phase dispersante sur la stabilité d'une émulsion du type eau dans huile.
- FIG. 1 is a schematic representation of the foam concentrate device according to the invention,
- FIG. 2 is a partial diagram in slight perspective of the foam concentrate device according to the invention comprising the dispersed phase reservoir, the high pressure pump, the connection means and the temperature regulation means,
- FIG. 3 is a partial diagram of the first alternative embodiment of the foam concentrate device according to the invention comprising the means for projecting the dispersed phase, the means for introducing the emulsifier into the jet and the withdrawal means,
- FIG. 4 is a partial diagram of the second alternative embodiment of the foam concentrate device according to the invention comprising the means for projecting the dispersed phase, two means for introducing the emulsifier and the dispersing phase respectively mounted in series and withdrawal means,
- FIG. 5 is a graph representing the percentage (%) of the droplets as a function of their diameter expressed in nanometers (nm) for an example of an emulsion of the oil in water type, comprising 10% of sunflower oil, 89% of water and 1% of Tween 20 emulsifier (registered trademark), and obtained by spraying a jet of sunflower oil, pressurized to 200 MPa, in water in which the Tween 20 (registered trademark) has previously been dissolved,
- FIG. 6 is a graph representing the percentage (%) of the droplets as a function of their diameter expressed in nanometers (nm) for an emulsion of the oil in water type, comprising 10% of sunflower oil, 89.5% of water and 0.5 % of Tween 20 emulsifier (registered trademark) and obtained according to the process.
- FIG. 7 is a graph representing the influence of the emulsifier / dispersing phase ratio on the stability of a water in oil type emulsion.
Pour des raisons de clarté, on désignera ci-après par émulsion tous les mélanges et émulsions obtenus suivant l'invention et par émulseur tous les dispositifs mélangeur, homogénéisateur, "microfluidizer", émulseur et homogénéisateur-émulseur.For reasons of clarity, the following will be designated by emulsion all mixtures and emulsions obtained according to the invention and by emulsifier all the mixing devices, homogenizer, "microfluidizer", foam concentrate and homogenizer-emulsifier.
Le dispositif pour la fabrication en continu ou en
discontinu d'une émulsion qui est représenté sur les
figures 1 à 4, comprend un réservoir 1 contenant une phase
dispersée et dont la sortie est connectée à une pompe à
haute pression 2. Une pompe de gavage, non représentée sur
les figures, sera avantageusement positionnée entre le
réservoir 1 et la pompe à haute pression 2 pour amorcer
cette dernière d'une manière classique. La sortie de la
pompe à haute pression 2 est reliée, en référence à la
figure 1, par des moyens de raccordement 3, à des moyens de
projection 4 de la phase dispersante sous la forme d'un jet
aiguille ou jet cohérent 5. Par ailleurs, les moyens de
raccordement 3, entre la pompe à haute pression 2 et les
moyens de projection 4, sont munis de moyens de
régulation 6 de la température de la phase dispersée, sous
pression dans lesdits moyens de raccordement 3, sur tout ou
partie de leur longueur. La sortie des moyens de
projection 4 est munie de moyens d'introduction 7 dans le
jet cohérent 5 d'un émulsifiant contenu dans un second
réservoir 8 relié aux dits moyens d'introduction 7 de telle
sorte qu'à leur sortie jaillisse un jet cohérent
résultant 9 constitué de la phase dispersée et de
l'émulsifiant. Le jet cohérent résultant 9 est alors mis en
contact avec la phase dispersante contenue dans des moyens
de soutirage 10 en continu ou en discontinu comme on le
verra plus loin. Le jet cohérent résultant 9 est de
préférence positionné en immersion dans ladite phase
dispersante pour bénéficier de l'énergie optimale, dudit
jet cohérent résultant, nécessaire à l'obtention d'une
émulsion fine.The device for continuous or
discontinuous emulsion which is represented on the
Figures 1 to 4, includes a
Selon une variante d'exécution du dispositif émulseur
selon l'invention, la sortie des moyens d'introduction 7
est munie de seconds moyens d'introduction 11, représentés
en traits pointillés sur la figure 1, dans le jet cohérent
résultant d'une phase dispersante contenue dans un
troisième réservoir 12, également représenté en traits
pointillés sur la figure 1, relié auxdits moyens
d'introduction 11 de telle sorte qu'à leur sortie jaillisse
un jet cohérent final 13 constitué de l'émulsion. Le jet
cohérent final 13, c'est-à-dire l'émulsion, est ensuite
recueilli en continu ou en discontinu dans les moyens de
soutirage 10.According to an alternative embodiment of the foam concentrate device
according to the invention, the output of the introduction means 7
is provided with second introduction means 11, shown
in dotted lines in FIG. 1, in the coherent jet
resulting from a dispersing phase contained in a
En référence à la figure 2, le réservoir 1,
contenant la phase dispersée, est relié à la pompe à haute
pression 2 par un tuyau 14. La pompe à haute pression 2 est
avantageusement une pompe aller et retour qui possède une
constante de temps très courte et qui ne présente donc pas
de temps mort. Elle permet d'obtenir une pression de
400 MPa tout en assurant un gros débit et une pression
constante. Les moyens de raccordement 3 entre la pompe à
haute pression 2 et les moyens de projection 4, non
représentés sur la figure 2, sont constitués par un tuyau
blindé 15 apte à véhiculer la phase dispersée pressurisée
et ils présentent un circuit de dérivation 16 muni de
vannes de contrôle 17 telles que des électrovannes. Le
circuit de dérivation 16 comprend des moyens de
régulation 6 de la température de la phase dispersée
pressurisée, représentés en traits pointillés sur la
figure 2. Les moyens de régulation 6 sont, par ailleurs,
constitués d'un serpentin à spires 18 entourant le tuyau
blindé 15 sur une partie du circuit de dérivation 16 et
relié à un échangeur calorifique 19.With reference to FIG. 2, the
Il va de soi que la longueur du serpentin à spires 18
dépend, notamment, des coefficients calorifiques du fluide
calorifique circulant dans ledit serpentin à spires 18 et
de la phase dispersée utilisée. De plus, les moyens de
raccordement 3 peuvent ne pas comporter de circuit de
dérivation 16 et le serpentin à spires 18 sera alors
positionné directement autour du tuyau blindé 15.It goes without saying that the length of the
Par ailleurs, les moyens de régulation 6 comprennent
également une sonde 20, montée de préférence en amont du
serpentin à spires 18 sur le circuit de dérivation 16,
permettant de contrôler la température de la phase
dispersée dans le tuyau blindé 15.Furthermore, the regulating means 6 comprise
also a
Selon une première variante du dispositif émulseur
selon l'invention représentée sur la figure 3, les moyens
de projection 4 sont classiquement montés à l'extrémité du
tuyau blindé 15, faisant face au sol et ils sont constitués
d'une buse 21 supportée par un porte-buse 22 comportant un
trou calibré 23. La buse 21 est classiquement constituée
d'un corps 24 comportant à son extrémité inférieure un
second trou calibré 25 et d'un pointeau 26 comportant un
troisième trou calibré 27 coaxial au premier 23 et au
second 25. Le diamètre du trou calibré 26 est
avantageusement compris entre 0.08 et 0.15 mm pour une
pression délivrée par la pompe à haute pression 2 de
200 MPa afin d'éviter que ledit trou calibré 26 ne
s'obstrue.According to a first variant of the foam concentrate device
according to the invention shown in Figure 3, the
Il va de soi que les moyens de projection 4 peuvent être dirigés vers le haut pour procurer un jet droit.It goes without saying that the projection means 4 can be directed upward to provide a straight stream.
La buse 21 procure un jet aiguille, c'est-à-dire un
jet de section étroite, ou jet cohérent 5 de la phase
dispersée qui est brutalement dépressurisée et qui jaillit
dans les moyens d'introduction 7. Lesdits moyens
d'introduction 7 sont positionnés à l'extrémité inférieure
du porte-buse 22 et sont constitués par un tube Venturi 28,
d'une longueur d'environ 15 mm pour une pression comprise
entre 200 MPa et 300 MPa, formant dans sa partie centrale
une chambre de mélange 29 et à son extrémité inférieure un
tube de focalisation 30. Le jet cohérent 5 jaillit ainsi
dans la chambre de mélange 29 où l'émulsifiant,
initialement contenu dans le réservoir 8 et qui est amené,
par un conduit flexible 31 muni d'une vanne de contrôle 17
et d'un système de régulation de débit 32, dans la chambre
de mélange 29 par effet Venturi, se mélangent pour procurer
dans le tube de focalisation 30 un jet cohérent
résultant 9.The
Il est à noter que le réservoir 8 est un réservoir
ouvert pour que l'émulsifiant soit à la pression
atmosphérique et puisse bénéficier de l'effet Venturi pour
être amené dans la chambre de mélange 29. Par ailleurs, il
serait envisageable d'introduire l'émulsifiant dans le jet
cohérent de la phase dispersée au moyen d'un jet incident
faisant un angle très petit avec ledit jet cohérent 5.It should be noted that the
Le tube de focalisation 30 est positionné en
immersion dans une phase dispersante statique ou quasi-statique
contenue dans les moyens de soutirage 10 qui sont
constitués d'un récipient cylindrique principal 33, d'un
récipient cylindrique médian 34 et d'un cylindre central 35
coaxiaux. Le récipient cylindrique principal 33 présente la
plus grande section et comprend deux ouvertures 36,37 dans
sa partie supérieure pour l'introduction d'un fluide
calorifique et deux autres ouvertures 38,39 dans sa partie
inférieure pour la sortie dudit fluide calorifique, comme
on le verra plus loin. Les ouvertures 36,37,38 et 39 du
récipient cylindrique principal 33 sont avantageusement
reliées à l'échangeur calorifique 19 par des moyens de
raccordement classiques non représentés sur les figures. Le
récipient cylindrique médian 34, positionné à l'intérieur
du récipient cylindrique principal 33, comprend un fond
renforcé 40 pour éviter sa déformation due à la pression du
jet cohérent résultant 9. Le cylindre central 35, ouvert à
ses deux extrémités est positionné dans le récipient
cylindrique médian 34 de telle sorte que son extrémité
inférieure 41 ne soit pas en contact avec le fond
renforcé 40. Par ailleurs, le récipient cylindrique
médian 34 et le cylindre central 35 comprennent
respectivement une ouverture 42 dans sa partie centrale
pour le soutirage de l'émulsion et une ouverture 43 dans sa
partie supérieure pour l'introduction de la phase
dispersante comme on le verra plus loin.The focusing
Il va de soi que les moyens de soutirage 10 peuvent être constitués d'un unique récipient cylindrique comprenant la phase dispersée et muni ou non d'une ouverture dans sa partie supérieure pour l'introduction de la phase dispersante et d'une autre ouverture dans sa partie inférieure pour le soutirage de l'émulsion soit en continu, soit en discontinu.It goes without saying that the withdrawal means 10 can consist of a single cylindrical container comprising the dispersed phase and whether or not provided with a opening in its upper part for the introduction of the dispersing phase and another opening in its lower part for drawing off the emulsion either continuous, or discontinuous.
Selon une seconde variante du dispositif émulseur
conforme à l'invention, représentée sur la figure 4, les
moyens de projection 4, tels que décrits précédemment,
procurent un jet cohérent 5 qui jaillit dans un premier
tube Venturi 28 tel que décrit précédemment permettant le
mélange de l'émulsifiant, préalablement contenu dans le
réservoir 8, avec la phase dispersée et procurant un jet
cohérent résultant 9 comme on la déjà vu. Ledit jet
cohérent résultant 9 jaillit alors dans un second tube
Venturi 44 monté en série avec le premier 28 et formant une
seconde chambre de mélange 45 dans sa partie centrale et un
second tube de focalisation 46 dans sa partie inférieure.
Le jet cohérent résultant 9 jaillit ainsi dans la seconde
chambre de mélange 45 où la phase dispersante, initialement
contenue dans le réservoir 12 puis amenée, par un conduit
flexible 31 muni d'une vanne de contrôle 17 et d'un système
de régulation de débit 32, dans la seconde chambre de
mélange 45 par effet Venturi, se mélange avec ledit jet
cohérent résultant 9 pour procurer l'émulsion qui s'écoule
dans le second tube de focalisation 46 sous la forme d'un
jet cohérent final 13.According to a second variant of the foam concentrate device
according to the invention, shown in Figure 4, the
projection means 4, as described above,
provide a
Il va de soi que le dispositif peut comprendre
plusieurs tubes Venturi montés en série permettant
d'introduire successivement dans le jet cohérent 5
plusieurs émulsifiants et plusieurs phases dispersantes
pour fabriquer des émulsions dites ternaires telles que des
émulsions du type eau/huile/eau.It goes without saying that the device can include
several Venturi tubes mounted in series allowing
to successively introduce into the
Le jet cohérent final 13, c'est-à-dire l'émulsion,
est recueilli dans les moyens de soutirage 10 placés à la
verticale sous le second tube de focalisation 46. Les
moyens de soutirage 10 sont alors constitués d'un simple
récipient cylindrique 47 muni d'une ouverture 48 dans sa
partie inférieure pour soutirer en continu l'émulsion comme
l'indique la flèche 49.The final
Naturellement, l'émulsion pourrait être soutirée en discontinu en utilisant un simple récipient cylindrique.Naturally, the emulsion could be drawn off in discontinuous using a simple cylindrical container.
On expliquera maintenant le fonctionnement du
dispositif émulseur selon l'invention en référence aux
figures 2, 3, 5 et 6. Pour réaliser une émulsion du type
huile dans eau par exemple, on place dans le réservoir 1 de
l'huile de tournesol qui correspondra dans ce cas à la
phase dispersée ; puis au moyen d'une pompe de gavage, non
représentée sur la figure 2, on amorce la pompe à haute
pression 2 qui met alors sous pression l'huile dans le
tuyau blindé 15. On actionne, ensuite si nécessaire, les
différentes vannes de contrôle 17 pour que l'huile circule
dans le circuit de dérivation 16 afin de la réguler en
température. L'huile sous pression jaillit de la buse 21
(figure 3) pour former un jet cohérent 5 à travers le tube
venturi 28. L'huile est pressurisée, de préférence, à une
pression supérieure ou égale à 200 MPa pour que le jet
cohérent 5 ait une énergie suffisante pour former
l'émulsion sans que la buse 21 ne s'obstrue. La vitesse de
l'huile peut alors atteindre 900 m.s-1 pour une pression de
200 MPa et un diamètre de la buse 21 compris entre 0.08
et 0.15 mm.The operation of the foam concentrate device according to the invention will now be explained with reference to FIGS. 2, 3, 5 and 6. To produce an oil-in-water type emulsion for example, place in
Pour des raisons de clarté, on désignera par Tween 20
l'émulsifiant utilisé, le Tween 20 étant une marque déposée
pour un émulsifiant. que l'on appellera par la suite
"Tween 20".For reasons of clarity, we will denote by
Par effet Venturi le "Tween 20" est aspiré par le jet
cohérent 5 d'huile avec laquelle il se mélange pour former
le jet cohérent résultant 9.By Venturi effect the "
Il est à noter que le "Tween 20", ne se dissout pas
dans la phase dispersée, c'est-à-dire l'huile. D'une
manière générale, l'émulsifiant ne se dissout que dans la
phase dispersante ; ainsi, le "Tween 20" se mélange d'une
manière homogène dans le jet cohérent 5 sans y être
dissout.It should be noted that the "
Le jet cohérent résultant 9 est alors introduit en
immersion dans l'eau, correspondant à la phase dispersante,
qui est injectée en continue dans le cylindre central 35
par l'ouverture 43 comme l'indique la flèche 50 de la
figure 3.The resulting
Lorsque le jet cohérent résultant 9 qui consiste dans
le mélange de l'huile et du "Tween 20" entre en contact
avec l'eau, des gouttelettes d'huiles se forment dans l'eau
et le "Tween 20" se positionne autour de ces gouttelettes
pour éviter que ces dernières se rassemblent et l'on
obtient ainsi une émulsion du type huile dans eau.
L'émulsion ainsi obtenue poursuit sa descente dans le
cylindre central 35 pour remonter ensuite entre les parois
du récipient cylindrique médian 34 et ledit cylindre
central 35, comme l'indique les flèches 51, et pour être
finalement soutirée par l'ouverture 42 comme l'indique la
flèche 52. L'émulsion peut être alors régulée en
température grâce au passage d'un fluide calorifique entre
le récipient cylindrique principal 33 et le récipient
cylindrique médian 34. Le fluide calorifique entre par les
ouvertures supérieures 36,37, comme l'indique les
flèches 53 et sort par les ouvertures inférieures 38,39,
comme l'indique les flèches 54 de la figure 3.When the resulting
La taille des gouttelettes de l'émulsion, et plus précisément leur diamètre, dépend notamment de l'énergie apportée sous forme d'agitation au milieu comme on l'a déjà vu mais aussi des fluides utilisé. Pour une émulsion du type huile dans eau par exemple, la taille des gouttelettes dépendra notamment du type d'huile utilisé.The size of the emulsion droplets, and more precisely their diameter, depends in particular on the energy brought in the form of agitation in the middle as we have already seen but also fluids used. For an emulsion of type oil in water for example, the size of the droplets will depend in particular on the type of oil used.
La figure 5 représente le pourcentage des
gouttelettes en fonction de leur diamètre, exprimé en
nanomètre (nm) pour une émulsion du type huile dans eau,
comprenant 10% d'huile de tournesol, 89% d'eau et 1%
d'émulsifiant "Tween 20", et obtenue en projetant un jet
d'huile de tournesol, pressurisée à 200 MPa, dans de l'eau
dans laquelle a été préalablement dissout le "Tween 20". La
forme générale de la courbe ainsi que le pic aux environs
de 500 nm indiquent que le diamètre moyen des gouttelettes
de l'émulsion est compris entre 500 et 600 nm. Pour une
émulsion comprenant 10% d'huile de tournesol, 89.5% d'eau
et 0.5% d'émulsifiant "Tween 20" et obtenue selon
l'invention, le pourcentage des gouttelettes en fonction de
leur diamètre, exprimé en nanomètre, représenté sur la
figure 6, présente une courbe différente. On constate, en
effet, un premier pic aux environs de 200 nm et un second
pic aux environs de 450 nm indiquant une stabilisation plus
rapide de la phase dispersée, c'est-à-dire de l'huile, puis
un léger phénomène de coalescence. On obtient donc une
émulsion dont la taille des gouttelettes est plus petite
pour une quantité moindre d'émulsifiant comme le précise la
figure 7.Figure 5 shows the percentage of
droplets according to their diameter, expressed in
nanometer (nm) for an oil-in-water type emulsion,
including 10% sunflower oil, 89% water and 1%
of emulsifier "
Le graphique de la figure 7 représente la
déstabilisation exprimée en pourcentage, en ordonnée, qui
correspond au pourcentage de la quantité de la phase
déstabilisée par rapport à sa quantité initiale, en
fonction du rapport émulsifiant/phase dispersée, en
abscisse, c'est-à-dire le rapport des pourcentages
d'émulsifiant et de phase dispersée de l'émulsion. La
courbe en traits pointillés correspond à une émulsion
obtenue en introduisant un jet d'eau, pressurisée à 200
MPa, dans de l'huile dans laquelle été préalablement
mélangé le "Tween 20" et la courbe en trait plein
correspond à une émulsion obtenue selon l'invention. On
observe, en référence à la figure 7, que la stabilisation,
c'est-à-dire une déstabilisation nulle, est obtenue à un
rapport d'environ 0.03 pour une émulsion conforme à
l'invention et à un rapport d'environ 0.12 pour l'autre
émulsion classiquement obtenue. Par conséquent, une plus
faible quantité d'émulsifiant est nécessaire pour
stabiliser l'émulsion. En effet, on peut raisonnablement
estimer que le "Tween 20" n'étant introduit d'une manière
homogène dans l'huile que quelques millisecondes avant
l'impact avec l'eau, en raison des dimensions du tube
Venturi 28 et de la vitesse de l'huile dans le jet
cohérent 5, seul l'émulsifiant nécessaire à la
stabilisation de l'interface des phases dispersée et
dispersante n'est requis et donc n'est apporté.The graph in Figure 7 represents the
destabilization expressed as a percentage, on the ordinate, which
corresponds to the percentage of the quantity of the phase
destabilized compared to its initial quantity, in
function of the emulsifier / dispersed phase ratio,
abscissa, i.e. the ratio of percentages
emulsifier and dispersed phase of the emulsion. The
curve in dotted lines corresponds to an emulsion
obtained by introducing a jet of water, pressurized to 200
MPa, in oil in which been previously
mixed the "
Il est évident que les valeurs portées sur les figures 5, 6 et 7 sont purement indicatives et varient en fonction des types d'émulsion. Par ailleurs, suivant les types d'émulsion et leurs applications, un émulsifiant approprié sera utilisé.It is obvious that the values carried on the Figures 5, 6 and 7 are purely indicative and vary in depending on the types of emulsion. Furthermore, according to types of emulsion and their applications, an emulsifier appropriate will be used.
Enfin, il va de soi que le procédé selon l'invention et le dispositif émulseur le mettant en oeuvre permettent de réaliser tous les types d'émulsion, notamment des émulsions du type eau dans huile ou du type ternaire, et les exemples que l'on vient de donner ne sont que des illustrations particulières en aucun cas limitatives quant aux domaines d'application de l'invention.Finally, it goes without saying that the method according to the invention and the foaming device using it make it possible to make all types of emulsion, especially emulsions of the water in oil type or of the ternary type, and the examples that we just gave are just illustrations particular in no way limiting as to the fields of application of the invention.
Claims (10)
- A process for manufacturing continuously or discontinuously a mixture or an emulsion from at least one emulsifying agent and at least two fluids considered to be immiscible, for example a fatty substance mixed with water and an appropriate emulsifying agent, said fluids defining a dispersed phase and a dispersing phase, characterised in that since the dispersed phase is either contained in an adapted tank or delivered continuously, at least the following steps are performed in order:the dispersed phase is pressurised by conventional high-pressure pumping means then,the dispersed phase is abruptly depressurised using means able to create a coherent jet (5) then,an appropriate emulsifying agent is then introduced into said coherent jet (5) using means of mixing the dispersed phase with said emulsifying agent and thus obtaining a resulting coherent jet (9) then,said resulting coherent jet (9) is brought into contact with the dispersing phase in order to obtain, finally, the emulsion.
- A process according to claim 1, characterised in that the fluid or fluids forming the dispersed phase is pressurised at a pressure above or equal to 200 Mpa.
- A process according to any one of the previous claims, characterised in that the temperature of the pressurised dispersed phase is controlled in accordance with a temperature scale of between -20°C and +80°C.
- A process according to any one of the previous claims, characterised in that the resulting coherent jet (9) is brought into contact with the dispersing phase by positioning said resulting coherent jet (9) in immersion in the dispersing phase in a static or quasi-static position.
- A process according to any one of the claims 1 to 4, characterised in that the resulting coherent jet (9) is brought into contact with the dispersing phase using means of introducing the dispersing phase into said resulting coherent jet (9) and simultaneously emulsifying them so forming a final coherent jet (13).
- A device for continuously or discontinuously manufacturing a mixture or an emulsion from at least one emulsifying agent and at least two fluids considered to be immiscible, for example a fatty liquid product mixed with water and an appropriate emulsifying agent, said fluids defining a dispersed phase and a dispersing phase, implementing the process according to claim 4 and comprising a high-pressure pump (2) the inlet of which is connected to a fluid source such as a tank (1) containing a dispersed phase, characterised in that the outlet of the high-pressure pump (2) is connected, by connection means (6), to means (4) of discharging the dispersed phase in the form of a coherent jet (5) engaging with means (7), connected to an open tank (8) and using the Venturi effect, of introducing an emulsifying agent into said coherent jet (5) so as to form a resulting coherent jet (9) in a focus tube (30) integral with the introduction means (7) and running, in immersion, into the dispersing phase contained in continuous or discontinuous emulsion bleed-off means (10).
- A device for continuously or discontinuously manufacturing a mixture or an emulsion from at least one additive and at least two fluids considered to be immiscible, for example a fatty liquid product mixed with water and an appropriate emulsifying agent, said fluids defining a dispersed phase and a dispersing phase, implementing the process according to claim 5 and comprising a high-pressure pump (2) the inlet of which is connected to a fluid source such as a tank (1) containing a dispersed phase, characterised in that the outlet of the high-pressure pump (2) is connected, by connection means (6), to means (4) of discharging the dispersed phase in the form of a coherent jet (5), fitted at their outlet with at least two means (7, 11) which are mounted in series, connected to an open tank (8) and (12) respectively and using the Venturi effect, of introducing respectively at least the emulsifying agent into said coherent jet (5) to form a resulting coherent jet (9) and the dispersing phase into said resulting coherent jet (9) to form a final coherent jet (13) and so to obtain the emulsion which is recovered continuously or discontinuously at the outlet of the second introduction means (11) by bleed-off means (10).
- An emulsifier device according to any one of the claims 6 and 7, characterised in that the connection means (3) between the high-pressure pump (2) and the discharging means (4), are fitted with temperature control means (6) over all or part of their length.
- An emulsifier device according to claim 8, characterised in that the temperature control means (8) are constituted by a heat sensor (20) positioned on the connection means (3) and by a spiral coil (18), connected to a heat exchanger (13), which surrounds said connection means (3).
- An emulsifier device according to any one of claims 6 to 9 characterised in that the bleed-off means (10) are fitted with temperature control means (33, 36, 37, 38, 39) connected to the heat exchanger (13).
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR9909448A FR2796568B1 (en) | 1999-07-21 | 1999-07-21 | PROCESS FOR PRODUCING EMULSIONS AND DEVICE THEREOF |
| FR9909448 | 1999-07-21 | ||
| PCT/FR2000/002106 WO2001005493A1 (en) | 1999-07-21 | 2000-07-21 | Method for making emulsions and implementing device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP1202795A1 EP1202795A1 (en) | 2002-05-08 |
| EP1202795B1 true EP1202795B1 (en) | 2004-06-16 |
Family
ID=9548342
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP00958582A Expired - Lifetime EP1202795B1 (en) | 1999-07-21 | 2000-07-21 | Method for making emulsions and implementing devices |
Country Status (7)
| Country | Link |
|---|---|
| EP (1) | EP1202795B1 (en) |
| AT (1) | ATE269148T1 (en) |
| AU (1) | AU7005600A (en) |
| CA (1) | CA2379754A1 (en) |
| DE (1) | DE60011623D1 (en) |
| FR (1) | FR2796568B1 (en) |
| WO (1) | WO2001005493A1 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR3066946B1 (en) * | 2017-05-30 | 2022-12-16 | Michelin & Cie | CONTINUOUS MIXING IN LIQUID PHASE FOR THE PRODUCTION OF COMPOSITES FOR USE IN ELASTOMERIC PRODUCTS |
| FR3066947B1 (en) * | 2017-05-30 | 2020-12-11 | Michelin & Cie | MIXING OF AN ELASTOMERIC COMPOSITE BY CONTINUOUS MIXING IN THE LIQUID PHASE |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CH559574A5 (en) * | 1973-10-18 | 1975-03-14 | Maier Kurt | Continuously metering detergent into running water - for washing cars using jet induction and mixing |
| DE2549086A1 (en) * | 1975-11-03 | 1977-05-18 | Helmut Mueller | Prodn. of low concn. emulsions - from viscous concentrates using double mixing to first prepare strong emulsion |
| ZA767406B (en) * | 1975-12-22 | 1977-11-30 | Ici Ltd | Method of dispersing an oil slick |
| GB2076672A (en) * | 1980-02-18 | 1981-12-09 | Unilever Ltd | Making foam |
| EP0399041A4 (en) * | 1988-04-25 | 1991-07-24 | Inzhenerny Tsentr "Transzvuk" | Method and device for preparation of emulsions |
| EP0616002B1 (en) * | 1992-09-18 | 1998-03-04 | Idemitsu Petrochemical Co., Ltd. | Process for producing polycarbonate powder |
-
1999
- 1999-07-21 FR FR9909448A patent/FR2796568B1/en not_active Expired - Fee Related
-
2000
- 2000-07-21 WO PCT/FR2000/002106 patent/WO2001005493A1/en not_active Ceased
- 2000-07-21 CA CA002379754A patent/CA2379754A1/en not_active Abandoned
- 2000-07-21 DE DE60011623T patent/DE60011623D1/en not_active Expired - Fee Related
- 2000-07-21 EP EP00958582A patent/EP1202795B1/en not_active Expired - Lifetime
- 2000-07-21 AU AU70056/00A patent/AU7005600A/en not_active Abandoned
- 2000-07-21 AT AT00958582T patent/ATE269148T1/en not_active IP Right Cessation
Also Published As
| Publication number | Publication date |
|---|---|
| DE60011623D1 (en) | 2004-07-22 |
| FR2796568B1 (en) | 2001-09-21 |
| FR2796568A1 (en) | 2001-01-26 |
| WO2001005493A1 (en) | 2001-01-25 |
| ATE269148T1 (en) | 2004-07-15 |
| WO2001005493A8 (en) | 2001-04-12 |
| AU7005600A (en) | 2001-02-05 |
| EP1202795A1 (en) | 2002-05-08 |
| CA2379754A1 (en) | 2001-01-25 |
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