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WO2018069331A1 - Appareil et procédé de mélange d'au moins deux liquides - Google Patents

Appareil et procédé de mélange d'au moins deux liquides Download PDF

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Publication number
WO2018069331A1
WO2018069331A1 PCT/EP2017/075829 EP2017075829W WO2018069331A1 WO 2018069331 A1 WO2018069331 A1 WO 2018069331A1 EP 2017075829 W EP2017075829 W EP 2017075829W WO 2018069331 A1 WO2018069331 A1 WO 2018069331A1
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WO
WIPO (PCT)
Prior art keywords
feed tube
feeding tube
tube outlet
outer feed
exit orifice
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/EP2017/075829
Other languages
English (en)
Inventor
Gloria JURADO GÁMIZ
Inmaculada MUÑOZ RUBIO
Antonio SERRANO CABO
María FLORES MOSQUERA
Alfonso M GAÑÁN-CALVO
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Ingeniatrics Tecnologias Sl
Universidad de Sevilla
Original Assignee
Ingeniatrics Tecnologias Sl
Universidad de Sevilla
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ingeniatrics Tecnologias Sl, Universidad de Sevilla filed Critical Ingeniatrics Tecnologias Sl
Publication of WO2018069331A1 publication Critical patent/WO2018069331A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40—Mixing liquids with liquids; Emulsifying
    • B01F23/45—Mixing liquids with liquids; Emulsifying using flow mixing
    • 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
    • B01F23/41—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
    • B01F23/41—Emulsifying
    • B01F23/414—Emulsifying characterised by the internal structure of the emulsion
    • B01F23/4143—Microemulsions
    • 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
    • B01F25/3131—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced in the centre of the conduit with additional mixing means other than injector mixers, e.g. screens, baffles or rotating elements
    • 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
    • B01F33/40—Mixers using gas or liquid agitation, e.g. with air supply tubes
    • B01F33/403—Mixers using gas or liquid agitation, e.g. with air supply tubes for mixing liquids
    • 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
    • B01F33/40—Mixers using gas or liquid agitation, e.g. with air supply tubes
    • B01F33/404—Mixers using gas or liquid agitation, e.g. with air supply tubes for mixing material moving continuously therethrough, e.g. using impinging jets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B7/00—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas
    • B05B7/02—Spray pistols; Apparatus for discharge
    • B05B7/04—Spray pistols; Apparatus for discharge with arrangements for mixing liquids or other fluent materials before discharge
    • B05B7/0408—Spray pistols; Apparatus for discharge with arrangements for mixing liquids or other fluent materials before discharge with arrangements for mixing two or more liquids
    • 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
    • B01F2025/91—Direction of flow or arrangement of feed and discharge openings
    • B01F2025/915—Reverse flow, i.e. flow changing substantially 180° in direction
    • 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
    • B01F2025/91—Direction of flow or arrangement of feed and discharge openings
    • B01F2025/916—Turbulent flow, i.e. every point of the flow moves in a random direction and intermixes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B7/00—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas
    • B05B7/02—Spray pistols; Apparatus for discharge
    • B05B7/04—Spray pistols; Apparatus for discharge with arrangements for mixing liquids or other fluent materials before discharge
    • B05B7/0416—Spray pistols; Apparatus for discharge with arrangements for mixing liquids or other fluent materials before discharge with arrangements for mixing one gas and one liquid
    • B05B7/0483—Spray pistols; Apparatus for discharge with arrangements for mixing liquids or other fluent materials before discharge with arrangements for mixing one gas and one liquid with gas and liquid jets intersecting in the mixing chamber

Definitions

  • the present disclosure relates generally to a apparatus and a method of mixing at least two liquids. More particularly, the present disclosure pertains to micromixing of liquids to obtain emulsions.
  • the present disclosure relates, in one embodiment, to a method of mixing at least two liquids.
  • the method includes providing a nozzle including a feeding tube having a feeding tube outlet.
  • the feeding tube is positioned in a pressure chamber containing a pressurized gas.
  • the pressure chamber includes a pressure chamber exit orifice substantially coaxial with the feeding tube outlet downstream of the feeding tube outlet.
  • the feeding tube outlet is axially offset from the pressure chamber exit orifice by an axial gap.
  • the method also includes introducing a first stream of a first liquid and a second stream of a second liquid into the feeding tube upstream from the feeding tube outlet.
  • the method further includes operating the nozzle in a flow blurring mode such that a reflux cell is formed in the feeding tube upstream from the feeding tube outlet. A turbulent mixing of the first and second liquids is thereby provided in the reflux cell.
  • An alternative embodiment includes ejecting a mixture of the first and second liquids out of the pressure chamber exit orifice.
  • Still another embodiment includes the mixture being in a form of droplets entrained in the gas.
  • each droplet including an emulsion of the first and second liquids.
  • Another embodiment includes drying the droplets to create dried mixture particles.
  • a further embodiment includes at least one of the first and second liquids including solids, and the dried mixture particles including the solids.
  • a further still embodiment includes forming an emulsion of the first and second liquids in the reflux cell and breaking the emulsion into droplets as the emulsion is ejected out of the pressure chamber exit orifice.
  • Yet another embodiment includes the first liquid and the second liquid including incompatible reagents.
  • the nozzle operation also includes forming a mixture of the first and second liquids in the reflux cell and breaking the mixture into droplets as the mixture is ejected out of the pressure chamber exit orifice.
  • the embodiment further includes reacting the incompatible reagents with each other inside each droplet so that each droplet acts as a microreactor.
  • Still another embodiment includes each of the first and second liquids being introduced into the feeding tube at separate inlets upstream of the reflux cell.
  • An even further embodiment includes the feeding tube being an outer feeding tube, and the feeding tube outlet being an outer feeding tube outlet.
  • the introduction of the first and second liquid streams further comprises introducing the first liquid into the outer feeding tube via a concentric inner feeding tube having an inner feeding tube outlet, and introducing the second liquid into the outer feeding tube at a second inlet upstream of the inner feeding tube outlet.
  • Another embodiment includes the inner feeding tube outlet being located upstream of the outer feeding tube outlet by a recess distance.
  • Still another embodiment includes the recess distance being configured to allow the reflux cell to form uninterrupted by the inner feeding tube.
  • One embodiment includes the recess distance being at least as great as an outlet diameter of the outer feeding tube outlet.
  • a further embodiment includes the nozzle operation including the reflux cell being formed in the outer feeding tube but not in the inner feeding tube.
  • a further still embodiment includes the first liquid having enough low viscosity to allow the first liquid to be introduced through the inner feeding tube.
  • An even further embodiment includes the introduction of the first and second liquid streams further including introducing a third stream of a third liquid into the feeding tube upstream from the feeding tube outlet.
  • the present disclosure also relates, in one embodiment, to a nozzle apparatus.
  • the nozzle apparatus includes a first inlet for receiving a first liquid stream, a second inlet for receiving a second liquid stream, and an outer feed tube.
  • the outer feed tube is configured to receive the first and second liquid streams and has an outer feed tube axis.
  • the outer feed tube further includes an outer feed tube outlet having an outer feed tube outlet diameter.
  • the nozzle apparatus further includes a pressure chamber surrounding the outer feed tube outlet for containing a pressurized gas.
  • the pressure chamber includes a pressure chamber exit orifice. The pressure chamber exit orifice is coaxial with the outer feed tube axis and has an exit orifice diameter.
  • the pressure chamber exit orifice is spaced from the outer feed tube outlet to define an axial gap between the pressure chamber exit orifice and the outer feed tube outlet.
  • the outer feed tube outlet diameter, the exit orifice diameter, and the axial gap are configured such that a reflux cell can form inside the outer feed tube when the first and second liquid streams are forced through the outer feed tube and the gas is forced through the axial gap.
  • a further embodiment includes an inner feed tube concentrically disposed in the outer feed tube, the first inlet being communicated with the inner feed tube.
  • Another embodiment includes the inner feed tube including an inner feed tube outlet, the inner feed tube outlet being recessed from the outer feed tube outlet by a recess distance.
  • Some embodiments include the recess distance configured to allow the reflux cell to form uninterrupted by the inner feed tube. [0024] Still another embodiment includes the recess distance being at least as great as the outer feed tube outlet diameter.
  • Some other embodiments include the outer feed tube outlet diameter being in a range of from 70 microns to 8 millimeters.
  • Yet another embodiment includes the outer feed tube outlet diameter being in a range of from 200 to 5000 microns.
  • the exit orifice diameter is in a range of from 90 to 120 percent of the outer feed tube outlet diameter.
  • the inner feed tube includes an inner feed tube outlet having an inner feed tube outlet diameter.
  • the axial gap is no greater than one fourth of the exit orifice diameter.
  • Yet another embodiment includes the outer feed tube outlet diameter being in a range of from 500 to 2000 microns.
  • inventions include the inner feed tube including an inner feed tube outlet having an inner feed tube outlet diameter.
  • Still other embodiments include the exit orifice diameter in a range of from 90 to 120 percent of the outer feed tube outlet diameter.
  • Further embodiments include the exit orifice diameter substantially equal to the outer feed tube outlet diameter.
  • Another further embodiment includes the outer feed tube outlet diameter being in a range of from 70 microns to 8 millimeters.
  • Yet further embodiments include the outer feed tube outlet diameter in a range of from 200 to 5000 microns.
  • Yet further embodiment includes the outer feed tube outlet diameter being in a range of from 500 to 2000 microns.
  • Still further embodiments include the axial gap no greater than one half of the exit orifice diameter.
  • Another embodiment includes the axial gap being no greater than one fourth of the exit orifice diameter.
  • Still another embodiment includes the outer feed tube including an inlet end opposite from the outer feed tube outlet. Both of the first and second inlets are communicated with the outer feed tube closer to the inlet end than to the outer feed tube outlet.
  • One advantage of the present invention is that it provides a technique for mixing of very viscous liquids, which are otherwise very difficult to mix. Mixing of liquids having viscosities up to 300,000 cP is possible by the techniques disclosed herein.
  • Fig. 1 is a cross-sectional side view of one embodiment of a nozzle apparatus.
  • Fig. 2 is a cross-sectional side view of another embodiment of a nozzle apparatus.
  • Fig. 3A is a photo of an example of poorly mixed liquids. It is noted that all of Figs. 3A-10B are actually photographs of dried samples of the liquid droplets which are representative of the mixing of the liquids in the droplets.
  • Fig. 3B is a photo of the example in Fig. 3A under a black light so as to show the fluorochrome introduced in one of the two liquids.
  • Fig. 4A is a photo of an example of substantially homogeneous liquid mixture achieved by the current disclosure.
  • Fig. 4B is a photo of the example in Fig. 4A under a black light so as to show the fluorochrome introduced in one of the two liquids.
  • Fig. 5A is a photo of another example of substantially homogeneous liquid mixture achieved by the current disclosure.
  • Fig. 5B is a photo of the example in Fig. 5A under a black light so as to show the fluorochrome introduced in one of the two liquids.
  • Fig. 6A is a photo of yet another example of substantially homogeneous liquid mixture achieved by the current disclosure.
  • Fig. 6B is a photo of the example in Fig. 6A under a black light so as to show the fluorochrome introduced in one of the two liquids.
  • Fig. 7A is a photo of still another example of substantially homogeneous liquid mixture achieved by the current disclosure.
  • Fig. 7B is a photo of the example in Fig. 7A under a black light so as to show the fluorochrome introduced in one of the two liquids.
  • Fig. 8A is a photo of a further example of substantially homogeneous liquid mixture achieved by the current disclosure.
  • Fig. 8B is a photo of the example in Fig. 8A under a black light so as to show the fluorochrome introduced in one of the two liquids.
  • Fig. 9A is a photo of a further still example of substantially homogeneous liquid mixture achieved by the current disclosure.
  • Fig. 9B is a photo of the example in Fig. 9A under a black light so as to show the fluorochrome introduced in one of the two liquids.
  • Fig. 10A is a photo of yet a further example of substantially homogeneous liquid mixture achieved by the current disclosure.
  • Fig. 10B is a photo of the example in Fig. 10A under a black light so as to show the fluorochrome introduced in one of the two liquids.
  • Fig. 1 1A is a droplet size distribution chart of the results of a first experiment achieved by the current disclosure.
  • Fig. 1 1 B is a droplet size distribution chart of the results of a second experiment under the same experimental conditions than 1 1A but with a liquid with higher viscosity achieved by the current disclosure.
  • Fig. 12A is a droplet size distribution chart of the results of a third experiment achieved by the current disclosure.
  • Fig. 12B is a droplet size distribution chart of the results of a fourth experiment under the same experimental conditions than 12A but with a liquid with higher viscosity achieved by the current disclosure.
  • Fig. 13A is a droplet size distribution chart of the results of a fifth experiment achieved by the current disclosure.
  • Fig. 13B is a droplet size distribution chart of the results of a sixth experiment with the same liquids than 13A but different pressure achieved by the current disclosure.
  • Fig. 13C is a droplet size distribution chart of the results of a seventh experiment with the same liquids than 13A and 13B but different pressure achieved by the current disclosure.
  • Fig. 14 is a droplet size distribution chart of the results of an eighth experiment achieved by the current disclosure as shown in Figs. 10A and 10B.
  • Fig. 15 is a schematic representation of an exemplary droplet achieved by the current disclosure. Fig. 15 is also representative of a dried particle made from a liquid droplet.
  • any part of the apparatus of the present disclosure may be made of any appropriate or suitable material including, but not limited to, metal, alloy, polymer, polymer mixture, wood, composite, or any combination thereof.
  • the nozzle apparatus 100 may include a first inlet 102 for receiving a first liquid stream 104 and a second inlet 106 for receiving a second liquid stream 108.
  • An outer feed tube 110 of the nozzle apparatus 100 may be configured to receive the first liquid stream 104 and second liquid stream 108.
  • the outer feed tube 110 may include an outer feed tube axis A1 , an outer feed tube outlet 112, and an inlet end 114 opposite from the outer feed tube outlet.
  • the outer feed tube outlet 112 may include an outer feed tube outlet diameter D1. Both the first inlet 102 and the second inlet 106 may be communicated with the outer feed tube 110 nearer the inlet end 114 than the outer feed tube outlet 112.
  • a pressure chamber 116 may surround the outer feed tube outlet 112.
  • the pressure chamber 116 may be configured to contain a pressurized gas 118, such as oxygen, nitrogen, carbon dioxide, air, and the like, and may include a pressure chamber exit orifice 120.
  • the pressure chamber exit orifice 120 may be coaxial with the outer feed tube axis A1 and may include an exit orifice diameter D2.
  • the outer feed tube outlet 112 and the pressure chamber exit orifice 120 may be spaced from each other to define an axial gap L1 between the pressure chamber exit orifice and the outer feed tube outlet.
  • the exit orifice diameter D2 may be in a range of from 90% to 120% of the outer feed tube outlet diameter D1.
  • Various embodiments may include the exit orifice diameter D2 being substantially equal to the outer feed tube outlet diameter D1.
  • the outer feed tube outlet diameter D1 being in the range of from about 70 microns to about 8 millimeters. Some embodiments may include the outer feed tube outlet diameter D1 being in the range of from about 200 microns to about 5000 microns. Some embodiments may include the outer feed tube outlet diameter D1 being in the range of from about 500 microns to about 2000 microns. In some embodiments, the axial gap L1 may be no greater than one half of the exit orifice diameter D2. In other embodiments, the axial gap L1 may be no greater than one fourth of the exit orifice diameter D2. These proportions may provide for a proper reflux cell 122 to be formed in the outer feed tube 110 for appropriate pressures and other conditions.
  • the outer feed tube outlet diameter D1 , the exit orifice diameter D2, and the axial gap L1 may be configured such that a reflux cell 122 may form inside the outer feed tube 110 when the first liquid stream 104 and the second liquid stream 108 are forced through the outer feed tube and the gas 118 is forced through the axial gap.
  • the nozzle apparatus 100 may further include an inner feed tube 124.
  • the inner feed tube 124 may be concentrically disposed in the outer feed tube 110.
  • the first inlet 102 may be communicated with the inner feed tube 124.
  • the inner feed tube 124 may include an inner feed tube outlet 126 with an inner feed tube outlet diameter D3.
  • the inner feed tube outlet diameter D3 may be any appropriate size.
  • Some embodiments may include the inner feed tube outlet diameter D3 in a range from about one quarter to about one half of the outer feed tube outlet diameter D1.
  • the inner feed tube outlet 126 may be recessed from the outer feed tube outlet 112 by a recess distance L2.
  • the recess distance L2 may allow for the reflux cell 122 to form without interruption by the inner feed tube 124.
  • the recess distance L2 may be at least as great as the outer feed tube outlet diameter D1.
  • the recess distance L2 may be up to about five times as great as the outer feed tube outlet diameter D1. These dimensions may allow for a proper reflux cell 122 to be formed in the outer feed tube 110.
  • Many embodiments include the recess distance L2 being sufficient that the reflux cell 122 may form in the outer feed tube 110 but not in the inner feed tube 124.
  • the present disclosure also relates to a method of mixing at least two liquids.
  • the method may include providing a nozzle 100 including a feeding tube 110 having a feeding tube outlet 112.
  • the feeding tube 110 may be positioned in a pressure chamber 116 containing a pressurized gas 118.
  • the pressure chamber 116 may include a pressure chamber exit orifice 120 substantially coaxial with the feeding tube outlet 112 downstream of the feeding tube outlet.
  • the feeding tube outlet 112 may be axially offset from the pressure chamber exit orifice 120 by an axial gap L1.
  • the method may also include introducing a first stream 104 of a first liquid and a second stream 108 of a second liquid into the feeding tube 110 upstream from the feeding tube outlet 112.
  • the nozzle 100 may be operated in a flow blurring mode such that a reflux cell 122 is formed in the feeding tube 110 upstream from the feeding tube outlet 112. A turbulent mixing of the first and second liquids may thereby be provided in the reflux cell 122.
  • the method may further include ejecting a mixture 128 of the first and second liquids 104, 108 out of the pressure chamber exit orifice 120.
  • the mixture 128 may be in the form of droplets 130 entrained in the gas 118.
  • each droplet 130 may include an emulsion of the first liquid 104 and the second liquid 108.
  • the second liquid 108 forms a matrix or external phase in which are dispersed minute droplets of the first liquid 104 which is the internal phase of the emulsion.
  • Some embodiments of the method may include drying the droplets 130 to create dried mixture particles 132.
  • the schematic representation of droplet 130 in Fig. 15 is also representative of a dried mixture particle 132.
  • first and second liquids 104, 108 may include at least one of the first and second liquids 104, 108 including solids that are then a part of the dried mixture particles 132.
  • the liquids 104, 108 may be highly viscous in some embodiments.
  • Other embodiments may include the liquids 104, 108 of any viscosity.
  • These liquids 104, 108 may be of any nature and may interact to form a solution instead of an emulsion.
  • the method may also include, in the introduction of the first stream 104 and second stream 108, forming an emulsion of the first and second liquids in the reflux cell 122.
  • the emulsion may be broken into droplets 130 as the emulsion is ejected out of the pressure chamber exit orifice 120.
  • Some embodiments of the method may include the first liquid 104 and the second liquid 108 including reagents that are incompatible with each other.
  • the operation of the nozzle 100 in a flow blurring mode step may further include forming a mixture 128 of the first and second liquids 104, 108 in the reflux cell 122.
  • the mixture 128 may be broken into droplets 130 as the mixture is ejected out of the pressure chamber exit orifice 120.
  • the incompatible reagents may react with each other inside each droplet 130 so that each droplet acts as a microreactor.
  • the method may also include introducing each of the first and second liquids 104, 108 into the feeding tube 110 at separate inlets 102, 106 upstream of the reflux cell 122. Some embodiments may also include introducing a third stream 134 of a third liquid into the feeding tube 110 upstream from the feeding tube outlet 112. The third liquid 134 may be introduced via one of the first and second inlets 102, 106 or may be introduced via a third inlet 136.
  • the feeding tube 110 may be an outer feeding tube in many embodiments of the method.
  • the feeding tube outlet 112 is an outer feeding tube outlet.
  • These embodiments may also include the introduction of the first liquid stream 104 into the inner feeding tube 124 at a first inlet 102 and introducing the second liquid stream 108 into the outer feeding tube 110 at a second inlet 106 upstream of the inner feeding tube outlet 126.
  • the inner feeding tube outlet 126 may be located upstream of the outer feeding tube outlet 112 by a recess distance L2.
  • the recess distance L2 may allow for the reflux cell 122 to form without interference from the inner feeding tube 124.
  • the recess distance L2 may be at least as great as an outlet diameter D1 of the outer feeding tube outlet 112.
  • the reflux cell 122 in the flow blurring step may be formed in the outer feeding tube 110 but not in the inner feeding tube 124.
  • the first liquid 104 may the proper viscosity in order to promote flow through the smaller inner tube 124.
  • Other embodiments may include the second liquid 108 having a greater viscosity than the first liquid 104.
  • Even further embodiments may include the liquids 104, 108 having the same or substantially similar characteristics, such as viscosity, especially when the single tube embodiment of Fig. 1 is used. It is also possible in some embodiments to allow the reflux cell to also form in the inner feeding tube if the inner feeding tube is of sufficient size.
  • Figs. 3A-10B are actually photographs of dried samples of the liquid droplets which are representative of the mixing of the liquids in the droplets.
  • the photos are taken through a confocal microscope.
  • the easiest way to observe and measure the mixture quality of the first and second liquids is to produce droplets through the claimed method and apparatus, dry the droplets, and put them on slides to be viewed under a microscope.
  • the hydrophobic liquid is supplemented with a fluorochrome to highlight the mixture quality. Once the droplets were dried, the fluorochrome remained and was observable under a microscope.
  • the "A" suffix figure is a photograph taken in normal light.
  • emulsifications can undesirably have a poor mixture of the two liquids.
  • the hydrophobic liquid to which flurochrome was added shown as the darker portions of Fig. 3A, did not mix homogeneously with the hydrophilic liquid. This result is shown by the representative dried sample shown in Figs. 3A and 3B.
  • Figs. 4A-10B the results of various successful experiments with the currently disclosed apparatus and method are shown. These results indicate a substantially homogeneous mixture is achieved in each droplet. These homogeneous mixtures can be achieved without premixing of the two liquids prior to feeding the liquids through the currently disclosed apparatus. As is shown in the following examples the current disclosure allows for mixing of very viscous fluids including liquids up to about 300,000 cP. Such high viscosity liquids can be very difficult to mix by prior art procedures.
  • the polymeric matrixes used in these examples are lota Carrageenan (CGI), Shellac (Sh), Methyl Cellulose (MC), Sodium alginate (Algogel), Gelatin and Nutrateric. It would be very difficult to pre-prepare emulsions of these liquids due to their high viscosities.
  • CGI Carrageenan
  • Shellac Shellac
  • MC Methyl Cellulose
  • Algogel Sodium alginate
  • Gelatin Gelatin and Nutrateric. It would be very difficult to pre-prepare emulsions of these liquids due to their high viscosities.
  • the m of gas/m of liquids data shows the ratio between the mass flow rate of the gas and the mass flow rate of the liquid (sum of liquids).
  • the "Entrapment” data shows the amount of ingredient (solution 1 here; flavor or natural extract) in the dried sample.
  • the “encapsulation efficiency” data shows the real amount of ingredient introduced in the dried sample times 100 divided
  • Solution 1 is a relatively low viscosity liquid which is able to be introduced through the inner tube 124. In these examples it is a flavor or an organic oil to which the fluorochrome has been added.
  • Solution 2 is an aqueous phase, for which different examples are shown for polymeric matrixes.
  • the polymeric matrixes used in these examples are lota Carrageenan (CGI), Shellac (Sh), Methyl Cellulose (MC), Maltodextrin (MD), Nutriose, and modified Starch (OSS).
  • the polymeric matrixes used in these examples are lota Carrageenan (CGI), Shellac (Sh), Methyl Cellulose (MC), Maltodextrin (MD), Nutrateric, Xanthan gum (Xan) and Hydroxypropylcellulose (KEF). No photographic results are shown for these tests. Table 4 is shown below:
  • KEF 5% KEF: 5% CGI: 1 % % (w/w)
  • Figs. 1 1A-14 show some examples of how droplet size distribution behaves.
  • the droplet size was measured with a Sympatec HELOS laser diffraction sensor.
  • Dv10 indicates the maximum particle diameter below which 10% of the sample volume exists.
  • Dv50 indicates the maximum particle diameter below which 50% of the sample volume exists.
  • Dv90 indicates the maximum particle diameter below which 90% of the sample volume exists.
  • the polymeric matrixes used in these examples are Gelatin, lota Carrageenan (CGI), Shellac (Sh), Methyl Cellulose (MC), Arabic Gum (GA), Starch (Clariaplus), modified Starch (OSS), Sodium alginate (Algogel) and Nutriose. Note that Figs.
  • Figs. 13A-13C (Table 8) can be compared to show the influence of pressure on droplet size. Table 8 is shown below: TABLE 8
  • the present disclosure also relates to the introduction of incompatible reagents to each other such that each droplet is a microreactor.
  • One embodiment includes the one step production of zinc carbonate crystals using two solutions that are very reactive when both contact each other. Both solutions may be nebulized using a single tube with two entrances. Air may be the pressuring gas. The droplets are obtained in air and may be recovered in a bath. As the droplets fly through the air, the mixture of the salts in the droplets start reacting and producing the zinc carbonate. In the recovery bath a suspension of ZnC0 3 is recovered. These suspension results are not to be confused with the dried product described in the previous Figures and Tables. Experimental results of the suspension are shown in Table 10 below:
  • Table 10 is just one example of potential results obtained by the current disclosure.
  • the mixed first and second liquids may form droplets, but they may also be converted into powder, granular particles, dust, and the like through any known treatment methods such as that described above with regard to Table 10.
  • This written description uses examples to disclose the invention and also to enable any person skilled in the art to practice the invention, including making and using any devices or systems.
  • the patentable scope of the invention is defined by the claims, and may include other examples that occur to those skilled in the art. Such other examples are intended to be within the scope of the claims if they have structural elements that do not differ from the literal language of the claims, or if they include equivalent structural elements with insubstantial differences from the literal language of the claims.

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  • Chemical Kinetics & Catalysis (AREA)

Abstract

Un procédé de mélange d'au moins deux liquides comprend la fourniture d'une buse (100) comprenant un tube d'alimentation (110) ayant une sortie de tube d'alimentation (112). Le tube d'alimentation est positionné dans une chambre de pression (116) contenant un gaz sous pression (118). La chambre de pression comprend un orifice de sortie de chambre de pression (120) sensiblement coaxial à la sortie de tube d'alimentation en aval de celui-ci. La sortie de tube d'alimentation est axialement décalée de l'orifice de sortie de chambre de pression par un espace axial. Le procédé comprend également l'introduction d'un premier flux (104) d'un premier liquide et d'un second flux (108) d'un second liquide dans le tube d'alimentation en amont de la sortie de tube d'alimentation. Le procédé comprend en outre le fonctionnement de la buse dans un mode de flou d'écoulement de telle sorte qu'une cellule de reflux soit formée dans le tube d'alimentation en amont de la sortie de tube d'alimentation. Un mélange turbulent des premier et second liquides est ainsi fourni dans la cellule de reflux.
PCT/EP2017/075829 2016-10-10 2017-10-10 Appareil et procédé de mélange d'au moins deux liquides Ceased WO2018069331A1 (fr)

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