EP0901810B1 - Méthode et dispositif pour la fabrication d'une dispersion de gouttelettes dans un liquide - Google Patents

Méthode et dispositif pour la fabrication d'une dispersion de gouttelettes dans un liquide Download PDF

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Publication number
EP0901810B1
EP0901810B1 EP98115928A EP98115928A EP0901810B1 EP 0901810 B1 EP0901810 B1 EP 0901810B1 EP 98115928 A EP98115928 A EP 98115928A EP 98115928 A EP98115928 A EP 98115928A EP 0901810 B1 EP0901810 B1 EP 0901810B1
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EP
European Patent Office
Prior art keywords
flow
liquid
vessel
droplet dispersion
flow direction
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.)
Expired - Lifetime
Application number
EP98115928A
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German (de)
English (en)
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EP0901810A2 (fr
EP0901810A3 (fr
Inventor
Christine Dr. Maul
Matthias Dr. Stenger
Jörg Tofahrn
Michael Van Teeffelen
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.)
Bayer AG
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Bayer AG
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Filing date
Publication date
Application filed by Bayer AG filed Critical Bayer AG
Publication of EP0901810A2 publication Critical patent/EP0901810A2/fr
Publication of EP0901810A3 publication Critical patent/EP0901810A3/fr
Application granted granted Critical
Publication of EP0901810B1 publication Critical patent/EP0901810B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime 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
    • 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
    • B01F25/30—Injector mixers
    • B01F25/31—Injector mixers in conduits or tubes through which the main component flows
    • B01F25/314—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit

Definitions

  • a variety of technical processes for the production of fine-particle spherical Polymers or microcapsules is based on the fact that initially a droplet dispersion or cores of finely divided, liquid or with a liquid shell solid material are generated, then by adding another Liquid, e.g. a hardener or an acid or base to change the pH the dispersion the droplets or the liquid surrounding the particles Shell is hardened or stabilized.
  • a hardener or an acid or base to change the pH the dispersion the droplets or the liquid surrounding the particles Shell is hardened or stabilized.
  • the problem is that the liquid is so gentle in the droplet dispersion to interfere that an agglomeration and coalescence of the droplets and thus a Disruption of the droplet size distribution is avoided.
  • the widely used microencapsulation process by coacervation or complex coacervation a droplet dispersion in one aqueous gelatin solution or an aqueous solution of gelatin and gum arabic generated at substantially neutral pH, the droplets with a Gelatin layer can be covered.
  • the encapsulation is carried out by adding a copolymer with the addition of an aqueous solution of an inorganic acid, if appropriate with subsequent lowering of the temperature of the dispersion.
  • Capsules are already so stable that they can be washed and, if necessary, added of formalin can be hardened with an increase in pH.
  • the suspension very sensitive to droplets coated with gelatin before acidification against mechanical stress. The mixture with the acid solution must therefore done very gently.
  • the object of the present invention is to provide a method and an apparatus for continuous mixing of a droplet dispersion with a liquid Introducing the liquid into a container through which the droplet dispersion flows to provide, in which the mixing of the liquid is gentle, i.e. if possible low mechanical stress is carried out.
  • the droplet dispersion is preferably axial to excite the circulating flow introduced into a cylindrical container, the introduction speed of the Droplet dispersion is 15 to 100 times larger than that due to the throughput average velocity determined by the cylindrical container ("throughflow velocity"). This causes an axial forward flow in the cylindrical container and a peripheral reverse flow with a corresponding flow deflection generated at a distance from the point of introduction for the droplet dispersion by the Droplet is run through several times.
  • the flow rate can through the cylindrical container in the range of 0.1 to 0.5 cm / s.
  • the introduction point for the droplet dispersion preferably projects axially into the cylindrical one Containers so that the cylindrical container on the back to the discharge point has an annular space in which the return flow is deflected into a forward flow becomes.
  • the liquid to be mixed into the droplet dispersion is preferably by the jacket of the cylindrical container is injected into the backflow.
  • the cylindrical container jacket has a plane perpendicular to the container axis Large number of nozzles through which the liquid is introduced.
  • the introduction speed for the liquid it can typically be 1 to 5 m / s.
  • the liquid jets are preferably injected with a directional component against the peripheral backflow of the droplet dispersion, so that the Liquid jets in the area surrounding the introduction point for the droplet dispersion Annulus create a peripheral forward flow.
  • the Ring space surrounding the inlet point causes a particularly intensive mass transfer.
  • the impulse component introduced by the liquid jets parallel to the container axis can be in the order of magnitude of the momentum input by the droplet dispersion lie, in particular about 1 to 10 times the momentum input by the Droplet dispersion.
  • the introduction takes place the droplet dispersion in the cylindrical container from the bottom up when the Droplets have a lower specific gravity than the continuous Phase.
  • the droplets experience a buoyancy, which leads to the fact that in the droplet concentration in the annular space surrounding the point of introduction for the droplet dispersion impoverished. Accordingly, the existing in the annulus peripheral upward flow has a reduced droplet concentration. This is particularly important if, for reasons of economy, droplet dispersions used with very high droplet concentrations of 40 to 60 vol% become.
  • the liquid is then injected into a droplet dispersion with significantly reduced droplet concentration, so the risk the agglomeration of droplets in the area of the injection is further reduced.
  • the flow direction through the cylindrical is preferred Container selected from top to bottom if the droplets have a greater density, than the continuous phase.
  • Fig. 1 shows in principle a container 1 in the form of a cylindrical column with a axially arranged inlet pipe 2 for the droplet dispersion.
  • the generation of the Droplet dispersion can be carried out by methods known per se. For example can the droplet dispersion by spraying the liquid forming the droplet be produced in an aqueous gelatin solution.
  • On a circumferential line perpendicular to Axis 3 of the cylindrical container 1 are a plurality of nozzles 4, for example provided with a diameter of 0.4 mm.
  • the number of nozzles can be, for example 12 to 120.
  • the nozzles are fed from an annular channel 5, in the the liquid is introduced through one or more supply lines 6.
  • the cross-sectional area the inlet tube 2 for the droplet dispersion can 1/12 to 1/45 of Cross-sectional area of the cylindrical container 1 amount.
  • Droplet dispersion shear rate below 20 / s, preferably below 10 / s.
  • the estimate of the shear rate is double Inflow velocity of the droplet dispersion through half the container radius divided.
  • the inlet pipe 2 for the droplet dispersion projects at least over one Length, which corresponds to the radius of the container 1, into this, so that the rear an annular space 7 is formed by the inlet point, in which the return flow 11 is deflected becomes.
  • the nozzles 4 are inclined upwards directed so that a peripheral forward flow 13 is excited in the annular space 7 becomes.
  • Fig. 2 shows an enlarged view of the flow conditions in the area of Annulus 7, the dashed lines 21 and 22 the boundaries between the Flow areas with a forward component on the one hand and a backflow component otherwise specify.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing Of Micro-Capsules (AREA)

Claims (10)

  1. Procédé pour mélanger en continu une dispersion de gouttelettes avec un liquide par introduction du liquide dans un récipient
    (1) traversé par la dispersion de gouttelettes, caractérisé en ce que le liquide est injecté dans la dispersion de gouttelettes sous forme d'une multiplicité de fins jets de liquide, de sorte que l'énergie cinétique des jets de liquide est dissipée à peu de distance du site d'injection et que la suite du mélange se déroule sous l'effet d'un courant de circulation (10, 11) produit dans le récipient (1) avec des vitesses de cisaillement inférieures à 20/s.
  2. Procédé selon la revendication 1, caractérisé en ce que la dispersion de gouttelettes est introduite axialement dans le récipient (1) sans courant de retour avec une vitesse qui est supérieure de 15 à 100 fois à la vitesse du courant traversant dans le récipient.
  3. Procédé selon la revendication 1 ou 2, caractérisé en ce que les jets de liquide présentent un diamètre de 0,1 à 0,8 mm.
  4. Procédé selon l'une des revendications 1 à 3, caractérisé en ce que la vitesse maximale du courant de circulation est supérieure de 5 à 20 fois à la vitesse du courant traversant.
  5. Procédé selon l'une des revendications 1 à 4, caractérisé en ce que le courant de circulation consiste en un courant axial (10) dans la direction du courant traversant et en un courant de retour périphérique (11).
  6. Procédé selon l'une des revendications 1 à 5, caractérisé en ce que l'injection du liquide a lieu dans un plan qui, par rapport à la direction du courant traversant, est situé sensiblement à la hauteur du site d'introduction pour la dispersion de gouttelettes, avec une composante de courant dans la direction du courant traversant, de sorte qu'un courant périphérique (13) est produit dans la direction du courant traversant en dessous du plan.
  7. Procédé selon l'une des revendications 1 à 6, caractérisé en ce que la direction du courant traversant (10) est dirigée vers le haut quand les gouttelettes sont plus légères spécifiquement que le milieu dispersant, et vers le bas quand les gouttelettes sont plus lourdes spécifiquement que le milieu dispersant.
  8. Dispositif pour le mélange continu d'un liquide avec une dispersion de gouttelettes contenant un récipient cylindrique (1) comportant une entrée centrale (2) pour la dispersion de gouttelettes et une multiplicité de buses d'injection (4) de faible diamètre qui débouchent dans le récipient (1) dans un plan de coupe de la paroi du récipient perpendiculairement à l'axe (3) et dans la direction du courant traversant (10) sensiblement à la hauteur de l'entrée (2).
  9. Dispositif selon la revendication 8, où les buses d'injection (4) comportent une composante de direction dans la direction du courant traversant et l'entrée est sous forme d'un tube d'entrée (2) faisant saillie dans le récipient (1), de sorte que le récipient (1) comporte en arrière du site d'entrée une cavité annulaire (7) entourant le tube d'entrée (2).
  10. Dispositif selon la revendication 8 ou 9, où le tube d'entrée (2) comporte une surface en section droite égale à 1/12 à 1/45 de la surface en section droite du récipient.
EP98115928A 1997-09-05 1998-08-24 Méthode et dispositif pour la fabrication d'une dispersion de gouttelettes dans un liquide Expired - Lifetime EP0901810B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19738870A DE19738870A1 (de) 1997-09-05 1997-09-05 Verfahren und Vorrichtung zur kontinuierlichen Vermischung einer Tröpfchendispersion mit einer Flüssigkeit
DE19738870 1997-09-05

Publications (3)

Publication Number Publication Date
EP0901810A2 EP0901810A2 (fr) 1999-03-17
EP0901810A3 EP0901810A3 (fr) 2001-02-07
EP0901810B1 true EP0901810B1 (fr) 2003-02-12

Family

ID=7841320

Family Applications (1)

Application Number Title Priority Date Filing Date
EP98115928A Expired - Lifetime EP0901810B1 (fr) 1997-09-05 1998-08-24 Méthode et dispositif pour la fabrication d'une dispersion de gouttelettes dans un liquide

Country Status (5)

Country Link
US (2) US6102309A (fr)
EP (1) EP0901810B1 (fr)
JP (1) JPH11137985A (fr)
DE (2) DE19738870A1 (fr)
HU (1) HUP9802004A3 (fr)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10206103A1 (de) * 2002-02-13 2003-08-21 Basf Ag Vorrichtung und Verfahren zur Herstellung von Formkörpern aus thermoplastischen Polymeren
SE525983C2 (sv) * 2003-10-13 2005-06-07 Metso Paper Inc Blandningsanordning för inblandning av ett vätskeformigt medium i ett annat vätskeformigt medium
DE102005056723B4 (de) * 2005-11-29 2012-08-30 Roland Damann Vorrichtung zum Vermischen und Reagieren eines Gases und/oder einer Flüssigkeit mit einem flüssigen Medium
GB201604412D0 (en) * 2016-03-15 2016-04-27 King S College London Method and system pressure drop estimation
NL2023054B1 (en) * 2019-05-02 2020-11-23 Water Iq Int B V Mixing device for mixing hydrogen peroxide and water

Family Cites Families (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB189627086A (en) * 1896-05-30 1897-01-30 Stanislas Dominique Gillet A New or Improved Burner for Lighting by Acetylene or other Gases Rich in Carbon.
US3242051A (en) * 1958-12-22 1966-03-22 Ncr Co Coating by phase separation
US3234307A (en) * 1962-10-03 1966-02-08 Dow Chemical Co Process for preparing pellets of substituted phenols
BE658300A (fr) * 1964-01-24
CH519448A (de) * 1968-04-11 1972-02-29 Inventa Ag Mischvorrichtung
US3419082A (en) * 1967-03-16 1968-12-31 Bliss E W Co Portable foam nozzle
JPS5273202A (en) * 1975-12-13 1977-06-18 Mitsubishi Heavy Ind Ltd Suction type fluid mixing nozzle
EP0053411B1 (fr) 1980-12-02 1985-02-06 Shell Internationale Researchmaatschappij B.V. Pistolet pour matière de remplissage convenant à l'injection dans des cavités
US4411398A (en) * 1981-04-20 1983-10-25 General Dynamics, Pomona Division Double fabric retractable wing construction
NL8104179A (nl) * 1981-09-10 1983-04-05 Talmer B V Werkwijze voor het toevoeren van vezelig isolatiemateriaal, in het bijzonder glaswolvezels, in de spouw van een spouwmuur.
US4637905A (en) * 1982-03-04 1987-01-20 Batelle Development Corporation Process of preparing microcapsules of lactides or lactide copolymers with glycolides and/or ε-caprolactones
US4545157A (en) * 1983-10-18 1985-10-08 Mccartney Manufacturing Company Center feeding water jet/abrasive cutting nozzle assembly
US4738614A (en) * 1986-07-25 1988-04-19 Union Carbide Corporation Atomizer for post-mixed burner
US5126381A (en) * 1988-12-19 1992-06-30 Dow Corning Corporation Bead processor
US5173007A (en) * 1989-10-23 1992-12-22 Serv-Tech, Inc. Method and apparatus for in-line blending of aqueous emulsion
FR2689418B1 (fr) * 1992-04-03 1994-07-01 Centre Nat Rech Scient Procede de preparation de micro-capsules ou de liposomes de tailles controlees par application d'un cisaillement constant sur une phase lamellaire.
US5637350A (en) * 1994-05-13 1997-06-10 A.P.I. Asphalt Prilling Inc. Encapsulation of asphalt prills
DE4421352C2 (de) * 1994-06-17 1997-03-20 Specker Helmut Verfahren und Vorrichtung zum Verdünnen eines Flüssigkonzentrats mit Wasser
US5645223A (en) * 1995-10-19 1997-07-08 Hull; Harold L. Liquid/foam/mixing/aeration adapter apparatus

Also Published As

Publication number Publication date
EP0901810A2 (fr) 1999-03-17
JPH11137985A (ja) 1999-05-25
HUP9802004A2 (hu) 1999-04-28
EP0901810A3 (fr) 2001-02-07
HUP9802004A3 (en) 2000-06-28
DE19738870A1 (de) 1999-03-18
US6102309A (en) 2000-08-15
HU9802004D0 (en) 1998-12-28
DE59807165D1 (de) 2003-03-20
US6170761B1 (en) 2001-01-09

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