EP2396108A1 - Procédé de production d'une dispersion et dispositif associé - Google Patents

Procédé de production d'une dispersion et dispositif associé

Info

Publication number
EP2396108A1
EP2396108A1 EP10701099A EP10701099A EP2396108A1 EP 2396108 A1 EP2396108 A1 EP 2396108A1 EP 10701099 A EP10701099 A EP 10701099A EP 10701099 A EP10701099 A EP 10701099A EP 2396108 A1 EP2396108 A1 EP 2396108A1
Authority
EP
European Patent Office
Prior art keywords
volume flow
substance
working fluid
dispersion
nozzle
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.)
Withdrawn
Application number
EP10701099A
Other languages
German (de)
English (en)
Inventor
Heike Schuchmann
Karsten Köhler
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.)
Karlsruher Institut fuer Technologie KIT
Original Assignee
Karlsruher Institut fuer Technologie KIT
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 Karlsruher Institut fuer Technologie KIT filed Critical Karlsruher Institut fuer Technologie KIT
Publication of EP2396108A1 publication Critical patent/EP2396108A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40—Mixing liquids with liquids; Emulsifying
    • B01F23/41—Emulsifying
    • 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
    • B01F23/48—Mixing liquids with liquids; Emulsifying characterised by the nature of the liquids
    • B01F23/482—Mixing liquids with liquids; Emulsifying characterised by the nature of the liquids using molten solids
    • 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
    • B01F23/70—Pre-treatment of the materials to be mixed
    • 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
    • B01F23/70—Pre-treatment of the materials to be mixed
    • B01F23/711—Heating materials, e.g. melting
    • 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
    • B01F23/80—After-treatment of the mixture
    • 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
    • B01F23/80—After-treatment of the mixture
    • B01F23/802—Cooling the mixture
    • 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
    • B01F25/105—Mixing heads, i.e. compact mixing units or modules, using mixing valves for feeding and mixing at least two components
    • 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
    • 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
    • B01F23/4146—Emulsions including solid particles, e.g. as solution or dispersion, i.e. molten material or material dissolved in a solvent or dispersed in a liquid
    • 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
    • B01F33/30—Micromixers
    • B01F33/301—Micromixers using specific means for arranging the streams to be mixed, e.g. channel geometries or dispositions
    • B01F33/3011—Micromixers using specific means for arranging the streams to be mixed, e.g. channel geometries or dispositions using a sheathing stream of a fluid surrounding a central stream of a different fluid, e.g. for reducing the cross-section of the central stream or to produce droplets from the central stream

Definitions

  • the invention relates to a method for producing a dispersion and a device for this using the formation of a melt emulsion.
  • dispersions are prepared by the solids required for the dispersion are brought by Feinstmahlung to the desired particle size and dispersed in a working fluid.
  • undesired contamination of the dispersion occurs.
  • the expense of solvent can be reduced or avoided that the material to be dispersed is melted in the working fluid under vigorous turbulence and formation of an emulsion and then cooled rapidly, whereby the distributed droplets in the emulsion be solidified. Due to the inhomogeneous cooling process, a reproducible formation of a uniform particle size is not given.
  • a protective colloid must be added which is stable at the melting temperature of the material to be dispersed. The choice of such stabilizers must be made individually for each substance. Temperature-resistant stabilizers are also expensive.
  • the object of the invention is therefore a method and a corresponding thereto
  • the invention is achieved by a process for preparing a dispersion of a solid material, in which the substance is melted by increasing the temperature above its melting point and guided in a first volume flow.
  • the first volume flow is combined with a second volume flow at a temperature below the melting point of the substance under turbulence, wherein at least one of the two volume flows contains a working fluid and droplets of the substance form after mixing the two volume flows of the second volume flow are solidified into particles, whereby the dispersion is formed from these and the working fluid.
  • the second, cooler volume flow fulfills in particular the task of rapidly cooling, solidifying and isolating the liquid, droplet-forming constituents of the substance, so that coalescence of the still liquid droplets or coagulation of the already solid particles is largely avoided.
  • materials for the preparation of the dispersion pharmaceutical products, color pigments, waxes and the like can be used.
  • At least one volume flow is mixed under high pressure via a homogenizing with the second flow, so that the mixing with different outlet cross-sections and pressures volume flows advantageous to the separation of the molten substance, the cooling and stabilization of the still liquid droplets or which already affect as a result of the cooling of these solidified by the second volume flow particles.
  • the first volume flow can be pressed with the molten substance through the homogenization, so that even by passing the homogenization of the substance undergoes sufficient comminution in droplets.
  • the cooling volume flow in several orifices which are arranged, for example, around the mouth of the at least one homogenization, can be increased.
  • Several homogenization openings of one volume flow can be connected to the corresponding outlets of the other volume flow to a processing unit, so that a corresponding throughput is ensured.
  • the cooling second volume flow can be forced through the homogenization and the molten material can be metered in the first volume flow at a lower pressure to the mouth of the at least one homogenization.
  • the still relatively large units such as drops or flow sections are sufficiently comminuted by the high, caused by the small cross-section of the homogenizing flow rate of the working medium of the second volume flow and cooled incidentally.
  • This procedure is particularly advantageous if the high-pressure pumps in front of the at least one homogenizing the melting temperatures of the substance should not be expected. This may be particularly relevant if the melting temperatures of the substance are very high.
  • the substance can be initially introduced in the first volume flow by the so-called pre-mix method or two-phase.
  • the premix process the substance is presented in a separate working medium as a melt emulsion.
  • the second volume flow contains the same or another working medium.
  • the working fluids are selected according to the properties of the dispersion to be prepared in conjunction with the properties of the material to be dispersed. It has been found that in most cases water can be used as the first and / or second working fluid, so that the process can be carried out inexpensively.
  • the two-phase process the molten substance without working medium is kept in a flow, while in the other volume flow, the working fluid is kept. The production of a melt emulsion is omitted, whereby the process is simplified.
  • the melt of the substance, so the first volume flow over the at least one Homogenmaschinesdüse brought or reasons of high melting temperatures to protect the high-pressure pumps via the line with lower pressure with the second, the working fluid-containing volume flow are mixed, in this case by the Homogenizing is performed.
  • temperature-resistant stabilizers such as emulsifiers or protective colloids omitted in the first volume flow.
  • a stabilizing agent or other auxiliaries be practical for the at least one homogenizing nozzle after the mouth, this can be metered with the second volume flow having a lower temperature, so that correspondingly temperature-sensitive reagents can be used.
  • one or more jets of the second working fluid may be directed at an angle greater than 1 ° and less than or equal to 180 ° to the mouth of the at least one homogenizing nozzle, with an angle of approximately 90 ° being particularly advantageous has proved.
  • Several such chambers with corresponding derivatives of the dispersion can be provided on a device for carrying out the method.
  • the dispersion may contain a method step for concentrating the particles.
  • known steps of filtration or ultrafiltration can take place.
  • the particles can be isolated in powder form.
  • reagents for better redispersion can be dosed accordingly.
  • the invention is further characterized by a device for producing a dispersion at least consisting of a first, adjustable to a melting point of a substance, the first volume flow with at least the molten substance leading line and another, a second volume flow with at least one working fluid dissolved under the melting temperature-conducting line, wherein both lines are combined with each other and at least one line at the mouth contains at least one homogenizing and at least one opening of the other line at an angle greater than 1 ° and less than 180 ° to the emerging from the homogenizing other Volume flow is directed and the mixed volume flows are derived by a common derivative.
  • a device for producing a dispersion at least consisting of a first, adjustable to a melting point of a substance, the first volume flow with at least the molten substance leading line and another, a second volume flow with at least one working fluid dissolved under the melting temperature-conducting line, wherein both lines are combined with each other and at least one line at the mouth contains at least one homogenizing and at least one opening of the
  • the cross section of the homogenizing nozzle is less than or equal to 1000 microns, preferably between 100 and 400 microns, wherein the cross section of the supply line may be a multiple of the cross section of the homogenizing.
  • the line directed towards the at least one homogenizing nozzle may have openings spaced apart from one another in the direction of the discharges. In this way, with one or a set of openings, the mouth of the homogenizing nozzle can be flowed directly, while the opening spaced therefrom, or a set of these, acts on the already provisionally mixed volume flows at a distance.
  • the distance of the mouths of the low-pressure line to the mouth of the at least one homogenizing nozzle can be between 0 mm and 100 mm.
  • the device may be connected downstream of the derivative of a device for the concentration of the dispersed material.
  • the invention will be explained with reference to the embodiments illustrated in Figures 1 to 5 of a sequence of the method according to the invention with elements of the apparatus for producing a dispersion. These show: Figure 1 is a schematic representation of an apparatus for imple out the method for producing a dispersion and
  • FIGS 2 to 5 different embodiments of the leadership of the method with different composite flow rates.
  • the schematically illustrated device 1 provides for the promotion of two volume flows 2, 3 along the arrows 4, 4a in a common chamber 5, in which they are mixed and are derived in a common discharge line 6.
  • the two volume flows 2, 3 are each pressurized by means of a pump 7, 8 and brought by means of a heat exchanger 9, 10 to a predetermined temperature.
  • One of the volume flows 2, 3 contains a, by means of the corresponding heat exchanger 9, 10 above its melting point heated, so molten material, the other one to a means of the corresponding heat exchanger 9, 10 brought to a temperature below the melting point of the substance Ar beitsfluid. It is understood that the working fluid can also be left at ambient temperature, whereby the corresponding heat exchanger can be omitted.
  • the volume flows 2, 3 are in each case with the necessary pressure by at least one Homogenmaschinesdüse 11 or the lines 12, 13 - the line 13 is connected according to line 12 in a manner not shown to the flow 3 - pressed into the chamber 5.
  • the pump 7 is a high-pressure pump, while the pump 8 due to the higher cross-section and possibly higher number of lines 12, 13 must provide a lower pressure.
  • the molten substance is transferred into individual droplets, which are cooled by the working fluid below the melting point and particles be solidified.
  • the working fluid further separates and stabilizes the particles and forms with them the dispersion draining off the effluent.
  • FIG. 2 shows schematically the premix process of the preparation of the dispersion
  • melt emulsion 16 15 of a melt emulsion 16 and the working fluid 17.
  • the melt emulsion 16 15 of a melt emulsion 16 and the working fluid 17.
  • the 16 consists of a working fluid 18, in which the substance 19 is melted and processed into a crude emulsion.
  • the crude emulsion leaves the homogenizing nozzle 11 under pressure and is impinged by the working fluid 17; the turbulent mixing of the crude emulsion and the working fluid produces small droplets 20 of the substance 19 which are added by the working fluid 17 at a temperature below the melting point of the substance 19 be cooled solid particles.
  • the droplets 20 or particles are prevented from coalescing and coagulating by the volume increase of the dispersion 15.
  • FIG. 3 shows an alternative premix process in which the melt emulsion 16 of substance 19 and working fluid 18 are metered into the chamber 5 at low pressure, while the working fluid is pressed under high pressure through the homogenization nozzle 11. Due to the strong pressure of the working fluid 17 due to the high pressure, the raw particles 21 of the substance 19 are shattered. The resulting smaller diameter droplets 20 are cooled to particles by the cooler working fluid 17 and solidified. The resulting dispersion 15 is derived.
  • the advantage of this method is the protection of the high-pressure pump, which only has to compress the cooler working fluid 17.
  • Figure 4 shows a method for producing the dispersion 15 by means of two phases, the molten substance 19 is pressed as a melt without working fluid through the Homogenticiansdüse 11 and then according to the embodiments of Figure 2 of the working fluid 17 to form the dispersion 15 is flown , Due to the smaller amount of working fluid in the dispersion 15, optionally may be dispensed with a concentration. The process may be cheaper due to the lower use of working fluid.
  • FIG. 5 shows the case, inverse to the method of FIG. 4, of a method for producing the dispersion 15 by means of two phases.
  • the melt of the cloth 19 is dosed at a low pressure while the working fluid 17 is pressed by the homogenizing nozzle 11. Due to the high flow velocity is a turbulent mixing of the melt of the substance 19, the one Emulsification of the substance 19 to small droplets 20 with a cooling and solidification of the result, whereby the dispersion 15 is formed.
  • the advantage of this method, apart from the use of the melt without working fluid, is a protection of the high-pressure pump in front of the homogenizing nozzle 11.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Colloid Chemistry (AREA)

Abstract

L'invention concerne un procédé et un dispositif de dispersion de matières au moyen d'une fusion et d'une émulsification de la matière. A cet effet, une matière est fondue dans un premier flux volumique (2) par une élévation de la température au-delà de son point de fusion. Un second flux volumique (3) contenant un fluide actif à une température inférieure à la température de fusion est mélangé en turbulence au premier flux volumique, de façon à former à partir de la matière des gouttelettes qui sont refroidies et dispersées sous forme de particules par le second flux volumique (3). Le fluide actif et les particules forment alors la dispersion. Il n'est pas nécessaire d'utiliser des agents émulsifiants pour stabiliser l'émulsion.
EP10701099A 2009-02-16 2010-01-19 Procédé de production d'une dispersion et dispositif associé Withdrawn EP2396108A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102009009060A DE102009009060B3 (de) 2009-02-16 2009-02-16 Verfahren zur Herstellung einer Dispersion und Vorrichtung hierzu
PCT/EP2010/000260 WO2010091769A1 (fr) 2009-02-16 2010-01-19 Procédé de production d'une dispersion et dispositif associé

Publications (1)

Publication Number Publication Date
EP2396108A1 true EP2396108A1 (fr) 2011-12-21

Family

ID=42040314

Family Applications (1)

Application Number Title Priority Date Filing Date
EP10701099A Withdrawn EP2396108A1 (fr) 2009-02-16 2010-01-19 Procédé de production d'une dispersion et dispositif associé

Country Status (3)

Country Link
EP (1) EP2396108A1 (fr)
DE (1) DE102009009060B3 (fr)
WO (1) WO2010091769A1 (fr)

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3887130A (en) * 1973-09-20 1975-06-03 Occidental Petroleum Canada Sulfur pelletizing
US4087498A (en) * 1975-10-31 1978-05-02 Union Oil Company Of California Method of producing sulfur particles
DE3538751A1 (de) * 1985-10-31 1987-05-07 Henkel Kgaa Verfahren zur herstellung von perlglanzdispersionen
DE3916465A1 (de) 1989-05-20 1990-11-22 Bayer Ag Herstellung kugelfoermiger dispersionen durch kristallisation von emulsionen
DE4329446A1 (de) * 1993-09-01 1995-03-02 Basf Ag Verfahren zur Herstellung von feinteiligen Farb- oder Wirkstoffzubereitungen
DE10048797A1 (de) * 2000-10-02 2002-04-18 Bayer Ag Wirkstoffhaltige Emulsionen
WO2004076050A2 (fr) * 2003-02-28 2004-09-10 Central Research Institute Of Electric Power Industry Procédé et appareil de production de particules fines
WO2008031780A2 (fr) * 2006-09-13 2008-03-20 Basf Se Procédé pour produire des dispersions à fines particules
DE102007014916A1 (de) * 2007-03-26 2008-10-02 Evonik Degussa Gmbh Verfahren und Vorrichtung zum Hochdruckdispergieren

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO2010091769A1 *

Also Published As

Publication number Publication date
WO2010091769A1 (fr) 2010-08-19
DE102009009060B3 (de) 2010-05-12

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