EP0570335B1 - Dispositif et procédé pour mélanger un composant pulvérulent solide dans un matériau liquide - Google Patents

Dispositif et procédé pour mélanger un composant pulvérulent solide dans un matériau liquide Download PDF

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Publication number
EP0570335B1
EP0570335B1 EP93810315A EP93810315A EP0570335B1 EP 0570335 B1 EP0570335 B1 EP 0570335B1 EP 93810315 A EP93810315 A EP 93810315A EP 93810315 A EP93810315 A EP 93810315A EP 0570335 B1 EP0570335 B1 EP 0570335B1
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EP
European Patent Office
Prior art keywords
line
means according
passage
interior
mixing
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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
EP93810315A
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German (de)
English (en)
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EP0570335A1 (fr
Inventor
Urs Liechti
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JETSOLUTIONS SA
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Urs Liechti
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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
    • B01F23/50—Mixing liquids with solids
    • 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
    • B01F25/50—Circulation mixers, e.g. wherein at least part of the mixture is discharged from and reintroduced into a receptacle
    • B01F25/53—Circulation mixers, e.g. wherein at least part of the mixture is discharged from and reintroduced into a receptacle in which the mixture is discharged from and reintroduced into a receptacle through a recirculation tube, into which an additional component is introduced
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/05—Stirrers
    • B01F27/11—Stirrers characterised by the configuration of the stirrers
    • B01F27/112—Stirrers characterised by the configuration of the stirrers with arms, paddles, vanes or blades
    • B01F27/1122—Stirrers characterised by the configuration of the stirrers with arms, paddles, vanes or blades anchor-shaped
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/05—Stirrers
    • B01F27/11—Stirrers characterised by the configuration of the stirrers
    • B01F27/114—Helically shaped stirrers, i.e. stirrers comprising a helically shaped band or helically shaped band sections
    • B01F27/1145—Helically shaped stirrers, i.e. stirrers comprising a helically shaped band or helically shaped band sections ribbon shaped with an open space between the helical ribbon flight and the rotating axis
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/23—Mixers with rotary stirring devices in fixed receptacles; Kneaders characterised by the orientation or disposition of the rotor axis
    • B01F27/232—Mixers with rotary stirring devices in fixed receptacles; Kneaders characterised by the orientation or disposition of the rotor axis with two or more rotation axes
    • B01F27/2322—Mixers with rotary stirring devices in fixed receptacles; Kneaders characterised by the orientation or disposition of the rotor axis with two or more rotation axes with parallel axes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B01F27/85—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with two or more stirrers on separate shafts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B01F27/90—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with paddles or arms 
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B01F27/92—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with helices or screws

Definitions

  • the invention relates to a device and a method for adding a pourable component to a liquid base, namely a device according to the preamble of claim 1 and a method according to the preamble of claim 10.
  • the device and the method serve in particular to produce mixtures, such as emulsions, suspensions and the like, for example pastes, ointments, lotions, creams etc., which are used for pharmaceutical or cosmetic purposes, the mixtures produced forming the end product or even further can be processed.
  • mixtures such as emulsions, suspensions and the like, for example pastes, ointments, lotions, creams etc., which are used for pharmaceutical or cosmetic purposes, the mixtures produced forming the end product or even further can be processed.
  • the device and the method can be provided, for example, for the batch-wise emulsification of a product which has at least two immiscible components, such as water and at least one fat and / or oil, the two immiscible components preferably being at about 60 to 80 ° C temperature be warmed before mixing them together.
  • a water-in-oil emulsion can first be produced, which is cooled during the emulsification process and, during a phase transition, changes into an oil-in-water emulsion which forms the end product.
  • Devices which are known on the market and are intended for batch operation for mixing a good, in particular for adding a pourable component to a liquid base, have a double-walled container which at least has a stirrer which can be rotated about a vertical axis, a homogenizer and a device which serves to introduce a cooling or heating fluid between the two walls of the container.
  • the homogenizer serves to vertically circulate the material moved by the stirrer and to reduce the emulsion droplets by shear in the production of emulsions.
  • Homogenizers which exert their shearing action by rotating tools are preferably installed in the known devices.
  • colloid mills, pin mills or dissolver disks working according to the rotor-stator principle can be inserted into the containers, one or the other homogenizer being preferred depending on the product to be manufactured.
  • an oil-in-water emulsion intended as a medicament is produced with the known devices, in which the oil is to be distributed in the form of fine droplets in the water, at least one oil is heated in a preheating container and mixed with the water in the liquid state aforementioned container mixed. The material formed from water and oil is then cooled with constant stirring and homogenization by a cooling fluid passed between the two walls of the container for a predetermined period of time. Additional components such as at least one active pharmaceutical ingredient and / or at least one dye are added to the liquid phase presented in the container during the mixing and emulsification process.
  • the invention is based on the object of creating a device and a method which do not have the disadvantages of the known devices and methods.
  • it should be possible to mix the components of the goods quickly and optimally with one another and to wet powdery components optimally when they are introduced into a liquid base composition, so that the product formed accordingly has a homogeneous composition regardless of the type of goods.
  • the device should be able to be used for the production of various mixtures, for example for the production of emulsions, suspensions, gels and the like.
  • a device according to the preamble of claim 1 is known from document EP-A-0 419 280. In it, however, the solid is mixed in two stages, vertically into circularly moving liquid flows.
  • the device for mixing a good shown in FIG. 1 and designated as a whole by 1 has a container 2.
  • This is essentially rotationally symmetrical, that is to say it has a vertical axis 3, and has a double-walled wall 4, at the lower end of which a floor 5 is connected.
  • the container 2 is also provided with a cover 6 detachably connected to the wall 4, which together with the wall 4 and the bottom 5 delimits an interior space 7.
  • the bottom 5 has an outlet 8 at the lower end, which is provided with a regulating element 9 which can optionally be locked and released for the outlet 8.
  • An anchor stirrer 10 and a spiral stirrer 11 are arranged in the interior 7 of the container 2, both of which can be rotated about their vertical axis by a common drive device 12.
  • the shafts 10a and 11a of the two stirrers 10 and 11 penetrate the cover 6 and can be driven in opposite directions by the motor 13 of the drive device 12 via a gear at speeds of, for example, 10 to 20 or 25 to 50 revolutions per minute.
  • the two stirrer arms 10b and 10c of the anchor stirrer 10 are adapted to the inner shape of the container 2 and have movable scrapers 13 which are pressed against the inner wall of the container 2 by the centrifugal force thereby generated when the stirrer 10 is rotated.
  • the device 1 also has a line 14 which connects the outlet 8 to the inlet 6a provided in the cover 6. Through this line 14, at least part of the material present in the container is passed through during the mixing and emulsification process and thereby circulated vertically.
  • the line 14 has a pump 15, an outlet valve 16 and a solids feed device 17 arranged downstream of the pump 15 in the flow direction. The latter essentially serves to admix at least one component consisting of solid particles to a liquid base compound passed through the line 14 by means of the pump 15.
  • FIGS. 2 and 3 Two embodiments of the solids introduction device 17, designated 17a and 17b, are shown in FIGS. 2 and 3 on a larger scale and in detail. They are essentially cylindrical, that is to say they have an axis 18, and have a passage 19 through which the liquid base material or a mixture produced during the mixing or emulsification process can be passed.
  • the passage 19 is formed by a cross-sectional constriction, has an oval, for example elliptical, cross section at least over part of its length and is formed by a cavity which is rectangular in cross section, for example square 20 interrupted, the cross-sectional area perpendicular to the passage 19 is slightly larger than the cross section of the passage 19.
  • a feed line 21 opens into the cavity 20, which serves to feed a bulk material, for example a powdered medicinal product, to the liquid matrix passed through the passage 19 to mix.
  • This feed line 21 has a metering element 22 connected to the solids introduction device 17, which - as shown in FIGS. 2 and 3 - can be designed as a flap valve 22a or pinch valve 22b.
  • the solids feed device 17 has two further feed lines 23 and 24 opening into the cavity 20, through which liquid additives can be added to the mixed material passed through the solids feed device 17.
  • a turbulence tube 25 connected to the line 14 via the inlet 6a and projecting into the interior 7. This serves to homogenize the material passed through the turbulence tube 25 and to optimally distribute it in the interior 7 of the container 2.
  • the turbulence tube 25, the lower end of which is shown on a larger scale and also in detail in FIG. 4, has an elongated, sleeve-like and essentially cylindrical housing 26 which has a bottom 26a with a circular opening 26b at the lower end.
  • An axially displaceable displacement element 27 is also arranged in the interior of the housing 26. This is essentially rotationally symmetrical and has an enlarged diameter at its end 27a facing the base 26a.
  • the actuating device 28 has a manually, electrically and / or hydraulically adjustable actuating element which serves for optionally enlarging or reducing the gap width s.
  • the turbulence tube 25 also has a baffle plate 29 arranged at the lower end, through which the material guided through the opening 26a is deflected and evenly distributed in the interior 7.
  • the device 1 has a heating and / or cooling device, not shown, with which a heating or cooling fluid can optionally be introduced into the intermediate space formed by the two wall parts of the double-walled container 2, in order to thereby heat or cool the material present in the container.
  • a batch of an oil-in-water emulsion is to be produced using a device described with reference to FIGS. 1 to 4, a batch of water is introduced into the interior 7 of the container 2 through an inlet (not shown in FIG. 1).
  • a heating fluid for example hot water and / or steam, is then passed through the intermediate space 5 of the wall 4 in order to heat the water present in the interior 7 of the container 2 to a temperature of, for example, 60 to 80 ° C.
  • a batch of at least one oil is heated in a preheating container to a temperature that is also 60 to 80 ° C.
  • a vacuum can be generated in container 2 in order to prevent the formation of air bubbles in the emulsion.
  • a vacuum pump used to generate the vacuum can be connected to the interior 7 of the container 2 via a connection (not shown in FIG. 1).
  • the shut-off device 9 is opened and at least some of the water present in the container 2 is passed through the line 14 by means of the conveying device 15.
  • the heated oil is mixed through the feed line 23 or 24 of the solids feed device 17 into the water passed through the passage 19.
  • the static pressure of the water jet passed through the line 14 in the cavity 20 is lower than in the other sections of the line 14 and preferably also less than the atmospheric pressure, so that the oil passes through the passage 19 water flowing through it is sucked in. If the device 1 is designed such that a negative pressure prevails in the interior 7 relative to the surroundings, the oil can also be sucked in by this negative pressure and conveyed into the interior 7.
  • the mix present in the container 2 is still - through successive time intervals or continuously - passed through the line 14 in order to convey this via the feed line 21 to at least one component consisting of solid particles, for example a powdery one , Active pharmaceutical ingredient and / or a powdery dye, these being sucked in at least in part by the negative pressure prevailing in the cavity 20.
  • solid particles for example a powdery one , Active pharmaceutical ingredient and / or a powdery dye, these being sucked in at least in part by the negative pressure prevailing in the cavity 20.
  • solids are taken up essentially in particles. This means that the powder column, which is conveyed through the line 21 and ends at one end in the cavity 20, is removed in particles by the liquid passed through the cavity 20.
  • This type of solids absorption has the advantage over the already known methods that the powder distributes itself relatively quickly and evenly in the material and that no agglomerates of solid particles can form during or after the powder has been introduced, since these particles are introduced during the process through the cavity 20 flowing liquid optimally wetted and distributed in this.
  • the liquid flow passed through the cavity 20 takes the form of an oval cross section at.
  • the powdery component is taken up via one of the two flatter interface regions of the jet, so that the distribution of the solid particles in the liquid flowing through the cavity 20 and also the wettability of the solid particles are additionally improved.
  • the emulsion produced can finally be removed from the device 1 by opening the outlet valve 16.
  • the mixed material passed through the line 14 is circulated vertically, homogenized through the turbulence tube 25 and evenly distributed in the interior 7.
  • the conveying path of the mixed material conveyed from the turbulence tube 25 into the interior 7 is indicated by the arrows 30 shown in FIGS. 1 and 4. Since the flow cross-section at the lower end of the turbulence tube 25 is reduced, the mixture passed through it is accelerated before it leaves the turbulence tube 25 and is pressed out of the turbulence tube 25 through the gap.
  • the mixture flowing out forms an annular jet which is deflected on the plate 29, whereupon the mixture is distributed uniformly in the interior 7.
  • the strength of the homogenization depends on the gap width s, the mixture being homogenized correspondingly more strongly by reducing the gap width s.
  • the device 1 now has the further advantage over the known devices that the mix is gently homogenized - that is, without a homogenizer, which has a movable tool for generating the shear effect - so that the molecular structures of those present in the mix Components are not destroyed. Furthermore, by regulating the gap width s, the strength of the homogenization can also be set depending on the product to be manufactured and on the physical and chemical properties of the starting materials used.
  • the end product When emulsifying, the end product may also form before the mix has cooled completely. In this case, in order to prevent the emulsion particles from further shrinking, the gap width s can be increased during the subsequent cooling process, so that the mixture is practically no longer homogenized, but is only circulated vertically.
  • the emulsion or suspension particles agglomerate during the production of emulsions and suspensions, that is to say they adhere to one another, as a result of which the quality of the product to be produced is deteriorated.
  • the gap width s can be reduced, so that an emulsion or a suspension with an optimal average particle size can thereby be produced.
  • the end face of the displacement element 27 facing the gap can be provided with holes and / or grooves (not shown in FIG. 4) and / or with cross teeth. Through such an end face, the mixing can be promoted by adjusting the gap width s and the homogenization of a mixed material passed through the turbulence tube 25 can be increased.
  • the baffle plate 29 serving for the uniform distribution of the mixed material flowing out of the turbulence tube 25 has different shapes can have.
  • it can also be curved, so that the material deflected by it is optimally distributed in the interior 7.
  • liquid additives such as preservatives, thickeners, perfumes and the like, can be sucked in during the mixing process via the feed lines 23 and 24 of the solids introduction device 17, so that no conveying devices serving to admix these substances are required.
  • the device 1 can of course also have an electronic control device in order to automatically carry out the control and / or regulating operations which are different for the mixing process.
  • the wall 4 of the container 2 can have thermal insulation and / or a pipe coil instead of the intermediate space 5, so that the cooling or heating fluid can be passed through the pipe coil.
  • an electrical heating device could also be provided, possibly with a cooling device can be combined so that the container can be cooled or heated.
  • the device can also have a cleaning device for cleaning the container in order to clean the inner wall of the container, the at least one stirrer and also the turbulence tube.

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

Claims (10)

  1. Dispositif servant à mélanger un composant solide pulvérulent à un matériau liquide comportant un récipient (2) présentant un espace intérieur (7) et au moins un agitateur (10, 11) monté à rotation dans ce dernier ainsi qu'une entrée (6a) débouchant dans l'espace intérieur (7), une sortie (8) conduisant à l'extérieur de l'espace intérieur (7), une conduite (14) reliant l'entrée (6a) à la sortie (8), comportant un dispositif transporteur (15) et à travers laquelle le matériau liquide et la matière de mélange constituée en partie de celui-ci sont entraînées pendant le processus de mélange, et un dispositif (17) de chargement de produit solide logé dans la conduite (14), caractérisé en ce que le dispositif (17) de chargement de produit solide comporte un passage (19) présentant un rétrécissement de section, à axe horizontal et dans lequel débouche une conduite d'amenée (21) servant à ajouter un composant solide pulvérulent à la matière entraînée à travers le passage (19).
  2. Dispositif selon la revendication 1, caractérisé en ce qu'au moins la partie du passage (19) dans laquelle débouche la conduite d'amenée (21) présente une section ovale de telle manière que la matière entraînée à travers cette partie du passage (19) prenne la forme d'une veine ayant une section ovale et en ce que la conduite d'amenée (21) est disposée de telle manière que le composant pulvérulent de la matière est absorbé par l'une des deux régions de surface de séparation plates de la veine de matière à section ovale qui est entraînée à travers ladite partie du passage (19).
  3. Dispositif selon l'une des revendications 1 ou 2, caractérisé en ce que le dispositif (17) de chargement de produit solide est disposé en aval du dispositif transporteur (15) par rapport à la direction de circulation.
  4. Dispositif selon l'une quelconque des revendications 1 à 3, caractérisé en ce que la conduite d'amenée (21) comporte un organe de dosage (22).
  5. Dispositif selon l'une quelconque des revendications 1 à 4, caractérisé en ce que le passage (19) à axe horizontal est interrompu par un espace creux (20) dans lequel débouche la conduite d'amenée (21).
  6. Dispositif selon la revendication 5, caractérisé en ce que le dispositif (17) de chargement de produit solide comporte au moins une conduite d'amenée (23, 24) débouchant dans l'espace creux (20) destinée à ajouter des produits supplémentaires liquides à la matière entraînée à travers le passage (19).
  7. Dispositif selon l'une quelconque des revendications 1 à 6, caractérisé en ce que, dans l'espace intérieur (7) du récipient (2) est prévu un tube à turbulence (25) disposé verticalement et relié, par l'intermédiaire de l'entrée (6a), à la conduite (14) comportant le dispositif (17) de chargement de produit solide afin de répartir de manière régulière la matière entraînée à travers la conduite (14) dans l'espace intérieur (7).
  8. Dispositif selon la revendication 7, caractérisé en ce que le tube à turbulence (25) comporte un boîtier (26) présentant un fond (26a) allongé en forme de douille dans lequel est disposé un élément déplaceur (27) déplaçable axialement et en ce que le fond (26a) comporte un trou (26b) et forme, à l'extrémité inférieure du boîtier (26), en association avec l'élément déplaceur (27), une fente de largeur variable.
  9. Dispositif selon l'une des revendications 7 ou 8, caractérisé en ce que le tube à turbulence (25) présente, à son extrémité inférieure, une plaque de déviation (29) fixée sur le fond (26a) du boîtier (26) afin de dévier la matière sortant du boîtier (26) et, de ce fait, de la répartir de manière régulière dans l'espace intérieur (7) du récipient (2).
  10. Procédé pour mélanger un composant solide pulvérulent à un matériau liquide dans un dispositif selon l'une quelconque des revendications 1 à 9, caractérisé en ce qu'au moins une partie du matériau liquide est entraînée à des intervalles de temps successifs ou en permanence à travers la conduite (14) et en ce que les composants pulvérulents sont ajoutés à la matière entraînée à travers la conduite (14).
EP93810315A 1992-04-30 1993-04-29 Dispositif et procédé pour mélanger un composant pulvérulent solide dans un matériau liquide Expired - Lifetime EP0570335B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CH139792 1992-04-30
CH1397/92 1992-04-30

Publications (2)

Publication Number Publication Date
EP0570335A1 EP0570335A1 (fr) 1993-11-18
EP0570335B1 true EP0570335B1 (fr) 1995-08-23

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EP (1) EP0570335B1 (fr)
DE (1) DE59300496D1 (fr)

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US6200937B1 (en) 1998-06-09 2001-03-13 Neutrogena Corporation Anti-residue shampoo and liquid toiletry production method
DE102007060455A1 (de) * 2007-12-12 2009-06-18 Deutsche Amphibolin-Werke Von Robert Murjahn Stiftung & Co. Kg Vorrichtung zum Durchmischen von Baumaterial

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IT1396114B1 (it) * 2009-09-23 2012-11-16 Samia S P A Impianto per la produzione di composizioni, quali stucchi, leganti e simili, particolarmente adatti all'impiego nell'industria conciaria e procedimento per la produzione di tali composizioni mediante un tale impianto.
IT1399085B1 (it) * 2010-03-25 2013-04-05 G S G Srl Macchina per il tattamento di miscele alimentari a rendimento migliorato.
FI122642B (fi) * 2010-09-16 2012-04-30 Outotec Oyj Laite ja menetelmä kahden liuoksen dispergoimiseksi toisiinsa neste-nesteuutossa
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DE3844174A1 (de) * 1988-12-29 1990-07-05 Fresenius Ag Anlage zur herstellung von konzentraten durch mischung von fluessigkeit mit loeslichem feststoff
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6200937B1 (en) 1998-06-09 2001-03-13 Neutrogena Corporation Anti-residue shampoo and liquid toiletry production method
DE102007060455A1 (de) * 2007-12-12 2009-06-18 Deutsche Amphibolin-Werke Von Robert Murjahn Stiftung & Co. Kg Vorrichtung zum Durchmischen von Baumaterial

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EP0570335A1 (fr) 1993-11-18
DE59300496D1 (de) 1995-09-28

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