EP1497020B1 - Method and device for homogenizing emulsions - Google Patents

Method and device for homogenizing emulsions Download PDF

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Publication number
EP1497020B1
EP1497020B1 EP03727282A EP03727282A EP1497020B1 EP 1497020 B1 EP1497020 B1 EP 1497020B1 EP 03727282 A EP03727282 A EP 03727282A EP 03727282 A EP03727282 A EP 03727282A EP 1497020 B1 EP1497020 B1 EP 1497020B1
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Prior art keywords
emulsion
shearing forces
sharp
less
milk
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German (de)
French (fr)
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EP1497020A1 (en
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Wolfgang Ehrfeld
Andreas Fredenhagen
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Ehrfeld Mikrotechnik BTS GmbH
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Ehrfeld Mikrotechnik BTS GmbH
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40Mixing liquids with liquids; Emulsifying
    • B01F23/41Emulsifying
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/40Static mixers
    • B01F25/45Mixers in which the materials to be mixed are pressed together through orifices or interstitial spaces, e.g. between beads
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00Other mixers; Mixing plants; Combinations of mixers
    • B01F33/30Micromixers

Definitions

  • the invention relates to a method for homogenizing emulsions, in particular milk, with which it is possible to crush the fat droplets by a homogenizer equipped with special microstructures at a substantially lower operating pressure than has hitherto been possible.
  • Homogenizing is an essential process step for milk processing. In order to obtain a supernatant or weeks stable emulsion, the fat droplets contained in the milk must be small and evenly distributed. In addition, a more full-bodied taste is achieved by this fine distribution.
  • the homogenization of milk today is done exclusively with high-pressure homogenizers. In this process, the milk is conveyed through a narrow gap with very high pressure in a process that has been tried and tested over the past 100 years, thereby reducing the fat globules to sizes in the range of 0.3 to 0.4 ⁇ m.
  • the energy required to break up the fat droplets is three orders of magnitude higher than the theoretically necessary energy required to increase the surface area of the fat phase. Assuming a uniform energy input over the volume, the actual energy input is still two orders of magnitude above the theoretical minimum. Despite continuous improvement of the process, most of the energy stored in the milk only causes warming.
  • microtechnology has been used successfully in many areas of industry. Due to the small structural dimensions, high heat transfer rates, fast mixing processes and very precise flow guidance are achieved. In the food industry, the particular advantages of microtechnology for process improvements, in particular for the improvement of fluid processes, have hitherto hardly been used.
  • Microstructures for the treatment of liquid samples are in US-B-6,368,871 described. These structures make it possible to combine the most diverse material flows and the treatment of sensitive macromolecules (DNA, proteins, ).
  • the staggered flow obstacles formed as microstructures preferably have the shape of rhombuses, triangles, sickles or other sharp-edged structures.
  • the production can be carried out with standard production methods of microtechnology such. B. LIGA technique, deep etching, spark erosion, laser ablation or mechanical micro-machining done.
  • the structures can be positively, materially or non-positively connected, for example by diffusion soldering, diffusion welding, Etektronenstrahlsch routineen, gluing or pressing.
  • Another method to inexpensively produce structures with fine flow obstructions is to use thin metal wires with another metal layer, e.g. As a silver layer to coat galvanically, then pressed in parallel and to fix on a support plate, for example by welding. The outer metal layer is then removed again by an etching solution, so that the desired structure is formed.
  • the shear forces required to produce uniformly small droplets of fat in an emulsion can also be produced by differently designed microstructures. Particularly suitable for this purpose is a perforated plate proved, the holes have a diameter of less than 1 micron. This hole diameter is particularly suitable for the homogenization of milk, in which the fat droplets before the emulsion have a diameter of 3 to 25 microns and after passage through the homogenizer should have only a uniform droplet size of less than 1 micron. A comparable effect is also achieved by microchannels whose narrowest cross-section is smaller than 1 ⁇ m.
  • femtosecond lasers are of particular interest for producing the apertured plate which can be used in accordance with the invention for homogenizing emulsions, since in the processing of materials with high thermal conductivity and comparatively low melting temperature (for example metals) the melt adhesions which generally occur when conventional laser beam sources are used can not significantly reduce the achievable precision. Even transparent materials such as organic materials can be processed with very little damage with these femtosecond lasers.
  • Such a perforated plate is preferably made of metal or of glass.

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

Abstract

Method and device for homogenizing emulsions, especially milk, wherein an emulsion is subjected to a high shearing force in a homoginizer equipped with microstructures.

Description

Gegenstand der Erfindung ist ein Verfahren zum Homogenisieren von Emulsionen, insbesondere von Milch, mit dem es gelingt, die Fetttröpfchen durch einen mit speziellen Mikrostrukturen ausgerüsteten Homogenisator bei einem wesentlich geringeren Betriebsdruck zu zerkleinern, als es bisher möglich gewesen ist.The invention relates to a method for homogenizing emulsions, in particular milk, with which it is possible to crush the fat droplets by a homogenizer equipped with special microstructures at a substantially lower operating pressure than has hitherto been possible.

Homogenisieren ist für die Milchverarbeitung ein wesentlicher Prozessschritt. Um eine Ober Tage oder Wochen stabile Emulsion zu erhalten, müssen die in der Milch enthaltenen Fetttröpfchen klein und gleichmäßig verteilt sein. Zusätzlich wird durch diese Feinverteilung ein vollmundigerer Geschmack erreicht. Das Homogenisieren von Milch erfolgt heute ausschließlich mit Hochdruckhomogenisatoren. Dabei wird die Milch in einem seit Ober 100 Jahren bewährten Verfahren durch einen schmalen Spalt mit sehr hohem Druck gefördert und dadurch die Fettkügelchen auf Größen im Bereich von 0,3 bis 0,4 µm zerkleinert.Homogenizing is an essential process step for milk processing. In order to obtain a supernatant or weeks stable emulsion, the fat droplets contained in the milk must be small and evenly distributed. In addition, a more full-bodied taste is achieved by this fine distribution. The homogenization of milk today is done exclusively with high-pressure homogenizers. In this process, the milk is conveyed through a narrow gap with very high pressure in a process that has been tried and tested over the past 100 years, thereby reducing the fat globules to sizes in the range of 0.3 to 0.4 μm.

Der Energieaufwand, der zum Zerkleinern der Fetttröpfchen eingesetzt wird, ist um drei Größenordnungen höher als der theoretisch notwendige Energieaufwand zur Oberflächenvergrößerung der Fettphase. Geht man von einem einheitlichen Energieeintrag über das Volumen aus, so liegt der tatsächliche Energieeintrag immer noch um zwei Größenordnungen über dem theoretischen Minimum. Trotz ständiger Weiterverbesserung des Verfahrens bewirkt der überwiegende Teil der in die Milch eingetragenen Energie lediglich eine Erwärmung.The energy required to break up the fat droplets is three orders of magnitude higher than the theoretically necessary energy required to increase the surface area of the fat phase. Assuming a uniform energy input over the volume, the actual energy input is still two orders of magnitude above the theoretical minimum. Despite continuous improvement of the process, most of the energy stored in the milk only causes warming.

So ist in der deutschen Patentanmeldung 197 00 810 ein Verfahren zur Homogenisierung von Milch beschrieben, bei dem die Milch durch eine ein- oder mehrstufige Düsendispergiervorrichtung gefördert wird. Scherkräfte, die durch vielfache Strömungsumlenkungen in engen Mikrostrukturen oder durch Löcher mit einem Durchmesser von unter 1. µm hervorgerufen werden, finden dabei keine Anwendung. Vielmehr erfolgt dort die Homogenisierung bei Düsendurchmessem über 100 µm durch die Düsenströmung, nicht aber durch die Zerscherung der Tröpfchen.So is in the German patent application 197 00 810 a method for the homogenization of milk is described, in which the milk is conveyed through a single- or multi-stage Düsendispergiervorrichtung. Shearing forces, the caused by multiple flow deflections in tight microstructures or holes with a diameter of less than 1 micron, find no application. Rather, there is the homogenization at Düsendurchmessem about 100 microns by the nozzle flow, but not by the shearing of the droplets.

Ein Verfahren zur Verringerung der Tröpfengröße von Photoemulsionen ist in US-A-5811227 beschrieben, bei dem eine Rohemulsion durch einen Faserfilter gepresst wird.One method of reducing the droplet size of photoemulsions is in US Pat US-A-5811227 described in which a raw emulsion is pressed through a fiber filter.

Eine Verbesserung des Wirkungsgrades würde zu einem ganz entscheidenden technischen Fortschritt führen. Neben der Absenkung des spezifischen Energieaufwandes könnte insbesondere auch eine wesentliche Vereinfachung der technischen Ausführung der Homogenisierungsanlage erreicht werden, was zu beträchtlichen Einsparungen bei den Herstellung- und Wartungskosten führen würde.An improvement of the efficiency would lead to a very decisive technical progress. In addition to lowering the specific energy consumption, in particular a substantial simplification of the technical design of the homogenization plant could be achieved, which would lead to considerable savings in the production and maintenance costs.

Bisher wurde die Mikrotechnik bereits in vielen Bereichen der Industrie erfolgreich eingesetzt. Hierbei werden durch die kleinen Strukturabmessungen hohe Wärmeübertragungsraten, schnelle Mischungsvorgänge und sehr präzise Strömungsführungen erreicht. Im Bereich der Lebensmittelindustrie sind die besonderen Vorteile der Mikrotechnik zu Prozessverbesserungen, insbesondere zur Verbesserung von Fluidprozessen, bisher noch kaum genutzt worden.So far, microtechnology has been used successfully in many areas of industry. Due to the small structural dimensions, high heat transfer rates, fast mixing processes and very precise flow guidance are achieved. In the food industry, the particular advantages of microtechnology for process improvements, in particular for the improvement of fluid processes, have hitherto hardly been used.

Mikrostrukturen zur Behandlung von flüssigen Proben sind in US-B-6 368 871 beschrieben. Diese Strukturen ermöglichen die Vereinigung Verschiedenster Stoffströme und die Behandlung empfindlicher Makromoleküle (DNA, Proteine,...).Microstructures for the treatment of liquid samples are in US-B-6,368,871 described. These structures make it possible to combine the most diverse material flows and the treatment of sensitive macromolecules (DNA, proteins, ...).

Es stellte sich deshalb die Aufgabe, ein Verfahren und eine Vorrichtung zum Homogenisieren von Emulsionen, insbesondere zum Homogenisieren von Milch zu entwickeln, durch die die technischen Vorteile des Einsatzes von Mikrostrukturen genutzt und die Fetttröpfchen in Emulsionen, insbesondere in Milch, gleichmäßig zerkleinert werden können und hierfür ein erheblich geringerer Betriebsdruck als bisher, vorzugsweise ein Betriebsdruck unter 50 bar, erforderlich ist.It was therefore an object to develop a method and an apparatus for homogenizing emulsions, in particular for homogenizing milk, by which the technical advantages of the use of microstructures can be used and the fat droplets in emulsions, especially in milk, can be uniformly comminuted and For this purpose, a considerably lower operating pressure than before, preferably an operating pressure below 50 bar, is required.

Es wurde nun gefunden, dass diese Aufgabe durch ein Verfahren gemäß Anspruch 1 und eine Vorrichtung gemäß Anspruch 5.It has now been found that this object is achieved by a method according to claim 1 and a device according to claim 5.

Die als Mikrostrukturen ausgebildeten, gegeneinander versetzten Strömungshindernisse haben vorzugsweise die Form von Rhomben, Dreiecken, Sicheln oder anderen scharfkantigen Strukturen.The staggered flow obstacles formed as microstructures preferably have the shape of rhombuses, triangles, sickles or other sharp-edged structures.

Als Materialien können beispielsweise korrosionsbeständige Stähle, aber auch keramische Werkstoffe verwendet werden. Die Herstellung kann mit Standardfertigungsverfahren der Mikrotechnik wie z. B. LIGA-Technik, Tiefenätztechnik, Funkenerosion, Laserablation oder mechanischer Mikrobearbeitung erfolgen. Die Strukturen können form-, stoff- oder kraftschlüssig verbunden werden, beispielsweise durch Diffusionslöten, Diffusionsschweißen, Etektronenstrahlschweißen, Kleben oder Verpressen. Eine weitere Methode, um kostengünstig Strukturen mit feinen Strömungshindernissen zu erzeugen, besteht darin, dünne Metalldrähte mit einer weiteren Metallschicht, z. B. einer Silberschicht galvanisch zu überziehen, danach parallel zu verpressen und auf einer Trägerplatte beispielsweise durch Verschweißen zu fixieren. Die äußere Metallschicht wird dann durch eine Ätzlösung wieder entfernt, so dass die gewünschte Struktur entsteht.As materials, for example corrosion-resistant steels, but also ceramic materials can be used. The production can be carried out with standard production methods of microtechnology such. B. LIGA technique, deep etching, spark erosion, laser ablation or mechanical micro-machining done. The structures can be positively, materially or non-positively connected, for example by diffusion soldering, diffusion welding, Etektronenstrahlschweißen, gluing or pressing. Another method to inexpensively produce structures with fine flow obstructions is to use thin metal wires with another metal layer, e.g. As a silver layer to coat galvanically, then pressed in parallel and to fix on a support plate, for example by welding. The outer metal layer is then removed again by an etching solution, so that the desired structure is formed.

Die Reinigung der Bauteile hat, insbesondere in der Lebensmitteltechnik, eine wichtige Bedeutung. Für den erfindungsgemäßen Homogenisator können dazu chemische Reinigungsmittel eingesetzt werden. Eine weitere Möglichkeit bietet eine Bauausführung, die eine mechanische Reinigung vorsieht. Die mikrostrukturierte Platte wird dabei durch eine Platte mit Öffnungen in Form der Strömungshindernisse in den Strömungsraum gesteckt, so dass die Reinigung durch Absenken der Mikrostrukturen erfolgen kann.

Fig.1
zeigt eine Anordnung der erfindungsgemäß besonders bevorzugten rhombischen Mikrostrukturen, die zur Erhöhung der Scherkräfte gegeneinander versetzt sind.
Fig. 2
zeigt die für die Erzeugung optimaler Scherkräfte wichtigen geometrischen Abmessungen (a), (b), (α), die entsprechend den Eigenschaften der zu homogenisierenden Emulsion und der zu erzielenden Fetttröpfchengröße variiert werden können. Weitere Variationsmöglichkeiten ergeben sich durch die Höhe der Mikrostrukturen und durch die Anzahl der hintereinander angeordneten Reihen der Mikrostrukturen.
Fig.3
zeigt den Aufbau eines erfindungsgemäße Mikrostrukturen enthaltenden Homogenisators. Dabei sind in der Homogenisiereinheit eine oder mehrere mikrostrukturierte Platten übereinander geschichtet, in denen die rhombischen Aussparungen am Rand scharfkantige Erhebungen zeigen, die für die Ausbildung erheblicher Scherkräfte verantwortlich sind. Gleichzeitig wird dargestellt, wie die Emulsion den Plattenstapel anströmt und wie sie ihn nach erfolgter Homogenisierung wieder verlässt. Dabei wird die Rohemulsion, also z.B. die Milch, mittels einer Pumpe durch die Homogenisiereinheit gedrückt und kann anschließend weiter verarbeitet werden.
Fig. 4
zeigt eine scharfkantige Mikrostruktur, die aus einer Schicht von Metalldrähten hergestellt worden ist, die mit einem zweiten Metall überzogen und nach paralleler Verpressung auf eine oder zwischen mehreren Trägerplatten fixiert sind. Anschließend ist dann das zweite Metall herausgelöst worden. Für dieses Verfahren werden vorteilhafter Weise Metalldrähte mit einem Durchmesser von weniger als 3 µm eingesetzt. Besonders zu empfehlen ist es, die Metalldrähte beim Herstellungsverfahren mit Silber zu überziehen.
The cleaning of components has, especially in food technology, an important importance. For the homogenizer according to the invention, chemical cleaning agents can be used for this purpose. Another possibility is a construction that provides a mechanical cleaning. The microstructured plate is inserted through a plate with openings in the form of flow obstacles in the flow space, so that the cleaning can be done by lowering the microstructures.
Fig.1
shows an arrangement of the invention particularly preferred rhombic microstructures, which are offset from each other to increase the shear forces.
Fig. 2
shows the important for the generation of optimal shear geometric dimensions (a), (b), (α), which can be varied according to the properties of the emulsion to be homogenized and the fat droplet size to be achieved. Further variations result from the height of the microstructures and the number of successively arranged rows of microstructures.
Figure 3
shows the structure of a homogenizer according to the invention containing microstructures. In this case, one or more microstructured plates are stacked in the homogenizing unit, in which the rhombic recesses at the edge show sharp-edged elevations which are responsible for the formation of considerable shearing forces. At the same time it is shown how the emulsion flows against the plate stack and how it leaves it again after homogenization. Here, the raw emulsion, so for example the milk, pressed by a pump through the homogenizer and can then be further processed.
Fig. 4
shows a sharp-edged microstructure, which has been produced from a layer of metal wires, which are coated with a second metal and fixed after parallel pressing on one or more support plates. Then then the second metal has been dissolved out. Metal wires with a diameter of less than 3 μm are advantageously used for this method. It is especially recommended to coat the metal wires with silver during the manufacturing process.

Die zur Erzeugung gleichmäßig kleiner Fetttröpfchen in einer Emulsion erforderlichen Scherkräfte können auch durch anders gestaltete Mikrostrukturen erzeugt werden. Als besonders geeignet hat sich hierfür eine Lochplatte erwiesen, deren Löcher einen Durchmesser von weniger als 1 µm aufweisen. Dieser Lochdurchmesser ist besonders zur Homogenisierung von Milch geeignet, bei der die Fetttröpfchen vor der Emulsion einen Durchmesser von 3 bis 25 µm aufweisen und nach der Passage durch den Homogenisator nur noch eine einheitliche Tröpfchengröße von weniger als 1 µm aufweisen sollen. Ein vergleichbarer Effekt wird auch durch Mikrokanäle erreicht, deren engster Querschnitt kleiner als 1 µm ist.The shear forces required to produce uniformly small droplets of fat in an emulsion can also be produced by differently designed microstructures. Particularly suitable for this purpose is a perforated plate proved, the holes have a diameter of less than 1 micron. This hole diameter is particularly suitable for the homogenization of milk, in which the fat droplets before the emulsion have a diameter of 3 to 25 microns and after passage through the homogenizer should have only a uniform droplet size of less than 1 micron. A comparable effect is also achieved by microchannels whose narrowest cross-section is smaller than 1 μm.

Zur Herstellung der erfindungsgemäß zum Homogenisieren von Emulsionen einsetzbaren Lochplatte ist der Einsatz von Femtosekunden-Lasem besonders interessant, da bei der Bearbeitung von Materialien mit hoher Wärmeleitfähigkeit und vergleichsweise geringer Schmelztemperatur (zum Beispiel bei Metallen) die beim Einsatz herkömmlicher Laserstrahlquellen im allgemeinen auftretenden Schmelzanhaftungen, die die erreichbare Präzision erheblich reduzieren können, nicht auftreten. Auch transparente Materialien wie organische Materialien lassen sich mit diesen Femtosekunden-Lasern sehr schädigungsarm bearbeiten.The use of femtosecond lasers is of particular interest for producing the apertured plate which can be used in accordance with the invention for homogenizing emulsions, since in the processing of materials with high thermal conductivity and comparatively low melting temperature (for example metals) the melt adhesions which generally occur when conventional laser beam sources are used can not significantly reduce the achievable precision. Even transparent materials such as organic materials can be processed with very little damage with these femtosecond lasers.

Eine derartige Lochplatte wird vorzugsweise aus Metall oder aus Glas hergestellt.Such a perforated plate is preferably made of metal or of glass.

Mit dem erfindungsgemäßen Verfahren gelingt es bei einem im Vergleich zum heutigem Standard von ca. 200 bar deutlich reduzierten Betriebsdruck unter 50 bar eine gleichmäßig homogenisierte Emulsion, insbesondere Milch mit einer Teilchengröße unter 1 µm zu erzeugen, die sich durch eine besonders hohe Haltbarkeit auszeichnet.With the method according to the invention, it is possible to produce a uniformly homogenized emulsion, in particular milk with a particle size of less than 1 .mu.m, which is distinguished by a particularly high durability with a significantly reduced operating pressure of less than 50 bar compared to the current standard of about 200 bar.

Claims (6)

  1. Method for homogenizing emulsions, wherein the emulsion is subjected to high shearing forces in a flow field by means of a homogenizer equipped with microstructures, characterized in that said shearing forces are generated by mutually offset flow obstacles in the shape of diamonds, triangles, crescents or other sharp-edged structures or by an apertured plate whose holes have a diameter of less than 1 µm.
  2. Method according to Claim 1, characterized in that the holes in the apertured plate are generated by a femtosecond laser.
  3. Method according to Claims 1 and 2, characterized in that it is used for milk homogenization so that the fat globules in the emulsion are reduced to a size of under 1 µm.
  4. Method according to Claims 1 to 3, characterized in that the operating pressure is under 50 bar.
  5. Device for milk homogenization according to Claims 1 to 4, characterized in that it has one or more microstructured, sharp-edged plates which are stacked on top of one another and which, as flow obstacles, exert high shearing forces on the stream of liquid, wherein the shearing forces are generated by offset flow obstacles in the shape of diamonds, triangles, crescents or other sharp-edged structures or by apertured plates whose holes have a diameter of less than 1 µm.
  6. Device as according to Claim 5, characterized in that it has an apertured plate with micro channels whose narrowest cross section is less than 1 µm.
EP03727282A 2002-04-17 2003-04-09 Method and device for homogenizing emulsions Expired - Lifetime EP1497020B1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10216947 2002-04-17
DE10216947A DE10216947B4 (en) 2002-04-17 2002-04-17 Method for homogenizing emulsions
PCT/EP2003/003657 WO2003086601A1 (en) 2002-04-17 2003-04-09 Method and device for homogenizing emulsions

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EP1497020B1 true EP1497020B1 (en) 2007-08-15

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US (1) US20050233040A1 (en)
EP (1) EP1497020B1 (en)
AT (1) ATE369907T1 (en)
AU (1) AU2003233959A1 (en)
DE (2) DE10216947B4 (en)
WO (1) WO2003086601A1 (en)

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CN108212237B (en) * 2013-03-06 2020-12-08 哈佛学院院长及董事 Apparatus and method for forming relatively monodisperse droplets
EP2798988B1 (en) 2013-04-29 2016-05-18 Melitta Professional Coffee Solutions GmbH & Co., KG Device for producing a milk foam
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US20050233040A1 (en) 2005-10-20
EP1497020A1 (en) 2005-01-19
DE50307961D1 (en) 2007-09-27
WO2003086601A1 (en) 2003-10-23
ATE369907T1 (en) 2007-09-15
DE10216947B4 (en) 2007-10-04
DE10216947A1 (en) 2003-11-06
AU2003233959A1 (en) 2003-10-27

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