EP1781402A1 - Verfahren zur mechanisch schonenden erzeugung von fein dispersen mikro-/nano-emulsionen mit enger tropfengrössenverteilung und vorrichtung zum durchführen des verfahrens - Google Patents
Verfahren zur mechanisch schonenden erzeugung von fein dispersen mikro-/nano-emulsionen mit enger tropfengrössenverteilung und vorrichtung zum durchführen des verfahrensInfo
- Publication number
- EP1781402A1 EP1781402A1 EP05776538A EP05776538A EP1781402A1 EP 1781402 A1 EP1781402 A1 EP 1781402A1 EP 05776538 A EP05776538 A EP 05776538A EP 05776538 A EP05776538 A EP 05776538A EP 1781402 A1 EP1781402 A1 EP 1781402A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- membrane body
- filter fabric
- membrane
- fluid phase
- subsequent
- 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.)
- Granted
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
- B01F23/411—Emulsifying using electrical or magnetic fields, heat or vibrations
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/30—Injector mixers
- B01F25/31—Injector mixers in conduits or tubes through which the main component flows
- B01F25/313—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced in the centre of the conduit
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/30—Injector mixers
- B01F25/31—Injector mixers in conduits or tubes through which the main component flows
- B01F25/313—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced in the centre of the conduit
- B01F25/3133—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced in the centre of the conduit characterised by the specific design of the injector
- B01F25/31331—Perforated, multi-opening, with a plurality of holes
- B01F25/313311—Porous injectors
-
- 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
- B01F27/21—Mixers with rotary stirring devices in fixed receptacles; Kneaders characterised by their rotating shafts
- B01F27/2122—Hollow 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
- B01F27/27—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices
- B01F27/272—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices with means for moving the materials to be mixed axially between the surfaces of the rotor and the stator, e.g. the stator rotor system formed by conical or cylindrical surfaces
Definitions
- the invention relates to a method for mechanically gentle production of finely dispersed micro / nano-emulsions with a narrow droplet size distribution.
- the invention relates to a device for carrying out the Ver ⁇ procedure.
- the production of finely dispersed emulsions is regarded as an important development goal for the food, pharmaceutical, cosmetics and chemical industries.
- the reason for this is the possibility of keeping such emulsions entmischungsstabil with sufficient smallness of the disperse droplets and the extremely large inner Interface for the adsorption of functional ingredients (eg active ingredients, flavors, dyes etc.).
- the dispersed droplets allow the construction of particle networks, which have a specific influence on the rheological properties of such emulsions.
- Membrane emulsification processes are a new area for machine / apparatus manufacturers. Traditionally, rotor / stator dispersing systems and high-pressure homogenizers are used for fine emulsification. In these devices, droplet dispersion takes place under extremely high mechanical stress on the disperse as well as the continuous phase. The membrane emulsification processes which have existed for about five years are very gentle from the conventional methods mentioned above, since the finely dispersed emulsion droplets are not produced by breaking larger droplets, but in their final size at the outlet openings Membrane pores formed and detached.
- the object of the invention is to provide a method for the mechanically gentle production of finely dispersed micro / nano-emulsions with a narrow droplet size distribution.
- the invention has the object to provide a device for carrying out the method according to the invention.
- emulsion droplets are produced on the surface of a membrane or filter fabric which is permeated by pores, in that a first fluid phase is pressed through these pores and the removal of the droplets from the membrane surface by their rotational movement in a second with the first immiscible fluid phase.
- the detachment of the fluid droplets from the membrane surface is effected by tangential and normal stresses acting on them and caused by the flow, assisted by additional centrifugal forces.
- diameter x large pore spacing (> 2x) is for producing a narrow
- the membrane overflow according to the invention which is realized with additionally efficient expansion flow fractions, permits the production of significantly smaller droplet diameters for a comparable pore diameter.
- the emulsifier according to the invention offers drop formation at comparable diameters of the drops produced the advantage of significantly reduced mechanical stress. This has advantages with regard to the preservation of native properties of functional content components, for example of proteins in the droplets or at their interfaces.
- the device according to the invention allows the simple modification and adaptation of the expansion flow overflow characteristic of the membrane according to the invention with regard to the proportion of the expansion flow to the total flow by variation of the eccentricity of the rotating diaphragm cylinder and / or easily exchanged flow installations.
- the inventive device is very compact, since the membrane body can be arranged in the housing with a narrow gap distance to the inner wall.
- FIG. 1 shows a device according to the invention in axial longitudinal section, the cut walls, however, are not shown schraf ⁇ fiert for simplicity;
- FIG. 2 shows a cross-section orthogonal to the longitudinal axis of the device shown in FIG. 1;
- FIG. 3 likewise an orthogonal cross-section to the longitudinal axis of a device according to the invention, in a further embodiment with flow internals;
- Fig. 5 is a graphical representation of the droplet number distributions (Qo distribution) taken at 1000 to 8000 revolutions per minute of the filter or membrane body from water droplets in sunflower oil (so-called Q 0 (x) distributions) with entry of the characteristic droplet sizes xgo.o and Xio, o. their ratio (X9o, o / xio, o) is used as a suitable measure of the droplet size distribution width, namely centric arrangement (Z) and eccentric arrangement (EZ).
- the reference numeral 1 denotes a continuous fluid phase, which is supplied from a suitable reservoir (not shown) under pump power to a port 2 and via this a gap 3.
- 4 denotes disperse drops and 5 denotes a membrane or filter fabric body, while 6 represents a cylinder body designed as a membrane cylinder.
- a hollow shaft formed rotary shaft is designated, which has an inner, centrally arranged bore 8.
- the shaft 7 is sealed by a dynamic mechanical seal 9.
- the bore 8 opens into an interior 10 of the filter fabric or membrane body 5.
- a conical component is arranged, which opens into an outlet connection 12.
- the conical component 11 and the outlet connection 12 form part of a housing 18.
- a disperse fluid phase is fed from a container, also not shown, by means of a motor-driven pump (not shown).
- the emulsion 14 leaves the housing 18 via the outlet connection 12.
- the filter fabric or membrane body 5 is arranged eccentrically, with defined adjustable eccentricity, relative to the housing 18.
- a flow installation (eg web 15) is arranged in the gap 3, which extends in the direction of the longitudinal axis 16 of the housing 18.
- the web 15 may also be helical or part of a spiral. It is also possible to provide within the gap 3 a plurality of such webs 15, spirals or helically extending webs 3 of different cross-sectional geometry.
- the diametrically oppositely directed arrows 17 are intended to indicate the approximately radially directed direction of flow of the disperse fluid phase 13 with respect to the filter fabric or membrane body 5.
- the disperse fluid phase 13 is pressed into the interior 10 of the rotating membrane cylinder body 6 by means of the motor-driven pump (not shown) via the rotational shaft 7 provided with an inner bore 8 and thus designed as a hollow shaft.
- the shaft 7 is dynamically sealed against the housing 18 by means of the mechanical seal 9. From there, the disperse fluid phase 13 passes through the membrane 5 placed on the cylinder body surface and forms the disperse droplets 4 on the outside thereof.
- the continuous fluid phase 1 is passed through the port 2 in the cylindrical housing 18 and flows through the gap 3 between the rotating membrane or filter fabric body 5 and housing 18 in the axial direction.
- the dispersed droplets 4 formed on the membrane surface are flowed on.
- the intensity of the flow is determined by the peripheral speed of the membrane or filter fabric body or cylinder 6, the gap width 3 and the eccentricity or flow structures attached to the outer cylinder wall (eg web (s), pins, knife / scraper). between this and the housing 18 set. If there is an eccentric arrangement of the diaphragm cylinder 6 in the cylindrical housing 18 (FIG. 2) between the diaphragm cylinder 6 and the housing 18, a mixed shear / expansion flow is produced which has improved dispersing properties.
- the rotational flow is defined with disturbing flow installations (eg web 15), preferably on the inner wall of the housing, according to the invention.
- disturbing flow installations eg web 15
- Such flow internals can be both straight and axially aligned, as well as helical, fitted.
- the mixture of disperse drops 4 and continuous fluid phase 1, the emulsion 14, is formed at the exit from the gap 3 in an outlet geometry, which preferably consists of a conical component 11 and an outlet connection 12.
- CPDN membrane Controlled Pore Distance Membrane
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Colloid Chemistry (AREA)
- Manufacturing Of Micro-Capsules (AREA)
- Cosmetics (AREA)
- Mixers Of The Rotary Stirring Type (AREA)
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102004040735A DE102004040735B4 (de) | 2004-08-23 | 2004-08-23 | Verfahren zur mechanisch schonenden Erzeugung von fein dispersen Mikro-/Nano-Emulsionen mit enger Tropfengrößenverteilung und Vorrichtung zum Durchführen des Verfahrens |
PCT/EP2005/008980 WO2006021375A1 (de) | 2004-08-23 | 2005-08-19 | Verfahren zur mechanisch schonenden erzeugung von fein dispersen mikro-/nano-emulsionen mit enger tropfengrössenverteilung und vorrichtung zum durchführen des verfahrens |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1781402A1 true EP1781402A1 (de) | 2007-05-09 |
EP1781402B1 EP1781402B1 (de) | 2008-02-27 |
Family
ID=35414500
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP05776538A Not-in-force EP1781402B1 (de) | 2004-08-23 | 2005-08-19 | Vorrichtung zur mechanisch schonenden erzeugung von fein dispersen mikro-/nano-emulsionen mit enger tropfengrössenverteilung |
Country Status (6)
Country | Link |
---|---|
US (1) | US8267572B2 (de) |
EP (1) | EP1781402B1 (de) |
JP (1) | JP4852042B2 (de) |
AT (1) | ATE387255T1 (de) |
DE (2) | DE102004040735B4 (de) |
WO (1) | WO2006021375A1 (de) |
Families Citing this family (23)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CA2908275C (en) | 2005-10-04 | 2019-04-09 | Jimmyash Llc | Fried food products having reduced fat content |
AU2006299381B2 (en) | 2005-10-04 | 2013-03-21 | Jimmyash Llc | Methods of making snack food products and products made thereby |
US9615601B2 (en) | 2005-10-04 | 2017-04-11 | Jimmyash Llc | Process for the controlled introduction of oil into food products |
GB0611888D0 (en) * | 2006-06-15 | 2006-07-26 | Micropore Technologies Ltd | An apparatus and method for membrane emulsification |
GB2444035A (en) * | 2006-11-25 | 2008-05-28 | Micropore Technologies Ltd | An apparatus and method for generating emulsions |
US8564783B2 (en) | 2008-05-15 | 2013-10-22 | Axsun Technologies, Inc. | Optical coherence tomography laser with integrated clock |
EP2260917A1 (de) * | 2009-05-29 | 2010-12-15 | Novoflow GmbH | Filtriersystem und Verfahren zur Optimierung der Filtrierleistung |
ES2473490T3 (es) | 2009-08-28 | 2014-07-07 | Kraft Foods R & D, Inc. | Método y aparato para preparar productos alimenticios aireados |
EP2374535A1 (de) * | 2010-04-06 | 2011-10-12 | Bühler AG | Verfahren und Vorrichtungen zur Vesikelbildung, insbesondere unter Verwendung von Block-Coplymeren |
DE102010017523A1 (de) * | 2010-06-22 | 2011-12-22 | Technische Universität Berlin | Verfahren und Mischvorrichtung zum Mischen von zwei Fluiden sowie deren Verwendung |
EP2402075A1 (de) * | 2010-06-28 | 2012-01-04 | Bühler AG | Verfahren und Vorrichtung zur Herstellung von Vesikeln |
EP2486975B1 (de) * | 2010-12-29 | 2015-09-23 | Wanhua Chemical Group Co., Ltd. | Hochgeschwindigkeitsmischreaktor und anwendung davon |
CA2823978C (en) | 2011-01-07 | 2018-05-01 | Junji Fukuda | Method of producing uniform polymer beads of various sizes |
JP5709130B2 (ja) * | 2011-03-31 | 2015-04-30 | 国立大学法人九州大学 | ミキシング効率に優れる、結晶微粒子の製造方法およびその装置 |
GB2494926B (en) * | 2011-09-26 | 2018-07-11 | Micropore Tech Ltd | Apparatus for particle production |
CN104884217A (zh) * | 2012-12-17 | 2015-09-02 | 罗门哈斯公司 | 单体液滴的生产 |
US9622948B2 (en) | 2012-12-20 | 2017-04-18 | Kao Germany Gmbh | Process for manufacturing an emulsion |
RU2015141069A (ru) | 2013-02-27 | 2017-04-05 | Ром Энд Хаас Компани | Эмульгирование с очисткой мембраны |
US10232333B2 (en) * | 2016-07-12 | 2019-03-19 | Micropore Technologies Ltd. | Azimuthally oscillating membrane emulsification for controlled droplet production |
WO2020186186A1 (en) | 2019-03-14 | 2020-09-17 | Moleaer, Inc. | A submersible nano-bubble generating device and method |
SG10201905946YA (en) * | 2019-06-26 | 2021-01-28 | Nat Univ Singapore | Systems and Methods for Fabricating Nanoparticles |
EP4126319A1 (de) | 2020-04-01 | 2023-02-08 | Merck Patent GmbH | Emulgiervorrichtung |
CN113617277B (zh) * | 2021-08-16 | 2023-05-23 | 广东涂百年新型材料有限公司 | 一种反射隔热弹性涂料生产用搅拌设备及其方法 |
Family Cites Families (17)
Publication number | Priority date | Publication date | Assignee | Title |
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JPS5372015A (en) * | 1976-12-08 | 1978-06-27 | Toyo Tire & Rubber Co Ltd | Pre-mixer for emulsion fuel prepataiton |
EP0209543A4 (de) | 1984-12-31 | 1989-07-11 | Internat Genetic Engineering I | Peptidfragmente menschlicher apolipoproteine, typspezifische antikörper und verwendungsverfahren. |
FR2589274B1 (fr) | 1985-10-28 | 1987-12-11 | Telephonie Ind Commerciale | Tete d'impression electrostatique |
JPH082416B2 (ja) * | 1988-09-29 | 1996-01-17 | 宮崎県 | エマルションの製造方法 |
JP2847107B2 (ja) * | 1989-02-16 | 1999-01-13 | 富士シリシア化学株式会社 | エマルジョンの調製方法 |
WO1993000156A1 (en) * | 1991-06-29 | 1993-01-07 | Miyazaki-Ken | Monodisperse single and double emulsions and production thereof |
JP3081880B2 (ja) * | 1998-03-30 | 2000-08-28 | 農林水産省食品総合研究所長 | マイクロスフィアの連続製造装置 |
GB9930322D0 (en) * | 1999-12-22 | 2000-02-09 | Univ Leeds | Rotating membrane |
JP3511238B2 (ja) * | 2000-10-13 | 2004-03-29 | 独立行政法人食品総合研究所 | マイクロスフィアの製造方法および製造装置 |
DE10127075C2 (de) * | 2001-06-02 | 2003-04-10 | Fraunhofer Ges Forschung | Vorrichtung und Verfahren zur Herstellung von Emulsionen mittels Membrankörpern |
WO2003014196A1 (en) | 2001-08-03 | 2003-02-20 | Akzo Nobel N.V. | Process to make dispersions |
US20060128815A1 (en) * | 2002-10-02 | 2006-06-15 | Clare Hugh J | Method for controlling droplet size of an emulsion when mixing two immiscible fluids |
JP4008796B2 (ja) * | 2002-11-06 | 2007-11-14 | 花王株式会社 | 酸性水中油型乳化物の製造法 |
DE10307568B4 (de) | 2003-02-22 | 2007-08-16 | ETH-Zürich, Institut für Lebensmittelwissenschaft, Laboratorium für Lebensmittelverfahrenstechnik | Verfahren zum Herstellen einer Membran mit Membranlöchern und nach diesem Verfahren hergestellte Mikro-/Nanomembran |
US7307104B2 (en) * | 2003-05-16 | 2007-12-11 | Velocys, Inc. | Process for forming an emulsion using microchannel process technology |
US7485671B2 (en) * | 2003-05-16 | 2009-02-03 | Velocys, Inc. | Process for forming an emulsion using microchannel process technology |
US7396550B2 (en) * | 2003-06-05 | 2008-07-08 | Angel Michael G | Time released nutritional product and method of manufacture |
-
2004
- 2004-08-23 DE DE102004040735A patent/DE102004040735B4/de not_active Expired - Fee Related
-
2005
- 2005-08-19 JP JP2007528699A patent/JP4852042B2/ja not_active Expired - Fee Related
- 2005-08-19 AT AT05776538T patent/ATE387255T1/de not_active IP Right Cessation
- 2005-08-19 WO PCT/EP2005/008980 patent/WO2006021375A1/de active IP Right Grant
- 2005-08-19 DE DE502005003021T patent/DE502005003021D1/de not_active Withdrawn - After Issue
- 2005-08-19 US US11/574,152 patent/US8267572B2/en not_active Expired - Fee Related
- 2005-08-19 EP EP05776538A patent/EP1781402B1/de not_active Not-in-force
Non-Patent Citations (1)
Title |
---|
See references of WO2006021375A1 * |
Also Published As
Publication number | Publication date |
---|---|
US8267572B2 (en) | 2012-09-18 |
JP4852042B2 (ja) | 2012-01-11 |
JP2008510607A (ja) | 2008-04-10 |
US20110038901A1 (en) | 2011-02-17 |
EP1781402B1 (de) | 2008-02-27 |
DE102004040735B4 (de) | 2006-11-23 |
WO2006021375A1 (de) | 2006-03-02 |
ATE387255T1 (de) | 2008-03-15 |
DE102004040735A1 (de) | 2006-03-09 |
DE502005003021D1 (de) | 2008-04-10 |
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Inventor name: GROHMANN, FRED-RAINER Inventor name: WINDHAB, ERICH, J. Inventor name: EISNER, DR. VERENA Inventor name: TROXLER, BEAT Inventor name: DUERIG, ANDREAS, KURT |
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