WO2018206190A1 - Procédé et dispositif pour obtenir des microparticules monodispersées - Google Patents

Procédé et dispositif pour obtenir des microparticules monodispersées Download PDF

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Publication number
WO2018206190A1
WO2018206190A1 PCT/EP2018/057145 EP2018057145W WO2018206190A1 WO 2018206190 A1 WO2018206190 A1 WO 2018206190A1 EP 2018057145 W EP2018057145 W EP 2018057145W WO 2018206190 A1 WO2018206190 A1 WO 2018206190A1
Authority
WO
WIPO (PCT)
Prior art keywords
suspension
solution
emulsion
nozzle body
nozzle
Prior art date
Application number
PCT/EP2018/057145
Other languages
German (de)
English (en)
Inventor
Bernd Stuke
Malte Bickelhaupt
Robert Giezendanner-Thoben
Haresh Anant Vaidya
Original Assignee
Robert Bosch Gmbh
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 Robert Bosch Gmbh filed Critical Robert Bosch Gmbh
Publication of WO2018206190A1 publication Critical patent/WO2018206190A1/fr

Links

Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B3/00—Drying solid materials or objects by processes involving the application of heat
    • F26B3/02—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air
    • F26B3/10—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air the gas or vapour carrying the materials or objects to be dried with it
    • F26B3/12—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air the gas or vapour carrying the materials or objects to be dried with it in the form of a spray, i.e. sprayed or dispersed emulsions or suspensions
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
    • F26B21/004—Nozzle assemblies; Air knives; Air distributors; Blow boxes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B1/00—Nozzles, spray heads or other outlets, with or without auxiliary devices such as valves, heating means
    • B05B1/30—Nozzles, spray heads or other outlets, with or without auxiliary devices such as valves, heating means designed to control volume of flow, e.g. with adjustable passages
    • B05B1/3033—Nozzles, spray heads or other outlets, with or without auxiliary devices such as valves, heating means designed to control volume of flow, e.g. with adjustable passages the control being effected by relative coaxial longitudinal movement of the controlling element and the spray head
    • B05B1/304—Nozzles, spray heads or other outlets, with or without auxiliary devices such as valves, heating means designed to control volume of flow, e.g. with adjustable passages the control being effected by relative coaxial longitudinal movement of the controlling element and the spray head the controlling element being a lift valve
    • B05B1/3046—Nozzles, spray heads or other outlets, with or without auxiliary devices such as valves, heating means designed to control volume of flow, e.g. with adjustable passages the control being effected by relative coaxial longitudinal movement of the controlling element and the spray head the controlling element being a lift valve the valve element, e.g. a needle, co-operating with a valve seat located downstream of the valve element and its actuating means, generally in the proximity of the outlet orifice

Definitions

  • the invention relates to a method for producing monodisperse microparticles having the features of the preamble of claim 1.
  • a solution in particular an aqueous polymer solution, a suspension or an emulsion is sprayed using a pressure atomizer and then dried.
  • the invention further relates to a device for producing monodisperse microparticles, wherein the device is suitable for carrying out the method according to the invention.
  • Monodisperse particles or monodisperse powders are used, for example, in the pharmaceutical, food and cosmetics industry and in a large number of different applications in research and development.
  • the preparation of such particles is often carried out by spray drying.
  • spray drying a solution, suspension or emulsion is atomized into fine droplets and then dried.
  • a simple spray dryer is exemplified in the published patent application DT 24 07 616 AI. It comprises a cylindrical drying space with at least one spray nozzle.
  • the spray nozzle has a first tube, via which a solution or suspension can be introduced into the drying space.
  • the first tube is surrounded by a second tube, by means of which hot air can be introduced into the drying space.
  • the introduced via the spray nozzle hot air flow has a high speed, so that the introduced via the first tube liquid is atomized by the hot air flow and intimately mixed with the hot air.
  • additionally tangentially oriented air streams are introduced through a pipe system surrounding the drying cylinder in the drying space, which flow inside helically along the cylinder wall.
  • the dried in the drying room Good is then fed to a cyclone, in which the particles are separated from the excess air.
  • the solution, suspension or emulsion must be very finely atomized. Because the size of the particles depends on the size of the drops generated during sputtering.
  • Microparticles in the form of very fine powders are used, for example, in additive manufacturing processes, in particular in 3D printing processes, for example selective laser melting, selective laser sintering or electron beam melting.
  • the pharmaceutical or cosmetics industry uses microparticles as a carrier of active ingredients.
  • the microparticles may include the active ingredients, so that a delayed release of the active ingredient takes place.
  • the present invention has for its object to simplify the production of very fine particles by spray drying. Furthermore, preferred applications for particles produced in this way are to be specified.
  • a solution in particular an aqueous polymer solution
  • a suspension or an emulsion is sprayed using a spray nozzle and then dried.
  • the solution, suspension or emulsion by means of the spray nozzle, the one received in a high-pressure bore of a nozzle body liftable Having nozzle needle for releasing and closing at least one injection opening formed in the nozzle body, injected under high pressure into a drying space.
  • media can be atomized, which have a relatively high viscosity.
  • These may be, in particular, complex liquids, such as, for example, aqueous polymer solutions.
  • a pressure which is above 200 bar, preferably above 300 bar and may be up to 2000 bar or more, for example 2500 bar.
  • Such high pressures allow the generation of droplets having an average droplet size of, for example, 2 ⁇ m to 100 ⁇ m, the droplet size corresponding substantially to the size of the particles to be produced.
  • the mean droplet size is preferably less than 40 ⁇ m, more preferably less than 20 ⁇ m. To achieve this, the pressure should preferably be well above 1000 bar.
  • Injection valves which have a nozzle needle liftably received in a high-pressure bore of a nozzle body for releasing and closing at least one injection opening formed in the nozzle body.
  • an injection valve for fuel in particular for diesel fuel, be used as a spray nozzle.
  • the size and / or distribution of the microparticles be adjusted via the size and / or the shape of the at least one injection opening. Because size and / or shape of the injection port determine the droplet size, so that on this the particle size is adjustable. Accordingly, spray nozzles can be provided with different nozzle geometries, so that particles of different sizes can be produced by replacing the spray nozzle. Alternatively or additionally, the size and / or distribution of the microparticles can be adjusted by changing the injection pressure. In this way, different sized particles can be produced using a single spray nozzle. This is particularly advantageous if the spray nozzle and thus the nozzle geometry are predetermined. Further alternatively or additionally, the size and / or distribution of the microparticles can be adjusted by changing the injection quantity and / or the injection pattern.
  • the droplets produced are held in suspension until dried. This means that the droplets do not come into contact with a wall of the drying space before they are dried. This prevents the droplets from precipitating on the wall of the drying room.
  • the solution, suspension or emulsion can be introduced directly or indirectly via a mixing chamber in the drying room. Since the introduction takes place under high pressure, the use of hot air or compressed air to atomize the liquid is unnecessary. The solution, suspension or emulsion can thus be injected directly into the drying room. If the introduction of the solution, suspension or emulsion in the drying space indirectly via a mixing chamber, another medium may be added, before the solution, suspension or emulsion enters the drying room. The high pulse of the high-pressure injection into the mixing chamber leads to an optimum mixing of the media, even if they are considered to be difficult to mix.
  • the mixing chamber is preferably formed in an adapter connected to the nozzle body of the spray nozzle. This ensures that the desired mixing is achieved before the solution, suspension or emulsion enters the drying room. In order to easily clean the adapter, it is proposed that this is detachably connected to the nozzle body of the spray nozzle.
  • the detachable connection also has the advantage that the adapter can be replaced depending on the particular medium to be added.
  • the solution, suspension or emulsion in the mixing chamber is preferably mixed with a liquid and / or a pulverulent solid, in particular an additive, a filler and / or a dye.
  • the pulverulent solid may be, for example, an active ingredient, so that microparticles can be produced which enclose this active ingredient.
  • the microparticles thus form spherical carriers for the active ingredient.
  • the pulverulent solid may also be a color pigment and / or a ferromagnetic material which has the function of a tracer.
  • the pulverulent solid is supplied as nanoparticles, so that the carrier material is able to envelop the solid.
  • the monodisperse microparticles are further processed immediately after their preparation in an additive manufacturing process.
  • the microparticles used in the additive manufacturing can be produced directly on site and in the required amount. This eliminates transport and storage costs.
  • the additive manufacturing process may be, in particular, an SD printing process according to the aforementioned methods (selective laser melting, selective laser sintering, electron beam melting). Before the dried microparticles are further processed in an additive manufacturing process, particles of a certain size can be selected, so that only these are further processed.
  • an apparatus for producing monodisperse microparticles which comprises a spray nozzle for atomizing a solution, suspension or emulsion and a drying space for drying the atomized solution, suspension or emulsion.
  • the spray nozzle has a nozzle needle liftably received in a high-pressure bore of a nozzle body for controlling at least one injection opening formed in the nozzle body, by means of which the solution, suspension or emulsion can be injected under high pressure into the drying space.
  • the injection under high pressure leads to a very fine atomization of the solution, suspension or emulsion, so that the smallest droplets are formed, which in turn allow the production of very small particles or very fine powder.
  • Under high pressure is understood in the present case a pressure which is above 200 bar, preferably above 300 bar and may be up to 2000 bar or more, for example 2500 bar.
  • Injection valves which have a nozzle needle liftably received in a high-pressure bore of a nozzle body for releasing and closing at least one injection opening formed in the nozzle body.
  • the spray nozzle is designed as an injection valve analogous to an injection valve for the injection of fuel, in particular diesel fuel.
  • the injection opening is arranged in the region of a nozzle tip of the nozzle body and / or coaxially to a longitudinal axis A of the nozzle body.
  • the spray jet can be optimally introduced into the drying space, wherein the shape and / or size of the injection opening determines the size of the droplets produced in this case.
  • the injection opening or - in the case of a multi-hole nozzle - the at least one further injection opening can be arranged laterally in the nozzle tip.
  • the lateral arrangement allows a variation of the spray pattern, wherein preferably a plurality of injection openings are optionally formed in different sizes and / or shapes in the nozzle tip.
  • the injection opening formed in the nozzle body opens into a mixing chamber which is formed in an adapter connected to the nozzle body and is connected to the drying space via at least one further injection opening formed in the adapter.
  • a further medium can be added, which may be in particular a liquid and / or a powdery solid.
  • the adapter is releasably connected to the nozzle body to facilitate the cleaning of the adapter and / or to allow the replacement of the adapter.
  • the apparatus for producing monodisperse microparticles is followed by an apparatus for additive production.
  • the microparticles used in additive manufacturing can be produced in this way on site and in the respectively required quantity. This eliminates transport and storage costs.
  • the device for additive manufacturing can be, in particular, a 3D printer, since fine plastic powders are often used in 3D printing. These can then be produced directly on site by means of the device according to the invention.
  • FIG. 1 shows a schematic longitudinal section through a spray nozzle for a device according to the invention or for carrying out the method according to the invention
  • FIG. 2 shows a schematic longitudinal section through a modified spray nozzle for a device according to the invention or for carrying out the method according to the invention
  • Fig. 3 is a schematic longitudinal sectional view through a spray nozzle with
  • the device 10 shown in FIG. 1 for the production of monodisperse microparticles 1 comprises a spray nozzle 2 and a drying space 7.
  • a solution, suspension or emulsion can be injected under high pressure into the drying space 7.
  • the spray nozzle 2 comprises a nozzle needle 5, which is received in a liftable manner for releasing and closing at least one injection opening 6 in a high-pressure bore 3 of a nozzle body 4.
  • the structure of the spray nozzle 2 thus corresponds to the structure of an injection valve, as it is used for the injection of fuel, in particular of diesel fuel, in the combustion chamber of an internal combustion engine. This also high injection pressures are achieved.
  • the injection of the solution, suspension or emulsion under high pressure into the drying chamber 7 makes it possible to produce very fine particles or very fine powders.
  • the solution, suspension or emulsion is first introduced as a spray 16 in the drying room 7. In the drying room 7, the drying of the spray 16, so that microparticles 1 are formed. The transition from the spray 16 to the dried microparticles 1 is indicated in FIG. 1 by a dashed line.
  • the spray nozzle 2 of FIG. 1 has an injection opening 6, which is arranged in the region of a nozzle tip 11, coaxial with a longitudinal axis A of the nozzle body 4. Alternatively or additionally, at least one injection opening 6 can also be arranged laterally in the nozzle tip 11. Such a spray nozzle 2 is shown by way of example in FIG. 2.
  • FIG. 3 A development of a spray nozzle 2 for a device 10 according to the invention is shown in FIG. 3.
  • the nozzle body 4 is connected to an adapter 9, in which a mixing chamber 8 is formed, into which the injection opening 6 opens.
  • the mixing chamber 8 Via a further injection opening 12, which is formed in the adapter 9, the mixing chamber 8 is connected to the drying chamber 7.
  • the entry into the drying space 7 is thus effected indirectly via the mixing chamber 8, specifically after the solution, suspension or emulsion to be injected has been mixed with another medium.
  • the further medium may in particular be a further liquid and / or a NEN act powdery solid.
  • the further medium passes into the mixing chamber 8 via a media supply 14, which in the present case is formed laterally in the adapter 9.
  • a media supply 14 which in the present case is formed laterally in the adapter 9.
  • an optimal mixing of the media is achieved due to the high-pressure injection, before the media reach the drying chamber 7.
  • this is preferably detachably connected to the nozzle body
  • FIG. 4 shows a device 10 for producing monodisperse microparticles 1 in combination with a device 13 for additive manufacturing.
  • the monodisperse microparticles 1 produced by the device 10 can thus be further processed directly.
  • the microparticles 1 are in the present case produced from a polymer melt which is heated to a predetermined temperature and fed to the spray nozzle 2.
  • the polymer melt is subjected to high pressure, so that the injection takes place in the drying chamber 7 under high pressure, preferably together with the injection of a protective gas.
  • the injection opening 6 of the spray nozzle 2 may be preceded by an adapter 9 similar to FIG.
  • the polymer melt When introduced into the drying chamber 7, the polymer melt is atomized, so that a spray 16 is formed, which dries in the drying room 7.
  • the dried material is fed from the drying chamber 7 to a cyclone 15 in order to deposit microparticles 1 of the same size.
  • Via a pipe connection 17 then reach the microparticles 1 produced by the device 10 to the device 13, which is a 3D printer.
  • the microparticles 1 are supplied by means of a feed device 18 to a pressure chamber 19 and constructed in a selective laser melting process with the aid of a laser 20 in layers and fused to form a workpiece 21.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Microbiology (AREA)
  • Glanulating (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Abstract

L'invention concerne un procédé pour obtenir des micro-particules monodispersées (1), selon lequel une solution, en particulier une solution polymère aqueuse, une suspension ou une émulsion est pulvérisée au moyen d'une buse de pulvérisation (2) puis séchée. Selon l'invention, la solution, la suspension ou l'émulsion de la buse de pulvérisation (2), qui présente une aiguille (5) logée dans un trou haute pression (3) d'un corps (4) de la buse de manière à pouvoir effectuer un mouvement de va-et-vient pour libérer et fermer au moins une ouverture d'injection (6) formée dans le corps (4) de la buse, est injectée sous haute pression dans une chambre sèche (7). L'invention concerne en outre un dispositif (10) pour l'obtention de microparticules dispersées (1), qui convient pour la mise en œuvre du procédé selon l'invention.
PCT/EP2018/057145 2017-05-10 2018-03-21 Procédé et dispositif pour obtenir des microparticules monodispersées WO2018206190A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102017207870.7A DE102017207870A1 (de) 2017-05-10 2017-05-10 Verfahren und Vorrichtung zur Herstellung monodisperser Mikropartikel
DE102017207870.7 2017-05-10

Publications (1)

Publication Number Publication Date
WO2018206190A1 true WO2018206190A1 (fr) 2018-11-15

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PCT/EP2018/057145 WO2018206190A1 (fr) 2017-05-10 2018-03-21 Procédé et dispositif pour obtenir des microparticules monodispersées

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DE (1) DE102017207870A1 (fr)
WO (1) WO2018206190A1 (fr)

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2407616A1 (de) 1974-02-15 1975-08-28 Kenji Saguchi Spruehtrockner
WO2003087335A2 (fr) * 2002-04-11 2003-10-23 Medimmune Vaccines, Inc. Conservation de matieres bioactives par sechage par pulverisation
JP2004092969A (ja) * 2002-08-30 2004-03-25 Fuji Photo Film Co Ltd 噴霧乾燥装置
JP2007029881A (ja) * 2005-07-28 2007-02-08 Toyota Motor Corp 塗布装置及び塗布方法
WO2011028105A2 (fr) * 2009-09-02 2011-03-10 Anro Spray Solutions Dispositif de séchage par pulvérisation
WO2011120155A1 (fr) * 2010-04-01 2011-10-06 The Governors Of The University Of Alberta Traitement par un fluide supercritique de biopolymères de haut poids moléculaire
US20140346698A1 (en) * 2011-08-16 2014-11-27 Nederlandse Organisatie Voor Toegepast-Natuurwetenschappelijk Onderzoek Tno Method of spray-drying and apparatus for spray-drying

Family Cites Families (5)

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Publication number Priority date Publication date Assignee Title
US3990938A (en) * 1971-07-16 1976-11-09 General Electric Company Recovery of polymer from solution
US4042653A (en) * 1974-07-31 1977-08-16 Scm Corporation Process for spray forming of discrete particles
WO1999030833A1 (fr) * 1997-12-17 1999-06-24 Universidad De Sevilla Dispositif et procede pour creer des particules seches
CN104771920B (zh) * 2015-03-22 2017-04-19 孙谨先 一种真空干燥电控定量微喷方法及其装置
CN206240095U (zh) * 2016-08-29 2017-06-13 昆明理工大学 一种制备超细复合粉体的装置

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2407616A1 (de) 1974-02-15 1975-08-28 Kenji Saguchi Spruehtrockner
WO2003087335A2 (fr) * 2002-04-11 2003-10-23 Medimmune Vaccines, Inc. Conservation de matieres bioactives par sechage par pulverisation
JP2004092969A (ja) * 2002-08-30 2004-03-25 Fuji Photo Film Co Ltd 噴霧乾燥装置
JP2007029881A (ja) * 2005-07-28 2007-02-08 Toyota Motor Corp 塗布装置及び塗布方法
WO2011028105A2 (fr) * 2009-09-02 2011-03-10 Anro Spray Solutions Dispositif de séchage par pulvérisation
WO2011120155A1 (fr) * 2010-04-01 2011-10-06 The Governors Of The University Of Alberta Traitement par un fluide supercritique de biopolymères de haut poids moléculaire
US20140346698A1 (en) * 2011-08-16 2014-11-27 Nederlandse Organisatie Voor Toegepast-Natuurwetenschappelijk Onderzoek Tno Method of spray-drying and apparatus for spray-drying

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
BOUCHARD A ET AL: "Effect of the spraying conditions and nozzle design on the shape and size distribution of particles obtained with supercritical fluid drying", EUROPEAN JOURNAL OF PHARMACEUTICS AND BIOPHARMACEUTICS, ELSEVIER SCIENCE PUBLISHERS B.V., AMSTERDAM, NL, vol. 70, no. 1, 1 September 2008 (2008-09-01), pages 389 - 401, XP024520623, ISSN: 0939-6411, [retrieved on 20080411], DOI: 10.1016/J.EJPB.2008.03.020 *

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