WO2003089130A1 - Microreacteurs - Google Patents

Microreacteurs Download PDF

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Publication number
WO2003089130A1
WO2003089130A1 PCT/DE2003/001144 DE0301144W WO03089130A1 WO 2003089130 A1 WO2003089130 A1 WO 2003089130A1 DE 0301144 W DE0301144 W DE 0301144W WO 03089130 A1 WO03089130 A1 WO 03089130A1
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WO
WIPO (PCT)
Prior art keywords
network
microreactors
cell
ceramic
open
Prior art date
Application number
PCT/DE2003/001144
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German (de)
English (en)
Inventor
Jörg ADLER
Reinhard Lenk
Tassilo Moritz
Original Assignee
Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V.
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 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. filed Critical Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V.
Publication of WO2003089130A1 publication Critical patent/WO2003089130A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00851—Additional features
    • B01J2219/00869—Microreactors placed in parallel, on the same or on different supports
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00873—Heat exchange
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28—HEAT EXCHANGE IN GENERAL
    • F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
    • F28F2260/00—Heat exchangers or heat exchange elements having special size, e.g. microstructures

Definitions

  • the invention relates to the fields of chemical engineering and ceramics and relates to microreactors which can be used, for example, for the synthesis of active substances or hazardous substances.
  • Microreactors are becoming increasingly important due to their advantages compared to macroscopic chemical reactors, for example because they have shorter response times, lower chemical consumption and less space.
  • Typical functions of microreactors are the mixing of gases and liquids, their temperature control (heating / cooling), and the setting of a defined residence time of the gases / liquids or their mixtures and reactants. This function is realized through the geometrical design of micro-volumes in which the gases / liquids are passed, linger, mixed, react.
  • Typical dimensions of the volume structuring in microreactors lie laterally in the range of 10-500 ⁇ m, the length, width and height ratio differing greatly depending on the function of the microvolume and often reaching the dimension of several mm in one dimension.
  • the surfaces of the microvolumes are partially specially designed to e.g. to enable intensive contact with an applied catalyst etc.
  • microreactors are manufactured according to the prior art by introducing free microvolumes, ie cavities, into the respective materials (eg metal, ceramic, plastic) from which the microreactor is constructed. This can be done by micromachining, such as milling and laser processing, by etching, by embossing or by molding master forms or negative forms previously produced using similar processes (W. Ehrfeld et al. DECHEMA monographs Vol. 132, Verlag Chemie Weinheim, pp. 1-28 , 1996).
  • structuring techniques result in high freedom of design for the microcavities in the surface, ie in the xy direction, while they are severely limited in the third dimension (z direction);
  • the structuring depth is usually limited, or can only be set imprecisely, and only goes into the depth at an angle of 90 ° or only with slight deviations of 90 ° from the xy surface.
  • Undercuts are generally not possible, but only possible by combining differently shaped parts, for example by sealing a channel structure with an intermediate layer.
  • Another disadvantage of these manufacturing methods is that the ratio of the volume of the cavities to the surrounding material from which it is made is usually very small, rarely greater than 1. This gives the microreactor a number of disadvantageous properties, e.g. a high heat capacity, which is unfavorable for the introduction or dissipation of reaction heat.
  • the object of the invention is to provide microreactors which have a three-dimensional microstructuring.
  • the microreactors according to the invention consist of a tight envelope with inlet and outlet openings.
  • One or more open-cell, three-dimensional microstructured networks made of polymers, glass, metal or ceramic or of compounds or of composites of these materials are arranged within the casing. These have mesh or cell widths of ⁇ 500 ⁇ m and an open porosity of> 50% by volume, and the microstructuring is carried out in the form of one or more cavities arranged three-dimensionally in all spatial directions, the ratio of cavity volume to network volume being greater than 1 is.
  • a network, a ceramic network, an open-cell foam ceramic, an open-cell metal foam, an open-cell glass foam and / or an open-cell polymer foam are advantageously used as the network.
  • the ceramic network or the open-cell foam ceramic consists of Al 2 0 3 or SiC.
  • the covering consists of polymers, glass, ceramics or metal or compounds or composites of them or of the same but dense material as the network, wherein the covering can consist wholly or partly of an optically transparent material.
  • the network further advantageously consists of a ceramic network or foam ceramic partially filled with metal or glass.
  • the mesh or cell widths are between 20 and 300 ⁇ m.
  • the network has different mesh or cell widths within the envelope.
  • the open porosity is between 75 and 90% by volume. It is particularly advantageous if the ratio of cavity volume to network volume is between 3 and 10.
  • the surface of the network is structured to increase the surface area.
  • the network consists entirely or partially of a catalytically active material or is completely or partially coated with a catalytically active material, it being possible for the catalytic material to be photoinitiatable, radiation-initiatable, chemically initiatable, thermally initiatable.
  • the material of the network consists entirely or partially of an electrically conductive material.
  • a plurality of networks are also separated within the envelope by dense or microporous separating layers with a pore size between 2 nm and 1 ⁇ m.
  • the network has anisotropic microstructuring.
  • the network consists of a material with three-dimensionally repeated microcavities in all spatial directions with structural widths in all three spatial directions of ⁇ 500 ⁇ m, in which the ratio of cavity to material volume is> 1 (advantageously> 3,> 8).
  • a material is used as the network, which is in the form of an open-cell, three-dimensional microstructured network with mesh or cell widths ⁇ 500 ⁇ m and an open porosity of> 50% by volume.
  • Three-dimensional microstructured open cell networks can be produced with cell widths of ⁇ 500 ⁇ m. They can consist of polymer, glass, metal or ceramic or of connections or composites of these materials. They have a ratio of cavity volume to material volume which is significantly greater than 1 and is typically 3 to 10, advantageously 7 to 9. Networks, in particular open-cell foams, have a very good cross-mixing ability of flowing gases or liquids. The flow resistance can be varied through the mesh or cell size, the pore volume and the dimensions of the respective network / foam, which results in defined dwellings for flowing liquids / gases depending on their viscosity.
  • microstructured open-cell networks / foams is very high (7000 to 10000 m 2 / m 3 ) and can be further increased by coating the materials forming the network / foam with additional microporous materials (so-called washcoats) and, for example, providing them with catalytically active substances become.
  • photocatalytically active coatings are applied to the material forming the network / foam and the dense walls of the microreactor are designed to be optically transparent, entirely or with viewing windows, so that photocatalysis can be triggered by the external excitation with a special light source. This is possible above all because the high porosity of the networks / foams allows the light to penetrate deeply into the cavities of the network / foam and thus onto the surface of the photocatalytically coated materials.
  • Networks / foams made of electrically conductive materials can be electrically heated directly by applying a voltage or indirectly heated in a microwave field.
  • Networks / foams made of materials with high thermal conductivity can be indirectly heated or cooled.
  • a microreactor made of an open-cell, three-dimensional microstructured network can be manufactured by providing a polymer, glass, metal or ceramic foam with a tight coating made of polymer, metal or ceramic, which has corresponding openings for the inlet and outlet of the liquids / Gases is provided.
  • a microreactor can also be produced by placing a three-dimensionally microstructured foam body in a thin-walled container made of polymer, metal, glass or ceramic, which is provided with the above-mentioned openings is introduced. Or the dense covering already arises during the foaming of the material (so-called molded foam) on the vessel walls of the mold into which the foam is foamed.
  • foams of differently fine or dense cell sizes and materials perpendicular or parallel or obliquely to the flow direction can be combined in one microreactor.
  • different effects e.g. successive mixing, reacting, tempering, separating
  • the same foams can also be coated and combined with different catalysts.
  • microstructured networks / foams can also be anisotropically structured by being deformed. This results in an elongation or compression of the meshes or cells in one direction and thus direction-dependent properties, e.g. Flow resistance, thermal and electrical properties etc. This deformation can also take place continuously over a certain dimension, so that there is a gradual change in the anisotropy and thus geometrically graded properties arise.
  • foam-like three-dimensional microstructured materials is possible and sensible, as e.g. can be produced by textile techniques from polymer threads, metal wires, ceramic and glass fibers or indirectly from glass and ceramics.
  • Openings for the insertion of sensors etc. can also be provided.
  • Generative processes such as SLS (selective laser sintering), 3DP (3D printing) and FDM (fused deposition modeling) can also be used to manufacture the networks.
  • SLS selective laser sintering
  • 3DP 3D printing
  • FDM fused deposition modeling
  • the positive connection of two or more parts of the casing is possible, for example, by laser welding or by means of joining foils.
  • a cuboid microreactor is made up of a network, the cavities of which are constructed as follows: Each cavity consists of a cavity with a diameter of approx. 300 ⁇ m, which is adjacent to an average of 12 cavities of the same type, the opening to the adjacent cavities being one in has an approximately circular cross-section with an average diameter of approx. 160 ⁇ m.
  • the network itself consists of thin rods made of aluminum oxide ceramic, which are on average about 50 ⁇ m thick and about 120 ⁇ m long. Four of these rods are connected to each other at their end points so that they form the cavities described.
  • the ratio of the volume of the cavities to the volume fraction of the rods forming the network is approximately 5.25, which corresponds to an open porosity of the network of 84%.
  • the cavities extend repeatedly in all three spatial directions; about 80 cavities in the x direction, approx. 40 in the y direction and approx. 12 in the z direction, resulting in a body with dimensions of approx. 20 x 10 x 3 mm.
  • the side surfaces of the body are made of dense aluminum oxide ceramic surfaces that have an additional thickness of 1 mm.
  • the surface of the ceramic rods is provided with a network of fine trenches that are approximately 100 nm wide and 10 nm deep.
  • a layer of very fine platinum particles is applied to the surface of the ceramic in the partial volume of the network.
  • a round outlet opening and two inlet openings with a diameter of 1 mm are offset in the middle or in the middle.
  • the uncoated part of the network connects directly to the two inlet openings, so that the inflowing media only come into contact with the catalytically active platinum on the surface of the network after passing 20 cavities in the x direction.
  • the microreactor serves as a catalytically supported mixing and reaction section which, when flowing through a liquid or gaseous medium, has a defined dwell time and reaction time depending on its viscosity.
  • a microreactor is made up of a combination of two different networks.
  • Network 1 is made up of cavities as described in Example 1.
  • a few nanometers thin layer of very fine titanium oxide particles is applied to the surface of the aluminum oxide ceramic rods of the network.
  • the cavities extend repeatedly in all three spatial directions; about 80 cavities in the x direction, about 80 in the y direction and about 12 in the z direction, resulting in a body with dimensions of approx. 20 x 20 x 3 mm.
  • the side surfaces xz and yz side surfaces of the body are formed from dense aluminum oxide ceramic surfaces which have an additional thickness of 1 mm.
  • a round outlet opening and inlet opening with a diameter of 1 mm are provided in the center.
  • the xy top of the network is delimited by a transparent, 1mm thick sapphire disc, the underside by a porous aluminum oxide ceramic surface with a pore size of about 50 nm.
  • network 2 with cavities consisting of a cavity with a diameter of approx. 250 ⁇ m , which is adjacent to on average 12 cavities of the same type, the opening to the adjacent cavities having an approximately circular cross section with an average diameter of approximately 120 ⁇ m.
  • the network itself consists of thin rods made of aluminum oxide ceramic, which are on average about 50 ⁇ m thick and about 100 ⁇ m long. Four of these rods are connected to each other at their end points so that they are as described Form cavities.
  • the ratio of the volume of the cavities to the volume fraction of the rods forming the network is approximately 3, which corresponds to an open porosity of the network of 75%.
  • the cavities extend repeatedly in all three spatial directions; about 100 cavities in the x direction, about 100 in the y direction and about 15 in the z direction, resulting in a body with dimensions of about 20 x 20 x 3 mm. Except for the upper xy surface, the side surfaces of the body are formed from dense aluminum oxide ceramic surfaces which have an additional thickness of 1 mm. On the surfaces forming the end faces of the microreactor, ie the two opposite yz outer surfaces of the microreactor, a round outlet opening and inlet opening with a diameter of 1 mm are provided in the center.
  • the entire microreactor thus has the dimensions of 22 x 22 x 9 mm.
  • the two networks form two reaction and residence spaces that are connected by the porous intermediate layer.
  • exposure to UV light from the outside through the sapphire surface can initiate a photocatalytic reaction on the titanium oxide surface of the rods with the medium supplied through the upper inlet opening. While some of the reaction products leave the reaction space through the upper outlet and e.g. is supplied again in the circuit, another part of the reaction products reaches the second reaction space through the porous intermediate layer and is mixed there with another medium fed through the lower inlet opening or further reacted.
  • a cuboid microreactor is made up of a network whose cavities are constructed as follows: Each cavity consists of a cuboid cavity with a dimension of approx. 100 ⁇ m in the x direction, approx. 80 ⁇ m in the y direction and approx. 300 ⁇ m in z-direction.
  • the network itself consists of thin rods made of silicon carbide ceramic, which are on average around 25 ⁇ m thick and form the edges of the cavities. The ratio of the volume of the cavities to the volume fraction of the rods forming the network is approximately 9.2, which corresponds to an open porosity of the network of 90%.
  • the cavities extend repeatedly in all three spatial directions; approx. 200 cavities in the x direction, approx. 125 in the y direction and approx. 10 in the z direction, resulting in a body with the dimensions of approx. 20 x 10 x 3 mm.
  • the side surfaces of the body are formed from dense silicon carbide ceramic surfaces, which have an additional thickness of 1 mm.
  • the two opposite y-z outer surfaces of the microreactor each have a round outlet or inlet opening with a diameter of 1 mm.
  • the microreactor serves as a temperature-controlled retention and reaction zone which, when flowing through a liquid or gaseous medium, has a defined retention time depending on its viscosity. Due to the good thermal conductivity of the silicon carbide ceramic, the cooling or heating can be carried out by means of a self-regulating heating / cooling element applied to the external xy surfaces.
  • a cuboid-shaped microreactor is built up from a network as in Example 3.
  • the respective outer cavities are filled with borosilicate glass, so that there is a tight outer wall made of borosilicate glass.
  • about 500 cavities are filled with borosilicate glass in the corners of the cuboid, whereby the space formed by the free cavities narrows evenly towards the two yz faces.
  • the ratio of the volume of the cavities to the volume fraction of the rods forming the network is approximately 9.2, which corresponds to an open porosity of the network of 90%.
  • the ratio of the open cavities to those filled with borosilicate glass is approximately 3.3.
  • a round outlet or inlet opening with a diameter of 1 mm is in the center of the two opposite y-z outer surfaces of the microreactor.
  • the microreactor serves as a mixing, dwell and reaction section. The closed corners of the cuboid microreactor result in particularly good guidance and mixing of the media supplied.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

L'invention a trait aux domaines de la technologie chimique et de la céramique et concerne les microréacteurs qui, par exemple, peuvent être utilisés pour la synthèse de substances actives ou de substances dangereuses. L'invention vise à fournir des microréacteurs qui disposent d'une microstructure tridimensionnelle. A cet effet, on utilise des microréacteurs comprenant une enveloppe étanche dotée d'orifices d'entrée et de sortie et dans laquelle au moins un réseau de microstructuration tridimensionnelle à alvéoles ouvertes réalisé en polymère, verre, métal ou céramique ou en composés ou en composites de ces matières et ayant des ouvertures de mailles ou d'alvéoles < 500 ñm et une porosité ouverte > 50 % en volume. La microstructuration a la forme d'au moins une cavité tridimensionnelle placée dans toutes le directions. Le rapport entre les volumes des cavités et le volume du réseau est supérieure à 1 .
PCT/DE2003/001144 2002-04-19 2003-04-03 Microreacteurs WO2003089130A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE2002118278 DE10218278B4 (de) 2002-04-19 2002-04-19 Mikroreaktor
DE10218278.7 2002-04-19

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WO2003089130A1 true WO2003089130A1 (fr) 2003-10-30

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WO (1) WO2003089130A1 (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1676632A1 (fr) * 2004-12-28 2006-07-05 Covion Organic Semiconductors GmbH Procédé pour la préparation de polymères
EP2303456A1 (fr) * 2008-07-08 2011-04-06 ETH Zurich Catalyseurs céramiques poreux et leurs procédés de production et d'utilisation
EP2440324A1 (fr) * 2009-06-12 2012-04-18 ETH Zurich Dispositif pour le traitement et le conditionnement d'une matière transportée par le dispositif
WO2016077287A1 (fr) 2014-11-11 2016-05-19 H.C. Starck Inc. Systèmes et procédés de microréacteur

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DE102005004075B4 (de) * 2005-01-28 2008-04-03 Umicore Ag & Co. Kg Keramischer Mikroreaktor
DE102007027837A1 (de) * 2007-06-13 2008-12-18 Eads Deutschland Gmbh Verfahren zur Herstellung einer metallischen Mikrostruktur für einen Mikroreaktor
DE102016217841B4 (de) 2016-09-19 2024-01-18 Ifl Ingenieurbüro Für Leichtbau Gmbh & Co Kg System aus einer Dispersionseinrichtung und einer Wärmeübertagungseinrichtung
DE102016117790A1 (de) * 2016-09-21 2018-03-22 Boraident Gmbh Komplexer monolithischer, poröser SiO₂-reicher Glasformkörper, ein Verfahren zu dessen Herstellung sowie dessen Verwendung

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US5690763A (en) * 1993-03-19 1997-11-25 E. I. Du Pont De Nemours And Company Integrated chemical processing apparatus and processes for the preparation thereof
WO2000021659A1 (fr) * 1998-10-09 2000-04-20 Motorola Inc. Dispositifs microfluidiques multicouches integres
WO2001012753A1 (fr) * 1999-08-17 2001-02-22 Battelle Memorial Institute Structure et procede catalytiques de synthese fischer-tropsch
WO2001012312A2 (fr) * 1999-08-17 2001-02-22 Battelle Memorial Institute Reacteur chimique et procede permettant de conduire des reactions catalytiques avec des reactifs en phase gazeuse
US6200536B1 (en) * 1997-06-26 2001-03-13 Battelle Memorial Institute Active microchannel heat exchanger

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DE19753249B4 (de) * 1997-12-01 2005-02-24 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Keramiknetzwerk, Verfahren zu dessen Herstellung und Verwendung
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US5051241A (en) * 1988-11-18 1991-09-24 Pfefferle William C Microlith catalytic reaction system
US5690763A (en) * 1993-03-19 1997-11-25 E. I. Du Pont De Nemours And Company Integrated chemical processing apparatus and processes for the preparation thereof
US6200536B1 (en) * 1997-06-26 2001-03-13 Battelle Memorial Institute Active microchannel heat exchanger
WO2000021659A1 (fr) * 1998-10-09 2000-04-20 Motorola Inc. Dispositifs microfluidiques multicouches integres
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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1676632A1 (fr) * 2004-12-28 2006-07-05 Covion Organic Semiconductors GmbH Procédé pour la préparation de polymères
WO2006069773A1 (fr) * 2004-12-28 2006-07-06 Merck Patent Gmbh Procede de production de polymeres
KR101244509B1 (ko) 2004-12-28 2013-03-18 메르크 파텐트 게엠베하 중합체의 제조 방법
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EP2303456A1 (fr) * 2008-07-08 2011-04-06 ETH Zurich Catalyseurs céramiques poreux et leurs procédés de production et d'utilisation
EP2440324A1 (fr) * 2009-06-12 2012-04-18 ETH Zurich Dispositif pour le traitement et le conditionnement d'une matière transportée par le dispositif
EP2440325A1 (fr) * 2009-06-12 2012-04-18 DSM IP Assets B.V. Dispositif destiné à mettre en uvre des réactions chimiques dans des conditions homogènes et hétérogènes
US8905080B2 (en) 2009-06-12 2014-12-09 Eth Zurich Device for processing and conditioning of material transported through the device
US8961892B2 (en) 2009-06-12 2015-02-24 Dsm Ip Assets B.V. Device for carrying out chemical reactions under homogenous and heterogenous conditions
WO2016077287A1 (fr) 2014-11-11 2016-05-19 H.C. Starck Inc. Systèmes et procédés de microréacteur
CN107073583A (zh) * 2014-11-11 2017-08-18 H.C.施塔克公司 微反应器系统和方法
EP3218098A4 (fr) * 2014-11-11 2018-05-23 H. C. Starck Inc Systèmes et procédés de microréacteur

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Publication number Publication date
DE10218278A1 (de) 2003-11-20
DE10218278B4 (de) 2005-12-01

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