DE102016202610A1 - Process for producing a porous functional body - Google Patents

Process for producing a porous functional body

Info

Publication number
DE102016202610A1
DE102016202610A1 DE102016202610.0A DE102016202610A DE102016202610A1 DE 102016202610 A1 DE102016202610 A1 DE 102016202610A1 DE 102016202610 A DE102016202610 A DE 102016202610A DE 102016202610 A1 DE102016202610 A1 DE 102016202610A1
Authority
DE
Germany
Prior art keywords
carrier substrate
step
material
catalytically active
hydrophobic liquid
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.)
Withdrawn
Application number
DE102016202610.0A
Other languages
German (de)
Inventor
Martin Schröter
Erhard Rieder
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Duerr Systems AG
Original Assignee
Duerr Systems AG
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 Duerr Systems AG filed Critical Duerr Systems AG
Priority to DE102016202610.0A priority Critical patent/DE102016202610A1/en
Publication of DE102016202610A1 publication Critical patent/DE102016202610A1/en
Application status is Withdrawn legal-status Critical

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D39/00Filtering material for liquid or gaseous fluids
    • B01D39/14Other self-supporting filtering material ; Other filtering material
    • B01D39/20Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • B01D39/2068Other inorganic materials, e.g. ceramics
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2239/00Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/10Filtering material manufacturing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/92Chemical or biological purification of waste gases of engine exhaust gases
    • B01D53/94Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
    • B01D53/9459Removing one or more of nitrogen oxides, carbon monoxide, or hydrocarbons by multiple successive catalytic functions; systems with more than one different function, e.g. zone coated catalysts

Abstract

A method for producing a porous functional body, in particular a catalytically active particle filter, in which the functional material, in particular the catalytically active material may have a local concentration gradient, comprises the following steps: Providing a carrier substrate which is at least partially composed of a porous and / or fibrous Filter material is formed, filling a predetermined portion of an inner volume of the carrier substrate with a hydrophobic liquid, removing a predetermined portion of the hydrophobic liquid from the carrier substrate, introducing a hydrophilic liquid, a functional material or a precursor material of a functional material, in particular a catalytically active material or a Precursor of a catalytically active material, in the carrier substrate and coating the carrier substrate with the functional material or the precursor material of a functional material ,

Description

  • The present invention relates to a method for producing a porous functional body, in particular a catalytically active particle filter.
  • A wide variety of porous functional bodies are known which are provided and configured to interact with liquid and / or gaseous fluids, the fluid or at least parts of the fluid penetrating into a porous structure of the functional body and having a functional material arranged or provided in the functional body interact so that the fluid undergoes a change in one of its state variables, its chemical properties and / or its composition. In addition to, for example, heat storage bodies, particulate filters, such as, for example, diesel particulate filters, form examples of porous functional bodies. Diesel particle filters are usually coated with catalytically active material as functional material by precipitation in aqueous solution of dissolved salts or by direct crystallization in aqueous liquids contained gels. In general, the liquid of the solution or gel substantially wets the entire body of the carrier substrate during the precipitation or crystallization process substantially homogeneously. As a result, the catalytically active material is also distributed homogeneously over the entire body of the carrier substrate.
  • In cases where a local concentration gradient of the catalytically active material or a precursor of a catalytically active material is desired, especially in cases where a controlled local concentration gradient in only one spatial direction is desired, such as for pure surface catalysis, various production methods have already been used tried. For example, a spray impregnation or a washcoat coating differentiated according to particle sizes of the catalytically active material are known. However, there is hitherto no known method which allows a coating of a carrier substrate with catalytically active material with a targeted local concentration gradient in a reliable manner without too much effort.
  • The invention is therefore based on the object to provide an improved process for producing a porous functional body, in particular a catalytically active particulate filter, with which a local concentration gradient of the functional material, in particular of the catalytically active material can be achieved.
  • This object is achieved by a method for producing a porous functional body, in particular a catalytically active particulate filter having the method steps specified in claim 1. Advantageous embodiments of the invention are the subject of the dependent claims.
  • The inventive method for producing a porous functional body, in particular a catalytically active particulate filter, comprises the following steps:
    • a) providing a carrier substrate, which is at least partially formed of a porous and / or fibrous filter material;
    • b) filling a predetermined portion of an internal volume of the carrier substrate with a hydrophobic liquid;
    • c) removing a predetermined proportion of the hydrophobic liquid from the carrier substrate;
    • d) introducing into the carrier substrate a hydrophilic liquid which contains a functional material or a precursor material of a functional material, in particular a catalytically active material or a precursor of a catalytically active material; and
    • e) coating the carrier substrate with the functional material or the precursor material of a functional material.
  • Porous functional bodies, in particular catalytically active particle filters, which have a local concentration gradient of the functional material, in particular of the catalytically active material, can be produced with the method according to the invention in a relatively simple and cost-effective manner. The local concentration gradient can be specifically influenced and is not necessarily limited to one spatial direction. The invention utilizes the physical phenomenon of surface tension at the interface between hydrophilic and hydrophobic liquids.
  • In the context of the invention, a material which selectively brings about an interaction with the fluid or a part of the fluid is, in particular, facilitated (eg catalysts, reactants, sorbents, etc.) or else prevented or suppressed (eg, inhibitors, ...), as well as a Vorstufematerial be understood for an aforementioned functional material.
  • In the context of the invention, a "catalytically active material" preferably comprises both a material which as such can develop or unfold a catalytic effect on at least one chemical conversion reaction or at least comprises a component or a component which is or is such as such in which a catalytic effect on at least one chemical conversion reaction can unfold or unfold, as well as a material which comprises a catalytically activatable material or a precursor material Provide a catalytic effect on at least one chemical reaction reaction in the context of an activation process includes understood.
  • In an advantageous embodiment of the invention, step b) comprises a step of degassing the carrier substrate. Preferably, energy is supplied to the carrier substrate and / or the hydrophobic liquid in step b), for example in the form of sound waves, ultrasonic waves and / or by mechanical shaking of the carrier substrate.
  • In an advantageous embodiment of the invention, the hydrophobic liquid is selected from n-paraffins, iso-paraffins or a mixture / a mixture thereof. Preferably, n-paraffin C10-C13, Isopar C, Isopar E, Isopar L and Isopar V can be used for the hydrophobic liquid.
  • In an advantageous embodiment of the invention, a solvent for the hydrophobic liquid is used to carry out step c). In the context of the invention, a solvent is understood in particular to mean a liquid which is suitable for removing, washing out or removing the hydrophobic liquid from the carrier substrate. The hydrophobic liquid preferably remains chemically unchanged. The solvent for the hydrophobic liquid is preferably selected from ketones, alcohols or paraffins having a lower boiling point than the hydrophobic liquid, preferably acetone, ethanol or n-hexane. In particular, the boiling point of the solvent is at least 25 K, preferably at least 50 K lower than the boiling point of the hydrophobic liquid. However, for carrying out a step c) according to the invention, the solvent may also be provided or designed to change the physical and / or chemical properties of the hydrophobic liquid in such a way that the hydrophobic liquid can escape locally from the carrier substrate or be expelled.
  • The residual solvent is preferably expelled. Stripping can be carried out, for example, by rinsing with an aqueous solution or a gas stream (eg, air, nitrogen, inert gas) as a rinsing agent. The flushing agent preferably has a controlled temperature for this purpose. For example, acetone and ethanol are good solvents for long chain alkanes and water, but n-hexane must be expelled by an air stream and typically requires an intermediate drying step.
  • In an advantageous embodiment of the invention, the hydrophilic liquid is water.
  • In an advantageous embodiment of the invention, the filter material of the carrier substrate is selected from aluminum oxide, titanium dioxide, silicon dioxide, zirconium oxide, cerium oxide and mixtures thereof.
  • In a further advantageous embodiment of the invention, the degree of removal of the hydrophobic liquid from the carrier substrate in step c) is variably adjustable. This can preferably be done by variably setting a contact time of the solvent. For example, the exposure time of the solvent may affect a depth of the catalytically active layer formed during subsequent steps d) and e).
  • In an advantageous embodiment of the invention, the coating in step e) is carried out by a failure process, a crystallization process or a washcoat process.
  • In a further advantageous embodiment of the invention, the steps b) to e) can be carried out repeatedly. Preferably, steps b) to e) are repeated with different predetermined sections of the internal volume of the carrier substrate in step b) and / or with different functional materials or precursor materials of functional materials, in particular catalytically active materials or different precursors of a catalytically active material in step d). In this way it is possible to produce porous functional bodies, in particular particle filters with a plurality of functional materials, in particular a plurality of catalytically active materials and / or with different local concentration gradients of functional materials, in particular catalytically active materials. Furthermore, it may be advantageous if a functional body is provided or coated with at least one functional material and with at least one catalytically active material according to the iterative process for producing a functional body set out above.
  • Optionally, after step e), a step of drying and / or a step of fixing may be performed.
  • With the method according to the invention for producing a porous functional body, in particular a catalytically active particulate filter, in particular the following advantages can be achieved:
    • - selectively selecting the locations with a local concentration gradient;
    • Selectively determining a depth of a local concentration gradient layer;
    • - possible preparation of multifunctional, catalytically active materials at different locations of the carrier substrate, so that a chronological sequence of catalytic reactions is possible;
    • - Setting a defined residence time of a fluid to be cleaned in special catalytic functions;
    • - avoiding restrictions on the access of the catalytically active material to the carrier substrate;
    • - Avoiding surface cover layers.
  • The invention also relates to a porous functional body which has been produced according to the method of the invention described above. The porous functional body is preferably a catalytically active particle filter.
  • The above and other advantages, features and applications of the invention will become more apparent from the following description of various embodiments of the manufacturing method.
  • The invention will be described in more detail below using the example of production processes for catalytically active particulate filters. As mentioned above, however, the production method according to the invention can advantageously be used generally in porous functional bodies.
  • A first embodiment describes a method for producing a simple, catalytically active particulate filter. The surface deposition of the catalytically active material or a precursor of the catalytically active material is intended, for example, by precipitation of salts and / or crystallization of gels to form zeolite structures.
  • In a first step, a carrier substrate is provided, which is formed at least partially from a porous or fibrous filter material. The filter material is for example aluminum oxide (Al 2 O 3 ), titanium dioxide (TiO 2 ), silicon dioxide (SiO 2 ), zirconium oxide (ZrO 2 ), cerium oxide (CeO 2 ) or a mixture of these compounds. For example, the carrier substrate is in the form of a monolith having numerous longitudinal channels separated longitudinally by porous walls, the dispersion side of the channels having an open inlet end and a closed outlet end and the permeation side of the channels having a closed inlet end and an open outlet end.
  • This carrier substrate is immersed in a hydrophobic liquid such as n-paraffin C10-C13 or Isopar C to Isopar V until its internal volume is filled with the hydrophobic liquid. This can be done, for example, by supplying energy to the liquid to degas the porous system of the carrier substrate. The energy is, for example, fed into the hydrophobic liquid by means of sound waves, preferably ultrasonic waves, or similar contactless energy transmission systems.
  • If the surface deposition of the catalytically active material or its precursor is to be restricted to a part of the physical extent of the carrier substrate or a part of the inner surface, this can be achieved by a corresponding limitation of the wetting with the hydrophobic liquid on only this preferred part of the carrier substrate , This method is preferred, for example, for monolithic, catalytically active support substrates, for example of the honeycomb or plate type, which are to receive a specific functionality at the inlet or outlet of the flow channel.
  • The carrier substrate filled or impregnated with the hydrophobic liquid is then rinsed or washed with a solvent for the hydrophobic liquid or immersed in a bath containing such a solvent. The solvent is, for example, acetone, n-decane or ethanol.
  • If necessary, if the catalytically active particulate filter is to be used, for example, as a crossflow type, the exposure time of the solvent can determine the depth of the surface layer in which the catalytically active material or its precursor is to be deposited. The filling level with the hydrophobic liquid in the carrier substrate remaining after the use of the solvent determines the depth of the catalytically active layer which is formed during the subsequent steps. This catalytically active layer depth then determines the residence time of a fluid to be cleaned in the special, catalytically active layer with a specific functionality which is matched to the particular application of the particle filter in the particulate filter produced.
  • Subsequently, the (residual) hydrophobic solvent is expelled, preferably with a hydrophilic liquid at a controlled temperature.
  • Subsequently, the carrier substrate with its prepared surface is brought into contact with a hydrophilic liquid containing the catalytically active material, its salts, gels or other precursors or mixtures thereof. The hydrophilic liquid is preferably water. Due to the physical phenomenon of the surface tension at the interface between the hydrophobic liquid and the hydrophilic liquid, the hydrophilic liquid wets only those portions of the support substrate on which the hydrophobic liquid has been previously removed by means of the solvent.
  • The coating of the carrier substrate with the catalytically active material is then carried out by precipitation, crystallization or washcoat processes with known process conditions which are generally known to the person skilled in the art. Optionally, this drying process is followed by a drying process and / or a fixing or calcination process (heat treatment).
  • A second exemplary embodiment describes a method for producing a catalytically active particle filter having a plurality of different, catalytically active materials with different local concentration gradients.
  • In a first step, the carrier substrate is coated with a catalytically active material, wherein the catalytically active material or its precursor may be distributed homogeneously over the entire body of the carrier substrate without appreciable concentration gradients. Subsequently, the carrier substrate is dried.
  • In a second step, the carrier substrate prepared in this way or a predetermined section thereof is wetted with a hydrophobic liquid with the aid of a degassing operation, as described above in connection with the first exemplary embodiment.
  • In a third step, the carrier substrate wetted with the hydrophobic liquid is brought into contact with a solvent for hydrophobic liquids, as described above in connection with the first exemplary embodiment.
  • In a fourth step, a hydrophilic liquid containing the catalytically active material, its salts, gels or other precursors is contacted with the support substrate or at least parts thereof. It also follows in this case a precipitation, crystallization or washcoat process with known process conditions, followed by a drying process and / or a fixing or calcination process.
  • The sequence of the above steps 2 to 4 can be repeated as desired in order to complete the catalytically active particle filter.
  • Additionally or alternatively, the local size distribution and / or the activation potentials or other properties influencing the local activity of the catalytically active material can also be varied in the same way.

Claims (13)

  1. Process for producing a porous functional body, in particular a catalytically active particle filter, comprising the steps: a) providing a carrier substrate, which is at least partially formed of a porous and / or fibrous filter material; b) filling a predetermined portion of an internal volume of the carrier substrate with a hydrophobic liquid; c) removing a predetermined proportion of the hydrophobic liquid from the carrier substrate; d) introducing into the carrier substrate a hydrophilic liquid which contains a functional material or a precursor material of a functional material, in particular a catalytically active material or a precursor of a catalytically active material; and e) coating the carrier substrate with the functional material or the precursor material of a functional material.
  2. The method of claim 1, wherein step b) comprises a step of degassing the carrier substrate.
  3. Method according to Claim 2, in which energy is supplied to the carrier substrate and / or the hydrophobic liquid in step b).
  4. A method according to any one of the preceding claims, wherein the hydrophobic liquid is selected from n-paraffins, iso-paraffins or a mixture thereof.
  5. Method according to one of the preceding claims, in which a solvent for the hydrophobic liquid is used to carry out the step c).
  6. The method of claim 5, wherein the hydrophobic liquid solvent is selected from ketones, alcohols or n-alkanes having a lower boiling point than the hydrophobic liquid or a mixture thereof.
  7. A method according to any one of the preceding claims, wherein the hydrophilic liquid is water.
  8. Method according to one of the preceding claims, wherein the degree of removal of the hydrophobic liquid from the carrier substrate in step c) is variably adjustable.
  9. Method according to one of the preceding claims, wherein the coating in step e) by a precipitation process, a crystallization process or a washcoat process takes place.
  10. Method according to one of the preceding claims, in which steps b) to e) are carried out repeatedly.
  11. The method of claim 10, wherein steps b) to e) are repeated with different predetermined portions of the internal volume of the carrier substrate in step b) and / or with different functional materials or precursors of functional materials in step d).
  12. Method according to one of the preceding claims, wherein after step e) a step of drying and / or a step of fixing are performed.
  13. Porous functional body, in particular catalytically active particle filter, produced according to a method according to one of the preceding claims.
DE102016202610.0A 2016-02-19 2016-02-19 Process for producing a porous functional body Withdrawn DE102016202610A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DE102016202610.0A DE102016202610A1 (en) 2016-02-19 2016-02-19 Process for producing a porous functional body

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE102016202610.0A DE102016202610A1 (en) 2016-02-19 2016-02-19 Process for producing a porous functional body
DE112017000880.8T DE112017000880A5 (en) 2016-02-19 2017-02-10 Process for producing a porous functional body
PCT/EP2017/052963 WO2017140583A1 (en) 2016-02-19 2017-02-10 Method for producing a porous functional body

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WO (1) WO2017140583A1 (en)

Citations (9)

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DE2546489A1 (en) * 1974-10-21 1976-04-22 Uop Inc A method for coating and impregnating of katalysatortraegern and apparatus for performing the method
EP0149912A2 (en) * 1984-01-19 1985-07-31 Corning Glass Works Treatment of monolithic catalyst supports
US20040001781A1 (en) * 2002-06-27 2004-01-01 Engelhard Corporation Multi-zone catalytic converter
DE10254661A1 (en) * 2002-11-22 2004-06-09 Umicore Ag & Co.Kg A method for coating a catalyst support comprising two different sub-structures with a catalytically active coating and thus obtained catalyst
US20040211172A1 (en) * 2003-04-24 2004-10-28 Chuanfu Wang Muffler and catalytic converter devices
US7097880B2 (en) * 2003-12-18 2006-08-29 Corning Incorporated Method for preparing catalysts
US20070215009A1 (en) * 2004-06-11 2007-09-20 Kabushiki Kaisha Toyota Chuo Kenkyusho Metal Oxide Nanoporous Material, Coating Composition to Obtain the Same, and Methods of Manufacturing Them
EP1897615A2 (en) * 1998-04-28 2008-03-12 Basf Catalysts Llc Monolithic catalysts and related process for manufacture
DE102007044585A1 (en) * 2007-09-19 2009-04-02 Süd-Chemie AG Process for the partial coating of catalytically active components on complex components

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US20070149399A1 (en) * 2005-12-22 2007-06-28 Ku Anthony Y Multifunctional catalyst and methods of manufacture thereof
DE102007029418A1 (en) * 2007-06-26 2009-01-08 Robert Bosch Gmbh Catalyst element, catalyst for exhaust aftertreatment of an internal combustion engine and method for producing a catalyst element according to the invention
DE102007056213A1 (en) * 2007-11-22 2009-05-28 Robert Bosch Gmbh Method for producing a shaped body through which exhaust gas can flow and exhaust system of an internal combustion engine
US8637422B2 (en) * 2010-03-29 2014-01-28 Tanaka Kikinzoku Kogyo K.K. Method for producing surface-supported catalyst
WO2012166833A1 (en) 2011-05-31 2012-12-06 Johnson Matthey Public Limited Company Dual function catalytic filter
US9861962B2 (en) * 2013-10-08 2018-01-09 Industry Foundation Of Chonnam National University Selective surface impregnation method for catalytically active materials on particulate catalyst support using mutual repulsive force and soblubility difference between hydrophilic solvent and hydrophobic solvent

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2546489A1 (en) * 1974-10-21 1976-04-22 Uop Inc A method for coating and impregnating of katalysatortraegern and apparatus for performing the method
EP0149912A2 (en) * 1984-01-19 1985-07-31 Corning Glass Works Treatment of monolithic catalyst supports
EP1897615A2 (en) * 1998-04-28 2008-03-12 Basf Catalysts Llc Monolithic catalysts and related process for manufacture
US20040001781A1 (en) * 2002-06-27 2004-01-01 Engelhard Corporation Multi-zone catalytic converter
DE10254661A1 (en) * 2002-11-22 2004-06-09 Umicore Ag & Co.Kg A method for coating a catalyst support comprising two different sub-structures with a catalytically active coating and thus obtained catalyst
US20040211172A1 (en) * 2003-04-24 2004-10-28 Chuanfu Wang Muffler and catalytic converter devices
US7097880B2 (en) * 2003-12-18 2006-08-29 Corning Incorporated Method for preparing catalysts
US20070215009A1 (en) * 2004-06-11 2007-09-20 Kabushiki Kaisha Toyota Chuo Kenkyusho Metal Oxide Nanoporous Material, Coating Composition to Obtain the Same, and Methods of Manufacturing Them
DE102007044585A1 (en) * 2007-09-19 2009-04-02 Süd-Chemie AG Process for the partial coating of catalytically active components on complex components

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WO2017140583A1 (en) 2017-08-24
DE112017000880A5 (en) 2018-10-25

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