WO2006125649A2 - Verfahren und vorrichtung zum auftragen von washcoat-suspensionen auf einen formkörper - Google Patents
Verfahren und vorrichtung zum auftragen von washcoat-suspensionen auf einen formkörper Download PDFInfo
- Publication number
- WO2006125649A2 WO2006125649A2 PCT/EP2006/005001 EP2006005001W WO2006125649A2 WO 2006125649 A2 WO2006125649 A2 WO 2006125649A2 EP 2006005001 W EP2006005001 W EP 2006005001W WO 2006125649 A2 WO2006125649 A2 WO 2006125649A2
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- channels
- honeycomb
- excess
- suspension
- washcoat
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims abstract description 62
- 239000000725 suspension Substances 0.000 title claims description 74
- 239000011148 porous material Substances 0.000 claims abstract description 50
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 239000003054 catalyst Substances 0.000 claims description 26
- 238000000465 moulding Methods 0.000 claims description 16
- 229910052751 metal Inorganic materials 0.000 claims description 12
- 239000002184 metal Substances 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 9
- 239000006185 dispersion Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- 150000002739 metals Chemical class 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 238000003860 storage Methods 0.000 claims description 5
- 230000009471 action Effects 0.000 claims description 4
- 229910001092 metal group alloy Inorganic materials 0.000 claims description 4
- 150000004645 aluminates Chemical class 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 239000010457 zeolite Substances 0.000 claims description 3
- 229910052878 cordierite Inorganic materials 0.000 claims description 2
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000004745 nonwoven fabric Substances 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 150000004760 silicates Chemical class 0.000 claims description 2
- 241000264877 Hippospongia communis Species 0.000 description 103
- 238000000576 coating method Methods 0.000 description 30
- 230000008569 process Effects 0.000 description 22
- 239000011248 coating agent Substances 0.000 description 21
- 239000007789 gas Substances 0.000 description 14
- 239000000919 ceramic Substances 0.000 description 13
- 239000006262 metallic foam Substances 0.000 description 10
- 238000007664 blowing Methods 0.000 description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 238000011049 filling Methods 0.000 description 8
- 238000000746 purification Methods 0.000 description 8
- 229910004298 SiO 2 Inorganic materials 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 6
- 229910044991 metal oxide Inorganic materials 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 6
- 229910010413 TiO 2 Inorganic materials 0.000 description 5
- 150000004706 metal oxides Chemical class 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 238000005119 centrifugation Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 241000243142 Porifera Species 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- 239000006260 foam Substances 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 238000010926 purge Methods 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- OWIKHYCFFJSOEH-UHFFFAOYSA-N Isocyanic acid Chemical compound N=C=O OWIKHYCFFJSOEH-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- -1 SiO 2 Chemical class 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- XLJMAIOERFSOGZ-UHFFFAOYSA-N anhydrous cyanic acid Natural products OC#N XLJMAIOERFSOGZ-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 239000012876 carrier material Substances 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 150000002736 metal compounds Chemical class 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical class [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910020203 CeO Inorganic materials 0.000 description 1
- 102000034530 Channels/pores Human genes 0.000 description 1
- 108091006155 Channels/pores Proteins 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- GEIAQOFPUVMAGM-UHFFFAOYSA-N ZrO Inorganic materials [Zr]=O GEIAQOFPUVMAGM-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 1
- 239000002318 adhesion promoter Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000010097 foam moulding Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000000284 resting effect Effects 0.000 description 1
- 229910052702 rhenium Inorganic materials 0.000 description 1
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 description 1
- 238000000518 rheometry Methods 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/56—Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional monoliths
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0215—Coating
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
- F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
- F01N3/24—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by constructional aspects of converting apparatus
- F01N3/28—Construction of catalytic reactors
- F01N3/2803—Construction of catalytic reactors characterised by structure, by material or by manufacturing of catalyst support
Definitions
- the invention relates to a method and an apparatus for the production of supported catalysts by applying a Washcoat suspension on a ducts or pores having shaped body as a carrier and the use of the thus obtained supported catalysts in the purification of exhaust gases, in particular exhaust gases of internal combustion engines.
- Catalysts based on coated moldings for example so-called monoliths or metal foams for the purification of exhaust gases, such as the oxidation of CO or hydrocarbons to CO 2 and water or the reduction of NO x with ammonia or urea to N 2 and water or the decomposition Of urea or its thermal decomposition product, the isocyanic acid, to ammonia and CO 2 , have long been known.
- these catalysts are constructed in such a way that a monolithic carrier material ("honeycomb" in the case of channels or ceramic or metal foam in the case of pores) traversed by channels or pores has a high surface area (high-surface area).
- Metal oxide coating for example of Al 2 O 3 , SiO 2 or TiO 2 , or their mixed oxides is coated and on these metal oxide surfaces the actually catalytically active metals or metal compounds, such as precious metals or transition metal oxides, and optionally additional promoter compounds /
- the metal oxide coatings alone are catalytically active, a typical example being the hydrolysis of isocyanic acid to ammonia on TiO 2 coated moldings.
- honeycombs consist of a honeycomb body, which consists of a honeycomb sheath and a carrier used therein, for example, a partially structured and wound sheet metal foil, can put together.
- a carrier used therein for example, a partially structured and wound sheet metal foil
- the honeycomb consists entirely of a purely ceramic shaped body.
- the honeycomb is essentially traversed by running parallel to the main axis of the honeycomb channels.
- Metal or ceramic foam are highly porous moldings that can assume any geometric shapes.
- the channels passing through a monolithic carrier can have an ordered or disordered channel structure, and furthermore the essentially parallel channels can also be interconnected (so-called open channel structures), for example also through porous channel walls.
- open channel structures a radial gas distribution within the honeycomb body is also made possible.
- the size of the honeycomb as well as the dimensioning of the channels is determined mainly by the dimension of the exhaust pipe systems, the required pressure losses and the required residence times of the exhaust gas. The same applies mutatis mutandis to the corresponding highly porous metallic and ceramic sponge or foam structures.
- materials such as Cordient, Steatite, Duranit® or silicon carbide or shaped bodies of silicon dioxide, aluminum oxides, aluminates or even metals and metal alloys are used as material for moldings which can be used according to the invention.
- the use of metals and metal alloys makes it possible, in particular, to produce complex structured shaped bodies, such as, for example, honeycombs with open channel structures or ceramic or metal foams whose pore structure has a particularly high internal surface area.
- the preparation of a catalyst based on a moldable body which can be used according to the invention is generally carried out by applying a washcoat (WC) to the surface of its internal cavities, that is to say, for example. As its channel walls, pores, etc. (coating), followed by drying followed by calcination at higher temperatures for solidification and final surface design of the washcoat. Thereafter, the catalytically active components are applied to the washcoat by impregnation steps, mostly from the aqueous solutions of their precursors. However, it is also possible to apply the active components or their precursor compounds directly with the coating process.
- WC washcoat
- shaped body an inner hollow body or channel-containing shaped body (hereinafter referred to simply as "shaped body") with the inorganic high-surface-area materials is possible by various methods.
- additives such as inorganic or organic binders, surfactants, catalytic active components, pore formers, rheology aids and other additives.
- washcoat suspension 4 dipping, sucking or pumping process is filled with this so-called washcoat suspension.
- honeycomb bodies are understood to mean honeycombs with complex structured honeycombs, in which the channels have elevations or depressions or blades.
- Open structures are also part of this type of support. In open structures are - P2006 / 005001
- Honeycomb or porous shaped body with high cell densities as well as honeycomb with complex structured and perforated channels (open structures) can not be coated by the previously known methods without undesirably great expense. In particular, blowing out the excess washcoat suspension with air is no longer possible with open channel structures or pore structures.
- blow-out air basically takes the path of least resistance (path of least pressure loss).
- path of least resistance path of least pressure loss.
- the blow-out air used in the sequence is discharged through the holes of the open structures into those already open channels or pore structures and the pressure of the blow-out air used is insufficient. to blow down the washcoat suspension from still partially filled channels or pores, in which the washcoat suspension is held by capillary forces.
- Even a few channels or pore structures completely emptied by purging lead to the described effect, so that only a few channels are to be emptied by blowing out alone.
- This effect which is particularly noticeable in honeycombs with open structures or porous ceramic and metal foams, is illustrated in FIG. 1:
- Fig. 1 shows a partial view of two parallel channels of a honeycomb, which are interconnected via a perforation (open structure). While the channel shown on the right already has been freed of excess washcoat by the blow-off air (the flow direction of the air is illustrated by the arrows), this is no longer possible in the channel shown on the left for the reason described above, so that blow-out alone is no longer possible Remaining and held by the capillary rest of washcoat in the lower region of the channel remains.
- Another object was a method for emptying such moldings, in particular with open and / or To provide complex channel or pore structures of excess used Washcoat suspension that solves the problems mentioned.
- the solution should be characterized by measures that can be easily implemented.
- the object has been inventively solved by the fact that in a first emptying step, the majority of excess liquid is removed by the action of an external force and in a second emptying step of remaining in Formkorper after the first emptying residual amount of excess liquid by contacting the Formkorpers of that End face, at which the excess was discharged in the first emptying step, is removed with a porous and / or channels bearing pad, wherein the pore and / or channel diameter of the support is less than or equal to the diameter of the inner cavities and / or channels of the Shaped body.
- the geometrical shape of the shaped body is in principle arbitrary, but it should have two substantially parallel flanges to each other.
- Cylindrical shaped bodies are preferably used.
- the shaped body used in the method according to the invention is preferably a ceramic or a metallic shaped body.
- the measure according to the invention can be used in conjunction with all known to those skilled in the art emptying measures. It can be used in conjunction with a blow-out method, with a centrifuging method as well as with the various other emptying methods.
- a special suction device as in DE 3803579 A1
- the application of a negative pressure can be dispensed with. Therefore, the automation of the discharge process by the inventive method is significantly favored.
- the inventively used porous or channels traversed support should, in order to achieve the most complete emptying, as completely as possible plane-parallel to the end face of the mold body completely. It is not absolutely necessary for the porous support used according to the invention to be in direct contact with the end face of the shaped body to be emptied. Rather, in the method according to the invention for compensating any unevenness, a flexible porosity can be achieved. se intermediate layer, in particular a flexible network can be used. In this way, a complete production of the contact between the outlet side of the molded article and the porous support used according to the invention is achieved, which lead to optimal results of the inventive method even with not completely planar end faces of molded articles and porous support to be emptied.
- An essential feature of the invention is, inter alia, the fact that the diameter of the channels or pores of the porous support used is on average less than or equal to the diameter of the inner cavities of the shaped body to be emptied, in particular the diameter of the hollow body to be emptied on the front side of the mold body to be emptied Channels or pores.
- the mean pore diameter or the individual pore cross-sectional area of the porous support calculated therefrom should therefore not be greater than the single-channel cross-sectional area or the average pore diameter at the front-outlet side of the shaped body to be emptied.
- the composition of the porous support is not bound to a specific material. It can be made of metal, ceramic, plastic or any other suitable to those skilled appear material. Combinations of various porous and / or channeled materials are also conceivable.
- the direct contact of the can be achieved according to opposite surfaces of Formkorper and support, in particular over the entire surface of the z ⁇ emptying Formkoroers.
- the diameter of the smallest pore of the overlay should not be less than the diameter of the largest particle of the coating suspension, dispersion or slurry. Otherwise, these components can no longer flow through the pores of the pad and there is a clogging of the porous pad.
- This requirement restricts the pore diameter of the porous support by means of a minimum pore diameter, which is expediently to be selected as a function of, for example, the washcoat suspension.
- a second shaped body preferably of the same type as the shaped body to be emptied, or even a second shaped body with the same or smaller channel diameter or pore diameter, based on the channel diameter, is used as porous or channel-covered support according to the invention or pore diameter of the emptied molding, used.
- the length of such a second shaped body can be significantly shorter than that of the shaped body to be emptied.
- the length or the height of the porous support used according to the invention or of the mold body used for the emptying should be at least high enough that the capillary force of the support or molded body resulting from the cross section or diameter and the pore length or channel length is capable to overcome in the Trager- or pore channels to be emptied acting capillary forces that prevent the outflow of the excess Washcoat- suspension.
- the molding article used for emptying according to the invention is 006/005001
- 11 preferably also metallic nature and has in the case of a honeycomb plane-parallel channels.
- a ceramic shaped body may also be used instead of a metallic shaped body.
- a honeycomb of the same type is used for emptying a metallic or ceramic honeycomb, the honeycomb body being emptied of the honeycomb body being emptied in the upper part in order to emptying it honeycomb to reach the front surface of the honeycomb to be emptied.
- porous overlays are open-pored sponges, nets, nonwovens (porous fleece) or comparable materials.
- the direct and complete contact of the porous support with the emptying surface of the molded body over the entire surface leads to a complete leakage of the excess washcoat in the mold.
- porous support Possible embodiments for the porous support are also combinations of a metallic or ceramic honeycomb with a fleece and / or a net and / or a sponge.
- An advantage of the inventive method is the simple technical feasibility. Furthermore, the process according to the invention effectively avoids the undesirable formation of bubbles at the channel or pore outlet side, which is often observed when using surfactant-containing coating suspensions.
- the shaped articles can first be partially emptied by means of another functional principle, in particular by suction, blowing out, centrifuging or simply flowing out.
- the abovementioned possibilities for partial emptying can also be used in combination with the emptying method according to the invention, in particular successively or simultaneously.
- the emptying process according to the invention can be used, in particular, as part of a complete coating process of moldings which are interconnected in regions and are essentially continuous through the mold body and have inner cavities.
- a method for coating a partially interconnected, substantially continuous by a mold body, having inner cavities Formkorpers, in particular a channels or pore structures having honeycomb or a porous metal foam with a washcoat suspension comprising the following steps
- step C) removing the excess of washcoat suspension remaining after step B) from the inner cavities of the shaped body to be coated by means of a porous support which is mounted on the end face of the shaped body on which the excess is to be removed mean pore diameter of the porous support less than or equal the average diameter of the channels of the molding is.
- step C) The complete removal of the excess in step C) can be used in combination with any method known to those skilled in the art for emptying such molded articles.
- the measure according to the invention according to step C) is used in connection with the application of centrifugal forces or inertial forces.
- centrifugal forces is meant those forces which are e.g. arise during acceleration or deceleration of the moldings and act on him.
- a variant of step B) may be that the partial emptying of the molded article takes place exclusively by the outflow of the excess washcoat suspension, due to its own weight, and then the emptying is carried out by the inventive emptying method using the porous support.
- steps A) and B) are carried out several times in succession before step C) is carried out.
- steps A) and B) are each run through three times in order to ensure that all channels or pores of the molded body with washcoat suspension have been completely filled at least once.
- the filling after step A) and / or the partial emptying step B) can be carried out by the action of vibrations, in order to increase the flow properties of the washcoat suspension to be aspirated or expelled.
- the steps A) and B) are already carried out in the presence of the porous support, in which case the partial emptying B) is carried out simultaneously 01
- step C) Application of the inventive emptying principle according to step C) is carried out.
- the above also applies mutatis mutandis to dispersions, slurries or solutions for the coating of the inner cavities or channels or pore structures of a molded article.
- Another object of the invention is a device used for filling and partial emptying of partially interconnected, substantially through a mold body continuous internal cavities of a molded article used apparatus (Kolbenzy- linderstrom), with the inventive coating method can be performed.
- the device according to the invention according to FIG. 2 is explained on the basis of a honeycomb body. Of course, what is said also applies to all other Formkorper such. Ceramic or metal foam.
- the device comprises a piston cylinder (a) for sucking in or emptying the washcoat suspension or dispersion, sludge or solution, a connecting plate (b) which is fixedly connected to the lower end of the piston cylinder and with the upper end side to be coated Can be tightly connected honeycomb, a receiving plate (c), which can be tightly connected on its upper side with the lower end face of the honeycomb to be coated, optionally one or more vibration units, which are fixed to the receiving plate (c), a hydraulically movable suspension ( f) with which the cylinder unit (a), the connecting plate (b) and the receiving plate (c) can be moved together horizontally (up and down movement), an intake / outlet pipe (d), on the lower side of the receiving plate ( c) and a storage trough (e) in which the washcoat suspension is presented.
- the tight connection of the honeycomb to be coated with the connecting plate (b) and the receiving plate (c) is preferred way by pressing the end faces of the honeycomb to corresponding sealing devices on the plates (b) and
- the connecting plate (b) and the receiving plate (c) are in each case in the area in which they are to receive the honeycomb to be filled, broken so that on the one hand on the KoI- benzylmder (a) a pressure or negative pressure can be established and on the other hand, the washcoat suspension can be sucked or pressed out through the suction / discharge pipe (d).
- the catalysts obtainable by the processes according to the invention can be used in particular as catalysts in the purification of exhaust gases, in particular those of internal combustion engines.
- the catalysts obtainable by the process according to the invention are, in particular, the purification of automobile and diesel exhaust gases.
- the catalysts prepared by the process according to the invention can be used as decomposition catalysts for ammonia precursor compounds, as oxidation catalysts, as catalysts for the removal of nitrogen oxides and as catalysts for the reduction of nitrogen oxides.
- washcoat suspensions consisting of support oxides or support oxide combinations selected from the group comprising TiO 2 , Al 2 O 3 , SiO 2 , CeO 2 , ZrO 2 or Zeolites, are used.
- washcoat suspensions consisting of support oxides or support oxide combinations selected from the group comprising TiO 2 , Al 2 O 3 , SiO 2 , CeO 2 , ZrO 2 or Zeolites.
- Trageroxide or Trageroxidkombinationen can in turn be doped or coated with metal oxides. It is also possible to use catalytically active compositions or compositions which directly catalytically active coatings are used directly.
- the active composition contains as additional components one or more metal oxide compounds selected from the group comprising the oxides of vanadium, tungsten, molybdenum, in particular V 2 O 5 , WO 3 , M0O 3 or noble metal salts, in particular those of palladium, platinum, Rhenium or rhodium.
- one or more metal oxide compounds selected from the group comprising the oxides of vanadium, tungsten, molybdenum, in particular V 2 O 5 , WO 3 , M0O 3 or noble metal salts, in particular those of palladium, platinum, Rhenium or rhodium.
- the catalytically active components can also be applied only in a subsequent step after the shaped body which has been coated and emptied according to the invention has been subjected to a temperature treatment.
- washcoat suspensions, dispersions or slurries which can be used in the process according to the invention may contain, in addition to inorganic carrier oxides, water, additives and catalytic active components.
- the washcoat suspensions used in the process according to the invention can be inorganic sols or gels, in particular SiO 2 , TiO 2 , Al 2 O 3, sols or gels for improving the adhesion of the resulting coating, additives such as organic mono- and polymers, in particular cellulose derivatives or acrylates as pore formers as well as adhesion promoters and / or surfactants as rheological aids.
- Moldings made of materials selected from the group consisting of cordierite, silicates, zeolites, silicon dioxide, silicon carbide, aluminum oxide and aluminates or mixtures of these substances are particularly suitable for the moldings to be emptied or coated by the novel processes as well as metals or metal alloys. Particularly preferred are metallic support structures.
- metal shaped bodies particularly preferred are complex-structured metal carriers and metal foams.
- ceramic honeycomb or Keramikschaume are used.
- the metal or Keramikformkorper used according to the invention can be pretreated by a thermal or chemical process in such a way that a later applied layer is improved in their adhesion. With the method according to the invention, molded articles with a high to very high cell or pore density can also be emptied.
- the catalysts prepared in this way can still undergo a drying step and subsequent calcining step.
- the further application of catalytically active compounds, such as noble metal compounds, is possible.
- the catalysts prepared in this way are used especially in gas purification processes, in particular in the purification of automobile exhaust gases. However, they can also be used in other catalytic processes, such as in the chemical industry or power generation.
- the present invention relates to a process for coating catalyst supports by means of a charging step of a support body which [Def. Al] on the outside with a washcoat suspension and a subsequent emptying step to remove the excess washcoat suspension.
- the filled or partially filled mold body with its outlet end face is brought into contact with a porous support, with the proviso that the average pore diameter or the calculated individual pore cross-sectional area of the support is not greater than the single cross-sectional area of a representative one Ka nal or pore channels at the front exit side of the catalyst carrier.
- the catalyst supports coated in this way can be used as supported catalysts, in particular for the purification of automobile exhaust gases.
- Figure 1 is an illustration of the air flow (arrows) for blowing out the excess washcoat suspension in open structures.
- the illustration shows two adjacent channels connected by perforations as a section of a honeycomb body.
- the air flow in the perforated channels follows that of the lowest pressure loss, after which, in such a case, a complete emptying of all channels becomes impossible due to the sole blowing out.
- the excess washcoat suspension is held in the channels by the capillary forces.
- FIG. 2 is a schematic representation of a piston-cylinder system according to the invention.
- Fig. 3 shows a honeycomb immediately after removal from the Kozy- benzylinderstrom according to Comparative Example 3.
- the channels are on the side of the exit surface (lower end face) still completely filled with excess washcoat suspension.
- FIG. 5a shows the view of a honeycomb to be coated, which is subsequently to be freed of excess washcoat (top) with attached second auxiliary honeycomb or support honeycomb (below) for the purpose of complete emptying according to Example 4.
- FIG. 5b shows a detailed view of the attachable auxiliary or supporting honeycomb according to example 4, wherein it can be seen that to ensure full coverage of the lower exit surface of the honeycomb to be emptied (not shown) with the upper end surface of the auxiliary honeycomb a small part of the honeycomb envelope Abrasion was removed.
- FIG. 6 is a view of the lower exit surface of a coated honeycomb completely freed from excess washcoat according to Example 4.
- FIG. 7 is a view of the lower exit surface of a honeycomb exclusively treated by centrifugation according to Comparative Example 5 without the use of an auxiliary honeycomb.
- Fig. 8 is a view of the lower exit surface of a honeycomb treated according to Example 6 by centrifugation in the presence of an auxiliary honeycomb.
- Fig. 9 is a view of the lower exit surface of a honeycomb treated according to Example 7 (blowout), whereby channels are not completely empty due to incomplete abutment of the auxiliary honeycomb over the entire surface of the exit surface of the honeycomb to be liberated by excess washcoat.
- FIG 10 is a view of the lower exit surface of a honeycomb treated according to Example 8, wherein the unevenness on the upper end side of the auxiliary honeycomb, which prevent a complete plane-parallel resting of the auxiliary honeycomb over the entire exit surface, by introducing a flexible network between the exit surface of the excess washcoat to be liberated honeycomb and the upper end surface of the auxiliary honeycomb be compensated.
- Example 1 Preparation of a typical washcoat suspension
- the plant consists essentially of a piston cylinder (a) for sucking or emptying the washcoat suspension, a connecting plate (b), which is connected at the lower end of the suction fixed to the suction cylinder and which is dimensioned in its underside so that exactly the upper end side of the honeycomb with the suction cylinder by pressing a receiving plate (c) can be tightly connected.
- a receiving plate c
- one or more vibration units can be attached to the receiving plate (c).
- This fixture (plates (c) and (b)) can move together with the cylinder unit (a) hydraulically up and down over the suspension (f).
- the pilot plant is supplemented by a storage tank (e), in which the washcoat suspension is filled.
- the washcoat suspension from Example 1 is in the storage tank
- the honeycomb is sealed into the holding device comprising the plates (b) and (c) by hydraulically pressing the honeycomb receiving plate (c) onto the connecting plate (b), and the piston-cylinder unit (a) together with the holding device comprising the plates (b ) and (c) hydraulically downwards over the suspension (f) so that the immersion tube (d) dips into the washcoat suspension.
- the cylinder piston (a) also hydraulically is moved upwards, whereby the washcoat suspension is sucked into the honeycomb via the suction pipe (d).
- the piston stroke is adjusted so that the washcoat suspension is sucked in at least to the extent that the upper end surface of the honeycomb is completely covered.
- a large part of the excess washcoat suspension is printed out again into the storage trough (e). This process is repeated at least twice, which ensures that all channels have been fully filled (flooded) at least once.
- the piston After three pumping and printing operations, the piston is held down for one minute after the last printing operation. Thereafter, the cylinder piston (a) together with the holding device comprising the plates (b) and (c) pneumatically over the suspension (f) moves back up, and finally the outlet pipe (d) is no longer immersed in the washcoat suspension.
- the honeycomb can be removed after appropriate pressure relief (relax the hydraulic system on the holding device) for further processing (emptying).
- a complex structured metal honeycomb with mixer function (from Emitec, Type:. MI) cm with a length of 7.5, a diameter of 7 cm and a cell density of 200 cpsi is pretreated h at 750 0 C in a calcining furnace under air atmosphere thermally. 4
- the cooled to room temperature honeycomb is then filled by the procedure described in Example 2.2. Thereafter, the test swab was removed.
- Fig. 3 the lower end side of the experimental honeycomb is shown. It can be clearly seen that the entire lower end surface of the honeycomb is still covered with washcoat suspension.
- Example 6 Coating of a Metallic Carrier Body with Mixing Function Using a Vibrating Unit and a Subsequent Centrifugation Step Using a Porous Pad
- Example 4 The experiment described in Example 4 is repeated, with the difference that the mutually facing surfaces of the honeycomb to be emptied and the auxiliary honeycomb (support honeycomb) had no complete, over the entire exit surface extending contact. This is provoked by the deliberate use of a honeycomb with a not quite planar frontal surface.
- FIG. 9 shows the exit side of the experimental honeycomb after the coating test. Even a small disturbance of the flat contact leads to an incomplete emptying and thus partial blockage of the channels.
- Example 8 Coating of a metallic carrier body with mixer function using a vibration unit and a combination of honeycomb and mesh as porous support
- Example 7 The experiment described in Example 7 is repeated, with the difference that between the opposite not completely plane-parallel surfaces additionally a layer of a flexible network (thread thickness: 0.3 mm, mesh size: 1.2 mm * 1.2 mm) placed becomes.
- all channels were now free of washcoat suspension after the coating process in the honeycomb to be coated and emptied (to be liberated from excess washcoat) (FIG. 10).
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Abstract
Description
Claims
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US11/915,368 US20080200328A1 (en) | 2005-05-25 | 2006-05-24 | Method and Device For Applying Washcoat Suspensions to a Molded Article |
EP06753870A EP1885495A2 (de) | 2005-05-25 | 2006-05-24 | Verfahren und vorrichtung zum auftragen von washcoat-suspensionen auf einen formkörper |
CA002605289A CA2605289A1 (en) | 2005-05-25 | 2006-05-24 | Method and device for applying washcoat suspensions to a molded article |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102005024124.7 | 2005-05-25 | ||
DE102005024124A DE102005024124A1 (de) | 2005-05-25 | 2005-05-25 | Verfahren und Vorrichtung zum Auftragen von Washcoat-Suspensionen auf einen Wabenkörper und deren Verwendung |
Publications (2)
Publication Number | Publication Date |
---|---|
WO2006125649A2 true WO2006125649A2 (de) | 2006-11-30 |
WO2006125649A3 WO2006125649A3 (de) | 2007-04-26 |
Family
ID=36658665
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/EP2006/005001 WO2006125649A2 (de) | 2005-05-25 | 2006-05-24 | Verfahren und vorrichtung zum auftragen von washcoat-suspensionen auf einen formkörper |
Country Status (5)
Country | Link |
---|---|
US (1) | US20080200328A1 (de) |
EP (1) | EP1885495A2 (de) |
CA (1) | CA2605289A1 (de) |
DE (1) | DE102005024124A1 (de) |
WO (1) | WO2006125649A2 (de) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7951338B2 (en) | 2006-03-24 | 2011-05-31 | Ngk Insulators, Ltd. | Catalytic converter |
US8491966B2 (en) * | 2007-03-19 | 2013-07-23 | Umicore Ag & Co. Kg | Method for introducing a catalytic coating into the pores of a ceramic honeycomb flow body |
Families Citing this family (16)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2006098210A1 (ja) * | 2005-03-15 | 2006-09-21 | Ihi Corporation | 保護コート及び金属構造体 |
JP2007296514A (ja) * | 2006-04-07 | 2007-11-15 | Ngk Insulators Ltd | 触媒体とその製造方法 |
DE102006027700A1 (de) * | 2006-06-14 | 2007-12-20 | Süd-Chemie AG | Vorrichtung und Verfahren zum Beschichten von Trägern mit katalytisch aktiven Materialien |
US8006637B2 (en) * | 2007-03-29 | 2011-08-30 | Corning Incorporated | Method and apparatus for membrane deposition |
DE102008046994B4 (de) | 2008-09-12 | 2015-02-12 | Süd-Chemie Ip Gmbh & Co. Kg | Harnstoff-Hydrolyse-Katalysator |
DE102009056145B3 (de) | 2009-11-27 | 2011-07-28 | Süd-Chemie AG, 80333 | Beschichtungssuspension zur Beschichtung von Katalysatorsubstraten |
WO2011080198A2 (en) * | 2009-12-29 | 2011-07-07 | Shell Internationale Research Maatschappij B.V. | Coating method for structured catalysts |
US20110160048A1 (en) * | 2009-12-29 | 2011-06-30 | Boumendjel Nariman | Coating method for structured catalysts |
EP2341120A1 (de) * | 2009-12-29 | 2011-07-06 | Shell Internationale Research Maatschappij B.V. | Beschichtungsverfahren für strukturierte Katalysatoren |
GB201000019D0 (en) | 2010-01-04 | 2010-02-17 | Johnson Matthey Plc | Coating a monolith substrate with catalyst component |
DE102010007499A1 (de) | 2010-02-09 | 2011-08-11 | Umicore AG & Co. KG, 63457 | Volumetrische Beschichtungsanordnung |
US9096923B2 (en) * | 2011-11-10 | 2015-08-04 | Corning Incorporated | Coating apparatus and method for forming a coating layer on monolith substrates |
CN105073223A (zh) | 2013-02-27 | 2015-11-18 | 康明斯排放处理公司 | 用于固定催化剂基板的物品 |
GB201311615D0 (en) * | 2013-06-03 | 2013-08-14 | Johnson Matthey Plc | Method of coating a substrate with a catalyst component |
US20210220813A1 (en) * | 2020-01-16 | 2021-07-22 | Johnson Matthey Public Limited Company | Pallet for supporting a catalyst monolith during coating |
GB202110212D0 (en) * | 2021-07-15 | 2021-09-01 | Microtech Ceramics Ltd | Washcoat method |
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- 2006-05-24 WO PCT/EP2006/005001 patent/WO2006125649A2/de not_active Application Discontinuation
- 2006-05-24 CA CA002605289A patent/CA2605289A1/en not_active Abandoned
- 2006-05-24 EP EP06753870A patent/EP1885495A2/de not_active Withdrawn
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US8491966B2 (en) * | 2007-03-19 | 2013-07-23 | Umicore Ag & Co. Kg | Method for introducing a catalytic coating into the pores of a ceramic honeycomb flow body |
Also Published As
Publication number | Publication date |
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DE102005024124A1 (de) | 2006-11-30 |
US20080200328A1 (en) | 2008-08-21 |
CA2605289A1 (en) | 2006-11-30 |
EP1885495A2 (de) | 2008-02-13 |
WO2006125649A3 (de) | 2007-04-26 |
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