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    • 专利摘要:
    “METHOD FOR COATING A FILTER SUBSTRATE UNDERSTANDING A PLANNING OF CHANNELS” A method for coating a filter substrate comprising a plurality of channels and an apparatus for them. The method comprises the steps of: (a) introducing a predetermined amount of a liquid into a containment medium at an upper end of the filter substrate; and (b) coating the channels having open ends at the upper end of the filter substrate with the liquid from the containment medium.
    公开号:BR112016021820B1
    申请号:R112016021820-5
    申请日:2015-03-24
    公开日:2021-01-05
    发明作者:Kaneshalingham ARULRAJ；Jenita Bhantoo；Jamie Savage；Andrew Smith；LiFeng Wang；Daisuke Yokota
    申请人:Johnson Matthey Public Limited Company；
    IPC主号:
    专利说明:

    FIELD OF INVENTION
    [001] The invention relates to a method for coating a filter substrate. The invention further provides an apparatus for coating a filter substrate. BACKGROUND OF THE INVENTION
    [002] A large number of emission control devices comprising coated filter substrates are manufactured each year. One of the main uses of such devices is for the filtration of particulate matter (PM), such as soot, produced by an internal combustion engine, particularly an internal combustion engine for vehicles. Emission control devices that comprise coated filter substrates are commonly used to remove MP produced by compression ignition engines, such as diesel engines. However, as environmental legislation is becoming more and more stringent, there is also a focus of interest in removing nanoparticles generated by gasoline engines.
    [003] One of the challenges in the manufacture of coated filter substrates concerns the application of a uniform coating on the walls of the filter substrate channels. This is due to the fact that each channel of a filter substrate generally has only one end open (the other end being closed, usually by obstruction), which is problematic for the application of a washable coating. It can be difficult to apply a washable coating to the channels of a filter substrate to obtain a desired coating depth, a regular coating depth in all distribution channels and a uniform washable coating within each channel.
    [004] A method that shows good results for uniformly applying the washable coating on the walls of a filter substrate is described in WO 2011/080525. WO 2011/080525 describes a method for coating a monolith substrate in honeycomb configuration comprising a plurality of channels with a liquid comprising a catalyst component, the method of which comprises the steps of: (i) securing a monolith substrate in honeycomb configuration substantially vertical; ii) introducing a predetermined volume of liquid into the substrate through open ends of the channels at a lower end of the substrate; (iii) hermetically retain the liquid introduced into the substrate; (iv) invert the substrate containing the retained liquid; and (v) applying a vacuum to open the ends of the substrate channels at the inverted, lower end of the substrate to remove the liquid along the channels of the substrate.
    [005] However, the method described in WO 2011/080525 can be inconvenient for certain applications. This method may not allow the location of the washable coating coating on the substrate wall (for example, wall covering or on the wall) to be easily controlled, and it may be necessary to use a washable coating with a viscosity within a specific range .
    [006] WO 99/47260 describes a general method for coating a monolithic support. A method for coating a substrate in a cellular flow configuration is exemplified in WO 99/47260. This method is typically used to apply a washable coating with a relatively high viscosity. SUMMARY OF THE INVENTION
    [007] The inventors have developed a method and apparatus for automatically and uniformly coating a filter substrate. In particular, the method allows the location of the washable coating lining on the channel walls of the filter substrate to be controlled and has short cycle times. The method also allows the amount of active material (for example, in the washable coating) that is coated on a filter substrate to be precisely controlled. This is important because the active material generally comprises a precious metal, which is expensive. It may also be possible, using the method and apparatus of the invention for the washable coating formulation to be applied directly to a filter substrate, without changing its viscosity.
    [008] The invention generally relates to a method for coating a filter substrate comprising a plurality of channels, the method of which comprises the steps of: (A) introducing a predetermined amount of a liquid into a containment medium at an upper end of the filter substrate; and (B) coating the channels having open ends at the upper end of the filter substrate with the liquid, preferably the predetermined amount of the liquid, from the containment medium.
    [009] The location of the containment medium at an upper end of the substrate filter means that the coating of the channels with the liquid is assisted by gravity. Step (b) may comprise coating the channels having open ends at the upper end of the filter substrate with the liquid from the containment medium, allowing the liquid to enter and / or fill the channels by gravity.
    [0010] An apparatus is also provided by the invention for coating a substrate with a liquid filter, which device comprises: (I) a containment means means for receiving a predetermined amount of the liquid; and (II) a liquid dosing head arranged to dispense the predetermined amount of liquid into the containment medium along an upper end of the filter substrate; wherein the containment means is located at an upper end of the filter substrate, and the liquid dosing head comprises a plurality of holes for dispensing liquid over the upper end of the filter substrate.
    [0011] The walls of the filter substrate channels comprise a porous material, which provides a barrier to particulate material (MP), but allows gases to flow through. It was possible to apply the washable coating first to the surface of the channel walls (i.e., substantial or complete "on the coating" wall) and form a membrane-like coating. Alternatively, most or all of the washable liner can be designed or forced into the porous material on the channel walls (i.e., substantial or complete "on the liner wall").
    [0012] When preparing a filter substrate with a wall covering, it is to be understood that in many cases, despite the majority of the washable coating (eg> 50% of the total mass of all catalyst components ) can form a coating on the wall, some of the washable coating will enter the filter substrate wall and form a coating on the wall. Likewise, when preparing a substrate with a filter liner on the wall, a part of the washable liner can remain as a liner on the wall, even though most of the washable liner forms a liner on the wall (for example,> 50% of the total mass of all components of the catalyst).
    [0013] It is advantageous to be able to control the location of the washable coating on the channel walls because the location of the washable coating can affect the back pressure of the filter substrate that is generated in use. The components of an exhaust gas that are brought into contact with the washable coating and the chemical reactions that will be performed by the active constituents of the washable coating can also be influenced by their location on the filter substrate.
    [0014] The invention can allow the filter substrate to be precisely coated to a desired coating depth (e.g. coating desired length along the length of the channels). The invention can also be used to coat the entire length of the channels, or just a small length (e.g., substrate face coating). When a coating is applied to a length of the part of the channels at both ends of the substrate, then the length of a coating on a channel (for example, an input channel) can overlap with a length of a coating on an adjacent channel (for example, a channel socket), the liners being separated by a wall of the substrate. The invention can allow good control over the amount of overlap between the coated ends.
    [0015] The method of the invention relates to the coating of a filter substrate, using a washable coating with a relatively low viscosity. Similar methods in the art generally require the use of a washable coating with a high viscosity to obtain a uniform coating depth. This is because a washable coating with a high viscosity can be dispensed evenly on the upper end of the substrate before it is pulled into the small openings of the channels in the substrate by means of a vacuum. A disadvantage of using high viscosity washable coatings in such methods is that it can be difficult to obtain a uniform coating depth for substrates with a large diameter.
    [0016] Surprisingly, it has been found that a uniform coating depth can be obtained using a low viscosity washable coating when the substrate is a filter substrate, particularly when the substrate has a relatively large diameter. Low viscosity washable coatings are advantageous because they are easier to process, require less time than to prepare high viscosity washable coatings, reduce batch-to-batch variability in the properties of the washable coating, and eliminate or reduce changes in the properties of the washable coating on aging.
    [0017] There are several aspects of the invention. A first aspect of the invention includes a first aspect of the method and a first aspect of the apparatus.
    [0018] A first aspect of the method of the invention relates to a method for coating a filter substrate comprising a plurality of channels, the method of which comprises the steps of:
    [0019] (A) introducing a predetermined amount of a liquid into a containment medium at an upper end of the filter substrate; and
    [0020] (B) applying a vacuum to a lower end of the filter substrate.
    [0021] In the first aspect of the method of the invention, the general step (b) coating the channels having open ends at the upper end of the filter substrate with the liquid from the containment means comprises, or is, the application of a vacuum to a lower end of the filter substrate.
    [0022] Typically, in the first aspect of the method, step (b) is generally a step of (b) applying a vacuum to a lower end of the filter substrate to withdraw the liquid from the containment medium along of the channels, having open ends at the upper end of the filter substrate (thus covering the channels).
    [0023] A first aspect of the apparatus of the present invention relates to an apparatus for coating a substrate with a liquid filter, which apparatus comprises: (I) a containment means means for receiving a predetermined amount of the liquid; (II) a liquid dosing head arranged to dispense the predetermined amount of liquid into the containment medium along an upper end of the filter substrate; and (III) means for applying a vacuum to a lower end of the filter substrate; wherein the containment means is located at an upper end of the filter substrate, and the liquid dosing head comprises a plurality of holes for dispensing liquid over the upper end of the filter substrate.
    [0024] The first aspect of the invention can be used to coat the channel wall of a filter substrate with the liquid. The step of applying the vacuum to a lower end of the filter substrate pulls the liquid into the walls of the substrate channels, which are made of a porous material.
    [0025] The invention also has a second aspect, which includes a second aspect of the method.
    [0026] A second aspect of the invention provides a method for coating a filter substrate comprising a plurality of channels, the method of which comprises the steps of: (A) introducing a predetermined amount of a liquid into a containment medium in an upper end of the filter substrate; and (B) draining the liquid from the containment medium to the filter substrate.
    [0027] In the second aspect of the method of the invention, the general step (b) coating the channels having open ends at the upper end of the filter substrate with the liquid from the containment medium comprises, or is, draining the liquid from the medium containment for the filter substrate.
    [0028] In the second aspect of the method, step (b) is generally a step of (b) draining the liquid from the containment medium into the channels that have open ends at the upper end of the filter substrate (coat so the channels).
    [0029] The second aspect of the invention can be used to coat the wall of the channels of a filter substrate with the liquid. The step of draining the liquid from the containment medium to the filter substrate allows the liquid to form a coating (for example membrane-like coating) on the surface of the substrate channel walls. BRIEF DESCRIPTION OF THE DRAWINGS
    [0030] Figure 1 shows a cross section of an apparatus according to the invention. The apparatus can be used to carry out a method of the invention. The apparatus comprises a washing head (1) which is used to deposit a washable coating (5) on a filter substrate (4) into the space defined by the wall (2) and the upper end face of the substrate (4) of the filter. A vacuum can be applied to the lower end of the filter substrate using a vacuum cone (3). DETAILED DESCRIPTION OF THE INVENTION
    [0031] The invention relates specifically to the coating of filter substrates with a liquid. A filter substrate has a different structure to a flow substrate.
    [0032] A flow substrate generally comprises a plurality of channels, generally extending through it, where each channel is open at both ends (i.e., an open end at the inlet part and an open end at the outlet). The channels are formed between a plurality of walls. The walls generally comprise a non-porous material.
    [0033] In contrast, a filter substrate comprises a plurality of channels, each channel having an open end and a closed end (e.g., a blocked or closed end). Each channel is typically separated from an adjacent or neighboring channel by a wall. The wall comprises, or consists essentially of, a porous material. Such porous materials are well known in the art.
    [0034] In general, a filter substrate comprises a plurality of air inlet channels and a plurality of outlet channels. Each input channel has an open end at a first end of the substrate and a closed end (for example, blocked or attached) end to a second end of the substrate (i.e., the second end represents the end opposite the first end), and each The outlet channel has a closed end (e.g., blocked or attached) at the first end of the substrate and an open end at the second end of the substrate.
    [0035] On a filter substrate, each channel has an open end at a first end of the substrate and an end closed at a second (i.e., opposite) end of the substrate is usually adjacent to a channel that has a closed end at the first end of the substrate and an open end at the second (i.e., opposite) end of the substrate. The communication of the fluid between the channels is through a wall (for example, through the porous material) of the substrate.
    [0036] The wall is typically 0.002 to 0.1 inch (0.05-2.54 mm) thick, such as 0.005 to 0.050 inch (0.12-1.27 mm), particularly 0.010 to 0.025 inches (0.25 to 0.64 mm).
    [0037] Typically, the channels of a filter substrate have alternately closed (for example blocked or closed) and open ends. Thus, each input channel can be adjacent to an output channel, and each output channel can be adjacent to an input channel. When viewed from each end of the filter substrate, the channels can look like a chessboard.
    [0038] However, the filter substrate can have an input channel (i.e., a "first" input channel) that is adjacent to another input channel (i.e., a "second" input channel) and, optionally, for an output channel, such as the "first" output channel and / or the "second" output channel. The filter substrate can have an outlet channel (ie, a "first" outlet channel), which is adjacent to another outlet channel (ie, a "second" outlet "channel) and, optionally, for a input channel, such as the "first" input channel and / or the "second" input channel.
    [0039] The filter substrate can have from 100 to 700 cells (or "channels") per square inch ("CPSI"), particularly 250 to 400 CPSI.
    [0040] The liquid can be a solution or a suspension. The suspension can be a colloidal suspension, such as a sol, or a non-colloidal suspension. When the liquid is a solution or a suspension, then it can be an aqueous solution or an aqueous suspension. Usually, the liquid is a suspension, particularly an aqueous suspension.
    [0041] The term "liquid" as used herein is synonymous with the term "washable coating".
    [0042] Typically, the liquid comprises a catalyst component. The term "catalyst component" encompasses any component that can be included in a washable coating formulation that contributes to the resulting emission control device activity, such as a platinum group metal (PGM), a support material (for example, refractory oxide) or a zeolite. It is to be understood that the term "catalyst component" does not require that the component itself has a catalytic activity, in the strict sense of the meaning of the term "catalyst" (for example, increasing the speed of the reaction). For example, the catalyst component can refer to a material that is capable of storing or absorbing NOx or a hydrocarbon. Liquids comprising a catalyst component are known to those skilled in the art. The catalyst component (s) included in the liquid will depend on the product that is to be manufactured.
    [0043] The coated filter substrate or product obtained by a method of the invention or using an apparatus of the invention can, for example, be a filter substrate, comprising an oxidation catalyst (for example, a catalyzed soot filter [CSF ]), a selective catalytic reduction (SCR) catalyst (for example, the product can then be called a selective catalytic reduction filter [SCRF] catalyst), an adsorbent NOx composition (for example, the product can then be called a lean NOx trap filter [LNTF]), a three-way catalyst composition (eg the product can then be called a gasoline particle filter [GPF]), a slip ammonia catalyst [ASC] or a combination of two or more of them (for example, a filter substrate comprising a selective SCR (catalytic reduction) catalyst and a slip ammonia catalyst [ASC]).
    [0044] In addition to the "catalyst component", the liquid can also comprise a formulation aid. The term "aid formulation" refers to a component that is included in the liquid to modify its physical or chemical properties for coating on a filter substrate. The formulation aid can, for example, help the dispersion of a catalytic component in the liquid or change the viscosity of the liquid. The formulation aid may not be present in the final product coated filter substrate (for example, it may decompose or degrade during calcination). The formulation aid can, for example, be an acid, a base, a thickening agent (for example, thickening organic compound) or a binder.
    [0045] It is to be understood that the type of coating (for example, on the wall or the wall) that is obtained will depend on a variety of factors, such as the viscosity of the liquid, the porosity of the filter substrate (that is, the porosity of the porous material that forms the walls of the filter substrate) and the particle size distribution of the solids dispersed in the liquid. The process conditions also affect the type of coating that is obtained. However, in general, the first aspect of the invention is able to provide substantial coating on the wall of a filter substrate and the second aspect of the invention is able to provide substantial coating on the wall of a filter substrate.
    [0046] Using the present invention, liquid coating filter substrates (e.g. washable coatings) having relatively low viscosities have been successfully achieved.
    [0047] Typically, the liquid may have a viscosity <600 cP (as measured at 20 ° C on a Brookfield RV DVII + Extra Pro viscometer using a SC4-27 spindle at 50 rpm spindle speed).
    [0048] Generally, the liquid has a viscosity of 5 cP to 600 cP, such as 10 cP and 600 cP (measured at 20 ° C on a Brookfield RV DVII + Extra Pro viscometer using a SC4-27 spindle at 50 rpm speed spindle). Thus, the liquid can have a viscosity of 10 to 500 cP, such as 15-250 cP (e.g., 50 to 200 cP) and, preferably, 20 to 50 cP.
    [0049] For example, the liquid may have a viscosity <500 cP (at a shear rate of 20 s-1 [as measured at 20 ° C on a Brookfield LV DVII + Pro viscometer using a SC4-27 spindle]). The liquid can have a viscosity of 10 to 500 cP, preferably 25 to 400 cP, and more preferably 50 to 200 cP.
    [0050] The liquid may have a viscosity <80 cP (at a shear rate of 66 s-1 [as measured at 20 ° C on a Brookfield LV DVII + Pro viscometer using a SC4-27 spindle]).
    [0051] It may be preferable, particularly in the second aspect of the invention, that the liquid has a viscosity between 5 and 100 cP, such as 10 to 100 cP, particularly 20 to 90 cP, preferably 25 to 80 cP, and even more preferably 35 at 65 cP (measured at 20 ° C on a Brookfield RV DVII + Extra Pro viscometer using a SC4-27 spindle at 50 rpm spindle speed).
    [0052] The liquid used in the first aspect of the invention may have a higher viscosity than the liquid used in the second aspect of the invention.
    [0053] The liquid in the second aspect has a viscosity that allows the liquid to gradually drain under gravity into the filter substrate.
    [0054] Generally, the liquid, particularly in the second aspect of the present invention, cannot comprise a thickener. In many cases, it is not necessary to modify the viscosity of the liquid for use in the second aspect of the invention.
    [0055] In general, the invention involves introducing a predetermined amount of a liquid into a containment medium at an upper end of the filter substrate. The upper end of the filter substrate is preferably an upper end face of the filter substrate.
    [0056] The predetermined value can be a predetermined volume and / or a predetermined mass of the liquid. It is preferred that the predetermined amount is a predetermined volume.
    [0057] Typically, the predetermined amount is a single dose of the liquid.
    [0058] Step (a) of the method of the invention can, in general, be a step of (a) introducing a predetermined amount of a liquid into a containment medium at an upper end of the substrate filter using a head dosing liquid. Typically, the liquid metering head is arranged to dispense the predetermined amount of liquid into the containment medium for the upper end of the filter substrate.
    [0059] It is preferred that step (a) is a step of (a) depositing a predetermined amount of a liquid within a containment medium at an upper end of the filter substrate, more preferably using a liquid metering head.
    [0060] Generally, the liquid metering head comprises a plurality of orifices for dispensing, preferably depositing, the liquid at the upper end of the filter substrate. The plurality of orifices are preferably arranged to dispense or deposit the liquid on the upper end face of the filter substrate. More preferably, the plurality of holes are arranged to deposit the liquid evenly on the upper end face of the filter substrate.
    [0061] The liquid dosing head can be a washing head. The wash head, particularly for the second aspect of the invention, must be able to dispense the liquid evenly over the upper end face of the filter substrate without dripping (for example, when the liquid has a low viscosity) or without blocking (for example, example, when the liquid has a high viscosity).
    [0062] When the liquid dosing head or the washing head comprises a plurality of holes arranged so as to deposit the liquid uniformly on the upper end face of the filter substrate, then preferably the plurality of holes is one plurality of circular holes, more preferably the plurality of circular holes have the same diameter (for example, the circular holes have the same diameter). It may be necessary to use a liquid dosing head having holes with several different diameters (as can be used with washable high viscosity coatings) to obtain a uniform coating depth.
    [0063] In general, the plurality of holes for depositing the liquid evenly on the upper end face of the filter substrate may be the only holes in the liquid dosing head or washing head for the deposition of the liquid on the face of upper end of the filter.
    [0064] Typically, the liquid dosing head is coupled to a liquid dispenser. The liquid dispenser can be manipulated using generally known principles. For example, there are commercially available machines capable of high-precision dosing by volume or by weight of liquids, for example used for filling in the food or painting industry. These machines are capable of handling liquids of many different viscosities and rheologies.
    [0065] The liquid dispenser is capable of dispensing a predetermined amount of the liquid, preferably from a container (for example, a vessel to contain a larger or larger volume of the liquid). The container can be shaken and will be replaced over time. Since the device provides accurately measured values and no liquid recycling takes place, the quality and composition of the liquid remains constant, and losses are reduced.
    [0066] An additional feature of the invention relates to the introduction of a predetermined amount of the liquid into a containment medium at an upper end of the filter substrate. The containment means is generally located on an upper end of the filter substrate (i.e., the filter substrate to be coated), preferably on an upper end face of the filter substrate.
    [0067] The containment means is to contain and / or locate the liquid at an upper end of the filter substrate, preferably an upper end face of the filter substrate. The containment means is for containing and / or locating the liquid on either the entire upper end face of the filter substrate or part of the upper end face of the filter substrate.
    [0068] Typically, the containment means is to contain and / or locate the liquid on substantially all or all of the upper end face of the filter substrate. The term "substantially all" in the present context refers to at least 95% of the surface area of the upper end face of the filter substrate, preferably at least 99% of the surface is of the upper end face of the filter substrate.
    [0069] When the containment medium is to contain and / or locate the liquid on the upper end face part of the filter substrate, then the containment medium may comprise a model for covering an area or areas of the upper end face of the filter substrate. The model is to prevent the liquid from seeping into an area or areas of the upper end face of the filter substrate and thereby prevent the liquid from entering any channels having open ends in the area or areas. The template is molded to cover or blank outside an area or areas of the upper end face of the filter substrate. This allows the manufacture of filter substrates, where, for example, a circumferential portion of the channels are not coated with the liquid substrates or filter that has portions coated with washable coatings of a different composition and / or concentration of different components.
    [0070] The model can be located on an upper end face of the filter substrate. The model is preferably contacted with an upper end face of the filter substrate.
    [0071] The containment means typically comprises a housing for receiving an upper end of the filter substrate. Not all filter substrates have a conventional circular cross-section, and some may have an oval or "race track" shape, sloping oval or other asymmetric cross section. Whatever the cross-section of the filter substrate, it is possible to adopt a box with the appropriate shape to receive the filter substrate, using conventional methods and techniques.
    [0072] Typically, the containment means or the housing thereof, comprises a wall or a plurality of walls. The wall or walls is / are contactable with, or arranged to contact, an upper end of the filter substrate, preferably an upper end face of the filter substrate, more preferably a circumferential edge of an upper end face of the substrate of the filter. The wall or walls provide a barrier that prevents liquid from seeping from the upper end face of the filter substrate and within an outer lateral surface of the filter substrate.
    [0073] The wall or walls can generally correspond to (for example in accordance with or be moldable with) the shape of the filter substrate cross section in the axial plane (ie, the transverse plane, as seen from a face of end of the filter substrate).
    [0074] The wall can be manufactured from conventional materials. For example, the wall may comprise a plastic material (for example polypropylene or PTFE), a metal (for example stainless steel or stainless steel coated with PTFE), or a ceramic. Combinations of different materials can be used.
    [0075] It is preferred that the containment means comprises a sealing means. The sealing means are intended to prevent liquid from seeping from the upper end face of the filter substrate and into an outer lateral surface of the filter substrate, such as when a vacuum is applied. The housing of the retainer or the wall or walls may comprise the sealing means.
    [0076] The sealing means may comprise, or consist of, a deformable, permeable base or, at least, an inflatable collar. It is preferred that the sealing means comprises at least one inflatable collar.
    [0077] The or each inflatable collar is normally contactable (that is, arranged to contact) and / or to engage (that is, arranged to engage) with an outer surface of the substrate, preferably an outer surface at the upper end of the substrate .
    [0078] The or each inflatable collar can be arranged to contact and / or interact with the outer surface of the filter substrate in a horizontal plane (ie, the axial plane). The inflatable collar or inflatable collars can be arranged to contact and / or engage with the part of or to completely surround the outer surface of the filter substrate in the horizontal plane (for example, an outer surface on one side of the substrate). For example, when the filter substrate has a circular cross section (for example, in the axial plane), then the inflatable collar or inflatable collars can be arranged to contact and / or engage with an arcuate portion or an entire circumference of the surface. outside of the filter substrate in the horizontal plane. It is preferred that the inflatable collar or inflatable collars are / are arranged to contact and / or interact with an entire circumferential length of an outer surface of the filter substrate.
    [0079] Typically, the or each inflatable collar is conformable, with an outer surface of the substrate. The or each inflatable collar can form a liquid or air tight seal around the filter substrate. The inflatable collar allows the device to accommodate variations in the filter diameter or circumference substrate. If all channels that have an open end at the top end of the filter substrate are being coated, it may not be possible to make a seal with a top end face of the filter substrate. In this way a suitable seal can be provided against an outer side at an upper end of the substrate filter to allow the liquid to be distributed over the entire upper end face of the filter substrate.
    [0080] It is preferred that the sealing means comprises only one inflatable collar or at least two inflatable collars (preferably only two inflatable collars), where each inflatable collar is for contacting and / or interacting with an outer surface of the substrate, more preferably an outer surface at the upper end of the substrate.
    [0081] The or each inflatable collar can be supported by the enclosure (for example, supported by an inner wall of the box) and preferably extends into an interior space of the housing.
    [0082] The containment means may comprise a permeable base to form a container or receptacle for the liquid. The permeable base can adjoin the wall or walls of the containment medium. The permeable base allows the liquid to be transferred to an upper end face of the filter substrate. The base or permeable part of it can be movable in the manner of a guillotine, iris or plug. The permeable base may be a perforated metal plate, a porous metal plate, a sintered metal sponge, a fabric, a nonwoven fabric or a synthetic open cell foam.
    [0083] In general, step (a) of the method of the invention may comprise the steps of: (a1) locating a containment medium at an upper end of a filter substrate, and then (A2) introducing a predetermined amount of a liquid into the containment medium (ie, at the upper end of the filter substrate). Step (a) of the method preferably comprises the steps of (ao) securing a vertical filter substrate, more preferably, holding a filter substrate vertically at a lower end of the filter substrate, (A1) the location of a containment means at an upper end of a filter substrate, and then (A2) introducing a predetermined amount of a liquid into the containment means (i.e., at the upper end of the filter substrate).
    [0084] The apparatus of the invention may further comprise a means for maintaining the substrate or a substrate support.
    [0085] An advantage of the invention is that substantially all of the liquid is retained within the filter substrate. This can ensure that there is not a significant excess of liquid that requires recycling and a uniform distribution can be achieved in the desired or standard coating arrangement. A particular advantage of the invention is that the use of expensive components of washable coatings (for example, precious metals) can be very well controlled, and it is not so necessary to specify the excess loads of these components in order to deal with process variations .
    [0086] Typically, step (b) of the method comprises coating the channels having open ends at the upper end of the filter substrate with the liquid from the containment and retention of substantially all of the liquid within the filter substrate. It is preferred that step (b) comprises coating the channels having open ends at the upper end of the filter substrate with the liquid from the containment and retention of substantially all of the liquid within the filter substrate, without recycling the liquid. The term "substantially all" in the present context refers to at least 99% of the predetermined amount of liquid, preferably at least 99.5% of the predetermined value, and most preferably all (i.e., 100%) of the predetermined amount of the liquid.
    [0087] In general, the method of the invention may comprise the step of (c) drying the filter substrate, preferably drying the liquid on the filter substrate, more preferably without inversion of the filter substrate.
    [0088] Step (c) may comprise (C1) drying the filter substrate, preferably drying the liquid on the filter substrate, more preferably without the inversion of the filter substrate, and then (c2) calcining the substrate filter, preferably without inversion of the filter substrate.
    [0089] Step (c) or steps (c1) and (c2) follows step (b). The filter substrate can be dried at 100 to 200 ° C (for example, for 5 to 60 minutes, particularly for 10 to 30 minutes). The drying step can be carried out to fix the liquid on the substrate.
    [0090] The method of the first aspect of the present invention involves (b) applying a vacuum to a lower end of the filter substrate. The apparatus of the first aspect of the invention comprises a means for applying a vacuum to a lower end of the filter substrate. In the method of the first aspect, step (b) may comprise (b) applying a vacuum to a lower end of the filter substrate, using the means for applying a vacuum.
    [0091] In general, step (b) of the first aspect comprises the step of (b) applying a vacuum to open the ends of the channels at a lower end of the filter substrate. Thus, step (b) comprises the step of (b) applying a vacuum to open the ends of the channels at a lower end of the filter substrate to coat the channels that have open ends at the top end of the filter substrate with the liquid a from containment means.
    [0092] Step (b) may comprise step (b) continuously applying a vacuum to a lower end of the filter substrate, preferably until the containment medium is substantially empty. The term "substantially empty" in this context refers to a containment medium containing less than 1% of the predetermined amount of liquid, preferably less than 0.5% of the predetermined amount of the predetermined amount of liquid.
    [0093] The vacuum is of drawing substantially all the liquid to the filter substrate. The term "substantially all" in the present context refers to at least 99% of the predetermined amount of liquid, preferably at least 99.5% of the predetermined value, and most preferably all (i.e., 100%) of the predetermined amount of the liquid. In addition to drawing substantially all of the liquid into the filter substrate, a vacuum typically ensures the liquid.
    [0094] Generally, the vacuum is -0.5 to -50 kPa (below atmospheric pressure), particularly from -1 to -30 kPa, and preferably from -5 to -20 kPa (for example, the vacuum applied to the filter substrate).
    [0095] The vacuum can be applied continuously for 0.25 to 15 seconds, such as 0.5 to 10 seconds, preferably 1 to 7.5 seconds (for example, 2 to 5 seconds).
    [0096] In general, high vacuum forces and / or longer vacuum durations result in a higher proportion of lining on the wall.
    [0097] The method of the first aspect may comprise the step of (b1) the formation of a watertight coupling between the lower end of the filter substrate and a means for applying a vacuum, and then (B2) applying a vacuum to the lower end of the filter substrate using the means to apply a vacuum.
    [0098] The medium for applying a vacuum typically comprises a funnel, such as a flow cone. The flow funnel or cone generally has an end for receiving a lower end of the filter substrate.
    [0099] The means for applying a vacuum may further comprise a seal to form a seal contact with the lower end of the substrate. The seal can be located at one end (wider end, for example) of the flow funnel or cone.
    [00100] Typically, the means for applying a vacuum comprises a vacuum generator, such as a vacuum pump. The vacuum generator can be connected to the funnel or cone flow by a conduit.
    [00101] In the method of the first aspect, step (a) can comprise the step of (A3) of retaining the liquid in the containment medium, particularly maintaining the predetermined amount of the liquid in the containment medium, for a period of rest. The rest period is the period of time that begins when the predetermined amount of liquid (i.e., completely introduced) has been introduced into the containment medium and ends when a vacuum is applied to a lower end of the filter substrate.
    [00102] The rest period can be at least 0.25 seconds, preferably at least 0.5 seconds, such as at least 1 second. In general, the rest period is no longer than 5 seconds, as there is no longer than 3.5 seconds and, preferably, no longer than 2 seconds. Longer periods of liquid leveling time increase the total time taken to coat a filter substrate (ie cycle time), which is undesirable for the industrial scale manufacture of such products.
    [00103] Generally, step (a3) precedes step (b) or step (b2) of the method. When the method comprises steps (Ao), (a1) or (A2), then step (a3) follows step (a2). When the method comprises step (b1), then step (a3) can occur before, after or simultaneously with step (b1). It is preferred that step (a3) follows step (b1).
    [00104] The method of the second aspect of the invention involves (b) draining the liquid from the containment medium to the filter substrate. In general, step (b) comprises step (b) draining the liquid by gravity (that is, only by gravity) from the containment medium, by gravity to the filter substrate.
    [00105] It is preferred that step (b) comprises the step of (b) draining the liquid from the containment medium to the filter substrate without applying a vacuum (e.g., to a lower end of the filter substrate, such as the open ends of the channels at a lower end of the filter substrate). More preferably, step (b) comprises step (b) draining the liquid from the containment medium into the filter substrate without applying a vacuum and without applying pressure to the upper end of the filter substrate. Pressure could, for example, be applied by blowing a gas (for example air) into the liquid in the containment medium or by mechanically applying pressure to the liquid in the containment medium.
    [00106] Advantageously, the first aspect of the invention can be used to prepare a coated filter substrate having a coating on the wall, whereas the second aspect of the invention can be used to prepare a coated filter substrate having a coating on the wall. It is to be understood that the reference to a wall covering means that most of the covering is present on the wall instead of on a wall surface. Likewise, it is to be understood that the reference to a wall covering means that most of the covering is on a wall surface (for example, as a membrane), rather than inside the wall itself, such as inside pores in the wall.
    [00107] In the second aspect of the invention, the coating depth of the liquid is determined by the predetermined amount of the liquid that is used. The liquid should be allowed to drain onto the filter substrate for a time sufficient to allow complete diffusion to occur, so that the desired coating depth is achieved.
    [00108] In the first or second aspects of the invention, the filter substrate can have a porosity of 40 to 75%, such as 45 to 70% (for example 45 to 65%) or 50 to 60%. The average pore size can be determined using mercury porosimetry according to conventional methods. Highly porous substrates can be prone to breakage during coating processes. In comparison with the prior art methods, the methods of the invention minimize substrate breaks because there is minimal manipulation of the substrate during the method.
    [00109] In the first or second aspects of the invention, particularly the first aspect of the invention, the filter substrate has, or the filter substrate walls have, an average pore size of 10 to 25 μm, such as 12 to 20 μm .
    [00110] The filter substrate can have a pore size distribution of 0.35 to 0.60, such as 0.40-0.55 [for example, where the pore size distribution is represented by [ (d50 - d10) / d50]. When a filter substrate has a narrow pore size distribution, it is difficult to obtain both (i) a uniform distribution of the washable coating along the lengths of the substrate channels and (ii) a uniform coating profile across a section the substrate. That is, thought to be due to the strong capillary forces that extract the washable coating on the canal walls before the washable coating can pass along the length of the canal. An advantage of the invention is that substrates coated with both (i) and (ii) can be manufactured, when a substrate having a narrow pore size distribution is used.
    [00111] It may be preferable (in the first or second aspects of the invention) that the filter substrate has a diameter (for example, when having a circular cross section) greater than or equal to 20.32 cm (8 inches). If the filter substrate has an elliptical cross-section, then preferably the filter substrate has an elliptical cross-sectional area greater than or equal to 324.32 cm2 (50.27 square inches).
    [00112] The liquid for use in the first or second aspects of the invention is preferably a washable catalytic coating. The washable catalytic coating is preferably a trap hydrocarbon composition, a three-way catalyst (TWC) composition, an NOx absorption composition, an oxidation catalyst composition, a selective catalytic reduction catalyst (SCR) composition, a composition of lean NOx catalyst or a slip ammonia catalyst (ASC) composition. Such washable catalytic coating compositions are well known in the art.
    [00113] In the first or second aspects of the invention, the liquid may comprise particles (for example, particles of a support material), wherein at least 90% of the particles have a particle size (i.e., a primary particle size) ) greater than 0.4 μm. Preferably, at least 90% of the particles have a particle size greater than 0.5 μm, more preferably greater than 1 μm, and even more preferably greater than 2 μm.
    [00114] In the first or second aspects of the invention, the liquid may comprise particles (for example, particles of a support material), wherein at least 90% of the particles have a particle size (i.e., a primary particle size) ) less than 25 μm. Preferably, at least 90% of the particles have a particle size of less than 20 μm, more preferably less than 15 μm, and even more preferably less than 10 μm.
    [00115] In the first aspect of the invention, the liquid is preferably a three-way catalyst (TWC) composition.
    [00116] In the second aspect of the invention, the liquid is preferably an oxidation catalyst composition or an SCR catalyst composition, more preferably, the liquid is an SCR catalyst composition.
    [00117] In general, the liquid may comprise a thickener. The thickening agent can be included to provide the liquid with a viscosity of either letting the liquid gradually drain into the filter substrate or so that it sits on top of the filter substrate until a vacuum is applied to remove it in the substrate.
    [00118] The invention can be used to coat an upper end face of the filter substrate. When coating an upper end face of the filter substrate, step (b) generally comprises coating the channels having open ends at the upper end of the filter substrate with the liquid from the containment to a depth of 10% or less, preferably 5% or less (e.g. 2.5% or less) of the axial length of the filter substrate.
    [00119] The filter substrate used in the present invention (for example, the first or second aspects of the invention) may have been pre-coated with a first liquid, such as from an upper or lower end, preferably the end bottom of the filter substrate. The lower end, in this context, refers to the opposite end of the substrate (i.e., the upper end), which is being coated according to the invention.
    [00120] Thus, the method may relate to a method for coating a pre-coated filter substrate comprising a plurality of channels, wherein the substrate of the pre-coated filter has been coated with a first liquid from an upper end , or a lower end (preferably the lower end) of a filter substrate, the method of which comprises the steps of: (A) introducing a predetermined amount of a second liquid into a containment means at the end / top of the substrate of the pre-coated filter; and (B) coating the channels having open ends at the upper end of the filter substrate pre-coated with the second liquid from the containment medium.
    [00121] The substrate of the pre-coated filter may have a plurality of channels, each with a wall covering and / or a wall covering.
    [00122] In principle, any method could be used to prepare a pre-coated filter substrate. It is preferable that a method of the invention, or the apparatus of the invention is used to prepare the substrate of the pre-coated filter.
    [00123] When the filter substrate has been coated according to the invention, then it can be coated from the opposite end, such as by coating using a method of the invention. The invention thus relates to methods of coating a filter substrate from each end (i.e., the first end and the second end).
    [00124] Thus, after step (c) of the method (for both the first and second aspects of the method), a second coating layer can be applied to the opposite end of the substrate. The method used to apply the second coating may be the same or different from that used to apply the first coating.
    [00125] The first aspect of the invention further provides a method for coating a filter substrate comprising a plurality of channels, the method of which comprises the steps of: (A) introducing a predetermined amount of a first liquid into a containment medium in an upper end of the filter substrate; (B) applying a vacuum to a lower end of the filter substrate; (C) drying the filter substrate; (D) inversion of the filter substrate (for example, containing the first liquid); (E) the introduction of a predetermined amount of a second liquid into a containment means at an inverted, lower end of the filter substrate; (F) applying a vacuum to the inverted, upper end of the filter substrate.
    [00126] The reference to the inverted, lower end of the substrate refers to the upper end of the substrate after it has been inverted. Likewise, the reference to the final, upper invert of the substrate refers to the lower end of the substrate after it has been inverted.
    [00127] Step (e) corresponds to step (a) of the first aspect of the invention, or as generally defined above. Step (f) corresponds to step (b) of the first aspect of the invention, or as generally defined above.
    [00128] The first aspect of the invention also provides a method for coating a filter substrate comprising a plurality of channels, the method of which comprises the steps of: (A) introducing a predetermined amount of a first liquid into a containment medium in an upper end of the filter substrate; (B) applying a vacuum to a lower end of the filter substrate; (C) drying the filter substrate; (D) inversion of the filter substrate (for example, containing the first liquid); (E) introducing a predetermined amount of a second liquid into a containment medium at an inverted, lower end of the filter substrate; (F) draining the liquid from the second containment medium to the filter substrate.
    [00129] Step (e) corresponds to step (a) of the second aspect of the invention, or as generally defined above. Step (f) corresponds to step (b) of the second aspect of the invention, or as generally defined above.
    [00130] The second aspect of the invention also relates to a method for coating a filter substrate comprising a plurality of channels, the method of which comprises the steps of: (A) introducing a predetermined amount of a first liquid into a medium containment at an upper end of the filter substrate; and (B) draining the liquid from the first containment medium to the filter substrate; (C) drying the filter substrate; (D) inversion of the filter substrate (for example, containing the first liquid); (E) the introduction of a predetermined amount of a second liquid into a containment means at an inverted, lower end of the filter substrate; and (F) drain the second liquid from the containment medium to the filter substrate.
    [00131] Step (e) corresponds to step (a) of the second aspect of the invention, or as generally defined above. Step (f) corresponds to step (b) of the second aspect of the invention, as generally defined above.
    [00132] The second aspect of the invention further provides a method for coating a filter substrate comprising a plurality of channels, the method of which comprises the steps of:
    [00133] (A) introducing a predetermined amount of a first liquid into a containment medium at an upper end of the filter substrate; and (G) draining the liquid from the first containment medium to the filter substrate; (H) drying the filter substrate; (I) the inversion of the filter substrate (for example, containing the first liquid); (J) the introduction of a predetermined amount of a second liquid into a containment means at an inverted, lower end of the filter substrate; (K) applying a vacuum to the inverted, upper end of the filter substrate.
    [00134] Step (e) corresponds to step (a) of the first aspect of the invention, or as generally defined above. Step (f) corresponds to step (b) of the first aspect of the invention, or as generally defined above.
    [00135] In general, the step of inverting the filter substrate is a 180 ° C substrate rotation step. After inversion of the substrate, the open ends of the channels that were initially at a lower end of the substrate will be at an upper end of the substrate. The second liquid will be introduced into the open ends of the channels that were at a lower end of the substrate before inversion.
    [00136] The first liquid and the second liquid can be the same (that is, they have the same composition) or they can be different (that is, they have a different composition).
    [00137] In the methods of the above invention, step (c) may comprise drying the filter substrate to form a pre-coated filter substrate. It is preferred that step (c) comprises drying the filter substrate to dry the liquid on the filter substrate and to form a pre-coated filter substrate.
    [00138] Step (c) may comprise (C1) drying the filter substrate, preferably drying the liquid on the filter substrate, and then (c2) calcining the filter substrate to form a pre-filter substrate. coated.
    [00139] The apparatus of the invention may or may not comprise means for reversing the substrate (for example, means for reversing the substrate of the filter containing the first liquid). DEFINITIONS
    [00140] The term "predetermined amount" as used herein refers to a total amount of liquid for introduction into the substrate that is sufficient to obtain a specific characteristic product, such as a desired coating specification. The quantity is "predetermined" in the sense that it is "pre-measured". Routine experiments can be carried out offline to observe the total amount of liquid that is needed to achieve the desired product characteristics. Such predetermined values can be easily determined and can be known from using other methods and apparatus for coating substrates in the art (for example, see WO 99/47260 and WO 1/080525 201).
    [00141] The term "single dose" as used herein refers to an amount of the liquid for coating a single substrate, typically to satisfy a desired product specification.
    [00142] Any reference to a "vacuum" as used herein refers to a pressure that is less than atmospheric pressure. The term "vacuum" is not to be interpreted in its literal sense as a space that is completely devoid of matter. The strength of the vacuum that is applied to the substrate will depend on the composition of the liquid and the type of substrate that is being used. The vacuum must be strong enough to clean the substrate cells as soon as there are no obstructions. Such vacuum forces or reduced pressures are well known in the art.
    [00143] Any reference to "substrate" as used herein, if a "filter substrate" or "flow-through substrate" encompasses a substrate monolith (eg, filter or flow-through monolithic substrate) substrate monolith).
    [00144] Any reference to "substantial on the wall" as used herein with reference to coating refers to a filter substrate, where a liquid comprising a catalyst component has been coated on a surface of the wall (i.e. substrate) such that> 50% of the catalyst component is disposed on a wall surface, particularly> 60% of the catalyst component, preferably> 70% of the catalyst component (for example,> 80% of the component catalyst), and more preferably> 90% of the catalyst component. When the liquid comprises a plurality of catalyst components, then typically> 50% of all catalyst components are arranged on a wall surface, particularly> 60% of the entire catalyst component, preferably> 70% of all components of the catalyst (e.g.,> 80% of all catalyst components), and more preferably> 90% of all catalyst components.
    [00145] Any reference to "substantial in the wall" as used herein with reference to coating refers to a filter substrate, where a liquid comprising a catalytic component resides within the wall (for example, the porous material / structure of the filter substrate wall) such that> 50% of the catalyst component resides inside the wall, particularly> 60% of the catalyst component, preferably> 70% of the catalyst component (eg> 80% of the catalyst component), and more preferably> 90% of the catalyst component. When the liquid comprises a plurality of catalyst components, then typically> 50% of all catalyst components reside within the wall, particularly> 60% of all catalyst components, preferably> 70% of all catalyst components. catalyst (e.g.> 80% of all catalyst components), and more preferably> 90% of all catalyst components.
    [00146] The amount of coating on the wall and the wall can be determined using scanning electron microscopy (SEM). EXAMPLES
    [00147] The invention will now be illustrated by the following non-limiting examples. Example 1
    [00148] Manufacture of a particulate gasoline filter (GPF)
    [00149] A washable coating for a particulate gasoline filter was prepared. The washable coating viscosity was modified by adding a rheology modifier to bring the washable coating viscosity up to 38 cP (measured at 20 ° C on a Brookfield RV DVII + Extra Pro viscometer using a SC4-27 spindle at 50 rpm speed spindle). The washable coating was formulated to provide a load of 0.8 g of washable coating in "3 and a load of 25 g PGM foot" 3. A particle size distribution of the support material that has been dispersed in the liquid is shown in the Table 1 below. TABLE 1

    [00150] Particle size measurements were obtained by Laser Diffraction Particle Size Analysis using a Malvern Mastersizer 2000, which is a volume-based technique (ie, D (v, 0.1), D (v, 0 , 5), D (v, 0.9) and D (v, 0.98) can also be referred to as DV10, DV50, Dv90 and Dv98 respectively (or D10, D50, D90 and D98, respectively) and a model applies of mathematical Mie theory to determine a particle size distribution.Diluted washable coating samples were prepared by sonication in distilled water, without surfactant for 30 seconds at 35 watts.
    [00151] The washable coating was used to coat a filter substrate (4.66 x 4.5 "C650 NGK ™ substrate) to a coating depth of 50% using the apparatus shown in Figure 1. A dose volume of 50 % of the washable coating was distributed by a containment medium located along an upper end face of the filter substrate A vacuum of -10 kPa applied to the lower end of the filter substrate for 120 seconds after the 50% dose volume was introduced in the middle of containment.
    [00152] After the coated filter substrate was dried and calcined, it was determined by SEM analysis that substantial coating on the substrate wall occurred. The average (average) coating length of the washable coating was found to be 57% of the axial length of the filter substrate. The distribution of coating lengths over the mean was less than ± 10%. Example 2 Manufacture of a particulate gasoline filter (GPF)
    [00153] A washable coating for a gasoline particle filter was prepared with a viscosity of 33 cP (measured at 20 ° C on a Brookfield LV viscometer with an SC4-21 spindle at 50 rpm). The washable coating was formulated to provide a charge of 0.4 g of "3 washable coating.
    [00154] The washable coating was used to coat a filter substrate (4.66 x 4.5 "C810 NGK substrate) to a 55% target coating depth, using the apparatus shown in Figure 1. A dose volume of 55 % of the washable coating was distributed by a containment medium located along an upper end face of the filter substrate A vacuum of -5 kPa was applied to the lower end of the filter substrate after the 55% dose volume was introduced into the containment medium.
    [00155] The average (average) coating length of the washable coating was found to be 58% of the axial length of the filter substrate. The distribution of coating lengths over the mean was less than ± 10%. Example 3 Manufacture of a catalytic soot filter (CSF)
    [00156] A washable coating for a catalyzed soot filter was prepared. The viscosity of the washable coating was 49 cP (measured at 20 ° C on a Brookfield RV DVII + Extra Pro viscometer using a SC4-27 spindle at 50 rpm spindle speed). The washable coating was formulated to provide a load of 0.35 g of washable coating in "3 and a load of 2 g PGM feet" 3.
    [00157] The washable coating was used to coat a filter substrate to a coating depth of 50% using the apparatus shown in Figure 1, without applying a vacuum. A dose volume of 50% of the washable coating was dispensed into a containment medium located on an upper end face of the filter substrate and was allowed to drain or immerse the channels of the filter substrate.
    [00158] After drying and calcining the substrate of the coated filter, it was determined by SEM analysis in which the coating of the substrate wall occurred. Examples 4 and 5 Manufacture of a catalytic soot filter (CSF)
    [00159] Two washable coatings for a catalyzed soot filter were prepared as shown in Table 2 below. Table 2
    * Measured at 20ºC on a Brookfield LV viscometer with an SC4-21 spindle at 50 rpm
    [00160] The washable coatings of Examples 4 and 5 were used to coat a filter substrate (143.8 mm x 129.5 mm SD091 Ibiden ™ substrate) using the apparatus shown in Figure 1.
    [00161] For Example 4, the target coating depth was 66%. A dose volume of 66% of the washable coating was dispensed into a containment medium located on an upper end face of the filter substrate. A vacuum of -5 kPa, was applied to the lower end of the filter substrate after the 66% dose volume was introduced into the containment medium.
    [00162] The average (average) coating length of the washable coating was found to be 65% of the axial length of the filter substrate. The distribution of coating lengths over the mean was less than ± 10%.
    [00163] For Example 5, the target coating depth was 46%. A dose volume of 46% of the washable coating was dispensed into a containment medium located on an upper end face of the filter substrate. A vacuum of -5 kPa, was applied to the lower end of the filter substrate after the dose volume of 46% was introduced into the containment medium.
    [00164] The average (average) coating length of the washable coating was found to be 48% of the axial length of the filter substrate. The distribution of coating lengths over the mean was less than ± 10%. Example 6 Manufacture of a catalytic soot filter (CSF) using a sol
    [00165] A washable coating using sol-like material for a catalyzed soot filter was prepared. The washable coating viscosity was modified by the addition of a rheology modifier to bring the washable coating viscosity to 2200 cP (measured at 20 ° C on a Brookfield RVDV-E viscometer using a # 4 spindle at 10 rpm, the speed of spindle). The washable coating was prepared by a sol that was formulated to provide a washable coating charge of 0.18 or 0.36 g in "3 and a load of 0.7 g PGM foot" 3. A particle size distribution of the material of support that has been dispersed in the liquid is shown in Table 3 below.

    [00166] The washable coating was used to coat a filter substrate (5.66 x 6 "558HG NGK substrate) to a coating depth of 50% using the apparatus shown in Figure 1. A dose volume of 50% of the coating washable was distributed by means of containment located on a upper end of the filter substrate.
    [00167] After the coated filter substrate was dried and calcined, it was determined by SEM analysis that substantial coating on the substrate wall occurred. The average (average) coating length of the washable coating was found to be 55% of the axial length of the filter substrate. Example 7 Manufacture of a catalytic soot filter (CSF) using a sol
    [00168] A washable coating using sol-like material was prepared with a viscosity of 810 cP (measured at 20 ° C on a Brookfield RVDV-E viscometer using a # 3 spindle at 10 spindle speed). The washable coating was formulated to provide a washable coating charge of 0.193 g in "3.
    [00169] The washable coating was used to coat a filter substrate (143.8 mm x 129.5 mm SD091 Ibiden ™ substrate) to a 55% target coating depth, using the apparatus shown in Figure 1. One dose volume 55% of the washable coating was dispensed into a containment medium located on an upper end face of the filter substrate. A vacuum of -20 kPa applied to the lower end of the filter substrate after the dose volume of 55% was introduced into the containment medium.
    [00170] The average (average) coating length of the washable coating was found to be 54% of the axial length of the filter substrate. The distribution of coating lengths over the mean was less than ± 10%. Examples 8 to 10 Manufacture of a selective catalytic reduction filter (SCRF ™) catalyst
    [00171] A series of vanadium containing washable SCR coatings were prepared as shown in Table 4 below.
    * Measured at 20ºC on a Brookfield LV viscometer with a SC4-21 spindle at 50 rpm; † measured at 20ºC on a Brookfield LV viscometer with an SC4-27 spindle at 50 rpm
    [00172] The washable coatings of Examples 8 to 10 were used to coat a filter substrate, as listed in Table 5, below, using the apparatus shown in Figure 1. In each case, the target coating depth was 75%. Table 5 shows the vacuum that was applied and the coating depth that was obtained for each part. Table 5
    t the distribution of coating lengths over the mean was less than ± 10%
    [00173] For the avoidance of doubt, the entire contents of any and all documents cited herein are incorporated by reference into this application.
    权利要求:
    Claims (15)
    [0001]
    1. Method for coating a filter substrate comprising a plurality of channels, each channel having an open end and a closed end, the method characterized by the fact that it comprises the steps of: (A) depositing a predetermined amount of a liquid into a containment means at an upper end of the filter substrate using a wash head, wherein the wash head comprises a plurality of orifices arranged to dispense the liquid on an upper end face of the filter substrate, and wherein the liquid has a viscosity of <600 cP, as measured at 20 ° C on a Brookfield RV DVII + Extra Pro viscometer using a SC4-27 spindle at 50 rpm spindle speed; and (B) coating the channels having open ends at the upper end of the filter substrate with a predetermined amount of liquid from the containment medium, by applying a vacuum to a lower end of the filter substrate to remove the liquid over the channels with open ends at the top end of the filter substrate.
    [0002]
    2. Method according to claim 1, characterized in that the liquid has a viscosity <500 cP (at a shear rate of 20 s-1), as measured at 20 ° C on a Brookfield RV DVII + viscometer Extra Pro using a SC4-27 spindle.
    [0003]
    Method according to either of Claims 1 or 2, characterized in that the liquid has a viscosity of 10 to 100 cP, as measured at 20 ° C in a Brookfield RV DVII + Extra Pro viscometer using a SC4- 27 to 50 rpm spindle speed.
    [0004]
    Method according to any one of claims 1 to 3, characterized in that the predetermined amount of the liquid is a predetermined volume of the liquid.
    [0005]
    Method according to any one of claims 1 to 4, characterized in that the predetermined amount of the liquid is a single dose of the liquid.
    [0006]
    Method according to any one of claims 1 to 5, characterized in that the containment means comprises a sealing means to prevent liquid from flowing from the upper end face of the filter substrate and to an outer lateral surface of the filter. filter substrate, wherein the sealing means comprises at least one inflatable collar.
    [0007]
    Method according to any one of claims 1 to 6, characterized in that the containment means comprises a model for covering an area or areas of an upper end face of the filter substrate.
    [0008]
    Method according to any one of claims 1 to 7, characterized in that the liquid is a solution or a suspension, preferably a colloidal suspension.
    [0009]
    Method according to any one of claims 1 to 8, characterized in that the liquid comprises a catalyst component, which is a platinum group metal (PGM), a support material or a zeolite.
    [0010]
    Method according to any one of claims 1 to 9, characterized in that the filter substrate has a porosity of 40 to 75%.
    [0011]
    Method according to any one of claims 1 to 10, characterized in that the filter substrate has walls, which have an average pore size of 10 to 25 μm.
    [0012]
    12. Method according to any one of claims 1 to 11, characterized in that the filter substrate has a pore size distribution of 0.35 to 0.60, where the pore size distribution is represented by (d50 - d10) / d50].
    [0013]
    Method according to any one of claims 1 to 12, characterized in that the filter substrate has a diameter greater than or equal to 20.32 cm (8 inches).
    [0014]
    Method according to any one of claims 1 to 13, characterized in that the liquid comprises particles, in which at least 90% of the particles have a particle size greater than 0.4 µm.
    [0015]
    Method according to any one of claims 1 to 14, characterized in that the liquid comprises particles, in which at least 90% of the particles have a particle size of less than 25 μm.
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    同族专利:
    公开号 | 公开日
    GB201504924D0|2015-05-06|
    DE112015001438T5|2016-12-29|
    CA2940500A1|2015-10-01|
    US20210008534A1|2021-01-14|
    PL3122458T3|2020-07-27|
    US10814318B2|2020-10-27|
    CN106132501B|2020-05-05|
    RU2016141552A|2018-04-25|
    GB2524662A|2015-09-30|
    GB201405277D0|2014-05-07|
    WO2015145122A3|2015-12-30|
    JP2017516642A|2017-06-22|
    JP6603236B2|2019-11-06|
    KR20170031649A|2017-03-21|
    US20180229228A1|2018-08-16|
    DK3122458T3|2020-03-09|
    GB2524662B|2017-12-06|
    WO2015145122A2|2015-10-01|
    RU2016141552A3|2018-10-29|
    HUE048372T2|2020-07-28|
    EP3122458B1|2020-01-08|
    CN106132501A|2016-11-16|
    EP3122458A2|2017-02-01|
    RU2716690C2|2020-03-13|
    ZA201605954B|2021-03-31|
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    法律状态:
    2019-12-31| B06U| Preliminary requirement: requests with searches performed by other patent offices: procedure suspended [chapter 6.21 patent gazette]|
    2020-11-24| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|
    2021-01-05| B16A| Patent or certificate of addition of invention granted [chapter 16.1 patent gazette]|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 24/03/2015, OBSERVADAS AS CONDICOES LEGAIS. |
    优先权:
    申请号 | 申请日 | 专利标题
    GBGB1405277.3A|GB201405277D0|2014-03-25|2014-03-25|Method for coating a filter substrate|
    GB1405277.3|2014-03-25|
    PCT/GB2015/050858|WO2015145122A2|2014-03-25|2015-03-24|Method for coating a filter substrate|
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