CN1835831A - Method for manufacturing honeycomb formed article, method for manufacturing honeycomb filter, and honeycomb filter - Google Patents

Abstract

A method for manufacturing a honeycomb formed article, which comprises an admixing step of admixing two or more types of aggregate particulate materials (first admixing) to prepare a compound for forming (dry powder) and then admixing the compound with water (second admixing) to prepare a compound for forming (wet powder), and a kneading step of kneading the compound for forming (wet powder) to prepare a body. The method for manufacturing a honeycomb formed article allows the prevention of the generation of internal defects without the adoption of a complicated process or a troublesome operation, with ease and simplicity.

Description

The manufacture method of honeycomb formed article, the manufacture method of amplifier case and amplifier case

Technical field

The present invention relates to for example to be suitable for to make control of dust with and the manufacture method of the honeycomb formed article of water treatment usefulness filter, the manufacture method and the amplifier case of amplifier case, relate to internal flaws such as effectively preventing aperture, fragment, burr in more detail, and can improve the manufacture method of the honeycomb formed article of intensity, the manufacture method and the excellent honeycomb formed article of strainability (arresting efficiency) of amplifier case.

Background technology

In with the various fields headed by chemistry, electric power, iron and steel, the industrial waste processing etc., the control of dust that be used for preventing environmental protection such as public hazards, reclaims purposes such as goods from high-temperature gas with and the water treatment filter, the cellular honeycomb structures that use is made of the pottery of hear resistance, corrosion resistance, mechanical strength excellence.For example, capture from the diesel particulate filter (DPF) of the particulate (cigarette ash) of diesel engine discharging and wait the control of dust filter that under high temperature, corrosive gas atmosphere, uses, the cellular honeycomb structures that constitutes by pottery with regard to use.

Example as the filter that uses cellular honeycomb structures (below be called " amplifier case "), can enumerate amplifier case for example shown in Figure 1 21, with the entrance side end face B of a plurality of cells 23 of cellular honeycomb structures 25 and outlet side end face C with the structure of sealing of hole portion 22 sealing of holes with intermeshing.According to the amplifier case 21 of this structure, if import processed gas G to cell 23 from entrance side end face B ₁, when then field trash next door 24 such as particulate is captured, see through the gas of the processing G in the cell 23 that porous wall 24 flows into adjacency ₂From outlet side end face C discharging, therefore can access and separate processed gas G ₁In the gas of the processing G of particulate ₂

This cellular honeycomb structures for example can obtain by the following method, promptly mix the shaping raw material of aggregate particle raw materials such as containing pottery and water and obtain moulding complex (wet-milling), mixing and molding obtains base soil with complex (wet-milling), with the base earth forming is honeycomb shape, dry and obtain honeycomb formed article, reburn into honeycomb formed article.But still there are internal flaws such as a large amount of apertures, fragment, burr in the cellular honeycomb structures according to above-mentioned manufacture method obtains, uses the strainability (arresting efficiency) of its filter can not say so fully.

Particularly in recent years, the pressure loss when reducing the gas permeation next door improves the disposal ability of filter, and the thin-walled property in next door develops by leaps and bounds.Thin its structure of cellular honeycomb structures in this next door is easy to generate internal flaws such as aperture, fragment, burr during fabrication, thereby the decline of the strainability of the filter that these internal flaws cause (arresting efficiency) is just becoming most penetrating problem.

What known above-mentioned internal flaw is the existence of the thick aggegation piece that forms owing to the microparticle agglutination in the aggregate particle raw material.Promptly, in aforesaid manufacture method, as forming method, the nozzles that have with the slit of the shape of next door complementation that use carry out extrusion molding more, but can stop up thick aggegation piece at this slit, thereby make the part of slit inaccessible, the supply of the base soil of this part is just hindered, and therefore can produce internal flaw in honeycomb formed article (and then cellular honeycomb structures).

In addition, require high strength for cellular honeycomb structures.This is owing to by realizing high strength, can improve the through performance of the filter that uses cellular honeycomb structures.It has been generally acknowledged that the porosity and through performance are proportional, therefore as a kind of means that reduce the pressure loss, raising filter process ability, the high porosityization of attempting cellular honeycomb structures sometimes.But the high porosity meeting causes intensity to descend, and therefore is difficult to be applicable to control of dust filters such as above-mentioned DPF.

In order to address this is that, the inventor has proposed a kind of manufacture method of ceramic honeycomb structure, promptly earlier aggregate particle raw material is made slurries, remove thick aggegation piece by the sieve of regulation sieve aperture, and then make powder, this powder is supplied in the modulation shaping raw material (for example with reference to patent documentation: the international brochure that discloses No. 01/058827).

Summary of the invention

But, though aforesaid manufacture method prevents the internal flaw of cellular honeycomb structures from removing thick aggegation piece, the viewpoint that improves intensity is very effective, but owing to need earlier aggregate particle raw material to be made slurries, thereby there are complex process, the numerous and diverse problem of operation.

The present invention carries out in view of the problem of above-mentioned conventional art, its purpose is to be provided under the condition of numerous and diverseization that is not accompanied by increase of process number purpose or operation, can prevent internal flaw easily, improve the manufacture method of the honeycomb formed article of intensity, the amplifier case that the manufacture method and the internal flaw of amplifier case is few, intensity is high and strainability (arresting efficiency) is excellent.

The inventor concentrates on studies in order to solve above-mentioned problem, found that by mix up to the shaping raw material that will contain aggregate particle raw material and water, in the mixing operation that obtains base soil, microparticle agglutination in the aggregate particle raw material that employing prevents to contain in the shaping raw material and in the aggegation piece that forms thick at least aggegation piece sneak into the means of base soil, can realize above-mentioned purpose, so that finished the present invention.That is, provide the manufacture method of following honeycomb formed article, the manufacture method and the amplifier case of amplifier case in the present invention.

[1] manufacture method of honeycomb formed article, its for use comprise two or more contain average grain diameter smaller or equal to the aggregate particle raw material of the particulate of 10 μ m and the shaping raw material of water, obtain the manufacture method of the honeycomb formed article of honeycomb formed article, comprise that obtaining moulding by the aggregate particle raw material (first mixes) that mixes two or more carries out the mixing mixing operation that obtains base soil with the mixed processes of complex (dry powder) and by this moulding is added water with complex (dry powder); With the base earth forming that obtains is the honeycomb shape of being separated and be formed with a plurality of cells by the next door, carries out drying, thereby obtains honeycomb formed article (being also referred to as first manufacture method of honeycomb formed article).

[2] manufacture method of honeycomb formed article, its for use comprise two or more contain average grain diameter smaller or equal to the aggregate particle raw material of the particulate of 10 μ m and the shaping raw material of water, obtain the manufacture method of the honeycomb formed article of honeycomb formed article, comprise aggregate particle raw material (first mixes) by mixing two or more obtain moulding with complex (dry powder) after, further add water and mix (second mixes) and obtain the mixed processes that complex (wet-milling) is used in moulding, and the mixing operation that obtains base soil by mixing this moulding with complex (wet-milling); With the base earth forming that obtains is the honeycomb shape of being separated and be formed with a plurality of cells by the next door, carries out drying, thereby obtains honeycomb formed article (being also referred to as second manufacture method of honeycomb formed article).

[3] manufacture method of above-mentioned [1] or [2] described honeycomb formed article, after described mixing operation and before described formed honeycomb shape, having the base earth forming that will obtain in mixing operation is the soil refining operation of regulation shape.

[4] manufacture method of any described honeycomb formed article of above-mentioned [1]～[3] before mixed processes, is implemented lining to the surface of aggregate particle raw material in advance.

[5] manufacture method of any described honeycomb formed article of above-mentioned [1]～[4], before mixed processes, classification aggregate particle raw material is got rid of the aggegation piece in advance.

[6] manufacture method of any described honeycomb formed article of above-mentioned [1]～[5] in mixed processes, is carried out first and is mixed, and making moulding is smaller or equal to 1 quality % with the residue (aggegation piece) of complex (dry powder) on the sieve of sieve aperture 500 μ m.

[7] manufacture method of any described honeycomb formed article of above-mentioned [1]～[6] when adding water, is further added the surfactant as dispersant.

[8] manufacture method of any described honeycomb formed article of above-mentioned [1]～[7], in mixed processes, shaping raw material applied pressurization and vibration on one side mix on one side.

[9] manufacture method of above-mentioned [8] described honeycomb formed article, described pressurization and vibration is produced by ultrasonic wave.

[10] manufacture method of above-mentioned [8] described honeycomb formed article, described pressurization and vibration be by accommodating shaping raw material and roundstone in container, vibration container and producing.

[11] manufacture method of any described honeycomb formed article of above-mentioned [1]～[7], mixed processes use the mixer with stirring vane to carry out, by the rotation of stirring vane, shaping raw material applied shearing force on one side mix on one side.

[12] manufacture method of above-mentioned [11] described honeycomb formed article makes stirring vane be rotated with the rotating speed more than or equal to 500rpm.

[13] manufacture method of above-mentioned [11] described honeycomb formed article makes stirring vane be rotated with the peripheral speed more than or equal to 2m/ second.

[14] manufacture method of any described honeycomb formed article of above-mentioned [1]～[13], mixed processes use the mixer with refrigerating function to carry out.

[15] manufacture method of any described honeycomb formed article of above-mentioned [1]～[14], mixed processes and mixing operation are undertaken by separately device respectively, carry out the mixer of mixed processes and carry out the mixing roll of mixing operation by online.

[16] manufacture method of any described honeycomb formed article of above-mentioned [1]～[15], use contains the aluminium oxide (Al of average grain diameter smaller or equal to 10 μ m as aggregate particle raw material ₂O ₃) particulate and/or average grain diameter be smaller or equal to the aluminium hydroxide (Al (OH) of 10 μ m ₃) the cordierite raw material of particulate.

[17] manufacture method of any described honeycomb formed article of above-mentioned [1]～[15] is used the material that contains aggregate particle raw material, water, also has pore-creating material and adhesive as shaping raw material.

[18] manufacture method of above-mentioned [17] described honeycomb formed article is used the microcapsules that are made of Foamex as described pore-creating material.

[19] manufacture method of any described honeycomb formed article of above-mentioned [1]～[18] is when adding described water, while this water of spraying adds mixing.

[20] manufacture method of any described honeycomb formed article of above-mentioned [1]～[19], described moulding are to use the extrusion molding that has with the nozzle of the slit of next door complementary shape.

[21] manufacture method of above-mentioned [20] described honeycomb formed article is used to contain as aggregate particle raw material and has been passed through the material of sieve aperture smaller or equal to the powder of 4/5 sieve of nozzle slot width.

[22] nozzle that the manufacture method of above-mentioned [20] described honeycomb formed article, extrusion molding use all intersection points at slit to be provided with dorsal pore carries out.

[23] manufacture method of any described honeycomb formed article of above-mentioned [20]～[22], at least a portion in the bight of the cell piece of the formation slit of described nozzle forms R.

[24] manufacture method of any described honeycomb formed article of above-mentioned [20]～[23], extrusion molding use the twin shaft continuous forming machine to carry out.

[25] manufacture method of any described honeycomb formed article of above-mentioned [20]～[24] when carrying out extrusion molding, makes base soil by behind the sieve of sieve aperture 160～278 μ m, extrudes from nozzle.

[26] manufacture method of amplifier case, any described manufacture method according to above-mentioned [1]～[25] obtains honeycomb formed article, obtain cellular honeycomb structures by burning till this honeycomb formed article, with a side opening portion of a plurality of cells of this cellular honeycomb structures and the opposite side peristome ground sealing of hole that intermeshes, obtain plugged honeycomb structure, again by burning till this plugged honeycomb structure, obtain amplifier case, constituting when the processed fluid that imports to a part of cell flows into the cell of adjacency through porous wall of described amplifier case, the field trash next door is captured.

[27] manufacture method of amplifier case, any described manufacture method according to above-mentioned [1]～[25] obtains honeycomb formed article, with a side opening portion of a plurality of cells of this honeycomb formed article and the opposite side peristome ground sealing of hole that intermeshes, obtain the sealing of hole honeycomb formed article, again by burning till this sealing of hole honeycomb formed article, obtain amplifier case, constituting when the processed fluid that imports to a part of cell flows into the cell of adjacency through porous wall of described amplifier case, the field trash next door is captured.

[28] amplifier case, it constitutes has cellular honeycomb structures and sealing of hole portion, described cellular honeycomb structures has a plurality of cells that separately formed by porous wall, described sealing of hole portion carries out sealing of hole to a side opening portion and the opposite side peristome of a plurality of cells with intermeshing, and when the processed fluid that imports to a part of cell flowed into the cell of adjacency through the next door, the field trash next door was captured; Cigarette ash leakage cell ratio by cigarette ash printing test evaluation is smaller or equal to 1 cell/1000 cells.

[29] above-mentioned [28] described amplifier case, cellular honeycomb structures is made of cordierite at least.

The manufacture method of the manufacture method of the honeycomb formed article that the present invention relates to and the amplifier case that the present invention relates to, by up to mix, in the mixing operation that obtains base soil, carry out mixed processes and mixing operation independently, can be difficult to produce the aggegation piece that forms by the microparticle agglutination in the aggregate particle raw material that contains in the shaping raw material more.Thereby, can suppress the aggegation piece and sneak in the base soil.

And then, the manufacture method of the manufacture method of the honeycomb formed article that the present invention relates to and the amplifier case that the present invention relates to, by adopting lining is implemented on the surface of aggregate particle raw material, classification aggregate particle raw material, mix and/or except water, also add surfactant when mixing, mix while applying pressurization and vibration, the rotation that utilizes stirring vane various preferable methods such as mixes while applying shearing force, the aggegation piece can be used the complex (wet-milling) from moulding and be got rid of, perhaps make the crushed material of aggegation piece be distributed to moulding equably with in the complex (wet-milling).Thereby, can suppress the aggegation piece and sneak in the base soil, prevent that thick at least aggegation piece from sneaking in the base soil.

And, manufacture method according to the manufacture method of the honeycomb formed article that the present invention relates to and the amplifier case that the present invention relates to, by adopting these methods, the aggegation piece that becomes the internal flaw reason is disappeared by pulverizing, therefore, can under the condition of numerous and diverseization of the complicated or operation of not earlier aggregate particle raw material not being made this operation of slurries, prevent internal flaw easily, improve intensity.In addition, the internal flaw of amplifier case of the present invention is few, intensity is high and strainability (arresting efficiency) excellence.In this manual, so-called intensity is meant at each intensity to the equal pressure pressurization, i.e. high isostatic strength.

Description of drawings

Fig. 1 is the schematic diagram of example that the amplifier case of cellular honeycomb structures has been used in expression.

Fig. 2 is the schematic diagram by the example explanation " honeycomb shape " of cellular honeycomb structures.

Fig. 3 is the schematic diagram that explanation is used for the checkout gear of cigarette ash printing test.

Fig. 4 is the chart of expression high isostatic strength result of the test.

Among the figure, 1,25 ... cellular honeycomb structures, 3,23 ... cell, 4,24 ... the next door, 22 ... sealing of hole portion, 21 ... amplifier case, 31 ... checkout gear, 32 ... support platform, 34 ... the cigarette ash generator, 36 ... sieve, 38 ... aiutage, 40 ... give tracheae, 42 ... transfer valve, 44 ... blast pipe, 46 ... fastening net, B ... the entrance side end face, C ... the outlet side end face, G ₁Processed gas, G ₂Handled gas.

The specific embodiment

Below, specifically describe manufacture method, the manufacture method of amplifier case and the preferred plan that amplifier case is used of implementing honeycomb formed article of the present invention, but the present invention is not limited to these embodiments.Can in the scope that does not break away from main points of the present invention,, carry out various changes, correction, improvement, replacement according to one of ordinary skill in the art's knowledge.If will implement or verify the present invention, can adopt with this specification in the identical method put down in writing or the method that is equal to, but suitable method is a method as described below.

(1) manufacture method of honeycomb formed article

The manufacture method of honeycomb formed article of the present invention provides first manufacture method of honeycomb formed article and second manufacture method of honeycomb formed article.The manufacture method of each honeycomb formed article is, have (i) mixed processes and (ii) mixing operation, and then preferably has a (iii) soil refining operation that the base earth forming that will obtain is the regulation shape in mixing operation, by carrying out base soil is made the (iv) molding procedure of honeycomb shape, obtain honeycomb formed article.

In this manual, when only being called the manufacture method of honeycomb formed article of the present invention, be meant first manufacture method of honeycomb formed article and second manufacture method of honeycomb formed article.In first manufacture method of honeycomb formed article, mix=the first and mix, in second manufacture method of honeycomb formed article, mix=the first and mix and/or second mixing.And, in second manufacture method of honeycomb formed article, be meant when only being called mixing that first mixing and second mixes both.In addition, in first manufacture method of honeycomb formed article, owing to do not obtain moulding with complex (wet-milling), do not specify that therefore the situation that moulding is put down in writing with complex (wet-milling) is that what to be put down in writing in second manufacture method with honeycomb formed article is prerequisite.And then, when only being called moulding and using complex, be meant moulding with complex (dry powder) and moulding usefulness complex (wet-milling) both.

(i) mixed processes

In mixed processes, contain two or more the aggregate particle raw material (first mix) of average grain diameter by mixing smaller or equal to the particulate of 10 μ m, obtain moulding with complex (dry powder).Then, in first manufacture method of honeycomb formed article, transfer to mixing operation, but in second manufacture method of honeycomb formed article, then mix (second mixes), obtain moulding complex (wet-milling) by further interpolation water.In addition, consider second manufacture method of honeycomb formed article,, put down in writing, but in first manufacture method of honeycomb formed article, in mixing operation, add these materials as the explanation of mixed processes for adding water, dispersant, additive etc.

The aggregate particle is the particle that becomes the main composition composition of cellular honeycomb structures (sintered body), and aggregate particle raw material is the material that becomes its raw material.As the aggregate particle raw material among the present invention, can enumerate for example cordierite raw material, mullite, aluminium oxide, aluminium titanates, lithium aluminium silicate, carborundum, silicon nitride or their mixture etc.But aggregate particle raw material is not limited to pottery, also can be metal.For example become the metallic silicon of the constitute of metallic silicon (Si)-carborundum (SiC) sintered body, can be used as the aggregate particle raw material among the present invention.

Said in this manual " cordierite raw material " is meant the material that can be exchanged into cordierite by burning till, and for example can enumerate talcum, kaolin, aluminium oxide, aluminium hydroxide, silica etc. are formed (2MgO2Al with the theory that consists of cordierite after burning till ₂O ₃5SiO ₂) the mixed material of mode etc.

Aggregate particle raw material among the present invention is to contain the material of average grain diameter smaller or equal to the particulate of 10 μ m.For this aggregate particle raw material, the microparticle agglutination that wherein contains and become easily the aggegation piece of the internal flaw reason of honeycomb formed article (and then cellular honeycomb structures), but manufacture method according to honeycomb formed article of the present invention, even use this aggregate particle raw material, also can obtain the few honeycomb formed article of internal flaw (and then cellular honeycomb structures).

As the particulate of average grain diameter, can enumerate the aluminium oxide (Al in the cordierite raw material for example smaller or equal to 10 μ m ₂O ₃) particulate (average grain diameter is about 1～10 μ m) or aluminium hydroxide (Al (OH) ₃) particulate (average grain diameter is about 0.2～10 μ m) etc.That is, use contains the aluminium oxide (Al of average grain diameter smaller or equal to 10 μ m as aggregate particle raw material ₂O ₃) particulate and/or average grain diameter be smaller or equal to the aluminium hydroxide (Al (OH) of 10 μ m ₃) during the cordierite raw material of particulate, can use the manufacture method of honeycomb formed article of the present invention aptly.When being called " average grain diameter " in this manual, be meant by liquid phase sedimentation to be measuring principle, to utilize the value of 50% particle diameter that the X ray through mode particle size distribution device that the X ray penetrant method detects (trade name for example: セ デ イ グ ラ Off 5000-02 type, (strain) Shimadzu Seisakusho Ltd. make etc.) measures with Stokes.

Shaping raw material among the present invention contains two or more above-mentioned aggregate particle raw material and at least as the water of its decentralized medium.Can contain other additives (for example pore-creating material, adhesive, dispersant etc.) as required.

The pore-creating material is to form pore by burn losing when burning till honeycomb formed article, increases the porosity, with the additive of the cellular honeycomb structures that obtains high porosity.Thereby, as the pore-creating material, can enumerate the combustible that when burning till honeycomb formed article, can burn mistake, for example graphite, wheat flour, starch, phenolic resins, polymethyl methacrylate, polyethylene or PETG etc. wherein especially can suit to use the microcapsules (acrylic resin system microcapsule etc.) that are made of Foamex.The microcapsules that are made of Foamex owing to be hollow, so not only add the cellular honeycomb structures that low amounts of resin can obtain high porosity, and heat production are few when burning till, and have the advantage of the generation that can reduce the crackle that thermal stress causes.

Adhesive is to give flowability to base soil when formed honeycomb, plays the additive of the reinforcing agent effect of keeping the mechanical strength of burning till preceding honeycomb formed article (the dry body of honeycomb).As adhesive, can use for example hydroxypropyl methylcellulose, methylcellulose, hydroxyethylcellulose, carboxymethyl cellulose or polyvinyl alcohol etc. aptly.

Dispersant (surfactant) is to be used to promote the dispersion to water such as aggregate particle raw material, with the moulding that the obtains homogeneous additive with complex.Thereby,, can use material aptly, for example ethylene glycol, dextrin, fatty acid soaps, polyalcohol etc. with surface-active effect as dispersant.The addition of dispersant (surfactant) is preferably less than 1.5 quality % in containing ratio.0.01～1 quality % more preferably.This is owing to can obtain desirable dispersion effect.

The characteristics of the manufacture method of honeycomb formed article of the present invention are, mixed processes is separated independently with the mixing operation of back carry out.In mixed processes, by mix aggregate particle raw material (first mixes) fully at the drying stage that does not add water, (second of back mix or mixing operation in) add water aftershaping raw material each composition, promptly two or more aggregate particle raw material and water can disperse equably at least, therefore the aggegation piece that is formed by the microparticle agglutination in the aggregate particle raw material is difficult to sneak into mixing in the back and in the base soil that obtains.In addition, by employed mixer, the aggegation piece that has generated also can be pulverized, and therefore can further suppress the aggegation piece and be blended in the base soil.

The manufacture method of honeycomb formed article of the present invention can adopt the method for in advance surface of aggregate particle raw material being implemented lining before mixing aptly.Like this, can be in the microparticle agglutination that suppresses aggregate particle raw material, the aggegation piece that easy pulverizing has generated.The aggregate particle raw material that lining is implemented on the surface has sale on market, if aluminium hydroxide then can be enumerated the material that uses stearic acid to carry out surface treatment and improve dispersiveness.

In addition, can get rid of the aggegation piece that mixes, suppress the aggegation piece and be blended in the base soil by prior classification aggregate particle raw material before mixing.Here, classification can utilize cyclone (utilizing centrifugal force to separate device with classification) etc. to carry out.

In second manufacture method of honeycomb formed article of the present invention, to the moulding complex (dry powder) that obtains by mixing aggregate particle raw material (first mixes), further adding water mixes (second mixing) and obtains moulding complex (wet-milling), this moment is as the water of decentralized medium, if be mixed together with complex (dry powder) with moulding, then most cases is difficult to disperse equably.Thereby, in second manufacture method of honeycomb formed article of the present invention, second mix preferably to moulding with complex (being mixed with the dry powder of two or more aggregate particle raw material) on one side one side spray water mix.Thus, can avoid moulding with the moisture content of complex (and then base soil, honeycomb formed article) because of the different inconsistent phenomenons in position, thereby can obtain can not causing the inconsistent cellular honeycomb structures of the porosity because of the position difference.Here, even do not obtaining moulding with complex (wet-milling), and add in first manufacture method of honeycomb formed article of the present invention of water, on one side preferred similarly spray water is on one side carried out mixing in mixing operation.

In the manufacture method of honeycomb formed article of the present invention, the concrete grammar during mixing is restriction not, uses the mixer of regulation, on one side when shaping raw material applied pressurization and vibration and mix on one side, can pulverize the aggegation piece, suppress the aggegation piece and sneak in the base soil.As the mixer of realizing this mixing, can illustration by ultrasonic wave realize pressurization and vibration ultrasonic dispersing machine, in container, accommodate shaping raw material and roundstone and vibrate the jar mill etc. that this container is realized pressurization and vibration.Particularly, utilizing the mixing of jar mill is the method that can access the excellence of the effect of the constituent that disperses shaping raw material equably.

The mixer that is used to mix also can use above-mentioned mixer in addition, and the aggegation piece that can pulverize is as required selected.Mixer can use any of indirect hybrid mode, direct hybrid mode.As indirect hybrid mode, utilize hyperacoustic dispersion machine except above-mentioned, utilize bubble to mix the mixer (for example ア コ one Co., Ltd. make positive mixer) etc. of (air mixed aeration) in addition.Directly hybrid mode can be further divided into the mixer that shell motion mode, internal motion mode or shell motion mode combine with the internal motion mode.As shell motion mode mixer, can enumerate twin-core type mixer, V-Mixer, cement mixer, shaking mixer etc. particularly; As the internal motion mode, can enumerate ribbon mixer, worm mixer, snare (ワ one Na) type mixer, kneading type mixer, omnipotent mixing and blending machine, nauta mixer (for example product of ホ ソ カ ワ ミ Network ロ Application Co., Ltd. manufacturing) etc. particularly.As the mixer that the shell motion mode combines with the internal motion mode, can enumerate the rotary-type Forced Mixing device of base, omnidirectional's blender (diffusion mixes, for example the product of Chiyoda Technical Researching Industry Co. Ltd.'s manufacturing) etc. particularly.

And then, in the manufacture method of honeycomb formed article of the present invention, use the regulation mixer, shaping raw material is stirred when mixing while applying shearing force, the aggegation piece that can pulverize microparticle agglutination in the aggregate particle raw material that contains in the shaping raw material and form can suppress the aggegation piece and sneak in the base soil.Especially in second manufacture method of honeycomb formed article of the present invention, in the mixing before being about to carry out mixing operation, promptly when the moulding that obtains mixes (second mixes) with complex (dry powder) interpolation water to mixing aggregate particle raw material (first mixes), if mix while applying shearing force, then suppressing the aggegation piece, to sneak into the effect of base soil obvious.

For shaping raw material is stirred while applying shearing force, be widely used in the mixer with the low speed rotation stirring vane about 20～200rpm (for example Sigma's kneader, ribbon mixer etc.) that powder mixes in the past always, mixing power and dispersion force are insufficient, and therefore expectation is used and can be rotated the mixing power of stirring vane and the mixer of dispersion force excellence more at high speed.

As the mixer of this mixing power and dispersion force excellence, can enumerate thousand generation the field skill grind the ultra high shear omnidirectional blender that industrial Co., Ltd. makes; the vertical-type comminutor that パ ウ レ Star Network Co., Ltd. makes; the mixing high-speed stirred comminutor SPG series that DALTON makes; the axial blender that China fir mountain heavy industry Co., Ltd. makes; the super mixer that Pacific Machinery ﹠ Engineering Co., Ltd. makes; the turbulent flow blender that ホ ソ カ ワ ミ Network ロ Application Co., Ltd. makes; the super blender that カ ワ Co., Ltd. makes; the strange formula blender of R type Airy that strange (Eirich) Co., Ltd. of Japan's Airy makes etc.

And then, as to shaping raw material while applying the preferred mixer that shearing force stirs, can enumerate in the cylindric drum of horizontal type, possess hoe shape or shovel shape stirring vane (plough) and cross cutter shape stirring vane (axe), plough is the center low speed rotation with the driving shaft that is configured in horizontal direction, axe is that the center rotates such mixer at a high speed with the driving shaft that is configured in vertical direction, promptly plough blender (trade name for example: plough blender, Pacific Machinery ﹠ Engineering Co., Ltd. makes, trade name: WA, ワ system Japanese firm makes, trade name WA-75, ヤ マ ト Kihan Co., Ltd. manufacturing etc.).According to above-mentioned plough blender, according to the suspension diffusion of plough with mutually combine according to the high speed shear effect of axe, and microparticle agglutination and the aggegation piece that forms in the aggregate particle raw material that contains in the pulverizing shaping raw material obtain the moulding complex that the crushed material of aggegation piece is evenly dispersed.

In addition, can use aptly and in the cylindric drum of longitudinal type, possess the multistage blade that constitutes by bur shape hypomere stirring vane and ring-type epimere stirring vane, this multistage blade is that the center rotates such mixer at a high speed with the driving shaft that is configured in vertical direction, be that (for example Mitsui Mining Co Ltd. BJ Offc makes the Henschel blender, trade name: Mitsui Henschel blender etc.).According to above-mentioned Henschel blender, mutually combine according to the shaping raw material coiling effect upward of hypomere stirring vane and strong shear action according to the epimere stirring vane, and the microparticle agglutination that contains in the pulverizing shaping raw material and the aggegation piece that forms obtain the moulding complex that the crushed material of aggegation piece is evenly dispersed.

But when mixing according to stirring vane, stirring vane so volumetric efficiency are low owing to existing, and adhere to shaping raw material between stirring vane self or container and stirring vane, so the raw material rate of recovery are also poor.In addition, also have the stirring vane abrasion and cause the shaping raw material contamination of heavy.And then there be the poor of peripheral speed in the blade root of stirring vane and periphery, therefore are difficult to disperse equably in container.Thereby, when these aspects become problem, while preferably adopt foregoing surface to aggregate particle raw material to implement the method for the method of lining, classification aggregate particle raw material, utilize ultrasonic wave or jar mill to apply method that pressurization and vibration mixes etc.

For the mixer of the stirring vane with rotation, so long as the rotating speed of stirring vane then is not particularly limited greater than the high speed of about 200rpm, but preferred rotating speed is more than or equal to 500rpm, more preferably 1000～5000rpm.About the peripheral speed of stirring vane without limits, but preferred peripheral speed is more than or equal to 2m/ second, more preferably 3～100m/ second.This be because, if rotating speed less than 5000rpm, perhaps peripheral speed was compared during then with preferred condition less than 2m/ second, the possibility that can not fully pulverize the aggegation piece improves.The upper limit separately is so long as stirring vane Continuous Drive stably is just unqualified, but considers the possibility that the abrasion acceleration of blade, the breakage of blade etc. produce, and is preferably rotating speed smaller or equal to 5000rpm, and peripheral speed is smaller or equal to 100m/ second.Here, the peripheral speed of stirring vane is meant the translational speed of the front end of stirring vane.

Be not particularly limited about mixing time, be preferably 5～30 minutes during for example with 500rpm rotation stirring vane, be preferably 3～20 minutes during with 1000rpm rotation stirring vane.If mixing time is less than above-mentioned scope, then the pulverizing of aggegation piece becomes insufficient easily, may prevent the generation of the internal flaw of honeycomb formed article (and then cellular honeycomb structures), and is therefore also not preferred.If surpass above-mentioned scope, then quicken the abrasion of mixer easily, its wear life may shorten, and is therefore also also not preferred.

In addition, all mixers that in mixed processes, use, the preferred mixer that uses with refrigerating function.This be because, can work steadily in the long term like this, get rid of the problems such as harmful effect of heating to shaping raw material.

When being called " crushed material of aggegation piece " in the present invention, being pulverized fully and got back to the crushed material as the graininess of primary particle, comprised also that the aggegation piece does not have to be pulverized fully but crushed material that its particle diameter diminishes except the aggegation piece.At this moment, the average grain diameter of the crushed material of aggegation piece is preferably smaller or equal to 200 μ m, more preferably smaller or equal to 100 μ m, especially is preferably smaller or equal to 50 μ m.

In the manufacture method of honeycomb formed article of the present invention, sieve with the sieve of complex (dry powder) by the moulding that will in first mixes, obtain with sieve aperture 500 μ m, measure the quality of the residue (aggegation piece) above the sieve, can estimate the admixture (utilizing the pulverizing situation of aggegation piece of mixer etc. or the formedness of pulverizing) of raw material.In the manufacture method of honeycomb formed article of the present invention, preferably be mixed to aggegation piece above the sieve smaller or equal to 1 quality %.More preferably be mixed to smaller or equal to 0.2 quality %.In addition, preferably according to employed shaping raw material, selection can obtain the mixer of this good mixing state at short notice.

In addition, the admixture of raw material can adopt thermobalance evaluation.Specifically, sampling ormal weight (for example 20mg) as the moulding of mixture with complex (dry powder) or moulding with complex (wet-milling), measure the mass loss of the crystallization water etc. of adhesive, raw material with thermobalance (TG).Measure stipulated number (for example 10 times) repeatedly, estimate the deviation of the rate of mass reduction of TG.For example, use the situation of the aluminium hydroxide of easy aggegation, if undercompounding, then aluminium hydroxide segregation, thus cause the deviation of the rate of mass reduction of TG to become big.In the manufacture method of honeycomb formed article of the present invention, the value (in this manual be called TG degree of mixing) of the standard deviation that preferably is mixed to rate of mass reduction after divided by the mean value of rate of mass reduction is for smaller or equal to 0.2.More preferably be mixed to smaller or equal to 0.1.Different with the manufacture method of honeycomb formed article of the present invention, when not carrying out independently mixed processes before mixing operation, the TG degree of mixing is about 0.5, is difficult to make the TG degree of mixing smaller or equal to 0.2.Here, much less, use the dry thing of base soil, formed body also can estimate according to the TG degree of mixing.

And then, can use X ray CT to estimate the admixture of raw material.Measure the Density Distribution of honeycomb formed article with X ray CT.If Density Distribution is even, then can be judged as raw material and mixes.The value (in this manual be called X ray CT degree of mixing) of the standard deviation of density measurement value that preferably is mixed to X ray CT after divided by the mean value of the density measurement value of X ray CT is for smaller or equal to 0.2.More preferably be mixed to smaller or equal to 0.1.Here, much less, not only honeycomb formed article even adopt the base soil that utilizes vacuum soil refining machine to be shaped to definite shape, also can be estimated according to the X ray CT degree of mixing.

The manufacture method of honeycomb formed article of the present invention has the effect of the constituent that disperses shaping raw material equably as mentioned above and pulverizes microparticle agglutination and the effect of the aggegation piece that forms.For example, the suitable microcapsules that are made of Foamex as the pore-creating material etc. because its proportion is little, therefore are difficult to be evenly dispersed in the shaping raw material in the past, but according to the manufacture method of honeycomb formed article of the present invention, the constituent that this proportion is little also can disperse equably.

Thereby the manufacture method of honeycomb formed article of the present invention can be used for using the microcapsules that are made of the Foamex situation as the pore-creating material at shaping raw material aptly.For this manufacture method, can avoid moulding with the pore-creating material containing ratio of complex (and then base soil, honeycomb formed article) according to the different inconsistent phenomenons that cause in position, therefore can obtain not can be because of the inconsistent cellular honeycomb structures of the position difference porosity, in that it is preferred aspect this.

Forming method as base soil, when adopting when using the nozzle that has with the slit of next door complementary shape to carry out the method for extrusion molding, preferably use to contain as aggregate particle raw material and passed through the raw material of sieve aperture smaller or equal to the powder of 4/5 sieve of nozzle slot width to base soil.More preferably use to contain and passed through the raw material of sieve aperture smaller or equal to the powder of 1/2 sieve of nozzle slot width.By removing the corase particles component in the aggregate particle raw material in advance, can prevent more effectively that honeycomb formed article (and then cellular honeycomb structures) from internal flaw taking place.

Here, use " raw material that contains the powder that has passed through sieve " to be meant, as long as the aggregate particle raw material with corase particles component by sieve, for the particulate raw material that does not have the corase particles component (aluminium oxide or aluminium hydroxide etc.), then not necessarily needs to pass through sieve.

(ii) mixing operation

Mixing operation is the operation that obtains base soil in second manufacture method of honeycomb formed article of the present invention in mixed processes by the mixing moulding that obtains with complex (wet-milling), in first manufacture method of honeycomb formed article of the present invention, it is the moulding that obtains in mixed processes to be added water with complex (dry powder) carry out the mixing operation that obtains base soil.Here, in first manufacture method of honeycomb formed article, except water, in this mixing operation, also can add dispersant, additive etc., the content (omit and describe) that related content can illustrate with reference to second manufacture method of honeycomb formed article (consider) in mixed processes.

Mixingly can use known in the past mixing roll, for example blender in Sigma's kneader, the spot uncle, the spiral mixing roll etc. extruded carry out.

In the manufacture method of honeycomb formed article of the present invention, be not particularly limited, but preferred foregoing mixed processes and this mixing operation adopt device separately to carry out respectively, carry out the mixer of mixed processes and carry out the mixing roll of mixing operation by online.This is can reduce particulate and recondense the possibility that forms the aggegation piece owing to being accompanied by conveying.

(iii) soil refines operation

Soil refining operation is that the base earth forming that will obtain as mentioned above is the operation of regulation shape.Shape about base soil is not particularly limited, but the preferably drum shape.

The soil refining can be used known in the past native refining machine, for example can extrude native refining machine and carries out by screw type.Especially, if use and to possess the vacuum decompression device that is used for removing the air that moulding contains with complex (and then base soil) the soil refining machine (the native refining machine of so-called vacuum) of (for example vavuum pump etc.), can access then that defective is few, the base soil of good forming ability, so it is preferred.

(iv) molding procedure

Molding procedure for by the base earth forming that will obtain as mentioned above for separately and be formed with the honeycomb shape of a plurality of cells by the next door, and carry out drying, obtain the operation of honeycomb formed article.

Cellular honeycomb structures 1 for example shown in Figure 2, said in this specification " honeycomb shape " are meant the shape of being separated and formed a plurality of cells 3 by next door 4.Global shape for honeycomb formed article is not particularly limited, for example except shown in Figure 2 cylindric, can also enumerate shapes such as quadrangular shape, triangular column.In addition, be not particularly limited, for example except quadrangle cell shown in Figure 2, can also enumerate shapes such as hexagon cell, triangle cell about the little chamber shape (the little chamber shape on the cross section vertical) of honeycomb formed article with the formation direction of cell.

Method about moulding is not particularly limited, and can use the known in the past methods of forming such as extrusion molding, injection moulding, extrusion forming, and the wherein preferred nozzle that has with the slit of next door complementary shape that uses carries out extrusion molding to the base soil that obtains as mentioned above.According to this method, can obtain having little chamber shape, the next door thickness of expectation, the honeycomb formed article of cell density easily.

In addition, use when having the nozzle of above-mentioned slit, be not particularly limited about the mode that imports the dorsal pore of base soil to this slit.For example can use a slit intersection point at interval and the nozzle of dorsal pore is set, the nozzle that also can use all intersection points at slit that dorsal pore is set carries out extrusion molding.Preferred nozzle is the nozzle that is provided with dorsal pore at all intersection points of slit.The situation of the nozzle of the slit intersection point in interval, the crimping point of base soil becomes the intersection point of cell, and base soil is assembled and crimping from four direction, therefore when mobile difference, be difficult to balancedly crimping, if crimping is harmonious poor, then produce defective at intersection point easily, this defective can cause high isostatic strength to descend.If use the nozzle that is provided with dorsal pore at all intersection points of slit, just can crimping at intersection point base soil, even therefore produce defective, also be difficult for making high isostatic strength to descend.

And then though without limits, preferred use forms the nozzle of R (being provided with curved surface) at least a portion in the bight of the cell piece that forms slit.More preferably use the bight of whole cell pieces all to form the nozzle of the form of R.The bight of the cell piece by making nozzle forms R, the enlarged areas of the intersection point portion of nozzle, and the mobile of base soil improves, and therefore is difficult to form at honeycomb formed article internal flaws such as fragment, burr.In addition, because the intersection point portion of honeycomb formed article is enhanced, so the intensity of honeycomb formed article improves, and then can improve high isostatic strength.

For nozzle, if at all intersection points of slit dorsal pore is set, then the distance of outlet shortens from the dorsal pore to the slit, and if form R in the bight of the cell piece that forms slit, then the mobile of base soil becomes more level and smooth.Therefore,, also can keep containing the flowing of base soil of this aggegation piece well, be difficult to make the aggegation piece to rest in the nozzle even the aggegation piece enters in the nozzle.If the aggegation piece stays for some time in nozzle, then base soil flowability herein will descend, and causes the crimping decline of base soil, when causing moulding the next door break, dry or when burning till the next door break.If use whole intersection points all to be provided with dorsal pore, and form the nozzle of R in the bight of the cell piece that forms slit, then can suppress to take place these problems at slit.

Be not particularly limited for the device that carries out extrusion molding, can use known in the past extrusion shaping machine (for example piston type extrusion shaping machine etc.), wherein preferably use the twin shaft continuous forming machine.The twin shaft continuous forming machine is compared with other extrusion shaping machines, is preferred from the aspect that can access uniform formed body.

In addition, also preferred one is carried out foregoing mixing operation and this molding procedure continuously.This be because, mixing operation and molding procedure are carried out integratedly, the productivity ratio excellence.As the mixing and molding machine of realizing this operation, can enumerate twin shaft continuous mixing extrusion shaping machine.

When carrying out extrusion molding, preferably base soil is extruded by nozzle by the back from the sieve of sieve aperture 160～278 μ m.Like this,, also can remove this aggegation piece, can prevent more positively that therefore honeycomb formed article (and then cellular honeycomb structures) from internal flaw taking place just in case in above-mentioned mixed processes, fail to pulverize the aggegation piece.If the sieve aperture of sieve is less than above-mentioned scope, then sieve is damaged easily, and is therefore also not preferred; If surpass above-mentioned scope, then be difficult to remove the aggegation piece, may prevent that therefore honeycomb formed article (and then cellular honeycomb structures) from internal flaw taking place, also also not preferred.

Be not particularly limited for drying means, can use known in the past seasonings such as heated-air drying, microwave drying, dielectric drying, drying under reduced pressure, vacuum drying, freeze drying.But, from whole honeycomb formed article can be rapidly and dry equably aspect consider, preferred compositions the drying means of heated-air drying and microwave drying or dielectric drying.

(2) manufacture method of amplifier case

In the manufacture method of amplifier case of the present invention, manufacture method according to above-mentioned honeycomb formed article obtains honeycomb formed article, obtain cellular honeycomb structures by burning till this honeycomb formed article, with a side opening portion of a plurality of cells of this cellular honeycomb structures and the opposite side peristome ground sealing of hole that intermeshes, obtain plugged honeycomb structure, by burning till this plugged honeycomb structure, obtain amplifier case, constituting when the processed fluid that imports to a part of cell flows into the cell of adjacency through porous wall of described amplifier case, the field trash next door is captured.This manufacture method owing to use the honeycomb formed article that internal flaw is few and intensity is high, therefore can produce the excellent amplifier case of strainability (arresting efficiency).

Method about ground sealing of hole that a side opening portion of a plurality of cells of cellular honeycomb structures and opposite side peristome are intermeshed, be not particularly limited, can enumerate following method, promptly paste adhesive tape in a side end face of cellular honeycomb structures, only the part of the cell correspondence of the needs sealing of hole of this adhesive tape is carried out perforate and as mask according to the Laser Processing that utilizes image to handle etc., the end face that is pasted with the cellular honeycomb structures of this mask is immersed in the ceramic slurries, the cell that needs sealing of hole to cellular honeycomb structures is filled ceramic slurries, form sealing of hole portion, after the opposite side end face of cellular honeycomb structures carried out same operation, drying sealing of hole portion burns till.

The pottery slurries can be made by mixing at least aggregate particle raw material and decentralized medium (for example water etc.).And then, also can add additives such as adhesive, dispersant as required.Kind for aggregate particle raw material is not particularly limited, but can use aptly and the same material of aggregate particle raw material that is used as the honeycomb formed article raw material.As adhesive, can use resins such as polyvinyl alcohol, methylcellulose; As dispersant, can use special carboxylic acid type high molecular surfactant.

The viscosity of pottery slurries preferably is adjusted in the scope of 5～50Pas, more preferably is adjusted in the scope of 10～30Pas.If the viscosity of ceramic slurries is low excessively, then there is the tendency that shrinks defective easily.The viscosity of slurries can be regulated according to the ratio of for example aggregate particle raw material and decentralized medium (for example water etc.) or amount of dispersant etc.

Burn till and be meant that sintering stiffener particle raw material makes it densified, to guarantee the operation of prescribed strength.Firing condition (temperature and time), according to the burning till of honeycomb formed article, sealing of hole portion burn till and constitute its kind of aggregate particle raw material and different, therefore can select felicity condition according to the kind of employed aggregate particle raw material.For example, when using the cordierite raw material, preferably burnt till 3～7 hours 1410～1440 ℃ temperature as aggregate particle raw material.If the not enough above-mentioned scope of firing condition (temperature and time), then the sintering of aggregate particle raw material may be insufficient, and is therefore also not preferred; If surpass above-mentioned scope, then the cordierite of Sheng Chenging may fusion, so also also not preferred.

In addition, if before burning till or in the temperature-rise period that burns till, burn and remove the operation (calcining) of the organic matter (adhesive, pore-creating material, dispersant etc.) in honeycomb formed article or the sealing of hole portion, then can further promote organic removing, therefore preferred.The ignition temperature of adhesive is about 200 ℃, and the ignition temperature of pore-creating material is about 300 ℃, so calcining heat can be about 200～1000 ℃.Be not particularly limited for calcination time, but be generally about 10～100 hours.

In addition, adopt following method also can produce amplifier case of the present invention, promptly the manufacture method according to above-mentioned honeycomb formed article obtains honeycomb formed article, with a side opening portion of a plurality of cells of this honeycomb formed article and the opposite side peristome ground sealing of hole that intermeshes, obtain the sealing of hole honeycomb formed article, by burning till this sealing of hole honeycomb formed article, obtain amplifier case, constituting when the processed fluid that imports to a part of cell flows into the cell of adjacency through porous wall of described amplifier case, the field trash next door is captured.

According to aforesaid manufacture method, identical with the manufacture method of front, owing to use the honeycomb formed article that internal flaw is few and intensity is high, therefore can produce the excellent amplifier case of strainability (arresting efficiency), in addition owing to carry out burning till of honeycomb formed article and burning till of sealing of hole portion simultaneously, therefore can reduce firing operation, have the advantage that can obtain amplifier case easily.Here, adopt this method sealing of hole, burn till, can fully similarly carry out with the method for front.

(3) amplifier case

Amplifier case of the present invention, it constitutes has cellular honeycomb structures and sealing of hole portion, described cellular honeycomb structures has a plurality of cells that separately formed by porous wall, described sealing of hole portion carries out sealing of hole to a side opening portion and the opposite side peristome of a plurality of cells with intermeshing, and when the processed fluid that imports to a part of cell flowed into the cell of adjacency through the next door, the field trash next door was captured; Cigarette ash leakage cell ratio by cigarette ash printing test evaluation is smaller or equal to 1 cell/1000 cells.

The present invention's said " cigarette ash printing test " is meant, in a side end face side direction cell of amplifier case, flow into particle, check the method (for example with reference to special fair 5-658 communique) of the internal flaw of amplifier case according to driving fit at the image of the particle that sieve trapped with aeration of opposite side end face side.

Cigarette ash printing test can use checkout gear 31 as shown in Figure 3 to carry out, its have with the state of gas-tight ground seal perimeter portion support amplifier case 21 support platform 32, be connected the supply of supporting on the platform 32 contain the gas of graphite cigarette ash generator 34, capture graphite particle sieve 36, reclaim aiutage 38 through the gas of sieve 36.Here, tracheae, symbol 42 expression transfer valves, symbol 44 expression blast pipes, the fastening net of symbol 46 expressions are given in symbol 40 expressions.

That is, supporting to place amplifier case on the platform 32, behind the upper surface of amplifier case driving fit sieve 36, installation aiutage 38 above this sieve 36 is fixed into the state that is clamped between support platform 32 and the aiutage 38 with amplifier case and sieve 36.In this state the gas of supplying with from cigarette ash generator 34 that contains graphite particle in a side end face side inflow cell 23 of amplifier case 21, observe the image of the graphite particle that driving fit captured at the sieve with aeration 36 of opposite side end face side.

When the next door of amplifier case 21 24 grades did not have internal flaw fully, graphite particle was caught by the next door 24 of amplifier case 21, therefore can not form the image of graphite particle at sieve 36.On the other hand, if there is internal flaw in the next door of amplifier case 21 24 grades, then the next door 24 of graphite particle by amplifier case 21 flows into the cell 23 of adjacency, captured by sieve 36, therefore at the image of sieve 36 formation graphite particles.

After carrying out aforesaid detection, be cigarette ash and leak the cell ratio being formed at value that the little number of chambers that is formed with the graphite particle image on the sieve is scaled the little number of chambers of per 1000 cells.Amplifier case of the present invention leaks the cell ratio with the cigarette ash about 2～20 cells of amplifier case/1000 cells in the past and has brought up to level smaller or equal to 1 cell/1000 cells.This amplifier case, internal flaw is few, strainability (arresting efficiency) excellence.

In addition, amplifier case of the present invention, being preferably at least, cellular honeycomb structures (being the part beyond the sealing of hole portion) is made of cordierite.Cordierite is because thermal coefficient of expansion is little, so the resistance to sudden heating excellence, can prevent the crackle that thermal stress causes effectively, is preferred therefore.

Embodiment

Below, specifically describe the present invention by embodiment, but the present invention is not limited to these embodiment.Here, about the average grain diameter of putting down in writing in embodiment shown below and the comparative example, use with the liquid phase sedimentation of Stokes as measuring principle, utilize the value of 50% particle diameter that the X ray through mode particle size distribution device that the X ray penetrant method detects (trade name for example: セ デ イ グ ラ Off 5000-02 type, (strain) Shimadzu Seisakusho Ltd. make etc.) measures.

Embodiment 1

[manufacturing of honeycomb formed article]

(shaping raw material)

As aggregate particle raw material, prepare cordierite raw material with the ratio mixing of talcum (average grain diameter 21 μ m) 40 quality %, kaolin (average grain diameter 11 μ m) 18.5 quality %, aluminium oxide (average grain diameter 7 μ m) 14.0 quality %, aluminium hydroxide (average grain diameter 2 μ m) 15 quality %, silica (average grain diameter 25 μ m) 12.5 quality %.And, with respect to above-mentioned aggregate particle raw material 100 mass parts, prepare as the first pore-creating material carbon (coke: average grain diameter 27 μ m) 25.0 mass parts, as pet resin (average grain diameter 37 μ m) 10.0 mass parts of the second pore-creating material, as hydroxypropyl methylcellulose 8.0 mass parts of adhesive.And then, prepare as dispersant (surfactant) fatty acid soaps (potassium laurate) 0.01 mass parts, as water 35 mass parts of decentralized medium.

(mixed processes: first mixes)

Use jar mill as mixer, above-mentioned aggregate particle raw material is added the first pore-creating material and the second pore-creating material, mixed again 10 minutes, obtain moulding complex (dry powder).Here, the rotating speed of jar mill is 40rpm.

(according to the evaluation of the aggegation piece on the sieve)

The moulding that obtains is taken out from jar mill with complex (dry powder),, measure the quality of the residue (aggegation piece) on the sieve, obtain the residue ratio (quality %) on the sieve, estimate its admixture with the sieve sieving 100g of sieve aperture 500 μ m.Show the result in the table 1.

Table 1

The test sequence number	Degree of mixing is estimated			Goods are estimated
						Aggegation piece (quality %) on the sieve	The TG degree of mixing	The X ray CT degree of mixing	Cigarette ash leaks cell ratio (1/1000)	High isostatic strength (MPa)
	Embodiment 1	0.0	0.05	0.09	0.2						1.9
Embodiment 2						0.0	0.03	0.05	0.1	1.8
	Embodiment 3	0.0	0.02	0.03	0.0						2.3
Embodiment 4						0.0	0.01	0.02	0.0	2.1
	Embodiment 5	0.0	0.01	0.02	0.0						2.2
Embodiment 6						-	0.03	0.05	0.0	2.5
	Embodiment 7	0.0	0.02	0.03	0.0						2.2
Embodiment 8						1	0.20	0.34	1.0	1.1
	Embodiment 9	0.07	0.08	0.14	0.2						1.5
Embodiment 10						0.0	0.03	0.05	0.0	2.3
	Embodiment 11	0.1	0.05	0.09	0.1						1.9
Embodiment 12						0.0	0.03	0.05	0.0	2.2
	Embodiment 13	0.2	0.12	0.20	0.3						1.4
Embodiment 14						0.05	0.06	0.10	0.1	1.8
	Embodiment 15	0.07	0.07	0.12	0.9						1.0
Comparative example 1						5.0	0.60	1.02	4.0	0.7
	Comparative example 2	-	-	-	-						-
Comparative example 3						1.5	0.30	0.51	1.5	0.9
	Comparative example 4	3	0.50	0.85	1.9						0.8

(mixed processes: second mixes)

Then, the mixed solution of above-mentioned dispersant and decentralized medium is sprayed, added in the above-mentioned jar mill (mixer), similarly mixed 2 minutes, obtain moulding complex (wet-milling).

(according to the evaluation of TG degree of mixing)

The moulding usefulness complex (wet-milling) that obtains is taken out 20mg from jar mill, the mass loss of the crystallization water of 10 adhesives of usefulness thermobalance (TG) mensuration, raw material etc.In 10 times were measured, the ratio with respect to the loss quality of original quality obtained respectively was as rate of mass reduction, and the value (TG degree of mixing) of the standard deviation of obtaining this rate of mass reduction after divided by the mean value of rate of mass reduction, estimated its admixture.Show the result in the table 1.

(mixing operation, soil refining operation)

Then, to the moulding complex (wet-milling) that obtains, it is mixing to use Sigma's kneader to carry out, and then uses the spiral mixing roll (vacuum soil refining machine) of extruding that possesses the vacuum decompression device to carry out the soil refining, obtains being extruded into the base soil of cylindric (external diameter 300mm φ).

(according to the evaluation of X ray CT degree of mixing)

Use X ray CT to measure the density of the cylindric base soil that 10 places obtain, obtain this 10 place with the standard deviation of the density measurement value value (X ray CT degree of mixing) after divided by the mean value of the density measurement value of X ray CT, estimate the admixture of raw material.Show the result in the table 1.Here, the analytical unit (zone) of X ray CT mensuration is 1mm * 1mm * 2mm.

(molding procedure)

Then, use the slit have with the shape of the next door complementation of honeycomb formed article as nozzle, all intersection point portions at slit possess dorsal pore, implemented the nozzle of R processing (forming R) in the bight of the cell piece that constitutes cell, and use the piston type extrusion shaping machine as make-up machine, carry out extrusion molding, obtain being separated and forming the article shaped of a plurality of cells by the base soil that obtains by the next door.At this moment, at the sieve of the internal configurations sieve aperture 233 μ m of piston type extrusion shaping machine, extrude from nozzle after making base soil by this sieve.This article shaped is carried out dielectric drying, heated-air drying, thereby bone dry obtains honeycomb formed article.Cut off two end faces of this honeycomb formed article, make it become given size.

The honeycomb formed article that obtains, end face (cell opening surface) is shaped as the circle of external diameter 229mm φ, and length is 254mm, and cell is shaped as the square chamber of 1.16mm * 1.16mm, next door thickness is 300 μ m, and cell density is about 300 cell/square inch (46.5 cells/cm ²), total little number of chambers is 19085 cells.

[manufacturing of amplifier case]

One side opening portion of a plurality of cells by making the honeycomb formed article that obtains as mentioned above and the opposite side peristome ground sealing of hole that intermeshes obtains the sealing of hole honeycomb formed article.Method as sealing of hole adopts following method, promptly paste adhesive tape in a side end face of honeycomb formed article, only the part of the cell correspondence of the needs sealing of hole of this adhesive tape is carried out perforate and as mask according to the Laser Processing that utilizes image to handle etc., the end face that is pasted with the honeycomb formed article of this mask is immersed in the ceramic slurries, the cell that needs sealing of hole to honeycomb formed article is filled ceramic slurries, forms sealing of hole portion.

The pottery slurries are to obtain as modulated, promptly, use the aggregate particle raw material identical as aggregate particle raw material with honeycomb formed article, with respect to aggregate particle raw material 100 mass parts, interpolation is as methylcellulose 0.5 mass parts of adhesive, as the special carboxylic acid type high molecular surfactant (trade name: Port イ ズ 530 of dispersant, Kao Corp makes) 0.3 mass parts, as water 50 mass parts of decentralized medium, mixed 30 minutes.Its viscosity is 25Pas.

The sealing of hole honeycomb formed article that heated-air drying obtains as mentioned above, behind the bone dry, burn till 7 hours these sealing of hole honeycomb formed articles 1420 ℃ temperature, obtain amplifier case, constituting when the processed fluid that imports to a part of cell sees through the porous wall inflow in abutting connection with cell of this amplifier case, the field trash next door is captured.

(according to the evaluation of cigarette ash printing test)

To the amplifier case that obtains, calculate cigarette ash according to cigarette ash printing test and leak the cell ratio, estimate the internal flaw degree of amplifier case, i.e. the strainability of filter (arresting efficiency).

Cigarette ash printing test is based on the method for putting down in writing in the special fair 5-658 communique, use checkout gear 31 as shown in Figure 3, its have with the state of gas-tight ground seal perimeter portion support amplifier case 21 support platform 32, be connected the supply of supporting on the platform 32 contain the gas of graphite particle cigarette ash generator 34, capture graphite particle sieve 36 (use calico), reclaim aiutage 38 through the gas of sieve 36.

At first,, aiutage 38 is installed, amplifier case 21 is fixed into the state that is clamped between support platform 32 and the aiutage 38 in the upper surface of amplifier case 21 at the amplifier case 21 of supporting to place on the platform 32 the foregoing description 1 and comparative example 1.The gas that contains graphite particle that to supply with about 70g/ hour amount from cigarette ash generator 34 is in a side end face side inflow cell of amplifier case 21 in this state, piles up the cigarette ash of the amount that 5g/ rises in amplifier case 21.

Then, behind the upper surface of amplifier case 21 driving fit sieve 36, aiutage 38 is installed once again above the sieve 36, amplifier case 21 and sieve 36 are fixed into the state that is clamped between support platform 32 and the aiutage 38 from this.The gas that contains graphite particle that to supply with about 70g/ hour amount from cigarette ash generator 34 is in a side end face side inflow cell 23 of amplifier case 21 in this state, observe the image (being stain) of the graphite particle that driving fit captured at the sieve with aeration 36 of opposite side end face side, count its quantity.

(according to the evaluation of high isostatic strength test)

To the amplifier case that obtains, the car gage JASO standard M505-87 that can issue according to the automatic driving skills art of civic organization implements the test of high isostatic strength.This test is to add sample (amplifier case) in the cylindrical container of rubber, with aluminium sheet as lid, carrying out each test to equal pressure pressurization compression in water, is to have simulated the test that the compressive load of amplifier case when being converted the device tank body and having controlled outer peripheral face increases the weight of.Moulding pressure value representation when result of the test is destroyed with amplifier case separately.Show the result in the table 1.

Embodiment 2,3

Except the ratio with the surfactant in the shaping raw material is set at 0.1 mass parts (embodiment 2), 1 mass parts (embodiment 3), make honeycomb formed article similarly to Example 1, make amplifier case according to the honeycomb formed article that obtains, in these processes, carry out each and estimate.Show the result in the table 1.

Embodiment 4

Aluminium hydroxide as shaping raw material uses the aluminium hydroxide that carries out surface modification with stearic acid, and the ratio of the surfactant in the shaping raw material is set at 0.1 mass parts, in addition, make honeycomb formed article similarly to Example 1, make amplifier case according to the honeycomb formed article that obtains, in these processes, carry out each and estimate.Show the result in the table 1.

Embodiment 5

Aluminium hydroxide as shaping raw material uses the aluminium hydroxide of removing the aggegation piece in advance with the classification of free vortex type centrifugal classifying, and the ratio of the surfactant in the shaping raw material is set at 0.1 mass parts, in addition, make honeycomb formed article similarly to Example 1, make amplifier case according to the honeycomb formed article that obtains, in these processes, carry out each and estimate.Show the result in the table 1.

Embodiment 6

In mixed processes (first mixes), use jar mill as mixer, in removing the aggregate particle raw material of aluminium hydroxide, add the first pore-creating material and the second pore-creating material, mixed 5 minutes, obtain moulding complex (dry powder); In mixed processes (second mixes), the ratio of the surfactant in the shaping raw material (dispersant) is set at 0.1 mass parts, and in the mixed solution of dispersant and decentralized medium, add aluminium hydroxide, disperse, it is added in the above-mentioned jar mill then with ultrasonic wave, mixed 5 minutes, obtain moulding with complex (wet-milling), in addition, make honeycomb formed article similarly to Example 1, make amplifier case according to the honeycomb formed article that obtains, in these processes, carry out each and estimate.Show the result in the table 1.

Embodiment 7

The ratio of the surfactant in the shaping raw material (dispersant) is set at 1 mass parts, and then, in mixing operation and molding procedure, use twin shaft continuous mixing extrusion shaping machine, one is carried out mixing and moulding continuously, in addition, makes honeycomb formed article similarly to Example 1, make amplifier case according to the honeycomb formed article that obtains, in these processes, carry out each and estimate.Show the result in the table 1.

Embodiment 8～13

The mixer in the change mixed processes, make honeycomb formed article similarly to Example 1, make amplifier case, in these processes, carry out each and estimate according to the honeycomb formed article that obtains.Show the result in the table 1.Here, in embodiment 8, using super blender (manufacturing of カ ワ Co., Ltd.), is that 500rpm, peripheral speed are to mix under the 2m/ condition of second at the rotating speed of stirring vane.In embodiment 9, use super mixer (Pacific Machinery ﹠ Engineering Co., Ltd.'s manufacturing), be that 700rpm, peripheral speed are to mix under the 6m/ condition of second at the rotating speed of stirring vane.In embodiment 10, use ultra high shear omnidirectional blender (thousand generation field skill grind industrial Co., Ltd. make), be that 4000rpm, peripheral speed are to mix under the 10m/ condition of second at the rotating speed of stirring vane.In embodiment 11, use mixing high-speed stirred comminutor (manufacturing of De Le ト Application), be that 1000rpm, peripheral speed are to mix under the 7m/ condition of second at the rotating speed of stirring vane.In embodiment 12, use vertical-type comminutor (manufacturing of パ ウ レ Star Network Co., Ltd.), be that 5000rpm, peripheral speed are to mix under the 9m/ condition of second at the rotating speed of stirring vane.In embodiment 13, use Henschel blender (trade name: Mitsui Henschel blender, Mitsui Mining Co Ltd. BJ Offc's manufacturing), be that 600rpm, peripheral speed are to mix under the 4.5m/ condition of second at the rotating speed of stirring vane.

Embodiment 14

In shaping raw material, making the amount of the first pore-creating material (carbon) is 5.0 mass parts with respect to aggregate particle raw material 100 mass parts, use acrylic resin system microcapsule (average grain diameter 50 μ m) as the second pore-creating material, and making its amount is 2.2 mass parts with respect to aggregate particle raw material 100 mass parts, and making the amount of the dispersant (surfactant) in the shaping raw material is 0.1 mass parts.In addition, use plough blender (trade name: プ ロ one シ エ ア ミ キ サ as mixer, Pacific Machinery ﹠ Engineering Co., Ltd. makes), in mixed processes, aggregate particle raw material is added first pore-creating material (carbon) and the adhesive, mix after 3 minutes, and then add the second pore-creating material and mixed 3 minutes.In addition, the plough blender stirring condition be, the plough driving shaft rotating speed be 100rpm, the rotating speed of axe driving shaft is 3000rpm, the peripheral speed of axe driving shaft is 40m/ second.Except each above-mentioned condition, make honeycomb formed article similarly to Example 1, make amplifier case according to the honeycomb formed article that obtains, in these processes, carry out each and estimate.Show the result in the table 1.

Embodiment 15

Mixer in the change mixed processes, and then in molding procedure, use the slit have with the shape of the next door complementation of honeycomb formed article as nozzle, a slit intersection point possesses dorsal pore at interval, and do not implement the nozzle of R processing in the bight of the cell piece that constitutes cell, in addition, make honeycomb formed article similarly to Example 1, make amplifier case according to the honeycomb formed article that obtains, in these processes, carry out each and estimate.Show the result in the table 1.Here, the mixer that uses is super mixer (Pacific Machinery ﹠ Engineering Co., Ltd.'s manufacturing), and the rotating speed of stirring vane is 700rpm, peripheral speed 20m/ second.

Comparative example 1

The amount of the dispersant in the shaping raw material (surfactant) is set at 0.1 mass parts, and use Sigma's kneader to mix 60 minutes as mixer, in addition, make honeycomb formed article similarly to Example 1, make amplifier case according to the honeycomb formed article that obtains, in these processes, carry out each and estimate.Show the result in the table 1.

Comparative example 2

Except the ratio with the surfactant in the shaping raw material is set at 2 mass parts, make honeycomb formed article similarly to Example 1, make amplifier case according to the honeycomb formed article that obtains, in these processes, carry out each and estimate.Show the result in the table 1.Yet wet-milling becomes state of aggregation in jar mill, fails to take out, and does not have moulding, can't obtain filter.

Comparative example 3,4

The mixer in the change mixed processes, make honeycomb formed article similarly to Example 1, make amplifier case, in these processes, carry out each and estimate according to the honeycomb formed article that obtains.Show the result in the table 1.Here, in comparative example 3, using Nauta mixer (manufacturing of ホ ソ カ ワ ミ Network ロ Application Co., Ltd.), is that 300rpm, peripheral speed are to mix under the 1.5m/ condition of second at the rotating speed of stirring vane.In comparative example 4, use ribbon mixer (manufacturing of ダ Le ト Application society), be that 100rpm, peripheral speed are to mix under the 0.5m/ condition of second at the rotating speed of stirring vane.

Embodiment 16

Use the slit intersection point in interval and the nozzle that base soil is imported the dorsal pore of slit is set as nozzle, manufacturing sequence according to the honeycomb formed article of embodiment 1, make 10 end faces (cell opening surface) and be shaped as the circle of external diameter 129mm φ, the honeycomb formed article of length 152.4mm, the desired value that makes cell structure is next door thickness 306 μ m (12mil), the about 200 cell/square inches (cpsi) of cell density.Then,, implement sealing of hole, drying separately, burn till, obtain 10 (sample sequence number 1～10) amplifier cases according to the manufacturing sequence of the amplifier case of embodiment 1.The result that the cell structure of amplifier case is carried out actual measurement is average out to next door thickness 313.65 μ m (12.3mil), the about 197 cell/square inches (cpsi) of cell density.

(according to the evaluation of high isostatic strength test)

To 10 samples that obtain, the car gage JASO standard M505-87 that can issue according to the automatic driving skills art of civic organization implements the test of high isostatic strength separately.With the results are shown in the table 2 of embodiment 2, wherein the mean value with 10 samples is shown among Fig. 4.

Embodiment 17

Use all intersection points to be provided with the nozzle that base soil is imported the dorsal pore of slit as nozzle, in addition make 10 (sample sequence number 1～10) amplifier cases similarly to Example 16, implement the high isostatic strength test separately at slit.Here, the result who cell structure is carried out actual measurement is average out to next door thickness 311.1 μ m (12.2mil), the about 191 cell/square inches (cpsi) of cell density.With the results are shown in the table 2 of the embodiment 3 of high isostatic strength test, wherein the mean value with 10 samples is shown among Fig. 4.

Table 2

	The sample sequence number	Embodiment 16	Embodiment 17
				High isostatic strength [MPa]	1	0.7	1.0
2	0.7	1.1
			3		0.6	1.3
4	0.7	1.1
			5		0.8	1.3
6	0.8	1.1
			7		0.8	1.1
8	0.7	0.9
			9		0.6	1.0
10	0.6	1.1
			Ave		0.70	1.10
Max	0.8	1.3
			Min		0.6	0.9
	σ	0.08					0.12
			N	10	10

(investigation)

Can know that from the result of table 1 amplifier case of embodiment 1～15, cigarette ash leak the cell ratio smaller or equal to 1.0 cells/1000 cells, internal flaw is few, strainability (arresting efficiency) excellence.On the other hand, there are many internal flaws in the amplifier case of comparative example 1～4 then more than or equal to 1.5 cells/1000 cells, and strainability (arresting efficiency) is insufficient.

In addition, amplifier case for embodiment 1 and comparative example 1, cut off and the result that part that cigarette ash leaks observes to take place separately be, the amplifier case of embodiment 1 can be seen the aperture about some aperture 0.5mm, it is the degree of the internal flaw that can allow, but the amplifier case of comparative example 1 is then seen burr about many length 10～100mm or fragment etc., has exceeded the degree of the internal flaw that can allow.

Can know that by table 2 and result shown in Figure 4 the minimum of embodiment 17 is not less than the peak of embodiment 16, the mean value of embodiment 17 exceeds embodiment 16 about 57%.Can confirm that if use the nozzle that is provided with dorsal pore at all intersection points of slit, compare with the nozzle that uses the slit intersection point in interval to be provided with dorsal pore, the high isostatic strength of amplifier case is improved.

Utilize possibility on the industry

The manufacture method of honeycomb formed article of the present invention, the amplifier case can be aptly few for the manufacture of internal flaw, that intensity is high and strainability (arresting efficiency) is excellent. In addition, amplifier case of the present invention, can be aptly be used for preventing the environmental protection such as public hazards, retrieve the control of dust that uses from the purposes such as goods of high-temperature gas with and filter for water treatment, especially capture from the diesel particulate filter of the particulate of diesel engine discharging.

Claims

(according to the modification of the 19th of treaty)

1. the manufacture method of (after the revisal) honeycomb formed article, its for use comprise two or more contain average grain diameter smaller or equal to the aggregate particle raw material of the particulate of 10 μ m and the shaping raw material of water, obtain the manufacture method of the honeycomb formed article of honeycomb formed article;

Comprise by mixing described two or more aggregate particle raw material (first mix) and obtain moulding with the mixed processes of complex (dry powder) and by described moulding is carried out the mixing mixing operation that obtains base soil with complex (dry powder) interpolation water;

At least in mixed processes, sneak in the base soil for fear of agglutinator, implement the resulting aggregate particle raw material of lining to the raw material classification of aggregate particle or to the surface of aggregate particle raw material in advance by using before beginning to mix, perhaps adopt while applying the method that pressurization and vibration mixes, suppress to generate agglutinator, and be mixed to the TG degree of mixing smaller or equal to 0.2;

With the base earth forming that obtains thus is the honeycomb shape of being separated and be formed with a plurality of cells by the next door, carries out drying, obtains described honeycomb formed article.

2. the manufacture method of the described honeycomb formed article of (after the revisal) claim 1, the moulding that obtains by first mixing is further added water with complex (dry powder) mix (second mixes), obtain moulding with complex (wet-milling), after this mixing, comprise the mixing operation that obtains base soil by mixing described moulding with complex (wet-milling).

3. (deletion)

4. (deletion)

5. (deletion)

6. (deletion)

7. the manufacture method of (after the revisal) claim 1 or 2 described honeycomb formed articles when adding described water, is further added the surfactant as dispersant.

8. (deletion)

9. (deletion)

10. the manufacture method of the described honeycomb formed article of (after the revisal) claim 1, described pressurization and vibration be by accommodating shaping raw material and roundstone in container, vibrate described container and produce.

The manufacture method of (11. after the revisal) claim 1 or 2 described honeycomb formed articles, described mixed processes use the mixer with stirring vane to carry out, by the rotation of described stirring vane, shaping raw material applied shearing force on one side mix on one side.

(12. deletion)

(13. deletion)

(14. deletion)

15. the manufacture method of (after the revisal) claim 1 or 2 described honeycomb formed articles, described mixed processes and mixing operation are undertaken by separately device respectively, carry out the mixer of described mixed processes and carry out the mixing roll of described mixing operation by online.

16. the manufacture method of (after the revisal) claim 1 or 2 described honeycomb formed articles contains the aluminium oxide (Al of average grain diameter smaller or equal to 10 μ m as described aggregate particle raw material use ₂O ₃) particulate and/or average grain diameter be smaller or equal to the aluminium hydroxide (Al (OH) of 10 μ m ₃) the cordierite raw material of particulate.

(17. deletion)

(18. deletion)

19. the manufacture method of (after the revisal) claim 1 or 2 described honeycomb formed articles is when adding described water, while this water of spraying adds mixing.

(20. deletion)

21. the manufacture method of (after the revisal) claim 1 or 2 described honeycomb formed articles is used to contain as described aggregate particle raw material and has been passed through sieve aperture smaller or equal to the extrusion molding of the honeycomb formed article material with the powder of 4/5 sieve of the slit width of nozzle.

(22. deletion)

(23. deletion)

(24. deletion)

(25. deletion)

(26. deletion)

(27. deletion)

(28. after the revisal) amplifier case, it constitutes has cellular honeycomb structures and sealing of hole portion, described cellular honeycomb structures has a plurality of cells that separately formed by porous wall, described sealing of hole portion carries out sealing of hole to a side opening portion and the opposite side peristome of a plurality of cells with intermeshing, and when the processed fluid that imports to a part of cell flowed into the cell of adjacency through the next door, field trash was captured in described next door; Moreover internal defects is few, and the cigarette ash leakage cell ratio that is printed test evaluation by cigarette ash is smaller or equal to 1 cell/1000 cells.

29. the described amplifier case of claim 28, described at least cellular honeycomb structures is made of cordierite.

The described amplifier case of (30. appending) claim 28, described cellular honeycomb structures is made by claim 1 or 2 described manufacture methods.

Claims (29)

1. the manufacture method of honeycomb formed article, its for use comprise two or more contain average grain diameter smaller or equal to the aggregate particle raw material of the particulate of 10 μ m and the shaping raw material of water, obtain the manufacture method of the honeycomb formed article of honeycomb formed article; Comprise by mixing described two or more aggregate particle raw material (first mix) and obtain moulding with the mixed processes of complex (dry powder) and by described moulding is carried out the mixing mixing operation that obtains base soil with complex (dry powder) interpolation water; With the described base earth forming that obtains is the honeycomb shape of being separated and be formed with a plurality of cells by the next door, carries out drying, thereby obtains honeycomb formed article.

2. the manufacture method of honeycomb formed article, its for use comprise two or more contain average grain diameter smaller or equal to the aggregate particle raw material of the particulate of 10 μ m and the shaping raw material of water, obtain the manufacture method of the honeycomb formed article of honeycomb formed article; Comprise by mix described two or more aggregate particle raw material (first mix) obtain moulding with complex (dry powder) after, further add water and mix (second mixes) and obtain the mixed processes that complex (wet-milling) is used in moulding, and the mixing operation that obtains base soil by mixing described moulding with complex (wet-milling); With the described base earth forming that obtains is the honeycomb shape of being separated and be formed with a plurality of cells by the next door, carries out drying, thereby obtains honeycomb formed article.

3. the manufacture method of claim 1 or 2 described honeycomb formed articles, after described mixing operation and before described formed honeycomb shape, having the base earth forming that will obtain in mixing operation is the soil refining operation of regulation shape.

4. the manufacture method of any described honeycomb formed article of claim 1～3 before described mixed processes, is implemented lining to the surface of described aggregate particle raw material in advance.

5. the manufacture method of any described honeycomb formed article of claim 1～4, before described mixed processes, the described aggregate particle of classification raw material is got rid of the aggegation piece in advance.

6. the manufacture method of any described honeycomb formed article of claim 1～5, in described mixed processes, carry out described first and mix, making described moulding is smaller or equal to 1 quality % with the residue (aggegation piece) of complex (dry powder) on the sieve of sieve aperture 500 μ m.

7. the manufacture method of any described honeycomb formed article of claim 1～6 when adding described water, is further added the surfactant as dispersant.

8. the manufacture method of any described honeycomb formed article of claim 1～7, in described mixed processes, shaping raw material applied pressurization and vibration on one side mix on one side.

9. the manufacture method of the described honeycomb formed article of claim 8, described pressurization and vibration is produced by ultrasonic wave.

10. the manufacture method of the described honeycomb formed article of claim 8, described pressurization and vibration be by accommodating shaping raw material and roundstone in container, vibrate described container and produce.

11. the manufacture method of any described honeycomb formed article of claim 1～7, described mixed processes uses the mixer with stirring vane to carry out, by the rotation of described stirring vane, shaping raw material applied shearing force on one side mix on one side.

12. the manufacture method of the described honeycomb formed article of claim 11 makes described stirring vane be rotated with the rotating speed more than or equal to 500rpm.

13. the manufacture method of the described honeycomb formed article of claim 11 makes described stirring vane be rotated with the peripheral speed more than or equal to 2m/ second.

14. the manufacture method of any described honeycomb formed article of claim 1～13, described mixed processes use the mixer with refrigerating function to carry out.

15. the manufacture method of any described honeycomb formed article of claim 1～14, described mixed processes and mixing operation are undertaken by separately device respectively, carry out the mixer of described mixed processes and carry out the mixing roll of described mixing operation by online.

16. the manufacture method of any described honeycomb formed article of claim 1～15 contains the aluminium oxide (Al of average grain diameter smaller or equal to 10 μ m as described aggregate particle raw material use ₂O ₃) particulate and/or average grain diameter be smaller or equal to the aluminium hydroxide (Al (OH) of 10 μ m ₃) the cordierite raw material of particulate.

17. the manufacture method of any described honeycomb formed article of claim 1～16 contains described aggregate particle raw material, described water as described shaping raw material use, also has the material of pore-creating material and adhesive.

18. the manufacture method of the described honeycomb formed article of claim 17 is used the microcapsules that are made of Foamex as described pore-creating material.

19. the manufacture method of any described honeycomb formed article of claim 1～18 is when adding described water, while this water of spraying adds mixing.

20. the manufacture method of any described honeycomb formed article of claim 1～19, described moulding are to use the extrusion molding that has with the nozzle of the slit of next door complementary shape.

21. the manufacture method of the described honeycomb formed article of claim 20 is used to contain as described aggregate particle raw material and has been passed through the material of sieve aperture smaller or equal to the powder of 4/5 sieve of nozzle slot width.

22. the nozzle that the manufacture method of the described honeycomb formed article of claim 20, described extrusion molding use all intersection points at described slit to be provided with dorsal pore carries out.

23. the manufacture method of any described honeycomb formed article of claim 20～22, at least a portion in the bight of the cell piece of the described slit of formation of described nozzle forms R.

24. the manufacture method of any described honeycomb formed article of claim 20～23, described extrusion molding use the twin shaft continuous forming machine to carry out.

25. the manufacture method of any described honeycomb formed article of claim 20～24 when carrying out described extrusion molding, makes described base soil by behind the sieve of sieve aperture 160～278 μ m, extrudes from described nozzle.

26. the manufacture method of amplifier case, any described manufacture method according to claim 1～25 obtains honeycomb formed article, obtain cellular honeycomb structures by burning till described honeycomb formed article, with a side opening portion of a plurality of cells of described cellular honeycomb structures and the opposite side peristome ground sealing of hole that intermeshes, obtain plugged honeycomb structure, again by burning till described plugged honeycomb structure, obtain amplifier case, constituting when the processed fluid that imports to a part of cell flows into the cell of adjacency through porous wall of described amplifier case, field trash is captured in described next door.

27. the manufacture method of amplifier case, any described manufacture method according to claim 1～25 obtains honeycomb formed article, with a side opening portion of a plurality of cells of described honeycomb formed article and the opposite side peristome ground sealing of hole that intermeshes, obtain the sealing of hole honeycomb formed article, again by burning till described sealing of hole honeycomb formed article, obtain amplifier case, constituting when the processed fluid that imports to a part of cell flows into the cell of adjacency through porous wall of described amplifier case, field trash is captured in described next door.

28. amplifier case, it constitutes has cellular honeycomb structures and sealing of hole portion, described cellular honeycomb structures has a plurality of cells that separately formed by porous wall, described sealing of hole portion carries out sealing of hole to a side opening portion and the opposite side peristome of a plurality of cells with intermeshing, and when the processed fluid that imports to a part of cell flowed into the cell of adjacency through the next door, field trash was captured in described next door; Cigarette ash leakage cell ratio by cigarette ash printing test evaluation is smaller or equal to 1 cell/1000 cells.

29. the described amplifier case of claim 28, described at least cellular honeycomb structures is made of cordierite.

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