WO2013038564A1 - ハニカム構造体の製造方法および排ガス浄化装置の製造方法 - Google Patents
ハニカム構造体の製造方法および排ガス浄化装置の製造方法 Download PDFInfo
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- WO2013038564A1 WO2013038564A1 PCT/JP2011/071272 JP2011071272W WO2013038564A1 WO 2013038564 A1 WO2013038564 A1 WO 2013038564A1 JP 2011071272 W JP2011071272 W JP 2011071272W WO 2013038564 A1 WO2013038564 A1 WO 2013038564A1
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- Prior art keywords
- honeycomb
- honeycomb structure
- honeycomb unit
- adhesive layer
- manufacturing
- Prior art date
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Definitions
- the present invention relates to a method for manufacturing a honeycomb structure and a method for manufacturing an exhaust gas purification device.
- a catalyst carrier capable of treating predetermined components contained in exhaust gas is used in the exhaust gas purification system.
- a honeycomb structure is known as a member for such a catalyst carrier.
- This honeycomb structure has, for example, a plurality of cells (through holes) extending from one end face of the honeycomb structure to the other end face along the longitudinal direction, and these cells carry a catalyst. They are partitioned from each other by cell walls. Therefore, when exhaust gas is circulated through such a honeycomb structure, substances such as HC, CO, and / or NOx contained in the exhaust gas are reformed by the catalyst supported on the cell walls, and these in the exhaust gas are changed. Ingredients can be processed.
- NOx in exhaust gas can be decomposed into nitrogen and water by using ammonia.
- Patent Document 1 discloses a honeycomb structure having a honeycomb unit containing zeolite as inorganic particles.
- Patent Document 2 a phosphate-based zeolite such as SAPO as inorganic particles.
- the honeycomb structure is manufactured, for example, by joining a plurality of honeycomb units containing inorganic particles via an adhesive layer paste to form an assembly.
- the adhesive layer paste used for the bonding process of such a honeycomb structure includes, for example, water, inorganic particles (for example, silica particles), a binder, and the like.
- the adhesive layer paste is dried, degreased, and By solidifying, an adhesive layer is formed and the honeycomb units are firmly bonded to each other.
- the SAPO (silicoalumina phosphate) particles have a characteristic that they shrink in volume when they absorb moisture and expand in volume when they release moisture. Therefore, when the honeycomb structure is bonded using the honeycomb unit containing SAPO particles, the problem that the honeycomb unit breaks easily occurs.
- the present invention has been made in view of such problems, and the present invention provides a method for manufacturing a honeycomb structure that is less likely to be damaged during or after the bonding process of the honeycomb unit as compared with the conventional honeycomb structure.
- the purpose is to provide.
- Another object of the present invention is to provide a method for manufacturing an exhaust gas purification apparatus including such a method for manufacturing a honeycomb structure.
- a method for manufacturing a honeycomb structure having a honeycomb unit including a plurality of cells extending from a first end face to a second end face along a longitudinal direction, each containing a silica alumina phosphate particle and partitioned by cell walls.
- the manufacturing method of the honeycomb structure is as follows: (A) preparing a plurality of honeycomb formed bodies; (B) firing each honeycomb formed body and forming a honeycomb unit having at least one joining surface on which the adhesive layer paste will be installed in the subsequent steps; (C) impregnating the entire honeycomb unit with water; (D) preparing an adhesive layer paste containing at least inorganic particles, a binder, and water; (E) applying the adhesive layer paste to the joint surface of the honeycomb unit and joining the honeycomb units together; (F) drying, degreasing and solidifying the adhesive layer paste to obtain an adhesive layer; And the amount of water to be impregnated is in the range of 15 wt% to 25 wt% with respect to the weight of the dried honeycomb unit.
- a method for manufacturing a honeycomb structure is provided.
- the silicoalumina phosphate particles may have a ratio Si / (Al + P) in a range of 0.11 to 0.33 in terms of molar ratio. .
- the silicoalumina phosphate particles are included in the dry honeycomb unit in a range of 230 g / L to 360 g / L with respect to the entire honeycomb unit. It may be included.
- the step of impregnating the entire honeycomb unit with water in (c) may include a step of immersing each honeycomb unit in water.
- the honeycomb unit may further include an inorganic binder.
- the honeycomb unit may further include inorganic fibers.
- the inorganic fiber may be one or more selected from the group consisting of alumina, silica, silicon carbide, silica alumina, glass, potassium titanate, and aluminum borate.
- a process for manufacturing a honeycomb structure Storing the honeycomb structure in a metal container in a state where a holding sealing material is disposed around the honeycomb structure; and
- a method of manufacturing an exhaust gas purifying apparatus characterized by comprising:
- the present invention it is possible to provide a method for manufacturing a honeycomb structure that is less likely to be damaged during or after the bonding process of the honeycomb unit as compared with a conventional honeycomb structure. Moreover, in this invention, it becomes possible to provide the manufacturing method of an exhaust gas purification apparatus containing the manufacturing method of such a honeycomb structure.
- FIG. 1 is a perspective view schematically showing an example of a honeycomb structure of the present invention.
- FIG. 2 is a perspective view schematically showing an example of a honeycomb unit constituting the honeycomb structure of FIG. 1. It is a flowchart which shows an example of the manufacturing method of the honeycomb structure by this invention.
- FIG. 1 schematically shows an example of the structure of a honeycomb structure according to the present invention.
- FIG. 2 schematically shows an example of a honeycomb unit which is a basic unit of the honeycomb structure shown in FIG.
- the honeycomb structure 100 has two end surfaces 110 and 115.
- the outer peripheral coat layer 120 is provided on the outer peripheral surface of the honeycomb structure 100 excluding both end surfaces.
- the honeycomb structure 100 includes, for example, a plurality of columnar ceramic honeycomb units 130 having a predetermined shape as shown in FIG. 2 via an adhesive layer 150 (in the example of FIG. 1, four honeycomb units having a sectional fan shape). By joining, a cylindrical honeycomb structure is formed.
- the honeycomb unit 130 extends from one end to the other end along the longitudinal direction of the honeycomb unit, and divides the cells from a plurality of cells (through holes) 121 opened at both end surfaces.
- Cell wall 123 Although not limited to this, in the example of FIG. 2, the cross section perpendicular to the longitudinal direction (Z direction) of the cell 121 is substantially square.
- the honeycomb structure having such a honeycomb unit purifies CO, HC, and / or NOx, etc. It can be used as a catalyst support.
- SAPO particles phosphate zeolite particles
- the honeycomb unit 130 includes silico alumina phosphate (SAPO) particles as inorganic particles.
- SAPO silico alumina phosphate
- the constructed honeycomb structure 100 can be used in a urea SCR system having a urea tank.
- urea contained in the urea tank reacts with water in the exhaust gas to generate ammonia (formula (1)).
- ammonia formula (1)
- this ammonia flows into each cell 121 of the honeycomb unit 130 from one end face (for example, the end face 110) of the honeycomb structure 100 together with the exhaust gas containing NOx, due to the catalytic action of SAPO contained in the cell wall 123. Then, the following reactions of the formulas (2-1) and (2-2) occur.
- the purified exhaust gas is discharged from the other end surface of the honeycomb structure 100 (for example, the end surface 115).
- NOx in the exhaust gas can be treated by flowing the exhaust gas through the honeycomb structure 100.
- the honeycomb structure 100 may be configured by joining a plurality of honeycomb units 130 via the adhesive layer 150 and then cutting the outer peripheral side along a predetermined shape.
- the adhesive layer 150 is formed by applying an adhesive layer paste containing water, inorganic particles (for example, silica particles), a binder, and the like to the side surface of the honeycomb unit 130, and drying, degreasing, and solidifying the paste. .
- the SAPO particles have a characteristic that volume contracts when water is absorbed and volume expands when water is released. Accordingly, when SAPO particles are employed as the inorganic particles constituting the honeycomb unit 130, the following problems are likely to occur.
- the adhesive layer paste In the bonding process of the honeycomb structure, when the adhesive layer paste is applied to the side surface of the honeycomb unit 130, a part of the moisture in the adhesive layer paste moves to the honeycomb unit 130 side. Thereby, the phosphate zeolite particles, that is, the honeycomb unit 130 are locally contracted on the contact surface with the adhesive layer paste. Thereafter, when the water moved to the honeycomb unit 130 side evaporates, the SAPO particles are locally expanded. Such a local contraction / expansion cycle of the honeycomb unit 130 may damage the honeycomb unit 130 during or after the bonding process of the honeycomb unit.
- the present invention provides a method for manufacturing a honeycomb structure for obtaining a honeycomb structure in which such problems are reduced or eliminated. That is, in the method for manufacturing a honeycomb structure according to the present invention, as will be described in detail later, in the honeycomb unit 130 containing SAPO particles, the honeycomb unit is significantly damaged during or after the bonding process of the honeycomb unit. A suppressed honeycomb structure 100 can be obtained.
- the honeycomb unit 130 includes SAPO particles. Furthermore, the honeycomb unit 130 may include an inorganic binder and inorganic fibers. The honeycomb unit 130 may further include inorganic particles other than the SAPO particles.
- the SAPO particles preferably have a ratio Si / (Al + P) in the range of 0.11 to 0.33, more preferably in the range of 0.16 to 0.28 in terms of molar ratio.
- the SAPO particles may be ion-exchanged with Fe, Cu, Ni, Co, Zn, Mn, Ti, Ag, or V.
- Fe or Cu is particularly preferable.
- the total amount of inorganic particles including SAPO particles may be included in the honeycomb unit in a range of 230 g / L to 360 g / L with respect to the entire honeycomb unit.
- the SAPO particles are contained in the dried honeycomb unit in a range of 270 g / L to 360 g / L with respect to the entire honeycomb unit.
- the inorganic binder contained in the honeycomb unit is preferably at least one selected from the group consisting of alumina sol, silica sol, titania sol, water glass, sepiolite, attapulgite, and boehmite.
- the inorganic fibers are preferably alumina, silica, silicon carbide, silica alumina, glass, potassium titanate, aluminum borate or the like. These may be used alone or in combination of two or more. Among the inorganic fibers, alumina is desirable.
- the cell density of the honeycomb unit 130 is preferably in the range of 15.5 to 186 cells / cm 2 (100 to 1200 cpsi), and is preferably in the range of 46.5 to 170 cells / cm 2 (300 to 1100 cpsi). More preferably, the range is 62.0 to 155 / cm 2 (400 to 1000 cpsi).
- the thickness of the cell wall 123 of the honeycomb unit 130 is not particularly limited, but the lower limit desirable from the viewpoint of the strength of the honeycomb unit is 0.1 mm, and the upper limit desirable from the viewpoint of the purification performance of the honeycomb structure is 0.4 mm. It is.
- the adhesive layer 150 of the honeycomb structure 100 is formed using the adhesive layer paste as a raw material.
- the thickness of the adhesive layer is preferably in the range of 0.3 to 2.0 mm. If the thickness of the adhesive layer is less than 0.3 mm, sufficient bonding strength cannot be obtained for the honeycomb unit. On the other hand, when the thickness of the adhesive layer exceeds 2.0 mm, the pressure loss of the honeycomb structure increases.
- the number of honeycomb units to be joined is appropriately selected according to the size of the honeycomb structure.
- a pore-forming agent such as balloons, which are fine hollow spheres composed of oxide ceramics, spherical acrylic particles, and graphite, may be added to the adhesive layer paste as a raw material.
- the outer peripheral coat layer 120 of the honeycomb structure 100 includes at least one of the same inorganic particles, inorganic binders, and inorganic fibers as the material constituting the honeycomb unit as described above, and is further formed using a paste containing an organic binder as a raw material. Is done.
- the outer peripheral coat layer 120 may be made of the same material as the adhesive layer 150 or may be a material different from the adhesive layer.
- the outer periphery coating layer paste as a raw material may contain a pore-forming agent such as balloons that are fine hollow spheres containing oxide ceramics, spherical acrylic particles, and graphite.
- the final thickness of the coat layer is preferably 0.1 mm to 2.0 mm.
- FIG. 3 shows a flowchart of an example of a method for manufacturing a honeycomb structure according to the present invention.
- the method for manufacturing a honeycomb structure according to the present invention includes: (A) a step of preparing a plurality of honeycomb formed bodies (step S110); (B) firing each honeycomb formed body and forming a honeycomb unit having at least one joining surface on which the adhesive layer paste will be installed in the subsequent steps (step S120); (C) a step of impregnating the entire honeycomb unit with water (step S130); (D) preparing an adhesive layer paste containing at least inorganic particles, a binder, and water (step S140); (E) applying the adhesive layer paste to the joint surfaces of the honeycomb units, and joining the honeycomb units together (step S150); (F) drying, degreasing and solidifying the adhesive layer paste to obtain an adhesive layer (step S160); In the step (c) of impregnating the entire honeycomb unit with water, the amount of water impregnated is in the
- Step S110 First, extrusion molding or the like is performed using a raw material paste containing inorganic particles as a main component and further added with an inorganic binder and inorganic fibers, if necessary, to produce a honeycomb unit molded body.
- the inorganic particles include SAPO particles.
- the inorganic particles may further include particles such as alumina, silica, titania, ceria, zirconia, and / or mullite.
- an organic binder, a dispersion medium, and a molding aid may be appropriately added to the raw material paste in accordance with the moldability.
- the organic binder is not particularly limited, and examples thereof include one or more organic binders selected from methyl cellulose, carboxymethyl cellulose, hydroxyethyl cellulose, polyethylene glycol, phenol resin, epoxy resin, and the like.
- the blending amount of the organic binder is preferably 1 to 10 parts by weight with respect to 100 parts by weight of the total of the inorganic particles and the inorganic binder.
- the dispersion medium is not particularly limited, and examples thereof include water, organic solvents (such as benzene) and alcohols (such as methanol). Although it does not specifically limit as a shaping
- molding adjuvant For example, ethylene glycol, dextrin, a fatty acid, fatty-acid soap, a polyalcohol etc. can be mentioned.
- the raw material paste is not particularly limited, but is preferably mixed and kneaded.
- the raw material paste may be mixed using a mixer or an attritor, or may be sufficiently kneaded using a kneader.
- molding raw material paste is not specifically limited, For example, it is preferable to shape
- the dryer used for drying is not particularly limited, and examples thereof include a microwave dryer, a hot air dryer, a dielectric dryer, a vacuum dryer, a vacuum dryer, and a freeze dryer.
- the degreasing conditions are not particularly limited, and are appropriately selected depending on the type and amount of the organic substance contained in the honeycomb formed body, but approximately 400 ° C. and 2 hours are preferable.
- a honeycomb formed body having a fan-shaped cross section (center angle 90 °) is manufactured.
- Step S120 Next, the formed body prepared in step S110 is fired to manufacture a honeycomb unit.
- the honeycomb unit has at least one bonding surface on which the adhesive layer paste is to be placed.
- the firing conditions are not particularly limited, but are preferably 600 to 1200 ° C, more preferably 600 to 1000 ° C. This is because if the firing temperature is less than 600 ° C., the sintering does not proceed and the strength as the honeycomb unit is lowered, and if it exceeds 1200 ° C., the sintering proceeds excessively and the purification rate of the exhaust gas is lowered. Because there is.
- each manufactured honeycomb unit is impregnated with water.
- This step is performed to prevent water from being introduced unevenly into the honeycomb unit. That is, by performing this process, when the adhesive layer paste is applied to the bonding side surface of the honeycomb unit in the subsequent step S150, the moisture contained in the adhesive layer paste is removed from the honeycomb unit adhesive layer paste. Adsorption only on the contact portion with the stub is avoided. In addition, such a problem that the honeycomb unit locally shrinks in volume due to such local moisture adsorption, or the honeycomb unit locally expands in volume due to subsequent drying of moisture is suppressed.
- the amount of water introduced into the honeycomb unit is in the range of 15 wt% to 25 wt% with respect to the dried honeycomb unit.
- the SAPO particles in the honeycomb unit adsorb moisture of the adhesive paste, and cracks due to volume changes are likely to occur in the honeycomb unit.
- the maximum amount of water that can be introduced into the honeycomb unit is 25 wt%. Even if more water is introduced, water overflows from the honeycomb unit, and water exceeding this amount is introduced into the honeycomb unit. It is difficult.
- Water is introduced throughout the honeycomb unit.
- the method for introducing water into the honeycomb unit is not particularly limited. However, in the usual case, the easiest method, that is, a method of impregnating the honeycomb unit in water is adopted.
- the method for adjusting the amount of introduced water is not particularly limited.
- the amount of introduced water may be adjusted to a desired value depending on the immersion time of the honeycomb unit in water and / or the conditions of the air blow treatment of the honeycomb unit after immersion (for example, air blow pressure and / or time). good.
- Step S140 Next, a paste for the adhesive layer is prepared.
- the adhesive layer paste has at least inorganic particles, a binder (organic binder and / or inorganic binder), and water.
- the adhesive layer paste may further contain inorganic fibers.
- the inorganic particles for example, alumina particles, silica particles, titania particles, zirconia particles, mullite, and / or zeolite are used.
- the organic binder is not particularly limited, and examples thereof include one or more selected from polyvinyl alcohol, methyl cellulose, ethyl cellulose, carboxymethyl cellulose, and the like. Among organic binders, carboxymethyl cellulose is desirable.
- the inorganic binder is not particularly limited, and examples thereof include alumina sol, silica sol, titania sol, water glass, white clay, kaolin, montmorillonite, sepiolite, attapulgite, and boehmite. These may be used alone or in combination of two or more.
- At least one selected from the group consisting of alumina sol, silica sol, titania sol, water glass, sepiolite, attapulgite, and boehmite is desirable.
- the material of the inorganic fiber is not particularly limited, but for example, alumina, silica, silicon carbide, silica alumina, glass, potassium titanate, aluminum borate or the like is used.
- Step S150 Next, the honeycomb units are joined to each other through the adhesive layer paste prepared in step S140 to form a honeycomb unit assembly (joining step).
- the honeycomb unit contains a sufficient amount of moisture in advance. For this reason, even if an adhesive layer paste is placed on the side surface of the honeycomb unit in this step, this makes it difficult for moisture to be locally adsorbed to the SAPO particles of the honeycomb unit at the adhesive layer paste / honeycomb unit interface. ing.
- honeycomb units are joined with the adhesive layer paste to form a cylindrical honeycomb assembly.
- Step S160 Next, the adhesive layer paste is dried, degreased, and solidified. At this time, the water impregnated in the honeycomb unit in the step (step S130) is also removed.
- the temperature of drying, degreasing, and solidification is not particularly limited, but is preferably in the range of 500 ° C to 900 ° C, for example.
- the adhesive layer paste is dried and solidified to change into an adhesive layer.
- a honeycomb unit having a predetermined shape can be assembled into a predetermined shape (for example, a cylinder), but a plurality of honeycomb units having the same shape (for example, a quadrangular prism) can be assembled, and the outer peripheral surface of the obtained honeycomb unit assembly can be diamond.
- an outer peripheral coat layer may be provided on the outer peripheral surface of the honeycomb structure.
- Example 1 First, SAPO particles 2800 parts by weight (average particle diameter 3 ⁇ m), boehmite (inorganic binder) 1120 parts by weight, alumina fibers 270 parts by weight (average fiber length 100 ⁇ m, average fiber diameter 6 ⁇ m), methylcellulose 380 parts by weight, oleic acid (molding aid) Agent) 310 parts by weight and 2400 parts by weight of water were added and mixed and kneaded to prepare a mixed composition.
- SAPO particles 2800 parts by weight average particle diameter 3 ⁇ m
- alumina fibers 270 parts by weight average fiber length 100 ⁇ m, average fiber diameter 6 ⁇ m
- methylcellulose 380 parts by weight methylcellulose 380 parts by weight
- oleic acid (molding aid) Agent) 310 parts by weight and 2400 parts by weight of water were added and mixed and kneaded to prepare a mixed composition.
- the SAPO particles used were those ion-exchanged with Cu (ion exchange amount: 2.7% by weight).
- the ratio Si / (Al + P) (molar ratio) of the SAPO particles was 0.16.
- this mixed composition was subjected to extrusion using an extruder to obtain a honeycomb formed body.
- honeycomb formed bodies were sufficiently dried using a vacuum microwave dryer, and degreased by holding at 400 ° C. for 2 hours. Thereafter, firing was carried out by holding at 700 ° C. for 2 hours to produce a columnar honeycomb unit (radius 132 mm) having a 1 ⁇ 4 circular fan cross section.
- the cell wall thickness of the honeycomb unit was 0.2 mm, and the cell density was 800 cpsi.
- the water content of the honeycomb unit was determined as follows.
- the amount of SAPO particles contained per liter of the honeycomb unit volume was 330 g.
- the weight (initial weight) of the obtained honeycomb unit was measured.
- honeycomb unit was placed in a water tank so that the longitudinal axis was in the vertical direction, and immersed in water for 5 minutes. Next, it was immersed in water for another 5 minutes, upside down.
- the honeycomb unit was taken out from the water tank, and after the water did not sag, the moisture of the honeycomb unit was sucked and dehydrated using a blower (wind speed 3 m / s). This treatment was carried out for 20 minutes from one end face side of the honeycomb unit. Thereafter, the same treatment was performed for 1 minute from the other end face side of the honeycomb unit.
- honeycomb unit was dried.
- the drying process was performed by placing the honeycomb unit on a table and blowing with a fan for 60 minutes.
- an adhesive layer paste having the following composition was used: Ceramic fiber 16.2 wt%, Silica glass 51.9 wt%, Carboxymethylcellulose 0.1 wt%, Silica sol 28.9 wt%, Polyvinyl alcohol 0.8 wt%, 1.9 wt% nonionic surfactant, Organic balloon 0.2 wt%.
- the adhesive layer paste was dried to form an adhesive layer. The thickness of the adhesive layer was 1.0 mm.
- Example 1 a honeycomb structure according to Example 1 was obtained.
- honeycomb unit portion (honeycomb unit portion; the same applies hereinafter) was visually observed. As a result, cracks and cracks were not observed in the honeycomb structure.
- Example 2 A honeycomb structure was manufactured in Example 2 by the same method as in Example 1. However, in Example 2, the honeycomb unit was dried by placing the honeycomb unit on a table and blowing with a fan for 30 minutes. Other manufacturing conditions are the same as those in Example 1.
- the water content of the honeycomb unit was 20%.
- Example 2 The appearance of the manufactured honeycomb structure according to Example 2 was visually observed. As a result, cracks and cracks were not observed in the honeycomb structure.
- Example 3 A honeycomb structure was manufactured in Example 3 by the same method as in Example 1. However, in Example 3, the honeycomb unit was dried by placing the honeycomb unit on a table and blowing with a fan for 10 minutes. Other manufacturing conditions are the same as those in Example 1.
- the water content of the honeycomb unit was 25%.
- Example 3 The appearance of the manufactured honeycomb structure according to Example 3 was visually observed. As a result, cracks and cracks were not observed in the honeycomb structure.
- Example 4 A honeycomb structure was manufactured in Example 3 by the same method as in Example 1. However, in Example 4, the ratio Si / (Al + P) (molar ratio) in the SAPO particles was 0.23. Other manufacturing conditions are the same as those in Example 1.
- the water content of the honeycomb unit was 15%.
- Example 4 The appearance of the manufactured honeycomb structure according to Example 4 was visually observed. As a result, cracks and cracks were not observed in the honeycomb structure.
- Example 5 A honeycomb structure was manufactured in Example 5 by the same method as in Example 4. However, in Example 5, the honeycomb unit was dried by placing the honeycomb unit on a table and blowing with a fan for 30 minutes. Other manufacturing conditions are the same as in Example 4.
- the water content of the honeycomb unit was 20%.
- Example 5 The appearance of the manufactured honeycomb structure according to Example 5 was visually observed. As a result, cracks and cracks were not observed in the honeycomb structure.
- Example 6 A honeycomb structure was manufactured in Example 6 by the same method as in Example 4. However, in Example 6, the honeycomb unit was dried by placing the honeycomb unit on a table and blowing with a fan for 10 minutes. Other manufacturing conditions are the same as in Example 4.
- the water content of the honeycomb unit was 25%.
- Example 6 The appearance of the manufactured honeycomb structure according to Example 6 was visually observed. As a result, cracks and cracks were not observed in the honeycomb structure.
- Example 7 A honeycomb structure was manufactured in Example 7 by the same method as in Example 1. However, in Example 7, the ratio Si / (Al + P) (molar ratio) in the SAPO particles was 0.28. Other manufacturing conditions are the same as those in Example 1.
- the water content of the honeycomb unit was 15%.
- Example 7 The appearance of the manufactured honeycomb structure according to Example 7 was visually observed. As a result, cracks and cracks were not observed in the honeycomb structure.
- Example 8 A honeycomb structure was manufactured in Example 8 by the same method as in Example 7. However, in Example 8, the honeycomb unit was dried by placing the honeycomb unit on a table and blowing with a fan for 30 minutes. Other manufacturing conditions are the same as in Example 7.
- the water content of the honeycomb unit was 20%.
- Example 8 The appearance of the manufactured honeycomb structure according to Example 8 was visually observed. As a result, cracks and cracks were not observed in the honeycomb structure.
- Example 9 A honeycomb structure was manufactured in Example 9 by the same method as in Example 7. However, in Example 9, the honeycomb unit was dried by placing the honeycomb unit on a table and blowing with a fan for 10 minutes. Other manufacturing conditions are the same as in Example 7.
- the water content of the honeycomb unit was 25%.
- Example 9 The appearance of the manufactured honeycomb structure according to Example 9 was visually observed. As a result, cracks and cracks were not observed in the honeycomb structure.
- Comparative Example 1 A honeycomb structure was produced in Comparative Example 1 by the same method as in Example 1. However, in Comparative Example 1, the honeycomb unit was dried by holding the honeycomb unit in a dryer at 60 ° C. for 40 minutes. Other manufacturing conditions are the same as those in Example 1.
- the water content of the honeycomb unit was 10%.
- Comparative Example 2 A honeycomb structure was produced in Comparative Example 2 by the same method as Comparative Example 1. However, in Comparative Example 2, the ratio Si / (Al + P) (molar ratio) in the SAPO particles was 0.23. Other manufacturing conditions are the same as those in Comparative Example 1.
- the water content of the honeycomb unit was 10%.
- Comparative Example 3 A honeycomb structure was produced in Comparative Example 3 by the same method as in Comparative Example 1. However, in Comparative Example 3, the ratio Si / (Al + P) (molar ratio) in the SAPO particles was 0.28. Other manufacturing conditions are the same as those in Comparative Example 1.
- the water content of the honeycomb unit was 10%.
- Table 1 shows the ratio of SAPO particles Si / (Al + P) (molar ratio) and water content (%) used in manufacturing the honeycomb structures according to Examples 1 to 9 and Comparative Examples 1 to 3. The drying conditions of the honeycomb unit are shown together. Table 1 also shows the appearance observation results (determination results for cracks) of each honeycomb structure.
- the moisture content of the honeycomb unit before the bonding process of the honeycomb unit is 10% (Comparative Examples 1 to 3), and the moisture content of the honeycomb unit is small. It is considered that cracks were generated in the honeycomb unit due to typical contraction / expansion of the SAPO particles.
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Abstract
Description
シリコアルミナリン酸塩の粒子を含み、長手方向に沿って、第1の端面から第2の端面に延伸する複数のセルがセル壁により区画されたハニカムユニットを有するハニカム構造体の製造方法であって、
当該ハニカム構造体の製造方法は、
(a)複数のハニカム成形体を準備する工程と、
(b)各ハニカム成形体を焼成して、以降の工程で接着層用ペーストが設置されることになる少なくとも一つの接合面を有する、ハニカムユニットを形成する工程と、
(c)各ハニカムユニットの全体に水を含浸させる工程と、
(d)少なくとも無機粒子、バインダ、および水を含む接着層用ペーストを準備する工程と、
(e)前記ハニカムユニットの前記接合面に前記接着層用ペーストを塗布し、各ハニカムユニット同士を接合する工程と、
(f)前記接着層用ペーストを乾燥、脱脂、固化して接着層を得る工程と、
を含み、前記(c)の各ハニカムユニットの全体に水を含浸させる工程において、含浸される水の量は、乾燥状態のハニカムユニットの重量に対して、15wt%~25wt%の範囲であることを特徴とするハニカム構造体の製造方法が提供される。
前記ハニカム構造体の周囲に保持シール材を配置した状態で、前記ハニカム構造体を金属容器に収納する工程と、
を有することを特徴とする排ガス浄化装置の製造方法が提供される。
CO(NH2)2+H2O → 2NH3+CO2 式(1)
このアンモニアが、NOxを含む排ガスとともに、ハニカム構造体100の一方の端面(例えば端面110)から、ハニカムユニット130の各セル121に流入した場合、セル壁123に含まれているSAPOの触媒作用により、以下の式(2-1)式および(2-2)の反応が生じる。
4NH3+4NO+O2 → 4N2+6H2O 式(2-1)
8NH3+6NO2 → 7N2+12H2O 式(2-2)
その後、浄化された排ガスは、ハニカム構造体100の他方の端面(例えば端面115)から排出される。このように、ハニカム構造体100内に排ガスを流通させることにより、排ガス中のNOxを処理することができる。
ここで、図1に示したハニカム構造体100の構成部材について、簡単に説明しておく。
ハニカムユニット130は、SAPO粒子を含む。さらに、ハニカムユニット130は、無機バインダおよび無機繊維を含んでも良い。ハニカムユニット130は、さらに、SAPO粒子以外の無機粒子を含んでも良い。
ハニカム構造体100の接着層150は、前述のように、接着層用ペーストを原料として形成される。
ハニカム構造体100の外周コート層120は、前述のようなハニカムユニットを構成する材料と同様の無機粒子、無機バインダ、および無機繊維の少なくとも一つを含み、さらに有機バインダを含むペーストを原料として形成される。あるいは、外周コート層120は、接着層150と同じ材料を用いることもできるし、接着層と異なる材料であっても良い。原料となる外周コート層ペーストには、必要に応じて、酸化物系セラミックを成分とする微小中空球体であるバルーンや、球状アクリル粒子、グラファイト等の造孔剤を添加しても良い。コート層の最終的な厚さは、0.1mm~2.0mmが好ましい。
以下、本発明によるハニカム構造体の製造方法について、詳しく説明する。
(a)複数のハニカム成形体を準備する工程(ステップS110)と、
(b)各ハニカム成形体を焼成して、以降の工程で接着層用ペーストが設置されることになる少なくとも一つの接合面を有する、ハニカムユニットを形成する工程(ステップS120)と、
(c)各ハニカムユニットの全体に水を含浸させる工程(ステップS130)と、
(d)少なくとも無機粒子、バインダ、および水を含む接着層用ペーストを準備する工程(ステップS140)と、
(e)前記ハニカムユニットの前記接合面に前記接着層用ペーストを塗布し、各ハニカムユニット同士を接合する工程(ステップS150)と、
(f)前記接着層用ペーストを乾燥、脱脂、固化して接着層を得る工程(ステップS160)と、
を含み、前記(c)の各ハニカムユニットの全体に水を含浸させる工程において、含浸される水の量は、乾燥状態のハニカムユニットの重量に対して、15wt%~25wt%の範囲である。
まず、無機粒子を主成分とし、さらに必要に応じて、無機バインダおよび無機繊維を添加した原料ペーストを用いて押出成形等を行い、ハニカムユニット成形体を作製する。
次に、ステップS110で準備された成形体が焼成され、ハニカムユニットが製造される。ハニカムユニットは、以降のステップS150において、接着層用ペーストが設置されることになる少なくとも一つの接合面を有する。
次に、作製された各ハニカムユニットに、水が含浸される。
次に、接着層用のペーストが調製される。
次に、ステップS140で調製された接着層用ペーストを介して、各ハニカムユニット同士が接合され、ハニカムユニット組立体が構成される(接合工程)。
次に、接着層用ペーストが乾燥、脱脂、および固化処理される。また、この際に、前記工程(ステップS130)において、ハニカムユニットに含浸されていた水も除去される。
(実施例1)
まず、SAPO粒子2800重量部(平均粒子径3μm)、ベーマイト(無機バインダ)1120重量部、アルミナ繊維270重量部(平均繊維長100μm、平均繊維径6μm)、メチルセルロース380重量部、オレイン酸(成形助剤)310重量部、および水2400重量部を加えて、混合、混練して、混合組成物を作製した。
ハニカムユニットの含水量(%)={(ハニカムユニットの含水重量(g)-ハニカムユニットの初期重量(g))/ハニカムユニットの初期重量(g)}×100
ハニカムユニットの含水量は、15%であった。
セラミックファイバー16.2wt%、
シリカガラス51.9wt%、
カルボキシメチルセルロース0.1wt%、
シリカゾル28.9wt%、
ポリビニルアルコール0.8wt%、
非イオン系界面活性剤1.9wt%、
有機バルーン0.2wt%。
接着層用ペーストを乾燥させ、接着層を形成した。接着層の厚さは、1.0mmとした。
実施例1と同様の方法により、実施例2にハニカム構造体を作製した。ただし、この実施例2では、ハニカムユニットの乾燥処理は、ハニカムユニットを台上に置き、30分間、扇風機で送風することにより実施した。その他の作製条件は、実施例1と同様である。
実施例1と同様の方法により、実施例3にハニカム構造体を作製した。ただし、この実施例3では、ハニカムユニットの乾燥処理は、ハニカムユニットを台上に置き、10分間、扇風機で送風することにより実施した。その他の作製条件は、実施例1と同様である。
実施例1と同様の方法により、実施例3にハニカム構造体を作製した。ただし、この実施例4では、SAPO粒子における比Si/(Al+P)(モル比)は、0.23であった。その他の作製条件は、実施例1と同様である。
実施例4と同様の方法により、実施例5にハニカム構造体を作製した。ただし、この実施例5では、ハニカムユニットの乾燥処理は、ハニカムユニットを台上に置き、30分間、扇風機で送風することにより実施した。その他の作製条件は、実施例4と同様である。
実施例4と同様の方法により、実施例6にハニカム構造体を作製した。ただし、この実施例6では、ハニカムユニットの乾燥処理は、ハニカムユニットを台上に置き、10分間、扇風機で送風することにより実施した。その他の作製条件は、実施例4と同様である。
実施例1と同様の方法により、実施例7にハニカム構造体を作製した。ただし、この実施例7では、SAPO粒子における比Si/(Al+P)(モル比)は、0.28であった。その他の作製条件は、実施例1と同様である。
実施例7と同様の方法により、実施例8にハニカム構造体を作製した。ただし、この実施例8では、ハニカムユニットの乾燥処理は、ハニカムユニットを台上に置き、30分間、扇風機で送風することにより実施した。その他の作製条件は、実施例7と同様である。
実施例7と同様の方法により、実施例9にハニカム構造体を作製した。ただし、この実施例9では、ハニカムユニットの乾燥処理は、ハニカムユニットを台上に置き、10分間、扇風機で送風することにより実施した。その他の作製条件は、実施例7と同様である。
実施例1と同様の方法により、比較例1にハニカム構造体を作製した。ただし、この比較例1では、ハニカムユニットの乾燥処理は、60℃の乾燥機中に、ハニカムユニットを40分間保持することにより実施した。その他の作製条件は、実施例1と同様である。
比較例1と同様の方法により、比較例2にハニカム構造体を作製した。ただし、この比較例2では、SAPO粒子における比Si/(Al+P)(モル比)は、0.23とした。その他の作製条件は、比較例1と同様である。
比較例1と同様の方法により、比較例3にハニカム構造体を作製した。ただし、この比較例3では、SAPO粒子における比Si/(Al+P)(モル比)は、0.28とした。その他の作製条件は、比較例1と同様である。
この表1の結果から、ハニカムユニットの接合工程前のハニカムユニットの含水量を15%~25%(実施例1~9)とすることにより、ワレおよびクラックが生じ難いハニカム構造体を製造することができることが確認された。
110 第1の端面
115 第2の端面
120 コート層
121 セル
123 セル壁
130 ハニカムユニット
150 接着層
Claims (8)
- シリコアルミナリン酸塩の粒子を含み、長手方向に沿って、第1の端面から第2の端面に延伸する複数のセルがセル壁により区画されたハニカムユニットを有するハニカム構造体の製造方法であって、
当該ハニカム構造体の製造方法は、
(a)複数のハニカム成形体を準備する工程と、
(b)各ハニカム成形体を焼成して、以降の工程で接着層用ペーストが設置されることになる少なくとも一つの接合面を有する、ハニカムユニットを形成する工程と、
(c)各ハニカムユニットの全体に水を含浸させる工程と、
(d)少なくとも無機粒子、バインダ、および水を含む接着層用ペーストを準備する工程と、
(e)前記ハニカムユニットの前記接合面に前記接着層用ペーストを塗布し、各ハニカムユニット同士を接合する工程と、
(f)前記接着層用ペーストを乾燥、脱脂、固化して接着層を得る工程と、
を含み、
前記(c)の各ハニカムユニットの全体に水を含浸させる工程において、含浸される水の量は、乾燥状態のハニカムユニットの重量に対して、15wt%~25wt%の範囲であることを特徴とするハニカム構造体の製造方法。 - 前記シリコアルミナリン酸塩の粒子は、モル比換算で、比Si/(Al+P)が0.11~0.33の範囲であることを特徴とする請求項1に記載のハニカム構造体の製造方法。
- 前記シリコアルミナリン酸塩の粒子は、前記乾燥状態のハニカムユニット中に、該ハニカムユニット全体に対して、230g/L~360g/Lの範囲で含まれていることを特徴とする請求項1または2に記載のハニカム構造体の製造方法。
- 前記(c)の各ハニカムユニットの全体に水を含浸させる工程は、各ハニカムユニットを水中に浸漬させる工程を有することを特徴とする請求項1乃至3のいずれか一つに記載のハニカム構造体の製造方法。
- 前記ハニカムユニットは、さらに無機バインダを有することを特徴とする請求項1乃至4のいずれか一つに記載のハニカム構造体の製造方法。
- 前記ハニカムユニットは、さらに無機繊維を有することを特徴とする請求項1乃至5のいずれか一つに記載のハニカム構造体の製造方法。
- 前記無機繊維は、アルミナ、シリカ、炭化ケイ素、シリカアルミナ、ガラス、チタン酸カリウム、およびホウ酸アルミニウムからなる群より選択される一種以上であることを特徴とする請求項6に記載のハニカム構造体の製造方法。
- 請求項1乃至7のいずれか一つに記載の方法を用いて、ハニカム構造体を製造する工程と、
前記ハニカム構造体の周囲に保持シール材を配置した状態で、前記ハニカム構造体を金属容器に収納する工程と、
を有することを特徴とする排ガス浄化装置の製造方法。
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