JPH0970513A - Exhaust gas filter and manufacturing method thereof - Google Patents

Abstract

(57) [Summary] [Object] The present invention has pores that are uniformly distributed, has an appropriate pressure loss and porosity, has an appropriate number of cells, has excellent filter characteristics, and further has a thermal expansion coefficient. The present invention aims to provide an exhaust gas filter that has a low heat resistance, excellent mechanical strength such as tensile strength, high thermal conductivity, and excellent thermal shock resistance, and a method for producing the same. The exhaust gas filter 1a of the present invention has a large number of cells 2 in the axial direction from the exhaust gas inlet side 6 to the exhaust gas outlet side 7, and either the exhaust gas inlet side 6 or the exhaust gas outlet side 7 of the cell 2 is provided. A ceramic exhaust gas filter 1 formed by alternately blocking one or the other with a blocking agent 3, the pressure loss between the exhaust gas inlet side 6 and the exhaust gas outlet side 7 under a blowing speed of 200 to 600 cm / sec. Is 30-1
It has a structure of 90 mmAq, preferably 50 to 150 mmAq.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an exhaust gas filter having excellent filter characteristics and suitable for removing fine particles discharged from a diesel engine, a boiler, a high temperature combustion apparatus and the like, and a method for producing the same.

[0002]

2. Description of the Related Art In recent years, deterioration of air pollution due to NO _x and suspended particulate matter (hereinafter referred to as fine particles) in metropolitan areas has become a problem. In particular, with regard to fine particles floating in the atmosphere, it is said that black smoke emitted from a diesel engine closes 30 to 40% of the whole fine particles, and among them, polycyclic aromatic hydrocarbons such as benzpyrene and the like. Since it contains a metamorphic substance and a carcinogenic ingredient, its countermeasures are urgently needed.

As a countermeasure against this, an exhaust gas purifying apparatus has been developed which collects fine particles in an exhaust system and then performs self-regeneration.

A ceramic monolithic wall flow type fine particle filter (hereinafter referred to as a ceramic monolithic filter) disclosed in US Pat. No. 4,364,761, which is the mainstream of conventional exhaust gas filters of this type, will be described below. . FIG. 4 is a side sectional view of a conventional ceramic monolithic filter. 50 is a cylindrical filter body made of honeycomb ceramics,
51 and 52 are a large number of cells formed in the filter body 50, 53 is an occluding agent that alternately blocks either the exhaust gas inlet side 54 or the exhaust gas outlet side 55 of the cells 51 and 52, and 56 is the filter body 50 and It is a porous wall that constitutes a partition wall between cells.

With respect to the ceramic monolithic filter constructed as described above, a method for collecting and regenerating the same will be described below. The exhaust gas outlet side 55 containing fine particles flows into the closed cell 51 and is pushed to the cell 52 which passes through the porous wall 56 and is closed on the adjacent inlet side. At this time, the fine particles are filtered as they pass through the porous wall 56, and the fine particles are collected in the porous wall 56. When the amount of collected fine particles increases, the porous wall 56 becomes clogged with fine particles,
The back pressure of the diesel engine exhaust system increases. Therefore, it is necessary to suppress the increase in the load on the engine due to the increase in back pressure by removing the fine particles when the amount of the collected fine particles exceeds a certain amount.

The fine particles are composed of a fixed carbon component and a soluble organic component which can be dissolved in an organic solvent, both of which are flammable and have a temperature difference of about 650 ° C. or more, though there is a slight temperature difference depending on the type of engine and load conditions. It will burn if heated to. Therefore, conventionally, a method of regenerating the porous wall 56 by burning these fine particles using a heating means such as an electric heater, a burner, or hot air has been attempted.

However, the conventional exhaust gas filter has a problem in heat stress due to the temperature gradient generated during the regeneration combustion. Cordierite, which is a typical low thermal expansion ceramic, was used. Then, in order to solve these problems, JP-A-62-22524
No. 9 discloses that the chemical composition of the main component is SiO ₂ 4 on a weight basis.
_{2 to} 56%, Al ₂ O _{3 to} 45%, MgO 12 to 16%, and the main component of the crystal phase is cordierite, and the honeycomb structure has a porosity of 30% or less and an axial direction of 40 to 40%. Thermal expansion coefficient between 800 ℃ is 0.8 × 10 ^-6 /
The thermal expansion coefficient between 40 ° C. and 800 ° C. in the layer direction is
There has been proposed a cordierite honeycomb structure catalyst carrier having characteristics of 1.0 × 10 ⁻⁶ / ° C. or less. Also,
In JP-A-2-52015, the chemical composition of the main component is S
iO ₂ 42 to 56 wt%, Al ₂ O ₃ 30-45% by weight,
A porous honeycomb filter having 12 to 16% by weight of MgO and a cordierite as a main component of a crystalline phase, having a porosity of 40% to 55% and a pore volume of 2 μm or less in diameter. A porous ceramic honeycomb filter characterized by being 0.015 cc / g or less has been proposed.

[0008]

However, in the above-mentioned conventional structure, when the porosity of the exhaust gas filter becomes 30% or less, the pressure loss between the exhaust gas inlet side and the exhaust side increases, so that the exhaust system of the diesel engine exhaust system is backed up. There is a problem in that the pressure rapidly increases and a large load is applied to the engine. Further, since the porosity is small, there is a problem that the collection time of fine particles in exhaust gas is short and the regeneration cycle is too short to be practical. Further, the porosity is 40 to 55.
% Exhaust gas filter, the size and shape of the pores, the state of distribution, the size of the cells formed in the axial direction of the exhaust gas filter and the number of cells per unit area There is a problem in that the pressure loss during the period may increase, and as a result, the load on the engine increases and the collection time of fine particles becomes short.

Therefore, in order to reduce the pressure loss between the inlet side and the outlet side of the exhaust gas filter, the exhaust gas filter having a porosity of 70 to 80% was produced by increasing the amount of the pore-forming agent added and variously studied. However, the mechanical strength is reduced and the thermal conductivity is reduced, resulting in the deterioration of the thermal shock resistance of the exhaust gas filter, and the problem of destruction without being able to withstand the thermal stress caused by the temperature gradient generated during regenerative combustion. It turned out to have points. Further, when the porosity is extremely increased, the pores are bonded to each other and large pores having a pore diameter of about 40 to 50 μm are generated, so that the fine particles in the exhaust gas are not trapped but released into the atmosphere, and the filter effect remarkably increases. It turned out that it had the problem of lowering.

The present invention solves the above-mentioned conventional problems, in which pores are evenly distributed, have proper pressure loss and porosity, have an appropriate number of cells, and have excellent filter characteristics.
Furthermore, the thermal expansion coefficient is small, the mechanical strength such as tensile strength is excellent, the thermal conductivity is large, the provision of an exhaust gas filter having excellent thermal shock resistance, and the exhaust gas filter which can mass-produce the excellent exhaust gas filter with high productivity. It is intended to provide a manufacturing method.

[0011]

In order to achieve this object, the exhaust gas filter and the method for producing the same of the present invention have the following configurations.

The exhaust gas filter according to claim 1 has a large number of cells in the axial direction from the exhaust gas inlet side to the exhaust gas side, and either the exhaust gas inlet side or the outlet side of the cells alternates. An exhaust gas filter made of ceramics, which is formed by being blocked with a blocking agent,
The pressure loss between the inlet side and the outlet side of the exhaust gas under the blowing speed of m / sec is 30 to 190 mmAq, preferably 50.
It has a configuration of about 150 mmAq. As the pressure loss becomes smaller than 50 mmAq, the fine particles in the exhaust gas tend to be released into the atmosphere without being collected.
If it is less than mmAq, the tendency is remarkable, and 150mmA
As the value exceeds q, the pressure loss between the inlet side and the outlet side of the exhaust gas tends to increase, and the load on the engine tends to increase. At 190 mmAq, this tendency further increases, which is not preferable.

The exhaust gas filter according to claim 2 has a large number of cells in the axial direction from the exhaust gas inlet side to the exhaust gas side, and either the exhaust gas inlet side or the outlet side of the cells alternates. It is an exhaust gas filter made of ceramics, which is formed by blocking with a blocking agent at room temperature to 850 ° C.
Coefficient of thermal expansion in the axial direction up to 4.5 × 10 ^-6 / ° C or less,
It is preferably 2.5 × 10 ⁻⁶ / ° C. or less, and the difference in thermal expansion coefficient between the axial direction and the layer direction is | 5.0 × 10 ⁻⁶ | / ° C. or less, preferably | 3.0 × 10 ^{− 6} | / ° C or less. The coefficient of thermal expansion of the exhaust gas filter in the axial direction from room temperature to 850 ° C exceeds 2.5 × 10 ^-6 / ° C, or the difference in the coefficient of thermal expansion in the axial direction and the layer direction from room temperature to 850 ° C is | 3. If it exceeds 0.0 × 10 ⁻⁶ | / ° C., the thermal stress due to the temperature gradient generated during the regeneration combustion cannot be endured and the alloy tends to be destroyed, which is not preferable.

The exhaust gas filter according to claim 3 has a large number of cells in the axial direction from the exhaust gas inlet side to the exhaust gas side, and either the exhaust gas inlet side or the outlet side of the cells alternates. An exhaust gas filter made of ceramics, which is formed by blocking with an occluding agent, and has an axial tensile strength of 40 kg / cm ² or more, preferably 80 kg / cm ^2.
Has a configuration that is Axial tensile strength of 80k
As it becomes smaller than g / cm ² , there is a tendency for it to break without being able to withstand the thermal stress due to the temperature gradient generated during regenerative combustion, and if it is less than 40 kg / cm ² , this tendency tends to appear, so that the engine tends to appear. When attached to the exhaust system, it is not preferable because it tends to be destroyed without being able to withstand the vibration of the automobile.

The exhaust gas filter according to claim 4 has a large number of cells in the axial direction from the exhaust gas inlet side to the exhaust gas side, and either the exhaust gas inlet side or the outlet side of the cells alternates. An exhaust gas filter made of ceramics, which is closed by a plugging agent and has a thermal conductivity in the axial direction of 0.100 kcal / mh ° C. or higher, preferably 0.
It has a structure of 200 kcal / mh ° C. or higher.
As the thermal conductivity in the axial direction becomes smaller than 0.200 kcal / mh ° C., the thermal shock resistance tends to deteriorate,
If it is less than kcal / mh ° C., it is remarkable, and the temperature gradient generated during regenerative combustion cannot be relaxed, and there is a tendency for destruction, which is not preferable.

The exhaust gas filter according to claim 5 has a large number of cells in the axial direction from the exhaust gas inlet side to the exhaust gas side, and either the exhaust gas inlet side or the outlet side of the cells alternates. An exhaust gas filter made of ceramics, which is formed by being blocked with a blocking agent, and has a configuration in which the number of cells per 1 cm ^{2 of} a cross section perpendicular to the axial direction is 9 to 64 cells. If the number of cells is less than 9, the collection efficiency of fine particles in the exhaust gas decreases, and if it exceeds 64, the pressure loss between the inlet side and the outlet side of the exhaust gas tends to increase, which is not preferable.

The exhaust gas filter according to claim 6 has a large number of cells in the axial direction from the exhaust gas inlet side to the exhaust gas side, and either the exhaust gas inlet side or the outlet side of the cells alternates. A ceramic exhaust gas filter formed by blocking with an occluding agent having an average pore diameter of 1 to
An exhaust gas filter having 20 μm pores uniformly distributed, and a porosity of 30 to 70%, preferably 40 to 60%.
Has a configuration that is If the average pore size is less than 1 μm, the pressure loss between the inlet side and the outlet side of the exhaust gas tends to increase, and if it exceeds 20 μm, the collection efficiency of fine particles in the exhaust gas tends to decrease, which is not preferable either. . Further, if the porosity is less than 40%, the pressure loss tends to increase, and if it exceeds 60%, the collection efficiency of fine particles tends to decrease and the tensile strength in the axial direction tends to decrease, which is not preferable.

The exhaust gas filter according to claim 7 is the exhaust gas filter according to claim 1, 2, 3, 4, 5 or 6, wherein the main components of the crystal phase of the ceramic are cordierite, mullite, aluminum titanate, spodumene and euclibutite. , At least one of potassium titanate, quartz, and corundum. When the main component of the crystal phase of the exhaust gas filter is occupied with these compounds, the coefficient of thermal expansion can be lowered and the thermal shock resistance can be increased.

The exhaust gas filter according to claim 8 has a large number of cells in the axial direction from the exhaust gas inlet side to the exhaust gas side, and either the exhaust gas inlet side or the outlet side of the cells alternates. A method for manufacturing an exhaust gas filter made of ceramics, which is formed by plugging an Al ₂
O ₃ -SiO ₂ based inorganic fiber and pulp and ceramic powder and and the slurry producing step of dispersing and mixing to obtain a slurry of water, cations in the slurry, the anionic or nonionic polymer coagulant and a high electrolyte inorganic coagulant, Aggregating step of adding the mixture of the above and aggregating the slurry, sheet forming step of obtaining a sheet by a papermaking method after aggregating, corrugating the sheet to form a honeycomb-shaped formed body or sheet into a rectangular shape and laminating rectangular sheets to form a laminate. It has a configuration including a molded body generating step of obtaining a body and a firing step of firing a honeycomb-shaped molded body or a laminated molded body. Where Al ₂ O ₃
-SiO ₂ type inorganic fiber is ceramic powder 100
50 to 150 parts by weight, preferably 70 to 150 parts by weight
130 parts by weight are used. When the amount is less than 70 parts by weight, good flocs cannot be obtained easily, and papermaking becomes difficult. As a result, the strength of the sheet tends to be weakened.
Especially when the amount is less than 50 parts by weight, the tendency is remarkable, and
The thermal expansion coefficient of the inorganic fiber itself tends to become stronger and the thermal expansion coefficient tends to increase as the amount exceeds 1 part by weight.
If the amount exceeds 50 parts by weight, the tendency is further strengthened, which is not preferable. The pulp is used in an amount of 2 to 15 parts by weight, preferably 5 to 10 parts by weight, based on 100 parts by weight of the ceramic powder. If the amount is less than 5 parts by weight, the sheet produced by the paper-making method tends to be rigid and hard to form a molded product, and if it exceeds 10 parts by weight, the distribution of pores tends to be uneven, and particularly 2 If the amount is less than 15 parts by weight or exceeds 15 parts by weight, the tendency becomes remarkable, which is not preferable. Water is 50 for 100 parts by weight of ceramic powder
00 to 10,000 parts by weight, preferably 7,000 to 900
0 parts by weight are used. When the amount is less than 7,000 parts by weight, the concentration of the slurry becomes high, so that papermaking tends to be difficult, and when it exceeds 9000 parts by weight, the thickness of the sheet by the papermaking method tends to be thin, which is not preferable. In the slurry generation process, AlC
preferable because the l ₃ · 6H ₂ O and adding an aqueous solution such as NaOH formation of a good floc is obtained. As the polymer flocculant, an amine-bonding polymer as a cation type, a polyacrylate as an anion type, and a polyacrylamide as a nonionic type are used, but a nonionic type is preferably used. This is because good floc formation can be obtained. As high-electrolyte inorganic coagulant, NaOH, KOH
Etc. are used. The ratio of polymer coagulant and inorganic coagulant is
The inorganic flocculant is used in an amount of 3 to 7, preferably 4 to 6 with respect to the polymer flocculant 1. A strong floc can be obtained by using an inorganic coagulant together.

The exhaust gas filter according to claim 9 has a large number of cells in the axial direction from the exhaust gas inlet side to the exhaust gas side, and either the exhaust gas inlet side or the outlet side of the cells alternates. A method of manufacturing an exhaust gas filter made of ceramics, which is blocked by a blocking agent, comprising: mixing a ceramic powder, a binder, a lubricant, a pore former, and water, and then kneading them to obtain a lump. It has a structure including a forming step, a forming step of forming a lump by an extrusion method to obtain a honeycomb formed body, and a firing step of drying and firing the honeycomb formed body. Here, as the binder, a cellulose-based one is preferable, and 5 to 25 parts by weight, preferably 10 parts by weight, relative to 100 parts by weight of the ceramic powder.
~ 20 parts by weight are used. When the amount is less than 10 parts by weight, particularly less than 5 parts by weight, the moldability of the honeycomb-shaped molded body tends to deteriorate, and when it is 20 parts by weight or more, especially more than 25 parts by weight, the shrinkage ratio in the firing step is large. Both of them are not preferable because they tend to occur. The lubricant is preferably a polymer ester type lubricant, and is used in an amount of 1 to 10 parts by weight, preferably 2 to 7 parts by weight, based on 100 parts by weight of the ceramic powder. If the amount is 2 parts by weight or less, especially less than 1 part by weight, the lump tends to adhere to the mold, and if it is 7 parts by weight or more, especially more than 10 parts by weight, the retention of the honeycomb formed body tends to deteriorate. Neither is preferable. Water is used in an amount of 10 to 60 parts by weight, preferably 20 to 40 parts by weight, based on 100 parts by weight of the ceramic powder. If it is 20 parts by weight or less, especially less than 10 parts by weight, the lump tends to be hard and extrusion molding tends to be difficult, and 40 parts by weight or more,
In particular, when the amount exceeds 60 parts by weight, it depends on the kind of the ceramic powder, but the formation of the honeycomb-shaped molded body is poor, and cracks are likely to occur on the surface of the molded body during drying.

The pore-forming agent is preferably polyethylene, carbon, wheat flour or the like, and is used in an amount of 20 to 70 parts by weight, preferably 30 to 60 parts by weight, based on 100 parts by weight of the ceramic powder. When it is less than 30 parts by weight, the porosity of the produced exhaust gas filter tends to be small and the pressure loss between the exhaust gas inlet side and the exhaust side tends to be large, and when it exceeds 60 parts by weight, the porosity increases. Since it is too much, the collection efficiency of the fine particles in the exhaust gas tends to be lowered, which is not preferable.

The exhaust gas filter according to claim 10 is
The structure according to claim 8 or 9, wherein the ceramic powder contains at least one of cordierite, mullite, aluminum titanate, spodumene, euclibutite, potassium titanate, silica, alumina, and a clay mineral as a main component. have. By using these ceramic powders, the thermal shock resistance can be remarkably improved.

The exhaust gas filter according to claim 11 is
In Claim 10, the main component of the clay mineral is K ₂ O, Si.
O ₂ , Al ₂ O ₃ , and the content of K ₂ O is 1.0 to
It has a composition of 6.0 wt%. When the content of K ₂ O is less than 1.0 wt%, the firing temperature tends to be high, and when it is 6.0% or more, the thermal expansion coefficient tends to be large, which is not preferable.

The exhaust gas filter according to claim 12 is
In claim 10, the main crystal phase of the clay mineral is sericite, kaolinite, or pyrophyllite. By having these constitutions, the moldability can be improved, and after firing, cristobalite having a large coefficient of thermal expansion hardly precipitates, and the occurrence rate of crazes and cracks can be remarkably reduced, thereby increasing the product yield. be able to.

[0025]

With this structure, the fine particles in the exhaust gas can be efficiently collected and can withstand the thermal stress.

[0026]

EXAMPLE An exhaust gas filter and a method for manufacturing the same according to one example of the present invention will be described in detail below.

(Examples 1 and 2) FIG. 1 (a) is an external perspective view of an exhaust gas filter according to the first embodiment of the present invention, and FIG. 1 (b) shows an exhaust gas filter according to the second embodiment of the present invention. FIG. 2 is a perspective view of a main part, and FIG. 2 is a cross-sectional view of the main part of the exhaust gas filter taken along line XX in the first embodiment of the present invention. 1a and 1b are exhaust gas filters in the first and second embodiments of the present invention, 2 is a cell, 3 is a blocking agent, 4 is an exhaust gas inlet, 5 is an exhaust gas outlet, 6 is an exhaust gas inlet side, and 7 is an exhaust gas outlet side. Is.

The method of manufacturing the exhaust gas filter of this embodiment having the above-described structure will be described below. Al
₂ O ₃ —SiO ₂ based inorganic fiber, pulp, aluminum titanate powder, and water were mixed in a ratio shown in (Table 1) and dispersed and mixed in a dedicated tank to obtain a slurry.

[0029]

[Table 1]

The obtained slurry was transferred to a dilution tank, water was added to a predetermined volume, and then an AlCl ₃ .6H ₂ O aqueous solution and a NaOH aqueous solution were added to adjust the pH to 7.2 to 7.8. Next, a mixture of a cation, anion or nonionic polymer coagulant and a high electrolyte inorganic coagulant is added to coagulate the slurry, which is composed of Al ₂ O ₃ —SiO ₂ based inorganic fibers, pulp and aluminum titanate powder. A sheet was prepared. Then, this sheet is rolled up while applying a blocking agent made of aluminum titanate at the same time as the corrugating process, or is laminated while being provided with a blocking agent made of aluminum titanate at the same time as the rectangular processing. Laminated body (second embodiment)
Was produced. The honeycomb shaped body (first example) or the laminated body (second example) was fired within a temperature range of 1500 to 1550 ° C. and then processed to obtain the exhaust gas filters of the first and second examples. .

Exhaust gas filters 1a and 1b of this embodiment
Has a columnar appearance, and a large number of cells 2 are formed in the axial direction from the exhaust gas inlet side 6 to the outlet side 7, and the cells 2 have either the exhaust gas inlet side 6 or the outlet side 7 alternately. The structure was closed with the blocking agent 3, and the number of cells per 1 cm ² of the cross section perpendicular to the axial direction was 36 cells.

Next, with respect to each of the obtained exhaust gas filters, pressure loss, thermal expansion coefficient, tensile strength, thermal conductivity, average pore diameter and porosity, and network pore distribution were measured. For pressure loss, use a blast type pressure loss meter with a water column manometer,
When the pressure loss between the inlet side and the outlet side of the exhaust gas was measured under a blowing speed of 40 cm / sec, it was 95 mm.
It was Aq. The coefficient of thermal expansion was measured using a vertical thermal dilatometer. Thermal expansion coefficient in the axial direction and a layer direction to 850 ° C. from room temperature is the 0.8 × 10 ^-6 / ℃, the difference in axial thermal expansion coefficient of up to 850 ° C. from room | 1.3 × 10 ^{- 6} ｜ / ℃
Met. The tensile strength was measured using a strength tester.
The tensile strength in the axial direction was 135 Kg / cm ² . The thermal conductivity was measured by a conventional method using a thermal conductivity meter. The thermal conductivity in the axial direction was 0.27 Kcal / mh ° C. The average pore size and porosity were determined by a conventional method using a mercury porosimeter. The average pore diameter was 12.5 μm, and the pores were uniformly distributed, and the porosity was 54%. Then powder X-ra
As a result of identifying the crystal phase by y-diffraction, it was found that aluminum titanate was the main component.

As described above, according to this embodiment, the coefficient of thermal expansion is small, the tensile strength is large, the thermal conductivity is large, the thermal shock resistance is excellent, the pores are uniformly distributed, and the proper pressure loss is obtained. It was found that an exhaust gas filter having a porosity and an appropriate number of cells and excellent filter characteristics can be obtained. In addition, the main component of the crystal phase of the exhaust gas filter is at least one of cordierite, mullite, aluminum titanate, spodumene, eucryptite, potassium titanate, quartz, and corundum as long as thermal shock resistance and filter characteristics are not impaired. It was found that those containing three or more had the same effect. Furthermore, even if the ceramic powder contains at least one of cordierite, mullite, aluminum titanate, spodumene, eucryptite, potassium titanate, silica, alumina, and a clay mineral as a main component, it is equivalent. It turns out that the effect of is obtained. The exhaust gas filters (a) and (b) of this example have a columnar appearance, and have a structure in which either the exhaust gas inlet side 6 or the outlet side 7 is alternately closed by a blocking agent 3, The number of cells per cm ^{2 in the} cross section perpendicular to the axial direction was 36 cells.

(Embodiment 3) FIG. 3 is a sectional view of an essential part of an exhaust gas filter according to a third embodiment of the present invention. 11 is an exhaust gas filter of the third embodiment of the present invention, 12 is a cell, 1
Reference numeral 3 is a blocking agent, 14 is an exhaust gas inlet, and 15 is an exhaust gas outlet. A method of manufacturing the exhaust gas filter 11 of the third embodiment having the above structure will be described below. The main crystal phase is sericite, which is a clay mineral containing 2.0 wt% of K ₂ O, a methylcellulose-based binder, a polymer ester-based lubricant and water in the ratios shown in (Table 2). And mix for 3 minutes with a high speed mixer, then 3 with a kneader.
The mixture was kneaded for 0 to 120 minutes to obtain a lump for extrusion molding.

[0035]

[Table 2]

Next, the obtained lump was used to form a columnar molded body having a large number of cells in the axial direction of 170 mm in diameter and 180 mm in height by using a vacuum extruder, and then this molded body was dried using a dryer. It was dried at a temperature of 80 to 100 ° C. for 24 hours. Then, the dried molded body was subjected to 1470 using an electric furnace.
The exhaust gas filter 11 of the third embodiment is processed by firing in a temperature range of 15 ° C to 1520 ° C to produce a fired body, and alternately closing one of the cells at both ends of the fired body with a blocking agent. It was made. The exhaust gas filter 11 of the third embodiment thus obtained has a columnar shape, and a large number of cells 12 are formed in the axial direction from the exhaust gas inlet side 16 toward the exhaust gas outlet side 17 inside the cell 12. Either the exhaust gas inlet side 16 or the exhaust gas outlet side 17 had a structure in which the exhaust gas inlet side 16 or the exhaust gas outlet side 17 was alternately blocked, and the number of cells per 1 cm ² of the cross section perpendicular to the axial direction was 49 cells.

Then, the physical properties of the obtained exhaust gas filter were measured in the same manner as in Example 1. As a result, the pressure loss between the inlet side and the outlet side of the exhaust gas was 124 mmAq under the blowing speed of 400 cm / sec. Further, the coefficient of thermal expansion in the axial direction from room temperature to 850 ° C. is 2.8 × 10 ⁻⁶ / ° C., and the difference between the coefficients of thermal expansion in the axial direction and the layer direction from room temperature to 850 ° C. is | 0.5 × 10 ^-6
It was | / ° C. The tensile strength in the axial direction is 175k.
It was g / cm ² . The thermal conductivity in the axial direction is 0.3.
It was 4 kcal / mh ° C. The average pore diameter is 7.
The pores were 8 μm and were uniformly distributed, and the porosity was 43%. Furthermore, as a result of identifying the crystal phase by powder X-ray diffraction, it was found that mullide was the main component.

As described above, according to this embodiment, the coefficient of thermal expansion is small, the tensile strength is large, the thermal conductivity is large, the thermal shock resistance is excellent, the pores are evenly distributed, and an appropriate pressure loss is obtained. It was found that an exhaust gas filter having a porosity and an appropriate number of cells and excellent in filter characteristics can be obtained. In addition, the main component of the crystal phase of the exhaust gas filter is cordierite, mullite, aluminum titanate, as long as thermal shock resistance and filter characteristics are not impaired.
Spojumen, Eucryptite. Potassium titanate,
It was also found that any material containing at least one of quartz and corundum is acceptable. The ceramic powder is cordierite. It has been found that the same effect can be obtained by using one containing at least one of aluminum titanate, spodumene, eucryptite, potassium titanate, silica, alumina, and a clay mineral as a main component. It was found that the main crystal phase of the clay mineral used as the ceramic powder has the same effect even if kaolinite or bilophyllite is used.

[0039]

As described above, the present invention has the following excellent effects. That is, the pressure loss between the exhaust gas inlet side and the outlet side of the exhaust gas filter is 30 to 190 m.
In mAq, the number of cells in the cross section perpendicular to the axial direction was 9 to 64 cells, and the pores having an average pore diameter of 1 to 20 μm were uniformly distributed to form a porosity of 30 to 70%. It is possible to realize an exhaust gas filter having excellent filter characteristics capable of efficiently collecting fine particles therein.

The coefficient of thermal expansion of the exhaust gas filter in the axial direction is 4.5 × 10 ^-6 / ° C or less, and the difference in the coefficient of thermal expansion in the axial direction and the layer direction is │5.0 × 10 ^-6 │ / ° C or less. Since the tensile strength in the axial direction was set to 40 kg / cm ² or more and the thermal conductivity in the axial direction was set to 0.100 kcal / mh ° C or more, thermal shock resistance that withstands thermal stress caused by the temperature gradient generated during regenerative combustion It is possible to realize an excellent exhaust gas filter.

Al ₂ O ₃ --SiO ₂ type inorganic fiber,
An exhaust gas filter is produced by a papermaking method using pulp or ceramic powder, or an exhaust gas filter is produced by an extrusion method using a ceramic powder, a binder, a lubricant, and a pore-forming agent, and the cross section is 1 cm perpendicular to the axial direction. ²⁰⁰ to 600c by setting the number of cells per ² to 9 to 64 cells
The pressure loss between the inlet side and the outlet side of the exhaust gas is 30 to 190 mmAq, the pores having an average pore diameter of 1 to 20 μm are uniformly distributed, and the porosity is 3 at a blowing speed of m / sec.
It is possible to realize a method for manufacturing an exhaust gas filter which has excellent filter characteristics of 0 to 70% and is suitable for mass production at low cost.

As a ceramic powder, cordierite,
Mullite, aluminum titanate, spodumene, eucryptite, potassium titanate, silica, alumina,
By using at least one of clay minerals as the main component, the main component of the crystalline phase of the exhaust gas filter is cordierite, mullite, aluminum titanate,
Spodumene, eucryptite, potassium titanate,
An exhaust gas filter having at least one of quartz and corundum can be obtained, and the coefficient of thermal expansion in the axial direction from room temperature to 850 ° C. is 4.5 × 10 ⁻⁶ / ° C. or less,
The difference in the coefficient of thermal expansion between the axial direction and the layer direction is | 5.0 × 10 ^-6 |
/ ° C or lower, axial tensile strength is 40 kg / cm ² or higher, axial thermal conductivity is 0.100 kcal / mh ° C
It is possible to realize the exhaust gas filter extremely excellent in thermal shock resistance and the method for manufacturing the exhaust gas filter as described above.

[Brief description of drawings]

FIG. 1A is an external perspective view of an exhaust gas filter according to a first embodiment of the present invention. FIG. 1B is a perspective view of an essential part of an exhaust gas filter according to a second embodiment of the present invention.

FIG. 2 is a sectional view of a main part of an exhaust gas filter taken along line XX in the first embodiment of the present invention.

FIG. 3 is a sectional view of an essential part of an exhaust gas filter according to a third embodiment of the present invention.

FIG. 4 is a side sectional view of a conventional ceramic monolithic filter.

[Explanation of symbols]

 1a, 1b Exhaust gas filter of the first and second examples 2 Cell 3 Clogging agent 4 Exhaust gas inlet 5 Exhaust gas outlet 6 Exhaust gas inlet side 11 Exhaust gas outlet side 11 Exhaust gas filter 12 Cell 13 Clogging agent 14 Exhaust gas flow Inlet 15 Exhaust gas outlet 16 Exhaust gas inlet side 17 Exhaust gas outlet side 50 Filter body 51, 52 Cell 53 Blocking agent 54 Exhaust gas inlet side 55 Exhaust gas outlet side 56 Porous wall

 ─────────────────────────────────────────────────── ─── Continuation of front page (72) Inventor Yukinori Ikeda 1006 Kadoma, Kadoma City, Osaka Prefecture Matsushita Electric Industrial Co., Ltd. (72) Koichi Watanabe 1006 Kadoma, Kadoma City, Osaka Matsushita Electric Industrial Co., Ltd. 72) Inventor St. Matsueda 1006 Kadoma, Kadoma City, Osaka Prefecture Matsushita Electric Industrial Co., Ltd.

Claims (12)

[Claims] 1. A plurality of cells are axially provided in the interior from an exhaust gas inlet side to an exhaust side, and one of the exhaust gas inlet side and the outlet side of the cells is alternately blocked by a blocking agent. A formed exhaust gas filter made of ceramic, wherein the pressure loss between the inlet side and the outlet side of the exhaust gas is 30 to 190 mm under a blowing speed of 200 to 600 cm / sec.
Exhaust gas filter having Aq, preferably 50 to 150 mmAq. 2. A plurality of cells are axially provided inside from the inlet side of the exhaust gas toward the outlet side, and one of the inlet side and the outlet side of the exhaust gas of the cells is alternately blocked by a blocking agent. The formed exhaust gas filter made of ceramic, which has a coefficient of thermal expansion in the axial direction from room temperature to 850 ° C. of 4.
5 × 10 ⁻⁶ / ° C. or less, preferably 2.5 × 10 ⁻⁶ / ° C. or less, and the difference in thermal expansion coefficient between the axial direction and the layer direction is | 5.
0 × 10 ⁻⁶ | / ° C. or less, preferably | 3.0 × 10 ⁻⁶ |
/ ° C or less, an exhaust gas filter. 3. A plurality of cells are axially provided inside from the inlet side to the outlet side of the exhaust gas, and one of the inlet side and the outlet side of the exhaust gas of the cells is alternately blocked by a blocking agent. An formed exhaust gas filter made of ceramic, having an axial tensile strength of 40 kg / cm ² or more, preferably 80 kg / cm ² . 4. A large number of cells are axially provided inside from the inlet side to the outlet side of the exhaust gas, and one of the inlet side and the outlet side of the exhaust gas of the cells is alternately blocked by a blocking agent. An formed exhaust gas filter made of ceramic, having a thermal conductivity in the axial direction of 0.1 kcal / mh ° C or higher, preferably 0.2 kcal / mh ° C or higher. 5. A plurality of cells are axially provided inside from the inlet side to the outlet side of the exhaust gas, and one of the inlet side and the outlet side of the exhaust gas of the cells is alternately blocked by a blocking agent. A formed exhaust gas filter made of ceramic, wherein the number of cells per 1 cm ² of the cross section perpendicular to the axial direction is 9 to
An exhaust gas filter having 64 cells. 6. A large number of cells are axially provided inside from the inlet side of the exhaust gas toward the outlet side, and one of the inlet side and the outlet side of the exhaust gas of the cells is alternately blocked by a blocking agent. A formed exhaust gas filter made of ceramics, having an average pore size of 1 to 20 μm uniformly distributed, and having a porosity of 30 to 70%, preferably 40 to 60%. An exhaust gas filter characterized by. 7. The main component of the crystal phase of the ceramic contains at least one of cordierite, mullite, aluminum titanate, spodumene, euclibutite, potassium titanate, quartz and corundum. The exhaust gas filter according to claim 1, 2, 3, 4, 5 or 6. 8. A plurality of cells are axially provided inside from the inlet side of the exhaust gas toward the outlet side, and one of the inlet side and the outlet side of the exhaust gas of the cells is alternately blocked by a blocking agent. a forming process for the preparation of a ceramic exhaust gas filter, a slurry producing step for obtaining a slurry and Al ₂ O ₃ -SiO ₂ -based inorganic fiber and pulp and ceramic powder and water dispersible mixture to a cation to the slurry ,
An anion or aggregating step of aggregating the slurry by adding a mixture of an anionic or nonionic polymer aggregating agent and a high electrolyte inorganic aggregating agent, a sheet forming step of obtaining a sheet by a papermaking method after aggregation, and corrugating the sheet. A honeycomb molded body or sheet is rectangularly processed to form a molded body by laminating rectangular sheets to obtain a laminated molded body, and a firing step of firing the honeycomb molded body or the laminated molded body. Exhaust gas filter manufacturing method. 9. A plurality of cells are axially provided inside from the inlet side of the exhaust gas toward the outlet side, and one of the inlet side and the outlet side of the exhaust gas of the cells is alternately blocked by a blocking agent. A method of manufacturing a formed ceramic exhaust gas filter, comprising: a lump producing step of obtaining a lump by kneading after mixing ceramic powder, a binder, a lubricant, a pore former and water, and the lump. A method for manufacturing an exhaust gas filter, comprising: a molded body forming step of forming a honeycomb-shaped formed body by subjecting the honeycomb-shaped formed body to an extrusion method; and a firing step of drying and then firing the honeycomb formed body. 10. The ceramic powder is cordierite,
Mullite, aluminum titanate, spodumene, euclibutite, potassium titanate, silica, alumina,
The method for producing an exhaust gas filter according to claim 8 or 9, characterized by containing at least one of those containing clay mineral as a main component. 11. The main component of the clay mineral is K ₂ O, Si
O ₂ , Al ₂ O ₃ , and the content of K ₂ O is 1.
It is 0-6.0 wt%, The manufacturing method of the exhaust gas filter of Claim 10 characterized by the above-mentioned. 12. The main crystal phase of the clay mineral is sericite,
The method for producing an exhaust gas filter according to claim 10, which is kaolinite or pyrophyllite.