JP3560408B2 - Diesel exhaust gas purification filter and method for producing the same - Google Patents

Diesel exhaust gas purification filter and method for producing the same Download PDF

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Publication number
JP3560408B2
JP3560408B2 JP02806996A JP2806996A JP3560408B2 JP 3560408 B2 JP3560408 B2 JP 3560408B2 JP 02806996 A JP02806996 A JP 02806996A JP 2806996 A JP2806996 A JP 2806996A JP 3560408 B2 JP3560408 B2 JP 3560408B2
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Japan
Prior art keywords
filter
cell
exhaust gas
honeycomb
particulates
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Expired - Fee Related
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JP02806996A
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JPH09220423A (en
Inventor
慶則 中山
友彦 中西
照高 影山
寿治 近藤
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株式会社デンソー
株式会社日本自動車部品総合研究所
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Description

[0001]
TECHNICAL FIELD OF THE INVENTION
INDUSTRIAL APPLICABILITY The present invention is used for removing at least particulates from substances contained in gas exhausted from an internal combustion engine such as a diesel engine and purifying hydrocarbons (HC) and carbon monoxide in exhaust gas. The present invention relates to a filter for collecting particulates.
[0002]
[Prior art]
Particulates emitted from internal combustion engines such as diesel engines contain substances harmful to the human body, and removing them has become an environmental issue. For this reason, conventionally, a method of collecting particulates with a filter provided in an exhaust system of a diesel engine, collecting a certain amount of the particulates, and burning and removing the particulates with an electric heater, a burner, or the like has been performed. There is also a method of lowering the burning temperature of particulates with a platinum group metal catalyst supported on a filter and burning the collected particulates continuously. In the case of the former method, in which the collected particulates are burned and removed by an electric heater, a burner, or the like, as the amount of collected particulates increases, the maximum temperature of the filter during combustion rises, and the filter is damaged by thermal stress applied to the filter. In some cases, control of the amount of trapped particulates is important, and the amount of trapped particulates has not been completely controlled. In the latter case of combustion using a catalyst, the combustion temperature is relatively low, and the thermal stress applied to the filter is small, so that the heat resistance is excellent.
[0003]
In the above-described method, a ceramic honeycomb structure is mainly used for collecting particulates, and cordierite having low thermal expansion is generally used as the material.
[0004]
In the diesel exhaust gas purifying filter targeted by the present invention, a cell opening at one end of a ceramic monolith having a honeycomb structure, for example, a cell opening at a gas inlet side is plugged every other cell, and a cell opening at a gas outlet side is closed. Only cells that are not plugged in the opening on the inlet side are plugged. Therefore, the exhaust gas passes through the pores on the side wall of the cell, and the particulates flowing with the exhaust gas are collected on the surface of the cell law wall and inside the pores of the cell law wall.
[0005]
[Problems to be solved by the invention]
The porous ceramic filter of the honeycomb structure has a structure in which the gas flows through the pores of several μm to several tens μm of the cell wall to the adjacent cells by alternately plugging both ends of the monolith honeycomb as described above. In addition, there is an advantage that the collection efficiency of particulates is higher than that of filters having other structures. In order to support a catalyst on this filter, when a high specific surface area material such as activated alumina is coated on the cell side wall surface and inside the pores of the cell side wall as the carrier, the high specific surface area material closes the pores of the cell side wall. As a result, there is a problem that the pressure loss is higher than that of a filter without coating. Since a high filter pressure loss leads to a decrease in engine output, the pressure loss should be as low as possible. However, if the porosity and the pore diameter of the filter are too large in order to reduce the pressure loss, there is a possibility that the collection efficiency of particulates may be reduced.
[0006]
When a ceramic carrier having a honeycomb structure is coated with a material having a high specific surface area such as activated alumina, several types having a defined particle size of activated alumina are known. Japanese Patent Publication No. 55-1818 discloses that the activated alumina particle size is 0.1 to 100 μm, but it is premised that the activated alumina is mixed with an amorphous alumina such as boehmite. It is said that the adhesive strength is improved. In Japanese Patent Publication No. 4-80736, it is effective to ensure a stable dispersibility of the activated alumina slurry by defining the average particle size of the activated alumina to be 20 μm or less. It is said that the adhesive strength is improved. However, in any case, when the activated alumina is coated on the ceramic carrier having the honeycomb structure, the purpose is to improve the adhesive strength in order to prevent peeling of the coating layer. These are flow-through type exhaust gas purifying devices, in which the exhaust gas does not pass through the honeycomb wall, but passes through a tubular passage formed by the wall, and is not a filter, but rather a filter. In order to increase the strength, the porosity of the wall is generally low and the pore diameter is small.
[0007]
The present invention provides a porous honeycomb filter having a structure in which a gas flows through pores of a cell wall to an adjacent cell by alternately plugging both ends of a porous monolith honeycomb having a honeycomb structure. It is an object of the present invention to provide a surface material which is uniformly coated not only on the surface of the cell side wall but also inside the pores of the cell side wall and does not cause a problem of high pressure loss.
[0008]
[Means for Solving the Problems]
According to the first aspect of the present invention, in the diesel exhaust gas purification filter having the porous ceramic honeycomb structure, the porosity of the cell side wall of the honeycomb structure is 40 to 65%, and the average pore diameter is 5 to 35 μm. By making 90% by weight or more of the high specific surface area material supported on the honeycomb structure body smaller than the average pore diameter of the honeycomb structure cell side wall, the diesel exhaust gas purification filter having the high specific surface material coating of the present invention has a pressure loss. Low.
[0009]
BEST MODE FOR CARRYING OUT THE INVENTION
The diesel exhaust gas purification filter of the present invention is obtained by coating a high specific surface area material such as activated alumina on a cell side wall surface and a cell side wall internal pore surface of a ceramic monolith honeycomb structure, and then coating a catalytic metal thereon. It is made by alternately plugging both ends of the honeycomb cell opening.
[0010]
Ceramic monolith honeycomb structure used in the present invention is preferably made conventionally with a low thermal expansion coefficient ceramic as known cordierite (chemical composition 2MgO · 2Al 2 O 3 · 5SiO 2), the porosity of the side walls Is preferably about 40% to 65%, more preferably about 45% to 60%, and the average pore diameter is preferably about 5 μm to 35 μm, and more preferably about 10 μm to 30 μm.
[0011]
On the other hand, the particle diameter of the high specific surface area material such as activated alumina to be coated on the honeycomb structure may be 90 wt% or more, preferably 95 wt% or more, smaller than the average pore diameter of the honeycomb structure. desirable. If more than 10 wt% of the high specific surface area material has a particle diameter larger than the average pore diameter of the honeycomb structure, the high specific surface material does not enter the pores inside the cell side wall of the honeycomb structure, and This is not preferable because the material having a high specific surface area covering the coating layer relatively increases, the thickness of the coating layer increases, and the pressure loss increases. When the particle diameter of the high specific surface area material is 90 wt% or more than the average pore diameter of the honeycomb structure, the high specific surface area material entering the pores inside the cell side wall increases. At this time, the excess of the high surface material slurry is sufficiently removed by air blow or suction with a cleaner, and the slurry is uniformly dispersed without blocking the inside of the pores and coated, so that an increase in pressure loss can be suppressed. The pressure loss is the difference between the air on the inlet side and the air on the outlet side when air flows into the filter from the inlet side of the filter and flows out of the filter from the outlet side of the filter. Is preferably 45 mmAq (water column) or less when measured under the condition of 2000 L / min (linear velocity 1.8 cm / sec).
[0012]
The diesel exhaust gas purification filter of the present invention has a structure for collecting particulates contained in exhaust gas of a diesel engine. Through the outlet of the adjacent cell. When passing through the cell wall, only the particulates in the exhaust gas are collected. At this time, when the porosity and the average pore diameter of the honeycomb before the activated alumina coating constituting the filter are smaller than the above ranges, the collection efficiency of the particulates is improved, but the pressure loss of the filter is increased and the engine output is reduced. Is not preferred. On the other hand, if it is larger than this range, the collection efficiency of particulates is undesirably reduced.
[0013]
The reason why the particle diameter of the high specific surface area material such as activated alumina is in the above range is that the high specific surface area material needs to enter the inside of the pores on the cell side walls of the honeycomb structure. Conventionally, a honeycomb-type monolithic carrier was coated with a high specific surface area material only on the surface of the cell side wall.However, in the case of a honeycomb type filter having a structure in which the exhaust gas passes through the inside of the pores of the cell side wall, it is included in the exhaust gas. At this time, it is necessary for the particulates to come into contact with the high specific surface area material inside the pores in order to be catalyzed since the particulates remain on the surface of the cell side wall of the filter and inside the pores of the cell side wall. It is. Therefore, the high specific surface area material needs the above particle size.
Further, the coating amount (supporting amount) of the high specific surface area material is preferably 20 to 75 g / L. If the coating amount is less than 20 g / L, the exhaust gas purification capacity is low, which is not preferable. On the other hand, if it is larger than 75 g / L, the pressure loss of the filter increases and the engine output decreases, which is not preferable.
[0014]
As the material having a high specific surface area in the present invention, besides activated alumina, silica, zirconia, titania, or a material containing two or more of these materials can be used.
[0015]
The diesel exhaust gas purification filter of the present invention collects at least particulates contained in exhaust gas of a diesel engine, and burns and removes the particulates. The reason why the filter is coated with a high specific surface area material such as activated alumina is preferably to provide a support for coating a platinum group catalytic metal. In general, platinum group catalyst metals are used as catalysts for lowering the burning temperature of particulates, and are also used as catalysts for oxidizing carbon monoxide and hydrocarbons. The filter of the present invention is preferably a filter carrying a metal catalyst comprising at least one platinum group element.
[0016]
Next, the diesel exhaust gas purification filter of the present invention will be specifically described with reference to FIGS. As shown in FIG. 1, this porous ceramic filter having a honeycomb structure is alternately plugged with plugging materials 1 at both ends of a monolith honeycomb to form a coating layer 4 made of activated alumina particles 3 on cell side walls 2 of the honeycomb filter. Is formed. If activated alumina having a particle size smaller than the average pore diameter of the filter is used as shown in FIG. 2 in which the portion A of FIG. 1 is enlarged, the filter is coated without closing the inside of the pore 5 on the cell side wall, so that the pressure loss of the filter is reduced. Little rise. However, when activated alumina having a particle diameter larger than the average pore diameter of the filter is used as shown in FIG. 3 in which the portion A of FIG. 1 is enlarged, the pores on the cell walls are closed, and the pressure loss of the filter increases significantly. I do. In addition, by supporting the platinum group catalyst metal on the coating portion of the activated alumina, the purification efficiency of particulates and other exhaust gas components (HC, CO, etc.) trapped inside the cell wall is enhanced. In these drawings, the description of the catalyst metal layer is omitted.
[0017]
Diesel exhaust gas containing particulates enters the cell from the cell inlet side 6, passes through the cell wall 2, and exits from the cell outlet side 7. At this time, the particulates are trapped on the cell wall surface and inside pores. The platinum group catalyst metal is usually coated anew after coating with activated alumina, but it is also possible to coat with a solution mixed with activated alumina.
[0018]
【Example】
A filter coated with the above materials can be suitably used as a low-pressure-loss diesel particulate filter. Examples and comparative examples are shown below.
[0019]
[Example 1]
Silica main ingredient, aluminum hydroxide, with talc, was adjusted to cordierite (2MgO · 2Al 2 O 3 · 5SiO 2) composition, then the carbon to a porous to these main raw materials , And then fired at a maximum temperature of 1350C to 1450C, a heating rate of 5C to 200C, and a holding time of 2 to 20 hours. , A porous cordierite honeycomb having a porosity of 55%, an average pore diameter of 28 μm, a cell side wall thickness of 0.45 mm, and 150 cells per square inch having a diameter of 140 mm and a length of 130 mm. A structure was obtained.
[0020]
On the other hand, as a material having a high specific surface area, 670 g of activated alumina (manufactured by Sumitomo Chemical Co., Ltd.) having a center particle size of 5 μm and particles having a particle size larger than 28 μm of 5 wt% or less and 330 g of alumina sol (manufactured by Nissan Chemical) are mixed together with 4 liters of water, The mixture was stirred to produce an activated alumina slurry.
[0021]
The porous cordierite honeycomb structure was completely immersed in an activated alumina slurry (wash coat). After that, excess slurry adhered as much as possible was removed with an air cleaner and compressed air. The coating was repeated to produce five types of honeycombs having different coating amounts. Thereafter, it was dried at 120 ° C. for 2 hours and fired at 800 ° C. The coating amount per unit volume was calculated from the difference in honeycomb weight before and after wash coating. <Coating amount [g / L] = (weight before coating−weight after coating) / honeycomb volume)>. Thereafter, it was immersed in a 0.1 mol / L chloroplatinic acid aqueous solution for 30 minutes, dried at 120 ° C. for 2 hours, and calcined at 800 ° C. to support platinum. The supported amount of platinum was about 2 g / L.
[0022]
Every other cell opening on the gas inlet side of the honeycomb structure supporting platinum was plugged, and only the cells not plugged on the inlet side on the gas outlet side were plugged. The plugging material is not particularly limited as long as it is a heat-resistant ceramic material such as cordierite, alumina, zirconia or the like having a temperature of 1000 ° C. or more, and a ceramic adhesive may be used. In this example, cordierite was used. In this way, filters with catalyst carriers having different activated alumina coating amounts were produced (carriers A-1 to A-4).
[0023]
[Example 2]
A filter similar to the porous cordierite honeycomb filter used in Example 1 was manufactured by the same method, and as a material having a high specific surface area, activated alumina having a center particle diameter of 2 μm and particles larger than 28 μm and 5% or less (Sumitomo) (670 g) was mixed with 330 g of alumina sol (manufactured by Nissan Chemical) and 4 liters of water, and the filter was wash-coated on a stirred activated alumina slurry. The coating was repeated to produce five types of filters having different coating amounts. After that, excess slurry adhered as much as possible was removed with an air cleaner and compressed air. Thereafter, it was dried at 120 ° C. for 2 hours and fired at 800 ° C. After examining the coating amount, it was immersed in an aqueous chloroplatinic acid solution for 30 minutes, dried at 120 ° C. for 2 hours, and baked at 800 ° C. to carry platinum. The supported amount of platinum was about 2 g / L.
[0024]
Thereafter, using cordierite, every other cell opening on the gas inlet side of the honeycomb structure supporting platinum was plugged, and only the cells not plugged on the inlet side on the gas outlet side were plugged. Then, a filter with a catalyst carrier was produced (carrier B-1 to carrier B-5).
[0025]
[Comparative Example 1]
A filter similar to the porous cordierite honeycomb filter used in Example 1 was manufactured by the same method, and 670 g of activated alumina (manufactured by Sumitomo Chemical) having a center particle diameter of 50 μm was converted to alumina sol (manufactured by Nissan Chemical) as a high specific surface area material. ) Was washed with 330 g of water and 4 liters of water, and the filter was wash-coated on a stirred activated alumina slurry. After that, excess slurry adhered as much as possible was removed with an air cleaner and compressed air. Coating was repeated to produce three types of filters having different coating amounts. Thereafter, it was dried at 120 ° C. for 2 hours and fired at 800 ° C. After calculating the coating amount, the film was immersed in a 0.1 mol / L chloroplatinic acid aqueous solution for 30 minutes, dried at 120 ° C. for 2 hours, and baked at 800 ° C. to support platinum. The supported amount of platinum was 2 g / L.
[0026]
Thereafter, using cordierite, every other cell opening on the gas inlet side of the honeycomb structure supporting platinum was plugged, and only the cells not plugged on the inlet side on the gas outlet side were plugged. Then, a filter with a catalyst carrier was produced (carrier C-1 to carrier C-3).
[0027]
[Comparative Example 2]
A filter similar to the porous cordierite honeycomb filter used in Example 1 was manufactured by the same method, and as a material having a high specific surface area, activated alumina having a center particle diameter of about 25 μm and containing 45 wt% of particles larger than 28 μm (Sumitomo) (670 g) was mixed with 330 g of alumina sol (manufactured by Nissan Chemical) and 4 liters of water, and the filter was wash-coated on a stirred activated alumina slurry. After that, excess slurry adhered as much as possible was removed with an air cleaner and compressed air. The coating was repeated to produce four types of filters having different coating amounts. Thereafter, it was dried at 120 ° C. for 2 hours and fired at 800 ° C. After calculating the coating amount, the film was immersed in a 0.1 mol / L chloroplatinic acid aqueous solution for 30 minutes, dried at 120 ° C. for 2 hours, and baked at 800 ° C. to support platinum. The supported amount of platinum was about 2 g / L.
[0028]
Thereafter, using cordierite, every other cell opening on the gas inlet side of the honeycomb structure supporting platinum was plugged, and only the cells not plugged on the inlet side on the gas outlet side were plugged. Then, a filter with a catalyst carrier was produced (carrier D-1 to carrier D-4).
[0029]
[Comparative Example 3]
A filter similar to the porous cordierite honeycomb filter used in Example 1 was produced by the same method, and about 2 g / L of platinum was supported in the same manner without coating with activated alumina, and the gas of the honeycomb structure was formed. Every other cell opening on the inlet side was plugged, and only the cells not plugged on the inlet side on the gas outlet side were plugged to produce a filter with a catalyst carrier (carrier E).
[0030]
Table 1 shows the coating amounts of the carriers prepared in Examples and Comparative Examples.
[0031]
[Table 1]
[0032]
(Measurement of pressure loss of filter with catalyst carrier)
For all the filters of the carriers A to E obtained in Examples 1 and 2 and Comparative Examples 1, 2 and 3, compressed air was flowed from the inlet side of the filters, and the differential pressure between the inlet side and the outlet side was measured. FIG. 4 shows the measurement results of the pressure loss. From this result, it is understood that the product of the present invention has a lower pressure loss than Comparative Examples 1 and 2 provided with a coating.
[0033]
(Measurement of filter pore distribution)
The pore distribution was measured for all filters of the carriers A to E obtained in Examples 1 and 2 and Comparative Examples 1, 2 and 3. FIG. 5 shows the relationship between the average pore diameter of the carrier and the coating amount of activated alumina. As the coating amount increases, the average pore diameter of the carrier decreases. The average pore size that is advantageous as a low pressure loss diesel purification filter is 5 μm to 35 μm.
[Brief description of the drawings]
FIG. 1 is a cross-sectional view of a diesel exhaust gas purification filter according to an example of the present invention or a comparative example.
FIG. 2 is an enlarged view of a portion A in FIG.
FIG. 3 is an enlarged view of a portion A in FIG. 1;
FIG. 4 is a graph showing measurement results of pressure loss of filters of an example and a comparative example.
FIG. 5 is a graph showing the relationship between the average pore diameter of the carrier and the coating amount of activated alumina in the filters of Examples and Comparative Examples.

Claims (3)

  1. By alternately plugging both ends of the cell opening of the ceramic honeycomb structure, the exhaust gas flows through the pores of the cell side wall of the honeycomb to the adjacent cells, and only the particulates contained in the exhaust gas are exposed to the surface and inside of the cell side wall. In a diesel exhaust gas purification filter having a porous ceramic filter adapted to be trapped by a catalyst metal burning the particulates on the surface and inside of the side wall, the ceramic honeycomb structure has pores on the cell side wall. Rate is 40 to 65%, the average pore diameter is 5 to 35 μm, and as the support for supporting the catalyst metal, a material having a high specific surface area occupying 90 wt% or more having a particle diameter smaller than the average pore diameter is 20 %. A diesel exhaust gas purification filter characterized in that the diesel exhaust gas purification filter carries 75 to 75 g / l .
  2. The filter according to claim 1, wherein a catalyst metal comprising at least one kind of platinum group element is supported.
  3. By alternately plugging both ends of the cell opening of the ceramic honeycomb structure, the exhaust gas flows through the pores of the cell side wall of the honeycomb and flows to the adjacent cells, and only the particulates contained in the exhaust gas are exposed to the surface and inside of the cell side wall. In the method for producing a diesel exhaust gas purification filter having a porous ceramic filter adapted to be trapped by a catalyst metal supporting the particulates on the surface and inside of the side wall, the ceramic honeycomb structure has a cell A carrier having a side wall porosity of 40 to 65%, an average pore diameter of 5 to 35 μm, and having a particle diameter smaller than the average pore diameter of the carrier for supporting the catalyst metal is 90%. wt % Of a material having a high specific surface area occupying 20% to 75 g / l of which is occupied by at least 20% by weight.
JP02806996A 1996-02-15 1996-02-15 Diesel exhaust gas purification filter and method for producing the same Expired - Fee Related JP3560408B2 (en)

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JPWO2013145316A1 (en) * 2012-03-30 2015-08-03 イビデン株式会社 Honeycomb filter and method for manufacturing honeycomb filter
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WO2010058834A1 (en) 2008-11-21 2010-05-27 日産自動車株式会社 Particulate substance removing material, particulate substance removing filter catalyst using particulate substance removing material, and method for regenerating particulate substance removing filter catalyst
US9222382B2 (en) 2008-11-21 2015-12-29 Nissan Motor Co., Ltd. Particulate matter purifying material, filter catalyst for purifying particulate matter using particulate matter purifying material, and method of regenerating filter catalyst for purifying particulate matter

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