Classifications

• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
  • B01D53/34—Chemical or biological purification of waste gases
  • B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
  • B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
  • B01D53/944—Simultaneously removing carbon monoxide, hydrocarbons or carbon making use of oxidation catalysts
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
  • B01D46/24—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D33/00—Filters with filtering elements which move during the filtering operation
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
  • B01D46/24—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies
  • B01D46/2403—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies characterised by the physical shape or structure of the filtering element
  • B01D46/2418—Honeycomb filters
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
  • B01D53/34—Chemical or biological purification of waste gases
  • B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
  • B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
  • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
  • B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
  • B01J23/56—Platinum group metals
  • B01J23/58—Platinum group metals with alkali- or alkaline earth metals
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J33/00—Protection of catalysts, e.g. by coating
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
  • B01J37/02—Impregnation, coating or precipitation
  • B01J37/024—Multiple impregnation or coating
  • B01J37/0242—Coating followed by impregnation
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
  • B01J37/02—Impregnation, coating or precipitation
  • B01J37/024—Multiple impregnation or coating
  • B01J37/0244—Coatings comprising several layers
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
  • B01J37/02—Impregnation, coating or precipitation
  • B01J37/024—Multiple impregnation or coating
  • B01J37/0248—Coatings comprising impregnated particles

Definitions

• the present invention relates to an exhaust gas-purifying catalyst capable of purifying particulate material (hereinafter, referred to as "PM") , which is contained in a diesel exhaust gas or the like and mainly contains carbon, from a low-temperature range.
• the exhaust gas-purifying catalyst according to the present invention is particularly useful as a catalyst for purifying exhaust gas for diesel engines because it can purify not only PM, but also HC, CO, or NO x .
• Known exhaust gas purifiers for diesel engines which have been developed up to date, are mainly classified into a trap type (wall flow structure) and an open type (straight flow structure) .
• a trap type exhaust gas purifier a clogged honeycomb structure (a diesel PM filter (hereinafter, referred to as a "DPF") ) made of ceramic is known.
• a DPF is known which includes a ceramic honeycomb structure with cells clogged at opposite ends of openings thereof in the form of a checkered pattern alternately.
• the DPF includes inlet cells each clogged at an exhaust gas downstream side thereof, outlet cells each arranged adjacent to the inlet cells and clogged at an exhaust gas upstream side thereof, and cell partition walls partitioning the inlet cells and the outlet cells from each other.
• exhaust gas is filtered by pores of the cell partition walls, which capture PM, so that emission of PM is suppressed.
• Japanese Patent Publication No. 7-106290 discloses a filter catalyst, the filter catalyst comprises a coating layer made of alumina, etc. and formed on surfaces of cell partition walls of a DPF, and a catalytic metal such as platinum (Pt) supported on the coating layer.
• a catalytic metal such as platinum (Pt) supported on the coating layer.
• Japanese Patent Application Publication No. 9-094434 also discloses a filter catalyst wherein a coating layer supporting a catalytic metal is formed not only on cell partition walls, but also on pores of the cell partition walls. Since the catalytic metal is also supported in the pores of the cell partition walls, the catalytic metal is likely to contact the PM. The PM captured by the pores can also be oxidized and burnt.
• Supporting alkali metal or alkaline earth metal on a coating layer of a filter catalyst, together with noble metal is also disclosed in Japanese Patent Application Publication No. 2003-049627 or Japanese Patent Application Publication No. 2003-049631. The alkali metal or alkaline earth metal forms a nitrate or sulfate in an exhaust gas.
• the filter catalyst including the coating layer supporting alkali metal or alkaline earth metal, together with noble metal also has a problem in that a sufficient PM oxidation performance cannot be exhibited in a general operation range of about 400 0 C or below.
• the present invention has been made in view of the above-mentioned problems, and it is an aspect of the invention to provide an exhaust gas-purifying catalyst which is capable of oxidizing PM even in a low-temperature range of 300 0 C or below and enhancing PM oxidation performance.
• the present invention provides an exhaust gas-purifying catalyst comprising: a filter substrate having a wall flow structure, the filter substrate including inlet cells each clogged at an exhaust gas downstream side of the inlet cell, outlet cells each arranged adjacent to the inlet cells and clogged at an exhaust gas upstream side of the outlet cell, and porous cell partition walls partitioning the inlet cells and the outlet cells from each other and having a plurality of pores; and a catalyst bed formed on the cell partition walls, wherein the catalyst bed contains a porous oxide, a noble metal supported on the porous oxide, and an alkali metal supported on the porous oxide in an amount of 0.6 mole or more per IL of the filter substrate, and oxidizes particulate material (PM) , which mainly contains carbon, and is captured by the filter substrate, from a low-temperature range of 300 0 C or below.
• the catalyst may further comprise a protection layer formed between the filter substrate and the catalyst bed, and made of an oxide reactable with the alkali
• FIG. 1 is an explanation view illustrating a structure of an exhaust gas-purifying catalyst according to an exemplary embodiment of the present invention
• FIG. 2 is a graph depicting a PM oxidation initiation temperature and a PM oxidation peak temperature
• FIG. 3 is a graph depicting a relation between temperature and differential pressure
• FIG. 4 is a graph depicting a relation between potassium supporting amount and PM oxidation initiation temperature.
• FIG. 5 is an explanation view illustrating a structure of an exhaust gas-purifying catalyst according to another exemplary embodiment of the present invention.
• the present invention provides an exhaust gas-purifying catalyst including a filter substrate and a- catalyst bed formed on cell partition walls of the filter substrate.
• the filter substrate has a wall flow structure similar to a conventional DPF including inlet cells each clogged at an exhaust gas downstream side thereof, outlet cells each arranged adjacent to the inlet cells and clogged at an exhaust gas upstream side thereof, and porous cell partition walls partitioning the inlet cells and the outlet cells from each other and having a plurality of pores.
• the filter substrate may be formed of a metal foam or a heat-resistant non-woven fabric.
• the filter substrate may also be made of heat-resistant ceramics such as cordierite or silicon carbide.
• a clayey slurry containing cordierite powder as a major component thereof is prepared. The prepared slurry is shaped by extrusion, and is then calcined. In place of the cordierite powder, a mixture of alumina powder, magnesia powder and silica powder having the same composition as the cordierite may be prepared. Openings of the cells at one end of the filter substrate are clogged in the form of a checkered pattern by clayey slurries having a shape similar to that of the cell openings, respectively.
• a filter substrate having a honeycomb structure can be fabricated.
• the cross-sectional shapes of the inlet cells and outlet cells may be triangular, square, hexagonal, circular, etc. Of course, they are not limited to such shapes.
• the cell partition walls have.a porous structure allowing an exhaust gas to pass therethrough. In order to form pores in the cell partition walls, combustible powder such as carbon powder, wood powder, starch, or resin powder is mixed with the slurry.
• pores are formed in the cell partition walls. It is possible to control the diameter and volume of the pores by adjusting the size and content of the combustible powder.
• the inlet cells and outlet cells are communicated with each other by the pores . Accordingly, although PM is captured in the pores, gas can flow from the inlet cells to the outlet cells via the pores.
• the cell partition walls have a porosity of 40% to 70%.
• the pores preferably have an average diameter of 10 ⁇ m to 40 ⁇ m.
• the cell partition walls have the porosity and average pore diameter ranging as described above, it is possible to suppress an- increase in pressure loss even when the catalyst bed is formed to range from 100g/L to 200g/L. It is also possible to suppress a decrease in strength. Thus, capture of PM can be more effectively achieved.
• the catalyst bed is provided at the cell partition walls of the filter substrate.
• the catalyst bed may be formed only on the surfaces of the cell partition walls, it is preferred that the catalyst bed be also formed on the surfaces of the pores in the cell partition walls.
• the catalyst bed contains a porous oxide, noble metal supported on the porous oxide, and alkali metal supported on the porous oxide.
• the porous oxide may include alumina, zirconia, titania, silica, or ceria conventionally used as a catalyst support, or a composite oxide or mixture of at least two of the catalyst supports. Among these materials, ⁇ -alumina having a large specific surface area is preferable.
• the noble metal supported on the porous oxide may be selected from Pt, Pd, Rh, Ir, Ru, etc. Among these elements, it is preferable to select Pt, which exhibits a high oxidation activity to PM.
• the supported amount of the noble metal ranges from O.lg to 5g per IL of the filter substrate. When the supported amount of the noble metal is less than the above range, it is impractical due to an excessively low activity. On the other hand, when the supported amount of the noble metal is more than the above range, saturated activity is exhibited, and the costs are increased.
• the supporting of the noble metal may be achieved by an adsorption supporting method, a impregnating supporting method, or the like using a solution containing a nitrate of the noble metal dissolved therein.
• the alkali metal supported on the porous oxide Na, K, Li, Cs, etc. maybe used.
• K is preferable which exhibits a particularly-high oxidation activity to PM.
• the supported amount of the alkali metal is 0.6 mole or more per IL of the filter substrate.
• the supported amount of the alkali metal is less than the above range, it is difficult to initiate oxidation of PM at a temperature of 300 0 C or below.
• the supported amount of the alkali metal have an upper limit of about 2 moles per IL of the filter substrate, for purification of exhaust gases of vehicles.
• the supported amount of the alkali metal exceeds the upper limit, a degradation in the activity of the noble metal occurs, thereby degrading the performance capable of purifying HC, CO, NO x , etc.
• the catalyst bed is formed by preparing a slurry of the porous oxide powder with a binder ingredient such as an alumina sol and water, applying the slurry to the cell partition walls, and calcining the applied slurry, thereby forming a coating layer.
• a slurry may be prepared using catalyst powder prepared by previously supporting the noble metal on the porous oxide powder.
• the supporting of the alkali metal may be performed after the formation of the catalyst bed using the prepared slurry.
• the application of the slurry to the cell partition walls may be achieved using a general dipping method. However, it is preferable to remove a surplus of the slurry filled in the pores, while forcibly filling the slurry in the pores of the cell partition walls by air blow or air suction.
• the formation amount of the coating layer or catalyst bed preferably ranges from 3Og to 200g per IL of the filter substrate.
• the formation amount of the coating layer or catalyst bed is less than 30g/L, it is impossible to prevent a degradation in the durability of the noble metal.
• the formation amount of the coating layer or catalyst bed exceeding 200g/L is impractical due to an excessively high pressure loss.
• a protection layer made of an oxide reactable with the alkali metal is formed between the filter substrate and the catalyst bed.
• the protection layer functions to suppress the alkali metal supported in the catalyst bed from migrating to the filter substrate in a high-temperature atmosphere, and thus, to suppress a degradation in the strength of the filter substrate. It is also possible to suppress a degradation in the concentration of the alkali metal in the catalyst bed caused by the migration of the alkali metal to the filter substrate. Accordingly, a degradation in PM oxidation activity can be suppressed.
• Examples of the oxide reactable with the alkali metal may be TiO 2 , SiO 2 , Al 2 O 3 , B 2 O 3 , P 2 O 5 , etc.
• the formation amount of the protection layer corresponds to a thickness of O.OOl ⁇ m to 5 ⁇ m or ranges from Ig to 5Og per IL of the filter substrate.
• the formation amount of the protection layer is less than the above range, it is difficult to suppress the migration of the alkali metal to the filter substrate.
• the formation amount of the protection layer exceeding the above range is impractical due to an excessive increase in pressure loss.
• alkali metal is supported in an amount of 0.6 mole or more per IL of the filter substrate.
• PM can be oxidized, is lowered, so that PM can be oxidized at a low temperature of 300 °C or below.
• the exhaust gas-purifying catalyst according to the present invention can purify PM by oxidation from a low-temperature range lower than 300 0 C, so that the PM oxidation performance can be considerably enhanced. As a result, accumulation of PM is suppressed, thereby suppressing an increase in pressure loss. Thus, continuous regeneration of the catalyst for PM purification can be stably achieved, so that it is possible to prevent defects such as cracks caused by forced regeneration.
• a protection layer made of an oxide reactable with the alkali metal is formed between the filter substrate and the catalyst bed, as described above, it is possible to suppress the alkali metal from migrating to the filter substrate by the protection layer.
• FIG. 1 illustrates an exhaust gas-purifying catalyst according to this example.
• This catalyst includes: a filter substrate 1 including inlet cells 10 each clogged at an exhaust gas downstream side thereof, outlet cells 11 each arranged adjacent to the inlet cells, and clogged at an exhaust gas upstream side thereof, and porous cell partition walls 12 partitioning the inlet cells 10 and the outlet cells 11 from each other; and a catalyst bed 2 formed on the surfaces of the cell partition walls 12 and on the surfaces of pores formed in the cell partition walls 12.
• a commercially-available DPF made of cordierite is used.
• This DPF has a test piece size (35cc, 30mm (diameter) x 50mm (length) ) , and a porosity of 60% to 67%, a pore volume of 0.58cc/g to 0.65cc/g, and an average pore diameter of 25 ⁇ m to 35 ⁇ m at the cell partition walls 12.
• a detailed description of the structure of the catalyst bed 2 will be given through a description of a method for manufacturing the catalyst bed 2.
• a slurry is prepared by mixing catalyst powder previously supporting Pt with Y-AI 2 O 3 powder (specific surface area of 220m 2 /g) , together with an alumina sol and ion-exchanged water, such that the mixture has a viscosity of lOOcps or less.
• the prepared slurry is milled such that solid grains thereof have an average diameter of l ⁇ m or less . Thereafter, the filter substrate 1 is dipped in the slurry, to allow the slurry to be introduced into the cells.
• the slurry is then sucked from the end of the filter substrate 1 opposite to the dipped end in a state in which the filter substrate 1 has been upwardly taken out of the slurry, to remove a surplus of the slurry from the filter substrate 1.
• the filter substrate 1 is calcined at 500 0 C for 3 hours. This procedure is performed two times, in order to adjust the formation of the coating layer such that the coating layer is formed on the inlet cells 10 and outlet cells 11 in substantially same amounts, respectively.
• the formation amount of the coating layer is 15Og per IL of the filter substrate 1.
• the coating layer is formed on the surfaces of the inlet cells 10 and outlet cells 11 and on the surfaces of the pores.
• the Pt supporting amount of the coating layer is 3g/L.
• Example 2 An exhaust gas-purifying catalyst according to Comparative Example 1 is prepared in the same manner as Example 1, except that the supported amount of Li is 0.3 mole/L. (Example 2) [0035] An exhaust gas-purifying catalyst according to Example
• Example 2 is prepared in the same manner as Example 1, except that a potassium acetate aqueous solution is used in place of the lithium acetate aqueous solution, and K is supported in the coating layer in an amount of 0.6 mole/L.
• Example 3 is prepared in the same manner as Example 1, except that a potassium acetate aqueous solution is used in place of the lithium acetate aqueous solution, and K is supported in the coating layer in an amount of 1.5 mole/L.
• An exhaust gas-purifying catalyst according to Comparative Example 2 is prepared in the same manner as Example 1, except that a potassium acetate aqueous solution is used in place of the lithium acetate aqueous solution, and K is supported in the coatinq layer in an amount of 0.3 mole/L.
• An exhaust qas-purifying catalyst according to Comparative Example 3 is prepared in the same manner as Example 1, except that the alkali metal is not supported.
• An exhaust gas-purifying catalyst according to Comparative Example 4 is prepared in the same manner as Example 1, except that a barium acetate aqueous solution is used in place of the lithium acetate aqueous solution, and Ba is supported in the coating layer in an amount of 0.3 mole/L.
• Each PM-attached catalyst was loaded in an evaluation apparatus, and was then subjected to an increase in temperature from room temperature to a temperature of 600 0 C at a rate of 10°C/min under the condition in which a model gas consisting of 10% of O 2 , 500 ppm of NO, and the balance of N 2 flowed through the catalyst at a flow rate of 0.03m 3 /min. •
• the catalysts of the examples exhibit a low PM oxidation initiation temperature and a low PM oxidation peak temperature, as compared to the catalysts of Comparative Examples 1 and 2. That is, it can be clearly seen that the catalysts of the examples can oxidize PM from a low-temperature range, and exhibit a high PM oxidation activity in the low-temperature range.
• the supported amount of K is preferable to be 1.5g/L, as compared to 0.6g/L, because the catalyst of Example 3 exhibits a lower temperatures than that of Example 2. Also, it can be seen that K is more preferable than Li because the catalyst of Example 2 exhibitsa lower temperatures than that of Example 1. On the other hand, it can be seen that Ba representing the alkaline earth metal of Comparative Example 4 has no effect obtained in a supported state.
• a plurality of catalysts were prepared in the same manner as that of Example 2, except that they had different K supporting amounts within a range of 0 mole/L to 1.5 mole/L, respectively.
• a PM oxidation initiation temperature was measured in accordance with the above-described method.
• FIG. 4 depicts the measured results.
• FIG. 5 illustrates an exhaust gas-purifying catalyst according to this example.
• the catalyst according to this example includes: a filter substrate 1 including inlet cells 10 each clogged at an exhaust gas downstream side thereof, outlet cells 11 each arranged adjacent to the inlet cells and clogged at an exhaust gas upstream side thereof, and cell partition walls 12 partitioning the inlet cells 10 and the outlet cells 11 from each other; a protection layer 3 formed on the surfaces of the cell partition walls 12 and on the surfaces of pores formed in the cell partition walls 12; and a catalyst bed 2 formed on the 'surface of the protection layer 3.
• This catalyst is identical to that of Example 2, except that the catalyst includes the protection layer 3. Accordingly, a detailed description of the structure of the catalyst bed 2 will be given through a description of a method for manufacturing the catalyst bed 2.
• the filter substrate 1 is dipped in a slurry, in which a silica sol is distributed, to allow the slurry to be introduced into the cells.
• the slurry is then sucked from the end of the filter substrate 1 opposite to the dipped end in a state in which the filter substrate 1 has been upwardly taken out of the slurry, to remove a surplus of the slurry from the filter substrate 1.
• the filter substrate 1 is calcined at 500 0 C for 3 hours. This procedure is performed two times, in order to adjust the formation of the protection layer such that the protection layer is formed on the inlet cells 10 and outlet cells 11 in substantially same amounts, respectively.
• the formation amount of the protection layer is 2Og per IL of the filter substrate 1 (substantially a thickness of I ⁇ m) .
• the catalyst bed 2 is formed in the same manner as that of Example 2. (Example 5)
• the protection layer 3 which is made of TiO 2 is formed in the same manner as that of Example 4, except that a titania sol is used in place of the silica sol. Thereafter, the catalyst bed 2 is formed in the same manner as that of Example 2. (Example 6)
• the protection layer 3 which is made of Al 2 O 3 is formed in the same manner as that of Example 4, except that an" alumina sol is used in place of the silica sol. Thereafter, the catalyst bed 2 is formed in the same manner as that of Example 2.
• Experimental Example 4 • Evaluation>
• a high-temperature durability test was carried out by maintaining the catalyst in a heated state in an electric furnace at 700 0 C for 10 hours. Thereafter, the above-described test was carried out to measure a PM oxidation initiation temperature.
• the strength of the filter substrate 1 was measured by Autograph. Based on the measured results, the catalysts were evaluated to be ⁇ O" when exhibiting a compressive strength of more than 2 MPa, N ⁇ ⁇ " when exhibiting a compressive strength ranging from 1.5 MPa to 2 MPa, or "X" when exhibiting a compressive strength of less than 1.5 MPa. Table 1 shows the evaluated results.
• Example 2 exhibits a degradation in substrate strength after the high-temperature durability test.
• a degradation in substrate strength can be suppressed by forming a protection layer, as in Examples 4 to 6.
• a protection layer made of SiO 2 or TiO 2 is formed, results similar to those of Comparative Example 3 supporting no K are obtained. In this case, accordingly, it is possible to greatly suppress a degradation in substrate strength.

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• Chemical Kinetics & Catalysis (AREA)
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• Geometry (AREA)
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• Exhaust Gas Treatment By Means Of Catalyst (AREA)
• Filtering Of Dispersed Particles In Gases (AREA)
• Exhaust Gas After Treatment (AREA)
• Processes For Solid Components From Exhaust (AREA)

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• 2006
  • 2006-01-17 JP JP2006008894A patent/JP2007190459A/ja active Pending
• 2007
  • 2007-01-15 EP EP07713661A patent/EP1979070A1/de not_active Withdrawn
  • 2007-01-15 WO PCT/JP2007/050857 patent/WO2007083779A1/en not_active Ceased
  • 2007-01-15 KR KR1020087017134A patent/KR20080078894A/ko not_active Ceased
  • 2007-01-15 CA CA002635082A patent/CA2635082A1/en not_active Abandoned
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