JPH09220423A - Diesel exhaust gas purifying filter and production thereof - Google Patents

Diesel exhaust gas purifying filter and production thereof

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Publication number
JPH09220423A
JPH09220423A JP2806996A JP2806996A JPH09220423A JP H09220423 A JPH09220423 A JP H09220423A JP 2806996 A JP2806996 A JP 2806996A JP 2806996 A JP2806996 A JP 2806996A JP H09220423 A JPH09220423 A JP H09220423A
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filter
cell
exhaust gas
honeycomb
average pore
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JP3560408B2 (en )
Inventor
Terutaka Kageyama
Toshiharu Kondo
Tomohiko Nakanishi
Yoshinori Nakayama
慶則 中山
友彦 中西
照高 影山
寿治 近藤
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Denso Corp
Nippon Soken Inc
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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Abstract

PROBLEM TO BE SOLVED: To provide a diesel exhaust gas purifying filter low in pressure loss and having material with a large surface area such as an activated alumina, depasited on the surface and the inside part of a honeycomb cell side wall. SOLUTION: The filter has a porous ceramic filter constituted so as to collect particulates contained in the exhaust gas on the surface and the inside part of the cell side wall 2 by alternately sealing both ends of the cell opening part of a ceramic honeycomb structural body to make the exhaust gas to flow to the adjacent cell through pores of the cell side wall 2 of the honeycomb. In such a case, the cell wall of the honeycomb structural body has 40-60% porosity and 5-35μm average pore diameter and is coated with a slurry containing the activated alumina having smaller particle diameter than the average pore diameter.

Description

【発明の詳細な説明】 DETAILED DESCRIPTION OF THE INVENTION

【0001】 [0001]

【発明の属する技術分野】本発明は、ディーゼルエンジン等の内燃機関から排出されるガスに含まれている物質のうち少なくともパティキュレートを除去し、排気ガス中の炭化水素(HC)、一酸化炭素を浄化するために用いられるパティキュレート捕集用のフィルタに関する。 The present invention relates to is to remove at least particulates of substance contained in the gas discharged from an internal combustion engine such as a diesel engine, hydrocarbons in the exhaust gas (HC), carbon monoxide about particulate filter for collecting used to purify.

【0002】 [0002]

【従来の技術】ディーゼルエンジン等の内燃機関から排出されるパティキュレートには、人体に有害な物質が含まれており、これを除去することが環境上の課題となっている。 BACKGROUND OF THE INVENTION particulates exhausted from an internal combustion engine such as a diesel engine contains harmful substances to the human body, the removal of this has become an issue on the environment. このため、従来では、ディーゼルエンジンの排気系に設けたフィルタでパティキュレートを捕集し、一定量捕集した後パティキュレートを電気ヒータやバーナ等で燃焼除去する方法が行われている。 Therefore, conventionally, by trapping particulates in a filter provided in an exhaust system of a diesel engine, a method for burning and removing the particulates after a certain amount trapped by an electric heater or a burner or the like is performed. また、フィルタに担持した白金族金属触媒でパティキュレートの燃焼温度を下げ、捕集したパティキュレートを連続的に燃焼させる方法もある。 Furthermore, lowering the combustion temperature of the particulate platinum group metal catalyst supported on the filter, there is a method to continuously burn the trapped particulates. 前者の捕集したパティキュレートを電気ヒータやバーナ等で燃焼除去する方法の場合、パティキュレートの捕集量が多いほど燃焼時のフィルタ最高温度が上昇し、フィルタにかかる熱応力でフィルタが破損することがあり、パティキュレートの捕集量制御が重要であり、完全に捕集量を制御するには至っていない。 In the method of collecting combustion remove particulates in an electric heater or a burner like the former, it rose filters the maximum temperature at the time of combustion as collection amount of particulates is large, the filter may be damaged by thermal stress on the filter that there is, it is important collection amount control of particulate matter, it does not come to control the complete collection amount is. 後者の触媒による燃焼の場合、燃焼温度が比較的低くなりフィルタにかかる熱応力が小さくなるため、耐熱性に優れている。 For combustion by the latter catalyst, the thermal stress is reduced in accordance with the relatively low will filter the combustion temperature, it has excellent heat resistance.

【0003】上記の方法において、パティキュレートの捕集にはおもに、セラミックのハニカム構造体を用いることが多く、その材質としては、低熱膨張性をしめすコーディエライトが一般的に用いられる。 [0003] In the above method, mainly in the collection of the particulates, often used honeycomb structural body of a ceramic, as the material thereof, cordierite indicating the low thermal expansion are generally used.

【0004】本発明の対象とするディーゼル排ガス浄化フィルタは、ハニカム構造のセラミックモノリスの片端のセル開口部、例えばガス入口側のセル開口部は一個おきに目封じしてあり、ガス出口側のセル開口部は入口側の開口部が目封じしていないセルについてのみ目封じする。 [0004] Diesel exhaust gas purification filter to which the present invention is a cell opening in one end of the ceramic monolith honeycomb structure, for example cell openings of the gas inlet side is Yes and sealed to one every other, the gas outlet side of the cell opening the opening of the inlet side is sealed only cells that are not plugged. したがって、排気ガスはセル側壁の細孔を通過し、 Thus, the exhaust gas passes through the pores of the cell side walls,
排気ガスとともに流れるパティキュレートはこのセル則壁の表面およびセル則壁の細孔内部で捕集される。 Particulates flowing together with the exhaust gas is trapped by the pore inner surface and the cell law walls of the cell rule walls.

【0005】 [0005]

【発明が解決しようとする課題】ハニカム構造の多孔質セラミックフィルタは前記のようにモノリスハニカムの両端を交互に目封じすることにより、ガスはセル壁の数μm〜数十μmの気孔を通過して隣接するセルに流れる構造のため、パティキュレートの捕集効率が他の構造のフィルタよりも高い利点がある。 Porous ceramic filter of honeycomb structure ## SUMMARY OF THE INVENTION] is by plugging the ends of the monolith honeycomb are alternately as described above, the gas passes through the several μm~ several tens μm pores of the cell walls for structural flowing in adjacent cells Te, there is a high advantage over filter collection efficiency of other structures of the particulate. このフィルタに触媒を担持するため、その担体として活性アルミナ等の高比表面積材料をセル側壁表面およびセル側壁の細孔内部にコーティングする場合、高比表面積材料がセル側壁の細孔を閉塞してしまい、コーティングしてないフィルタに比べ圧力損失が高くなるという問題がある。 For carrying the catalyst on the filter, when coating a high specific surface area material such as active alumina within the pores of the cell sidewall surfaces and the cell side wall as a carrier, high specific surface area material to close the pores of the cell side wall put away, there is a problem that pressure loss becomes higher than a filter that is not coated. フィルタの圧力損失が高いとエンジン出力の低下につながるため、圧力損失はできるだけ低いほうがよい。 Since the pressure loss of the filter is high leading to a drop in the engine output, the pressure loss should be as low as possible. しかし、圧力損失を低くするため、フィルタの気孔率、気孔径を大きくしすぎるとパティキュレートの捕集効率を低下させてしまう恐れがある。 However, to reduce the pressure loss, the porosity of the filter, there is a possibility that when the pore diameter is too large would reduce the collecting efficiency of particulates.

【0006】ハニカム構造のセラミック担体に活性アルミナ等の高比表面積材料をコーティングする場合、活性アルミナの粒径を規定したものがいくつか公知となっている。 [0006] When coating a high specific surface area material such as activated alumina ceramic support of honeycomb structure, that defines the particle size of the active alumina has a few known. 特公昭55−1818号公報では、活性アルミナ粒径を0.1〜100μmであると規定しているが、ベーマイト等の無定形アルミナと混合することが前提であり、これにより活性アルミナコーティング層の接着強度が向上するとしている。 In JP-B 55-1818 discloses While the activated alumina particle diameter is defined to be 0.1 to 100 [mu] m, a prerequisite to be mixed with amorphous alumina boehmite, thereby the active alumina coating layer the adhesive strength is to be enhanced. また、特公平4−80736号公報では、活性アルミナの平均粒径を20μm以下であると規定することにより、活性アルミナスラリーの安定した分散性を確保するのに有効であり、活性アルミナコーティング層の接着強度が向上するとしている。 Further, in Kokoku 4-80736 discloses, by defining an average particle size of the activated alumina and is 20μm or less, it is effective in ensuring a stable dispersion of active alumina slurry, the active alumina coating layer the adhesive strength is to be enhanced. しかし、いずれも、ハニカム構造のセラミック担体に活性アルミナをコーティングしたとき、コーティング層の剥離を防止するために接着強度を向上させることを目的としている。 However, either, when coated activated alumina to ceramic carrier of honeycomb structure, it is an object of the bonding strength is improved to prevent peeling of the coating layer. そしてこれらはフロースルー型排ガス浄化装置であって、排ガスがハニカムの壁の中を通過せず、その壁で形成された管状通路を通過する形式のもので、フィルタと呼べるものではなく、壁の強度を強くするため一般に壁の気孔率は低く気孔径は小さいものである。 And these are flow-through exhaust gas purifying apparatus, the exhaust gas does not pass through the walls of the honeycomb, of the type that passes through the tubular passage formed by the wall, and not to call the filter, the walls of the the porosity of generally the wall to increase the intensity is intended pore diameter lower is small.

【0007】本発明は、ハニカム構造の多孔質モノリスハニカムの両端を交互に目封じすることにより、ガスがセル壁の気孔を通過して隣接するセルに流れる構造の多孔質ハニカムフィルタにおいて、活性アルミナ等の高表面材料をセル側壁の表面だけでなく、セル側壁の細孔内部にも均一にコーティングし、しかも圧損失が高いという問題を生じないものを提供することを目的とするものである。 [0007] The present invention, by plugging the ends of the porous monolith honeycomb of the honeycomb structure alternately in the porous honeycomb filter structure that flows in the cell gas is adjacent through the pores of the cell walls, activated alumina not only high surface material of the surface of the cell side walls etc., also uniformly coated within the pores of the cell side walls, yet it is an object to provide what does not cause a problem that pressure loss is high.

【0008】 [0008]

【課題を解決するための手段】請求項1記載の発明によれば、多孔質セラミックハニカム構造体を有するディーゼル排ガス浄化フィルタにおいて、このハニカム構造体のセル側壁の気孔率が40〜65%で、平均細孔径が5 According to the Summary of the invention of claim 1, wherein, in the diesel exhaust gas purification filter having a porous ceramic honeycomb structure, the porosity of the cell side wall of the honeycomb structure at 40 to 65%, the average pore diameter of 5
〜35μmであり、これに担持される高比表面積材料の90wt%以上が上記ハニカム構造体セル側壁の平均細孔径よりも小さくすることによって、本発明の高比表面材料のコーティングを有するディーゼル排ガス浄化フィルタを圧力損失の低いものとすることができる。 A ~35Myuemu, by more than 90 wt% of the high specific surface area material to be carried is smaller than the average pore diameter of the honeycomb structure cells sidewall to diesel exhaust gas purification having a coating of high specific surface material of the present invention the filter can be made low pressure loss.

【0009】 [0009]

【発明の実施の形態】本発明のディーゼル排ガス浄化フィルタは、セラミックモノリスハニカム構造体のセル側壁表面及びセル側壁内部細孔表面に活性アルミナ等の高比表面積材料を被覆し、その上に触媒金属を被覆し、次いで得られたハニカムのセル開口部の両端を交互に目封じすることにより作られる。 Diesel exhaust gas purification filter of the embodiment of the present invention is the high specific surface area material such as active alumina coated on the cell sidewall surfaces and a cell sidewall interior pore surfaces of the ceramic monolith honeycomb structure, the catalyst metal thereon coated and then both ends of the cell openings of the obtained honeycomb to be produced by alternately plugged.

【0010】本発明に用いるセラミックモノリスハニカム構造体は、従来低熱膨張係数セラミックスとして知られているコーディエライト(化学組成2MgO・2Al [0010] ceramic monolith honeycomb structure used in the present invention, cordierite conventionally known as a low thermal expansion coefficient ceramic (chemical composition 2MgO · 2Al
2 2 O 3・5SiO 2 )で作られているのが好ましく、側壁の気孔率は約40%〜65%であるのが好ましく、より好ましくは約45%〜60%であり、平均細孔径は約5μm〜35μmであるのが好ましく、より好ましくは約10μm〜30μmである。 Is preferably made of 3 · 5SiO 2), it is preferable porosity of the side walls is approximately 40% to 65%, more preferably from about 45% to 60%, average pore size about 5μm~ is preferably from 35 [mu] m, more preferably about 10 m to 30 m.

【0011】一方、前記ハニカム構造体にコーティングする活性アルミナ等の高比表面積材料の粒径は、その9 Meanwhile, the particle size of the high specific surface area material such as activated alumina coated on the honeycomb structure, the 9
0wt%以上、好ましくは95wt%以上が前記ハニカム構造体の平均細孔径よりも小さな粒径であることが望ましい。 0 wt% or more, preferably it is desirable least 95 wt% are smaller particle size than the average pore diameter of the honeycomb structure. 高比表面積材料の粒径が前記ハニカム構成体の平均細孔径よりも大きいものが10wt%より多い場合、高比表面材料は前記ハニカム構造体のセル側壁内部の細孔に入らず、セル側壁表面を覆う高比表面積材料が相対的に増加し、コーティング層の膜厚が厚くなり圧損上昇が大きくなるので好ましくない。 If those particle diameter of the high specific surface area material is greater than the average pore diameter of the honeycomb structure is more than 10 wt%, high specific surface material does not enter the pores of the internal cell wall of the honeycomb structure, the cell sidewall surfaces high specific surface area material to cover relatively increased, undesirably the film thickness is thick becomes pressure loss increase of the coating layer increases. また、高比表面積材料の9 In addition, a high specific surface area material 9
0wt%以上のものの粒径が前記ハニカム構造体の平均細孔径よりも小さい場合、セル側壁内部の細孔に入る高比表面積材料が増加する。 If the particle size of 0 wt% or more of less than the average pore diameter of the honeycomb structure, a high specific surface area material entering the pores of the internal cell sidewalls is increased. このときエアーブローまたは、 At this time, air blow or,
クリーナによる吸引を十分行ない余分な高表面材料スラリーを取り除き、細孔内を閉塞させることなく均一に分散させてコーティングすることで、圧損の上昇を抑えることができる。 The suction by the cleaner removes enough deeds excess high surface material slurry to coat uniformly dispersed without blockage of the pores, it is possible to suppress an increase in pressure loss. 圧損は、フィルタの入口側よりフィルタ内にエアーを流入させ、フィルタの出口側よりフィルタ外へエアーを流出させたとき、入口側と出口側のエアーの差であり、入口側より流入させるエアー量は2000 Pressure loss is caused to flow into the air from the inlet side of the filter in the filter, when allowed to flow out the air to filter out from the outlet side of the filter, the difference of the air inlet side and the outlet side, an air amount that flows from the inlet side 2000
L/分(線速度1.8cm/秒)の条件で測定して、45 As measured under the conditions of L / min (linear velocity 1.8 cm / sec), 45
mmAq(水柱)以下であることが望ましい。 mmAq (water column) is desirably less.

【0012】本発明のディーゼル排ガス浄化フィルタは、ディーゼルエンジンの排ガス中に含まれるパティキュレートを捕集するための構造として入口側のセルから流入したガスは出口側のセルは目封じされているため、 [0012] Diesel exhaust gas purification filter of the present invention, since the gas flowing from the inlet side of the cell as a structure for trapping particulates contained in diesel engine exhaust gas cells at the outlet side is sealed ,
セル側壁を通り抜け隣接するセルの出口から排出される。 It is discharged from the outlet of the adjacent cells through the cell sidewalls. セル壁を通り抜けるとき排ガス中のパティキュレートのみが捕集される。 Only particulates in exhaust gases when passing through the cell walls are collected. このとき、フィルタを構成する活性アルミナ被覆前のハニカムの気孔率と平均細孔径が前記の範囲より小さい場合、パティキュレートの捕集効率が向上するが、フィルタの圧力損失が高くなりエンジン出力が低下するので好ましくない。 At this time, when the average pore size and porosity of the honeycomb before activated alumina coating constituting the filter is less than the range described above, but improves the efficiency of collecting particulates, the engine output increases the pressure loss of the filter is reduced undesirably. また、この範囲より大きいとパティキュレートの捕集効率が低下するので好ましくない。 Also, undesirable collection efficiency in this range is larger than the particulates is lowered.

【0013】また、活性アルミナ等の高比表面積材料の粒子径が前記のような範囲である理由は、高比表面積材料が前記ハニカム構造体のセル側壁の細孔内部に侵入する必要があるためである。 [0013] The reason the particle diameter of the high specific surface area material such as activated alumina is in the range as above, it is necessary to high specific surface area material from entering within the pores of the cell wall of the honeycomb structure it is. 従来、高比表面積材料をハニカム型モノリス担体にコーティングするのはセル側壁の表面のみであったが、排ガスがセル側壁の細孔内部を通過するような構造のハニカム型フィルタの場合、排ガスに含まれるパティキュレートがフィルタのセル側壁の表面上およびセル側壁の細孔内部に留まるので、このとき、パティキュレートはこの高比表面積材料と細孔内部で接触することが、触媒作用を受けるために必要である。 Conventionally, a high specific surface area material to coat the honeycomb monolithic support was only the surface of the cell side walls, the case of the honeycomb filter structure as exhaust gas passes through the pores of the cell sidewalls, contained in the exhaust gas since particulate matter remains within the pores of the surface and the cell side walls of the cell side wall of the filter, this time, particulates be contacted within this high specific surface area material and the pores need to be catalyzed it is. したがって、高比表面積材料は前記の粒径が必要である。 Therefore, high specific surface area material is required particle size of the can. また、前記高比表面積材料のコート量(担持量) Further, the coating amount of the high specific surface area material (supported amount)
は20〜75g/Lが好ましい。 The 20~75g / L is preferred. コート量が20g/L Coat amount of 20g / L
よりも少ない場合、排ガスの浄化能力が低く好ましくない。 If less than, undesirable low exhaust gas purification capability. また75g/Lよりも大きい場合、フィルタの圧損が高くなってエンジン出力が低下するため好ましくない。 The greater than 75 g / L, undesirable because the engine output is reduced by pressure loss of the filter becomes high.

【0014】本発明における高比表面積材料としては活性アルミナの他シリカ、ジルコニア、チタニア、又はこれらの内の2種以上を含むものを使用することができる。 [0014] The high specific surface area material in the present invention may be used other silica activated alumina, zirconia, titania, or those containing two or more of these.

【0015】本発明のディーゼル排ガス浄化フィルタは、少なくともディーゼルエンジンの排ガスに含まれているパティキュレートを捕集し、燃焼除去させるものである。 [0015] Diesel exhaust gas purification filter of the present invention is to collecting particulates contained in the exhaust gas at least a diesel engine, is intended to burn removed. 活性アルミナ等の高比表面積物質をフィルタにコーティングするのは、好ましくは白金族触媒金属をコーティングさせるための担体にするためである。 For coating a high specific surface area material such as activated alumina filter is to preferably to a carrier for coated platinum group metal catalyst. 一般に白金族触媒金属はパティキュレートの燃焼温度を下げる触媒として用いられ、さらに一酸化炭素や炭化水素の酸化触媒として用いられている。 Generally the platinum group metal catalyst is used as a catalyst to reduce the combustion temperature of particulates, it has been used as further oxidation catalyst of carbon monoxide and hydrocarbons. 本発明のフィルタは、好ましくは少なくとも一種類の白金族元素からなる金属触媒を担持してあるフィルタである。 Filter of the present invention is preferably a filter that is carrying a metal catalyst composed of at least one platinum group elements.

【0016】次に、本発明のディーゼル排ガス浄化フィルタについて図1〜3をもって具体的に説明する。 [0016] Next, the diesel exhaust gas purification filter of the present invention will be described with FIGS. 図1 Figure 1
のように、このハニカム構造の多孔質セラミックフィルタはモノリスハニカムの両端の目封じ材1で交互に目封じすることにより、ハニカム型フィルタのセル側壁2に活性アルミナ粒子3からなるコーティング層4を形成している。 As described above, by the porous ceramic filter of the honeycomb structure to be plugged alternately plugging material 1 across the monolith honeycomb, forming a coating layer 4 made of activated alumina particles 3 on the cell side wall 2 of the honeycomb filter are doing. 図1のA部を拡大した図2のようにフィルタの平均細孔径よりも小さな粒径の活性アルミナを用いれば、セル側壁の細孔5の内部を閉塞することなくコーティングされるのでフィルタの圧損上昇が少ない。 The use of activated alumina smaller particle size than the average pore size of the filter as shown in FIG. 2 an enlarged portion A of FIG. 1, the pressure loss of the filter since the coated without clogging the inside of pores 5 of the cell side wall rise is small. しかし、図1のA部を拡大した図3のようにフィルタの平均細孔径よりも大きな粒径の活性アルミナを用いた場合、 However, when using the activated alumina particle diameter larger than the average pore size of the filter as shown in FIG. 3 an enlarged portion A of FIG. 1,
セル壁の細孔を閉塞させるので、フィルタの圧損は大幅に上昇する。 Since occlude the pores of the cell walls, pressure loss of the filter is greatly increased. また、活性アルミナのコーティング部分に白金族触媒金属を担持することで、セル壁内部で捕集されたパティキュレートおよび他の排ガス成分(HC,C Moreover, by supporting a platinum group catalyst metal in the coating portion of the activated alumina, particulates trapped within the cell walls and other exhaust gas components (HC, C
O等)の浄化効率を高めている。 To enhance the purification efficiency of the O, etc.). 尚、これらの図面において触媒金属層の記載は省略している。 Incidentally, the description of the catalytic metal layer in these drawings has been omitted.

【0017】パティキュレートを含むディーゼル排ガスは、セル入口側6からセル内に進入し、セル壁2を通過してセル出口側7から出ていく。 [0017] Diesel exhaust gas containing particulates, enters the cell inlet side 6 in the cell, leaving the cell outlet 7 passes through the cell walls 2. このとき、パティキュレートはセル壁表面および内部の細孔で捕集される。 At this time, particulates are captured by the cell wall surface and inside of the pores. 白金族触媒金属は、通常活性アルミナをコーティングした後にあらためてコーティングするが、活性アルミナと混合した溶液でコーティングすることも可能である。 Platinum group catalyst metal, although again coated after coating the normal activated alumina, can also be coated with a solution mixed with activated alumina.

【0018】 [0018]

【実施例】以上のような材料を用いてコーティングしたフィルタは、低圧損のディーゼルパティキュレートフィルタとして好適に用いることができる。 Filter coated with EXAMPLES above-mentioned materials can be suitably used as a diesel particulate filter of low pressure loss. 以下に、その実施例と比較例を示す。 The following is a comparative example and its embodiments.

【0019】〔実施例1〕主原料にシリカ、水酸化アルミニウム、タルクを用い、コーディエライト(2MgO [0019] Example 1 Main raw material silica, aluminum hydroxide, using talc, cordierite (2MgO
・2Al 23・5SiO 2 )組成になるように調整し、つぎに多孔質にするためのカーボンをこれら主原料に対して20wt%添加して、公知の押し出し製法でセラミックハニカム構造体を作製し、1350℃〜1450 · 2Al 2 O 3 · 5SiO 2 ) and adjusted to the composition, then the carbon to a porous added 20 wt% with respect to these main raw materials, produce a ceramic honeycomb structure by a known extrusion method and, 1350 ℃ ~1450
℃の最高温度、5 ℃〜200℃の昇温速度、2〜20時間の保持時間で焼成して、気孔率が55%、平均細孔径28μmの細孔特性を持ち、セル側壁厚さ0.45mm、 Maximum temperature of ° C., heating rate of 5 ° C. to 200 DEG ° C., and calcined at a retention time of 2-20 hours, a porosity of 55%, has a pore properties of average pore diameter of 28 .mu.m, the cell sidewall thickness 0. 45mm,
1平方インチあたりのセル数が150個の直径140m The number of cells per square inch 150 pieces with a diameter of 140m
m、長さ130mmの多孔質コーディエライトハニカム構造体を得た。 m, to obtain a porous cordierite honeycomb structure length 130 mm.

【0020】一方、高比表面積材料として、中心粒径5 Meanwhile, as a high specific surface area material, the mean particle size of 5
μmで、粒径が28μmより大きい粒子が5wt%以下の活性アルミナ(住友化学製)670gとアルミナゾル(日産化学製)330gを水4リッターとともに混合し、攪拌して活性アルミナスラリーを作製した。 In [mu] m, the particle size is 28μm particles larger than 5 wt% or less of the active alumina (manufactured by Sumitomo Chemical) 670 g and alumina sol (Nissan Chemical Industries) 330 g was mixed with water 4 liters to prepare activated alumina slurry and stirred.

【0021】前記の多孔質コーディエライトハニカム構造体を活性アルミナスラリーに完全に浸した(ウォッシュコート)。 [0021] completely immersed in the porous cordierite honeycomb structure activated alumina slurry (washcoat). その後、エアークリーナーおよび圧縮エアーで余分に付着したスラリーをできるだけ完全に取り除いた。 Then, to remove the slurry excessively deposited in the air cleaner and compressed air as completely as possible. コーティングを繰り返してコート量の異なる5種類のハニカムを作製した。 We were prepared five different honeycomb that the coat weight by repeating the coating. さらにその後、120℃で2 Thereafter, 2 at 120 ° C.
時間乾燥し、800℃で焼成した。 And drying time, and calcined at 800 ° C.. 単位体積当たりのコート量はウォッシュコート前後のハニカム重量差から算出した<コート量〔g/L〕=(コート前重量−コート後重量)/ハニカム体積)>。 The coating amount was calculated from the honeycomb weight difference before and after the washcoat per unit volume <coat weight [g / L] = (coating weight before - weight after coating) / honeycomb volume)>. この後、0.1mol /L After this, 0.1mol / L
の塩化白金酸水溶液中に30分浸し、120℃で2時間乾燥させた後、800℃で焼成して白金を担持させた。 Soak for 30 minutes in an aqueous solution of chloroplatinic acid, dried 2 hours at 120 ° C., was supported platinum was fired at 800 ° C..
白金の担持量は約2g/Lであった。 Supported amount of platinum was about 2 g / L.

【0022】白金を担持させたハニカム構造体のガス入口側のセル開口部を一個おきに目封じし、ガス出口側では入口側で目封じしてないセルについてのみ目封じした。 [0022] The cell openings of the gas inlet side of the honeycomb structure of carrying platinum plugged to one every other, in the gas outlet side was sealed only cells that are not plugged at the inlet side. 目封じ材はコーディエライト、アルミナ、ジルコニアなどの1000℃以上の耐熱性のあるセラミック材料であれば特に限定せず、セラミック製の接着剤でもよい。 Plugging material cordierite, alumina not particularly limited as long as the ceramic material with a 1000 ° C. or higher heat resistance, such as zirconia, or a ceramic adhesive. この実施例においてはコーディエライトを用いた。 With cordierite in this embodiment.
このようにして、活性アルミナコート量の異なる触媒担体付きフィルタを作製した(担体A−1〜担体A− Thus, to produce a different catalyst support with filter active alumina coating amount (carrier A-. 1 to support A-
4)。 4).

【0023】〔実施例2〕実施例1で用いた多孔質コーディエライトハニカムフィルタと同様のフィルタを同様の方法で作製し、高比表面積材料として、中心粒径2μ [0023] Example 2 was prepared in the porous cordierite honeycomb filter and the same method as the same filter used in Example 1, as a high specific surface area material, the center particle size 2μ
mで、28μmより大きな粒子が5%以下の活性アルミナ(住友化学製)670gをアルミナゾル(日産化学製)330g及び水4リッターとともに混合し、攪拌した活性アルミナスラリーに前記フィルタをウォッシュコートした。 In m, mixed large particles of 5% or less of the active alumina (Sumitomo Chemical Co., Ltd.) 670 g of alumina sol (manufactured by Nissan Chemical) 330 g and with water 4 liters than 28 .mu.m, the filter was washcoated stirred activated alumina slurry. コーティングを繰り返してコート量の異なる5種類のフィルタを作製した。 We were prepared with five different filter coating amount Repeat coating. その後、エアークリーナーおよび圧縮エアーで余分に付着したスラリーをできるだけ完全に取り除いた。 Then, to remove the slurry excessively deposited in the air cleaner and compressed air as completely as possible. さらにその後、120℃で2時間乾燥し、800℃で焼成した。 Thereafter, it dried 2 hours at 120 ° C., and calcined at 800 ° C.. コート量を調べた後、 After examining the coating amount,
塩化白金酸水溶液中に30分浸し、120℃で2時間乾燥させた後、800℃で焼成して白金を担持させた。 Soaked 30 minutes in an aqueous solution of platinum chloride acid, dried 2 hours at 120 ° C., was supported platinum was fired at 800 ° C.. 白金の担持量は約2g/Lであった。 Supported amount of platinum was about 2 g / L.

【0024】その後、コーディエライトを用いて、白金を担持させたハニカム構造体のガス入口側のセル開口部を一個おきに目封じし、ガス出口側では入口側で目封じしてないセルについてのみ目封じし、触媒担体付きフィルタを作製した(担体B−1〜担体B−5)。 [0024] Then, using cordierite, the cell openings of the gas inlet side of the platinum honeycomb structure was supported plugged into one every the cells that are not plugged at the inlet side in the gas outlet side and only plugging, to prepare a catalyst support with the filter (carrier B-. 1 to support B-5).

【0025】〔比較例1〕実施例1で用いた多孔質コーディエライトハニカムフィルタと同様のフィルタを同様の方法で作製し、高比表面積材料として、中心粒径50 [0025] Comparative Example 1 The same filter and the porous cordierite honeycomb filter used in Example 1 was prepared in the same manner as a high specific surface area material, the central particle size 50
μmの活性アルミナ(住友化学製)670gをアルミナゾル(日産化学製)330g及び水4リッターとともに混合し、攪拌した活性アルミナスラリーに前記フィルタをウォッシュコートした。 By mixing the active alumina (Sumitomo Chemical Co.) 670 g of μm alumina sol (manufactured by Nissan Chemical) with 330g and water 4 liters, the filter was washcoated stirred activated alumina slurry. その後、エアークリーナーおよび圧縮エアーで余分に付着したスラリーをできるだけ完全に取り除いた。 Then, to remove the slurry excessively deposited in the air cleaner and compressed air as completely as possible. コーティングを繰り返してコート量の異なる3種類のフィルタを作製した。 It was prepared three kinds of filters having different coating amount Repeat coating. さらにその後、 Thereafter,
120℃で2時間乾燥し、800℃で焼成した。 Dried 2 hours at 120 ° C., and calcined at 800 ° C.. コート量を算出した後、0.1mol /Lの塩化白金酸水溶液中に30分浸し、120℃で2時間乾燥させた後、800 After calculating the coating amount, soaked 30 minutes in an aqueous solution of chloroplatinic acid in 0.1 mol / L, dried 2 hours at 120 ° C., 800
℃で焼成して白金を担持させた。 And fired at ℃ was supported platinum. 白金の担持量は2g/ The amount of supported platinum is 2g /
Lであった。 It was L.

【0026】その後、コーディエライトを用いて、白金を担持させたハニカム構造体のガス入口側のセル開口部を一個おきに目封じし、ガス出口側では入口側で目封じしてないセルについてのみ目封じし、触媒担体付きフィルタを作製した(担体C−1〜担体C−3)。 [0026] Then, using cordierite, the cell openings of the gas inlet side of the platinum honeycomb structure was supported plugged into one every the cells that are not plugged at the inlet side in the gas outlet side and only plugging, to prepare a catalyst support with the filter (carrier C-. 1 to carrier C-3).

【0027】〔比較例2〕実施例1で用いた多孔質コーディエライトハニカムフィルタと同様のフィルタを同様の方法で作製し、高比表面積材料として、中心粒径約2 [0027] Comparative Example 2 was produced in the porous cordierite honeycomb filter and the same method as the same filter used in Example 1, as a high specific surface area material, the mean particle size of about 2
5μmで、28μmより大きな粒子を45wt%含む活性アルミナ(住友化学製)670gをアルミナゾル(日産化学製)330g及び水4リッターとともに混合し、攪拌した活性アルミナスラリーに前記フィルタをウォッシュコートした。 In 5 [mu] m, by mixing the active alumina (Sumitomo Chemical Co., Ltd.) 670 g of the large particles containing 45 wt% of alumina sol (manufactured by Nissan Chemical) with 330g and water 4 liters than 28 .mu.m, the filter was washcoated stirred activated alumina slurry. その後、エアークリーナーおよび圧縮エアーで余分に付着したスラリーをできるだけ完全に取り除いた。 Then, to remove the slurry excessively deposited in the air cleaner and compressed air as completely as possible. コーティングを繰り返してコート量の異なる4 Repeat coating different coating amount 4
種類のフィルタを作製した。 To produce a kind of filter. さらにその後、120℃で2時間乾燥し、800℃で焼成した。 Thereafter, it dried 2 hours at 120 ° C., and calcined at 800 ° C.. コート量を算出した後、0.1mol /Lの塩化白金酸水溶液中に30分浸し、120℃で2時間乾燥させた後、800℃で焼成して白金を担持させた。 After calculating the coating amount, soaked 30 minutes in an aqueous solution of chloroplatinic acid in 0.1 mol / L, dried 2 hours at 120 ° C., was supported platinum was fired at 800 ° C.. 白金の担持量は約2g/Lであった。 Supported amount of platinum was about 2 g / L.

【0028】その後、コーディエライトを用いて、白金を担持させたハニカム構造体のガス入口側のセル開口部を一個おきに目封じし、ガス出口側では入口側で目封じしてないセルについてのみ目封じし、触媒担体付きフィルタを作製した(担体D−1〜担体D−4)。 [0028] Then, using cordierite, the cell openings of the gas inlet side of the platinum honeycomb structure was supported plugged into one every the cells that are not plugged at the inlet side in the gas outlet side and only plugging, to prepare a catalyst support with the filter (carrier D-. 1 to carrier D-4).

【0029】〔比較例3〕実施例1で用いた多孔質コーディエライトハニカムフィルタと同様のフィルタを同様の方法で作製し、活性アルミナによるコーティングをせずに白金を同様にして約2g/L担持させ、ハニカム構造体のガス入口側のセル開口部を一個おきに目封じし、 [0029] Comparative Example 3 The same filter and the porous cordierite honeycomb filter used in Example 1 was prepared in the same manner, approximately in the same manner platinum without coating with activated alumina 2 g / L is supported, the cell openings of the gas inlet side of the honeycomb structure plugged into one every
ガス出口側では入口側で目封じしてないセルについてのみ目封じし、触媒担体付きフィルタを作製した(担体E)。 In the gas outlet side sealed only for the cells that are not plugged on the inlet side, to prepare a catalyst support with the filter (carrier E).

【0030】表1に実施例および比較例で作製した担体のコート量を記載する。 [0030] describes the coating amount of the carrier produced in Examples and Comparative Examples in Table 1.

【0031】 [0031]

【表1】 [Table 1]

【0032】(触媒担体付きフィルタの圧力損失の測定)実施例1,2、比較例1,2,3により得られた担体A〜担体Eのすべてのフィルタについて、フィルタの入口側から圧縮エアーを流し、入口側と出口側の差圧を測定した。 [0032] (catalyst carrier with the measurement of the pressure loss of the filter) Examples 1 and 2, for all the filters of the resulting carrier A~ carrier E Comparative Examples 1, 2 and 3, the compressed air from the inlet side of the filter flow was measured differential pressure between the inlet side and the outlet side. 圧力損失の測定結果を図4に示す。 Figure 4 shows the measurement results of the pressure loss. この結果より、本発明品はコーティングを施した比較例1,2よりも圧損が低いことがわかる。 From the results, the product of the present invention it can be seen that the pressure loss is less than the comparative examples 1 and 2 were coated.

【0033】(フィルタの細孔分布測定)実施例1, [0033] (pore size distribution measurement of the filter) Example 1,
2、比較例1,2,3により得られた担体A〜担体Eのすべてのフィルタについて、細孔分布を測定した。 2, for all of the filters of the resulting carrier A~ carrier E in Comparative Example 1, 2 and 3 were measured pore distribution. 担体の平均細孔径と活性アルミナのコート量の関係を図5に示す。 The relationship between the average pore diameter and coating amount of the active alumina support is shown in FIG. コート量が増加していくと担体の平均細孔径は小さくなっていく。 When the coating amount is gradually increased by an average pore diameter of the carrier becomes smaller. 低圧損のディーゼル浄化用フィルタとして有利な平均細孔径は5μm〜35μmである。 Preferred average pore size as a diesel purifying filter of the low-pressure loss is 5Myuemu~35myuemu.

【図面の簡単な説明】 BRIEF DESCRIPTION OF THE DRAWINGS

【図1】本発明の1例の又は比較例のディーゼル排ガス浄化フィルタの横断面図。 Figure 1 is a cross-sectional view of the diesel exhaust gas purification filter of an example or a comparative example of the present invention.

【図2】図1のA部拡大図。 [Figure 2] A part enlarged view of FIG. 1.

【図3】図1のA部拡大図。 [Figure 3] A part enlarged view of FIG. 1.

【図4】実施例、比較例のフィルタの圧力損失の測定結果を示すグラフ。 [4]] is a view showing a measurement result of the pressure loss of the filter of the comparative example.

【図5】実施例、比較例のフィルタにおける担体の平均細孔径と活性アルミナのコート量の関係を示すグラフ。 [5]] is a view showing a relationship between the coating amount of the average pore diameter and activated alumina support in the filter of Comparative Example.

───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl. 6識別記号 庁内整理番号 FI 技術表示箇所 B01J 23/40 B01D 53/36 ZAB F01N 3/02 301 104B (72)発明者 影山 照高 愛知県刈谷市昭和町1丁目1番地 日本電 装株式会社内 (72)発明者 近藤 寿治 愛知県刈谷市昭和町1丁目1番地 日本電 装株式会社内 ────────────────────────────────────────────────── ─── front page continued (51) Int.Cl. 6 identification symbol Agency Docket No. FI art display portion B01J 23/40 B01D 53/36 ZAB F01N 3/02 301 104B (72) inventor Kageyama Terudaka Aichi Kariya Showacho 1-chome 1 address Japan electrical instrumentation within Co., Ltd. (72) inventor Toshiharu Kondo Kariya, Aichi Showacho 1-chome 1 address Japan electrical instrumentation within Co., Ltd.

Claims (2)

    【特許請求の範囲】 [The claims]
  1. 【請求項1】 セラミックハニカム構造体のセル開口部の両端を交互に目封じすることによりハニカムのセル側壁の気孔を通過して排ガスを隣接するセルに流し、排ガスに含まれるパティキュレートのみをセル側壁の表面および内部で捕集するようにした多孔質セラミックフィルタを有し、前記パティキュレートを燃焼する触媒金属を前記側壁表面及び内部に担持したディーゼル排ガス浄化フィルタにおいて、前記セラミックハニカム構造体が、 1. A ceramic both ends of cell openings of the honeycomb structure through the pores of the cell side walls of the honeycomb by alternately plugged sink in cells adjacent the exhaust gas, cell only particulates contained in the exhaust gas has a porous ceramic filter which is adapted to collect at the surface and inside of the side wall, in the diesel exhaust gas purification filter catalyst metal for burning the particulates carrying said sidewall surface and in the interior, the ceramic honeycomb structure,
    そのセル側壁の気孔率が40〜65%で、平均細孔径が5〜35μmであり、前記触媒金属を担持する担体として、その平均細孔径よりも小さい粒径のものが90wt% In the porosity of the cell side walls 40 to 65% and an average pore diameter of 5 to 35 m, as a carrier for carrying the catalyst metal, those particle size smaller than the average pore diameter 90 wt%
    以上を占める高比表面積材料を担持していることを特徴とするディーゼル排ガス浄化フィルタ。 Diesel exhaust gas purification filter which is characterized by carrying a high specific surface area material accounts for at least.
  2. 【請求項2】 少なくとも一種類の白金族元素からなる触媒金属が担持されている請求項1記載のフィルタ。 Wherein at least one filter according to claim 1, wherein the catalytic metal is supported of platinum group elements.
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