JP2021159868A - 柱状ハニカム構造体及びその製造方法 - Google Patents
柱状ハニカム構造体及びその製造方法 Download PDFInfo
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- JP2021159868A JP2021159868A JP2020064972A JP2020064972A JP2021159868A JP 2021159868 A JP2021159868 A JP 2021159868A JP 2020064972 A JP2020064972 A JP 2020064972A JP 2020064972 A JP2020064972 A JP 2020064972A JP 2021159868 A JP2021159868 A JP 2021159868A
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- sealing portion
- honeycomb structure
- mass
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- columnar honeycomb
- Prior art date
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Images
Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/02—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust
- F01N3/021—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters
- F01N3/022—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters characterised by specially adapted filtering structure, e.g. honeycomb, mesh or fibrous
- F01N3/0222—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters characterised by specially adapted filtering structure, e.g. honeycomb, mesh or fibrous the structure being monolithic, e.g. honeycombs
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
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- B01D46/2403—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies characterised by the physical shape or structure of the filtering element
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- B01D46/2425—Honeycomb filters characterized by parameters related to the physical properties of the honeycomb structure material
- B01D46/244—Honeycomb filters characterized by parameters related to the physical properties of the honeycomb structure material of the plugs
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Abstract
【解決手段】外周側壁と、外周側壁の内周側に配置され、第一底面から第二底面まで延び、第一底面が開口して第二底面に平均空隙率が4%以下の目封止部を有する複数の第1セルと、外周側壁の内周側に配置され、第一底面から第二底面まで延び、第一底面に平均空隙率が4%以下の目封止部を有し、第二底面が開口する複数の第2セルとを備え、複数の第1セルと複数の第2セルは隔壁を挟んで交互に隣接配置されている柱状ハニカム構造体。
【選択図】図2
Description
外周側壁と、外周側壁の内周側に配置され、第一底面から第二底面まで延び、第一底面が開口して第二底面に平均空隙率が4%以下の目封止部を有する複数の第1セルと、外周側壁の内周側に配置され、第一底面から第二底面まで延び、第一底面に平均空隙率が4%以下の目封止部を有し、第二底面が開口する複数の第2セルとを備え、複数の第1セルと複数の第2セルは隔壁を挟んで交互に隣接配置されている柱状ハニカム構造体。
[2]
第一底面及び第二底面の目封止部の平均気孔率は共に、65%〜75%である[1]に記載の柱状ハニカム構造体。
[3]
外周側壁と、外周側壁の内周側に配置され、第一底面から第二底面まで延び、第一底面が開口して第二底面に目封止部を有する複数の第1セルと、外周側壁の内周側に配置され、第一底面から第二底面まで延び、第一底面に目封止部を有し、第二底面が開口する複数の第2セルとを備え、複数の第1セルと複数の第2セルは隔壁を挟んで交互に隣接配置されている柱状ハニカム構造体の製造方法であって、
それぞれの目封止部は、第1セル及び第2セルの目封止部を形成すべき開口部に目封止部形成用スラリーを充填し、その後、充填された当該スラリーを乾燥及び焼成する方法で形成されることを含み、
当該目封止部形成用スラリーは、セラミックス原料100質量部に対して、増粘剤を0.1〜0.5質量部、バインダーを0.2〜1.0質量部、造孔材を7〜15質量部、水を30〜50質量部含有する、
柱状ハニカム構造体の製造方法。
[4]
前記目封止部形成用スラリーは、セラミックス原料100質量部に対して、増粘剤を0.2〜0.4質量部、バインダーを0.2〜0.5質量部、造孔材を7〜15質量部、水を35〜40質量部含有する[3]に記載の柱状ハニカム構造体の製造方法。
[5]
前記目封止部形成用スラリーは、ブルックフィールド形単一回転式B型粘度計を用いて、JIS R1652:2003の粘度測定方法により25℃、1.04sec-1のせん断速度で測定した粘度が、250〜350dPa・秒である[3]又は[4]に記載の柱状ハニカム構造体の製造方法。
[6]
造孔材が発泡樹脂である[3]〜[5]の何れか一項に記載の柱状ハニカム構造体の製造方法。
[7]
造孔材は、レーザー回折・散乱法により求めた体積基準の累積粒度分布におけるD80が55μm超、D90が70μm超の粉末である[3]〜[6]の何れか一項に記載の柱状ハニカム構造体の製造方法。
図1及び図2には、ウォールフロー型の自動車用排ガスフィルタ及び/又は触媒担体として適用可能な柱状ハニカム構造体(100)の模式的な斜視図及び断面図がそれぞれ例示されている。この柱状ハニカム構造体(100)は、外周側壁(102)と、外周側壁(102)の内周側に配置され、第一底面(104)から第二底面(106)まで延び、第一底面(104)が開口して第二底面(106)に目封止部(109)を有する複数の第1セル(108)と、外周側壁(102)の内周側に配置され、第一底面(104)から第二底面(106)まで延び、第一底面(104)に目封止部(109)を有し、第二底面(106)が開口する複数の第2セル(110)とを備える。この柱状ハニカム構造体(100)においては、第1セル(108)及び第2セル(110)が隔壁(112)を挟んで交互に隣接配置されている。
・目封止部の形成されていない隔壁部の試験片を採取し、当該試験片の気孔率P1(隔壁部の気孔率)を測定する。
・目封止部を含む隔壁部の試験片を採取し、当該試験片の気孔率P(隔壁部+目封止部の気孔率)を測定する。
・目封止部を含む隔壁部の試験片において、隔壁部の気孔を含む体積V1を測定する。
・目封止部を含む隔壁部の試験片において、目封止部の気孔を含む体積V2を測定する。
目封止部の気孔率をP2とすると、P、P1、P2、V1及びV2は式(1)の関係を満たす。
P=P1×V1/(V1+V2)+P2×V2/(V1+V2) ・・・(1)
従って、P2は式(2)により求めることができる。
P2=P×(V1+V2)/V2−P1×V1/V2 ・・・(2)
目封止部における気孔率P2を各底面について任意の20箇所測定し、その平均値を各底面における目封止部の平均気孔率とする。
なお、目封止部を含む隔壁部の試験片において、隔壁部の気孔を含む体積V1の体積割合をv1、目封止部の気孔を含む体積V2の体積割合をv2とすると、P2は式(3)により求めてもよい。
P2=P×(v1+v2)/v2−P1×v1/v2 ・・・(3)
目封止部を有する柱状ハニカム構造体は、目封止部の形成方法を除いて公知の製造方法によって製造可能であるが以下に例示的に説明する。まず、セラミックス原料、分散媒、造孔材及びバインダーを含有する原料組成物を混練して坏土を形成した後、坏土を押出成形することにより所望の柱状ハニカム構造体に成形する。原料組成物中には分散剤等の添加剤を必要に応じて配合することができる。押出成形に際しては、所望の全体形状、セル形状、隔壁厚み、セル密度等を有する口金を用いることができる。
コージェライト化原料100質量部に、造孔材を3.5質量部、分散媒を65質量部、有機バインダーを6質量部、分散剤を1.0質量部、それぞれ添加し、混合、混練して坏土を調製した。コージェライト化原料としては、アルミナ、水酸化アルミニウム、カオリン、タルク、及びシリカを使用した。分散媒としては水を使用し、造孔材としては例えば、グラファイト等のカーボン、小麦粉、澱粉、フェノール樹脂、ポリメタクリル酸メチル等のアクリル樹脂、ポリエチレン、又はポリエチレンテレフタレート等の有機造孔材を挙げることができる。有機バインダーとしては例えば、ヒドロキシプロピルメチルセルロース、メチルセルロース、ヒドロキシエチルセルロース、カルボキシメチルセルロース、ポリビニルアルコール等を使用し、分散剤としては例えば、エチレングリコール、デキストリン、脂肪酸石鹸、ポリアルコール、ラウリン酸カリウム石鹸等を好適に用いることができる。
全体形状:直径117mm×高さ122mmの円柱状
セルの流路方向に垂直な断面におけるセル形状:正方形
セル密度(単位断面積当たりのセルの数):300セル/平方インチ
隔壁厚み:203μm(口金の仕様に基づく公称値)
表1に記載の組成をもつ実施例及び比較例の各目封止部形成用スラリーを調合した。バインダーとしてはメチルセルロース、ヒドロキシエチルメチルセルロースを使用した。増粘剤としてはポリエチレンオキシドを使用した。分散剤としてはポリアルコールを使用した。造孔材としてはアクリル樹脂を使用した。
先述した「スキージ方式」を用いて、第1セル及び第2セルが交互に隣接配置するように目封止部形成用スラリーを両底面に充填した。その後、大気雰囲気下で100〜230℃×100秒以下の条件で乾燥を行った。次いで、大気雰囲気下で約200℃で加熱脱脂し、更に大気雰囲気下で、1410〜1450℃の温度で、3〜10時間焼成することにより、目封止部を有する柱状ハニカム構造体を得た。
焼成後の各柱状ハニカム構造体について、キーエンス社製形状解析レーザー顕微鏡VK X250/260を用いて、目封止部の平均深さ及び平均空隙率を先述した手順で測定した。また、焼成後の各柱状ハニカム構造体について、ポロシメータ(Micromeritics社製型式Auto PoreIV)を用いて、先述した方法により目封止部の平均気孔率を測定した。結果を表1に示す。
エロージョン特性を以下の手順で評価した。得られた焼成後の各柱状ハニカム構造体を缶体にキャニング(収納)して、キャニングされた柱状ハニカム構造体をガスバーナ試験機に配置した。次に、ガスバーナ試験機によりSiC製の砥粒を柱状ハニカム構造体の一方の底面に衝突させた。砥粒を衝突させる条件としては、以下の通りである。
投入砥粒量:30g
柱状ハニカム構造体に流入させるガスの温度:700℃
柱状ハニカム構造体に流入させるガスの流量:10Nm3/分
試験時間:30分とし、その間砥粒を少しずつ投入した。
エロージョン量は、産業用CTを用いて、砥粒を衝突させた底面における全セルの目封止エロージョン深さを測定し、平均値をエロージョン量とした。各セルの目封止エロージョン深さはCT観測断面図から実際に砥粒で目封止部が削れた最大深さ(底面からのセルの延びる方向への距離)を測定値とした。結果を表1に示す。比較例1では、エロージョン量は2.5mmであったことに対して、比較例2では、目封止部分が完全に貫通することが観察された。一方、比較例3では、エロージョン量は2.5mmであった。実施例1、実施例2、実施例3では、エロージョン量は1.0mmに抑制されていることを確認できた。
巻き締め試験によりキャニング模擬試験を実施した。各柱状ハニカム構造体の外周側壁にマットを巻き、その上に厚さ1mm程度の金属板(SUS304)巻いた。この状態で、柱状ハニカム構造体を巻き締め試験機に設置して、金属板の外周にワイヤーを巻き、圧力を上げながらワイヤーを徐々に締め上げていき、目封止部剥がれの発生有無を確認した。比較例1、比較例2、比較例3、実施例1、実施例2、実施例3共に、1.1MPaまでの圧力において目封止部剥がれは発生しないことを確認した。
上記の試験結果から分かる通り、比較例1はエロージョンの防止効果が十分ではない。比較例1に対して比較例2は、目封止部形成用スラリー中の造孔材の含有量を減らすことで、目封止部の平均気孔率を低下させた。しかしながら、逆に平均空隙率が大きくなってしまい、エロージョンに対する特性が向上しなかった。比較例1の目封止部を断面観察すると、内部に空隙が多く観察された。
102 外周側壁
104 第一底面
106 第二底面
108 第一セル
109 目封止部
110 第二セル
112 隔壁
120 チャック
121 フィルム
122 スキージ
124 目封止部形成用スラリー
125 セル
126 孔
Claims (7)
- 外周側壁と、外周側壁の内周側に配置され、第一底面から第二底面まで延び、第一底面が開口して第二底面に平均空隙率が4%以下の目封止部を有する複数の第1セルと、外周側壁の内周側に配置され、第一底面から第二底面まで延び、第一底面に平均空隙率が4%以下の目封止部を有し、第二底面が開口する複数の第2セルとを備え、複数の第1セルと複数の第2セルは隔壁を挟んで交互に隣接配置されている柱状ハニカム構造体。
- 第一底面及び第二底面の目封止部の平均気孔率は共に、65%〜75%である請求項1に記載の柱状ハニカム構造体。
- 外周側壁と、外周側壁の内周側に配置され、第一底面から第二底面まで延び、第一底面が開口して第二底面に目封止部を有する複数の第1セルと、外周側壁の内周側に配置され、第一底面から第二底面まで延び、第一底面に目封止部を有し、第二底面が開口する複数の第2セルとを備え、複数の第1セルと複数の第2セルは隔壁を挟んで交互に隣接配置されている柱状ハニカム構造体の製造方法であって、
それぞれの目封止部は、第1セル及び第2セルの目封止部を形成すべき開口部に目封止部形成用スラリーを充填し、その後、充填された当該スラリーを乾燥及び焼成する方法で形成されることを含み、
当該目封止部形成用スラリーは、セラミックス原料100質量部に対して、増粘剤を0.1〜0.5質量部、バインダーを0.2〜1.0質量部、造孔材を7〜15質量部、水を30〜50質量部含有する、
柱状ハニカム構造体の製造方法。 - 前記目封止部形成用スラリーは、セラミックス原料100質量部に対して、増粘剤を0.2〜0.4質量部、バインダーを0.2〜0.5質量部、造孔材を7〜15質量部、水を35〜40質量部含有する請求項3に記載の柱状ハニカム構造体の製造方法。
- 前記目封止部形成用スラリーは、ブルックフィールド形単一回転式B型粘度計を用いて、JIS R1652:2003の粘度測定方法により25℃、1.04sec-1のせん断速度で測定した粘度が、250〜350dPa・秒である請求項3又は4に記載の柱状ハニカム構造体の製造方法。
- 造孔材が発泡樹脂である請求項3〜5の何れか一項に記載の柱状ハニカム構造体の製造方法。
- 造孔材は、レーザー回折・散乱法により求めた体積基準の累積粒度分布におけるD80が55μm超、D90が70μm超の粉末である請求項3〜6の何れか一項に記載の柱状ハニカム構造体の製造方法。
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