JP5814374B2 - シリコアルミノホスフェート粒子、ハニカム構造体及びその製造方法並びに排ガス浄化装置 - Google Patents
シリコアルミノホスフェート粒子、ハニカム構造体及びその製造方法並びに排ガス浄化装置 Download PDFInfo
- Publication number
- JP5814374B2 JP5814374B2 JP2013528898A JP2013528898A JP5814374B2 JP 5814374 B2 JP5814374 B2 JP 5814374B2 JP 2013528898 A JP2013528898 A JP 2013528898A JP 2013528898 A JP2013528898 A JP 2013528898A JP 5814374 B2 JP5814374 B2 JP 5814374B2
- Authority
- JP
- Japan
- Prior art keywords
- honeycomb structure
- honeycomb
- silicoaluminophosphate particles
- surface area
- silicoaluminophosphate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 40
- 239000007789 gas Substances 0.000 claims description 35
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 33
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- 238000000034 method Methods 0.000 claims description 17
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- 239000000463 material Substances 0.000 claims description 13
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- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 claims description 6
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- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 3
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Images
Classifications
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- 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
- F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
- F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
- F01N3/24—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by constructional aspects of converting apparatus
- F01N3/28—Construction of catalytic reactors
- F01N3/2803—Construction of catalytic reactors characterised by structure, by material or by manufacturing of catalyst support
-
- 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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/82—Phosphates
- B01J29/84—Aluminophosphates containing other elements, e.g. metals, boron
- B01J29/85—Silicoaluminophosphates (SAPO compounds)
-
- 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
- B01D53/9404—Removing only nitrogen compounds
- B01D53/9409—Nitrogen oxides
- B01D53/9413—Processes characterised by a specific catalyst
- B01D53/9418—Processes characterised by a specific catalyst for removing nitrogen oxides by selective catalytic reduction [SCR] using a reducing agent in a lean exhaust gas
-
- B01J35/56—
-
- B01J35/60—
-
- B01J35/615—
-
- 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
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B37/00—Compounds having molecular sieve properties but not having base-exchange properties
- C01B37/06—Aluminophosphates containing other elements, e.g. metals, boron
- C01B37/08—Silicoaluminophosphates (SAPO compounds), e.g. CoSAPO
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/54—Phosphates, e.g. APO or SAPO compounds
-
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- C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/02—Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
- C04B2237/10—Glass interlayers, e.g. frit or flux
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
- C04B2237/32—Ceramic
- C04B2237/34—Oxidic
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
- C04B2237/70—Forming laminates or joined articles comprising layers of a specific, unusual thickness
- C04B2237/708—Forming laminates or joined articles comprising layers of a specific, unusual thickness of one or more of the interlayers
Description
水中に、濃度が85質量%のリン酸水溶液9.8部、濃度が95質量%の水酸化アルミニウム水溶液7.0部、固形分が30質量%のシリカゾル5.5部及び構造規定剤としてのモルホリン11.3部を順次添加して、撹拌し、前駆体ゲルを得た。次に、前駆体ゲルをオートクレーブ(200ml)に封入した後、回転速度10rpmで回転させながら、昇温速度5℃/分で200℃まで昇温して、24時間保持し、シリコアルミノホスフェート粒子を作製した。
シリコンドリフトエネルギー分散型X線分析装置XFlash5030(Bruker社製)を用いて、シリコアルミノホスフェート粒子のAl及びPの物質量の和に対するSiの物質量の比を測定した。
ICPS−8100(島津製作所社製)を用いて、ICP発光分析することにより、シリコアルミノホスフェート粒子の銅イオンによる交換量を測定した。
レーザー回折式粒度分布測定装置MAS5001(マルバーン社製)を用いて、シリコアルミノホスフェート粒子の平均一次粒径を測定した。
自動比表面積/細孔分布測定装置トライスター3000(島津製作所社製)を用いて、相対圧P/P0に対する吸着量V[cm3(STP)・g−1]のプロット、即ち、窒素吸脱着等温線を作成し、BET多点法及びt−プロット法を用いて、シリコアルミノホスフェート粒子の比表面積及び外表面積を求めた。具体的には、比表面積は、相対圧P/P0に対するP/V(P0−P)[g・cm3(STP)−1]のプロット、即ち、BETプロットから求め、外表面積は、吸着層の厚さt[nm]に対するP/V(P0−P)[g・cm3(STP)−1]のプロット、即ち、t−プロットから求めた。
実施例及び比較例のシリコアルミノホスフェート粒子3000部、ベーマイト1190部、平均繊維径が6μm、平均繊維長が100μmのアルミナ繊維720部、メチルセルロース290部、オレイン酸310部及びイオン交換水1820部を混合混練して、原料ペーストを作製した。
ハニカムユニットにクラックが発生しているかどうかを目視で評価した。なお、クラックが発生している場合を×、クラックが発生していない場合を○として、判定した。
ハニカムユニットから、ダイヤモンドカッターを用いて、直径が25.4mm、長さが76.2mmの円柱状の試料を切り出した。
(NOxの流入量−NOxの流出量)/(NOxの流入量)×100
で表されるNOxの浄化率[%]を算出した。
11、11’、11’’ ハニカムユニット
11a 貫通孔
11b 隔壁
12 外周コート層
13 接着層
20 保持シール材
30 金属容器
100 排ガス浄化装置
Claims (16)
- Al及びPの物質量の和に対するSiの物質量の比が0.16以上0.33以下であり、 比表面積が250m2/g以上450m2/g以下であり、 外表面積が10m2/g以上35m2/g以下であることを特徴とするシリコアルミノホスフェート粒子。
- 比表面積が300m2/g以上440m2/g以下であることを特徴とする請求項1に記載のシリコアルミノホスフェート粒子。
- 比表面積が320m2/g以上400m2/g以下であることを特徴とする請求項2に記載のシリコアルミノホスフェート粒子。
- 外表面積が15m2/g以上30m2/g以下であることを特徴とする請求項1乃至3のいずれか一項に記載のシリコアルミノホスフェート粒子。
- 外表面積が20m2/g以上30m2/g以下であることを特徴とする請求項4に記載のシリコアルミノホスフェート粒子。
- 銅イオン及び/又は鉄イオンによりイオン交換されていることを特徴とする請求項1乃至5のいずれか一項に記載のシリコアルミノホスフェート粒子。
- 複数の貫通孔が隔壁を隔てて長手方向に並設されているハニカムユニットを有するハニカム構造体であって、 前記ハニカムユニットは、原料ペーストの焼成物からなり、 前記原料ペーストは、請求項1乃至6のいずれか一項に記載のシリコアルミノホスフェート粒子及び無機バインダを含むことを特徴とするハニカム構造体。
- 前記ハニカムユニットは、見掛けの体積当たりの前記シリコアルミノホスフェート粒子の含有量が230g/L以上360g/L以下であり、 前記見掛けの体積は、空隙の体積を含む外周の体積であることを特徴とする請求項7に記載のハニカム構造体。
- 前記無機バインダは、アルミナゾル、シリカゾル、チタニアゾル、水ガラス、セピオライト、アタパルジャイト及びベーマイトからなる群より選択される一種以上に含まれる固形分であることを特徴とする請求項7又は8に記載のハニカム構造体。
- 前記原料ペーストは、無機繊維、鱗片状物質、テトラポット状物質及び三次元針状物質からなる群より選択される一種以上をさらに含むことを特徴とする請求項7乃至9のいずれか一項に記載のハニカム構造体。
- 前記無機繊維は、アルミナ、シリカ、炭化ケイ素、シリカアルミナ、ガラス、チタン酸カリウム及びホウ酸アルミニウムからなる群より選択される一種以上であり、 前記鱗片状物質は、ガラス、白雲母、アルミナ及びシリカからなる群より選択される一種以上であり、 前記テトラポット状物質は、酸化亜鉛であり、 前記三次元針状物質は、アルミナ、シリカ、炭化ケイ素、シリカアルミナ、ガラス、チタン酸カリウム、ホウ酸アルミニウム及びベーマイトからなる群より選択される一種以上であることを特徴とする請求項10に記載のハニカム構造体。
- 複数の前記ハニカムユニットを有することを特徴とする請求項7乃至11のいずれか一項に記載のハニカム構造体。
- 空間速度が80000/hとなるように200℃の模擬ガスを当該ハニカム構造体に流した場合のNOxの浄化率が85%以上であり、 前記空間速度は、当該ハニカム構造体の見掛けの体積[m3]に対する前記模擬ガスの流量[m3/h]の比であり、 前記模擬ガスは、一酸化窒素の濃度が350ppmであり、アンモニアの濃度が350ppmであり、酸素の濃度が10%であり、水の濃度が5%であり、二酸化炭素の濃度が5%であり、窒素バランスであることを特徴とする請求項7乃至12のいずれか一項に記載のハニカム構造体。
- コージェライトを含み、複数の貫通孔が隔壁を隔てて長手方向に並設されているハニカムユニットを有し、 請求項1乃至6のいずれか一項に記載のシリコアルミノホスフェート粒子が前記隔壁に担持されていることを特徴とするハニカム構造体。
- 複数の貫通孔が隔壁を隔てて長手方向に並設されているハニカムユニットを有するハニカム構造体を製造する方法であって、 請求項1乃至6のいずれか一項に記載のシリコアルミノホスフェート粒子及び無機バインダを含む原料ペーストを押出成形する工程と、 該押出成形された原料ペーストを焼成して前記ハニカムユニットを作製する工程を有することを特徴とするハニカム構造体の製造方法。
- 請求項7乃至14のいずれか一項に記載のハニカム構造体の両端面を除く外周面に保持シール材が配置されている状態で、金属容器に収容されていることを特徴とする排ガス浄化装置。
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