JP6701581B2 - 酸素吸放出材 - Google Patents
酸素吸放出材 Download PDFInfo
- Publication number
- JP6701581B2 JP6701581B2 JP2018036269A JP2018036269A JP6701581B2 JP 6701581 B2 JP6701581 B2 JP 6701581B2 JP 2018036269 A JP2018036269 A JP 2018036269A JP 2018036269 A JP2018036269 A JP 2018036269A JP 6701581 B2 JP6701581 B2 JP 6701581B2
- Authority
- JP
- Japan
- Prior art keywords
- oxygen storage
- ceria
- release material
- oxygen
- composite oxide
- 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.)
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- 229910052760 oxygen Inorganic materials 0.000 title claims description 120
- 239000001301 oxygen Substances 0.000 title claims description 120
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims description 112
- 239000000463 material Substances 0.000 title claims description 71
- 239000011148 porous material Substances 0.000 claims description 109
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 54
- 239000002131 composite material Substances 0.000 claims description 50
- 239000007789 gas Substances 0.000 claims description 30
- 239000003054 catalyst Substances 0.000 claims description 23
- 229910052684 Cerium Inorganic materials 0.000 claims description 21
- 238000002441 X-ray diffraction Methods 0.000 claims description 19
- 229910052726 zirconium Inorganic materials 0.000 claims description 17
- 230000001186 cumulative effect Effects 0.000 claims description 14
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 11
- 229910052753 mercury Inorganic materials 0.000 claims description 11
- 229910052727 yttrium Inorganic materials 0.000 claims description 11
- 239000000654 additive Substances 0.000 claims description 9
- 230000000996 additive effect Effects 0.000 claims description 9
- 229910052747 lanthanoid Inorganic materials 0.000 claims description 9
- 150000002602 lanthanoids Chemical class 0.000 claims description 9
- 238000002459 porosimetry Methods 0.000 claims description 8
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 7
- 229910052779 Neodymium Inorganic materials 0.000 claims description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims description 3
- 238000000746 purification Methods 0.000 claims description 3
- 239000000243 solution Substances 0.000 description 48
- 239000002994 raw material Substances 0.000 description 25
- 229910052799 carbon Inorganic materials 0.000 description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 17
- 239000000843 powder Substances 0.000 description 16
- 239000000126 substance Substances 0.000 description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 15
- 150000002736 metal compounds Chemical class 0.000 description 14
- 239000012298 atmosphere Substances 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 11
- 238000005259 measurement Methods 0.000 description 10
- 150000002926 oxygen Chemical class 0.000 description 8
- 238000001694 spray drying Methods 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 7
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 7
- 229910002091 carbon monoxide Inorganic materials 0.000 description 7
- 239000006185 dispersion Substances 0.000 description 6
- 239000008188 pellet Substances 0.000 description 6
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 238000010304 firing Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 4
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 4
- 229910017493 Nd 2 O 3 Inorganic materials 0.000 description 4
- 229920002873 Polyethylenimine Polymers 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- HKVFISRIUUGTIB-UHFFFAOYSA-O azanium;cerium;nitrate Chemical compound [NH4+].[Ce].[O-][N+]([O-])=O HKVFISRIUUGTIB-UHFFFAOYSA-O 0.000 description 3
- VZJJZMXEQNFTLL-UHFFFAOYSA-N chloro hypochlorite;zirconium;octahydrate Chemical compound O.O.O.O.O.O.O.O.[Zr].ClOCl VZJJZMXEQNFTLL-UHFFFAOYSA-N 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 239000000446 fuel Substances 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000001747 exhibiting effect Effects 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000009461 vacuum packaging Methods 0.000 description 2
- 239000011800 void material Substances 0.000 description 2
- 229920006310 Asahi-Kasei Polymers 0.000 description 1
- DCKZTSFDSXADDE-UHFFFAOYSA-N O.O.O.O.O.O.O.[Pr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O Chemical compound O.O.O.O.O.O.O.[Pr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O DCKZTSFDSXADDE-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- XMPZTFVPEKAKFH-UHFFFAOYSA-P ceric ammonium nitrate Chemical compound [NH4+].[NH4+].[Ce+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O XMPZTFVPEKAKFH-UHFFFAOYSA-P 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000010436 fluorite Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000004043 responsiveness Effects 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- VXNYVYJABGOSBX-UHFFFAOYSA-N rhodium(3+);trinitrate Chemical compound [Rh+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VXNYVYJABGOSBX-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- IINACGXCEZNYTF-UHFFFAOYSA-K trichloroyttrium;hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Cl-].[Y+3] IINACGXCEZNYTF-UHFFFAOYSA-K 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
- -1 zirconium oxynitrate dihydrate Chemical class 0.000 description 1
Classifications
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- 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
- B01D53/9445—Simultaneously removing carbon monoxide, hydrocarbons or nitrogen oxides making use of three-way catalysts [TWC] or four-way-catalysts [FWC]
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- B01J21/066—Zirconium or hafnium; Oxides or hydroxides thereof
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- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
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- F01N3/0828—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by using absorbents or adsorbents characterised by the absorbed or adsorbed substances
- F01N3/0864—Oxygen
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- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
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- F01N3/18—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 methods of operation; Control
- F01N3/20—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 methods of operation; Control specially adapted for catalytic conversion ; Methods of operation or control of catalytic converters
- F01N3/2006—Periodically heating or cooling catalytic reactors, e.g. at cold starting or overheating
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Description
先ず、硝酸アンモニウムセリウム(和光純薬工業株式会社製、試薬特級)39.06g及びオキシ硝酸ジルコニウム2水和物(和光純薬工業株式会社製、和光一級)21.05gをイオン交換水250gに溶解して原料溶液Aを調製した。また、平均分子量が10000のポリエチレンイミン(和光純薬工業株式会社製)0.1gをイオン交換水270gに溶解し、さらに、エチレンジアミン(和光純薬工業株式会社製、和光特級)をスポイトで14滴加えて原料溶液Bを調製した。このとき、原料溶液Aと原料溶液Bとを2mlずつ混合した溶液のpHが2.6となるように、エチレンジアミンを原料溶液Bに少しずつ加えた。
先ず、硝酸アンモニウムセリウム(和光純薬工業株式会社製、試薬特級)35.08g及びオキシ塩化ジルコニウム8水和物(和光純薬工業株式会社製、和光特級)24.21gをイオン交換水420gに溶解して原料溶液Aを調製した。また、平均分子量が10000のポリエチレンイミン(和光純薬工業株式会社製)0.1gをイオン交換水470gに溶解し、さらに、エチレンジアミン(和光純薬工業株式会社製、和光特級)約20mlを添加して原料溶液Bを調製した。このとき、原料溶液Aと原料溶液Bとを2mlずつ混合した溶液のpHは8.75であった。
カーボン分散水溶液を添加しなかった以外は実施例2と同様にして乾燥粉末を得た。この乾燥粉末を110℃で乾燥し、さらに、大気中、400℃で3時間加熱した後、実施例1と同様にして還元焼成及び大気中での焼成を行い、セリア−ジルコニア複合酸化物多孔体(酸素吸放出材)を得た。この酸素吸放出材中のCeとZrのモル比は、仕込みモル比でCe:Zr=46:54であった。
先ず、硝酸アンモニウムセリウム(和光純薬工業株式会社製、試薬特級)87.72g及びオキシ塩化ジルコニウム8水和物(和光純薬工業株式会社製、和光特級)60.53gをイオン交換水1100gに溶解して原料溶液Aを調製した。また、平均分子量が10000のポリエチレンイミン(和光純薬工業株式会社製)0.25gをイオン交換水120gに溶解し、さらに、エチレンジアミン(和光純薬工業株式会社製、和光特級)約29mlを添加して原料溶液Bを調製した。このとき、原料溶液Aと原料溶液Bとを2mlずつ混合した溶液のpHは2.1であった。
カーボン分散水溶液を添加しなかった以外は比較例1と同様にして乾燥粉末を得た。この乾燥粉末を110℃で乾燥し、さらに、大気中、400℃で3時間加熱した後、実施例1と同様にして還元焼成及び大気中での焼成を行い、セリア−ジルコニア複合酸化物多孔体(酸素吸放出材)を得た。この酸素吸放出材中のCeとZrのモル比は、仕込みモル比でCe:Zr=46:54であった。
先ず、硝酸アンモニウムセリウム(和光純薬工業株式会社製、試薬特級)83.68g、オキシ塩化ジルコニウム8水和物(和光純薬工業株式会社製、和光特級)52.74g、硝酸プラセオジム7水和物(三津和化学薬品株式会社製、特級)6.38g及び塩化イットリウム6水和物(三津和化学薬品株式会社製)6.71gをイオン交換水1000gに溶解して原料溶液Aを調製した。また、平均分子量が10000のポリエチレンイミン(和光純薬工業株式会社製)0.25gをイオン交換水1200gに溶解し、さらに、エチレンジアミン(和光純薬工業株式会社製、和光特級)60gを添加して原料溶液Bを調製した。このとき、原料溶液Aと原料溶液Bとを2mlずつ混合した溶液のpHは8.4であった。
実施例4と同様にして調製した金属化合物のナノコロイド溶液400mlにイオン交換水400mlを添加して体積基準で2倍に希釈したナノコロイド溶液を用いた以外は実施例1と同様にして噴霧乾燥(スプレードライ)を行い、乾燥粉末を得た。この乾燥粉末に、実施例4と同様にして、水洗、ろ過による回収、乾燥、加熱、還元焼成、大気流通下での焼成を施して、プラセオジムとイットリウムとを含有する4元系セリア−ジルコニア複合酸化物多孔体(酸素吸放出材)を得た。この酸素吸放出材中のCeとZrとPrとYのモル比は、仕込みモル比でCe:Zr:Pr:Y=42.18:47.13:4.26:6.43であり、Ce/Zr=0.895かつ(Ce+Pr+Y)/Zr=1.122であり、(Ce+Pr+Y/2)/(Zr+Y/2)=0.986であった。
実施例及び比較例で得られた酸素吸放出材をそれぞれ真空包装袋(旭化成パックス株式会社製「KN−201」)に約3g入れ、卓上真空包装機(株式会社TOSEI製「V−380GF」)を用いて15秒間脱気して封入した。この酸素吸放出材を冷間等方圧プレス機(日機装株式会社製)を用いて1000kg/cm2の圧力で圧粉した。得られた圧粉体を破砕して0.5〜2mm径に整粒し、測定用試料を作製した。水銀パラメータとして接触角:130degrees、表面張力:485mN/m、密度:13.5335g/mlを用いて、水銀ポロシメーター(カンタクローム株式会社製「PoreMaster60GT」)により、前記測定用試料(約0.3g)の対数微分細孔容積分布を求めた。その結果を図1及び図2に示す。
実施例及び比較例で得られた各酸素吸放出材のX線回折パターンを、試料水平型多目的X線回折装置(株式会社リガク製「Ultima IV」)を用い、CuKαをX線源として、管電圧:40kV及び電流:40mAの条件で測定した。なお、測定範囲が2θ≒12〜17deg又は13〜16degの場合には、〔条件1〕スキャンスピード:1deg/min及びサンプリング幅:0.01degに設定して測定し、測定範囲が2θ≒10〜65degの場合には、〔条件2〕スキャンスピード:10deg/min及びサンプリング幅:0.05degに設定して測定した。図3及び図4には、〔条件1〕で測定した2θ≒12〜17deg又は13〜16degにおけるX線回折パターンを示す。また、図5及び図6には、〔条件2〕で測定した2θ≒27〜32degにおけるX線回折パターンを示す。図3及び図4に示した2θ=14〜15degの範囲内にあるピークは、規則相(パイロクロア相、κ相)に由来するピークであり、図5及び図6に示した2θ=29〜30degの範囲内にあるピークは、最強線ピークである。
Al2O3−ZrO2−La2O3−Y2O3−Nd2O3複合酸化物担体(Al2O3:ZrO2:La2O3:Y2O3:Nd2O3=30質量%:60質量%:4質量%:4質量%:2質量%)に10質量%の硝酸ロジウム溶液を希釈して含浸させ、大気中、500℃で焼成してRh担持Al2O3−ZrO2−La2O3−Y2O3−Nd2O3複合酸化物(Rh担持量:0.2質量%)を得た。このRh担持Al2O3−ZrO2−La2O3−Y2O3−Nd2O3複合酸化物と実施例及び比較例で得られた各酸素吸放出材とを質量比1:1で乳鉢を用いて粉体混合し、得られた混合物を圧粉成形した後、得られた成形体を破砕・分級して粒径が0.5〜1mmのペレット触媒を作製した。
各ペレット触媒0.5gを反応管に充填し、固定床流通反応装置(株式会社ベスト測器製)にセットした。このペレット触媒に、測定温度400℃又は600℃、ガス流量10L/minの条件で、リーンガス(O2:1%、残部:N2)を3分間供給した後、窒素ガスを1分間供給し、さらに、リッチガス(CO:2%、残部:N2)を3分間供給し、リッチガス供給時の触媒出ガス中のCO2濃度を測定した。その結果、温度600℃で前記リッチガスを3分間供給した場合には、実施例1〜3のいずれのペレット触媒においても、3分間経過後のCO2濃度はほぼゼロであり、積算CO2量はほぼ理論値となった。このことからCeO2の酸素利用効率が高いことが確認された。
Claims (7)
- パイロクロア相及びκ相のうちの少なくとも一方の規則相を有し、
水銀圧入法により測定される中心細孔直径が70nm〜1μmであり、
前記中心細孔直径の0.5倍〜2倍の範囲内の細孔直径を有する細孔の積算細孔容積が水銀圧入法により測定される10nm〜10μmの範囲内の細孔直径を有する細孔の積算細孔容積の40%以上である、
セリア−ジルコニア複合酸化物多孔体からなることを特徴とする酸素吸放出材。 - CuKαを用いたX線回折測定により得られる前記セリア−ジルコニア複合酸化物多孔体のX線回折パターンにおいて、2θ=14〜15degの範囲内にある前記規則相に由来するピークの強度Iordと2θ=29〜30degの範囲内にある最強線ピークの強度Imaxとの比(Iord/Imax)が0.03以上であることを特徴とする請求項1に記載の酸素吸放出材。
- 前記セリア−ジルコニア複合酸化物多孔体中のCeとZrの含有モル比がCe:Zr=40:60〜60:40であることを特徴とする請求項1又は2に記載の酸素吸放出材。
- 前記セリア−ジルコニア複合酸化物多孔体が、Ce以外のランタノイド及びYからなる群から選択される少なくとも1種の添加元素を更に含有するものであることを特徴とする請求項1〜3のうちのいずれか一項に記載の酸素吸放出材。
- 前記添加元素がLa、Pr、Nd及びYからなる群から選択される少なくとも1種であることを特徴とする請求項4に記載の酸素吸放出材。
- 前記セリア−ジルコニア複合酸化物多孔体中のCeとZrと前記添加元素の含有モル比が、0.667≦Ce/Zr≦1.5、かつ、0.667≦(Ce+M)/Zr≦1.5〔式中、Mは添加元素を表す〕であることを特徴とする請求項4又は5に記載の酸素吸放出材。
- 請求項1〜6のうちのいずれか一項に記載の酸素吸放出材を含有することを特徴とする排ガス浄化用触媒。
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